international quality assurance programme (iqap) … · 2016. 8. 31. · z-scores obtained by...

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary ReportBIOLOGICAL SPECIMEN

2015/2

This report contains the data received from laboratories participating in the current exercise. The results compiled in this report are not intended to be an overview of the quality of work and cannot be interpreted as such. These comments do not reflect the general state of the art within the profession.

Participant results are reported using a randomly assigned "WebCode". This code maintains participant's anonymity, provides linking of the various report sections, and will change with every report.

Samples Substances Concentrations Comments on substances

Sample 1 Buprenorphine 1150 ng/ml

Norbuprenorphine 23 0 ng/ml

Sample 2 Tenamfetamine (MDA) 920 ng/ml

Sample 3 Methadone 2300 ng/ml

Sample 4 Nordazepam 1150 ng/ml

Test Samples InformationSamples Comments on samples

Sample 1 To prepare BS-1, urine was spiked with an aqueous solution of buprenorphine hydrochloride (1150ng base/ml) and a methanol solution of norbuprenorphine (2300ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 2 To prepare BS-2, urine was spiked with an aqueous solution of tenamfetamine hydrochloride (920ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised

Sample 3 To prepare BS-3, urine was spiked with an aqueous solution of methadone hydrochloride (2300ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 4 To prepare BS-4, urine was spiked with a methanol solution of nordazepam (1150ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

2015/2-BS Copyright (c) 2016 UNODC

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

2

Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 NPS reported by ICE participants Page 5

Codes and Abbreviations Page 7

Sample 1 Analysis Page 8 Identified substances Page 8

Statement of findings Page 10 Identification methods Page 14

Summary Page 17 Z-Scores Page 18 Sample 2 Analysis Page 23 Identified substances Page 23

Statement of findings Page 25 Identification methods Page 29

Summary Page 32 Z-Scores Page 33


Statement of findings Page 38 Identification methods Page 42 Summary Page 45

Z-Scores Page 46


Statement of findings Page 51 Identification methods Page 56 Summary Page 59

Z-Scores Page 60

Introduction An important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. This report provides information on analytical results of laboratories participating in the Seized Materials (SM) group. In order to maintain confidentiality, the participating laboratories have been

assigned random “Web Codes”, which change every round. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact.

Comments from the International Panel of Forensic Experts Participation of Laboratories In the 2015/2 round of the ICE programme, results were submitted within both the Seized materials (SM)

and Biological Specimens (BS) test groups by 19 laboratories in 60 countries. Within the SM test group,

there were 15 participating laboratories from 5 countries and within the BS test group, results were

submitted by 86 laboratories from 42 countries. Qualitative Analysis The analytical technique most commonly used for screening of test samples in the BS test group was enzyme immunoassays (57% of participants), while GC-MS (84%) was the most commonly used technique for identification/confirmation of the components in the test samples. The results for the qualitative identification of the controlled substances in the BS test group are shown in the table 1.

Table 1. Qualitative performance of participants in the 2015/2 round of ICE.

Test sample BS-1

(Buprenorphine) BS-1

(Norbuprenorphine)

Correct identification 66% 40%

Test sample BS-2

(MDA) BS-3

(Methadone) BS-4

(Nordazepam)

Correct identification 74% 88% 87%

BS-1 contained a mixture of buprenorphine and norbuprenorphine which were identified by 6 %, and 40% of participants respectively. There were four false positive results and seven false negatives (where neither component was identified). Twenty laboratories did not carry out analysis for both buprenorphine and norbuprenorphine. BS-2 contained MDA, which was correctly identified by 74% of participants, while there were ten false positive results, eleven false negatives and eleven laboratories did not carry out analysis for this substance BS-3 contained methadone, which was correctly identified by 88% of participants. There were seven false positives, five false negatives and six laboratories did not carry out analysis for Methadone. Finally, BS-4 contained Nordazepam, which was correctly identified by 87% of laboratories. There were six false positives, five false negative results and six laboratories did not carry out analysis for this substance Laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. ICE participants are reminded that test samples can contain any of the substances in the ICE menu and as such if methods are available, all substances should be considered

3

Quantitative Analysis The four test samples in the BS group for the 2015/2 round of ICE contained a total of five components and

36 (42%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to

note that 92% of laboratories quantified at least two components and 41% performed quantification of all components present. GC-MS was used by 56% of participants for quantification, followed by LC/MS(/MS), which was used by 33% of participants. Z-scores obtained by participants in quantification are shown in table 2 (percentage + no. of labs indicated)

z-score

Test sample

BS-1 (Buprenorphine) BS-1 (Norbuprenorphine)

|z| < 2, satisfactory 84% (21) 82% (14)

2 ≤ |z| ≤ 3, questionable 8% (2) 19% (3)

|z| > 3, unsatisfactory 8% (2) -

z-score BS-2 (MDA) BS-3 (Methadone) BS-3 (Nordazepam)

|z| < 2, satisfactory 70% (19) 88% (30) 70% (21)

2 ≤ |z| ≤ 3, questionable 7% (2) 6% (2) 7% (2)

|z| > 3, unsatisfactory 25% (7) 6% (2 23% (7)

According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation. Participants with z-scores outside acceptable limits should review their quantification procedures. In the 2015/1 round of ICE, eleven laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Eight of

these laboratories participated and performed quantification in the 2015/2 round with 100% improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. One laboratory also

obtained a questionable z-score and two laboratories also obtained unsatisfactory z-scores in 2015/ . Eight laboratories obtained unsatisfactory z-scores in ICE 2015/1 with |z| ≥ 3. Of these laboratories, five participated in ICE 2015/2 and performed quantification, with 4 (80%) improving their performance in at least one substance. Three (60%) of these laboratories also obtained an unsatisfactory z-score in the 2015/2 round of the ICE programme and one laboratory obtained a questionable z-score Laboratories that need to perform quantitation routinely are encouraged to participate regularly in external proficiency testing or collaborative exercises such as the ICE programme. This will enable laboratories to assess the quality of their quantitative methods through the z-score values obtained. Laboratories reporting

false positive or false negative results should investigate the root causes and corrective actions taken promptly in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. UNODC would like to acknowledge the valuable contribution of the Chemical Metrology Laboratory of the Health Sciences Authority, Singapore, for the provision of specific software used for the quantitative statistical calculations in the ICE programme.

4

New Psychoactive Substances (NPS) reported by laboratories participating in the 2015/2 round of the ICE programme During the 2015/2 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 190 reports of 115 substances. The most commonly reported substances were synthetic cannabinoids (28%) followed by synthetic cathinones (24%) and phenethylamine group substances (20%) as shown in figure 1.

Figure 1. NPS reported by ICE laboratories during the 2015/2 round of ICE

In terms of the mechanism of action of the NPS reported by ICE participants, 43% were stimulants, while

28% were synthetic cannabinoid receptor agonists (SCRA’s) and 19% were hallucinogenic substances as

shown in figure 2

28%

24% 20%

16%

5% 3% 2% 2%

Synthetic cannabinoids

Synthetic cathinones

Phenethylamines

Others

Piperazines

Ketamine and phencyclidinetype substances

Aminoindanes

Tryptamines

5

Figure 2. Mode of action of NPS most commonly reported by ICE participants in the 2015/2 round of ICE

NPS most commonly reported by laboratories participating in ICE 2015/2 The substance most often reported by ICE participants was the hallucinogenic phenethylamine 25I-NBOMe followed by the stimulant cathinone alpha-PVP and the synthetic cannabinoid receptor agonist MDMB CHMICA. For further details on these substances and others reported to the UNODC Early Warning Advisory, ICE participants can log on to the UNODC ICE portal and select the icon for the Early Warning Advisory on New Psychoactive substances as shown below.

43%

28%

19%

5% 2% 3%

Stimulants

SCRAs

Hallucinogens

Sedatives/Hypnotics

Dissociatives

Opioids

6

Codes and Abbreviations

Tech Code Name

100 Agglutination Techniques

110 Enzyme Immunoassay Techniques

120 Fluorescence Polarization Immunoassay

130 Radioimmunoassay

140 Colorimetric reactions

141 Marquis reagent (sulphuric acid, formaldehyde)

142 Cobalt thiocyanate

150 Thin Layer Chromatography

160 High/Ultra High Performance Liquid Chromatography

161 High Performance Liquid Chromatography with diode array detection

170 Gas Chromatography NPD

171 Gas Chromatography FID

172 Gas Chromatography ECD

180 Gas Chromatography/Mass Spectrometry

190 Fourier Transform Infrared Spectrometry

200 Spectrophotometry (visible, UV)

210 Others (specify)

211 NMR

220 Microcrystal test

230 Liquid chromatography/mass spectrometry

231 Liquid chromatography/tandem mass spectrometry

(+) “positive”: Indicates that the analyte is identified; for presumptive tests (e.g. colour reactions), indicates that a positive reaction was obtained.

