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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMEN 2016/2

INTERNATIONAL QUALITY ASSURANCE … PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMEN6 2016/2 This report contains the data received from

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Page 1: INTERNATIONAL QUALITY ASSURANCE … PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMEN6 2016/2 This report contains the data received from

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary ReportBIOLOGICAL SPECIMENS

2016/2

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This report contains the data received from laboratories participating in the current exercise. The results compiled in this report are not intended to be an overview of the quality of work and cannot be interpreted as such. These comments do not reflect the general state of the art within the profession.

Participant results are reported using a randomly assigned "WebCode". This code maintains participant's anonymity, provides linking of the various report sections, and will change with every report.

Samples Substances Concentrations Comments on substances

Sample 1 Morphine (Total) 1138 ng/ml

Sample 2 Benzoylecgonine 690 ng/ml

Methylecgonine 350 ng/ml

Morphine (Total) 1138 ng/ml

Sample 3 3,4-Methylenedioxymetamfetamine (MDMA) 1955 ng/ml

Sample 4 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

1724 ng/ml

Test Samples InformationSamples Comments on samples

Sample 1 To prepare BS-1, urine was spiked with an aqueous solution of morphine sulphate (1138ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

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

Sample 3 To prepare BS-3, urine was spiked with an aqueous solution of MDMA hydrochloride (1955ng base/ml) . The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 4 To prepare BS-4, urine was spiked with a methanol solution of 2C-B hydrochloride (1724ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

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Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 NPS reported by ICE participants Page 5

Codes and Abbreviations Page 7 Sample 1 Analysis Page 8 Identified substances Page 8

Statement of findings Page 10 Identification methods Page 15

Summary Page 18 Z-Scores Page 19 Sample 2 Analysis Page 22 Identified substances Page 22

Statement of findings Page 24 Identification methods Page 29

Summary Page 32 Z-Scores Page 33 Sample 3 Analysis Page 41

Identified substances Page 41 Statement of findings Page 43 Identification methods Page 48 Summary Page 51

Z-Scores Page 52 Sample 4 Analysis Page 55

Identified substances Page 55 Statement of findings Page 57 Identification methods Page 62 Summary Page 65

Z-Scores Page 66

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Introduction

Comments from the International Panel of Forensic Experts

Participation of Laboratories In the 2016/2 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 225 laboratories in 73 countries. Within the SM test group, there were 181 participating laboratories from 67 countries and within the BS test group, results were submitted by 89 laboratories from 44 countries.1 Qualitative Analysis The analytical techniques most commonly used for screening of test samples in the BS test group were enzyme immunoassays (55% of participants), while GC-MS (81%) was the most commonly used technique for identification/confirmation of the components in the test samples. The results for the qualitative identification of the sample components in the BS test group, the number of false positive/negative results and the analyses not performed are shown in the table 1.

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

Test sample BS-1 (Morphine)

BS-2 (Benzoylecgonine)

BS-2 (Methylecgonine)

BS-2 (Morphine)

Correct identification 79% 69% 71% 75% Number of false

positives 3 8

Number of false negatives 6 4

Number of analyses not performed

(ANP) 8 4

Test sample BS-3 BS-4

(MDMA) (2C-B)

Correct identification 90% 61% Number of false

positives 8 1

Number of false negatives 2 12

Number of analyses not performed

(ANP) 3 24

1 A small number of laboratories received test samples from the 2016/1 ICE round due to an administrative error and they

have received individual evaluation reports based on the analyses they carried out,.

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An important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. This report provides information on analytical results of laboratories participating in the Seized Materials (SM) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact. The ICE programme is a UNODC mandated activity and is implemented through regular budget funds and through the UNODC Global Scientific and Forensic Programme – Support Project (GLOU54), which operationalizes the forensic aspects of the UNODC Thematic Programme on Research, Trend Analysis and Forensics"

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Laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. ICE participants are reminded that test samples can contain any of the substances in the ICE menu and as such if methods are available, all substances should be considered. Quantitative Analysis The test samples in the BS group for the 2016/2 round of ICE contained a total of six components and 39 (44%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to note that 92% of laboratories quantified at least two components and 33% performed quantification of all components present. GC-MS was used by 58% of participants for quantification, followed by LC/MS(/MS), which was used by 45% of participants. Z-scores obtained by participants in quantification are shown in the table below (percentage + no. of labs indicated).

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

z-score

Test sample

BS-1 (Morphine)

BS-2 (Benzoylecgonine)

BS-2 (Methylecgonine)

|z| < 2, satisfactory 84% (26) 83% (29) 83% (19) 2 ≤ |z| ≤ 3,

questionable 10% (3) 14% (5) 13% (3)

|z| > 3, unsatisfactory 6% (2) 3% (1) 4%(1)

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

|z| < 2, satisfactory 87% (27) 81% (29) 90% (18) 2 ≤ |z| ≤ 3,

questionable 6% (2) 8% (3) 10% (2)

|z| > 3, unsatisfactory 6% (2) 11% (4) 0 According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation. Participants with z-scores outside acceptable limits should review their quantification procedures. In the 2016/1 round of ICE, seven laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Six of these laboratories participated and performed quantification in the 2016/2 round with five laboratories obtaining satisfactory z-scores in all of their quantitative analysis, while one laboratory obtainine a questionable z-score in its analysis. Seven laboratories obtained unsatisfactory z-scores in ICE 2016/1 with |z| ≥ 3. Of these laboratories, six participated in ICE 2016/2 and performed quantification, with all improving their performance to obtain satisfactory z-scores in at least one sample. Two of these laboratories also obtained unsatisfactory z-scores and three obtained questionable z-scores. Laboratories that need to perform quantitation routinely are encouraged to participate regularly in external proficiency testing or collaborative exercises such as the ICE programme. This will enable laboratories to assess the quality of their quantitative methods through the z-score values obtained. Laboratories reporting false positive or false negative results should investigate the root causes and corrective actions taken promptly in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. UNODC would like to acknowledge the valuable contribution of the Chemical Metrology Laboratory of the Health Sciences Authority, Singapore, for the provision of specific software used for the quantitative statistical calculations in the ICE programme.

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

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

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

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

32%

32%

20%

7% 4% 2% 2%

1%

Synthetic cannabinoids

Synthetic cathinones

Others

Phenethylamines

Ketamine and phencyclidinetype substances

Tryptamines

Aminoindanes

Piperazines

42%

32%

9%

7% 6%

4%

Stimulants

SCRA's

Opioids

Hallucinogens

Dissociatives

Sedatives/Hypnotics

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NPS most commonly reported by laboratories participating in ICE 2016/2 The substances most often reported by ICE participants were the synthetic cannabinoid receptor agonists 5F-MDMB-PINACA (methyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate, AB-CHMINACA (N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-1H-indazole-3-carboxamide and the synthetic opioid furanylfentanyl (N-(1-phenethylpiperidin-4-yl)-N-phenylfuran-2-carboxamide. For further details on these substances and others reported to the UNODC Early Warning Advisory, ICE participants can log on to the UNODC ICE portal and select the icon for the Early Warning Advisory on New Psychoactive substances as shown below.

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Codes and Abbreviations

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

(+) “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.

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Identified substances for Test Sample 1

Code Identified Substances123WGB MORPHINE

1PWJNH Morphine

1TTIML None

1TZH5Y 7 amino flunitrazepam

3DKQOQ Morphine

419F4M morphine

44TU44 Morphine

4GHNH4 morphine

4YLFBL morphine

66ZO6A morphine

6CVGQ6 Morphine, Total

6JIYPR Morfina

6V1XQX Morphine

8IIDK3 morphine

ALUS4Z MORPHINE

AVERAC morphine

CQGC6C Morphine

CRKFUT morphine

DUZUY3 Morphine

DZKP99 Morphine

EGCC8D Morphine

EHOHKH MORPHINE

ERZR0K morfina

EXR666 MORPHINE

FFAFFI MORPHINE

FQFOEF Morphine

FZ5ZGY morphine

GIGLLN morphine

HZ4SSF Morphine

IGGUCG Morphine

IGGZSA Morphine

IM9MIS Morphine

ITEOXF Morphine

J77027 opiates / opioids

JHMWJW morphine, norbuprenorphine

JL1GTU Morphine

JPRPXO Morphine

KFFG6N Morphine

KQ4LD7 Not detected

KSEXBG no drugs detected

Sample 1 Analysis

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Code Identified SubstancesL6XLFB Morphine

LALDP0 morphine

LB5MQU Morphine

LMAFMM Codeine and 7-Aminoflunitrazepam

MDKNFX Morphine

MM3MAK Morphine

MQULMG morphine

NNNKNN metanfetamina

NOGTSO Morphine

O55XS5 Morphine

OOIXLI Morphine

OSOXXO Morfine

P45IGJ morphine

PB44MH Morphine

PFCACT morphine

PMG9F9 morphine

PPPPYM morphine

QDJMOE Morphine

QPIOKN morphine

RFIBGP Morphine

RQEEOE morphine

RSYHBH 7-aminoflunitrazepam

RXYG2Q Morphine

U5AWA0 Morphine

U8NKUE Morphine

V8HYSI Morphine

VAXCAO Morphine

VE1EEZ None

VLA1JO morphine

W3E7JE MORPHINE

WFA0FD morphine

WVFKZV Morphine

XIKHP6 morphine

XZURKZ morphine

YZOFYZ Morphine

Z25SYN Morphine

ZVTR4A 7-Aminoflunitrazepam

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Code Morphine (Total)

0O03BD -

The test sample 2016/2/BS-1 do not found to contain any drugs.

