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EUPT – SRM13April/May 2018
EU Proficiency Test on the Analysis of Pesticides Residues
Requiring Single Residue Methods
in Soybean Flour
Chemisches und Veterinäruntersuchungsamt
Stuttgart
Final Report
EU Reference Laboratories for Residues of Pesticides Single Residue MethodsEURL-SRM
EU PROFICIENCY TESTEUPT-SRM13, 2018
Residues of PesticidesRequiring
Single Residue Methods
Test Item: Soybean Flour
Final Report Part One: Resutls Evaluation (excl. Phosphine)
Michelangelo AnastassiadesPat Schreiter
Anja BarthHubert Zipper
approved by Michelangelo Anastassiades released on 31 October, 2018
The EURL-SRM is accredited by the DAkkS according to EN ISO/IEC 17043. The accreditation is valid for the proficiency testing programs listed in the certificate.
Publication of parts of this EUPT-SRM13 final report by individuals or organizations shall always refer to the original document that can be found under: http://www.eurl-pesticides.eu/library/docs/srm/EUPT_SRM13_FinalReport.pdf
Picture on the book cover: Tharakorn Arunothai, www.shutterstock.com, 219828004
Organisers
Michelangelo Anastassiades
Head of EURL-SRM (Single Residue Methods)CVUA StuttgartDepartment of Residues and ContaminantsSchaflandstrasse 3/2D-70736 Fellbach
Phone: +49-711-3426-1124Fax: +49-711-588176E-Mail: [email protected]
Advisory Group:
Amadeo Fernández-Alba EURL-FV, University of Almería (UAL), ES
Miguel Gamón EURL-FV, Laboratorio Agroalimentario Generalitat Valenciana (LAGV), ES
Mette Erecius Poulsen EURL-CF, National Food Institute (DTU), Søborg, DK
Ralf Lippold EURL-AO, CVUA Freiburg, DE
Philippe Gros Service Commun des Laboratoires (SCL) / Laboratoire de Montpellier, FR
Magnus Jezussek Bavarian Health and Food Safety Authority (LGL), Erlangen, DE
André de Kok Netherlands Food and Consumer Product Safety Authority (NVWA), Wageningen, NL
Sonja Masselter Austrian Agency for Health and Food Safety (AGES), Innsbruck, AT
Finbarr O’Regan Pesticide Control Laboratory (PCL), Department of Agriculture, Food and the Marine, IE
Tuija Pihlström National Food Agency (Livsmedelsverket), Uppsala, SE
Patrizia Pelosi National Institute of Health (ISS), Roma, IT
Carmelo Rodríguez University of Almería (UAL), ES
Quality Control Group:
Antonio Valverde University of Almería, ES
Paula Medina European Food Safety Authority (EFSA)
Organising Team:
EURL for Pesticides Requiring Single Residue Methods hosted by CVUA Stuttgart
Pat Schreiter, Senior Food Chemist
Anja Barth, Chemical Technician
Hubert Zipper, Senior Food Chemist
Carmen Wauschkuhn, Senior Food Chemist
Eric Eichhorn, Food Chemist
Nadine Kotte, Food Chemist
Giovanna Cerchia, Chemical Technician
Dorothea Mack, Chemical Technician
Sigrid Schüler, Chemical Technician
Sahra Söhnholz, Chemical Technician
Cristin Wildgrube, Chemical Technician
EURL for Pesticides in Cereals and Feedingstuff, National Food Institute, Technical University of DenmarkJens-Ole Frimann, Software Programmer
EUPT-Coordinator:
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FOREWORD
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FOREWORD
Regulation 882/2004/EC [1] defines the general tasks and duties of the EU Reference Laboratories (EURLs) for Food, Feed and Animal Health1 including the organisation of comparative tests (proficiency tests = PTs). These PTs are carried out on an annual basis and aim to improve the quality, accuracy and comparability of the analytical results generated by EU Member States within the framework of the EU coordinated control programs as well as national monitoring programs. By participating in PTs laboratories can assess and at the same time demonstrate their analytical performance. The attention to details paid by laboratories during PT-analysis, together with the need to identify errors and to take corrective actions in cases of underper-formance, typically lead to improvements in the quality of analytical results.
According to Article 28 of Regulation 396/2005/EC on maximum residue levels of pesticides in or on food and feed of plant and animal origin [2], all laboratories analysing for pesticide residues within the frame-work of official controls shall participate in the European Union Comparative Proficiency Tests (EUPTs) for pesticide residues. Each Official Laboratory (OfL) must participate in EUPTs concerning the commodities included in its area of competence.
Since 2006 the EURL for pesticide residues requiring the use of Single Residue Methods, EURL-SRM, has an-nually conducted one scheduled Proficiency Test. Five of those thirteen EUPT-SRMs were conducted in col-laboration with the EURL for pesticide residues in Fruits and Vegetables (EURL-FV) with apple juice (EUPT-SRM1, 2006), carrot homogenate (EUPT-SRM3, 2008), apple purée (EUPT-SRM5, 2010), potato homogenate (EUPT-SRM8, 2013) and spinach homogenate (EUPT-SRM11, 2016) as test items. Further four EUPT-SRMs were conducted in collaboration with the EURL for pesticide residues in Cereals and Feeding Stuff (EURL-CF) with wheat flour (EUPT-C1/SRM2, 2007), oat flour (EUPT-C3/SRM4, 2009), rice flour (EUPT-C5/SRM6, 2011) and maize flour (EUPT-C9/SRM10, 2015) as test items. The remaining four EUPT-SRMs were organized by the EURL-SRM unilaterally, two of them used commodities from plant origin with low fett content : milled dry lentils (EUPT-SRM7, 2012) and soybean slour (EUPT-SRM12, 2017). The EUPT-SRM9 was the only EUPT-SRM so far, in which a commodity of animal origin (cow’s milk) was used. The current PT using flour of whole soybeans was the first one using a commodity with low water and high oil content (approx. 22 %).
Participation in the respective EUPTs is mandatory for all NRLs for pesticides requiring Single Residue Meth- ods (NRL-SRMs) and for all OfLs analysing pesticide residues within the framework of national or EU control programs in commodities represented by the respective EUPT test item. Laboratories in EU Member States analysing pesticide residues within the frame of import controls according to Reg. 669/2009/EC are also considered as performing official controls in the sense of Reg. 882/2005/EC and 396/2005/EC and are thus also obliged to take part in EUPTs. OfLs from EFTA countries (Iceland, Norway and Switzerland) contributing data to the EU-coordinated community control programs, EU laboratories analysing official organic samples within the frame of Reg. 889/2008/EC, as well as OfLs from EU-acceding or -candidate countries (FYROM, Montenegro, Serbia and Turkey) are also invited to take part. A limited number of laboratories from third countries are allowed to take part in this exercise, too. However, only results submitted by labs from EU and EFTA countries are included in the calculation of the assigned values. In order to have sufficient results for evaluation of phosphine, a few private laboratories were exceptionally invided to participate in the present PT. These private labs were also allowed to report results also for any other pesticides in the target pesti-cides list, but those results was neither used to establish the assigned values nor be presented in this report.
1 Formerly known as Community Reference Laboratories (CRLs)
Based on information about the commodity scope and labs’ NRL-status a tentative list of EU-labs consid-ered as being obliged to participate in the EUPTs is published at the beginning of each year. The pesticide scope is not taken into account in these lists. NRLs and OfLs listed as being obliged to participate in an EUPT exercise in a given year but deciding not to take part, are always asked to state the reason(s) for their non-participation. The same applies to laboratories originally registering to participate in a certain EUPT but finally not submitting results.
DG-SANTE has full access to all data of EUPTs including the lab-code/lab-name key. The same applies to all NRLs as far as laboratories belonging to their own country networks are concerned. Results for this EUPT or a series of EUPTs, evaluated on a country by country basis, may be further presented to the European Commission Standing Committee on Plants, Animals, Food and Feed (PAFF)-Section Pesticides Residues ,or during the EURL-Workshops.
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CONTENT
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CONTENT
FOREWORD ................................................................................................................................................................................v
INTRODUCTION ..................................................................................................................................................................ix
1. TEST ITEM AND BLANk MATERIAL ..............................................................................................1
1.1 Selection of PT-Commodity and of Compounds for the Target Pesticides List ................1
1.2 Small Scale Preliminary Investigation on Analytes during Homogenisation ...................1
1.3 Preparation and Bottling of the Blank Material ......................................................................................2
1.4 Preparation and Bottling of the Blank Material ......................................................................................2
1.5 Packaging and Delivery of PT Materials to Participants ..................................................................3
1.6 Analytical Methods ........................................................................................................................................................3
1.7 Homogeneity Test ..........................................................................................................................................................4
1.8 Storage Stability Test ..................................................................................................................................................5
1.9 Transport Stability Test .............................................................................................................................................7
1.10 Organisational Aspects ..............................................................................................................................................8
2. EVALUATION RULES ........................................................................................................................................11
2.1 False Positives and Negatives ..............................................................................................................................11
2.2 Assigned Values (xpt) and Calculation of the Respective Uncertainties (u(xpt)) .............11
2.3 Fixed Target Standard Deviation using FFP-Approach (FFP-σpt) .............................................. 12
2.4 z-Scores ............................................................................................................................................................................... 12
2.5 Laboratory Classification ...................................................................................................................................... 12
3. PARTICIPATION ................................................................................................................................................. 15
4. RESULTS ......................................................................................................................................................................... 19
4.1 Overview of Results ................................................................................................................................................... 19
4.2 Analysis of Blank Material .....................................................................................................................................30
4.3 Assigned Values and Target Standard Deviations .............................................................................30
4.4 Assessment of Laboratory Performance ................................................................................................... 32
5. ACkNOWLEDGEMENTS ............................................................................................................................. 53
6. REFERENCES ............................................................................................................................................................. 53
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7. APPENDICES .......................................................................................................................................................... A-1
Appendix 1 ................. List of Laboratories Registered to Participate in the EUPT-SRM13 A-1
Appendix 2 ................. Shipment Evaluation .........................................................................................................A-5
Appendix 3 ................. Data of Homogeneity Test ...........................................................................................A-6
Appendix 4 ................. Data of Stability Test ........................................................................................................A-8
Appendix 5 ................. Histograms and kernel Density Estimates of z-score Distributions A-11
Appendix 6 ................. Graphic Presentation of z-Scores ........................................................................... A-13
Appendix 7 ................. Possible Reasons Reported for Poor Performance ..................................A-26
Appendix 8 ................. General EUPT Protocol (8th Ed.) ...............................................................................A-39
Appendix 9 ................. Specific Protocol of EUPT-SRM13 ...........................................................................A-47
Appendix 10 ............... Calendar and Target Pesticides List of EUPT-SRM13 ...............................A-51
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INTRODUCTION
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european CommIssIon – eu-proFICIenCy test on resIdues oF pestICIdes
requIrIng sIngle resIdue methods
test Item: soybean Flour
EUPT-SRM13, 2018
INTRODUCTION
On 23 Januar, 2018 all relevant National Reference Laboratories (NRLs) of the 28 EU-Member States (MS), as well as all relevant EU-Official Laboratories (OfLs) whose contact details were available to the organis-ers (EURL-SRM) were invited to participate in the 13th European Commission‘s Proficiency Test Requiring Single Residue Methods (EUPT-SRM13). The EUPT-SRM13-Website contained links to the Announcement/Invitation Letter, the Calendar, as well as to the Target Pesticides List (see Appendix 11). The Target Pesti-cides List contained 25 compounds potentially being present in the test item. 9 of them were compulsory compounds and were thus considered in the Category A/B classification (based on scope). The compounds of the Target Pesticides List were selected based on a number of criteria and following consultation with the EUPT-Scientific Committee. For each compound a residue definition valid for the PT and the minimum required reporting level (MRRL) were stipulated. Links to the latest version of the “General Protocol” (see Appendix 9) containing information common to all EUPTs and to the “Specific Protocol” (see Appendix 10) valid for the current PT were also provided. The laboratories were able to register on-line from 27 February to 16 March, 2018.
Based on its commodity scope (fruit and vegetables, feed, and commodities with high fett content) and its NRL-status (NRL-SRMs) a tentative status of a laboratory to be obliged to participate in the EUPT-SRM13 was stored in the DataPool, so that every participant can see it during the registration. To ensure that all relevant official laboratories were informed about this EUPT, the NRLs were asked to forward the invitation to all relevant official laboratories within their countries. It was made clear that the status of the labora-tories was only tentative, and the real obligation to participate was based on Reg. 396/2005/EC and Reg. 882/2004/EC. Obliged labs that did not intend to participate were asked to provide an explanation.
In total 114 participating labs from EU and EFTA countries, 2 OfLs from an EU candidate country and 8 labo-ratories from third countries submitted results of at least one compound. Except 5 laboratories from EU and EFTA countries all other registered laboratories have submitted results.
The proficiency test EUPT-SRM13 was conducted using organic soybean flour originated from Austria and organic soybeans from EU countries. The test item was prepared by spiking the soybeans with 15 com-pounds highly concentrated dissolved in standard solutions, milling, filtering and mixing with the organic soybean flour. More details are given in Chapter 1 “Test Materials and Blank Material”.
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1. TEST ITEM / Selection of PT-Commodity and of Compounds for the Target Pesticides List
1. TEST ITEM AND BLANk MATERIAL
1.1 Selection of PT-Commodity and of Compounds for the Target Pesticides List
In agreement with the EUPT- Scientific Committee soybean flour was chosen as commodity for the EUPT-SRM13.
The compounds to be included in the Target Pesticides List (Appendix 11) were selected by the organiser and the EUPT-Scientific Committee (Advisory Group and Quality Control Group) taking the following points into account: 1) the present and upcoming scope of the EU-coordinated control program; 2) a pesticide pri-ority list, ranking the pesticides according to their risk potential; 3) the relevance of pesticides to the specific commodity; 4) the overall scope and capability of the OfLs as assessed in previous PTs or surveys.
For the production of the test item and the blank material, one batch of organic soybean flour were pur-chased from a food processing company and checked for the absence of the analytes on the Target Pesti-cides List. None of the target pesticides was detected except phosphonic acid at 0.04 mg/kg and bromide ion at 1.3 mg/kg. More soybean flour of the same batch was purchased. This batch was finally used for the preparation of the blank material and for the preparation of the test item by spiking with 15 compounds (see Section , p. 3).
The minimum required reporting levels (MRRLs) were set at 0.003 mg/kg for haloxyfop; at 0.005 mg/kg for carbofuran and phosphine; at 0.01 mg/kg for 2,4-D, chlormequate-Cl, cyromazine, fluazifop, mepiquat-Cl, 2,4-DB, chlorate, fenoxaprop, perchlorate and quizalofop; at 0.02 mg/kg for ethephon, bentazone, diquat, glufosinate, MPP, N-acetyl glufosinate, and N-acetyl glyphosate, and paraquat; at 0.03 mg/kg for glypho-sate; at 0.05 mg/kg for AMPA and phosphonic acid and at 2.0 mg/kg for bromide ion.
1.2 Small Scale Preliminary Investigation on the Behavior of the Analytes during Ho-mogenisation
In order to estimate the loss of spiked analytes during the preparation of the test material, several prelimi- nary spiking experiments were performed at a small scale.
1.2.1 Recovery Study
A recovery study (n = 5) for all analytes listed on the Target Pesticides List was conducted. Recover-ies were found to be (65 %) 93 – 117 %.
1.2.2 Investigation on Homogeneity and on the Behavior of Analytes during Test Material Prepa-ration using soybean flour in comparison with soybeans
The experiments consisted of spiking one portion (100 g) of soybean flour and one portion (100 g) of soy- beans with a representative selection of pesticides listed on the Target Pesticides List as a mixture. The spiking was conducted in a metallic container. The spiked soybeans were dried and afterwards ground in a Thermomix® adding dried ice. The test materials both prepared with soybean flour and soybean were homogenized with blank soybean flour 1:10. These small scale test materials were analyzed for the yield of all spiked analytes using QuEChERS method and QuPPe PO method (n = 7).
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Results showed that with the test material prepared with soybean flour acceptable yields (86 % – 109 %) could be obtained. However the results for homogeniety were not satisfying (RSD 22 % – 30 %)
Test material which was prepared with soybeans homogenized with soybean flour, obtained yields showed acceptable results for some analytes but also very low yields (37 % – 38 %) especially in case of highly polar pesticides. Here results for homogeniety were satisfying (RSD 4 % – 15 %).
It was concluded that another test is needed where the spiking of soybeans is conducted in a plastic con- tainer.
1.2.3 Investigation on the Behavior of Analytes during Test Material Preparation using Soybeans
1 kg soybeans was spiked with a representative selection of pesticides listed on the Target Pesticides List as a mixture. The spiking was conducted in a plastic container. The spiked soybeans were dried and after- wards ground in a Thermomix adding dried ice. This small scale test material was analyzed for the yield of all spiked analytes using QuEChERS method and QuPPe PO method (n = 4).
Yields obtained with the test material which was prepared in a plastic container showed satisfying results ((65 %) 90 – 119 %) and also satisfying homogeneity (RSD 2 % – 12 % (26 %)).
Using soybeans for spiking (in a plastic container) followed by dilution and homogenization with soybean flour was considered appropriate for the preparation of the test item.
1.3 Preparation and Bottling of the Blank Material
Treatment of blank soybeans was conducted to obtain the same conditions present in the sample material.
2.5 kg soybeans were spiked with a solvent mixture which corresponded both in volume and composition to the spiking solution (see below). These soybeans were dried and ground in a Thermomix® adding dry ice. Approximately 50 kg organic soybean flour from 5 packages, each containing 20 kg, were pooled in a large metal vessel, where it was layered with the processed blank soybeans. The blank material was mixed with a drum-hoop mixer over 10 h. Approximately 200 g portions of the well-mixed blank soybean flour were weighed out into labelled and leak-proof screw-capped polyethylene plastic bottles, sealed and stored in a freezer at about −20 °C until distribution to participants.
1.4 Preparation and Bottling of the Blank Material
The test item was prepared in the same way as the blank material described above, but instead of adding pure solvent 150 ml of an equally composed mixture containing the target analytes was added. The mixture contained 14 different compounds and was prepared as described in Table 1-1 (p. 3)..
These two processed soybean flours and approximately 50 kg organic soybean flour from 5 packages were layered, and pooled in a large metal vessel. The spiked material was mixed with a drum-hoop mixer over 10 h. Approximately 200 g portions of the well-mixed spiked soybean flour were weighed out into labelled and leak-proof screw-capped polyethylene plastic bottles, sealed and stored in a freezer at about −20 °C until distribution to participants.
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1. TEST ITEM and Blank Material / Investigation on Analysis of Carbofuran and Bifenazate
1.5 Packaging and Delivery of PT Materials to Participants
Three days prior to the sample delivery, one bottle of test item and one of blank material, both deep frozen, as well as were packed into thermo-insulated polystyrene boxes, filled with four cooling elements and stored at −20 °C for three days, so that at the day of delivery the cooling elements were deep frozen. Once the parcel was picked up by DHL, the recipient received an e-mail from the shipping company entailing the individual online tracking number.
Among the 122 packages sent to laboratories in EU and EFTA countries, 106 (87 %) reached the participating labs within 24 hours and 11 packages within 48 hours. Due to the remote location of certain laboratories and holidays in certain countires, the remaining 5 packages took 3 days to arrive. The delivery to countries outside the EU and EFTA zones was accomplished within 48 hours in 3 cases, within 72 hours in 2 cases, within 4 days in 1 case, and more than 7 days in 4 cases. The latter was, however, due to delays at the customs. Overall, the EUPT-materials arrived at the laboratories very cold within two days. All material was accetped by the participants. Details on the shipment duration are shown in Appendix 2.
At this point organisers would like to appeal to the participants to follow their own parcels via the online tracking tool of the shipping company in order to maintain the ability to take the necessary measures in case of delays, e.g., contacting the customs to ask for an acceleration of the clearance procedure or to place the parcel in a cool place until clearance is granted. The participants are furthermore encouraged to con-tact the local office of the shipping company to ensure optimal delivery in case of opening time.
1.6 Analytical Methods
The analytical methods used by the organisers to check the homogeneity and storage-stability of the tar- get analytes contained in the test item as well as the absence of target analytes in the blank material are summarized in Table 1-2 (p. 4). For more details on the methods used, please refer to the EURL-SRM website: http://www.eurl-pesticides.eu (EURL-SRM-website Services Methods).
Table 1-1: Analytes spiked into 50 kg soybean flour for the preparation of the test material
Analytes dissolved in 50 ml H2O Theor. Conc. Analytes dissolved in 100 ml Aceton Theor. Conc.
Compound Amount [mg/kg] Compound Amount [mg/kg]
Bromide-K 1097.84 mg 14.742 1) 2,4-DB 10.238 mg 0.205
Cyromazine 5.64 mg 0.113
Glyphosate 50.27 mg 1.005
Mepiquat-Cl 6.8 mg 0.136
Perchlorate-Na 6.473 mg 0.105 2)
Diquat-dibromid hydrate 152.203 mg 1.549 3) Spiking using Stock Solution (1 mg/ml ACN) Theor. Conc.
Glufosinate-Al 11.098 mg 0.203 4) Compound Amount [mg/kg]
MPPA 8.826 mg 0.177 Haloxyfop (free acid) 0.8 ml 0.016
N-Acetyl-glyphosate 30 mg 0.600 Fluazifop (free acid) 2.6 ml 0.052
Phosphonic acid 103.064 mg 2.061 Quizalofop (free acid) 3.0 ml 0.060
1) as bromide ion; 2) as perchlorate; 3) as diquate dication; 4) as glufosinate
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1.7 Homogeneity Test
After filling the test item in the bottles, 10 bottles were randomly chosen for the homogeneity test and two analytical portions were taken from each for analysis. Both the order of sample preparation and the order of extract injection into the analytical instruments were random. Matrix-matched calibration using extract prepared from blank material or procedural calibration using blank material were applied for quantifica-tion. Analytical portions of 1 g for phosphine and 5 g for all other compounds were used.
Table 1-2: Analytical methods used by the organisers to check for the homogeneity and storage-stability of the pesticides present in the test item and to demonstrate the absence of other pesticides in the blank material.
Compound Extraction IS Determinative analysis Notes
2,4-DB Modified QuEChERS-method [3] involving: weighing of 5 g soybean flour into a sealable vessel, addition of 10 ml H2O, extraction with ACN (15 min), addition of partitioning salts (4 g MgSO4, 1 g NaCl, 1 g trisodium citrate dihydrate and 0.5 g disodium hydrogenci-trate sesquihydrate), 1 min shaking, centrifugation, addition of IS / ILISs to raw extract and direct determination by LC-MS/MS in the ESI (neg.) and ESI (pos) mode.
BNPU LC-MS/MS ESI (neg)
Fluazifop BNPU LC-MS/MS ESI (neg)
Haloxyfop BNPU / Haloxyfop D4 LC-MS/MS ESI (neg)
Quizalofop BNPU / Quizalofop D3 LC-MS/MS ESI (neg)
2,4-D* BNPU LC-MS/MS ESI (neg)
Bentazone* BNPU LC-MS/MS ESI (neg)
Carbofuran* Chlorpyrifos D10 LC-MS/MS ESI (pos)
Fenoxaprop* BNPU LC-MS/MS ESI (neg) –
Bromide ion QuPPe-PO method [5] involving: weighing of 5 g soybean flour into a sealable vessel, addition of ILISs, addition of methanol containing 1 % formic acid, shaking, centrifugation, Filtration, cleanup with C18 and pos-sibly dilution with MeOH containing 1 % formic acid. Determination by LC-MS/MS in the ESI (neg.) or ESI (pos.) mode.
– LC-MS/MS ESI (neg) QuPPe M1.3
Cyromazine Cyromazine D4 LC-MS/MS ESI (pos) QuPPe M4.2
Glufosinate Glufosinate D3 LC-MS/MS ESI (neg) QuPPe M1.3
Glyphosate Glyphosate 13C 15N LC-MS/MS ESI (neg) QuPPe M1.3
Mepiquat Mepiquat D3 LC-MS/MS ESI (pos) QuPPe M4.2
MPP MPP D3 LC-MS/MS ESI (neg) QuPPe M1.3
N-Acetyl-Glyphosate N-Acetyl-Glyphosate 13C2
15NLC-MS/MS ESI (neg) QuPPe M1.3
Perchlorate Perchlorate 18O4 LC-MS/MS ESI (neg) QuPPe M1.4
Phosphonic acid Phosphonic acid 18O3 LC-MS/MS ESI (neg) QuPPe M1.4
AMPA* AMPA 13C 15N LC-MS/MS ESI (neg) QuPPe M1.3
Chlorate* Chlorate 18O3 LC-MS/MS ESI (neg) QuPPe M1.4
Chlormequat* Chlormequat D4 LC-MS/MS ESI (pos) QuPPe M4.2
Ethephon* Ethephon D4 LC-MS/MS ESI (pos) QuPPe M4.2
N-Acetyl-Glufosinate* N-Acetyl-Glufosinate D3 LC-MS/MS ESI (neg) QuPPe M1.3
Paraquat* Paraquat D6 LC-MS/MS ESI (pos) QuPPe M4.1
Diquat QuPPe-PO method [5] involving: weighing of 5 g soybean flour into a sealable vessel, addition of ILIS, addition a 1:1 mixture of methanol+ aqueous HCl 0.1 M, shaking, centrifu-gation, Filtration, cleanup with C18 and determination by LC-MS/MS in the ESI (pos.) mode.
Diquat 13C2 LC-MS/MS ESI (pos) QuPPe M4.1
Phosphine xxxxxxxxxxxxxxxxxx H2S GC-MS EI (pos)
* : To check for absence in Blank Material
1. TEST ITEM and Blank Material / Storage Stability Test
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The statistical evaluation of the homogeneity test data was performed according to the International Har- monized Protocols published by IUPAC, ISO and AOAC [4, 6]. An overview of the statistical evaluations of the homogeneity test is shown in Table 1-3. The individual residue data of the homogeneity test is given in Appendix 3.
The acceptance criterion for the test item to be sufficiently homogeneous for the Proficiency Test was that ssam
2 is smaller than c with ssam being the between-bottle sampling standard deviation and c = F1 × σall
2 + F2 × san2, F1 and F2 being constants with values of 1.88 and 1.01, respectively, and applying
when duplicate samples are taken from 10 bottles. σall2 = 0.3 × FFP-RSD (25 %) × the analytical sampling
mean of the analyte, and san is the estimate of the analytical standard deviation.
As all target compounds passed the homogeneity test, the test item was considered to be sufficiently ho-mogenous and suitable for the EUPT-SRM13.
1.8 Storage Stability Test
In the Specific Protocol laboratories were recommended storing the samples in the freezer until analysis. The stability test samples were thus also stored under the same conditions. Shortly after the shipment of the samples to the participants, three of the spare test item bottles were chosen randomly and all analyti-cal portions necessary for all three stability tests were weighed into the vessels in which the analysis was
COMPULSORY COMPOUNDS
Brom
ide
ion
Cyro
maz
ine
Flua
zifo
p
free
aci
d
Gly
phos
ate
Hal
oxyf
op
free
aci
d
Mep
iqua
t-Cl
Analytical portion size [g] 5 5 5 5 5 5
Mean [mg/kg] 14.6 0.107 0.049 0.924 0.016 0.126
ssam2 2.34 × 10-1 6.76 × 10-6 2.73 × 10-6 4.58 × 10-4 4.34 × 10-8 2.82 × 10-5
c 3.30 × 100 1.62 × 10-4 2.89 × 10-5 1.27 × 10-2 3.27 × 10-6 2.15 × 10-4
Passed/Failed passed passed passed passed passed passed
Table 1-3: Statistical evaluation of homogeneity test data (n = 20), details please see Appendix 3.
OPTIONAL COMPOUNDS
2.4-
DB
fr
ee a
cid
Diq
uat
dica
tion
Glu
fosi
-nat
e
MPP
N-A
cety
l-G
lyph
osat
e
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
free
aci
d
Phos
phin
e (t
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Analytical portion size [g] 5 5 5 5 5 5 5 5 1 1
Mean [mg/kg] 0.177 1.46 0.197 0.175 0.759 0.103 1.99 0.058 0.168 0.068
ssam2 1.44 × 10-5 3.41 × 10-3 2.25 × 10-4 5.90 × 10-5 1.79 × 10-3 3.91 × 10-6 7.33 × 10-3 2.06 × 10-6 2.34 × 10-7 0 × 10-0
c 4.11 × 10-4 3.44 × 10-2 8.71 × 10-4 4.19 × 10-4 8.58 × 10-3 1.48 × 10-4 5.46 × 10-2 4.24 × 10-5 8.71 × 10-8 1.14 × 10-4
Passed/Failed passed passed passed passed passed passed passed passed passed passed
EUPT-SRM13 | 2018 (Soybean Flour)
6
to be conducted. The portions of stability tests 1 were extracted immediately and those of stability tests 2 and 3 were placed in the freezer at −20 °C until analysis as described in Section 1.6 (p. 3). The extracts of all stability tests corresponding to one method were stored in the freezer at −20 °C and measured iso-chronically (within the same sequence) at a day suitable for the laboratory.
Stability test 1 (extraction shortly after shipment): 03 May 2018 (analytes via QuPPe-Methods) 25 April 2018 (analytes via QuEChERS-Methods) 28 May 2018 (phosphine (PH3-Tube)) 20 June 2018 (phosphine (test item))
Stability test 2 (extraction five weeks or more after shipment): 22 May 2018 (analytes via QuPPe-Methods) 17 May 2018 (analytes via QuEChERS-Methods) 19 June 2018 (phosphine (PH3-Tube)) 19 July 2018 (phosphine (test item))
Stability test 3 (extraction at least four weeks after deadline for results submission): 18 June 2018 (analytes via QuPPe-Methods) 07 June 2018 (analytes via QuEChERS-Methods) 18 July 2018 (phosphine (PH3-Tube)) 24 Sept. 2018 (phosphine (test item))
A target compound is considered to be adequately stable if |yi − y| ≤ 0.3 × σpt, where yi is the mean value of the last period of the stability test, y is the mean value of the first period of the stability test and σpt the standard deviation used for proficiency assessment, typically 25 % of the assigned value. With the excep-tion of phosphine all other analytes contained in the test item showed a stability within the acceptable limits when stored under the recommended conditions (−18 °C) within a period exceeding the duration of the exercise by two weeks (Table 1-4, p. 7). For the compounds passing the test it is assumed that, if the recommended storage conditions were followed, the influence of sample storage on the results of these analytes was negligible at least throughout the duration of the EUPT.
In the case of phosphine (PH3-Tube) the determined concentration in day 3 was lower than that deter-mined in day 1 by 20.0 %. This decline was significantly higher than the tolerance of 8.725 % (= 0.3σpt us-ing FFP-RSD of 25 %). In case of phosphine (PT-Sample), compared with the concentration on day 1, the determined concentration in day 3 declined only 4.25 %. However, the determined concentration in day 2 deviated by 17.29 % that was higher than the tolerance of 0.3σpt.
This fluctuation of the results of the stability test and the broad standard diviation reflected the fact that the analytical method was not robust. The analytical results of phosphine is thus associated with a considerable uncertainty. The determined deviations are probably related more to spurious analytical errors rather than to degradation. The higher concentration in day 2 compared to day 1 also points towards this direction. As analysis of phosphine is an optional compound in the PT, no further measures concerning its stability were deemed necessary, but report will be issued separately for its evaluation.
The results of all analyses conducted within the framework of the stability test are shown in Table 1-4 and Appendix 4.
1. TEST ITEM and Blank Material / Transport Stability Test
7
TesT
ITem
1
Table 1-4: Results of storage stability test (storage at -18 ºC). Please see the text or Appendix 4 for the dates of analysis for each analytes.
COMPULSORY COMPOUNDS
Brom
ide
ion
Cyro
maz
ine
Flua
zifo
p
free
aci
d
Gly
phos
ate
Hal
oxyf
op
free
aci
d
Mep
iqua
t-Cl
Storage at −18 ºC (mean values in mg/kg)
Analysis 1 13.729 0.105 0.050 0.913 0.016 0.123
Analysis 2 14.054 0.105 0.050 0.964 0.016 0.128
Analysis 3 14.110 0.111 0.049 0.933 0.017 0.131
Deviation [mg/kg] ([%]) Analysis 3 vs. Analysis 1
0.381 (2.8 %)
0.006 (5.3 %)
0.001 (-1.7 %)
0.02 (2.2 %)
0.001 (7.1 %)
0.008 (6.2 %)
0.3 × σpt [mg/kg] 1.152 0.007 0.004 0.068 0.001 0.009
Passed/Failed passed passed passed passed passed passed
COMPULSORY COMPOUNDS
2.4-
DB
fr
ee a
cid
Diq
uat
dica
tion
Glu
fosi
-nat
e
MPP
N-A
cety
l-G
lyph
osat
e
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
free
aci
d
Phos
phin
e (t
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Storage at −18 ºC (mean values in mg/kg)
Analysis 1 0.177 1.423 0.186 0.170 0.734 0.101 1.922 0.058 0.180 0.063
Analysis 2 0.183 1.359 0.183 0.174 0.773 0.101 1.959 0.059 0.149 0.069
Analysis 3 0.165 1.422 0.186 0.165 0.742 0.108 1.939 0.058 0.188 0.080
Deviation [mg/kg] ([%]) Analysis 3 vs. Analysis 1
0.012 (-7.0 %)
0.001 (-0.1 %)
0 (0 %)
0.004 (-2.6 %)
0.008 (1.1 %)
0.007 (6.5 %)
0.016 (0.9 %)
0.001 (-1.2 %)
0.008 (4.25 %)
0.013 (20.0 %)
0.3 × σpt [mg/kg] 0.014 0.128 0.014 0.014 0.063 0.007 0.140 0.004 0.007 0.003
Passed/Failed passed passed passed passed passed passed passed passed passed failed
1.9 Transport Stability Test
With the exception of 7 laboratories with remote location or being on holiday and further 5 laboratories where the shipments were retarded due to customs clearance delays or remote location, all other 120 laboratories (91 %) received their test items within 48 hours. Among these 120 laboratories 106 received the parcels within one day. As no significantly negative influence of the long transport duration on the results from the 12 laboratories receiving the parcels more than 72 hours upon shipment was detected, the organisers decided not to conduct the transport stability test in the current PT.
EUPT-SRM13 | 2018 (Soybean Flour)
8
1.10 Organisational Aspects
1.10.1 Laboratory Status as Mandatory to Participation
Based on available information on NRL-status and commodity scope as recorded in the EURL-DataPool, the EU and EFTA OfLs and NRLs are designated as "mandatory to participate in the current PT" or "participation on voluntary basis". The available information on the pesticide scope covered by the laboratories was not considered due to concerns that might not be up-to-date and/or not applicable to the present commod-ity (soybean). The OfLs can provide the organisers and their NRLs their reasons and ask for changing their status. The NRLs were reminded of their responsibility for their network and to ensure that all obliged OfLs within their network were informed of this EUPT. All NRLs and OfLs were informed that the status of obli-gation was tentative and the real obligation for participation is deriving from Art. 28 of Reg. 396/2005/EC (for OfLs) and Art. 33 of Reg. 882/2004/EC (for NRL-SRMs). Following DG-SANTE instructions, obliged labs that were not intending to participate in the EUPT-SRM13 were instructed to provide explanations for their non-participation.
1.10.2 Announcement / Invitation and EUPT-SRM13-Website
Within the EURL-Web-Portal an EUPT-SRM13-Website was constructed with links to all documents relevant to this EUPT (i.e., Announcement/Invitation Letter, Calendar, Target Pesticides List, Specific Protocol and General EUPT Protocol). These documents were uploaded to the EURL-Web-Portal and the CIRCA BC.
The Announcement/Invitation Letter for the EUPT-SRM13 was published on the EUPT-SRM13-Website in January 2018 and was sent to all NRL-SRMs, all OfLs analysing pesticide residues in food and feeding stuff within the framework of official controls, all laboratories performing import controls according to Reg. 669/2009/EC, as far as they were tracked in the EURL-DataPool, as well as to EU laboratories analys-ing official organic samples within the frame of Reg. 889/2008/EC. The latter laboratories were considered eligible but not obliged to participate. It was indicated to the OfLs that their obligation to participate in EUPTs arises from Reg. 396/2005/EC, irrespective of the content of the tentative list of obliged laboratories. NRLs and OfLs from EFTA and EU-candidate countries were also invited if their contact data was available. A number of laboratories from third countries were also invited to take part in this exercise. The acceptance of their registration was decided, however, on a case by case basis, and the laboratories were informed in-dividually of the acceptance or rejection of their registration. Furthermore, in order to obtain sufficient data for statistical evaluation of phosphine, a few private laboratories were exceptionally invited to participate in the current PT. These private laboratories were allowed to submitted also results for other analytes. However, their results for other analytes were neither be included in the establischmen of the assigned values nor present in the final report.
1.10.3 Registration and Confidentiality
Like in the previous PT in 2017 (EUPT-SRM12) the participants were able to register for this EUPT via a web-site connected to the EURL-DataPool. All laboratories being obliged to participate in the current EUPT, re-gardless of whether they were intending to participate in this exercise or not, were requested to either register or to state their reasons for non-participation using the same website.
1. TEST ITEM and Blank Material / Organisational Aspects
9
TesT
ITem
1
Upon registration or change of registration status, the labs received an electronic confirmation about their participation or non-participation in the current PT. Three days before sample shipment, participating laboratories were provided via e-mail with a unique laboratory code as well as the login data to access the online Result-Submission-Website. This ensured confidentiality throughout the entire duration of the PT.
For further information on confidentiality please refer to the General EUPT Protocol (Appendix 9).
1.10.4 Distribution of the Test Items and the Blank Material
One bottle of test item (approx. 200 g), one bottle of blank material (approx. 200 g) were shipped on 23 April, 2018 to each participant in thermo-insulated polystyrene boxes with cooling pads. All the parcels hve been precooled at -20 °C for three days before shipment.
Two weeks prior to the shipment, detailed instructions on how to treat the test item and blank material upon receipt were provided to the participating laboratories in the Specific Protocol (Appendix 10).
1.10.5 Submission of Results and Additional Information
An online submission tool allowed participants to submit their results via the Internet. Using their individ-ual login data, all participants had access to the Result-Submission-Website from a week after the sample shipment until the result submission deadline (30 May 2018). Participants were asked not only to report their analytical results but also to state whether the compounds on the Target Pesticides List were part of their routine scope and to indicate their experience with the analysis of these compounds. In addition, laboratories had to provide details about the methods applied and to state their own reporting limits (RLs) for each target compound they had analysed. The participants had furthermore the possibility to make statements as regards the condition of the material received. This information could be submitted from the day of shipment onwards.
1.10.6 Actions following Results Submission and Distribution Preliminary Report
Where information on analytical methods or results was inconsistent, laboratories were contacted. Labo-ratories that had originally registered to participate in the current PT but finally did not submit any results, were asked to provide explanations. On 19 June, 2018, the preliminary report on the EUPT-SRM13 with the preliminary assigned values was released and sent to the participants. Laboratories having submitted false positive or negative results were asked to provide information on the methods used for analysing those compounds. In addition, participants were asked to investigate the reasons for results with | z-score | > 2 and to report them. In order to have the complete and correct data for the evaluation, a reminder was sent to the participants again to fill in all the data requested on the submission page for the methodological information.
In order to obtain feedback from the participants and to improve the service quality in the future, the proofreading version of this final report (part one: results evaluation) is accompanied by a survey on EUPT-SRM13. This survey contains 5 questions on the organisation (general, registration, information and instruc-tion provided, shipment/delivery, test item, blank material and results submission pages), on the relevance of the used matrix (soybean flour) to the routine work, on the assigned values of the analytes, as well as on the preliminary report and wishes as regards the commodities and/or analytes to be included in the upcoming two EUPT-SRMs. The survey evaluation and compilation of comments will be published soon.
2. EVALUATION RULES / False Positives and Negatives
11
Eva
luat
ion
Ru
lE
2
2. EVALUATION RULES
2.1 False Positives and Negatives
2.1.1 False Positives (FPs)
Any reported result with a concentration at or above the Minimum Required Reporting Level (MRRL) of an analyte in the Target Pesticides List which was (a) not detected by the organiser, even following repetitive analysis, and/or (b) not detected by the overwhelming majority (e.g. > 95 %) of the participants that ana-lysed for this compound, is treated as a false positive result. Results of an analyte absent in the test item but with a value lower than the MRRL are excluded by the organiser and not considered as false positives. No z-scores are calculated for false positive results.
2.1.2 False Negatives (FNs)
These are results of target analytes reported as “analysed” but without reporting numerical values, al-though they were used by the organiser to prepare the test item and were detected, at or above the MRRL, by the organiser and the overwhelming majority of the participating laboratories. In accordance with the General Protocol z-scores for false negatives are calculated using the MRRL as the result, or using the lab’s reporting-limit (RL), if this is lower. Any RLs that are higher than the MRRL are not taken into account. Fol-lowing the General Protocol, results reported as “< RL” without providing a numerical value are also judged as false negatives if the RL exceeds the MRRL.
2.2 Assigned Values (xpt) and Calculation of the Respective Uncertainties (u(xpt))
In accordance with EUPT-General Protocol (Appendix 8) the assigned values xpt of each pesticide in the PT is established using the mean value of robust statistics using Algorithms A (x*) [6] of all reported results from EU and EFTA countries. Results associated with obvious mistakes and gross errors may be excluded from the population for the establishment of the assigned values. The add-in “RobStat” provided by Royal Society of Chemistry was used to calculate the assigned values with the convergence criterion = 10-6.
The uncertainty of the assigned values of each analyte is calculated according to ISO 13528:2015 [6] using the following equation:
u(xpt) = 1.25 × [(s*)/ p ]
Where u(xpt) is the uncertainty of the assigned value in mg/kg, s* is the robust standard deviation estimate in mg/kg and p is the number of data points considered (= the number of results used to calculate the assigned value). The factor 1.25 is based on the standard deviation of the median, or the efficiency of the median as an estimate of the mean, in a large set of results drawn from a normal distribution.
The tolerance for the uncertainty of the assigned value of each pesticide is calculated as 0.3 × FFP-σpt, where FFP-σpt is the target standard deviation of the assigned value derived using a fixed standard deviation of 25 % (see Section 2.3). If u(xpt) < 0.3 × FFP-σpt, is met, then the uncertainty of the assigned value is consi-dered to be negligible and not needed to be considered in the interpretation of the proficiency test results.
EUPT-SRM13 | 2018 (Soybean Flour)
12
2.3 Fixed Target Standard Deviation using FFP-Approach (FFP-σpt)
Based on experience from previous EU Proficiency Tests on fruit and vegetables and cereals, the EUPT-Sci-entific Committee agreed to apply a fixed fit-for-purpose relative standard deviation (FFP-RSD) of 25 % for calculating the z-scores. The fixed target standard deviation using the fit-for-purpose approach (FFP-σpt), for each individual target analyte is calculated by multiplying the assigned value by the FFP-RSD of 25 %. In addition, the robust relative standard deviation of the assigned value (CV*) is calculated for informative purposes.
2.4 z-Scores
For each combination of laboratory and target analyte a z-score is calculated according to the following equation:
zi = (xi – xpt) / FFP-σpt
Where − xi is the result for the target analyte (i) as reported by the participant
(For results considered as false negatives, xi is set as equal to the respective minimum required reporting level (MRRL) or the laboratory reporting level (RL), if RL < MRRL.)
