Quick viewing(Text Mode)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

BIOLOGICAL SPECIMENS 2013/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 Codes and Abbreviations Page 4 Sample 1 Analysis Page 5 Identified substances Page 5 Statement of findings Page 7 Identification methods Page 11 Summary Page 13 Z-Scores Page 14 Sample 2 Analysis Page 18 Identified substances Page 18 Statement of findings Page 20 Identification methods Page 24 Summary Page 26 Z-Scores Page 27 Sample 3 Analysis Page 33 Identified substances Page 33 Statement of findings Page 34 Identification methods Page 38 Summary Page 40 Z-Scores Page 41 Sample 4 Analysis Page 43 Identified substances Page 43 Statement of findings Page 44 Identification methods Page 48 Summary Page 50

Test Samples Information

Samples Comments on samples Sample 1 To prepare BS-1, urine was spiked with Morphine sulphate (3057ng/ml, 2300ng base/ml), Codeine (1150ng base/ml) and 6-Monoacetylmorphine (576 ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised. Sample 2 To prepare BS-2, urine was spiked with Amfetamine sulfate (1562ng/ml, 1143ng base/ml), Nordazepam (1727ng/ml), (457ng/ml) and (464ng/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised. Sample 3 To prepare BS-3, urine was spiked with Sodium gammahydroxybutyrate (14427ng GHB/ml, ). The spiked urine was dispensed in 50ml aliquots and lyophilised

Sample 4 BS-4 was a blank test sample prepared from urine containing no substance in the ICE menu. The sample contained urine spiked with Ephedrine hydrochloride (2700ng/ml, 2308ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Samples Substances Concentrations Comments on substances Sample 1 Morphine (Total) 2300 ng/ml 6-Monoacetylmorphine (6-MAM) 576 ng/ml Codeine 1150 ng/ml Sample 2 Nordazepam 1727 ng/ml Oxazepam 457 ng/ml Amfetamine 1143 ng/ml Temazepam 464 ng/ml Sample 3 gamma-Hydroxybutyric acid (GHB) 14427 ng/ml Sample 4 [blank sample]

2013/1-BS (2) Copyright (c) 2013 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. Two rounds are offered per year with each round presenting participants with four different test samples for analysis.

This report provides information on the 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

Samples within both the Seized materials (SM) and Biological Specimens (BS) test group were sent to 167 laboratories in 57 countries. 68 laboratories participated in the BS test group and 58 (85%) laboratories submitted the results of their analysis in time for inclusion in the summary report, with 96% using the ICE portal for return of results. The almost universal usage of the ICE portal continues to be a high endorsement of its utility.

Qualitative and Quantitative Analysis of the biological specimens test samples

Overall, the level of performance in identification of the test samples was good given the inherently higher level of difficulty in the analysis of biological specimens compared to seized materials. The complexity of the test samples in ICE 2013/1 was increased in order to challenge the participants. BS-1 contained morphine, 6-monoacetylmorphine and codeine, which were identified by 79%, 79% and 91% of participants respectively. It is encouraging to note that 71% of participants identified all three components in BS-1 and only five false positive results were reported. BS-2 contained amphetamine and a mixture of three (nordazepam, oxazepam and temazepam). While only 42% of participants identified all four components, 86% identified at least one of the benzodiazepines and 65% identified the amphetamine present. There were eight false positive results including four for . While the benzodiazepines present are metabolites of diazepam, their presence alone does not represent use of diazepam. BS-3 contained gammahydroxybutyric acid (GHB), a new substance on the ICE menu for the BS test group and 22% of participants identified its presence, while 64% of participants did not carry out analysis for identification of GHB. It is recognized that while GHB may not be commonly analysed by all participants, it has been included in the ICE menu as it represents an example of a more recently abused substance and at the Commission on Narcotic Drugs in March 2013, GHB was transferred from schedule IV to schedule II of the Convention of Psychotropic Substances of 1971. BS-4 was a blank test sample containing no substances from the ICE menu. Although it did contain ephedrine, a precursor to methamphetamine. 19% of participants identified the ephedrine and among five false positives, there was one for methamphetamine.

The results for quantitative analysis within the BS test group were excellent. For BS-1 24 out of 25 (96%) laboratories quantified the morphine, 21 out of 22 (95%) quantified 6-MAM and 22 out of 23 (96%) quantified codeine with acceptable Z-scores. Within BS-2, the quantitation results were equally as good with 20 of 21 (95%) laboratories quantifying the amfetamine, 20 out of 22 (91%) the nordazepam, 13 of 16 (81%) the oxazepam and 14 out of 16 (88%) the temazepam with acceptable Z-scores. Within BS-3, 7 out of 9 (87%) participants quantified the GHB present with acceptable Z-scores. It is encouraging to note that of those laboratories who did carry out quantification, 52% performed quantification on at least seven of the eight substances in all test samples. The predominant analytical techniques used by participants for quantification within the BS test group were GC/MS (79%), followed by LC/MS (38%) and others at (17%).

Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. Also, laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. Participation in ICE also helps in monitoring the effect of corrective actions.

(3) 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

2013/1-BS (4) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 1 Analysis

Identified substances for Test Sample 1 Code Identified Substances 0709WO 6-MAM, Morphine, Codeine 1C2WN2 opiates 1M39MI codeine, morphine, 6-monoacetylmorphine 2I1J7W codeine, 6 MAM and morphine 3ESBDT CODEINE, ACETYLMORPHINE 5A0LTW morphine, 6-MAM, codeine 5D8EIT Morphine, Heroin and Codeine 6H33U3 Codeine and 6-MAM 6ZZZCD morphine,codeine, 6-monoacethylmorphine 76JL37 morphine, 6-MAM, codeine 7HEM7O Codeine 98KDM8 Morphine, codeine and monoacetly-morphine ABBR1D Morphine,O6-monoacetylmorphine,codeine AKQ21O morphine, codeine and 6-acetyl-morphine ANXWGY Codeine, morphine and 6-Monoacethylmorphine BBRB0E Morphine BJG4OO 6-MAM, codeine, morphine BPL9ZY morphine, 6-MAM, codeine BVABMB 6-MAM, codeine, morphine CUH0QQ CODEINE, MORPHINE AND MORPHINE-6-ACETYL. CWOOM9 codeine, morphine, 6-mam CZJD27 morphine, codeine D7TTWV OPIÁCEOS DONO2Y 6-MAM, codeine, morphine ERWOWW Codeine FNSUKR 6-monoacetilmorfina, morfina, codeina ILS9UP Codeine, Morphine, 6-Monoacetylmorphine J2FAYZ opiates J6WWIX Heroin abuse JBUJJA Codeine JLCQ3D CODEINE JWS3VW morphine, codeine, 6-mam JZ6JTH Amphetamine KHMLHA Morphine, Codeine, 6-monoacetylmorphine. KKPG9K 6-Monoacetylmorphine, Morphine and Codeine LFLTTZ Opiates M8E6T6 morphine, codeine, 6-monoacetylomorphine NDS3R3 codeine, morphine, monoacetylmorphine OOOQSO 6-monoacetylmorphine, morphine, codeine PSXQYE Morphine, Codeine, 6-MAM