123WGB +

1PWJNH +

We found Morphine in BS-1

1TTIML -

We did not find any drugs. We found only caffein and Procaine.-

3DKQOQ +

Urine specimen contains 1017.1 ng/mL Morphine

419F4M +

Positive to morphine.

4444FB +

44TU44 +

Sample is positive for Morphine

4GHNH4 +

4YLFBL +

Positive to morphine.

66ZO6A +

6CVGQ6 +

Morphine, Total- Detected > 0.5mg/L

6JIYPR +

Hubo Consumo de Morfina

6V1XQX +

This person consumed morphine and/or heroin.

8IIDK3 +

morphine is an analgesic opiate used in France to treat intense pain; it is also a controlled drug in France. Morphine is also a metabolite of heroine (controlled drug) and 3 antitussive drugs (codeine, pholdocine, ethylmorphine)

ALUS4Z +

AVERAC +

CQGC6C +

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

CRKFUT +

DUZUY3 +

The presence of Morphine in urine indicates consumption of the drug itself or the intake of other drugs.

DZKP99 +

can be issued from medical prescription or from heroin

Statement of findings for Test Sample 1

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Code Morphine (Total)

EGCC8D +

Sample BS1 found to contain morphine, measured value 1271 ng/ml

EHOHKH +

MORPHINE DETECTED

EP2WDI ANP

ERZR0K +

Preliminary test followed by the analytical confirmation, then the quantification.

EXR666 +

FFAFFI +

In sample 2016/2/BS-1 was found an confirmed the presence of MORPHINE

FQFOEF +

Morphine intake

FZ5ZGY +

sample BS-1 contain morphine

GIGLLN +

Morphine use or abuse.

GTUFSO +

GXURZK ANP

Test sample 2016/2/BS-1 does not contain controlled drugs therefore Negative.

HZ4SSF +

-

IGGUCG +

The sample contains morphine.

IGGZSA +

IKPH39 +

MORPHINE DI-TMS DERIVATIVE

IM9MIS +

In the sample was detected Morphine, this finding indicates that Morphine was consumed.

ITEOXF +

Morphine was identified by GC-MS.

J77027 ANP

The test sample 2016/2/BS-1 shows a positive result over 2000 ng/mL.

JHMWJW +

coffeine, theophylline

JL1GTU +

JPRPXO +

JYO93J -

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

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Code Morphine (Total)

KFFG6N +

Free morphine was detected at concentration of 952.2 ng/mL in the 2016/2/BS-1 sample.

KQ4LD7 -

The specimen was not detected

KSEXBG -

général extraction with four range of pH

L6XLFB +

LALDP0 +

use of morphine

LB5MQU +

Morphine is a narcotic analgesic found in the opium poppy. It is a schedule II controlled substance in the United States.

MDKNFX +

Morphine

MM3MAK +

Morphine was found in the sample. The finding is in accordance with the intake of morphine or heroine, that metabolizes to morphine.

MQULMG +

positive

NNNKNN ANP

metanfetamina: positivo

NOGTSO +

Morphine intake (not heroin)

NW11JK ANP

No common drugs were detected in the sample of 2016/2/BS-1

O55XS5 +

Drugs detected, quantification was not performed

OOIXLI +

GC/MS: Relation m/z, time retention (tR ) the reference material Morphine are equivalents to those sample 2016/2/BS-1

OSOXXO +

P45IGJ +

after chemical analysis was performed the sample was contine 1225.ng/ml morphine

PB44MH +

Sample BS-1 is positive for Morphine

PFCACT +

intake of morphine

PMG9F9 +

PPPPYM +

morphine

Q6EK5S ANP

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

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Code Morphine (Total)

QDJMOE +

In the urine sample (2016-2/BS1) morphine was found.

QPIOKN +

Consistent with previous use of morphine or very pure heroin

RFIBGP +

Sample code number 2016/2/BS-1 was found to contain morphine (concentration 1239 ng/ml)

RQEEOE +

RXYG2Q +

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

U5AWA0 +

Morphine is detected in urine by GC-MS

U5T5NQ +

U8NKUE +

Confirms prior use of heroin/morphine

V8HYSI +

Morphine

VAXCAO +

Morphine was identified in the sample.

VE1EEZ ANP

Sample 2016/2/BS-1 found not to contain any drugs

VLA1JO +

W3E7JE +

WFA0FD +

presence of morphine

WVFKZV +

Morphine was detected in BS-1 sample.

XIKHP6 +

XXMXQX -

XZURKZ ANP

Only free morphine was measured.

YZOFYZ +

Toxicological examination revealed the presence of morphine

Z25SYN +

Morphine detected.

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Code 7-Aminoflunitrazepam

ZVTR4A +

LMAFFM +

1TZH5Y +

RSYHBH +

FVJJJE +

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Identification methods for Test Sample 1

Code 100 110 120 150 160 161 170 180 230 231 210

0O03BD SI

123WGB S I

1PWJNH S I

1TTIML I SI Dipro drug lab screen

1TZH5Y SI

3DKQOQ S SI

419F4M S I

4444FB S I

44TU44 S SI S LC-TOF

4GHNH4 I S BIOCHIP

4YLFBL S I I

66ZO6A S S I SI

6CVGQ6 S I

6JIYPR I SI S randox

6V1XQX S I I

8IIDK3 S I I

ALUS4Z SI I

AVERAC S I

CQGC6C I

CRKFUT S I

DUZUY3 S I I

DZKP99 S I I

EGCC8D S I I

EHOHKH S S SI I

EP2WDI S I

ERZR0K S I

EXR666 S I

FFAFFI SI I

FQFOEF I S KIMS

FVJJJE S I I

FZ5ZGY S I

GIGLLN I I I S

GTUFSO SI S immunochromatographic test

GXURZK I I S Drug Test Kit

Analytical Technique Codes

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

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Code 100 110 120 150 160 161 170 180 230 231 210

HZ4SSF SI

IGGUCG I S Multi-Drug Screen Test Panel

IGGZSA S I SI

IKPH39 SI

IM9MIS I S Lateral Flow Immunoassay

ITEOXF S I

J77027 S

JHMWJW SI I

JL1GTU S I

JPRPXO I S TRIAGE 8-Sure Step

JYO93J S SI

KFFG6N S I SI

KQ4LD7 SI

KSEXBG SI I S immunochromatographique

L6XLFB S I I

LALDP0 S I

LB5MQU I LC-QTOF

LMAFMM S I I

MDKNFX S I SI

MM3MAK S SI

MQULMG SI

NNNKNN S

NOGTSO S I

NW11JK SI

O55XS5 SI

OOIXLI I

OSOXXO I

P45IGJ S S I

PB44MH S I I I

PFCACT S I SI

PMG9F9 SI I SI

PPPPYM SI I I

Q6EK5S S SI I

QDJMOE SI SI

QPIOKN S I I

RFIBGP SI I

RQEEOE SI

RSYHBH SI SI

RXYG2Q S I I

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Code 100 110 120 150 160 161 170 180 230 231 210

U5AWA0 S I

U5T5NQ S I

U8NKUE SI I

V8HYSI S I I S Kinetics Interactions of Microparticles

VAXCAO SI I

VE1EEZ SI

VLA1JO S S I I

W3E7JE S I

WFA0FD S S SI

WVFKZV S I

XIKHP6 I I

XXMXQX SI

YZOFYZ S SI I I LCHRMS

Z25SYN I

ZVTR4A SI I I

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

Frequency of use of screening and identification techniques:

Summary for test sample 1The response summary of all 89 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

Code Name Technique

NNNKNN Metamfetamine 120

Response SummaryParticipants: 89

Morphine (Total): 70

JHMWJW Norbuprenorphine 231

LMAFMM Codeine 180/230

False negatives for BS-1 (technique(s) used or ANP)

Code: XXMXQX (110), 0O03BD (180), KSEXBG (161/180), KQ4LD7 (180), JYO93 (180),

1TTIML (150)

8 laboratories did not carry out analysis for morphine

GXURZK, XZURKZ, NW11JK, J77027, Q6EK5S, VE1EEZ, EP2WDI, NNNKNN

Response Summary

Participants 89Technique 100 110 120 150 160 161 170 180 210 230 231

Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

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

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

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

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17

(%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

18

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1146 ng/ml

Substance: BS‐1; Morphine UNODC value = 1138 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐3.6