− xpt is the assigned value for the target analyte (i) − FFP-σpt is the standard deviation for proficiency assessment using the fit-for-purpose approach
(see above).
Any z-scores > 5 are set at 5 in calculations of combined z-scores (see 2.5.2).
The z-scores are classified as follows:
|z| ≤ 2 acceptable 2 < |z| < 3 questionable |z| ≥ 3 unacceptable
For results considered as false negatives, z-scores are calculated using the MRRL or the RL, if RL < MRRL. No z-scores are allocated to false positive results.
2.5 Laboratory Classification
2.5.1 Category A and B classification
Based on the scope of target analytes covered by the laboratories in this exercise, laboratories are subdi-vided into Categories (A and B) in accordance with the rules in the General Protocol (Appendix 8). To be classified into Category A a laboratory should
a) have analysed at least 90 % of the compulsory pesticides on the Target Pesticides List,b) have correctly reported concentration values for at least 90 % of the compulsory pesticides pre-
sent in the test item, c) not have reported any false positive results.
2. EVALUATION RULES / Laboratory Classification
13
Eva
luat
ion
Ru
lE
2
2.5.2 Combined z-Scores
For informative purposes and to allow comparison of the overall performance of the laboratories the Av-erage of the Absolute z-Scores (AAZ) is calculated for laboratories with 5 or more z-scores. Combined z-scores are, however, considered to be of lesser importance than the individual z-scores.
Average of the Absolute z-Scores (AAZ)
The AAZ is calculated using the following formula:
where “n” is the number of each laboratory’s z-scores that are considered in this formula. This includes z-scores assigned for false negative results. For the calculation, any z-score > 5 is set at 5.
AAZn
nz
AAZ ii∑
== 1
3. Participation
15
Part
iciP
atio
n
3
3. PARTICIPATION
121 laboratories from 37 countries (28 EU-Member States, 2 EFTA- countries, 1 EU-candidate country and 6 third countries) originally registered for participation in the EUPT-SRM13. An overview of the participating laboratories and countries is given in Table 3-1. A list of all individual laboratories that registered for this EUPT is presented in Appendix 1. Croatia was the only EU-country not represented by an NRL-SRM. Malta was represented by its proxy-NRL-SRM based in the United Kingdom.
Out of the 109 EU OfLs having registered for participation in the current PT five laboratories from Three co-nutries, among them the NRL-SRM in Italy, failed to submit any results and reported after the PT “technical problems/problems with instruments” or “target pesticides out of routien analytical scope” as the reason for no results submitted.
All 12 laboratories from non-EU countries submitted results (4 from EFTA countries, 2 from one EU-can-didate country and 6 from third countries). For the first time one OfL from Iceland has participated in an EUPT-SRM. The results submitted by the laboratories located in Serbia (EU candidate country) and by the 6 laboratories located in third countries were not taken into account when calculating the assigned values.
In total, 151 EU-OfLs, including NRL-SRMs, regardless of their commodity scope, as well as all EU-OfLs ana-lysing for pesticide residues in food and feed with high oil content and very low water content, were origi-nally considered as being obliged to participate in the present EUPT. These laboratories were invited to log in the registration page and register for their participation in the current PT or to provide an explanation for their non-participation.
30 obliged laboratories explained their non-participation with the fact that the matrix (soybeans) or the SRM13 target pesticides or both were out of their routine scope, partly due to a lack of required instru-ments. One obliged laboratory was not able to participate in because of the relocation of this laboratory. Excluding those 31 laboratories that provided sufficient explanations, the number of EU-laboratories con-sidered as being obliged decreased to 120. Out of the 92 obliged laboratories that have registered for this PT 88 laboratories finally submitted result. In addition, 17 OfLs registered for participation on voluntary basis, and 16 of them submitted results. Out of the 120 obliged OfLs 28 (23 %) did neither register for the PT nor provide any explanation for non-participation. These laboratories originated from 8 countries as fol-lows: HR (1×), FR (2×), DE (3×), IT (8×), PL (4×), RO (4×), ES (5×), and UK (1×).
In order to have sufficient results for evaluation of phosphine, eleven private laboratories worldwide were exceptionally invided to participate in the present PT. These private laboratories were also allowed to re-port results for any other pesticides in the target pesticides list if they wish. Participants from private labo-ratories will receive the certificate and the final report, however, their results, except those for phosphine, were not considered in the establishment of assigned values and their participation will not be shown in the final report.
EUPT-SRM13 | 2018 (Soybean Flour)
16
EU: NRLs and OfLs
Contracting Country 1)
Labs originally
considered as obliged (*based on
scope)
Labs providing sufficient expl.
for non-participation Finally considered as obliged
Registered for Participation
Submitted Results Obliged labs
non particip. w/o
giving expl.
Notes
During Registration All NRL- SRMs All NRL-
SRMs
AL/ BE/ NL 1 1 1 1
AT 1 1 1 1 1 1
BE 6 1 5 5 + [1] 1 5 + [1] 1
BE/ BG/ FR/ LU 1 1 1 1
BG 2 1 1 1 1 1 1
CY 2 1 1 1 1 1 1 HR has not yet established an NRL-SRM.
CZ 3 3 3 1 3 1
DE 25 5 20 17 + [3] 1 16 + [3] 1 3
DE/ MT 1 1 1 1
DK 2 1 1 1 1 1 1
EE 3 1 2 2 1 2 1
FI 2 2 2 2 2 2 FI has appointed two NRL-SRMs.
FR 7 7 5 + [3] 1 5 + [3] 1 2
GR 2 2 2 + [1] 2 2 + [1] 2
HR 5 1 4 3 3 1 GR has appointed two NRL-SRMs.
HU 4 4 4 + [1] 1 4 + [1] 1
IE 1 1 1 1 1 1
IT 23 5 18 10 1 9 0 8
IT/ MT 1 1 1 1
LT 1 1 1 + [1] 1 1 + [1] 1
LU 1 1 1 1 1 1 *MT-NRL-SRM represented by proxy by the UK-NRL-SRM; MT subcontracted routine analy-sis to an OfLs in DE and IT
LV 1 1 1 1 1 1
MT 0* 0* 0* 0* 0* *MT-NRL-SRM represented by proxy by the UK-NRL-SRM; MT subcontracted routine analy-sis to an OfLs in DE and IT
NL 2 2 2 1 2 1
PL 11 5 6 2 + [1] 1 2 + [1] 1 4
PO 1 1 1 + [1] 1 + [1]
PT 1 1 1 1 1 1
RO 7 2 5 1 1 4
SE 2 2 2 1 2 1
SI 3 1 2 2 1 2 1
SK 1 1 1 1 1 1
ES 24 7 17 12 + [4] 2 10 + [3] 2 5 ES has appointed two NRL-SRMs
ES/ MT 1 1 1 1
UK/MT 1 1 1 1 1 1 UK-NRL-SRM represents also MT
UK 2 2 1 + [1] 1 + [1] 1
EU-total 151 31 120 92 + [17] 28 88 + [16] 27 28
Table 3-1: Number of laboratories listed as being obliged to participate in the EUPT-SRM13, labs that registered to participate, and labs that finally submitted results (grouped by contracting country)
3. Participation
17
Part
iciP
atio
n
3
Table 3-1 (cont.): Number of laboratories listed as being obliged to participate in the EUPT-SRM13, labs that registered to partici-pate, and labs that finally submitted results (grouped by contracting country)
EFTA
Contracting Country 1)
Labs originally
considered as obliged (*based on
scope)
Labs providing sufficient expl.
for non-participation Finally considered as
obliged
Registered for Participation
Submitted Results Obliged labs
non particip. w/o
giving expl.
NotesPrior to
PTDuring the
PT All NRL- SRMs All NRL-
SRMs
NO [1] 1 [1] 1
CH [3] – [3] –
EU+EFTA Total 92 + [21] 28 88 + [20] 27
Third Countries / EU candidate country
BR 1 – 1 –
BY 1 – 1 –
CR 1 – 1 –
PE 1 – 1 –
RS 2 – 2 –
SG 1 – 1 –
TH 1 – 1 –
Third Countries / EU candidate country Total 8 8
Overall Sum 120 121 28 116 27
4. RESULTS / Overview of Results
19
Resu
lts
4
4. RESULTS
4.1 Overview of Results
An overview of the percentage of laboratories having targeted each of the analytes present in the Target Pesticides List is shown in Table 4-1.
Table 4-2 (p. 20) gives an overview of all results submitted by each laboratory. The individual numerical results reported by the laboratories are shown in Table 4-8 (p. 36) and Table 4-9 (p. 42) for compulsory and optional, respectively. Detailed information about the analytical methods used by the laboratories is shown on the web under “EUPT-SRM13 - Supplementary Information” accessible via the the link: http://www.eurl-pesticides.eu/library/docs/srm/EUPT-SRM13_Supplementary_Information.pdf.
Labs analysed for the compound
CompoundsPresent
in test item
EU 1)- and EFTA-Labs EU obliged Labs only
No. 2) % (based on n = 109 3)) No. 2) % (based on n = 120 4))
Com
puls
ory
Com
poun
ds
2,4-D No 88 81 % 73 61 %
Bromide ion Yes 62 57 % 47 39 %
Chlormequat-Cl No 88 81 % 72 60 %
Cyromazine Yes 79 72 % 63 53 %
Ethephon No 75 69 % 60 50 %
Fluazifop Yes 86 79 % 70 58 %
Glyphosate Yes 83 76 % 68 57 %
Haloxyfop Yes 81 74 % 67 56 %
Mepiquat-Cl Yes 86 79 % 71 59 %
Opt
iona
l Com
poun
ds
2,4-DB Yes 52 48 % 43 36 %
Bentazone No 73 67 % 60 50 %
Carbofuran No 77 71 % 62 52 %
Chlorate No 56 51 % 42 35 %
Diquat Yes 30 28 % 21 18 %
Fenoxaprop No 41 38 % 33 28 %
Glufosinate Yes 44 40 % 33 28 %
MPP Yes 25 23 % 17 14 %
N-Acetyl-Glufosinate No 23 21 % 17 14 %
AMPA No 56 51 % 43 36 %
N-Acetyl-Glyphosate Yes 23 21 % 18 15 %
Paraquat No 29 27 % 21 18 %
Perchlorate Yes 55 50 % 41 34 %
Phosphonic acid Yes 45 41 % 32 27 %
Quizalofop Yes 62 57 % 50 42 %
Phsophine (Test Item) Yes 11 10 % 5 4 %
Phosphine (PH3-Tube) Yes 11 10 % 5 4 %
1) Including official laboratories participating on voluntary basis2) Laboratories representing more than one country were counted only once.3) 109 is the number of participating OfLs from EU and EFTA countries (including NRLs and official laboratories participating on voluntary basis)
having registered for the present PT and submitted at least one result.4) 120 is the number of OfLs (including NRLs) from EU countries, which were finally considered as obliged to participate in the EUPT-SRM13 (taking
into account any explanations for non-participation).
Table 4-1: Percentage of EU and EFTA laboratories that have analysed for the compounds in the Target Pesticides List
EUPT-SRM13 | 2018 (Soybean Flour)
20
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
1 A ND V ND ND V V V V 8 / 5 V ND ND 1 A V ND ND ND 7 / 2 15 / 7
2 B ND V ND FN ND V V V FN 9 / 4 V ND ND ND 2 B V ND V ND ND FN V V 12 / 5 21 / 9
3 B ND V V V 4 / 3 V ND ND 3 B ND 4 / 1 8 / 4
4 x A ND V ND V ND V V V V 9 / 6 ND ND 4 x A V ND ND V V V V 9 / 5 18 / 11
5 x B ND ND ND V V V V 7 / 4 ND ND ND 5 x B V 4 / 1 11 / 5
6 A ND V ND V ND V V V V 9 / 6 ND ND ND 6 A V V V 6 / 3 15 / 9
7 x B ND V V V 4 / 3 V ND ND 7 x B ND 4 / 1 8 / 4
8 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 8 x A V V 6 / 3 15 / 9
10 A ND V ND V ND V V V V 9 / 6 ND ND ND 10 A ND V V V 7 / 3 16 / 9
11 A ND V ND V ND V V V V 9 / 6 V ND ND 11 A ND ND V FN FN V V 10 / 4 19 / 10
12 x A ND V ND V ND V V V V 9 / 6 V ND ND 12 x A ND ND V 6 / 2 15 / 8
13 x A ND V ND V ND V V V V 9 / 6 V ND ND 13 x A V ND V V ND ND V V V V 13 / 8 22 / 14
14 A ND V ND V ND V V V V 9 / 6 V ND ND ND 14 A V ND V ND ND V V V V V 14 / 8 23 / 14
15 A ND V ND V ND V V V V 9 / 6 ND ND ND 15 A V V ND ND V V V V 11 / 6 20 / 12
16 A ND V ND V ND V V V V 9 / 6 V ND ND ND 16 A ND V ND V V V V V 12 / 7 21 / 13
17 B ND ND V ND V V V 7 / 4 ND ND 17 B V ND V V V V V 9 / 6 16 / 10
19 x A ND V ND V ND V V V V 9 / 6 V ND ND 19 x A ND 4 / 1 13 / 7
20 x A ND V ND V ND V V V V 9 / 6 V ND ND 20 x A V 4 / 2 13 / 8
21 A ND V ND ND V V V V 8 / 5 ND ND 21 A V ND ND V ND 7 / 2 15 / 7
22 x A ND V ND V ND V V V V 9 / 6 V ND ND 22 x A V ND 5 / 2 14 / 8
23 B ND ND V V V V 6 / 4 V ND 23 B ND ND 4 / 1 10 / 5
24 x A ND ND V ND V V V V 8 / 5 V ND ND 24 x A 3 / 1 11 / 6
25 B ND V ND V V V V 7 / 5 ND ND 25 B 2 / 0 9 / 5
26 A ND V ND V ND V V V V 9 / 6 V ND ND ND 26 A V V V V 8 / 5 17 / 11
27 A ND V ND V ND V V V V 9 / 6 ND ND ND 27 A V ND V V ND ND ND V V V 13 / 6 22 / 12
28 B ND V 2 / 1 28 B 0 / 0 2 / 1
29 x A ND V ND V ND V V V V 9 / 6 ND ND 29 x A 2 / 0 11 / 6
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2: Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
4. RESULTS / Overview of Results
21
Resu
lts
4
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
1 A ND V ND ND V V V V 8 / 5 V ND ND 1 A V ND ND ND 7 / 2 15 / 7
2 B ND V ND FN ND V V V FN 9 / 4 V ND ND ND 2 B V ND V ND ND FN V V 12 / 5 21 / 9
3 B ND V V V 4 / 3 V ND ND 3 B ND 4 / 1 8 / 4
4 x A ND V ND V ND V V V V 9 / 6 ND ND 4 x A V ND ND V V V V 9 / 5 18 / 11
5 x B ND ND ND V V V V 7 / 4 ND ND ND 5 x B V 4 / 1 11 / 5
6 A ND V ND V ND V V V V 9 / 6 ND ND ND 6 A V V V 6 / 3 15 / 9
7 x B ND V V V 4 / 3 V ND ND 7 x B ND 4 / 1 8 / 4
8 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 8 x A V V 6 / 3 15 / 9
10 A ND V ND V ND V V V V 9 / 6 ND ND ND 10 A ND V V V 7 / 3 16 / 9
11 A ND V ND V ND V V V V 9 / 6 V ND ND 11 A ND ND V FN FN V V 10 / 4 19 / 10
12 x A ND V ND V ND V V V V 9 / 6 V ND ND 12 x A ND ND V 6 / 2 15 / 8
13 x A ND V ND V ND V V V V 9 / 6 V ND ND 13 x A V ND V V ND ND V V V V 13 / 8 22 / 14
14 A ND V ND V ND V V V V 9 / 6 V ND ND ND 14 A V ND V ND ND V V V V V 14 / 8 23 / 14
15 A ND V ND V ND V V V V 9 / 6 ND ND ND 15 A V V ND ND V V V V 11 / 6 20 / 12
16 A ND V ND V ND V V V V 9 / 6 V ND ND ND 16 A ND V ND V V V V V 12 / 7 21 / 13
17 B ND ND V ND V V V 7 / 4 ND ND 17 B V ND V V V V V 9 / 6 16 / 10
19 x A ND V ND V ND V V V V 9 / 6 V ND ND 19 x A ND 4 / 1 13 / 7
20 x A ND V ND V ND V V V V 9 / 6 V ND ND 20 x A V 4 / 2 13 / 8
21 A ND V ND ND V V V V 8 / 5 ND ND 21 A V ND ND V ND 7 / 2 15 / 7
22 x A ND V ND V ND V V V V 9 / 6 V ND ND 22 x A V ND 5 / 2 14 / 8
23 B ND ND V V V V 6 / 4 V ND 23 B ND ND 4 / 1 10 / 5
24 x A ND ND V ND V V V V 8 / 5 V ND ND 24 x A 3 / 1 11 / 6
25 B ND V ND V V V V 7 / 5 ND ND 25 B 2 / 0 9 / 5
26 A ND V ND V ND V V V V 9 / 6 V ND ND ND 26 A V V V V 8 / 5 17 / 11
27 A ND V ND V ND V V V V 9 / 6 ND ND ND 27 A V ND V V ND ND ND V V V 13 / 6 22 / 12
28 B ND V 2 / 1 28 B 0 / 0 2 / 1
29 x A ND V ND V ND V V V V 9 / 6 ND ND 29 x A 2 / 0 11 / 6
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
EUPT-SRM13 | 2018 (Soybean Flour)
22
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
30 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 30 x A V ND V V ND ND V ND V V V 15 / 8 24 / 14
31 A ND V ND V ND V V V V 9 / 6 ND ND ND 31 A V ND ND ND V V V 10 / 4 19 / 10
32 x A ND ND V ND V V V V 8 / 5 V ND ND ND 32 x A V ND ND ND V V V V V 13 / 7 21 / 12
33 A ND V ND V ND V V V V 9 / 6 V ND ND ND 33 A ND V ND V V V 10 / 5 19 / 11
34 A ND V ND V ND V V V V 9 / 6 V ND ND ND 34 A V ND V V ND ND V ND V V V V V 17 / 10 26 / 16
35 A ND ND V ND V V V V 8 / 5 V ND ND ND 35 A V V V ND ND V V V 12 / 7 20 / 12
36 x A ND ND V ND V V V V 8 / 5 V ND ND ND 36 x A V V V ND V ND V V V 13 / 8 21 / 13
37 A ND V ND V ND V V V V 9 / 6 ND 37 A V V ND ND V V V 8 / 5 17 / 11
38 B ND ND ND V V 5 / 2 ND 38 B ND V 3 / 1 8 / 3
39 B V 1 / 1 39 B 0 / 0 1 / 1
40 B V 1 / 1 40 B ND 1 / 0 2 / 1
41 B ND FP V V V 5 / 3 V 41 B V V ND FP V V V 8 / 6 13 / 9
42 B ND ND V V V V 6 / 4 ND 42 B ND 2 / 0 8 / 4
43 B V 1 / 1 43 B ND 1 / 0 2 / 1
44 B ND V 2 / 1 ND ND ND 44 B V ND V 6 / 2 8 / 3
45 B ND V ND V ND V V V V 9 / 6 V ND ND ND 45 B V ND V V FP ND FN ND V V V 15 / 7 24 / 13
46 A ND V ND V ND V V V V 9 / 6 V ND ND ND 46 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
47 B 0 / 0 ND 47 B 1 / 0 1 / 0
48 A ND V ND V ND V V V V 9 / 6 ND ND ND 48 A ND ND V V V 8 / 3 17 / 9
49 x A ND V ND V ND V V V V 9 / 6 V ND 49 x A 2 / 1 11 / 7
50 A ND V ND V ND V V V V 9 / 6 V ND ND ND 50 A ND V V V 8 / 4 17 / 10
51 x B ND V ND V ND V V 7 / 4 51 x B 0 / 0 7 / 4
52 A ND V ND V ND V V V V 9 / 6 V ND ND ND 52 A V V V ND ND ND V V V 13 / 7 22 / 13
53 B ND ND V ND V V 6 / 3 ND 53 B 1 / 0 7 / 3
54 x A ND V ND V ND V V V V 9 / 6 ND ND 54 x A ND ND 4 / 0 13 / 6
55 A ND V ND V ND V V V V 9 / 6 FN ND ND 55 A FN ND FN V V 8 / 2 17 / 8
56 A ND V ND V ND V V V V 9 / 6 ND ND ND 56 A V 4 / 1 13 / 7
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
4. RESULTS / Overview of Results
23
Resu
lts
4
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
30 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 30 x A V ND V V ND ND V ND V V V 15 / 8 24 / 14
31 A ND V ND V ND V V V V 9 / 6 ND ND ND 31 A V ND ND ND V V V 10 / 4 19 / 10
32 x A ND ND V ND V V V V 8 / 5 V ND ND ND 32 x A V ND ND ND V V V V V 13 / 7 21 / 12
33 A ND V ND V ND V V V V 9 / 6 V ND ND ND 33 A ND V ND V V V 10 / 5 19 / 11
34 A ND V ND V ND V V V V 9 / 6 V ND ND ND 34 A V ND V V ND ND V ND V V V V V 17 / 10 26 / 16
35 A ND ND V ND V V V V 8 / 5 V ND ND ND 35 A V V V ND ND V V V 12 / 7 20 / 12
36 x A ND ND V ND V V V V 8 / 5 V ND ND ND 36 x A V V V ND V ND V V V 13 / 8 21 / 13
37 A ND V ND V ND V V V V 9 / 6 ND 37 A V V ND ND V V V 8 / 5 17 / 11
38 B ND ND ND V V 5 / 2 ND 38 B ND V 3 / 1 8 / 3
39 B V 1 / 1 39 B 0 / 0 1 / 1
40 B V 1 / 1 40 B ND 1 / 0 2 / 1
41 B ND FP V V V 5 / 3 V 41 B V V ND FP V V V 8 / 6 13 / 9
42 B ND ND V V V V 6 / 4 ND 42 B ND 2 / 0 8 / 4
43 B V 1 / 1 43 B ND 1 / 0 2 / 1
44 B ND V 2 / 1 ND ND ND 44 B V ND V 6 / 2 8 / 3
45 B ND V ND V ND V V V V 9 / 6 V ND ND ND 45 B V ND V V FP ND FN ND V V V 15 / 7 24 / 13
46 A ND V ND V ND V V V V 9 / 6 V ND ND ND 46 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
47 B 0 / 0 ND 47 B 1 / 0 1 / 0
48 A ND V ND V ND V V V V 9 / 6 ND ND ND 48 A ND ND V V V 8 / 3 17 / 9
49 x A ND V ND V ND V V V V 9 / 6 V ND 49 x A 2 / 1 11 / 7
50 A ND V ND V ND V V V V 9 / 6 V ND ND ND 50 A ND V V V 8 / 4 17 / 10
51 x B ND V ND V ND V V 7 / 4 51 x B 0 / 0 7 / 4
52 A ND V ND V ND V V V V 9 / 6 V ND ND ND 52 A V V V ND ND ND V V V 13 / 7 22 / 13
53 B ND ND V ND V V 6 / 3 ND 53 B 1 / 0 7 / 3
54 x A ND V ND V ND V V V V 9 / 6 ND ND 54 x A ND ND 4 / 0 13 / 6
55 A ND V ND V ND V V V V 9 / 6 FN ND ND 55 A FN ND FN V V 8 / 2 17 / 8
56 A ND V ND V ND V V V V 9 / 6 ND ND ND 56 A V 4 / 1 13 / 7
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
EUPT-SRM13 | 2018 (Soybean Flour)
24
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
57 x B ND V V 3 / 2 ND ND 57 x B V 3 / 1 6 / 3
58 B V 1 / 1 58 B ND 1 / 0 2 / 1
59 B 0 / 0 59 B ND 1 / 0 1 / 0
60 A ND ND V ND V V V V 8 / 5 V ND ND 60 A ND V V ND ND V 9 / 4 17 / 9
61 x A ND ND V ND V V V V 8 / 5 ND ND 61 x A 2 / 0 10 / 5
62 B ND V ND V ND V V 7 / 4 ND ND 62 B V V ND ND V V V 9 / 5 16 / 9
63 A ND V ND V ND V V V V 9 / 6 V ND ND ND 63 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
64 B ND V 2 / 1 ND 64 B ND 2 / 0 4 / 1
65 A ND FN ND V V V V V 8 / 5 ND ND 65 A 2 / 0 10 / 5
66 B ND ND V V FN 5 / 2 ND ND 66 B 2 / 0 7 / 2
67 B ND V ND V V V V 7 / 5 ND ND ND 67 B V V ND V V V 9 / 5 16 / 10
68 x A ND V ND V ND V V V 8 / 5 ND ND 68 x A 2 / 0 10 / 5
69 A ND V ND V ND V V V V 9 / 6 V ND ND ND 69 A ND V V V 8 / 4 17 / 10
70 B ND V V 3 / 2 70 B 0 / 0 3 / 2
71 A ND ND V ND V V V V 8 / 5 V ND ND ND 71 A V V ND ND V ND V 11 / 5 19 / 10
72 A ND V ND V ND V V V V 9 / 6 V ND ND ND 72 A ND V V V 8 / 4 17 / 10
73 A ND ND V ND V V V V 8 / 5 ND ND 73 A V ND 4 / 1 12 / 6
74 x A ND V ND V ND V V V V 9 / 6 V ND ND 74 x A 3 / 1 12 / 7
76 x A ND ND V ND V V V V 8 / 5 V ND 76 x A V ND V ND ND FN ND 9 / 3 17 / 8
77 x B ND V V 3 / 2 ND 77 x B 1 / 0 4 / 2
78 x A ND V ND V ND V V V V 9 / 6 78 x A V 1 / 1 10 / 7
79 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 79 x A V V V 7 / 4 16 / 10
80 x B ND ND V V V V 6 / 4 ND 80 x B ND 2 / 0 8 / 4
82 B ND V V 3 / 2 ND ND 82 B 2 / 0 5 / 2
83 A ND V ND V ND V V V V 9 / 6 V ND ND ND 83 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
84 B ND V V V 4 / 3 ND 84 B 1 / 0 5 / 3
85 A ND V ND V ND V V V 8 / 5 V ND ND ND 85 A V FN FN 7 / 2 15 / 7
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
4. RESULTS / Overview of Results
25
Resu
lts
4
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
57 x B ND V V 3 / 2 ND ND 57 x B V 3 / 1 6 / 3
58 B V 1 / 1 58 B ND 1 / 0 2 / 1
59 B 0 / 0 59 B ND 1 / 0 1 / 0
60 A ND ND V ND V V V V 8 / 5 V ND ND 60 A ND V V ND ND V 9 / 4 17 / 9
61 x A ND ND V ND V V V V 8 / 5 ND ND 61 x A 2 / 0 10 / 5
62 B ND V ND V ND V V 7 / 4 ND ND 62 B V V ND ND V V V 9 / 5 16 / 9
63 A ND V ND V ND V V V V 9 / 6 V ND ND ND 63 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
64 B ND V 2 / 1 ND 64 B ND 2 / 0 4 / 1
65 A ND FN ND V V V V V 8 / 5 ND ND 65 A 2 / 0 10 / 5
66 B ND ND V V FN 5 / 2 ND ND 66 B 2 / 0 7 / 2
67 B ND V ND V V V V 7 / 5 ND ND ND 67 B V V ND V V V 9 / 5 16 / 10
68 x A ND V ND V ND V V V 8 / 5 ND ND 68 x A 2 / 0 10 / 5
69 A ND V ND V ND V V V V 9 / 6 V ND ND ND 69 A ND V V V 8 / 4 17 / 10
70 B ND V V 3 / 2 70 B 0 / 0 3 / 2
71 A ND ND V ND V V V V 8 / 5 V ND ND ND 71 A V V ND ND V ND V 11 / 5 19 / 10
72 A ND V ND V ND V V V V 9 / 6 V ND ND ND 72 A ND V V V 8 / 4 17 / 10
73 A ND ND V ND V V V V 8 / 5 ND ND 73 A V ND 4 / 1 12 / 6
74 x A ND V ND V ND V V V V 9 / 6 V ND ND 74 x A 3 / 1 12 / 7
76 x A ND ND V ND V V V V 8 / 5 V ND 76 x A V ND V ND ND FN ND 9 / 3 17 / 8
77 x B ND V V 3 / 2 ND 77 x B 1 / 0 4 / 2
78 x A ND V ND V ND V V V V 9 / 6 78 x A V 1 / 1 10 / 7
79 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 79 x A V V V 7 / 4 16 / 10
80 x B ND ND V V V V 6 / 4 ND 80 x B ND 2 / 0 8 / 4
82 B ND V V 3 / 2 ND ND 82 B 2 / 0 5 / 2
83 A ND V ND V ND V V V V 9 / 6 V ND ND ND 83 A V ND V V ND ND V ND V V V 15 / 8 24 / 14
84 B ND V V V 4 / 3 ND 84 B 1 / 0 5 / 3
85 A ND V ND V ND V V V 8 / 5 V ND ND ND 85 A V FN FN 7 / 2 15 / 7
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
EUPT-SRM13 | 2018 (Soybean Flour)
26
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
86 A ND ND V ND V V V V 8 / 5 V ND ND ND 86 A V V ND V ND V V 11 / 6 19 / 11
87 A ND ND V ND V V V V 8 / 5 V ND ND ND 87 A V 5 / 2 13 / 7
88 A ND V ND V ND V V V V 9 / 6 V ND ND ND 88 A ND V V V V V 10 / 6 19 / 12
89 A ND V ND V ND V V V V 9 / 6 V ND ND ND 89 A V ND FN V ND ND FN ND V V V 15 / 6 24 / 12
90 B FN 1 / 0 ND 90 B 1 / 0 2 / 0
91 A ND V ND V ND V V V V 9 / 6 V ND ND ND 91 A ND V ND V V V V 11 / 6 20 / 12
92 A ND V ND V ND V V V V 9 / 6 ND 92 A V V V ND ND V 7 / 4 16 / 10
93 A ND V ND V ND V V V V 9 / 6 V ND ND ND 93 A V ND V ND ND V V V 12 / 6 21 / 12
94 B V 1 / 1 94 B 0 / 0 1 / 1
95 B V 1 / 1 95 B 0 / 0 1 / 1
96 B ND ND V V V V V 7 / 5 ND 96 B 1 / 0 8 / 5
97 A ND V ND V ND V V V V 9 / 6 V ND ND ND 97 A V ND V V ND ND V FN FN 13 / 5 22 / 11
98 A ND V ND V ND V V V V 9 / 6 V ND ND ND 98 A ND V ND V V V V V 12 / 7 21 / 13
99 B ND V 2 / 1 ND 99 B 1 / 0 3 / 1
100 x B ND V V V 4 / 3 100 x B 0 / 0 4 / 3
101 A ND ND V ND V V V V 8 / 5 V ND ND ND 101 A V ND V V ND ND ND V V V 14 / 7 22 / 12
102 B V 1 / 1 102 B 0 / 0 1 / 1
103 B V 1 / 1 103 B 0 / 0 1 / 1
104 A ND V ND V ND V V V V 9 / 6 104 A 0 / 0 9 / 6
105 A ND V ND V ND V V V V 9 / 6 V ND ND ND 105 A ND FN V ND ND V V V V 13 / 6 22 / 12
106 B ND V ND V V 5 / 3 106 B ND V V 3 / 2 8 / 5
107 B ND ND V V V V 6 / 4 V ND ND 107 B V V ND ND 7 / 3 13 / 7
109 A ND ND V ND V V V V 8 / 5 FN ND ND ND 109 A FN V FN ND ND FN ND FN 12 / 1 20 / 6
110 B ND ND V V 4 / 2 ND 110 B V ND ND V 5 / 2 9 / 4
111 B V ND ND V 4 / 2 ND 111 B V 2 / 1 6 / 3
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
4. RESULTS / Overview of Results
27
Resu
lts
4
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
86 A ND ND V ND V V V V 8 / 5 V ND ND ND 86 A V V ND V ND V V 11 / 6 19 / 11
87 A ND ND V ND V V V V 8 / 5 V ND ND ND 87 A V 5 / 2 13 / 7
88 A ND V ND V ND V V V V 9 / 6 V ND ND ND 88 A ND V V V V V 10 / 6 19 / 12
89 A ND V ND V ND V V V V 9 / 6 V ND ND ND 89 A V ND FN V ND ND FN ND V V V 15 / 6 24 / 12
90 B FN 1 / 0 ND 90 B 1 / 0 2 / 0
91 A ND V ND V ND V V V V 9 / 6 V ND ND ND 91 A ND V ND V V V V 11 / 6 20 / 12
92 A ND V ND V ND V V V V 9 / 6 ND 92 A V V V ND ND V 7 / 4 16 / 10
93 A ND V ND V ND V V V V 9 / 6 V ND ND ND 93 A V ND V ND ND V V V 12 / 6 21 / 12
94 B V 1 / 1 94 B 0 / 0 1 / 1
95 B V 1 / 1 95 B 0 / 0 1 / 1
96 B ND ND V V V V V 7 / 5 ND 96 B 1 / 0 8 / 5
97 A ND V ND V ND V V V V 9 / 6 V ND ND ND 97 A V ND V V ND ND V FN FN 13 / 5 22 / 11
98 A ND V ND V ND V V V V 9 / 6 V ND ND ND 98 A ND V ND V V V V V 12 / 7 21 / 13
99 B ND V 2 / 1 ND 99 B 1 / 0 3 / 1
100 x B ND V V V 4 / 3 100 x B 0 / 0 4 / 3
101 A ND ND V ND V V V V 8 / 5 V ND ND ND 101 A V ND V V ND ND ND V V V 14 / 7 22 / 12
102 B V 1 / 1 102 B 0 / 0 1 / 1
103 B V 1 / 1 103 B 0 / 0 1 / 1
104 A ND V ND V ND V V V V 9 / 6 104 A 0 / 0 9 / 6
105 A ND V ND V ND V V V V 9 / 6 V ND ND ND 105 A ND FN V ND ND V V V V 13 / 6 22 / 12
106 B ND V ND V V 5 / 3 106 B ND V V 3 / 2 8 / 5
107 B ND ND V V V V 6 / 4 V ND ND 107 B V V ND ND 7 / 3 13 / 7
109 A ND ND V ND V V V V 8 / 5 FN ND ND ND 109 A FN V FN ND ND FN ND FN 12 / 1 20 / 6
110 B ND ND V V 4 / 2 ND 110 B V ND ND V 5 / 2 9 / 4
111 B V ND ND V 4 / 2 ND 111 B V 2 / 1 6 / 3
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
EUPT-SRM13 | 2018 (Soybean Flour)
28
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
112 A ND V ND V ND V V V V 9 / 6 V ND ND ND 112 A V ND V V ND ND V ND V V V V V 17 / 10 26 / 16
113 B 0 / 0 113 B V V 2 / 2 2 / 2
114 B 0 / 0 114 B V V 2 / 2 2 / 2
3rd-115 B ND ND V V FN V 6 / 3 FN ND 3rd-115 B V V ND 5 / 2 11 / 5
3rd-116 B ND V ND V ND V V V 8 / 5 ND ND 3rd-116 B V V 4 / 2 12 / 7
3rd-117 A ND V ND V ND V V V V 9 / 6 V ND 3rd-117 A V ND ND 5 / 2 14 / 8
3rd-118 B ND V V ND FN V 6 / 3 ND ND 3rd-118 B V ND FP FP 6 / 1 12 / 4
3rd-119 B ND V 2 / 1 V ND 3rd-119 B 2 / 1 4 / 2
3rd-120 B ND ND V 3 / 1 ND 3rd-120 B V ND 3 / 1 6 / 2
3rd-121 B ND V 1 / 1 ND ND 3rd-121 B FN* ND 1 / 0 2 / 1
3rd-122 B ND V V ND V V V 7 / 5 3rd-120 B V 1 / 1 8 / 6
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
4. RESULTS / Overview of Results
29
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4
Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)
Compulsory Compounds Optional Compounds Optional Compounds Total
Compulsory Compound listed in Target List 2,
4-D
Brom
ide
ion
Chlo
rmeq
uat-
Cl
Cyro
maz
ine
Ethe
phon
Flua
zifo
p
Gly
phos
ate
Hal
oxyf
op
Mep
iqua
t-Cl
Ana
lyse
d / c
orre
ctly
foun
d am
ong
COM
PULS
ORY
com
poun
ds
(max
. 13
/ 8)
2,4-
DB
Bent
azon
e
Carb
ofur
an
Chlo
rate Optional / Additional
Compound listed in Target List D
iqua
t
Feno
xapr
op
Glu
fosi
nate
MPP
N-A
cety
l-G
lufo
sina
te
AM
PA
N-A
cety
l-G
lyph
osat
e
Para
quat
Perc
hlor
ate
Phos
phon
ic a
cid
Qui
zalo
fop
Phso
phin
e (T
est I
tem
)
Phos
phin
e (P
H3-
Tube
)
Ana
lyse
d / c
orre
ctly
foun
d am
ong
OP
TIO
NA
L co
mpo
unds
(m
ax. 2
1 / 1
5)A
naly
sed
/ cor
rect
ly fo
und
amon
gCO
MPU
LSO
RY a
nd O
PTI
ON
AL
com
poun
ds
(max
. 21
/ 15)
within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD
present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in
Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes
evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated
in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No
Lab- Code SRM13-
NRL- SRM Cat. 2)
Lab- Code SRM13-
NRL- SRM Cat. 2)
112 A ND V ND V ND V V V V 9 / 6 V ND ND ND 112 A V ND V V ND ND V ND V V V V V 17 / 10 26 / 16
113 B 0 / 0 113 B V V 2 / 2 2 / 2
114 B 0 / 0 114 B V V 2 / 2 2 / 2
3rd-115 B ND ND V V FN V 6 / 3 FN ND 3rd-115 B V V ND 5 / 2 11 / 5
3rd-116 B ND V ND V ND V V V 8 / 5 ND ND 3rd-116 B V V 4 / 2 12 / 7
3rd-117 A ND V ND V ND V V V V 9 / 6 V ND 3rd-117 A V ND ND 5 / 2 14 / 8
3rd-118 B ND V V ND FN V 6 / 3 ND ND 3rd-118 B V ND FP FP 6 / 1 12 / 4
3rd-119 B ND V 2 / 1 V ND 3rd-119 B 2 / 1 4 / 2
3rd-120 B ND ND V 3 / 1 ND 3rd-120 B V ND 3 / 1 6 / 2
3rd-121 B ND V 1 / 1 ND ND 3rd-121 B FN* ND 1 / 0 2 / 1
3rd-122 B ND V V ND V V V 7 / 5 3rd-120 B V 1 / 1 8 / 6
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant
2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)
V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.
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Table 4-3: Numerical values of analyte concentration in the blank material reported by the participating laboratories
Compound MRRL
[mg/kg]Assigned Value
[mg/kg]
Conc. in Blank Material
[mg/kg]
Conc. in Test Item
[mg/kg]
RL
[mg/kg] Reported by
Bromide ion 2 15.4 0.14 4.29 1 SRM13-74
0.374 9.886 0.05 SRM13-34
0.4 14.1 2 SRM13-72
0.543 14.4 0.3 SRM13-3rd-118
0.66 15.9 0.2 SRM13-45
0.702 12.9 2 SRM13-92
0.725 14.1 2 SRM13-67
0.783 17.8 0.2 SRM13-13
0.8 14.6 0.5 SRM13-6
1.2 12 1 SRM13-112
1.5 11.6 1 SRM13-98
3.7 18 2 SRM13-31
10.4 27.9 5 SRM13-97
Glyphosate 0.03 0.903 0.002 0.859 0.01 SRM13-98
AMPA 0.05 not present 0.0923 0.0906 (= FP) 0.05 SRM13-3rd-118
Paraquat 0.02 not present 0.497 0.495 (= FP) 0.05 SRM13-3rd-118
Perchlorate 0.01 0.100 0.0035 0.0825 0.005 SRM13-67
0.004 0.102 0.01 SRM13-98
Phosphonic acid 0.05 1.87 0.02 1.59 0.01 SRM13-14
0.039 2.45 0.05 SRM13-98
Phsophine (Test Item) 0.005 – 0.00001 0.21 0.0001 SRM13-113
Phosphine (PH3-Tube) 0.005 – 0.00001 0.106 0.0001 SRM13-113
4.2 Analysis of Blank Material
In 68 cases the laboratories reported detecting of target pesticides in the blank material under their report-ing limit or MRRLs (data not shown). In further 22 cases (Table 4-3) the laboratories reported numerical re-sults for the concentration of taget pesticides detected in the blank material, among them there were four cases (2× bromide ion, 1× paraquat and 1× AMPA) where participants reported detections in the blank ma-terial at levels higher than both their own RLs and above the MRRL. All these four cases indicated contami-nation in the procedure or background value in the system. In the two cases of paraquat (MRRL = 0.02 mg/kg) at 0.497 mg/kg and AMPA (MRRL = 0.05 mg/kg) at 0.0923 mg/kg, both reported by SRM13-3rd-118, this laboratory has also detected these two analytes in the test item at the comparable levels although they were neither spiked to the test item nor detected by other laboratories. In the two cases of bromide ion (MRRL = 2 mg/kg) at 3.7 mg/kg (reported by SRM13-31) and 10.4 mg/kg (reported by SRM13-97) the par-ticipants would have achieved much better z-scores if the reported results would have been substrated from the concentration in the blank material. The affected laboratories are encouraged to find the reasons behind these contamination / background value.
4.3 Assigned Values and Target Standard Deviations
The assigned value (xpt) of each analyte present in the test item was established as the mean of robust sta-tistics (x*) of all numerical results submitted by laboratories from EU and EFTA countries calculated using Algorithm A [6, Appendix 8]. Results from third country laboratories were not taken into account. Except the calculation of phosphine the results reported by private laboratories were also not taken into account. Based on these assigned values, z-scores were calculated for all submitted results using the FFP-approach
4. RESULTS / Assigned Values and Target Standard Deviations
31
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4
(Section 4.4.3, p. 34), and a preliminary report was released on 19 June, 2018. The uncertainties (u(xpt)) of the assigned values were calculated as described under Section 2.2, p. 11.
In the case of diquat the very wide distribution of participants’ results (CV* 52.8 %) resulted in the robust mean being assosiated with a statistical uncertainty exceeding the tolerance (Table 4-5, p. 32). The Sci-entific Committee therefore decided to evaluate the robust mean and z-scores for diquat for informative purposes only.
In the case of phosphine (both in the test item and in the PH3-tube), althouth the results submitted from private laboratories routinely analysing this compound were taken into account, the total number of re-sults (18) were low and the results distribution were extremely wide with a CV*-value of 93.1 % for phos-phine in the test item and 74.8 % for phosphine in the PH3-Tube. A reliable statistical evaluation for these two parameter was therefore not possible. A special report on phsophine with discussion about the ana-lytical difficulties will be issued.
The CV*-values of all other compulsory and optional analytes were lower than the FFP-RSD of 25 %. The av-erage CV*s of compulsory analytes based on the entire population of EU-and EFTA-laboratories was 21.2 %, and the average CV*s of optional analytes based on the entire population excluding diquat, phosphine (test tiem) and phosphine (PH-Tube) was 22.0 %. Both were clearly lower than the FFP-RSD of 25 %.