2013/1-BS (5) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances QHGM5Q Morphine, Codeine, 6-MAM RFGGQG codeine, morphine, 6-monoacetylmorphine SAV6NX 6MAM, Morphine and codeine TTAVXV Morphine, codeine and 6-monoacetyl-morphine UM0M1S Codeine, Morphine, 6-MAM VHDEKU Codeine+morphine+6MAM WIYO85 Opiates WWSTWW morphine, codeine and 6-monoacetylmorphine XA9AAA Morfine - Codeine - 6-MAM XDXVS9 Codeine and 6-Monoacetylmorphine XJZEEE Codeine, Morphine, 6-MA XLEICI CODEINE XTLXKX Morphine, Codeine, 6-Monoacetylmorphine XXHQNV Morphine and 6-MAM YCEET4 cideine,MAM, morphine

2013/1-BS (6) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 1

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) 0709WO + + + - 1C2WN2 + + + morphine codeine 6-monoacetylmorphine caffeine 1M39MI + + + sample positive for opiates 2I1J7W + + +

3ESBDT + + ANP Codeine and Acetylmorphine were detected. 5A0LTW + + +

5D8EIT + + - The sample contain: 2560 ng/mL of morphine, 1200 ng/ml of coedine. Heroin and caffeine was also detected. 6H33U3 + + ANP Codeine and 6-MAM was detected in sample BS1 but quantification analysis was not performed. 6ZZZCD + + + 2013/1/BS-1 urine sample contain morphine,codine,6-monoacethylmorphine(heroine user) 76JL37 + + + Findings indicate that the person consumed heroin. 7HEM7O - + -

98KDM8 + + + The urine was found to contain morphine, codeine and monoacetyl-morphine. ABBR1D + + +

AKQ21O + + + The presence of morphine, codeine and 6-acetyl-morphine indicates the use of heroin. ANXWGY + + + Codeine, morphine and 6-Monoacethylmorphine detected

2013/1-BS (7) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) BBRB0E ANP + + we found morphine in BS-1 as a controlled substance BJG4OO + + + There was heroine consumption BPL9ZY + + + We also found caffeine in BS-1. BVABMB + + + sample positive to 6 MAM: 425.2 ng/ml (cut-off 100 ng/ml) sample positive to codeine:591.3 ng/ml (cut-off 100 ng/ml) sample positive to total morphine:1845.3 ng/ml (cut-off 100 ng/ml) CUH0QQ + + + IN THE ROUND AS LABELED "ROUND ICE 2013/1 SAMPLE BS-1" DETECTED CODEINE, MORPHINE AND MORPHINE-6-ACETYL. CUUFFQ + + +

CWOOM9 + + + Compatible with consum of heroin CZJD27 ANP + + Test sample contains morphine and codeine at 2739.84 ng/mL and 1199.05 ng/mL respectively using GCMS D7TTWV ANP ANP ANP POSITIVO (PRESUNTIVO) DONO2Y + + + 6-MAM was detected in urine. Results indicate the previous use of heroin, a controlled narcotic (illegal).

The concentration of GHB reflect the physiological concentrations. ERWOWW - + - Codeine was identified by GC/MS FNSUKR + + + La coincidencia entre los tiempos de retención y fragmentogramas de una muestra biológica analizada en las mismas condiciones de un estandar indica la presencia de 6 monoacetilmorfina, morfina y codeína en esta. FZZZZQ ANP ANP ANP

ILS9UP + + + Codeine, Morphine, 6-Monoacetylmorphine J2FAYZ + + + we have not received standards

2013/1-BS (8) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) J6WWIX + + + Presence of 6-MAM JBUJJA - + + free JLCQ3D - + - The sample BS-1 contain CODEINE JWS3VW + + +

JZ6JTH - - -

KHMLHA + + + In the urine sample analyzed, was detected and confirmed the presence of Morphine, Codeine, 6- monoacetylmorphine. KKPG9K + + + The sample contains 6-Monoacetylmorphine, morphine and codeine. LFLTTZ - + + Codeine, Morphine and metabolites M8E6T6 + + + use of opiates MDKW7J + + +

NDS3R3 + + + consumption of diacetylmorphine OOOQSO + + +

PSXQYE + + + Sample is positive for Morphine, Codeine and 6-MAM QHGM5Q + + +

RFGGQG + + + sample positive for opiates SAV6NX + + + Morphine and codeine are metabolites of 6MAM. Presence of 6MAM indicates a heroin consumption. 6MAM, Morphine and codeine are controlled narcotics in France

2013/1-BS (9) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 6- Monoacetylmorphin Codeine Morphine (Total) e (6-MAM) TTAVXV + + + The 6-monoacetylmorphine detection indicates heroin consumption, codeine could be present as heroin impurity or could come from the intake of the drug itself. Finally, morphine could come from the heroin or codeine consumption or could come from the intake of the drug itself. UM0M1S + + + Screening by immunoassay technich : Positive Conformation by GC-MS : Positive VHDEKU + + + Sample containing morphine+codeine+6MAM which indivates consumation of heroine WIYO85 + - + BS1positive for: Morphine & 6MAM WWSTWW + + +

