(ICE) Summary Report

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

BIOLOGICAL SPECIMENS 2016/2

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 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 15 Summary Page 18 Z-Scores Page 19 Sample 2 Analysis Page 22 Identified substances Page 22 Statement of findings Page 24 Identification methods Page 29 Summary Page 32 Z-Scores Page 33 Sample 3 Analysis Page 41 Identified substances Page 41 Statement of findings Page 43 Identification methods Page 48 Summary Page 51 Z-Scores Page 52 Sample 4 Analysis Page 55 Identified substances Page 55 Statement of findings Page 57 Identification methods Page 62 Summary Page 65 Z-Scores Page 66 Test Samples Information Samples Comments on samples Sample 1 To prepare BS-1, urine was spiked with an aqueous solution of morphine sulphate (1138ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 2 To prepare BS-2, urine was spiked with aqueous solutions of morphine sulphate (1138ng base/ml) and benzoylecgonine (690ng base/ml) and a methanol solution of methylecgonine (350ng 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 MDMA hydrochloride (1955ng 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 2C-B hydrochloride (1724ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Samples Substances Concentrations Comments on substances Sample 1 Morphine (Total) 1138 ng/ml Sample 2 Benzoylecgonine 690 ng/ml Methylecgonine 350 ng/ml Morphine (Total) 1138 ng/ml Sample 3 3,4-Methylenedioxymetamfetamine (MDMA) 1955 ng/ml Sample 4 4-Bromo-2,5-dimethoxyphenethylamine (2C- 1724 ng/ml B)

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.

2 2016/2-BS Copyright (c) 2017 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 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. The ICE programme is a UNODC mandated activity and is implemented through regular budget funds and through the UNODC Global Scientific and Forensic Programme – Support Project (GLOU54), which operationalizes the forensic aspects of the UNODC Thematic Programme on Research, Trend Analysis and Forensics" Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2016/2 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 225 laboratories in 73 countries. Within the SM test group, there were 181 participating laboratories from 67 countries and within the BS test group, results were submitted by 89 laboratories from 44 countries.1

Qualitative Analysis

The analytical techniques most commonly used for screening of test samples in the BS test group were enzyme immunoassays (55% of participants), while GC-MS (81%) was the most commonly used technique for identification/confirmation of the components in the test samples. The results for the qualitative identification of the sample components in the BS test group, the number of false positive/negative results and the analyses not performed are shown in the table 1.

Table 1. Qualitative performance of participants in the 2016/2 round of ICE.

BS-1 BS-2 BS-2 BS-2 Test sample (Morphine) (Benzoylecgonine) (Methylecgonine) (Morphine)

Correct identification 79% 69% 71% 75% Number of false 3 8 positives Number of false 6 4 negatives Number of analyses not performed 8 4 (ANP) BS-3 BS-4 Test sample (MDMA) (2C-B) Correct identification 90% 61% Number of false 8 1 positives Number of false 2 12 negatives Number of analyses not performed 3 24 (ANP)

1 A small number of laboratories received test samples from the 2016/1 ICE round due to an administrative error and they have received individual evaluation reports based on the analyses they carried out,.

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.

Quantitative Analysis

The test samples in the BS group for the 2016/2 round of ICE contained a total of six components and 39 (44%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to note that 92% of laboratories quantified at least two components and 33% performed quantification of all components present. GC-MS was used by 58% of participants for quantification, followed by LC/MS(/MS), which was used by 45% of participants. Z-scores obtained by participants in quantification are shown in the table below (percentage + no. of labs indicated).

Table 2. Quantitative performance of participants in the 2016/2 round of ICE.

Test sample z-score BS-1 BS-2 BS-2 (Morphine) (Benzoylecgonine) (Methylecgonine) |z| < 2, satisfactory 84% (26) 83% (29) 83% (19) 2 ≤ |z| ≤ 3, 10% (3) 14% (5) 13% (3) questionable |z| > 3, unsatisfactory 6% (2) 3% (1) 4%(1)

z-score BS-2 (Morphine) BS-3 (MDMA) BS-4 (2C-B)

|z| < 2, satisfactory 87% (27) 81% (29) 90% (18) 2 ≤ |z| ≤ 3, 6% (2) 8% (3) 10% (2) questionable |z| > 3, unsatisfactory 6% (2) 11% (4) 0

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 2016/1 round of ICE, seven laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Six of these laboratories participated and performed quantification in the 2016/2 round with five laboratories obtaining satisfactory z-scores in all of their quantitative analysis, while one laboratory obtainine a questionable z- score in its analysis.

Seven laboratories obtained unsatisfactory z-scores in ICE 2016/1 with |z| ≥ 3. Of these laboratories, six participated in ICE 2016/2 and performed quantification, with all improving their performance to obtain satisfactory z-scores in at least one sample. Two of these laboratories also obtained unsatisfactory z-scores and three obtained questionable z-scores.

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.

2016/2-BS 4 Copyright (c) 2017 UNODC New Psychoactive Substances (NPS) reported by laboratories participating in the 2016/2 round of the ICE programme During the 2016/2 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 225 reports of 135 substances. The most commonly reported substances were equally from the groups of synthetic cathinones (32%) and synthetic cannabinoids (32%) as shown in figure 1.

Synthetic cannabinoids 2% 2% 1% 7% 4% Synthetic cathinones 32% Others

Phenethylamines

Ketamine and phencyclidine type substances 20% Tryptamines

Aminoindanes 32% Piperazines

Figure 1. NPS reported by ICE laboratories during the 2016/2 round of ICE

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (42%), while 31% were synthetic cannabinoid receptor agonists (SCRA’s) and 9% were synthetic opioids (which included seven fentanyl derivatives) as shown in figure 2.

4% 6% 7%

42% Stimulants

9% SCRA's Opioids Hallucinogens Dissociatives Sedatives/Hypnotics

32%

Figure 2. Mode of action of NPS reported by ICE participants in the 2016/2 round of ICE

NPS most commonly reported by laboratories participating in ICE 2016/2

The substances most often reported by ICE participants were the synthetic cannabinoid receptor agonists 5F-MDMB-PINACA (methyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate, AB- CHMINACA (N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-1H-indazole-3-carboxamide and the synthetic opioid furanylfentanyl (N-(1-phenethylpiperidin-4-yl)-N-phenylfuran-2-carboxamide. 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.

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 123WGB MORPHINE 1PWJNH Morphine 1TTIML None 1TZH5Y 7 amino flunitrazepam 3DKQOQ Morphine 419F4M morphine 44TU44 Morphine 4GHNH4 morphine 4YLFBL morphine 66ZO6A morphine 6CVGQ6 Morphine, Total 6JIYPR Morfina 6V1XQX Morphine 8IIDK3 morphine ALUS4Z MORPHINE AVERAC morphine CQGC6C Morphine CRKFUT morphine DUZUY3 Morphine DZKP99 Morphine EGCC8D Morphine EHOHKH MORPHINE ERZR0K morfina EXR666 MORPHINE FFAFFI MORPHINE FQFOEF Morphine FZ5ZGY morphine GIGLLN morphine HZ4SSF Morphine IGGUCG Morphine IGGZSA Morphine IM9MIS Morphine ITEOXF Morphine J77027 opiates / opioids JHMWJW morphine, norbuprenorphine JL1GTU Morphine JPRPXO Morphine KFFG6N Morphine KQ4LD7 Not detected KSEXBG no drugs detected

Code Identified Substances L6XLFB Morphine LALDP0 morphine LB5MQU Morphine LMAFMM Codeine and 7-Aminoflunitrazepam MDKNFX Morphine MM3MAK Morphine MQULMG morphine NNNKNN metanfetamina NOGTSO Morphine O55XS5 Morphine OOIXLI Morphine OSOXXO Morfine P45IGJ morphine PB44MH Morphine PFCACT morphine PMG9F9 morphine PPPPYM morphine QDJMOE Morphine QPIOKN morphine RFIBGP Morphine RQEEOE morphine RSYHBH 7-aminoflunitrazepam RXYG2Q Morphine U5AWA0 Morphine U8NKUE Morphine V8HYSI Morphine VAXCAO Morphine VE1EEZ None VLA1JO morphine W3E7JE MORPHINE WFA0FD morphine WVFKZV Morphine XIKHP6 morphine XZURKZ morphine YZOFYZ Morphine Z25SYN Morphine ZVTR4A 7-Aminoflunitrazepam

