INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

Home , Camazepam, Delorazepam, Medazepam, Nordazepam

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

BIOLOGICAL SPECIMENS 2017/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 2 Comments from the International Panel of Forensic Experts Page 2 NPS reported by ICE participants Page 4 Codes and Abbreviations Page 6 Sample 1 Analysis Page 7 Identified substances Page 7 Statement of findings Page 8 Identification methods Page 11 Summary Page 14 Sample 2 Analysis Page 15 Identified substances Page 15 Statement of findings Page 18 Identification methods Page 23 Summary Page 26

Z- Scores Page 27 Sample 3 Analysis Page 37 Identified substances Page 37 Statement of findings Page 39 Identification methods Page 44 Summary Page 47

Z- Scores Page 48 Sample 4 Analysis Page 51 Identified substances Page 51 Statement of findings Page 54 Identification methods Page 59 Summary Page 62

Z- Scores Page 63 Test Samples Information

Samples Comments on samples Sample 1 BS-1 was a blank urine test sample containing no substances from the ICE menu.

Sample 2 To prepare BS-2, urine was spiked with an aqueous solution of amfetamine sulphate (1270ng base/ml) and methanol solutions of nordazepam (1960ng base/ml), oxazepam (570ng/ml) and temazepam (580ng/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 gamma-hydroxybutyric acid (GHB) (16560ng/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 (860ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Samples Substances Concentrations Comments on substances Sample 1 [blank sample] Sample 2 Amfetamine 1270 ng/ml Nordazepam 1960 ng/ml Oxazepam 570 ng/ml Temazepam 580 ng/ml Sample 3 gamma-Hydroxybutyric acid (GHB) 16560 ng/ml Sample 4 Morphine 860 ng/ml

2 2017/1-BS Copyright (c) 2017 UNODC 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 Biological Specimens (BS) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact. Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2017/1 round of the ICE programme, results were submitted within both the Seized Materials (SM)and Biological Specimens (BS) test groups by 238 laboratories in 76 countries. Within the SM test group, there were 201 participating laboratories from 68 countries and within the BS test group, results were submitted by 96 laboratories from 45 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the BS test group were enzyme immunoassays (56% of participants), while GC-MS (84%) was the most commonly used technique for identification/confirmation of the components in the test samples. The results for the qualitative identification of the sample components in the BS test group, the number of false positive/negative results and the analyses not performed are shown in table 1.

Table 1. Qualitative performance of participants in the 2017/1 round of ICE.

BS-1 BS-2 BS-2 BS-2 BS-2 Test sample (Blank) (Amfetamine) (Nordazepam) (Oxazepam) (Temazepam) Correct 99% 88% 94% 63% 75% identification Number of false 1 7 positives Number of false - 0 negatives Number of analyses not - 3 performed (ANP)

BS -3 BS-4 Test sample (GHB ) ( Morphine ) Correct 34% 88% identification Number of false 0 positives 7 1 Number of false 14 4 negatives Number of analyses not 49 6 performed (ANP)

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 2017/1 round of ICE contained a total of six components and 43 (46%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to note that 93% of laboratories quantified at least two components and 37% performed quantification of all components present. GC-MS was used by 49% of participants for quantification, followed by LC/MS(/MS), which was used by 33% of participants. z-scores obtained by participants in quantification are shown in the table below (percentage + no. of labs indicated).

Table 2. Quantitative performance of participants in the 2017/1 round of ICE.

Test sample z-score BS-2 BS-2 BS-2 (Amfetamine) (Nordazepam) (Oxazepam) |z| < 2, satisfactory 86% (31) 86% (31) 82% (23) 2 ≤ |z| ≤ 3, 6% (2) 6% (2) 4% (1) questionable |z| > 3, 8% (3) 8% (3) 14% (4) unsatisfactory

z-score BS-2 (Temazepam) BS-3 (GHB) BS-4 (Morphine)

|z| < 2, satisfactory 77% (28) 84% (16) 77% (30) 2 ≤ |z| ≤ 3, 6% (2) 5% (1) 13% (5) questionable |z| > 3, 3% (1) 11% (2) 10% (4) unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation. Participants with z-scores outside acceptable limits should review their quantification procedures.

In the 2016/2 round of ICE, ten laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Eight of these laboratories participated and performed quantification in the 2017/1 round with six laboratories improving their performance in quantitation for at least one substance. Four of these laboratories also obtained questionable z-scores and five of these laboratories also obtained unsatisfactory z-scores in their quantitative performance in 2017/1. Nine laboratories obtained unsatisfactory z-scores in ICE 2016/2 with |z| ≥ 3. Of these laboratories, five participated in ICE 2017/1 and performed quantification, with 4 (80%) improving their performance to obtain satisfactory z-scores. Three of these laboratories also obtained questionable z-scores and two of these laboratories also obtained unsatisfactory z-scores in their quantitative performance in 2017/1.

The following laboratories obtained a single action signal or warning signal in the two successive rounds of 2016/2 and 20167/1 and shall take this as anomaly, which requires further investigation: UTSOWL, 3FMD3X, 8MFF1T, AMMRSO, DDA5D2, IQJAM7, NDP7T7 and VLHXHH.

Laboratories that need to perform quantitation routinely are encouraged to participate regularly in external proficiency testing or collaborative exercises such as the ICE programme. This will enable laboratories to assess the quality of their quantitative methods through the z-score values obtained. Laboratories reporting false positive or false negative results should investigate the root causes and corrective actions taken promptly in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. UNODC would like to acknowledge the valuable contribution of the Chemical Metrology Laboratory of the Health Sciences Authority, Singapore, for the provision of specific software used for the quantitative statistical calculations in the ICE programme.

4 New Psychoactive Substances (NPS) reported by laboratories participating in the 2017/1 round of the ICE programme.

During the 2017/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 148 reports of 93 substances. The most commonly reported substances were synthetic cathinones (36%) followed by synthetic cannabinoids (25%) as shown in figure 1.

5% 3% 25% 8% Synthetic cannabinoids

Synthetic cathinones

Others

Phenethylamines

Ketamine and phencyclidine type substances 23% Tryptamines

36%

Figure 1. NPS reported by ICE laboratories during the 2017/1round of ICE

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (50%), while 16% were synthetic cannabinoid receptor agonists (SCRA’s) and 13% were synthetic opioids as shown in figure 2. 2% 8%

Stimulants

11% SCRA's

Opioids

Hallucinogens 50% Dissociatives 13% Sedatives/Hypnotics

16%

Figure 2. Mode of action of NPS most commonly reported by ICE participants in the 2017/1 round of ICE

NPS most commonly reported by laboratories participating in ICE 2017/1.

The substance most often reported by ICE participants was the synthetic cathinone ephylone (N- ethylpentylone) followed by the synthetic opioid U-47700 (3,4-dichloro-N-((1S,2S)-2- (dimethylamino)cyclohexyl)-N-methylbenzamide). This is the first time a synthetic opioid has been among the substances most reported by ICE participants. U-47700 was placed under International Control (Schedule I of the Single Convention on Narcotic Drugs of 1961) at the 2017 Meeting of the Commission on Narcotic Drugs. The decision became effective on 22 April 2017.

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. https://www.unodc.org/LSS/Home/ICE

6 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 3FMD3X GHB 8LCBAB none AMMRSO no found DDSBTD - DFYDDD None GBGZ1G NA GNAW99 Unknown GUGPPP not detected HVHHFH No found drugs KHJBOK no MXA7O5 no NDP7T7 none OOO3GD / PCBAPT no drugs found Q4WQSQ Not present QZEZZZ - T0B0D0 None TTTGKV None USDN2N NONE UUXUUM NO WEB9SQ Abs WZUJSD - XNXEE6 NO FOUND Z4YCUT NONE ZGAWTE Not detected.