(-) “negative”: Indicates that the analyte is not identified.

(ANP): Analysis not performed.



7

Identified substances for Test Sample 1

Code Identified Substances0ALKWG Buprenorphine and Norbuprenorphine

0SXBBB Buprenorphine

22ZFEN Buprenorphine and Norbuprenorphine

3FY8Y9 buprenorphine and its metabolite nor-buprenorphine

5OLO5M Buprenorphine

5QGV32 Buprenorphine

7Q4ADS Buprenorphine ,Norbuprenorphine

7YA3XU BUPRENORPHINE, NORBUPRENORPHINE

88RVB3 N/A

8MQQYQ Buprenorphine or Norbuprenorphine

996M14 buprenorpine, norbuprenorphine

9E2RZU N/A

9VUGWB Buprenorphine

AAAFFQ Buprenorphine - Norbuprenorphine

BC7BAB buprenorphine,norbuprenorphine

BP0DBV Bupernorfina

BWCXLW buprenorfina, norbuprenorfina

BY165X Buprenorphine

DPDAYD BUPRENORPHINE

EQEEWZ Buprenorphine

EXJVPS Buprenorphine

FMTRIK None

FYOWRE BUPRENORPHINE

GELLLL Buprenorphine, norbuprenorphine

GF0Z2P buprenorphine

HB5JT5 Buprenorphine

I6BH66 Buprenorphine

J25JY8 BUPRENORPHINE, NORBUPRENORPHINE

JVU1US Buprenorphine, Norbuprenorphine

KCJJPI Buprenorphine, Norbuprenorphine

KIJ0C1 Buprenorphine and Norbuprenorphine

M3C1BY Buprenorphine

MPPDD7 buprenorphine and norbuprenorphine

N6TRAA none

NNNNAN Benzodiazepines, 7-Aminoflunitrazepam

NXXJIQ Buprenorphine

P2Z5XG Buprenorphine and Norbuprenorphine

PK1A71 None

PPPP1V Buprenorphine and norbuprenorphine

PY9S99 Buprenorphine

Sample 1 Analysis



8

Code Identified SubstancesQ37TVM Buprenorphine

QBJ8XI Buprenorphine

QEZOMA Not found

QLXQLQ Buprenorphine, Norbuprenorphine

QQVAUA buprenophine and norbuprenorphine

SLI666 buprenorphine

T1CLWX norbuprenorphine

UAKW5A cafeine

UNYP77 buprenorphine,norbuprenorphine

UUOIZR Buprenorphine

UY6AYY Bupernorphine, Norbupernorphine

VFVLEV Buprenorphine,nor-buprenorphine

VSRRNL none

WIC39B Buprenorphine and metabolite

WJUDYX buprenorphine

WWWSHS Buprenorphine and norbuprenorphine

X1RK1O Buprenorphine

XXJ0ZJ buprenorphine, norbuprenorphine

YFSRHH buprenorphine

YODSHO Buprenorphine y Norbuprenorphine

Z5VQQQ Buprenorphine and Norbuprenorphine



9

Code Buprenorphine Norbuprenorphine 0ALKWG + +

Its primary uses in medicine are in the treatment of those addicted to opiates such as heroine, but it may also be used to treat pain.It is not classified narcotics in but in Schedule I.Norbuprenorphine is the metabolite of buprenorphine.

0M60M0 ANP ANPNo common drugs were detected in the sample of 2015/2/BS-1.

0SXBBB + ANPBuprenorphine was detected in BS-1 sample.

22ZFEN + +Toxicological examination revealed the presence of Buprenorphine.

3FY8Y9 + +

5OLO5M + ANP

5P55XC ANP ANP

5QGV32 + ANPBuprenorphine is detected in urine. Glucuronides are not detected in the sample, which may imply manipulation of the urine sample

7Q4ADS + +-

7RUIPQ + ANP

7YA3XU + +

88RVB3 ANP ANPNo drugs or metabolites which ESG analyse were detected in this sample

8MQQYQ ANP ANPBuprenorphine or Norbuprenorphine were identified by Enzyme Immunoassay Techniques

8SSZSA - -

996M14 + +

9E2RZU - -No banned substances were detected using two solvent systems.

9VUGWB + ANPBuprenorphine detected.

9XQEUA - -

AAAFFQ + +In the sample was detected Buprenorphine and the metabolite Norbuprenorphine , this findings indicates that Buprenorphine was consumed.

BC7BAB + +buprenorphine, norbuprenorphine

BP0DBV + -Buprenorfina

Statement of findings for Test Sample 1



10

Code Buprenorphine Norbuprenorphine BUXMNK ANP ANP

Test Sample 2015/2/BS-1 does not contain controlled drugs therefore Negative.

BWCXLW + +caffeina

BXEXX5 ANP ANP

BY165X + ANPBuprenorphine is an opiod analgesic drug related to morphine and dihydrocodeine. It can also be used for heroin substitute treatment, it is a class C drug controlled under the

DFR6BO + +

DMRWDM ANP ANP

DPDAYD + -

EQEEWZ + ANPThe buprenorphine could come from the intake of the drug itself.

EUQHEC + +

EXJVPS + ANPFound to contain Beprenorphine

FMTRIK ANP ANPIn the sample 2015/2/BS-1 was not found controlled drugs.

FYOWRE + ANP

GELLLL + +This person consumed buprenorphine.

GF0Z2P + -Urine spiked with buprenorphine

HB5JT5 + -Buprenorphine was identified in the sample.

HFC4CC + +

HRY0TR ANP ANP

I6BH66 + ANP

IA1XAA + +

IG5EKJ - -Controlled drug and the substances listed in ICE menu were not detected in the test sample 2015/2/BS-1.

J25JY8 + +

JVU1US + +Sample is positive for Buprenorphine and Norbuprenorphine

KCJJPI + +Bupernorphine, Norbuprenorphine



11

Code Buprenorphine Norbuprenorphine KIJ0C1 + +

Buprenorphine is identified by imunochromatographic and confirmed by LC/MS/MS at semi-quantitaive concentration 145 ng/mlNorbuprenorphine is identified by imunochromatographic and confirmed by LC/MS/MS at semi-quantitaive concentration 140 ng/ml

L5JCLR ANP ANP

LBBBNB ANP ANP

M3C1BY + ANPCG-MS, Library, relation mass (m/z), equivalente Buprenorphine

MPPDD7 + +Adverse Analytical Finding for buprenorphine and norbuprenorphine

N6TRAA ANP ANP At the BS1 urine sample analyzed there were not found: amphetamines, barbiturates, benzodiazepines, cannabinoids, cocaine and metabolites neither opiates.

NNNNAN ANP ANP

NXXJIQ + ANP

P2Z5XG + +The sample contains buprenorphine and norbuprenorphine

PK1A71 - ANPBased on the above analysis, the sample found not to contain controlled drug.

PKNNLY - -

PPPP1V + +Buprenorphine and norbuprenorphine were found by LC/MS/MS.

PY9S99 + -Buprenorphine detected

Q37TVM + -Buprenorphine - positive

QBJ8XI + ANPScreening procedure positive to buprenorphine.

QEZOMA - -Not found

QKQQFO ANP ANP

QLXQLQ + +

QQNS9W ANP ANP

QQVAUA + +Presence of buprenorphine and metabolite

SJEVRS ANP ANPNo se encontró drogas de abuso, con las técnicas empleadas

SLI666 + -detox treatment of opioid addiction



12

Code Buprenorphine Norbuprenorphine T1CLWX - +

buprenorphine and norbuprenorphine

UAKW5A - -Identification was done according with WADA criteria

UEO7XX ANP ANPNo drugs detected for the tests that have been conducted, in the urine specimen

UMTD0Z ANP ANP

UNYP77 + +Sample 1 contains buprenorphine and its metabolite buprenorphine traces

UUOIZR + ANP

UY6AYY + +Sample 2015/2/BS-1 found to contain 1194.31 ng/ml of Bupernorphine and 1336.84 ng/ml of Norbupernorphine.