Table 4-4: Assigned values, uncertainties of assigned values and CV* values calculated for all compounds present in the test item
Assigned Value and CV* Based on the Entire Population of Results from EU and EFTA Laboratories
Compound No. of FNs
No. of numerical
results (EU+EFTA)
Assigned Value
[mg/kg]
u(xpt) 1) [mg/kg]
u(xpt) Tolerance
[mg/kg]
Judgementfor
UAV-testCV* 2)
[%]
Com
puls
ory
Co
mpo
unds
Bromide ion 1 61 15.3 +/-0.58988 1.1517 passed 24.0
Cyromazine 1 78 0.097 +/-0.00323 0.0073 passed 23.5
Fluazifop 1 85 0.049 +/-0.00136 0.0037 passed 20.3
Glyphosate 83 0.903 +/-0.02798 0.0677 passed 22.6
Haloxyfop 81 0.017 +/-0.00048 0.013 passed 20.4
Mepiquat-Cl 2 84 0.124 +/-0.00387 0.0093 passed 22.9
Average 3) CV* 21.2
Opt
iona
l Co
mpo
unds
2,4-DB 2 50 0.183 +/-0.00669 0.0137 passed 20.7
Diquat 4) 1 29 1.70 +/-0.20868 0.1267 failed 52.8 4)
Glufosinate 3 41 0.192 +/-0.01073 0.0144 passed 28.7
MPP 1 24 0.188 +/-0.00908 0.0141 passed 18.9
N-Acetyl-Glyphosate 5 18 0.835 +/-0.05185 0.0626 passed 21.1
Perchlorate 2 53 0.100 +/-0.00289 0.0075 passed 16.9
Phosphonic acid 3 42 1.86 +/-0.08723 0.1398 passed 24.3
Quizalofop 2 60 0.052 +/-0.00198 0.0039 passed 23.6
Phsophine (Test Item) 5) 11 + 7 6) 0.092 +/-0.02517 0.0069 failed 93.1 5)
Phosphine (PH3-Tube) 5) 11 + 7 6) 0.040 +/-0.00877 0.003 failed 74.8 5)
Average 3) CV* 22.0
1: u(xpt) : Uncertainty of assigned value calculated as shown under Section 2.2 (p. 38)2: CV* : Relative standard deviation based on robust statistics3: The average CV* is given for information purposes only. CV*s of individual compounds or average CV*s of individual compounds or related
compounds over many PTs are more meaningfull and conclusive.4: Excluded from the calculation of the average CV*s and the assigned values as well as z-scores were calculated for informative purpose only.5: Excluded from the calculation of the average CV*s and from this report, will be evaluated and discussed in a separate report.6: 7 results reported by private laboratories which were exceptionally invited to analyte phosphine
EUPT-SRM13 | 2018 (Soybean Flour)
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4.4 Assessment of Laboratory Performance
4.4.1 False Positives
Five results were preliminarily judged as false positives: AMPA (2x), ethephon (1x), N-acetyl glufosinate (1x) and paraquat (1x). In cases where the reported concentration of a compound not present in the Test Item was lower than the respective MRRL the results were preliminarily not judged as false positives. This con-cerned carbofuran, chlorate and AMPA in one case each.
Among EU- and EFTA-laboratories three laboratories reported in three cased numerical results for three analytes (ethephon, N-Acetyl-Glufosinate and AMPA) on the Target Pesticides List but not present in the test material. Two other false positive results (AMLA and paraquat) were reported by one laboratory from third countries. All these analytes were neither detected by the organisers nor by the overwhelming majority of the participants (Table 4-5). These five results exceeded the laboratories’ reporting limits for these com-pounds, were higher than the respective MRRLs in the Target Pesticides List, and were, therefore, judged as false positives.
Three laboratories reported in three cases numerical results for carbofuran (0.0028 mg/kg), chlorate (0.0043 mg/kg), and AMPA (0.002 mg/kg), which were lower than the laboratories’ RLs or MRRL. Following the rules in the General Protocol these two results were not judged as false positives, although they actu-ally should not be reported.
4.4.2 False Negatives
Among the compulsory compounds there were 7 cases (2× fluazifop, 2× Mepiquat-Cle-Cl, 1× bromide ion, 1× cyromazine and 1× haloxyfop) where the participants reported “analysed, but not detected” for target compounds which were spiked to the test item and detected by the majority of the laboratories target-ing them (Table 4-6, p. 33). Five of them were reported by laboratories from EU and EFTA countries and represented 1.0 % of the total 477 results reported by the EU/EFTA laboratories for compulsory target compounds present in the test item. The total 7 esults, including the other two reportet by laboratories from third countires, represented 1.4 % of the total 504 results from all participating laboratories. As the as-signed values for these seven analytes were sufficiently distant from the MRRLs, these results were judged as false negatives. In one case of cyromazine the “false negative” judgement resulted from the fact that the laboratory had a reporting limit at a similar level to the assigned value.
Compound PT-Code Analysed Reported Result [mg/kg]
RL [mg/kg]
MRRL [mg/kg] Judgement
Ethephon SRM13-41 Yes 0.368 0.01 0.02 FP
Opt
iona
l Com
poun
ds
Carbofuran SRM13-7 Yes 0.0028 – 0.005 –
Chlorate SRM13-67 Yes 0.0043 0.005 0.01 –
N-Acetyl-Glufosinate SRM13-45 Yes 1.26 0.02 0.02 FP
AMPA SRM13-41 Yes 0.078 0.01 0.05 FP
SRM13-98 Yes 0.002 0.01 0.05 –
SRM13-3rd-118 Yes 0.0906 0.05 0.05 FP
Paraquat SRM13-3rd-118 Yes 0.495 0.05 0.02 FP
Table 4-5: Overview of false positive and potentially false positive results reported by participating laboratories
4. RESULTS / Assessment of Laboratory Performance
33
Resu
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4
Compound PT-Code Analysed Detected RL [mg/kg]
MRRL [mg/kg]
Assigned Value
[mg/kg]Judgement
Com
puls
ory
Com
poun
ds
Bromide ion SRM13-65 Yes No 12.5 2 15.4 False Negative
Cyromazine SRM13-2 Yes No 0.01 0.01 0.097 False Negative
Fluazifop SRM13-90 Yes No 0.005 0.01 0.049 False Negative
SRM13-3rd-118 Yes No 0.01 False Negative
Haloxyfop SRM13-3rd-115 Yes No 0.003 0.003 0.017 False Negative
Mepiquat-Cl SRM13-2 Yes No 0.01 0.01 0.124 False Negative
SRM13-66 Yes No 0.01 False Negative
Opt
iona
l Com
poun
ds
2,4-DB SRM13-55 Yes No 0.01 0.01 0.183 False Negative
SRM13-109 Yes No 0.01 False Negative
SRM13-3rd-115 Yes No 0.01 False Negative
Diquat SRM13-109 Yes No 0.02 0.02 1.70 False Negative
Glufosinate SRM13-55 Yes No 0.04 0.02 0.192 False Negative
SRM13-89 Yes No 0.02 False Negative
SRM13-105 Yes No 0.1 False Negative
SRM13-3rd-121 Yes No 0.5 False Negative*
MPP SRM13-109 Yes No 0.02 0.02 0.188 False Negative
N-Acetyl- Glyphosate
SRM13-45 Yes No 0.02 0.02 0.835 False Negative
SRM13-55 Yes No 0.04 False Negative
SRM13-76 Yes No mg/kg False Negative
SRM13-89 Yes No 0.02 False Negative
SRM13-109 Yes No 0.02 False Negative
Perchlorate SRM13-2 Yes No 0.01 0.01 0.100 False Negative
SRM13-109 Yes No 0.01 False Negative
Phosphonic acid SRM13-11 Yes No 0.05 0.05 1.86 False Negative
SRM13-85 Yes No 0.1 False Negative
SRM13-97 Yes No 0.1 False Negative
Quizalofop SRM13-47 Yes No – 0.01 0.052 False Negative
SRM13-66 Yes No 0.01 False Negative
SRM13-3rd-115 Yes No 0.01 False Negative
SRM13-3rd-118 Yes No 0.01 False Negative
*: Laboratory’s RL >> MRRL; in accordance with the General Protocole judged as false negative.
Table 4-6: Overview of false negative results reported by participating laboratories (including 3rd country laboratories)
Among the optional compounds there were 23 cases (4× N-acetyl-glyphosate, 4× Quizalofop, 3× 2,4-DB, 4× glufosinate, 3× phosphonic acid, 2× perchlorate, 1× diquat and 1× MPP) where the participants report-ed “analysed, but not detected” for target compounds that were spiked to the test item and detected by the majority of the laboratories targeting them (Table 4-6). In one case of glufosinate the “false negative” judgement resulted from the fact that the laboratory had a higher reporting limit than the assigned value, as this is the rule stated in the General Protocol. The 19 false negative results reported by EU/EFTA labora-tories accounted for 5.3 % of the total 358 results reported by the EU/EFTA laboratories for optional target compounds. The 23 false negative results reported in total represented 6.2 % of the 372 results reported by all participating labs for optional compounds.
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4.4.3 Laboratory Performance Based on z-Scores
All individual z-scores were calculated using the FFP-RSD of 25 % and the assigned values derived from the entire population of results received from EU/EFTA laboratories. Table 4-7 shows the overall classification of z-scores achieved by all laboratories for compulsory and optional compounds. The respective rules are shown in Section 2.4 (p. 12). Among the laboratories from EU and EFTA countries “Acceptable” z-scores were achieved by 82 – 97 % (91 % on average) of the labs in the case of compulsory compounds and by 74 – 92 % (85 % on average) in the case of optional compounds excluding diquat and phosphine. Overall, 89 % of the results submitted by EU- and EFTA-countries were acceptable, 5 % questionable and 10 % unac-ceptable (including false negatives). The respective overall figures of 3rd country labs were 74 %, 5 % and 21 %.
A compilation of all individual results and z-scores for each laboratory is shown in Table 4-8 (p. 36) and Table 4-9 (p. 42) for compulsory and optional compounds, respectively. The corresponding kernel density histograms showing the distribution of the reported results are shown in Appendix 5. A graphic represen-tation of the z-score distribution of each target analyte present in the test item can be seen in Appendix 6.
4. RESULTS / Assessment of Laboratory Performance
35
Resu
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4
Table 4-7: Overall performance based on z-score classification
EU and EFTA laboratories
Compound No. of results 1)
Acceptable Questionable Unacceptable 1) FNs
No. (%) No. (%) No. (%) No.
Com
puls
ory
Com
poun
ds
Bromide ion 62 56 (90 %) 2 (3 %) 4 (6 %) 1
Cyromazine 79 65 (82 %) 8 (10 %) 6 (8 %) 1
Fluazifop 86 83 (97 %) 2 (2 %) 1 (1 %) 1
Glyphosate 83 78 (94 %) 2 (2 %) 3 (4 %) 0
Haloxyfop 81 78 (96 %) 2 (2 %) 1 (1 %) 0
Mepiquat-Cl 86 76 (88 %) 2 (2 %) 8 (9 %) 2
Subtotal (average) 477 436 (91 %) 18 (4 %) 23 (5 %) 5
Opt
iona
l Co
mpo
unds
2)
2,4-DB 52 48 (92 %) 1 (2 %) 3 (6 %) 2
Glufosinate 44 37 (84 %) 2 (5 %) 5 (11 %) 3
MPP 25 20 (80 %) 2 (8 %) 3 (12 %) 1
N-Acetyl-Glyphosate 23 17 (74 %) (0 %) 6 (26 %) 5
Perchlorate 55 47 (85 %) 3 (5 %) 5 (9 %) 2
Phosphonic acid 45 36 (80 %) 2 (4 %) 7 (16 %) 3
Quizalofop 62 54 (87 %) 5 (8 %) 3 (5 %) 2
Subtotal (average) 306 259 (85 %) 15 (5 %) 32 (10 %) 18
Overall EU/EFTA (Average) 783 695 (89 %) 33 (4 %) 55 (7 %) 23
3rd country laboratories
Compound No. of results 1)
Acceptable Questionable Unacceptable 1) FNs
No. (%) No. (%) No. (%) No.
Com
puls
ory
Com
poun
ds
Bromide ion 4 4 (100 %) 0 (0 %) 0
Cyromazine 5 4 (80 %) 1 (20 %) 0 (0 %) 0
Fluazifop 3 2 (67 %) 1 (33 %) 1
Glyphosate 7 6 (86 %) 1 (14 %) 0
Haloxyfop 4 2 (50 %) 1 (25 %) 1 (25 %) 1
Mepiquat-Cl 4 3 (75 %) 1 (25 %) 0
Subtotal (average) 27 21 (78 %) 2 (7 %) 4 (15 %) 2
Opt
iona
l Co
mpo
unds
2)
2,4-DB 3 2 (67 %) (0 %) 1 (33 %) 1
Glufosinate 6 5 (83 %) (0 %) 1 (17 %) 1
MPP
N-Acetyl-Glyphosate
Perchlorate
Phosphonic acid
Quizalofop 2 (0 %) (0 %) 2 (100 %) 2
Subtotal (average) 11 7 (64 %) 0 (0 %) 4 (36 %) 4
Overall 3rd country (Average) 38 28 (74 %) 2 (5 %) 8 (21 %) 6
1) including false negatives (FNs)2) excluding diquat and phosphine
EUPT-SRM13 | 2018 (Soybean Flour)
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COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
1 8 / 5 A 20.5 1.3 0.0534 0.3 1 8 / 5 A 0.922 0.1 0.0159 -0.2 0.123 0.0
2 9 / 4 B 15.5 0.0 FN -3.6 0.052 0.2 2 9 / 4 B 0.631 -1.2 0.014 -0.7 FN -3.7
3 4 / 3 B 0.0818 -0.6 0.0463 -0.2 3 4 / 3 B 0.0147 -0.5
4 x 9 / 6 A 18.5 0.8 0.1 0.1 0.0718 1.8 4 x 9 / 6 A 0.926 0.1 0.016 -0.2 0.124 0.0
5 x 7 / 4 B 0.0473 -0.2 5 x 7 / 4 B 0.4327 -2.1 0.0241 1.7 0.0829 -1.3
6 9 / 6 A 14.6 -0.2 0.107 0.4 0.0485 -0.1 6 9 / 6 A 0.95 0.2 0.0127 -1.0 0.115 -0.3
7 x 4 / 3 B 0.113 0.7 0.0335 -1.3 7 x 4 / 3 B 0.0157 -0.3
8 x 9 / 6 A 16.4 0.3 0.111 0.6 0.0466 -0.2 8 x 9 / 6 A 0.924 0.1 0.0151 -0.4 0.12 -0.1
10 9 / 6 A 14.8 -0.1 0.0464 -2.1 0.0213 -2.3 10 9 / 6 A 0.999 0.4 0.0151 -0.4 0.11 -0.4
11 9 / 6 A 14.3 -0.3 0.102 0.2 0.0539 0.4 11 9 / 6 A 1.12 1.0 0.0177 0.2 0.0959 -0.9
12 x 9 / 6 A 12.8 -0.7 0.1 0.1 0.052 0.2 12 x 9 / 6 A 1.04 0.6 0.017 0.0 0.154 1.0
13 x 9 / 6 A 17.8 0.6 0.23 5.5 0.038 -0.9 13 x 9 / 6 A 1.06 0.7 0.0139 -0.7 0.301 5.7
14 9 / 6 A 14.8 -0.1 0.112 0.6 0.0701 1.7 14 9 / 6 A 0.821 -0.4 0.0181 0.3 0.12 -0.1
15 9 / 6 A 12.1 -0.8 0.0997 0.1 0.0632 1.1 15 9 / 6 A 0.733 -0.8 0.0181 0.3 0.128 0.1
16 9 / 6 A 19.3 1.0 0.072 -1.0 0.062 1.0 16 9 / 6 A 1.17 1.2 0.019 0.5 0.131 0.2
17 7 / 4 B 0.0848 -0.5 0.0426 -0.5 17 7 / 4 B 0.615 -1.3 0.0182 0.3
19 x 9 / 6 A 20.3 1.3 1.18 44.7 0.068 1.5 19 x 9 / 6 A 1.22 1.4 0.017 0.0 1.33 39.0
20 x 9 / 6 A 16.5 0.3 0.101 0.2 0.0422 -0.6 20 x 9 / 6 A 0.969 0.3 0.0144 -0.6 0.149 0.8
21 8 / 5 A 14.3 -0.3 0.048 -0.1 21 8 / 5 A 0.839 -0.3 0.016 -0.2 0.147 0.7
22 x 9 / 6 A 16.4 0.3 0.0772 -0.8 0.0406 -0.7 22 x 9 / 6 A 1.05 0.7 0.0147 -0.5 0.132 0.3
23 6 / 4 B 0.052 0.2 23 6 / 4 B 1.02 0.5 0.017 0.0 0.138 0.5
24 x 8 / 5 A 0.121 1.0 0.065 1.3 24 x 8 / 5 A 1 0.4 0.021 1.0 0.167 1.4
25 7 / 5 B 18.7 0.9 0.118 0.9 0.052 0.2 25 7 / 5 B 0.019 0.5 0.125 0.0
26 9 / 6 A 15.0 -0.1 0.085 -0.5 0.032 -1.4 26 9 / 6 A 0.65 -1.1 0.011 -1.4 0.16 1.2
27 9 / 6 A 17.3 0.5 0.084 -0.5 0.046 -0.3 27 9 / 6 A 1.02 0.5 0.01 -1.6 0.15 0.8
28 2 / 1 B 0.0565 0.6 28 2 / 1 B
29 x 9 / 6 A 23.61 2.1 0.08 -0.7 0.072 1.8 29 x 9 / 6 A 0.893 0.0 0.015 -0.4 0.089 -1.1
30 x 9 / 6 A 12.9 -0.6 0.114 0.7 0.049 0.0 30 x 9 / 6 A 1.04 0.6 0.049 7.6 0.149 0.8
31 9 / 6 A 18.0 0.7 0.075 -0.9 0.049 0.0 31 9 / 6 A 0.959 0.2 0.016 -0.2 0.108 -0.5
32 x 8 / 5 A 0.0842 -0.5 0.0455 -0.3 32 x 8 / 5 A 1.02 0.5 0.0157 -0.3 0.118 -0.2
33 9 / 6 A 11.3 -1.1 0.092 -0.2 0.0531 0.3 33 9 / 6 A 0.883 -0.1 0.017 0.0 0.118 -0.2
34 9 / 6 A 9.886 -1.4 0.105 0.3 0.047 -0.2 34 9 / 6 A 0.779 -0.5 0.016 -0.2 0.088 -1.2
35 8 / 5 A 0.04 -2.3 0.037 -1.0 35 8 / 5 A 1.23 1.4 0.011 -1.4 0.151 0.9
36 x 8 / 5 A 0.0786 -0.8 0.0496 0.0 36 x 8 / 5 A 0.721 -0.8 0.0171 0.1 0.0841 -1.3
37 9 / 6 A 16.4 0.3 0.087 -0.4 0.057 0.6 37 9 / 6 A 1.29 1.7 0.022 1.2 0.15 0.8
38 5 / 2 B 0.0483 -0.1 38 5 / 2 B 0.131 0.2
39 1 / 1 B 39 1 / 1 B 0.983 0.4
40 1 / 1 B 40 1 / 1 B 1.09 0.8
41 5 / 3 B 0.0686 1.6 41 5 / 3 B 1.17 1.2 0.0226 1.4
42 6 / 4 B 0.075 -0.9 0.038 -0.9 42 6 / 4 B 0.014 -0.7 0.111 -0.4
43 1 / 1 B 43 1 / 1 B 0.794 -0.5
44 2 / 1 B 44 2 / 1 B 1.989 4.8
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
Table 4-8: Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
4. RESULTS / Assessment of Laboratory Performance
37
Resu
lts
4
COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
1 8 / 5 A 20.5 1.3 0.0534 0.3 1 8 / 5 A 0.922 0.1 0.0159 -0.2 0.123 0.0
2 9 / 4 B 15.5 0.0 FN -3.6 0.052 0.2 2 9 / 4 B 0.631 -1.2 0.014 -0.7 FN -3.7
3 4 / 3 B 0.0818 -0.6 0.0463 -0.2 3 4 / 3 B 0.0147 -0.5
4 x 9 / 6 A 18.5 0.8 0.1 0.1 0.0718 1.8 4 x 9 / 6 A 0.926 0.1 0.016 -0.2 0.124 0.0
5 x 7 / 4 B 0.0473 -0.2 5 x 7 / 4 B 0.4327 -2.1 0.0241 1.7 0.0829 -1.3
6 9 / 6 A 14.6 -0.2 0.107 0.4 0.0485 -0.1 6 9 / 6 A 0.95 0.2 0.0127 -1.0 0.115 -0.3
7 x 4 / 3 B 0.113 0.7 0.0335 -1.3 7 x 4 / 3 B 0.0157 -0.3
8 x 9 / 6 A 16.4 0.3 0.111 0.6 0.0466 -0.2 8 x 9 / 6 A 0.924 0.1 0.0151 -0.4 0.12 -0.1
10 9 / 6 A 14.8 -0.1 0.0464 -2.1 0.0213 -2.3 10 9 / 6 A 0.999 0.4 0.0151 -0.4 0.11 -0.4
11 9 / 6 A 14.3 -0.3 0.102 0.2 0.0539 0.4 11 9 / 6 A 1.12 1.0 0.0177 0.2 0.0959 -0.9
12 x 9 / 6 A 12.8 -0.7 0.1 0.1 0.052 0.2 12 x 9 / 6 A 1.04 0.6 0.017 0.0 0.154 1.0
13 x 9 / 6 A 17.8 0.6 0.23 5.5 0.038 -0.9 13 x 9 / 6 A 1.06 0.7 0.0139 -0.7 0.301 5.7
14 9 / 6 A 14.8 -0.1 0.112 0.6 0.0701 1.7 14 9 / 6 A 0.821 -0.4 0.0181 0.3 0.12 -0.1
15 9 / 6 A 12.1 -0.8 0.0997 0.1 0.0632 1.1 15 9 / 6 A 0.733 -0.8 0.0181 0.3 0.128 0.1
16 9 / 6 A 19.3 1.0 0.072 -1.0 0.062 1.0 16 9 / 6 A 1.17 1.2 0.019 0.5 0.131 0.2
17 7 / 4 B 0.0848 -0.5 0.0426 -0.5 17 7 / 4 B 0.615 -1.3 0.0182 0.3
19 x 9 / 6 A 20.3 1.3 1.18 44.7 0.068 1.5 19 x 9 / 6 A 1.22 1.4 0.017 0.0 1.33 39.0
20 x 9 / 6 A 16.5 0.3 0.101 0.2 0.0422 -0.6 20 x 9 / 6 A 0.969 0.3 0.0144 -0.6 0.149 0.8
21 8 / 5 A 14.3 -0.3 0.048 -0.1 21 8 / 5 A 0.839 -0.3 0.016 -0.2 0.147 0.7
22 x 9 / 6 A 16.4 0.3 0.0772 -0.8 0.0406 -0.7 22 x 9 / 6 A 1.05 0.7 0.0147 -0.5 0.132 0.3
23 6 / 4 B 0.052 0.2 23 6 / 4 B 1.02 0.5 0.017 0.0 0.138 0.5
24 x 8 / 5 A 0.121 1.0 0.065 1.3 24 x 8 / 5 A 1 0.4 0.021 1.0 0.167 1.4
25 7 / 5 B 18.7 0.9 0.118 0.9 0.052 0.2 25 7 / 5 B 0.019 0.5 0.125 0.0
26 9 / 6 A 15.0 -0.1 0.085 -0.5 0.032 -1.4 26 9 / 6 A 0.65 -1.1 0.011 -1.4 0.16 1.2
27 9 / 6 A 17.3 0.5 0.084 -0.5 0.046 -0.3 27 9 / 6 A 1.02 0.5 0.01 -1.6 0.15 0.8
28 2 / 1 B 0.0565 0.6 28 2 / 1 B
29 x 9 / 6 A 23.61 2.1 0.08 -0.7 0.072 1.8 29 x 9 / 6 A 0.893 0.0 0.015 -0.4 0.089 -1.1
30 x 9 / 6 A 12.9 -0.6 0.114 0.7 0.049 0.0 30 x 9 / 6 A 1.04 0.6 0.049 7.6 0.149 0.8
31 9 / 6 A 18.0 0.7 0.075 -0.9 0.049 0.0 31 9 / 6 A 0.959 0.2 0.016 -0.2 0.108 -0.5
32 x 8 / 5 A 0.0842 -0.5 0.0455 -0.3 32 x 8 / 5 A 1.02 0.5 0.0157 -0.3 0.118 -0.2
33 9 / 6 A 11.3 -1.1 0.092 -0.2 0.0531 0.3 33 9 / 6 A 0.883 -0.1 0.017 0.0 0.118 -0.2
34 9 / 6 A 9.886 -1.4 0.105 0.3 0.047 -0.2 34 9 / 6 A 0.779 -0.5 0.016 -0.2 0.088 -1.2
35 8 / 5 A 0.04 -2.3 0.037 -1.0 35 8 / 5 A 1.23 1.4 0.011 -1.4 0.151 0.9
36 x 8 / 5 A 0.0786 -0.8 0.0496 0.0 36 x 8 / 5 A 0.721 -0.8 0.0171 0.1 0.0841 -1.3
37 9 / 6 A 16.4 0.3 0.087 -0.4 0.057 0.6 37 9 / 6 A 1.29 1.7 0.022 1.2 0.15 0.8
38 5 / 2 B 0.0483 -0.1 38 5 / 2 B 0.131 0.2
39 1 / 1 B 39 1 / 1 B 0.983 0.4
40 1 / 1 B 40 1 / 1 B 1.09 0.8
41 5 / 3 B 0.0686 1.6 41 5 / 3 B 1.17 1.2 0.0226 1.4
42 6 / 4 B 0.075 -0.9 0.038 -0.9 42 6 / 4 B 0.014 -0.7 0.111 -0.4
43 1 / 1 B 43 1 / 1 B 0.794 -0.5
44 2 / 1 B 44 2 / 1 B 1.989 4.8
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
EUPT-SRM13 | 2018 (Soybean Flour)
38
Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
45 9 / 6 B 15.9 0.1 0.186 3.7 0.022 -2.2 45 9 / 6 B 0.736 -0.7 0.02 0.7 0.141 0.6
46 9 / 6 A 15.12 -0.1 0.106 0.4 0.047 -0.2 46 9 / 6 A 0.912 0.0 0.016 -0.2 0.095 -0.9
47 0 / 0 B 47 0 / 0 B
48 9 / 6 A 32.6 4.5 0.0792 -0.7 0.0538 0.4 48 9 / 6 A 0.713 -0.8 0.0198 0.7 0.155 1.0
49 x 9 / 6 A 21.85 1.7 0.058 -1.6 0.033 -1.3 49 x 9 / 6 A 0.756 -0.7 0.019 0.5 0.655 17.2
50 9 / 6 A 17.1 0.5 0.0988 0.1 0.0472 -0.2 50 9 / 6 A 1.31 1.8 0.0192 0.6 0.124 0.0
51 x 7 / 4 B 17.1 0.5 0.097 0.0 51 x 7 / 4 B 0.97 0.3 0.122 -0.1
52 9 / 6 A 16.2 0.2 0.101 0.2 0.052 0.2 52 9 / 6 A 0.794 -0.5 0.018 0.3 0.115 -0.3
53 6 / 3 B 0.1 0.1 0.039 -0.8 53 6 / 3 B 0.096 -0.9
54 x 9 / 6 A 15.8 0.1 0.092 -0.2 0.044 -0.4 54 x 9 / 6 A 1.21 1.4 0.014 -0.7 0.126 0.1
55 9 / 6 A 12.9 -0.6 0.11 0.5 0.052 0.2 55 9 / 6 A 0.667 -1.0 0.019 0.5 0.133 0.3
56 9 / 6 A 13.1 -0.6 0.119 0.9 0.0613 1.0 56 9 / 6 A 0.916 0.1 0.023 1.5 0.103 -0.7
57 x 3 / 2 B 0.104 0.3 57 x 3 / 2 B 0.148 0.8
58 1 / 1 B 58 1 / 1 B 0.867 -0.2
59 0 / 0 B 59 0 / 0 B
60 8 / 5 A 0.117 0.8 0.0507 0.1 60 8 / 5 A 0.772 -0.6 0.0137 -0.7 0.12 -0.1
61 x 8 / 5 A 0.116 0.8 0.052 0.2 61 x 8 / 5 A 0.987 0.4 0.017 0.0 0.142 0.6
62 7 / 4 B 20.0 1.2 0.0446 -2.2 0.0413 -0.6 62 7 / 4 B 0.0117 -1.2
63 9 / 6 A 13.63 -0.4 0.103 0.3 0.053 0.3 63 9 / 6 A 0.68 -1.0 0.0155 -0.3 0.021 -3.3
64 2 / 1 B 64 2 / 1 B 0.751 -0.7
65 8 / 5 A FN -3.5 0.073 -1.0 0.054 0.4 65 8 / 5 A 0.65 -1.1 0.018 0.3 0.115 -0.3
66 5 / 2 B 0.054 0.4 66 5 / 2 B 0.023 1.5 FN -3.7
67 7 / 5 B 14.1 -0.3 0.0379 -2.4 0.0345 -1.2 67 7 / 5 B 1.09 0.8 0.108 -0.5
68 x 8 / 5 A 13.7 -0.4 0.143 1.9 0.043 -0.5 68 x 8 / 5 A 0.0058 -2.6 0.173 1.6
69 9 / 6 A 13.7 -0.4 0.095 -0.1 0.047 -0.2 69 9 / 6 A 0.849 -0.2 0.014 -0.7 0.107 -0.5
70 3 / 2 B 70 3 / 2 B 0.962 0.3 0.128 0.1
71 8 / 5 A 0.0996 0.1 0.0516 0.2 71 8 / 5 A 0.788 -0.5 0.014 -0.7 0.112 -0.4
72 9 / 6 A 14.1 -0.3 0.0894 -0.3 0.0431 -0.5 72 9 / 6 A 0.896 0.0 0.0164 -0.1 0.093 -1.0
73 8 / 5 A 0.22 5.1 0.074 2.0 73 8 / 5 A 0.833 -0.3 0.022 1.2 0.127 0.1
74 x 9 / 6 A 4.29 -2.9 0.0472 -2.1 0.0431 -0.5 74 x 9 / 6 A 0.56 -1.5 0.0168 0.0 0.133 0.3
76 x 8 / 5 A 0.0716 -1.0 0.0287 -1.7 76 x 8 / 5 A 0.69 -0.9 0.0166 -0.1 0.0657 -1.9
77 x 3 / 2 B 0.084 -0.5 77 x 3 / 2 B 0.122 -0.1
78 x 9 / 6 A 12.4 -0.8 0.045 -2.1 0.055 0.5 78 x 9 / 6 A 0.722 -0.8 0.025 1.9 0.109 -0.5
79 x 9 / 6 A 12.5 -0.7 0.094 -0.1 0.05 0.1 79 x 9 / 6 A 1.182 1.2 0.015 -0.4 0.11 -0.4
80 x 6 / 4 B 0.062 1.0 80 x 6 / 4 B 2.3 6.2 0.025 1.9 0.131 0.2
82 3 / 2 B 17.0 0.4 0.096 0.0 82 3 / 2 B
83 9 / 6 A 3.0 -3.2 0.104 0.3 0.047 -0.2 83 9 / 6 A 0.48 -1.9 0.016 -0.2 0.028 -3.1
84 4 / 3 B 0.12 1.0 0.069 1.6 84 4 / 3 B 0.017 0.0
85 8 / 5 A 9.0 -1.7 0.132 1.4 0.038 -0.9 85 8 / 5 A 0.02 0.7 0.185 2.0
86 8 / 5 A 0.116 0.8 0.0538 0.4 86 8 / 5 A 0.896 0.0 0.0236 1.6 0.165 1.3
87 8 / 5 A 0.0898 -0.3 0.0451 -0.3 87 8 / 5 A 0.692 -0.9 0.017 0.0 0.111 -0.4
88 9 / 6 A 16.9 0.4 0.0263 -2.9 0.048 -0.1 88 9 / 6 A 1.1 0.9 0.014 -0.7 0.104 -0.6
89 9 / 6 A 16.5 0.3 0.081 -0.7 0.051 0.1 89 9 / 6 A 0.931 0.1 0.015 -0.4 0.075 -1.6
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
4. RESULTS / Assessment of Laboratory Performance
39
Resu
lts
4
Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
45 9 / 6 B 15.9 0.1 0.186 3.7 0.022 -2.2 45 9 / 6 B 0.736 -0.7 0.02 0.7 0.141 0.6
46 9 / 6 A 15.12 -0.1 0.106 0.4 0.047 -0.2 46 9 / 6 A 0.912 0.0 0.016 -0.2 0.095 -0.9
47 0 / 0 B 47 0 / 0 B
48 9 / 6 A 32.6 4.5 0.0792 -0.7 0.0538 0.4 48 9 / 6 A 0.713 -0.8 0.0198 0.7 0.155 1.0
49 x 9 / 6 A 21.85 1.7 0.058 -1.6 0.033 -1.3 49 x 9 / 6 A 0.756 -0.7 0.019 0.5 0.655 17.2
50 9 / 6 A 17.1 0.5 0.0988 0.1 0.0472 -0.2 50 9 / 6 A 1.31 1.8 0.0192 0.6 0.124 0.0
51 x 7 / 4 B 17.1 0.5 0.097 0.0 51 x 7 / 4 B 0.97 0.3 0.122 -0.1
52 9 / 6 A 16.2 0.2 0.101 0.2 0.052 0.2 52 9 / 6 A 0.794 -0.5 0.018 0.3 0.115 -0.3
53 6 / 3 B 0.1 0.1 0.039 -0.8 53 6 / 3 B 0.096 -0.9
54 x 9 / 6 A 15.8 0.1 0.092 -0.2 0.044 -0.4 54 x 9 / 6 A 1.21 1.4 0.014 -0.7 0.126 0.1
55 9 / 6 A 12.9 -0.6 0.11 0.5 0.052 0.2 55 9 / 6 A 0.667 -1.0 0.019 0.5 0.133 0.3
56 9 / 6 A 13.1 -0.6 0.119 0.9 0.0613 1.0 56 9 / 6 A 0.916 0.1 0.023 1.5 0.103 -0.7
57 x 3 / 2 B 0.104 0.3 57 x 3 / 2 B 0.148 0.8
58 1 / 1 B 58 1 / 1 B 0.867 -0.2
59 0 / 0 B 59 0 / 0 B
60 8 / 5 A 0.117 0.8 0.0507 0.1 60 8 / 5 A 0.772 -0.6 0.0137 -0.7 0.12 -0.1
61 x 8 / 5 A 0.116 0.8 0.052 0.2 61 x 8 / 5 A 0.987 0.4 0.017 0.0 0.142 0.6
62 7 / 4 B 20.0 1.2 0.0446 -2.2 0.0413 -0.6 62 7 / 4 B 0.0117 -1.2
63 9 / 6 A 13.63 -0.4 0.103 0.3 0.053 0.3 63 9 / 6 A 0.68 -1.0 0.0155 -0.3 0.021 -3.3
64 2 / 1 B 64 2 / 1 B 0.751 -0.7
65 8 / 5 A FN -3.5 0.073 -1.0 0.054 0.4 65 8 / 5 A 0.65 -1.1 0.018 0.3 0.115 -0.3
66 5 / 2 B 0.054 0.4 66 5 / 2 B 0.023 1.5 FN -3.7
67 7 / 5 B 14.1 -0.3 0.0379 -2.4 0.0345 -1.2 67 7 / 5 B 1.09 0.8 0.108 -0.5
68 x 8 / 5 A 13.7 -0.4 0.143 1.9 0.043 -0.5 68 x 8 / 5 A 0.0058 -2.6 0.173 1.6
69 9 / 6 A 13.7 -0.4 0.095 -0.1 0.047 -0.2 69 9 / 6 A 0.849 -0.2 0.014 -0.7 0.107 -0.5
70 3 / 2 B 70 3 / 2 B 0.962 0.3 0.128 0.1
71 8 / 5 A 0.0996 0.1 0.0516 0.2 71 8 / 5 A 0.788 -0.5 0.014 -0.7 0.112 -0.4
72 9 / 6 A 14.1 -0.3 0.0894 -0.3 0.0431 -0.5 72 9 / 6 A 0.896 0.0 0.0164 -0.1 0.093 -1.0
73 8 / 5 A 0.22 5.1 0.074 2.0 73 8 / 5 A 0.833 -0.3 0.022 1.2 0.127 0.1
74 x 9 / 6 A 4.29 -2.9 0.0472 -2.1 0.0431 -0.5 74 x 9 / 6 A 0.56 -1.5 0.0168 0.0 0.133 0.3
76 x 8 / 5 A 0.0716 -1.0 0.0287 -1.7 76 x 8 / 5 A 0.69 -0.9 0.0166 -0.1 0.0657 -1.9
77 x 3 / 2 B 0.084 -0.5 77 x 3 / 2 B 0.122 -0.1
78 x 9 / 6 A 12.4 -0.8 0.045 -2.1 0.055 0.5 78 x 9 / 6 A 0.722 -0.8 0.025 1.9 0.109 -0.5
79 x 9 / 6 A 12.5 -0.7 0.094 -0.1 0.05 0.1 79 x 9 / 6 A 1.182 1.2 0.015 -0.4 0.11 -0.4
80 x 6 / 4 B 0.062 1.0 80 x 6 / 4 B 2.3 6.2 0.025 1.9 0.131 0.2
82 3 / 2 B 17.0 0.4 0.096 0.0 82 3 / 2 B
83 9 / 6 A 3.0 -3.2 0.104 0.3 0.047 -0.2 83 9 / 6 A 0.48 -1.9 0.016 -0.2 0.028 -3.1
84 4 / 3 B 0.12 1.0 0.069 1.6 84 4 / 3 B 0.017 0.0
85 8 / 5 A 9.0 -1.7 0.132 1.4 0.038 -0.9 85 8 / 5 A 0.02 0.7 0.185 2.0
86 8 / 5 A 0.116 0.8 0.0538 0.4 86 8 / 5 A 0.896 0.0 0.0236 1.6 0.165 1.3
87 8 / 5 A 0.0898 -0.3 0.0451 -0.3 87 8 / 5 A 0.692 -0.9 0.017 0.0 0.111 -0.4
88 9 / 6 A 16.9 0.4 0.0263 -2.9 0.048 -0.1 88 9 / 6 A 1.1 0.9 0.014 -0.7 0.104 -0.6
89 9 / 6 A 16.5 0.3 0.081 -0.7 0.051 0.1 89 9 / 6 A 0.931 0.1 0.015 -0.4 0.075 -1.6
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
EUPT-SRM13 | 2018 (Soybean Flour)
40
Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
90 1 / 0 B FN -3.6 90 1 / 0 B
91 9 / 6 A 12.4 -0.8 0.108 0.5 0.0579 0.7 91 9 / 6 A 1.01 0.5 0.0142 -0.6 0.149 0.8
92 9 / 6 A 12.9 -0.6 0.115 0.7 0.0403 -0.7 92 9 / 6 A 0.967 0.3 0.014 -0.7 0.137 0.4
93 9 / 6 A 13.0 -0.6 0.111 0.6 0.055 0.5 93 9 / 6 A 0.82 -0.4 0.018 0.3 0.15 0.8
94 1 / 1 B 18.473 0.8 94 1 / 1 B
95 1 / 1 B 95 1 / 1 B 0.121 -0.1
96 7 / 5 B 0.0895 -0.3 0.058 0.7 96 7 / 5 B 0.954 0.2 0.0166 -0.1 0.0986 -0.8
97 9 / 6 A 27.9 3.3 0.102 0.2 0.048 -0.1 97 9 / 6 A 0.832 -0.3 0.019 0.5 0.027 -3.1
98 9 / 6 A 11.6 -1.0 0.084 -0.5 0.054 0.4 98 9 / 6 A 0.859 -0.2 0.018 0.3 0.125 0.0
99 2 / 1 B 99 2 / 1 B 0.115 -0.3
100 x 4 / 3 B 16.3 0.2 0.049 0.0 100 x 4 / 3 B 0.019 0.5
101 8 / 5 A 0.101 0.2 0.025 -2.0 101 8 / 5 A 1.038 0.6 0.009 -1.9 0.198 2.4
102 1 / 1 B 7.82 -2.0 102 1 / 1 B
103 1 / 1 B 103 1 / 1 B 13.5 55.8
104 9 / 6 A 23.0 2.0 0.075 -0.9 0.025 -2.0 104 9 / 6 A 0.678 -1.0 0.012 -1.2 0.11 -0.4
105 9 / 6 A 10.3 -1.3 0.088 -0.4 0.041 -0.7 105 9 / 6 A 0.366 -2.4 0.0071 -2.3 0.19 2.1
106 5 / 3 B 0.94 34.8 106 5 / 3 B 0.93 0.1 0.1 -0.8
107 6 / 4 B 0.06 0.9 107 6 / 4 B 0.93 0.1 0.02 0.7 0.09 -1.1
109 8 / 5 A 0.168 2.9 0.0451 -0.3 109 8 / 5 A 0.824 -0.3 0.0199 0.7 0.122 -0.1
110 4 / 2 B 110 4 / 2 B 0.55 -1.6 0.143 0.6
111 4 / 2 B 19.9 1.2 111 4 / 2 B 0.089 -1.1
112 9 / 6 A 12.0 -0.9 0.12 1.0 0.06 0.9 112 9 / 6 A 0.85 -0.2 0.02 0.7 0.117 -0.2
113 0 / 0 B 113 0 / 0 B
114 0 / 0 B 114 0 / 0 B
