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

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report BIOLOGICAL SPECIMEN 2018/2

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 14 Summary Page 17 Z-Scores Page 18 Sample 2 Analysis Page 22 Identified substances Page 22 Statement of findings Page 24 Identification methods Page 28 Summary Page 31 Z-Scores Page 32 Sample 3 Analysis Page 35 Identified substances Page 35 Statement of findings Page 37 Identification methods Page 41 Summary Page 44 Z-Scores Page 45 Sample 4 Analysis Page 48 Identified substances Page 48 Statement of findings Page 50 Identification methods Page 54 Summary Page 57 Z-Scores Page 58

Test Samples Information

Samples Comments on samples Sample 1 To prepare BS-1, urine was spiked with methanolic solutions of Buprenorphine HCl (570ng base/ml) and Norbuprenorphine (580ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised Sample 2 To prepare BS-2, urine was spiked with an aqueous solution of Tenamfetamine HCl (1150ng 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 Mephedrone HCl (479ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 4 To prepare BS-4, urine was spiked with an aqueous solution of Morphine sulphate (580ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Samples Substances Concentrations Comments on substances Sample 1 Buprenorphine 570 ng/ml Norbuprenorphine 580 ng/ml Sample 2 Tenamfetamine (MDA) 1150 ng/ml Sample 3 Mephedrone 479 ng/ml Sample 4 Morphine (Total) 580 ng/ml

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 2018/2 round of the ICE programme, results were submitted within both the Sei zed Materials (SM) and Biological Specimens (BS) test groups by 231 laboratories in 77 countries. Within the BS test group, results were submitted by 82 laboratories from 46 countries and within the SM test group, there were 194 participating laboratories from 69 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the BS test group were immunoassays (67% of participants), while GC-MS (78%) 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 table 1.

BS-2 BS-1 BS-1 BS-3 BS-4 Test sample Tenamfetamine Buprenorphine Norbuprenorphine Mephedrone Morphine (MDA) Correct 67% 48% 81% 47% 80% identification At least 1 drug: 68% Number of false 2 10 4 5 positives Number of false 10 8 17 11 negatives Number of analyses not 16 7 26 5 performed (ANP)

Table 1. Qualitative performance of participants in the 2018/2 round of ICE.

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

In general, the number of false positives reported for the four test samples has increased slightly from previous round. 6 laboratories found reported amfetamine for BS-2 (MDA). The number of false negative results and analyses not performed for buprenorphine and mephedrone in BS-1 and BS-3 respectively are concerning. Laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken as soon as possible 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 2018/2 round of ICE contained a total of five components and 38 (46%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to note that 78% of laboratories quantified at least two components and 52% performed quantification of at least three test sample. LC/MS(/MS), used by 57% of participants, was the most commonly used technique for quantitation, followed by, GC-MS which was used by 55% of participants. z-scores obtained by participants in quantification are shown in the table below (percentage + no. of labs indicated).

Test sample BS-2 z-score BS-1 BS-1 BS-3 BS-4 Tenamfetamine Buprenorphine Norbuprenorphine Mephedrone Morphine (MDA) |z| < 2, 87% (21) 87% (14) 87% (27) 85% (17) 84% (30) satisfactory 2 ≤ | z| ≤ 3, 0% (0) 13% (2) 6.5% (2) 0% (0) 8% (3) questionable |z| > 3, 13% (3) 0% (0) 6.5% (2) 15% (3) 8% (3) unsatisfactory

Table 2. Quantitative performance of participants in the 2018/2 round of ICE.

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 as soon as possible.

Of the 4 laboratories that obtained a single action or warning signal in ICE rounds 2017/2 and 2018/1, all 4 participated in 2018/2 and 2 of these improved their performance in quantitation. The laboratories IN9RUR and YCH0DH also obtained action or warning signals in 2018/2.

The following laboratories obtained a single action signal or warning signal in the two successive rounds of 2018/1 and 2018/2 and shall take this as anomaly, which requires further investigation: A0OXAA, IN9RUR and YCH0DH.

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 .

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New Psychoactive Substances (NPS) reported by laboratories participating in the 2018/2 round of the ICE programme

During the 2018/2 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 175 reports of 116 substances. The most commonly reported substances were synthetic cannabinoids (35%) followed by synthetic cathinones as shown in figure 1.

Phencyclidine-type Tryptamines substances 2% 6%

Phenethylamines 9% Synthetic cannabinoids 35%

Other substances 22%

Synthetic cathinones 26%

Figure 1. NPS reported by ICE laboratories during the 2018/2 round of IC E

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances reported were synthetic cannabinoid receptor agonists (SCRA) (35%), while 34% were stimulants as shown in figure 2.

Sedatives/Hypnotics Others 5% 3%

Dissociatives Synthetic 5% cannabinoid receptor agonists 35% Opioids 8%

Hallucinogens 10%

Stimulants 34%

Figure 2. Mode of action of NPS reported by ICE participants in the 2018/2 round of ICE

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

NPS most commonly reported by laboratories participating in ICE 2018/2

The substances most often reported by ICE participants was ketamine followed equally by the synthetic cannabinoid receptor agonists 5F-MDMB-PINACA (methyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)- 3,3-dimethylbutanoate and 5F-MDMB-PICA (methyl 2-(1-(5-fluoropentyl)-1H-indole-3-carboxamido)-3,3- dimethylbutanoate.

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

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Sample 1 Analysis

Identified substances for Test Sample 1

Code Identified Substances 00000O Norbuprenorphine 1HEGK1 no 2KL95S Buprenorphine 2UHVZC Buprenorphine 3WPSZE Buprenorphine, norbuprenorphine 3ZOOHF Buprenorphine, norbuprenorfine 4NNLPS buprenorphine and norbuprenorphine 4XHLLX Buprenorhine+Norbup. 6Z2TA9 Buprenorphine, Norbuprenorphine 777IU7 Buprenorphine 8WW6WW Buprenorphine 9MWBRW Buprenorphine, Norbuprenorphine A0OXAA buprenorphine AOALOI Buprenorphine + Norbuprenorphine BYZEPB buprenorphine, norbuprenorphine BZSSB8 Buprenorphine & Norbuprenorphine CUNPOI buprenorphine and norbuprenorphine D33SRV it was not detected D4772O buprenorphine and nor-buprenorphine DDY2DD Buprenorphine and Norbuprenorphine E47YBI BUPRENORPHINE AND NORBUPRENORPHINE EBDJXR Buprenorphine and Norbuprenorphine FEA6EH Buprenorphine and metabolite GGTDYG Buprenorphine, Norbuprenorphine H8FZWN NO DRUGS FOUND HOLD90 Buprenorphine and norbuprenorphine HSWKUL Burprenorphine and Norbuprenorphine IN9RUR buprenorphine, norbuprenorphine JFTVTM Presumptive positive for buprenorphine JPOZ8N Buprenorphine, Norbuprenorphine KDZKKK Buprenorphine,norbuprenorphine KTKKKF NONE KRRRN6 Buprenorphine LE41AE Methadone,Buprenorphine,Norbuprenorphine LLFN8Z Buprenorphine, Norbuprenorphine LM8PKA Buprenorphine and Norbuprenorphine M777NY Norbuprenorphine, buprenorphine MAH4QP Buprenorphine, Norbuprenorphine MCACFX Buprenophine and Norbuprenophine MDVYFO GHB and Cafaine

