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FAPAS® Report 04261
Aflatoxins B & G &/or total in Maize
May-June 2015
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FAPAS Report 04261
PARTICIPANT LABORATORY NUMBER
Participants can log in to FAPAS SecureWeb at any time to obtain their laboratory number for this proficiency test.
Laboratory numbers are displayed in SecureWeb next to the download link for this report.
REPORT INTEGRITY
FAPAS reports are distributed as Adobe® Certified Document Services (CDS) Adobe® PDF documents [1]. The use of Adobe® CDS allows the PDF files to certify that the author of the report is FAPAS and that the document has not been altered in anyway. A blue ribbon and information bar indicates this validation when the document is opened using Adobe® Reader v7 or later.
Hard copies of FAPAS reports can never incorporate this level of integrity and consequently when a FAPAS report is printed a watermark, stating that printed copies are not controlled, appears on every page.
End users of FAPAS reports should ensure that either the opened PDF file displays a valid FAPAS digital signature or that the content of any hard copy exactly matches the content of a PDF file that displays a valid FAPAS digital signature.
QUALITY SYSTEMS
FAPAS® is accredited by UKAS as complying with the requirements of ISO/IEC 17043:2010 [2].
Fera is an ISO 9001 certified organisation.
0009
Fera hereby excludes all liability for any claim, loss, demands or damages of any kind whatsoever (whether such claims, loss, demands or damages were foreseeable, known or otherwise) arising out of or in connection with the preparation of any technical or scientific report, including without limitation, indirect or consequential loss or damage; loss of actual or anticipated profits (including loss of profits on contracts); loss of revenue; loss of business; loss of opportunity; loss of anticipated savings; loss of goodwill; loss of reputation; loss or damage to or corruption of data; loss of use of money or otherwise, and whether or not advised of the possibility of such claim, loss demand or damages and whether arising in tort (including negligence), contract or otherwise. This statement does not affect your statutory rights.
Nothing in this disclaimer excludes or limits Fera liability for: (a) death or personal injury caused by Fera negligence (or that of its employees, agents or directors); or (b) the tort of deceit; [or (c) any breach of the obligations implied by Sale of Goods Act 1979 or Supply of Goods and Services Act 1982 (including those relating to the title, fitness for purpose and satisfactory quality of goods);] or (d) any liability which may not be limited or excluded by law (e) fraud or fraudulent misrepresentation.
The parties agree that any matters are governed by English law and irrevocably submit to the non-exclusive jurisdiction of the English courts.
© Copyright Fera Science Ltd (Fera) 2015. All rights reserved.
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FAPAS Report 04261
SUMMARY
1. The test material for FAPAS® proficiency test 04261 was dispatched in May 2015. Each
participant received a maize test material to be analysed for aflatoxins B1, B2, G1, G2
and/or total aflatoxin (AFB1, AFB2, AFG1, AFG2, total AF).
2. An assigned value (xa) was determined for each analyte and in conjunction with the
standard deviation for proficiency (σp) was used to calculate a z-score for each result.
3. Results for this proficiency test are summarised as follows:
analyte assigned value, xa µg/kg
number of scores, |z| ≤2
total number of scores
% |z| ≤2
AFB1 3.80 48 55 87
AFB2 1.89 45 50 90
AFG1 1.07 45 51 88
AFG2 1.00 45 50 90
AF (total) 7.67 57 61 93
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FAPAS Report 04261
CONTENTS
1. INTRODUCTION 5
1.1. Proficiency Testing 5
2. TEST MATERIAL 5
2.1. Preparation 5 2.2. Homogeneity 5 2.3. Dispatch 5
3. RESULTS 5
4. STATISTICAL EVALUATION OF RESULTS 6
4.1. Calculation of the Assigned Value, xa 6 4.2. Standard Deviation for Proficiency, σp 6 4.3. Individual z-Scores 6
5. INTERPRETATION OF SCORES 7
6. REFERENCES 7
TABLES
Table 1: Results and z-Scores 8
Table 2: Participants’ Comments 13
Table 3: Assigned Values and Standard Deviations for Proficiency 13
Table 4: Number and Percentage of z-Scores where |z| ≤2 13
FIGURES
Figure 1: z-Scores for AFB1 14
Figure 2: z-Scores for AFB2 15
Figure 3: z-Scores for AFG1 16
Figure 4: z-Scores for AFG2 17
Figure 5: z-Scores for AF (total) 18
APPENDICES
APPENDIX I: Analytical Methods Used by Participants 19
APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details 25
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1. INTRODUCTION
1.1. Proficiency Testing
Proficiency testing aims to provide an independent assessment of the competence of participating laboratories. Together with the use of validated methods, proficiency testing is an essential element of laboratory quality assurance.