Statement of findings for Test Sample 1

Code [blank sample] 0H72WR Drugs Not Detected 1111EF 1A3AXJ 35TZAW 3FMD3X GHB was detected in sample BS1 2017/1. 4FF58F 66OQY6 6V10VI 7BVRLF 7FEMIN 84HKVU 8LCBAB We did not find any drugs. We found only caffein. 8MFF1T 8TPBUN 8VX7GU AG3666 AMMRSO no drugs found in the sample 2017/1/BS-1 B1KV8H BBKEUE BHWJHB BNGG0M CPUSPP CTTCT3 D1AYDM Not detected. DB4Y6M BLANK DDA5D2 Negative DDSBTD - DFYDDD In Sample 2017/1/BS-1 no drug was found DHUDIC The substances that were tested for weren´t found to be present in the sample analysed. DQMUDL EPEVE2 Sample contains no substances from ICE menu FBYTRU No common drugs were detected in sample 2017/1/BS-1 FWXVWL GAHHTQ GBGZ1G Sample was negative during screening for all drug groups tested at our laboratory. Creatinine levels were satisfactory. GMUMBE Negative GNAW99 We found two stain in TLC plate for this sample but because we did not have all of the refrences we could not identify them.

Code [blank sample] GUGPPP blank GXJGYM a preliminar screenning by EIA with no possitive results H2PHCD HB4JKY HHLH88 Performed by GS/MS Method and Caffeine was found. HVHHFH Sample code number 2017/1/BS-1 was found doesn't contain controlled drugs. IJS22F IQIQAI Common drugs not detected. IQJAM7 IVV5RV (remark :caffeine present) JRKD4U THE SAMPLE BS-1 ANALYZED DOES NOT CONTAINS CONTROLLED DRUGS ( AMPHETAMINE, BENZODIAZEPINES,COCAINE/METABOLITES,OPIATES,11-NOR-DELTA9- THC-9-CARBOXYLIC ACID,BARBITURATES. JSZABT No proof of drug abuse. K3KSJ9 KHJBOK KJPKK4 L3ZOZH LJTLFH M8VO1Z MXA7O5 blank sampke NCMGK4 NDP7T7 NGAJ1Y NP5333 OOO3GD no drugs were found PCBAPT caffeine, ibuprophen PQFUYI PXJDZ1 Q4WQSQ Screening test, GC/MS: Not to be present QZEZZZ - RNJJ8Z SOK66J SV8SSS SZZ1BZ Negative. T0B0D0 Sample 2017/1/BS-1 found not to contain any drugs TBORSX TG33JW TISIQZ Negative the screening method TTTGKV No control drugs found

Code [blank sample] U5KOOL UCTGCC UIUDEC No drug was found in the sample number 1 USDN2N UTSOWL UUXUUM No drugs or controlled drugs detected V6ZRMH VLHXHH after analysis performed the sample contained caffeine VN2UVV Drugs were not detected in BS-1 sample VR1QQH The urine screen did not indicate the presence of any of the targeted drugs. W5TXOT No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-1. WEB9SQ WZRRBA Examination of the sample coded 2017/1/BS-1 did not reveal the presence of any controlled drugs WZUJSD negative XNXEE6 NO FOUND Y3AFEE YFYCWJ No se detectó YGKDY2 No controlled drug from ICE 2017/01 menu is detected YSKXXD No drugs were found in this sample. Z4YCUT ZGAWTE Not detected drugs into 2017/1/BS-1 sample by Enzyme Immunoassay Techniques (EIA) and by Gas Chromatgraphy/Mass Spectrometry (CG/MS).

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 100 110 120 140 141 150 160 161 170 180 230 231 210 0H72WR I 1111EF I I 1A3AXJ I S chemical immunochromatographic 35TZAW S I I 3FMD3X I SI S Dip test 4FF58F S I LC/QTOF 6V10VI S I I 7BVRLF S SI I 7FEMIN S I I 84HKVU SI I S Multi-Drug Screen Test Panel 8LCBAB I SI Dipro drug lab screen 8MFF1T S I 8TPBUN I SI I 8VX7GU S I I SI Kinetic Interaction of Microparticles in Solution AG3666 S I AMMRSO S SI S I B1KV8H S I I BBKEUE S I I BHWJHB S SI S LC-QTOF BNGG0M S I CPUSPP S I I CTTCT3 I I S inmunocromatografía flujo lateral D1AYDM S I SI DB4Y6M S I DDA5D2 S SI SI DDSBTD S SI I DFYDDD SI SI DHUDIC S I DQMUDL I LC/TOF EPEVE2 S SI S LC-TOF FBYTRU SI FWXVWL S SI I GAHHTQ S SI I

Code 100 110 120 140 141 150 160 161 170 180 230 231 210 GBGZ1G S I GMUMBE S SI GNAW99 SI GUGPPP SI GXJGYM S I I LC-QTOF H2PHCD I HB4JKY S I HHLH88 S I HVHHFH SI I IJS22F S I IQIQAI S I IQJAM7 S I IVV5RV I I SI JRKD4U SI SI JSZABT I I S K3KSJ9 S I KHJBOK I I KJPKK4 I S zivia kit multitest L3ZOZH S I LJTLFH S I M8VO1Z S I SI MXA7O5 SI NCMGK4 SI NDP7T7 I I S immunochromatographie NGAJ1Y S I NP5333 S SI OOO3GD S I I PCBAPT S I I PQFUYI SI SI I PXJDZ1 SI I I Q4WQSQ S I QZEZZZ SI RNJJ8Z S I SOK66J S I I SV8SSS I SI SZZ1BZ S I T0B0D0 SI TBORSX S I TG33JW S I I

Code 100 110 120 140 141 150 160 161 170 180 230 231 210 TISIQZ SI SI TTTGKV S S I I U5KOOL S I I UCTGCC S I I UIUDEC S I USDN2N I UTSOWL I I Triage 8- ALERE Sure Step UUXUUM SI I V6ZRMH S I SI VLHXHH S I VN2UVV S I VR1QQH SI W5TXOT SI WEB9SQ SI WZRRBA S SI I WZUJSD S I XNXEE6 I S MULTIDRUG TEST Y3AFEE S I I SI one step immonochromatographic assay YFYCWJ S YGKDY2 SI SI YSKXXD S I Z4YCUT I ZGAWTE S I

RESPONSE SUMMARY FOR TEST SAMPLE 1

Participants: 96

The response summary of all 96 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:

BS-1 was a blank test sample containing no substances from the ICE menu

False positives for Test Sample-1:

Round Code: Substance reported: Tech Code: 3FMD3X GHB 230

False negatives for Test Sample-1 (techniques(s) used for ANP):

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 96 Technique 100 110 120 140 141 150 160 161 170 180 210 Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

(%) 2.1 56.3 3.1 1.0 1.0 2.1 0.0 0.0 0.0 27.1 12.5

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7 (%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3 Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2 (%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

1514 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 0H72WR Nordazepam and Amfetamine 1111EF OXAZEPAM, TEMAZEPAM, NORDAZEPAM, AMFETAMINE 1A3AXJ Oxazepam, Temazepam, Nordazepam and Amphethamine 35TZAW Amphétamine, Nordazepam, Oxazepam, Temazepam 3FMD3X Amphetamine, oxazepam, medazepam, nordazepam, temazepam, diazepam 4FF58F Amfetamine, Nordazepam, Oxazepam, Temazepam 66OQY6 amphetamine, nordiazepam, temazepam 6V10VI amfetamine, nordazepam, temazepam 7BVRLF amphetamines, benzodiazepines 7FEMIN Anfetamina, Temazepam, Nordiazepam 84HKVU Amfetamine, Nordazepam, Oxazepam,Temazepam 8LCBAB Amfetamine, Oxazepam, 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 8MFF1T BENZODIACEPINES AND ANPHETAMINES 8TPBUN Amfetamine, Nordazepam 8VX7GU Amphetamine, Nordiazepam, Temazepam, Oxazepam AG3666 Amfetamine, Nordazepam, Temazepam, Oxazepam AMMRSO Amfetamine, Nordazepam, Oxazepam, Temazepam B1KV8H anfetamina, nordazepam BBKEUE Amfetamine, Nordazepam, Oxazepam, Temazepam BHWJHB Amphetamine, temazepam, nordiazepam, oxazepam BNGG0M amphetamine, nardazepam, oxazepam, temazepam CPUSPP Amfetamine; Nordazepam; Temazepam; Oxazepam CTTCT3 amphetamine, nordiazepam,oxacepam,temazepam D1AYDM Amfetamine, Nordazepam, Oxazepam, Temazepam DB4Y6M AMPHETAMINE, NORDAZEPAM, OXAZEPAM, TEMAZEPAM DDA5D2 amphetamine, nordazepam, oxazepam, temazepam DDSBTD Amfetamine, Nordazepam,Oxazepam,Temazepam DFYDDD Nordazepam, Oxazepam, Temazepam DHUDIC Amphetamine, Oxazepam and Nordazepam DQMUDL Amphetamine; Nordiazepam, Oxazepam, Temazepam EPEVE2 Amfetamine, Nordazepam, Oxazepam, Temazepam FBYTRU Amfetamine and Nordazepam FWXVWL Amfetamine, Benzodiazepines and metabolites: Oxazepam, Temazepam, Nordazepam GAHHTQ Amfetamine, Nordazepam GBGZ1G Amphetamine and Nordazepam GMUMBE Amphetamine, Nordiazepam, Oxazepam, Temazepam GNAW99 Amfetamine GUGPPP amfetamine,nordazepam,temazepam,oxazepam GXJGYM nordazepam, temazepam, oxazepam, amphetamine H2PHCD nordazepam, temazepam

