International Quality Assurance Programme (Iqap)

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

BIOLOGICAL SPECIMENS 2014/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 4 NPS reported by ICE participants Page 5 Codes and Abbreviations Page 11 Sample 1 Analysis Page 12 Identified substances Page 12 Statement of findings Page 14 Identification methods Page 18 Summary Page 20 Z-Scores Page 21 Sample 2 Analysis Page 25 Identified substances Page 25 Statement of findings Page 27 Identification methods Page 31 Summary Page 33 Z-Scores Page 34 Sample 3 Analysis Page 38 Identified substances Page 38 Statement of findings Page 40 Identification methods Page 44 Summary Page 46 Z-Scores Page 47 Sample 4 Analysis Page 49 Identified substances Page 49 Statement of findings Page 51 Identification methods Page 55 Summary Page 57 Z-Scores Page 58 Test Samples Information

Samples Comments on samples Sample 1 To prepare BS-1, urine was spiked with aqueous solutions of Cocaine hydrochloride (3450ng base/ml) and Benzoylecgonine hydrate (8060ng base/ml). Methylecgonine (2300ng base/ml) was added as a solution in acetonitrile. The spiked urine was dispensed in 50ml aliquots and lyophilised. Sample 2 To prepare BS-2, urine was spiked with an aqueous solution of Morphine sulphate (170ng base/ml) and ethanolic solutions of Codeine (1160ng base/ml) and 6-Monoacetylmorphine (17320 ng base/ml). The urine was dispensed in 50ml aliquots and lyophilised. Sample 3 7RSUHSDUH%6XULQHZDVVSLNHGZLWKDPHWKDQROLFVROXWLRQRIQRU¨7+&FDUER[\OLFDFLG (230ng/ml). The urine was dispensed in 50ml aliquots and lyophilised.

Sample 4 To prepare BS-4, urine was spiked with an ethanolic solution of 4-Bromo-2,5-dimethoxyphenethylamine (1590ng/ml). The urine was dispensed in 50ml aliquots and lyophilised.

Samples Substances Concentrations Comments on substances Sample 1 Benzoylecgonine 8060 ng/ml Cocaine 3450 ng/ml Methylecgonine 2300 ng/ml Sample 2 6-Monoacetylmorphine (6-MAM) 17320 ng/ml Codeine 1160 ng/ml Morphine (Total) 170 ng/ml Sample 3 QRU¨7+&FDUER[\OLFDFLG 230 ng/ml Sample 4 4-Bromo-2,5-dimethoxyphenethylamine (2C- 1590 ng/ml B)

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. Two rounds are offered per year with each round presenting participants with four different test samples for analysis. 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.

Revision of calculation of z-scores in ICE

Following a recommendation from the International Panel of Forensic Experts and in order to allow ICE participants to interpret their z-scores in line with recommendations in ISO 13528:2005 and ISO/IEC guide 43-1:1997(E), UNODC have introduced an revision to the method used to calculate the z-scores. z-score is a statistical parameter used in proficiency tests and collaborative exercises as a measure of performance in quantitative analysis. They are calculated as:

z = (x-X)/ σ̂ where x = result of participant, X = assigned value of component being quantified and σ̂ is the standard deviation for proficiency assessment (SDPA).

One of the methods recommended in ISO 13528:2005 for determining the assigned value X is to use the consensus value from participants. Using this method, the SDPA is also calculated from the standard deviation of the results of participants. Initial estimates of X and σ known as x* and s* are calculated as:

x* = median of xi (i = 1,2,……p) where p = number of participants s* = 1.483 median of │xi-x*│

Using these estimates, an iterative calculation (for details see ISO13528:2005, Annex C) is carried out to determine the final values of the robust average (x*) and robust standard deviation (s*) and the z-scores are calculated as z = (xi-x*)/s*

Consequently 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. 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

Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2014/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 182 laboratories in 59 countries. Within the SM test group, there were 151 participating laboratories from 57 countries, representing a 16% increase from the 2013/2 round. Within the BS test group, results were submitted by 72 laboratories from 38 countries, also corresponding to an increase of 16 % in the number of participants compared to the previous round.

Qualitative Analysis

The most commonly used technique for screening of test samples in the SM test group was the marquis reagent (42% of participants), while GC-MS (89%) was the most commonly used technique for identification/confirmation followed by FTIR (37%). The results for the qualitative identification of the controlled substances were excellent for all test samples in the SM group. 93% and 98% of participants correctly identified the 1-(3-chlorophenyl)piperazine and metamfetamine in SM-1 and SM-2 respectively. It is encouraging to note that 93% of participants identified the 1-(3-chlorophenyl)piperazine (94% identified this substance in 2013/2), indicating a continued excellent level of awareness of participants in the identification of this New Psychoactive Substance (NPS). 97% of participants correctly identified the ketamine in SM-3, an increase from 92% who correctly identified ketamine, when this was last used as a test sample in 2011/2. Finally, 99% of participants identified the cocaine in SM-4.

8 false positive results were reported for the four test samples in the SM group and there were only 7 false negative results. The detection limits of the different analytical techniques were taken into consideration when ascribing false positive results and as such laboratories who detected the trace amounts of Morphine and Codeine in SM-1 need not consider their results as false positives.

Quantitative Analysis

The proportion of participants who carried out quantitative analysis, 48 (32%) for SM-1, 83 (55%) for SM-2, 69 (46%) for SM-3 and 107 (71%) for SM-4 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-4. 1-(3-chlorophenyl)piperazine is a relatively new substance In the ICE menu and there was a 5% increase in the number of laboratories who performed quantitative analysis for this drug compared to the previous round. It is also encouraging to note that 111 (74%) of participants in the SM test group performed quantitation. Of these, 38% quantified all test samples and 78% of laboratories quantified at least two of the 4 test samples. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 50% used GC-FID, 24% used HPLC and 19% used GC-MS

Analysis of the z-scores showed that 94% of participants provided acceptable quantitative results with |z| < 3 for 1-(3-chlorophenyl)piperazine in SM-1, 89% for metamphetamine in SM-2, 87% for ketamine in SM-3 and 87% for cocaine in SM-4. Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. z-score values obtained assist participating laboratories in evaluating their performance and should be monitored over time as part of each laboratory’s quality assurance programme. Participants with z-scores outside acceptable limits should review their quantification procedures. 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. Participation in the ICE programme also helps in monitoring the effect of corrective actions.

New Psychoactive Substances (NPS) reported by laboratories participating in the 2014/1 round of the ICE programme

During the 2014/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 320 reports of 146 substances. The most commonly reported substances were synthetic cannabinoids followed by synthetic cathinones and phenethylamine group substances as shown in figure 1.

2% 1% 3% 3% 3%

Synthetic cannabinoids 32% Phenethylamines 14% Synthetic cathinones Tryptamines Others Plant-based substances 7% Piperazines Phencyclidine type substances Aminoindanes Unverified

19% 16%

Figure 1. NPS reported by ICE laboratories during the 2014/1 round of ICE

The substances that were most commonly reported by participants are shown in table 1.  25I-NBOMe (1-(4-iodo-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) was the substance most often reported  25C-NBOMe (1-(4-chloro-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) and methylone (2-Methylamino-1-(3,4-methylenedioxyphenyl)propan-1-one) were equally the second most reported substances  The synthetic cannabinoids, APINACA (1-pentyl-N-tricyclo[3.3.1.13,7]dec-1-yl-1H-indazole-3- carboxamide) and MAM-2201 ([1-(5-Fluoropentyl)-1H-indol-3-yl](4-methyl-1-naphthalenyl)- methanone) completed the list.

Table 1. Substances most commonly reported by ICE participants in 2014/1 round of ICE

Substance IUPAC Name Structure

2-(4-Iodo-2,5-dimethoxyphenyl)-N-(2- 25I-NBOMe methoxybenzyl)ethanamine

2-(4-Chloro-2,5-dimethoxyphenyl)-N- 25C- (2-methoxybenzyl)ethanamine NBOMe

1-(1,3-Benzodioxol-5-yl)-2- Methylone (methylamino)propan-1-one

1-Pentyl-N-(tricyclo[3.3.1.13,7]dec-2-yl)- 1H-indazole-3-carboxamide - 1-(1,3- APINACA benzodioxol-5-yl)-2- (methylamino)propan-1-one (1:1)

[1-(5-Fluoropentyl)-1H-indol-3-yl](4- MAM-2201 methylnaphthalen-1-yl)methanone

Table 2 shows the namesand structures of the NPS that were reported for the first time to UNODC during the 2014/1 round of ICE.