‐2.9

‐1.5‐1.4

‐1.1

‐0.8 ‐0.7 ‐0.7‐0.5 ‐0.5 ‐0.4 ‐0.4 ‐0.3 ‐0.3 ‐0.2

0.0

0.1 0.10.3 0.3 0.4 0.5 0.5

0.60.8

1.2 1.3 1.3

2.1

2.6

3.5

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00

JPRP

XO

WFA

0FD

JHMWJW

XZURK

Z

MM3M

AK

66ZO

6A

FQFO

EF

3DKQ

OQ

EXR6

66

6V1X

QX

4444

FB

V8HY

SI

GIGLLN

IGGZSA

NOGT

SO

L6XLFB

MDK

NFX

HZ4SSF

VLA1

JO

8IIDK3

P45IGJ

IGGUCG

RFIBGP

EGCC

8D

PB44

MH

44TU

44

YZOFYZ

PMG9

F9

6JIYPR

ERZR0K

CRKFUT

19

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐1; Morphine

-6

-4

-2

0

2

4

6z-

scor

e

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

LC‐MSGC‐MS

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Z-Scores for Test Sample 1

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Concentration (ng/ml)

Deviation from robust average

z-score

JPRPXO 432 -714 -3.6WFA0FD 582 -564 -2.9JHMWJW 852 -295 -1.5XZURKZ 873 -273 -1.4MM3MAK 925 -221 -1.166ZO6A 998 -148 -0.8FQFOEF 1016 -130 -0.73DKQOQ 1017 -129 -0.7EXR666 1052 -94 -0.56V1XQX 1052 -94 -0.54444FB 1063 -83 -0.4V8HYSI 1076 -70 -0.4GIGLLN 1087 -59 -0.3IGGZSA 1090 -56 -0.3NOGTSO 1110 -36 -0.2L6XLFB 1137 -9 0.0MDKNFX 1160 14 0.1HZ4SSF 1175 29 0.1VLA1JO 1200 54 0.38IIDK3 1212 66 0.3P45IGJ 1225 79 0.4IGGUCG 1238 92 0.5RFIBGP 1239 93 0.5EGCC8D 1271 125 0.6PB44MH 1307 161 0.844TU44 1387 241 1.2YZOFYZ 1395 249 1.3PMG9F9 1410 264 1.36JIYPR 1550 404 2.1ERZR0K 1663 517 2.6CRKFUT 1829 683 3.5

CodeMorphine

21

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Identified substances for Test Sample 2

Code Identified Substances0O03BD Methylecgonine

123WGB MORPHINE, ECGONINE METHYL ESTER

1PWJNH Morphine and Methylecgonine

1TTIML Buprenorphine

1TZH5Y buprenorphine

3DKQOQ Morphine, Methylecgonine

419F4M Benzoylecgonine, Methylecgonine, Morphine

44TU44 Benzoylecgonine, Methylecgonine, Morphine

4GHNH4 morphine, methylecgonine, benzoylecgonine

4YLFBL morphine, methylecgonine and benzoylecgonine

66ZO6A morphine, Methylecgonine, Benzoylecgonine

6CVGQ6 Morphine, Total, Benzoylecgonine, Ecognine Methyl Ester

6JIYPR Morfina

6V1XQX Morphine, cocaine, methylecgonine, benzoylecgonine

8IIDK3 Morphine, Benzoylecgonine (BZE) and methylecgonine (EME)

ALUS4Z COCAINE, MORPHINE

AVERAC morphine, cocaine

CQGC6C Morphine, Benzoylecgonine and Methylecgonine

CRKFUT morphine, benzoylecgonine, methylecgonine

DUZUY3 Morphine, Benzoylecgonine, Methylecgonine.

DZKP99 Morphine, BZE, EME

EGCC8D Morphine, benzoylecgonine, methylecgonine

EHOHKH BENZOYLECGONINE, METHYLECGONINE ESTER AND MORPHINE

EP2WDI Benzoylecoginine

ERZR0K Morphine and Benzoilecgonine

EXR666 MORPHINE, ECGONINE METHYL ESTER, BENZOYL ECGONINE

FFAFFI MORPHINE, BENZOYLECGONINE AND METHYLECGONINE

FQFOEF Morphine, Benzoylecgonine, methylecgonine

FZ5ZGY morphine, ME,BE

GIGLLN morphine, benzoylecgonine

GXURZK Benzoylecgonine

HZ4SSF Morphine,Benzoylecgonine,Methylecgonine

IGGUCG Morphine, benzoylecgonine, methylecgonine

IGGZSA Morphine, benzoylecgonine, methylecgonine

IM9MIS Morphine, Benzoylecgonine,Methylecgonine

ITEOXF Cocaine, Morphine

J77027 Opiates / opioids and Cocaine and/or metabolites

JHMWJW morphine, benzoylecgonine

JL1GTU Morphine, Methylecgonine and Benzoylecgonine

JPRPXO Morphine, Benzoyecgonine, Methylester

Sample 2 Analysis

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Code Identified SubstancesKFFG6N Morphine, benzoylecgonine, methylecgonine

KQ4LD7 Ecgonine methyl ester

KSEXBG Benzoylecgonine

L6XLFB Morphine, Benzoylecgonine, Methylecgonine

LALDP0 methylecgonine, morphine

LB5MQU Mophine, Cocaine metabolites (benzoylecgonine, ecgonine methyl ester)

LMAFMM Norbuprenorphine

MDKNFX Morphine, Benzoylecgonine, Methylecgonine

MM3MAK Morphine, benzoylecgonine

MQULMG cocaïne

NNNKNN cocaína; opiáceos

NOGTSO Morphine, ecgoninne methyl ester and benzoylecgonine

NW11JK Ecgonine methyl ester

O55XS5 Morphine, Benzoylecgonine, Methylecgonine

OOIXLI Methylecgonine, Benzoylecgonine, Morphine

OSOXXO morfine, benzoilecgonine

P45IGJ morphine + methylecognine

PB44MH Morphine

PFCACT morphine,benzoylecgonine, methylecgonine

PMG9F9 morphine, benzoylecgonine, methylecgonine

PPPPYM morphine and benzoylecgonine

Q6EK5S Methylecgonine

QDJMOE Morphine, benzoilecogine and methylecgonine

QPIOKN BZE and EME and morphine

RFIBGP Morphine, benzoylecgonine, methylecgonine

RQEEOE Benzoylecgonine,Methylecgonine and morphine

RSYHBH buprenorphine and norbuprenorphine

RXYG2Q Morphine and Benzoylecgonine

U5AWA0 Morphine, Benzoylecgonine and Methylecgonine

U8NKUE Morphine and Benzoylecgonine

V8HYSI Morphine, Benzoylecgonine, Methylecgonine

VAXCAO Methylecgonine

VE1EEZ None

VLA1JO morphine, benzoylecgonine

W3E7JE MORPHINE, COCAINE

WFA0FD morphine, benzoylecgonine and methylecgonine

WVFKZV Methylecgonine

XIKHP6 morphine, methylecgonine

XZURKZ morphine, BZE

YZOFYZ Morphine, Benzyl Ecgonine, Methyl Ecgonine

Z25SYN Morphine and methylecgonine

ZVTR4A Buprenorphine and norbuprenorphine

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Code Benzoylecgonine Methylecgonine Morphine (Total)

0O03BD - + -

The test sample 2016/2/BS-2 was found to contain methylecgonine.

123WGB - + +

1PWJNH - + +

We found Morphine and Methylecgonine in BS-2

1TTIML - - -

We found also caffein.

3DKQOQ ANP + +

Urine specimen contains 962.3 ng/mL Morphine. Methylecgonine is detected as well.

419F4M + + +

Positive to benzoylecgonine and methylecgonine (cocaine main metabolites). Positive to morphine.

4444FB + + +

44TU44 + + +

Sample is positive for Benzoylecgonine, Methylecgonine and Morphine

4GHNH4 + + +

4YLFBL + + +

Positive to benzoylecgonine and methylecgonine (cocaine main metabolites). Positive to morphine.

66ZO6A + + +

6CVGQ6 + + +

Morphine, Total- Detected > 0.5mg/LBenzoylecgonine- ~ 0.5mg/LEcgonine Methyl Ester- ~ 0.4mg/L

6JIYPR + + +

Hubo consumo de morfina

6V1XQX + + +

This person consumed morphine and/or heroin and cocaine.

8IIDK3 + + +

morphine (cf.above) BZE and EME are 2 metabolites of cocaine (controlled drug). their presence prove a cocaine absorption

ALUS4Z + + +

AVERAC + + +

CQGC6C + + +

In the sample labeled 2016/2/BS-2 Morphine, Benzoylecgonine and Methylecgonine were detected.

CRKFUT + + +

Consumption of cocaine and morphine

DUZUY3 + + +

The presence of Morphine in urine indicates consumption of the drug itself or the intake of other drugs. The presence of Benzoylecgonine and Methylecgonine in urine indicates Cocaine consumption.

Statement of findings for Test Sample 2

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Code Benzoylecgonine Methylecgonine Morphine (Total)

DZKP99 + + +

morphine can be issued from medical prescription or from heroinbze + eme issued from cocaine (only metabolites detected)

EGCC8D + + +

Sample BS2 found to contain morphine (measured value 1215 ng/ml), benzoylecgonine (measured value 1065 ng/ml), methylecgonine(measured value 410 ng/ml)

EHOHKH + + +

BENZOYLECGONINE, METHYLECGONINE ESTER AND MORPHINE DETECTED

EP2WDI + ANP ANP

ERZR0K + - +

Preliminary test followed by the analytical confirmation, then the quantification.

