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INTERNATIONAL COLLABORATIVE EXERCISES (ICE) ICE 2019/2 Summary Report ICE Round 2019/2 BIOLOGICAL SPECIMENS

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INTERNATIONAL COLLABORATIVE

EXERCISES (ICE)

ICE

20

19

/2

Summary Report

ICE Round 2019/2

BIOLOGICAL SPECIMENS

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International Collaborative Exercises (ICE)

Summary report 2019/2- Biological Specimens

Copyright © 2020 UNODC

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ICE 2019/2-BS

Final summary report for ICE 2019/2 Biological Specimens Test Group

Original language: English

© United Nations, July 2020. All rights reserved, worldwide.

The designations employed and the presentation of material in this publication do not imply the expression of

any opinion whatsoever on the part of the Secretariat of the United Nations concerning the legal status of any

country, territory, city or area, or of its authorities, or concerning the delimitation of its frontiers or boundaries.

This publication has not been formally edited.

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International Collaborative Exercises (ICE)

Summary report 2019/2- Biological Specimens

Copyright © 2020 UNODC

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ICE 2019/2-BS

Acknowledgements

The Laboratory and Scientific Section (LSS) of the UNODC, headed by Dr. Justice Tettey, wishes to express its

appreciation and thanks to all laboratories for participating in the International Collaborative Exercises (ICE)

round 2019/2.

The valuable comments and contribution from the following members of the International Panel of Forensic

Experts are gratefully acknowledged:

Mr. Benoit Archambault, Health Canada, Canada

Mr. Elvio Dias Botelho, Brazilian Federal Police, Brazil

Prof. Heesun Chung, Sungkyunkwan University, Republic of Korea

Prof. Niamh Nic Daéid, University of Dundee, Scotland, UK

Mr. Scott Oulton, Drug Enforcement Administration, USA

Ms. Catherine Quinn, Victoria Police, Australia

Prof. Franco Tagliaro, University of Verona, Italy

Dr. Angeline Tiong Whei Yap, Health Sciences Authority, Singapore

In addition, LSS 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.

The ICE is coordinated by Ms. Yen Ling Wong, Scientific Affairs Officer, a staff member of LSS. The assistance

and the contributions of the following LSS staff members are gratefully acknowledged.

Dr. Conor Crean, Scientific Affairs Officer

Mr. Joao Rodrigues, Scientific Affairs Officer

Ms. Romana Luger, Research Assistant

Dr. Gerd Krapf, Laboratory Technician

Mr. Michael Bell, Laboratory Technician

Ms. Mikaela Edwards, Individual Contractor

For additional information or comments, please contact:

Ms. Yen Ling Wong

ICE Coordinator

Scientific Affairs Officer

Laboratory and Scientific Section

UNODC, Vienna International Centre

Wagramer Strasse 5, P.O. Box 500

A-1400, Vienna, AUSTRIA

Email: [email protected]

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International Collaborative Exercises (ICE)

Summary report 2019/2- Biological Specimens

Copyright © 2020 UNODC

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ICE 2019/2-BS

Contents

1. Codes and Abbreviations ..............................................................................................................................4

2. Test samples information .............................................................................................................................5

3. Introduction ..................................................................................................................................................6

4. Comments from the International Panel of Forensic Experts ......................................................................7

5. New Psychoactive Substances (NPS) reported .............................................................................................9

6. Summary of responses for Test Sample-1 ................................................................................................. 11

7. Summary of responses for Test Sample-2 ................................................................................................. 15

8. Summary of responses for Test Sample-3 ................................................................................................. 20

9. Summary of responses for Test Sample-4 ................................................................................................. 24

10. ANNEX 1: Participants’ results for Test Sample-1 ..................................................................................... 28

11. ANNEX 2: Participants’ results for Test Sample-2 ..................................................................................... 40

12. ANNEX 3: Participants’ results for Test Sample-3 ..................................................................................... 52

13. ANNEX 4: Participants’ results for Test Sample-4 ..................................................................................... 64

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ICE 2019/2-BS

1. Codes and Abbreviations

(+) “positive” Indicates that the analyte is identified; for presumptive tests (e.g. colour reactions), indicates

that a positive reaction was obtained.

(-) “negative” Indicates that the analyte is not identified.

(ANP) Analysis not performed.

Tech Code Name

100 Agglutination techniques

110 Enzyme immunoassay techniques

120 Fluorescence polarization immunoassay

130 Radioimmunoassay

140 Colorimetric reactions

141 Marquis test

142 Cobalt thiocyanate test

150 Thin layer chromatography (TLC)

160 High/ultra high performance liquid chromatography with ultraviolet-visible spectroscopy (HPLC/UPLC)

161 High/ultra high performance liquid chromatography with diode array detection (HPLC-DAD or UPLC-DAD)*

170 Gas chromatography with nitrogen-phosphorous detection (GC-NPD)

171 Gas chromatography with flame ionization detection (GC-FID)

172 Gas chromatography with electron capture detection (GC-ECD)

180 Gas chromatography with mass spectrometry (GC-MS)

190 Fourier transform infrared spectrometry (FTIR)

200 Spectrophotometry (visible, UV)

210 Others

211 Nuclear magnetic resonance spectroscopy (NMR)

220 Microcrystal test

230 Liquid chromatography with mass spectrometry (LC-MS)

231 Liquid chromatography with tandem mass spectrometry (LC-MS/MS)

*similar to 160

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ICE 2019/2-BS

2. Test samples information

The following four (4) test samples for the Biological Specimens test group were prepared by a private

company under subcontract with the Laboratory and Scientific Section, UNODC:

Test Sample-1 (BS-1)

To prepare BS-1, urine was spiked with an ethanolic solution of MDMA hydrochloride to achieve a final

concentration of 920 ng base/ml. The spiked urine was dispensed in 25 ml aliquots and lyophilised.

Test Sample-2 (BS-2)

To prepare BS-2, urine was spiked with an ethanolic solution of ketamine hydrochloride and a methanolic

solution of norketamine to achieve final concentrations of 920 ng base/ml and 1150 ng base/ml, respectively.

The spiked urine was dispensed in 25ml aliquots and lyophilised.

Test Sample-3 (BS-3)

To prepare BS-3, urine was spiked with an aqueous solution of morphine sulphate to achieve a final

concentration of 690 ng base/ml. The spiked urine was dispensed in 25ml aliquots and lyophilised.