VFVLEV + +

VSRRNL ANP ANPIn the sample labeled 2015/2 BS-1 were not detected amphetamines, barbiturates, benzodiazepines, cannabinoides, cocaine metabolites and opiates

VVVIWA + +

WIC39B + +Consistent with use of buprenorphine

WJUDYX + -After chemical analysis was performed the sample was found to contain 47.2 ppm buprenorphine.

WWWSHS + +The result indicates the intake of buprenorphine.

X1RK1O + -Sample BS-1 was found to contain buprenorphine

XXJ0ZJ + +

YFSRHH + -

YODSHO + +

Z5VQQQ + +In the test simple 2015/2/BS-1the drugs Buprenorphine its metabolite Norbuprenorphine were found.

ZEPQ8E + +

ZHHNHG ANP ANP



13

Identification methods for Test Sample 1

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

0ALKWG S I I I

0M60M0 SI

0SXBBB S I

22ZFEN S I

3FY8Y9 S I S one step immonochromatographic assay

5OLO5M SI I I I

5QGV32 S I

7Q4ADS SI

7RUIPQ S I I

7YA3XU SI S I

88RVB3 SI I

8MQQYQ S I

8SSZSA S I

996M14 SI

9E2RZU SI I I DIP STRIP TEST

9VUGWB S I

9XQEUA SI

AAAFFQ I S Lateral Flow Immunoassay

BC7BAB I SI I

BP0DBV S I

BUXMNK I I S DRUG TEST KIT

BWCXLW S I

BXEXX5 S I

BY165X I I I SI HRMS

DFR6BO S I I

DMRWDM

S I

DPDAYD S I

EQEEWZ S I I I S inmunocromatografía

EUQHEC SI S immunochromatographic test

EXJVPS SI I

FMTRIK S I

FYOWRE S I

GELLLL S I I

Analytical Technique Codes

Legend: S ... used for Screening I ... used for Identification SI ... used for both



14

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

GF0Z2P SI I I SI

HB5JT5 S SI I

HFC4CC S I I

I6BH66 I I S

IA1XAA S I I

IG5EKJ I

J25JY8 S I I

JVU1US S SI

KCJJPI S I I I SI KIMS technique

KIJ0C1 I S Immunochromatographic

L5JCLR S I

LBBBNB S I I

M3C1BY S I

MPPDD7 SI I S

N6TRAA S I

NNNNAN SI I

NXXJIQ I I

P2Z5XG SI

PK1A71 I

PKNNLY I

PPPP1V S I I

PY9S99 S I I

Q37TVM I SI Dipro drug lab screen

QBJ8XI SI SI

QEZOMA SI I

QKQQFO S SI

QLXQLQ S SI I

QQNS9W I

QQVAUA S SI SI

SJEVRS S I I SI

SLI666 SI

T1CLWX S I SI

UAKW5A S SI

UEO7XX S I

UMTD0Z S I

UNYP77 S I S Randox,biochip

UUOIZR S I

UY6AYY SI

VFVLEV I S Triage 8; Sure Step Cup



15

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

VSRRNL S I

VVVIWA S I

WIC39B S I I

WJUDYX S I I I

WWWSHS

S I SI

X1RK1O S I

XXJ0ZJ I I S biochip

YFSRHH SI I I SI

YODSHO S I I

Z5VQQQ S I I

ZEPQ8E S I I

ZHHNHG S I



16


Frequency of use of screening and identification techniques:

Summary for test sample 1The response summary of all 86 participating laboratories for the identification of BS-1, frequency of use of screening andidentification techniques and false positives and negatives:

Identification of test sample 1:

False positives for Test Sample 1

Code Name Technique

Response Summary Participants: 130

NNNNAN Nordazepam, Oxazepam 141/200

NNNNAN 7-Aminoflunitrazepam, Temazepam 141/200


Section 100 110 120 141 150

Response SummaryParticipants: 86

Buprenorphine: 57

Norbuprenorphine: 34

Section 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

Screening 1 49 7 2 3 0 0 0 0 0 17 0 2 6 12

1.2% 57.0% 8.1% 2.3% 3.5% 0.0% 0.0% 0.0% 0.0% 0.0% 19.8% 0.0% 2.3% 7.0% 14.0%

Identification 1 6 2 1 5 2 11 4 1 1 72 1 8 22 4

1.2% 7.0% 2.3% 1.2% 5.8% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 9.3% 25.6% 4.7%

# labs using this technique

1 49 8 2 6 2 11 4 1 1 72 1 9 24 13

1.2% 57.0% 9.3% 2.3% 7.0% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 10.5% 27.9% 15.1%


False negatives for SM-1 (technique(s) used or ANP)

Code: 9E2RZU (150/171), 9XQEUA, (110), IG5EKJ (180), PKNNLY (180), QEZOMA (110/180)

8SSZSA (180), UAKW5A (180)

20 laboratories did not carry out nalysis for either buprenorphine or norbuprenorphine

DMRWDM, L5JCLR, SJEVRS, 8MQQYQ, QQNS9W, QKQQFO, BUXMNK, VSRRNL, 5P55XC,

0M60M0, ZHHNHG, FMTRIK, UMTD0Z, BXEXX5, 88RVB3, N6TRAA, NNNNAN, UEO7XX,

HRY0TR, LBBBNB

17

Substance: BS-1; Buprenorphine

Round: 2015/2

Z-Score Report per Sample per Substance

Robust average = 979 ng/mlUNODC value = 1150 ng/ml

z-scores can be interpreted by participants in line with ISO 13528:2005, section 7.4.2 and ISO/IEC guide43-1:1997(E) as follows:

|z| < 2 = satisfactory 2 ≤ |z| ≤ 3 = questionable

|z| > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

‐3.4

‐3.0

‐2.6

‐1.7

‐1.3‐1.1

‐0.6‐0.3

‐0.1 ‐0.10.0

0.1 0.10.3 0.4 0.4

0.5 0.60.8 0.8 0.8 0.9

0.9 1.0

‐4.0

‐3.0

‐2.0

‐1.0

0.0

1.0

2.0

3.0

4.0

WJUDY

X

KIJ0C1

BWCX

LW

VFVLEV

7Q4A

DS

GF0Z2P

VVVIWA

I6BH

66

ZEPQ

8E

JVU1U

S

996M

14

PPPP

1V

KCJJP

I

BC7B

AB

FYOWRE

GELLLL

3FY8Y9

P2Z5XG

5OLO

5M

UY6AY

Y

QLXQLQ

5QGV3

2

HFC4

CC

0ALKWG

UUO

IZR

6.6

18

Round: 201


-10

-8

-6

-4

-2

0

2

4

6

8

10z-

scor

e

Dispersion of z-scores using different analytical techniques for the quantification of buprenorphine in 2015/2 BS-1

GC/MS LC/MSHPLC

19

Substance: BS-1; norbuprenorphine

Round: 2015/2


Robust average = 2038 ng/mlUNODC value = 23 0 ng/ml





‐2.2 ‐2.2

‐1.2‐1.0 ‐0.8

‐0.1 0.0

0.0 0.0 0.1 0.20.3 0.4

0.6

1.31.5

2.4

‐4.0

‐3.0

‐2.0

‐1.0

0.0

1.0

2.0

3.0

4.0

VFVLEV

KIJ0C1

P2Z5XG

J25JY8

UY6AY

Y

JVU1U

S

QLXQLQ

BC7B

AB

KCJJPI

ZEPQ

8E

GELLLL

0ALKWG

PPPP

1V

996M

14

7Q4A

DS

3FY8Y9

VVVIWA

20

Round: 201


-10.0

-8.0

-6.0

-4.0

-2.0

0.0

2.0

4.0

6.0

8.0

10.0z-

scor

e

Dispersion of z-scores using different analytical techniques for the quantification of norbuprenorphine in 2015/2 BS-1

GC/MS LC/MSHPLC

21

Z-Scores for Test Sample 1



Concentration (ng/ml)

Deviation from

robust average

z-score

WJUDYX 47 -932 -3.4KIJ0C1 145 -834 -3.0

BWCXLW 270 -709 -2.6VFVLEV 509 -470 -1.77Q4ADS 620 -359 -1.3GF0Z2P 663 -317 -1.1VVVIWA 820 -159 -0.6I6BH66 895 -84 -0.3ZEPQ8E 940 -39 -0.1JVU1US 948 -31 -0.1996M14 977 -2 0.0PPPP1V 1003 24 0.1KCJJPI 1011 32 0.1BC7BAB 1070 91 0.3FYOWRE 1087 108 0.4GELLLL 1090 111 0.43FY8Y9 1107 128 0.5P2Z5XG 1136 157 0.65OLO5M 1190 211 0.8UY6AYY 1194 215 0.8QLXQLQ 1210 231 0.85QGV32 1213 234 0.9HFC4CC 1230 251 0.90ALKWG 1259 280 1.0UUOIZR 2797 1818 6.6