EXR666 + + +

FFAFFI + + +

In sample 2016/2/BS-2 was found an confirmed the presence of MORPHINE, BENZOYLECGONINE AND METHYLECGONINE

FQFOEF + + +

Morphine and Cocaine intake

FZ5ZGY + + +

sample BS-2 contain morphine,methylecgonine,benzoilecgonine

GIGLLN + ANP +

Morphine use/abuse and cocaine abuse.

GTUFSO + + +

GXURZK + ANP ANP

Test sample 2016/2/BS-2 was found to contain controlled drugs for Benzoylecgonine therefore Positive for the Screening and Confirmatory Tests with concentration value of 621.79 ng/ml.

HZ4SSF + + +

-

IGGUCG + + +

The sample contains morphine, benzoylecgonine, methylecgonine.

IGGZSA + + +

IKPH39 + + +

BENZOYLECGONINE-TMS/ METHYL ECGONINE TMS/ MORPHINE DI-TMS DERIVATIVE

IM9MIS + + +

In the sample was detected Morphine, this finding indicates that Morphine was consumed.n the sample were detected Benzoylecgonine and Methylecgonine, this finding indicates that Cocaine was consumed.

ITEOXF - - +

Cocaine and Morphine were identified by GC-MS.

J77027 ANP ANP ANP

The test sample 2016/2/BS-2 shows a positive result over 2000 ng/mL for opiates/opioids and over 300 ng/mL for cocaine and/or metabolites.

JHMWJW + - +

coffeine, theophylline

JL1GTU + + +

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Code Benzoylecgonine Methylecgonine Morphine (Total)

JPRPXO + + +

JYO93J - - -

Examination and analyses performed on BS2 did not reveal any positive findings of toxicological significance.

KFFG6N + + +

Free morphine was detected at concentration of 1215.2 ng/mL, benzoylecgonine was detected at concentration of 630.9 ng/mL and methylecgonine was detected at concentration of 545.9 ng/mL in the 2016/2/BS-2 sample.

KQ4LD7 - + -

The specimen to contain Ecgonine methyl ester

KSEXBG + - -

specific extraction, identification with HPLC/DAD, confirmation by GC/MS using Tmcs derivatisation.the curve was realised with doping blank urine

L6XLFB + + +

LALDP0 ANP + +

use of cocaine, morphine

LB5MQU + + +

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

MDKNFX + + +

Morphine.Cocaine metabolites: benzoylecgonine, methylecgonine

MM3MAK + ANP +

Morphine was found in the sample. The finding is in accordance with the intake of morphine or heroine, that metabolizes to morphine. Benzoylecgonine was in addition found in the sample. This is an inactive metabolite of cocaine, and shows the intake of cocaine.

MQULMG - - -

positive

NNNKNN ANP ANP ANP

cocaína metabolito: positivoopiáceos: positivo

NOGTSO + + +

Cocaine intake and morphine

NW11JK ANP + ANP

Ecgonine methyl ester was detected in the sample of 2016/2/BS-2

O55XS5 + + +

Drugs detected, quantification was not performed

OOIXLI + + +

GC/MS: Relation m/z, time retention (tR ) the reference material methylecgonine, Benzoylecgonine, Morphine are equivalents to those sample 2016/2/BS-2

OSOXXO + ANP +

P45IGJ ANP + +

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

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Code Benzoylecgonine Methylecgonine Morphine (Total)

PB44MH ANP ANP +

Sample BS-2 is positive for Morphine

PFCACT + + +

intake of morphine and cocaine

PMG9F9 + + +

PPPPYM + ANP +

morphine,benzoylecgonine and cafeine

Q6EK5S - + ANP

After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) and Gas Chromatography/Mass Spectrometry (GC/MS), was detected methylecgonine substance in the urine sample 2016/2/BS-2.

QDJMOE + + +

In the urine sample (2016-2/BS2) morphine, benzoilecogine and methylecgonine were found.

QPIOKN + + +

Consistent with use of cocaine and morphine or very pure heroin

RFIBGP + + +

Sample code number 2016/2/BS-2 was found to contain morphine (concentration 1229 ng/ml) and cocaine metabolites: benzoylecgonine (concentration 766 ng/ml), methylecgonine (concentration 389 ng/ml)

RQEEOE + + +

RXYG2Q + - +

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

U5AWA0 + + +

Morphine, Benzoylecgonine and Methylecgonine are detected in urine by GC-MS

U5T5NQ + + +

U8NKUE + ANP +

confirms prior use of heroin/morphine and cocaine

V8HYSI + + +

Morphine, Benzoylecgonine, Methylecgonine

VAXCAO - + -

Methylecgonine was identified in the sample.

VE1EEZ ANP ANP ANP

Sample 2016/2/BS-2 found not to contain any drugs

VLA1JO + + +

W3E7JE + + +

WFA0FD + + +

presence of morphine and cocaine metabolites

WVFKZV ANP + -

Methylecgonine was detected in BS-2 sample.

XIKHP6 - + +

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Code Benzoylecgonine Methylecgonine Morphine (Total)

XXMXQX - ANP -

XZURKZ ANP ANP ANP

YZOFYZ + + +

Toxicological examination revealed the presence of morphine, benzyl ecgonine and methyl ecgonine.

Z25SYN ANP + +

Morphine and methylecgonine detected.

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Code Buprenorphine Norbuprenorphine +

+

ANP

+ +

+

ZVTR4A

LMAFFM

1TZH5Y

RSYHBH

FVJJJE

+

-

+

+

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Identification methods for Test Sample 2

Code 100 110 120 150 160 161 170 180 230 231 210

0O03BD SI

123WGB S I

1PWJNH S I

1TTIML I SI Dipro drug lab screen

1TZH5Y SI

3DKQOQ S SI

419F4M S I

4444FB S I

44TU44 S SI S LC-TOF

4GHNH4 I S BIOCHIP

4YLFBL S I I

66ZO6A S S I SI

6CVGQ6 S I

6JIYPR I SI S randox

6V1XQX S I I

8IIDK3 S I I

ALUS4Z SI I

AVERAC S I

CQGC6C I

CRKFUT S I

DUZUY3 S I I

DZKP99 S I I

EGCC8D S I I

EHOHKH S S SI I

EP2WDI S I

ERZR0K S I

EXR666 S I

FFAFFI SI I

FQFOEF I S KIMS

FVJJJE S I I

FZ5ZGY S I

GIGLLN I I I S

GTUFSO SI S immunochromatographic test

GXURZK I I S Drug Test Kit

Analytical Technique Codes

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

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Code 100 110 120 150 160 161 170 180 230 231 210

HZ4SSF SI

IGGUCG I S Multi-Drug Screen Test Panel

IGGZSA S I SI

IKPH39 SI

IM9MIS I S Lateral Flow Immunoassay

ITEOXF S I

J77027 S

JHMWJW SI I

JL1GTU S I

JPRPXO I S TRIAGE 8-Sure Step

JYO93J S SI

KFFG6N S I SI

KQ4LD7 SI

KSEXBG SI I S immunochromatographique

L6XLFB S I I

LALDP0 S I

LB5MQU I LC-QTOF

LMAFMM S I I

MDKNFX S I SI

MM3MAK S SI

MQULMG SI

NNNKNN S

NOGTSO S I

NW11JK SI

O55XS5 SI

OOIXLI I

OSOXXO I

P45IGJ S S I

PB44MH S I I I

PFCACT S I SI

PMG9F9 SI I SI

PPPPYM SI I I

Q6EK5S S SI I

QDJMOE SI SI

QPIOKN S I I

RFIBGP SI I

RQEEOE SI

RSYHBH SI SI

RXYG2Q S I I

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Code 100 110 120 150 160 161 170 180 230 231 210

U5AWA0 S I

U5T5NQ S I

U8NKUE SI I

V8HYSI S I I S Kinetics Interactions of Microparticles

VAXCAO SI I

VE1EEZ SI

VLA1JO S S I I

W3E7JE S I

WFA0FD S S SI

WVFKZV S I

XIKHP6 I I

XXMXQX SI

YZOFYZ S SI I I LCHRMS

Z25SYN I

ZVTR4A SI I I

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

Frequency of use of screening and identification techniques:

Summary for test sample 2The response summary of all 89 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

Response SummaryParticipants: 89

Benzoylecgonine: 60

Methylecgonine: 62

Morphine (Total): 66

False negatives for BS-2 where no components were identified (technique(s) used or ANP)

Code: 1TTIML (150), JYO93J (180), XXMXQX (110), MQULMG (110)

4 laboratories did not carry out analysis for any of the components present

J77027, NNNKNN, XZURKZ, VE1EEZ

Code Name Technique1TIML Buprenorphine 150419F4M 6-Monoacetylmorphine 2306V1XQX Cocaine 180ALUS4Z Cocaine 230/231ITEOXF Cocaine 180MQULMG Cocaine 110W3E7JE Cocaine 180

Response Summary

Participants 88Technique 100 110 120 150 160 161 170 180 210 230 231

Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

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

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

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

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17

(%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

32

AVERAC Cocaine 180

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 630 ng/ml

Substance: BS‐2; Benzoylecgonine UNODC value = 690 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐2.8

