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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMENS 2017/1

INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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Page 1: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary ReportBIOLOGICAL SPECIMENS

2017/1

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Samples Substances Concentrations Comments on substances

Sample 1 [blank sample]

Sample 2 Amfetamine 1270 ng/ml

Nordazepam 1960 ng/ml

Oxazepam 570 ng/ml

Temazepam 580 ng/ml

Sample 3 gamma-Hydroxybutyric acid (GHB) 16560 ng/ml

Sample 4 Morphine 860 ng/ml

Test Samples Information

Samples Comments on samples

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

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

Sample 3 To prepare BS-3, urine was spiked with an aqueous solution of gamma-hydroxybutyric acid (GHB) (16560ng/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

Sample 4 To prepare BS-4, urine was spiked with an aqueous solution of morphine sulphate (860ng base/ml). The spiked urine was dispensed in 50ml aliquots and lyophilised.

2017/1-BS Copyright (c) 2017 UNODC

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

Table of contents Introduction Page 2

Comments from the International Panel of Forensic Experts Page 2

NPS reported by ICE participants Page 4 Codes and Abbreviations Page 6

Sample 1 Analysis Page 7 Identified substances Page 7 Statement of findings Page 8 Identification methods Page 11 Summary Page 14

Sample 2 Analysis Page 15 Identified substances Page 15 Statement of findings Page 18 Identification methods Page 23 Summary Page 26 Z-Scores Page 27

Sample 3 Analysis Page 37 Identified substances Page 37 Statement of findings Page 39 Identification methods Page 44 Summary Page 47 Z-Scores Page 48

Sample 4 Analysis Page 51

Identified substances Page 51 Statement of findings Page 54 Identification methods Page 59 Summary Page 62 Z-Scores Page 63

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IntroductionAn important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. This report provides information on analytical results of laboratories participating in the Biological Specimens (BS) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact.

Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2017/1 round of the ICE programme, results were submitted within both the Seized Materials (SM)and Biological Specimens (BS) test groups by 238 laboratories in 76 countries. Within the SM test group, there were 201 participating laboratories from 68 countries and within the BS test group, results were submitted by96 laboratories from 45 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the BS test group were enzyme immunoassays (56% of participants), while GC-MS (84%) was the most commonly used technique for identification/confirmation of the components in the test samples. The results for the qualitative identification of the sample components in the BS test group, the number of false positive/negative results and the analysesnot performed are shown in table 1.

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

Test sample BS-1 BS-2

(Amfetamine) BS-2

(Nordazepam) BS-2

(Oxazepam) BS-2

(Temazepam) (Blank)

Correct identification

99% 88% 94% 63% 75%

Number of false positives

1 7

Number of false negatives

- 0

Number of analyses not

performed (ANP) - 3

Test sample BS-3 BS-4

(GHB) ( Morphine )

Correct identification

34% 88%

Number of false positives 7 10

Number of false negatives

14 4

Number of analyses not

performed (ANP) 49 6

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.

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Quantitative Analysis

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

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

z-score

Test sample

BS-2 (Amfetamine)

BS-2 (Nordazepam)

BS-2 (Oxazepam)

|z| < 2, satisfactory 86% (31) 82% (23)

2 ≤ |z| ≤ 3, questionable

6% (2) 4% (1)

|z| > 3, unsatisfactory

86% (31)

6% (2)

8% (3) 8% (3) 14% (4)

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

|z| < 2, satisfactory 77% (28) 84% (16) 77% (30)

2 ≤ |z| ≤ 3, questionable

6% (2) 5% (1) 13% (5)

|z| > 3, unsatisfactory

3% (1) 11% (2) 10% (4)

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

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

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

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

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

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

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

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

25%

36%

23%

8%

5% 3%

Synthetic cannabinoids

Synthetic cathinones

Others

Phenethylamines

Ketamine and phencyclidinetype substances

Tryptamines

50%

16%

13%

11%

8%

2%

Stimulants

SCRA's

Opioids

Hallucinogens

Dissociatives

Sedatives/Hypnotics

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

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

For further details on these substances and others reported to the UNODC Early Warning Advisory, ICE participants can log on to the UNODC ICE portal and select the icon for the Early Warning Advisory on New Psychoactive substances as shown below. https://www.unodc.org/LSS/Home/ICE

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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 Substances3FMD3X GHB

8LCBAB none

AMMRSO no found

DDSBTD -

DFYDDD None

GBGZ1G NA

GNAW99 Unknown

GUGPPP not detected

HVHHFH No found drugs

KHJBOK no

MXA7O5 no

NDP7T7 none

OOO3GD /

PCBAPT no drugs found

Q4WQSQ Not present

QZEZZZ -

T0B0D0 None

TTTGKV None

USDN2N NONE

UUXUUM NO

WEB9SQ Abs

WZUJSD -

XNXEE6 NO FOUND

Z4YCUT NONE

ZGAWTE Not detected.

Sample 1 Analysis

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Code [blank sample]

0H72WR Drugs Not Detected

1111EF

1A3AXJ

35TZAW

3FMD3X GHB was detected in sample BS1 2017/1.

4FF58F

66OQY6

6V10VI

7BVRLF

7FEMIN

84HKVU

8LCBAB We did not find any drugs. We found only caffein.

8MFF1T

8TPBUN

8VX7GU

AG3666

AMMRSO no drugs found in the sample 2017/1/BS-1

B1KV8H

BBKEUE

BHWJHB

BNGG0M

CPUSPP

CTTCT3

D1AYDM Not detected.

DB4Y6M BLANK

DDA5D2 Negative

DDSBTD -

DFYDDD In Sample 2017/1/BS-1 no drug was found

DHUDIC The substances that were tested for weren´t found to be present in the sample analysed.

DQMUDL

EPEVE2 Sample contains no substances from ICE menu

FBYTRU No common drugs were detected in sample 2017/1/BS-1

FWXVWL

GAHHTQ

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

GMUMBE Negative

GNAW99 We found two stain in TLC plate for this sample but because we did not have all of the refrences we could not identify them.

Statement of findings for Test Sample 1

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Code [blank sample]

GUGPPP blank

GXJGYM a preliminar screenning by EIA with no possitive results

H2PHCD

HB4JKY

HHLH88 Performed by GS/MS Method and Caffeine was found.

HVHHFH Sample code number 2017/1/BS-1 was found doesn't contain controlled drugs.

IJS22F

IQIQAI Common drugs not detected.

IQJAM7

IVV5RV (remark :caffeine present)

JRKD4U THE SAMPLE BS-1 ANALYZED DOES NOT CONTAINS CONTROLLED DRUGS ( AMPHETAMINE, BENZODIAZEPINES,COCAINE/METABOLITES,OPIATES,11-NOR-DELTA9-THC-9-CARBOXYLIC ACID,BARBITURATES.

JSZABT No proof of drug abuse.

K3KSJ9

KHJBOK

KJPKK4

L3ZOZH

LJTLFH

M8VO1Z

MXA7O5 blank sampke

NCMGK4

NDP7T7

NGAJ1Y

NP5333

OOO3GD no drugs were found

PCBAPT caffeine, ibuprophen

PQFUYI

PXJDZ1

Q4WQSQ Screening test, GC/MS: Not to be present

QZEZZZ -

RNJJ8Z

SOK66J

SV8SSS

SZZ1BZ Negative.

T0B0D0 Sample 2017/1/BS-1 found not to contain any drugs

TBORSX

TG33JW

TISIQZ Negative the screening method

TTTGKV No control drugs found

2017/1-BS Copyright (c) 2017 UNODC

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Code [blank sample]

U5KOOL

UCTGCC

UIUDEC No drug was found in the sample number 1

USDN2N

UTSOWL

UUXUUM No drugs or controlled drugs detected

V6ZRMH

VLHXHH after analysis performed the sample contained caffeine

VN2UVV Drugs were not detected in BS-1 sample

VR1QQH The urine screen did not indicate the presence of any of the targeted drugs.

W5TXOT No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-1.

WEB9SQ

WZRRBA Examination of the sample coded 2017/1/BS-1 did not reveal the presence of any controlled drugs

WZUJSD negative

XNXEE6 NO FOUND

Y3AFEE

YFYCWJ No se detectó

YGKDY2 No controlled drug from ICE 2017/01 menu is detected

YSKXXD No drugs were found in this sample.

Z4YCUT

ZGAWTE Not detected drugs into 2017/1/BS-1 sample by Enzyme Immunoassay Techniques (EIA) and by Gas Chromatgraphy/Mass Spectrometry (CG/MS).