XA9AAA + + + Codeine was consumed, Morphine indicates an opiate was consumed and 6-MAM marker of Heroin indicate this opiate was consumed. XDXVS9 + + ANP On analysis, the sample of 2013/1/BS-1 found to contain Codeine and 6-Monoacetylmorphine. XJZEEE ANP ANP ANP Free morphine was measured. XLEICI - + - Codeine was found in BS-1. Quantitation was not performed. XTLXKX + + + Heroine abuse. XXHQNV + + + Morphine and 6-MAM are metabolites of Heroin YCEET4 + + +

2013/1-BS (10) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 110 120 150 161 170 171 180 230 231 210 0709WO SI 1C2WN2 S I I 1M39MI S SI 2I1J7W S I I 3ESBDT S I I 5A0LTW S I I 5D8EIT S I 6H33U3 I 6ZZZCD S I 76JL37 S I I 7HEM7O S I I 98KDM8 S I ABBR1D S I I AKQ21O S I SI I ANXWGY S I BBRB0E S I BJG4OO S I BPL9ZY S SI SI BVABMB SI CUH0QQ S I CUUFFQ S I CWOOM9 S I I CZJD27 I I S DT kits D7TTWV S DONO2Y S I I ERWOW S I W FNSUKR S I FZZZZQ SI ILS9UP S I I S Kinetic Interactions of microparticles J2FAYZ I I immunochem J6WWIX S I I JBUJJA S I I I JLCQ3D SI I

2013/1-BS (11) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 110 120 150 161 170 171 180 230 231 210 JWS3VW S I JZ6JTH S I I KHMLHA S I KKPG9K SI S Multi-Drug Screen Test Panel LFLTTZ I S Dipromed Drulab screen M8E6T6 S I MDKW7J SI I NDS3R3 S S I OOOQSO S I PSXQYE S S I I QHGM5Q I I SI I RFGGQG S SI SAV6NX S I I TTAVXV S I I I I UM0M1S S I VHDEKU SI I WIYO85 S I WWSTW S I I W XA9AAA S I S Lateral Flow Immunoassay XDXVS9 I SI XLEICI S I XTLXKX S I I XXHQNV S I YCEET4 I

2013/1-BS (12) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 1 The response summary of all 54 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:

H Response Summary Participants: 58

6-Monoacetylmorphine (6-MAM): 46 Codeine: 53 Morphine (Total): 46

False positives for Test Sample 1

Code Name Technique DONO2Y gamma-Hydroxybutyric acid 180 J6WWIX Methadone 180 JZ6JTH Amfetamine 230 5D8EIT Morphine-3-glucuronide 180 J2FAYZ Methadone 180

False negatives for BS-1(techinque(s) used or ANP) . Within BS-1, there were: 12 false negatives for Morphine 5 false negatives for Codeine 12 false negatives for 6-Monoacetylmorphine

Frequency of use of screening and identification techniques:

ResponseResponse Summary Summary Participants: 54 Participants: 58 110 120 Section 110 120 150 161 170 171 180 230 231 210 Screening 36 8 4 0 0 0 9 1 1 4 62.1% 13.8% 6.9% 0.0% 0.0% 0.0% 15.5% 1.7% 1.7% 6.9% Identification 4 0 3 11 2 2 49 5 12 2 6.9% 0.0% 5.2% 19.0% 3.4% 3.4% 84.5% 8.6% 20.7% 3.4% # labs using 36 8 7 11 2 2 49 6 12 6 this 62.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3% technique

2013/1-BS (13) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 1

6-Monoacetylmorphine (6- MAM) Codeine Morphine (Total) CODE MAD: 100.0 MAD: 119.5 MAD: 440.4 Conc. * AbsDev ZScore Conc. * AbsDev ZScore Conc. * AbsDev ZScore 0709WO 500.0 52.5 0.4 1100.0 34.0 0.2 2750.0 477.5 0.7 5A0LTW 690.0 137.5 0.9 1020.0 46.0 0.3 2540.0 267.5 0.4 5D8EIT 1200.0 134.0 0.8 2560.0 287.5 0.4 76JL37 436.0 116.5 0.8 1268.0 202.0 1.1 2300.0 27.5 0.0 ABBR1D 480.0 72.5 0.5 960.0 106.0 0.6 2239.0 33.5 0.1 BJG4OO 4119.0 3566.5 24.1 21619.0 20553.0 116.1 34982.0 32709.5 50.1 BPL9ZY 626.0 73.5 0.5 1270.0 204.0 1.2 2406.7 134.2 0.2 BVABMB 425.2 127.3 0.9 591.3 474.7 2.7 1845.3 427.2 0.7 CWOOM9 420.0 132.5 0.9 990.0 76.0 0.4 1950.0 322.5 0.5 CZJD27 1199.1 133.1 0.8 2739.8 467.3 0.7 DONO2Y 556.0 3.5 0.0 1121.0 55.0 0.3 1722.0 550.5 0.8 ILS9UP 647.0 94.5 0.6 1063.0 3.0 0.0 2472.0 199.5 0.3 J2FAYZ 575.0 22.5 0.2 1311.0 245.0 1.4 1555.0 717.5 1.1 J6WWIX 510.0 42.5 0.3 930.0 136.0 0.8 1818.0 454.5 0.7 KKPG9K 549.0 3.5 0.0 1069.0 3.0 0.0 2878.0 605.5 0.9 LFLTTZ 1000.0 1272.5 2.0 M8E6T6 650.0 97.5 0.7 1545.0 479.0 2.7 2245.0 27.5 0.0 MDKW7J 590.0 37.5 0.3 1300.0 234.0 1.3 2000.0 272.5 0.4 PSXQYE 705.0 152.5 1.0 1063.0 3.0 0.0 2508.0 235.5 0.4 QHGM5Q 450.0 102.5 0.7 900.0 166.0 0.9 1980.0 292.5 0.4 SAV6NX 730.0 177.5 1.2 1321.0 255.0 1.4 3319.0 1046.5 1.6 WIYO85 578.0 25.5 0.2 1510.0 762.5 1.2 WWSTWW 500.0 52.5 0.4 1220.0 154.0 0.9 2240.0 32.5 0.0 XJZEEE 769.0 216.5 1.5 984.0 82.0 0.5 2629.0 356.5 0.5 XTLXKX 580.0 27.5 0.2 974.0 92.0 0.5 2726.0 453.5 0.7