‐2.5 ‐2.4

‐1.5‐1.2

‐1.1‐1.0 ‐0.9

‐0.6 ‐0.6‐0.4 ‐0.4 ‐0.4 ‐0.3

‐0.2‐0.1 0.0

0.0 0.1 0.10.2 0.3

0.5 0.5 0.5 0.6 0.6 0.60.8

1.2 1.2

1.7

2.0

2.8

6.7

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00

6JIYPR

NOGT

SO

CRKFUT

JPRP

XO

4YLFBL

FQFO

EF

VLA1

JO

GIGLLN

XZURK

Z

JHMWJW

WFA

0FD

6CVG

Q6

IGGUCG

QPIOKN

V8HY

SI

GXURZK

KFFG

6N

EP2W

DI

MM3M

AK

HZ4SSF

66ZO

6A

44TU

44

4444

FB

EXR6

66

YZOFYZ

6V1X

QX

RFIBGP

8IIDK3

KSEXBG

MDK

NFX

PMG9

F9

IGGZSA

EGCC

8D

L6XLFB

ERZR0K

33

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 348 ng/ml

Substance: BS‐2; Methylecgonine UNODC value = 350 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐2.7

‐2.0

‐1.7

‐1.0‐0.8

‐0.7 ‐0.7 ‐0.7‐0.4

0.0 0.1 0.1 0.1 0.20.4 0.4 0.5 0.5 0.6

0.8

1.8

2.5

3.7

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.006JIYPR

FQFO

EF

P45IGJ

QPIOKN

4YLFBL

L6XLFB

44TU

44

MDK

NFX

8IIDK3

HZ4SSF

6CVG

Q6

IGGZSA

CRKFUT

66ZO

6A

EXR6

66

WFA

0FD

RFIBGP

4444

FB

6V1X

QX

EGCC

8D

IGGUCG

KFFG

6N

PMG9

F9

34

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1149 ng/ml

Substance: BS‐2; Morphine UNODC value = 1138 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐4.7

‐3.1

‐1.6 ‐1.5

‐1.1 ‐1.1 ‐1.1

‐0.6 ‐0.5 ‐0.5 ‐0.4‐0.3

‐0.1 ‐0.1

0.0 0.0 0.00.3 0.4 0.4 0.5 0.5 0.6

0.7 0.7 0.70.9

1.3

1.5

2.3

3.0

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00JPRP

XO

WFA

0FD

XZURK

Z

MM3M

AK

FQFO

EF

6V1X

QX

3DKQ

OQ

GIGLLN

JHMWJW

V8HY

SI

L6XLFB

4444

FB

IGGZSA

PB44

MH

HZ4SSF

66ZO

6A

EXR6

66

VLA1

JO

EGCC

8D

IGGUCG

YZOFYZ

RFIBGP

P45IGJ

MDK

NFX

6JIYPR

8IIDK3

NOGT

SO

PMG9

F9

44TU

44

ERZR0K

CRKFUT

35

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐2; Benzoylecgonine

-10

-8

-6

-4

-2

0

2

4

6

8

10

z-sc

oreDispersion of z-scores using different analytical techniques for the

quantification of benzoylecgonine in 2016/2 BS-2

HPLC LC‐MSGC‐MS

36

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐2; Methylecgonine

-6

-4

-2

0

2

4

6

z-sc

ore

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

LC‐MSGC‐MS

37

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐2; Morphine

-6

-4

-2

0

2

4

6

z-sc

ore

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

LC‐MS

GC‐MS

38

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Concentration (ng/ml)

Deviation from

robust average

z-scoreConcentr

ation (ng/ml)

Deviation from

robust average

z-score

6JIYPR 42.2 -590 -2.8 JPRPXO 319 -830 -4.7NOGTSO 100 -532 -2.5 WFA0FD 613 -536 -3.1CRKFUT 116 -516 -2.4 XZURKZ 864 -285 -1.6JPRPXO 317 -315 -1.5 MM3MAK 879 -270 -1.54YLFBL 365 -267 -1.2 FQFOEF 955 -194 -1.1FQFOEF 392 -240 -1.1 6V1XQX 962 -187 -1.1VLA1JO 420 -212 -1.0 3DKQOQ 962 -187 -1.1GIGLLN 434 -198 -0.9 GIGLLN 1039 -110 -0.6XZURKZ 501 -131 -0.6 JHMWJW 1058 -91 -0.5JHMWJW 513 -119 -0.6 V8HYSI 1062 -87 -0.5WFA0FD 544 -88 -0.4 L6XLFB 1075 -74 -0.46CVGQ6 544 -88 -0.4 4444FB 1097 -52 -0.3IGGUCG 549 -83 -0.4 IGGZSA 1130 -19 -0.1QPIOKN 558 -74 -0.3 PB44MH 1140 -9 -0.1V8HYSI 585 -47 -0.2 HZ4SSF 1150 1 0.0GXURZK 622 -10 -0.1 66ZO6A 1155 6 0.0KFFG6N 631 -1 0.0 EXR666 1157 8 0.0EP2WDI 635 3 0.0 VLA1JO 1200 51 0.3MM3MAK 648 16 0.1 EGCC8D 1215 66 0.4HZ4SSF 650 18 0.1 IGGUCG 1223 74 0.466ZO6A 680 48 0.2 YZOFYZ 1229 80 0.544TU44 694 62 0.3 RFIBGP 1229 80 0.54444FB 732 100 0.5 P45IGJ 1246 97 0.6EXR666 735 103 0.5 MDKNFX 1265 116 0.7YZOFYZ 748 116 0.5 6JIYPR 1270 121 0.76V1XQX 754 122 0.6 8IIDK3 1276 127 0.7RFIBGP 766 134 0.6 NOGTSO 1310 161 0.98IIDK3 771 139 0.6 PMG9F9 1370 221 1.3KSEXBG 809 177 0.8 44TU44 1417 268 1.5MDKNFX 884 252 1.2 ERZR0K 1560 411 2.3PMG9F9 898 266 1.2 CRKFUT 1668 523 3.0IGGZSA 986 354 1.7EGCC8D 1065 433 2.0L6XLFB 1229 597 2.8ERZR0K 2061 1429 6.7

Code

Morphine

Code

Benzoylecgonine

Z-Scores for Test Sample 2

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Concentration (ng/ml)

Deviation from

robust average

z-score

6JIYPR 135 -212 -2.7FQFOEF 188 -159 -2.0P45IGJ 213 -134 -1.7QPIOKN 264 -83 -1.04YLFBL 282 -65 -0.8L6XLFB 293 -54 -0.744TU44 293 -54 -0.7MDKNFX 295 -52 -0.78IIDK3 312 -35 -0.4HZ4SSF 350 3 0.06CVGQ6 352 5 0.1IGGZSA 358 11 0.1CRKFUT 359 12 0.166ZO6A 361 14 0.2EXR666 377 30 0.4WFA0FD 383 36 0.4RFIBGP 389 42 0.54444FB 391 44 0.56V1XQX 392 45 0.6EGCC8D 410 63 0.8IGGUCG 488 141 1.8KFFG6N 546 199 2.5PMG9F9 645 298 3.7

Methylecgonine

Code

Z-Scores for Test Sample 2

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

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40

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Identified substances for Test Sample 3

Code Identified Substances0O03BD MDMA

123WGB MDMA

1PWJNH MDMA

1TTIML None

1TZH5Y none

3DKQOQ MDMA

419F4M MDMA

44TU44 MDMA

4GHNH4 MDMA, methamphetamine

4YLFBL MDMA

66ZO6A MDMA

6CVGQ6 MDMA

6JIYPR Morfina - Metilecgonina-Benzoilecgonina

6V1XQX MDMA

8IIDK3 MDMA

ALUS4Z MDMA

AVERAC mdma

CQGC6C 3,4-Methylenedioxymetamfetamine (MDMA)

CRKFUT MDMA

DUZUY3 MDMA

DZKP99 MDMA

EGCC8D MDMA

EHOHKH 3,4-METHYLENEDIOXY-METHAMPHETAMINE (MDMA)

EP2WDI MDMA

ERZR0K 3, 4-Methylendioxymetamfetamine (MDMA)

EXR666 MDMA

FFAFFI (MDMA) 3,4-METHYLENEDIOXYMETAMFETAMINE

FQFOEF MDMA

FZ5ZGY MDMA

GIGLLN MDMA

GXURZK MDMA

HZ4SSF 3,4-Methylenedioxymetamfetamine (MDMA)

IGGUCG MDMA

IGGZSA MDMA

IM9MIS 3,4-Methylenedioxymetamfetamine

ITEOXF 3,4-Methylenedioxymetamfetamine (MDMA)

JHMWJW MDMA

JL1GTU 3,4-Methylenedioxymetamfetamine (MDMA)

JPRPXO MDMA, MDA

KFFG6N MDMA

Sample 3 Analysis

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Code Identified SubstancesKQ4LD7 MDMA

KSEXBG MDMA

L6XLFB MDMA

LALDP0 MDMA (3,4-Methylenedioxymetamfetamine)