2017/1-BS Copyright (c) 2017 UNODC

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Identification methods for Test Sample 1

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

0H72WR I

1111EF I I

1A3AXJ I S chemical immunochromatographic

35TZAW S I I

3FMD3X I SI S Dip test

4FF58F S I LC/QTOF

6V10VI S I I

7BVRLF S SI I

7FEMIN S I I

84HKVU SI I S Multi-Drug Screen Test Panel

8LCBAB I SI Dipro drug lab screen

8MFF1T S I

8TPBUN I SI I

8VX7GU S I I SI Kinetic Interaction of Microparticles in Solution

AG3666 S I

AMMRSO S SI S I

B1KV8H S I I

BBKEUE S I I

BHWJHB S SI S LC-QTOF

BNGG0M S I

CPUSPP S I I

CTTCT3 I I S inmunocromatografía flujo lateral

D1AYDM S I SI

DB4Y6M S I

DDA5D2 S SI SI

DDSBTD S SI I

DFYDDD SI SI

DHUDIC S I

DQMUDL I LC/TOF

EPEVE2 S SI S LC-TOF

FBYTRU SI

FWXVWL S SI I

GAHHTQ S SI I

Analytical Technique Codes

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

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Code 100 110 120 140 141 150 160 161 170 180 230 231 210

GBGZ1G S I

GMUMBE S SI

GNAW99 SI

GUGPPP SI

GXJGYM S I I LC-QTOF

H2PHCD I

HB4JKY S I

HHLH88 S I

HVHHFH SI I

IJS22F S I

IQIQAI S I

IQJAM7 S I

IVV5RV I I SI

JRKD4U SI SI

JSZABT I I S

K3KSJ9 S I

KHJBOK I I

KJPKK4 I S zivia kit multitest

L3ZOZH S I

LJTLFH S I

M8VO1Z S I SI

MXA7O5 SI

NCMGK4 SI

NDP7T7 I I S immunochromatographie

NGAJ1Y S I

NP5333 S SI

OOO3GD S I I

PCBAPT S I I

PQFUYI SI SI I

PXJDZ1 SI I I

Q4WQSQ S I

QZEZZZ SI

RNJJ8Z S I

SOK66J S I I

SV8SSS I SI

SZZ1BZ S I

T0B0D0 SI

TBORSX S I

TG33JW S I I

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Code 100 110 120 140 141 150 160 161 170 180 230 231 210

TISIQZ SI SI

TTTGKV S S I I

U5KOOL S I I

UCTGCC S I I

UIUDEC S I

USDN2N I

UTSOWL I I Triage 8- ALERE Sure Step

UUXUUM SI I

V6ZRMH S I SI

VLHXHH S I

VN2UVV S I

VR1QQH SI

W5TXOT SI

WEB9SQ SI

WZRRBA S SI I

WZUJSD S I

XNXEE6 I S MULTIDRUG TEST

Y3AFEE S I I SI one step immonochromatographic assay

YFYCWJ S

YGKDY2 SI SI

YSKXXD S I

Z4YCUT I

ZGAWTE S I

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RESPONSE SUMMARY FOR TEST SAMPLE 1

Participants: 96

The response summary of all 96 participating laboratories for the identification of BS-1, frequency of use of screening and identification techniques and false positives and negatives:

Identification of Test Sample-1:

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

False positives for Test Sample-1:

Round Code: Substance reported: Tech Code:

3FMD3X GHB 230

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

Frequency of use of screening, identification and quantification techniques:

Response Summary

Participants 96

Technique 100 110 120 140 141 150 160 161 170 180 210

Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

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

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7

(%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2

(%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

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Identified substances for Test Sample 2

Code Identified Substances0H72WR Nordazepam and Amfetamine

1111EF OXAZEPAM, TEMAZEPAM, NORDAZEPAM, AMFETAMINE

1A3AXJ Oxazepam, Temazepam, Nordazepam and Amphethamine

35TZAW Amphétamine, Nordazepam, Oxazepam, Temazepam

3FMD3X Amphetamine, oxazepam, medazepam, nordazepam, temazepam, diazepam

4FF58F Amfetamine, Nordazepam, Oxazepam, Temazepam

66OQY6 amphetamine, nordiazepam, temazepam

6V10VI amfetamine, nordazepam, temazepam

7BVRLF amphetamines, benzodiazepines

7FEMIN Anfetamina, Temazepam, Nordiazepam

84HKVU Amfetamine, Nordazepam, Oxazepam,Temazepam

8LCBAB Amfetamine, Oxazepam, 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

8MFF1T BENZODIACEPINES AND ANPHETAMINES

8TPBUN Amfetamine, Nordazepam

8VX7GU Amphetamine, Nordiazepam, Temazepam, Oxazepam

AG3666 Amfetamine, Nordazepam, Temazepam, Oxazepam

AMMRSO Amfetamine, Nordazepam, Oxazepam, Temazepam

B1KV8H anfetamina, nordazepam

BBKEUE Amfetamine, Nordazepam, Oxazepam, Temazepam

BHWJHB Amphetamine, temazepam, nordiazepam, oxazepam

BNGG0M amphetamine, nardazepam, oxazepam, temazepam

CPUSPP Amfetamine; Nordazepam; Temazepam; Oxazepam

CTTCT3 amphetamine, nordiazepam,oxacepam,temazepam

D1AYDM Amfetamine, Nordazepam, Oxazepam, Temazepam

DB4Y6M AMPHETAMINE, NORDAZEPAM, OXAZEPAM, TEMAZEPAM

DDA5D2 amphetamine, nordazepam, oxazepam, temazepam

DDSBTD Amfetamine, Nordazepam,Oxazepam,Temazepam

DFYDDD Nordazepam, Oxazepam, Temazepam

DHUDIC Amphetamine, Oxazepam and Nordazepam

DQMUDL Amphetamine; Nordiazepam, Oxazepam, Temazepam

EPEVE2 Amfetamine, Nordazepam, Oxazepam, Temazepam

FBYTRU Amfetamine and Nordazepam

FWXVWL Amfetamine, Benzodiazepines and metabolites: Oxazepam, Temazepam, Nordazepam

GAHHTQ Amfetamine, Nordazepam

GBGZ1G Amphetamine and Nordazepam

GMUMBE Amphetamine, Nordiazepam, Oxazepam, Temazepam

GNAW99 Amfetamine

GUGPPP amfetamine,nordazepam,temazepam,oxazepam

GXJGYM nordazepam, temazepam, oxazepam, amphetamine

H2PHCD nordazepam, temazepam

Sample 2 Analysis

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Code Identified SubstancesHB4JKY amphetamines, benzodiazepam

HHLH88 Nordazepam, Temazepam, Delorazepam,Caffeine.

HVHHFH Amfetamine, Oxazepam, Temazepam and Nordazepam

IJS22F amfetamine, nordazepam, temazepam

IQIQAI Nordazepam, Temazepam, Amphetamine

IQJAM7 nordazepam, oxazepam

IVV5RV amphetamine

JRKD4U AMPHETAMINE,NORDAZEPAM,TEMAZEPAM,OXAZEPAM

JSZABT amfetamine, nordazepa, oxazepam, temazepam

K3KSJ9 Amfetamine, Nordiazepam and Temazepam

KHJBOK Amphetamine, Nordazepam, Temazepam

L3ZOZH Amfetamine, Temazepan, Nordazepam,oxacepam

LJTLFH Amphetamine & Nordazepam

M8VO1Z Amfetamine, Nordazepam, Oxazepam, Temazepam

MXA7O5 AMF and Benzos

NCMGK4 amphetamine, nordazepam and temazepam

NDP7T7 temazepam, nordazepam, oxazepam, amfetamine

NGAJ1Y Amphetamine, Nordazepam, Temazepam

NP5333 amfetamine,nordazepam,temazepam,oxazepam

OOO3GD amphetamine/nordazepam/temazepam

PCBAPT amfetamine

PQFUYI AMPHETAMINE, NORDIAZEPAM, OXAZEPAM, TEMAZEPAM

PXJDZ1 amphetamine,benzo

Q4WQSQ Amfetamine, Nordazepam, Temazepam, Oxazepam

QZEZZZ Amfetamine,Nordazepam,Oxazepam,Temazepam

RNJJ8Z anphetamine, nordazepam, temazepam, oxazepam

SOK66J Amphetamine, Nordiazepam, Oxazepam, Temazepam

SV8SSS Amphetamine, nordazepam, temazepam

SZZ1BZ amfetamine, nordazepam, temazepam, oxazepam

T0B0D0 Amfetamine, Nordazepam and Temazepam

TBORSX Amfetamine

TISIQZ Amphetamine ; nordiazepam ; oxazepam

TTTGKV oxazepam, camazepam,nordazepam and amphetamine

U5KOOL Amfetamine, nordiazepam, temazepam and oxazepam

UCTGCC Nordazepam, Oxazepam, Temazepam

UIUDEC amfetamine, nordazepam and temazepam

USDN2N Amphetamine, oxazepam, Nordazepam, Temazepam.

UTSOWL Amphetamine, Benzodiazepines

UUXUUM Amphetamine and Nordazepam

V6ZRMH Nordiazepam, amfetamine

VLHXHH amphetamine+ nordazepam

VN2UVV Nordazepam and Amfetamine

VR1QQH Amphetamine, Nordiazepam, Oxazepam, Temazepam

W5TXOT nordazepam

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Page 18: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Identified SubstancesWEB9SQ amfetamine, nordazepam,oxazepam,temazepam

WZRRBA Amfetamine, Nordazepam, Oxazepam and Temazepam

WZUJSD methamphetamine,nordazepam

XNXEE6 FOUND

Y3AFEE amphetamine, nordazepam, oxazepam, temazepam

YFYCWJ Benzodiacepinas

YGKDY2 Nordiazepam, temazepam and oxazepam

YSKXXD amfetamine, nordazepam, oxazepam, temazepam

Z4YCUT Amfetamine, Nordazepam, Oxazepam, Temazepam

ZGAWTE Amfetamine, Nordazepam and Temazepam.