Deviation from

robust average

z-score

VFVLEV 138 -1900 -2.2KIJ0C1 140 -1898 -2.2P2Z5XG 1060 -978 -1.2J25JY8 1227 -811 -1.0UY6AYY 1337 -701 -0.8JVU1US 1988 -50 -0.1QLXQLQ 2020 -18 0.0BC7BAB 2060 22 0.0KCJJPI 2060 22 0.0ZEPQ8E 2140 102 0.1GELLLL 2172 134 0.20ALKWG 2306 268 0.3PPPP1V 2359 321 0.4996M14 2575 537 0.67Q4ADS 3100 1062 1.33FY8Y9 3337 1299 1.5VVVIWA 4100 2062 2.4

Code

Buprenorphine

Norpbuprenorphine

Code

22


Code Identified Substances0ALKWG MDA (Tenamfetamine)

0M60M0 Tenamfetamine (MDA)

0SXBBB Tenamfetamine (MDA)

22ZFEN Tenamfetamine

3FY8Y9 MDA

5OLO5M Tenamfetamine (MDA)

5P55XC MDA

5QGV32 MDA

7Q4ADS Tenamfetamine (MDA)

7YA3XU MDA

88RVB3 Tenamphetamine (MDA)

8MQQYQ Tenamfetamine, 6-MAM

8SSZSA MDA

996M14 Tenamfetamine

9E2RZU Amphetamine type stimulants

9VUGWB Tenamfetamine (MDA)

9XQEUA amphetamine type

AAAFFQ Tenamfetamine

BC7BAB tenamfetamine (MDA)

BXEXX5 MDA

BY165X MDA

DPDAYD MDA

EQEEWZ MDA (methylenedioxyamphetamine)

EXJVPS MDA

FMTRIK TENAMFETAMINE

FYOWRE MDA

GELLLL MDA

GF0Z2P MDA

HB5JT5 3,4-methylenedioxy-amphetamine(MDA, Tenamfetamine)

I6BH66 MDA

IG5EKJ GHB

J25JY8 3,4 MDA

JVU1US Tenamfetamine (MDA)

KCJJPI MDA

KIJ0C1 Tenamphetamine (MDA)

MPPDD7 MDA

N6TRAA Tenamfetamine (MDA)

NNNNAN Amfetamine

NXXJIQ Tenamfetamine/MDA/

P2Z5XG Tenamfetamine (MDA)

Sample 2 Analysis



23

Code Identified SubstancesPK1A71 Tenamfetamine (MDA)

PPPP1V MDA

PY9S99 Tenamfetamine (MDA)

Q37TVM AMFETAMINE TYPE STIMULANTS

QEZOMA MDA

QKQQFO mda

QLXQLQ MDA

QQNS9W MDA

QQVAUA MDA

SLI666 MDA

T1CLWX amphetamines

UAKW5A Bupremorphine

UEO7XX Tenamfetamine (MDA)

UNYP77 MDMA

UUOIZR Tenamfetamine

UY6AYY MDA

VFVLEV Tenamfetamine (MDA)

VSRRNL none

WIC39B Methylenedioxyamphetamine

WJUDYX Amfetamine

WWWSHS MDA

X1RK1O Methylenedioxyamphetamine (MDA)

XXJ0ZJ MDA

YFSRHH MDA(tenamfetamine)

YODSHO MDA (Tenamfetanine)

Z5VQQQ Tenamfetamine (MDA)

ZHHNHG MDA



24

Code Tenamfetamine (MDA)

0ALKWG +MDA is an amphetamine classified narcotic in . It's also a metabolite of MDMA and MDEA

0M60M0 +Tenamfetamine (MDA) was detected in the sample of 2015/2/BS-2.

0SXBBB +Tenamfetamine (MDA) was detected in BS-2 sample.

22ZFEN +Toxicological examination revealed the presence of Tenamfetamine

3FY8Y9 +

5OLO5M +

5P55XC ANP

5QGV32 +MDA is detected in urine. A positive test may be caused by the intake of MDA. MDA may also be formed in the body after intake of MDMA. MDA is a substance with stimulating and hallucinogenic effects similar to ecstasy

7Q4ADS +-

7RUIPQ +

7YA3XU +

88RVB3 +This sample was found to contain 884 ng/ml MDA. The cut off used by this laboratory is 200 ng/ml. Therefore this sample is considered to be positive for the presence of MDA.

8MQQYQ +Tenamfetamine and 6-MAM were identified by GC-MS

8SSZSA +First the sample was analyzed by Architect (Immunoassay) giving positive for MDA( >1000 ng/mL). It was confim with a solid phase column extraction with GC-MS.

996M14 +

9E2RZU -Amphetamine was detected in the sample, using two solvent systems but was not quantified .

9VUGWB +Tenamfetamine (MDA) detected.

9XQEUA -

AAAFFQ +In the sample was detected Tenamfetamine, this finding indicates that Tenamfetamine was consumed.

BC7BAB +tenamfetamine (MDA)

BP0DBV -




25


BUXMNK ANPTest Sample 2015/2/BS-2 does not contain controlled drugs therefore Negative.

BWCXLW -caffeina, paracetamolo

BXEXX5 +

BY165X +Paracetamol was also detected in this sample. MDA is a stimulant drug and has no therapeutic use, it is illicitly manufactured and marketed in the form of tablets and capsules. It is commonly referred to as 'ecstasy' and is a Class A drug under the .

DFR6BO +

DMRWDM ANP

DPDAYD +

EQEEWZ +The MDA detection indicates consume of MDMA, however the MDA could come from intake of the drug itself.

EUQHEC +

EXJVPS +Found to contain MDA

FMTRIK +In the sample 2015/2/BS-2 was found and confirmed the presence of TENAMFETAMINE (MDA)

FYOWRE +

GELLLL +This person consumed MDA.

GF0Z2P +MDMA taking (ecstasy)

HB5JT5 +MDA was identified in the sample. Further Amphetamine-propionyl was also identified by GC-MS. However, library match hit was 27 only.

HFC4CC +

HRY0TR ANP

I6BH66 +

IA1XAA +

IG5EKJ -The test sample 2015/2/BS-2 was found to contain the controlled drug gamma-hydroxybutyric acid (GHB).

J25JY8 +

JVU1US +Sample is positive for MDA



26


KCJJPI +MDA

KIJ0C1 +not Identified by imunochromatographic but identified by LC/MS/MS at semi-quantitaive concentration 514 ng/ml

L5JCLR ANP

LBBBNB ANP

M3C1BY ANP

MPPDD7 +Adverse Analytical FInding for MDA

N6TRAA +At the BS2 urine sample analyzed there was found Tenamfetamine (MDA).At the BS2 urine sample analyzed there were not found barbiturates, benzodiazepines, cannabinoids, cocaine and metabolites neither opiates.

NNNNAN -

NXXJIQ +

P2Z5XG +The sample contains tenamfetamine (MDA)

PK1A71 +Based on the above analysis, the sample found to contain Tenamfetamine (MDA)

PKNNLY -

PPPP1V +MDA was found by LC/MS/MS.

PY9S99 +Tenamfetamine (MDA) detected

Q37TVM -MDMA - positiveAmfetamine - positive

QBJ8XI ANP

QEZOMA +The sample correspond: MDA

QKQQFO +

QLXQLQ +

QQNS9W +

QQVAUA +Presence of MDA

SJEVRS ANPNo se encontró drogas de abuso,con las técnicas empleadas



27


SLI666 +MDA consumer

T1CLWX +MDA and acetaminophen

UAKW5A -Identification was done according with WADA criteria

UEO7XX +The findings detected the presence of MDA in the urine specimen. All other drugs for which tests have been conducted were negative.

UMTD0Z ANP

UNYP77 -Sample 2 contains MDMA

UUOIZR +

UY6AYY +Sample 2015/2/BS-2 found to contain 163.157 ng/ml of MDA

VFVLEV +

VSRRNL ANPIn the sample labeled 2015/2 BS-2 were not detected amphetamines, barbiturates, benzodiazepines, cannabinoides, cocaine metabolites and opiates

VVVIWA +

WIC39B +Consistent with use of methylenedioxyamphetamine

WJUDYX - After chemical analysis was performed the sample was found to contain 278.4 ppm Amphetamine.