LB5MQU MDMA

MDKNFX 3,4-Methylenedioxymethamfetamine (MDMA)

MM3MAK MDMA

MQULMG MDMA

NNNKNN metanfetamina

NOGTSO MDMA

NW11JK 3,4-Methylenedioxy-metamfetamine (MDMA)

O55XS5 3,4-Methylendioxy-metamfetamine (MDMA)

OOIXLI 3,4-Methylenedioxymetamfetamine (MDMA)

OSOXXO MDMA

P45IGJ MDMA

PB44MH MDMA

PFCACT MDMA

PMG9F9 MDMA

PPPPYM MDMA

Q6EK5S 3,4-methylenedioxy-metamfetamine (MDMA)

QDJMOE 3,4-Methylenedioxy-methamfetamine (MDMA)

QPIOKN MDMA

RFIBGP MDMA

RQEEOE MDMA

RXYG2Q 3,4-Methylenedioxymetamfetamine (MDMA)

U5AWA0 MDMA

U8NKUE MDMA

V8HYSI MDMA

VAXCAO 3,4-methylendioxy-metamfetamine (MDMA)

VE1EEZ 3,4-Methylenedioxymetamfetamine

VLA1JO MDMA

W3E7JE MDMA

WFA0FD MDMA

WVFKZV 3,4-Methylenedioxy-metamfetamine (MDMA)

XIKHP6 MDMA

XXMXQX MDMA

XZURKZ MDMA

YZOFYZ MDMA

Z25SYN MDMA

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42

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

0O03BD +

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

123WGB +

1PWJNH +

We found MDMA in BS-3

1TTIML -

We did not find any drugs.

3DKQOQ +

MDMA is detected in Urine specimen.

419F4M +

Positive to 3,4-Methylenedioxymetamfetamine (MDMA).

4444FB +

44TU44 +

Sample is positive for 3,4-Methylenedioxymetamfetamine (MDMA)

4GHNH4 +

4YLFBL +

Positive to 3,4-methylenedioximethamphetamine (MDMA).

66ZO6A +

6CVGQ6 +

3,4-methylenedioxy-N-methylamphetamine (MDMA)- Detected > 0.5mg/L

6JIYPR +

Hubo consumo de Morfina y consumo de Cocaina

6V1XQX +

This person consumed MDMA.

8IIDK3 +

MDMA is a controlled narcotic in France that in consumed for its entactogenic, psychedelic and psychostimulant effects.

ALUS4Z +

AVERAC +

CQGC6C +

In the sample labeled 2016/2/BS-3 3,4-Methylenedioxymetamfetamine (MDMA) was detected.

CRKFUT +

Consumption of MDMA

DUZUY3 +

The presence of MDMA in urine indicates consumption of the drug itself.

DZKP99 +

from drug abuse

Statement of findings for Test Sample 3

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43

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

EGCC8D +

Sample BS3 found to contain 3,4-Methylenedioxymetamfetamine (MDMA), measured value 1360 ng/ml

EHOHKH +

3,4-METHYLENEDIOXY-METHAMPHETAMINE (MDMA) DETECTED

EP2WDI +

The urine was analysed and found to contain methylenedioxymethylamphetamine (MDMA).

ERZR0K +

Immunoassay test was performed, then confirmed by GC-MS, subsequently quantified.

EXR666 +

FFAFFI +

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

FQFOEF +

MDMA intake

FVJJJE +

FZ5ZGY +

sample BS-3 contain MDMA

GIGLLN +

Abuse of extasy.

GTUFSO +

GXURZK +

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

HZ4SSF +

-

IGGUCG +

The sample contains MDMA.

IGGZSA +

IKPH39 +

Methylenedioxymetamfetamine

IM9MIS +

In the sample was detected 3,4-Methylenedioxymetamfetamine, this finding indicates that 3,4-Methylenedioxymetamfetamine was consumed.

ITEOXF +

3,4-Methylenedioxymetamfetamine (MDMA) was identified by GC-MS.

J77027 ANP

The test sample 2016/2/BS-3 does not show any group of substances (amphetamines, benzodiazepines, cannabinoids, cocaine or metabolites and opiates/opioids) over the cut-off.

JHMWJW +

JL1GTU +

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44

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

JPRPXO +

JYO93J -

Examination and analyses performed on BS3 did not reveal any positive findings of toxicological significance.

KFFG6N +

MDMA was detected at concentration of 2589.9 ng/mL in the 2016/2/BS-3 sample.

KQ4LD7 +

The specimen to contain 3,4-Methylenedioxymethamphetamine (MDMA)

KSEXBG +

Specific extraction, identification with HPLC/DAD, confirmation by GC/MS using HFBA derivatisation. the curve was realised with doping blank urine

L6XLFB +

LALDP0 +

use of MDMA (3,4-Methylenedioxymetamfetamine)

LB5MQU +

MDMA is a synthetic stimulant drug in the amphetamine class. MDMA is a schedule I controlled substance in the United States.

MDKNFX +

3,4-Methylenedioxymethamfetamine (MDMA)

MM3MAK +

The sample was found to contain MDMA (extacy), which is a drug with stimulating and hallucinogenic effects.

MQULMG +

positive

NNNKNN ANP

metanfetamina: positivo

NOGTSO +

MDMA intake

NW11JK +

3,4-Methylenedioxy-metamfetamine (MDMA) was detected in the sample of 2016/2/BS-3

O55XS5 +

Drugs detected, quantification was not performed

OOIXLI +

GC/MS: Relation m/z, time retention (tR ) the reference material 3,4-Methylenedioxymetamfetamine (MDMA) are equivalents to those sample 2016/2/BS-3

OSOXXO +

P45IGJ +

after chemical analysis was performed the sample was contine 297.9 MDMA

PB44MH +

Sample BS-3 is positive for MDMA

PFCACT +

intake of MDMA

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

PMG9F9 +

PPPPYM +

MDMA and cafeine

Q6EK5S +

After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA), the High Performance Liquid Chromatography with diode array detection (HPLC/DAD) and Gas Chromatography/Mass Spectrometry (GC/MS), was 3,4-methylenedioxy-metamfetamine (MDMA) substance in the urine sample 2016/2/BS-3.

QDJMOE +

In the urine sample (2016-2/BS3) 3,4-Methylenedioxy-methamfetamine (MDMA) was found.

QPIOKN +

Consistent with use of MDMA

RFIBGP +

Sample code number 2016/2/BS-3 was found to contain 3,4-Methylenedioxymetamfetamine (MDMA) (concentration 2632 ng/ml)

RQEEOE +

RXYG2Q +

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

U5AWA0 +

MDMA is detected in urine by GC-MS

U5T5NQ +

U8NKUE +

confirms prior use of MDMA

V8HYSI +

MDMA

VAXCAO +

MDMA was identified in the sample.

VE1EEZ +

Sample 2016/2/BS-3 found to contain 3,4-Methylenedioxymetamfetamine

VLA1JO +

W3E7JE +

WFA0FD +

presence of MDMA

WVFKZV +

3,4-Methylenedioxy-metamfetamine (MDMA) was detected in BS-3 sample.

XIKHP6 +

XXMXQX +

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

XZURKZ ANP

YZOFYZ +

Toxicological examination revealed the presence of MDMA

Z25SYN +

MDMA detected.

2016/2-BS Copyright (c) 2017 UNODC

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

Code [blank sample]ZVTR4A

LMAFFM

1TZH5Y

RSYHBH

+

+

+

+

47

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Identification methods for Test Sample 3

Code 100 110 120 150 160 161 170 180 230 231 210

0O03BD SI

123WGB S I

1PWJNH S I

1TTIML I SI Dipro drug lab screen

1TZH5Y SI

3DKQOQ S SI

419F4M S I

4444FB S I

44TU44 S SI S LC-TOF

4GHNH4 I S BIOCHIP

4YLFBL S I I

66ZO6A S S I SI

6CVGQ6 S I

6JIYPR I SI S randox

6V1XQX S I I

8IIDK3 S I I

ALUS4Z SI I

AVERAC S I

CQGC6C I

CRKFUT S I

DUZUY3 S I I

DZKP99 S I I

EGCC8D S I I

EHOHKH S S SI I

EP2WDI S I

ERZR0K S I

EXR666 S I

FFAFFI SI I

FQFOEF I S KIMS

FVJJJE S I I

FZ5ZGY S I

GIGLLN I I I S

GTUFSO SI S immunochromatographic test

GXURZK I I S Drug Test Kit

Analytical Technique Codes

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

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Code 100 110 120 150 160 161 170 180 230 231 210

HZ4SSF SI

IGGUCG I S Multi-Drug Screen Test Panel

IGGZSA S I SI

IKPH39 SI

IM9MIS I S Lateral Flow Immunoassay

ITEOXF S I

J77027 S

JHMWJW SI I

JL1GTU S I

JPRPXO I S TRIAGE 8-Sure Step

JYO93J S SI

KFFG6N S I SI

KQ4LD7 SI

KSEXBG SI I S immunochromatographique

L6XLFB S I I

LALDP0 S I

LB5MQU I LC-QTOF

LMAFMM S I I

MDKNFX S I SI

MM3MAK S SI

MQULMG SI

NNNKNN S

NOGTSO S I

NW11JK SI

O55XS5 SI

OOIXLI I

OSOXXO I

P45IGJ S S I

PB44MH S I I I

PFCACT S I SI

PMG9F9 SI I SI

PPPPYM SI I I

Q6EK5S S SI I

QDJMOE SI SI

QPIOKN S I I

RFIBGP SI I

RQEEOE SI

RSYHBH SI SI

RXYG2Q S I I

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Code 100 110 120 150 160 161 170 180 230 231 210