Statement of findings for Test Sample 1

Code Morphine (Total) 0O03BD - The test sample 2016/2/BS-1 do not found to contain any drugs. 123WGB +

1PWJNH + We found Morphine in BS-1 1TTIML - We did not find any drugs. We found only caffein and Procaine. -

3DKQOQ + Urine specimen contains 1017.1 ng/mL Morphine 419F4M + Positive to morphine. 4444FB +

44TU44 + Sample is positive for Morphine 4GHNH4 +

4YLFBL + Positive to morphine. 66ZO6A +

6CVGQ6 + Morphine, Total- Detected > 0.5mg/L 6JIYPR + Hubo Consumo de Morfina 6V1XQX + This person consumed morphine and/or heroin. 8IIDK3 + morphine is an analgesic opiate used in France to treat intense pain; it is also a controlled drug in France. Morphine is also a metabolite of heroine (controlled drug) and 3 antitussive drugs (codeine, pholdocine, ethylmorphine) ALUS4Z +

AVERAC +

CQGC6C + In the sample labeled 2016/2/BS-1 Morphine was detected. CRKFUT +

DUZUY3 + The presence of Morphine in urine indicates consumption of the drug itself or the intake of other drugs. DZKP99 + can be issued from medical prescription or from heroin

Code Morphine (Total) EGCC8D + Sample BS1 found to contain morphine, measured value 1271 ng/ml EHOHKH + MORPHINE DETECTED EP2WDI ANP

ERZR0K + Preliminary test followed by the analytical confirmation, then the quantification. EXR666 +

FFAFFI + In sample 2016/2/BS-1 was found an confirmed the presence of MORPHINE FQFOEF + Morphine intake

FZ5ZGY + sample BS-1 contain morphine GIGLLN + Morphine use or abuse. GTUFSO +

GXURZK ANP Test sample 2016/2/BS-1 does not contain controlled drugs therefore Negative. HZ4SSF + - IGGUCG + The sample contains morphine. IGGZSA +

IKPH39 + MORPHINE DI-TMS DERIVATIVE IM9MIS + In the sample was detected Morphine, this finding indicates that Morphine was consumed. ITEOXF + Morphine was identified by GC-MS. J77027 ANP The test sample 2016/2/BS-1 shows a positive result over 2000 ng/mL. JHMWJW + coffeine, theophylline JL1GTU +

JPRPXO +

JYO93J - Examination and analyses performed on BS1 did not reveal any positive findings of toxicological significance.

Code Morphine (Total) KFFG6N + Free morphine was detected at concentration of 952.2 ng/mL in the 2016/2/BS-1 sample. KQ4LD7 - The specimen was not detected KSEXBG - général extraction with four range of pH L6XLFB +

LALDP0 + use of morphine LB5MQU + Morphine is a narcotic analgesic found in the opium poppy. It is a schedule II controlled substance in the United States.

MDKNFX + Morphine MM3MAK + Morphine was found in the sample. The finding is in accordance with the intake of morphine or heroine, that metabolizes to morphine. MQULMG + positive NNNKNN ANP metanfetamina: positivo NOGTSO + Morphine intake (not heroin) NW11JK ANP No common drugs were detected in the sample of 2016/2/BS-1 O55XS5 + Drugs detected, quantification was not performed OOIXLI + GC/MS: Relation m/z, time retention (tR ) the reference material Morphine are equivalents to those sample 2016/2/BS-1 OSOXXO +

P45IGJ + after chemical analysis was performed the sample was contine 1225.ng/ml morphine PB44MH + Sample BS-1 is positive for Morphine PFCACT + intake of morphine PMG9F9 +

PPPPYM + morphine Q6EK5S ANP After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA), High Performance Liquid Chromatography with diode array detection (HPLC/DAD) and Gas Chromatography/Mass Spectrometry (GC/MS), was not detected substances in the urine sample 2016/2/BS-1.

Code Morphine (Total) QDJMOE + In the urine sample (2016-2/BS1) morphine was found. QPIOKN + Consistent with previous use of morphine or very pure heroin RFIBGP + Sample code number 2016/2/BS-1 was found to contain morphine (concentration 1239 ng/ml) RQEEOE +

RXYG2Q + Using EIA and GC-MS techniques, Morphine was detected in the urine specimen which is considered as a controlled drug. U5AWA0 + Morphine is detected in urine by GC-MS U5T5NQ +

U8NKUE + Confirms prior use of heroin/morphine V8HYSI + Morphine VAXCAO + Morphine was identified in the sample. VE1EEZ ANP Sample 2016/2/BS-1 found not to contain any drugs VLA1JO +

W3E7JE +

WFA0FD + presence of morphine WVFKZV + Morphine was detected in BS-1 sample. XIKHP6 +

XXMXQX -

XZURKZ ANP Only free morphine was measured. YZOFYZ + Toxicological examination revealed the presence of morphine Z25SYN + Morphine detected.

Code 7- Aminoflunitrazepam

ZVTR4A +

LMAFFM +

1TZH5Y +

RSYHBH +

FVJJJE +

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 100 110 120 150 160 161 170 180 230 231 210 0O03BD SI 123WGB S I 1PWJNH S I 1TTIML I SI Dipro drug lab screen 1TZH5Y SI 3DKQOQ S SI 419F4M S I 4444FB S I 44TU44 S SI S LC-TOF 4GHNH4 I S BIOCHIP 4YLFBL S I I 66ZO6A S S I SI 6CVGQ6 S I 6JIYPR I SI S randox 6V1XQX S I I 8IIDK3 S I I ALUS4Z SI I AVERAC S I CQGC6C I CRKFUT S I DUZUY3 S I I DZKP99 S I I EGCC8D S I I EHOHKH S S SI I EP2WDI S I ERZR0K S I EXR666 S I FFAFFI SI I FQFOEF I S KIMS FVJJJE S I I FZ5ZGY S I GIGLLN I I I S GTUFSO SI S immunochromatographic test GXURZK I I S Drug Test Kit

Code 100 110 120 150 160 161 170 180 230 231 210 HZ4SSF SI IGGUCG I S Multi-Drug Screen Test Panel IGGZSA S I SI IKPH39 SI IM9MIS I S Lateral Flow Immunoassay ITEOXF S I J77027 S JHMWJW SI I JL1GTU S I JPRPXO I S TRIAGE 8-Sure Step JYO93J S SI KFFG6N S I SI KQ4LD7 SI KSEXBG SI I S immunochromatographique L6XLFB S I I LALDP0 S I LB5MQU I LC-QTOF LMAFMM S I I MDKNFX S I SI MM3MAK S SI MQULMG SI NNNKNN S NOGTSO S I NW11JK SI O55XS5 SI OOIXLI I OSOXXO I P45IGJ S S I PB44MH S I I I PFCACT S I SI PMG9F9 SI I SI PPPPYM SI I I Q6EK5S S SI I QDJMOE SI SI QPIOKN S I I RFIBGP SI I RQEEOE SI RSYHBH SI SI RXYG2Q S I I

Code 100 110 120 150 160 161 170 180 230 231 210 U5AWA0 S I U5T5NQ S I U8NKUE SI I V8HYSI S I I S Kinetics Interactions of Microparticles VAXCAO SI I VE1EEZ SI VLA1JO S S I I W3E7JE S I WFA0FD S S SI WVFKZV S I XIKHP6 I I XXMXQX SI YZOFYZ S SI I I LCHRMS Z25SYN I ZVTR4A SI I I

Summary for test sample 1 The response summary of all 89 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: 89

Morphine (Total): 70

False positives for Test Sample 1

Code Name Technique JHMWJW Norbuprenorphine 231 LMAFMM Codeine 180/230 NNNKNN Metamfetamine 120

False negatives for BS-1 (technique(s) used or ANP) Code: XXMXQX (110), 0O03BD (180), KSEXBG (161/180), KQ4LD7 (180), JYO93 (180), 1TTIML (150) 8 laboratories did not carry out analysis for morphine GXURZK, XZURKZ, NW11JK, J77027, Q6EK5S, VE1EEZ, EP2WDI, NNNKNN