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Code Identified Substances O7OFOO caffeine OD2E2Y buprenorphine OXYY2Y Buprenorphine and norbuprenorphine. P6DPPB buprenorphine (and metabolite norbuprenorphine) PDXSBK Buprenorphine, Norbuprenorphine PHPXWP Buprenorphine, Norbuprenorphine PKPP6Z buprenorphine QZQQJK Buprenorphine,Norbuprenorphine RKBNUU buprenorphine ROX4OE caffeine RTTT7I Buprenorphine T4ABZZ Buprenorphine URVVJU Buprenorphine UUYZCH Buprenorphine WWWLML Buprenorphine, Norbuprenorphine XHGD6Q buprenorphine and norbuprnorphine XTHTTP Buprenorphine YCH0DH Buprenorphine YZTBB3 Buprenorphine + Norbuprenorphine ZXDXXD Opiates

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Statement of findings for Test Sample 1

Code Buprenorphine Norbuprenorphine 00000O - + Analytical adverse finding for norbuprenorphine 0OG0ZF ANP ANP

1HEGK1 ANP ANP Methylecgonine, norketamine, buprenorphine and GBL are not measured 2KL95S + ANP Buprenorphine detected 2UHVZC + +

3WPSZE + + This person consumed buprenorphine. 3ZOOHF + + no 4NNLPS + + Presence of buprenorphine and its metabolite 4XHLLX + + Sample positive for buprenorphine and metabolite 5XCFLX ANP ANP

6Z2TA9 + +

71IHN1 ANP ANP

72FDEJ - - Listed drugs could not be detected in the test sample 2018/2/BS-1. 777IU7 + ANP BS-1 was screened positive for Buprenorphine 8RXHHN - ANP

8WW6WW + ANP Buprenorphine was detected in BS-1 sample. 9D9AM9 - ANP

9MWBRW + + The presence of buprenorphine and its metabolite in urine indicates the intake of buprenorphine. A0OXAA + ANP detoxication treatment AOALOI + + Screening 161Tech Confirmation 180 Tech BYZEPB + + buprenorphine, norbuprenorphine BZSSB8 + + Buprenorphine & Norbuprenorphine were identified by GC-MS C55QDO ANP ANP

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Code Buprenorphine Norbuprenorphine CJKDKK - -

CUNPOI + +

D33SRV ANP ANP a spot was seen but not detected D4772O + + Nor-buprenorphine: only cualitative results DDY2DD + + No comments DGSFEM ANP ANP

E47YBI + +

E62NRW ANP ANP

EBDJXR + + The presence of Buprenorphine and norbuprenorphine in the sample indicates buprenorphine consumption. EJ94XN ANP ANP The sample has negative results for : BARBITURATES, BENZODIAZEPINES, CANNABINOIDS, COCAINE and/or METABOLITES, OPIATES/OPIOIDS. FEA6EH + + Findings are consistent with the use of buprenorphine. FSFDFS ANP ANP No common drugs were detected in sample 2018/2/BS-1. GCFZSF - -

GGTDYG + + Drug result: Buprenorphine, Norbuprenorphine. Indicative of opioid consumption. H8FZWN ANP ANP caffeine HOLD90 + + We found buprenorphine as a psychotropic substance and norbuprenorphine as an uncontrolled drugs based on INCB Green List regulation. HSWKUL + + Burprenorphine is an opioid used to treat pain and opioid addiction. In the United States buprenorphine is a Schedule III substance. Norbuprenorphine is an active metabolite of buprenorphine and is not scheduled in the United States. IN9RUR + + positive JFTVTM + ANP Presumptive positive was obtained for buprenorphine, however this was not unequivocally confirmed JPOZ8N + +

KDZKKK + + Sample 2018/2/BS-1 contain buprenorphine, norbuprenorphine. KRRRN6 + - In the sample was detected Buprenorphine, this finding indicates that Buprenorphine was consumed.

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Code Buprenorphine Norbuprenorphine KTKKKF ANP ANP SAMPLE 2018/2/BS-1 FOUND NOT TO CONTAIN ANY DRUGS LE41AE + + The drugs detected are synthetic opioids.Methadone is being used as a treatment for addiction to other opioids.Buprenorpine is used to treat opioid addiction,acute and chronic pain.Norbuprenorphine is the active metabolite of buprenorphine. LJJTNL + +

LLFN8Z + + Buprenorphine, Norbuprenorphine LM8PKA + + In urine sample nº 1, buprenorphine e norbuprenorphine were identified. M777NY + +

MAH4QP + + The sample contains drugs MCACFX + + Opioid drugs MDVYFO ANP ANP after chemical analysis was performed the sample was contained GHB and Cafaine N4VNND ANP ANP

N8S888 - -

O7OFOO - - Caffeine is a xanthine stimulant. OD2E2Y + -

OKMKHO - -

OOIA3T - ANP

OXYY2Y + + The sample contains buprenorphine and norbuprenorphine. P6DPPB + +

PDXSBK + + Buprenorphine Detected Norbuprenorphine Detected PHPXWP + + Sample is positive for Buprenorphine and Norbuprenorphine. PKPP6Z + -

QZQQJK + + - RKBNUU + - the sample contains buprenorphine, a narcotic analgesic drug. ROX4OE ANP ANP

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Code Buprenorphine Norbuprenorphine RTTT7I + ANP Buprenorphine detected. T4ABZZ + - Sample BS-1 containing 609Ng/Ml of Buprenorphine TCLLL5 - - No drugs detected using Gas Chromatography/Mass Spectrometry (GCMS) URVVJU + ANP Buprenorphine, which is an analgesic opioid, was found in the urine, but the metabolites buprenorphine glucuronide and norbuprenorphine glucuronide was not found, this could indicate a manipulated sample if it came from a real donor. UUYZCH + ANP Buprenorphine therapy or abuse. WWWLML + +