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Page 19: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Amfetamine Nordazepam Oxazepam Temazepam

0H72WR + + - -

Nordazepam and Amfetamine Detected

1111EF + + + +

1A3AXJ + + + +

those drugs were identified by LC/MS/MS

35TZAW + + + +

3FMD3X + + + +

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

4FF58F + + + +

66OQY6 ANP ANP ANP ANP

6V10VI + + - +

7BVRLF + + - +

amphetamine, nordiazepam, temazepam

7FEMIN + + + +

84HKVU + + + +

The sample contains amfetamine, nordazepam, oxazepam and temazepam.

8LCBAB + - + -

We found: Amfetamine, Oxazepam, 4-Bromo-2,5-dimethoxyphenethylamine (2C-B)

8MFF1T - + - +

NORDAZEPAM AND TEMAZEPAM

8TPBUN + + - -

Amfetamine, Nordazepam

8VX7GU + + + +

AG3666 + + + +

Amfetamine, Nordazepam, Temazepam and Oxazepam were identified by GCMS analysis.

AMMRSO + + + +

Amfetamine, Nordazepam, Oxazepam, Temazepam were found in the sample 2017/1/BS-2

B1KV8H + + - -

positivo para anfetamina y nordazepam

BBKEUE + + + +

BHWJHB + + + +

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

BNGG0M + + + +

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

Statement of findings for Test Sample 2

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Page 20: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Amfetamine Nordazepam Oxazepam Temazepam

CPUSPP + + + +

CTTCT3 + + + +

The presence of nordiazepam, oxacepam, temazepam in urine indicates consumption of diazepam, or the consumption of each of the benzodiacepines themselves. The presence of amphetamine in urine indicates the consumption of amphetamine by itself or the consumption of metanphetamine.

D1AYDM + + + +

Positive to amfetamine, nordazepam, oxazepam and temazepam.

DB4Y6M + + + +

DDA5D2 + + + +

presence of amphetamine and diazepam metabolites

DDSBTD + + + +

DFYDDD - + + +

In Sample 2017/1/BS-2 the drugs Nordazepam, Oxazepam, Temazepam were found.

DHUDIC + + + ANP

It was detected the presence of Amphetamine, Oxazepam and Nordazepam in the sample analysed.

DQMUDL + + + +

Amphetamine is a central nervous system stimulant, and is a Schedule II substance in the United States. Nordiazepam is a long acting benzodiazepine, and is a Schedule IV substance in the United States. Oxazepam is a short to intermediate acting benzodiazepine and is a Schedule IV substance in the United States. Temazepam is an intermediate acting benzodiazepine and is a Schedule IV drug in the United States. Nordiazepam, oxazepam and temazepam can all also be metabolites of Diazepam.

EPEVE2 + + + +

Sample is positive for Amfetamine, Nordazepam, Oxazepam, Temazepam

FBYTRU + + ANP ANP

Amfetamine and Nordazepam were detected in sample 2017/1/BS-2

FWXVWL + + + +

GAHHTQ + + ANP -

Amfetamine and Nordazepam were identified in the sample.

GBGZ1G + + ANP ANP

The sample tested positive for Amphetamine type stimulants and Benzodiazapines on screening. Creatinine levels were satisfactory.

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

Nordazepam was confirmed in the sample, however no validated quantification procedure is in place at our laboratory therefore quantification was not done.

GMUMBE + + + +

Positive for amphetamine and benzodiazepines

GNAW99 + ANP ANP ANP

We found two other stains in TLC plate for this sample but becaus we did not have refrence drugs we could not identify them

GUGPPP + + + +

drugs detected

GXJGYM + + + +

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

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Page 21: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Amfetamine Nordazepam Oxazepam Temazepam

H2PHCD ANP + ANP +

use of benzodiazepines (nordazepam, temazepam)

HB4JKY + + ANP +

amphetamine, temazepam, nordazepam

HHLH88 - + - +

Confirmed my GS/MS Method.

HVHHFH + + + +

Sample code number 2017/1/BS-2 was found to contain amfetamine (concentration 1189 ng/ml), oxazepam (concentration 647 ng/ml), temazepam (concentration 634 ng/ml) and nordazepam (concentration 2049 ng/ml).

IJS22F + + - +

IQIQAI + + ANP +

Amphetamine, nordazepam and temazepam detected.

IQJAM7 - + + ANP

IVV5RV + + + +

illegal drugs (amphetamine) and benzodiazepines (metabolites): nordazepam, oxazepam and temazepam. Caffeine present.

JRKD4U + + + +

THE SAMPLE BS-2 ANALYZED DOES CONTAINS AMPHETAMINE AND BENZODIAZEPINE METABOLITES ( NORDAZEPAM,TEMAZEPAM,OXAZEPAM)

JSZABT + + + +

Abuse of "speed". Use of medicinal drugs containing nordazepam and temazepam. Oxazepam is probably the metabolite of these two.

K3KSJ9 + + - +

2017/1/BS-2 found to contain 113 ng/ml of Amfetamine,1462.46 ng/ml of Nordiazepam and 389.8 ng/ml of Temazepam

KHJBOK + + - +

KJPKK4 ANP ANP ANP ANP

L3ZOZH + + + +

LJTLFH + + ANP ANP

The urine was analysed and found to contain Amphetamine and Nordazepam.

M8VO1Z + + + +

MXA7O5 + + + +

consumer of AMF and benzos

NCMGK4 + + - +

NDP7T7 + + + +

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

NGAJ1Y + + - +

NP5333 + + + +

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

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Page 22: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Amfetamine Nordazepam Oxazepam Temazepam

OOO3GD + + ANP +

sample was spiked with amphetamine , nordazepam and temazepam

PCBAPT + + + +

nordazepam, oxazepam, temazepam, caffeine

PQFUYI + + + +

PXJDZ1 + - - -

Q4WQSQ + + + +

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

QZEZZZ + + + +

-

RNJJ8Z + + + +

SOK66J + + + +

Amphetamine ~ 0.7mg/LNordiazepam Detected > 1mg/LOxazepam ~ 0.5mg/LTemazepam ~0.5mg/L

SV8SSS + + - +

SZZ1BZ + + + +

Positive to amfetamine, nordazepam, temazepam, oxazepam.

T0B0D0 + + ANP +

Sample 2017/1/BS-2 found to contain Amfetamine, Nordazepam and Temazepam

TBORSX + + + +

Amfetamine,Oxazepam

TG33JW + + + -

TISIQZ + + + -

Analytical Adverse Finding for amphetamine, nordiazepam and oxazepam.

TTTGKV + + + -

by using CR & GC-MS techniques ( Oxazepam , Camazepam , Nordazepam ) were detected in urine sample.

by using LC-MS (Amphetamine) was detected.

U5KOOL + + + +

The presence of amphetamine in the urine sample shows previous use of the drug.The presence of nordiazepam, temazepam and oxazepam in the urine is consistent with previous use of diazepam.

UCTGCC ANP + + +

Nordazepam, Oxazepam, Temazepam were detected

UIUDEC + + - +

In urine sample number two was identified amfetamine, nordazepam and temazepam

USDN2N + + + +

The coincidence between the retention time and mass-fragmentogram from a reference standard, analyzed at the same conditions that the biological sample, indicates the presence of Amphetamine, oxazepam, Nordazepam and Temazepam in the biological sample.

UTSOWL + + - +

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Page 23: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Amfetamine Nordazepam Oxazepam Temazepam

UUXUUM + + ANP ANP

Amphetamine and Nordazepam detected in the sample

V6ZRMH + + - -

The presence of nordiazepam in urine indicates the use of diazepam or nordiazepam.The presence of amfetamine in urine indicates the use of amfetamine.

VLHXHH + + - -

after analysis performed the sample contained amphetamine +nordazepam+caffeine

VN2UVV + + ANP ANP

Nordazepam and Amfetamine were detected in BS-2 sample

VR1QQH + + + +

The urine sample screened positive for the presence of amphetamine, and also nordiazepam, oxazepam and temazepam (indicative of benzodiazepine consumption).

W5TXOT - + - -

The test sample 2017/1/BS-2 was found to contain the controlled drug nordazepam.

WEB9SQ + + + +

Detected: amphetamines, benzodiazepines

WZRRBA + + + +

Examination of the sample coded 2017/1/BS-2 revealed the presence of amphetamine, nordazepam, oxazepam and temazepam.

WZUJSD - + ANP ANP

2017/1/BS-2 contain methamphetamine, nordazepam

XNXEE6 + + + +

NORDAZEPAM, TEMAZEPAM, OXAZEPAM, ANFETAMINE

Y3AFEE + + + +

YFYCWJ ANP ANP ANP ANP

Positivo

YGKDY2 - + + +

Nordiazepam, temazepam and oxazepam were qualitatively reported as nordiazepam was above the upper limit of linearity in 2017/01/BS-02.