Frequency of use of screening and identification techniques:

Response Summary Participants 89 Technique 100 110 120 150 160 161 170 180 210 230 231 Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

(%) 3.4 54.5 4.5 2.3 1.1 3.4 0.0 25.0 12.5 3.4 10.2

Identification (No.) 0 5 1 5 0 6 1 71 3 6 35

(%) 0.0 5.7 1.1 5.7 0.0 6.8 1.1 80.7 3.4 6.8 39.8

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17 (%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1146 ng/ml Substance: BS‐1; Morphine UNODC value = 1138 ng/ml

4.00

3.5

3.00 2.6

2.1 2.00

1.3 1.2 1.3

1.00 0.8 0.6 0.4 0.5 0.5 0.3 0.3 0.1 0.1 0.00 ‐3.6 0.0 ‐0.2 ‐0.4 ‐0.3 ‐0.3 ‐0.5 ‐0.5 ‐0.4 ‐0.7 ‐0.7 ‐1.00 ‐0.8 ‐1.1 ‐1.4 ‐1.5 ‐2.00

‐3.00 ‐2.9

‐4.00 6JIYPR 8IIDK3 P45IGJ L6XLFB V8HYSI RFIBGP HZ4SSF GIGLLN IGGZSA 4444FB YZOFYZ ERZR0K VLA1JO EXR666 JPRPXO 44TU44 XZURKZ CRKFUT FQFOEF 66ZO6A EGCC8D 6V1XQX IGGUCG PMG9F9 WFA0FD PB44MH NOGTSO MDKNFX 3DKQOQ JHMWJW MM3MAK

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 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 signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

19 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐1; Morphine

Dispersion of z-scores using different analytical techniques for the quantification of morphine in 2016/2 BS-1 6

0 z-score

-2

-4

LC‐MS GC‐MS

-6

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

Z-Scores for Test Sample 1

Morphine Code Concentration Deviation from z-score (ng/ml) robust average JPRPXO 432 -714 -3.6 WFA0FD 582 -564 -2.9 JHMWJW 852 -295 -1.5 XZURKZ 873 -273 -1.4 MM3MAK 925 -221 -1.1 66ZO6A 998 -148 -0.8 FQFOEF 1016 -130 -0.7 3DKQOQ 1017 -129 -0.7 EXR666 1052 -94 -0.5 6V1XQX 1052 -94 -0.5 4444FB 1063 -83 -0.4 V8HYSI 1076 -70 -0.4 GIGLLN 1087 -59 -0.3 IGGZSA 1090 -56 -0.3 NOGTSO 1110 -36 -0.2 L6XLFB 1137 -9 0.0 MDKNFX 1160 14 0.1 HZ4SSF 1175 29 0.1 VLA1JO 1200 54 0.3 8IIDK3 1212 66 0.3 P45IGJ 1225 79 0.4 IGGUCG 1238 92 0.5 RFIBGP 1239 93 0.5 EGCC8D 1271 125 0.6 PB44MH 1307 161 0.8 44TU44 1387 241 1.2 YZOFYZ 1395 249 1.3 PMG9F9 1410 264 1.3 6JIYPR 1550 404 2.1 ERZR0K 1663 517 2.6 CRKFUT 1829 683 3.5

Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 0O03BD Methylecgonine 123WGB MORPHINE, ECGONINE METHYL ESTER 1PWJNH Morphine and Methylecgonine 1TTIML Buprenorphine 1TZH5Y buprenorphine 3DKQOQ Morphine, Methylecgonine 419F4M Benzoylecgonine, Methylecgonine, Morphine 44TU44 Benzoylecgonine, Methylecgonine, Morphine 4GHNH4 morphine, methylecgonine, benzoylecgonine 4YLFBL morphine, methylecgonine and benzoylecgonine 66ZO6A morphine, Methylecgonine, Benzoylecgonine 6CVGQ6 Morphine, Total, Benzoylecgonine, Ecognine Methyl Ester 6JIYPR Morfina 6V1XQX Morphine, cocaine, methylecgonine, benzoylecgonine 8IIDK3 Morphine, Benzoylecgonine (BZE) and methylecgonine (EME) ALUS4Z COCAINE, MORPHINE AVERAC morphine, cocaine CQGC6C Morphine, Benzoylecgonine and Methylecgonine CRKFUT morphine, benzoylecgonine, methylecgonine DUZUY3 Morphine, Benzoylecgonine, Methylecgonine. DZKP99 Morphine, BZE, EME EGCC8D Morphine, benzoylecgonine, methylecgonine EHOHKH BENZOYLECGONINE, METHYLECGONINE ESTER AND MORPHINE EP2WDI Benzoylecoginine ERZR0K Morphine and Benzoilecgonine EXR666 MORPHINE, ECGONINE METHYL ESTER, BENZOYL ECGONINE FFAFFI MORPHINE, BENZOYLECGONINE AND METHYLECGONINE FQFOEF Morphine, Benzoylecgonine, methylecgonine FZ5ZGY morphine, ME,BE GIGLLN morphine, benzoylecgonine GXURZK Benzoylecgonine HZ4SSF Morphine,Benzoylecgonine,Methylecgonine IGGUCG Morphine, benzoylecgonine, methylecgonine IGGZSA Morphine, benzoylecgonine, methylecgonine IM9MIS Morphine, Benzoylecgonine,Methylecgonine ITEOXF Cocaine, Morphine J77027 Opiates / opioids and Cocaine and/or metabolites JHMWJW morphine, benzoylecgonine JL1GTU Morphine, Methylecgonine and Benzoylecgonine JPRPXO Morphine, Benzoyecgonine, Methylester

Code Identified Substances KFFG6N Morphine, benzoylecgonine, methylecgonine KQ4LD7 Ecgonine methyl ester KSEXBG Benzoylecgonine L6XLFB Morphine, Benzoylecgonine, Methylecgonine LALDP0 methylecgonine, morphine LB5MQU Mophine, Cocaine metabolites (benzoylecgonine, ecgonine methyl ester) LMAFMM Norbuprenorphine MDKNFX Morphine, Benzoylecgonine, Methylecgonine MM3MAK Morphine, benzoylecgonine MQULMG cocaïne NNNKNN cocaína; opiáceos NOGTSO Morphine, ecgoninne methyl ester and benzoylecgonine NW11JK Ecgonine methyl ester O55XS5 Morphine, Benzoylecgonine, Methylecgonine OOIXLI Methylecgonine, Benzoylecgonine, Morphine OSOXXO morfine, benzoilecgonine P45IGJ morphine + methylecognine PB44MH Morphine PFCACT morphine,benzoylecgonine, methylecgonine PMG9F9 morphine, benzoylecgonine, methylecgonine PPPPYM morphine and benzoylecgonine Q6EK5S Methylecgonine QDJMOE Morphine, benzoilecogine and methylecgonine QPIOKN BZE and EME and morphine RFIBGP Morphine, benzoylecgonine, methylecgonine RQEEOE Benzoylecgonine,Methylecgonine and morphine RSYHBH buprenorphine and norbuprenorphine RXYG2Q Morphine and Benzoylecgonine U5AWA0 Morphine, Benzoylecgonine and Methylecgonine U8NKUE Morphine and Benzoylecgonine V8HYSI Morphine, Benzoylecgonine, Methylecgonine VAXCAO Methylecgonine VE1EEZ None VLA1JO morphine, benzoylecgonine W3E7JE MORPHINE, COCAINE WFA0FD morphine, benzoylecgonine and methylecgonine WVFKZV Methylecgonine XIKHP6 morphine, methylecgonine XZURKZ morphine, BZE YZOFYZ Morphine, Benzyl Ecgonine, Methyl Ecgonine Z25SYN Morphine and methylecgonine ZVTR4A Buprenorphine and norbuprenorphine

Statement of findings for Test Sample 2

Code Benzoylecgonine Methylecgonine Morphine (Total) 0O03BD - + - The test sample 2016/2/BS-2 was found to contain methylecgonine. 123WGB - + +

1PWJNH - + + We found Morphine and Methylecgonine in BS-2 1TTIML - - - We found also caffein.