Code Identified Substances HB4JKY amphetamines, benzodiazepam HHLH88 Nordazepam, Temazepam, Delorazepam,Caffeine. HVHHFH Amfetamine, Oxazepam, Temazepam and Nordazepam IJS22F amfetamine, nordazepam, temazepam IQIQAI Nordazepam, Temazepam, Amphetamine IQJAM7 nordazepam, oxazepam IVV5RV amphetamine JRKD4U AMPHETAMINE,NORDAZEPAM,TEMAZEPAM,OXAZEPAM JSZABT amfetamine, nordazepa, oxazepam, temazepam K3KSJ9 Amfetamine, Nordiazepam and Temazepam KHJBOK Amphetamine, Nordazepam, Temazepam L3ZOZH Amfetamine, Temazepan, Nordazepam,oxacepam LJTLFH Amphetamine & Nordazepam M8VO1Z Amfetamine, Nordazepam, Oxazepam, Temazepam MXA7O5 AMF and Benzos NCMGK4 amphetamine, nordazepam and temazepam NDP7T7 temazepam, nordazepam, oxazepam, amfetamine NGAJ1Y Amphetamine, Nordazepam, Temazepam NP5333 amfetamine,nordazepam,temazepam,oxazepam OOO3GD amphetamine/nordazepam/temazepam PCBAPT amfetamine PQFUYI AMPHETAMINE, NORDIAZEPAM, OXAZEPAM, TEMAZEPAM PXJDZ1 amphetamine,benzo Q4WQSQ Amfetamine, Nordazepam, Temazepam, Oxazepam QZEZZZ Amfetamine,Nordazepam,Oxazepam,Temazepam RNJJ8Z anphetamine, nordazepam, temazepam, oxazepam SOK66J Amphetamine, Nordiazepam, Oxazepam, Temazepam SV8SSS Amphetamine, nordazepam, temazepam SZZ1BZ amfetamine, nordazepam, temazepam, oxazepam T0B0D0 Amfetamine, Nordazepam and Temazepam TBORSX Amfetamine TISIQZ Amphetamine ; nordiazepam ; oxazepam TTTGKV oxazepam, camazepam,nordazepam and amphetamine U5KOOL Amfetamine, nordiazepam, temazepam and oxazepam UCTGCC Nordazepam, Oxazepam, Temazepam UIUDEC amfetamine, nordazepam and temazepam USDN2N Amphetamine, oxazepam, Nordazepam, Temazepam. UTSOWL Amphetamine, Benzodiazepines UUXUUM Amphetamine and Nordazepam V6ZRMH Nordiazepam, amfetamine VLHXHH amphetamine+ nordazepam VN2UVV Nordazepam and Amfetamine VR1QQH Amphetamine, Nordiazepam, Oxazepam, Temazepam W5TXOT nordazepam

Code Identified Substances WEB9SQ amfetamine, nordazepam,oxazepam,temazepam WZRRBA Amfetamine, Nordazepam, Oxazepam and Temazepam WZUJSD methamphetamine,nordazepam XNXEE6 FOUND Y3AFEE amphetamine, nordazepam, oxazepam, temazepam YFYCWJ Benzodiacepinas YGKDY2 Nordiazepam, temazepam and oxazepam YSKXXD amfetamine, nordazepam, oxazepam, temazepam Z4YCUT Amfetamine, Nordazepam, Oxazepam, Temazepam ZGAWTE Amfetamine, Nordazepam and Temazepam.

Statement of findings for Test Sample 2

Code Amfetamine Nordazepam Oxazepam Temazepam 0H72WR + + - - Nordazepam and Amfetamine Detected 1111EF + + + +

1A3AXJ + + + + those drugs were identified by LC/MS/MS 35TZAW + + + +

3FMD3X + + + + Amphetamine (2374.28 ng/mL), oxazepam (1270.68 ng/mL), medazepam (3643.41 ng/mL), nordazepam (3577.85 ng/mL), temazepam (not quantified) and diazepam (< 5.0 ng/mL) were detected in sample BS2 2017/1. 4FF58F + + + +

66OQY6 ANP ANP ANP ANP

6V10VI + + - +

7BVRLF + + - + amphetamine, nordiazepam, temazepam 7FEMIN + + + +

84HKVU + + + + The sample contains amfetamine, nordazepam, oxazepam and temazepam. 8LCBAB + - + - We found: Amfetamine, Oxazepam, 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 8MFF1T - + - + NORDAZEPAM AND TEMAZEPAM 8TPBUN + + - - Amfetamine, Nordazepam 8VX7GU + + + +

AG3666 + + + + Amfetamine, Nordazepam, Temazepam and Oxazepam were identified by GCMS analysis. AMMRSO + + + + Amfetamine, Nordazepam, Oxazepam, Temazepam were found in the sample 2017/1/BS-2 B1KV8H + + - - positivo para anfetamina y nordazepam BBKEUE + + + +

BHWJHB + + + + Amphetamine was found in urine, indicationg intake of amphetamine or a drug that metabolizes to amphetamine. Amphetamine is a stimulating drug. Temazepam, nordiazepam and oxazepam was in addition found. All these drugs are metabolites of diazepam, and could be explained by intake of diazepam: as these drugs in addition can be taken as individual drugs a combination of intake can not be ruled out.

BNGG0M + + + + In the sample were found: amphetamine, nardazepam, oxazepam, temazepam

Code Amfetamine Nordazepam Oxazepam Temazepam CPUSPP + + + +

CTTCT3 + + + + The presence of nordiazepam, oxacepam, temazepam in urine indicates consumption of diazepam, or the consumption of each of the benzodiacepines themselves. The presence of amphetamine in urine indicates the consumption of amphetamine by itself or the consumption of metanphetamine. D1AYDM + + + + Positive to amfetamine, nordazepam, oxazepam and temazepam. DB4Y6M + + + +

DDA5D2 + + + + presence of amphetamine and diazepam metabolites DDSBTD + + + +

DFYDDD - + + + In Sample 2017/1/BS-2 the drugs Nordazepam, Oxazepam, Temazepam were found. DHUDIC + + + ANP It was detected the presence of Amphetamine, Oxazepam and Nordazepam in the sample analysed. DQMUDL + + + + Amphetamine is a central nervous system stimulant, and is a Schedule II substance in the United States. Nordiazepam is a long acting benzodiazepine, and is a Schedule IV substance in the United States. Oxazepam is a short to intermediate acting benzodiazepine and is a Schedule IV substance in the United States. Temazepam is an intermediate acting benzodiazepine and is a Schedule IV drug in the United States. Nordiazepam, oxazepam and temazepam can all also be metabolites of Diazepam. EPEVE2 + + + + Sample is positive for Amfetamine, Nordazepam, Oxazepam, Temazepam FBYTRU + + ANP ANP Amfetamine and Nordazepam were detected in sample 2017/1/BS-2 FWXVWL + + + +

GAHHTQ + + ANP - Amfetamine and Nordazepam were identified in the sample. GBGZ1G + + ANP ANP The sample tested positive for Amphetamine type stimulants and Benzodiazapines on screening. Creatinine levels were satisfactory.