3rd-115 6 / 3 B 0.087 -0.4 3rd-115 6 / 3 B 1.07 0.7 FN -3.3 0.123 0.0
3rd-116 8 / 5 B 12.9 -0.6 0.07 -1.1 3rd-116 8 / 5 B 0.6 -1.3 0.007 -2.3 0.11 -0.4
3rd-117 9 / 6 A 15.8 0.1 0.0689 -1.2 0.0433 -0.5 3rd-117 9 / 6 A 0.175 -3.2 0.0119 -1.2 0.152 0.9
3rd-118 6 / 3 B 14.4 -0.2 0.0831 -0.6 FN -3.2 3rd-118 6 / 3 B 0.715 -0.8
3rd-119 2 / 1 B 0.0407 -0.7 3rd-119 2 / 1 B
3rd-120 3 / 1 B 3rd-120 3 / 1 B 0.9 0.0
3rd-121 1 / 1 B 3rd-121 1 / 1 B 0.919 0.1
3rd-122 7 / 5 B 16.8 0.4 0.147 2.1 3rd-122 7 / 5 B 0.903 0.0 0.019 0.5 0.27 4.7
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
4. RESULTS / Assessment of Laboratory Performance
41
Resu
lts
4
Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds
COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
90 1 / 0 B FN -3.6 90 1 / 0 B
91 9 / 6 A 12.4 -0.8 0.108 0.5 0.0579 0.7 91 9 / 6 A 1.01 0.5 0.0142 -0.6 0.149 0.8
92 9 / 6 A 12.9 -0.6 0.115 0.7 0.0403 -0.7 92 9 / 6 A 0.967 0.3 0.014 -0.7 0.137 0.4
93 9 / 6 A 13.0 -0.6 0.111 0.6 0.055 0.5 93 9 / 6 A 0.82 -0.4 0.018 0.3 0.15 0.8
94 1 / 1 B 18.473 0.8 94 1 / 1 B
95 1 / 1 B 95 1 / 1 B 0.121 -0.1
96 7 / 5 B 0.0895 -0.3 0.058 0.7 96 7 / 5 B 0.954 0.2 0.0166 -0.1 0.0986 -0.8
97 9 / 6 A 27.9 3.3 0.102 0.2 0.048 -0.1 97 9 / 6 A 0.832 -0.3 0.019 0.5 0.027 -3.1
98 9 / 6 A 11.6 -1.0 0.084 -0.5 0.054 0.4 98 9 / 6 A 0.859 -0.2 0.018 0.3 0.125 0.0
99 2 / 1 B 99 2 / 1 B 0.115 -0.3
100 x 4 / 3 B 16.3 0.2 0.049 0.0 100 x 4 / 3 B 0.019 0.5
101 8 / 5 A 0.101 0.2 0.025 -2.0 101 8 / 5 A 1.038 0.6 0.009 -1.9 0.198 2.4
102 1 / 1 B 7.82 -2.0 102 1 / 1 B
103 1 / 1 B 103 1 / 1 B 13.5 55.8
104 9 / 6 A 23.0 2.0 0.075 -0.9 0.025 -2.0 104 9 / 6 A 0.678 -1.0 0.012 -1.2 0.11 -0.4
105 9 / 6 A 10.3 -1.3 0.088 -0.4 0.041 -0.7 105 9 / 6 A 0.366 -2.4 0.0071 -2.3 0.19 2.1
106 5 / 3 B 0.94 34.8 106 5 / 3 B 0.93 0.1 0.1 -0.8
107 6 / 4 B 0.06 0.9 107 6 / 4 B 0.93 0.1 0.02 0.7 0.09 -1.1
109 8 / 5 A 0.168 2.9 0.0451 -0.3 109 8 / 5 A 0.824 -0.3 0.0199 0.7 0.122 -0.1
110 4 / 2 B 110 4 / 2 B 0.55 -1.6 0.143 0.6
111 4 / 2 B 19.9 1.2 111 4 / 2 B 0.089 -1.1
112 9 / 6 A 12.0 -0.9 0.12 1.0 0.06 0.9 112 9 / 6 A 0.85 -0.2 0.02 0.7 0.117 -0.2
113 0 / 0 B 113 0 / 0 B
114 0 / 0 B 114 0 / 0 B
3rd-115 6 / 3 B 0.087 -0.4 3rd-115 6 / 3 B 1.07 0.7 FN -3.3 0.123 0.0
3rd-116 8 / 5 B 12.9 -0.6 0.07 -1.1 3rd-116 8 / 5 B 0.6 -1.3 0.007 -2.3 0.11 -0.4
3rd-117 9 / 6 A 15.8 0.1 0.0689 -1.2 0.0433 -0.5 3rd-117 9 / 6 A 0.175 -3.2 0.0119 -1.2 0.152 0.9
3rd-118 6 / 3 B 14.4 -0.2 0.0831 -0.6 FN -3.2 3rd-118 6 / 3 B 0.715 -0.8
3rd-119 2 / 1 B 0.0407 -0.7 3rd-119 2 / 1 B
3rd-120 3 / 1 B 3rd-120 3 / 1 B 0.9 0.0
3rd-121 1 / 1 B 3rd-121 1 / 1 B 0.919 0.1
3rd-122 7 / 5 B 16.8 0.4 0.147 2.1 3rd-122 7 / 5 B 0.903 0.0 0.019 0.5 0.27 4.7
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)
EUPT-SRM13 | 2018 (Soybean Flour)
42
Table 4-9: Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
1 7 / 2 A 0.231 1.0 1 7 / 2 A 0.0455 -0.5 1.2 -1.2
2 12 / 5 B 0.174 -0.2 0.137 -1.1 2 12 / 5 B FN -3.6 0.142 -3.7 0.083 2.4 2.94 2.9
3 4 / 1 B 0.146 -0.8 3 4 / 1 B 0.054 0.2
4 x 9 / 5 A 0.187 -0.1 0.862 0.1 4 x 9 / 5 A 0.101 0.1 2.38 1.1 0.0572 0.4
5 x 4 / 1 B 5 x 4 / 1 B 0.0842 -0.6
6 6 / 3 A 6 6 / 3 A 0.115 0.6 1.973 0.2
7 x 4 / 1 B 0.1557 -0.6 7 x 4 / 1 B 0.0395 -1.0
8 x 6 / 3 A 0.156 -0.6 0.644 -0.9 8 x 6 / 3 A 0.113 0.5 0.0377 -1.1
10 7 / 3 A 10 7 / 3 A 0.0996 0.0 0.902 -2.1
11 10 / 4 A 0.225 0.9 11 10 / 4 A 0.0915 -0.3 FN -3.9
12 x 6 / 2 A 0.16 -0.5 0.803 -0.2 12 x 6 / 2 A 0.055 0.2
13 x 13 / 8 A 0.285 2.2 0.194 0.1 0.215 0.6 0.784 -0.2 13 x 13 / 8 A 0.109 0.4 2.36 1.1 0.0557 0.3 7.59 13.8
14 14 / 8 A 0.192 0.2 0.131 -1.3 14 14 / 8 A 0.104 0.2 1.59 -0.6 0.0512 -0.1 1.39 -0.7
15 11 / 6 A 0.261 1.4 0.173 -0.3 0.613 -1.1 15 11 / 6 A 0.0726 -1.1 2.01 0.3
16 12 / 7 A 0.219 0.8 0.286 2.0 16 12 / 7 A 0.093 -0.3 1.6 -0.6 0.066 1.1
17 9 / 6 B 0.0687 -2.6 17 9 / 6 B 0.0763 -0.9 1.94 0.2 0.0546 0.2
19 x 4 / 1 A 0.232 1.1 19 x 4 / 1 A 0.065 1.0
20 x 4 / 2 A 0.157 -0.6 20 x 4 / 2 A 0.0968 -0.1 0.0437 -0.6
21 7 / 2 A 0.863 0.1 21 7 / 2 A 0.043 -0.7 0.529 -2.8
22 x 5 / 2 A 0.2 0.4 0.198 0.1 22 x 5 / 2 A
23 4 / 1 B 0.2 0.4 23 4 / 1 B 0.056 0.3
24 x 3 / 1 A 0.19 0.2 24 x 3 / 1 A 0.059 0.5
25 2 / 0 B 25 2 / 0 B
26 8 / 5 A 0.14 -0.9 0.16 -0.7 26 8 / 5 A 0.16 2.4 2.2 0.7 0.023 -2.2
27 13 / 6 A 0.24 1.0 0.17 -0.4 27 13 / 6 A 0.12 0.8 1.623 -0.5 0.03 -1.7 2.44 1.7
28 0 / 0 B 28 0 / 0 B
29 x 2 / 0 A 29 x 2 / 0 A 0.071 1.5
30 x 15 / 8 A 0.203 0.4 0.189 -0.1 0.189 0.0 1.18 1.7 30 x 15 / 8 A 0.093 -0.3 2.05 0.4 0.062 0.8 1.35 -0.8
31 10 / 4 A 31 10 / 4 A 0.092 -0.3 1.47 -0.8 0.878 -1.9
32 x 13 / 7 A 0.142 -0.9 32 x 13 / 7 A 0.096 -0.1 1.98 0.2 0.0515 0.0 1.59 -0.3
33 10 / 5 A 0.218 0.8 0.18 -0.2 33 10 / 5 A 0.097 -0.1 1.91 0.1 0.061 0.7
34 17 / 10 A 0.176 -0.2 0.201 0.2 0.181 -0.1 16.685 76.0 34 17 / 10 A 0.089 -0.4 1.982 0.3 0.058 0.5 1.979 0.7
35 12 / 7 A 0.131 -1.1 0.183 -0.2 0.307 2.5 35 12 / 7 A 0.048 -2.1 1.278 -1.3 0.037 -1.1 1.563 -0.3
36 x 13 / 8 A 0.197 0.3 0.154 -0.8 0.171 -0.4 0.733 -0.5 36 x 13 / 8 A 0.0728 -1.1 1.65 -0.5 0.0505 -0.1 0.742 -2.3
37 8 / 5 A 0.24 1.0 0.19 0.0 37 8 / 5 A 0.11 0.4 2.04 0.4
38 3 / 1 B 38 3 / 1 B 0.102 0.1 0.0499 -0.2
39 0 / 0 B 39 0 / 0 B
40 1 / 0 B 40 1 / 0 B
41 8 / 6 B 0.217 0.7 0.23 0.8 0.159 -0.6 0.743 -0.4 41 8 / 6 B 7.5 12.1 0.0713 1.5
42 2 / 0 B 42 2 / 0 B 0.052 0.0
43 1 / 0 B 43 1 / 0 B
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
4. RESULTS / Assessment of Laboratory Performance
43
Resu
lts
4
Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
1 7 / 2 A 0.231 1.0 1 7 / 2 A 0.0455 -0.5 1.2 -1.2
2 12 / 5 B 0.174 -0.2 0.137 -1.1 2 12 / 5 B FN -3.6 0.142 -3.7 0.083 2.4 2.94 2.9
3 4 / 1 B 0.146 -0.8 3 4 / 1 B 0.054 0.2
4 x 9 / 5 A 0.187 -0.1 0.862 0.1 4 x 9 / 5 A 0.101 0.1 2.38 1.1 0.0572 0.4
5 x 4 / 1 B 5 x 4 / 1 B 0.0842 -0.6
6 6 / 3 A 6 6 / 3 A 0.115 0.6 1.973 0.2
7 x 4 / 1 B 0.1557 -0.6 7 x 4 / 1 B 0.0395 -1.0
8 x 6 / 3 A 0.156 -0.6 0.644 -0.9 8 x 6 / 3 A 0.113 0.5 0.0377 -1.1
10 7 / 3 A 10 7 / 3 A 0.0996 0.0 0.902 -2.1
11 10 / 4 A 0.225 0.9 11 10 / 4 A 0.0915 -0.3 FN -3.9
12 x 6 / 2 A 0.16 -0.5 0.803 -0.2 12 x 6 / 2 A 0.055 0.2
13 x 13 / 8 A 0.285 2.2 0.194 0.1 0.215 0.6 0.784 -0.2 13 x 13 / 8 A 0.109 0.4 2.36 1.1 0.0557 0.3 7.59 13.8
14 14 / 8 A 0.192 0.2 0.131 -1.3 14 14 / 8 A 0.104 0.2 1.59 -0.6 0.0512 -0.1 1.39 -0.7
15 11 / 6 A 0.261 1.4 0.173 -0.3 0.613 -1.1 15 11 / 6 A 0.0726 -1.1 2.01 0.3
16 12 / 7 A 0.219 0.8 0.286 2.0 16 12 / 7 A 0.093 -0.3 1.6 -0.6 0.066 1.1
17 9 / 6 B 0.0687 -2.6 17 9 / 6 B 0.0763 -0.9 1.94 0.2 0.0546 0.2
19 x 4 / 1 A 0.232 1.1 19 x 4 / 1 A 0.065 1.0
20 x 4 / 2 A 0.157 -0.6 20 x 4 / 2 A 0.0968 -0.1 0.0437 -0.6
21 7 / 2 A 0.863 0.1 21 7 / 2 A 0.043 -0.7 0.529 -2.8
22 x 5 / 2 A 0.2 0.4 0.198 0.1 22 x 5 / 2 A
23 4 / 1 B 0.2 0.4 23 4 / 1 B 0.056 0.3
24 x 3 / 1 A 0.19 0.2 24 x 3 / 1 A 0.059 0.5
25 2 / 0 B 25 2 / 0 B
26 8 / 5 A 0.14 -0.9 0.16 -0.7 26 8 / 5 A 0.16 2.4 2.2 0.7 0.023 -2.2
27 13 / 6 A 0.24 1.0 0.17 -0.4 27 13 / 6 A 0.12 0.8 1.623 -0.5 0.03 -1.7 2.44 1.7
28 0 / 0 B 28 0 / 0 B
29 x 2 / 0 A 29 x 2 / 0 A 0.071 1.5
30 x 15 / 8 A 0.203 0.4 0.189 -0.1 0.189 0.0 1.18 1.7 30 x 15 / 8 A 0.093 -0.3 2.05 0.4 0.062 0.8 1.35 -0.8
31 10 / 4 A 31 10 / 4 A 0.092 -0.3 1.47 -0.8 0.878 -1.9
32 x 13 / 7 A 0.142 -0.9 32 x 13 / 7 A 0.096 -0.1 1.98 0.2 0.0515 0.0 1.59 -0.3
33 10 / 5 A 0.218 0.8 0.18 -0.2 33 10 / 5 A 0.097 -0.1 1.91 0.1 0.061 0.7
34 17 / 10 A 0.176 -0.2 0.201 0.2 0.181 -0.1 16.685 76.0 34 17 / 10 A 0.089 -0.4 1.982 0.3 0.058 0.5 1.979 0.7
35 12 / 7 A 0.131 -1.1 0.183 -0.2 0.307 2.5 35 12 / 7 A 0.048 -2.1 1.278 -1.3 0.037 -1.1 1.563 -0.3
36 x 13 / 8 A 0.197 0.3 0.154 -0.8 0.171 -0.4 0.733 -0.5 36 x 13 / 8 A 0.0728 -1.1 1.65 -0.5 0.0505 -0.1 0.742 -2.3
37 8 / 5 A 0.24 1.0 0.19 0.0 37 8 / 5 A 0.11 0.4 2.04 0.4
38 3 / 1 B 38 3 / 1 B 0.102 0.1 0.0499 -0.2
39 0 / 0 B 39 0 / 0 B
40 1 / 0 B 40 1 / 0 B
41 8 / 6 B 0.217 0.7 0.23 0.8 0.159 -0.6 0.743 -0.4 41 8 / 6 B 7.5 12.1 0.0713 1.5
42 2 / 0 B 42 2 / 0 B 0.052 0.0
43 1 / 0 B 43 1 / 0 B
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
EUPT-SRM13 | 2018 (Soybean Flour)
44
Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
44 6 / 2 B 0.319 2.7 44 6 / 2 B 0.138 1.5
45 15 / 7 B 0.194 0.2 0.24 1.0 1.08 19.0 FN -3.9 45 15 / 7 B 0.143 1.7 1.17 -1.5 0.07 1.4 2.62 2.2
46 15 / 8 A 0.182 0.0 0.174 -0.4 0.17 -0.4 0.71 -0.6 46 15 / 8 A 0.102 0.1 1.93 0.1 0.049 -0.2 5.07 7.9
47 1 / 0 B 47 1 / 0 B FN -4.0
48 8 / 3 A 48 8 / 3 A 0.0892 -0.4 2.07 0.4 0.0463 -0.4
49 x 2 / 1 A 0.164 -0.4 49 x 2 / 1 A 0.057 0.4
50 8 / 4 A 0.183 0.0 50 8 / 4 A 0.101 0.1 2.29 0.9
51 x 0 / 0 B 51 x 0 / 0 B
52 13 / 7 A 0.216 0.7 0.205 0.3 0.225 0.8 52 13 / 7 A 0.11 0.4 1.84 -0.1 0.0504 -0.1 3.116 3.3
53 1 / 0 B 53 1 / 0 B
54 x 4 / 0 A 54 x 4 / 0 A 0.04 -0.9
55 8 / 2 A FN -3.8 FN -3.6 FN -3.9 55 8 / 2 A 1.4 -1.0 0.056 0.3
56 4 / 1 A 56 4 / 1 A 0.098 -0.1 0.0596 0.6
57 x 3 / 1 B 57 x 3 / 1 B 0.102 0.1
58 1 / 0 B 58 1 / 0 B
59 1 / 0 B 59 1 / 0 B
60 9 / 4 A 0.176 -0.2 0.172 -0.4 0.165 -0.5 60 9 / 4 A 0.0925 -0.3 0.0502 -0.1
61 x 2 / 0 A 61 x 2 / 0 A
62 9 / 5 B 0.371 3.7 62 9 / 5 B 0.115 0.6 1.96 0.2 0.0568 0.4 0.864 -2.0
63 15 / 8 A 0.19 0.2 0.7 10.6 0.156 -0.7 0.769 -0.3 63 15 / 8 A 0.033 -2.7 0.387 -3.2 0.044 -0.6 0.43 -3.0
64 2 / 0 B 64 2 / 0 B
65 2 / 0 A 65 2 / 0 A
66 2 / 0 B 66 2 / 0 B FN -3.2
67 9 / 5 B 0.177 -0.3 0.173 -0.3 67 9 / 5 B 0.0825 -0.7 1.95 0.2 0.0301 -1.7
68 x 2 / 0 A 68 x 2 / 0 A
69 8 / 4 A 0.234 1.1 69 8 / 4 A 0.193 3.7 1.86 0.0 0.046 -0.5
70 0 / 0 B 70 0 / 0 B
71 11 / 5 A 0.155 -0.6 0.203 0.2 0.977 0.7 71 11 / 5 A 0.117 0.7 1.25 -1.1
72 8 / 4 A 0.164 -0.4 72 8 / 4 A 0.0921 -0.3 1.75 -0.2 0.0486 -0.3
73 4 / 1 A 0.152 -0.8 73 4 / 1 A
74 x 3 / 1 A 0.139 -1.0 74 x 3 / 1 A
76 x 9 / 3 A 0.174 -0.2 0.166 -0.5 FN -3.9 76 x 9 / 3 A 0.0221 -2.3 3.48 4.2
77 x 1 / 0 B 77 x 1 / 0 B
78 x 1 / 1 A 0.133 -1.2 78 x 1 / 1 A
79 x 7 / 4 A 0.132 -1.1 0.105 -1.8 79 x 7 / 4 A 0.041 -0.8
80 x 2 / 0 B 80 x 2 / 0 B
82 2 / 0 B 82 2 / 0 B
83 15 / 8 A 0.19 0.2 0.13 -1.3 0.15 -0.8 0.65 -0.9 83 15 / 8 A 0.023 -3.1 0.37 -3.2 0.055 0.2 1.5 -0.5
84 1 / 0 B 84 1 / 0 B
85 7 / 2 A 0.173 -0.2 85 7 / 2 A 0.102 0.1 FN -3.9
86 11 / 6 A 0.319 3.0 0.224 0.7 0.979 0.7 86 11 / 6 A 2.13 0.6 0.0517 0.0 1.28 -1.0
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
4. RESULTS / Assessment of Laboratory Performance
45
Resu
lts
4
Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
44 6 / 2 B 0.319 2.7 44 6 / 2 B 0.138 1.5
45 15 / 7 B 0.194 0.2 0.24 1.0 1.08 19.0 FN -3.9 45 15 / 7 B 0.143 1.7 1.17 -1.5 0.07 1.4 2.62 2.2
46 15 / 8 A 0.182 0.0 0.174 -0.4 0.17 -0.4 0.71 -0.6 46 15 / 8 A 0.102 0.1 1.93 0.1 0.049 -0.2 5.07 7.9
47 1 / 0 B 47 1 / 0 B FN -4.0
48 8 / 3 A 48 8 / 3 A 0.0892 -0.4 2.07 0.4 0.0463 -0.4
49 x 2 / 1 A 0.164 -0.4 49 x 2 / 1 A 0.057 0.4
50 8 / 4 A 0.183 0.0 50 8 / 4 A 0.101 0.1 2.29 0.9
51 x 0 / 0 B 51 x 0 / 0 B
52 13 / 7 A 0.216 0.7 0.205 0.3 0.225 0.8 52 13 / 7 A 0.11 0.4 1.84 -0.1 0.0504 -0.1 3.116 3.3
53 1 / 0 B 53 1 / 0 B
54 x 4 / 0 A 54 x 4 / 0 A 0.04 -0.9
55 8 / 2 A FN -3.8 FN -3.6 FN -3.9 55 8 / 2 A 1.4 -1.0 0.056 0.3
56 4 / 1 A 56 4 / 1 A 0.098 -0.1 0.0596 0.6
57 x 3 / 1 B 57 x 3 / 1 B 0.102 0.1
58 1 / 0 B 58 1 / 0 B
59 1 / 0 B 59 1 / 0 B
60 9 / 4 A 0.176 -0.2 0.172 -0.4 0.165 -0.5 60 9 / 4 A 0.0925 -0.3 0.0502 -0.1
61 x 2 / 0 A 61 x 2 / 0 A
62 9 / 5 B 0.371 3.7 62 9 / 5 B 0.115 0.6 1.96 0.2 0.0568 0.4 0.864 -2.0
63 15 / 8 A 0.19 0.2 0.7 10.6 0.156 -0.7 0.769 -0.3 63 15 / 8 A 0.033 -2.7 0.387 -3.2 0.044 -0.6 0.43 -3.0
64 2 / 0 B 64 2 / 0 B
65 2 / 0 A 65 2 / 0 A
66 2 / 0 B 66 2 / 0 B FN -3.2
67 9 / 5 B 0.177 -0.3 0.173 -0.3 67 9 / 5 B 0.0825 -0.7 1.95 0.2 0.0301 -1.7
68 x 2 / 0 A 68 x 2 / 0 A
69 8 / 4 A 0.234 1.1 69 8 / 4 A 0.193 3.7 1.86 0.0 0.046 -0.5
70 0 / 0 B 70 0 / 0 B
71 11 / 5 A 0.155 -0.6 0.203 0.2 0.977 0.7 71 11 / 5 A 0.117 0.7 1.25 -1.1
72 8 / 4 A 0.164 -0.4 72 8 / 4 A 0.0921 -0.3 1.75 -0.2 0.0486 -0.3
73 4 / 1 A 0.152 -0.8 73 4 / 1 A
74 x 3 / 1 A 0.139 -1.0 74 x 3 / 1 A
76 x 9 / 3 A 0.174 -0.2 0.166 -0.5 FN -3.9 76 x 9 / 3 A 0.0221 -2.3 3.48 4.2
77 x 1 / 0 B 77 x 1 / 0 B
78 x 1 / 1 A 0.133 -1.2 78 x 1 / 1 A
79 x 7 / 4 A 0.132 -1.1 0.105 -1.8 79 x 7 / 4 A 0.041 -0.8
80 x 2 / 0 B 80 x 2 / 0 B
82 2 / 0 B 82 2 / 0 B
83 15 / 8 A 0.19 0.2 0.13 -1.3 0.15 -0.8 0.65 -0.9 83 15 / 8 A 0.023 -3.1 0.37 -3.2 0.055 0.2 1.5 -0.5
84 1 / 0 B 84 1 / 0 B
85 7 / 2 A 0.173 -0.2 85 7 / 2 A 0.102 0.1 FN -3.9
86 11 / 6 A 0.319 3.0 0.224 0.7 0.979 0.7 86 11 / 6 A 2.13 0.6 0.0517 0.0 1.28 -1.0
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
EUPT-SRM13 | 2018 (Soybean Flour)
46
Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
87 5 / 2 A 0.146 -0.8 87 5 / 2 A 0.0679 -1.3 0.0508 -0.1
88 10 / 6 A 0.18 -0.1 0.247 1.2 0.233 1.0 88 10 / 6 A 0.11 0.4 2.12 0.5 0.052 0.0
89 15 / 6 A 0.167 -0.3 FN -3.6 0.162 -0.6 FN -3.9 89 15 / 6 A 0.102 0.1 2.24 0.8 0.052 0.0 1.45 -0.6
90 1 / 0 B 90 1 / 0 B
91 11 / 6 A 0.134 -1.1 0.215 0.6 0.72 -0.5 91 11 / 6 A 0.106 0.3 0.688 -2.5 0.0547 0.2
92 7 / 4 A 0.0954 -2.0 0.19 0.0 92 7 / 4 A 0.101 0.1 0.0332 -1.4 1.74 0.1
93 12 / 6 A 0.216 0.7 0.181 -0.2 93 12 / 6 A 0.14 1.6 2.4 1.1 0.068 1.2 1.8 0.2
94 0 / 0 B 94 0 / 0 B
95 0 / 0 B 95 0 / 0 B
96 1 / 0 B 96 1 / 0 B 0.0613 0.7
97 13 / 5 A 0.234 1.1 0.227 0.7 0.169 -0.4 97 13 / 5 A 0.099 0.0 FN -3.9 0.063 0.9 1.9 0.5
98 12 / 7 A 0.147 -0.8 0.199 0.2 98 12 / 7 A 0.102 0.1 2.45 1.3 0.054 0.2
99 1 / 0 B 99 1 / 0 B
100 x 0 / 0 B 100 x 0 / 0 B
101 14 / 7 A 0.104 -1.7 0.188 -0.1 0.617 9.1 101 14 / 7 A 0.335 9.5 2.133 0.6 0.023 -2.2 1.922 0.5
102 0 / 0 B 102 0 / 0 B
103 0 / 0 B 103 0 / 0 B
104 0 / 0 A 104 0 / 0 A
105 13 / 6 A 0.193 0.2 FN -3.6 0.066 -2.6 0.938 0.5 105 13 / 6 A 0.09 -0.4 1.67 -0.4 0.035 -1.3
106 3 / 2 B 106 3 / 2 B 2.4 1.1
107 7 / 3 B 0.16 -0.5 0.23 0.8 107 7 / 3 B 0.1 3.7 1.41 -0.7
109 12 / 1 A FN -3.8 0.114 -1.6 FN -3.6 FN -3.9 109 12 / 1 A FN -3.6 0.045 -0.5 FN -4.0
110 5 / 2 B 110 5 / 2 B 0.087 -0.5 0.768 -2.2
111 2 / 1 B 111 2 / 1 B 0.096 -0.1
112 17 / 10 A 0.24 1.2 0.185 -0.1 0.198 0.2 1.04 1.0 112 17 / 10 A 0.106 0.3 2.02 0.3 0.081 2.2 1.6 -0.2
113 2 / 2 B 113 2 / 2 B
114 2 / 2 B 114 2 / 2 B
3rd-115 5 / 2 B FN -3.8 0.183 -0.2 3rd-115 5 / 2 B FN -3.6 1.11 -1.4
3rd-116 4 / 2 B 0.166 -0.5 3rd-116 4 / 2 B 0.27 -3.4
3rd-117 5 / 2 A 0.131 -1.1 0.166 -0.5 3rd-117 5 / 2 A
3rd-118 6 / 1 B 3rd-118 6 / 1 B FN -3.6 0.913 -1.9
3rd-119 2 / 1 B 0.188 0.1 3rd-119 2 / 1 B
3rd-120 3 / 1 B 0.2 0.2 3rd-120 3 / 1 B
3rd-121 1 / 0 B FN -3.6 3rd-121 1 / 0 B
3rd-122 1 / 1 B 0.223 0.7 3rd-122 1 / 1 B
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
4. RESULTS / Assessment of Laboratory Performance
47
Resu
lts
4
Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds
COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate
COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat
MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02
Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)
CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Lab code
SRM13-
NRL-SRM
Analysed / corr. found, max. 13 / 8
Cat.* Conc. [mg/kg]
z-Score § (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
Conc. [mg/kg]
z-Score (FFP-RSD
= 25 %)
87 5 / 2 A 0.146 -0.8 87 5 / 2 A 0.0679 -1.3 0.0508 -0.1
88 10 / 6 A 0.18 -0.1 0.247 1.2 0.233 1.0 88 10 / 6 A 0.11 0.4 2.12 0.5 0.052 0.0
89 15 / 6 A 0.167 -0.3 FN -3.6 0.162 -0.6 FN -3.9 89 15 / 6 A 0.102 0.1 2.24 0.8 0.052 0.0 1.45 -0.6
90 1 / 0 B 90 1 / 0 B
91 11 / 6 A 0.134 -1.1 0.215 0.6 0.72 -0.5 91 11 / 6 A 0.106 0.3 0.688 -2.5 0.0547 0.2
92 7 / 4 A 0.0954 -2.0 0.19 0.0 92 7 / 4 A 0.101 0.1 0.0332 -1.4 1.74 0.1
93 12 / 6 A 0.216 0.7 0.181 -0.2 93 12 / 6 A 0.14 1.6 2.4 1.1 0.068 1.2 1.8 0.2
94 0 / 0 B 94 0 / 0 B
95 0 / 0 B 95 0 / 0 B
96 1 / 0 B 96 1 / 0 B 0.0613 0.7
97 13 / 5 A 0.234 1.1 0.227 0.7 0.169 -0.4 97 13 / 5 A 0.099 0.0 FN -3.9 0.063 0.9 1.9 0.5
98 12 / 7 A 0.147 -0.8 0.199 0.2 98 12 / 7 A 0.102 0.1 2.45 1.3 0.054 0.2
99 1 / 0 B 99 1 / 0 B
100 x 0 / 0 B 100 x 0 / 0 B
101 14 / 7 A 0.104 -1.7 0.188 -0.1 0.617 9.1 101 14 / 7 A 0.335 9.5 2.133 0.6 0.023 -2.2 1.922 0.5
102 0 / 0 B 102 0 / 0 B
103 0 / 0 B 103 0 / 0 B
104 0 / 0 A 104 0 / 0 A
105 13 / 6 A 0.193 0.2 FN -3.6 0.066 -2.6 0.938 0.5 105 13 / 6 A 0.09 -0.4 1.67 -0.4 0.035 -1.3
106 3 / 2 B 106 3 / 2 B 2.4 1.1
107 7 / 3 B 0.16 -0.5 0.23 0.8 107 7 / 3 B 0.1 3.7 1.41 -0.7
109 12 / 1 A FN -3.8 0.114 -1.6 FN -3.6 FN -3.9 109 12 / 1 A FN -3.6 0.045 -0.5 FN -4.0
110 5 / 2 B 110 5 / 2 B 0.087 -0.5 0.768 -2.2
111 2 / 1 B 111 2 / 1 B 0.096 -0.1
112 17 / 10 A 0.24 1.2 0.185 -0.1 0.198 0.2 1.04 1.0 112 17 / 10 A 0.106 0.3 2.02 0.3 0.081 2.2 1.6 -0.2
113 2 / 2 B 113 2 / 2 B
114 2 / 2 B 114 2 / 2 B
3rd-115 5 / 2 B FN -3.8 0.183 -0.2 3rd-115 5 / 2 B FN -3.6 1.11 -1.4
3rd-116 4 / 2 B 0.166 -0.5 3rd-116 4 / 2 B 0.27 -3.4
3rd-117 5 / 2 A 0.131 -1.1 0.166 -0.5 3rd-117 5 / 2 A
3rd-118 6 / 1 B 3rd-118 6 / 1 B FN -3.6 0.913 -1.9
3rd-119 2 / 1 B 0.188 0.1 3rd-119 2 / 1 B
3rd-120 3 / 1 B 0.2 0.2 3rd-120 3 / 1 B
3rd-121 1 / 0 B FN -3.6 3rd-121 1 / 0 B
3rd-122 1 / 1 B 0.223 0.7 3rd-122 1 / 1 B
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as
EUPT-SRM13 | 2018 (Soybean Flour)
48
4.4.4 Laboratory Classification Based on Scope
All participating laboratories having reported at least one result were classified into categories A or B ac-cording to the rules stated in Section 2.5 (p. 12). Following the rules defined in the General Protocol (8th Edition, see Appendix 8), a laboratory had to fulfill the following conditions in order to be classified into Category A in the present PT: a) analysis of at least eight out of the nine compulsory pesticides on the Target Pesticides List; b) correct detection of at least five out of the six compulsory pesticides present in the test item, and c) no false positive results.
A total of 64 EU and EFTA laboratories (59 %) were classified into Category A and 45 (41 %) into Category B. One out of the 8 EU candidate and third-country laboratories was classified into Category A. Considering only the compulsory compounds the laboratories from EU and EFTA countries classified into Category A achieved an overall AAZ of 0.8 (n = 362), whereas those classified into Category B achieved an overall AAZ of 1.1 (n = 110). When including laboratories from EU candidate and third countries, the AAZ for compsul-sory compounds remains the same (n = 367) and for optional compounds decreased to 1.0 (n = 131).
Table 4-10 and Table 4-11 (p. 50) show the details of laboratories classified into Category A and B, respec-tively. For informative purposes, the overall AAZ was calculated for laboratories with 5 or more individual z-scores among the compulsory compounds. For the AAZ calculation any z-scores > 5 were set at 5.
COMPULSORY Compounds Bromide ion Cyromazine Fluazifop Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %
Lab code SRM13-
NRL-SRM
Analysed / corr. found 1) z-Scores z-Scores z-Scores z-Scores z-Scores z-Scores AAZ 2)
1 8 / 5 1.3 0.3 0.1 -0.2 0.0 0.4
4 x 9 / 6 0.8 0.1 1.8 0.1 -0.2 0.0 0.5
6 9 / 6 -0.2 0.4 -0.1 0.2 -1.0 -0.3 0.4
8 x 9 / 6 0.3 0.6 -0.2 0.1 -0.4 -0.1 0.3
10 9 / 6 -0.1 -2.1 -2.3 0.4 -0.4 -0.4 1.0
11 9 / 6 -0.3 0.2 0.4 1.0 0.2 -0.9 0.5
12 x 9 / 6 -0.7 0.1 0.2 0.6 0.0 1.0 0.4
13 x 9 / 6 0.6 5.5 -0.9 0.7 -0.7 5.7 2.2
14 9 / 6 -0.1 0.6 1.7 -0.4 0.3 -0.1 0.5
15 9 / 6 -0.8 0.1 1.1 -0.8 0.3 0.1 0.5
16 9 / 6 1.0 -1.0 1.0 1.2 0.5 0.2 0.8
19 x 9 / 6 1.3 44.7 1.5 1.4 0.0 39.0 2.4
20 x 9 / 6 0.3 0.2 -0.6 0.3 -0.6 0.8 0.5
21 8 / 5 -0.3 -0.1 -0.3 -0.2 0.7 0.3
22 x 9 / 6 0.3 -0.8 -0.7 0.7 -0.5 0.3 0.6
24 x 8 / 5 1.0 1.3 0.4 1.0 1.4 1.0
26 9 / 6 -0.1 -0.5 -1.4 -1.1 -1.4 1.2 1.0
27 9 / 6 0.5 -0.5 -0.3 0.5 -1.6 0.8 0.7
29 x 9 / 6 2.1 -0.7 1.8 0.0 -0.4 -1.1 1.0
30 x 9 / 6 -0.6 0.7 0.0 0.6 7.6 0.8 1.3
31 9 / 6 0.7 -0.9 0.0 0.2 -0.2 -0.5 0.41) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned
values based on the entire population. For the calculation of the AAZ the value “5” was applied where the z-score was higher than 5 (shown in square brackets).
FN = false negative results
Table 4-10: Category A laboratories ordered by lab-codes
4. RESULTS / Assessment of Laboratory Performance
49
Resu
lts
4
COMPULSORY Compounds Bromide ion Cyromazine Fluazifop Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %
Lab code SRM13-
NRL-SRM
Analysed / corr. found 1) z-Scores z-Scores z-Scores z-Scores z-Scores z-Scores AAZ 2)
32 x 8 / 5 -0.5 -0.3 0.5 -0.3 -0.2 0.4
33 9 / 6 -1.1 -0.2 0.3 -0.1 0.0 -0.2 0.3
34 9 / 6 -1.4 0.3 -0.2 -0.5 -0.2 -1.2 0.6
35 8 / 5 -2.3 -1.0 1.4 -1.4 0.9 1.4
36 x 8 / 5 -0.8 0.0 -0.8 0.1 -1.3 0.6
37 9 / 6 0.3 -0.4 0.6 1.7 1.2 0.8 0.8
46 9 / 6 -0.1 0.4 -0.2 0.0 -0.2 -0.9 0.3
48 9 / 6 4.5 -0.7 0.4 -0.8 0.7 1.0 1.4
49 x 9 / 6 1.7 -1.6 -1.3 -0.7 0.5 17.2 1.8
50 9 / 6 0.5 0.1 -0.2 1.8 0.6 0.0 0.5
52 9 / 6 0.2 0.2 0.2 -0.5 0.3 -0.3 0.3
54 x 9 / 6 0.1 -0.2 -0.4 1.4 -0.7 0.1 0.5
55 9 / 6 -0.6 0.5 0.2 -1.0 0.5 0.3 0.5
56 9 / 6 -0.6 0.9 1.0 0.1 1.5 -0.7 0.8
60 8 / 5 0.8 0.1 -0.6 -0.7 -0.1 0.5
61 x 8 / 5 0.8 0.2 0.4 0.0 0.6 0.4
63 9 / 6 -0.4 0.3 0.3 -1.0 -0.3 -3.3 0.9
65 8 / 5 -3.5FN -1.0 0.4 -1.1 0.3 -0.3 1.1
68 x 8 / 5 -0.4 1.9 -0.5 -2.6 1.6 1.4
69 9 / 6 -0.4 -0.1 -0.2 -0.2 -0.7 -0.5 0.4
71 8 / 5 0.1 0.2 -0.5 -0.7 -0.4 0.4
72 9 / 6 -0.3 -0.3 -0.5 0.0 -0.1 -1.0 0.4
73 8 / 5 5.1 2.0 -0.3 1.2 0.1 1.7
74 x 9 / 6 -2.9 -2.1 -0.5 -1.5 0.0 0.3 1.2
76 x 8 / 5 -1.0 -1.7 -0.9 -0.1 -1.9 1.1
78 x 9 / 6 -0.8 -2.1 0.5 -0.8 1.9 -0.5 1.1
79 x 9 / 6 -0.7 -0.1 0.1 1.2 -0.4 -0.4 0.5
83 9 / 6 -3.2 0.3 -0.2 -1.9 -0.2 -3.1 1.5
85 8 / 5 -1.7 1.4 -0.9 0.7 2.0 1.3
86 8 / 5 0.8 0.4 0.0 1.6 1.3 0.8
87 8 / 5 -0.3 -0.3 -0.9 0.0 -0.4 0.4
88 9 / 6 0.4 -2.9 -0.1 0.9 -0.7 -0.6 0.9
89 9 / 6 0.3 -0.7 0.1 0.1 -0.4 -1.6 0.5
91 9 / 6 -0.8 0.5 0.7 0.5 -0.6 0.8 0.7
92 9 / 6 -0.6 0.7 -0.7 0.3 -0.7 0.4 0.6
93 9 / 6 -0.6 0.6 0.5 -0.4 0.3 0.8 0.5
97 9 / 6 3.3 0.2 -0.1 -0.3 0.5 -3.1 1.3
98 9 / 6 -1.0 -0.5 0.4 -0.2 0.3 0.0 0.4
101 8 / 5 0.2 -2.0 0.6 -1.9 2.4 1.4
104 9 / 6 2.0 -0.9 -2.0 -1.0 -1.2 -0.4 1.3
105 9 / 6 -1.3 -0.4 -0.7 -2.4 -2.3 2.1 1.5
109 8 / 5 2.9 -0.3 -0.3 0.7 -0.1 0.9
112 9 / 6 -0.9 1.0 0.9 -0.2 0.7 -0.2 0.7
3rd-117 9 / 6 0.1 -1.2 -0.5 -3.2 -1.2 0.9 1.21) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned
values based on the entire population. For the calculation of the AAZ the value “5” was applied where the z-score was higher than 5 (shown in square brackets).
FN = false negative results
Table 4-11 (cont.): Category A laboratories ordered by lab-codes
EUPT-SRM13 | 2018 (Soybean Flour)
50
Table 4-11: Category B laboratories ordered by lab-codes
COMPULSORY Compounds Bromide ion Cyromazine Fluazifop Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %
Lab code SRM13-
NRL-SRM
Analysed / corr. found 1) z-Scores z-Scores z-Scores z-Scores z-Scores z-Scores AAZ 2)
2 9 / 4 0.0 -3.6FN 0.2 -1.2 -0.7 -3.7FN
3 4 / 3 -0.6 -0.2 -0.5
5 x 7 / 4 -0.2 -2.1 1.7 -1.3
7 x 4 / 3 0.7 -1.3 -0.3
17 7 / 4 -0.5 -0.5 -1.3 0.3
23 6 / 4 0.2 0.5 0.0 0.5
25 7 / 5 0.9 0.9 0.2 0.5 0.0 0.5
28 2 / 1 0.6
38 5 / 2 -0.1 0.2
39 1 / 1 0.4
40 1 / 1 0.8
41 5 / 3 1.6 1.2 1.4
42 6 / 4 -0.9 -0.9 -0.7 -0.4
43 1 / 1 -0.5
44 2 / 1 4.8
45 9 / 6 0.1 3.7 -2.2 -0.7 0.7 0.6 1.3
47 0 / 0
51 x 7 / 4 0.5 0.0 0.3 -0.1
53 6 / 3 0.1 -0.8 -0.9
57 x 3 / 2 0.3 0.8
58 1 / 1 -0.2
59 0 / 0
62 7 / 4 1.2 -2.2 -0.6 -1.2
64 2 / 1 -0.7
66 5 / 2 0.4 1.5 -3.7FN
67 7 / 5 -0.3 -2.4 -1.2 0.8 -0.5 1
70 3 / 2 0.3 0.1
77 x 3 / 2 -0.5 -0.1
80 x 6 / 4 1.0 6.2 1.9 0.2
82 3 / 2 0.4 0.0
84 4 / 3 1.0 1.6 0.0
90 1 / 0 -3.6FN
94 1 / 1 0.8
95 1 / 1 -0.1
96 7 / 5 -0.3 0.7 0.2 -0.1 -0.8 0.4
99 2 / 1 -0.3
100 x 4 / 3 0.2 0.0 0.5
102 1 / 1 -2.0
103 1 / 1 55.8
106 5 / 3 34.8 0.1 -0.8
107 6 / 4 0.9 0.1 0.7 -1.1
1) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned
values based on the entire population. For the calculation of the AAZ the value “5” was applied where the z-score was higher than 5 (shown in square brackets).
FN = false negative results
4. RESULTS / Assessment of Laboratory Performance
51
Resu
lts
4
COMPULSORY Compounds Bromide ion Cyromazine Fluazifop Glyphosate Haloxyfop Mepiquat-Cl
MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01
Assigned Value [mg/kg] 15.356 0.097 0.049 0.903 0.017 0.124
CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %
Lab code SRM13-
NRL-SRM
Analysed / corr. found 1) z-Scores z-Scores z-Scores z-Scores z-Scores z-Scores AAZ 2)
110 4 / 2 -1.6 0.6
111 4 / 2 1.2 -1.1
113 0 / 0
114 0 / 0
3rd-115 6 / 3 -0.4 0.7 -3.3FN 0.0
3rd-116 8 / 5 -0.6 -1.1 -1.3 -2.3 -0.4 1.1
3rd-118 6 / 3 -0.2 -0.6 -3.2FN -0.8
3rd-119 2 / 1 -0.7
3rd-120 3 / 1 0.0
3rd-121 1 / 1 0.1
3rd-122 7 / 5 0.4 2.1 0.0 0.5 4.7 1.51) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned
values based on the entire population. For the calculation of the AAZ the value “5” was applied where the z-score was higher than 5 (shown in square brackets).
FN = false negative results
Table 4-12 (cont.): Category B laboratories ordered by lab-codes
4.4.5 Feedback from Laboratories in Case of Poor Results
Like in the previous EUPT-SRMs, as a follow-up measure to this EUPT, all participating laboratories having achieved questionable (2 < |z-score| < 3) or unacceptable (|z-score| ≥ 3) results were asked to in-vestigate the reasons for their poor performance and to report them to the organisers. The aim of this measure is to sensibilize the laboratories to investigate the sources of errors. A compilation of the feedback received by the laboratories is given in Appendix 7. With this compilation it is intended to make all partici-panting labs aware of common and potential error sources so that they can be avoided or eliminated in the future. This information also provides input to NRLs on how to better assist OfLs within the network in improving their performance.
