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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMENS 2013/1

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) … · 2013. 10. 9. · CWOOM9 codeine, morphine, 6-mam CZJD27 morphine, codeine D7TTWV OPIÁCEOS DONO2Y 6-MAM, codeine, morphine

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  • INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

    INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

    Summary ReportBIOLOGICAL SPECIMENS

    2013/1

  • Samples Substances Concentrations Comments on substancesSample 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]

    Test Samples Information

    Samples Comments on samplesSample 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), Oxazepam (457ng/ml) and Temazepam (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.

    2013/1-BS Copyright (c) 2013 UNODC(2)

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

    Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3

    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

  • 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 benzodiazepines (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 diazepam. 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)

  • Codes and Abbreviations

    Tech Code Name100 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

    (+) “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.

    2013/1-BS Copyright (c) 2013 UNODC(4)

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

  • Identified substances for Test Sample 1

    Code Identified Substances0709WO 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

    Sample 1 Analysis

    2013/1-BS Copyright (c) 2013 UNODC(5)

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

  • Code Identified SubstancesQHGM5Q 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 Copyright (c) 2013 UNODC(6)

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

  • Code 6-Monoacetylmorphine (6-MAM)

    Codeine Morphine (Total)

    0709WO + + +-

    1C2WN2 + + +morphinecodeine6-monoacetylmorphinecaffeine

    1M39MI + + +sample positive for opiates

    2I1J7W + + +

    3ESBDT + + ANPCodeine 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 + + ANPCodeine 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

    Statement of findings for Test Sample 1

    2013/1-BS Copyright (c) 2013 UNODC(7)

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

  • Code 6-Monoacetylmorphine (6-MAM)

    Codeine Morphine (Total)

    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 ANPPOSITIVO (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 Copyright (c) 2013 UNODC(8)

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

  • Code 6-Monoacetylmorphine (6-MAM)

    Codeine Morphine (Total)

    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 Copyright (c) 2013 UNODC(9)

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

  • Code 6-Monoacetylmorphine (6-MAM)

    Codeine Morphine (Total)

    TTAVXV + + +The 6-monoacetylmorphine detection indicates heroin consumption, codeine could bepresent 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 theintake of the drug itself.

    UM0M1S + + +Screening by immunoassay technich : PositiveConformation 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 + + ANPOn analysis, the sample of 2013/1/BS-1 found to contain Codeine and 6-Monoacetylmorphine.

    XJZEEE ANP ANP ANPFree 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 Copyright (c) 2013 UNODC(10)

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

  • Identification methods for Test Sample 1

    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

    ERWOWW

    S I

    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

    Analytical Technique Codes

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

    2013/1-BS Copyright (c) 2013 UNODC(11)

    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

    WWSTWW

    S I I

    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 Copyright (c) 2013 UNODC(12)

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

  • DONO2Y gamma-Hydroxybutyric acid 180

    J6WWIX Methadone 180

    JZ6JTH Amfetamine

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

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

    110 120

    Response Summary Participants: 54

    Frequency of use of screening and identification techniques:

    H

    Summary for test sample 1The response summary of all 54 participating laboratories for the identification of BS-1, frequency of use of screening andidentification techniques and false positives and negatives:

    Identification of test sample 1:

    False positives for Test Sample 1

    Response SummaryParticipants: 58

    6-Monoacetylmorphine (6-MAM): 46

    Codeine: 53

    Morphine (Total): 46

    Code Name Technique

    230

    5D8EIT Morphine-3-glucuronide 180

    J2FAYZ Methadone 180

    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 this technique

    36 8 7 11 2 2 49 6 12 662.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3%

    Response Summary Participants: 58

    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

  • Z-Scores for Test Sample 1

    CODE

    6-Monoacetylmorphine (6-MAM)MAD: 100.0

    CodeineMAD: 119.5

    Morphine (Total)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/MADAbsDev = 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 Copyright (c) 2013 UNODC

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

    (14)

  • Substance: BS-1/6-Monoacetylmorphine (6-MAM) 100MAD =Median = 552.5

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 576

    (15)

  • Substance: BS-1/Codeine 120MAD =Median = 1066

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 1150

    (16)

  • Substance: BS-1/Morphine (Total) 440.4MAD =Median = 2272.5

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 2300

    (17)

  • Identified substances for Test Sample 2

    Code Identified Substances0709WO 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

    Sample 2 Analysis

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  • Code Identified SubstancesQHGM5Q 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

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  • Code Amfetamine Nordazepam Oxazepam Temazepam0709WO + + + +

    -

    1C2WN2 + + + +amphetamineoxazepamnordiazepamtemazepamcaffeine

    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

    Statement of findings for Test Sample 2

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  • Code Amfetamine Nordazepam Oxazepam TemazepamBBRB0E + 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 demoxepam 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 standardCUH0QQ + + + -

    IN THE ROUND AS LABELED "ROUND ICE 2013/1 SAMPLE BS-2" DETECTED DIAZEPAM, OXAZEPAM, NORDIAZEPAM AND AMPHETAMINE.