Amphetamine was confirmed in the sample and quantified at 1198 ng/ml.

Nordazepam was confirmed in the sample, however no validated quantification procedure is in place at our laboratory therefore quantification was not done. GMUMBE + + + + Positive for amphetamine and benzodiazepines GNAW99 + ANP ANP ANP We found two other stains in TLC plate for this sample but becaus we did not have refrence drugs we could not identify them GUGPPP + + + + drugs detected

GXJGYM + + + + a preliminar positive result for benzodiacepines and amphetamines in EIA. A confirmation for CG/MS and LC/QTOF

Code Amfetamine Nordazepam Oxazepam Temazepam H2PHCD ANP + ANP + use of benzodiazepines (nordazepam, temazepam) HB4JKY + + ANP + amphetamine, temazepam, nordazepam HHLH88 - + - + Confirmed my GS/MS Method. HVHHFH + + + + Sample code number 2017/1/BS-2 was found to contain amfetamine (concentration 1189 ng/ml), oxazepam (concentration 647 ng/ml), temazepam (concentration 634 ng/ml) and nordazepam (concentration 2049 ng/ml). IJS22F + + - +

IQIQAI + + ANP + Amphetamine, nordazepam and temazepam detected. IQJAM7 - + + ANP

IVV5RV + + + + illegal drugs (amphetamine) and benzodiazepines (metabolites): nordazepam, oxazepam and temazepam. Caffeine present. JRKD4U + + + + THE SAMPLE BS-2 ANALYZED DOES CONTAINS AMPHETAMINE AND BENZODIAZEPINE METABOLITES ( NORDAZEPAM,TEMAZEPAM,OXAZEPAM) JSZABT + + + + Abuse of "speed". Use of medicinal drugs containing nordazepam and temazepam. Oxazepam is probably the metabolite of these two. K3KSJ9 + + - + 2017/1/BS-2 found to contain 113 ng/ml of Amfetamine, 1462.46 ng/ml of Nordiazepam and 389.8 ng/ml of Temazepam KHJBOK + + - +

KJPKK4 ANP ANP ANP ANP

L3ZOZH + + + +

LJTLFH + + ANP ANP The urine was analysed and found to contain Amphetamine and Nordazepam. M8VO1Z + + + +

MXA7O5 + + + + consumer of AMF and benzos NCMGK4 + + - +

NDP7T7 + + + + general extraction, identification and confirmation with HPLC/DAD, the curve was realised in different concentration NGAJ1Y + + - +

NP5333 + + + + amfetamine, nordazepam,temazepam,oxazepam were found in the sample BS-2 at the detection limit.

Code Amfetamine Nordazepam Oxazepam Temazepam OOO3GD + + ANP + sample was spiked with amphetamine , nordazepam and temazepam PCBAPT + + + + nordazepam, oxazepam, temazepam, caffeine PQFUYI + + + +

PXJDZ1 + - - -

Q4WQSQ + + + + Screening test (EIA). Positive ; GC/MS: Relation m/z, time retention (tR ) the reference material Amfetamine, Nordazepam, Temazepam, Oxazepam are equivalents to those sample 2017/1/ BS-2 QZEZZZ + + + + - RNJJ8Z + + + +

SOK66J + + + + Amphetamine ~ 0.7mg/L Nordiazepam Detected > 1mg/L Oxazepam ~ 0.5mg/L Temazepam ~0.5mg/L SV8SSS + + - +

SZZ1BZ + + + + Positive to amfetamine, nordazepam, temazepam, oxazepam. T0B0D0 + + ANP + Sample 2017/1/BS-2 found to contain Amfetamine, Nordazepam and Temazepam TBORSX + + + + Amfetamine,Oxazepam TG33JW + + + -

TISIQZ + + + - Analytical Adverse Finding for amphetamine, nordiazepam and oxazepam. TTTGKV + + + - by using CR & GC-MS techniques ( Oxazepam , Camazepam , Nordazepam ) were detected in urine sample.

by using LC-MS (Amphetamine) was detected. U5KOOL + + + + The presence of amphetamine in the urine sample shows previous use of the drug. The presence of nordiazepam, temazepam and oxazepam in the urine is consistent with previous use of diazepam. UCTGCC ANP + + + Nordazepam, Oxazepam, Temazepam were detected UIUDEC + + - + In urine sample number two was identified amfetamine, nordazepam and temazepam USDN2N + + + + The coincidence between the retention time and mass-fragmentogram from a reference standard, analyzed at the same conditions that the biological sample, indicates the presence of Amphetamine, oxazepam, Nordazepam and Temazepam in the biological sample. UTSOWL + + - +

Code Amfetamine Nordazepam Oxazepam Temazepam UUXUUM + + ANP ANP Amphetamine and Nordazepam detected in the sample V6ZRMH + + - - The presence of nordiazepam in urine indicates the use of diazepam or nordiazepam.The presence of amfetamine in urine indicates the use of amfetamine. VLHXHH + + - - after analysis performed the sample contained amphetamine +nordazepam+caffeine VN2UVV + + ANP ANP Nordazepam and Amfetamine were detected in BS-2 sample VR1QQH + + + + The urine sample screened positive for the presence of amphetamine, and also nordiazepam, oxazepam and temazepam (indicative of benzodiazepine consumption). W5TXOT - + - - The test sample 2017/1/BS-2 was found to contain the controlled drug nordazepam. WEB9SQ + + + + Detected: amphetamines, benzodiazepines WZRRBA + + + + Examination of the sample coded 2017/1/BS-2 revealed the presence of amphetamine, nordazepam, oxazepam and temazepam. WZUJSD - + ANP ANP 2017/1/BS-2 contain methamphetamine, nordazepam XNXEE6 + + + + NORDAZEPAM, TEMAZEPAM, OXAZEPAM, ANFETAMINE Y3AFEE + + + +

YFYCWJ ANP ANP ANP ANP Positivo YGKDY2 - + + + Nordiazepam, temazepam and oxazepam were qualitatively reported as nordiazepam was above the upper limit of linearity in 2017/01/BS-02. YSKXXD + + + + In this sample amfetamine, nordazepam, oxazepam, temazepam were found, which indicates that person consumed amfetamine and diazepam. Z4YCUT + + + +

ZGAWTE + + - + It was detected Amfetamine, Temazepam and Nordazepam into 2017/1/BS-2 sample by Gas Chromatography/Mass Spectrometry (GC/MS).

Identification methods for Test Sample 2

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

RESPONSE SUMMARY FOR TEST SAMPLE 2

Participants: 96

The response summary of all 96 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:

Substance Name Number of laboratories correctly identifying: Amfetamine 84 Nordazepam 90 Oxazepam 60 Temazepam 72

False positives for Test Sample-2:

Round Code: Substance reported: Tech Code: 3FMD3X Medazepam, Diazepam 230 8LCBAB 2C-B 150/Dipro screen TTTGKV Camazepam N/A WZUJSD Methamphetamine 150 TG33JW Tenamfetamine 231 KJPKK4 Methylecgonine 180

False negatives for Test Sample-2 (techniques(s) used for ANP):

Where none of the four components were identified or were not considered for analysis

Round Code: Answer Code: Tech Code: 66OQY6 ANP - KJPKK4 ANP - YFYGWJ ANP -

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 96 Technique 100 110 120 140 141 150 160 161 170 180 210 Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

(%) 2.1 56.3 3.1 1.0 1.0 2.1 0.0 0.0 0.0 27.1 12.5

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7 (%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2 (%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

2726 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 1103 ng/ml Substance: BS-2; Amfetamine UNODC value = 1270 ng/ml

4.0

3.0 2.7

2.0

1.3 0.9 1.0 0.9 0.7 0.7 0.5 0.6 0.6 0.6 0.6 0.4 0.5 0.3 0.3 0.1 0.1 7.9 17.7 0.0 -6.1 0.0

-0.2 -0.2 -0.3

- 0.6 -0.6 0.5 -0.7 -0.6 -

-1.0 - -0.9 0.8

-1.3 -1.2

-1.5 -1.5 -2.0

-2.5 -3.0

-4.0 IN GU ZZZ 58F FEE JJ8Z VE2 K3KSJ9 RN JSZABT 4FF SOK66J Y3A YSKXXD CPUSPP QZE EPE NP5333 TBORSX 7FEM 66OQY6 DDSBTD BBKEUE TG33JW VLHXHH 8VX7 8TPBUN GUGPPP GBGZ1G 3FMD3X U5KOOL BHWJHB HVHHFH DDA5D2 DB4Y6M WZRRBA UTSOWL D1AYDM M8VO1Z MXA7O5 BNGG0M FWXVWL AMMRSO

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.