*) Concentration: ng/ml

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

2013/1-BS (14) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-1/6-Monoacetylmorphine (6-MAM) Median = 552.5 MAD = 100 UNODC value = 576

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

(15) Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-1/Codeine Median = 1066 MAD = 120 UNODC value = 1150

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

(16) Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-1/Morphine (Total) Median = 2272.5 MAD = 440.4 UNODC value = 2300

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 2 Analysis

Identified substances for Test Sample 2 Code Identified Substances 0709WO Amfetamine, Nordiazepam, Oxazepam, Temazepam 1C2WN2 amphetamines 1M39MI oxazepam, nordiazepam, temazepam and amphetamine 2I1J7W nordazepam, oxazeam, temazepam and amfetamine 3ESBDT Nordazepam 5A0LTW nordazepam, temazepam, oxazepam, amfetamine 5D8EIT Nordazepam, oxazepam, temazepam, theobromine 6H33U3 Nordazepam and Temazepam 6ZZZCD nordazepam,methamphetamine(traces) 76JL37 amfetamine, nordazepam, temazepam, oxazepam 7HEM7O Nordazepam 98KDM8 Nordiazepam and amphetmaine ABBR1D Amphetamine,Nordazepam,Oxazepam,Temazepam AKQ21O amphetamine, nordiazepam, temazepam and oxazepam ANXWGY Nordazepam and temazepam BBRB0E amphetamine BJG4OO temazepam, nordazepam BPL9ZY diazepam, nordazepam,oxazepam, temazepam BVABMB amphetamine, oxazepam, nordiazepam, temazepam CUH0QQ AMPHETAMINE, NORDIAZEPAM, OXAZEPAM AND DIAZEPAM CWOOM9 Amfetamine, nordazepam CZJD27 amphetamine, nordazepam, oxazepam D7TTWV ANFETAMINAS + BENZODIACEPINAS DONO2Y amfetamine ERWOWW Amphetamine and Nordazepam FNSUKR Temazepam, nordiazepam ILS9UP Amphetamine J2FAYZ amphetamine, benzodizepines J6WWIX Amphetamine, benzos JLCQ3D DESMETHYLDIAZEPAM JWS3VW diazepam, nordazepam, temazepam, amphetamine JZ6JTH THC KHMLHA Temazepam, Amphetamine. KKPG9K Amfetamine, Nordazepam and Temazepam. LFLTTZ Amphetamine groups, benzodiazepines M8E6T6 nordazepam, temazepam, amphetamines MDKW7J codeine, morphine and 6acetylmorphine NDS3R3 amphetamine, temazepam, nordazepam, oxazepam OOOQSO amphetamine, diazepam, nordazepam, oxazepam, temazepam PSXQYE Amfetamine, Nordazepam, Oxazepam, Temazepam

2013/1-BS (18) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances QHGM5Q Amfetamine, Nordazepam, Oxazepam, Temazepam RFGGQG oxazepam, nordiazepam, temazepam and amphetamine SAV6NX Amfetamine, Nordazepam, oxazepam and Temazepam TTAVXV Amphetamine, oxazepam, nordiazepam and temazepam. UM0M1S Nordazepam, Amphetamine VHDEKU Amphetamine+nordazepam+Temazepam WIYO85 AMPHETAMINE & BENZO WWSTWW amphetamine, nordazepam, oxazepam and temazepam XA9AAA Amfetamine - Nordazepam XDXVS9 Nordazepam and Temazepam XJZEEE Amphetamine, Temazepam, Nordiazepam XLEICI Nordazepam XTLXKX Amphetamine, Nordazepam, Oxazepam, Temazepam XXHQNV Nordazepamand Oxazepam YCEET4 amfetamine

2013/1-BS (19) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 2

Code Amfetamine Nordazepam Oxazepam Temazepam 0709WO + + + + - 1C2WN2 + + + + amphetamine oxazepam nordiazepam temazepam caffeine 1M39MI + + + + sample positive for benzodiazepines and amphetamine 2I1J7W + + + +

3ESBDT - + - - Nordazepam was detected. 5A0LTW + + + +

5D8EIT - + + + The sample contain 2105.43 ng/mL of nordazepam. Oxazepam, temazepam, theobromine and caffeine was detected. 6H33U3 ANP + ANP + Nordazepam and Temazepam was detected in sample BS2 but quantification analysis was not performed. 6ZZZCD - + ANP - 2013/1/BS-2 urine contain methamphetamine(traces),nordazepam(diazepam, methamphetamine user) 76JL37 + + + + Findings indicate that the person consumed amfetamine and one of or the combination of 1,4 - benzodiazepines. 7HEM7O - + - -

98KDM8 + + - - The urine was found to contain nordiazepam and amphetamine. ABBR1D + + + +

AKQ21O + + + + The presence of amphetamine indicates the use of amphetamine. The presence of nordiazepam, temazepam and oxazepam indicates the use of diazepam. ANXWGY ANP + ANP + Nordazepam and temazepam detected

2013/1-BS (20) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine Nordazepam Oxazepam Temazepam BBRB0E + ANP ANP ANP we found amphetamine in BS-2 as a controlled substance BJG4OO - + ANP + There was temazepam consumption BPL9ZY - + + + We also found caffeine and in BS-2. BVABMB + + + + sample positive to amphetamine:1197.2 (cut-off 250 ng/ml) sample positive to oxazepam:213.6 (cut-off 100 ng/ml) sample positive to nordiazepam :805.3 ng/ml (cut-off 100 ng/ml)

sample positive to temazepam: no quantification performed due to lack of certified standard CUH0QQ + + + - IN THE ROUND AS LABELED "ROUND ICE 2013/1 SAMPLE BS-2" DETECTED DIAZEPAM, OXAZEPAM, NORDIAZEPAM AND AMPHETAMINE. CUUFFQ + + + +

CWOOM9 + + - -

CZJD27 + + + ANP Test sample contains amphetamine (1066.26 ng/mL) using GCMS and nordazepam(1652.28 ng/mL) and oxazepam (1035.11ng/mL) using LCMSMS D7TTWV ANP ANP ANP ANP POSITIVO (PRESUNTIVO) DONO2Y + + + + Amfetamine was detected in urine. Results indicate the previous consumption of controlled narcotic (illegal), amfetamine or metamfetamine. The concentration of GHB reflect the physiological concentrations. ERWOWW + + - - Amphetamine and Nordazepam were identified by GC/MS FNSUKR ANP + - + La coincidencia entre los tiempos de retención y fragmentogramas de un material de referencia analizado en las mismas condiciones de una muestra biológica indica la presencia de temazepam y nordiazepam en esta. FZZZZQ - ANP ANP ANP