Test Sample-4 (BS-4)

To prepare BS-4, urine was spiked with a methanolic solution of temazepam to achieve a final concentration

of 920 ng base/ml. The spiked urine was dispensed in 25ml aliquots and lyophilised.

All test samples were prepared from urine free of all major groups of abused drugs. Metabolites of caffeine

may be present. No preservatives were added to the urine samples. All analytes spiked into the test samples

were commercially sourced reference standards.

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ICE 2019/2-BS

6662

77

94100 102

116

129 132 131

151

159

179173

184 185

204 204 204

195

222

213

26 2733

4237

4754

6258

62

72 74

8690

9592

96 9793

87

101 104

0

50

100

150

200

250

No

. o

f la

bo

rato

rie

s

ICE round

SM BS

3. Introduction

An important element of the UNODC International Quality Assurance Programme (IQAP) is the

implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both

developing and developed countries to continuously monitor their performance in drug testing on a truly

global scale. This report provides information on analytical results of laboratories participating in the Biological

Specimens (BS) test group. In order to maintain confidentiality, the participating laboratories have been

assigned random “Round 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". Figure 1 shows the growth of the programme in recent years for both the Seized Materials (SM)

and the Biological Specimens (BS) test groups.

Figure 1. Growth of the ICE programme (as of 4 June 2020)

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ICE 2019/2-BS

4. Comments from the International Panel of Forensic Experts

4.1 Participation of Laboratories in ICE round 2019/2

In the 2019/2 round of the ICE programme, results were submitted within both the Seized Materials (SM)

and Biological Specimens (BS) test groups by 258 laboratories in 77 countries. Within the BS test group,

results were submitted by 104 laboratories from 48 countries and within the SM test group, there were

213 participating laboratories from 67 countries.

4.2 Qualitative Analysis

The analytical techniques most commonly used for screening of test samples in the BS test group were

immunoassays (68% of participants). GC-MS (72% of participants) was the most commonly used technique

for identification/confirmation of the components in the test samples, followed by LC-MS/MS (43% of

participants). The results for the qualitative identification of the sample components in the BS test group,

the number of false positive/negative results and the analyses not performed are shown in Table 1.

Table 1. Performance of participants in the 2019/2 round of ICE.

Test sample BS-1

(MDMA)

BS-2 BS-3 BS-4

(Ketamine) (Norketamine) (Morphine) (Temazepam)

Correct identification

by participants 87.5%

81.7% 69.2% 83.7% 81.7%

At least 1 component: 83.7%

Number of false

positives 4 6 9 14

Number of false

negatives 7 8 6 6

Number of analyses

not performed 6 9 11 13

Overall, the number of laboratories with correct identifications were slightly lesser than the previous round.

An increase in the total number of false positives and false negatives reported was also observed. In

addition, the number of analyses not performed has also increased from the previous round. It is of concern

that 14 laboratories obtained false positives for BS-4 (Temazepam). Laboratories reporting false positive or

false negative results should investigate the reasons for this and corrective actions should be taken as soon

as possible 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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ICE 2019/2-BS

4.3 Quantitative Analysis

The test samples in the BS group for the 2019/2 round of ICE contained a total of five components and 43

(41%) of participating laboratories performed quantification. Of these laboratories, it is encouraging to

note that 81% of laboratories quantified at least two components and 44% performed quantification of all

five components. GC-MS, used by 53% of participants, was the most commonly used technique for

quantitation, followed by LC-MS/MS, which was used by 47% of participants. z-Scores obtained by

participants in quantification are shown in Table 2 below (percentage + no. of labs indicated).

Table 2. Quantitative performance of participants in the 2019/2 round of ICE.

In general, the performance of laboratories improved with more laboratories achieving acceptable z-scores.

According to the recommendations in ISO 13528:2015, an unacceptable 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 as soon as possible.

The following laboratories obtained a single action signal or warning signal in the two successive rounds of

2019/1 and 2019/2 and shall take this as anomaly, which requires further investigation: 1WXG1M, 2ZHQMZ,

HLV08P and NHMXHX.

Of the 4 laboratories that obtained a single action or warning signal in ICE rounds 2018/2 and 2019/1, 3

laboratories improved their performance in round 2019/2 while 1 laboratory obtained action or warning

signals in this round: 2ZHQMZ.

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.

z-score

Test sample

BS-1

(920 ng/ml

MDMA)

BS-2

(920 ng/ml Ketamine)

BS-2

(1150 ng/ml Norketamine)

BS-3

(690 ng/ml Morphine)

BS-4

(920 ng/ml Temazepam)

|z| ≤ 2.00,

acceptable 94.6% (35) 82.8% (24) 100.0% (21) 86.1% (31) 84.4% (27)

2.00 < |z| < 3.00,

questionable 0.0% (0) 6.9% (2) 0.0% (0) 2.8% (1) 6.3% (2)

|z| ≥ 3.00,

unacceptable 5.4% (2) 10.3% (3) 0.0% (0) 11.1% (4) 9.4% (3)

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ICE 2019/2-BS

5. New Psychoactive Substances (NPS) reported

During the 2019/2 round of ICE, participating laboratories provided information on NPS that had been

identified in their laboratories. In total there were 336 reports of 178 substances and the most

commonly reported substances were synthetic cathinones (31%) followed by synthetic cannabinoids

(26%) as shown in Figure 2.

Figure 2. Distribution of classes of NPS reported by ICE laboratories during the 2019/2 round of ICE

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances

reported were stimulants (35%), while 25% were synthetic cannabinoid receptor agonists (SCRA) and

19% were hallucinogens as shown in Figure 3.

Figure 3. Distribution of NPS reported by ICE participants in the 2019/2 round of ICE according to the

mode of action

Synthetic

cannabinoids

26%

Synthetic

cathinones

31%

Other

substances

19%

Phenethylamines

13%

Phencyclidine-type

substances

6%

Tryptamines

5%

Synthetic cannabinoid

receptor agonists

25%

Stimulants

35%

Hallucinogens

19%

Opioids

3%

Dissociatives

6%

Sedatives/Hypnotics

7%

Others

5%

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ICE 2019/2-BS

The substances most often reported by ICE participants are listed in Table 3 below in descending order.

4F-MDMB-BINACA, 5F-MDMB-PICA and Etizolam were placed under international control at the 63rd

session of the Commission on Narcotic Drugs in March 2020 and these decisions will enter into force on

3rd November 2020.