2827 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-2; Amfetamine

Dispersion of z-scores using different analytical techniques for the quantification of Amfetamine in 2017/1 BS-2 6

0 score - z

-2

-4 GC/MS LC/MS

-6

2928 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 1840 ng/ml Substance: BS-2; Nordazepam UNODC value = 1960 ng/ml

4.00

3.1 3.00

2.00 1.8 1.8

1.00 0.8 0.8 0.7 0.8 0.6 0.6 0.6 0.4 0.5 0.5 0.5 0.2 0.1 5.6 0.00 -5.1 -4.7

- 0.0

- -0.1 0.2 0.2 0.1 -0.3 -0.3 - -0.4

-0.7 -0.7 -0.7 -1.00 -0.8 -1.1 -1.2

-2.00 -2.0 -2.1

-3.00

-4.00 YDM ORSX USPP KOOL A5D2 3KSJ9 K RNJJ8Z JSZABT Y3AFEE 4FF58F QZEZZZ EPEVE2 YSKXXD CP IQJAM7 BBKEUE TB 8TPBUN 8MFF1T 84HKVU 7FEMIN 66OQY6 DDSBTD TG33JW GXJGYM GUGPPP 3FMD3X U5 DD DB4Y6M HVHHFH BHWJHB WZRRBA UTSOWL D1A MXA7O5 M8VO1Z BNGG0M FWXVWL AMMRSO

3029 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-2; Nordazepam Dispersion of z-scores using different analytical techniques for the quantification of Nordazepam in 2017/1 BS-2 6

0 score - z

-2

-4

LC/MS HPLC GC/MS -6

3130 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 529 ng/ml Substance: BS-2; Oxazepam UNODC value = 570 ng/ml

4.00

3.00

2.1 2.00

1.3

0.9 0.9 1.00 0.8 0.6 0.4 0.4 0.4

7.9 8.9 43.1 0.00

-4.5 -0.2 -0.2

- -0.4 0.3 -0.3 -0.3 -0.3 -0.5 -0.6 -0.7

- -1.00 - 0.9 0.8

-1.1 -1.0

-1.6 -2.00

-3.00

-4.00 G0M 33JW EMIN JSZABT 4FF58F Y3AFEE SOK66J QZEZZZ EPEVE2 TBORSX CPUSPP 7F DDSBTD BBKEUE IQJAM7 TG 84HKVU GXJGYM GUGPPP 3FMD3X U5KOOL DDA5D2 BHWJHB MXA7O5 M8VO1Z DB4Y6M HVHHFH BNG D1AYDM FWXVWL AMMRSO

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.

3231 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-2; Oxazepam Dispersion of z-scores using different analytical techniques for the quantification of Oxazepam in 2017/1 BS-2 6

0 score - z

-2

-4

LC/MS HPLC GC/MS -6

3332 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 530 ng/ml Substance: BS-2; Temazepam UNODC value = 580 ng/ml

4.00

3.00

1.9 2.00 1.7 1.5

0.9 0.9 1.00 0.8 0.7 0.7 0.4 0.2 0.1 0.2 0.1 0.1 0.1 4.7 0.00

-0.2 - -0.3 -0.3 -0.3 -0.3 0.3 -0.6 -1.00 -0.8

- - -1.0 0.9 0.9 -1.2 -1.2

-2.00

-2.4

-3.00 - 3.0

-4.00 JGYM SOWL 3KSJ9 PUSPP JSZABT 4FF58F K Y3AFEE SOK66J QZEZZZ EPEVE2 C 7FEMIN BBKEUE NDP7T7 TG33JW TBORSX 8MFF1T 84HKVU 66OQY6 U5KOOL DDA5D2 DDSBTD GX GUGPPP UT DB4Y6M M8VO1Z BHWJHB HVHHFH WZRRBA D1AYDM FWXVWL BNGG0M AMMRSO

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.

3433 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-2; Temazepam

Dispersion of z-scores using different analytical techniques for the quantification of Temazepam in 2017/1 BS-2 6

0 score - z

-2

-4 HPLC GC/MS LC/MS

-6

3534 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 2

Amfetamine Nordazepam Deviation Deviation Code Concentration from Code Concentration from z-score z-score (ng/ml) robust (ng/ml) robust average average K3KSJ9 113 -990 -6.1 GXJGYM 265 -1575 -5.1 SOK66J 695 -408 -2.5 IQJAM7 404 -1436 -4.7 Y3AFEE 854 -249 -1.5 DDA5D2 1206 -634 -2.1 RNJJ8Z 860 -243 -1.5 CPUSPP 1232 -608 -2.0 8VX7GU 901 -202 -1.3 K3KSJ9 1462 -378 -1.2 EPEVE2 912 -191 -1.2 TBORSX 1500 -340 -1.1 7FEMIN 957 -146 -0.9 U5KOOL 1600 -240 -0.8 4FF58F 967 -136 -0.8 BNGG0M 1625 -215 -0.7 QZEZZZ 995 -108 -0.7 D1AYDM 1626 -214 -0.7 TBORSX 1000 -103 -0.6 8TPBUN 1638 -202 -0.7 DDSBTD 1009 -94 -0.6 BBKEUE 1710 -130 -0.4 BBKEUE 1010 -93 -0.6 WZRRBA 1750 -90 -0.3 YSKXXD 1020 -83 -0.5 66OQY6 1757 -83 -0.3 BNGG0M 1050 -53 -0.3 EPEVE2 1774 -66 -0.2 UTSOWL 1064 -39 -0.2 DDSBTD 1787 -53 -0.2 BHWJHB 1076 -27 -0.2 MXA7O5 1801 -39 -0.1 U5KOOL 1100 -3 0.0 7FEMIN 1807 -33 -0.1 D1AYDM 1115 12 0.1 AMMRSO 1826 -14 0.0 JSZABT 1122 19 0.1 DB4Y6M 1878 38 0.1 TG33JW 1145 42 0.3 TG33JW 1914 74 0.2 AMMRSO 1147 44 0.3 FWXVWL 1975 135 0.4 GUGPPP 1170 67 0.4 JSZABT 1987 147 0.5 8TPBUN 1181 78 0.5 8MFF1T 1989 149 0.5 HVHHFH 1189 86 0.5 GUGPPP 2000 160 0.5 FWXVWL 1194 91 0.6 M8VO1Z 2017 177 0.6 66OQY6 1197 94 0.6 RNJJ8Z 2028 188 0.6 GBGZ1G 1198 95 0.6 UTSOWL 2028 188 0.6 M8VO1Z 1201 98 0.6 HVHHFH 2049 209 0.7 DDA5D2 1209 106 0.7 BHWJHB 2071 231 0.8 NP5333 1223 120 0.7 YSKXXD 2085 245 0.8 WZRRBA 1240 137 0.9 4FF58F 2094 254 0.8 MXA7O5 1252 149 0.9 Y3AFEE 2385 545 1.8 DB4Y6M 1305 202 1.3 84HKVU 2407 567 1.8 CPUSPP 1532 429 2.7 QZEZZZ 2800 960 3.1 3FMD3X 2374 1271 7.9 3FMD3X 3578 1738 5.6 VLHXHH 3950 2847 17.7