ILS9UP + + + + Amphetamine, Nordazepam, Temazepam, Oxazepam J2FAYZ + + + + we have not received standards

2013/1-BS (21) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine Nordazepam Oxazepam Temazepam J6WWIX + + + + Presence of metabolites JBUJJA - - - ANP

JLCQ3D - + - - The sample BS-2 contain DESMETHYLDIAZEPAM JWS3VW + + - +

JZ6JTH - ANP ANP ANP

KHMLHA + ANP - + In the urine sample analyzed, was detected and confirmed the presence of Temazepam, Amphetamine. KKPG9K + + - + The sample contains amfetamine, nordazepam and temazepam. LFLTTZ + - - - Amphetamin M8E6T6 ANP + - + use of benzodiazepines and amphetamines MDKW7J + + + +

NDS3R3 + + + + consumption of amphetamine and diazepam or OOOQSO + + + +

PSXQYE + + + + Sample is positive for Amfetamine, Nordazepam, Oxazepam and Temazepam QHGM5Q + + + +

RFGGQG + + + + sample positive for benzodiazepines and amphetamine SAV6NX + + + + Amfetamine is used for recreationnal purposes. It's a controlled narcotic in France. Nordazepam, oxazepam and temazepam are benzodiazepines, used for their and sedativ properties and also to treat epilepsy. Are also 3 metabolites of diazepam and their presence may indicates a diazepam consumption.

2013/1-BS (22) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine Nordazepam Oxazepam Temazepam TTAVXV + + + + The oxazepam, nordiazepam and temazepam detection indicates most likely: diazepam consumption, nevertheless the presence of these substances could come from the intake of the drugs itself or come from the intake of any other that produces diazepam as a metabolite. The amphetamine detection indicates the intake of the drug itself or could come from the metabolism of other drugs such as methamphetamine. UM0M1S + + - - Screening by immunoassay technich : Positive Conformation by GC-MS : Positive VHDEKU + + - + Sample containing Amphetamine+Nordazepam+Temazepam, substances under control WIYO85 + + + + BS2 positive for:amphetamine, nordazepam, oxazepam & temazepam WWSTWW + + + +

XA9AAA + + - - Amfetamine was detected, no other drugs as methamfetamine or drugs metabolizing to amfetamine were identified, this indicate that amfetamine was consumed In the sample was detected Nordazepam, this finding indicate that Nordazepam was consumed XDXVS9 - + - + On analysis, the sample of 2013/1/BS-2 found to contain Nordazepam and Temazepam. XJZEEE ANP ANP ANP ANP

XLEICI - + - - Nordazepam was found in BS-2. Quantitation was not performed. XTLXKX + + + + 1. "Speed" (amphetamine) abuse. 2. Consumption of nordazepam and temazepam is most likely. However, use of other benzodiazepine type drug (e.g. diazepam) can not be excluded. XXHQNV ANP + + - Nordazepam and Oxazepam are common metabolites of 1-4, Benzodiazepines groups of drugs YCEET4 + ANP ANP ANP

2013/1-BS (23) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 2

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

Analytical Technique Codes Code 110 120 150 161 170 171 180 230 231 210 0709WO SI 1C2WN2 S I I 1M39MI S SI 2I1J7W S I I 3ESBDT S I I 5A0LTW S I I 5D8EIT S I 6H33U3 I 6ZZZCD S I 76JL37 S I I 7HEM7O S I I 98KDM8 S I ABBR1D S I I AKQ21O S I SI I ANXWGY S I BBRB0E S I BJG4OO S I BPL9ZY S SI SI BVABMB SI CUH0QQ S I CUUFFQ S I CWOOM9 S I I CZJD27 I I S DT kits D7TTWV S DONO2Y S I I ERWOW S I W FNSUKR S I FZZZZQ SI ILS9UP S I I S Kinetic Interactions of microparticles J2FAYZ I I immunochem J6WWIX S I I JBUJJA S I I I JLCQ3D SI I

2013/1-BS (24) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 110 120 150 161 170 171 180 230 231 210 JWS3VW S I JZ6JTH S I I KHMLHA S I KKPG9K SI S Multi-Drug Screen Test Panel LFLTTZ I S Dipromed Drulab screen M8E6T6 S I MDKW7J SI I NDS3R3 S S I OOOQSO S I PSXQYE S S I I QHGM5Q I I SI I RFGGQG S SI SAV6NX S I I TTAVXV S I I I I UM0M1S S I VHDEKU SI I WIYO85 S I WWSTW S I I W XA9AAA S I S Lateral Flow Immunoassay XDXVS9 I SI XLEICI S I XTLXKX S I I XXHQNV S I YCEET4 I

2013/1-BS (25) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary for test sample 2 The response summary of all 54 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:

H Response Summary Participants: 58

Amfetamine: 39 Nordazepam: 49 Oxazepam: 30 Temazepam: 37 False positives for Test Sample 2 Code Name Technique 6ZZZCD Metamfetamine 150 BBRB0E Diazepam 150 BPL9ZY Diazepam, Demoxazepam 231 CUH0QQ Diazepam 180 DONO2Y gamma-Hydroxybutyric acid (GHB) 180 JZ6JTH NameQRU¨7+&FDUER[\OLFDFLG Technique 180 MDKW75 Codeine, Morphine, 6-MAM in report JWS3VW Diazepam 180

False negatives for BS-2 (techinque(s) used or ANP) . Within BS-2, there were: 19 false negatives for Amfetamine 9 false negatives for Nordazepam 28 false negatives for Oxazepam 21 false negatives for Temazepam