XHGD6Q + + Buprenorphine is a semi-synthetic opioid analgesic used for the substitutive management of opiate dependant individuals. It is mainly metabolized by N-dealkylation into norbuprenorphine. XTHTTP + ANP

XY777I + +

YCH0DH + ANP Caffeine YD4O4O + +

YZTBB3 + + Buprenorphine and it's metabolite Norbuprenorphine ZTYWOT ANP ANP Test sample 2018/2/BS-1 does not contain controlled drugs therefore Negative for Screening and Confirmatory analyses. ZXDXXD + - Buprenorfine

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Identification methods for Test Sample 1

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

Analytical Technique Codes Code 100 110 120 150 161 170 171 180 230 231 210 00000O SI SI 0OG0ZF S I 2KL95S I 2UHVZC I I 3WPSZE S I I 3ZOOHF I I 4NNLPS SI S SI 4XHLLX S I 5XCFLX S I I 6Z2TA9 S I S I 71IHN1 S I 72FDEJ SI 777IU7 SI I 8RXHHN S I I 8WW6W S I W 9D9AM9 SI I 9MWBRW S I SI A0OXAA SI AOALOI SI I SI Immunochimique.ochromatog raphique BYZEPB SI SI BZSSB8 S I C55QDO S I CJKDKK S I CUNPOI S I I D33SRV SI D4772O S I I DDY2DD S I I DGSFEM I E47YBI S I E62NRW S I EBDJXR I SI S lateral flow inmnunochromatographic assay EJ94XN S

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Code 100 110 120 150 161 170 171 180 230 231 210 FEA6EH S I SI FSFDFS SI GCFZSF S SI GGTDYG SI H8FZWN S I I HOLD90 S I I HSWKUL I LC-QTOF IN9RUR I SI SFC-MS/MS JFTVTM SI SI JPOZ8N S I LC/QTOF KDZKKK S I KRRRN6 I S Lateral Flow Immunoassay KTKKKF SI LE41AE S I I LJJTNL S I I I LLFN8Z I I I Kinetic Interactions of Microparticles LM8PKA I M777NY S I I SI MAH4QP S I SI MCACFX I I S chemical immunoessay techniques MDVYFO S SI N4VNND I SI S randox N8S888 I I TRIAGE8, ALERE Cup O7OFOO SI SI OD2E2Y S I I OKMKHO I I S Immunoassay Techniques OOIA3T S I OXYY2Y SI P6DPPB I SI PDXSBK S I I PHPXWP S I S LC-TOF PKPP6Z S I SI QZQQJK SI RKBNUU S I ROX4OE S I RTTT7I S I I T4ABZZ S I I TCLLL5 I

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Code 100 110 120 150 161 170 171 180 230 231 210 URVVJU S SI UUYZCH I I S WWWLM S I SI L XHGD6Q S I I I XTHTTP S SI I SI XY777I S I I YCH0DH S I YD4O4O S I I YZTBB3 I S immunoassay test ZTYWOT I I S DTK ZXDXXD I SI Buprenorfine Dipro Drug lab screen

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RESPONSE SUMMARY FOR TEST SAMPLE 1

Participants: 82

The response summary of all 82 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:

Substance Name Number of laboratories correctly identifying: Buprenorphine 55 Norbuprenorphine 40

False positives for Test Sample-1:

Round Code Substance Reported Tech Code LE41AE Methadone 231 MDVYFO gamma -Hydroxybutyric acid 180

False negatives for Test Sample-1:

Round Code Tech Code 72FDEJ 180 8RXHHN 180 9D9AM9 150, 180 CJKDKK 150 GCFZSF 180 N8S888 180 O7OFOO 180, 231 OKMKHO 150, 180 OOIA3T 180 TCLLL5 180

Analysis not performed for Test Sample-1:

0OG0ZF, 1HEGK1, 5XCFLX, 71IHN1, C55QDO, D33SRV, DGSFEM, E62NRW, EJ94XN, FSFDFS, H8FZWN, KTKKKF MDVYFO, N4VNND, ROX4OE and ZTYWOT.

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 82

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

Screening (No.) 2 45 1 0 3 0 1 0 0 0 15 12 3 15 (%) 2.4 54.9 1.2 0.0 3.7 0.0 1.2 0.0 0.0 0.0 18.3 14.6 3.7 18.3 Identification (No.) 0 3 0 0 8 0 7 2 1 0 64 1 9 33 (%) 0.0 3.7 0.0 0.0 9.8 0.0 8.5 2.4 1.2 0.0 78.0 1.2 11.0 40.2 Quantification (No.) 0 0 0 0 0 1 0 0 0 0 7 0 2 13 (%) 0.0 0.0 0.0 0.0 0.0 4.2 0.0 0.0 0.0 0.0 29.2 0.0 8.3 54.2

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Z-Score Report per Sample per Substance:

Round: 2018/2 Substance: BS-1; Buprenorphine Robust average: 626 ng/ml UNODC value: 570 ng/ml

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

that requires investigation.

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Z-Score Report per Sample per Substance:

Round: 2018/2 Substance: BS-1; Norbuprenorphine Robust average: 553 ng/ml UNODC value: 580 ng/ml

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

that requires investigation.

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Z-Score Report per Sample per Substance:

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Z-Scores for Test Sample 1

Buprenorphine Norbuprenorphine Deviation Deviation Code Concentration from Code Concentration from z-score z-score (mass%) robust (mass%) robust average average 4XHLLX 20.0 -606.0 -1.8 4XHLLX 40.0 -513.0 -2.3 4NNLPS 136.0 -490.0 -1.5 QZQQJK 225.0 -328.0 -1.5 2UHVZC 153.3 -472.8 -1.4 2UHVZC 352.0 -201.0 -0.9 CUNPOI 260.0 -366.0 -1.1 DDY2DD 406.0 -147.0 -0.7 M777NY 344.0 -282.0 -0.9 FEA6EH 487.0 -66.0 -0.3 QZQQJK 400.0 -226.0 -0.7 CUNPOI 49 0.0 -63.0 -0.3 DDY2DD 435.0 -191.0 -0.6 PHPXWP 496.0 -57.0 -0.3 UUYZCH 454.0 -172.0 -0.5 XHGD6Q 528.0 -25.0 -0.1 FEA6EH 542.0 -84.0 -0.3 LLFN8Z 534.0 -19.0 -0.1 PHPXWP 561.0 -65.0 -0.2 3WPSZE 550.0 -3.0 0.0 LLFN8Z 601.0 -25.0 -0.1 XY777I 654.0 10 1.0 0.5 T4ABZZ 609.0 -17.0 -0.1 4NNLPS 678.0 125.0 0.6 3WPSZE 626.0 0.0 0.0 MAH4QP 780.0 227.0 1.0 XY777I 668.0 42.0 0.1 M777NY 781.0 228.0 1.0 XTHTTP 715.7 89.7 0.3 6Z2TA9 980.0 427.0 1.9 XHGD6Q 716.0 90.0 0.3 WWWLML 1003.0 450.0 2.0 A0OXAA 781 .0 155.0 0.5 URVVJU 802.0 176.0 0.5 D4772O 850.0 224.0 0.7 MAH4QP 890.0 264.0 0.8 OXYY2Y 1075.0 449.0 1.4 6Z2TA9 1890.0 1264.0 3.8 WWWLML 1971.0 1345.0 4.1 YCH0DH 9017.0 8391.0 25.6