Table 3. Most commonly reported NPS by laboratories participating in ICE 2019/2

Name Convention Schedule Effective date of

international control

4F-MDMB-BINACA

methyl 2-(1-(4-fluorobutyl)-1H-

indazole-3-carboxamido)-3,3-

dimethylbutanoate

1971 II 3rd November 2020

5F-MDMB-PICA

methyl 2-(1-(5-fluoropentyl)-1H-

indole-3-carboxamido)-3,3-

dimethylbutanoate

1971 II 3rd November 2020

Ketamine 2-(2-chlorophenyl)-2-

(methylamino)cyclohexan-1-one Currently not under international control

Etizolam

4-(2-chlorophenyl)-2-ethyl-9-

methyl-6H-thieno[3,2-f][1,2,4]-

triazolo[4,3-a][1,4]diazepine

1971 IV 3rd November 2020

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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ICE 2019/2-BS

6. Summary of responses for Test Sample-1

The summary of responses of all 104 participating laboratories for the identification of BS-1:

Correct identification of Test Sample-1:

False positives for Test Sample-1 (technique(s) used):

False negatives for Test Sample-1 with respect to MDMA (technique(s) used):

Round Code Tech Code

HHJU84 180

K15R1P 130

KFCL1O 150

NHMXHX 110, 150

SS6REF 180

TOVQID 180

XAL8XE 180

Analysis not performed for Test Sample-1 with respect to MDMA:

1HO1NR, 5U54R5, IVVPXY, V2TTTI, VCNWXW and YXYYWO

Frequency of use of screening, identification and quantification techniques:

Test Sample 1: Response Summary

No of Participants: 104 (Qualitative); 37 (Quantitative)

Technique 100

110 120 130 140 150 161 170 172 180 190 210 230 231

Screening (No.) 2 54 2 1 0 1 1 1 0 20 1 1 4 9

(%) 1.9 51.9 1.9 1.0 0.0 1.0 1.0 1.0 0.0 19.2 1.0 1.0 3.8 8.7

Identification

(No.

0 3 1 1 1 7 7 1 2 75 0 1 14 45

(%) 0.0 2.9 1.0 1.0 1.0 6.7 6.7 1.0 1.9 72.1 0.0 1.0 13.5 43.3

Quantification (No.) 0 0 0 0 0 0 0 0 0 15 0 1 3 15

(%) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 40.5 0.0 2.7 8.1 40.5

Substance Name Number of laboratories Percentage

MDMA 91 87.5%

Round Code Substance Reported Tech Code

4MVDPF Mephedrone 231

KFCL1O Methadone 150

TOVQID Metamfetamine 180

UDA9RR Metamfetamine 150

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

Round: 2019/2

Substance: BS-1; MDMA

-1.7

0

-1.4

5 -1.0

1

-0.9

7

-0.9

5

-0.8

9

-0.8

7

-0.8

2

-0.6

4

-0.6

4

-0.6

4

-0.4

7

-0.4

0

-0.3

8

-0.3

8

-0.3

1

-0.2

7

-0.1

8

-0.1

8

-0.1

5

-0.1

5

-0.1

4

-0.0

2

0.0

9

0.1

9

0.4

2

0.5

1

0.6

0

0.8

2

0.8

6 1.1

4

1.3

7

1.4

1

1.5

6

1.6

2

3.7

3

70.6

1

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

GGGGLA

PZKF1X

KW

AGZD

GO

UDX1

NCHVCR

Y4BXDJ

PEW

PPB

VVVM

VL

7BA2IC

U1LAJJ

T5552F

JBCBBB

S67HVA

8T85GY

OLKLLL

00EM

0W

QNIW

GB

QCYPRL

XN31XS

9L2893

HNCPVB

YCBZM

P

QSJN

NV

RREHHH

4Q

OCQ

S

IKQ

DO

Z

LVFR11

3YZ7RO

BBBPDA

JHHAXC

HLV08P

PIP

PUP

UFDUCR

DUPO

OO

1W

XG1M

JGW

JYI

KL7XB8

Z-scores can be interpreted by participants in line with ISO 13528:2015*, section 9.4.2 as follows: IzI ≤ 2.00 is considered to be acceptable 2.00 < IzI < 3.00 is considered to be questionable (or warning signal) IzI ≥ 3.00 is considered to be unacceptable (or action signal)

A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

Robust mean: 785 ng/ml

Robust SD: 225 ng/ml

Robust CV%: 28.6%

UNODC value: 920 ng/ml

Max reported: 16638 ng/ml

Min reported: 404 ng/ml

No of labs: 37

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

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ICE 2019/2-BS

Z-Scores for Test Sample-1

Code

MDMA

Concentration

(ng/ml)

Deviation

from robust

average

(ng/ml)

z-score

GGGGLA 404 -381 -1.70

PZKF1X 460 -325 -1.45

KWAGZD 558 -227 -1.01

GOUDX1 567 -218 -0.97

NCHVCR 572 -213 -0.95

Y4BXDJ 585 -200 -0.89

PEWPPB 588 -197 -0.87

VVVMVL 600 -185 -0.82

7BA2IC 640 -145 -0.64

U1LAJJ 641 -144 -0.64

T5552F 642 -143 -0.64

JBCBBB 678 -107 -0.47

S67HVA 694 -91 -0.40

8T85GY 700 -85 -0.38

OLKLLL 700 -85 -0.38

00EM0W 716 -69 -0.31

QNIWGB 725 -60 -0.27

QCYPRL 744 -41 -0.18

XN31XS 745 -40 -0.18

9L2893 750 -35 -0.15

HNCPVB 750 -35 -0.15

YCBZMP 753 -32 -0.14

QSJNNV 780 -5 -0.02

RREHHH 805 20 0.09

4QOCQS 827 42 0.19

IKQDOZ 879 94 0.42

LVFR11 899 114 0.51

3YZ7RO 920 135 0.60

BBBPDA 969 184 0.82

JHHAXC 978 193 0.86

HLV08P 1040 255 1.14

PIPPUP 1093 308 1.37

UFDUCR 1100 315 1.41

DUPOOO 1135 350 1.56

1WXG1M 1148 363 1.62

JGWJYI 1622 837 3.73

KL7XB8 16638 15853 70.61

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ICE 2019/2-BS

7. Summary of responses for Test Sample-2

The summary of responses of all 104 participating laboratories for the identification of BS-2:

Correct identification of Test Sample-2:

False positives for Test Sample-2 (technique(s) used):

False negatives for Test Sample-2 with respect to Ketamine (and/or metabolite) (technique(s) used):

Round Code Tech Code Round Code

Round Code

Tech Code

DUPOOO 180 KFCL1O 150

GGHZVX 150, 180 NHMXHX 150

HHJU84 180 PEWPPB 230, 231

K15R1P 130 XAL8XE 180

Analysis not performed for Test Sample-2 with respect to Ketamine (and metabolite):

1HO1NR, 5U54R5, HPX5UF, IVVPXY, TOVQID, YCBZMP, YMCYXY, YXYYWO and Z6ATVN

Frequency of use of screening, identification and quantification techniques:

Test Sample 2: Response Summary

No of Participants: 104 (Qualitative); 29 (Quantitative)

Technique 100

110 120 130 140 150 161 170 172 180 190 210 230 231

Screening (No.) 2 54 2 1 0 1 1 1 0 20 1 1 4 9

(%) 1.9 51.9 1.9 1.0 0.0 1.0 1.0 1.0 0.0 19.2 1.0 1.0 3.8 8.7

Identification

(No.