Frequency of use of screening and identification techniques: Response Summary

ResponseParticipants: Summary 54

Participants: 58 Section 110 120 Section 110 120 150 161 170 171 180 230 231 210 Screening 36 8 4 0 0 0 9 1 1 4 62.1% 13.8% 6.9% 0.0% 0.0% 0.0% 15.5% 1.7% 1.7% 6.9% Identification 4 0 3 11 2 2 49 5 12 2 6.9% 0.0% 5.2% 19.0% 3.4% 3.4% 84.5% 8.6% 20.7% 3.4% # labs using 36 8 7 11 2 2 49 6 12 6 this 62.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3% technique

2013/1-BS (26) Copyright (c) 2013 UNODC

2013/1-BS (14) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 2

Amfetamine Nordazepam Oxazepam CODE MAD: 138.0 MAD: 241.9 MAD: 48.0 Conc. * AbsDev ZScore Conc. * AbsDev ZScore Conc. * AbsDev ZScore 0709WO 1130.0 11.5 0.1 1500.0 152.1 0.4 350.0 120.0 1.7 5A0LTW 1740.0 621.5 3.0 1652.0 0.1 0.0 410.0 60.0 0.8 5D8EIT 2105.4 453.3 1.3 76JL37 1271.0 152.5 0.7 1888.0 235.9 0.7 ABBR1D 1320.0 201.5 1.0 1830.0 177.9 0.5 450.0 20.0 0.3 BJG4OO 33383.0 31730.9 88.6 BPL9ZY 1253.3 398.8 1.1 370.1 99.9 1.4 BVABMB 1197.2 78.7 0.4 805.3 846.8 2.4 213.6 256.4 3.6 CWOOM9 950.0 168.5 0.8 1240.0 412.1 1.2 CZJD27 1066.3 52.2 0.3 1652.3 0.1 0.0 1035.1 565.1 7.9 DONO2Y 1205.0 86.5 0.4 2146.0 493.9 1.4 518.0 48.0 0.7 ILS9UP 1106.0 12.5 0.1 J2FAYZ 242.0 876.5 4.3 765.0 887.1 2.5 113.0 357.0 5.0 J6WWIX 1107.0 11.5 0.1 612.0 1040.1 2.9 645.0 175.0 2.5 KKPG9K 890.0 228.5 1.1 LFLTTZ 1642.0 523.5 2.6 M8E6T6 1900.0 247.9 0.7 MDKW7J 1100.0 18.5 0.1 1600.0 52.1 0.1 420.0 50.0 0.7 PSXQYE 806.0 312.5 1.5 3500.0 1847.9 5.2 470.0 0.0 0.0 QHGM5Q 995.0 123.5 0.6 1350.0 302.1 0.8 460.0 10.0 0.1 SAV6NX 1101.0 17.5 0.1 2004.0 351.9 1.0 497.2 27.2 0.4 WIYO85 960.0 158.5 0.8 1570.0 82.1 0.2 481.0 11.0 0.2 WWSTWW 1231.0 112.5 0.6 1580.0 72.1 0.2 550.0 80.0 1.1 XJZEEE 1606.0 487.5 2.4 1888.0 235.9 0.7 XTLXKX 1027.0 91.5 0.4 1523.0 129.1 0.4 450.0 20.0 0.3

*) Concentration: ng/ml

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

2013/1-BS (27) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Temazepam CODE MAD: 112.0 Conc. * AbsDev ZScore 0709WO 420.0 80.0 0.5 5A0LTW 1050.0 550.0 3.3 5D8EIT 76JL37 ABBR1D 460.0 40.0 0.2 BJG4OO 17160.0 16660.0 100.4 BPL9ZY 363.0 137.0 0.8 BVABMB CWOOM9 CZJD27 DONO2Y ILS9UP J2FAYZ 138.0 362.0 2.2 J6WWIX 233.0 267.0 1.6 KKPG9K 360.0 140.0 0.8 LFLTTZ M8E6T6 MDKW7J 460.0 40.0 0.2 PSXQYE 1900.0 1400.0 8.4 QHGM5Q 480.0 20.0 0.1 SAV6NX 612.0 112.0 0.7 WIYO85 517.0 17.0 0.1 WWSTWW 500.0 0.0 0.0 XJZEEE 961.0 461.0 2.8 XTLXKX 447.0 53.0 0.3

2013/1-BS (28) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-2/Amfetamine Median = 1118.5 MAD = 138. UNODC value = 1143

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

(29) Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-2/Nordazepam Median = 1652.1 MAD = 241.9 UNODC value = 1727

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

(30) Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-2/Oxazepam Median = 470 MAD = 48 UNODC value = 457

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

(31) Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-2/Temazepam Median = 500 MAD = 112 UNODC value = 464

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 3 Analysis

Identified substances for Test Sample 3 Code Identified Substances 0709WO GHB 2I1J7W GHB 3ESBDT None 5A0LTW GHB 76JL37 GHB ABBR1D GHB AKQ21O GHB BPL9ZY GHB, GBL CUH0QQ NONE DONO2Y GHB J2FAYZ nordiazepam below cut-off JLCQ3D ANY DRUGS JZ6JTH Morphine MDKW7J amphetamine, nodiazepam, oxazepam and temazepam PSXQYE gamma-Hydroxybutyric acid (GHB) SAV6NX GHB WWSTWW GHB XA9AAA GHB XTLXKX gamma-Hydroxybutyric acid

2013/1-BS (33) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 3

Code gamma- Hydroxybutyric acid (GHB) 0709WO + - 1C2WN2 ANP caffeine 1M39MI ANP

2I1J7W +

3ESBDT ANP Negative 5A0LTW +

5D8EIT ANP The contain caffeine. 6H33U3 ANP No drugs detected in sample BS3. 6ZZZCD ANP

76JL37 + Findings indicate that the person consumed GHB. 7HEM7O -

98KDM8 ANP

ABBR1D +

AKQ21O + The presence of GHB indicates the use of GHB or GBL. ANXWGY ANP No drugs was detected BBRB0E ANP we did not find any controlled drug in BS-3

2013/1-BS (34) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code gamma- Hydroxybutyric acid (GHB) BJG4OO ANP not detected any of the substances investigated BPL9ZY + We also found caffeine in BS-3. BVABMB ANP

CUH0QQ - IN THE ROUND AS LABELED "ROUND ICE 2013/1 SAMPLE BS-3" NOT DETECTED METABOLITES OF COCAINE, CANNABINOIDS, BENZODIAZEPINES, AMPHETAMINES, PHENOTHIAZINES AND TRICYCLIC . CUUFFQ ANP