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Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 00000O MDA 0OG0ZF MDA 1HEGK1 MDA 2KL95S Tenamfetamine 2UHVZC Mephedrone 3WPSZE MDA 3ZOOHF Tenamfetamine/MDA/ 4NNLPS MDA 4XHLLX MDA 5XCFLX MDA 6Z2TA9 MDA 71IHN1 MDA 777IU7 Tenamfetamine (MDA) 8RXHHN MDA, Buphenorphine 8WW6WW Tenamfetamine (MDA) 9MWBRW MDA A0OXAA MDA AOALOI Amphetamine BYZEPB MDA BZSSB8 Amfetamine & Tenamfetamine (MDA) C55QDO Tenamfetamine CJKDKK Amphétamine, Méthamphétamine CUNPOI MDA D33SRV amfetamine D4772O MDA DDY2DD MDA E47YBI MDA E62NRW amphetamines EBDJXR MDA FEA6EH Methylenedioxyamphetamine FSFDFS Tenamfetamine (MDA) GCFZSF MDA GGTDYG MDA H8FZWN NO DRUGS FOUND HOLD90 Tenamfetamine HSWKUL MDA IN9RUR MDA JFTVTM MDA JPOZ8N MDA KDZKKK MDA

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

Code Identified Substances KRRRN6 Tenamfetamine KTKKKF TENAMFETAMINE (MDA) LE41AE MDA LLFN8Z MDA LM8PKA Tenamfetamine M777NY MDA MAH4QP MDA MCACFX Mephedrone and Tenamfetamine (MDA) MDVYFO MDA,Amfetamine and cafaine N8S888 MDA O7OFOO Tenamfetamine (MDA) OD2E2Y tenamfetamine(MDA) OKMKHO 3,4 Methylenedioxymetanfetamina (MDMA) OOIA3T Tenamfetamine (MDA) OXYY2Y Tenamfetamine (MDA) P6DPPB MDA PDXSBK MDA PHPXWP MDA PKPP6Z MDA QZQQJK Tenamfetamine (MDA) RKBNUU tenamfetamine (MDA) ROX4OE MDA, caffeine, theobromine RTTT7I Tenamfetamine (MDA) T4ABZZ MDA TCLLL5 Tenamfetamine (MDA) URVVJU MDA UUYZCH MDA WWWLML Tenamfetamine (MDA) XHGD6Q MDA XTHTTP Tenamfetamine YCH0DH Precusors of Sintesis de MDA, MDMA: N-formyl-MDA, 3,4MDP2P YZTBB3 Tenamfetamine ZXDXXD Amfetamine type stimulans

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Statement of findings for Test Sample 2

Code Tenamfetamine (MDA) 00000O + Analytical adverse finding for MDA 0OG0ZF +

1HEGK1 ANP

2KL95S + Tenamfetamine (MDA) detected 2UHVZC -

3WPSZE + This person consumed MDA. 3ZOOHF + no 4NNLPS + Presence of MDA (methylendioxyamphetamine) 4XHLLX + Sample positive for tenamfetamine 5XCFLX + Indicates use of Tenamfetamine (MDA). 6Z2TA9 +

71IHN1 + The urine was analysed and found to contain MDA. 72FDEJ - Listed drugs could not be detected in the test sample 2018/2/BS-2. 777IU7 + BS-2 was positive for Tenamfetamine (MDA) 8RXHHN +

8WW6WW + Tenamfetamine (MDA) was detected in BS-2 sample. 9D9AM9 -

9MWBRW + The presence of MDA in urine indicates the intake of MDA. A0OXAA + MDA abuse AOALOI ANP Confirmation by 180 Analytical code BYZEPB + MDA BZSSB8 + Amfetamine & Tenamfetamine (MDA) were identified by GC-MS C55QDO + Toxicological examination revealed the presence of Tenamfetamine

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Code Tenamfetamine (MDA) CJKDKK -

CUNPOI +

D33SRV ANP a spot with amfetamine s Rf was detected D4772O -

DDY2DD + No comments DGSFEM ANP

E47YBI +

E62NRW ANP

EBDJXR + The presence of MDA in the sample indicate consumption of MDA itself or consupmtion of MDMA. MDA is a metabolite of MDMA. EJ94XN ANP The sample has negative results for : BARBITURATES, BENZODIAZEPINES, CANNABINOIDS, COCAINE and/or METABOLITES, OPIATES/OPIOIDS. FEA6EH + Findings are consistent with use of MDA. FSFDFS + Tenamfetamine (MDA) was detected in sample 2018/2/BS-2. GCFZSF + It was detected the presence of MDA GGTDYG + Drug result: MDA. H8FZWN ANP caffeine HOLD90 + We found Tenamfetamine (MDA) as a psychotropic substance based on INCB Green List regulation. HSWKUL + 3,4-Methylenedioxyamphetamine(MDA)isacentralnervoussystemstimulantandalsoa metabolite of MDMA and MDEA. MDA is a Schedule I substance in the United States. IN9RUR + positive JFTVTM + The urine specimen was found to contain MDA, demonstrating the prior ingestion of MDA or possibly MDEA JPOZ8N +

KDZKKK + Sample 2018/2/BS-2 contain 3,4-metilendioxiamphetamine(MDA). KRRRN6 + In the sample was detected Tenamfetamine, this finding indicates that Tenamfetamine was consumed.