3DKQOQ ANP + + Urine specimen contains 962.3 ng/mL Morphine. Methylecgonine is detected as well. 419F4M + + + Positive to benzoylecgonine and methylecgonine (cocaine main metabolites). Positive to morphine. 4444FB + + +

44TU44 + + + Sample is positive for Benzoylecgonine, Methylecgonine and Morphine 4GHNH4 + + +

4YLFBL + + + Positive to benzoylecgonine and methylecgonine (cocaine main metabolites). Positive to morphine. 66ZO6A + + +

6CVGQ6 + + + Morphine, Total- Detected > 0.5mg/L Benzoylecgonine- ~ 0.5mg/L Ecgonine Methyl Ester- ~ 0.4mg/L 6JIYPR + + + Hubo consumo de morfina 6V1XQX + + + This person consumed morphine and/or heroin and cocaine. 8IIDK3 + + + morphine (cf.above) BZE and EME are 2 metabolites of cocaine (controlled drug). their presence prove a cocaine absorption ALUS4Z + + +

AVERAC + + +

CQGC6C + + + In the sample labeled 2016/2/BS-2 Morphine, Benzoylecgonine and Methylecgonine were detected. CRKFUT + + + Consumption of cocaine and morphine DUZUY3 + + + The presence of Morphine in urine indicates consumption of the drug itself or the intake of other drugs. The presence of Benzoylecgonine and Methylecgonine in urine indicates Cocaine consumption.

Code Benzoylecgonine Methylecgonine Morphine (Total) DZKP99 + + + morphine can be issued from medical prescription or from heroin bze + eme issued from cocaine (only metabolites detected) EGCC8D + + + Sample BS2 found to contain morphine (measured value 1215 ng/ml), benzoylecgonine (measured value 1065 ng/ml), methylecgonine(measured value 410 ng/ml) EHOHKH + + + BENZOYLECGONINE, METHYLECGONINE ESTER AND MORPHINE DETECTED EP2WDI + ANP ANP

ERZR0K + - + Preliminary test followed by the analytical confirmation, then the quantification. EXR666 + + +

FFAFFI + + + In sample 2016/2/BS-2 was found an confirmed the presence of MORPHINE, BENZOYLECGONINE AND METHYLECGONINE FQFOEF + + + Morphine and Cocaine intake

FZ5ZGY + + + sample BS-2 contain morphine,methylecgonine,benzoilecgonine GIGLLN + ANP + Morphine use/abuse and cocaine abuse. GTUFSO + + +

GXURZK + ANP ANP Test sample 2016/2/BS-2 was found to contain controlled drugs for Benzoylecgonine therefore Positive for the Screening and Confirmatory Tests with concentration value of 621.79 ng/ml. HZ4SSF + + + - IGGUCG + + + The sample contains morphine, benzoylecgonine, methylecgonine. IGGZSA + + +

IKPH39 + + + BENZOYLECGONINE-TMS/ METHYL ECGONINE TMS/ MORPHINE DI-TMS DERIVATIVE IM9MIS + + + In the sample was detected Morphine, this finding indicates that Morphine was consumed. n the sample were detected Benzoylecgonine and Methylecgonine, this finding indicates that Cocaine was consumed. ITEOXF - - + Cocaine and Morphine were identified by GC-MS. J77027 ANP ANP ANP The test sample 2016/2/BS-2 shows a positive result over 2000 ng/mL for opiates/opioids and over 300 ng/mL for cocaine and/or metabolites. JHMWJW + - + coffeine, theophylline JL1GTU + + +

Code Benzoylecgonine Methylecgonine Morphine (Total) JPRPXO + + +

JYO93J - - - Examination and analyses performed on BS2 did not reveal any positive findings of toxicological significance. KFFG6N + + + Free morphine was detected at concentration of 1215.2 ng/mL, benzoylecgonine was detected at concentration of 630.9 ng/mL and methylecgonine was detected at concentration of 545.9 ng/mL in the 2016/2/BS-2 sample. KQ4LD7 - + - The specimen to contain Ecgonine methyl ester KSEXBG + - - specific extraction, identification with HPLC/DAD, confirmation by GC/MS using Tmcs derivatisation. the curve was realised with doping blank urine L6XLFB + + +

LALDP0 ANP + + use of cocaine, morphine LB5MQU + + + Morphine is a narcotic analgesic found in the opium poppy. It is a schedule II controlled substance in the United States. Benzoylecgonine and ecgonine methyl ester are an inactive metabolites of cocaine, which is a naturally occurring stimulant in the coca plant. Benzoylecgonine and ecgonine methyl ester are not controlled in the United states.

MDKNFX + + + Morphine. Cocaine metabolites: benzoylecgonine, methylecgonine MM3MAK + ANP + Morphine was found in the sample. The finding is in accordance with the intake of morphine or heroine, that metabolizes to morphine. Benzoylecgonine was in addition found in the sample. This is an inactive metabolite of cocaine, and shows the intake of cocaine. MQULMG - - - positive NNNKNN ANP ANP ANP cocaína metabolito: positivo opiáceos: positivo NOGTSO + + + Cocaine intake and morphine NW11JK ANP + ANP Ecgonine methyl ester was detected in the sample of 2016/2/BS-2 O55XS5 + + + Drugs detected, quantification was not performed OOIXLI + + + GC/MS: Relation m/z, time retention (tR ) the reference material methylecgonine, Benzoylecgonine, Morphine are equivalents to those sample 2016/2/BS-2 OSOXXO + ANP +

P45IGJ ANP + + after chemical analysis was performed the sample was contine 1245.5 morphine + 213.4 methylecognine

Code Benzoylecgonine Methylecgonine Morphine (Total) PB44MH ANP ANP + Sample BS-2 is positive for Morphine PFCACT + + + intake of morphine and cocaine PMG9F9 + + +

PPPPYM + ANP + morphine,benzoylecgonine and cafeine Q6EK5S - + ANP After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) and Gas Chromatography/Mass Spectrometry (GC/MS), was detected methylecgonine substance in the urine sample 2016/2/BS-2. QDJMOE + + + In the urine sample (2016-2/BS2) morphine, benzoilecogine and methylecgonine were found. QPIOKN + + + Consistent with use of cocaine and morphine or very pure heroin RFIBGP + + + Sample code number 2016/2/BS-2 was found to contain morphine (concentration 1229 ng/ml) and cocaine metabolites: benzoylecgonine (concentration 766 ng/ml), methylecgonine (concentration 389 ng/ml) RQEEOE + + +

RXYG2Q + - + Using EIA and GC-MS techniques, Morphine and Cocaine metabolite (Benzoylecgonine) were detected in the urine specimen which are considered as controlled drugs. U5AWA0 + + + Morphine, Benzoylecgonine and Methylecgonine are detected in urine by GC-MS U5T5NQ + + +

U8NKUE + ANP + confirms prior use of heroin/morphine and cocaine V8HYSI + + + Morphine, Benzoylecgonine, Methylecgonine VAXCAO - + - Methylecgonine was identified in the sample. VE1EEZ ANP ANP ANP Sample 2016/2/BS-2 found not to contain any drugs VLA1JO + + +

W3E7JE + + +

WFA0FD + + + presence of morphine and cocaine metabolites WVFKZV ANP + - Methylecgonine was detected in BS-2 sample. XIKHP6 - + +

Code Benzoylecgonine Methylecgonine Morphine (Total) XXMXQX - ANP -

XZURKZ ANP ANP ANP

YZOFYZ + + + Toxicological examination revealed the presence of morphine, benzyl ecgonine and methyl ecgonine. Z25SYN ANP + + Morphine and methylecgonine detected.