Table 2. Substances reported to UNODC for the first time by ICE participants in 2014/1 round of ICE

Common name/ IUPAC name Structure Abbreviation

Methoxphenidine, 1-(1-(2-methoxyphenyl)-2- MXP phenylethyl)piperidine

2-(methylamino)-1-(thiophen-2- bk-MPA yl)propan-1-one

methyl 1-(2-phenylethyl)-4- [phenyl(propanoyl)amino]piperidi Carfentanyl ne-4-carboxylate

7-chloro-5-(2-chlorophenyl)-1- methyl-1,3-dihydro-2H-1,4- Diclazepam benzodiazepin-2-one

8-bromo-1-methyl-6-(pyridin-2- Pyrazolam yl)-4H-[1,2,4]triazolo[4,3- a][1,4]benzodiazepine

2- 1-(2-fluorophenyl)-N- Fluoromethamph methylpropan-2-amine etamine, 2-FMA

7 naphthalen-1-yl(1-pentyl-1H- THJ-018 indazol-3-yl)methanone

methyl N-{[1-(5-fluoropentyl)-1H- 5F-AMB indazol-3-yl]carbonyl}valinate

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1- AB-CHMINACA (cyclohexylmethyl)-1H-indazole- 3-carboxamide

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1-(2- AB-FUBINACA(2- fluorobenzyl)-1H-indazole-3- fluorobenzyl) carboxamide

quinolin-8-yl-1-(4-fluorobenzyl)- FUB-PB-22 1H-indole-3-carboxylate

8 (4-methylpiperazin-1-yl)(1- Mepirapim, pentyl-1H-indol-3-yl)methanone

N-(2-methoxyethyl)-N-{[2-(1- pentyl-1H-indol-3-yl)-1,3-thiazol- PTI-2 4-yl]methyl}propan-2-amine

N-ethyl-N-{[2-(1-pentyl-1H-indol- 3-yl)-1,3-thiazol-4- PTI-1 yl]methyl}ethanamine

1-(5-fluoropentyl)-N- (naphthalen-1-yl)-1H-indazole-3- 5F-NNE1 carboxamide

[1-(5-fluoropentyl)-1H-indazol-3- THJ-2201 yl](naphthalen-1-yl)methanone

9 α- 1-phenyl-2-(pyrrolidin-1- pyrrolidinoheptiop yl)heptan-1-one henone, alpha-

PHpP

1-(3-methylphenyl)-2-(pyrrolidin- 3-MePPP 1-yl)propan-1-one

2-(ethylamino)-1-phenylpentan- 1-one

2-MMC, 2-Methyl- 2-(methylamino)-1-(2- N- methylphenyl)propan-1-one, methylcathinone

3,4- 1-(3,4-dimethylphenyl)-2- Dimethylethcathin (ethylamino)propan-1-one one

2-(ethylamino)-1-(4- methylphenyl)pentan-1-one

2-amino-1-(4-bromo-2,5- bk-2C-B dimethoxyphenyl)ethanone

2-(1H-indol-3-yl)-N- N- methylethanamine methyltryptamine

All laboratories participating in the UNODC International Collaborative Exercises can access the UNODC Early Warning Advisory on New Psychoactive Substances by logging on to their account and selecting the link as shown in the image below

11 Introduction

Revision of calculation of z-scores in ICE

z = (x-X)/ σ̂ where x = result of participant, X = assigned value of component being quantified and σ̂ is the standard deviation for proficiency assessment (SDPA).

x* = median of xi (i = 1,2,……p) where p = number of participants s* = 1.483 median of │xi-x*│

Consequently 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

12 Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2014/1 round of the ICE programme, results were submitted within both the Seized materials (SM) and Biological Specimens (BS) test groups by 182 laboratories in 59 countries. Within the SM test group, there were 151 participating laboratories from 57 countries, representing a 16% increase from the 2013/2 round. Within the BS test group, results were submitted by 72 laboratories from 38 countries, also corresponding to an increase of 16 % in the number of participants compared to the previous round.

Qualitative analysis

Overall, the level of performance in identification of the test samples was good given the inherently higher level of difficulty in the analysis of biological specimens compared to seized materials due to their low concentration and multi-component composition. The complexity of the test samples in ICE 2014/1 was designed in order to challenge the participants. Overall, within the BS test group, the most common technique used by participants for the screening of test samples were enzyme immunoassay techniques (56% of labs), while GC/MS was used by 85% of participants for identification followed by LC/MS which was used by 18% of participating laboratories. BS-1 contained cocaine and the two metabolites, benzoylecgonine and methylecgonine, which were identified by 86%, 79% and 65% of participants respectively. There was only one false positive result and while there were 15 false negatives and a total of 35 analyses not performed, it is recognised that some laboratories identify the use of cocaine based solely on identification of the parent drug or one of its metabolites. BS-2 also contained multiple components and the morphine, codeine and 6- monoacetylmorphine present were identified by 86%, 85% and 86% of participants respectively. In this test sample 4 false positives for morphine-glucuronides were reported and there were 13 false negative results and 19 analyses not performed. The 11-nor-delta9-THC-9-carboxylic acid in BS-3 was identified by 89% of participants. There were no false positive results, only one false negative result and seven laboratories did not carry out analysis for 11-nor-delta9-THC-9-carboxylic acid in this test sample. For the second round in succession, 2C-B, a newly introduced substance in the biological specimens ICE menu was included as a test sample. The 2C-B was identified by 49 % of participants, a figure comparable to the 50% who identified this substance in the 2013/2 round of ICE. There were no false positive results reported, seven false negatives and 30 laboratories did not carry out analysis for 2C-B in this test sample.

Quantitative analysis

The four test samples in the BS test group for the 2014/1 round of ICE contained a total of 8 components. 31 (43%) of participating laboratories performed quantitation. Of these laboratories, 78 % quantified at least two components and 16% quantified all the components in the test samples. GC-MS was used by 65% of participants for quantification followed by LC/MS which was used by 22% of participants. The results for quantitative analysis within the BS test group were excellent. For BS-1, 92% of laboratories obtained acceptable quantitative results with |z| <3 for methylecgonine. Acceptable z-scores were obtained for benzoylecgonine and cocaine by 95% and 81% of laboratories respectively. Within BS-2, 100% of labs who quantified 6-monoacetylmorphine, 92% who quantified codeine and 75% who quantified the morphine obtained acceptable z-scores. 96% of labs obtained acceptable z-scores for the 11-nor-delta9-THC-9- carboxylic acid in BS-3 and while only 9 labs quantified the 2C-B in BS-4, 100% obtained acceptable z- scores. The results of ICE participants for the quantitative analysis of the morphine present in BS-2 show considerable variability. This could in part be explained by the pH dependent hydrolysis of some of the 6-MAM also present in the test sample during the course of analyte extraction/enrichment. UNODC are investigating this issue, will contact ICE participants and provide feedback in due course.

Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. z-score values obtained assist participating laboratories in evaluating their performance and should be monitored over time as part of each laboratory’s quality assurance programme. Participants with Z-scores outside acceptable limits should review their quantification procedures. 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. Participation in the ICE programme also helps in monitoring the effect of corrective actions.

New Psychoactive Substances (NPS) reported by laboratories participating in the 2014/1 round of the ICE programme

2% 1% 3% 3% 3%

Synthetic cannabinoids 32% Phenethylamines 14% Synthetic cathinones Tryptamines Others Plant-based substances 7% Piperazines Phencyclidine type substances Aminoindanes Unverified

19% 16%

Figure 1. NPS reported by ICE laboratories during the 2014/1 round of ICE

The substances that were most commonly reported by participants are shown in table 1.  25I-NBOMe (1-(4-iodo-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) was the substance most often reported  25C-NBOMe (1-(4-bromo-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) and methylone (2-Methylamino-1-(3,4-methylenedioxyphenyl)propan-1-one) were equally the second most reported substances  The synthetic cannabinoids, APINACA (1-pentyl-N-tricyclo[3.3.1.13,7]dec-1-yl-1H-indazole-3- carboxamide) and MAM-2201 ([1-(5-Fluoropentyl)-1H-indol-3-yl](4-methyl-1-naphthalenyl)- methanone) completed the list.

Table 1. Substances most commonly reported by ICE participants in 2014/1 round of ICE

Substance IUPAC Name Structure

2-(4-Iodo-2,5-dimethoxyphenyl)-N-(2- 25I-NBOMe methoxybenzyl)ethanamine

2-(4-Chloro-2,5-dimethoxyphenyl)-N- 25C- (2-methoxybenzyl)ethanamine NBOMe

1-(1,3-Benzodioxol-5-yl)-2- Methylone (methylamino)propan-1-one

1-Pentyl-N-(tricyclo[3.3.1.13,7]dec-2-yl)- 1H-indazole-3-carboxamide - 1-(1,3- APINACA benzodioxol-5-yl)-2- (methylamino)propan-1-one (1:1)

[1-(5-Fluoropentyl)-1H-indol-3-yl](4- MAM-2201 methylnaphthalen-1-yl)methanone

15 Table 2 shows the names and structures of the NPS that were reported for the first time to UNODC during the 2014/1 round of ICE.