In the current PT, excluding diquat, phosphine (Test Item) and phosphine (PH3-Tube) that showed an unac-ceptble uncertainty of their assigned values, in total 821 results for the analytes present in the test items and 5 false positive results were reported by 116 participants. 98 results by 51 laboratories were allocated with |z| > 2, and thereof 63 results by 40 laboratories with |z| ≥ 3 (see Section Table 4-7, p. 35). Among EU and EFTA laboratories, |z| > 2 was assigned to 33 results by 23 laboratories, and |z| ≥ 3 to 55 results by 33 laboratories. All these laboratories and those having obtained false positive results were asked to provide a feedback. Overall, 43 laboratories responced to the organisers with (possible) reasons for their poor per-formance in 86 cases. In 7 cases the real reasons for generating biased results could not be clarified, despite of intensive investigation. The most frequently reported error sources were “lack of experience” (28 cases) and often combined with “matrix effect not properly compensated” (20 cases) and/or “use of inappropri-ate procedure” (21 cases). The current matrix “soybean flour”, a dry matrix with high content on fat (approx. 20 %) and even with starch and biological surfactant lecithin, was surely a difficult matrix and out of the routine analytical scope. Lacking of experience with soy beans, part of the participants applied in the PT
EUPT-SRM13 | 2018 (Soybean Flour)
52
simply the the extraction solvents and procedures which work usually well for fruit and vegetable but not for soybeans. During the investigation a few participants observed that addition of water and soaking enhance the extraction yield (Appendix 7). Compared with the previouse EUPT-SRMs, the percentage of
“transcription error” was high in this PT (14 cases). Most of the transcription errors occured during results submission, in particular if the submission tool didn’t work correctly and one was under stress. Together with other EURLs, the organiser is working on a new, and hopefully more comfortable and stable submis-sion tool. The transcription errors occured also during typing of the concentration of the calibration solu-tion.
Other error sources commonly reported were: “error in concentration of analytical standard/calibration stock” (9 cases) or “procedure not properly conducted/error during sample preparation“ (8 cases), “inap-propriate calibration “ (4 cases), “detection signals strongly interferred by matrix components/strong chro-matographic interferences“ (each 3 cases), “misunderstanding of the definition of the analyte”, “sample weight too small, homogeneity not waranteed“, “error in the evaluation/interpretation of measurement data“, “technical problems/diffculties with measurement instrumentation“ and “contamination“ (each 2 cases) as well as “error in the conversion factor“, “sample amount not sufficient for conducting confirma-tion analysis” and “reporting limit higher than the assigned value“ (each one case). The responses from the other labratories are pending.
5. Acknowledgements / 6. References
53
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5. ACkNOWLEDGEMENTS
The organisers wish to thank the members of the EUPT Scientific Committee (Quality Control Group and Advisory Group) for their valuable advice. Special thanks also go to Jens-Ole Frimann for his support in establishing the online result submission tool.
6. REFERENCES
[1] Regulation (EC) N° 882/2004 of the European Parliament and of the Council on official controls per-formed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules. Published at OJ of the EU L191 of 28.05.2004
[2] Regulation (EC) N° 396/2005, published at OJ of the EU L70 of 16.03.2005, as last amended by Regula-tion 839/2008 published at OJ of the EU L234 of 30.08.2008.
[3] http://www.crl-pesticides.eu/userfiles/file/EurlSRM/EurlSrm_Observations_AcidicPesticides.pdf
[4] Thompson M., Ellison S.L.R. and Wood R., The International Harmonized Protocol for the Proficiency Testing of Analytical Chemistry Laboratories (IUPAC Technical Report). Pure Appl. Chem., Vol. 78, No. 1, pp. 145 – 196, 2006
[5] http://quppe.eu/
[6] ISO 13528:2015: Statistical methods for use in proficiency testing by interlaboratory comparisons.
Appendix 1. List of Laboratories Registered to Participate in the EUPT-SRM13
Part
iciP
atio
n
a1
A-1
7. APPENDICES
Country (Location)
Analysed on behalf of Institution City NRL*-
SRMReported
results
Austria AT AGES Innsbruck (LSI-PLMA) Innsbruck x Yes
Belgium BE WIV-ISP (Belgian Scientific Institute of Public Health) Brussels x Yes
Belgium BE; BG; FR; LU
Primoris - Belgium Gent - Zwijnaarde Yes
Bulgaria BG CLCTC Sofia x Yes
Croatia HR Euroinspekt - Croatiakontrola Zagreb Yes
Croatia HR Inspecto d.o.o. Laboratorij Osijek (Industrijska zona Nemetin)
Yes
Croatia HR NZJZ dr.A.Štampar Zagreb Yes
Cyprus CY FP lab of S.G.L Nicosia x Yes
Czech Republic
CZ Central Institute for Supervising and Testing in Agriculture Brno Yes
Czech Republic
CZ Czech Agriculture and Food Inspection Authority Prague x Yes
Czech Republic
CZ VSCHT Praha, Analyza potravin Praha 6 Yes
Denmark DK Fodevarestyrelsen Ringsted x Yes
Estonia EE PMK, JSL Saku Yes
Estonia EE Tartu Laboratory of Health Boa Tartu x Yes
Finland FI Finnish Customs Laboratory Espoo x Yes
Finland FI Finnish Food Safety Authority Helsinki x Yes
France FR ANSES-LSAL Maisons-Alfort Cedex x Yes
France FR CAMP 66 perpignan Yes
France FR CAPINOV Landerneau Yes
France FR CERECO GARONS Yes
France FR GIRPA BEAUCOUZE Yes
France FR INOVALYS Le Mans Yes
France FR Laboratoire du SCL Montpellier Yes
France FR SCL Laboratoire de Paris Massy Cedex Yes
France BE PHYTOCONTROL NIMES Yes
Germany BE LUFA-ITL GmbH Kiel Yes
Germany DE BfUL FB 42 Nossen Yes
Germany DE Bundesamt für Verbraucherschutz und Lebensmittelsi-cherheit
Berlin-Marienfelde x Yes
Germany DE CVUA Münsterland Emscher-Lippe Münster Yes
Germany DE CVUA RRW Krefeld Yes
Germany DE Eurofins SOFIA GmbH Berlin Yes
Germany DE Institut für Hygiene und Umwel Hamburg No
Germany DE Kwalis Qualitätsforschung Fulda Dipperz Yes
Germany DE Labor Friedle GmbH Tegernheim Yes
Germany DE Landesamt für Landwirtschaft, Lebensmittelsicherheit und Fischerei
Rostock Yes
Germany DE Landesamt für Verbraucherschut Halle/Saale Yes
Germany DE Landeslabor Berlin-Brandenburg Potsdam Yes
Germany DE Landesuntersuchungsamt - ILC Speyer Speyer Yes
* only for EU-Member States
Appendix 1 List of Laboratories Registered to Participate in the EUPT-SRM13
(a): participating labs of EU and EFTA Member States
EUPT-SRM13 | 2018 (Soybean Flour)
A-2
Country (Location)
Analysed on behalf of Institution City NRL*-
SRMReported
results
Germany DE Landesuntersuchungsanstalt für das Gesundheits- und Veterinärwesen Sachsen Reichenbachstr. 71/73 01217 Dresden Germany
Dresden Yes
Germany DE LAVES Futtermittelinstitut Stade Stade Yes
Germany DE LAVES, LVI Oldenburg Oldenburg Yes
Germany DE LGL Erlangen Yes
Germany DE LLG Halle Halle/Saale Yes
Germany DE LTZ Augustenberg Karlsruhe Yes
Germany DE LUFA Speyer Speyer Yes
Germany DE Stadt Duesseldorf - Abteilung Duesseldorf Yes
Germany DE State Laboratory Schleswig-Holstein Neumünster Yes
Germany DE; MT Eurofins Dr. Specht Laboratorien GmbH Hamburg Yes
Germany LT GALAB Laboratories GmbH Hamburg Yes
Greece GR AGROLAB-RDS Thessaloniki Yes
Greece GR Benaki Pesticide Residue Labor Kifissia x Yes
Greece GR General Chemical State Laboratory, A Chemical Division, Pesticide Residues Laboratory
Athens x Yes
Hungary HU Food Chain Safety Centre Non-profit Ltd. Pesticide Resi-due Analytical Laboratory, Hódmezővásárhely
Hódmezovásárhely Yes
Hungary HU Food Chain Safety Centre Nonprofit Ltd. Pesticide Residue Analytical Laboratory, Miskolc
Miskolc Yes
Hungary HU Food Chain Safety Centre Non-profit Ltd., Pesticide Resi-due Analytical Laboratory, Szolnok
Szolnok Yes
Hungary HU National Food Chain Safety Office, Directorate of Plant Protection, Soil Conservation and Agri-environment - Pesticide Analytical Laboratory, Velence
Velence x Yes
Hungary HU Wessling Hungary Ltd. Food Testing Laboratory Budapest Yes
Ireland IE PCL, Backweston Lab Complex Co. Kildare x Yes
Italy IT APPA Bolzano Bolzano Yes
Italy IT ARPA Puglia Bari Yes
Italy IT ARPAE Ferrara Laboratorio Tema Ferrara Yes
Italy IT ARPAV Verona Verona Yes
Italy IT Contaminanti Ambientali Perugia Yes
Italy IT Istituto Superiore di Sanità Rome x No
Italy IT Istituto Zooprofilattico Sperimentale Abruzzo e Molise Teramo Yes
Italy IT IZS Sardegna - Lab Chimica Ambientale e Tossicologia Sassari Yes
Italy IT IZS Sicilia - Pesticide Lab Palermo Yes
Italy IT USL Toscana centro - Lab. Sani Firenze Yes
Italy IT; MT Istituto Zooprofilattico Sperimentale Lombardia ed Emilia Romagna
Brescia Yes
Italy RO IZSLT Roma Yes
Latvia LV Research Institute BIOR Riga x Yes
Lithuania LT NMVRVI Vilnius x Yes
Luxembourg LU LNS-ALI Dudelange x Yes
Norway NO NIBIO, Biotechnology and Plant Health, Pesticides and Natural Products Chemistry
Aas Yes
Poland PL IPP-NRI, Bialystok Bialystok Yes
Poland PL Wojewódzka Stacja Sanitarno-Epidemiologiczna w Opolu Opole Yes
Poland PL WSSE w Warszawie Warszawa x Yes
Poland PO J.S. Hamilton Poland S.A. Gdynia Yes
Poland PO UO-Technologia Grójec Yes
Portugal PT Laboratório Regional de Veterinária e Segurança Alimen-tar
Funchal Madeira Island
x Yes
* only for EU-Member States
Appendix 1-a (cont.): participating labs of EU and EFTA member states
Appendix 1. List of Laboratories Registered to Participate in the EUPT-SRM13
A-3
Part
iciP
atio
n
a1Country (Location)
Analysed on behalf of Institution City NRL*-
SRMReported
results
Slovakia SK Veterinary and Food Institute in Bratislava Bratislava x Yes
Slovenija SI National Laboratory for Health, Environment and Food - Maribor (location Ljubljana)
Ljubljana Yes
Slovenija SI NLZOH-Maribor Maribor x Yes
Spain ES AINIA PATERNA, VALENCIA Yes
Spain ES Analytica Alimentaria Almeria Yes
Spain ES CNA (AECOSAN) Majadahonda (Ma-drid)
x Yes
Spain ES CNTA San Adrián (Navarra) Yes
Spain ES DIRECCION TERRITORIAL COMERCIO Valencia No
Spain ES EUROFINS SICA AGRIQ, S.L. VÍCAR (ALMERIA) Yes
Spain ES Lab Agroalim. de Extremadura Cáceres Yes
Spain ES Lab Agroamb Zaragoza Zaragoza Yes
Spain ES Lab. Agroalimentario y de Sani El Palmar-Murcia No
Spain ES Laboratori Agència de Salut Pública de Barcelona Barcelona Yes
Spain ES Laboratorio Agrario Abegondo. A Coruña No
Spain ES Laboratorio Agrario Regional, Burgos Yes
Spain ES Laboratorio Arbitral Agroalimentario Madrid x Yes
Spain ES Laboratorio SOIVRE Tenerife Santa Cruz de Tener-ife. Canay Island
Yes
Spain ES LABORATORIOS ECOSUR, S.A. Lorquí (Murcia) Yes
Spain ES LPSVJAEN Mengibar (Jaén) Yes
Spain ES; MT LAGV Burjassot-Valencia Yes
Sweden SE Eurofins Food&Feed Sweden AB Lidkoping Yes
Sweden SE Livsmedelsverket, Dep of Chemi Uppsala x Yes
Switzerland CH Kantonales Labor Zürich Zurich Yes
Switzerland CH Kantonales Labor, Gesundheitsdepartement Basel-Stadt Basel Yes
Switzerland CH LABORATORIUM DER URKANTONE BRUNNEN Yes
The Netherlands
AL; BE; NL
Eurofins Lab Zeeuws-Vlaanderen Graauw Yes
The Netherlands
BE Dr. A. Verwey B.V. Rotterdam Yes
The Netherlands
BE Groen Agro Control Delfgauw Yes
The Netherlands
BE Nofalab B.V. Schiedam Yes
The Netherlands
NL NVWA - NRL for Pesticide Residues in Food and Feed Wageningen x Yes
The Netherlands
NL RIKILT - Wageningen University Wageningen Yes
United Kingdom
UK; MT Fera Science Ltd York x Yes
United Kingdom
UK Concept Life Sciences Ltd Bar Hill Yes
United Kingdom
UK Eurofins Food Testing UK Wolverhampton Yes
* only for EU-Member States
Appendix 1-a (cont.): participating labs of EU and EFTA member states
EUPT-SRM13 | 2018 (Soybean Flour)
A-4
Appendix 1-b: Participating labs from EU candidate countries and third countries
Country Institution City Reported results
Belarus Food testing laboratory/BelGIM Minsk Yes
Brazil LANAGRO/MG Pedro Leopoldo Yes
Costa Rica LABORATORIO DE ANÁLISIS DE RESIDUOS DE AGROQUÍMI-COS
San José Yes
Peru Unidad del Centro de Control de Insumos y Residuos Tóxicos - SENASA
Lima Yes
Serbia GZZJZ Belgrade Belgrade Yes
Serbia SP LABORATORIJA A.D. BECEJ Yes
Singapore Agri-Food and Veterinary Authority Veterinary Public Health Laboratory Pesticide Residue Section
Singapore Yes
Thailand Central Laboratory Bangkok Yes
Appendix 2. Shipment Evaluation
A-5
A2
Ship
men
t evA
luAt
ion
Appendix 2 Shipment Evaluation
Compilation of shipment duration
1 day 106 labs (81 %)
2 days 14 labs (11 %)
3 days: 7 labs (5 %): 3× IT, ES, PT, USA, AU
> 4 days: 5 labs (4 %): SR, TH, CR, BR, PE
A-6
EUPT-SRM13 | 2018 (Soybean Flour)
Appendix 3 Data of Homogeneity Test
Glyphosate Haloxyfop Mepiquat-Cl
Sample No. Portion 1 [mg/kg]
Portion 2 [mg/kg] Sample No. Portion 1
[mg/kg]Portion 2 [mg/kg] Sample No. Portion 1
[mg/kg]Portion 2 [mg/kg]
No. 024 0.840 0.938 No. 024 0.017 0.017 No. 024 0.121 0.136
No. 036 0.923 0.973 No. 036 0.016 0.018 No. 036 0.130 0.135
No. 047 1.017 0.973 No. 047 0.016 0.015 No. 047 0.131 0.124
No. 066 0.885 0.891 No. 066 0.017 0.016 No. 066 0.115 0.128
No. 077 0.914 0.999 No. 077 0.017 0.017 No. 077 0.128 0.134
No. 090 0.866 0.936 No. 090 0.016 0.016 No. 090 0.125 0.132
No. 110 0.842 0.814 No. 110 0.017 0.016 No. 110 0.105 0.113
No. 122 0.825 1.029 No. 122 0.016 0.017 No. 122 0.121 0.125
No. 142 0.969 0.938 No. 142 0.016 0.015 No. 142 0.132 0.128
No. 167 0.922 0.976 No. 167 0.016 0.016 No. 167 0.125 0.141mean / AV* 0.924 / 0.903 mean / AV* 0.016 / 0.017 mean / AV* 0.126 / 0.124
COMPULSORY COMPOUNDSBromide ion Cyromazine Fluazifop
Sample No. Portion 1 [mg/kg]
Portion 2 [mg/kg] Sample No. Portion 1
[mg/kg]Portion 2 [mg/kg] Sample No. Portion 1
[mg/kg]Portion 2 [mg/kg]
No. 024 14.2 15.3 No. 024 0.098 0.116 No. 024 0.053 0.050
No. 036 14.3 16.5 No. 036 0.112 0.121 No. 036 0.050 0.051
No. 047 14.8 14.0 No. 047 0.113 0.106 No. 047 0.045 0.048
No. 066 15.9 14.6 No. 066 0.099 0.109 No. 066 0.054 0.049
No. 077 14.4 14.9 No. 077 0.108 0.108 No. 077 0.052 0.053
No. 090 15.1 15.7 No. 090 0.105 0.108 No. 090 0.050 0.047
No. 110 12.2 13.0 No. 110 0.101 0.094 No. 110 0.048 0.048
No. 122 13.7 15.3 No. 122 0.100 0.104 No. 122 0.049 0.051
No. 142 14.2 13.6 No. 142 0.113 0.106 No. 142 0.049 0.047
No. 167 13.9 16.8 No. 167 0.105 0.116 No. 167 0.049 0.048mean / AV* 14.6 / 15.4 mean / AV* 0.107 / 0.097 mean / AV* 0.049 / 0.049
* mean / AV = Average value of the homogeneity test data [mg/kg] / Assigned value of PT [mg/kg] derived from the population of EU-/EFTA-Laboratories
Appendix 3. Data of Homogeneity Test
A-7
Ho
mo
gen
eity
A3
N-Acetyl-Glyphosate Perchlorate Phosphonic acid QuizalofopSample
No.Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
No. 024 0.696 0.769 No. 024 0.099 0.109 No. 024 1.874 2.082 No. 024 0.061 0.061
No. 036 0.832 0.880 No. 036 0.104 0.117 No. 036 2.161 2.197 No. 036 0.056 0.062
No. 047 0.772 0.817 No. 047 0.108 0.100 No. 047 2.079 2.025 No. 047 0.057 0.056
No. 066 0.725 0.792 No. 066 0.103 0.106 No. 066 1.931 2.011 No. 066 0.063 0.060
No. 077 0.739 0.821 No. 077 0.096 0.111 No. 077 1.902 2.094 No. 077 0.062 0.061
No. 090 0.739 0.750 No. 090 0.104 0.106 No. 090 1.947 2.055 No. 090 0.060 0.054
No. 110 0.654 0.633 No. 110 0.095 0.092 No. 110 1.774 1.668 No. 110 0.056 0.057
No. 122 0.666 0.779 No. 122 0.100 0.100 No. 122 1.866 2.013 No. 122 0.056 0.059
No. 142 0.794 0.762 No. 142 0.110 0.104 No. 142 2.086 2.011 No. 142 0.059 0.055
No. 167 0.716 0.835 No. 167 0.095 0.106 No. 167 1.882 2.209 No. 167 0.057 0.055mean / AV* 0.759 / 0.835 mean / AV* 0.103 / 0.100 mean / AV* 1.99 / 1.86 mean / AV* 0.058 / 0.052
OPTIONAL COMPOUNDS2,4-DB Diquat Glufosinate MPP
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
No. 024 0.187 0.192 No. 024 1.59 1.24 No. 024 0.195 0.211 No. 024 0.164 0.189
No. 036 0.181 0.187 No. 036 1.52 1.64 No. 036 0.211 0.255 No. 036 0.187 0.197
No. 047 0.163 0.167 No. 047 1.29 1.35 No. 047 0.181 0.192 No. 047 0.179 0.178
No. 066 0.194 0.164 No. 066 1.46 1.46 No. 066 0.212 0.202 No. 066 0.171 0.177
No. 077 0.183 0.185 No. 077 1.42 1.61 No. 077 0.216 0.174 No. 077 0.172 0.188
No. 090 0.179 0.169 No. 090 1.39 1.41 No. 090 0.213 0.207 No. 090 0.174 0.179
No. 110 0.172 0.179 No. 110 1.31 1.44 No. 110 0.160 0.167 No. 110 0.155 0.151
No. 122 0.173 0.184 No. 122 1.67 1.57 No. 122 0.149 0.180 No. 122 0.157 0.175
No. 142 0.166 0.180 No. 142 1.47 1.29 No. 142 0.213 0.184 No. 142 0.179 0.173
No. 167 0.165 0.176 No. 167 1.52 1.49 No. 167 0.182 0.237 No. 167 0.171 0.192mean / AV* 0.177 / 0.183 mean / AV* 1.46 / 1.70 ‡ mean / AV* 0.197 / 0.192 mean / AV* 0.489 / 0.188
* mean / AV = Average value of the homogeneity test data [mg/kg] / Assigned value of PT [mg/kg] derived from the population of EU-/EFTA-Laboratories
‡ : statistically uncertain
OPTIONAL COMPOUND (PHOSPHINE)Phsophine (Test Item) Phosphine (PH3-Tube)
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
Sample No.
Portion 1 [mg/kg]
Portion 2 [mg/kg]
No. 001 0.187 0.189 No. 001 0.068 0.082
No. 006 0.170 0.191 No. 005 0.059 0.068
No. 013 0.178 0.185 No. 008 0.077 0.060
No. 016 0.175 0.192 No. 011 0.079 0.064
No. 031 0.167 0.183 No. 017 0.064 0.078
No. 100 0.184 0.180 No. 021 0.063 0.067
No. 114 0.177 0.197 No. 026 0.073 0.059
No. 140 0.170 0.185 No. 041 0.057 0.060
No. 154 0.176 0.192 No. 048 0.062 0.069
No. 172 0.186 0.191 No. 051 0.073 0.076mean / AV* 0.183 / – mean / AV* 0.068 / –
EUPT-SRM13 | 2018 (Soybean Flour)
A-8
* RSD = relative standard diviation
Appendix 4 Data of Stability Test
COMPULSORY COMPOUNDSBormide Ion Cyromazine
AV [mg/kg] 15.4 AV [mg/kg] 0.097
Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 14.4 14.9 13.3 13.8 14.3 13.9 No. 077 0.108 0.108 0.099 0.100 0.116 0.108
No. 110 12.2 13.0 13.8 14.0 14.1 13.8 No. 110 0.101 0.094 0.108 0.104 0.109 0.108
No. 142 14.2 13.6 14.0 15.5 14.6 13.9 No. 142 0.113 0.106 0.103 0.113 0.109 0.114
Mean [mg/kg] 13.73 14.05 14.11 Mean [mg/kg] 0.105 0.105 0.111
RSD* [%] 7.5 % 4.3 % 0.9 % RSD* [%] 6.2 % 4.2 % 1.5 %
Diviation [%] (ref. 1st Anaylsis) — 2.4 % 2.8 % — -0.4 % 5.3 %
Fluazifop Glyphosate
AV [mg/kg] 0.049 AV [mg/kg] 0.903
Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 0.052 0.053 0.051 0.046 0.048 0.051 No. 077 0.914 0.999 0.938 0.942 0.998 0.909
No. 110 0.048 0.048 0.050 0.051 0.052 0.047 No. 110 0.842 0.814 1.017 0.905 0.919 0.819
No. 142 0.049 0.047 0.051 0.050 0.047 0.047 No. 142 0.969 0.938 0.951 1.030 0.922 1.031
Mean [mg/kg] 0.050 0.050 0.049 Mean [mg/kg] 0.913 0.964 0.933
RSD* [%] 5.5 % 2.6 % 3.0 % RSD* [%] 8.0 % 2.7 % 6.1 %
Diviation [%] (ref. 1st Anaylsis) — 0.4 % -1.7 % — 5.6 % 2.2 %
Haloxyfop Mepiquat-Cl
AV [mg/kg] 0.017 AV [mg/kg] 0.124
Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 0.017 0.017 0.016 0.019 0.018 0.015 No. 077 0.128 0.134 0.121 0.123 0.139 0.128
No. 110 0.017 0.016 0.015 0.016 0.017 0.018 No. 110 0.105 0.113 0.140 0.128 0.123 0.135
No. 142 0.016 0.015 0.016 0.015 0.019 0.017 No. 142 0.132 0.128 0.126 0.131 0.129 0.133
Mean [mg/kg] 0.016 0.016 0.017 Mean [mg/kg] 0.123 0.128 0.131
RSD* [%] 3.7 % 6.6 % 4.4 % RSD* [%] 10.0 % 4.7 % 1.7 %
Diviation [%] (ref. 1st Anaylsis) — 0.1 % 7.1 % — 3.8 % 6.2 %
/ Compulsory Compounds
Appendix 4. Data of Stability Test
A-9
Sta
bili
ty
a4
Phosphonic acid Quizalofop
AV [mg/kg] 1.86 AV [mg/kg] 0.052
Date 03.05.2018 22.05.2018 18.06.2018 Date 25.04.2018 17.05.2018 07.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 1.90 2.09 1.84 1.94 2.09 1.94 No. 077 0.062 0.061 0.064 0.060 0.053 0.057
No. 110 1.77 1.67 2.01 1.97 1.94 1.81 No. 110 0.056 0.057 0.057 0.057 0.056 0.063
No. 142 2.09 2.01 1.90 2.09 1.86 1.99 No. 142 0.059 0.055 0.056 0.057 0.059 0.058
Mean [mg/kg] 1.92 1.96 1.94 Mean [mg/kg] 0.058 0.059 0.058
RSD* [%] 9.2 % 3.1 % 3.6 % RSD* [%] 4.7 % 5.4 % 4.1 %
Diviation [%] (ref. 1st Anaylsis) — 1.9 % 0.9 % — 0.3 % -1.2 %
* RSD = relative standard diviation; ‡ : statistically uncertain
OPTIONAL COMPOUNDS2,4-DB Diquat
AV [mg/kg] 0.183 AV [mg/kg] 1.70 ‡
Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 0.181 0.187 0.188 0.169 0.157 0.170 No. 077 1.42 1.61 1.24 1.45 1.63 1.23
No. 110 0.172 0.179 0.190 0.184 0.161 0.175 No. 110 1.31 1.44 1.43 1.27 1.48 1.45
No. 142 0.166 0.180 0.184 0.182 0.165 0.162 No. 142 1.47 1.29 1.42 1.35 1.34 1.40
Mean [mg/kg] 0.177 0.183 0.165 Mean [mg/kg] 1.42 1.36 1.42
RSD* [%] 3.3 % 2.3 % 1.6 % RSD* [%] 5.7 % 1.5 % 3.5 %
Diviation [%] (ref. 1st Anaylsis) — 3.1 % -7.0 % — -4.5 % -0.1 %
Glufosinate MPP
AV [mg/kg] 0.192 AV [mg/kg] 0.188
Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 0.216 0.174 0.192 0.201 0.202 0.218 No. 077 0.172 0.188 0.163 0.180 0.175 0.171
No. 110 0.160 0.167 0.166 0.174 0.175 0.159 No. 110 0.155 0.151 0.171 0.174 0.164 0.154
No. 142 0.213 0.184 0.191 0.176 0.149 0.211 No. 142 0.179 0.173 0.172 0.185 0.155 0.172
Mean [mg/kg] 0.186 0.183 0.186 Mean [mg/kg] 0.170 0.174 0.165
RSD* [%] 10.4 % 7.2 % 11.9 % RSD* [%] 8.7 % 2.2 % 4.3 %
Diviation [%] (ref. 1st Anaylsis) — -1.3 % 0.0 % — 2.7 % -2.6 %
N-Acetyl-Glyphosate Perchlorate
AV [mg/kg] 0.835 AV [mg/kg] 0.100
Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 077 0.739 0.821 0.705 0.798 0.823 0.800 No. 077 0.096 0.111 0.094 0.097 0.109 0.105
No. 110 0.654 0.633 0.773 0.771 0.735 0.659 No. 110 0.095 0.092 0.106 0.100 0.109 0.105
No. 142 0.794 0.762 0.753 0.840 0.648 0.785 No. 142 0.110 0.104 0.101 0.107 0.109 0.110
Mean [mg/kg] 0.734 0.773 0.742 Mean [mg/kg] 0.101 0.101 0.108
RSD* [%] 10.6 % 2.9 % 8.3 % RSD* [%] 7.0 % 4.8 % 1.3 %
Diviation [%] (ref. 1st Anaylsis) — 5.4 % 1.1 % — -0.4 % 6.5 %
Appendix 4 (cont.): Data of Stability Test / Optional Compounds
EUPT-SRM13 | 2018 (Soybean Flour)
A-10
* RSD = relative standard diviation
OPTIONAL COMPOUNDS (PHOSPHINE)Phosphine (Test Item) Phosphine (PH3-Tube)
AV [mg/kg] – AV [mg/kg] –
Date 20.06.2018 19.07.2018 24.09.2018 Date 28.05.2018 19.06.2018 18.07.2018
Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]
No. 006 0.170 0.191 0.147 0.156 0.194 0.182 No. 005 0.059 0.068 0.073 0.065 0.075 0.076
No. 016 0.175 0.192 0.149 0.150 0.184 0.189 No. 017 0.064 0.078 0.064 0.067 0.090 0.083
No. 140 0.170 0.185 0.142 0.152 0.194 0.186 No. 026 0.073 0.059 0.075 0.072 0.082 0.078
Mean [mg/kg] 0.180 0.149 0.188 Mean [mg/kg] 0.067 0.069 0.080
RSD* [%] 1.69 % 1.58 % 0.90 % RSD* [%] 5.61 % 6.11 % 6.73 %
Diviation [%] (ref. 1st Anaylsis)
— -17.29 % 4.25 % Diviation [%] (ref. 1st Anaylsis) — 3.8 % 20.0 %
Appendix 4 (cont.): Data of Stability Test / Optional Compounds
Appendix 5. Histograms and kernel Density Estimates of z-score Distributions
A-11
A5
His
tog
rAm
m-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
02468
10121416182022242628
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468
10121416182022242628
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468
1012141618202224
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468
1012141618202224
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
14
16
18
20
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
14
16
Appendix 5 Histograms and kernel Density Estimates of z-score DistributionsHistograms and kernel Density Estimates of z-score* Distributions(Results from EU and EFTA Laboratories only)
Mepiquate-Cl (AV derived from entire population)
* Cut-off at z-score = 5;
Haloxyfop (AV derived from entire population)
Range of z-scores
Fluazifop (AV derived from entire population)
Glyphosate (AV derived from entire population)
Cyromazine (AV derived from entire population)
Compulsory Compounds
Bromide Ion (AV derived from entire population)
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Range of z-scores Range of z-scores
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Range of z-scores Range of z-scores
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Range of z-scores Range of z-scores
Range of z-scores Range of z-scores
EUPT-SRM11 | 2016 (Spinach Homogenate)
A-12
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
14
16
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
14
16
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
14
16
18
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50
2
4
6
8
10
12
* Cut-off at z-score = 5;
Phosphonic acid (AV derived from entire population)
Perchlorate (AV # derived from entire population)
Quizalofop (AV # derived from entire population)
Range of z-scores
MPP (AV derived from entire population)
N-Acetyl-Glyphosate (AV derived from entire population)
Glufosinate (AV derived from entire population)
Appendix 5 (cont.) Histograms and kernel Density Estimates of z-score* Distributions(Results from EU and EFTA Laboratories only)
* Cut-off at z-score = 5# excluding diquat and phosphine due to high uncertainty of their assigned values
Optional Compounds #
2,4-DB (AV derived from entire population)
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Range of z-scores Range of z-scores
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Coun
t of z
-sco
res
Range of z-scores Range of z-scores
Range of z-scores Range of z-scores
|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable
|z-score| ≥ 3 unacceptable
Coun
t of z
-sco
res
Range of z-scores
Appendix 6. Graphic Presentation of z-Scores
A-13
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
65
83
*74
102
85
34
105
33
98
112
15
*78
91
*79
*12
*30
55
92
93
56
63
*68
69
67
72
11
21
6
10
14
26
46
2
*54
45
52
*100
*8
*22
37
*20
89
88
82
50
*51
27
*13
31
94
*4
25
16
111
62
*19
1
*49
104
*29
97
48
App
endi
x 6
Gra
phic
Pre
sent
atio
n of
z-S
core
s: C
ompu
lsor
y Co
mpo
unds
Brom
ide
Ion
(Ass
ign
ed v
alu
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d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
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labs
90 %
ques
tiona
ble
2 la
bs3
%un
acce
ptab
le4
labs
6 %
fals
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gativ
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lab
Ass
igne
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=15
.4 m
g/kg
CV
* =
24.0
%M
RRL
=2.
0 m
g/kg
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-14
-5-4-3-2-1012345
2
88
67
35
62
*78
10
*74
*49
*76
16
65
31
42
104
*22
*36
48
*29
89
3
27
*77
98
*32
17
26
37
105
72
96
87
33
*54
*79
69
82
*51
50
71
15
*4
*12
53
*20
52
101
11
97
63
*57
83
34
46
6
91
55
*8
93
14
*7
*30
92
*61
86
60
25
56
84
112
*24
85
*68
109
45
73
*13
106
*19
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-Sc
ores
: Com
puls
ory
Com
poun
ds
Cyro
maz
ine
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le65
labs
82 %
ques
tiona
ble
8 la
bs10
%un
acce
ptab
le6
labs
8 %
fals
e ne
gativ
e1
lab
Ass
igne
d va
lue
=0.
097
mg/
kgC
V*
=23
.5 %
MRR
L =
0.01
mg/
kg
5.15.5
34.844.7
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
Appendix 6. Graphic Presentation of z-Scores
A-15
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
90
10
45
101
104
*76
26
*49
*7
67
35
*13
42
85
53
92
*22
105
62
*20
17
*68
72
*74
*54
87
109
*32
27
3
*8
34
46
69
83
50
*5
21
88
97
38
6
*30
31
*100
*36
*79
60
89
71
2
*12
23
25
52
55
*61
63
33
1
48
86
11
65
66
98
*78
93
28
37
91
96
107
112
56
16
*80
15
*24
*19
41
84
14
*4
*29
73
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-Sc
ores
: Com
puls
ory
Com
poun
ds
Flua
zifo
p(A
ssig
ned
val
ue
and
CV
* d
eriv
ed fr
om e
nti
re p
opu
lati
on)
acce
ptab
le83
labs
97 %
ques
tiona
ble
2 la
bs2
%un
acce
ptab
le1
lab
1 %
fals
e ne
gativ
e1
lab
Ass
igne
d va
lue
=0.
049
mg/
kgC
V*
=20
.3 %
MRR
L =
0.01
mg/
kg
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-16
-5-4-3-2-1012345
105
*5
83
110
*74
17
2
26
65
55
104
63
*76
87
48
*36
*78
15
45
64
*49
60
34
71
43
52
93
14
109
97
73
21
69
112
98
58
33
*29
72
86
46
56
1
*8
*4
106
107
89
6
96
31
70
92
*20
*51
39
*61
10
*24
91
23
27
*32
101
*12
*30
*22
*13
40
67
88
11
16
41
*79
*54
*19
35
37
50
44
*80
103
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-Sc
ores
: Com
puls
ory
Com
poun
ds
Gly
phos
ate
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le78
labs
94 %
ques
tiona
ble
2 la
bs2
%un
acce
ptab
le3
labs
4 %
fals
e ne
gativ
e0
lab
Ass
igne
d va
lue
=0.
903
mg/
kgC
V*
=22
.6 %
MRR
L =
0.03
mg/
kg
6.255.8
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
Appendix 6. Graphic Presentation of z-Scores
A-17
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
*68
105
101
27
26
35
62
104
6
60
*13
2
42
*54
69
71
88
92
91
*20
3
*22
*29
*79
89
*8
10
63
*7
*32
1
*4
21
31
34
46
83
72
*76
96
*74
*12
*19
23
33
*61
84
87
*36
11
52
65
93
98
14
15
17
16
25
*49
55
97
*100
50
48
109
45
85
107
112
*24
37
73
41
56
66
86
*5
*78
*80
*30
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-Sc
ores
: Com
puls
ory
Com
poun
ds
Hal
oxyf
op(A
ssig
ned
val
ue
and
CV
* d
eriv
ed fr
om e
nti
re p
opu
lati
on)
acce
ptab
le78
labs
96 %
ques
tiona
ble
2 la
bs2
%un
acce
ptab
le1
lab
1 %
fals
e ne
gativ
e0
lab
Ass
igne
d va
lue
=0.
017
mg/
kgC
V*
=20
.4 %
MRR
L =
0.00
3 m
g/kg
7.6
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-18
-5-4-3-2-1012345
2
66
63
97
83
*76
89
*5
*36
34
*29
111
107
72
46
11
53
96
106
56
88
69
31
67
*78
10
*79
104
42
87
71
6
52
65
99
112
*32
33
*8
14
60
95
*51
*77
109
1
*4
50
25
98
*54
73
15
70
16
38
*80
*22
55
*74
92
23
45
*61
110
21
*57
*20
*30
91
27
37
93
35
*12
48
26
86
*24
*68
85
105
101
*13
*49
*19
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-Sc
ores
: Com
puls
ory
Com
poun
ds
Mep
iqua
t-Cl
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le76
labs
88 %
ques
tiona
ble
2 la
bs2
%un
acce
ptab
le8
labs
9 %
fals
e ne
gativ
e2
labs
Ass
igne
d va
lue
=0.
124
mg/
kgC
V*
=22
.9 %
MRR
L =
0.01
mg/
kg 5.7 17.2 39.0
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
Appendix 6. Graphic Presentation of z-Scores
A-19
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
55
109
101
35
*79
91
*74
26
*32
3
87
98
71
*7
*8
*20
*12
107
*49
72
89
85
2
*76
34
60
88
46
50
*24
63
83
14
105
45
*36
*22
23
*30
52
93
41
33
16
11
1
*19
69
97
112
*13
86
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
2,4-
DB
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le48
labs
92 %
ques
tiona
ble
1 la
b2
%un
acce
ptab
le3
labs
6 %
fals
e ne
gativ
e2
labs
Ass
igne
d va
lue
=0.
183
mg/
kgC
V*
=20
.7 %
MRR
L =
0.01
mg/
kg
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-20
-5-4-3-2-1012345
55
89
105
17
92
*79
109
83
14
*78
2
73
*36
26
*76
60
46
67
33
93
35
112
*4
101
*30
*13
*22
98
34
71
52
86
97
41
107
27
37
45
88
15
16
44
62
63
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
Glu
fosi
nate
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le37
labs
84 %
ques
tiona
ble
2 la
bs5
%un
acce
ptab
le5
labs
11 %
fals
e ne
gativ
e3
labs
Ass
igne
d va
lue
=0.
192
mg/
kgC
V*
=28
.7 %
MRR
L =
0.02
mg/
kg
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
17.6
Appendix 6. Graphic Presentation of z-Scores
A-21
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
109
105
83
63
41
89
60
97
27
46
*36
15
67
34
*30
37
92
112
*13
91
52
88
35
101
45
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
MPP
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le20
labs
80 %
ques
tiona
ble
2 la
bs8
%un
acce
ptab
le3
labs
12 %
fals
e ne
gativ
e1
lab
Ass
igne
d va
lue
=0.
188
mg/
kgC
V*
=18
.9 %
MRR
L =
0.02
mg/
kg
9.1
19.0
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-22
-5-4-3-2-1012345
45
55
*76
89
109
15
*8
83
46
91
*36
41
63
*13
*12
*4
21
105
71
86
112
*30
34
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
N-A
cety
l-G
lyph
osat
e(A
ssig
ned
val
ue
and
CV
* d
eriv
ed fr
om r
esu
lts
wit
h ac
idic
tra
nsf
orm
atio
n)
acce
ptab
le17
labs
74 %
ques
tiona
ble
0 la
b0
%un
acce
ptab
le6
labs
26 %
fals
e ne
gativ
e5
labs
Ass
igne
d va
lue
=0.
835
mg/
kgC
V*
=21
.1 %
MRR
L =
0.02
mg/
kg76.0
:w
ith a
cidi
c tr
ansf
orm
atio
n:w
ithou
t tra
nsfo
rmat
ion
empt
y:no
dat
a
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
Appendix 6. Graphic Presentation of z-Scores
A-23
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
2
109
83
63
35
87
15
*36
17
67
*5
110
34
48
105
11
31
72
60
16
*30
*32
111
*20
33
56
97
10
*4
50
92
38
46
*57
85
89
98
14
91
112
*13
37
52
88
*8
6
62
71
27
44
93
45
26
69
101
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
Perc
hlor
ate
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
; ass
ign
ed v
alu
e an
d z-
scor
es fo
r in
form
ativ
e p
urp
ose
only
)
acce
ptab
le47
labs
85 %
ques
tiona
ble
3 la
bs5
%un
acce
ptab
le5
labs
9 %
fals
e ne
gativ
e2
labs
Ass
igne
d va
lue
=0.
100
mg/
kgC
V*
=16
.9 %
MRR
L =
0.01
mg/
kg
9.5
:w
ith IL
IS:w
ith o
ther
ISs
:with
out I
Ssem
pty:
no d
ata
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-24
-5-4-3-2-1012345
11
85
97
2
83
63
91
10
45
35
55
31
14
16
27
*36
105
72
52
69
33
46
17
67
62
6
*32
34
15
112
37
*30
48
88
86
101
26
89
50
*13
*4
93
106
98
41
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
Phos
phon
ic a
cid
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le36
labs
80 %
ques
tiona
ble
2 la
bs4
%un
acce
ptab
le7
labs
16 %
fals
e ne
gativ
e3
labs
Ass
igne
d va
lue
=1.
86 m
g/kg
CV
* =
24.3
%M
RRL
=0.
05 m
g/kg
12.1
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
Appendix 6. Graphic Presentation of z-Scores
A-25
A6
z-sc
ore
dis
trib
uti
on
-5-4-3-2-1012345
47
66
*76
26
101
27
67
92
105
35
*8
*7
*54
*79
21
*20
63
109
1
69
48
72
46
38
60
52
*36
87
14
*32
86
42
88
89
3
98
17
91
*12
83
*13
23
55
62
*49
*4
34
*24
56
33
96
*30
97
*19
16
93
45
*29
41
112
2
107
App
endi
x 6
(con
t.)
Gra
phic
Pre
sent
atio
n of
z-S
core
s: O
ptio
nal C
ompo
unds
Qui
zalo
fop
(Ass
ign
ed v
alu
e an
d C
V*
der
ived
from
en
tire
pop
ula
tion
)
acce
ptab
le54
labs
87 %
ques
tiona
ble
5 la
bs8
%un
acce
ptab
le3
labs
5 %
fals
e ne
gativ
e2
labs
Ass
igne
d va
lue
=0.
052
mg/
kgC
V*
=23
.6 %
MRR
L =
0.01
mg/
kg
(Res
ults
from
EU
and
EFT
A L
abor
ator
ies
only
, * =
NRL
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-26
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Bromide ion Assigned value: 15.4 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
65 -3.5 (FN)
No Our conclution is that this method ""EURL (CRL) Single Residue Method Ver.1, 2009 for Bromide ion"" is not suitable analysis for this type matrices as Soybean Flour. Comment from the Organizer: Looking at the results of the participants employing methods of this type, I must say that the result distribution was remarkably narrow with the median being close to the assigned value. So, the method seems to work, although it is surely not recom-mendable to inject many extracts of this type of commodities (high fat content), to avoid fat accumulation in the injector. We ourselves have used the QuPPe method for the homogeneity and stability tests of bromide. I was personally concerned whether the unsaturated fatty acids would be brominated thus consuming bromide, but a cross-check with the derivatization method resulted in similar results. If you like to study this issue a bit more I would recommend conducting a standard addition experiment and maybe comparing the slope of the standard addition experiment with the slope of the normal calibration curve (in solvent).