    CUUFFQ + + + +

    CWOOM9 + + - -

    CZJD27 + + + ANPTest 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 ANPPOSITIVO (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

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  • Code Amfetamine Nordazepam Oxazepam TemazepamJ6WWIX + + + +

    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 medazepam

    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 anxiolytic and sedativ properties and also to treat epilepsy. Are also 3 metabolites of diazepam and their presence may indicates a diazepam consumption.

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  • Code Amfetamine Nordazepam Oxazepam TemazepamTTAVXV + + + +

    The oxazepam, nordiazepam and temazepam detection indicates most likely: diazepamconsumption, nevertheless the presence of these substances could come from the intake ofthe drugs itself or come from the intake of any other benzodiazepine that producesdiazepam as a metabolite.The amphetamine detection indicates the intake of the drug itself or could come from themetabolism of other drugs such as methamphetamine.

    UM0M1S + + - -Screening by immunoassay technich : PositiveConformation 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 consumedIn 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

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  • Identification methods for Test Sample 2

    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

    ERWOWW

    S I

    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

    Analytical Technique Codes

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

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  • 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

    WWSTWW

    S I I

    XA9AAA S I S Lateral Flow Immunoassay

    XDXVS9 I SI

    XLEICI S I

    XTLXKX S I I

    XXHQNV S I

    YCEET4 I

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

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    Section 110 120

    Response Summary Participants: 54

    Frequency of use of screening and identification techniques:

    H

    Summary for test sample 2The response summary of all 54 participating laboratories for the identification of BS-2, frequency of use of screening andidentification techniques and false positives and negatives:

    Identification of test sample 2:

    False positives for Test Sample 2

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

    Response SummaryParticipants: 58

    Amfetamine: 39

    Nordazepam: 49

    Oxazepam: 30

    Temazepam: 37

    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

    Code

    Name TechniqueMDKW75 Codeine, Morphine, 6-MAM in report

    JWS3VW Diazepam 180

    Name6ZZZCD Metamfetamine 150

    BBRB0E Diazepam 150

    BPL9ZY Diazepam, Demoxazepam 231

    CUH0QQ Diazepam 180

    DONO2Y gamma-Hydroxybutyric acid (GHB) 180

    JZ6JTH 180

    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 this technique

    36 8 7 11 2 2 49 6 12 662.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3%

    Response Summary Participants: 58

  • Z-Scores for Test Sample 2

    CODEAmfetamineMAD: 138.0

    NordazepamMAD: 241.9

    OxazepamMAD: 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/MADAbsDev = 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

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  • CODETemazepamMAD: 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

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    (28)

  • Substance: BS-2/Amfetamine 138.MAD =Median = 1118.5

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 1143

    (29)

  • Substance: BS-2/Nordazepam 241.9MAD =Median = 1652.1

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 1727

    (30)

  • Substance: BS-2/Oxazepam 48MAD =Median = 470

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 457

    (31)

  • Substance: BS-2/Temazepam 112MAD =Median = 500

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 464

    (32)

  • Identified substances for Test Sample 3

    Code Identified Substances0709WO 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

    Sample 3 Analysis

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  • Code gamma-Hydroxybutyric acid (GHB)

    0709WO +-

    1C2WN2 ANPcaffeine

    1M39MI ANP

    2I1J7W +

    3ESBDT ANPNegative

    5A0LTW +

    5D8EIT ANPThe contain caffeine.

    6H33U3 ANPNo 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 ANPNo drugs was detected

    BBRB0E ANPwe did not find any controlled drug in BS-3

    Statement of findings for Test Sample 3

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  • Code gamma-Hydroxybutyric acid (GHB)

    BJG4OO ANPnot 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 ANTIDEPRESSANTS.