YSKXXD + + + +

In this sample amfetamine, nordazepam, oxazepam, temazepam were found, which indicates that person consumed amfetamine and diazepam.

Z4YCUT + + + +

ZGAWTE + + - +

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

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Page 24: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Identification methods for Test Sample 2

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

0H72WR I

1111EF I I

1A3AXJ I S chemical immunochromatographic

35TZAW S I I

3FMD3X I SI S Dip test

4FF58F S I LC/QTOF

6V10VI S I I

7BVRLF S SI I

7FEMIN S I I

84HKVU SI I S Multi-Drug Screen Test Panel

8LCBAB I SI Dipro drug lab screen

8MFF1T S I

8TPBUN I SI I

8VX7GU S I I SI Kinetic Interaction of Microparticles in Solution

AG3666 S I

AMMRSO S SI S I

B1KV8H S I I

BBKEUE S I I

BHWJHB S SI S LC-QTOF

BNGG0M S I

CPUSPP S I I

CTTCT3 I I S inmunocromatografía flujo lateral

D1AYDM S I SI

DB4Y6M S I

DDA5D2 S SI SI

DDSBTD S SI I

DFYDDD SI SI

DHUDIC S I

DQMUDL I LC/TOF

EPEVE2 S SI S LC-TOF

FBYTRU SI

FWXVWL S SI I

GAHHTQ S SI I

Analytical Technique Codes

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

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Page 25: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

GBGZ1G S I

GMUMBE S SI

GNAW99 SI

GUGPPP SI

GXJGYM S I I LC-QTOF

H2PHCD I

HB4JKY S I

HHLH88 S I

HVHHFH SI I

IJS22F S I

IQIQAI S I

IQJAM7 S I

IVV5RV I I SI

JRKD4U SI SI

JSZABT I I S

K3KSJ9 S I

KHJBOK I I

KJPKK4 I S zivia kit multitest

L3ZOZH S I

LJTLFH S I

M8VO1Z S I SI

MXA7O5 SI

NCMGK4 SI

NDP7T7 I I S immunochromatographie

NGAJ1Y S I

NP5333 S SI

OOO3GD S I I

PCBAPT S I I

PQFUYI SI SI I

PXJDZ1 SI I I

Q4WQSQ S I

QZEZZZ SI

RNJJ8Z S I

SOK66J S I I

SV8SSS I SI

SZZ1BZ S I

T0B0D0 SI

TBORSX S I

TG33JW S I I

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Page 26: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

TISIQZ SI SI

TTTGKV S S I I

U5KOOL S I I

UCTGCC S I I

UIUDEC S I

USDN2N I

UTSOWL I I Triage 8- ALERE Sure Step

UUXUUM SI I

V6ZRMH S I SI

VLHXHH S I

VN2UVV S I

VR1QQH SI

W5TXOT SI

WEB9SQ SI

WZRRBA S SI I

WZUJSD S I

XNXEE6 I S MULTIDRUG TEST

Y3AFEE S I I SI one step immonochromatographic assay

YFYCWJ S

YGKDY2 SI SI

YSKXXD S I

Z4YCUT I

ZGAWTE S I

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Page 27: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

RESPONSE SUMMARY FOR TEST SAMPLE 2

Participants: 96

The response summary of all 96 participating laboratories for the identification of BS-2, frequency of use of screening and identification techniques and false positives and negatives:

Identification of Test Sample-2:

Substance Name Number of laboratories correctly identifying:

Amfetamine 84

Nordazepam 90

Oxazepam 60

Temazepam 72

False positives for Test Sample-2:

Round Code: Substance reported: Tech Code:

3FMD3X Medazepam, Diazepam 230

8LCBAB 2C-B 150/Dipro screen

TTTGKV Camazepam N/A

WZUJSD Methamphetamine 150

TG33JW Tenamfetamine 231

KJPKK4 Methylecgonine 180

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

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

Round Code: Answer Code: Tech Code:

66OQY6 ANP -

KJPKK4 ANP -

YFYGWJ ANP -

Frequency of use of screening, identification and quantification techniques:

Response Summary

Participants 96

Technique 100 110 120 140 141 150 160 161 170 180 210

Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

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

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7

(%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2

(%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

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

Z-Score Report per Sample per Substance

Robust average = 1103 ng/ml

UNODC value = 1270 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 = satisfactory2 ≤ IzI ≤ 3 = questionable

IzI > 3 = unsatisfactory

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

anomaly has occured that requires inverstigation.

-6.1

-2.5

-1.5 -1.5

-1.3 -1.2

-0.9-0.8

-0.7 -0.6 -0.6 -0.6- 0.5

-0.3 -0.2-0.2

0.0

0.1 0.10.3 0.3

0.4 0.5 0.5 0.6 0.6 0.6 0.6 0.7 0.70.9 0.9

1.3

2.7

7.9 17.7

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

K3

KSJ

9

SOK

66J

Y3A

FEE

RN

JJ8

Z

8V

X7G

U

EPE

VE2

7FE

MIN

4FF

58F

QZE

ZZZ

TBO

RSX

DD

SBTD

BB

KEU

E

YSK

XX

D

BN

GG

0M

UTS

OW

L

BH

WJH

B

U5

KO

OL

D1

AYD

M

JSZA

BT

TG33

JW

AM

MR

SO

GU

GP

PP

8TP

BU

N

HV

HH

FH

FWX

VW

L

66O

QY6

GB

GZ1

G

M8

VO

1Z

DD

A5

D2

NP

5333

WZR

RB

A

MX

A7

O5

DB

4Y6

M

CP

USP

P

3FM

D3

X

VLH

XH

H

2728

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Z-Score Report per Sample per Substance

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

-6

-4

-2

0

2

4

6

z-sc

ore

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

GC/MS LC/MS

2829

Page 30: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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

Z-Score Report per Sample per Substance

Robust average = 1840 ng/ml

UNODC value = 1960 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 = satisfactory2 ≤ IzI ≤ 3 = questionable

IzI > 3 = unsatisfactory

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

-5.1 -4.7

-2.1 -2.0

-1.2-1.1

-0.8 -0.7 -0.7 -0.7

-0.4-0.3 -0.3 -0.2 -0.2 -0.1 -0.1 0.0

0.10.2

0.4 0.5 0.5 0.5 0.6 0.6 0.6 0.7 0.8 0.8 0.8

1.8 1.8

3.1

5.6

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

GX

JGYM

IQJA

M7

DD

A5

D2

CP U

SPP

K3

KSJ

9

TBO

RSX

U5

KO

OL

BN

GG

0M

D1

AYD

M

8TP

BU

N

BB

KEU

E

WZR

RB

A

66O

QY6

EPEV

E2

DD

SBTD

MX

A7

O5

7FE

MIN

AM

MR

SO

DB

4Y6

M

TG33

JW

FWX

VW

L

JSZA

BT

8M

FF1

T

GU

GP

PP

M8

VO

1Z

RN

JJ8

Z

UTS

OW

L

HV

HH

FH

BH

WJH

B

YSK

XX

D

4FF

58F

Y3A

FEE

84H

KV

U

QZE

ZZZ

3FM

D3

X

2930

Page 31: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Score Report per Sample per Substance

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

-6

-4

-2

0

2

4

6

z-sc

ore

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

GC/MSLC/MS

HPLC

3031

Page 32: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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

Z-Score Report per Sample per Substance

Robust average = 529 ng/ml

UNODC value = 570 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.

-4.5

-1.6

-1.1 - 1.0

- 0.9 - 0.8-0.7

-0.6-0.5

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

0.4 0.4 0.40.6

0.80.9 0.9

1.3

2.1

7.9 8.9 43.1

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

GX

JGYM

CP

USP

P

BN

GG

0M

7F E

MIN

TG33

JW

JSZA

BT

D1

AYD

M

U5

KO

OL

BH

WJH

B

DD

SBTD

DD

A5

D2

GU

GP

PP

TBO

RSX

AM

MR

SO

SOK

66J

EPEV

E2

4FF

58F

MX

A7

O5

BB

KEU

E

M8

VO

1Z

QZE

ZZZ

FWX

VW

L

DB

4Y6

M

HV

HH

FH

84H

KV

U

3FM

D3

X

IQJA

M7

Y3A

FEE

3132

Page 33: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Score Report per Sample per Substance

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

-6

-4

-2

0

2

4

6

z-sc

ore

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

GC/MSLC/MS

HPLC

3233

Page 34: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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

Z-Score Report per Sample per Substance

Robust average = 530 ng/ml

UNODC value = 580 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 quest ionable 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.