0 3 1 1 1 7 7 1 2 75 0 1 14 45

(%) 0.0 2.9 1.0 1.0 1.0 6.7 6.7 1.0 1.9 72.1 0.0 1.0 13.5 43.3

Quantification (No.) 0 0 0 0 0 0 0 0 0 11 0 1 1 13

(%) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 37.9 0.0 3.4 3.4 44.8

Substance Name Number of laboratories Percentage

Ketamine 85 81.7%

Norketamine 72 69.2%

At least one component 87 83.7%

Round Code Substance Reported Tech Code

IVVPXY MDMA 180

K15R1P Buprenorphine, norbuprenorphine 130

KFCL1O Morphine 150

PEWPPB 6-Monoacetylmorphine 230, 231

SS6REF Methylecgonine 180

XAL8XE Amfetamine, temazepam,

nordazepam

180, 231

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

Round: 2019/2

Substance: BS-2; Ketamine

-2.06

-1.42

-1.20

-1.04

-0.81

-0.59

-0.54

-0.47

-0.40

-0.29

-0.29

-0.26

-0.24

-0.18

-0.15

-0.15

-0.13

-0.10

-0.06

0.00

0.15

0.40 0.83

1.03 1.42

2.22

3.41

4.19

7.79

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

KL7XB8

7BA2IC

3YZ7RO

GOUDX1

T5552F

PIPPUP

BBBPDA

00EM0W

RREHHH

QSJNNV

U1LAJJ

QNIWGB

IKQDOZ

VVVMVL

8T85GY

9L2893

Y4BXDJ

QCYPRL

LVFR11

XN31XS

JBCBBB

1WXG1M

JHHAXC

GGGGLA

PZKF1X

JGWJYI

2ZHQMZ

HLV08P

4QOCQS

Robust mean: 955 ng/ml

Robust SD: 364 ng/ml

Robust CV%: 38.1%

UNODC value: 920 ng/ml

Max reported: 3790 ng/ml

Min reported: 205.15 ng/ml

No of labs: 29

Z-scores can be interpreted by participants in line with ISO 13528:2015*, section 9.4.2 as follows: IzI ≤ 2.00 is considered to be acceptable 2.00 < IzI < 3.00 is considered to be questionable (or warning signal) IzI ≥ 3.00 is considered to be unacceptable (or action signal)

A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

Round: 2019/2

Substance: BS-2; Norketamine

-1.62

-1.50 -1.07

-0.80

-0.54

-0.48

-0.31

-0.29

-0.27

-0.22

-0.20

-0.13

-0.05

0.01

0.62

0.65 0.97

1.06

1.12 1.43 1.90

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

KL7XB8

T5552F

GOUDX1

8T85GY

PIPPUP

00EM0W

BBBPDA

XN31XS

QCYPRL

VVVMVL

QNIWGB

QSJNNV

U1LAJJ

RREHHH

LVFR11

4QOCQS

1WXG1M

JHHAXC

IKQDOZ

GGGGLA

HLV08P

Z-scores can be interpreted by participants in line with ISO 13528:2015*, section 9.4.2 as follows: IzI ≤ 2.00 is considered to be acceptable 2.00 < IzI < 3.00 is considered to be questionable (or warning signal) IzI ≥ 3.00 is considered to be unacceptable (or action signal)

A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

Robust mean: 885 ng/ml

Robust SD: 482 ng/ml

Robust CV%: 54.5%

UNODC value: 1150 ng/ml

Max reported: 1800 ng/ml

Min reported: 103.95 ng/ml

No of labs: 21

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

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ICE 2019/2-BS

Z-Scores for Test Sample-2

Code

Ketamine

Code

Norketamine

Concentration

(ng/ml)

Deviation

from robust

average

(ng/ml)

z-score Concentration

(ng/ml)

Deviation

from robust

average

(ng/ml)

z-score

KL7XB8 205 -750 -2.06 KL7XB8 104 -781 -1.62

7BA2IC 440 -515 -1.42 T5552F 163 -722 -1.50

3YZ7RO 518 -437 -1.20 GOUDX1 370 -515 -1.07

GOUDX1 576 -379 -1.04 8T85GY 500 -385 -0.80

T5552F 661 -294 -0.81 PIPPUP 626 -259 -0.54

PIPPUP 742 -213 -0.59 00EM0W 652 -233 -0.48

BBBPDA 757 -198 -0.54 BBBPDA 734 -151 -0.31

00EM0W 783 -172 -0.47 XN31XS 745 -140 -0.29

RREHHH 810 -145 -0.40 QCYPRL 756 -129 -0.27

QSJNNV 850 -105 -0.29 VVVMVL 780 -105 -0.22

U1LAJJ 850 -105 -0.29 QNIWGB 790 -95 -0.20

QNIWGB 860 -95 -0.26 QSJNNV 820 -65 -0.13

IKQDOZ 869 -86 -0.24 U1LAJJ 860 -25 -0.05

VVVMVL 890 -65 -0.18 RREHHH 890 5 0.01

8T85GY 900 -55 -0.15 LVFR11 1181 296 0.62

9L2893 901 -54 -0.15 4QOCQS 1200 315 0.65

Y4BXDJ 907 -48 -0.13 1WXG1M 1350 465 0.97

QCYPRL 918 -37 -0.10 JHHAXC 1395 510 1.06

LVFR11 933 -22 -0.06 IKQDOZ 1424 539 1.12

XN31XS 955 0 0.00 GGGGLA 1573 688 1.43

JBCBBB 1010 55 0.15 HLV08P 1800 915 1.90

1WXG1M 1100 145 0.40 JHHAXC 1256 301 0.83 GGGGLA 1330 375 1.03 PZKF1X 1470 515 1.42 JGWJYI 1762 807 2.22 2ZHQMZ 2197 1242 3.41 HLV08P 2480 1525 4.19 4QOCQS 3790 2835 7.79