WWWSHS +The result indicates the intake of MDA

X1RK1O +Sample BS-2 was found to contain methylenedioxyamphetamine (MDA)

XXJ0ZJ +

YFSRHH +

YODSHO +

Z5VQQQ +In the test simple 2015/2/BS-2the drug Tenamfetamine (MDA) was found.

ZEPQ8E +

ZHHNHG +Consumption of MDA



28


Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

0ALKWG S I I I

0M60M0 SI

0SXBBB S I

22ZFEN S I


5OLO5M SI I I I

5QGV32 S I

7Q4ADS SI

7RUIPQ S I I

7YA3XU SI S I

88RVB3 SI I

8MQQYQ S I

8SSZSA S I

996M14 SI


9VUGWB S I

9XQEUA SI


BC7BAB I SI I

BP0DBV S I


BWCXLW S I

BXEXX5 S I


DFR6BO S I I

DMRWDM

S I

DPDAYD S I



EXJVPS SI I

FMTRIK S I

FYOWRE S I

GELLLL S I I





29

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

GF0Z2P SI I I SI

HB5JT5 S SI I

HFC4CC S I I

I6BH66 I I S

IA1XAA S I I

IG5EKJ I

J25JY8 S I I

JVU1US S SI



L5JCLR S I

LBBBNB S I I

M3C1BY S I

MPPDD7 SI I S

N6TRAA S I

NNNNAN SI I

NXXJIQ I I

P2Z5XG SI

PK1A71 I

PKNNLY I

PPPP1V S I I

PY9S99 S I I


QBJ8XI SI SI

QEZOMA SI I

QKQQFO S SI

QLXQLQ S SI I

QQNS9W I

QQVAUA S SI SI

SJEVRS S I I SI

SLI666 SI

T1CLWX S I SI

UAKW5A S SI

UEO7XX S I

UMTD0Z S I


UUOIZR S I

UY6AYY SI




30

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

VSRRNL S I

VVVIWA S I

WIC39B S I I

WJUDYX S I I I

WWWSHS

S I SI

X1RK1O S I


YFSRHH SI I I SI

YODSHO S I I

Z5VQQQ S I I

ZEPQ8E S I I

ZHHNHG S I



31



Summary for test sample The response summary of all 86 participating laboratories for the identification of BS-2, frequency of use of screening andidentification techniques and false positives and negatives:


False positives for Test Sample

Code Name Technique



Section 120 141 150 160

9E2RZU Amfetamine 150/171

IG5EKJ GHB 180

NNNNAN Cocaine, Amfetamine 141/200

Q37TVM Amfetamine, MDMA 150

UNYP77 MDMA 150

WJUDYX Amfetamine 231

False negatives for BS-2 (technique(s) used or ANP)

9E2RZU (150/171), 9XQEUA (110), BP0DBV (180), BWCXLW (180), IG5EKJ (180), NNNNAN

(141/200) PKNNLY (180/180), Q37TVM (150), UNYP77 (150/150), WJUDYX (231)

11 laboratories did not carry out nalysis for MDA

5P55XC, BUXMNK, DMRWDM, HRY0TR, L5JCLR, LBBBNB, M3C1BY, QBJ8XI, SJEVRS,

UMTD0Z, VSRRNL


Tenamfetamine (MDA): 64

Section 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

Screening 1 49 7 2 3 0 0 0 0 0 17 0 2 6 12

1.2% 57.0% 8.1% 2.3% 3.5% 0.0% 0.0% 0.0% 0.0% 0.0% 19.8% 0.0% 2.3% 7.0% 14.0%

Identification 1 6 2 1 5 2 11 4 1 1 72 1 8 22 4

1.2% 7.0% 2.3% 1.2% 5.8% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 9.3% 25.6% 4.7%


1 49 8 2 6 2 11 4 1 1 72 1 9 24 13

1.2% 57.0% 9.3% 2.3% 7.0% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 10.5% 27.9% 15.1%


8MQQYQ 6-Monoacetylmorphine 180

UAKW5A Buprenorphine 180

32

Substance: BS-2; MDA

Round: 2015/2







‐3.4

‐2.2

‐1.9‐1.6

‐1.0 ‐1.0

‐0.6

‐0.3‐0.2 ‐0.1

‐0.1 0.0 0.0

0.00.1 0.2 0.2

0.3 0.40.5 0.6

1.1

3.0

‐4.0

‐3.0

‐2.0

‐1.0

0.0

1.0

2.0

3.0

4.0

UY6AY

Y

BC7B

AB

KIJ0C1

GF0Z2P

VFVLEV

I6BH

66

3FY8Y9

QLXQLQ

JVU1U

S

VVVIWA

88RV

B3

5P55

XC

5QGV

32

KCJJPI

FYOWRE

0ALKWG

PPPP

1V

996M

14

HFC4

CC

7Q4A

DS

QQVA

UA

ZEPQ

8E

GELLLL

J25JY8

5OLO

5M

SLI666

ZHHNHG

P2Z5XG

7.2 12.74.5

‐4.3

4.0

33

Round: 201


-6

-4

-2

0

2

4

6z-

scor

e

Dispersion of z-scores using different analytical techniques for the quantification of MDA in 2015/2 BS-2

GC/MS LC/MSHPLC

34





Deviation from robust average

z-score

UY6AYY 163 -738 -4.3BC7BAB 320 -581 -3.4KIJ0C1 514 -387 -2.2GF0Z2P 581 -320 -1.9VFVLEV 618 -283 -1.6I6BH66 723 -178 -1.03FY8Y9 730 -171 -1.0QLXQLQ 798 -103 -0.6JVU1US 848 -53 -0.3VVVIWA 870 -31 -0.288RVB3 884 -17 -0.15P55XC 890 -11 -0.15QGV32 896 -5 0.0KCJJPI 897 -4 0.0

FYOWRE 902 1 0.00ALKWG 923 22 0.1PPPP1V 929 28 0.2996M14 930 29 0.2HFC4CC 960 59 0.37Q4ADS 975 74 0.4QQVAUA 980 79 0.5ZEPQ8E 996 95 0.6GELLLL 1089 188 1.1J25JY8 1412 511 3.0

5OLO5M 1590 689 4.0SLI666 1670 769 4.5

ZHHNHG 2145 1244 7.2P2Z5XG 3089 2188 12.7

CodeMDA

35


Code Identified Substances0ALKWG Methadone

0M60M0 Methadone

0SXBBB Methadone

22ZFEN Methadone

3FY8Y9 methadone

5OLO5M Methadone

5P55XC methadone

5QGV32 Methadone

7Q4ADS Methadone

7YA3XU METHADONE

88RVB3 Methadone

8MQQYQ Methadone

8SSZSA METHADONE

996M14 metadone

9E2RZU N/A

9VUGWB Methadone

AAAFFQ Methadone

BC7BAB methadone

BP0DBV Metadona

BWCXLW metadone

BXEXX5 Methadone

BY165X Methadone

DPDAYD METHADONE

EQEEWZ Methadone

FMTRIK METHADONE

FYOWRE METHADONE

GELLLL Methadone

GF0Z2P METHADONE

HB5JT5 Methadone

I6BH66 Methadone

IG5EKJ Methadone

J25JY8 METHADONE

JVU1US Methadone

KCJJPI Methadone

KIJ0C1 Methadone

L5JCLR methadone

M3C1BY Methadone

MPPDD7 methadon (and EDDP)

N6TRAA Methadone

NNNNAN cocaine, codeine, morphine

Sample 3 Analysis



36

Code Identified SubstancesNXXJIQ Methadone

P2Z5XG Methadone

PK1A71 Methadone

PPPP1V Methadone

PY9S99 Methadone

Q37TVM Methadone

QBJ8XI Metadone

QEZOMA METHADONE

QKQQFO methadone

QLXQLQ Methadone

QQNS9W METHADONE

QQVAUA Methadone

SJEVRS Metadona

SLI666 methadone

T1CLWX methadone

UAKW5A Methadone

UEO7XX Methadone

UMTD0Z METHADONE

UNYP77 methadone

UUOIZR Methadone

UY6AYY Methadone

VFVLEV Methadone

VSRRNL Methadone

WIC39B methadone

WJUDYX Methadone

WWWSHS Methadone

X1RK1O Methadone

XXJ0ZJ methadone

YFSRHH methadone

YODSHO Metadona

Z5VQQQ Methadone

ZHHNHG methadone



37

Code Methadone 0ALKWG +

Methadone is one of the drugs substitutes authorized in the treatment of the major drug dependancies in opiates.It's classified narcotics in .