Table 2. Substances reported to UNODC for the first time by ICE participants in 2014/1 round of ICE

Common name/ IUPAC name Structure Abbreviation

Methoxphenidine, 1-(1-(2-methoxyphenyl)-2- MXP phenylethyl)piperidine

2-(methylamino)-1-(thiophen-2- bk-MPA yl)propan-1-one

methyl 1-(2-phenylethyl)-4- [phenyl(propanoyl)amino]piperidi Carfentanyl ne-4-carboxylate

7-chloro-5-(2-chlorophenyl)-1- methyl-1,3-dihydro-2H-1,4- Diclazepam benzodiazepin-2-one

8-bromo-1-methyl-6-(pyridin-2- Pyrazolam yl)-4H-[1,2,4]triazolo[4,3- a][1,4]benzodiazepine

2- 1-(2-fluorophenyl)-N- Fluoromethamph methylpropan-2-amine etamine, 2-FMA

naphthalen-1-yl(1-pentyl-1H- THJ-018 indazol-3-yl)methanone

16 methyl N-{[1-(5-fluoropentyl)-1H- 5F-AMB indazol-3-yl]carbonyl}valinate

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1- AB-CHMINACA (cyclohexylmethyl)-1H-indazole- 3-carboxamide

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1-(2- AB-FUBINACA(2- fluorobenzyl)-1H-indazole-3- fluorobenzyl) carboxamide

quinolin-8-yl-1-(4-fluorobenzyl)- FUB-PB-22 1H-indole-3-carboxylate

(4-methylpiperazin-1-yl)(1- Mepirapim, pentyl-1H-indol-3-yl)methanone

17 N-(2-methoxyethyl)-N-{[2-(1- pentyl-1H-indol-3-yl)-1,3-thiazol- PTI-2 4-yl]methyl}propan-2-amine

N-ethyl-N-{[2-(1-pentyl-1H-indol- 3-yl)-1,3-thiazol-4- PTI-1 yl]methyl}ethanamine

1-(5-fluoropentyl)-N- (naphthalen-1-yl)-1H-indazole-3- 5F-NNE1 carboxamide

[1-(5-fluoropentyl)-1H-indazol-3- THJ-2201 yl](naphthalen-1-yl)methanone

α- 1-phenyl-2-(pyrrolidin-1- pyrrolidinoheptiop yl)heptan-1-one henone, alpha-

PHpP

1-(3-methylphenyl)-2-(pyrrolidin- 3-MePPP 1-yl)propan-1-one

18 2-(ethylamino)-1-phenylpentan- 1-one

2-MMC, 2-Methyl- 2-(methylamino)-1-(2- N- methylphenyl)propan-1-one, methylcathinone

3,4- 1-(3,4-dimethylphenyl)-2- Dimethylethcathin (ethylamino)propan-1-one one

2-(ethylamino)-1-(4- methylphenyl)pentan-1-one

2-amino-1-(4-bromo-2,5- bk-2C-B dimethoxyphenyl)ethanone

2-(1H-indol-3-yl)-N- N- methylethanamine methyltryptamine

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

Codes and Abbreviations

(+) “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.

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

Sample 1 Analysis

Identified substances for Test Sample 1

Code Identified Substances 0JDQRT Cocaine and benzoilecgonine 11L1F1 Methylecgonine 1NHAHH COCAINE AND BENZOYLECGONINE METABOLITES 1RTHUB Benzoylecgonine 1SE4LC cocaine, benzoylecgonine, methylecgonine 2ACHJY COCAINA BENZOILECGONINA METILECGONINA 2WKWWU Benzoylecgonine, Methylecgonine,Cocaine 3KYD8K Benzoylecgonine, Cocaine, Methylecgonine 3NUFZQ Benzoylecognine 5MIQ5K Cocaína/metabolito 6JPGEG cocaine, benzoylecgonine, methylecgonine 7SLBJ5 cocaine, methylecgonine 8EJHSP Cocaine, Benzoyl ecgonine, méthyl ecgonine 9KCFVW Benzoylecgonine and methylecgonine 9YKLH6 cocaine and metabolites A4WEB4 benzoylecgonine and cocaine AQUCAA Cocaine and methylecgonine B6S6UH Cocaine, benzoyl ecgonine BZBECD Methyl ecgonine and cocaine CNHIT2 Cocaine and benzoylecgonine CRAICM Cocaine and/or its metabolites DG9DD6 Cocaine and metabolites DOK333 COCAINE DPK69B benzoilecgonine and cocaine DSLONZ cocaine and metabolites DTNZDN Cocaine and metabolites, benzoylecgonine and methylecgonine E3AATH Methylecgonine, cocaine, benzoilecgonine FHDI00 Cocaine FS47ZT cocaine, benzylecgonine FSSA3M cocaïne and metabolites GFGG5J cocaine, BE GLLLLQ methylecgonine, benzoylecgonine, cocaine GXW2Q2 COCAINE AND METABOLITES HFFKMX Benzoylecgonine, Cocaine , Methylecgonine IIRIR8 Cocaine ,Benzoylecgonine ,Methylecgonine KKHEMK Cocaine and metabolites KV7QCV cocaine LGPKEB cocaine and Benzoylecgonine LNEUXP Cocaine, BEG MCUQ4O cocaine, benzoylegconine, ecgonine methyl ester

Code Identified Substances MNURNG cocaine, benzoylecgonine, methylecgonine MX7EK9 cocaine NQMMS5 Benzoylecgonine,Cocaine,Methylecgonine OYUAUJ Cocaine QIIMQZ Cocaine and or metabolites QJH28U Cocaine, Benzoylecgonine, Methylecgonine. R9TZTO Benzoylecgonine, Cocaine, Methylecgonine RFJ8SV BEG-COC-MEG S4Z1YG benzoilecgonine SHUSPS Benzoylecgonine, Cocaine Methylecgonine TTZTHH Benzoylecgonine TZRY6I cocainem Benzoylecgonine, Methylecgonine U9T99A Cocaine, Benzoylecgonine and Methylecgonine UJUUJR Cocaine, Benzoyl Ecgonine, Methyl Ecgonine, Caffeine VEYSDV Benzolylecgonine, Cocaine. VVVIVC Cocaine and metabolites W2SWWW Cocaine, Methylecgonine WKG8OD cocaine and it's metabolits Benzoylecgonine and methyl ecgonine WLWPCL Cocaine XPJJCF Cocaine,benzoylecgonine, methylecgonine XRGZII Cocaine, Benzoylecgonine, Methylecgonine. XSHEX7 COCAINE and/or METABOLITES YEYYWY Cocaine, benzoylecgonine, methylecgonine, cocaethilene YYMBZQ COCAINE ZBO09R COCAINE, BENZOYLECGONINE, METHYLECGONINE ZUYDSS Cocaine, BZE ZZYFHY Cocaine, Benzoylecgonine and Methylecgonine

Statement of findings for Test Sample 1

Code Benzoylecgonine Cocaine Methylecgonine 0JDQRT + + ANP In the urine sample cocaine and its metabolite benzoilecgonine were found. 11L1F1 - - +

1NHAHH + + + THE SAMPKLE No. 2014/1/BS-1 WAS FOUND COCAINE AND BENZOYLECGONINE METABOLITES 1RTHUB + ANP ANP Sample 2014/1/BS1 contains Benzoylecgonine therefore positive for both screening and confirmatory tests. 1SE4LC + + + This person consumed cocaine. 2ACHJY + + + HUBO CONSUMO DE COCAINA 2WKWWU + + + Cocaine, Benzoylecgonine and Methylecgonine indicate that cocaine was consumed.

3KYD8K + + + Screening by immunoassay technique : Positive Confirm by GC-MS : Positive 3NUFZQ + ANP ANP The person who provided the specimen has consumed cocaine. 5MIQ5K ANP ANP ANP Positivo 6JPGEG + + + Use of cocaine. 7SLBJ5 ANP + + use of cocaine 8EJHSP + + + Prise de Cocaine 9KCFVW + ANP + In urine sample number one was identified benzoylecgonine and methylecgonine. Cocaine wasn't researched. 9YKLH6 + + + The urine analyzed contains cocaine and metabolites of cocaine. These results indicate a cocaine absorption. A4WEB4 + + - Analytical Adverse Finding for benzoylecgonine and cocaine in the sample. AQUCAA - + + Cocaine and methylecgonine detected. B6S6UH + + ANP Cocaine abuse. BD3BFB + + +

BKPN2U + + ANP

BZBECD ANP + + Methyl ecgonine and cocaine detected in BS-1.