Oxazepam Temazepam Deviation Deviation Code Concentration from Code Concentration from z-score z-score (ng/ml) robust (ng/ml) robust average average GXJGYM 110 -419 -4.5 GXJGYM 180 -350 -3.0 CPUSPP 376 -153 -1.6 UTSOWL 248 -282 -2.4 BNGG0M 425 -104 -1.1 CPUSPP 386 -144 -1.2 7FEMIN 432 -97 -1.0 K3KSJ9 390 -140 -1.2 TG33JW 448 -81 -0.9 BNGG0M 410 -120 -1.0 JSZABT 450 -79 -0.8 TG33JW 419 -111 -0.9 D1AYDM 460 -69 -0.7 D1AYDM 420 -110 -0.9 U5KOOL 470 -59 -0.6 66OQY6 437 -93 -0.8 BHWJHB 485 -44 -0.5 DDA5D2 462 -68 -0.6 DDSBTD 496 -33 -0.4 BBKEUE 490 -40 -0.3 DDA5D2 499 -30 -0.3 AMMRSO 494 -36 -0.3 GUGPPP 500 -29 -0.3 SOK66J 496 -34 -0.3 TBORSX 500 -29 -0.3 TBORSX 500 -30 -0.3 AMMRSO 502 -27 -0.3 QZEZZZ 500 -30 -0.3 SOK66J 510 -19 -0.2 GUGPPP 508 -22 -0.2 EPEVE2 510 -19 -0.2 EPEVE2 538 8 0.1 4FF58F 565 36 0.4 U5KOOL 540 10 0.1 MXA7O5 569 40 0.4 FWXVWL 541 11 0.1 BBKEUE 570 41 0.4 DB4Y6M 542 12 0.1 M8VO1Z 585 56 0.6 DDSBTD 549 19 0.2 QZEZZZ 600 71 0.8 M8VO1Z 555 25 0.2 FWXVWL 613 84 0.9 BHWJHB 576 46 0.4 DB4Y6M 615 86 0.9 4FF58F 608 78 0.7 HVHHFH 647 118 1.3 8MFF1T 608 78 0.7 84HKVU 729 200 2.1 JSZABT 622 92 0.8 3FMD3X 1271 742 7.9 HVHHFH 634 104 0.9 IQJAM7 1368 839 8.9 7FEMIN 640 110 0.9 Y3AFEE 4575 4046 43.1 WZRRBA 700 170 1.5 84HKVU 733 203 1.7 Y3AFEE 747 217 1.9 NDP7T7 1073 543 4.7

Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 35TZAW GHB 3FMD3X None 4FF58F GHB 84HKVU gamma-Hydroxybutyric acid (GHB) 8LCBAB none 8VX7GU GHB AG3666 gamma-Hydroxybutyric acid (GHB) AMMRSO gamma-Hydroxybutyric acid (GHB) BBKEUE GHB BHWJHB GHB BNGG0M gamma-Hydroxybutyric acid (GHB) CPUSPP gamma-Butyrolactone (GBL) D1AYDM gamma-Hydroxybutyric acid (GHB) DDA5D2 GHB DDSBTD - DFYDDD None EPEVE2 gamma-Hydroxybutyric acid (GHB) FWXVWL gamma-Hydroxybutyric acid (GHB) GBGZ1G NA GUGPPP gamma-Hydroxybutyric acid HVHHFH GHB JSZABT GHB KHJBOK no M8VO1Z GHB MXA7O5 no NCMGK4 GHB NDP7T7 GBL NP5333 GHB PCBAPT no drugs found PQFUYI GHB Q4WQSQ Not present QZEZZZ gamma-Hydroxybutyric acid (GHB) RNJJ8Z GHB SOK66J GHB SV8SSS morphin T0B0D0 None TTTGKV none USDN2N NONE UUXUUM GHB VLHXHH GHB

Code Identified Substances VR1QQH Morphine - indicative WEB9SQ gamma-hydroxybutyric-acid WZRRBA gamma-hydroxybutyric acid WZUJSD - XNXEE6 FOUND Y3AFEE GHB YSKXXD GHB Z4YCUT gamma-Hydroxybutyric acid (GHB) ZGAWTE Ibuprofen and Cocaine

Statement of findings for Test Sample 3

Code gamma- Hydroxybutyric acid (GHB) 0H72WR - Drugs Not Detected 1111EF ANP

1A3AXJ ANP

35TZAW +

3FMD3X - No drugs were detected in sample BS3 2017/1. 4FF58F +

66OQY6 ANP

6V10VI -

7BVRLF ANP

7FEMIN ANP

84HKVU + The sample contains gamma-Hydroxybutyric acid (GHB). 8LCBAB ANP We did not find any drugs. We found only caffein. 8MFF1T -

8TPBUN -

8VX7GU +

AG3666 + gamma-Hydroxybutyric acid (GHB) was identified by GCMS analysis. AMMRSO + gamma-Hydroxybutyric acid (GHB) was found in the sample 2017/1/BS-3 B1KV8H ANP

BBKEUE +

BHWJHB + GHB was found in urine. GHB is a CNS depressant. BNGG0M + in the sample is detected gamma-Hydroxybutyric acid (GHB) CPUSPP -

Code gamma- Hydroxybutyric acid (GHB) CTTCT3 ANP

D1AYDM + Positive to gamma-hydroxybutyric acid (GHB). DB4Y6M ANP BLANK DDA5D2 + Presence of GHB DDSBTD ANP - DFYDDD ANP In Sample 2017/1/BS-3 no drug was found DHUDIC ANP The substances that were tested for weren´t found to be present in the sample analysed. DQMUDL ANP

EPEVE2 + Sample is positive for gamma-Hydroxybutyric acid (GHB) FBYTRU ANP No common drugs were detected in sample 2017/1/BS-3 FWXVWL +

GAHHTQ ANP

GBGZ1G ANP Sample was negative during screening for all drug groups tested at our laboratory. Creatinine levels were satisfactory. GMUMBE ANP Negative GNAW99 ANP

GUGPPP + drugs detected GXJGYM ANP a preliminar screenning by EIA with no possitive results H2PHCD ANP

HB4JKY ANP

HHLH88 - Performed by GS/MS Method and Caffeine was found. HVHHFH + Sample code number 2017/1/BS-3 was found to contain gamma-Hydroxybutyric acid (concentration 15980 ng/ml) IJS22F ANP

IQIQAI ANP Common drugs not detected.

Code gamma- Hydroxybutyric acid (GHB) IQJAM7 ANP

IVV5RV ANP (remark : caffeine, nicotine en quinine present) JRKD4U ANP THE SAMPLE BS-3 ANALYZED DOES NOT CONTAINS CONTROLLED DRUGS ( AMPHETAMINE, BENZODIAZEPINES,COCAINE/METABOLITES,OPIATES,11-NOR-DELTA9- THC-9-CARBOXYLIC ACID,BARBITURATES. JSZABT + Abuse of GBL or GHB or 1,4-butanediol. K3KSJ9 -

KHJBOK ANP

KJPKK4 ANP

L3ZOZH ANP ibuprofen positive LJTLFH ANP

M8VO1Z +

MXA7O5 - blank sample NCMGK4 +

NDP7T7 - general extraction, identification and confirmation with GC/MS NGAJ1Y ANP

NP5333 + gamma-Hydroxybutyric acid was found in the sample BS-3 at the detection limit. OOO3GD ANP no drugs were found PCBAPT - caffeine, ibuprophen,aripiprazole PQFUYI +

PXJDZ1 -

Q4WQSQ ANP Screening test, GC/MS,: Not to be present. QZEZZZ + - RNJJ8Z +

Code gamma- Hydroxybutyric acid (GHB) SOK66J + GHB ~ 23mg/L SV8SSS -

SZZ1BZ ANP Negative. T0B0D0 ANP Sample 2017/1/BS-3 found not to contain any drugs TBORSX + gamma-Hydroxybutyric acid (GHB) TG33JW +

TISIQZ ANP Negative in the screening method TTTGKV ANP no control drugs found U5KOOL ANP

UCTGCC ANP

UIUDEC ANP No drug was found in the sample number 3 USDN2N ANP

UTSOWL ANP

UUXUUM + GHB detected in the sample V6ZRMH ANP

VLHXHH + after analysis performed the sample contained GHB +CAFFEINE VN2UVV ANP Drugs were not detected in BS-3 sample VR1QQH ANP The urine sample screened indicative for the presence of morphine. W5TXOT ANP No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-3. WEB9SQ + other WZRRBA + Examination of the sample coded 2017/1/BS-3 revealed the presence of gamma-hydroxybutyric acid (GHB). WZUJSD ANP negative XNXEE6 + GHB

Code gamma- Hydroxybutyric acid (GHB) Y3AFEE +

YFYCWJ ANP No se detectó YGKDY2 ANP No controlled drug from ICE 2017/01 menu is detected YSKXXD + In this sample GHB was found, which indicates that person consumed GHB. Z4YCUT +

ZGAWTE ANP It was detected Ibuprofen and Cocaine into 2017/1/BS-3 sample by Gas Chromatography/Mass Spectrometry (GC/MS).