0M60M0 +Methadone was detected in the sample of 2015/2/BS-3.

0SXBBB +Methadone was detected in BS-3 sample.

22ZFEN +Toxicological examination revealed the presence of methadone

3FY8Y9 +

5OLO5M +

5P55XC ANP

5QGV32 +Methadone is detected in the urine sample. The metabolite EDDP is not detected in the sample. Urine may be manipulated

7Q4ADS +-

7RUIPQ +

7YA3XU +

88RVB3 +This sample was found to contain less than 1000ng/ml (approx. 2087 ng/ml) methadone. The cut off used by this laboratory is 250 ng/ml. Therefore this sample is considered positive for the presence of methadone

8MQQYQ +Methadone was identified by GC-MS

8SSZSA +First the sample was analyzed by Architect (Immunoassay) giving positive for Methadone( >1000 ng/mL). It was confim with a solid phase column extraction with GC-MS.

996M14 +

9E2RZU -No banned substances were detected using two solvent systems.

9VUGWB +Methadone detected.

9XQEUA -

AAAFFQ +In the sample was detected Methadone, this finding indicates that Methadone was consumed.

BC7BAB +methadone

BP0DBV +Metadona




38

Code Methadone BUXMNK ANP

Test Sample 2015/2/BS-3 does not contain controlled drugs therefore Negative.

BWCXLW +caffeina, metabolita EDDP

BXEXX5 +

BY165X +Methadone is a prescribed opiate analgesic which can be used in heroin substitution programmes, it is a Class A drug controlled under the . Paracetamol is a common analgesic available over-the-counter and in combination with number of other drugs.

DFR6BO +

DMRWDM ANP

DPDAYD +

EQEEWZ +The methadone could come from the intake of the drug itself.

EUQHEC +

EXJVPS ANP

FMTRIK +In the sample 2015/2/BS-3 was found and confirmed the presence of METHADONE

FYOWRE +

GELLLL +This person consumed methadone.

GF0Z2P +Methadone taking

HB5JT5 +Methadone was identified in the sample.

HFC4CC +

HRY0TR ANP

I6BH66 +

IA1XAA +

IG5EKJ +The test sample 2015/2/BS-3 was found to contain the controlled drug methadone.

J25JY8 +

JVU1US +Sample is positive for Methadone

KCJJPI +Methadone



39

Code Methadone KIJ0C1 +

Methadone is identified by imunochromatographic and confirmed by LC/MS/MS at semi-quantitaive concentration 283 ng/ml

L5JCLR +use of methadone

LBBBNB ANP

M3C1BY +CG-MS retention time and relation mass (m/z) the reference material Methadone are equivalent simple 2015/2/BS-3

MPPDD7 +Adverse Analytical Finding for methadon (and EDDP)

N6TRAA + At the BS3 urine sample analyzed there was found Methadone. At the BS3 urine sample analyzed there were not found barbiturates, benzodiazepines, cannabinoids neither cocaine and metabolites.

NNNNAN -

NXXJIQ +

P2Z5XG +The sample contains methadone

PK1A71 +Based on the above analysis, the sample found to contain Methadone

PKNNLY -

PPPP1V +Methadone was found by LC/MS/MS.

PY9S99 +Methadone detected

Q37TVM +Methadone - positive

QBJ8XI +Positive to metadone.

QEZOMA +The sample correspond: Methadone

QKQQFO +

QLXQLQ +

QQNS9W +

QQVAUA +Presence of methadone

SJEVRS +Hubo consumo de Metadona

SLI666 +detox treatment of opioid addiction



40

Code Methadone T1CLWX +

methadone

UAKW5A +Identification was done according with WADA criteria

UEO7XX +The findings detected the presence of Methadone in the urine specimen. All other drugs for which tests have been conducted were negative.

UMTD0Z +The coincidence between the relative retention times and mass-fragmentograms fron a reference standard analysed at the same conditions that the biological sample indicates the presence of methadone.

UNYP77 +Sample 3 contains methadone

UUOIZR +

UY6AYY +Sample 2015/2/BS-3 found to contain 2643.157 ng/ml of Methadone.

VFVLEV +

VSRRNL +In the sample labeled 2015/2 BS-3 was detected methadone

VVVIWA +

WIC39B +Consistent with use of methadone

WJUDYX +After chemical analysis was performed the sample was found to contain 1.015 ppm Methadone.

WWWSHS +The result indicates the intake of methadone

X1RK1O +Sample BS-3 was found to contain methadone

XXJ0ZJ +

YFSRHH +

YODSHO +

Z5VQQQ +In the test simple 2015/2/BS-3 the drug Methadone was found.

ZEPQ8E +

ZHHNHG +



41


Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

0ALKWG S I I I

0M60M0 SI

0SXBBB S I

22ZFEN S I


5OLO5M SI I I I

5QGV32 S I

7Q4ADS SI

7RUIPQ S I I

7YA3XU SI S I

88RVB3 SI I

8MQQYQ S I

8SSZSA S I

996M14 SI


9VUGWB S I

9XQEUA SI


BC7BAB I SI I

BP0DBV S I


BWCXLW S I

BXEXX5 S I


DFR6BO S I I

DMRWDM

S I

DPDAYD S I



EXJVPS SI I

FMTRIK S I

FYOWRE S I

GELLLL S I I





42

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

GF0Z2P SI I I SI

HB5JT5 S SI I

HFC4CC S I I

I6BH66 I I S

IA1XAA S I I

IG5EKJ I

J25JY8 S I I

JVU1US S SI



L5JCLR S I

LBBBNB S I I

M3C1BY S I

MPPDD7 SI I S

N6TRAA S I

NNNNAN SI I

NXXJIQ I I

P2Z5XG SI

PK1A71 I

PKNNLY I

PPPP1V S I I

PY9S99 S I I


QBJ8XI SI SI

QEZOMA SI I

QKQQFO S SI

QLXQLQ S SI I

QQNS9W I

QQVAUA S SI SI

SJEVRS S I I SI

SLI666 SI

T1CLWX S I SI

UAKW5A S SI

UEO7XX S I

UMTD0Z S I


UUOIZR S I

UY6AYY SI




43

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

VSRRNL S I

VVVIWA S I

WIC39B S I I

WJUDYX S I I I

WWWSHS

S I SI

X1RK1O S I


YFSRHH SI I I SI

YODSHO S I I

Z5VQQQ S I I

ZEPQ8E S I I

ZHHNHG S I



44






Code Name Technique


NNNNAN Morphine, Metamfetamine, MDMA 141/200

NNNNAN Cocaine, Amfetamine, Codeine, MDA 141/200180


Section 100 110 120 141 150



Code: 9E2RZU (150/171), 9XQEUA, (110), NNNNAN (.41/200), PKNNLY (180), QEZOMA

(110/180)

6 laboratories did not carry out nalysis for Methadone

EXJVPS, BUXMNK, 5P55XC, HRY0TR, LBBBNB, DMRWDM


Methadone: 76

Section 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

Screening 1 49 7 2 3 0 0 0 0 0 17 0 2 6 12

1.2% 57.0% 8.1% 2.3% 3.5% 0.0% 0.0% 0.0% 0.0% 0.0% 19.8% 0.0% 2.3% 7.0% 14.0%

Identification 1 6 2 1 5 2 11 4 1 1 72 1 8 22 4

1.2% 7.0% 2.3% 1.2% 5.8% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 9.3% 25.6% 4.7%


1 49 8 2 6 2 11 4 1 1 72 1 9 24 13

1.2% 57.0% 9.3% 2.3% 7.0% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 10.5% 27.9% 15.1%