Further details of the FAPAS® proficiency testing scheme are available in our protocols [3, 4].
2. TEST MATERIAL
2.1. Preparation
Preparation of the samples for this proficiency test was sub-contracted to a laboratory meeting the quality requirements of the scheme’s accreditation [2].
The test material was procured from a retail source and was found to contain no detectable AFB1, AFB2, AFG1 or AFG2. The test material was spiked with a solution of AFB1, AFB2, AFG1 and AFG2 and further mixed
Samples were stored at -20°C until dispatch.
2.2. Homogeneity
To test for homogeneity, randomly selected test materials were analysed in duplicate. Testing was sub-contracted to a laboratory meeting the quality requirements of the scheme’s accreditation [2].
These data showed sufficient homogeneity and were not included in the subsequent calculation of the assigned values.
2.3. Dispatch
The start date was 1 May 2015. Test materials were sent to 67 participants.
3. RESULTS
The instructions for reporting results were as follows:
• Determine the level of aflatoxins B1, B2, G1, G2 and/or total aflatoxin, present in the test material, in μg/kg, as received, corrected for recovery.
Results were submitted by 66 participants (99%) before the closing date for this test, 11 June 2015.
Each participant was given a laboratory number, assigned in order of receipt of results. The reported analyte concentrations are given in Table 1.
Participants’ comments are given in Table 2.
The analytical methods used by each participant are summarised in APPENDIX I.
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4. STATISTICAL EVALUATION OF RESULTS
The results submitted by participants were statistically analysed in order to provide an assigned value for each analyte. The assigned values were then used in combination with the standard deviation for proficiency, σp, to calculate a z-score for each result. The procedure follows that recommended in the IUPAC International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories [5].
Further details on the procedure followed can be found in the relevant protocols [3, 4].
4.1. Calculation of the Assigned Value, xa
The assigned value, xa, for each analyte was derived from the consensus of the results submitted by participants.
The following results were excluded from the calculation of the assigned value:
i) non numerical results i.e. qualitative or semi-quantitative results,
ii) results reported as approximately 10, 100 or 1000 × greater or smaller than the majority of submitted results (as these were considered to be reporting errors),
iii) results from participants not quoting a percentage recovery, EXCEPT for total AF, where participants submitted results that were the sum of their recovery corrected individual aflatoxins.
For AFB1, AFB2, AFG1, AFG2 and AF (total), this procedure was straightforward and the robust mean was chosen as the assigned value.
The assigned values for all analytes are shown in Table 3.
4.2. Standard Deviation for Proficiency, σp
The standard deviation for proficiency, σp, was set at a value that reflects best practice for the analyses in question.
For AFB1, AFB2, AFG1, AFG2 and AF (total), σp was derived from the appropriate form of the Horwitz equation [6]. The values for σp used to calculate z-scores from the reported results of this test are given in Table 3.
4.3. Individual z-Scores
Participants’ z-scores were calculated as:
p
axxzσ
)( −=
where x = the participant’s reported result,
xa = the assigned value and σp = the standard deviation for proficiency.
Participants’ z-scores for all analytes are given in Table 1 and are shown as histograms in Figures 1–5. It is possible for the z-scores published in this report to differ slightly from the z-score that can be calculated using the formula given above. These differences arise from the necessary rounding of the actual assigned values and standard deviations for proficiency prior to their publication in Table 3.
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The number and percentage of z-scores in the range -2 ≤ z ≤ 2 for all analytes are given in Table 4.