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ICE 2019/2-BS

8. Summary of responses for Test Sample-3

The summary of responses of all 104 participating laboratories for the identification of BS-3:

Correct identification of Test Sample-3:

False positives for Test Sample-3 (technique(s) used):

False negatives for Test Sample-3 with respect to Morphine (technique(s) used):

Round Code Tech Code

CVDCCW 180

GGHZVX 150, 180

IVVPXY 180

KFCL1O 150

SS6REF 180

XAL8XE 180

Analysis not performed for Test Sample-3 with respect to Morphine:

1IH7T1, 33GBDB, 5U54R5, 6DFVYY, HPX5UF, L0ZAGA, UFDUCR, V2TTTI, VLAS0P, YCBZMP and YXYYWO

Frequency of use of screening, identification and quantification techniques:

Test Sample 3: Response Summary

No of Participants: 104 (Qualitative); 36 (Quantitative)

Technique 100

110 120 130 140 150 161 170 172 180 190 210 230 231

Screening (No.) 2 54 2 1 0 1 1 1 0 20 1 1 4 9

(%) 1.9 51.9 1.9 1.0 0.0 1.0 1.0 1.0 0.0 19.2 1.0 1.0 3.8 8.7

Identification

(No.

0 3 1 1 1 7 7 1 2 75 0 1 14 45

(%) 0.0 2.9 1.0 1.0 1.0 6.7 6.7 1.0 1.9 72.1 0.0 1.0 13.5 43.3

Quantification (No.) 0 0 0 0 0 0 1 0 0 18 0 1 2 11

(%) 0.0 0.0 0.0 0.0 0.0 0.0 2.8 0.0 0.0 50.0 0.0 2.8 5.6 30.6

Substance Name Number of laboratories Percentage

Morphine 87 83.7%

Round Code Substance Reported Tech Code

BCKYTY Hydromorphone 180, 231

CVDEWN Morphine-3-O-glucuronide 180

GGHZVX Methadone 150, 180

IVVPXY Temazepam* 180

K15R1P Methadone 130

KFCL1O Benzoylecgonine 150

SS6REF MDMA 180

UDA9RR Morphine-3-O-glucuronide 150

YMCYXY Codeine, MAM 180

* possible transcription error

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

Round: 2019/2

Substance: BS-3; Morphine

-4.10

-3.52

-3.25 -2.73

-1.43

-1.18

-0.88

-0.67

-0.60

-0.54

-0.38

-0.35

-0.26

-0.24

-0.19

-0.10

-0.03

0.07

0.07

0.11

0.22

0.23

0.26

0.36

0.40 0.68

0.78

0.80

0.82

0.83

0.99

1.03

1.09

1.09

1.59

32.91

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

KL7XB8

NHMXHX

JGWJYI

PEWPPB

IKQDOZ

GGGGLA

VVVMVL

XN31XS

4QOCQS

S67HVA

QNIW

GB

DUPOOO

T5552F

YMMZBM

KWAGZD

PIPPUP

7BA2IC

JBCBBB

RREHHH

8T85GY

9L2893

U1LAJJ

LVFR11

HLV08P

NCHVCR

Z6ATVN

QCYPRL

3YZ7RO

1WXG1M

BBBPDA

GOUDX1

00EM0W

Y4BXDJ

PZKF1X

QSJNNV

2ZHQMZ

Z-scores can be interpreted by participants in line with ISO 13528:2015*, section 9.4.2 as follows: IzI ≤ 2.00 is considered to be acceptable 2.00 < IzI < 3.00 is considered to be questionable (or warning signal) IzI ≥ 3.00 is considered to be unacceptable (or action signal)

A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

Robust mean: 634 ng/ml

Robust SD: 141 ng/ml

Robust CV%: 22.3%

UNODC value: 690 ng/ml

Max reported: 5290 ng/ml

Min reported: 55.04 ng/ml

No of labs: 36

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

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ICE 2019/2-BS

Z-Scores for Test Sample-3

Code

Morphine

Concentration

(ng/ml)

Deviation

from robust

average

(ng/ml)

z-score

KL7XB8 55 -579 -4.10

NHMXHX 136 -498 -3.52

JGWJYI 175 -459 -3.25

PEWPPB 248 -386 -2.73

IKQDOZ 432 -202 -1.43

GGGGLA 468 -166 -1.18

VVVMVL 510 -124 -0.88

XN31XS 540 -94 -0.67

4QOCQS 550 -84 -0.60

S67HVA 558 -76 -0.54

QNIWGB 580 -54 -0.38

DUPOOO 585 -49 -0.35

T5552F 598 -36 -0.26

YMMZBM 600 -34 -0.24

KWAGZD 608 -26 -0.19

PIPPUP 620 -14 -0.10

7BA2IC 630 -4 -0.03

JBCBBB 645 11 0.07

RREHHH 645 11 0.07

8T85GY 650 16 0.11

9L2893 665 31 0.22

U1LAJJ 667 33 0.23

LVFR11 671 37 0.26

HLV08P 686 52 0.36

NCHVCR 691 57 0.40

Z6ATVN 730 96 0.68

QCYPRL 745 111 0.78

3YZ7RO 748 114 0.80

1WXG1M 750 116 0.82

BBBPDA 752 118 0.83

GOUDX1 774 140 0.99

00EM0W 780 146 1.03

Y4BXDJ 789 155 1.09

PZKF1X 789 155 1.09

QSJNNV 860 226 1.59

2ZHQMZ 5290 4656 32.91

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ICE 2019/2-BS

9. Summary of responses for Test Sample-4

The summary of responses of all 104 participating laboratories for the identification of BS-4:

Correct identification of Test Sample-4:

False positives for Test Sample-4 (technique(s) used):

False negatives for Test Sample-4 with respect to Temazepam (technique(s) used):

Round Code Tech Code Round Code

Round Code

Tech Code

GGHZVX 150, 180 PEWPPB 230, 231

KFCL1O 150 SS6REF 180

NHMXHX 150 XAL8XE 180, 231

Analysis not performed for Test Sample-4 with respect to Temazepam:

1HO1NR, 1IH7T1, 5U54R5, FJUGNL, HPX5UF, N0N0VK, NSUYMO, PZKF1X, TOVQID, UFDUCR,

V2TTTI, YCBZMP and YXYYWO

Frequency of use of screening, identification and quantification techniques:

Test Sample 4: Response Summary

No of Participants: 104 (Qualitative); 32 (Quantitative)

Technique 100

110 120 130 140 150 161 170 172 180 190 210 230 231

Screening (No.) 2 54 2 1 0 1 1 1 0 20 1 1 4 9

(%) 1.9 51.9 1.9 1.0 0.0 1.0 1.0 1.0 0.0 19.2 1.0 1.0 3.8 8.7

Identification

(No.