-3.0

-2.4

-1.2 -1.2

-1.0-0.9 - 0.9

-0.8-0.6

-0.3 -0.3 - 0.3 -0.3 -0.3-0.2

0.1 0.1 0.1 0.1 0.2 0.20.4

0.7 0.70.8

0.9 0.9

1.5

1.71.9

4.7

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

GX

JGYM

UT

SOW

L

CP

USP

P

K3

KSJ

9

BN

GG

0M

TG33

JW

D1

AYD

M

66O

QY6

DD

A5

D2

BB

KEU

E

AM

MR

SO

SOK

66J

TBO

RSX

QZE

ZZZ

GU

GP

PP

EPEV

E2

U5

KO

OL

FWX

VW

L

DB

4Y6

M

DD

SBTD

M8

VO

1Z

BH

WJH

B

4FF

58F

8M

FF1

T

JSZA

BT

HV

HH

FH

7FE

MIN

WZR

RB

A

84H

KV

U

Y3A

FEE

ND

P7T

7

3334

Page 35: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Score Report per Sample per Substance

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

-6

-4

-2

0

2

4

6

z-sc

ore

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

GC/MS LC/MSHPLC

3435

Page 36: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Scores for Test Sample 2

2017/1-BS Copyright (c) 2017 UNODC

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

Concentration (ng/ml)

Deviation from

robust

average

z-score

K3KSJ9 113 -990 -6.1

SOK66J 695 -408 -2.5

Y3AFEE 854 -249 -1.5

RNJJ8Z 860 -243 -1.5

8VX7GU 901 -202 -1.3

EPEVE2 912 -191 -1.2

7FEMIN 957 -146 -0.9

4FF58F 967 -136 -0.8

QZEZZZ 995 -108 -0.7

TBORSX 1000 -103 -0.6

DDSBTD 1009 -94 -0.6

BBKEUE 1010 -93 -0.6

YSKXXD 1020 -83 -0.5

BNGG0M 1050 -53 -0.3

UTSOWL 1064 -39 -0.2

BHWJHB 1076 -27 -0.2

U5KOOL 1100 -3 0.0

D1AYDM 1115 12 0.1

JSZABT 1122 19 0.1

TG33JW 1145 42 0.3

AMMRSO 1147 44 0.3

GUGPPP 1170 67 0.4

8TPBUN 1181 78 0.5

HVHHFH 1189 86 0.5

FWXVWL 1194 91 0.6

66OQY6 1197 94 0.6

GBGZ1G 1198 95 0.6

M8VO1Z 1201 98 0.6

DDA5D2 1209 106 0.7

NP5333 1223 120 0.7

WZRRBA 1240 137 0.9

MXA7O5 1252 149 0.9

DB4Y6M 1305 202 1.3

CPUSPP 1532 429 2.7

3FMD3X 2374 1271 7.9

VLHXHH 3950 2847 17.7

Code

Amfetamine

Concentration (ng/ml)

Deviation from

robust

average

z-score

GXJGYM 265 -1575 -5.1

IQJAM7 404 -1436 -4.7

DDA5D2 1206 -634 -2.1

CPUSPP 1232 -608 -2.0

K3KSJ9 1462 -378 -1.2

TBORSX 1500 -340 -1.1

U5KOOL 1600 -240 -0.8

BNGG0M 1625 -215 -0.7

D1AYDM 1626 -214 -0.7

8TPBUN 1638 -202 -0.7

BBKEUE 1710 -130 -0.4

WZRRBA 1750 -90 -0.3

66OQY6 1757 -83 -0.3

EPEVE2 1774 -66 -0.2

DDSBTD 1787 -53 -0.2

MXA7O5 1801 -39 -0.1

7FEMIN 1807 -33 -0.1

AMMRSO 1826 -14 0.0

DB4Y6M 1878 38 0.1

TG33JW 1914 74 0.2

FWXVWL 1975 135 0.4

JSZABT 1987 147 0.5

8MFF1T 1989 149 0.5

GUGPPP 2000 160 0.5

M8VO1Z 2017 177 0.6

RNJJ8Z 2028 188 0.6

UTSOWL 2028 188 0.6

HVHHFH 2049 209 0.7

BHWJHB 2071 231 0.8

YSKXXD 2085 245 0.8

4FF58F 2094 254 0.8

Y3AFEE 2385 545 1.8

84HKVU 2407 567 1.8QZEZZZ 2800 960 3.1

3FMD3X 3578 1738 5.6

Code

Nordazepam

3536

Page 37: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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

Concentration (ng/ml)

Deviation from

robust

average

z-score

GXJGYM 110 -419 -4.5

CPUSPP 376 -153 -1.6

BNGG0M 425 -104 -1.1

7FEMIN 432 -97 -1.0

TG33JW 448 -81 -0.9

JSZABT 450 -79 -0.8

D1AYDM 460 -69 -0.7

U5KOOL 470 -59 -0.6

BHWJHB 485 -44 -0.5

DDSBTD 496 -33 -0.4

DDA5D2 499 -30 -0.3

GUGPPP 500 -29 -0.3

TBORSX 500 -29 -0.3

AMMRSO 502 -27 -0.3

SOK66J 510 -19 -0.2

EPEVE2 510 -19 -0.2

4FF58F 565 36 0.4

MXA7O5 569 40 0.4

BBKEUE 570 41 0.4

M8VO1Z 585 56 0.6

QZEZZZ 600 71 0.8

FWXVWL 613 84 0.9

DB4Y6M 615 86 0.9

HVHHFH 647 118 1.3

84HKVU 729 200 2.1

3FMD3X 1271 742 7.9

IQJAM7 1368 839 8.9

Y3AFEE 4575 4046 43.1

Oxazepam

Code Concentration (ng/ml)

Deviation from

robust

average

z-score

GXJGYM 180 -350 -3.0

UTSOWL 248 -282 -2.4

CPUSPP 386 -144 -1.2

K3KSJ9 390 -140 -1.2

BNGG0M 410 -120 -1.0

TG33JW 419 -111 -0.9

D1AYDM 420 -110 -0.9

66OQY6 437 -93 -0.8

DDA5D2 462 -68 -0.6

BBKEUE 490 -40 -0.3

AMMRSO 494 -36 -0.3

SOK66J 496 -34 -0.3

TBORSX 500 -30 -0.3QZEZZZ 500 -30 -0.3

GUGPPP 508 -22 -0.2

EPEVE2 538 8 0.1

U5KOOL 540 10 0.1

FWXVWL 541 11 0.1

DB4Y6M 542 12 0.1

DDSBTD 549 19 0.2

M8VO1Z 555 25 0.2

BHWJHB 576 46 0.4

4FF58F 608 78 0.7

8MFF1T 608 78 0.7

JSZABT 622 92 0.8

HVHHFH 634 104 0.9

7FEMIN 640 110 0.9

WZRRBA 700 170 1.5

84HKVU 733 203 1.7

Y3AFEE 747 217 1.9

NDP7T7 1073 543 4.7

Code

Temazepam

3637

Page 38: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Identified substances for Test Sample 3

Code Identified Substances35TZAW GHB

3FMD3X None

4FF58F GHB

84HKVU gamma-Hydroxybutyric acid (GHB)

8LCBAB none

8VX7GU GHB

AG3666 gamma-Hydroxybutyric acid (GHB)

AMMRSO gamma-Hydroxybutyric acid (GHB)

BBKEUE GHB

BHWJHB GHB

BNGG0M gamma-Hydroxybutyric acid (GHB)

CPUSPP gamma-Butyrolactone (GBL)

D1AYDM gamma-Hydroxybutyric acid (GHB)

DDA5D2 GHB

DDSBTD -

DFYDDD None

EPEVE2 gamma-Hydroxybutyric acid (GHB)

FWXVWL gamma-Hydroxybutyric acid (GHB)

GBGZ1G NA

GUGPPP gamma-Hydroxybutyric acid

HVHHFH GHB

JSZABT GHB

KHJBOK no

M8VO1Z GHB

MXA7O5 no

NCMGK4 GHB

NDP7T7 GBL

NP5333 GHB

PCBAPT no drugs found

PQFUYI GHB

Q4WQSQ Not present

QZEZZZ gamma-Hydroxybutyric acid (GHB)

RNJJ8Z GHB

SOK66J GHB

SV8SSS morphin

T0B0D0 None

TTTGKV none

USDN2N NONE

UUXUUM GHB

VLHXHH GHB

Sample 3 Analysis

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3738

Page 39: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Identified SubstancesVR1QQH Morphine - indicative

WEB9SQ gamma-hydroxybutyric-acid

WZRRBA gamma-hydroxybutyric acid

WZUJSD -

XNXEE6 FOUND

Y3AFEE GHB

YSKXXD GHB

Z4YCUT gamma-Hydroxybutyric acid (GHB)

ZGAWTE Ibuprofen and Cocaine

2017/1-BS Copyright (c) 2017 UNODC

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3839

Page 40: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code gamma-Hydroxybutyric acid (GHB)

0H72WR -

Drugs Not Detected

1111EF ANP

1A3AXJ ANP

35TZAW +

3FMD3X -

No drugs were detected in sample BS3 2017/1.

4FF58F +

66OQY6 ANP

6V10VI -

7BVRLF ANP

7FEMIN ANP

84HKVU +

The sample contains gamma-Hydroxybutyric acid (GHB).

8LCBAB ANP

We did not find any drugs. We found only caffein.

8MFF1T -

8TPBUN -

8VX7GU +

AG3666 +

gamma-Hydroxybutyric acid (GHB) was identified by GCMS analysis.