CWOOM9 -

CZJD27 ANP No drugs found based on test performed D7TTWV ANP NO SE DETECTÓ DONO2Y + The concentration of GHB (>10 mg/L) reflect a suspicion case of recreative use or drug-facilitated crime. ERWOWW -

FNSUKR ANP En inmunoensayo una concentración menor al punto de corte indica que el sistema analítico no detectó la presencia de cocaína, cannabinoides , anfetaminas, barbitúricos ni benzodiacepinas. FZZZZQ ANP

ILS9UP ANP

J2FAYZ - we have not received standards J6WWIX ANP

JBUJJA ANP

2013/1-BS (35) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code gamma- Hydroxybutyric acid (GHB) JLCQ3D ANP The sample BS-3 no contain any drugs JWS3VW ANP

JZ6JTH ANP

KHMLHA ANP

KKPG9K ANP

LFLTTZ ANP

M8E6T6 ANP

MDKW7J ANP

NDS3R3 ANP

OOOQSO ANP

PSXQYE + Sample is positive for Gamma-Hydroxybutyric acid (GHB) QHGM5Q -

RFGGQG ANP

SAV6NX + GHB is a controlled substance since 1999 in France. GHB has been used in a medical setting as a general anesthesic. GHB is a central nervous system used as an intoxicant TTAVXV ANP

UM0M1S -

VHDEKU ANP

2013/1-BS (36) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code gamma- Hydroxybutyric acid (GHB) WIYO85 - BS3 was negative for supplied standards WWSTWW +

XA9AAA + GHB was detected, cuantitication was not performed, but the sample concentration was greater than a urine sample containing 10000 ng/ml XDXVS9 ANP On analysis, no drugs found in the sample of 2013/1/BS-3. XJZEEE ANP

XLEICI ANP

XTLXKX + Abuse of GHB salt or GBL or 1,4-butanediol, if there is no succinic semialdehyde dehydrogenase deficiency (SSADH). XXHQNV ANP None Detected YCEET4 ANP

2013/1-BS (37) Copyright (c) 2013 UNODC 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

Analytical Technique Codes Code 110 120 150 161 170 171 180 230 231 210 0709WO SI 1C2WN2 S I I 1M39MI S SI 2I1J7W S I I 3ESBDT S I I 5A0LTW S I I 5D8EIT S I 6H33U3 I 6ZZZCD S I 76JL37 S I I 7HEM7O S I I 98KDM8 S I ABBR1D S I I AKQ21O S I SI I ANXWGY S I BBRB0E S I BJG4OO S I BPL9ZY S SI SI BVABMB SI CUH0QQ S I CUUFFQ S I CWOOM9 S I I CZJD27 I I S DT kits D7TTWV S DONO2Y S I I ERWOW S I W FNSUKR S I FZZZZQ SI ILS9UP S I I S Kinetic Interactions of microparticles J2FAYZ I I immunochem J6WWIX S I I JBUJJA S I I I JLCQ3D SI I

2013/1-BS (38) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 110 120 150 161 170 171 180 230 231 210 JWS3VW S I JZ6JTH S I I KHMLHA S I KKPG9K SI S Multi-Drug Screen Test Panel LFLTTZ I S Dipromed Drulab screen M8E6T6 S I MDKW7J SI I NDS3R3 S S I OOOQSO S I PSXQYE S S I I QHGM5Q I I SI I RFGGQG S SI SAV6NX S I I TTAVXV S I I I I UM0M1S S I VHDEKU SI I WIYO85 S I WWSTW S I I W XA9AAA S I S Lateral Flow Immunoassay XDXVS9 I SI XLEICI S I XTLXKX S I I XXHQNV S I YCEET4 I

2013/1-BS (39) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 3 The response summary of all 54 participating laboratories for the identification of BS-3, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 3:

Response Summary Participants: 58

gamma-Hydroxybutyric acid (GHB): 13

False positives for Test Sample 3

Name Technique CodeJZ6JTH Morphine 230 J2FAYZ Name Nordazepam Technique 180 MDKW75 Amfetamine, Nordazepam, in report MDKW75 Oxazepam, Temazepam in report

False negatives for BS-3 . Within BS-3, there were: 8 false negatives for GHB by participants using analytical techniques CUHOQQ (180), QHGM5Q (171/180), UM0MIS (180), WIYO85 (231), ERWOWW (180)

CWOOM9 (180), 7HEM7O (171/180), J2FAYZ (180) 37 false negatives by particpants who did not carry out analyses for GHB

Frequency of use of screening and identification techniques: R Response Summary Response Summary Participants: 54 Participants: 58 Section Section 110 120 150 161 170 171 180 230 231 210 Screening 36 8 4 0 0 0 9 1 1 4 62.1% 13.8% 6.9% 0.0% 0.0% 0.0% 15.5% 1.7% 1.7% 6.9% Identification 4 0 3 11 2 2 49 5 12 2 6.9% 0.0% 5.2% 19.0% 3.4% 3.4% 84.5% 8.6% 20.7% 3.4% # labs using 36 8 7 11 2 2 49 6 12 6 this 62.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3% technique

2013/1-BS (40) Copyright (c) 2013 UNODC

2013/1-BS (14) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 3

gamma-Hydroxybutyric acid (GHB) CODE MAD: 1114.5 Conc. * AbsDev ZScore 0709WO 15500.0 575.0 0.3 5A0LTW 14350.0 575.0 0.3 ABBR1D 16500.0 1575.0 1.0 BPL9ZY 14300.0 625.0 0.4 DONO2Y 17.8 14907.2 9.0 140100.0 125175. 75.8 PSXQYE 0 SAV6NX 14283.0 642.0 0.4 WWSTWW 15579.0 654.0 0.4 XTLXKX 10543.0 4382.0 2.7

*) Concentration: ng/ml

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

2013/1-BS (41) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: BS-3/gamma-Hydroxybutyric acid (GHB) Median = 14925 MAD = 1114.5 UNODC value = 14427

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 76JL37 ephedrine 1M39MI ephedrine BPL9ZY ephedrine KKPG9K ephedrine MDKW7J ephedrine NDS3R3 ephedrine WWSTWW ephedrine OOOQSO ephedrine RFGGQG ephedrine UM0M1S ephedrine 5D8EIT ephedrine

Response Summary Participants: 58

2013/1-BS (43) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 4

Code [blank sample] 0709WO -

1C2WN2 caffeine

1M39MI sample positive for ephedrine

2I1J7W

3ESBDT Negative

5A0LTW

5D8EIT The sample contain pseudoephedrine / ephedrine and caffeine.