B?, G?
83 -3.2 Yes no experience at all with analysis of bromide using LC-MS/MS; not appropriate ex-traction procedure (use of only MeOH without hydration)
D, G
74 -2.9 Yes significant matrix effect. We have not much experience with this matrix C, D
29 2.1 No Reason not found. We may consider to attribute the overestimated result to the procedural standard calibration that we applied; there is the possibility of increased values due to the inherent correction with recovery of this kind of calibration
L?, U
97 3.3 No The samples blank (042) and SRM sample (130) have been analyzed in the same sequence including a reference sample containing 10 mg/kg bromide ion. In the SRM-blank sample (042) 10 mg/kg bromide are detected. While the detected concentration in the SRM sample (bottle 130) is 27.9 mg/kg, this calculated using a slope obtained by standard addition method on the blank 042 sample and undi-luted samples measurements. The extracts are analyzed both undiluted and 5 times diluted. The results of the 5 times diluted extract have been calculated using a slope with a result of 18.4 mg/kg. The peak of the bromide ion does not show a good shape and the measured amounts in the extract are outside the calibration range. Because the results of the 5 times diluted extract are outside the calibration range and the poor peak shape of bromide, the results of the undiluted measurements have been reported. The used method are optimized and validated for fresh product. The reason for poor result is not clear. Further investigation for dried product is needed.
U
Appendix 7 Possible Reasons Reported for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-27
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
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Cyromazine Assigned value: 0.097 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
2 -3.6 (FN)
Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.
B, G
88 -2.9 Yes "we analyzed cyromazine with two methods in our lab; the QuEChERS method and the QuPPe method. We detected 0,09 mg/kg cyromazine with the QuEPP method and 0,026 mg/kg cyromazine with the QuEChERS method. Only the QuEChERS method is validated for cyromazine and we have no experience in the analysis of cyromazine with QuPPe. For these reasons we trusted the results of the QuEChERS method more than the results of the QuEPP method. Because of the results of the EUPT-SRM13 we will validate the QuPPe method for cyromazine and use the QuEChERS method only for screening."
D, G
67 -2.4 Yes Matrix effect (result from the analysis with the Sweet-Method which usually works well, even for difficult matrix, but obviousely not for soy flour in this PT. Using QuPPe and a HILIC column the result was 0.0094 mg/kg but with high Ionensuppression of approx. 50%.
C
35 -2.3 Yes on classical vegetables, we’ve not problems with cyromazine analysed by Quechers methodology. But we have no experience with soybean flour. Low recovery can be explained by a matrix effect and difficulties on the integration of the cyromazine peak. Quppe as recommended by EURL with specific chromatographic conditions should be better.
C, D
Bromide ion Assigned value: 15.4 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
48 4.5 Yes wir haben unsere Bromid-Analyse in dem Soja-Mehl des SRM13 noch einmal näher untersucht. Wir verwenden die Methode DIN EN 13191-2 (2000-10) mit GC-ECD-Detektion. Wir verwenden sie für Gemüse, hauptsächlich Salat und bisher schien die Methode sehr robust zu sein - wir haben bisher alle Bromid-Ringversuche bestanden. Ein Problem ist die geringe vorgeschriebene Einwaagemenge für trockene Proben. Da die Konzentration an Bromid im Sojamehl ebenfalls recht niedrig war, mussten wir knapp an der Bestimmungsgrenze messen. Wir haben die Analyse des Ringver-suchs wiederholt, parallel auch einen alten Ringversuch in Brokkoli. Das Ergebnis der Wiederholung in Sojamehl war zwar etwas niedriger als vorher, aber immer noch zu hoch, während die Konzentration in Brokkoli mit dem Referenzwert übereinstimmte. Wir ziehen daraus den Schluss, dass unsere Analysenmethode für das Sojamehl (und vermutlich andere trockene Proben) nicht geeignet ist. Wir wollten aber ohnehin die Bromid-Bestimmung auf die QuPPe-Methode und LC-MS/MS-Detektion umstellen.
C, G
EUPT-SRM13 | 2018 (Soybean Flour)
A-28
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Cyromazine Assigned value: 0.097 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
62 -2.2 Yes The recovery obtained in the spiked sample of the blank material was 67 %. It com-plains with the acceptance criteria for recovery in routinary analysis (60-140%), so recovery factor was not applied to correct sample concentration. The low recovery obtained would explain the low concentration submitted for ciromazine (0.0446 mg/kg).
K
78 -2.1 (Yes) No experience; The reason for the poor performance is probably due to problems with extraction efficiency (human error or matrix effect). Investigations in progress.
C, D
74 -2.1 Yes significant matrix effect. We have not much experience with this matrix C, D
3rd-122 2.1 Yes "Error calculation, because we used a factor of two during the calculation of the results for these pesticides. The implementation of the analytical method for theses pesticide is in process in our laboratory; but we consider to send our result of these pesticide to SRM13 as an opportunity in order to have a preliminary evaluation of our analytical performance. Currently we don’t include these pesticide on the scope our analytical method for routine analysis. "
D, F
109 2.9 (Yes) It’s probably a standard problem (ordered 7 years ago). A new one will be ordered and a comparison made
E?
45 3.7 Yes Matrix effect (Area of ILIS of cyromazine in the sample extract was half so big as that in the calitration solutions); Einen Pipettierfehler der Lösung des Internen Stand-ards schließe ich aus, da wir alle Internen Standards in einer Dotierlösung haben. Was ich unter den gegebenen Umständen nicht sagen kann ist, ob beim Ansetzen der Lösung ein Pipettierfehler vorgelegen hat. Den Extrakt haben wir zusätzlich verdünnt gemessen. Allerdings habe wir bei der Verdünnung den Internen Standard aufgestockt (Verdünnung mit Blankextrakt dem interner Standard für Aufarbeitung zugesetzt wurde). Hier bei erhalten wir einen Gehalt von 0,081mg/kg. Allerdings ist die Fläche des IS im verd. Extrakt auch etwas niedriger als in den Kalibrierlösungen. Aktuell setzen wir gerade unsere Stamm- und Arbeitslösungen neu an. Es ist geplant die LVU nach Austausch der Lösungen erneut aufzuarbeiten und die Parameter zu bestimmen. Im Zuge der Nachanalyse der LVU werden wir ggf. die Bestimmung auch gegen eine über das Gesamtverfahren aufgearbeitete Kalibrierung durchführen.
E
106 34.8 Yes Transcription error resulting from difficulties of the submission tool J
19 44.7 Yes Concentration of calibration standard not correct (too low) E
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-29
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
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a7Fluazifop Assigned value: 0.049 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
3rd-118 -3.2 (FN)
Yes Our standard solution was Fluazifop-butyl, not free acid N
45 -2.2 No Reason not found U
Glyphoaste Assigned value: 0.903 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
105 -2.4 Yes Out of lab routine scope, we don’t have the experience yet. D
5 -2.1 (Yes) Our lab don`t consider the result of glyphosate as poor performance. The reasons are: our 2 analysts have made overall 6 replacates of the sample SRM13, 6 replicates of recovery (addition to blank SRM13). All above mentioned replicates were analysed with two analytical chormatographic columns: ACCLAIM Trinity and Hypercarb. We have made several dilutions to explore dependance between concentration and dilution factor: 4 graphs each has 6 points=> 24 dilutions. Our LC/MS/MS piping is metallic, so we have to passive the piping. We can`t change pipes into plastic, because plastic pipes don`t tolerate pressure very well. It was the first time to analyse soya matrix for us and Quppe method didn`t perform very well. At the moment we don`t use IS, because it is very expensive to buy it just for PT. If we start analyse samples then we consider to buy it. Perhaps IS facilitates the analysis.
A, D
44 4.8 Yes few experience (less than one year), matrix effect and too less sample used for analy-sis. The result reported was from a sample weight of 0.2 g with clean extract. With a sample weight of 0.5 g, the extract was dirty and, therefore, the result (0.821 mg/kg) was not submitted.
C, D, I
80 6.2 Yes Very likely due to matrice - we never analyse such heavy matrice (20% fat). We do quantification with Standard addition for glyphosate, this seems not appropriate for difficult matrices. Our first results using external calibration gave concentrations of 1.25 mg/kg. With our second extern calibration with more calibartion points we got 1.08 mg Glypho-sate/kg. Comment from Organizer: Standard addition may indeed be associated with an error if the function is curved. If the lower part of the curve is still linear you may skip the upper points and just do a one-point standard addition. Otherwise dilution will help you to reach the linear range. If you use isotope labelled standard it should also behave similarly to the native one in terms of non-linearity, so the ratio should be expectedly still close to linear even if you work within a non-linear range.
C, D; L
103 55.8 (Yes) our method is a screening method used only to determinate if glyphosate is more then 0,1 mg/kg we checked our result and we observed we made a mistake with the amount of inter-nal standard but also in this case we have a lower z-score > 3. we think that the only way to solve our problems is use ionic chromatography.
Haloxyfop Assigned value: 0.017 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
3rd-115 -3.3 (FN)
Yes No IS was used and therefore the matrix effect not properly compensated. After us-ing IS (Bentazon-D7) the result was 0.173 mg/kg.
C
3rd-116 -2.3 Yes For Haloxyfop, we had 2 group of results, in interval from 0,004mg/kg to 0,009mg/kg, and group with 2 results of 0,014mg/kg and 0,015mg/kg. We calculated the average of first group of results without last two and it was a mistake. If we had calculated the average of all results, z-score would have been satisfactory.
F
105 -2.3 Yes Matrix in not within our routine scope. D
EUPT-SRM13 | 2018 (Soybean Flour)
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Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Mepiquat Assigned value: 0.124 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
2 -3.7 (FN)
Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.
B, G
66 -3.7 (FN)
Yes Transcription error under stress caused by technical problem with LC-MS/MS (actually 0.175 mg/kg)
J
63 -3.3 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.
C, G
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-31
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
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2,4-DB Assigned value: 0.183 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
55 -3.8 (FN)
Yes Transcritption error (actually not analysed), not routinely analysed J
109 -3.8 (FN)
Yes transcriptional error, actually not analysed J
86 3.0 Yes This poor performance was probably due to the use of an old calibration solution. We did not detect this problem as our 2,4-DB recovery was correct. New standard ordered, investigation ongoing.
E
Mepiquat Assigned value: 0.124 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
97 -3.1 Yew "The sample has been hydrolyzed by adding water to the weighted fraction of sam-ple. After 10 minutes the extraction is started by acidified methanol extraction. The calculations have been checked and it was OK. The normal used method applies for fruits and vegetables. Because of the sample are an dried product an additional step of hydrolyzation has been applied for the analysis of the SRM material. An investigation has been carried out for the hydrolyzation time by adding water to different fractions of the SRM sample and proceeding to the extraction step after 10 min and over two nights. The results are below: - Starting with the extraction after 10 minutes hydrolyzation time: concentration of mepiquat is 0.026 mg/kg. The results of the first and reported results is 0.027 mg/kg and the waiting time was 15 min. - Starting with the extraction after 2 nights hydrolyzation time: concentration of mepiquat is 0.077 mg/kg . The reason for poor results is a non optimal extraction time of the dried product. This will be further investigated.
D, G
83 -3.1 Yes we have never analyzed Mepiquat in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 0,120 mg/kg
C, D, G
105 2.1 Yes Matrix in not in our routine scope. D
49 17.2 Yes conversion factor for mepiquat ion to mepiquate chlorate was incorrect Q
101 2.4 No The result of the repeat is 0.076 mg / kg. This gives a Z-score of -1.56, which satisfies, which satisfies. No deviations in integration, calibration, standards and control sam-ple were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. The original z-score was just above 2. This in combination with the good scores of the reanalysis is the conclusion that the deviation only applies to the sequence in which the ring test was measured.
U
3rd-122 4.7 Yes Error calculation, because we used a factor of two during the calculation of the results for these pesticides. The implementation of the analytical method for theses pesticide is in process in our laboratory; but we consider to send our result of these pesticide to SRM13 as an opportunity in order to have a preliminary evaluation of our analytical performance. Currently we don’t include these pesticide on the scope our analytical method for routine analysis.
D, F
19 39 Yes Concentration of calibration standard not correct (too low) E
EUPT-SRM13 | 2018 (Soybean Flour)
A-32
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Glufosinate Assigned value: 0.192 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
55 -3.6 (FN)
Yes Transcritption error (actually not analysed), not routinely analysed J
89 -3.6 (FN)
Yes No experience with this analyte, re-analysed and evaluated: 0.981 mg/kg, z-score = 0.7
D
105 -3.6 (FN)
Yes Out of lab routine scope, we don’t have the experience yet. D
3rd-121 -3.6 (FN)
Yes detected concentration 0.182 mg/kg < RL (0.5 mg/kg), therefore no numerical result reported.
H
17 -2.6 Yes two analysis and two other for recovery were conducted; errors occured during sample preparation and lack of material no repeatation was possible; no information about the recovery was available, and the result was not corrected by the recovery.
B, R, P
44 2.7 Yes few experience (less than one year), matrix effect and too less sample used for analy-sis. The result reported was from a sample weight of 0.2 g with clean extract. With a sample weight of 0.5 g, the extract was dirty and, therefore, the result (0.19 mg/kg) was not submitted.
C, D, I
62 3.7 Yes The recovery obtained in the spiked sample of the blank material was 42 %. It does not complain with the acceptance criteria for recovery in routinary analysis (60-140%), so recovery factor was applied to correct sample concentration. However, we should have demonstrate good reproducibility before apply this recovery factor
K
63 10.6 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.
C, G
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-33
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
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a7MPP Assigned value: 0.188 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
109 -3.6 (FN)
Yes transcriptional error, actually not analysed J
105 -2.6 Yes Out of lab routine scope, we don’t have the experience yet. D
35 2.5 Yes we have no experience with this compound (not analysed till today in the labora-tory). Analysed to test us. A correction with glyphosate C13 was done but MPP D3 for recovery correction should be better
D, L
101 9.1 No The result of the repeat is 0.268 mg / kg. This gives a Z-score of 1.7, which satisfies. No deviations in integration, calibration, standards and control sample were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. This component is kept in the control card and there are no deviations in the chard. Because the re-analysis is good, this deviation also applies only to the sequence in which it was measured.
U
45 19 Yes bad chromatography (small and wide peak, perhaps column not sufficiently precon-ditioned)
B?, M
N-Acetyl glyphosate Assigned value: 0.835 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
45 -3.9 (FN)
Yes transcrpition errer (confusing between n-acetyl-glyphosate and n-ycetyl-glufosi-nate); ich muss gestehen, dass ich mir bei dem N-Acetyl-Glyphosat nicht die Abwei-chung zum assigned value angesehen hatte. Wir haben das N-Acetyl-Glyphosat gegen das isotopenmarkierte Glyphosat als Internem Standard ausgewertet. Bei der erneuten Durchsicht der Daten ist mir aufgefallen, dass die Widerfindung für das N-Acetylglyphosat um den Faktor 2 zu hoch ist, während die Wiederfindung für Glyphosat i.O. ist (98%). Die Fläche des Internen Standards ist im LVU-Probenextrakt geringer als in den Kalibrierlösungen, was den Überbefund erklären könnte (für die Kalibrierung dotieren wir den Blank-Extrakt an, keine Kalibrierung über Gesamtver-fahren). Auswertung ohne internen Standard gegen die externe Kalibrierung liefert etwas geringere Werte von ~1,0 mg/kg. Aktuell setzen wir gerade unsere Stamm- und Arbeitslösungen neu an. Es ist geplant die LVU nach Austausch der Lösungen erneut aufzuarbeiten und die Parameter zu bestimmen. Im Zuge der Nachanalyse der LVU werden wir ggf. die Bestimmung auch gegen eine über das Gesamtverfahren aufgearbeitete Kalibrierung durchführen.
J
55 -3.9 (FN)
Yes Transcritption error (actually not analysed) The N acetylglyphosate is not analyzed because the Hypercarb column is too tricky to maintain in routine flow. So we let it for an ionic column and it’s impossible to get it
J
76 -3.9 (FN)
Yes Transcription error. (This was a result submission error. This compound is not part of the laboratory’s scope. It is not a true false negative result, the laboratory does not currently analyse for n-acetyl-glyphosate.)
J
89 -3.9 (FN)
Yes No experience with this analyte D
109 -3.9 (FN)
Yes transcriptional error, actually not analysed J
34 76 Yes Standard used (pure substance) for calculation was probably degradeted (cp. with a new standard resulted to a factor of 25.)
E
EUPT-SRM13 | 2018 (Soybean Flour)
A-34
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Perchlorate Assigned value: 0.100 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
2 -3.6 (FN)
Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.
B, G
109 -3.6 (FN)
Yes transcriptional error, actually not analysed J
83 -3.1 Yes we have never analyzed perchlorate in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 0,090 mg/kg.
C, D, G
63 -2.7 (Yes) We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.
C, G
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-35
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
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a7Perchlorate Assigned value: 0.100 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
35 -2.1 Yes we have no experience with soybean flour. A correction with fosetyl D15 is done and usually give us good results. Perchlorate O18 for recovery correction should be better.
D, L
26 2.4 Yes Soy matrix little analyzed by the laboratory - essentially water-rich matrix - no ac-creditation on perchlorate; Intégration large sur la 1ère analyse et ajouts dosé trop importants par rapport à la concentration cible. Relance avec ajouts dosé plus faibles (0,2 et 0,4) qui permettent d'obtenir un résultat conforme. Suivi de ce paramètre sur les essais ultérieurs.
D
69 3.7 Yes Precipitation of stock solution (1mg/ml MeOH with 5% FA) stored at -20 °C that was not redisolved at ambient temperature. New stock prepared in 50% MeOH/50% Water with 5% FA. No ppt even stored at low temperature. With new stock: conc. determined at 0,077 mg/kg, corresponding to a z.score of -0.9; Recovery: 77%
E
101 9.5 No The cause was probably the concentration of the blank that was forgotten to take of the result. The result after blank correction is (0.355-0.214) 0.121 mg / kg. This yields a Z score of 0.85. This does meet. The deviation of perchlorate applies, however, only to this sequence. In "regular" samples no blank is included and therefore no blank deduction is possible.
U
Phosphonic acid Assigned value: 1.86 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
11 -3.9 (FN)
Yes Transcription error resulting from difficulties of the submision tool (actually not analysed at all)
J
97 -3.9 (FN)
Yes The peak of phosphonic acid detected in the sample fulfills the criteria of retention time and MRM ratio, (see the chromatograms 1 and 2). By adding a known amount of phosphonic acid to a second fraction of the sample, by applying the standard addi-tion method, the detected peak splits in to two peaks that are not totally separated. The detected peak of phosphonic acid in the first fraction without addition is consid-ered as false positive and the results are not reported. Because of a poor z-score the extracts analyses performed on the SRM material are repeated with a 20 times extra dilution of the extracts compared to the initial meas-urements performed by the first analyses of the SRM samples. The obtained peaks shape was good and the splitting in the spiked extract was not observed, (see the chromatograms 3 and 4). The reason for poor results is an insufficient chromatography method application. A new method will be developed using a different column with more separation power.
F, G
2 -3.7 Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuEChERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.
B, G
EUPT-SRM13 | 2018 (Soybean Flour)
A-36
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Phosphonic acid Assigned value: 1.86 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
83 -3.2 Yes Until now, we have never analyzed Phosphonic acid in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 2,90 mg/kg.
C, D, G
63 -3.2 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.
C, G
91 -2.5 Yes Despite the fact, that the isotopically labelled phosphorus acid standard has been used and the prepared spike in the blank matrix has provided a satisfactory value, these measures did not provide effective help in case of the correct determination of phosphonic acid as incurred residues. After re-extraction of sample, when 2.5 g was weighted and soaking time was extended to 30 min (instead of 10 min in original procedure), we obtained the concentration of phosphonic acid 1.871 mg/kg. Considering this fact the soaking time seems to be the key parameter for our originally reported concentration level of phosphonic acid.
G
41 12.1 (Yes) in the same analytical batch we processed the EUPT_SRM12 material and we obtained the acceptable result for this molecule. So we believed that EUPT_SRM13 results was good. Now we are testing our standard pool and single Phosphonic acid solution to verify the retention time and possible degradation of other pesticides in pool to Phosphonic acid.
E?
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
Appendix 7. Possible Reasons Reported for Poor Performance
A-37
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
Rea
son
foR
poo
R peR
foRm
an
ce
a7Quizalofop Assigned value: 0.052 mg/kg
LabCode z-Score Source of error localized? Reason / Remarks
47 -4 (FN)
Yes The active substance that we analyzed is Quizalofop-ethyl CAS No. 76578. (The analy-sis was carried out by extraction with acetonitrile, cleaning with PSA and evaporation of the extract in a stream of nitrogen. The addition made to the white sample at the level of 0.01 mg / kg gives a correct recovery of 68%.)
U
66 -3.2 (FN)
Yes Transcription error under stress caused by technical problem with LC-MS/MS (actually 0.034 mg/kg)
J
3rd-118 -3.2 (FN)
Yes Our standard solution was Quizalofop-ethyl, not free acid N
76 -2.3 Yes Ne experience and special matrix effect of soybean flour. (Soybean flour is not tested routinely in our laboratory. There was a poor recovery of quizalofop in the lab soybean flour spike (56%) analysed with this PT scheme. This poor recovery is unique to soybean flour and not other cereals analysed by the laboratory. The lab did not correct for recovery. If the lab had corrected for recovery in the spike then the z-score would have been acceptable.)
C, D
26 -2.2 Yes Soy matrix little analyzed by the laboratory - essentially water-rich matrix - no ac-creditation on quizalofop; Sous dosage lors de la 1ère analyse, rendement pris en compte lors du rendu. Relance conforme. Problème ponctuel d'extraction
D
101 -2.2 No The result of the repeat is 0.030 mg / kg. This gives a Z-score of -1.7, which satisfies. No deviations in integration, calibration, standards and control sample were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. The original z-score was just below -2. This in combination with the good scores of the reanalysis is the conclusion that the deviation only applies to the sequence in which the ring test was measured.
U
112 2.2 Yes the evaluation of this non-conformity showed that the standard used for Quizalofop was 20% too low, presumably due to precipitation. When correcting for this factor, we would have found a value of 0,064 mg/kg, thus well within the acceptable range
U
2 2.4 Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.
B, G
EUPT-SRM13 | 2018 (Soybean Flour)
A-38
Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)
A: Technical problems/diffculties with measurement instrumentation
B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value
I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault
K: Result not corrected for low recoveryL: Inappropriate calibration
M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences
N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined
False Positive ResultsAnalyte LabCode Reason / Remarks
Ethephon 41 we determined the pesticide using only one transition and now we are trying to use a second qualifier transition to be compliant to SANTE regulation
G
N-Acetyl glufosinate
45 transcrition errer (confusing between n-acetyl-glyphosate and n-ycetyl-glufosinate) J
AMPA 41 we quantified an interfering peak, so we tried to change the quantifier ion F, M
AMPA 3rd-118 For Glyphosate we use HPLC with post column derivertizer and analysis Glyphosate and AMPA (N-Acetyl-Glyphosate not analysis), we found AMPA in blank. Our LC con-dition had the wrong separation due to dry soybean matrix or N-Acetyl-Glyphosate . We will purchase N-Acetyl-Glyphosate standard and check again. Comment form Organizer: Contamination
C, M, O
Paraquat 3rd-118 Paraquat we use LC-MS, Idenitfication not enough for dry soybeans matrix due to we found paraquat in sample blank cannot separate paraquat with matrix in soybeans Comment form Organizer: Contamination
C, O
A-39
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
A8
Gen
erA
l Pro
toco
(8th
ed
.)
Appendix 8. General EUPT Protocol (8th Ed.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 1
of 1
6
GEN
ERA
L PR
OTO
CO
L fo
r EU
Pro
ficie
ncy
Test
s on
Pes
ticid
e R
esid
ues
in
Foo
d an
d Fe
ed
Intr
oduc
tion
This
pro
toco
l con
tain
s ge
nera
l pro
cedu
res
valid
for
all E
urop
ean
Uni
on P
rofic
ienc
y Te
sts
(EU
PTs)
or
gani
sed
on b
ehal
f of
the
Eur
opea
n C
omm
issi
on,
DG
-SAN
TE1
by t
he f
our
Euro
pean
Uni
on
Ref
eren
ce L
abor
ator
ies
(EU
RLs
) re
spon
sibl
e fo
r pe
stic
ide
resi
dues
in
food
and
fee
d. T
hese
EU
PTs
are
dire
cted
at l
abor
ator
ies
belo
ngin
g to
the
Net
wor
k2 of
Nat
iona
l Ref
eren
ce L
abor
ator
ies
(NR
Ls)
and
Offi
cial
Lab
orat
orie
s (O
fLs)
of t
he E
U M
embe
r St
ates
. OfL
s fro
m E
FTA
coun
tries
and
EU
-Can
dida
te c
ount
ries
are
also
wel
com
e to
par
ticip
ate
in th
e EU
PTs.
OfL
s fro
m T
hird
cou
ntrie
s m
ay b
e pe
rmitt
ed to
par
ticip
ate
on a
cas
e-by
-cas
e ba
sis.
The
follo
win
g fo
ur E
UR
Ls f
or p
estic
ide
resi
dues
wer
e ap
poin
ted
by D
G-S
ANTE
bas
ed o
n re
gula
tion
(EC
) 625
/201
73 :
EU
RL
for F
ruits
and
Veg
etab
les
(EU
RL-
FV),
EU
RL
for C
erea
ls a
nd F
eedi
ngst
uffs
(EU
RL-
CF)
,
EU
RL
for F
ood
of A
nim
al O
rigin
and
Com
mod
ities
with
Hig
h Fa
t Con
tent
(EU
RL-
AO) a
nd
EU
RL
for p
estic
ides
requ
iring
Sin
gle
Res
idue
Met
hods
(EU
RL-
SRM
).
The
aim
of t
hese
EU
PTs
is to
obt
ain
info
rmat
ion
rega
rdin
g th
e qu
ality
, acc
urac
y an
d co
mpa
rabi
lity
of p
estic
ide
resi
due
data
in fo
od a
nd fe
ed re
porte
d to
the
Euro
pean
Uni
on w
ithin
the
fram
ewor
k of
th
e na
tiona
l co
ntro
l pr
ogra
mm
es a
nd t
he
EU m
ultia
nnua
l co
-ord
inat
ed c
ontro
l pr
ogra
mm
e4 . Pa
rtici
patin
g la
bora
torie
s w
ill be
pro
vide
d w
ith a
n as
sess
men
t of t
heir
anal
ytic
al p
erfo
rman
ce th
at
1 DG
-SA
NTE
= E
urop
ean
Com
mis
sion
, Hea
lth a
nd F
ood
Saf
ety
Dire
ctor
ate-
Gen
eral
2 F
or m
ore
info
rmat
ion
abou
t the
EU
RL/
NR
L/O
fL-N
etw
ork
plea
se re
fer t
o th
e E
UR
L-W
eb-p
orta
l und
er:
ht
tp://
ww
w.e
url-p
estic
ides
.eu
3 Reg
ulat
ion
(EU
) 201
7/62
5 of
the
Eur
opea
n P
arlia
men
t and
of t
he C
ounc
il on
offi
cial
con
trols
and
oth
er o
ffici
al a
ctiv
ities
pe
rform
ed to
ens
ure
the
appl
icat
ion
of fo
od a
nd fe
ed la
w, r
ules
on
anim
al h
ealth
and
wel
fare
, pla
nt h
ealth
and
pla
nt
prot
ectio
n pr
oduc
ts..
Pub
lishe
d at
OJ
of th
e E
U L
95 o
f 07.
04.2
017
4 Eur
opea
n C
omm
issi
on P
rofic
ienc
y Te
sts
for P
estic
ide
Res
idue
s in
Fru
its a
nd V
eget
able
s, T
rend
s in
Ana
lytic
al
Che
mis
try, 2
010,
29
(1),
70 –
83.
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 2
of 1
6
they
can
use
to
dem
onst
rate
the
ir an
alyt
ical
per
form
ance
and
com
pare
the
mse
lves
with
oth
er
parti
cipa
ting
labo
rato
ries.
EU
PT-O
rgan
iser
s an
d Sc
ient
ific
Com
mitt
ee
EUPT
s ar
e or
gani
sed
by in
divi
dual
EU
RLs
, or b
y m
ore
than
one
EU
RL,
in jo
int c
olla
bora
tion.
An O
rgan
isin
g Te
am i
s ap
poin
ted
by t
he E
UR
L(s)
in
char
ge.
This
tea
m i
s re
spon
sibl
e fo
r al
l ad
min
istra
tive
and
tech
nica
l m
atte
rs
conc
erni
ng
the
orga
nisa
tion
of
the
PT,
e.g.
th
e PT
-an
noun
cem
ent,
prod
uctio
n of
Tes
t Ite
m a
nd B
lank
Mat
eria
l, th
e un
derta
king
of
hom
ogen
eity
and
st
abilit
y te
sts,
pac
king
and
shi
pmen
t of t
he T
est I
tem
and
Bla
nk M
ater
ial,
hand
ling
and
eval
uatio
n of
the
res
ults
and
met
hod
info
rmat
ion
subm
itted
by
the
parti
cipa
nts
and
the
draf
ting
of t
he
prel
imin
ary
and
final
repo
rts.
To c
ompl
emen
t the
inte
rnal
exp
ertis
e of
the
EUR
Ls, a
gro
up o
f ext
erna
l con
sulta
nts
that
form
the
EUPT
-Sci
entif
ic C
omm
ittee
(EU
PT-S
C)5 h
as b
een
esta
blis
hed
and
appr
oved
by
DG
-SAN
TE. T
he
EUPT
-SC
con
sist
s of
exp
ert
scie
ntis
ts w
ith m
any
year
s of
exp
erie
nce
in P
Ts a
nd/o
r pe
stic
ide
resi
due
anal
ysis
. The
act
ual c
ompo
sitio
n of
the
EUPT
-SC
, the
affi
liatio
n of
eac
h m
embe
r is
show
n on
the
EU
RL-
Web
site
. The
mem
bers
of
the
EUPT
-SC
will
also
be
liste
d in
the
Spe
cific
Pro
toco
l an
d th
e Fi
nal R
epor
t of e
ach
EUPT
.
The
EUPT
-SC
is m
ade
up o
f the
follo
win
g tw
o su
bgro
ups:
a)
An in
depe
nden
t Qua
lity
Con
trol
Gro
up (E
UPT
-QC
G) a
nd
b)
An A
dvis
ory
Gro
up (E
UPT
-AG
).
The
EUPT
-SC
’s r
ole
is t
o he
lp t
he O
rgan
iser
s m
ake
deci
sion
s re
gard
ing
the
EUPT
des
ign:
the
se
lect
ion
of th
e co
mm
odity
, the
sel
ectio
n of
pes
ticid
es to
be
incl
uded
in th
e Ta
rget
Pes
ticid
e Li
st
(see
bel
ow),
the
esta
blis
hmen
t of t
he M
inim
um R
equi
red
Rep
ortin
g Le
vels
(MR
RLs
), th
e st
atis
tical
tre
atm
ent a
nd e
valu
atio
n of
par
ticip
ants
resu
lts (i
n an
onym
ous
form
), an
d th
e dr
aftin
g an
d up
datin
g of
doc
umen
ts s
uch
as th
e G
ener
al a
nd S
peci
fic P
T Pr
otoc
ols
and
the
Fina
l EU
PT-R
epor
ts.
The
EUPT
-QC
G h
as th
e ad
ditio
nal f
unct
ion
of s
uper
visi
ng t
he q
ualit
y of
EU
PTs
and
of a
ssis
ting
the
EUR
Ls in
con
fiden
tial a
spec
ts s
uch
as th
e ch
oice
of
the
pest
icid
es to
be
pres
ent i
n th
e Te
st
Item
and
the
conc
entra
tions
at w
hich
they
sho
uld
be p
rese
nt.
5 Lin
k to
the
List
of c
urre
nt m
embe
rs o
f the
EU
PT
Sci
entif
ic C
omm
ittee
: ht
tp://
ww
w.e
url-p
estic
ides
.eu/
libra
ry/d
ocs/
allc
rl/E
UP
T-S
C.p
df
Appendix 8 General EUPT Protocol (8th Ed.)
EUPT-SRM13 | 2018 (Soybean Flour)
A-40
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 4
of 1
6
NR
Ls a
re r
espo
nsib
le f
or c
heck
ing
whe
ther
all
rele
vant
OfL
s w
ithin
the
ir ne
twor
k ar
e in
clud
ed in
th
e lis
t of
obl
igat
ed la
bora
torie
s an
d w
heth
er t
he c
onta
ct in
form
atio
n an
d co
mm
odity
-sco
pes
are
corr
ect.
OfL
s ar
e fu
rther
mor
e ur
ged
to k
eep
thei
r ow
n pr
ofile
s w
ithin
the
EU
RL-
Dat
aPoo
l up
-to-d
ate,
es
peci
ally
thei
r com
mod
ity a
nd p
estic
ide
scop
es a
nd th
eir c
onta
ct in
form
atio
n.
Labs
tha
t ar
e ob
liged
to
parti
cipa
te in
a g
iven
EU
PT,
and
that
are
not
abl
e to
par
ticip
ate,
mus
t pr
ovid
e th
e re
ason
s fo
r th
eir
non-
parti
cipa
tion
with
out p
reju
dice
of a
ny le
gal a
ctio
n ta
ken
agai
nst
them
for
not p
artic
ipat
ing.
Thi
s al
so a
pplie
s to
any
par
ticip
atin
g la
bora
torie
s th
at th
en fa
il to
rep
ort
resu
lts.
Base
d on
Reg
. (E
C)
625/
2017
, O
fLs
not
payi
ng t
he E
UPT
sam
ple
deliv
ery
fee
will
be i
nitia
lly
war
ned
that
thei
r pa
rtici
patio
n in
sub
sequ
ent E
UPT
s co
uld
be d
enie
d. In
cas
e of
a r
epet
itive
non
-pa
ymen
t, th
e EU
PT o
rgan
iser
s w
ill in
form
the
com
pete
nt a
utho
rity
to ta
ke a
ctio
n.
Con
fiden
tialit
y an
d C
omm
unic
atio
n
The
prop
rieto
r of a
ll EU
PT d
ata
is D
G-S
ANTE
and
as
such
has
acc
ess
to a
ll in
form
atio
n.
For
each
EU
PT,
the
labo
rato
ries
are
give
n a
uniq
ue c
ode
(lab
code
), in
itial
ly o
nly
know
n to
th
emse
lves
and
the
Org
anis
ers.
In th
e fin
al E
UPT
-Rep
ort,
the
nam
es o
f par
ticip
atin
g la
bora
torie
s w
ill no
t be
linke
d to
thei
r lab
orat
ory
code
s. It
sho
uld
be n
oted
, how
ever
, tha
t the
Org
anis
ers,
at t
he
requ
est
by D
G-S
ANTE
, m
ay p
rese
nt t
he E
UPT
-resu
lts o
n a
coun
try-b
y-co
untry
bas
is.
It m
ay
ther
efor
e be
pos
sibl
e th
at a
link
bet
wee
n co
des
and
labo
rato
ries
coul
d be
mad
e, e
spec
ially
for
th
ose
coun
tries
whe
re o
nly
one
labo
rato
ry h
as p
artic
ipat
ed.
Furth
erm
ore,
the
EUR
Ls r
eser
ve th
e rig
ht t
o sh
are
EUPT
res
ults
and
cod
es a
mon
gst
them
selv
es:
for
exam
ple,
for
the
pur
pose
of
eval
uatin
g ov
eral
l lab
or c
ount
ry p
erfo
rman
ce a
s re
ques
ted
by D
G-S
ANTE
.
As la
id d
own
in R
egul
atio
n 62
5/20
17, N
RLs
are
resp
onsi
ble
for s
uppo
rting
and
impr
ovin
g th
eir o
wn
OfL
-Net
wor
k. O
n re
ques
t fro
m t
he N
RLs
, th
e EU
RLs
will
prov
ide
them
with
the
PT-
code
s of
the
pa
rtici
patin
g O
fLs
belo
ngin
g to
the
ir O
fL-N
etw
ork.
Thi
s w
ill al
low
NR
Ls t
o fo
llow
the
par
ticip
atio
n an
d pe
rform
ance
of t
he la
bora
torie
s w
ithin
thei
r net
wor
k.
Com
mun
icat
ion
betw
een
parti
cipa
ting
labo
rato
ries
durin
g th
e te
st o
n m
atte
rs c
once
rnin
g a
PT
exer
cise
is n
ot p
erm
itted
from
the
star
t of t
he P
T ex
erci
se u
ntil
the
dist
ribut
ion
of th
e pr
elim
inar
y re
port.
For
each
EU
PT t
he o
rgan
isin
g EU
RL
prep
ares
a s
peci
fic E
UPT
-Web
site
whe
re a
ll re
leva
nt
docu
men
ts in
thei
r lat
est v
ersi
on a
re li
nked
.
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 3
of 1
6
The
EUPT
-SC
typi
cally
mee
ts o
nce
a ye
ar, a
fter t
he E
UPT
s of
all
four
pes
ticid
e EU
RLs
hav
e be
en
cond
ucte
d, t
o di
scus
s th
e ev
alua
tion
of t
he E
UPT
-resu
lts a
nd t
o co
nsul
t with
the
EU
RLs
in t
heir
deci
sion
mak
ing.
Upc
omin
g EU
PTs
are
also
pla
nned
dur
ing
thes
e m
eetin
gs.
The
EUPT
-Org
anis
ing
Team
and
the
EUPT
-SC
toge
ther
form
the
EUPT
-Pan
el.
The
deci
sion
s of
the
EUPT
-Pan
el w
ill be
doc
umen
ted.
This
pre
sent
EU
PT G
ener
al P
roto
col w
as jo
intly
dra
fted
by th
e EU
PT-S
C a
nd th
e EU
RLs
and
was
ap
prov
ed b
y D
G-S
ANTE
.
EUPT
Par
ticip
ants
With
in th
e Eu
rope
an U
nion
all
NR
Ls o
pera
ting
in th
e sa
me
area
as
the
orga
nisi
ng E
UR
L, a
s w
ell
as a
ll O
fLs
who
se s
cope
ove
rlaps
with
tha
t of
the
EU
PT,
are
lega
lly o
blig
ed t
o pa
rtici
pate
in
EUPT
s. T
he le
gal o
blig
atio
n of
NR
Ls a
nd O
fLs
to p
artic
ipat
e in
EU
PTs
aris
es fr
om:
- Ar
t. 28
of
Reg
. 39
6/20
05/E
C6
(for
all
OfL
s an
alys
ing
for
pest
icid
e re
sidu
es w
ithin
the
fra
mew
ork
of o
ffici
al c
ontro
ls7 o
f foo
d or
feed
)
- Ar
t. 10
1 (1
)(a) o
f Reg
. (EC
) 625
/201
7 (fo
r all
NR
Ls)
The
four
EU
RLs
will
annu
ally
issu
e an
d di
strib
ute,
via
the
EUR
L-w
ebsi
te, a
join
t lis
t of a
ll O
fLs
that
m
ust p
artic
ipat
e in
eac
h of
the
EUPT
s to
be
cond
ucte
d w
ithin
a g
iven
yea
r. Th
e lis
t of o
blig
ed la
bs
will
be u
pdat
ed e
very
yea
r to
take
acc
ount
of a
ny c
hang
es in
the
lab
prof
iles.
Inte
rim u
pdat
es w
ill be
issu
ed to
elim
inat
e an
y po
ssib
le e
rror
s.
6 R
egul
atio
n (E
C) N
o 39
6/20
05, p
ublis
hed
at O
J of
the
EU
L70
of 1
6.03
.200
5, a
s la
st a
men
ded
by R
egul
atio
n 83
9/20
08
publ
ishe
d at
OJ
of th
e E
U L
234
of 3
0.08
.200
8.
7 Offi
cial
con
trols
in th
e se
nse
of R
eg. (
EC
) 625
/201
7. T
his
incl
udes
labs
invo
lved
in c
ontro
ls w
ithin
the
fram
ewor
k of
na
tiona
l and
/or E
U-c
ontro
lled
prog
ram
mes
as
wel
l as
labs
invo
lved
in im
port
cont
rols
acc
ordi
ng to
Reg
ulat
ion
669/
2009
/EC
.
OR
GAN
ISER
S EU
PT-A
G
EUPT
-QC
G
EUPT
-Pan
el
EUPT
-SC
Appendix 8. General EUPT Protocol (8th Ed.)
A-41
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
A8
Gen
erA
l Pro
toco
(8th
ed
.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 5
of 1
6
The
offic
ial l
angu
age
used
in a
ll EU
PTs
is E
nglis
h.
Anno
unce
men
t / In
vita
tion
Lette
r
At
leas
t 3
mon
ths
befo
re
the
dist
ribut
ion
of
the
Test
Ite
m
the
EUR
Ls
will
publ
ish
an
Anno
unce
men
t/Inv
itatio
n le
tter
on th
e EU
RL-
web
-por
tal a
nd d
istri
bute
it v
ia e
-mai
l to
the
NR
L/O
fL
mai
ling
list a
vaila
ble
to th
e EU
RLs
. Thi
s le
tter w
ill in
form
abo
ut th
e co
mm
odity
to b
e us
ed a
s Te
st
Item
, as
wel
l as
links
to th
e te
ntat
ive
EUPT
-Tar
get P
estic
ide
List
and
the
tent
ativ
e E
UPT
-Cal
enda
r.
Targ
et P
estic
ide
List
This
list
con
tain
s al
l ana
lyte
s (p
estic
ides
and
met
abol
ites)
to b
e so
ught
, alo
ng w
ith t
he M
inim
um
Req
uire
d R
epor
ting
Leve
ls (
MR
RLs
) va
lid f
or th
e sp
ecifi
c EU
PT. T
he M
RR
Ls a
re ty
pica
lly b
ased
up
on
the
low
est
MR
Ls
foun
d ei
ther
in
R
egul
atio
n 39
6/20
05/E
C
or
Com
mis
sion
D
irect
ive
2006
/125
/EC
(Bab
y Fo
od D
irect
ive)
.
Labs
mus
t exp
ress
thei
r res
ults
as
stat
ed in
the
Targ
et P
estic
ides
Lis
t.
Spec
ific
Prot
ocol
For
each
EU
PT t
he o
rgan
izin
g EU
RL
will
publ
ish
a Sp
ecifi
c Pr
otoc
ol a
t lea
st 2
wee
ks b
efor
e th
e Te
st I
tem
is d
istri
bute
d to
the
par
ticip
atin
g la
bora
torie
s. T
he S
peci
fic P
roto
col w
ill co
ntai
n al
l the
in
form
atio
n pr
evio
usly
inc
lude
d in
the
Inv
itatio
n Le
tter
but
in i
ts f
inal
ver
sion
, in
form
atio
n on
pa
ymen
t an
d de
liver
y, in
stru
ctio
ns o
n ho
w t
o ha
ndle
the
Tes
t Ite
m u
pon
rece
ipt
and
on h
ow t
o su
bmit
resu
lts, a
s w
ell a
s an
y ot
her r
elev
ant i
nfor
mat
ion.