Identification methods for Test Sample 3

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

RESPONSE SUMMARY FOR TEST SAMPLE 3

Participants: 96

The response summary of all 96 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:

Substance Name Number of laboratories correctly identifying: GHB 33

False positives for Test Sample-3:

Round Code: Substance reported: Tech Code: SV8SSS Morphine 150/180 VR1QQH Morphine 231 ZGAWTE Cocaine 180 CPUSPP GBL 180 KJPKK4 MDMA 180 NDP7T7 GBL 180

False negatives for Test Sample-3 (techniques(s) used for ANP):

Round Code: Answer Code: Tech Code: Round Code: Answer Code: Tech Code: K3KSJ9 - 231 0H72WR - 180 6V10VI - 231 PXJDZ1 - 110 8MFF1T - 180 PCBAPT - 180 HHLH88 - 180 CPUSPP - 150 MXA7O5 - 180 8TPBUN - 231 3FMD3X - 180 NDP7T7 - 180 SV8SSS - 180/231

Forty nine laboratories did not carry out analysis for GHB in test sample 3

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 96 Technique 100 110 120 140 141 150 160 161 170 180 210 Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

(%) 2.1 56.3 3.1 1.0 1.0 2.1 0.0 0.0 0.0 27.1 12.5

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7 (%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2 (%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

4847 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 17382 ng/ml Substance: BS-3; GHB UNODC value = 16560 ng/ml

4.00

3.3

3.00

2.2 1.9 2.00

1.1 1.00 0.9

0.4

6.5 0.00

-0.2 -0.2 -0.1

- -0.5 0.4 -0.4

- -0.5 -0.6 0.6 -1.00 -0.9

-1.3

-1.7 -2.00

-3.00

-4.00 B RNJJ8Z JSZABT SOK66J Y3AFEE QZEZZZ EPEVE2 TBORSX BBKEUE TG33JW GUGPPP 35TZAW BHWJH HVHHFH DDA5D2 D1AYDM M8VO1Z BNGG0M FWXVWL AMMRSO

4948 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-3; GHB

Dispersion of z-scores using different analytical techniques for the quantification of GHB in 2017/1 BS-3 6

0 score - z

-2

-4 GC/MS LC/MS

-6

5049 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 3

GHB Code Concentration Deviation from z-score (ng/ml) robust average JSZABT 12340 -5042 -1.7 BNGG0M 13500 -3882 -1.3 TG33JW 14763 -2619 -0.9 D1AYDM 15500 -1882 -0.6 BHWJHB 15615 -1767 -0.6 GUGPPP 15840 -1542 -0.5 HVHHFH 15980 -1402 -0.5 EPEVE2 16060 -1322 -0.4 35TZAW 16100 -1282 -0.4 BBKEUE 16850 -532 -0.2 M8VO1Z 16908 -474 -0.2 QZEZZZ 17000 -382 -0.1 FWXVWL 18700 1318 0.4 TBORSX 20000 2618 0.9 RNJJ8Z 20760 3378 1.1 SOK66J 23200 5818 1.9 AMMRSO 24000 6618 2.2 DDA5D2 27400 10018 3.3 Y3AFEE 37101 19719 6.5

Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 0H72WR Morphine and 6-MAM 1111EF MORPHINE 1A3AXJ Morphine, Hydromorphone 35TZAW Morphine 3FMD3X Morphine 4FF58F Morphine 66OQY6 morphine 6V10VI morphine 7BVRLF opiates 7FEMIN Morphine 84HKVU Morphine 8LCBAB Opiates 8MFF1T MORPHINE 8TPBUN Morphine 8VX7GU Morphine AG3666 Morphine AMMRSO Morphine BBKEUE Morphine BHWJHB Morphine BNGG0M Morphine (Total) CPUSPP Morphine CTTCT3 Morphine D1AYDM Morphine (total) DB4Y6M MORPHINE DDA5D2 morphine DDSBTD Morphine DFYDDD Morphine DHUDIC Morphine DQMUDL Morphine EPEVE2 Morphine FWXVWL Morphine GAHHTQ Morphine, 11-nor-delta9- THC-9-carboxylic acid GBGZ1G Morphine GMUMBE Morphine GNAW99 Morphine GUGPPP Morphine GXJGYM MORPHINE H2PHCD morphine HB4JKY opiates HHLH88 Morphine, Caffeine, Ibuprofen, Umbelliferone.

Code Identified Substances HVHHFH Morphine IJS22F morphine IQIQAI Morphine, 6-MAM IQJAM7 morphine IVV5RV morphine JRKD4U MORPHINE JSZABT morphine K3KSJ9 morphine KHJBOK no M8VO1Z Morphine MXA7O5 MOR NCMGK4 morphine NDP7T7 NONE NGAJ1Y Morphine, 6-Monoacetylmorphine (6-MAM) NP5333 morphine OOO3GD morphine PCBAPT morphine PQFUYI MORPHINE PXJDZ1 opiates , opioids Q4WQSQ Morphine QZEZZZ Morphine (Total) RNJJ8Z morphine SOK66J Morphine (Total) SV8SSS morphin, codeine SZZ1BZ morphine T0B0D0 None TBORSX Morphine TISIQZ Morphine TTTGKV Morphine U5KOOL Morphine UCTGCC Morphine UIUDEC morphine USDN2N Morphine UTSOWL Morphine UUXUUM Morphine V6ZRMH Morphine VLHXHH MORPHINE VN2UVV Morphine and 6-Monoacetylmorphine (6-MAM) VR1QQH Morphine WEB9SQ morphine WZRRBA Morphine WZUJSD morphine-3-O-glucuronide XNXEE6 FOUND Y3AFEE morphine

Code Identified Substances YFYCWJ Morfina YGKDY2 Morphine YSKXXD morphine Z4YCUT Morphine ZGAWTE Not detected.

Statement of findings for Test Sample 4

Code Morphine (Total) 0H72WR + Morphine and 6-MAM Detected 1111EF +

1A3AXJ + Those drugs were identified by LC/MS/MS 35TZAW +

3FMD3X + Morphine (1563.45 ng/mL) was detected in sample BS4 2017/1. 4FF58F +

66OQY6 ANP Free morphine was measured 6V10VI +

7BVRLF + moprhine 7FEMIN +

84HKVU + The sample contains morphine. 8LCBAB + We found: Morphine total and Codeine 8MFF1T + NO COMMENTS 8TPBUN + Morphine 8VX7GU +

AG3666 + Morphine was identified by GCMS analysis. AMMRSO + Morphine was found in the sample 2017/1/BS-4 B1KV8H -

BBKEUE +

BHWJHB + 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.

BNGG0M + in the sample is detected Morphine (Total) CPUSPP +

Code Morphine (Total) CTTCT3 + The presence of morphine in urine indicates morphine consumption or other drugs such as heroin and codeine. D1AYDM + Positive to morphine. DB4Y6M +

DDA5D2 + Presence of morphine DDSBTD +

DFYDDD + In Sample 2017/1/BS-4 the drug morphine was found. DHUDIC + It was detected the presence of Morphine in the sample analysed. DQMUDL + Morhphine is a narcotic analgesic found in the opium poppy. It is a Schedule II substance in the United States. EPEVE2 + Sample is positive for Morphine FBYTRU ANP No common drugs were detected in sample 2017/1/BS-4 FWXVWL +

GAHHTQ + Morphine and 11-nor-delta9- THC-9-carboxylic acid were identified in the sample. GBGZ1G + The sample was positive for opiates on screening. Creatinine levels were satisfactory.