0 3 1 1 1 7 7 1 2 75 0 1 14 45

(%) 0.0 2.9 1.0 1.0 1.0 6.7 6.7 1.0 1.9 72.1 0.0 1.0 13.5 43.3

Quantification (No.) 0 0 0 0 0 0 2 0 1 11 0 1 2 12

(%) 0.0 0.0 0.0 0.0 0.0 0.0 6.3 0.0 3.1 34.4 0.0 3.1 6.3 37.5

Substance Name Number of laboratories Percentage

Temazepam 85 81.7%

Round Code Substance Reported Tech Code Round Code Substance Reported Tech Code

2ZHQMZ Diazepam 180 NHMXHX Morphine* 150, 161

BCKYTY Diazepam 180, 231 PEWPPB Nordazepam 230, 231

GGHZVX Nordazepam 150, 180 PZKF1X Oxazepam 180

J0Q014 Diazepam 180, 231 TOVQID Zolpidem 180

K15R1P Nordazepam 130 WLNP5E Metamfetamine 230

KFCL1O Benzoylecgonine 150 XAL8XE 6-Monoacetylmorphine,

codeine, morphine

180, 231

N0N0VK Nordazepam 150, 172 YMCYXY Nordiazepam 180

* possible transcription error

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

Round: 2019/2

Substance: BS-4; Temazepam

-1.48

-1.23

-1.18

-1.03

-0.97

-0.95

-0.90

-0.81

-0.71

-0.53

-0.52

-0.47

-0.32

-0.02

-0.02

0.02

0.02

0.09

0.13

0.14

0.16

0.24

0.26

0.42

0.57

0.61 1.00

2.32

2.37

4.05

7.68

27.82

-4.00

-3.00

-2.00

-1.00

0.00

1.00

2.00

3.00

4.00

Z6ATVN

PIPPUP

DUPOOO

00EM0W

7BA2IC

JHHAXC

VVVMVL

4QOCQS

GOUDX1

EYQYPG

VCNWXW

3YZ7RO

KL7XB8

JBCBBB

QSJNNV

BBBPDA

8T85GY

RREHHH

QNIWGB

LVFR11

QCYPRL

U1LAJJ

KWAGZD

HLV08P

S67HVA

XN31XS

9L2893

Y4BXDJ

IKQDOZ

1WXG1M

GGGGLA

2ZHQMZ

Z-scores can be interpreted by participants in line with ISO 13528:2015*, section 9.4.2 as follows: IzI ≤ 2.00 is considered to be acceptable 2.00 < IzI < 3.00 is considered to be questionable (or warning signal) IzI ≥ 3.00 is considered to be unacceptable (or action signal)

A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occurred that requires investigation.

Robust mean: 895 ng/ml

Robust SD: 273 ng/ml

Robust CV%: 30.5%

UNODC value: 920 ng/ml

Max reported: 8488 ng/ml Min reported: 490 ng/ml No of labs: 32

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ICE 2019/2-BS

Z-Score Report per Sample per Substance:

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ICE 2019/2-BS

Z-Scores for Test Sample-4

Code

Temazepam

Concentration (ng/ml)

Deviation from robust

average (ng/ml)

z-score

Z6ATVN 490 -661 -1.48

PIPPUP 558 -593 -1.23

DUPOOO 573 -578 -1.18

00EM0W 613 -538 -1.03

7BA2IC 630 -521 -0.97

JHHAXC 636 -515 -0.95

VVVMVL 650 -501 -0.90

4QOCQS 674 -477 -0.81

GOUDX1 700 -451 -0.71

EYQYPG 751 -400 -0.53

VCNWXW 752 -399 -0.52

3YZ7RO 766 -385 -0.47

KL7XB8 808 -343 -0.32

JBCBBB 890 -261 -0.02

QSJNNV 890 -261 -0.02

BBBPDA 899 -252 0.02

8T85GY 900 -251 0.02

RREHHH 920 -231 0.09

QNIWGB 930 -221 0.13

LVFR11 933 -218 0.14

QCYPRL 939 -212 0.16

U1LAJJ 961 -190 0.24

KWAGZD 965 -187 0.26

HLV08P 1010 -141 0.42

S67HVA 1051 -100 0.57

XN31XS 1062 -89 0.61

9L2893 1168 17 1.00

Y4BXDJ 1527 376 2.32

IKQDOZ 1543 392 2.37

1WXG1M 2000 849 4.05

GGGGLA 2992 1841 7.68

2ZHQMZ 8488 7337 27.82

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ICE 2019/2-BS

10. ANNEX 1: Participants’ results for Test Sample-1

Identified substances for Test Sample 1

Code Identified Substances

00EM0W MDMA

14X0XQ MDMA

181PAR 3,4-methylenedioxymethamphetamine (MDMA)

1IH7T1 3,4-Methylenedioxymetamfetamine (MDMA)

1WXG1M MDMA

2ZHQMZ MDMA

33GBDB MDMA

3AIJ73 3,4-Methylenedioxymetamfetamine (MDMA)

3YZ7RO MDMA

4MVDPF MDMA and methadrone

4QOCQS MDMA

6DFVYY MDMA

700RJC 3,4-Methylenedioxymetamfetamine (MDMA)

7BA2IC MDMA

7KX1K4 3,4-Methylenedioxymetamfetamine (MDMA)

8T85GY MDMA

9L2893 MDMA

9X92FT 3,4-Methylenedioxymetamfetamine (MDMA)

AR2BHL MDMA

BBBPDA 3,4-Methylenedioxymetamfetamine (MDMA)

BCKYTY MDMA

BIQY5S MDMA

CVDCCW MDMA

CVDEWN MDMA

D07DV8 MDMA

D9SYSS MDMA

DUPOOO MDMA

DZITOQ 3,4-Methylenedioxymetamfetamine (MDMA)