Hom
ogen
eity
of t
he T
est I
tem
The
Test
Ite
m w
ill be
tes
ted
for
hom
ogen
eity
typ
ical
ly b
efor
e di
strib
utio
n to
par
ticip
ants
. Th
e ho
mog
enei
ty t
ests
usu
ally
invo
lve
the
anal
ysis
of
two
repl
icat
e an
alyt
ical
por
tions
, ta
ken
from
at
leas
t ten
rand
omly
cho
sen
units
of t
reat
ed T
est I
tem
. Bot
h, s
ampl
e pr
epar
atio
n an
d m
easu
rem
ents
sh
ould
be
cond
ucte
d in
rand
om o
rder
.
The
hom
ogen
eity
test
dat
a ar
e st
atis
tical
ly e
valu
ated
acc
ordi
ng to
ISO
135
28, A
nnex
B o
r to
the
In
tern
atio
nal H
arm
oniz
ed P
roto
cols
join
tly p
ublis
hed
by IS
O, A
OAC
and
IUPA
C. T
he r
esul
ts o
f all
hom
ogen
eity
test
s ar
e pr
esen
ted
to th
e EU
PT-S
C. I
n sp
ecia
l cas
es, w
here
the
abov
e ho
mog
enei
ty
test
crit
eria
are
not
met
, th
e EU
PT-S
C c
onsi
derin
g al
l re
leva
nt a
spec
ts (
e.g.
the
hom
ogen
eity
re
sults
of
othe
r pe
stic
ides
spi
ked
at t
he s
ame
time,
the
ove
rall
dist
ribut
ion
of t
he p
artic
ipan
ts’
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 6
of 1
6
resu
lts, t
he a
naly
tical
diff
icul
ties
face
d du
ring
the
test
, kno
wle
dge
of th
e an
alyt
ical
beh
avio
ur o
f the
pe
stic
ide
ques
tion)
may
dec
ide
to o
verr
ule
the
test
. Th
e re
ason
s of
thi
s ov
erru
ling
have
to
be
trans
pare
ntly
exp
lain
ed in
the
Fina
l EU
PT-R
epor
t.
Stab
ility
of t
he a
naly
tes
cont
aine
d in
the
Test
Item
The
Test
Item
s w
ill al
so b
e te
sted
for
stab
ility
- ac
cord
ing
to IS
O 1
3528
, Ann
ex B
. The
tim
e de
lay
betw
een
the
first
and
the
last
sta
bilit
y te
st m
ust e
xcee
d th
e pe
riod
of th
e EU
PT-e
xerc
ise.
Typ
ical
ly
the
first
ana
lysi
s is
car
ried
out
shor
tly b
efor
e th
e sh
ipm
ent
of t
he T
est
Item
s an
d th
e la
st o
ne
shor
tly a
fter
the
dead
line
for
subm
issi
on o
f res
ults
. To
bette
r re
cogn
ise
trend
s an
d ga
in a
dditi
onal
ce
rtain
ty o
ne o
r mor
e ad
ditio
nal t
ests
may
be
cond
ucte
d by
the
Org
anis
ers.
At l
east
6 s
ub-s
ampl
es
(ana
lytic
al p
ortio
ns) s
houl
d be
ana
lyse
d on
eac
h te
st d
ay (e
.g. 2
ana
lytic
al p
ortio
ns w
ithdr
awn
from
th
ree
rand
omly
cho
sen
cont
aine
rs O
R 6
por
tions
with
draw
n fro
m a
sin
gle
cont
aine
r). In
prin
cipl
e al
l pe
stic
ides
con
tain
ed in
the
Test
Item
sho
uld
be c
heck
ed fo
r sta
bilit
y. H
owev
er, i
n in
divi
dual
cas
es,
whe
re s
uffic
ient
kno
wle
dge
exis
ts t
hat
the
stab
ility
of a
cer
tain
ana
lyte
is
very
unl
ikel
y to
be
sign
ifica
ntly
af
fect
ed
durin
g st
orag
e (e
.g.
base
d on
ex
perie
nce
from
pa
st
stab
ility
test
s or
kn
owle
dge
of it
s ph
ysic
oche
mic
al p
rope
rties
), th
e O
rgan
iser
s, a
fter
cons
ulta
tion
with
the
EU
PT-
QC
G, m
ay d
ecid
e to
om
it a
spec
ific
stab
ility
test
. The
EU
PT-S
C w
ill fin
ally
dec
ide
whe
ther
ana
lyte
s fo
r w
hich
the
sta
bilit
y te
st w
as n
ot u
nder
take
n w
ill be
incl
uded
in t
he f
inal
rep
ort,
cons
ider
ing
all
rele
vant
asp
ects
suc
h as
the
dist
ribut
ion
of th
e pa
rtici
pant
’s re
sults
(CV*
).
A pe
stic
ide
is c
onsi
dere
d to
be
adeq
uate
ly s
tabl
e if
| yi -y
| ≤ 0.
3×σ p
t, w
here
yi th
e m
ean
valu
e of
the
last
per
iod
of th
e st
abilit
y te
st, y
is th
e m
ean
valu
e of
the
first
per
iod
of th
e st
abilit
y te
st a
nd σ
pt th
e st
anda
rd d
evia
tion
used
for p
rofic
ienc
y as
sess
men
t (ty
pica
lly 2
5% o
f the
ass
igne
d va
lue)
.
The
resu
lts o
f all
stab
ility
test
s ar
e pr
esen
ted
to th
e EU
PT-S
C. I
n sp
ecia
l cas
es w
here
the
abov
e st
abilit
y te
st c
riter
ia a
re n
ot m
et,
the
EUPT
-SC
con
side
ring
all
rele
vant
asp
ects
(e.
g. t
he p
ast
expe
rienc
e w
ith th
e st
abilit
y of
the
com
poun
d, th
e ov
eral
l dis
tribu
tion
the
parti
cipa
nts’
res
ults
, the
m
easu
rem
ent
varia
bilit
y, a
naly
tical
diff
icul
ties
face
d du
ring
the
test
and
kno
wle
dge
abou
t th
e an
alyt
ical
beh
avio
ur o
f the
pes
ticid
e qu
estio
n) m
ay d
ecid
e to
ove
rrul
e th
e te
st. T
he re
ason
s of
this
ov
erru
ling
will
be tr
ansp
aren
tly e
xpla
ined
in th
e Fi
nal E
UPT
-Rep
ort.
The
Org
anis
ers
may
als
o de
cide
to c
ondu
ct a
dditi
onal
sta
bilit
y te
sts
at d
iffer
ent s
tora
ge c
ondi
tions
th
an th
ose
reco
mm
ende
d to
the
parti
cipa
nts
e.g.
at a
mbi
ent t
empe
ratu
re.
Con
side
ring
know
ledg
e ab
out t
he e
xpec
ted
susc
eptib
ility
of p
estic
ides
in th
e Te
st It
em to
pos
sibl
e lo
sses
, th
e O
rgan
iser
s w
ill ch
oose
the
shi
pmen
t co
nditi
ons
to b
e su
ch t
hat
pest
icid
e lo
sses
are
m
inim
ised
(e.
g. s
hipm
ent
of f
roze
n sa
mpl
es,
addi
tion
of d
ry i
ce).
As s
hipm
ent
time
can
diffe
r
EUPT-SRM13 | 2018 (Soybean Flour)
A-42
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 7
of 1
6
betw
een
labs
/cou
ntrie
s it
is r
ecom
men
ded
that
the
Org
anis
ers
cond
uct a
dditi
onal
sta
bilit
y te
sts
at
cond
ition
s si
mul
atin
g sh
ipm
ent.
Shou
ld c
ritic
al lo
sses
be
dete
cted
for c
erta
in p
estic
ides
the
EUPT
-SC
will
be in
form
ed (o
r the
EU
PT-Q
CG
bef
ore
or d
urin
g th
e te
st).
Cas
e-by
-cas
e de
cisi
ons
may
be
take
n co
nsid
erin
g al
l re
leva
nt a
spec
ts i
nclu
ding
the
shi
pmen
t tim
e of
the
sam
ples
to
each
la
bora
tory
.
Met
hodo
logi
es to
be
used
by
the
part
icip
ants
Parti
cipa
ting
labo
rato
ries
are
inst
ruct
ed to
use
the
anal
ytic
al p
roce
dure
(s) t
hat t
hey
wou
ld r
outin
ely
empl
oy in
offi
cial
con
trol a
ctiv
ities
(m
onito
ring
etc.
). W
here
an
anal
ytic
al m
etho
d ha
s no
t yet
bee
n es
tabl
ishe
d ro
utin
ely
this
sho
uld
be s
tate
d.
Gen
eral
pro
cedu
res
for r
epor
ting
resu
lts
Parti
cipa
ting
labo
rato
ries
are
resp
onsi
ble
for
repo
rting
th
eir
own
quan
titat
ive
resu
lts
to
the
Org
anis
er w
ithin
the
stip
ulat
ed d
eadl
ine.
Any
pes
ticid
e th
at w
as t
arge
ted
by a
par
ticip
atin
g la
bora
tory
sho
uld
be re
porte
d as
“ana
lyse
d”. E
ach
labo
rato
ry w
ill be
abl
e to
rep
ort o
nly
one
resu
lt fo
r eac
h an
alyt
e de
tect
ed in
the
Test
Item
. The
con
cent
ratio
ns o
f the
pes
ticid
es d
etec
ted
shou
ld b
e ex
pres
sed
in ‘m
g/kg
’ unl
ess
indi
cate
d ot
herw
ise
in th
e sp
ecifi
c pr
otoc
ol.
The
Test
Ite
m is
inte
ntio
nally
tre
ated
with
pes
ticid
es w
here
as t
he B
lank
Mat
eria
l is
anal
ysed
to
ensu
re th
at it
doe
s no
t con
tain
any
of t
he p
estic
ides
in th
e Ta
rget
Pes
ticid
es L
ist,
at o
r abo
ve, t
he
spec
ified
MR
RLs
. Bot
h th
e Te
st It
em a
nd B
lank
Mat
eria
l hav
e to
be
anal
ysed
by
the
parti
cipa
ting
labo
rato
ries
and
any
pest
icid
e de
tect
ed in
them
mus
t be
repo
rted.
Cor
rect
ion
of re
sults
for r
ecov
ery
Acco
rdin
g to
the
Met
hod
Valid
atio
n an
d Q
ualit
y C
ontro
l Pr
oced
ures
for
Pes
ticid
e R
esid
ues
Anal
ysis
in F
ood
and
Feed
8 , it
is c
omm
on p
ract
ice
that
pes
ticid
e an
alys
is re
sults
are
not
cor
rect
ed
for r
ecov
ery
if th
e re
cove
ry ra
tes
rang
e be
twee
n 70
and
120
%. C
orre
ctio
n of
resu
lts fo
r rec
over
y is
re
com
men
ded
if th
e av
erag
e re
cove
ry is
sig
nific
antly
diff
eren
t fro
m 1
00 %
(ty
pica
lly if
out
side
the
70 –
120
%
rang
e).
Appr
oach
es
for
reco
very
co
rrec
tion
expl
icitl
y st
ated
in
th
e D
G-S
ANTE
do
cum
ent a
re th
e us
e of
rec
over
y co
rrec
tion
fact
ors,
the
use
of s
tabl
e is
otop
e la
belle
d an
alog
ues
8 Doc
umen
t N°
SA
NTE
/118
13/2
017;
Met
hod
Valid
atio
n an
d Q
ualit
y C
ontro
l Pro
cedu
res
for P
estic
ide
Res
idue
s An
alys
is
in F
ood
and
Feed
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 8
of 1
6
of th
e ta
rget
ana
lyte
s as
Inte
rnal
Sta
ndar
ds (I
LIS
s), t
he ‘p
roce
dura
l cal
ibra
tion’
app
roac
h as
wel
l as
the
appr
oach
of ‘
stan
dard
add
ition
’ with
add
ition
s of
ana
lyte
(s)
bein
g m
ade
to a
naly
tical
por
tions
. R
esul
ts m
ay b
e co
rrect
ed f
or r
ecov
ery
only
in c
ases
whe
re t
his
corre
ctio
n is
app
lied
in r
outin
e pr
actic
e (in
clud
ing
case
s of
MR
L-vi
olat
ions
). La
bora
torie
s ar
e re
quire
d to
rep
ort
whe
ther
the
ir re
sults
wer
e ad
just
ed f
or r
ecov
ery
and,
if
a re
cove
ry f
acto
r w
as u
sed,
the
rec
over
y ra
te (
in
perc
enta
ge) m
ust a
lso
be re
porte
d. N
o re
cove
ry d
ata
are
requ
ired
whe
re c
orre
ctio
n fo
r rec
over
y is
au
tom
atic
by
addi
ng a
mou
nts
of a
naly
tes
to t
he t
est
porti
on f
or u
sing
the
‘st
anda
rd a
dditi
on’
appr
oach
, or
isot
opic
ally
-labe
lled
inte
rnal
sta
ndar
ds (
in b
oth
case
s w
ith s
piki
ng in
to th
e Te
st It
em
at t
he b
egin
ning
of
the
extra
ctio
n pr
oced
ures
) or
pro
cedu
ral
calib
ratio
n. I
n th
ese
case
s, t
he
labo
rato
ries
shou
ld re
port
the
actu
al a
ppro
ach
that
was
follo
wed
.
Met
hodo
logy
info
rmat
ion
All l
abor
ator
ies
are
requ
este
d to
pro
vide
info
rmat
ion
on th
e an
alyt
ical
met
hod(
s) th
ey h
ave
used
. A
com
pila
tion
of th
e m
etho
dolo
gy in
form
atio
n su
bmitt
ed b
y al
l par
ticip
ants
is p
rese
nted
in a
n An
nex
of t
he f
inal
rep
ort
or i
n a
sepa
rate
rep
ort.
Whe
re n
eces
sary
the
met
hods
are
eva
luat
ed a
nd
disc
usse
d, e
spec
ially
in t
hose
cas
es w
here
the
res
ult
dist
ribut
ion
is n
ot u
nim
odal
or
very
bro
ad
(e.g
. CV*
> 3
5 %
). If
no s
uffic
ient
info
rmat
ion
on th
e m
etho
dolo
gy u
sed
is p
rovi
ded,
the
Org
anis
er
rese
rves
the
rig
ht n
ot t
o ac
cept
the
ana
lytic
al r
esul
ts r
epor
ted
by t
he p
artic
ipan
ts c
once
rned
or
even
refu
se p
artic
ipat
ion
in th
e fo
llow
ing
PT.
Res
ults
eva
luat
ion
The
proc
edur
es u
sed
for t
he tr
eatm
ent a
nd a
sses
smen
t of r
esul
ts a
re d
escr
ibed
bel
ow.
Fals
e Po
sitiv
e re
sults
Thes
e ar
e re
sults
of p
estic
ides
from
the
Targ
et P
estic
ides
Lis
t, th
at a
re re
porte
d, a
t or a
bove
, the
ir re
spec
tive
MR
RL
alth
ough
the
y w
ere:
(i)
not
dete
cted
by
the
Org
anis
er,
even
afte
r re
peat
ed
anal
yses
, an
d/or
(ii)
not
det
ecte
d by
the
ove
rwhe
lmin
g m
ajor
ity (
e.g.
> 9
5 %
) of
the
par
ticip
atin
g la
bora
torie
s th
at h
ad ta
rget
ed th
e sp
ecifi
c pe
stic
ides
. In
certa
in in
stan
ces,
cas
e-by
-cas
e de
cisi
ons
by th
e EU
PT-P
anel
may
be
nece
ssar
y.
Any
resu
lts r
epor
ted
low
er th
an th
e M
RR
L w
ill no
t be
cons
ider
ed a
s fa
lse
posi
tives
, eve
n th
ough
th
ese
resu
lts s
houl
d no
t hav
e be
en re
porte
d.
Appendix 8. General EUPT Protocol (8th Ed.)
A-43
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
A8
Gen
erA
l Pro
toco
(8th
ed
.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 9
of 1
6
Fals
e N
egat
ive
resu
lts
Thes
e ar
e re
sults
for
pes
ticid
es r
epor
ted
by t
he la
bora
torie
s as
’ana
lyse
d’ b
ut w
ithou
t re
porti
ng
num
eric
al v
alue
s al
thou
gh t
hey
wer
e: a
) us
ed b
y th
e O
rgan
iser
to
treat
the
Tes
t Ite
m a
nd b
) de
tect
ed b
y th
e O
rgan
iser
as
wel
l as
the
maj
ority
of
the
parti
cipa
nts
that
had
tar
gete
d th
ese
spec
ific
pest
icid
es a
t or
abov
e th
e re
spec
tive
MR
RLs
. R
esul
ts r
epor
ted
as ’<
RL’
(R
L= R
epor
ting
Lim
it of
the
labo
rato
ry) w
ill be
con
side
red
as n
ot d
etec
ted
and
will
be ju
dged
as
fals
e ne
gativ
es. I
n ce
rtain
inst
ance
s, c
ase-
by-c
ase
deci
sion
s by
the
EUPT
-Pan
el m
ay b
e ne
cess
ary.
In c
ases
of t
he a
ssig
ned
valu
e be
ing
less
than
a fa
ctor
of 3
tim
es th
e M
RR
L, fa
lse
nega
tives
will
ty
pica
lly n
ot b
e as
sign
ed.
The
EUPT
-Pan
el m
ay d
ecid
e to
tak
e ca
se-b
y-ca
se d
ecis
ions
in
this
re
spec
t afte
r co
nsid
erin
g al
l rel
evan
t fac
tors
suc
h as
the
resu
lt di
strib
utio
n an
d th
e re
porti
ng li
mits
of
the
affe
cted
labs
.
Es
timat
ion
of th
e as
sign
ed v
alue
(xpt
)
In o
rder
to
min
imis
e th
e in
fluen
ce o
f ou
t-lyi
ng r
esul
ts o
n th
e st
atis
tical
eva
luat
ion,
the
ass
igne
d va
lue
x pt
(= c
onse
nsus
con
cent
ratio
n) w
ill ty
pica
lly b
e es
timat
ed u
sing
rob
ust
estim
ate
of t
he
parti
cipa
nt’s
mea
n (x
*) a
s de
scrib
ed in
ISO
135
28:2
0159 ,
taki
ng in
to a
ccou
nt th
e re
sults
rep
orte
d by
EU
and
EFT
A co
untri
es l
abor
ator
ies
only
. In
spe
cial
jus
tifia
ble
case
s, t
he E
UPT
-Pan
el m
ay
deci
de t
o el
imin
ate
certa
in r
esul
ts t
race
ably
ass
ocia
ted
with
gro
ss e
rrors
(se
e “O
mis
sion
or
Excl
usio
n of
resu
lts” b
elow
) or t
o us
e on
ly th
e re
sults
of a
sub
grou
p co
nsis
ting
of la
bora
torie
s th
at
have
repe
ated
ly d
emon
stra
ted
good
per
form
ance
for t
he s
peci
fic c
ompo
und
in th
e pa
st.
O
mis
sion
or E
xclu
sion
of r
esul
ts
Befo
re e
stim
atin
g th
e as
sign
ed v
alue
res
ults
ass
ocia
ted
with
obv
ious
mis
take
s ha
ve t
o be
ex
amin
ed to
dec
ide
whe
ther
they
sho
uld
be r
emov
ed fr
om th
e po
pula
tion.
Suc
h gr
oss
erro
rs m
ay
incl
ude
inco
rrec
t rec
ordi
ng (
e.g.
due
to tr
ansc
riptio
n er
rors
by
the
parti
cipa
nt, d
ecim
al p
oint
faul
ts
or t
rans
pose
d di
gits
, in
corr
ect
unit)
, ca
lcul
atio
n er
rors
(e.
g. m
issi
ng f
acto
rs),
anal
ysis
of
a w
rong
sa
mpl
e/ex
tract
(e.
g. a
spi
ked
blan
k), u
se o
f wro
ng c
once
ntra
tions
of s
tand
ard
solu
tions
, inc
orre
ct
9 D
IN I
SO
135
28:2
015,
Sta
tistic
al m
etho
ds f
or u
se in
pro
ficie
ncy
test
ing
by in
terla
bora
tory
com
paris
ons,
Int
erna
tiona
l O
rgan
izat
ion
for
Sta
ndar
diza
tion.
The
rein
a s
peci
fic r
obus
t m
etho
d fo
r de
term
inat
ion
of t
he c
onse
nsus
mea
n an
d st
anda
rd d
evia
tion
with
out t
he n
eed
for r
emov
al o
f dev
iatin
g re
sults
is d
escr
ibed
(Alg
orith
m A
in A
nnex
C).
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 10
of 1
6
data
pro
cess
ing
(e.g
. int
egra
tion
of w
rong
pea
k), m
ajor
dev
iatio
ns fr
om th
e an
alyt
ical
pro
cedu
re,
inap
prop
riate
sto
rage
or
trans
port
cond
ition
s (in
cas
e of
sus
cept
ible
com
poun
ds),
and
the
use
of
inap
prop
riate
pro
cedu
res
that
dem
onst
rabl
y le
ad t
o si
gnifi
cant
ly b
iase
d re
sults
(e.
g. d
ue t
o de
grad
atio
n or
inc
ompl
ete
extra
ctio
n).
Whe
re t
he O
rgan
iser
s (e
.g.
afte
r th
e pu
blic
atio
n of
the
pr
elim
inar
y re
port)
rec
eive
inf
orm
atio
n of
suc
h gr
oss
erro
rs,
havi
ng a
sig
nific
ant
impa
ct o
n a
gene
rate
d re
sult,
the
affe
cted
resu
lts w
ill be
exa
min
ed o
n a
case
-by-
case
bas
is to
dec
ide
whe
ther
, or
not
, the
y sh
ould
be
excl
uded
from
the
popu
latio
n us
ed fo
r rob
ust s
tatis
tics.
Res
ults
may
als
o be
om
itted
e.g
. if a
n in
appr
opria
te m
etho
d ha
s be
en u
sed
even
if th
ey a
re n
ot o
utlie
rs.
All d
ecis
ions
to
omit/
excl
ude
resu
lts w
ill be
dis
cuss
ed w
ith t
he E
UPT
-SC
and
the
rea
soni
ng f
or t
he o
mis
sion
of
each
res
ult
clea
rly s
tate
d in
the
fin
al E
UPT
-Rep
ort.
How
ever
, z
scor
es w
ill be
cal
cula
ted
for
all
resu
lts ir
resp
ectiv
e of
the
fact
that
they
wer
e om
itted
from
the
calc
ulat
ion
of th
e as
sign
ed v
alue
.
Om
itted
res
ults
mig
ht b
e in
tere
stin
g as
the
y m
ight
giv
e in
dica
tions
abo
ut p
ossi
ble
sour
ce(s
) of
er
rors
. The
Org
anis
ers
will
thus
ask
the
rele
vant
lab(
s) to
pro
vide
feed
back
on
poss
ible
sou
rces
of
erro
rs (s
ee a
lso
“follo
w-u
p ac
tiviti
es”).
Unc
erta
inty
of t
he a
ssig
ned
valu
e
The
unce
rtain
ty o
f the
ass
igne
d va
lues
u(x
pt) i
s ca
lcul
ated
acc
ordi
ng to
ISO
135
28:2
015
as:
𝑢𝑢 (𝑥𝑥
𝑝𝑝𝑝𝑝)=
1,25×
𝑠𝑠∗ √𝑝𝑝
whe
re s*
is th
e ro
bust
sta
ndar
d de
viat
ion
and 𝑝𝑝
is th
e nu
mbe
r of r
esul
ts.
In c
erta
in c
ases
, and
con
side
ring
all r
elev
ant f
acto
rs (e
.g. t
he re
sult
dist
ribut
ion,
mul
timod
ality
), th
e nu
mbe
r of
sub
mitt
ed r
esul
ts,
info
rmat
ion
rega
rdin
g an
alyt
e ho
mog
enei
ty/s
tabi
lity,
inf
orm
atio
n re
gard
ing
the
use
of m
etho
dolo
gies
that
mig
ht p
rodu
ce a
bia
s th
at w
ere
used
by
the
parti
cipa
nts)
, th
e EU
PT-P
anel
may
con
side
r th
e as
sign
ed v
alue
of
a sp
ecifi
c an
alyt
e to
be
too
unce
rtain
and
de
cide
tha
t th
e re
sults
sho
uld
not
be e
valu
ated
, or
onl
y ev
alua
ted
for
info
rmat
ive
purp
oses
. The
pr
ovis
ions
of I
SO 1
3528
:201
5 co
ncer
ning
the
unce
rtain
ty o
f the
ass
igne
d va
lue
will
be ta
ken
into
ac
coun
t.
St
anda
rd d
evia
tion
of th
e as
sign
ed v
alue
(tar
get s
tand
ard
devi
atio
n)
The
targ
et s
tand
ard
devi
atio
n of
the
ass
igne
d va
lue
(FFP
- σpt)
will
be c
alcu
late
d us
ing
a Fi
t-For
-Pu
rpos
e ap
proa
ch w
ith a
fixe
d R
elat
ive
Stan
dard
Dev
iatio
n (F
FP-R
SD) o
f 25%
as
follo
ws:
EUPT-SRM13 | 2018 (Soybean Flour)
A-44
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 11
of 1
6
FFP-σ p
t = 0.
25 ×
x pt
Th
e pe
rcen
tage
FFP
-RSD
is s
et a
t 25%
bas
ed o
n ex
perie
nce
from
res
ults
of
prev
ious
EU
PTs10
. Th
e EU
PT-P
anel
res
erve
s th
e rig
ht t
o al
so e
mpl
oy o
ther
app
roac
hes
on a
cas
e-by
-cas
e ba
sis
cons
ider
ing
anal
ytic
al d
iffic
ultie
s an
d ex
perie
nce
gain
ed fr
om p
revi
ous
prof
icie
ncy
test
s.
For i
nfor
mat
ive
purp
oses
the
robu
st re
lativ
e st
anda
rd d
evia
tion
(CV*
) is
calc
ulat
ed a
ccor
ding
to IS
O
1352
8:20
15;
Cha
pter
7.7
(C
onse
nsus
val
ue f
rom
par
ticip
ant
resu
lts)
follo
win
g Al
gorit
hm A
in
Anne
x C
.
z
scor
es
This
par
amet
er is
cal
cula
ted
usin
g th
e fo
llow
ing
form
ula:
𝑧𝑧 𝑖𝑖=(𝑥𝑥
𝑖𝑖−𝑥𝑥 𝑝𝑝
𝑝𝑝)𝐹𝐹𝐹𝐹
𝐹𝐹-𝜎𝜎 𝑝𝑝
𝑝𝑝
whe
re x
i is
the
valu
e re
porte
d by
the
lab
orat
ory,
xpt
is
the
assi
gned
val
ue,
and
FFP-σ p
t is
the
st
anda
rd d
evia
tion
usin
g FF
P ap
proa
ch.
Z sc
ores
will
be r
ound
ed t
o on
e de
cim
al p
lace
. Fo
r th
e ca
lcul
atio
n of
com
bine
d z
scor
es (s
ee b
elow
) the
orig
inal
z s
core
s w
ill be
use
d an
d ro
unde
d to
one
de
cim
al p
lace
afte
r cal
cula
tion.
Any
z sc
ores
> 5
will
be t
ypic
ally
rep
orte
d as
‘> 5
’ and
a v
alue
of
‘5’ w
ill be
use
d to
cal
cula
te
com
bine
d z
scor
es (s
ee b
elow
).
Z sc
ores
will
be in
terp
rete
d in
the
follo
win
g w
ay, a
s is
set
in th
e IS
O 1
7043
:201
011:
|z
| 2
.0
Ac
cept
able
2.
0
|z| <
3.0
Que
stio
nabl
e
|z
| ≥ 3
.0
U
nacc
epta
ble
For r
esul
ts c
onsi
dere
d as
fals
e ne
gativ
es, z
sco
res
will
be c
alcu
late
d us
ing
the
MR
RL
or R
L (th
e la
bora
tory
’s R
epor
ting
Lim
it) if
the
RL
< M
RR
L. T
he E
UPT
-Pan
el w
ill de
cide
whe
ther
, or n
ot, t
hese
va
lues
sho
uld
appe
ar in
the
z sc
ore
hist
ogra
ms.
10 C
ompa
rativ
e S
tudy
of t
he M
ain
Top-
dow
n A
ppro
ache
s fo
r th
e E
stim
atio
n of
Mea
sure
men
t Unc
erta
inty
in M
ultir
esid
ue
Ana
lysi
s of
Pes
ticid
es in
Fru
its a
nd V
eget
able
s. J
. Agr
ic. F
ood
Che
m.,
2011
, 59(
14),
7609
-761
9.
11 IS
O/IE
C 1
7043
:201
0. C
onfo
rmity
ass
essm
ent –
Gen
eral
requ
irem
ents
for p
rofic
ienc
y te
stin
g
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 12
of 1
6
C
ateg
ory
A a
nd B
cla
ssifi
catio
n
The
EUPT
-Pan
el w
ill de
cide
if a
nd h
ow t
o cl
assi
fy t
he la
bora
torie
s in
to tw
o ca
tego
ries
- A
or B
. C
urre
ntly
, la
bora
torie
s th
at a
re a
ble
to a
naly
se a
t le
ast
90%
of
the
com
puls
ory
pest
icid
es in
the
ta
rget
pes
ticid
es li
st,
have
cor
rect
ly d
etec
ted
and
quan
tifie
d a
suffi
cien
tly h
igh
perc
enta
ge o
f th
e pe
stic
ides
pre
sent
in
the
Test
Ite
m (
at l
east
90
%)
and
repo
rted
no f
alse
pos
itive
s w
ill ha
ve
dem
onst
rate
d ‘s
uffic
ient
sco
pe’
and
can
ther
efor
e be
cla
ssifi
ed i
nto
Cat
egor
y A.
For
the
90%
cr
iterio
n th
e nu
mbe
r of p
estic
ides
nee
ded
to b
e co
rrec
tly a
naly
sed
to h
ave
suffi
cien
t sco
pe w
ill be
ca
lcul
ated
by
mul
tiply
ing
the
num
ber
of c
ompu
lsor
y pe
stic
ides
from
the
Targ
et P
estic
ides
Lis
t by
0.9
and
roun
ding
to
the
near
est
full
num
ber
with
0.5
dec
imal
s be
ing
roun
ded
dow
nwar
ds (
see
som
e ex
ampl
es in
Tab
le 1
).
Tabl
e 1.
No.
of p
estic
ides
from
the
Targ
et P
estic
ides
Lis
t nee
ded
to b
e ta
rget
ed o
r pes
ticid
es p
rese
nt
in th
e Te
st It
em th
at n
eed
to b
e co
rrec
tly d
etec
ted
and
quan
tifie
d to
hav
e su
ffici
ent s
cope
.
No.
of c
ompu
lsor
y pe
stic
ides
pre
sent
in th
e Te
st It
em /
Targ
et
Pest
icid
es L
ist (
N)
90 %
N
o. o
f pes
ticid
es n
eede
d to
be
corr
ectly
det
ecte
d an
d qu
antif
ied
/ tar
gete
d to
hav
e su
ffici
ent
scop
e (n
) n
3 2.
7 3
N
4 3.
6 4
5 4.
5 4
N -
1
6 5.
4 5
7 6.
3 6
8 7.
2 7
9 8.
1 8
10
9.0
9 11
9.
9 10
12
10
.8
11
13
11.7
12
14
12
.6
13
15
13.5
13
N -
2
16
14.4
14
17
15
.3
15
18
16.2
16
19
17
.1
17
20
18
18
21
18.9
19
22
19
.8
20
23
20.7
21
24
21
.6
22
25
22.5
22
N
- 3
26
23.4
23
Appendix 8. General EUPT Protocol (8th Ed.)
A-45
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
A8
Gen
erA
l Pro
toco
(8th
ed
.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 13
of 1
6
O
vera
ll pe
rfor
man
ce o
f lab
orat
orie
s - c
ombi
ned
z sc
ores
For
eval
uatio
n of
the
ove
rall
perfo
rman
ce o
f la
bora
torie
s w
ithin
Cat
egor
y A
, th
e Av
erag
e of
the
Sq
uare
d z
scor
e (A
Z2 )12
,13 (
see
belo
w) w
ill be
use
d. T
he A
Z2 is
calc
ulat
ed a
s fo
llow
s:
nzAZ
n ii
1
2
2
Whe
re n
is th
e nu
mbe
r of z
sco
res
to b
e co
nsid
ered
in th
e ca
lcul
atio
n. In
the
calc
ulat
ion
of th
e AZ
2 , z
scor
es h
ighe
r th
an 5
will
be s
et a
s 5.
Bas
ed o
n th
e AZ
2 ac
hiev
ed, t
he la
bora
torie
s are
cla
ssifi
ed
as fo
llow
s:
AZ
2 2
.0
G
ood
2.
0
AZ2 <
3.0
Satis
fact
ory
AZ
2 ≥ 3
.0
U
nsat
isfa
ctor
y
Com
bine
d z
scor
es a
re c
onsi
dere
d to
be
of le
sser
impo
rtanc
e th
an t
he in
divi
dual
z s
core
s. T
he
EUPT
-Pan
el r
etai
ns t
he r
ight
not
to
calc
ulat
e AZ
2 if
it is
con
side
red
as n
ot b
eing
use
ful o
r if
the
num
ber o
f res
ults
repo
rted
by a
ny p
artic
ipan
t is
cons
ider
ed to
be
too
low
.
In th
e ca
se o
f EU
PT-S
RM
s, w
here
onl
y a
few
resu
lts p
er la
b m
ay b
e av
aila
ble,
the
Aver
age
of th
e Ab
solu
te z
sco
res
(AAZ
) m
ay b
e ca
lcul
ated
for
info
rmat
ive
purp
oses
, bu
t on
ly f
or la
bs t
hat h
ave
repo
rted
enou
gh r
esul
ts t
o ob
tain
5 o
r m
ore
z sc
ores
. Fo
r th
e ca
lcul
atio
n of
the
AAZ
, z
scor
es
high
er th
an 5
will
also
be
set a
s 5.
Labo
rato
ries
with
in C
ateg
ory
B w
ill be
rank
ed a
ccor
ding
to th
e to
tal n
umbe
r of p
estic
ides
that
they
co
rrec
tly re
porte
d to
be
pres
ent i
n th
e Te
st It
em. T
he n
umbe
r of a
ccep
tabl
e z
scor
es a
chie
ved
will
be p
rese
nted
, too
. The
EU
RL-
Pane
l ret
ains
the
right
to c
alcu
late
com
bine
d z
scor
es (
see
abov
e)
also
for
labs
with
in C
ateg
ory
B, e
.g. f
or in
form
ativ
e pu
rpos
es, p
rovi
ded
that
a m
inim
um n
umbe
r of
resu
lts (z
sco
res)
hav
e be
en re
porte
d.
12 F
orm
erly
nam
ed “S
um o
f squ
ared
z s
core
s (S
Z2 )”
13 L
abor
ator
y as
sess
men
t by
com
bine
d z
scor
e va
lues
in p
rofic
ienc
y te
sts:
exp
erie
nce
gain
ed t
hrou
gh t
he E
UP
T fo
r pe
stic
ide
resi
dues
in fr
uits
and
veg
etab
les.
Ana
l. B
ioan
al. C
hem
., 20
10, 3
97, 3
061–
3070
.
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 14
of 1
6
Publ
icat
ion
of re
sults
The
EUR
Ls w
ill pu
blis
h a
prel
imin
ary
repo
rt, c
onta
inin
g te
ntat
ive
assi
gned
val
ues
and
z sc
ore
valu
es f
or a
ll pe
stic
ides
pre
sent
in
the
Test
Ite
m,
with
in 2
mon
ths
of t
he d
eadl
ine
for
resu
lt su
bmis
sion
.
The
Fina
l EU
PT R
epor
t will
be p
ublis
hed
afte
r th
e EU
PT-P
anel
has
dis
cuss
ed th
e re
sults
. Tak
ing
into
acc
ount
tha
t th
e EU
PT-P
anel
mee
ts n
orm
ally
onl
y on
ce a
yea
r (ty
pica
lly in
late
sum
mer
or
autu
mn)
to d
iscu
ss th
e re
sults
of a
ll EU
PTs
orga
nise
d by
the
EUR
Ls e
arlie
r in
the
year
, the
fina
l re
port
may
be
publ
ishe
d up
to
10 m
onth
s af
ter
the
dead
line
for
resu
lts s
ubm
issi
on.
Res
ults
su
bmitt
ed b
y no
n-EU
/EFT
A la
bora
torie
s m
ight
not
alw
ays
be u
sed
in t
he t
able
s or
fig
ures
in t
he
final
repo
rt.
Cer
tific
ates
of p
artic
ipat
ion
Toge
ther
with
the
Fina
l EU
PT-R
epor
t, th
e EU
RL
Org
anis
er w
ill de
liver
a C
ertif
icat
e of
Par
ticip
atio
n to
eac
h pa
rtici
patin
g la
bora
tory
sho
win
g th
e z
scor
es a
chie
ved
for
each
indi
vidu
al p
estic
ide,
the
co
mbi
ned
z sc
ores
cal
cula
ted
(if a
ny),
and
the
clas
sific
atio
n in
to C
ateg
ory
A or
B.
Feed
back
At a
ny ti
me
befo
re, d
urin
g or
afte
r the
PT
parti
cipa
nts
have
the
poss
ibilit
y to
con
tact
the
Org
anis
ers
and
mak
e su
gges
tions
or
in
dica
te
erro
rs.
Afte
r th
e di
strib
utio
n of
th
e Fi
nal
EUPT
-Rep
ort,
parti
cipa
ting
labo
rato
ries
will
be g
iven
the
oppo
rtuni
ty to
giv
e th
eir f
eedb
ack
to th
e O
rgan
iser
s an
d m
ake
sugg
estio
ns fo
r fut
ure
impr
ovem
ents
.
Cor
rect
ion
of e
rror
s
Shou
ld e
rror
s be
dis
cove
red
in a
ny o
f the
doc
umen
ts is
sued
prio
r to
the
EUPT
(C
alen
dar,
Targ
et
Pest
icid
es L
ist,
Spec
ific
Prot
ocol
, Gen
eral
Pro
toco
l) th
e co
rrect
ed d
ocum
ents
will
be u
ploa
ded
onto
th
e w
ebsi
te a
nd in
the
case
of s
ubst
antia
l erro
rs th
e pa
rtici
pant
s w
ill be
info
rmed
. Bef
ore
star
ting
the
exer
cise
par
ticip
ants
sho
uld
mak
e su
re t
o do
wnl
oad
the
late
st v
ersi
on o
f th
ese
docu
men
ts.
If su
bsta
ntia
l erro
rs a
re d
isco
vere
d in
the
Prel
imin
ary
EUPT
-Rep
ort t
he O
rgan
iser
s w
ill di
strib
ute
a ne
w c
orre
cted
ver
sion
, whe
re it
will
be s
tate
d th
at th
e pr
evio
us v
ersi
on is
no
long
er v
alid
.
EUPT-SRM13 | 2018 (Soybean Flour)
A-46
Appendix 8 (cont.) General EUPT Protocol (8th Ed.)
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 15
of 1
6
Whe
re s
ubst
antia
l er
rors
are
dis
cove
red
in t
he F
inal
EU
PT-R
epor
t th
e EU
PT-P
anel
will
deci
de
whe
ther
a c
orrig
endu
m w
ill be
issu
ed a
nd h
ow t
his
shou
ld lo
ok.
The
onlin
e ve
rsio
n of
the
fin
al
repo
rt w
ill be
repl
aced
by
the
new
one
and
all
affe
cted
labs
will
be c
onta
cted
.
Whe
re e
rror
s ar
e di
scov
ered
in
EUPT
-Cer
tific
ates
the
rel
evan
t la
bora
torie
s w
ill be
sen
t ne
w
corr
ecte
d on
es. W
here
nec
essa
ry th
e la
bora
torie
s w
ill be
ask
ed to
retu
rn th
e ol
d on
es.
Follo
w-u
p ac
tiviti
es
Labo
rato
ries
are
expe
cted
to u
nder
take
follo
w-u
p ac
tiviti
es to
trac
e ba
ck th
e so
urce
s of
erro
neou
s or
stro
ngly
dev
iatin
g re
sults
(ty
pica
lly t
hose
with
|z|
> 2
.0)
- in
clud
ing
all
fals
e po
sitiv
es.
Even
re
sults
with
in |z
| ≤
2.0
may
hav
e to
be
chec
ked
if th
ere
is in
dica
tions
of
a si
gnifi
cant
pos
itive
or
nega
tive
bias
.
Upo
n re
ques
t, th
e la
bora
tory
’s c
orre
spon
ding
NR
L an
d EU
RL
are
to b
e in
form
ed o
f the
out
com
e of
an
y in
vest
igat
ive
activ
ities
for
fal
se p
ositi
ves,
fal
se n
egat
ives
and
for
res
ults
with
|z|
≥ 3
.0.
Con
cern
ing
z sc
ores
bet
wee
n 2.
0 an
d 3.
0 th
e co
mm
unic
atio
n of
the
outc
ome
of fo
llow
-up
activ
ities
is
opt
iona
l but
hig
hly
enco
urag
ed w
here
the
sour
ce o
f dev
iatio
n co
uld
be id
entif
ied
and
coul
d be
of
inte
rest
to o
ther
labs
.
Acco
rdin
g to
inst
ruct
ions
from
DG
-SAN
TE, t
he “P
roto
col f
or m
anag
emen
t of u
nder
perfo
rman
ce in
com
para
tive
test
ing
and/
or la
ck o
f col
labo
ratio
n of
Nat
iona
l Ref
eren
ce L
abor
ator
ies
(NR
Ls) w
ith
EU R
efer
ence
Lab
orat
orie
s (E
UR
Ls) a
ctiv
ities
” is
to b
e fo
llow
ed.
NR
Ls w
ill be
con
side
red
as u
nder
perf
orm
ing
in re
latio
n to
sco
pe if
in a
t lea
st tw
o of
the
last
four
EUPT
s fa
lling
with
in th
eir r
espo
nsib
ility
area
if th
ey: a
) hav
en’t
parti
cipa
ted,
or b
) tar
gete
d le
ss th
an
90%
of t
he c
ompu
lsor
y pe
stic
ides
in th
e ta
rget
list
s (8
0% fo
r SR
M-c
ompo
unds
), or
c) d
etec
ted
less
than
90%
of
the
com
puls
ory
com
poun
ds p
rese
nt i
n th
e te
st i
tem
s (8
0% f
or S
RM
-com
poun
ds).
Addi
tiona
lly,
NR
Ls t
hat
obta
ined
AZ2
high
er t
han
3 in
tw
o co
nsec
utiv
e EU
PTs
of t
he l
ast
four
EUPT
s, w
ill be
con
side
red
as u
nder
perf
orm
ing
in a
ccur
acy.
A tw
o-st
ep p
roto
col e
stab
lishe
d by
DG
-SAN
TE w
ill be
app
lied
as s
oon
as u
nder
perfo
rman
ce o
f an
NR
L is
det
ecte
d14:
Phas
e 1:
Id
entif
ying
the
orig
in o
f the
bad
resu
lts (f
ailu
re in
EU
PTs)
.
14 A
rticl
e 10
1 of
Reg
ulat
ion
(EC
) 625
/201
7
8th
Edi
tion:
Rev
ised
23th
Jan
uary
, 201
8
Pag
e 16
of 1
6
Ac
tions
: On
the
spot
vis
its a
nd tr
aini
ng if
nec
essa
ry a
nd re
petit
ion
of th
e co
mpa
rativ
e te
st if
feas
ible
and
clo
se th
e as
sess
men
t of r
esul
ts b
y th
e E
UR
L.