Code Buprenorphine Norbuprenorphine ZVTR4A + +

LMAFFM - +

1TZH5Y + ANP

RSYHBH + +

FVJJJE + +

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 89 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: 89

Benzoylecgonine: 60 Methylecgonine: 62 Morphine (Total): 66

False positives for Test Sample 2

Code Name Technique 1TIML Buprenorphine 150 419F4M 6-Monoacetylmorphine 230 6V1XQX Cocaine 180 ALUS4Z Cocaine 230/231 ITEOXF Cocaine 180 MQULMG Cocaine 110 W3E7JE Cocaine 180 AVERAC Cocaine 180

False negatives for BS-2 where no components were identified (technique(s) used or ANP) Code: 1TTIML (150), JYO93J (180), XXMXQX (110), MQULMG (110) 4 laboratories did not carry out analysis for any of the components present J77027, NNNKNN, XZURKZ, VE1EEZ

Frequency of use of screening and identification techniques: Response Summary

Participants 88 Technique 100 110 120 150 160 161 170 180 210 230 231 Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

(%) 3.4 54.5 4.5 2.3 1.1 3.4 0.0 25.0 12.5 3.4 10.2

Identification (No.) 0 5 1 5 0 6 1 71 3 6 35

(%) 0.0 5.7 1.1 5.7 0.0 6.8 1.1 80.7 3.4 6.8 39.8

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17 (%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 630 ng/ml Substance: BS‐2; Benzoylecgonine UNODC value = 690 ng/ml

4.00

3.00 2.8

2.0 2.00 1.7

1.2 1.2

1.00 0.8 0.6 0.6 0.6 0.5 0.5 0.5 0.2 0.3 0.0 0.1 0.1 6.7 0.00 ‐0.1 0.0 ‐0.2 ‐0.4 ‐0.4 ‐0.4 ‐0.3 ‐0.6 ‐0.6 ‐1.00 ‐1.0 ‐0.9 ‐1.1 ‐1.2 ‐1.5 ‐2.00

‐2.5 ‐2.4 ‐3.00 ‐2.8

‐4.00 6JIYPR 8IIDK3 4YLFBL L6XLFB V8HYSI RFIBGP HZ4SSF GIGLLN IGGZSA 4444FB YZOFYZ ERZR0K VLA1JO EXR666 JPRPXO KSEXBG 44TU44 XZURKZ CRKFUT FQFOEF KFFG6N 66ZO6A QPIOKN EP2WDI 6V1XQX GXURZK EGCC8D IGGUCG 6CVGQ6 PMG9F9 WFA0FD NOGTSO MDKNFX JHMWJW MM3MAK

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 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 signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

33 Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 348 ng/ml Substance: BS‐2; Methylecgonine UNODC value = 350 ng/ml

4.00 3.7

3.00

2.5

2.00 1.8

1.00 0.8 0.5 0.5 0.6 0.4 0.4 0.1 0.1 0.2 0.0 0.1 0.00

‐0.4 ‐0.7 ‐0.7 ‐0.7 ‐1.00 ‐0.8 ‐1.0

‐1.7 ‐2.00 ‐2.0

‐2.7 ‐3.00

‐4.00 6JIYPR 8IIDK3 P45IGJ 4YLFBL L6XLFB RFIBGP HZ4SSF IGGZSA 4444FB EXR666 44TU44 CRKFUT FQFOEF KFFG6N 66ZO6A QPIOKN 6V1XQX EGCC8D IGGUCG 6CVGQ6 PMG9F9 WFA0FD MDKNFX

34 Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1149 n g/ml Substance: BS‐2; Morphine UNODC value = 1138 ng/ml

4.00

3.0 3.00

2.3

2.00 1.5 1.3

0.9 1.00 0.7 0.7 0.7 0.6 0.4 0.4 0.5 0.5 0.3 0.0 0.0 0.0 0.00 ‐4.7 ‐0.1 ‐0.1 ‐0.3 ‐0.4 ‐0.5 ‐0.5 ‐0.6 ‐1.00 ‐1.1 ‐1.1 ‐1.1

‐1.5 ‐1.6 ‐2.00

‐3.00 ‐3.1

‐4.00 6JIYPR 8IIDK3 P45IGJ L6XLFB V8HYSI RFIBGP HZ4SSF GIGLLN IGGZSA YZOFYZ 4444FB VLA1JO ERZR0K EXR666 JPRPXO 44TU44 XZURKZ CRKFUT FQFOEF 66ZO6A 6V1XQX EGCC8D IGGUCG PMG9F9 WFA0FD NOGTSO PB44MH MDKNFX 3DKQOQ JHMWJW MM3MAK

35 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐2; Benzoylecgonine

Dispersion of z-scores using different analytical techniques for the quantification of benzoylecgonine in 2016/2 BS-2 10

0 z-score

-2

-4

-6

-8

HPLC GC‐MS LC‐MS -10

36 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐2; Methylecgonine

Dispersion of z-scores using different analytical techniques for the quantification of methylecgonine in 2016/2 BS-2 6

0 z-score

-2

-4

LC‐MS GC‐MS

-6

37 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐2; Morphine

Dispersion of z-scores using different analytical techniques for the quantification of morphine in 2016/2 BS-2 6

0 z-score

-2

-4 LC‐MS GC‐MS -6

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

Z-Scores for Test Sample 2

Benzoylecgonine Morphine Deviation Deviation Concentr Code Concentration from Code from z-score ation z-score (ng/ml) robust robust (ng/ml) average average 6JIYPR 42.2 -590 -2.8 JPRPXO 319 -830 -4.7 NOGTSO 100 -532 -2.5 WFA0FD 613 -536 -3.1 CRKFUT 116 -516 -2.4 XZURKZ 864 -285 -1.6 JPRPXO 317 -315 -1.5 MM3MAK 879 -270 -1.5 4YLFBL 365 -267 -1.2 FQFOEF 955 -194 -1.1 FQFOEF 392 -240 -1.1 6V1XQX 962 -187 -1.1 VLA1JO 420 -212 -1.0 3DKQOQ 962 -187 -1.1 GIGLLN 434 -198 -0.9 GIGLLN 1039 -110 -0.6 XZURKZ 501 -131 -0.6 JHMWJW 1058 -91 -0.5 JHMWJW 513 -119 -0.6 V8HYSI 1062 -87 -0.5 WFA0FD 544 -88 -0.4 L6XLFB 1075 -74 -0.4 6CVGQ6 544 -88 -0.4 4444FB 1097 -52 -0.3 IGGUCG 549 -83 -0.4 IGGZSA 1130 -19 -0.1 QPIOKN 558 -74 -0.3 PB44MH 1140 -9 -0.1 V8HYSI 585 -47 -0.2 HZ4SSF 1150 1 0.0 GXURZK 622 -10 -0.1 66ZO6A 1155 6 0.0 KFFG6N 631 -1 0.0 EXR666 1157 8 0.0 EP2WDI 635 3 0.0 VLA1JO 1200 51 0.3 MM3MAK 648 16 0.1 EGCC8D 1215 66 0.4 HZ4SSF 650 18 0.1 IGGUCG 1223 74 0.4 66ZO6A 680 48 0.2 YZOFYZ 1229 80 0.5 44TU44 694 62 0.3 RFIBGP 1229 80 0.5 4444FB 732 100 0.5 P45IGJ 1246 97 0.6 EXR666 735 103 0.5 MDKNFX 1265 116 0.7 YZOFYZ 748 116 0.5 6JIYPR 1270 121 0.7 6V1XQX 754 122 0.6 8IIDK3 1276 127 0.7 RFIBGP 766 134 0.6 NOGTSO 1310 161 0.9 8IIDK3 771 139 0.6 PMG9F9 1370 221 1.3 KSEXBG 809 177 0.8 44TU44 1417 268 1.5 MDKNFX 884 252 1.2 ERZR0K 1560 411 2.3 PMG9F9 898 266 1.2 CRKFUT 1668 523 3.0 IGGZSA 986 354 1.7 EGCC8D 1065 433 2.0 L6XLFB 1229 597 2.8 ERZR0K 2061 1429 6.7

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

Z-Scores for Test Sample 2

Methylecgonine Deviation Code Concentration from z-score (ng/ml) robust average 6JIYPR 135 -212 -2.7 FQFOEF 188 -159 -2.0 P45IGJ 213 -134 -1.7 QPIOKN 264 -83 -1.0 4YLFBL 282 -65 -0.8 L6XLFB 293 -54 -0.7 44TU44 293 -54 -0.7 MDKNFX 295 -52 -0.7 8IIDK3 312 -35 -0.4 HZ4SSF 350 3 0.0 6CVGQ6 352 5 0.1 IGGZSA 358 11 0.1 CRKFUT 359 12 0.1 66ZO6A 361 14 0.2 EXR666 377 30 0.4 WFA0FD 383 36 0.4 RFIBGP 389 42 0.5 4444FB 391 44 0.5 6V1XQX 392 45 0.6 EGCC8D 410 63 0.8 IGGUCG 488 141 1.8 KFFG6N 546 199 2.5 PMG9F9 645 298 3.7

Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 0O03BD MDMA 123WGB MDMA 1PWJNH MDMA 1TTIML None 1TZH5Y none 3DKQOQ MDMA 419F4M MDMA 44TU44 MDMA 4GHNH4 MDMA, methamphetamine 4YLFBL MDMA 66ZO6A MDMA 6CVGQ6 MDMA 6JIYPR Morfina - Metilecgonina-Benzoilecgonina 6V1XQX MDMA 8IIDK3 MDMA ALUS4Z MDMA AVERAC mdma CQGC6C 3,4-Methylenedioxymetamfetamine (MDMA) CRKFUT MDMA DUZUY3 MDMA DZKP99 MDMA EGCC8D MDMA EHOHKH 3,4-METHYLENEDIOXY-METHAMPHETAMINE (MDMA) EP2WDI MDMA ERZR0K 3, 4-Methylendioxymetamfetamine (MDMA) EXR666 MDMA FFAFFI (MDMA) 3,4-METHYLENEDIOXYMETAMFETAMINE FQFOEF MDMA FZ5ZGY MDMA GIGLLN MDMA GXURZK MDMA HZ4SSF 3,4-Methylenedioxymetamfetamine (MDMA) IGGUCG MDMA IGGZSA MDMA IM9MIS 3,4-Methylenedioxymetamfetamine ITEOXF 3,4-Methylenedioxymetamfetamine (MDMA) JHMWJW MDMA JL1GTU 3,4-Methylenedioxymetamfetamine (MDMA) JPRPXO MDMA, MDA KFFG6N MDMA

Code Identified Substances KQ4LD7 MDMA KSEXBG MDMA L6XLFB MDMA LALDP0 MDMA (3,4-Methylenedioxymetamfetamine) LB5MQU MDMA MDKNFX 3,4-Methylenedioxymethamfetamine (MDMA) MM3MAK MDMA MQULMG MDMA NNNKNN metanfetamina NOGTSO MDMA NW11JK 3,4-Methylenedioxy-metamfetamine (MDMA) O55XS5 3,4-Methylendioxy-metamfetamine (MDMA) OOIXLI 3,4-Methylenedioxymetamfetamine (MDMA) OSOXXO MDMA P45IGJ MDMA PB44MH MDMA PFCACT MDMA PMG9F9 MDMA PPPPYM MDMA Q6EK5S 3,4-methylenedioxy-metamfetamine (MDMA) QDJMOE 3,4-Methylenedioxy-methamfetamine (MDMA) QPIOKN MDMA RFIBGP MDMA RQEEOE MDMA RXYG2Q 3,4-Methylenedioxymetamfetamine (MDMA) U5AWA0 MDMA U8NKUE MDMA V8HYSI MDMA VAXCAO 3,4-methylendioxy-metamfetamine (MDMA) VE1EEZ 3,4-Methylenedioxymetamfetamine VLA1JO MDMA W3E7JE MDMA WFA0FD MDMA WVFKZV 3,4-Methylenedioxy-metamfetamine (MDMA) XIKHP6 MDMA XXMXQX MDMA XZURKZ MDMA YZOFYZ MDMA Z25SYN MDMA

Statement of findings for Test Sample 3

Code 3,4- Methylenedioxymet amfetamine (MDMA)

0O03BD + The test sample 2016/2/BS-3 was found to contain 3,4-Methylenedioxy metamfetamine (MDMA). 123WGB +

1PWJNH + We found MDMA in BS-3 1TTIML - We did not find any drugs.

3DKQOQ + MDMA is detected in Urine specimen. 419F4M + Positive to 3,4-Methylenedioxymetamfetamine (MDMA). 4444FB +

44TU44 + Sample is positive for 3,4-Methylenedioxymetamfetamine (MDMA) 4GHNH4 +

4YLFBL + Positive to 3,4-methylenedioximethamphetamine (MDMA). 66ZO6A +

6CVGQ6 + 3,4-methylenedioxy-N-methylamphetamine (MDMA)- Detected > 0.5mg/L 6JIYPR + Hubo consumo de Morfina y consumo de Cocaina 6V1XQX + This person consumed MDMA. 8IIDK3 + MDMA is a controlled narcotic in France that in consumed for its entactogenic, psychedelic and psychostimulant effects. ALUS4Z +

AVERAC +

CQGC6C + In the sample labeled 2016/2/BS-3 3,4-Methylenedioxymetamfetamine (MDMA) was detected. CRKFUT + Consumption of MDMA DUZUY3 + The presence of MDMA in urine indicates consumption of the drug itself. DZKP99 + from drug abuse

Code 3,4- Methylenedioxymet amfetamine (MDMA)

EGCC8D + Sample BS3 found to contain 3,4-Methylenedioxymetamfetamine (MDMA), measured value 1360 ng/ml EHOHKH + 3,4-METHYLENEDIOXY-METHAMPHETAMINE (MDMA) DETECTED EP2WDI + The urine was analysed and found to contain methylenedioxymethylamphetamine (MDMA). ERZR0K + Immunoassay test was performed, then confirmed by GC-MS, subsequently quantified. EXR666 +

FFAFFI + In sample 2016/2/BS-3 was found an confirmed the presence of (MDMA) 3,4-METHYLENEDIOXYMETAMFETAMINE FQFOEF + MDMA intake FVJJJE +

FZ5ZGY + sample BS-3 contain MDMA GIGLLN + Abuse of extasy. GTUFSO +

GXURZK + Test sample 2016/2/BS-3 was found to contain controlled drugs for MDMA therefore Positive for the Screening and Confirmatory Tests with concentration value of 1,876.46 ng/ml. HZ4SSF + - IGGUCG + The sample contains MDMA. IGGZSA +

IKPH39 + Methylenedioxymetamfetamine IM9MIS + In the sample was detected 3,4-Methylenedioxymetamfetamine, this finding indicates that 3,4- Methylenedioxymetamfetamine was consumed. ITEOXF + 3,4-Methylenedioxymetamfetamine (MDMA) was identified by GC-MS. J77027 ANP The test sample 2016/2/BS-3 does not show any group of substances (amphetamines, benzodiazepines, cannabinoids, cocaine or metabolites and opiates/opioids) over the cut-off. JHMWJW +

JL1GTU +

Code 3,4- Methylenedioxymet amfetamine (MDMA)

JPRPXO +

JYO93J - Examination and analyses performed on BS3 did not reveal any positive findings of toxicological significance. KFFG6N + MDMA was detected at concentration of 2589.9 ng/mL in the 2016/2/BS-3 sample. KQ4LD7 + The specimen to contain 3,4-Methylenedioxymethamphetamine (MDMA) KSEXBG + Specific extraction, identification with HPLC/DAD, confirmation by GC/MS using HFBA derivatisation. the curve was realised with doping blank urine L6XLFB +

LALDP0 + use of MDMA (3,4-Methylenedioxymetamfetamine) LB5MQU + MDMA is a synthetic stimulant drug in the amphetamine class. MDMA is a schedule I controlled substance in the United States.