5. INTERPRETATION OF SCORES
In normal circumstances, over time, about 95% of z-scores will lie in the range -2 ≤ z ≤ 2. Occasional scores in the range 2 <|z| <3 are to be expected, at a rate of 1 in 20. Whether or not such scores are of importance can only be decided by considering them in the context of the other scores obtained by that laboratory.
Scores where |z| >3 are to be expected at a rate of about 1 in 300. Given this rarity, such z-scores very strongly indicate that the result is not fit-for-purpose and almost certainly requires investigation.
The consideration of a set or sequence of z-scores over time provides more useful information than a single z-score. Examples of suitable methods of comparison are provided in the IUPAC International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories [5].
6. REFERENCES
1 Adobe Certified Document Services, http://www.adobe.com/misc/pki/cds_cp.html, accessed 10/05/2015.
2 ISO/IEC 17043:2010, Conformity assessment – General requirements for proficiency testing.
3 FAPAS, 2014, Protocol for Proficiency Testing Schemes, Part 1 – Common Principles, Version 4, Issued May 2014.
4 FAPAS, 2014, Protocol for Proficiency Testing Schemes, Part 2 – FAPAS®, Version 3, Issued May 2014.
5 Thompson, M., Ellison, S.L.R. and Wood, R., 2006, The International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories, Pure Appl. Chem., 78, No. 1, 145–196.
6 Thompson, M., 2000, Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing, Analyst, 125, 385-386.
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Table 1: Results and z-Scores
laboratory number
analyte
AFB1 AFB2 AFG1 AFG2 AF (total) assigned value
3.80 µg/kg assigned value
1.89 µg/kg assigned value
1.07 µg/kg assigned value
1.00 µg/kg assigned value
7.67 µg/kg
result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score
µg/kg µg/kg µg/kg µg/kg µg/kg
001 3.02 93.53 -0.9 1.14 96.71 -1.8 3.55 97.79 10.5 1.12 97.58 0.6 8.83 96.40 0.7
002 3.6 83.9 -0.2 1.90 84.0 0.0 0.91 83.0 -0.7 1.11 65.7 0.5 7.5 -0.1
003 3.70 91 -0.1 1.63 96 -0.6 0.68 97 -1.7 0.71 82 -1.3 6.72 -0.6
004 3.8 113 0.0 2.1 102 0.5 1.0 107 -0.3 1.0 102 0.0 7.9 0.1
005 3.32 79.3 -0.6 1.67 86.9 -0.5 0.97 85.5 -0.4 0.97 89.6 -0.1 6.94 85.3 -0.4
006 3.1 95 -0.8 1.9 97 0.0 0.9 93 -0.7 0.9 93 -0.4 6.8 95 -0.5
007 3.83 96 0.0 1.85 96 -0.1 0.93 96 -0.6 0.91 96 -0.4 7.52 96 -0.1
008 3.23 96 -0.7 2.00 89 0.3 0.76 95 -1.3 0.81 81 -0.9 6.80 -0.5
009 4.04 83 0.3 2.04 89 0.4 1.24 71 0.7 1.17 76 0.8 8.49 0.5
010 3.90 87.3 0.1 1.98 91.5 0.2 1.03 88.4 -0.2 1.02 91.4 0.1 7.93 0.2
011 3.7 76 -0.1 1.8 69 -0.2 1.1 68 0.1 1.0 88 0.0 7.6 0.0
012 5.5 -1.3
013 3.18 79 -0.7 1.89 102 0.0 1.12 79 0.2 1.20 80 0.9 7.39 - -0.2
014 4.2 100 0.5 2 100 0.3 1.07 88.3 0.0 0.95 100 -0.2 8.2 100 0.3
015 7.3 -0.2
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1: Results and z-Scores
laboratory number
analyte
AFB1 AFB2 AFG1 AFG2 AF (total) assigned value
3.80 µg/kg assigned value
1.89 µg/kg assigned value
1.07 µg/kg assigned value