AMMRSO +

gamma-Hydroxybutyric acid (GHB) was found in the sample 2017/1/BS-3

B1KV8H ANP

BBKEUE +

BHWJHB +

GHB was found in urine. GHB is a CNS depressant.

BNGG0M +

in the sample is detected gamma-Hydroxybutyric acid (GHB)

CPUSPP -

Statement of findings for Test Sample 3

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3940

Page 41: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code gamma-Hydroxybutyric acid (GHB)

CTTCT3 ANP

D1AYDM +

Positive to gamma-hydroxybutyric acid (GHB).

DB4Y6M ANP

BLANK

DDA5D2 +

Presence of GHB

DDSBTD ANP

-

DFYDDD ANP

In Sample 2017/1/BS-3 no drug was found

DHUDIC ANP

The substances that were tested for weren´t found to be present in the sample analysed.

DQMUDL ANP

EPEVE2 +

Sample is positive for gamma-Hydroxybutyric acid (GHB)

FBYTRU ANP

No common drugs were detected in sample 2017/1/BS-3

FWXVWL +

GAHHTQ ANP

GBGZ1G ANP

Sample was negative during screening for all drug groups tested at our laboratory. Creatinine levels were satisfactory.

GMUMBE ANP

Negative

GNAW99 ANP

GUGPPP +

drugs detected

GXJGYM ANP

a preliminar screenning by EIA with no possitive results

H2PHCD ANP

HB4JKY ANP

HHLH88 -

Performed by GS/MS Method and Caffeine was found.

HVHHFH +

Sample code number 2017/1/BS-3 was found to contain gamma-Hydroxybutyric acid (concentration 15980 ng/ml)

IJS22F ANP

IQIQAI ANP

Common drugs not detected.

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4041

Page 42: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code gamma-Hydroxybutyric acid (GHB)

IQJAM7 ANP

IVV5RV ANP

(remark : caffeine, nicotine en quinine present)

JRKD4U ANP

THE SAMPLE BS-3 ANALYZED DOES NOT CONTAINS CONTROLLED DRUGS ( AMPHETAMINE, BENZODIAZEPINES,COCAINE/METABOLITES,OPIATES,11-NOR-DELTA9-THC-9-CARBOXYLIC ACID,BARBITURATES.

JSZABT +

Abuse of GBL or GHB or 1,4-butanediol.

K3KSJ9 -

KHJBOK ANP

KJPKK4 ANP

L3ZOZH ANP

ibuprofen positive

LJTLFH ANP

M8VO1Z +

MXA7O5 -

blank sample

NCMGK4 +

NDP7T7 -

general extraction, identification and confirmation with GC/MS

NGAJ1Y ANP

NP5333 +

gamma-Hydroxybutyric acid was found in the sample BS-3 at the detection limit.

OOO3GD ANP

no drugs were found

PCBAPT -

caffeine, ibuprophen,aripiprazole

PQFUYI +

PXJDZ1 -

Q4WQSQ ANP

Screening test, GC/MS,: Not to be present.

QZEZZZ +

-

RNJJ8Z +

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4142

Page 43: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code gamma-Hydroxybutyric acid (GHB)

SOK66J +

GHB ~ 23mg/L

SV8SSS -

SZZ1BZ ANP

Negative.

T0B0D0 ANP

Sample 2017/1/BS-3 found not to contain any drugs

TBORSX +

gamma-Hydroxybutyric acid (GHB)

TG33JW +

TISIQZ ANP

Negative in the screening method

TTTGKV ANP

no control drugs found

U5KOOL ANP

UCTGCC ANP

UIUDEC ANP

No drug was found in the sample number 3

USDN2N ANP

UTSOWL ANP

UUXUUM +

GHB detected in the sample

V6ZRMH ANP

VLHXHH +

after analysis performed the sample contained GHB +CAFFEINE

VN2UVV ANP

Drugs were not detected in BS-3 sample

VR1QQH ANP

The urine sample screened indicative for the presence of morphine.

W5TXOT ANP

No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-3.

WEB9SQ +

other

WZRRBA +

Examination of the sample coded 2017/1/BS-3 revealed the presence of gamma-hydroxybutyric acid (GHB).

WZUJSD ANP

negative

XNXEE6 +

GHB

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4243

Page 44: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code gamma-Hydroxybutyric acid (GHB)

Y3AFEE +

YFYCWJ ANP

No se detectó

YGKDY2 ANP

No controlled drug from ICE 2017/01 menu is detected

YSKXXD +

In this sample GHB was found, which indicates that person consumed GHB.

Z4YCUT +

ZGAWTE ANP

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

2017/1-BS Copyright (c) 2017 UNODC

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4344

Page 45: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Identification methods for Test Sample 3

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

0H72WR I

1111EF I I

1A3AXJ I S chemical immunochromatographic

35TZAW S I I

3FMD3X I SI S Dip test

4FF58F S I LC/QTOF

6V10VI S I I

7BVRLF S SI I

7FEMIN S I I

84HKVU SI I S Multi-Drug Screen Test Panel

8LCBAB I SI Dipro drug lab screen

8MFF1T S I

8TPBUN I SI I

8VX7GU S I I SI Kinetic Interaction of Microparticles in Solution

AG3666 S I

AMMRSO S SI S I

B1KV8H S I I

BBKEUE S I I

BHWJHB S SI S LC-QTOF

BNGG0M S I

CPUSPP S I I

CTTCT3 I I S inmunocromatografía flujo lateral

D1AYDM S I SI

DB4Y6M S I

DDA5D2 S SI SI

DDSBTD S SI I

DFYDDD SI SI

DHUDIC S I

DQMUDL I LC/TOF

EPEVE2 S SI S LC-TOF

FBYTRU SI

FWXVWL S SI I

GAHHTQ S SI I

Analytical Technique Codes

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

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Code 100 110 120 140 141 150 160 161 170 180 230 231 210

GBGZ1G S I

GMUMBE S SI

GNAW99 SI

GUGPPP SI

GXJGYM S I I LC-QTOF

H2PHCD I

HB4JKY S I

HHLH88 S I

HVHHFH SI I

IJS22F S I

IQIQAI S I

IQJAM7 S I

IVV5RV I I SI

JRKD4U SI SI

JSZABT I I S

K3KSJ9 S I

KHJBOK I I

KJPKK4 I S zivia kit multitest

L3ZOZH S I

LJTLFH S I

M8VO1Z S I SI

MXA7O5 SI

NCMGK4 SI

NDP7T7 I I S immunochromatographie

NGAJ1Y S I

NP5333 S SI

OOO3GD S I I

PCBAPT S I I

PQFUYI SI SI I

PXJDZ1 SI I I

Q4WQSQ S I

QZEZZZ SI

RNJJ8Z S I

SOK66J S I I

SV8SSS I SI

SZZ1BZ S I

T0B0D0 SI

TBORSX S I

TG33JW S I I

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4546

Page 47: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

TISIQZ SI SI

TTTGKV S S I I

U5KOOL S I I

UCTGCC S I I

UIUDEC S I

USDN2N I

UTSOWL I I Triage 8- ALERE Sure Step

UUXUUM SI I

V6ZRMH S I SI

VLHXHH S I

VN2UVV S I

VR1QQH SI

W5TXOT SI

WEB9SQ SI

WZRRBA S SI I

WZUJSD S I

XNXEE6 I S MULTIDRUG TEST

Y3AFEE S I I SI one step immonochromatographic assay

YFYCWJ S

YGKDY2 SI SI

YSKXXD S I

Z4YCUT I

ZGAWTE S I

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Page 48: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

RESPONSE SUMMARY FOR TEST SAMPLE 3

Participants: 96

The response summary of all 96 participating laboratories for the identification of BS-3, frequency of use of

screening and identification techniques and false positives and negatives:

Identification of Test Sample-3:

Substance Name Number of laboratories correctly identifying:

GHB 33

False positives for Test Sample-3:

Round Code: Substance reported: Tech Code:

SV8SSS Morphine 150/180

VR1QQH Morphine 231

ZGAWTE Cocaine 180

CPUSPP GBL 180

KJPKK4 MDMA 180

NDP7T7 GBL 180

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

Round Code: Answer Code: Tech Code: K3KSJ9 - 231

6V10VI - 231

8MFF1T - 180

HHLH88 - 180

MXA7O5 - 180

3FMD3X - 180

Round Code: Answer Code: Tech Code: 0H72WR - 180

PXJDZ1 - 110

PCBAPT - 180

CPUSPP - 150

8TPBUN - 231

NDP7T7 - 180

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

Frequency of use of screening, identification and quantification techniques:

Response Summary

Participants 96

Technique 100 110 120 140 141 150 160 161 170 180 210

Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

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

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7

(%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2

(%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

SV8SSS - 180/231

4748

Page 49: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

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

Z-Score Report per Sample per Substance

Robust average = 17382 ng/ml

UNODC value = 16560 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 = satisfactory2 ≤ IzI ≤ 3 = questionable

IzI > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a quest ionable 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.