Phas
e 2:
If
the
resu
lts s
till r
evea
l und
erpe
rform
ance
the
Com
mis
sion
sha
ll be
info
rmed
offi
cial
ly b
y
the
EUR
L in
clud
ing
a re
port
of th
e m
ain
findi
ngs
and
corre
ctiv
e ac
tions
.
Th
e C
omm
issi
on s
hall
info
rm th
e C
ompe
tent
Aut
horit
y an
d re
quire
that
app
ropr
iate
act
ions
are
take
n.
U
nder
perfo
rman
ce ru
les
for t
he O
fLs
will
be e
stab
lishe
d at
a la
ter s
tage
.
Dis
clai
mer
The
EUPT
-Pan
el r
etai
ns th
e rig
ht to
cha
nge
any
parts
of t
his
EUPT
– G
ener
al P
roto
col b
ased
on
new
sci
entif
ic o
r tec
hnic
al in
form
atio
n. A
ny c
hang
es w
ill be
com
mun
icat
ed in
due
cou
rse.
Appendix 9. Specific Protocol of EUPT-SRM13
A-47
A9
Spec
ific
pro
toco
l
Appendix 9 Specific Protocol of EUPT-SRM13
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 1
of 7
SP
ECIF
IC P
ROTO
COL
for t
he 1
3th E
U P
rofic
ienc
y Te
st
on P
estic
ides
requ
iring
Sin
gle
Resi
due
Met
hods
EU
PT –
SRM
13 (2
018)
(r
elea
sed
on 0
9.Ap
ril, 2
018)
Intr
oduc
tion
This
prot
ocol
is c
ompl
emen
tary
to th
e va
lid v
ersio
n of
the
"Gen
eral
Pro
toco
l for
EU
Pro
ficie
ncy
Test
s fo
r Pes
ticid
e Re
si-
dues
in F
ood
and
Feed
" co
verin
g al
l EU
PTs.
Th
e EU
PT-S
RM13
is o
rgan
ised
by t
he E
U R
efer
ence
Lab
orat
ory
for
pest
icid
es r
equi
ring
Sing
le R
esid
ue M
etho
ds (
EURL
– SR
M) w
hich
is a
ccre
dite
d ac
cord
ing
to IS
O 1
7043
as p
rovi
ders
of p
rofic
ienc
y te
sts.
Th
e EU
PT-S
RM13
dea
ls w
ith th
e an
alys
is of
SRM
-pes
ticid
es in
dry
soy
bean
s an
d is
to b
e pe
rfor
med
by
all N
atio
nal R
efer
-en
ce L
abor
ator
ies
for
Sing
le R
esid
ue M
etho
ds (N
RL-S
RMs)
as
wel
l as
by a
ll of
ficia
l EU
labo
rato
ries
(OfL
s) in
volv
ed in
offi
-ci
al p
estic
ide
resid
ue c
ontr
ols
as fa
r as
thei
r sc
ope
over
laps
with
that
of t
he E
UPT
-SRM
13. T
his
incl
udes
labo
rato
ries
in-
volv
ed in
impo
rt c
ontr
ol w
ithin
the
fram
e of
Reg
. 669
/200
9/EC
. A s
peci
al E
UPT
-SRM
13-W
ebsi
te c
onta
inin
g lin
ks t
o th
e m
ost i
mpo
rtan
t doc
umen
ts o
f rel
evan
ce w
as c
onst
ruct
ed.
A pr
elim
inar
y se
lect
ion
of th
e la
bora
torie
s co
nsid
ered
to b
e ob
liged
to p
artic
ipat
e in
the
pres
ent w
as d
one
base
d on
the
info
rmat
ion
in th
e of
ficia
l Lab
-Net
wor
k-da
taba
se h
oste
d in
the
EURL
Dat
aPoo
l and
con
sider
ing
the
com
mod
ity sc
ope
only
(n
ot th
e pe
stic
ide
scop
e). T
he s
tatu
s of
the
OfL
s co
ncer
ning
thei
r par
ticip
atio
n in
the
curr
ent P
T w
as s
how
n on
the
regi
s-tr
atio
n pa
ge. A
s fa
r as
the
EU
PT-S
RM13
is c
once
rned
, all
OfL
s an
alys
ing
pest
icid
es o
f fo
od a
nd f
eed
in t
he c
omm
odity
gr
oup
“hig
h oi
l con
tent
and
ver
y lo
w w
ater
con
tent
” w
ere
cons
ider
ed a
s ob
liged
to
part
icip
ate
in t
his
PT. O
fLs
liste
d as
“o
blig
ed t
o pa
rtic
ipat
e in
the
EU
PT-S
RM13
” bu
t no
t in
tend
ing
to p
artic
ipat
e ha
d to
sta
te t
heir
reas
ons
for
non-
part
icip
atio
n du
ring
the
onlin
e re
gist
ratio
n of
the
EU
PT-S
RM13
, whi
ch la
sted
from
26
Febr
uary
till
16
Mar
ch, 2
018.
The
fe
edba
ck re
ceiv
ed d
urin
g re
gist
ratio
n is
cons
ider
ed in
the
final
list
of o
blig
ed la
bora
torie
s.
Test
Item
and
Bla
nk M
ater
ial
This
EUPT
dea
ls w
ith th
e an
alys
is of
pes
ticid
e re
sidue
s in
Soyb
ean
Flou
r.
Part
icip
ants
will
rece
ive
two
bott
les c
onta
inin
g:
1) c
a. 2
00 g
Tes
t Ite
m w
ith a
sele
ctio
n of
incu
rred
and
spik
ed a
naly
tes f
rom
the
Targ
et P
estic
ides
Lis
t.
2) c
a. 2
00 g
Bla
nk M
ater
ial,
that
can
be
used
for r
ecov
ery
expe
rimen
ts a
s w
ell a
s fo
r th
e pr
epar
atio
n of
mat
rix-
mat
ched
cal
ibra
tion
stan
dard
s
Sp
ecifi
c Pr
otoc
ol |
EU
PT –
SRM
12 (2
017)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 2
of 7
U
sing
rand
omly
cho
sen
bott
les,
the
Org
anize
rs w
ill c
heck
the
Test
Item
for s
uffic
ient
hom
ogen
eity
and
for t
he s
tabi
lity
of
the
pest
icid
es c
onta
ined
ove
r the
per
iod
of th
e ex
erci
se. T
he B
lank
Mat
eria
l will
be
also
che
cked
to p
rove
that
non
e of
the
pest
icid
es o
n th
e Ta
rget
Pes
ticid
es L
ist is
con
tain
ed a
t rel
evan
t lev
els.
Targ
et A
naly
tes a
nd M
RRLs
The
Test
Item
will
con
tain
sev
eral
pes
ticid
es fr
om th
e EU
PT-S
RM13
Tar
get
Pest
icid
es L
ist.
Labo
rato
ries
shou
ld r
ead
this
list c
aref
ully
, as
it sh
ows
how
the
resid
ues
are
expe
cted
to b
e re
port
ed a
s w
ell a
s th
e M
inim
um R
equi
red
Repo
rtin
g Le
v-el
s (M
RRLs
). Th
e M
RRL
valu
es w
ill b
e us
ed to
hel
p id
entif
y fa
lse p
ositi
ve a
nd fa
lse n
egat
ive
resu
lts a
nd fo
r the
cal
cula
tion
of z
-sco
res
for
false
neg
ativ
es. M
ake
sure
to d
ownl
oad
the
late
st v
ersi
on o
f the
EU
PT-S
RM13
Tar
get P
estic
ides
Lis
t be
-fo
re st
artin
g w
ith a
naly
sis a
nd re
sult
repo
rtin
g.
Plea
se n
ote,
the
defin
ition
s of t
he fo
llow
ing
targ
et p
estic
ides
was
mod
ified
:
“Chl
orm
equa
t cat
ion”
and
“m
epiq
uat c
atio
n” w
ere
chan
ged
to “
chlo
rmeq
uat c
hlor
ide”
and
“m
epiq
uat c
hlor
ide”
re
spec
tivel
y, to
refle
ct th
e ne
w w
ordi
ng o
f the
MRL
-reg
ulat
ion
“P
hosp
hane
” w
as c
hang
ed to
“Ph
opha
ne (p
hosp
hine
, inc
l. ph
osph
ane
rele
ased
from
pho
sphi
de s
alts
)”, t
o re
flect
th
e ne
w w
ordi
ng o
f the
MRL
-reg
ulat
ion
It sh
ould
not
be
assu
med
that
onl
y pe
stic
ides
regi
ster
ed fo
r use
in S
oybe
ans a
re p
rese
nt in
the
Test
Item
. Sh
ipm
ent o
f Tes
t Ite
m
Test
item
and
Bla
nk M
ater
ial a
re p
lann
ed to
be
ship
ped
on 2
3 Ap
ril, 2
018.
Co
oled
Tes
t Ite
m a
nd B
lank
Mat
eria
l will
be
pack
ed in
ther
mo-
boxe
s to
geth
er w
ith c
ool g
el p
acks
and
shi
pped
from
Ger
-m
any
via
DHL
expr
ess
parc
el t
o th
e pa
rtic
ipan
ts. P
rior
to s
hipm
ent
a re
min
der
will
be
sent
to th
e pa
rtic
ipat
ing
labo
rato
-rie
s by
e-m
ail.
La
bora
torie
s mus
t mak
e th
eir o
wn
arra
ngem
ents
for t
he re
ceip
t of t
he p
acka
ge. T
hey
shou
ld in
form
the
Org
anise
rs o
f any
pu
blic
hol
iday
s in
the
ir co
untr
y/ci
ty d
urin
g th
e w
eek
of t
he s
hipm
ent,
and
mus
t m
ake
the
nece
ssar
y ar
rang
emen
ts t
o re
ceiv
e th
e sh
ipm
ent,
even
if th
e la
bora
tory
is c
lose
d.
Shou
ld a
ny c
ompl
icat
ions
dur
ing
ship
men
t, de
liver
y or
the
cus
tom
s be
exp
ecte
d, t
he p
artic
ipat
ing
labo
rato
ries
shou
ld
prov
ide
the
Org
anize
rs in
adv
ance
with
con
tact
info
rmat
ion
of p
ossib
le c
onta
ct p
erso
ns o
f th
e la
b (e
.g. m
obile
pho
ne
num
bers
) as
wel
l as
inst
ruct
ions
in lo
cal l
angu
age
expl
aini
ng t
he n
eed
to k
eep
the
pack
age
in f
reez
er d
urin
g de
lay
in
tran
sit a
nd d
eliv
ery.
Thi
s inf
orm
atio
n w
ill b
e at
tach
ed to
the
pack
age.
Af
ter
the
pack
ages
wer
e pi
cked
up
and
stor
ed in
the
DHL
del
iver
y sy
stem
, eac
h pa
rtic
ipan
t w
ill b
e in
form
ed b
y DH
L ab
out t
he tr
acki
ng n
umbe
r of h
is p
acka
ge. T
he p
artic
ipan
ts c
an fo
llow
the
deliv
ery
stat
e of
thei
r ow
n pa
ckag
es o
nlin
e.
Onc
e a
pack
age
has a
rriv
ed th
e re
cipi
ent c
ount
ry a
nd a
n un
expe
cted
del
ay is
not
ices
, the
par
ticip
ant h
imse
lf is
stro
ngly
en
cour
aged
to
cont
act
his
loca
l DHL
Exp
ress
or
the
cust
oms
in o
rder
to
acce
lera
te t
he c
lear
ance
and
del
iver
y pr
oce-
dure
s.
EUPT-SRM13 | 2018 (Soybean Flour)
A-48
Appendix 9 (cont.) Specific Protocol of EUPT-SRM13
Spec
ific
Prot
ocol
| E
UPT
– S
RM12
(201
7)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 3
of 7
In
stru
ctio
ns o
n ha
ndlin
g th
e Te
st It
em
Both
Tes
t Ite
m a
nd B
lank
mat
eria
l are
pro
vide
d as
mill
ed fl
our.
Onc
e ar
rived
, the
Tes
t Ite
m s
houl
d be
sto
red
deep
froz
en
(at -
18°C
or l
ower
) unt
il an
alys
is in
ord
er to
avo
id a
ny p
ossib
le d
eter
iora
tion/
spoi
lage
and
to m
inim
ize p
estic
ide
degr
ada-
tion.
Be
fore
ana
lytic
al p
ortio
ns a
re ta
ken
for a
naly
sis, t
he T
est I
tem
sho
uld
be m
ixed
thor
ough
ly in
its
entir
ety.
Dur
ing
mix
ing,
tr
y to
kee
p te
mpe
ratu
res l
ow to
avo
id lo
sses
of s
usce
ptib
le p
estic
ides
. Pa
rtic
ipat
ing
labo
rato
ries
shou
ld u
se th
eir r
outin
e st
anda
rd o
pera
ting
proc
edur
es fo
r ext
ract
ion,
cle
an-u
p an
d an
alyt
i-ca
l mea
sure
men
t as
wel
l as
thei
r ow
n re
fere
nce
stan
dard
s fo
r ide
ntifi
catio
n an
d qu
antif
icat
ion
purp
oses
. Lab
orat
orie
s m
ay a
lso e
mpl
oy m
etho
ds n
ot y
et im
plem
ente
d ro
utin
ely,
for
exa
mpl
e if
they
are
in t
he t
est-
phas
e of
impl
emen
ting
them
. In
this
case
the
limite
d ex
perie
nce
and
the
non-
incl
usio
n of
the
anal
ytes
in th
e ro
utin
e sc
ope
shou
ld b
e in
dica
ted
in
the
EUPT
-SRM
13 R
esul
t Sub
mis
sion
Web
site
. Th
e ho
mog
enei
ty te
sts
will
be
cond
ucte
d us
ing
5 g
for Q
uECh
ERS
and
QuP
Pe a
men
able
pes
ticid
es. A
s su
b-sa
mpl
ing
varia
-bi
lity
incr
ease
s with
dec
reas
ing
anal
ytic
al p
ortio
n siz
e, su
ffici
ent h
omog
enei
ty c
an b
e gu
aran
teed
onl
y fo
r sam
ple
port
ions
eq
ual t
o or
big
ger t
han
the
used
por
tion
size
in th
e ho
mog
enei
ty te
st.
Resu
lts su
bmis
sion
web
site
Sam
ple
rece
ipt a
ckno
wle
dgem
ent,
anal
ytic
al re
sults
and
met
hod
info
rmat
ion
are
to b
e su
bmitt
ed v
ia th
e fo
llow
ing
web
-sit
e: E
UPT
-SRM
13 re
sult
subm
issio
n w
ebsi
te.
Su
b-Pa
ge 0
(Sam
ple
rece
ipt a
ckno
wle
dgem
ent)
, acc
essib
le fr
om 2
5 Ap
ril, 2
018.
Sub-
Page
s 1-3
(ana
lytic
al re
sults
and
met
hod
info
rmat
ion)
acc
essib
le fr
om 3
0 Ap
ril, t
ill 2
2 M
ay, 2
018.
The
dead
line
for r
esul
t sub
miss
ion
is 2
2 M
ay, 2
018
at 1
6 h
(CES
T).
- Log
in C
rede
ntia
l and
Lab
-Cod
e
To a
cces
s th
e da
ta-s
ubm
issi
on f
orm
s pa
rtic
ipan
ts m
ust
use
thei
r un
ique
logi
n cr
eden
tials
(use
rnam
e an
d pa
ssw
ord)
. Th
e lo
gin
cred
entia
l tog
ethe
r with
the
EUPT
-SRM
13 la
b-co
des
will
be
prov
ided
to e
ach
of th
e pa
rtic
ipat
ing
labo
rato
ries
on th
e sh
ipm
ent d
ay.
- Sam
ple
Rece
ipt a
nd A
ccep
tanc
e (S
ub-P
age
0)
Onc
e th
e la
bora
tory
has
rec
eive
d th
e pa
ckag
e it
mus
t re
port
to
the
orga
nise
r vi
a th
e EU
PT-S
RM13
Res
ult
Subm
issi
on
Web
site
(sub
-pag
e 0)
the
date
of r
ecei
pt, t
he c
ondi
tion
of th
e Te
st It
em, a
nd it
s ac
cept
ance
. For
labo
rato
ries
in th
e EU
- an
d EF
TA c
ount
ries
and
EU c
andi
date
cou
ntrie
s, th
e de
adlin
e fo
r ac
cept
ance
is 2
7 Ap
ril, 2
018.
If a
labo
rato
ry d
oes
not
resp
ond
by th
is de
adlin
e, th
e O
rgan
isers
will
ass
ume
that
Tes
t Ite
m a
nd B
lank
Mat
eria
l hav
e be
en re
ceiv
ed a
nd a
ccep
ted.
An
y pa
rtici
pant
s th
at h
ave
not r
ecei
ved
the
Test
Item
s by
the
27 A
pril
at n
oon,
they
mus
t inf
orm
the
Org
anise
r vi
a e-
mai
l (E
URL-
SRM
@cv
uas.b
wl.d
e). T
he O
rgan
iser w
ill c
onsu
lt th
e sh
ippi
ng c
ompa
ny to
loca
lize
the
pack
age
and
decid
e on
furt
her
actio
ns in
cludi
ng n
ew sh
ipm
ent,
if ne
cess
ary.
Sp
ecifi
c Pr
otoc
ol |
EU
PT –
SRM
12 (2
017)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 4
of 7
- R
epor
ting
qual
itativ
e an
d qu
antit
ativ
e Re
sults
(Sub
-Pag
e 1
and
2)
To re
port
thei
r res
ults
, lab
orat
orie
s mus
t acc
ess t
he E
UPT
-SRM
13 R
esul
t Sub
mis
sion
Web
site
. Al
l res
ults
mus
t be
repo
rted
on
this
web
site
by 2
2 M
ay, 2
018
at 1
6 h
(CES
T). T
he w
ebsit
e w
ill n
ot b
e ac
cess
ible
afte
r thi
s de
adlin
e, a
nd a
ll re
sults
subm
itted
afte
rwar
ds w
ill n
ot b
e ac
cept
ed.
Befo
re e
nter
ing
the
resu
lts, p
leas
e st
udy
the
Targ
et P
estic
ide
List
car
eful
ly, i
n pa
rtic
ular
the
res
idue
def
initi
ons
that
ap
ply
to th
e EU
PT, w
hich
are
not
nec
essa
rily
give
n in
full
on th
e Re
sult
Subm
issio
n W
ebsi
te.
The
follo
win
g fie
lds w
ill b
e av
aila
ble
for r
epor
ting
the
quan
titat
ive
resu
lts:
-
“Con
cent
ratio
n in
mg/
kg”:
the
pest
icid
e co
ncen
trat
ions
that
wou
ld b
e re
port
ed in
rout
ine
wor
k. R
esul
ts s
houl
d no
t be
rep
orte
d w
here
a p
estic
ide
was
not
det
ecte
d, o
r w
as d
etec
ted
belo
w th
e RL
(Rep
ortin
g Li
mit)
of t
he la
-bo
rato
ry o
r the
MRR
L. R
esul
ts re
port
ed a
s “<
RL”
or “
< #,
# m
g/kg
” w
ill b
e co
nsid
ered
as „
Not
Det
ecte
d”.
The
resid
ue le
vels
of th
e pe
stic
ides
mus
t be
repo
rted
in m
g/kg
usin
g th
e fo
llow
ing
sign
ifica
nt fi
gure
s:
Le
vels
<0.0
10 m
g/kg
to b
e ex
pres
sed
to 2
sign
ifica
nt fi
gure
s, e
.g. 0
.005
8 m
g/kg
;
Leve
ls ≥
0.01
0 m
g/kg
to b
e ex
pres
sed
to 3
sign
ifica
nt fi
gure
s, e
.g. 0
.156
, 1.6
4, 1
0.3
mg/
kg
Reco
very
-cor
rect
ed r
esul
ts s
houl
d be
rep
orte
d on
ly w
here
thi
s re
flect
s th
e ro
utin
e la
b’s
proc
edur
e; o
ther
wis
e th
e no
n-re
cove
ry-c
orre
cted
res
ult
shou
ld b
e re
port
ed.
Whe
re a
res
ult
was
cor
rect
ed f
or r
ecov
ery
the
ap-
proa
ch(e
s) fo
llow
ed to
ach
ieve
this
corr
ectio
n (e
.g. s
tand
ard
addi
tions
to sa
mpl
e po
rtio
ns, p
roce
dura
l cal
ibra
tion,
re
cove
ry m
ust b
e re
port
ed in
the
resp
ectiv
e fie
lds
in S
ubpa
ge 3
fact
or, u
se o
f ILI
S).
-
“Con
c. in
bla
nk in
mg/
kg”:
con
cent
ratio
n va
lues
of a
ny p
estic
ides
from
the
Targ
et P
estic
ide
List
det
erm
ined
in
the
Blan
k M
ater
ial (
even
at l
evel
s bel
ow th
e M
RRL)
. -
“Exp
erie
nce
with
this
com
poun
d”: U
se th
e dr
opdo
wn-
men
u to
indi
cate
for h
ow m
any
year
s you
hav
e be
en a
na-
lysin
g fo
r eac
h co
mpo
und
usin
g th
e m
etho
d ap
plie
d in
this
EUPT
.
- Rep
ortin
g In
form
atio
n on
Ana
lytic
al M
etho
dolo
gy (S
ub-P
age
3)
On
sub-
page
3 o
f the
“EU
PT-S
RM13
Res
ult S
ubm
issi
on W
ebsi
te”
the
part
icip
atin
g la
bora
torie
s m
ust p
rovi
de C
OM
PLET
E in
form
atio
n on
the
ana
lytic
al m
etho
d(s)
app
lied
to a
ll pe
stic
ides
whi
ch w
ere
anal
ysed
, irr
espe
ctiv
e of
whe
ther
the
y w
ere
dete
cted
or n
ot.
The
part
icip
atin
g la
bora
torie
s ar
e ur
ged
to th
orou
ghly
fill-
in a
ll re
ques
ted
info
rmat
ion
and
cont
rol i
t car
eful
ly in
ord
er to
m
inim
ize
the
adm
inist
rativ
e bu
rden
of c
olle
ctin
g an
d co
rrec
ting
it a
post
erio
ri.
If no
suf
ficie
nt in
form
atio
n on
the
met
hodo
logy
use
d is
pro
vide
d, t
he O
rgan
iser
s re
serv
e th
e rig
ht n
ot t
o ac
cept
the
an
alyt
ical
resu
lts re
port
ed b
y th
e pa
rtic
ipan
t or t
o re
fuse
par
ticip
atio
n is
futu
re E
UPT
-SRM
s.
For
deta
iled
info
rmat
ion
on
the
colu
mns
on
su
b-pa
ge
3 pl
ease
re
fer
to
the
Guid
e on
Re
sult
Subm
issio
n (h
ttp:
//w
ww
.eur
l-pes
ticid
es.e
u/lib
rary
/doc
s/sr
m/E
UPT
-SRM
13_S
hort
_Gui
de_S
ubPa
ges.
pdf).
O
nce
your
re
sults
ar
e co
mpl
etel
y su
bmitt
ed, p
leas
e ex
port
them
via
the
func
tion
on th
e su
bmis
sion
Mai
n Pa
ge a
s a
csv-
form
at. T
his
file
can
be v
iew
ed v
ia E
xcel
, and
you
can
eas
ily c
heck
you
r ent
ries s
tore
d in
the
data
base
.
Appendix 9. Specific Protocol of EUPT-SRM13
A-49
Appendix 9 (cont.) Specific Protocol of EUPT-SRM13
A9
Spec
ific
pro
toco
l
Sp
ecifi
c Pr
otoc
ol |
EU
PT –
SRM
12 (2
017)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 5
of 7
Su
bcon
trac
ting
The
follo
win
g ta
sk w
as su
bcon
trac
ted
to th
e EU
RL-C
F, S
øbor
g, D
enm
ark:
a)
Gene
ratio
n of
the
logi
n cr
eden
tials
b)
Adm
inist
ratio
n of
EU
PT-S
RM13
resu
lt su
bmiss
ion
web
site
Follo
w-u
p ac
tions
Afte
r the
dist
ribut
ion
of th
e EU
PT-S
RM13
Pre
limin
ary
Repo
rt, l
abor
ator
ies
with
poo
r res
ults
(hig
h ab
solu
te z
-sco
res,
false
ne
gativ
es o
r fa
lse p
ositi
ves)
will
be
aske
d to
pro
vide
info
rmat
ion
conc
erni
ng th
e re
ason
s fo
r th
is an
d po
ssib
le c
orre
ctiv
e ac
tions
. Thi
s in
form
atio
n w
ill b
e fo
rwar
ded
to t
he c
orre
spon
ding
NRL
-SRM
s up
on r
eque
st. A
ll EU
PT-S
RM13
-par
ticip
ants
ar
e w
elco
me
to a
sk th
e EU
RL-S
RM fo
r tec
hnic
al a
ssist
ance
. Th
e O
rgan
iser
mig
ht a
sk la
bora
torie
s to
pro
vide
miss
ing
met
hodo
logy
info
rmat
ion
that
is im
port
ant
for
the
eval
uatio
n an
d in
terp
reta
tion
of th
e PT
. Ac
cord
ing
to in
stru
ctio
ns b
y DG
-SAN
TE,
the
“Pro
toco
l for
man
agem
ent
of u
nder
perf
orm
ance
in c
ompa
rativ
e te
stin
g an
d/or
lack
of c
olla
bora
tion
of N
atio
nal R
efer
ence
Lab
orat
orie
s (N
RLs)
with
Com
mun
ity r
efer
ence
labo
rato
ries
(CRL
s)
activ
ities
” w
ill b
e fo
llow
ed b
y N
RLs.
Do
cum
ents
All d
ocum
ents
rela
ted
to th
e EU
PT–S
RM13
can
be
foun
d in
the
EURL
-Doc
umen
t Rep
osito
ry (C
IRCA
-BC)
. Lin
ks to
the
doc-
umen
ts c
an a
lso b
e fo
und
in th
e EU
PT-S
RM13
Web
site
. Fo
r fur
ther
info
rmat
ion
plea
se c
onta
ct th
e or
gani
zers
EU
RL-S
RM@
cvua
s.bw
l.de
Plea
se c
heck
the
EUPT
-SRM
13 W
ebsi
te b
efor
e st
artin
g w
ith th
e an
alys
is to
mak
e su
re th
at y
ou h
ave
the
late
st v
ersi
on o
f al
l doc
umen
ts a
vaila
ble.
In c
ase
of m
ajor
cha
nges
the
part
icip
ants
will
be
info
rmed
via
e-m
ail.
Part
icip
atio
n fe
es a
nd p
aym
ent d
etai
ls
To c
over
the
cos
ts o
f pro
duct
ion,
han
dlin
g an
d sh
ipm
ent
of t
he P
T-M
ater
ials
the
follo
win
g fe
es w
ill b
e ch
arge
d fo
r on
e un
it of
the
PT-M
ater
ial t
o th
e pa
rtic
ipat
ing
labo
rato
ries:
- OfL
s (in
clud
ing
NRL
s) fr
om E
U c
ount
ries,
EU-c
andi
date
cou
ntrie
s and
EFT
A co
untr
ies:
200
€
- Lab
s bas
ed in
third
cou
ntrie
s: 3
50 €
An
invo
ice
issu
ed t
o th
e "i
nvoi
ce a
ddre
ss"
stat
ed in
the
reg
istr
atio
n fo
rm w
ill b
e se
nt t
o th
e in
voic
e e-
mai
l add
ress
st
ated
dur
ing
regi
stra
tion.
Sho
uld
the
paym
ent b
eing
take
n ca
re o
f by
anot
her d
epar
tmen
t/in
stitu
tion,
the
reci
pien
t of
the
invo
ice
is re
ques
ted
to fo
rwar
d th
e in
voic
e ac
cord
ingl
y. D
etai
ls o
f pay
men
t will
be
give
n in
the
invo
ices
. Pa
ymen
t is
expe
cted
to b
e m
ade
with
in 3
0 da
ys u
pon
the
date
of s
hipm
ent
unle
ss s
peci
al in
form
atio
n w
as p
rovi
ded
by
the
part
icip
ant d
urin
g re
gist
ratio
n an
d/or
oth
erw
ise a
gree
d be
twee
n pa
rtic
ipan
t and
org
anise
r.
If fo
r any
reas
on p
aym
ent c
anno
t be
carr
ied
out b
efor
e th
is d
ate,
ple
ase
cont
act t
he O
rgan
izer t
o gi
ve e
xpla
natio
ns.
If no
pay
men
t or n
o pr
oof o
f pay
men
t is
rece
ived
and
no
expl
anat
ion
is g
iven
to th
e O
rgan
izers
, the
Org
anize
rs re
serv
e
Sp
ecifi
c Pr
otoc
ol |
EU
PT –
SRM
12 (2
017)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 6
of 7
th
e rig
ht to
exc
lude
the
resu
lts o
f the
con
cern
ed la
bora
torie
s fr
om th
e Fi
nal E
UPT
-Rep
ort o
r to
refu
se it
s pa
rtic
ipat
ion
in fu
ture
EU
PT-S
RMs.
Ba
nk D
etai
ls:
Bank
acc
ount
hol
der:
La
ndes
ober
kass
e Ba
den
Wue
rtte
mbe
rg
Bank
Nam
e :
Bade
n W
uert
tem
berg
isch
e Ba
nk
IBAN
: DE
02
6005
010
1 74
95 5
301
02
BIC/
SWIF
T:
SOLA
DEST
XXX
Paye
e id
entif
icat
ion
text
:
VAT
of C
VUA
Stut
tgar
t Se
e in
voic
e (im
port
ant a
nd M
UST
be
indi
cate
d!)
DE 8
11 6
00 5
10
To fa
cilit
ate
trac
king
of m
oney
tran
sfer
the
spec
ial p
ayee
iden
tific
atio
n te
xt (=
invo
ice
num
ber)
as
show
n in
the
invo
ice
MU
ST b
e in
dica
ted
in th
e re
mitt
ance
. M
ore
deta
ils fo
r ban
k-re
mitt
ance
are
giv
en in
the
invo
ices
. Ca
lend
ar o
f EU
PT-S
RM13
(p
leas
e se
e ht
tp:/
/ww
w.e
url-p
estic
ides
.eu/
libra
ry/d
ocs/
srm
/EU
PT-S
RM13
_Cal
enda
r.pdf
)
Targ
et P
estic
ides
List
of E
UPT
-SRM
13
(ple
ase
see
http
://w
ww
.eur
l-pes
ticid
es.e
u/lib
rary
/doc
s/sr
m/E
UPT
-SRM
13_T
arge
tPes
ticid
eList
)
EUPT-SRM13 | 2018 (Soybean Flour)
A-50
Appendix 9 (cont.) Specific Protocol of EUPT-SRM13
Spec
ific
Prot
ocol
| E
UPT
– S
RM12
(201
7)
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) CV
UA
Stut
tgar
t, Sc
hafla
ndst
r. 3/
2, D
E-70
736
Fellb
ach
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 7
of 7
Co
ntac
t inf
orm
atio
n
EU R
efer
ence
Lab
orat
ory
for S
ingl
e Re
sidu
e M
etho
ds (E
URL
-SRM
) Ch
emisc
hes u
nd V
eter
inär
unte
rsuc
huns
amt S
tutt
gart
Sc
hafla
ndst
r. 3/
2,
D-
7073
6 Fe
llbac
h
Germ
any
e-m
ail:
EURL
-SRM
@cv
uas.
bwl.d
e
Fax:
+49
342
6 11
24
Org
anis
ing
Gro
up a
t the
EU
RL-S
RM (S
tutt
gart
)
Mic
hela
ngel
o An
asta
ssia
des
phon
e: +
49 3
426
1124
Pa
t Sch
reite
r ph
one:
+49
342
6 10
29
Carm
en W
ausc
hkuh
n
phon
e: +
49 3
426
1159
Hu
bert
Zip
per
phon
e: +
49 3
426
1141
An
ja B
arth
ph
one:
+49
342
6 19
35
Giov
anna
Cer
chia
ph
one:
+49
342
6 11
14
Advi
sory
Gro
up
Amad
eo F
erná
ndez
-Alb
a EU
RL-F
V, U
nive
rsity
of A
lmer
ía (U
AL),
ES
Mig
uel G
amón
EU
RL-F
V, L
abor
ator
io A
groa
limen
tario
Gen
eral
itat V
alen
cian
a (L
AGV)
, ES
Met
te E
reci
us P
oulse
n EU
RL-C
F, N
atio
nal F
ood
Inst
itute
(DTU
), Sø
borg
, DK
Ralf
Lipp
old
EURL
-AO
, CVU
A Fr
eibu
rg, D
E Ph
ilipp
e Gr
os
Serv
ice
Com
mun
des
Lab
orat
oire
s (SC
L) /
Labo
rato
ire d
e M
ontp
ellie
r, FR
M
agnu
s Jez
usse
k Ba
varia
n He
alth
and
Foo
d Sa
fety
Aut
horit
y (L
GL),
Erla
ngen
, DE
Andr
é de
Kok
N
ethe
rland
s Foo
d an
d Co
nsum
er P
rodu
ct S
afet
y Au
thor
ity (N
VWA)
, Am
ster
dam
, NL
Sonj
a M
asse
lter
Aust
rian
Agen
cy fo
r Hea
lth a
nd F
ood
Safe
ty (A
GES)
, Inn
sbru
ck, A
T
Finb
arr O
’Reg
an
Pest
icide
Con
trol
Labo
rato
ry (P
CL),
Dept
. of A
gricu
lture
, Foo
d an
d th
e M
arin
e (D
AFM
) IR
Tuija
Pih
lströ
m
Swed
ish N
atio
nal F
ood
Agen
cy (S
NFA
-Liv
smed
elsv
erke
t), U
ppsa
la, S
E Ca
rmel
o Ro
dríg
uez
Uni
vers
ity o
f Alm
ería
(UAL
), Sp
ain
Qua
lity
Cont
rol G
roup
Anto
nio
Valv
erde
Uni
vers
ity o
f Alm
ería
(UAL
), ES
Pa
ula
Med
ina
Euro
pean
Foo
d Sa
fety
Aut
horit
y (E
FSA)
Appendix 10. Calendar and Target Pesticides List of EUPT-SRM13
A-51
Cale
nd
ar a
nd
T a
rgeT
Pes
TiCi
de l
isT
a10
EU R
efer
ence
Lab
orat
ory
Requ
iring
Sin
gle
Resi
due
Met
hods
(EU
RL-S
RM)
CVU
A St
uttg
art,
Scha
fland
str.
3/2,
DE-
7073
6 Fe
llbac
h, G
erm
any
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
eurl-
srm
@cv
uas.
bwl.d
e Pa
ge 1
of 1
TARG
ET P
ESTI
CIDE
LIST
fo
r the
EU
PT –
SRM
13 2
018,
Dry
Soy
bean
s up
date
on
14.0
3.20
18
Com
poun
ds P
oten
tially
Pre
sent
in T
est I
tem
Li
sted
in
MRR
L (m
g/kg
)
Com
puls
ory
Com
poun
ds (w
ill b
e co
nsid
ered
in C
ateg
ory
A/B
clas
sific
atio
n)
2,4-
D (fr
ee a
cid,
no
hydr
olys
is st
ep to
be
appl
ied)
M
ACP-
Reg.
0.
01
Brom
ide
ion
MAC
P-Re
g.
2
Chlo
rmeq
uat c
hlor
ide
MAC
P-Re
g.
0.01
Cyro
maz
ine
MAC
P-Re
g.
0.01
Ethe
phon
M
ACP-
Reg.
0.
02
Flua
zifo
p (fr
ee a
cid,
no
hydr
olys
is st
ep to
be
appl
ied)
M
ACP-
Reg.
0.
01
Gly
phos
ate
(par
ent o
nly)
M
ACP-
Reg.
0.
03
Halo
xyfo
p (fr
ee a
cid,
no
hydr
olys
is st
ep to
be
appl
ied)
M
ACP-
Reg.
0.
003
Mep
iqua
t chl
orid
e
MAC
P-Re
g.
0.01
Opt
iona
l Com
poun
ds (w
ill N
OT
be c
onsi
dere
d in
Cat
egor
y A/
B cl
assi
ficat
ion)
2,4-
DB (f
ree
acid
, no
hydr
olys
is st
ep to
be
appl
ied)
N
CP-W
D 0.
01
Bent
azon
e (fr
ee a
cid,
no
hydr
olys
is st
ep to
be
appl
ied)
–
0.02
Carb
ofur
an (s
um, e
xcep
t 3-O
H-CF
) M
ACP-
Reg.
0.
005
Chlo
rate
(ani
on)
NCP
-WD
0.01
Diqu
at (d
icat
ion)
N
CP-W
D 0.
02
Feno
xapr
op (f
ree
acid
, no
hydr
olys
is st
ep to
be
appl
ied)
–
0.01
Glu
fosi
nate
N
CP-W
D 0.
02
MPP
(met
abol
ite o
f glu
fosi
nate
) N
CP-W
D 0.
02
N-A
cety
l-Glu
fosi
nate
(met
abol
ite o
f glu
fosi
nate
) N
CP-W
D 0.
02
AMPA
(met
abol
ite o
f gly
phos
ate)
N
CP-W
D 0.
05
N-A
cety
l-Gly
phos
ate
(met
abol
ite o
f gly
phos
ate)
N
CP-W
D 0.
02
Para
quat
(dic
atio
n)
NCP
-WD
0.02
Perc
hlor
ate
(ani
on)
Cont
amin
ant
0.01
Phos
phan
e (p
hosp
hine
, inc
l. Ph
osph
ane
rele
ased
from
pho
sphi
de sa
lts)
NCP
-WD
0.00
5
Phos
phon
ic a
cid
NCP
-WD
0.05
Qui
zalo
fop
(free
aci
d, n
o hy
drol
ysis
step
to b
e ap
plie
d)
NCP
-WD
0.01
MAC
P-Re
g.: M
ACP
Regu
latio
n
NCP
-WD:
Wor
king
Doc
umen
t SAN
CO/1
2745
/201
3, 2
1 –2
2 N
ovem
ber 2
017
rev.
9(1
)
Not
e: T
his
docu
men
t may
be
subj
ect t
o m
inor
cha
nges
. In
case
of s
igni
fican
t cha
nges
the
orga
nize
rs w
ill s
end
e-m
ails
. In
any
case
ple
ase
chec
k ou
r web
site
perio
dica
lly to
mak
e su
re y
ou a
re u
sing
the
late
st a
vaila
ble
vers
ion.
For a
ny fu
rthe
r cla
rific
atio
n do
n’t h
esita
te to
con
tact
us u
nder
eur
l-srm
@cv
uas.
bwl.d
e
The
EUPT
-SRM
13 O
rgan
isin
g Te
am
Appendix 10 Calendar and Target Pesticides List of EUPT-SRM13
EU R
efer
ence
Lab
orat
ory
Requ
iring
Sin
gle
Resi
due
Met
hods
(EU
RL-S
RM)
CVU
A St
uttg
art,
Scha
fland
str.
3/2,
DE-
7073
6 Fe
llbac
h, G
erm
any
Web
site:
ww
w.e
url-p
estic
ides
.eu,
E-M
ail:
EURL
-SRM
@cv
uas.
bwl.d
e Pa
ge 1
of 1
CC AALL EE
NNDD
AARR
ff oorr tt
hh ee EE
UUPP TT
–– SS
RR MM11 33
So
ybea
ns
(rel
ease
d on
23
Janu
ary,
201
8)
Activ
ity
Who
? Da
tes
Ope
ning
of t
he E
UPT
-SRM
13 W
ebsi
te
with
link
s to
all r
elev
ant d
ocum
ents
(C
alen
dar,
Targ
et P
estic
ides
Lis
t, G
ener
al P
roto
col)
EURL
-SRM
23
Jan.
, 201
8
Regi
stra
tion
via
“EU
PT-R
egis
trat
ion
Web
site
”
(Not
e: O
blig
ed L
abor
ator
ies M
UST
ent
er th
is W
ebsit
e an
d ei
ther
regi
s-te
r or g
ive
expl
anat
ions
for n
on-p
artic
ipat
ion)
All L
abor
ator
ies i
nter
este
d in
par
ticip
atio
n an
d al
l ob
liged
labs
eve
n if
not
inte
rest
ed
26 F
eb. –
16
Mar
ch 2
018
Disp
atch
of E
UPT
-SRM
13-S
peci
fic P
roto
col
EURL
-SRM
Ap
ril 2
018
Prep
arat
ion
of E
UPT
-SRM
13-T
est I
tem
(p
relim
inar
y te
sts S
piki
ng /
Hom
ogen
izatio
n)
EURL
-SRM
M
arch
201
8 –
April
201
8
Hom
ogen
eity
Tes
ts
EURL
-SRM
M
arch
201
8 –
April
201
8
Stab
ility
Tes
ts
EURL
-SRM
Ap
ril –
June
201
8
Ship
men
t of E
UPT
-SRM
13 T
est I
tem
(+
rem
inde
r of u
pcom
ing
parc
el a
rriv
al)
EURL
-SRM
23
Apr
il, 2
018
Conf
irmat
ion
of sa
mpl
e Re
ceip
t and
acc
epta
nce
via
“EU
PT-S
RM13
Res
ult S
ubm
issi
on W
ebsi
te",
(S
ub-P
age
0)
Part
icip
atin
g La
bs
with
in 4
8 h
of re
ceip
t
Resu
lt Su
bmis
sion
(P
estic
ide
scop
e, R
esul
ts, M
etho
d In
fo) i
n
“EU
PT-S
RM13
Res
ult S
ubm
issi
on W
ebsi
te",
(S
ub-P
ages
1 –
3)
Part
icip
atin
g La
bs
30 A
pril
– 22
May
201
8
Prel
imin
ary
Repo
rt
(onl
y co
mpi
latio
n of
resu
lts a
nd p
relim
inar
y as
signe
d va
lues
) EU
RL-S
RM
June
201
8
EUPT
Eva
luat
ion
Mee
ting
EUPT
-SC,
DG-
SAN
TE
–
Surv
ey to
col
lect
reas
ons f
or u
nder
perf
orm
ance
an
d m
issin
g in
form
atio
n on
met
hods
EU
RL-S
RM /
Pa
rtic
ipat
ing
Labs
Ju
ne /
July
201
8
Fina
l Rep
ort
EURL
-SRM
De
c. 2
018
REM
ARK:
Ple
ase
note
that
the
date
s men
tione
d ab
ove
may
be
subj
ect t
o m
inor
cha
nges
. In
the
case
of c
hang
es th
e pa
r-tic
ipan
ts w
ill b
e in
form
ed v
ia e
-mai
l. Bu
t ple
ase,
still
che
ck p
erio
dica
lly o
ur w
ebsi
te fo
r pos
sible
upd
ates
in c
ase
the
emai
l doe
s not
get
thro
ugh
to y
ou.
Cont
act:
eurl-
srm
@cv
uas.
bwl.d
e
The
EUPT
-SRM
Tea
m
European Union Reference Laboratory for pesticides requiring Single Residue Methods (EURL – SRM) hosted at Chemisches Veterinäruntersuchungsamt Stuttgart (CVUA Stuttgart)
Schaflandstr. 3/2 70736 Fellbach Germany Tel: + 49 711 3426 1124Fax: + 49 711 58 81 76
http://www.srm.eurl-pesticides.eue-mail: [email protected]