1.00 µg/kg assigned value
7.67 µg/kg
result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score
µg/kg µg/kg µg/kg µg/kg µg/kg
016 6.48 -0.7
017 3.6 109.7 -0.2 2.0 87.7 0.3 1.2 117.2 0.5 0.9 109.3 -0.4 7.7 106 0.0
018 12.35 73 10.2 16.00 75 4.9
019 3.82 99 0.0 1.81 97 -0.2 0.85 89 -0.9 0.90 96 -0.4 7.38 95 -0.2
020 4.74 91 1.1 2.63 93 1.8 1.25 96 0.8 1.27 96 1.2 9.89 94 1.3
021 3.25 83 -0.7 1.43 84 -1.1 0.72 95 -1.5 0.64 86 -1.6 6.04 -1.0
022 4.718 115.46 1.1 3.449 80.62 3.8 1.099 70.27 0.1 0.786 70.69 -1.0 10.052 84.26 1.4
023 4.07 100 0.3 1.91 100 0.0 1.17 100 0.4 1.14 100 0.6 8.29 100 0.4
024 3.5 110 -0.4 1.72 100 -0.4 1.26 100 0.8 1.03 100 0.1 7.51 100 -0.1
025 5 90.8 1.4 3 91.8 2.7 1 88.4 -0.3 1 82.8 0.0
026 5.83 2.4 8.18 0.3
027 3.03 100.0 -0.9
028 1.07 69.36 -3.3 1.15 83.88 -1.8 2.15 94.14 4.6 3.78 98.66 12.7 8.15 0.3
029 0.85 90.84% -3.5 0.93 84.51% -2.3 1.50 92.83% 1.8 3.50 76.11% 11.4 6.78 86.07% -0.5
030 5.6 80 - 120 -1.2
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1: Results and z-Scores
laboratory number
analyte
AFB1 AFB2 AFG1 AFG2 AF (total) assigned value
3.80 µg/kg assigned value
1.89 µg/kg assigned value
1.07 µg/kg assigned value
1.00 µg/kg assigned value
7.67 µg/kg
result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score
µg/kg µg/kg µg/kg µg/kg µg/kg
031 3.34 103.1 -0.6 1.55 100.3 -0.8 0.93 100.9 -0.6 0.92 97.9 -0.4 6.74 100.5 -0.6
032 3.38 94.82 -0.5 1.66 94.90 -0.6 0.86 97.29 -0.9 0.89 98.36 -0.5 6.79 96.34 -0.5
033 4.55 100 0.9 2.40 95 1.2 1.30 95 1.0 1.30 105 1.4 9.55 1.1
034 4.20 86 0.5 1.87 96 0.0 1.23 80 0.7 0.79 90 -0.9 8.09 0.2
035 3.34 90.83 -0.6 1.51 98.01 -0.9 0.83 100.46 -1.0 0.84 95.62 -0.7 6.52 96.23 -0.7
036 2.7 82.3% -2.9
037 4.0 89.7 0.2 1.9 94.4 0.0 1.1 90.1 0.1 1.0 87.1 0.0 8.0 0.2
038 3.23 97.20 -0.7 1.82 92.40 -0.2 1.03 93.30 -0.2 0.99 97.20 0.0 7.08 95.10 -0.4
039 3.696 99 -0.1 1.81 100 -0.2 0.836 100 -1.0 0.941 100 -0.3 7.283 100 -0.2
040 4.556 89.2 0.9 2.345 81.2 1.1 1.148 101.5 0.3 1.313 87.7 1.4
041 3.98 96 0.2 2.00 95 0.3 1.24 95 0.7 1.05 96 0.2 8.27 96 0.4
042 3.87 Standard Addition 0.1 1.84 Standard Addition -0.1 0.95 Standard Addition -0.5 0.96 Standard Addition -0.2 7.62 Standard Addition 0.0
043 3.62 -0.2 1.87 0.0 1.08 0.0 0.92 -0.4 7.49 -0.1
044 4 88.3 0.2 1.727 88.5 -0.4 0.8 110.5 -1.1 0.938 118.8 -0.3 7.465 -0.1
045 8 0.2
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1: Results and z-Scores
laboratory number
analyte
AFB1 AFB2 AFG1 AFG2 AF (total) assigned value
3.80 µg/kg assigned value
1.89 µg/kg assigned value
1.07 µg/kg assigned value
1.00 µg/kg assigned value
7.67 µg/kg
result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score
µg/kg µg/kg µg/kg µg/kg µg/kg
046 7.5 -0.1
047 4.02 0.3 2.06 0.4 0.81 -1.1 1.06 0.3 7.95 0.2
048 2.84 110.08 -1.1 1.35 107.30 -1.3 0.82 105.51 -1.1 0.68 102.61 -1.5 5.69 107.56 -1.2
049 2.65 -1.4 2.35 5.4
050 3.52 96.3 -0.3 2.13 82.6 0.6 1.06 102.9 0 1.18 51.2 0.8 7.89 92.1 0.1
051 3.50 120 -0.4 1.74 114 -0.4 1.01 102 -0.3 0.93 103 -0.3 7.18 110 -0.3