-1.7

-1.3

-0.9

-0.6 -0.6 -0.5 -0.5 -0.4 -0.4

-0.2 -0.2 -0.1

0.4

0.9

1.1

1.9

2.2

3.3

6.5

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

JSZA

BT

BN

GG

0M

TG33

JW

D1

AYD

M

BH

WJH

B

GU

GP

PP

HV

HH

FH

EPEV

E2

35T

ZAW

BB

KEU

E

M8

VO

1Z

QZE

ZZZ

FWX

VW

L

TBO

RSX

RN

JJ8

Z

SOK

66J

AM

MR

SO

DD

A5

D2

Y3A

FEE

4849

Page 50: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Score Report per Sample per Substance

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

-6

-4

-2

0

2

4

6

z-sc

ore

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

GC/MS LC/MS

4950

Page 51: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Z-Scores for Test Sample 3

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Concentration

(ng/ml)

Deviation from

robust averagez-score

JSZABT 12340 -5042 -1.7

BNGG0M 13500 -3882 -1.3

TG33JW 14763 -2619 -0.9

D1AYDM 15500 -1882 -0.6

BHWJHB 15615 -1767 -0.6

GUGPPP 15840 -1542 -0.5

HVHHFH 15980 -1402 -0.5

EPEVE2 16060 -1322 -0.4

35TZAW 16100 -1282 -0.4

BBKEUE 16850 -532 -0.2

M8VO1Z 16908 -474 -0.2

QZEZZZ 17000 -382 -0.1

FWXVWL 18700 1318 0.4

TBORSX 20000 2618 0.9

RNJJ8Z 20760 3378 1.1

SOK66J 23200 5818 1.9

AMMRSO 24000 6618 2.2

DDA5D2 27400 10018 3.3

Y3AFEE 37101 19719 6.5

Code

GHB

5051

Page 52: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Identified substances for Test Sample 4

Code Identified Substances0H72WR Morphine and 6-MAM

1111EF MORPHINE

1A3AXJ Morphine, Hydromorphone

35TZAW Morphine

3FMD3X Morphine

4FF58F Morphine

66OQY6 morphine

6V10VI morphine

7BVRLF opiates

7FEMIN Morphine

84HKVU Morphine

8LCBAB Opiates

8MFF1T MORPHINE

8TPBUN Morphine

8VX7GU Morphine

AG3666 Morphine

AMMRSO Morphine

BBKEUE Morphine

BHWJHB Morphine

BNGG0M Morphine (Total)

CPUSPP Morphine

CTTCT3 Morphine

D1AYDM Morphine (total)

DB4Y6M MORPHINE

DDA5D2 morphine

DDSBTD Morphine

DFYDDD Morphine

DHUDIC Morphine

DQMUDL Morphine

EPEVE2 Morphine

FWXVWL Morphine

GAHHTQ Morphine, 11-nor-delta9- THC-9-carboxylic acid

GBGZ1G Morphine

GMUMBE Morphine

GNAW99 Morphine

GUGPPP Morphine

GXJGYM MORPHINE

H2PHCD morphine

HB4JKY opiates

HHLH88 Morphine, Caffeine, Ibuprofen, Umbelliferone.

Sample 4 Analysis

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Code Identified SubstancesHVHHFH Morphine

IJS22F morphine

IQIQAI Morphine, 6-MAM

IQJAM7 morphine

IVV5RV morphine

JRKD4U MORPHINE

JSZABT morphine

K3KSJ9 morphine

KHJBOK no

M8VO1Z Morphine

MXA7O5 MOR

NCMGK4 morphine

NDP7T7 NONE

NGAJ1Y Morphine, 6-Monoacetylmorphine (6-MAM)

NP5333 morphine

OOO3GD morphine

PCBAPT morphine

PQFUYI MORPHINE

PXJDZ1 opiates , opioids

Q4WQSQ Morphine

QZEZZZ Morphine (Total)

RNJJ8Z morphine

SOK66J Morphine (Total)

SV8SSS morphin, codeine

SZZ1BZ morphine

T0B0D0 None

TBORSX Morphine

TISIQZ Morphine

TTTGKV Morphine

U5KOOL Morphine

UCTGCC Morphine

UIUDEC morphine

USDN2N Morphine

UTSOWL Morphine

UUXUUM Morphine

V6ZRMH Morphine

VLHXHH MORPHINE

VN2UVV Morphine and 6-Monoacetylmorphine (6-MAM)

VR1QQH Morphine

WEB9SQ morphine

WZRRBA Morphine

WZUJSD morphine-3-O-glucuronide

XNXEE6 FOUND

Y3AFEE morphine

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Code Identified SubstancesYFYCWJ Morfina

YGKDY2 Morphine

YSKXXD morphine

Z4YCUT Morphine

ZGAWTE Not detected.

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Page 55: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Morphine (Total)

0H72WR +

Morphine and 6-MAM Detected

1111EF +

1A3AXJ +

Those drugs were identified by LC/MS/MS

35TZAW +

3FMD3X +

Morphine (1563.45 ng/mL) was detected in sample BS4 2017/1.

4FF58F +

66OQY6 ANP

Free morphine was measured

6V10VI +

7BVRLF +

moprhine

7FEMIN +

84HKVU +

The sample contains morphine.

8LCBAB +

We found: Morphine total and Codeine

8MFF1T +

NO COMMENTS

8TPBUN +

Morphine

8VX7GU +

AG3666 +

Morphine was identified by GCMS analysis.

AMMRSO +

Morphine was found in the sample 2017/1/BS-4

B1KV8H -

BBKEUE +

BHWJHB +

Morphine is detected in urine. This indicates intake of morphine, or heroine which is metabolized to morphine in the body. Morphine is an analgesic opiate.

BNGG0M +

in the sample is detected Morphine (Total)

CPUSPP +

Statement of findings for Test Sample 4

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Code Morphine (Total)

CTTCT3 +

The presence of morphine in urine indicates morphine consumption or other drugs such as heroin and codeine.

D1AYDM +

Positive to morphine.

DB4Y6M +

DDA5D2 +

Presence of morphine

DDSBTD +

DFYDDD +

In Sample 2017/1/BS-4 the drug morphine was found.

DHUDIC +

It was detected the presence of Morphine in the sample analysed.

DQMUDL +

Morhphine is a narcotic analgesic found in the opium poppy. It is a Schedule II substance in the United States.

EPEVE2 +

Sample is positive for Morphine

FBYTRU ANP

No common drugs were detected in sample 2017/1/BS-4

FWXVWL +

GAHHTQ +

Morphine and 11-nor-delta9- THC-9-carboxylic acid were identified in the sample.

GBGZ1G +

The sample was positive for opiates on screening. Creatinine levels were satisfactory.

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

GMUMBE +

Positive for opiates

GNAW99 +

GUGPPP +

drugs detected

GXJGYM +

Preliminar positive results by EIA for opiods/ opiates confirmated by CG/MS and LC/QTOF

H2PHCD +

use of morphine

HB4JKY +

morphine

HHLH88 +

Confirmed my GS/MS Method.

HVHHFH +

Sample code number 2017/1/BS-4 was found to contain morphine (concentration 839 ng/ml)

IJS22F +

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Page 57: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Morphine (Total)

IQIQAI +

Morphine and 6-MAM detected.

IQJAM7 +

IVV5RV +

(remark :caffeine present)

JRKD4U +

THE SAMPLE BS-4 ANALYZED DOES CONTAINS AN OPIATE ( MORPHINE).

JSZABT +

Abuse of pure heroin or morphine or use of medicinal morphine.

K3KSJ9 +

2017/1/BS-4 found to contain 190.7 ng/ml of Morphine

KHJBOK -

KJPKK4 ANP

L3ZOZH +

paracetamol positive

LJTLFH ANP

M8VO1Z +

MXA7O5 +

opioid consumer

NCMGK4 +

NDP7T7 -

NGAJ1Y +

NP5333 +

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

OOO3GD +

PCBAPT +

caffeine, acetaminophen

PQFUYI +

PXJDZ1 +

Q4WQSQ +

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

QZEZZZ +

-

RNJJ8Z +

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Code Morphine (Total)

SOK66J +

Morphine, Total Detected > 0.5mg/L

SV8SSS +

SZZ1BZ +

Positive to morphine.

T0B0D0 ANP

Sample 2017/1/BS-4 found not to contain any drugs

TBORSX +

Morphine

TG33JW +

TISIQZ +

Analytical Adverse Finding for Morphine (free) with a concentration of 0,9 µg/ml

TTTGKV +

by using CR & GC-MS techniques ( Morphine ) was detected in urine sample.

U5KOOL +

The presence of morphine in the urine sample shows previous use of the drug.

UCTGCC +

Morphine was detected

UIUDEC +

In urine sample number four was identified morphine

USDN2N +

The coincidence between the retention time and mass-fragmentogram from a reference standard, analyzed at the same conditions that the biological sample, indicates the presence of Morphine in the biological sample.

UTSOWL +

UUXUUM +

Morphine detected in the sample

V6ZRMH +

The presence of morphine in urine indicates the use of morphine

VLHXHH +

after analysis performed the sample contained MOAPHINE + CAFFEINE

VN2UVV +

Morphine and 6-Monoacetylmorphine (6-MAM) were detected in BS-4 sample

VR1QQH +

The urine sample screened positive for the presence of morphine.