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Code Tenamfetamine (MDA) KTKKKF + SAMPLE 2018/2/BS-2 FOUND TO CONTAIN TENAMFETAMINE (MDA) LE41AE + MDA is a psychotropic amphetamine derivative.It is a minor metabolite of MDMA.It can also be found at low conentrations in MDMA tablets. LJJTNL +

LLFN8Z + MDA LM8PKA + In urine nº 2, tenamfetamine was identified. M777NY +

MAH4QP + The sample contains drugs MCACFX + Narcotic drugs MDVYFO + after chemical analysis was performed the sample was contained MDA and Amfetamine N4VNND -

N8S888 +

O7OFOO + Tenamfetamine (MDA) is a stimulant. OD2E2Y +

OKMKHO - La sustancia encontrada fue obtenida mediante GS-MS OOIA3T +

OXYY2Y + The sample contains Tenamfetamine (MDA). P6DPPB +

PDXSBK + Methylenedioxyamphetamine Detected > 1mg/L PHPXWP + Sample is positive for MDA. PKPP6Z +

QZQQJK + - RKBNUU + the sample contains tenamfetamine (MDA), an amphetamine type stimulant drug. ROX4OE +

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Code Tenamfetamine (MDA) RTTT7I + Tenamfetamine (MDA) detected. T4ABZZ + Sample BS-2 Containing 1290 Ng/Ml of MDA TCLLL5 + Tenamfetamine detected using GCMS. URVVJU + The sample was found to contain MDA, which is a drug with stimulating and hallucinogenic effects. The finding could be due to intake of MDA or as a metabolite after MDMA (extacy) intake. UUYZCH + Tenamphetamine abuse. WWWLML +

XHGD6Q + 3,4-Methylenedioxyamphetamine (MDA), is an empathogen-entactogen, psychostimulant, and psychedelic drug of the amphetamine family that is encountered mainly as a recreational drug. Due to its euphoriant and hallucinogenic effects, the drug is a controlled substance and its possession and sale are illegal in France. MDA is also a primary metabolite, the product of hepatic N-dealkylation of MDMA (ecstasy). XTHTTP +

XY777I +

YCH0DH - Caffeine, Theobromine

YD4O4O +

YZTBB3 + tenamfetamine ZTYWOT ANP Test sample 2018/2/BS-2 does not contain controlled drugs therefore Negative for Screening and Confirmatory analyses. ZXDXXD - MDMA, Amfetamine

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Identification methods for Test Sample 2

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

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

RESPONSE SUMMARY FOR TEST SAMPLE 2

Participants: 82

The response summary of all 82 participating laboratories for the identification of BS-2, frequency of use of screening and identification techniques and false positives and negatives:

Correct Identification of Test Sample-2:

Substance Name Number of laboratories correctly identifying: Tenamfetamine (MDA) 67

False positives for Test Sample-2:

Round Code Substance Reported Tech Code 2UHVZC Mephedrone 230, 231 8RXHHN Buprenorphine 180 AOALOI Amfetamine 161, 180 BZSSB8 Amfetamine 180 CJKDKK Amfe tamine, Metamfetamine 150 D33SRV Amfetamine 150 MCACFX Mephedrone 161, 180 MDVYFO Amfetamine 180 OKMKHO 3,4 -methylenedioxymetamfetamine (MDMA) 150, 180 ZXDXXD 3,4 -Methylenedioxymetamfetamine (MDMA), 150 Amfetamine

False negatives for Test Sample-2:

Round Code Tech Code Round Code Tech Code 2UHVZC 230, 231 N4VNND 170 72FDEJ 180 OKMKHO 150, 180 9D9AM9 150, 180 YCH0DH 180 CJKDKK 150 ZXDXXD 150

Analysis not performed for Test Sample-2:

AOALOI, D33SRV, DGSFEM, E62NRW, EJ94XN, H8FZWN and ZTYWOT.

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 82

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

Screening (No.) 2 45 1 0 3 0 1 0 0 0 15 12 3 15 (%) 2.4 54.9 1.2 0.0 3.7 0.0 1.2 0.0 0.0 0.0 18.3 14.6 3.7 18.3 Identification (No.) 0 3 0 0 8 0 7 2 1 0 64 1 9 33 (%) 0.0 3.7 0.0 0.0 9.8 0.0 8.5 2.4 1.2 0.0 78.0 1.2 11.0 40.2 Quantification (No.) 0 0 0 0 0 0 0 0 0 0 15 1 3 11 (%) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 48.4 3.2 9.7 35.5

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INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Score Report per Sample per Substance:

Round: 2018/2 Substance: BS-2; Tenamfetamine (MDA) Robust average: 1080 ng/ml UNODC value: 1150 ng/ml

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 occurred that requires investigation.

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Z-Score Report per Sample per Substance:

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

Z-Scores for Test Sample 2

Tenamfetamine (MDA) Deviation Code Concentration from z-score (mass%) robust average N8S888 373.0 -707.0 -2.5 6Z2TA9 650.0 -430.0 -1.5 DDY2DD 690.0 -390.0 -1.4 4XHLLX 700.0 -380.0 -1.3 MDVYFO 718.0 -362.0 -1.3 WWWLML 755.0 -325. 0 -1.1 OXYY2Y 792.7 -287.3 -1.0 MAH4QP 820.0 -260.0 -0.9 ROX4OE 950.0 -130.0 -0.5 LLFN8Z 992.0 -88.0 -0.3 1HEGK1 993.0 -87.0 -0.3 UUYZCH 1003.0 -77.0 -0.3 URVVJU 1032.0 -48.0 -0.2 D4772O 1053.7 -26.3 -0.1 3WPSZE 1073.0 -7.0 0.0 M777NY 1111.0 31.0 0.1 PHPXWP 1125.0 45.0 0.2 FEA6EH 1153.0 73.0 0.3 4NNLPS 1167.0 87.0 0.3 XTHTTP 1171.7 91.7 0.3 5XCFLX 1181.8 101.8 0.4 QZQQJK 1210.0 130.0 0.5 XY777I 1283.0 203.0 0.7 T4ABZZ 1290.0 210.0 0.7 XHGD6Q 1297.0 217.0 0.8 8RXHHN 1301.0 221.0 0.8 777I U7 1306.3 226.3 0.8 JPOZ8N 1357.0 277.0 1.0 A0OXAA 1921.0 841.0 3.0 CUNPOI 2200.0 1120.0 3.9 IN9RUR 2573.0 1493.0 5.3