EYQYPG MDMA

FAAKAX MDMA

FJUGNL MDMA

FPKXPP MDMA

FSYPJK 3,4-Methylenedioxymetamfetamine (MDMA)

GGGGLA MDMA

GGGW8M MDMA

GGHZVX MDMA

GOUDX1 MDMA

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ICE 2019/2-BS

Code Identified Substances

HLV08P MDMA

HNCPVB MDMA

HPX5UF MDMA

IKQDOZ MDMA

J0Q014 MDMA

JBCBBB MDMA

JGWJYI MDMA

JHHAXC MDMA

JVDIJJ 3,4-Methylenedioxy-metamfetamine (MDMA)

KFCL1O Méthadon

KHHBSB MDMA

KL7XB8 MDMA

L0ZAGA 3,4-Methylenedioxymetamfetamine (MDMA)

LVFR11 MDMA

MMMLHE MDMA

MRELLV MDMA

N0N0VK MDMA

N4NRKA MDMA

NCHVCR MDMA

NSUYMO 3,4-methylenedioximetamfetamine (MDMA)

OLKLLL 3,4-Methylenedioxymetamfetamine (MDMA)

PBRKVK MDMA

PEWPPB MDMA

PIPPUP mdma

PZKF1X MDMA

QCYPRL MDMA (ecstasy

QDQIQG MDMA

QSJNNV MDMA

RNZXZZ MDMA

RREHHH MDMA

S67HVA MDMA

T5552F MDMA

TOVQID Metanfetamina

U1LAJJ MDMA

UDA9RR Amfetamine type stimulans

UFDUCR 3,4-Methylenedioxymetamfetamine (MDMA)

UW5SKG 3,4-Methylenedioxymetamfetamine (MDMA)

V2TTTI None

VG8Y34 3,4-Methylenedioxymetamfetamine (MDMA)

VLAS0P MDMA

VVVMVL MDMA

WFEBOC MDMA

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ICE 2019/2-BS

Code Identified Substances

WLNP5E MDMA

X4J6QG 3,4-Methylendioxy-metamfetamine (MDMA)

XN31XS MDMA

Y4BXDJ 3,4-Methylenedioxymetamfetamine (MDMA)

YCBZMP 3,4-Methylenedioxymetamfetamine (MDMA)

YMCYXY amphetamines

YMMZBM MDMA

YXARNC 3,4-Methylenedioxymethamphetamine (MDMA)

YXCAHN 3,4-Methylenedioxymetamfetamine (MDMA)

Z1X7PA MDMA

Z6ATVN MDMA

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ICE 2019/2-BS

Statement of findings for Test Sample 1

Code 3,4-Methylenedioxymetamfetamine (MDMA)

00EM0W + Presence of MDMA

14X0XQ + Toxicological examination revealed the presence of MDMA

181PAR + we found MDMA as psychotropic substance based on INCB Green List Regulation

1HO1NR ANP

1IH7T1 + Sample 2019/2/BS/1 found to contain 3,4-Methylenedioxymetamfetamine (MDMA)

1WXG1M + MDMA

2ZHQMZ +

33GBDB + After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) as screening thecnique and Gas Chromatography/Mass Spectrometry (GC/MS) as confirmatory thecnique, was detected substance 3,4-Methylenedioxy-metanfetamine (MDMA) in the urine sample 2019/2/BS-1.

3AIJ73 + MDMA was identified by GC-MS

3YZ7RO + The sample contains MDMA

4MVDPF + Drugs listed were detected

4QOCQS + MDMA

5U54R5 ANP

6DFVYY + Screening by 161Tech

700RJC + The drug (MDMA) was confimed in urine that means the person is using MDMA drug

7BA2IC +

7KX1K4 + The sample contains MDMA.

8T85GY + Positive for MDMA

9L2893 ANP

9X92FT +

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

AR2BHL +

MDMA found

BBBPDA + 3,4-Methylenedioxymetamfetamine (MDMA)

BCKYTY + MDMA was not detected by immunoassay as it's concentration was below our established cut-off, but was identified by both GC/MS and LC-MS/MS, sample BS-1

BIQY5S + MDMA detected.

CVDCCW + MDMA detected

CVDEWN + It was detected the presence of MDMA in the sample analysed.

D07DV8 + Demonstrates prior ingestion of MDMA

D9SYSS + In the biological sample were identified: MDMA and caffeine.

DUPOOO + MDMA was detected using LC/MS/MS which indicate use of controlled drug

DZITOQ + the drug tha was fond is 3,4-Methylenedioxymetamfetamine (MDMA), confirmed by HPLC and GC/MS.

EYQYPG + 3,4-Methylenedioxy-N-Methylamphetamine (MDMA) Detected > 0.5mg/L

FAAKAX + The coincidence between the relative retention time and mass -fragmentograms from a reference standard analysed at the same conditions that the biological sample, indicates the detection of MDMA and Caffeine.

FJUGNL +

FPKXPP + Drug result: MDMA. Indicative of "ecstasy" consumption.

FSYPJK +

GGGGLA +

GGGW8M + MDMA (N-Methyl-3,4-methylenedioxyamphetamine) was identified in the sample.

GGHZVX + Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with MDMA

GOUDX1 +

HHJU84 - Listed drugs could not be detected in sample 2019/2/BS-1.

HLV08P + Sample 2019/2/BS-1 was found containing MDMA

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

HNCPVB + Consistent with use of MDMA.

HPX5UF + The urine was analysed and found to contain Methylenedioxymethylamphetamine (MDMA).

HYMHGB +

IKQDOZ + positive

IVVPXY ANP Not detected.

J0Q014 + CAFFEINE

JBCBBB + MDMA (Extacy) is detected in urine. This indicates intake of MDMA (Extacy), which is a drug with stimulating and hallucinogenic effects.

JGWJYI + MDMA consumption

JHHAXC +

JVDIJJ + In sample BS-1 the drug 3,4-Methylenedioxy-metamfetamine (MDMA) was detected.

K15R1P -

KFCL1O -

KHHBSB + MDMA was detected in the urine sample considering LOD=25 ng/mL

KL7XB8 + After chemical analysis was performed the sample contains MDMA + Caffeine

KWAGZD +

L0ZAGA + 3,4-Methylenedioxymetamfetamine (MDMA) was detected in sample 2019/2/BS-1.

LVFR11 +

MMMLHE +

MRELLV + positive for MDMA

N0N0VK + Sample 2019/2/BS-1 contain MDMA.