45

Substance: BS-3; Methadone

Round: 2015/2







‐2.4

‐2.0

‐1.5‐1.3 ‐1.2

‐1.2 ‐1.1

‐0.8 ‐0.8

‐0.4 ‐0.4 ‐0.3‐0.1 ‐0.1 ‐0.1

0.0 0.1 0.1 0.10.2

0.3 0.30.6 0.6

0.7 0.80.9 0.9

1.1 1.11.3

1.7

‐4.0

‐3.0

‐2.0

‐1.0

0.0

1.0

2.0

3.0

4.0

WJUDY

X

KIJ0C1

22ZFEN

VFVLEV

P2Z5XG

BWCX

LW

3FY8Y9

5OLO

5M

L5JCLR

996M

14

J25JY8

5P55

XC

QQVA

UA

8SSZSA

GF0Z2P

QLXQLQ

SJEV

RS

VVVIWA

PPPP

1V

88RV

B3

GELLLL

FYOWRE

5QGV

32

SLI666

I6BH

66

HFC4

CC

UY6AY

Y

ZEPQ

8E

0ALKWG

7Q4A

DS

BC7B

AB

JVU1U

S

UUO

IZR

ZHHNH

G

8.14.4

46

Round: 201


-4

-3

-2

-1

0

1

2

3

4z-

scor

es

Dispersion of z-scores using different analytical techniques for the quantification of Methadone in 2015/2 BS-3

GC/MS LC/MSHPLC

47





Deviation from robust average

z-score

WJUDYX 1 -1914 -2.4KIJ0C1 283 -1632 -2.022ZFEN 736 -1179 -1.5VFVLEV 830 -1085 -1.3P2Z5XG 910 -1005 -1.2

BWCXLW 974 -941 -1.23FY8Y9 1031 -884 -1.15OLO5M 1280 -635 -0.8L5JCLR 1302 -613 -0.8996M14 1595 -320 -0.4J25JY8 1602 -313 -0.45P55XC 1660 -255 -0.3QQVAUA 1800 -115 -0.18SSZSA 1840 -75 -0.1GF0Z2P 1860 -55 -0.1QLXQLQ 1928 13 0.0SJEVRS 1998 83 0.1VVVIWA 2000 85 0.1PPPP1V 2006 91 0.188RVB3 2087 172 0.2GELLLL 2175 260 0.3

FYOWRE 2184 269 0.35QGV32 2367 452 0.6SLI666 2430 515 0.6I6BH66 2497 582 0.7HFC4CC 2533 618 0.8UY6AYY 2643 728 0.9ZEPQ8E 2648 733 0.90ALKWG 2778 863 1.17Q4ADS 2800 885 1.1BC7BAB 2980 1065 1.3JVU1US 3329 1414 1.7UUOIZR 5490 3575 4.4ZHHNHG 8451 6536 8.1

CodeMethadone

48


Code Identified Substances0ALKWG Nordazepam

0M60M0 Nordazepam

0SXBBB Nordazepam

22ZFEN nordazepam

3FY8Y9 nordazepam

5OLO5M Nordazepam

5P55XC nordiazepam

5QGV32 Nordazepam

7Q4ADS Nordazepam

7YA3XU METHAMPHETAMINE, NORDIAZEPAM

88RVB3 Nordiazepam

8MQQYQ Nordazepam

8SSZSA NORDAZEPAM

996M14 Nordazepam

9E2RZU OXAZEPAM

9VUGWB Nordazepam

9XQEUA benzodiazepines type

AAAFFQ Nordazepam

BC7BAB nordazepam

BP0DBV Nordazepam

BUXMNK Nordazepam

BWCXLW nordazepam

BXEXX5 Nordazepam

BY165X Nordiazepam and Paracetamol

DMRWDM Nordiazepam

DPDAYD NORDIAZEPAM

EQEEWZ Nordiazepam

EXJVPS Benzodiazepines

FMTRIK NORDIAZEPAM

FYOWRE NORDIAZEPAM

GELLLL Nordazepam

GF0Z2P NORDAZEPAM

HB5JT5 Nordazepam

I6BH66 Nordazepam

IG5EKJ Nordazepam

J25JY8 NORDAZEPAM

JVU1US Nordazepam

KIJ0C1 Nordiazepam

L5JCLR nordazepam

LBBBNB Nordazepam

Sample 4 Analysis



49

Code Identified SubstancesM3C1BY Nordazepam

MPPDD7 Desmethyldiazepam

N6TRAA Nordazepam

NNNNAN cocaine, opiates/opium

NXXJIQ Nordazepam

P2Z5XG Nordazepam

PK1A71 Nordazepam

PPPP1V Nordiazepam

PY9S99 Nordazepam

Q37TVM BENZODIAZEPINES

QBJ8XI Nordazepam

QEZOMA Nordazepam

QKQQFO nordiazepam

QLXQLQ Nordazepam

QQVAUA Nordazepam

SJEVRS Nordiazepam

SLI666 nordazepam

T1CLWX benzodiazepines

UAKW5A Nordiazepam

UEO7XX Nordazepam (DMDZ)

UMTD0Z NORDAZEPAM

UNYP77 benzodiazepines

UUOIZR Nordazepam

UY6AYY Nordazepam

VFVLEV Nordazepam

VSRRNL Nordazepan

WIC39B Nordiazepam

WJUDYX temazepam

WWWSHS nordiazepam

X1RK1O Nordazepam

XXJ0ZJ nordazepam

YFSRHH nordazepam

YODSHO Nordazepm

Z5VQQQ Nordazepam

ZHHNHG benzodiazepines



50

Code Nordazepam 0ALKWG +

Nordazepam is a 1,4-benzodiazepine derivative, is a drug used to treat the anxiety and in the cases of alcoholic weanings;nordazepam is not classified narcotic in but in Schedule I.

0M60M0 +Nordazepam was detected in the sample of 2015/2/BS-4.

0SXBBB +Nordazepam was detected in BS-4 sample.

22ZFEN +Toxicological examination revealed the presence of nordiazepam.

3FY8Y9 +

5OLO5M +

5P55XC ANP

5QGV32 +Nordazepam is detected in urine. Nordazepam is a metabolite of diazepam, but is also marketed as a medicine in some countries. The finding may imply intake of diazepam/nordiazepam or other benzodiazepines that metabolizes to nordiazepam

7Q4ADS +-

7RUIPQ +

7YA3XU +

88RVB3 +This sample was found to contain less than 300 ng/ml (approx. 1155 ng/ml) nordiazepam. The cut off used by this laboratory is 100 ng/ml. Therefore this sample is considered positive for the presence of Nordiazepam.

8MQQYQ +Nordazepam was identified by GC-MS

8SSZSA +First the sample was analyzed by Architect (Immunoassay) giving positive for Nordazepam ( >1000 ng/mL). It was confim with a solid phase column extraction with GC-MS.

996M14 +

9E2RZU -Oxazepam (Benzodiazepines) was detected in the sample, using two solvent systems but was not quantified .

9VUGWB +Nordazepam detected.

9XQEUA -

AAAFFQ +In the sample was detected Nordazepam, this finding indicates that Nordazepam was consumed.

BC7BAB +nordazepam




51

Code Nordazepam BP0DBV +

Nordazepam

BUXMNK +Test Sample 2015/2/BS-4 was found to contain controlled drugs for Nordazepam therefore Positive for the Screening and Confirmatory Tests with concentration value of 885.71 ng/ml.

BWCXLW +caffeina

BXEXX5 +

BY165X +Nordiazepam is a pharmacologically active breakdown product of a number of benzodiazepine drugs including diazepam and chlordiazepoxide, both of which are prescribed for the treatment of anxiety. Paracetamol is a common analgesic available over-the-counter and in combination with a number of other drugs.

DFR6BO +

DMRWDM +The urine was analysed and found to contain nordiazepam.

DPDAYD +

EQEEWZ +Nordiazepam could come from the intake of the drug itself or from de metabolism of the other benzodiazepines.

EUQHEC +

EXJVPS ANPFound to contain Benzodiazepine drug

FMTRIK +In the sample 2015/2/BS-4 was found and confirmed the presence of NORDIAZEPAM

FYOWRE +

GELLLL +This person consumed nordazepam, or other benzodiazepine.

GF0Z2P +Metabolite ( Diazepam, Temazepam) and/or nordazepam taking

HB5JT5 +Nordazepam was identified in the sample. Very small peak compatible to Medozepam was identified by GC-MS. But library match hit was 38. Further Cannabinol-pentafluoropropionate was identified by GC-MS. However library match hit was 33 only.

HFC4CC +

HRY0TR ANP

I6BH66 +

IA1XAA +

IG5EKJ +The test sample 2015/2/BS-4 was found to contain the controlled drug nordazepam.



52

Code Nordazepam J25JY8 +

JVU1US +Sample is positive for Nordazepam

KCJJPI +

KIJ0C1 +Nordiazepam is identified by imunochromatographic and confirmed by LC/MS/MS at semi-quantitaive concentration 250 ng/ml

L5JCLR +use of benzodiazepines

LBBBNB +After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) and Gas Chromatography/Mass Spectrometry (GC/MS), was detected nordazepam substance in the urine sample 2015/2/BS-4.