    CUUFFQ ANP

    CWOOM9 -

    CZJD27 ANPNo drugs found based on test performed

    D7TTWV ANPNO SE DETECTÓ

    DONO2Y +The concentration of GHB (>10 mg/L) reflect a suspicion case of recreative use or drug-facilitated crime.

    ERWOWW -

    FNSUKR ANPEn 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

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  • Code gamma-Hydroxybutyric acid (GHB)

    JLCQ3D ANPThe 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

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  • 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 ANPOn 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 ANPNone Detected

    YCEET4 ANP

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

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

  • Identification methods for Test Sample 3

    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

    ERWOWW

    S I

    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

    Analytical Technique Codes

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

    2013/1-BS Copyright (c) 2013 UNODC(38)

    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

    WWSTWW

    S I I

    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 Copyright (c) 2013 UNODC(39)

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

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

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

    Section

    Response Summary Participants: 54

    R

    Frequency of use of screening and identification techniques:

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

    Identification of test sample 3:

    False positives for Test Sample

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

    Response SummaryParticipants: 58

    gamma-Hydroxybutyric acid (GHB): 13

    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

    Code

    Name TechniqueMDKW75 Amfetamine, Nordazepam, in report

    MDKW75 Oxazepam, Temazepam in report

    NameJZ6JTH Morphine 230

    J2FAYZ Nordazepam 180

    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 this technique

    36 8 7 11 2 2 49 6 12 662.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3%

    Response Summary Participants: 58

  • Z-Scores for Test Sample 3

    CODE

    gamma-Hydroxybutyric acid (GHB)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

    PSXQYE 140100.0 125175.075.8

    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/MADAbsDev = 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 Copyright (c) 2013 UNODC

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  • Substance: BS-3/gamma-Hydroxybutyric acid (GHB) 1114.5MAD =Median = 14925

    Round: 2013/1

    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/MADAbsDev = 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

    Z-Score Report per Sample per Substance

    UNODC value = 14427

    (42)

  • Identified substances for Test Sample 4

    Sample 4 Analysis

    2013/1-BS Copyright (c) 2013 UNODC(43)

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

    Code

    Response Summary Participants: 58

    Identified Substances76JL37 ephedrine

    1M39MI ephedrine

    BPL9ZY ephedrine

    KKPG9K ephedrine

    MDKW7J ephedrine

    NDS3R3 ephedrine

    WWSTWW ephedrine

    OOOQSO ephedrine

    RFGGQG ephedrine

    UM0M1S ephedrine

    5D8EIT ephedrine

  • 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

    Statement of findings for Test Sample 4

    2013/1-BS Copyright (c) 2013 UNODC(44)

    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 Copyright (c) 2013 UNODC(45)

    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 Copyright (c) 2013 UNODC(46)

    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 Copyright (c) 2013 UNODC(47)

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

  • Identification methods for Test Sample 4

    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

    ERWOWW

    S I

    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

    Analytical Technique Codes

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

    2013/1-BS Copyright (c) 2013 UNODC(48)

    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

    WWSTWW

    S I I

    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 Copyright (c) 2013 UNODC(49)

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

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

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

    False positives for Test Sample 4Code

    R

    Frequency of use of screening and identification techniques:

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

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

    Response SummaryParticipants: 54

    Identified substances for Test Sample 4

    Code

    CodeCode

    Name TechniqueJ2FAYZ Nordazepam 180

    Name

    Name

    DONO2Y Gamma-Hydroxybutyric acid (GHB) 180

    JZ6JTH Methylecgonine, Benzoylecgonine 230

    XLEICI Phenmetrazine 180

    YCEET4 Metamfetamine 180

    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 this technique

    36 8 7 11 2 2 49 6 12 662.1% 13.8% 12.1% 19.0% 3.4% 3.4% 84.5% 10.3% 20.7% 10.3%

    Response Summary Participants: 58

    Identified Substances76JL37 ephedrine

    1M39MI ephedrine

    BPL9ZY ephedrine

    KKPG9K ephedrine

    MDKW7J ephedrine

    NDS3R3 ephedrine

    WWSTWW ephedrine

    OOOQSO ephedrine

    RFGGQG ephedrine

    UM0M1S ephedrine

    5D8EIT ephedrine

    (50)

  • The Laboratory and Scientific SectionUNODC, International CentreWagramer Strasse 5, P.O. Box 500A-1400, Vienna, AUSTRIAEmail: [email protected]

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    (51)