Code Benzoylecgonine Cocaine Methylecgonine CNHIT2 + + - In the sample labeled round ICE 2014-1 sample BS-1 cocaine and benzoylecgonine was detected CRAICM ANP ANP ANP The reported analytical findings detected the presence of cocaine and/or its metabolites in the urine same, BS-1. This analytical finding is the result of primary screening and additional confirmatory tests should be performed. DG9DD6 + + + Cocaine, Benzoylecgonine, Methylecgonine DOK333 - + - Extraction of sample and TLC analysis using two solvent systems and HPLC confirmed the sample as COCAINE with concentration or purity as 6500ng/ml. DPK69B + + ANP

DSLONZ + + + The presence of cocaine in urine indicates early cocaine comsuption. After a single dose cocaine can be found in urine within the next 24 hours, methylecgonine and benzoilecgonine could be found within the next 48 hours. DTNZDN + + + Cocaine is a controlled narcotic in France. Cocaine is a strong CNS stimulant and local anesthesic. E3AATH + + + 1. Results of screening test were positive for cocaine and metabolites. 2. Retention time and fragmentation pattern obtained with the biological sample are equivalent to those obtained with "Methylecgonine, cocaine and benzoilecgonine" (Reference material). FHDI00 ANP + ANP On analysis, the sample of 2014/1/BS-1 found to contain Cocaine FS47ZT + + +

FSSA3M + + +

GFGG5J + + ANP

GLLLLQ + + + Use of cocaine GXW2Q2 + + + POSITIVE HFFKMX + + +

IIRIR8 + + + quantification not performed KKHEMK + + + Previous use of cocaine KV7QCV + + + sample contains cocaine LGPKEB + + ANP positive to cocaine consumption LNEUXP + + ANP Positive for Cocaine and BEG MCUQ4O + + +

Code Benzoylecgonine Cocaine Methylecgonine MNURNG + + + consuption of cocaine MX7EK9 + + - after chemical analysis was performed, the sample was found to contain cocaine and its metabolites ( 18.9 ng/ml of cocaine and benzoylecgonine). NQMMS5 + + + - OTJOOE + + +

OYUAUJ - + - Samples also contains Cafeine Q99KOM + + ANP

QIIMQZ - + - Cocaine QJH28U + + + The coincidence between the retention times and mass fragmentograms from a reference material analysed in the same conditions that the biological sample indicates the presence of Cocaine, Benzoylecgonine and Methylecgonine. R9TZTO + + + Sample is positive for Cocaine, Benzoylecgonine and Methylecgonine RFJ8SV + + + It is frecuntly susbstance found in cocaine consumer RY5KEY ANP ANP ANP

S4Z1YG + ANP ANP Sample cntain cocaine metabolite-benzoilecgonine.Cocaine user. SHUSPS + + +

TTZTHH + ANP ANP Benzoylecgonine TZRY6I + + +

U9T99A + + + The sample contains cocaine, benzoylecgonine and methylecgonine. UJUUJR + + + Toxicological examination of sample BS-1 revealed the presence of Cocaine, Benzoyl Ecgonine and Methyl Ecgonine. VEYSDV + + ANP In the urine sample analyzed was detected and confirmated the presence of Benzolylecgonine, Cocaine. VVVIVC + + + Recent cocaine consumption W2SWWW ANP + + Cocaine and Methylecgonine were detected in the sample WKG8OD + + + sample spiked with cocaine and it's major metabolites BZE and ME WLWPCL - + - Cocaine was identified by GC/MS

Code Benzoylecgonine Cocaine Methylecgonine XPJJCF + + +

XRGZII + + +

XSHEX7 + + + Methylecgonine -Cocaine -Benzoylecgonine YEYYWY + + + Cocaine consumption, possibly together with alcohol. YYMBZQ - + +

ZBO09R + + + Screening test positive cocaine and/or metabolites. CG-MS retention time and relation mass (m/z) the reference material cocaine, benzoylecgonine and methylecgonine are equivalente sample 2014/1/BS-1 ZUYDSS ANP ANP ANP

ZZYFHY + + +

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 100 110 120 150 160 161 170 171 180 230 231 210 0JDQRT S I SI 11L1F1 I I 1NHAHH SI I 1RTHUB I I S Drug Test Kit 1SE4LC S I I 2ACHJY S I S Randox 2WKWW S I S Lateral Flow Immunoassay U 3KYD8K S SI 3NUFZQ S I 5MIQ5K S 6JPGEG S I I SI I 7SLBJ5 S I 8EJHSP S I 9KCFVW S I 9YKLH6 S I A4WEB4 SI I S AQUCAA S I B6S6UH S I I I S BD3BFB S I BKPN2U SI BZBECD S I CNHIT2 S I CRAICM S S DG9DD6 S SI DOK333 SI I S Test strips DPK69B I DSLONZ S I I DTNZDN S I I E3AATH S I FHDI00 I SI FS47ZT S I I FSSA3M S I I GFGG5J S I SI I GLLLLQ S I

Code 100 110 120 150 160 161 170 171 180 230 231 210 GXW2Q2 I SI I HFFKMX I SI SI IIRIR8 SI KKHEMK S I KV7QCV S I I LGPKEB SI LNEUXP S I MCUQ4O I SI SI MNURNG S S I S biochip technology-Randox MX7EK9 S I NQMMS5 SI OTJOOE SI S test panel OYUAUJ SI I Q99KOM SI QIIMQZ I SI Diprodruglab screen QJH28U S I R9TZTO S SI I S LC-TOF RFJ8SV S I I RY5KEY SI S4Z1YG SI I SHUSPS SI I TTZTHH S S I I I Orbitrap TZRY6I S I U9T99A SI S Multi-Drug Screen Test Panel UJUUJR S SI I VEYSDV S I VVVIVC S I I W2SWW S I W WKG8OD S I I WLWPCL S I XPJJCF I XRGZII S I I I XSHEX7 SI S KIMS YEYYWY S I I YYMBZQ S I ZBO09R S I ZZYFHY S I I

Summary for test sample 1 The response summary of all 72 participating laboratories for the identification of BS-1, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 1:

Response Summary

Participants: 72

Benzoylecgonine: 57 Cocaine: 62 Methylecgonine: 47

False positives for Test Sample 1

Code Name Technique HFFKMX Codeine 230/231

False negatives and analysis not performed for BS-1

Benzoylecgonine: 7 false negatives and 8 analysis not performed

Cocaine: 1 false negative and 9 analysis not performed

Methylecgonine: 7 false negatives and 18 analysis not performed

Frequency of use of screening and identification techniques: Response Summary Participants: Response 130 Summary Participants: 72 141 142 Section 100 110 120 150 160 161 170 171 180 230 231 210 Screening 3 40 8 4 0 0 1 0 16 3 5 10 4.2% 55.6% 11.1% 5.6% 0.0% 0.0% 1.4% 0.0% 22.2% 4.2% 6.9% 13.9% Identification 0 4 1 6 3 9 2 1 61 8 13 2 0.0% 5.6% 1.4% 8.3% 4.2% 12.5% 2.8% 1.4% 84.7% 11.1% 18.1% 2.8% # labs using 3 40 9 8 3 9 3 1 61 8 15 11 this technique 4.2% 55.6% 12.5% 11.1% 4.2% 12.5% 4.2% 1.4% 84.7% 11.1% 20.8% 15.3% 29 2014/1-BS Copyright (c) 2014 UNODC

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

Z-Scores for Test Sample 1

Benzoylecgonine Cocaine Methylecgonine Deviation Deviation Deviation Code Concentration Concentration Concentration from from robust z-score from robust z-score z-score (ng/ml) (ng/ml) (ng/ml) robust average average average 1RTHUB 8557 906 0.5 - -- - - 1SE4LC 8619 968 0.6 2765 -675 -0.7 1767 -242 -0.4 2ACHJY 9887 2236 1.3 4708 1268 1.8 3693 1684 2.7 3NUFZQ 8917 1266 0.7 ------7SLBJ5 ------2337 328 0.5 8EJHSP 5550 -2101 -1.2 ------9YKLH6 7922 271 0.2 2959 -481 -0.5 1891 -118 -0.2 B6S6UH 6910 -741 -0.4 2980 -460 -0.4 - -- DOK333 6500 3060 4.1 - -- DTNZDN 8826 1175 0.7 4440 1000 1.4 2722 713 1.1 GFGG5J 3934 -3717 -2.2 3727 287 0.5 - -- GLLLLQ 160 -7491 -4.4 8740 5300 7 100 -1909 -3.0 HFFKMX 6274 -1377 -0.8 4557 1117 1.6 2049 40 0.1 KV7QCV 9400 1749 1 3300 -140 0 1700 -309 -0.5 LGPKEB 7480 -171 -0.1 3428 -12 0.1 - -- LNEUXP 9400 1749 1 3500 60 0.2 - -- MX7EK9 - -- 19 -3421 -4.2 - -- NQMMS5 7500 -151 -0.1 3100 -340 -0.3 2050 41 0.1 OYUAUJ - - - 3725 285 0.5 - -- Q99KOM 7377 -274 -0.2 - - - 3736 1727 2.7 R9TZTO 7390 -261 -0.2 3665 225 0.4 2117 108 0.2 TTZTHH 8540 889 0.5 ------VVVIVC 5277 -2374 -1.4 2323 -1117 -1.3 - -- XPJJCF 8601 950 0.6 1830 -1610 -1.9 512 -1497 -2.4 YEYYWY 6500 -1151 -0.7 2900 -540 -0.5 - -- ZUYDSS 9143 1492 0.9 3070 -370 -0.3 - -- ZZYFHY ------1290 -719 -1.1

Robust average = 7651 Round: 2014/1 UNODC value = 8060 Substance: BS-1/Benzoylecgonine 4.0

3.0

2.0

1.3 1.0 1.0 0.9 1.0 0.7 0.7 0.5 0.5 0.6 0.6 0.2 ‐4.4 0.0 ‐0.2 ‐0.2 ‐0.1 ‐0.1 ‐0.4 ‐0.7 ‐1.0 ‐0.8 ‐1.2 ‐1.4 ‐2.0