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Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 00000O mephedrone 1HEGK1 mephedrone 2UHVZC MDA, Ketamine 3WPSZE Mephedrone 3ZOOHF no 4NNLPS mephedrone 6Z2TA9 Mephedrone, Methcathinone 9MWBRW Mephedrone A0OXAA mephedrone AOALOI Mephedrone BYZEPB MEPHEDRONE BZSSB8 Mephedrone & gamma-Hydroxybutyric acid (GHB) CUNPOI 4-MMC (mephedrone) D4772O mephedrone DDY2DD Mephedrone GCFZSF Mephedrone H8FZWN NO DRUGS FOUND HOLD90 Mephedrone HSWKUL Mephedrone IN9RUR mephedrone JFTVTM Mephedrone JPOZ8N Mephedrone KDZKKK mephedrone KTKKKF NONE LE41AE MEPHEDRONE LLFN8Z 4-methylmethcathinone LM8PKA - M777NY Mephedrone MAH4QP Mephedrone MCACFX gamma-Hydroxybutyric acid (GHB) MDVYFO Cafaine O7OFOO Caffeine OD2E2Y mephedrone OXYY2Y Mephedrone P6DPPB mephedrone PDXSBK Mephedrone QZQQJK Mephedrone RKBNUU mephedrone ROX4OE caffeine RTTT7I -

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Code Identified Substances URVVJU Mephedrone UUYZCH Mephedrone WWWLML Mephedrone XHGD6Q Mephedrone XTHTTP Mephedrone YZTBB3 Mephedrone ZXDXXD none

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Statement of findings for Test Sample 3

Code Mephedrone 00000O + Analytical adverse finding for mephedrone 0OG0ZF ANP

1HEGK1 ANP

2KL95S ANP Drug not detected 2UHVZC -

3WPSZE + This preson consumed mephedrone. 3ZOOHF - no 4NNLPS + Presence of mephedrone (4-MMC) 4XHLLX ANP Sample is negative for tested substances 5XCFLX ANP

6Z2TA9 +

71IHN1 ANP

72FDEJ - Listed drugs could not be detected in the test sample 2018/2/BS-3. 777IU7 ANP BS-3 was negative for the screened drugs of abuse 8RXHHN ANP

8WW6WW ANP No drugs detected in BS-3 sample 9D9AM9 ANP

9MWBRW + The presence of mephedrone in urine indicates the intake of mephedrone. A0OXAA + mephedrone consumption AOALOI + 161 and 180 Analytical code BYZEPB + MEPHEDRONE BZSSB8 + Mephedrone & gamma-Hydroxybutyric acid (GHB) were identified by GC-MS C55QDO - No drugs were detected

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Code Mephedrone CJKDKK -

CUNPOI +

D33SRV ANP

D4772O +

DDY2DD +

DGSFEM ANP

E47YBI ANP NEGATIVE E62NRW ANP

EBDJXR ANP

EJ94XN ANP The sample has negative results for : BARBITURATES, BENZODIAZEPINES, CANNABINOIDS, COCAINE and/or METABOLITES, OPIATES/OPIOIDS. FEA6EH ANP

FSFDFS ANP No common drugs were detected in sample 2018/2/BS-3. GCFZSF + It was detected the presence of Mephedrone GGTDYG ANP No targeted drugs detected. H8FZWN ANP CAFFEINE HOLD90 + We found Mephedrone as a psychotropic substance based on INCB Green List regulation. HSWKUL + Mephedrone is a psychoactive phenethylamine derivative that is structurally related to methcathinone and amphetamine. In the United States it is a Schedule I substance. IN9RUR + positive JFTVTM + The urine specimen was found to contain mephedrone demonstrating the prior ingestion of the drug. JPOZ8N +

KDZKKK + Sample 2018/2/BS-3 contain mephedrone. KRRRN6 ANP

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Code Mephedrone KTKKKF ANP SAMPLE 2018/2/BS-3 FOUND NOT TO CONTAIN ANY DRUGS LE41AE + Mephedrone is a NPS and belongs to the cathinone group.It is an illicit substance since 2007. LJJTNL +

LLFN8Z + 4-methylmethcathinone LM8PKA - In urine nº 3 no drugs were identified. M777NY +

MAH4QP + The sample contains drugs MCACFX - Synthetic drug MDVYFO - after chemical analysis was performed the sample was contained Cafaine N4VNND ANP

N8S888 -

O7OFOO - caffeine is a xanthine stimulant. OD2E2Y +

OKMKHO -

OOIA3T -

OXYY2Y + The sample contains mephedrone. P6DPPB +

PDXSBK + Mephedrone Detected PHPXWP - Sample contains no substances from ICE menu. PKPP6Z ANP

QZQQJK + - RKBNUU + the sample contains mephedrone, a synthetic stimulant drug of the cathinone class. ROX4OE ANP

RTTT7I ANP Common drugs not detected

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Code Mephedrone T4ABZZ -

TCLLL5 - No drugs detected using GCMS. URVVJU + The sample was found to contain mephedrone, which is a designer drug (synthetic cathinone) with stimulating effects. UUYZCH + Mephedrone abuse. WWWLML +

XHGD6Q + Mephedrone, also known as 4-methyl methcathinone (4-MMC) or 4-methyl ephedrone, is a synthetic stimulant drug of the cathinone classe. It is classified as an illegal drug in France since 2010. XTHTTP +

XY777I +

YCH0DH - Caffeine, Theobromine

YD4O4O +

YZTBB3 + Mephedrone ZTYWOT ANP Test sample 2018/2/BS-3 does not contain controlled drugs therefore Negative for Screening and Confirmatory analyses. ZXDXXD - We did not find any drugs

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

Identification methods for Test Sample 3

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

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

RESPONSE SUMMARY FOR TEST SAMPLE 3

Participants: 82

The response summary of all 82 participating laboratories for the identification of BS-3, frequency of use of screening and identification techniques and false positives and negatives:

Correct Identification of Test Sample-3:

Substance Name Number of laboratories correctly identifying: Mephedrone 39

False positives for Test Sample-3:

Round Code Substance Reported Tech Code 2UHVZC Ketamine, Tenamfetamine (MDA) 230, 231 BZSSB8 gamma -Hydroxybutyric acid (GHB) 180 MCACFX gamma -Hydroxybutyric acid (GHB) 161, 180 N8S888 Buprenorphine 180

False negatives for Test Sample-3:

Round Code Tech Code Round Code Tech Code 2UHVZC 230 , 231 O7OFOO 180 , 231 3ZOOHF 150 , 180 OKMKHO 150 , 180 72FDEJ 180 OOIA3T 180 C55QDO 180 PHPXWP 180 CJKDKK 150 T4ABZZ 180, 231 LM8PKA 231 TCLLL5 180 MCACFX 161 , 180 YCH0DH 180 MDVYFO 180 ZXDXXD 150 N8S888 180

Analysis not performed for Test Sample-3:

0OG0ZF, 2KL95S, 4XHLLX, 5XCFLX, 71IHN1, 777IU7, 8RXHHN, 8WW6WW, 9D9AM9, D33SRV, DGSFEM, E47YBI, E62NRW, EBDJXR, EJ94XN, FEA6EH, FSFDFS, GGTDYG, H8FZWN, KTKKKF, KRRRN6, N4VNND, PKPP6Z, ROX4OE, RTTT7I and ZTYWOT.