MDKNFX + 3,4-Methylenedioxymethamfetamine (MDMA) MM3MAK + The sample was found to contain MDMA (extacy), which is a drug with stimulating and hallucinogenic effects. MQULMG + positive NNNKNN ANP metanfetamina: positivo NOGTSO + MDMA intake NW11JK + 3,4-Methylenedioxy-metamfetamine (MDMA) was detected in the sample of 2016/2/BS-3 O55XS5 + Drugs detected, quantification was not performed OOIXLI + GC/MS: Relation m/z, time retention (tR ) the reference material 3,4-Methylenedioxymetamfetamine (MDMA) are equivalents to those sample 2016/2/BS-3 OSOXXO +

P45IGJ + after chemical analysis was performed the sample was contine 297.9 MDMA PB44MH + Sample BS-3 is positive for MDMA PFCACT + intake of MDMA

Code 3,4- Methylenedioxymet amfetamine (MDMA)

PMG9F9 +

PPPPYM + MDMA and cafeine Q6EK5S + After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA), the High Performance Liquid Chromatography with diode array detection (HPLC/DAD) and Gas Chromatography/Mass Spectrometry (GC/MS), was 3,4-methylenedioxymetamfetamine (MDMA) substance in the urine sample 2016/2/BS-3. QDJMOE + In the urine sample (2016-2/BS3) 3,4-Methylenedioxy-methamfetamine (MDMA) was found. QPIOKN + Consistent with use of MDMA RFIBGP + Sample code number 2016/2/BS-3 was found to contain 3,4-Methylenedioxymetamfetamine (MDMA) (concentration 2632 ng/ml) RQEEOE +

RXYG2Q + Using EIA and LC-MS/MS techniques, MDMA was detected in the urine specimen which is considered as a controlled drug. U5AWA0 + MDMA is detected in urine by GC-MS U5T5NQ +

U8NKUE + confirms prior use of MDMA V8HYSI + MDMA VAXCAO + MDMA was identified in the sample. VE1EEZ + Sample 2016/2/BS-3 found to contain 3,4-Methylenedioxymetamfetamine VLA1JO +

W3E7JE +

WFA0FD + presence of MDMA WVFKZV + 3,4-Methylenedioxy-metamfetamine (MDMA) was detected in BS-3 sample. XIKHP6 +

XXMXQX +

Code 3,4- Methylenedioxymet amfetamine (MDMA)

XZURKZ ANP

YZOFYZ + Toxicological examination revealed the presence of MDMA Z25SYN + MDMA detected.

Code [blank sample] ZVTR4A + LMAFFM +

1TZH5Y + RSYHBH +

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 89 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: 89

3,4-Methylenedioxymetamfetamine 78 (MDMA):

False positives for Test Sample 3

Code Name Technique 4GHNH4 Metamfetamine 180 GTUFSO MDEA , MDA 180 JPRPXO MDA 180 6JIYPR Morphine, benzoylecgonine, methylecgonine N/A NNNKNN Metamfetamine 120

False negatives for BS-3 (technique(s) used or ANP) Code: 1TTIML (150), JYO93J (180), 3 laboratories did not carry out analysis for the component present J77027, NNNKNN, XZURKZ

Frequency of use of screening and identification techniques: Response Summary Participants 87 Technique 100 110 120 150 160 161 170 180 210 230 231 Screening (No.) 3 47 4 2 1 3 0 22 11 3 9 (%) 3.4 54.0 4.6 2.3 1.1 3.4 0.0 25.3 12.6 3.4 10.3 Identification (No.) 0 5 1 5 0 6 1 70 3 6 34 (%) 0.0 5.7 1.1 5.7 0.0 6.9 1.1 80.5 3.4 6.9 39.1 Quantification (No.) 0 1 0 0 0 3 0 21 0 2 17 (%) 0.0 2.7 0.0 0.0 0.0 8.1 0.0 56.8 0.0 5.4 45.9

Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 2012 ng/ml Substance: BS‐3; MDMA UNODC value = 1955 ng/ml

4.00

3.0 3.00

1.9 2.00 1.7

1.2 1.1 1.1 1.2 1.0 1.00 0.7 0.5 0.6 0.4 0.2 0.2 0.1 0.1 0.1 0.1 0.00 ‐5.2 ‐3.9 ‐3.8 ‐0.1 ‐0.1 0.0 0.0 ‐0.3 ‐0.2 ‐0.4 ‐0.4 ‐0.4 ‐0.7 ‐0.6 ‐1.00

‐1.5

‐2.00 ‐2.0

‐3.00 ‐2.8 ‐3.1

‐4.00 6JIYPR 8IIDK3 P45IGJ 4YLFBL L6XLFB V8HYSI RFIBGP HZ4SSF GIGLLN IGGZSA 4444FB YZOFYZ ERZR0K VLA1JO JPRPXO EXR666 44TU44 XZURKZ KSEXBG CRKFUT FQFOEF 66ZO6A KFFG6N QPIOKN 6V1XQX IGGUCG GXURZK EGCC8D PMG9F9 WFA0FD PB44MH NOGTSO XXMXQX MDKNFX JHMWJW MM3MAK

52 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐3; MDMA

Dispersion of z-scores using different analytical techniques for the quantification of MDMA in 2016/2 BS-3 6

0 z-score

-2

-4

Enzyme LC‐MS immunoassay HPLC GC‐MS -6

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

Z-Scores for Test Sample 3

MDMA Code Concentration Deviation from z-score (ng/ml) robust average P45IGJ 298 -1714.1 -5.2 FQFOEF 709 -1303 -3.9 JPRPXO 746 -1266 -3.8 XXMXQX 1001 -1011 -3.1 KSEXBG 1086 -926 -2.8 EGCC8D 1360 -652 -2.0 6JIYPR 1530 -482 -1.5 GIGLLN 1782 -230 -0.7 WFA0FD 1800 -212 -0.6 HZ4SSF 1875 -137 -0.4 GXURZK 1876 -135 -0.4 IGGZSA 1880 -132 -0.4 4YLFBL 1908 -104 -0.3 6V1XQX 1934 -78 -0.2 MM3MAK 1983 -29 -0.1 66ZO6A 1991 -21 -0.1 MDKNFX 1997 -15 0.0 EXR666 2000 -12 0.0 L6XLFB 2033 21 0.1 8IIDK3 2046 34 0.1 PMG9F9 2050 38 0.1 V8HYSI 2059 47 0.1 4444FB 2078 66 0.2 44TU44 2085 73 0.2 ERZR0K 2140 128 0.4 PB44MH 2177 165 0.5 NOGTSO 2200 188 0.6 IGGUCG 2255 243 0.7 JHMWJW 2342 330 1.0 QPIOKN 2375 363 1.1 XZURKZ 2380 368 1.1 VLA1JO 2400 388 1.2 YZOFYZ 2415 403 1.2 KFFG6N 2590 578 1.7 RFIBGP 2632 620 1.9 CRKFUT 3000 988 3.0

Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 0O03BD 2C-B 123WGB NEGATIVE 1PWJNH 2C-B 1TTIML 4-Bromo-2,5- dimethoxyphenethylamine (2C-B) 1TZH5Y 2 CB 44TU44 2C-B 4GHNH4 2C-B 4YLFBL 2C-B 66ZO6A 2C-B 6CVGQ6 2C-B 6V1XQX 2C-B 8IIDK3 2-CB CQGC6C None DUZUY3 4-Bromo-2-5-dimethoxyphenethylamine (2-CB) DZKP99 2CB EGCC8D 2C-B EHOHKH 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE (2C-B) EXR666 NEGATIVE FFAFFI (2-CB) 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE FQFOEF 2-CB FZ5ZGY - GIGLLN 2C-B HZ4SSF 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) IGGZSA 2C-B IM9MIS 4-Bromo-2,5-dimethoxyphenethylamine JHMWJW 2CB JL1GTU 4-Bromo-2,5-dimethoxyphenethylamine (2-CB) KFFG6N 2C-B KQ4LD7 2CB KSEXBG 2CB L6XLFB 2C-B LB5MQU 2C-B LMAFMM 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) MDKNFX 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) MM3MAK 2C-B NW11JK 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) O55XS5 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) PFCACT 2-CB QDJMOE 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) QPIOKN 2CB

Code Identified Substances RFIBGP 2C-B RQEEOE 2C-B RSYHBH 2-CG RXYG2Q 2C-B (4-Bromo-2,5-dimethoxyphenethylamine) U5AWA0 2C-B U8NKUE Morphine (indicated) V8HYSI 4-Bromo-2,5-dimethoxyphenethylamine VE1EEZ None VLA1JO 2-CB W3E7JE none found WFA0FD 2C-B WVFKZV 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) XIKHP6 2C-B XZURKZ 2C-B YZOFYZ 2 C-B Z25SYN 2C-B ZVTR4A 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

Statement of findings for Test Sample 4

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) 0O03BD + The test sample 2016/2/BS-4 was found to contain 4-bromo-2,5-dimethoxyphenthylamine (2C-B). 123WGB ANP

1PWJNH + We found 2C-B in BS-4 1TTIML + We found also Ephedrine. 1TZH5Y + positive to 2 CB 3DKQOQ ANP Drugs are not detected. 419F4M ANP Negative. 4444FB +