U5AWA0 S I

U5T5NQ S I

U8NKUE SI I

V8HYSI S I I S Kinetics Interactions of Microparticles

VAXCAO SI I

VE1EEZ SI

VLA1JO S S I I

W3E7JE S I

WFA0FD S S SI

WVFKZV S I

XIKHP6 I I

XXMXQX SI

YZOFYZ S SI I I LCHRMS

Z25SYN I

ZVTR4A SI I I

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

Frequency of use of screening and identification techniques:

Summary for test sample 3The response summary of all 89 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 3

Code Name Technique

Response Summary

Participants 87

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

Screening (No.) 3 47 4 2 1 3 0 22 11 3 9

(%) 3.4 54.0 4.6 2.3 1.1 3.4 0.0 25.3 12.6 3.4 10.3

Identification (No.) 0 5 1 5 0 6 1 70 3 6 34

(%) 0.0 5.7 1.1 5.7 0.0 6.9 1.1 80.5 3.4 6.9 39.1

Quantification (No.) 0 1 0 0 0 3 0 21 0 2 17(%) 0.0 2.7 0.0 0.0 0.0 8.1 0.0 56.8 0.0 5.4 45.9

Response SummaryParticipants: 89

3,4-Methylenedioxymetamfetamine (MDMA):

78

4GHNH4 Metamfetamine 180

GTUFSO MDEA, MDA 180

JPRPXO MDA 180

False negatives for BS-3 (technique(s) used or ANP)

Code: 1TTIML (150), JYO93J (180),

3 laboratories did not carry out analysis for the component present

J77027, NNNKNN, XZURKZ

6JIYPR Morphine, benzoylecgonine, methylecgonine N/A

NNNKNN Metamfetamine 120

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 2012 ng/ml

Substance: BS‐3; MDMA UNODC value = 1955 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐5.2 ‐3.9 ‐3.8

‐3.1‐2.8

‐2.0

‐1.5

‐0.7 ‐0.6‐0.4 ‐0.4 ‐0.4 ‐0.3 ‐0.2

‐0.1 ‐0.1 0.0 0.0

0.1 0.1 0.1 0.1 0.2 0.20.4

0.5 0.60.7

1.0 1.1 1.1 1.2 1.2

1.71.9

3.0

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00

P45IGJ

FQFO

EF

JPRP

XO

XXMXQ

X

KSEXBG

EGCC

8D

6JIYPR

GIGLLN

WFA

0FD

HZ4SSF

GXURZK

IGGZSA

4YLFBL

6V1X

QX

MM3M

AK

66ZO

6A

MDK

NFX

EXR6

66

L6XLFB

8IIDK3

PMG9

F9

V8HY

SI

4444

FB

44TU

44

ERZR0K

PB44

MH

NOGT

SO

IGGUCG

JHMWJW

QPIOKN

XZURK

Z

VLA1

JO

YZOFYZ

KFFG

6N

RFIBGP

CRKFUT

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐3; MDMA

-6

-4

-2

0

2

4

6

z-sc

ore

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

LC‐MSGC‐MSHPLCEnzyme

immunoassay

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Z-Scores for Test Sample 3

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Concentration (ng/ml)

Deviation from robust average

z-score

P45IGJ 298 -1714.1 -5.2FQFOEF 709 -1303 -3.9JPRPXO 746 -1266 -3.8XXMXQX 1001 -1011 -3.1KSEXBG 1086 -926 -2.8EGCC8D 1360 -652 -2.06JIYPR 1530 -482 -1.5GIGLLN 1782 -230 -0.7WFA0FD 1800 -212 -0.6HZ4SSF 1875 -137 -0.4GXURZK 1876 -135 -0.4IGGZSA 1880 -132 -0.44YLFBL 1908 -104 -0.36V1XQX 1934 -78 -0.2MM3MAK 1983 -29 -0.166ZO6A 1991 -21 -0.1MDKNFX 1997 -15 0.0EXR666 2000 -12 0.0L6XLFB 2033 21 0.18IIDK3 2046 34 0.1PMG9F9 2050 38 0.1V8HYSI 2059 47 0.14444FB 2078 66 0.244TU44 2085 73 0.2ERZR0K 2140 128 0.4PB44MH 2177 165 0.5NOGTSO 2200 188 0.6IGGUCG 2255 243 0.7JHMWJW 2342 330 1.0QPIOKN 2375 363 1.1XZURKZ 2380 368 1.1VLA1JO 2400 388 1.2YZOFYZ 2415 403 1.2KFFG6N 2590 578 1.7RFIBGP 2632 620 1.9CRKFUT 3000 988 3.0

CodeMDMA

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Identified substances for Test Sample 4

Code Identified Substances0O03BD 2C-B

123WGB NEGATIVE

1PWJNH 2C-B

1TTIML 4-Bromo-2,5- dimethoxyphenethylamine (2C-B)

1TZH5Y 2 CB

44TU44 2C-B

4GHNH4 2C-B

4YLFBL 2C-B

66ZO6A 2C-B

6CVGQ6 2C-B

6V1XQX 2C-B

8IIDK3 2-CB

CQGC6C None

DUZUY3 4-Bromo-2-5-dimethoxyphenethylamine (2-CB)

DZKP99 2CB

EGCC8D 2C-B

EHOHKH 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE (2C-B)

EXR666 NEGATIVE

FFAFFI (2-CB) 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE

FQFOEF 2-CB

FZ5ZGY -

GIGLLN 2C-B

HZ4SSF 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

IGGZSA 2C-B

IM9MIS 4-Bromo-2,5-dimethoxyphenethylamine

JHMWJW 2CB

JL1GTU 4-Bromo-2,5-dimethoxyphenethylamine (2-CB)

KFFG6N 2C-B

KQ4LD7 2CB

KSEXBG 2CB

L6XLFB 2C-B

LB5MQU 2C-B

LMAFMM 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

MDKNFX 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

MM3MAK 2C-B

NW11JK 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

O55XS5 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

PFCACT 2-CB

QDJMOE 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

QPIOKN 2CB

Sample 4 Analysis

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Code Identified SubstancesRFIBGP 2C-B

RQEEOE 2C-B

RSYHBH 2-CG

RXYG2Q 2C-B (4-Bromo-2,5-dimethoxyphenethylamine)

U5AWA0 2C-B

U8NKUE Morphine (indicated)

V8HYSI 4-Bromo-2,5-dimethoxyphenethylamine

VE1EEZ None

VLA1JO 2-CB

W3E7JE none found

WFA0FD 2C-B

WVFKZV 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

XIKHP6 2C-B

XZURKZ 2C-B

YZOFYZ 2 C-B

Z25SYN 2C-B

ZVTR4A 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

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Code 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

0O03BD +

The test sample 2016/2/BS-4 was found to contain 4-bromo-2,5-dimethoxyphenthylamine (2C-B).

123WGB ANP

1PWJNH +

We found 2C-B in BS-4

1TTIML +

We found also Ephedrine.

1TZH5Y +

positive to 2 CB

3DKQOQ ANP

Drugs are not detected.

419F4M ANP

Negative.

4444FB +

44TU44 +

Sample is positive for 2C-B

4GHNH4 +

4YLFBL +

Positive to 4-bromo-2,5-dimethoxyphenethylamine (2C-B).

66ZO6A +

6CVGQ6 +

4-Bromo 2,5-dimethoxyphenethylamine (2C-B)- Detected

6JIYPR ANP

6V1XQX +

This person consumed 2C-B.

8IIDK3 +

2-CB is a controlled narcotic in France. It haspsychedelic effect similar to those of MDMA

ALUS4Z -

AVERAC ANP

CQGC6C ANP

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

CRKFUT ANP

DUZUY3 +

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

DZKP99 +

from drug abuse

Statement of findings for Test Sample 4

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Code 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

EGCC8D +

Sample BS4 found to contain 4-Bromo-2,5-dimethoxyphenethylamine (2C-B), measured value 1303 ng/ml

EHOHKH +

4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE (2C-B) DETECTED

EP2WDI ANP

The urine was analysed for common drugs of abuse with a negative result.

ERZR0K -

Immunoassay test was performed, then confirmed by GC-MS.

EXR666 ANP

FFAFFI +

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

FQFOEF +

2-CB intake

FVJJJE +

FZ5ZGY ANP

-

GIGLLN +

Abuse of 2C-B.

GTUFSO +

GXURZK ANP

Test sample 2016/2/BS-4 does not contain controlled drugs therefore Negative.