052 4.00 94.8 0.2 1.94 102.6 0.1 1.13 98.4 0.3 1.05 99.8 0.2 8.12 98.9 0.3
053 4.7 86 1.1 2.0 84 0.3 0.9 99 -0.7 1.0 80 0.0 8.6 0.5
054 3.79 101 0.0 2.00 96.5 0.3 1.16 96.7 0.4 1.04 96.6 0.2 7.99 / 0.2
055 3.7 84% -0.1 1.8 98% -0.2 1.1 76% 0.1 0.94 84% -0.3 7.5 -0.1
056 3.15 83 -0.8 2.73 96.3 2.0 1.906 101.9 3.5 1.212 86.5 1.0 8.999 91.925 0.8
057 3.82 95.1 0.0 2.16 98.0 0.7 1.17 94.2 0.4 0.83 96.0 -0.8 7.98 0.2
058 7.69 90 4.6 3.89 90 4.8 1.80 90 3.1 1.78 90 3.6 15.2 90 4.5
059 5.8 89 -1.1
060 6.83 42.1 3.6 30.2 47.5 68.1 3.08 23.0 8.5 28.2 25.8 123.8
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1: Results and z-Scores
laboratory number
analyte
AFB1 AFB2 AFG1 AFG2 AF (total) assigned value
3.80 µg/kg assigned value
1.89 µg/kg assigned value
1.07 µg/kg assigned value
1.00 µg/kg assigned value
7.67 µg/kg
result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score result recovery, %
z-score
µg/kg µg/kg µg/kg µg/kg µg/kg
061 3.796 88.3 0.0 1.507 88.5 -0.9 0.888 110.5 -0.8 0.929 118.8 -0.3 7.120 -0.3
062 5.9 -1.0
063 3.6 -0.2 6.7 -0.6
064 6.76 95.8 3.5 1.85 96.2 -0.1 1.35 92.1 1.2 0.51 89.3 -2.2 10.5 93.4 1.7
065 3.61 -2.4
066 7.3 -0.2
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 2: Participants’ Comments
participant number comments
024 Results for AFB2 , AFG1 , AFG2 are less than our reporting limits (5, 2.5 and 5 respectively)
035 Results for the test material 'as received' CORRECTED for recovery
047 standard addition
049 Not corrected for recovery
060 matrix-extracted calibration curve
066 Method AOAC 991.31 Fluorimetric, this result is not corrected by % recovery (our recovery is 90%).We do not understand how we fill the space for recovery therefore we decided to leave unfilled space.
comments are as submitted by participants
Table 3: Assigned Values and Standard Deviations for Proficiency
analyte data points, n
assigned value, xa µg/kg
uncertainty, u
standard deviation for proficiency, σp
AFB1 51 3.80 0.0917 Horwitz [6] 0.836
AFB2 48 1.89 0.0459 Horwitz [6] 0.416
AFG1 49 1.07 0.0332 Horwitz [6] 0.236
AFG2 48 1.00 0.0262 Horwitz [6] 0.22
AF (total) 50 7.67 0.149 Horwitz [6] 1.69
Table 4: Number and Percentage of z-Scores where |z| ≤2
analyte number of scores, |z| ≤2
total number of scores
% |z| ≤2
AFB1 48 55 87
AFB2 45 50 90
AFG1 45 51 88
AFG2 45 50 90
AF (total) 57 61 93
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Figure 1: z-Scores for AFB1
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Figure 2: z-Scores for AFB2
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Figure 3: z-Scores for AFG1
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Figure 4: z-Scores for AFG2
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Figure 5: z-Scores for AF (total)
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APPENDIX I: Analytical Methods Used by Participants
Methods are tabulated according to the information supplied by participants, but some responses may have been combined or edited for clarity.