‐2.2

‐3.0

‐4.0 XPJJCF 1SE4LC 8EJHSP GLLLLQ 2ACHJY VVVIVC 9YKLH6 LGPKEB ZUYDSS R9TZTO TTZTHH GFGG5J LNEUXP B6S6UH YEYYWY 1RTHUB KV7QCV 3NUFZQ HFFKMX DTNZDN Q99KOM NQMMS5 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

31 Z-Score Report per Sample per Substance

Round: 2014/1 Robust average = 3440 UNODC value = 3450 Substance: BS-1/Cocaine

4.0

3.0

2.0 1.8 1.6 1.4

1.0 0.4 0.5 0.5 0.1 0.2 ‐4.3 ‐4.2 0.0 0.0 4.1 7.0 ‐0.3 ‐0.3 ‐0.5 ‐0.5 ‐0.4 ‐1.0 ‐0.7

‐1.3

‐2.0 ‐1.9

‐3.0

‐4.0 XPJJCF 1SE4LC GLLLLQ 2ACHJY VVVIVC 9YKLH6 LGPKEB ZUYDSS R9TZTO GFGG5J LNEUXP B6S6UH DOK333 YEYYWY OYUAUJ KV7QCV MX7EK9 HFFKMX DTNZDN YYMBZQ NQMMS5

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

32 Z-Score Report per Sample per Substance

Round: 2014/1 Robust average = 2009 UNODC value = 2300 Substance: BS-1/Methylecgonine

4.0

3.0 2.7 2.7

2.0

1.1 1.0 0.5 0.2 0.1 0.1 0.0

‐0.2 ‐0.5 ‐0.4 ‐1.0 ‐1.1

‐2.0

‐2.4 ‐3.0 ‐3.0

‐4.0 XPJJCF 7SLBJ5 1SE4LC GLLLLQ ZZYFHY 2ACHJY 9YKLH6 R9TZTO KV7QCV HFFKMX DTNZDN Q99KOM NQMMS5

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

Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 0JDQRT Morphine, 6-Acetylmorphine and codeine. 11L1F1 6-MAM, total morphine 1NHAHH OPIATES 6 ACETYLMORPHINE 1RTHUB Morphine and Codeine 1SE4LC 6-MAM, codeine, morphine 2ACHJY MORFINA CODEINA 6 MAM 2WKWWU Codeine, Morphine, 6-MAM 3KYD8K 6-MAM, Codeine, Morphine 3NUFZQ Codeine, monoacetylmorphine, diamorphine (heroin). 5MIQ5K Opiáceos 6JPGEG Morphine, codeine, 6-MAM 7SLBJ5 codeine, morphine, 6-MAM, heroin 8EJHSP Morphine, Codéine, 6 MAM 9KCFVW Codeine and 6-monoacetyl-morphine 9YKLH6 6-MAM, morphine, codeine A4WEB4 morphine AQUCAA Morphine, codeine and 6-MAM B6S6UH Morphine, codeine, 6-MAM BZBECD Codeine, Morphine and 6-Monoacetylmorphine (6-MAM) CNHIT2 Codeine, morphine and 6-monoacetylmorphine CRAICM Opiates and/or its metabolites DG9DD6 OPIATES DOK333 HEROIN DPK69B codeine, heroine, MAM, morphine DSLONZ Codeine, 6 monoacetilmorfine and morfine DTNZDN Morphine, Codein, 6 MAM E3AATH Morphine, codeine, 6-MAM FHDI00 Codeine, Morphine and 6-Monoacetylmorphine FS47ZT morphine, codeine, 6-monoacetylmorphine FSSA3M 6MAM, codeine and morphine GFGG5J 6-MAM, codeine, morphine GLLLLQ 6-MAM, codeine, morphine GXW2Q2 MORPHINE AND METABOLITES HFFKMX 6-Monoacetylmorphine, Codeine, Morphine IIRIR8 6-Monoacetylmorphine (6-MAM) , Morphine ,Codeine ) KKHEMK 6-monacetylmorphine, codeine and morphine KV7QCV morphine, codeine, 6-mam LGPKEB opiates, 6MAM, codeine and morphine LNEUXP Morphine, codeine, 6-AM MNURNG codeine, morphine, 6-MAM

Code Identified Substances MX7EK9 opiates NQMMS5 6-Monoacetylmorphine,Codeine,Morphine OYUAUJ Codeine, Morphine QIIMQZ Opiates QJH28U Morphine, Codeine, 6-Monoacetylmorphine. R9TZTO Codeine, Morphine,6-Monoacetylmorphine RFJ8SV Codeina-6-MAM RY5KEY Opiates Drug S4Z1YG morphine, 6-MAM SHUSPS Codeine, 6-Monoacetylmorphine (6-MAM), Morphine TTZTHH Codeine, Morphine(Total),6-Monoacetylmorphine TZRY6I morphine,codeine, 6-MAM U9T99A 6-Monoacetylmorphine, Morphine and Codeine UJUUJR 6-monoacetylmorphine, codeine, morphine and caffeine VEYSDV 6-Monoacetylmorphine, Morphine Total, Codeine VVVIVC Opiates W2SWWW Morphine, Codeine, 6-Monoacetylmorphine (6-MAM) WKG8OD MORPHINE, 6-MAM and CODEINE WLWPCL 6-MAM, Codeine, Morphine XPJJCF morphine, 6-monoacetylmorphine, codeine XRGZII 6-Monoacetylmorphine (6-MAM), Codeine, Morphine total XSHEX7 OPIATES/OPIOIDS YEYYWY 6-MAM, morphine, codeine YYMBZQ OPIATES ZBO09R MORPHINE, CODEINE,6-MONOACETYLMORPHINE ZUYDSS Codeine, Morphine, 6-MAM ZZYFHY Heroin metabolites (6-Monoacetylmorphine (6-MAM) and free Morphine) and Codeine

Statement of findings for Test Sample 2

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) 0JDQRT + + + In the urine sample morphine, 6-Acetylmorphine and codeine were found. 11L1F1 + - +

1NHAHH + + - THE SAMPLE No.2014/1/BS-2 WAS FOUND 6 ACETYLMORPHINE 1RTHUB ANP + + Sample 2014/1/BS2 contains Morphine and Codeine therefore positive for both screening and confirmatory tests. 1SE4LC + + + This person consumed heroin. 2ACHJY + + + HUBO CONSUMO DE MORFINA Y CODEINA 2WKWWU + + + Codeine was consumed, Morphine indicates an opiate was consumed and 6-MAM marker of Heroin indicate this opiate was consumed. 3KYD8K + + + Screening by immunoassay technique : Positive Confirm by GC-MS : Positive 3NUFZQ + + ANP The person who provided the specimen has consumed heroin. 5MIQ5K ANP ANP ANP Positivo 6JPGEG + + + Use of heroin. 7SLBJ5 + + + use of heroin 8EJHSP + + + recent taking of heroin with codeine (Illicit heroin often contains small amounts of codeine)

9KCFVW + + - In urine sample number two was identified Codeine and 6-monoacetyl-morphine. 9YKLH6 + + + The urine analyzed contains 6-MAM, morphine and codeine. 6-MAM indicates a heroin absorption. A4WEB4 - - + Analytical Adverse Finding for morphine in the sample. Metabolits were present in a very small amount i.e. < Limit of Detection. AQUCAA + + + Morphine, codeine and 6-MAM detected. B6S6UH + + + Heroine abuse. BD3BFB + + +

BKPN2U ANP ANP ANP

BZBECD + + + Codeine, Morphine and 6-Monoacetylmorphine (6-MAM) detected in BS-2.

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) CNHIT2 + + + In the sample labeled round ICE 2014-1 sample BS-2 Codeine, morphine and 6- monoacetylmorphine was detected CRAICM ANP ANP ANP The reported analytical findings detected the presence of opiates and/or its metabolites in the urine same, BS-2. This analytical finding is the result of primary screening and additional confirmatory tests should be performed. DG9DD6 + + + Codeine, 6-Monoacetylmorphine (6-MAM), Morphine DOK333 - - - Extraction of sample and TLC analysis using two solvent systems and HPLC confirmed the sample as HEROIN with concentration or purity as 161000 ng/ml. DPK69B + + +

DSLONZ + + + The presence of 6 monoacetylmorfine in urine indicates heroin comsuption. Morfine could come from the heroin intake or come from the comsuption of the individual agents per se. Codeine could come as a heroin impurity or from the intake of the drug itself. DTNZDN + + + The presence of 6MAM is a conclusive evidence of prior heroin use. Heroin is metabolized to morphine. heroin undergoes rapid deacetylation to 6 MAM, 6MAM is further deacetylated to morphine. Heroin is a controlled narcotic in France E3AATH + + + 1. Results of screening test were positive for opiates and metabolites. 2. Retention time and fragmentation pattern obtained with the biological sample are equivalent to those obtained with "Morphine, codeine and 6-MAM" (Reference material). FHDI00 + + + On analysis, the sample of 2014/1/BS-2 found to contain Codeine, Morphine and 6- Monoacetylmorphine FS47ZT + + +