M3C1BY +Screening test (EIA) positive Benzodiazepine. CG-MS retention time and relation mass (m/z) the reference material Nordazepam are equivalent simple 2015/2/BS-4

MPPDD7 +Adverse Analytical Finding for desmethyldiazepam (nordazepam)

N6TRAA +At the BS4 urine sample analyzed there was found Nordazepam.At the BS4 urine sample analyzed there were not found: amphetamines, barbiturates, cannabinoids, cocaine and metabolites neither opiates.

NNNNAN -

NXXJIQ +

P2Z5XG +The sample contains nordazepam

PK1A71 +Based on the above analysis, the sample found to contain Nordazepam

PKNNLY +

PPPP1V +Nordiazepam was found by LC/MS/MS.

PY9S99 +Nordazepam detected

Q37TVM -Oxazepam

QBJ8XI +Positive to nordazepam.

QEZOMA +The sample correspond: Nordazepam

QKQQFO +

QLXQLQ +



53

Code Nordazepam QQNS9W ANP

QQVAUA +Presence of nordazepam

SJEVRS +Hubo consumo de benzodiacepinas, detectándose el metabolito activo Nordiazepam.

SLI666 +benzos user

T1CLWX +nordiazepam

UAKW5A +Identification was done according with WADA criteria

UEO7XX +The findings detected the presence of Nordazepam in the urine specimen. All other drugs for which tests have been conducted were negative.

UMTD0Z +The coincidence between the relative retention times and mass-fragmentograms fron a reference standard analysed at the same conditions that the biological sample indicates the presence of Nordazepam.

UNYP77 ANPSample 4 contains benzodiazepines.

UUOIZR +

UY6AYY +Sample 2015/2/BS-4 found to contain 2189.47 ng/ml of Nordazepam.

VFVLEV +

VSRRNL +In the sample labeled 2015/2 BS-4 was detected Nordazepam

VVVIWA +

WIC39B +Consistent with use of nordiazepam

WJUDYX -After chemical analysis was performed the sample was found to contain 481.5ppm temazepam.

WWWSHS +The result indicates the intake of diazepam or nordiazepam

X1RK1O +Sample BS-4 was found to contain nordazepam

XXJ0ZJ +

YFSRHH +

YODSHO +

Z5VQQQ +In the test simple 2015/2/BS-4 the drug Nordazepam was found.



54

Code Nordazepam ZEPQ8E +

ZHHNHG ANP



55


Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

0ALKWG S I I I

0M60M0 SI

0SXBBB S I

22ZFEN S I


5OLO5M SI I I I

5QGV32 S I

7Q4ADS SI

7RUIPQ S I I

7YA3XU SI S I

88RVB3 SI I

8MQQYQ S I

8SSZSA S I

996M14 SI


9VUGWB S I

9XQEUA SI


BC7BAB I SI I

BP0DBV S I


BWCXLW S I

BXEXX5 S I


DFR6BO S I I

DMRWDM

S I

DPDAYD S I



EXJVPS SI I

FMTRIK S I

FYOWRE S I

GELLLL S I I





56

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

GF0Z2P SI I I SI

HB5JT5 S SI I

HFC4CC S I I

I6BH66 I I S

IA1XAA S I I

IG5EKJ I

J25JY8 S I I

JVU1US S SI



L5JCLR S I

LBBBNB S I I

M3C1BY S I

MPPDD7 SI I S

N6TRAA S I

NNNNAN SI I

NXXJIQ I I

P2Z5XG SI

PK1A71 I

PKNNLY I

PPPP1V S I I

PY9S99 S I I


QBJ8XI SI SI

QEZOMA SI I

QKQQFO S SI

QLXQLQ S SI I

QQNS9W I

QQVAUA S SI SI

SJEVRS S I I SI

SLI666 SI

T1CLWX S I SI

UAKW5A S SI

UEO7XX S I

UMTD0Z S I


UUOIZR S I

UY6AYY SI




57

Code 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

VSRRNL S I

VVVIWA S I

WIC39B S I I

WJUDYX S I I I

WWWSHS

S I SI

X1RK1O S I


YFSRHH SI I I SI

YODSHO S I I

Z5VQQQ S I I

ZEPQ8E S I I

ZHHNHG S I



58






Code Name Technique



Section 100 110 120 141 150 160


7YA3XU Metamfetamine 231

9E2RZU Oxazepam 150/171

NNNNAN Cocaine, opiates/opium 141/200

Q37TVM Oxazepam 150

WJUDYX Temazepam 160/231


Code: 9E2RZU (150/171), 9XQEUA, (110), NNNNAN (141/200), Q37TVM (150), WJUDYX

(160/231)

6 laboratories did not carry out Analysis for Nordazepam

EXJVPS , 5P55XC, HRY0TR, UNYP77, ZHHNHG, QQNS9W


Nordazepam: 75

Section 100 110 120 141 150 160 161 170 171 172 180 200 230 231 210

Screening 1 49 7 2 3 0 0 0 0 0 17 0 2 6 12

1.2% 57.0% 8.1% 2.3% 3.5% 0.0% 0.0% 0.0% 0.0% 0.0% 19.8% 0.0% 2.3% 7.0% 14.0%

Identification 1 6 2 1 5 2 11 4 1 1 72 1 8 22 4

1.2% 7.0% 2.3% 1.2% 5.8% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 9.3% 25.6% 4.7%


1 49 8 2 6 2 11 4 1 1 72 1 9 24 13

1.2% 57.0% 9.3% 2.3% 7.0% 2.3% 12.8% 4.7% 1.2% 1.2% 83.7% 1.2% 10.5% 27.9% 15.1%


59

Substance: BS-4; Nordazepam

Round: 2015/2







‐1.5 ‐1.44

‐1.1 ‐1.1 ‐1.0

‐0.5 ‐0.5‐0.3 ‐0.2

‐0.1 ‐0.1 ‐0.1 ‐0.1 ‐0.1 0.0

0.2 0.20.4

0.6

1.0 1.0

2.02.1

‐4.0

‐3.0

‐2.0

‐1.0

0.0

1.0

2.0

3.0

4.0

BC7B

AB

KIJ0C1

GF0Z2P

QQVA

UA

BUXM

NK

7Q4A

DS

P2Z5XG

5OLO

5M

VVVIWA

ZEPQ

8E

I6BH

66

5P55

XC

HFC4

CC

SJEV

RS

GELLLL

996M

14

5QGV

32

PPPP

1V

FYOWRE

88RV

B3

J25JY8

QLXQLQ

0ALKWG

3FY8Y9

VFVLEV

L5JCLR

JVU1U

S

UY6AY

Y

UUO

IZR

BWCX

LW

‐5.1 ‐4.8

189156.45.54.5

60

Round: 201


-6

-5

-4

-3

-2

-1

0

1

2

3

4z-

scor

es

Dispersion of z-scores using different analytical techniques for the quantification of Nordazeam in 2015/2 BS-4

GC/MS LC/MSHPLC

61




Concentration

(ng/ml)

Deviation from

robust average

z-score

BC7BAB 200 882 -5.1KIJ0C1 250 832 -4.8GF0Z2P 817 265 -1.5QQVAUA 830 252 -1.4BUXMNK 886 196 -1.17Q4ADS 890 192 -1.1P2Z5XG 900 182 -1.05OLO5M 990 92 -0.5VVVIWA 1000 82 -0.5ZEPQ8E 1037 45 -0.3I6BH66 1047 35 -0.25P55XC 1060 22 -0.1HFC4CC 1060 22 -0.1SJEVRS 1061 21 -0.1GELLLL 1065 17 -0.1996M14 1070 12 -0.15QGV32 1078 4 0.0PPPP1V 1118 37 0.2FYOWRE 1122 41 0.288RVB3 1155 74 0.4J25JY8 1180 99 0.6

QLXQLQ 1248 167 1.00ALKWG 1264 183 1.03FY8Y9 1430 349 2.0VFVLEV 1451 370 2.1L5JCLR 1867 786 4.5JVU1US 2040 959 5.5UY6AYY 2189 1108 6.4UUOIZR 3700 2619 15.0BWCXLW 33990 32909 189.0

Code

Nordazepam

62

The Laboratory and Scientific SectionUNODC, International CentreWagramer Strasse 5, P.O. Box 500A-1400, Vienna, AUSTRIAEmail: [email protected]



63

international quality assurance programme (iqap) … · 2016. 8. 31. · z-scores obtained by...

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