Method Used Accredited laboratory number
yes 001 002 003 007 008 009 011 012 015 017 020 022 023 024 032 034 035 036 037 038 040 041 042 044 048 050 051 054 057 058 059 061 064
no 005 016 029 030 033 043 049 055 060 063 065 066
Method Based On laboratory number
International Standard 002 003 009 011 012 017 038 044 048 057 058 061 066
National Standard 001 007 015 022 032 035 041 042 051 054 060
Paper Published In An International Journal 005
Manufacturer/Kit Instructions/Technical Note 008 016 030 037 050 059 063 065
In house method 020 023 024 029 033 034 036 040 049 055 064
Sample Weight (g) laboratory number
≥2 - <5 024 029 030 033 063
≥5 - <10 035 036 042 044 049 050 051 055 060 061 064 065
≥10 - <25 007 009 011 012 015 016 020 023 034 041 054 057 058
≥25 - <50 003 017 032 038 040 048 059 066
≥50 001 002 005 008 022 037 043
Extraction Solvent Components laboratory number
acetone 007
acetonitrile 011 023 024 032 033 038 049 051 064
heptane 009
methanol 001 005 009 011 012 015 016 022 029 030 034 035 036 037 042 043 044 049 055 057 058 059 060 061 063 065 066
sodium chloride solution 009 023 042
water 002 003 007 008 009 011 015 016 017 020 024 032 034 036 037 038 040 042 043 048 049 050 054 055 060 063 064
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Extraction Procedure laboratory number
add NaCl 001 022 029 034 043 048 055 060 066
blend / homogenise with solvent 005 008 017 029 030 034 041 042 057 059 060
hot water extraction 065
maceration / homogenisation 020
shake with solvent 007 009 012 015 016 023 024 030 033 036 038 040 042 049 063 064
shaking 032 058
sonicate/ultrasonic bath 064
Ultra Turrax 002 011 034 037 043
ultrasonic extraction 054
vortex mix 035 042 050 060
Extraction Type laboratory number
single 001 002 005 007 008 009 011 016 017 020 023 024 029 030 032 034 036 037 041 042 043 048 049 050 054 055 057 059 060 063 065 066
multiple 003 012 015 022 033 035 038 040 044 051 058 061 064
Sample Work Up laboratory number
centrifuge 012 015 023 024 029 030 032 042 049 050 055 060 064
defatted with hexane 009
dilute 005 030 042 060 065
evaporate 029 033 060
filter 007 008 011 017 020 022 029 034 035 036 037 041 042 043 048 055 057 060 065 066
none 054
pH adjustment 016 038 043
Ultra Turrax 002
inmunoaffinity column 044
mix 065
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Sample Clean-up by Immunoaffinity Column (Brand)
laboratory number
R-Biopharm Rhone 002 008 009 020 037 038 041 042 044 050 057 058 061
VICAM 001 005 007 011 022 029 034 035 043 048 055 066
Micotox 033
AflaTest-P 060
IneratSep VAR-3 032
Sample Clean-up by SPE laboratory number
Romer Labs 033 040 041 051 054 064
Micotox 001 017 038
AflaTest-P 035
IneraSep VAR-3 032
Mycotoxin Determination laboratory number
ELISA 012 015 016 036 059 063 065
fluorometric 058 066
HPLC 001 002 003 005 007 008 009 011 017 020 023 029 032 034 035 037 038 040 041 042 043 044 048 050 054 055 057 060 061 064
ELISA EuroProxima 030
Immunoassay 049
LC-MS/MS 024 033 051
UPLC 022
HPLC Injection Volume (μl) laboratory number
≥5 - <10 017 032 033 044 061
≥10 - <25 001 008 022 035 041 054 055 064
≥25 - <50 009 020 023 024
≥50 - <100 005 007 011 029 034 043 048 051 057 058 060
≥100 - <150 002 003 037 038 040 050
≥150 042
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HPLC Column Packing laboratory number
C18 002 003 005 007 008 009 011 017 020 022 023 024 029 032 033 034 037 041 042 043 044 048 050 051 054 055 057 058 060 061 064
endcapped 001 034 040 043
Inertsil ODS - 3V 038
Waters High Strength Silica (HSS) C18 035