44TU44 + Sample is positive for 2C-B 4GHNH4 +

4YLFBL + Positive to 4-bromo-2,5-dimethoxyphenethylamine (2C-B). 66ZO6A +

6CVGQ6 + 4-Bromo 2,5-dimethoxyphenethylamine (2C-B)- Detected 6JIYPR ANP

6V1XQX + This person consumed 2C-B. 8IIDK3 + 2-CB is a controlled narcotic in France. It haspsychedelic effect similar to those of MDMA ALUS4Z -

AVERAC ANP

CQGC6C ANP In the sample labeled 2016/2/BS-4 no drugs were detected. CRKFUT ANP

DUZUY3 + The presence of 4-Bromo-2-5-dimethoxyphenethylamine (2-CB) in urine could come from he intake of the drug itself. DZKP99 + from drug abuse

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) EGCC8D + Sample BS4 found to contain 4-Bromo-2,5-dimethoxyphenethylamine (2C-B), measured value 1303 ng/ml EHOHKH + 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE (2C-B) DETECTED EP2WDI ANP The urine was analysed for common drugs of abuse with a negative result. ERZR0K - Immunoassay test was performed, then confirmed by GC-MS. EXR666 ANP

FFAFFI + In sample 2016/2/BS-4 was found an confirmed the presence of (2-CB) 4-BROMO-2,5- DIMETHOXYPHENETHYLAMINE FQFOEF + 2-CB intake FVJJJE +

FZ5ZGY ANP - GIGLLN + Abuse of 2C-B. GTUFSO +

GXURZK ANP Test sample 2016/2/BS-4 does not contain controlled drugs therefore Negative. HZ4SSF + - IGGUCG -

IGGZSA +

IKPH39 + 4-Bromo-2,5-dimetoxifenetilamina IM9MIS + In the sample was detected 4-Bromo-2,5-dimethoxyphenethylamine, this finding indicates that 4- Bromo-2,5-dimethoxyphenethylamine was consumed.

ITEOXF -

J77027 ANP The test sample 2016/2/BS-4 does not show any group of substances (amphetamines, benzodiazepines, cannabinoids, cocaine or metabolites and opiates/opioids) over the cut-off. JHMWJW +

JL1GTU +

JPRPXO -

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) JYO93J - Examination and analyses performed on BS4 did not reveal any positive findings of toxicological significance. KFFG6N + 2C-B was detected at concentration of 1489.7 ng/mL in the 2016/1/BS-4 sample.

KQ4LD7 + The specimen to contain 2,5-dimethoxy-4-bromophenethylamine (2CB) KSEXBG + Specific extraction, identification and confirmation by HPLC/DAD, the curve was realised with doping blank urine L6XLFB +

LALDP0 ANP

LB5MQU + 2C-B is a synthetic hallucinogen in the phenethylamine class. 2C-B is schedule I controlled substance in the United States. LMAFMM +

MDKNFX + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) MM3MAK + The sample was found to contain 2C-B, which is a designer drug with stimulating and hallucinogenic effects. MQULMG - negative NNNKNN ANP

NOGTSO -

NW11JK + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected in the sample of 2016/2/BS-4 O55XS5 + Drugs detected, quantification was not performed OOIXLI ANP

OSOXXO ANP

P45IGJ -

PB44MH ANP

PFCACT + intake of 2-CB PMG9F9 -

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) PPPPYM ANP cafeine Q6EK5S ANP After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA), High Performance Liquid Chromatography with diode array detection (HPLC/DAD) and Gas Chromatography/Mass Spectrometry (GC/MS), was not detected substances in the urine sample 2016/2/BS-4. QDJMOE + In the urine sample (2016-2/BS4) 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was found. QPIOKN + Consistent with use of 2CB RFIBGP + Sample code number 2016/2/BS-4 was found to contain 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) (concentration 1803 ng/ml) RQEEOE +

RSYHBH + Adverse Analytical Finding for 2-CB RXYG2Q + Using GC-MS as a screening and confirmatory techniques, psychedelic substance was found in the urine specimen which is considered to be as a controlled drug. U5AWA0 + 2C-B is detected in urine by GC-MS U5T5NQ +

U8NKUE ANP confirms prior use of heroin/morphine/codeine or the ingestion of poppy seeds (this is indicated only as < 5ng/ml spike) V8HYSI + 4-Bromo-2,5-dimethoxyphenethylamine VAXCAO - Not identified. VE1EEZ ANP Sample 2016/2/BS-4 found not to contain any drugs VLA1JO +

W3E7JE -

WFA0FD + presence of 2C-B WVFKZV + 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected in BS-4 sample. XIKHP6 +

XXMXQX ANP

XZURKZ ANP

Code 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) YZOFYZ + Toxicological examination revealed the presence of 2 C-B Z25SYN + 2C-B detected. ZVTR4A +

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 89 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: 89

4-Bromo-2,5-dimethoxyphenethylamine 54 (2C-B):

False positives for Test Sample 4

Code Name Technique U8NKUE Morphine (Total) 231

False negatives for BS-4 (technique(s) used or ANP) Code: PMG9F9 (231), NOGTSO (180), JPRPXO (180), ERZR0K (180), P45IGJ (180), VAXCAO (150/180), JYO93J (180), MQULMG (110), W3E7JE (180), ALUS4Z (230/231), ITEOXF (180), IGGUCG (180) 24 laboratories did not carry out analysis for the component present OSOXXO, XXMXQX, GXURZK, CQGC6C, EXR666, OOIXLI, XZURKZ, 3DKQOQ, CRKFUT, AVERAC, PB44MH, 419F4M, J77027, U8NKUE, Q6EK5S, VE1EEZ, 123WGB, EP2WDI, LALDP0, FZ5ZGY, PPPPYM, NNNKNN, 6JIYPR, FZ5ZGY

Frequency of use of screening and identification techniques:

Response Summary

Participants 89 Technique 100 110 120 150 160 161 170 180 210 230 231 Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

(%) 3.4 54.5 4.5 2.3 1.1 3.4 0.0 25.0 12.5 3.4 10.2

Identification (No.) 0 5 1 5 0 6 1 71 3 6 35 (%) 0.0 5.7 1.1 5.7 0.0 6.8 1.1 80.7 3.4 6.8 39.8

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17 (%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1513 n g/ml Substance: BS‐4; 2C‐B UNODC value = 1724 ng/ml

4.00

3.00

2.00 1.6

1.1 1.00 0.9 0.6 0.7 0.3 0.4 0.2 0.3 0.1 17.8 0.00 ‐0.1 ‐0.2 ‐0.4 ‐0.5 ‐1.00 ‐0.8 ‐0.8

‐1.2

‐1.7 ‐2.00 ‐2.1 ‐2.3

‐3.00

‐4.00 8IIDK3 L6XLFB RFIBGP HZ4SSF GIGLLN 4444FB IGGZSA VLA1JO 1TZH5Y KSEXBG XZURKZ 44TU44 FQFOEF 66ZO6A KFFG6N 6V1XQX EGCC8D WFA0FD MDKNFX JHMWJW MM3MAK z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 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 signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

66 Z‐Score Report per Sample per Substance

Round:2016/2 Substan BS‐4; 2C‐B

Dispersion of z-scores using different analytical techniques for the quantification of 2C-B in 2016/2 BS-4 6

0 z-score

-2

-4 HPLC GC‐MS LC‐MS

-6

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

Z-Scores for Test Sample 4

2C-B Deviation Code Concentration from z-score (ng/ml) robust average FQFOEF 510 -964 -2.4 KSEXBG 626 -848 -2.1 VLA1JO 790 -684 -1.7 WFA0FD 1010 -464 -1.2 GIGLLN 1160 -314 -0.8 XZURKZ 1174 -300 -0.7 EGCC8D 1303 -171 -0.4 L6XLFB 1345 -129 -0.3 MDKNFX 1414 -60 -0.1 KFFG6N 1490 16 0.0 44TU44 1574 100 0.2 IGGZSA 1620 146 0.4 8IIDK3 1644 170 0.4 4444FB 1658 184 0.5 MM3MAK 1684 210 0.5 66ZO6A 1777 303 0.8 RFIBGP 1803 329 0.8 HZ4SSF 1900 426 1.1 6V1XQX 1979 505 1.3 JHMWJW 2175 701 1.8

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