FSSA3M + + +

GFGG5J + + +

GLLLLQ + + + Use of heroine GXW2Q2 + + + POSITIVE HFFKMX + - +

IIRIR8 + + + quantification not performed KKHEMK + + + Consistent with previous use of heroin KV7QCV + + + saple contains morphine and 6 mam , and codeine LGPKEB + + + positive to heroin consumption

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) LNEUXP + + + Positive for morphine, codeine, 6-acetylmorphine MCUQ4O + + + Morphine, codeine, 6-monoacetylmorphine MNURNG + + + consuption of diacetylmorphine MX7EK9 ANP - + after chemical analysis was performed, the sample was found to contain morphine and its metabolites. NQMMS5 + + + - OTJOOE + + +

OYUAUJ + + + Samples also contains 6-MAM and Cafeine Q99KOM + + +

QIIMQZ - + + Codeine, morphine QJH28U + + + The coincidence between the retention times and mass fragmentograms from a reference material analysed in the same conditions that the biological sample indicates the presence of Morphine,Codeine, 6-Monoacetylmorphine. R9TZTO + + + Sample is positive for Codeine, Morphine and 6-Monoacetylmorphine RFJ8SV + + - We don´t found this substance frecuently in the laboratory, it is a substance I hope found in heroin consumer RY5KEY ANP ANP +

S4Z1YG + ANP + Sample contain morphine, 6-monoacetylmorphine.Heroine user. SHUSPS + + +

TTZTHH + + + Codeine, Morphine(Total), 6-Monoacetylmorphine TZRY6I + + +

U9T99A + + + The sample contains 6-Monoacetylmorphine, morphine and codeine. UJUUJR + + + Toxicological examination of sample BS-2 revealed the presence of 6-monoacetylmorphine, codeine and morphine. VEYSDV + + + In the urine sample analyzed was detected and confirmated the presence of 6- Monoacetylmorphine, Morphine Total and Codeine. VVVIVC + + + Recent heroin consumption

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) W2SWWW + + + Morphine, Codeine and 6-Monoacetylmorphine (6-MAM) were detected in the sample WKG8OD + + + sample spiked with MORPHINE 6-MAM and CODEINE (similar to a consumption of heroine) WLWPCL + + + 6-MAM, Codeine, Morphine were identified by GC/MS XPJJCF + + +

XRGZII + + +

XSHEX7 + + + Morphine-Codeine -6-Monoacetylmorphine (6-MAM) YEYYWY + + + Heroine consumption. YYMBZQ - + +

ZBO09R + + + Screening test positive Opites and/or metabolites. CG-MS retention time and relation mass (m/z) the reference material morphine, codeine, 6-monoacetylmorphine are equivalente sample 2014/1/BS-2 ZUYDSS ANP ANP ANP Only free morphine wad measured. ZZYFHY + + ANP

Identification methods for Test Sample 2

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

Summary for test sample 2 The response summary of all 72 participating laboratories for the identification of BS-2, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 2:

Response Summary Participants: 72

6-Monoacetylmorphine (6-MAM): 61 Codeine: 61 Morphine 62

False positives for Test Sample 2

Code Name Technique A4WEB4 Morphine-6-glucuronide 230 DSLONZ Morphine-3-O-glucuronide 180 IIRIR8 Morphine-3-O-glucuronide 180 IIRIR8 Morphine-6-glucuronide 180

False negatives and analysis not performed for BS-2

6-Monoacetylmorphine: 4 false negatives and 7 analyses not performed

Coodeine: 5 false negative and 6 analyses not performed

Morphine: 4 false negatives and 6 analyses not performed

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

Z-Scores for Test Sample 2

6-Monoacetylmorphine Codeine Morphine Deviation Deviation Deviation Concentr Concentr Concentr Code from from from ation z-score ation z-score ation z-score robust robust robust (ng/ml) (ng/ml) (ng/ml) average average average 1RTHUB - - - 1289 123 1 15902 14184 13.4 1SE4LC 16637 1520 0.3 1315 149 0.7 4601 2883 2.7 2ACHJY 3259 -11858 -2.4 194 -972 -4.6 486 -1232 -1.2 7SLBJ5 21650 6533 1.3 1524 358 2 1594 -124 -0.1 8EJHSP 7140 -7977 -1.6 395 -771 -4 1191 -527 -0.5 9YKLH6 12272 -2845 -0.6 1240 74 0 1594 -124 -0.1 A4WEB4 ------514-1204 -1.1 B6S6UH 14229 -888 -0.2 1068 -98 -0.5 1520 -198 -0.2 DTNZDN 27609 12492 2.5 1595 429 2 12124 10406 9.8 GFGG5J 15474 357 0.1 1136 -30 -0.1 7908 6190 5.8 GLLLLQ 21940 6823 1.4 1740 574 2.7 26280 24562 23.2 HFFKMX 17185 2068 0.4 873 -293 -1.4 840 -878 -0.8 KV7QCV 13000 -2117 -0.4 1600 434 2 1100 -618 -0.6 LGPKEB 6275 -8842 -1.8 1254 88 0.4 2592 874 0.8 LNEUXP 10800 -4317 -0.9 740 -426 -2 12500 10782 10.2 NQMMS5 15500 383 0.1 1160 -6 0 900 -818 -0.8 OYUAUJ 17050 1933 0.4 1270 104 0.5 830 -888 -0.8 Q99KOM 25331 10214 2.1 1214 48 0.2 1360 -358 -0.3 R9TZTO 15323 206 0.0 1052 -114 -0.5 766 -952 -0.9 TTZTHH 17993 2876 0.6 1150 -16 0 14258 12540 11.8 VVVIVC 16395 1278 0.3 1202 36 0.2 1170 -548 -0.5 XPJJCF 10621 -4496 -0.9 1092 -74 0 3637 1919 1.8 YEYYWY 1108 -14009 -2.8 850 -316 -1.5 990 -728 -0.7 ZUYDSS 16410 1293 0.3 707 -459 -2.2 818 -900 -0.9 ZZYFHY - - - 1270 104 0.5 ---

Round: 2014/1 Robust average = 15117 UNODC value = 17320 Substance: BS-2/6-Monoacetylmorphine (6-MAM)

4.0

3.0 2.5

2.1 2.0 1.3 1.4

1.0 0.6 0.4 0.4 0.3 0.3 0.3 0.0 0.1 0.1 0.0

‐0.2 ‐0.4 ‐0.6 ‐1.0 ‐0.9 ‐0.9

‐1.6 ‐2.0 ‐1.8

‐2.4 ‐3.0 ‐2.8

‐4.0 XPJJCF 7SLBJ5 8EJHSP 1SE4LC GLLLLQ 2ACHJY 9YKLH6 VVVIVC LGPKEB ZUYDSS R9TZTO GFGG5J TTZTHH LNEUXP B6S6UH OYUAUJ YEYYWY KV7QCV HFFKMX DTNZDN Q99KOM NQMMS5

Round: 2014/1 Robust average = 1166 UNODC value = 1160 Substance: BS-2/Codeine 4.0

3.0 2.7

2.0 2.0 2.0 1.7

1.0 0.7 0.5 0.5 0.6 0.3 0.4 0.2 0.2 ‐4.6 0.0 0.0 ‐0.1 ‐0.1 ‐0.3 ‐0.5 ‐0.5 ‐1.0

‐1.5 ‐1.4 ‐2.0 ‐2.0 ‐2.2

‐3.0

‐3.6 ‐4.0 XPJJCF 7SLBJ5 1SE4LC 8EJHSP GLLLLQ ZZYFHY 2ACHJY VVVIVC 9YKLH6 LGPKEB ZUYDSS R9TZTO GFGG5J TTZTHH LNEUXP B6S6UH OYUAUJ YEYYWY 1RTHUB KV7QCV HFFKMX DTNZDN Q99KOM NQMMS5

45 Z-Score Report per Sample per Substance

Round: 2014/1 Robust average = 1719 UNODC value = 170 Substance: BS-2/Morphine 4.0

3.0 2.7

2.0 1.8

1.0 0.8

0.0 5.8 9.8 10.2 11.8 13.4 23.2 ‐0.2 ‐0.1 ‐0.1 ‐0.3 ‐0.6 ‐0.5 ‐0.5 ‐1.0 ‐0.8 ‐0.7 ‐0.9 ‐0.9 ‐0.8 ‐0.8 ‐1.2 ‐1.1

‐2.0

‐3.0

‐4.0 XPJJCF 7SLBJ5 1SE4LC 8EJHSP GLLLLQ 2ACHJY VVVIVC 9YKLH6 LGPKEB ZUYDSS R9TZTO TTZTHH GFGG5J LNEUXP B6S6UH OYUAUJ YEYYWY 1RTHUB KV7QCV HFFKMX DTNZDN A4WEB4 Q99KOM NQMMS5