HPLC Column Temperature (°C) laboratory number
ambient 001 002 003 020 038 040 041 042 054 058 064
>ambient - <50 005 007 008 009 011 017 022 023 024 029 032 033 034 035 037 043 044 048 050 051 055 061
≥50 057 060
Mobile Phase Components laboratory number
acetate 023 024 033
acetic acid 064
acetone 023
acetonitrile 007 011 029 032 034 042 043 055 058
formic acid 023 060
HNO3 & KBr (for Kobra Cell) 007 042 043 050
methanol 005 007 009 011 022 024 029 032 034 035 037 038 041 042 043 050 051 055 058 060 064
water 001 002 003 005 007 008 009 011 017 020 023 024 029 032 034 037 038 040 041 043 044 048 054 055 057 058 060 061 064
Mobile Phase Flow Rate (ml/min) laboratory number
<0.25 033 035
≥0.25 - <0.75 007 011 017 022 023 024 044 050 060 061 064
≥0.75 - <1.25 001 002 003 005 008 009 020 029 032 034 037 041 043 048 055 057 058
≥1.25 - <1.75 038 042
≥1.75 - <2.25 040 054
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Post Column Mobile Phase Flow Rate (ml/min)
laboratory number
<0.25 033 041 055
≥0.25 - <0.75 007 017 023 038 058
≥0.75 001 003 043 048 054
HPLC Pre Column Derivatisation laboratory number
fluorescamine 032
none 020 023 033 041 043 044 054 061
KBr Derivetised 038
photochemical reactor 001
HPLC Post Column Derivatisation laboratory number
Kobra cell 002 003 007 008 020 038 040 042 043 048 050
pyridinium bromide perbromide (C5H6Br3N) 009 057 058
saturated iodine 041 055
TFA 032
none 001 023 033 044 061
photochemical 005
photochemical reactor 029
photochemische NSD 034
PHRED Photochemical Reactor for Enhanced Detection
017
Source of Standards laboratory number
Fluka 050
R-Biopharm Rhone 008 012 015 020 058 063 065
Romer Labs 016 023 033 040 054
Sigma/Aldrich 005 009 011 034 037 038 044 048 055 061 064
Supelco 002 003 029 032 035 057 059 060
VICAM 001 066
Micotox 017
biopure 007 043
Coring 007 042
Discovery Fine Chemicals 049
Fermentek 022
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Source of Standards (continued) laboratory number
JRC-IRMM 037
LGC standards 030
pribolab 041
HPLC Detector Type laboratory number
fluorescence 001 002 003 005 007 008 009 011 017 020 022 029 032 034 035 037 038 040 041 042 043 048 050 054 055 057 058
MS-MS 023 033 044 051 060 061 064
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APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details
1. FAPAS SECUREWEB
Access to the secure area of our website is only available to participants in our proficiency tests. Please contact us if you require a UserID and Password. FAPAS SecureWeb allows participants to:
• Obtain their laboratory numbers for the proficiency tests in which they have participated.
• View the results they submitted in past and current proficiency tests.
• Submit their results and methods for current tests.
• Review future tests they have ordered.
• Order proficiency tests, reference materials and quality control materials.
• Freely download copies of reports (PDF file), of proficiency tests in which they have participated.
• View charts of their z-scores obtained in previous FAPAS® proficiency tests.
2. PROTOCOL
The Protocols [3, 4] set out how FAPAS® is organised. Copies can be downloaded from our website.
3. CONTACT DETAILS
This report was prepared and authorised on behalf of FAPAS by Jennifer Leak (Round Coordinator). Participants with any comments or concerns about this proficiency test should contact:
FAPAS
Fera Science Ltd (Fera) Sand Hutton
York YO41 1LZ
UK
Tel: +44 (0)1904 462100 Fax: +44 (0)1904 500440
www.fapas.com
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