W5TXOT -

No controlled drugs of the ICE 2017/1 menu were detected in the test sample 2017/1/BS-4.

WEB9SQ +

Detected: opiates

WZRRBA +

Examination of the sample coded 2017/1/BS-4 revealed the presence of morphine.

WZUJSD -

2017/1/BS-4 contain opiates.

XNXEE6 +

MORPHINE

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Page 59: INTERNATIONAL QUALITY ASSURANCE · PDF fileSample 3 gamma-Hydroxybutyric acid (GHB) ... (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate ... positive reaction was obtained. (-)

Code Morphine (Total)

Y3AFEE +

YFYCWJ ANP

Positivo

YGKDY2 +

Morphine was qualitatively reported as morphine was above the upper limit of linearity in 2017/01/BS-04.

YSKXXD +

In this sample morphine was found, which indicates that person consumed morphine.

Z4YCUT +

ZGAWTE ANP

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

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Identification methods for Test Sample 4

Code 100 110 120 140 141 150 160 161 170 180 230 231 210

0H72WR I

1111EF I I

1A3AXJ I S chemical immunochromatographic

35TZAW S I I

3FMD3X I SI S Dip test

4FF58F S I LC/QTOF

6V10VI S I I

7BVRLF S SI I

7FEMIN S I I

84HKVU SI I S Multi-Drug Screen Test Panel

8LCBAB I SI Dipro drug lab screen

8MFF1T S I

8TPBUN I SI I

8VX7GU S I I SI Kinetic Interaction of Microparticles in Solution

AG3666 S I

AMMRSO S SI S I

B1KV8H S I I

BBKEUE S I I

BHWJHB S SI S LC-QTOF

BNGG0M S I

CPUSPP S I I

CTTCT3 I I S inmunocromatografía flujo lateral

D1AYDM S I SI

DB4Y6M S I

DDA5D2 S SI SI

DDSBTD S SI I

DFYDDD SI SI

DHUDIC S I

DQMUDL I LC/TOF

EPEVE2 S SI S LC-TOF

FBYTRU SI

FWXVWL S SI I

GAHHTQ S SI I

Analytical Technique Codes

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

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Code 100 110 120 140 141 150 160 161 170 180 230 231 210

GBGZ1G S I

GMUMBE S SI

GNAW99 SI

GUGPPP SI

GXJGYM S I I LC-QTOF

H2PHCD I

HB4JKY S I

HHLH88 S I

HVHHFH SI I

IJS22F S I

IQIQAI S I

IQJAM7 S I

IVV5RV I I SI

JRKD4U SI SI

JSZABT I I S

K3KSJ9 S I

KHJBOK I I

KJPKK4 I S zivia kit multitest

L3ZOZH S I

LJTLFH S I

M8VO1Z S I SI

MXA7O5 SI

NCMGK4 SI

NDP7T7 I I S immunochromatographie

NGAJ1Y S I

NP5333 S SI

OOO3GD S I I

PCBAPT S I I

PQFUYI SI SI I

PXJDZ1 SI I I

Q4WQSQ S I

QZEZZZ SI

RNJJ8Z S I

SOK66J S I I

SV8SSS I SI

SZZ1BZ S I

T0B0D0 SI

TBORSX S I

TG33JW S I I

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Code 100 110 120 140 141 150 160 161 170 180 230 231 210

TISIQZ SI SI

TTTGKV S S I I

U5KOOL S I I

UCTGCC S I I

UIUDEC S I

USDN2N I

UTSOWL I I Triage 8- ALERE Sure Step

UUXUUM SI I

V6ZRMH S I SI

VLHXHH S I

VN2UVV S I

VR1QQH SI

W5TXOT SI

WEB9SQ SI

WZRRBA S SI I

WZUJSD S I

XNXEE6 I S MULTIDRUG TEST

Y3AFEE S I I SI one step immonochromatographic assay

YFYCWJ S

YGKDY2 SI SI

YSKXXD S I

Z4YCUT I

ZGAWTE S I

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RESPONSE SUMMARY FOR TEST SAMPLE 4

Participants: 96

The response summary of all 96 participating laboratories for the identification of BS-4, frequency of use of

screening and identification techniques and false positives and negatives:

Identification of Test Sample-4:

Substance Name Number of laboratories correctly identifying:

Morphine 84

False positives for Test Sample-4:

Round Code: Substance Name: Tech Code:

OH72WR 6-Monoacetylmorphine 180

GAHHTQ delta-9-THC acid 180

IQIQAI 6-Monoacetylmorphine 180

NGAJ1Y 6-Monoacetylmorphine 180

SV8SSS Codeine 180

VN2UVV 6-Monoacetylmorphine 180

WZUJSP Morphine 3-glucuronide 150

PXJDZI Morphine 3-glucuronide, Codeine 180

8LCBAB Codeine 150

False negatives for Test Sample-4 (techniques(s) used for ANP):

Round Code: Substance Name: Tech Code:

B1KV8H - 150

W5TXOT - 180

NDP7T7 - 180

WZUJSD - 150

KHJBOK - 150

FBYTRU

ANP

ZGAWTE

ANP

KJPKK4 ANP

T0B0D0 ANP

LJTLFH ANP

Frequency of use of screening, identification and quantification techniques:

Response Summary

Participants 96

Technique 100 110 120 140 141 150 160 161 170 180 210

Screening (No.) 2 54 3 1 1 2 0 0 0 26 12

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

Identification (No.) 0 3 0 0 0 6 1 7 1 81 7

(%) 0.0 3.1 0.0 0.0 0.0 6.3 1.0 7.3 1.0 84.4 7.3

Quantification (No.) 0 1 0 0 0 0 1 4 0 28 2

(%) 0.0 1.8 0.0 0.0 0.0 0.0 1.8 7.0 0.0 49.1 3.5

6263

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Z-Score Report per Sample per Substance

Round: 2017/1 Robust average = 822 ng/ml

Substance: BS-4; Morphine UNODC value = 860 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.

-3.4

-2.3

-1.4 - 1.4 -1.3-1.2

-1.0 -0.9-0.7

-0.6 -0.6-0.5 -0.5

- 0.4- 0.3 - 0.3

-0.2-0.1

0.0 0.0 0.0

0.0 0.1 0.2 0.20.3

0.4 0.4 0.5 0.60.7

1.6

2.1

2.62.8

3.4

4.0

6.5 14.3

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

K3

KSJ

9

UTS

OW

L

CP

USP

P

8TP

BU

N

GX

JGYM

QZE

ZZZ

8V

X7

GU

66O

QY6

JSZA

BT

BH

WJH

B

D1

AYD

M

EPEV

E2

7FE

MIN

Y3A

FEE

DD

SBTD

YSK

XX

D

BN

GG

0M

TBO

RSX

TG33

JW

DD

A5

D2

M8

VO

1Z

GU

GP

PP

HV

HH

FH

AM

MR

SO

NP

5333

BB

KEU

E

TISI

QZ

FWX

VW

L

IQJA

M7

DB

4Y6

M

4FF

58F

GB

GZ1

G

84H

KV

U

MX

A7

O5

8M

FF1

T

RN

JJ8

Z

3FM

D3

X

VLH

XH

H

WZR

RB

A

6364

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Z-Score Report per Sample per Substance

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

GC/MS LC/MS

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Z-Scores for Test Sample 4

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Concentration

(ng/ml)

Deviation from

robust averagez-score

K3KSJ9 191 -631 -3.4

UTSOWL 398 -424 -2.3

CPUSPP 553 -269 -1.4

8TPBUN 564 -258 -1.4

GXJGYM 570 -252 -1.3

QZEZZZ 600 -222 -1.2

8VX7GU 639 -183 -1.066OQY6 656 -166 -0.9

JSZABT 685 -137 -0.7

BHWJHB 710 -112 -0.6

D1AYDM 710 -112 -0.6

EPEVE2 725 -97 -0.5

7FEMIN 728 -94 -0.5

Y3AFEE 750 -72 -0.4

DDSBTD 769 -53 -0.3

YSKXXD 769 -53 -0.3

BNGG0M 780 -42 -0.2

TBORSX 800 -22 -0.1

TG33JW 817 -5 0.0

DDA5D2 821 -1 0.0

M8VO1Z 821 -1 0.0

GUGPPP 831 9 0.0

HVHHFH 839 17 0.1

AMMRSO 850 28 0.2

NP5333 852 30 0.2

BBKEUE 880 58 0.3TISIQZ 900 78 0.4

FWXVWL 902 80 0.4

IQJAM7 914 92 0.5

DB4Y6M 932 110 0.6

4FF58F 958 136 0.7

GBGZ1G 1114 292 1.6

84HKVU 1221 399 2.1

MXA7O5 1311 489 2.6

8MFF1T 1339 517 2.8

RNJJ8Z 1461 639 3.4

3FMD3X 1563 741 4.0

VLHXHH 2035 1213 6.5

WZRRBA 3500 2678 14.3

Code

Morphine

6566

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