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

Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 0JDQRT 11-Nor-delta9-THC-9-carboxylic acid 11L1F1 THC-COOH 1NHAHH CANNABINOIDES 1RTHUB Tetrahydrocannabinol 1SE4LC THC-COOH 2ACHJY ACIDO NOR DELTA 9 TETRAHIDROCANNABINOL 2WKWWU delta 9-THC-COOH 3KYD8K QRU¨7+&FDUER[\OLFDFLG 3NUFZQ THCA 5MIQ5K Cannabinoides 6JPGEG 11-nor-ƩTHC-9-carboxylic acid 7SLBJ5 QRU¨7+&FDUER[\OLFDFLG 8EJHSP 11-Carboxy THC 9KCFVW 11-nor-delta9-THC-9-carboxylic acid. 9YKLH6 11-nor-delta9-THC-9-carboxylic acid AQUCAA 11-nor-delta-9-THC-9-carboxylic acid B6S6UH QRU¨7+&FDUER[\OLFDFLG BZBECD 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid CNHIT2 QRU¨7+&FDUER[\OLFDFLG CRAICM Cannabinoids and/or its metabolites DG9DD6 cANNABINOIDS DOK333 CANNABINOIDS (THC) DSLONZ Carboxy-Delta-9-THC DTNZDN Cannabis (THCCOOH) E3AATH 11-nor-delta9-THC-9-carboxylic acid FS47ZT THCCOOH FSSA3M THC-COOH (cannabis) GFGG5J carboxylic acid GLLLLQ 11-nor-delta9-THC-9-carboxylic acid GXW2Q2 CANNABIS METABOLITE HFFKMX QRU¨7+&FDUER[\OLFDFLG IIRIR8 QRU¨7+&FDUER[\OLFDFLG KKHEMK Cannabis metabolite KV7QCV THCC LGPKEB 11 nor delta 9 THC-cooh LNEUXP THC-COOH MCUQ4O 11-nor-delta9-THC-9-carboxylic acid MNURNG THC acid MX7EK9 cannabis NQMMS5 QRU¨7+&FDUER[\OLFDFLG

Code Identified Substances OYUAUJ QRU¨7+&FDUER[\OLFDFLG QIIMQZ Cannabinoids QJH28U QRU¨7+&FDUER[\OLFDFLG R9TZTO QRU¨7+&FDUER[\OLFDFLG RFJ8SV Delta9-THC-Carboxi RY5KEY QRU¨7+&FDUER[\OLFDFLG S4Z1YG tetrahidrocannabinolic acid SHUSPS -THC TTZTHH 11-nor-delta9-THC-9-carboxylic acid TZRY6I 11-nor-d9-thc-9-carboxylic acid U9T99A QRU¨7+&FDUER[\OLFDFLG UJUUJR QRU¨7+&FDUER[\OLFDFLG VEYSDV 11-nor-delta 9-THC-9-carboxylic acid VVVIVC THC-COOH WKG8OD 11-nor-delta 9 thc-9-carboxylic acid WLWPCL 11-nor-delta-9-THC-9-carboxylic acid XPJJCF 11-nor-delta9-THC XRGZII 11-nor-delta9-THC-9-carboxylic acid XSHEX7 CANNABINOIDS YEYYWY THCCOOH YYMBZQ CANNABINOIDS ZBO09R QRU¨7+&FDUER[LOLFDFLG ZUYDSS THC-COOH ZZYFHY 11nor delta 9tetrahidrocannabinol carboxylic acid

Statement of findings for Test Sample 3

Code QRU¨7+& carboxylic acid 0JDQRT + In the urine sample cannabinoids were found. 11L1F1 +

1NHAHH + THE SAMPLE No.2014/1/BS-3 WAS FOUND 11-COOH-TETRAHYDROCANNABINOL 1RTHUB + Sample 2014/1/BS3 contains Tetrahydrocannabinol therefore positive for both screening and confirmatory tests. 1SE4LC + This person consumed cannabis products. 2ACHJY + HUBO CONSUMO DE MARIHUANA 2WKWWU + delta 9-THC-COOH indicates that THC was consumed. 3KYD8K + Screening by immunoassay technique : Positive Confirm by GC-MS : Positive 3NUFZQ + The person who provided the specimen has consumed cannabis. 5MIQ5K ANP Positivo 6JPGEG + Use of cannabis. 7SLBJ5 + use of cannabinoids 8EJHSP + Prise de Cannabis 9KCFVW + In urine sample number three was identified 11-nor-delta9-THC-9-carboxylic acid. 9YKLH6 + The urine analyzed contains 11-nor-delta9-THC-9-carboxylic acid This indicates an absorption of cannabis. A4WEB4 - There was no screening for Hydroxybutyric (GHB) and Butyrolactone (GBL) because no reference standard is available. AQUCAA + 11-nor-delta-9-THC-9-carboxylic acid detected. B6S6UH + Cannabis abuse. BD3BFB +

BKPN2U ANP

BZBECD + 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid detected in BS-3

Code QRU¨7+& carboxylic acid CNHIT2 + ,QWKHVDPSOHODEHOHGURXQG,&(VDPSOH%6QRU¨7+&FDUER[\OLFDFLGZDV detected CRAICM ANP The reported analytical findings detected the presence of cannabinoids and/or its metabolites in the urine same, BS-3. This analytical finding is the result of primary screening and additional confirmatory tests should be performed. DG9DD6 + QRU¨7+&FDUER[\OLFDFLG DOK333 + Extraction of sample and TLC analysis using two solvent systems and HPLC confirmed the sample DV'(/7$7(75$+<'52&$11$%,12/ ¨7+& DPK69B ANP

DSLONZ + The presence of Carboxy-Delta-9-THC in urine indicates cannabis comsuption or cannabis related products comsuption. DTNZDN + Presence of THCCOOH, cannabis metabolite is conclusive evidence of prior cannabis use. Cannabis is a controlled narcotic in France E3AATH + 1. Results of screening test were positive for cannabinoids and metabolites. 2. Retention time and fragmentation pattern obtained with the biological sample are equivalent to those obtained with "11-nor-delta9-THC-9-carboxylic acid" (Reference material). FHDI00 ANP On analysis, no drugs found in the sample of 2014/1/BS-3. FS47ZT +

FSSA3M +

GFGG5J +

GLLLLQ + Use of cannabinoides GXW2Q2 + POSITIVE HFFKMX +

IIRIR8 + quantification not performed KKHEMK + Previous use of cannabis KV7QCV + sample contains cannabis LGPKEB + positive to cannabis consumption LNEUXP + Positive for THC-COOH MCUQ4O +

Code QRU¨7+& carboxylic acid MNURNG + consumption of cannabis product MX7EK9 + DIWHUFKHPLFDODQDO\VLVZDVSHUIRUPHGWKHVDPSOHZDVIRXQGWRFRQWDLQ7+&PHWDEROLWH QRU¨ -THC-9-carboxylic acid). NQMMS5 + - OTJOOE +

OYUAUJ +

Q99KOM +

QIIMQZ + QRU¨7+&FDUER[\OLFDFLG QJH28U + The coincidence between the retention times and mass fragmentograms from a reference material DQDO\VHGLQWKHVDPHFRQGLWLRQVWKDWWKHELRORJLFDOVDPSOHLQGLFDWHVWKHSUHVHQFHRIQRU¨ THC-9-carboxylic acid. R9TZTO + 6DPSOHLVSRVLWLYHIRUQRU¨7+&FDUER[\OLFDFLG RFJ8SV + One of the metobite we found in smoker of marihuana RY5KEY + QRU¨7+&FDUER[\OLFDFLGZDVGHWHFWHGDWDOHYHODERYHWKHFXWRII QJP/ YDOXHDQG therefore positive for the drug Cannabis. S4Z1YG + Sample contain tetrahidrocannabinolic acid. Marihuana(hasišs)user SHUSPS +

TTZTHH + 11-nor-delta9-THC-carboxylic acid TZRY6I +

U9T99A + 7KHVDPSOHFRQWDLQVQRU¨7+&FDUER[\OLFDFLG UJUUJR + 7R[LFRORJLFDOH[DPLQDWLRQRIVDPSOH%6UHYHDOHGWKHSUHVHQFHRIQRU¨7+&FDUER[\OLF acid . VEYSDV + In the urine sample analyzed was detected and confirmated the presence of 11-nor-delta 9-THC-9- carboxylic acid. VVVIVC + Cannabis consumption W2SWWW ANP No drugs were detected in the sample WKG8OD + sample spiked with11-nor-delta 9 thc-9-carboxylic acid (similar to a consumtion of THC) WLWPCL + 11-nor-delta-9-THC-9-carboxylic acid was identified by GC/MS

Code QRU¨7+& carboxylic acid XPJJCF +

XRGZII +

XSHEX7 + QRU¨7+&FDUER[\OLFDFLG YEYYWY + Cannabis consumption. YYMBZQ +

ZBO09R + Screening test positive cannabinoids. CG-MS retention time and relation mass (m/z) the reference PDWHULDOQRU¨7+&FDUER[LOLFDFLGDUHHTXLYDOHQWHVDPSOH%6 ZUYDSS ANP

ZZYFHY +

Identification methods for Test Sample 3

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

Summary for test sample 3 The response summary of all 72 participating laboratories for the identification of BS-3, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 3:

Response Summary Participants: 72

QRU¨7+&FDUER[\OLFDFLG: 64

False positives for Test Sample 3

Code Name Technique

False negatives and analysis not performed for BS-3

1 false negatives and 7 analyses not performed

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

Z-Scores for Test Sample 3

11-nor-∆9-THC-9-carboxylic acid Deviation Code Concentration from z-score (ng/ml) robust average 1RTHUB 206 15 0.3 1SE4LC 127 -64 -1.1 2ACHJY 179 -12 -0.2 3NUFZQ 240 49 0.9 8EJHSP 40 -151 -2.7 9YKLH6 148 -43 -0.8 B6S6UH 169 -22 -0.4 DTNZDN 154 -37 -0.7 GFGG5J 289 98 1.7 GLLLLQ 212810 212619 3771.8 HFFKMX 132 -59 -1.0 KKHEMK 131 -60 -1.1 KV7QCV 210 19 0.3 LGPKEB 183 -8 -0.1 LNEUXP 222 31 0.6 NQMMS5 205 14 0.3 OYUAUJ 275 84 1.5 Q99KOM 216 25 0.5 R9TZTO 185 -6 -0.1 RY5KEY 109 -82 -1.4 TTZTHH 267 76 1.4 VVVIVC 229 38 0.7 XPJJCF 150 -42 -0.7 YEYYWY 221 30 0.5 ZUYDSS 172 -19 -0.3 ZZYFHY 190 -1 0.0

Round: 2014/1 Robust average = 191 Substance: BS-3/QRU¨7+&FDUER[\OLFDFLG UNODC value = 230

4.0

3.0

2.0 1.7 1.5 1.4

0.9 1.0 0.7 0.5 0.5 0.6 0.3 0.3 0.3

0.0 0.0 ‐0.2 ‐0.1 ‐0.1 3772 ‐0.4 ‐0.3 ‐1.0 ‐0.8 ‐0.7 ‐0.7 ‐1.1 ‐1.1 ‐1.0 ‐1.4 ‐2.0

‐3.0 ‐2.7

‐4.0 XPJJCF 8EJHSP 1SE4LC GLLLLQ ZZYFHY RY5KEY 2ACHJY VVVIVC 9YKLH6 LGPKEB ZUYDSS R9TZTO TTZTHH GFGG5J LNEUXP B6S6UH YEYYWY OYUAUJ 1RTHUB KV7QCV 3NUFZQ HFFKMX DTNZDN KKHEMK Q99KOM NQMMS5

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

Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 0JDQRT 2CB 11L1F1 2C-B 1NHAHH NONE 1SE4LC 2C-B 2WKWWU 2C-B 3KYD8K 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 6JPGEG 2C-B 8EJHSP 2-CB 9KCFVW 4-Bromo-2,5-dimethoxyphenethylamine 9YKLH6 2-CB A4WEB4 2CB B6S6UH 2-CB CNHIT2 No detected CRAICM none DG9DD6 2C-B DOK333 N/A DTNZDN 4-bromo 2,5 dimethoxyphenethylamine E3AATH 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) FSSA3M 2-CB GXW2Q2 2C-B HFFKMX 4-Bromo-2,5-dimethoxyphenethylamine IIRIR8 NEGATIVE KV7QCV 2-CB MCUQ4O 4-bromo-2,5-dimethoxyphenethylamine(2-C-B) NQMMS5 4-Bromo-2,5-dimethoxyphenethylamine OYUAUJ 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) QIIMQZ none QJH28U None. R9TZTO 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) RFJ8SV 2C-P S4Z1YG - SHUSPS 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) TTZTHH NIL VEYSDV None VVVIVC 2-CB W2SWWW 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) WKG8OD 2C-B XSHEX7 HALLUCINOGENIC DRUGS YEYYWY 2-CB YYMBZQ BDMPEA

Code Identified Substances ZBO09R 4-Bromo-2.5-dimethoxyphenethylamin ZUYDSS 2C-B ZZYFHY 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

Statement of findings for Test Sample 4

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) 0JDQRT + In the urine sample 2CB (4-Bromo-2,5-dimethoxyphenethylamine) was found 11L1F1 +

1NHAHH ANP NONE 1RTHUB ANP Sample 2014/1/BS4 does not contain controlled drugs as performed. 1SE4LC + This person consumed 2C-B. 2ACHJY ANP NO HUBO CONSUMO DE DROGAS. 2WKWWU + 2C-B was detected, this indicate that 2C-B was consumed. 3KYD8K + Screening and confirm by GC-MS : Positive 3NUFZQ ANP

5MIQ5K ANP No se detectó 6JPGEG + Use of 2C-B. 7SLBJ5 ANP

8EJHSP + Prise de 2-CB 9KCFVW + In urine sample number four was identified 4-Bromo-2,5-dimethoxyphenethylamine. 9YKLH6 + The urine analyzed contains 2-CB.

A4WEB4 + Analytical Adverse Finding for 2CB in the sample. AQUCAA ANP Common drugs not detected. B6S6UH + 2-CB consumption. BD3BFB +

BKPN2U ANP

BZBECD ANP No drugs detected in BS-4 CNHIT2 - In the sample labeled sample round ICE 2014-1 BS-4 not any substances were detected

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) CRAICM ANP The reported analytical findings did not detect the presence of drugs in the urine sample, BS-4. DG9DD6 + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) DOK333 - No narcotic substances ( Banned Substances) were detected using TLC with two (2) solvent systems. DPK69B ANP

DSLONZ ANP

DTNZDN + 2 CB is a psychedelic phenethylamine of the 2C family. 2 CB is a solid as a white powder sometimes pressed in tablet or gel caps. The drug is usaually taken orally but can also be insufflated or vaporized. 2 CB is a controlled narcotic in France. E3AATH + 1. Results of screening test were positive for amphetamines. 2. Retention time and fragmentation pattern obtained with the biological sample are equivalent to those obtained with "4-Bromo-2,5-dimethoxyphenethylamine (2C-B)" (Reference material). FHDI00 ANP On analysis, no drugs found in the sample of 2014/1/BS-4. FS47ZT ANP

FSSA3M +

GFGG5J -

GLLLLQ -

GXW2Q2 + POSITIVE HFFKMX +

IIRIR8 -

KKHEMK ANP

KV7QCV + sample contains 2 CB LGPKEB ANP no drugs of abuse LNEUXP ANP

MCUQ4O +

MNURNG ANP

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) MX7EK9 ANP after chemical analysis was performed, the sample was not found to contain controlled drugs. NQMMS5 + - OTJOOE +

OYUAUJ + Samples also contains Cafeine Q99KOM ANP

QIIMQZ ANP

QJH28U ANP In immunoassay a minor concentration to the cut-off means that the analytical system did not detect the presence of the investigated substances. R9TZTO + Sample is positive for 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) RFJ8SV +

RY5KEY ANP

S4Z1YG ANP - SHUSPS +

TTZTHH +

TZRY6I ANP

U9T99A ANP

UJUUJR ANP Toxicological examination of sample BS-4 yielded negative result. VEYSDV ANP In the urine sample analyzed was not detected the presence of controlled drugs. VVVIVC +

W2SWWW + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected in the sample WKG8OD + sample spiked with 2C-B (CONSUMTION TO SYNTHETIC DRUG) WLWPCL -

XPJJCF -

XRGZII ANP

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) XSHEX7 + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) YEYYWY + Designer drugs consumption. YYMBZQ +

ZBO09R + Screening test positive Amfetamines. CG-MS relation mass (m/z) are equivalente 4-Bromo-2.5- dimethoxyphenethylamin sample 2014/1/BS-4 ZUYDSS ANP

ZZYFHY +

Identification methods for Test Sample 4

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

Summary for test sample 4 The response summary of all 72 participating laboratories for the identification of BS-4, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 4: Response Summary Participants: 72

4-Bromo-2,5-dimethoxyphenethylamine 35 (2C-B):

False positives for Test Sample 4

Code Name Technique

False negatives and analysis not performed for BS-4

7 false negatives and 30 analyses not performed

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

Z-Scores for Test Sample 4

4-Bromo-2,5-dimethoxyphenethylamine (2C-B) Code Concentration Deviation from z-score (ng/ml) robust average 8EJHSP 1242 34 0.1 B6S6UH 1443 235 1.0 DTNZDN 781 -427 -1.9 HFFKMX 1480 272 1.2 KV7QCV 1200 -8 0.0 NQMMS5 1100 -108 -0.5 R9TZTO 1264 56 0.2 ZUYDSS 889 -319 -1.4 ZZYFHY 1295 87 0.4

Round: 2014/1 Substance: BS-4/4-Bromo-2,5-dimethoxyphenethylamine (2C-B) Robust average = 1209 UNODC value = 1590

4.0

3.0

2.0

1.2 1.0 1.0 0.4 0.1 0.2 0.0 0.0 ‐0.5 ‐1.0

‐1.4 ‐2.0 ‐1.9

‐3.0

‐4.0 8EJHSP ZZYFHY ZUYDSS R9TZTO B6S6UH KV7QCV HFFKMX DTNZDN NQMMS5

68 69 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

The Laboratory and Scientific Section UNODC, International Centre Wagramer Strasse 5, P.O. Box 500 A-1400, Vienna, AUSTRIA Email: [email protected]