HZ4SSF +

-

IGGUCG -

IGGZSA +

IKPH39 +

4-Bromo-2,5-dimetoxifenetilamina

IM9MIS +

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

ITEOXF -

J77027 ANP

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

JHMWJW +

JL1GTU +

JPRPXO -

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Code 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

JYO93J -

Examination and analyses performed on BS4 did not reveal any positive findings of toxicological significance.

KFFG6N +

2C-B was detected at concentration of 1489.7 ng/mL in the 2016/1/BS-4 sample.

KQ4LD7 +

The specimen to contain 2,5-dimethoxy-4-bromophenethylamine (2CB)

KSEXBG +

Specific extraction, identification and confirmation by HPLC/DAD,the curve was realised with doping blank urine

L6XLFB +

LALDP0 ANP

LB5MQU +

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

LMAFMM +

MDKNFX +

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

MM3MAK +

The sample was found to contain 2C-B, which is a designer drug with stimulating and hallucinogenic effects.

MQULMG -

negative

NNNKNN ANP

NOGTSO -

NW11JK +

4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected in the sample of 2016/2/BS-4

O55XS5 +

Drugs detected, quantification was not performed

OOIXLI ANP

OSOXXO ANP

P45IGJ -

PB44MH ANP

PFCACT +

intake of 2-CB

PMG9F9 -

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Code 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

PPPPYM ANP

cafeine

Q6EK5S ANP

After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA), High Performance Liquid Chromatography with diode array detection (HPLC/DAD) and Gas Chromatography/Mass Spectrometry (GC/MS), was not detected substances in the urine sample 2016/2/BS-4.

QDJMOE +

In the urine sample (2016-2/BS4) 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was found.

QPIOKN +

Consistent with use of 2CB

RFIBGP +

Sample code number 2016/2/BS-4 was found to contain 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) (concentration 1803 ng/ml)

RQEEOE +

RSYHBH +

Adverse Analytical Finding for 2-CB

RXYG2Q +

Using GC-MS as a screening and confirmatory techniques, psychedelic substance was found in the urine specimen which is considered to be as a controlled drug.

U5AWA0 +

2C-B is detected in urine by GC-MS

U5T5NQ +

U8NKUE ANP

confirms prior use of heroin/morphine/codeine or the ingestion of poppy seeds (this is indicated only as < 5ng/ml spike)

V8HYSI +

4-Bromo-2,5-dimethoxyphenethylamine

VAXCAO -

Not identified.

VE1EEZ ANP

Sample 2016/2/BS-4 found not to contain any drugs

VLA1JO +

W3E7JE -

WFA0FD +

presence of 2C-B

WVFKZV +

4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected in BS-4 sample.

XIKHP6 +

XXMXQX ANP

XZURKZ ANP

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Code 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

YZOFYZ +

Toxicological examination revealed the presence of 2 C-B

Z25SYN +

2C-B detected.

ZVTR4A +

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Identification methods for Test Sample 4

Code 100 110 120 150 160 161 170 180 230 231 210

0O03BD SI

123WGB S I

1PWJNH S I

1TTIML I SI Dipro drug lab screen

1TZH5Y SI

3DKQOQ S SI

419F4M S I

4444FB S I

44TU44 S SI S LC-TOF

4GHNH4 I S BIOCHIP

4YLFBL S I I

66ZO6A S S I SI

6CVGQ6 S I

6JIYPR I SI S randox

6V1XQX S I I

8IIDK3 S I I

ALUS4Z SI I

AVERAC S I

CQGC6C I

CRKFUT S I

DUZUY3 S I I

DZKP99 S I I

EGCC8D S I I

EHOHKH S S SI I

EP2WDI S I

ERZR0K S I

EXR666 S I

FFAFFI SI I

FQFOEF I S KIMS

FVJJJE S I I

FZ5ZGY S I

GIGLLN I I I S

GTUFSO SI S immunochromatographic test

GXURZK I I S Drug Test Kit

Analytical Technique Codes

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

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Code 100 110 120 150 160 161 170 180 230 231 210

HZ4SSF SI

IGGUCG I S Multi-Drug Screen Test Panel

IGGZSA S I SI

IKPH39 SI

IM9MIS I S Lateral Flow Immunoassay

ITEOXF S I

J77027 S

JHMWJW SI I

JL1GTU S I

JPRPXO I S TRIAGE 8-Sure Step

JYO93J S SI

KFFG6N S I SI

KQ4LD7 SI

KSEXBG SI I S immunochromatographique

L6XLFB S I I

LALDP0 S I

LB5MQU I LC-QTOF

LMAFMM S I I

MDKNFX S I SI

MM3MAK S SI

MQULMG SI

NNNKNN S

NOGTSO S I

NW11JK SI

O55XS5 SI

OOIXLI I

OSOXXO I

P45IGJ S S I

PB44MH S I I I

PFCACT S I SI

PMG9F9 SI I SI

PPPPYM SI I I

Q6EK5S S SI I

QDJMOE SI SI

QPIOKN S I I

RFIBGP SI I

RQEEOE SI

RSYHBH SI SI

RXYG2Q S I I

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Code 100 110 120 150 160 161 170 180 230 231 210

U5AWA0 S I

U5T5NQ S I

U8NKUE SI I

V8HYSI S I I S Kinetics Interactions of Microparticles

VAXCAO SI I

VE1EEZ SI

VLA1JO S S I I

W3E7JE S I

WFA0FD S S SI

WVFKZV S I

XIKHP6 I I

XXMXQX SI

YZOFYZ S SI I I LCHRMS

Z25SYN I

ZVTR4A SI I I

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

Frequency of use of screening and identification techniques:

Summary for test sample 4The response summary of all 89 participating laboratories for the identification of BS-4, frequency of use of screening andidentification techniques and false positives and negatives:

Identification of test sample 4:

False positives for Test Sample 4

Code Name Technique 231

Response SummaryParticipants: 89

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

54

U8NKUE Morphine (Total)

False negatives for BS-4 (technique(s) used or ANP)

Code: PMG9F9 (231), NOGTSO (180), JPRPXO (180), ERZR0K (180), P45IGJ (180), VAXCAO

(150/180), JYO93J (180), MQULMG (110), W3E7JE (180), ALUS4Z (230/231), ITEOXF (180),

IGGUCG (180)

24 laboratories did not carry out analysis for the component present

OSOXXO, XXMXQX, GXURZK, CQGC6C, EXR666, OOIXLI, XZURKZ, 3DKQOQ, CRKFUT,

AVERAC, PB44MH, 419F4M, J77027, U8NKUE, Q6EK5S, VE1EEZ, 123WGB, EP2WDI,

LALDP0, FZ5ZGY, PPPPYM, NNNKNN, 6JIYPR, FZ5ZGY

Response Summary

Participants 89Technique 100 110 120 150 160 161 170 180 210 230 231

Screening (No.) 3 48 4 2 1 3 0 22 11 3 9

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

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

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

Quantification (No.) 0 1 0 0 0 3 0 22 0 2 17

(%) 0.0 2.6 0.0 0.0 0.0 7.9 0.0 57.9 0.0 5.3 44.7

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Z‐Score Report per Sample per Substance

Round: 2016/2 Robust average = 1513 ng/ml

Substance: BS‐4; 2C‐B UNODC value = 1724 ng/ml

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows:IzI < 2 = satisfactory

2 ≤ IzI ≤ 3 = questionableIzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

‐2.3

‐2.1

‐1.7

‐1.2

‐0.8 ‐0.8

‐0.5 ‐0.4‐0.2

‐0.1

0.10.2 0.3 0.3 0.4

0.6 0.70.9

1.1

1.6

17.8

‐4.00

‐3.00

‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00

FQFO

EF

KSEXBG

VLA1

JO

WFA

0FD

GIGLLN

XZURK

Z

EGCC

8D

L6XLFB

MDK

NFX

KFFG

6N

44TU

44

IGGZSA

8IIDK3

4444

FB

MM3M

AK

66ZO

6A

RFIBGP

HZ4SSF

6V1X

QX

JHMWJW

1TZH

5Y

66

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Z‐Score Report per Sample per Substance

Round:2016/2Substan BS‐4; 2C‐B

-6

-4

-2

0

2

4

6

z-sc

ore

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

HPLC LC‐MSGC‐MS

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Z-Scores for Test Sample 4

2016/2-BS Copyright (c) 2017 UNODC

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

Concentration (ng/ml)

Deviation from

robust average

z-score

FQFOEF 510 -964 -2.4KSEXBG 626 -848 -2.1VLA1JO 790 -684 -1.7WFA0FD 1010 -464 -1.2GIGLLN 1160 -314 -0.8XZURKZ 1174 -300 -0.7EGCC8D 1303 -171 -0.4L6XLFB 1345 -129 -0.3MDKNFX 1414 -60 -0.1KFFG6N 1490 16 0.044TU44 1574 100 0.2IGGZSA 1620 146 0.48IIDK3 1644 170 0.44444FB 1658 184 0.5

MM3MAK 1684 210 0.566ZO6A 1777 303 0.8RFIBGP 1803 329 0.8HZ4SSF 1900 426 1.16V1XQX 1979 505 1.3JHMWJW 2175 701 1.8

Code

2C-B

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

2016/2-BS Copyright (c) 2017 UNODC

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

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