The presence of Morphine was confirmed and quantified at 1114 ng/ml. The sample was also negative for Codeine, eliminating Codeine intake as a source of the Morphine in Urine. GMUMBE + Positive for opiates GNAW99 +

GUGPPP + drugs detected GXJGYM + Preliminar positive results by EIA for opiods/ opiates confirmated by CG/MS and LC/QTOF H2PHCD + use of morphine HB4JKY + morphine HHLH88 + Confirmed my GS/MS Method. HVHHFH + Sample code number 2017/1/BS-4 was found to contain morphine (concentration 839 ng/ml) IJS22F +

Code Morphine (Total) IQIQAI + Morphine and 6-MAM detected. IQJAM7 +

IVV5RV + (remark :caffeine present) JRKD4U + THE SAMPLE BS-4 ANALYZED DOES CONTAINS AN OPIATE ( MORPHINE). JSZABT + Abuse of pure heroin or morphine or use of medicinal morphine. K3KSJ9 + 2017/1/BS-4 found to contain 190.7 ng/ml of Morphine KHJBOK -

KJPKK4 ANP

L3ZOZH + paracetamol positive LJTLFH ANP

M8VO1Z +

MXA7O5 + opioid consumer NCMGK4 +

NDP7T7 -

NGAJ1Y +

NP5333 + morphin was found in the sample BS-4 at the detection limit. OOO3GD +

PCBAPT + caffeine, acetaminophen PQFUYI +

PXJDZ1 +

Q4WQSQ + Screening test (EIA). Positive. GC/MS: Relation m/z, time retention (tR ) the reference material Morphine are equivalents to those sample 2017/1 /BS-4 QZEZZZ + - RNJJ8Z +

Code Morphine (Total) SOK66J + Morphine, Total Detected > 0.5mg/L SV8SSS +

SZZ1BZ + Positive to morphine. T0B0D0 ANP Sample 2017/1/BS-4 found not to contain any drugs TBORSX + Morphine TG33JW +

TISIQZ + Analytical Adverse Finding for Morphine (free) with a concentration of 0,9 µg/ml TTTGKV + by using CR & GC-MS techniques ( Morphine ) was detected in urine sample. U5KOOL + The presence of morphine in the urine sample shows previous use of the drug.

UCTGCC + Morphine was detected UIUDEC + In urine sample number four was identified morphine USDN2N + The coincidence between the retention time and mass-fragmentogram from a reference standard, analyzed at the same conditions that the biological sample, indicates the presence of Morphine in the biological sample. UTSOWL +

UUXUUM + Morphine detected in the sample V6ZRMH + The presence of morphine in urine indicates the use of morphine VLHXHH + after analysis performed the sample contained MOAPHINE + CAFFEINE VN2UVV + Morphine and 6-Monoacetylmorphine (6-MAM) were detected in BS-4 sample VR1QQH + The urine sample screened positive for the presence of morphine. W5TXOT - No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-4. WEB9SQ + Detected: opiates WZRRBA + Examination of the sample coded 2017/1/BS-4 revealed the presence of morphine. WZUJSD - 2017/1/BS-4 contain opiates. XNXEE6 + MORPHINE

Code Morphine (Total) Y3AFEE +

YFYCWJ ANP Positivo YGKDY2 + Morphine was qualitatively reported as morphine was above the upper limit of linearity in 2017/01/BS-04. YSKXXD + In this sample morphine was found, which indicates that person consumed morphine. Z4YCUT +

ZGAWTE ANP Not detected drugs into 2017/1/BS-4 sample by Gas Chromatgraphy/Mass Spectrometry (CG/MS).

Identification methods for Test Sample 4

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

RESPONSE SUMMARY FOR TEST SAMPLE 4

Participants: 96

The response summary of all 96 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:

Substance Name Number of laboratories correctly identifying: Morphine 84 False positives for Test Sample-4:

Round Code: Substance Name: Tech Code: OH72WR 6-Monoacetylmorphine 180 GAHHTQ delta-9-THC acid 180 IQIQAI 6-Monoacetylmorphine 180 NGAJ1Y 6-Monoacetylmorphine 180 SV8SSS Codeine 180 VN2UVV 6-Monoacetylmorphine 180 WZUJSP Morphine 3-glucuronide 150 PXJDZI Morphine 3-glucuronide, Codeine 180 8LCBAB Codeine 150 False negatives for Test Sample-4 (techniques(s) used for ANP):

Round Code: Substance Name: Tech Code: B1KV8H - 150 W5TXOT - 180 NDP7T7 - 180 WZUJSD - 150 KHJBOK - 150 FBYTRU ANP ZGAWTE ANP KJPKK4 ANP T0B0D0 ANP LJTLFH ANP

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 96 Technique 100 110 120 140 141 150 160 161 170 180 210 Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

(%) 2.1 56.3 3.1 1.0 1.0 2.1 0.0 0.0 0.0 27.1 12.5

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7 (%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2 (%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

6362 Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 822 ng/ml Substance: BS-4; Morphine UNODC value = 860 ng/ml

4.0 4.00

3.4

3.00 2.8 2.6

2.1 2.00 1.6

1.00 0.7 0.6 0.4 0.4 0.5 0.3 0.1 0.2 0.2 0.0 6.5 14.3 0.00 0.0 0.0 0.0 -0.1

- - 0.3 - 0.3 0.2 - 0.4

- -0.5 0.5 -0.6 -0.6 -1.00 -0.7 -0.9 -1.0 -1.2 -1.3 -1.4 -1.4

-2.00

-2.3

-3.00

-3.4

-4.00 BUN EZZZ OWL USPP JGYM 3KSJ9 TISIQZ JSZABT K RNJJ8Z Y3AFEE 4FF58F QZ EPEVE2 YSKXXD CP 7FEMIN NP5333 BBKEUE IQJAM7 TBORSX TG33JW 8TP 8VX7GU 84HKVU 8MFF1T 66OQY6 DDSBTD VLHXHH GX GUGPPP GBGZ1G 3FMD3X UTS BHWJHB DDA5D2 M8VO1Z HVHHFH DB4Y6M WZRRBA D1AYDM FWXVWL MXA7O5 BNGG0M AMMRSO

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 thatan anomaly has occured that requires inverstigation.

6463 Z-Score Report per Sample per Substance

Round: 2017/1 Substance: BS-4; Morphine

Dispersion of z-scores using different analytical techniques for the quantification of Morphine in 2017/1 BS-4 6

0 score - z

-2

-4 GC/MS LC/MS

-6

6564 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 4

Morphine Code Concentration Deviation from z-score (ng/ml) robust average K3KSJ9 191 -631 -3.4 UTSOWL 398 -424 -2.3 CPUSPP 553 -269 -1.4 8TPBUN 564 -258 -1.4 GXJGYM 570 -252 -1.3 QZEZZZ 600 -222 -1.2 8VX7GU 639 -183 -1.0 66OQY6 656 -166 -0.9 JSZABT 685 -137 -0.7 BHWJHB 710 -112 -0.6 D1AYDM 710 -112 -0.6 EPEVE2 725 -97 -0.5 7FEMIN 728 -94 -0.5 Y3AFEE 750 -72 -0.4 DDSBTD 769 -53 -0.3 YSKXXD 769 -53 -0.3 BNGG0M 780 -42 -0.2 TBORSX 800 -22 -0.1 TG33JW 817 -5 0.0 DDA5D2 821 -1 0.0 M8VO1Z 821 -1 0.0 GUGPPP 831 9 0.0 HVHHFH 839 17 0.1 AMMRSO 850 28 0.2 NP5333 852 30 0.2 BBKEUE 880 58 0.3 TISIQZ 900 78 0.4 FWXVWL 902 80 0.4 IQJAM7 914 92 0.5 DB4Y6M 932 110 0.6 4FF58F 958 136 0.7 GBGZ1G 1114 292 1.6 84HKVU 1221 399 2.1 MXA7O5 1311 489 2.6 8MFF1T 1339 517 2.8 RNJJ8Z 1461 639 3.4 3FMD3X 1563 741 4.0 VLHXHH 2035 1213 6.5 WZRRBA 3500 2678 14.3

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