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 82

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

Screening (No.) 2 45 1 0 3 0 1 0 0 0 15 12 3 15 (%) 2.4 54.9 1.2 0.0 3.7 0.0 1.2 0.0 0.0 0.0 18.3 14.6 3.7 18.3 Identification (No.) 0 3 0 0 8 0 7 2 1 0 64 1 9 33 (%) 0.0 3.7 0.0 0.0 9.8 0.0 8.5 2.4 1.2 0.0 78.0 1.2 11.0 40.2 Quantification (No.) 0 0 0 0 0 0 1 0 0 0 6 1 1 10 (%) 0.0 0.0 0.0 0.0 0.0 0.0 5.0 0.0 0.0 0.0 30.0 5.0 5.0 50.0

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Z-Score Report per Sample per Substance:

Round: 2018/2 Substance: BS-3; Mephedrone Robust average: 329 ng/ml UNODC value: 479 ng/ml

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

that requires investigation.

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Z-Score Report per Sample per Substance:

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

Z-Scores for Test Sample 3

Mephedrone Deviation Code Concentration from z-score (mass%) robust average CUNPOI 70.0 -259.0 -2.0 A0OXAA 77.0 -252.0 -1.9 DDY2DD 118.0 -211.0 -1.6 QZQQJK 245.0 -84.0 -0.6 3WPSZE 261.0 -68.0 -0.5 D4772O 273.0 -56.0 -0.4 4NNLPS 285.0 -44.0 -0.3 JPOZ8N 288.0 -41.0 -0.3 UUYZCH 304.0 -25.0 -0.2 URVVJU 317.0 -12.0 -0.1 OXYY2Y 320.0 -9.0 -0.1 M777NY 349.0 20.0 0.1 XTHTTP 351.8 22.8 0.2 XHGD6Q 409.0 80.0 0.6 IN9RUR 412.0 83.0 0.6 1HEGK1 418.0 89.0 0.7 XY777I 450.0 121.0 0.9 WWWLML 746.0 417.0 3.2 MAH4QP 750.0 421.0 3.2 6Z2TA9 920.0 591.0 4.5

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Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 00000O morphine 0OG0ZF morphine 1HEGK1 morphine 2KL95S Morphine 2UHVZC Morphine 3WPSZE Morphine 3ZOOHF no 4NNLPS morphine 4XHLLX Morphine 5XCFLX Morphine 6Z2TA9 Morphine 71IHN1 Morphine 8RXHHN Morphine 8WW6WW Morphine 9D9AM9 MDMA (N-Methyl-3,4-methylenedioxyamphetamine), Morphine 9MWBRW Morphine A0OXAA morphine AOALOI 06MAM BYZEPB MORPHINE BZSSB8 6-Monoacetylmorphine (6-MAM) & Morphine (Total) CJKDKK MAM, Codéine CUNPOI morphine D4772O Morphine DDY2DD Morphine DGSFEM morphine E47YBI MORPHINE TOTAL E62NRW opiates EJ94XN OPIATES FEA6EH Morphine GCFZSF Morphine GGTDYG Morphine H8FZWN MORPHINE HOLD90 Morphine HSWKUL Morphine IN9RUR morphine JFTVTM Morphine JPOZ8N Morphine KDZKKK morphine KRRRN6 Morphine-3-O-glucuronide KTKKKF NONE

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

Code Identified Substances LE41AE MORPHINE LLFN8Z Morphine LM8PKA Morphine M777NY Morphine MAH4QP Morphine MCACFX Morphine MDVYFO Morphine and cafiene N4VNND Morphine N8S888 MORPHINE OKMKHO Mofina OXYY2Y Morphine P6DPPB morphine PDXSBK Morphine PHPXWP Morphine PKPP6Z morphine QZQQJK Morphine (Total) RKBNUU morphine ROX4OE morphine, caffeine RTTT7I Morphine T4ABZZ Morphine URVVJU Morphine UUYZCH Morphine WWWLML Morphine XHGD6Q Morphine XTHTTP Morphine YCH0DH MORPHINE YZTBB3 Morphine ZTYWOT Morphine (Total) ZXDXXD Opiates

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Statement of findings for Test Sample 4

Code Morphine (Total) 00000O + Analytical adverse finding for morphine 0OG0ZF +

1HEGK1 ANP

2KL95S + Morphine detected 2UHVZC +

3WPSZE + This person consumed morphine. 3ZOOHF - no 4NNLPS + Presence of morphine 4XHLLX + Sample positive for morphine 5XCFLX + Since morphine was detected - Indicates use of morphine. 6Z2TA9 +

71IHN1 + The urine was analysed and found to contain Morphine. 72FDEJ - Listed drugs could not be detected in the test sample 2018/2/BS-4. 777IU7 - BS-4 was negative for the screened drugs of abuse 8RXHHN +

8WW6WW + Morphine was detected in BS-4 sample 9D9AM9 +

9MWBRW + The presence of morphine in urine indicates the intake of morphine, or heroin. A0OXAA + drug treatment AOALOI ANP 161and 180 analytical code BYZEPB + MORPHINE BZSSB8 + 6-Monoacetylmorphine (6-MAM) & Morphine (Total) were identified by GC-MS C55QDO ANP

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Code Morphine (Total) CJKDKK -

CUNPOI +

D33SRV -

D4772O +

DDY2DD +

DGSFEM + use of morphine E47YBI +

E62NRW + morphine EBDJXR -

EJ94XN ANP The sample has negative results for : BARBITURATES, BENZODIAZEPINES, CANNABINOIDS, COCAINE and/or METABOLITES, OPIATES/OPIOIDS. it has a positive results for OPIATES which for a confirmatory test is requiered. FEA6EH + Findings are consistent with the use of morphine or heroin. FSFDFS ANP No common drugs were detected in sample 2018/2/BS-4. GCFZSF + It was detected the presence of Morphine GGTDYG + Drug result: Morphine. Please note that the presence of morphine in urine may occur as a result of the consumption of poppy seed products, medications containing codeine and/or morphine, or illicit drugs. H8FZWN - CAFFEINE HOLD90 + We found Morphine as a narcotics substance based on INCB Yellow List regulation. HSWKUL + Morphine is narcotic analgesic found in the opium poppy. It is a Schedule II substance in the United States. IN9RUR + positive JFTVTM + The urine specimen was found to contain morphine, demonstrating the prior ingestion of morphine, or more commonly heroin, which breaks down (metabolises) in the body to morphine JPOZ8N +

KDZKKK + Sample 2018/2/BS-4 contain morphine.