6H33U3 No drugs detected in sample BS4.

6ZZZCD

76JL37 Findings indicate that the person consumed ephedrine or pseudoephedrine.

7HEM7O

98KDM8

ABBR1D

AKQ21O No drugs found.

ANXWGY No drugs was detected

BBRB0E we did not find any controlled drug in BS-4

BJG4OO not detected any of the substances investigated

2013/1-BS (44) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code [blank sample] BPL9ZY We also found caffeine and ephedrine in BS-4.

BVABMB

CUH0QQ IN THE ROUND AS LABELED "ROUND ICE 2013/1 SAMPLE BS-4" NOT DETECTED METABOLITES OF COCAINE, CANNABINOIDS, BENZODIAZEPINES, AMPHETAMINES, PHENOTHIAZINES AND TRICYCLIC ANTIDEPRESSANTS. CUUFFQ

CWOOM9

CZJD27 No drugs found based on test performed

D7TTWV NO SE DETECTÓ

DONO2Y The concentration of GHB reflect the physiological concentrations.

ERWOWW

FNSUKR En inmunoensayo una concentración menor al punto de corte indica que el sistema analítico no detectó la presencia de cocaína, cannabinoides , anfetaminas, barbitúricos ni benzodiacepinas.

FZZZZQ

ILS9UP

J2FAYZ we have not received standards

J6WWIX

JBUJJA

JLCQ3D The sample BS-4 no contain any drugs

JWS3VW

2013/1-BS (45) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code [blank sample] JZ6JTH

KHMLHA

KKPG9K The sample contains ephedrine.

LFLTTZ

M8E6T6

MDKW7J sample 5 contains ephedrine (GC-MS)

NDS3R3 ephedrine was found in the sample

OOOQSO ephedrine was identified in sample 2013/1/BS-4 by LC/MS and its presence was confirmed by LC/MS/MS

PSXQYE Sample contains no substance from the ICE menu

QHGM5Q

RFGGQG sample positive for ephedrine

SAV6NX

TTAVXV

UM0M1S Screening and conformation by GC-MS : Positive

VHDEKU

WIYO85 BS4 was negative for supplied standards

WWSTWW Ephedrine is found in BS-4, but ephedrine is not the controlled drug.

2013/1-BS (46) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code [blank sample] XA9AAA

XDXVS9 On analysis, no drugs found in the sample of 2013/1/BS-4.

XJZEEE

XLEICI Phenmetrazine was found in BS-4.

XTLXKX

XXHQNV None Detected

YCEET4

2013/1-BS (47) Copyright (c) 2013 UNODC 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

Analytical Technique Codes Code 110 120 150 161 170 171 180 230 231 210 0709WO SI 1C2WN2 S I I 1M39MI S SI 2I1J7W S I I 3ESBDT S I I 5A0LTW S I I 5D8EIT S I 6H33U3 I 6ZZZCD S I 76JL37 S I I 7HEM7O S I I 98KDM8 S I ABBR1D S I I AKQ21O S I SI I ANXWGY S I BBRB0E S I BJG4OO S I BPL9ZY S SI SI BVABMB SI CUH0QQ S I CUUFFQ S I CWOOM9 S I I CZJD27 I I S DT kits D7TTWV S DONO2Y S I I ERWOW S I W FNSUKR S I FZZZZQ SI ILS9UP S I I S Kinetic Interactions of microparticles J2FAYZ I I immunochem J6WWIX S I I JBUJJA S I I I JLCQ3D SI I

2013/1-BS (48) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 110 120 150 161 170 171 180 230 231 210 JWS3VW S I JZ6JTH S I I KHMLHA S I KKPG9K SI S Multi-Drug Screen Test Panel LFLTTZ I S Dipromed Drulab screen M8E6T6 S I MDKW7J SI I NDS3R3 S S I OOOQSO S I PSXQYE S S I I QHGM5Q I I SI I RFGGQG S SI SAV6NX S I I TTAVXV S I I I I UM0M1S S I VHDEKU SI I WIYO85 S I WWSTW S I I W XA9AAA S I S Lateral Flow Immunoassay XDXVS9 I SI XLEICI S I XTLXKX S I I XXHQNV S I YCEET4 I

2013/1-BS (49) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 4 The response summary of all 54 participating laboratories for the identification of BS-4, frequency of use of screening and identification techniques and false positives and negatives:

Identified substances for Test Sample 4 Code Identified Substances 76JL37 ephedrine 1M39MI ephedrine BPL9ZY ephedrine KKPG9K ephedrine MDKW7J ephedrine NDS3R3 ephedrine WWSTWW ephedrine OOOQSO ephedrine RFGGQG ephedrine UM0M1S ephedrine 5D8EIT ephedrine

False positives for Test Sample 4 Code Name Code Name Technique Code DONO2Y G amma-Hydroxybutyric acid (GHB) 180 JZ6JTH Methyle cgonine , Benzoylecgonine 230 XLEICI Phenmetrazine 180 YCEET4 MetamfetaminName ee 1 180 Technique J2FAYZ Nordazepam 180

Frequency of use of screening and identification techniques: Response R Summary

Participants: 58

Section 110 120 150 161 170 171 180 230 231 210 Screening 36 8 4 0 0 0 9 1 1 4 62.1% 13.8% 6.9% 0.0% 0.0% 0.0% 15.5% 1.7% 1.7% 6.9% Identification 4 0 3 11 2 2 49 5 12 2 6.9% 0.0% 5.2% 19.0% 3.4% 3.4% 84.5% 8.6% 20.7% 3.4% # labs using 36 8 7 11 2 2 49 6 12 6 this 62.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3% technique 2013/1-BS Copyright (c) 2013 UNODC (50)

Response Summary Participants: 54

2013/1-BS (14) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

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

2013/1-BS (51) Copyright (c) 2013 UNODC