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

Code Morphine (Total) KRRRN6 + In the sample was detected Morphine-3-O-glucuronide, this finding indicates that Morphine consumed. KTKKKF ANP SAMPLE 2018/2/BS-4 FOUND NOT TO CONTAIN ANY DRUGS LE41AE + Morphine is a narcotic analgesic.It is the primary constituent of crude opium.It is a control drug and it is prescribed for the treatment of severe pain.Morphine is also the metabolite of codeine and heroin. LJJTNL +

LLFN8Z + Morphine LM8PKA + In urine nº 4, morphine was identified. M777NY +

MAH4QP + The sample contains drugs MCACFX + Opioid drug MDVYFO + after chemical analysis was performed the sample was contained Morphine and Cafaine N4VNND + There was Morphine consumption. N8S888 +

O7OFOO - Examination and analysis performed on 2018/BS-4 did not reveal any positive findings of toxicological significance OD2E2Y -

OKMKHO - La sustancia fue detectada mediante tecnica de inmunoensayo (test Screening), no pudo ser detectada mediante Cromatografia de Gases Masas y cromatografia de capa fina OOIA3T -

OXYY2Y + The sample contains morphine. P6DPPB +

PDXSBK + Morphine, total Detected ~ 0.5mg/L PHPXWP + Sample is positive for Morphine. PKPP6Z +

QZQQJK + -

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

Code Morphine (Total) RKBNUU + the sample contains morphine, a narcotic analgesic drug. ROX4OE +

RTTT7I + Morphine detected. T4ABZZ + Sample BS-4 containing 619 Ng/Ml of Morphine TCLLL5 - No drugs detected using GCMS URVVJU + Morphine is detected in urine. This indicates intake of morphine, or heroine which is metabolized to morphine in the body. Morphine is an analgesic opiate. UUYZCH + Morphine therapy is the most probable (other alkaloids are not identified). WWWLML +

XHGD6Q + Morphine is a pain medication (analgesic effect) of the opiate family. Morphine is an alkaloid molecule extracted from opium. It acts directly on the central nervous system to decrease the feeling of pain. XTHTTP +

XY777I +

YCH0DH + Caffeine, Theobromine

YD4O4O +

YZTBB3 + Morphine ZTYWOT + Test sample 2018/2/BS-4 was found to contain controlled drugs for Morphine (Total) therefore Positive for the Screening and Confirmatory analyses with concentration value of 621.08 ng/ml. ZXDXXD + Morphine

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

Identification methods for Test Sample 4

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

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

RESPONSE SUMMARY FOR TEST SAMPLE 4

Participants: 82

The response summary of all 82 participating laboratories for the identification of BS-4, frequency of use of screening and identification techniques and false positives and negatives:

Correct Identification of Test Sample-4:

Substance Name Number of laboratories correctly identifying: Morphine 66

False positives for Test Sample-4:

Round Code Substance Reported Tech Code 9D9AM9 3,4 -Methylenedioxymetamfetamine (MDMA) 150 , 180 AOALOI 6-Monoacetylmorphine (6 -MAM) 161 , 180 BZSSB8 6-Monoacetylmorphine (6 -MAM) 180 CJKDKK 6-Monoacetylmorphine (6 -MAM), codeine 150 KRRRN6 Morphine -3-O-glucuronide 180

False negatives for Test Sample-4:

Round Code Tech Code Round Code Tech Code 3ZOOHF 150 , 180 O7OFOO 180 , 231 72FDEJ 180 OD2E2Y 230 777IU7 110 OKMKHO 150 , 180 CJKDKK 150 OOIA3T 180 D33SRV 150 TCLLL5 180 EBDJXR 231

Analysis not performed for Test Sample-4:

AOALOI, C55QDO, EJ94XN, FSFDFS and KTKKKF.

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 82

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

Screening (No.) 2 45 1 0 3 0 1 0 0 0 15 12 3 15 (%) 2.4 54.9 1.2 0.0 3.7 0.0 1.2 0.0 0.0 0.0 18.3 14.6 3.7 18.3 Identification (No.) 0 3 0 0 8 0 7 2 1 0 64 1 9 33 (%) 0.0 3.7 0.0 0.0 9.8 0.0 8.5 2.4 1.2 0.0 78.0 1.2 11.0 40.2 Quantification (No.) 0 0 0 0 0 0 0 0 0 0 19 1 2 12 (%) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 52.8 2.8 5.6 33.3

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

Z-Score Report per Sample per Substance:

Round: 2018/2 Substance: BS-4; Morphine Robust average: 494 ng/ml UNODC value: 580 ng/ml

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

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 occurred that requires investigation.

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

Z-Score Report per Sample per Substance:

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

Z-Scores for Test Sample 4

Morphine Deviation Code Concentration from z-score (mass%) robust average DDY2DD 151.0 -343.0 -2.8 M777NY 320.0 -174.0 -1.4 1HEGK1 334.0 -160.0 -1.3 2UHVZC 334.8 -159.2 -1.3 6Z2TA9 380.0 -114.0 -0.9 3WPSZE 384.0 -110.0 -0.9 UUYZCH 385.0 -109.0 -0.9 ROX4OE 395.0 -99.0 -0.8 BYZEPB 400.0 -94.0 -0.8 5XCFLX 401.9 -92.1 -0.7 WWWLML 406.0 -88.0 -0.7 XY777I 433.0 -61.0 -0.5 8RXHHN 443.0 -51.0 -0.4 FEA6EH 451.0 -43.0 -0.3 00000O 455.0 -39.0 -0.3 QZQQJK 465.0 -29.0 -0.2 D4772O 468.9 -25.1 -0.2 URVVJU 474.0 -20.0 -0.2 LLFN8Z 478.0 -16.0 -0.1 PDXSBK 486.0 -8.0 -0.1 N8S888 521.0 27.0 0.2 PHPXWP 525.0 31.0 0.2 CUNPOI 530.0 36.0 0.3 XHGD6Q 539.0 45.0 0.4 JPOZ8N 547.0 53.0 0.4 4XHLLX 550.0 56.0 0.4 XTHTTP 610.7 116.7 0.9 T4ABZZ 619.0 125.0 1.0 ZTYWOT 621.1 127.1 1.0 4NNLPS 629.0 135.0 1.1 MAH4QP 680.0 186.0 1.5 OXYY2Y 774.2 280.2 2.2 A0OXA A 829.0 335.0 2.7 IN9RUR 1090.0 596.0 4.8 MDVYFO 1214.0 720.0 5.8 N4VNND 6195.0 5701.0 45.8

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

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