N4NRKA + The presence of MDMA in the sample indicates consumption of MDMA itself.

NCHVCR + recent intake of MDMA

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

NHMXHX -

NSUYMO + In the sample was detected MDMA, this finding indicates that MDMA was consumed

OLKLLL + Positive to 3,4-Methylenedioxymetamfetamine (MDMA)

PBRKVK +

PEWPPB +

PIPPUP + mdma CONSUMPION

PZKF1X +

QCYPRL + MDMA, well known as Ecstasy, an illegal drug, is a psychoactive drug primarily used as a recreational drug. The desired effects include altered sensations, increased energy, empathy, and pleasure.

QDQIQG + Sample positive for MDMA

QNIWGB +

QSJNNV +

RNZXZZ +

RREHHH + -

S67HVA + this person consumed MDMA

SS6REF -

T5552F +

TOVQID - Metanfetamina positivo

U1LAJJ + The laboratory identifed MDMA in urine.

UDA9RR + MDMA, Metamfetamine

UFDUCR + The sample BS-1 was found to be positive for 3,4-Methylenedioxymetamfetamine (MDMA)

UW5SKG + 3,4-Methylenedioxymetamfetamine (MDMA) was detected in BS-1 sample.

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

V2TTTI ANP According to the cut off values established by the laboratory; Barbiturate 200 ng/ml, THC 50 ng/ml, Cocaine150 ng/ml, Benzodiacepine 200 ng/ml and Opiate 2000 ng/ml. None drug metabolite was detected. Amphetamin, hallucinogenic drugs and any other controlled drugs are not analyze by the laboratory.

VCNWXW ANP Drugs were not detected in BS-1

VG8Y34 + In the urine sample labeled BS-1/2/2019 3,4-Methylenedioxymetamfetamine (MDMA) was found

VLAS0P + Sample 2019/2/BS-1 contains MDMA.

VVVMVL +

WFEBOC + IN BS-1 IT WAS DETECTED MDMA

WLNP5E + MDMA is a central nervous stimulant. MDMA is a Schedule I substance in the United States.

X4J6QG + in the analyzed urine sample it was detected and confirmed the prensence of 3,4-Methylendioxy- metamfetamine (MDMA).

XAL8XE -

XN31XS + Use of Ecstasy

Y4BXDJ +

YCBZMP + Test sample 2019/2/BS-1 was found to contain controlled drugs for3,4- Methylenedioxymetamfetamine (MDMA), therefore Positive for the Screening and Confirmatory analyses with concentration value of 753.06 ng/ml.

YMCYXY + MDAM

YMMZBM + Analytical Adverse Finding for MDMA

YXARNC + 3,4-Methylenedioxymethamphetamine (MDMA) was detected in BS-1 sample.

YXCAHN + use of MDMA

YXYYWO ANP The sample has negative results for : AMFETAMINE TYPE STIMULANTS, BARBITURATES, BENZODIAZEPINES, CANNABINOIDS COCAINE and/or METABOLITES, OPIATES/OPIOIDS. HALLUCINOGENIC DRUGS not performed. Z1X7PA + The presence of MDMA in urine indicates the intake of MDMA

Z6ATVN + HUBO CONSUMO DE MDMA

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Code 3,4-Methylenedioxymetamfetamine (MDMA)

ZO0USM +

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Identification methods for Test Sample 1

Analytical Technique Codes

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

00EM0W S SI I

14X0XQ S SI I

181PAR S I I

1HO1NR S I

1IH7T1 SI

1WXG1M S I

2ZHQMZ S I

33GBDB S I

3AIJ73 S I

3YZ7RO S I

4MVDPF I

4QOCQS SI I

6DFVYY S SI SI

700RJC SI

7BA2IC S I SI I

7KX1K4 SI S Q-TOF LC-MS

8T85GY S I

9X92FT I I

AR2BHL S I I I

BBBPDA S SI SI

BCKYTY S I I

BIQY5S S I I

CVDCCW I

CVDEWN S I

D07DV8 SI I

D9SYSS I SI

DUPOOO S I I

DZITOQ I I S chimical immunoassay techniques

EYQYPG S I I

FAAKAX I

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

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ICE 2019/2-BS

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

FJUGNL I

FPKXPP SI

FSYPJK S I

GGGGLA I I Triage 8, CUP Alere

GGGW8M I S Multi-Drug Test Panel(urine)

GGHZVX S I I

GOUDX1 S I I

HHJU84 S SI

HLV08P S I

HNCPVB S SI SI

HPX5UF S I

HYMHGB S I I

IKQDOZ I SI SFC-MS/MS

IVVPXY S I

J0Q014 S I I

JBCBBB SI I SI QTOF

JGWJYI S I

JHHAXC S I

JVDIJJ SI SI

K15R1P SI

KFCL1O I S

KHHBSB I S Immunoassay

KL7XB8 S I I

KWAGZD S I I

L0ZAGA SI

LVFR11 S I SI

MMMLHE SI

MRELLV S I

N0N0VK S I I I S Randox biochip technology,ketamines N4NRKA I I S lateral flow

NCHVCR S I SI LC-MS²

NHMXHX SI I I

NSUYMO I S Lateral Flow Inmunnoassay

OLKLLL S SI

PBRKVK I I S cobas analyzer

PEWPPB I I

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ICE 2019/2-BS

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

PIPPUP SI

PZKF1X S I

QCYPRL S I I

QDQIQG I S Chromatographic immunoassay

QNIWGB S I I

QSJNNV S I

RNZXZZ S I

RREHHH SI

S67HVA S I I

SS6REF SI

T5552F I I I Kinetic Interactions of Microparticles

TOVQID S I

U1LAJJ S I I

UDA9RR I SI Dipro Drug lab screen

UFDUCR S I I

UW5SKG S I I

V2TTTI S I HPLC MS-MS

VCNWXW S SI

VG8Y34 I

VLAS0P I

VVVMVL S I I LC-HR-MS-ORBITRAP

WFEBOC S I

WLNP5E I LC-QTOF

X4J6QG SI SI I

XAL8XE I I I

XN31XS I I S

Y4BXDJ S I LC/QTOF

YCBZMP I S DTK

YMCYXY SI I

YMMZBM SI SI

YXARNC S I

YXCAHN I

YXYYWO S

Z1X7PA S I SI

Z6ATVN S I I S randox

ZO0USM SI S doa L MultiGnost

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ICE 2019/2-BS

11. ANNEX 2: Participants’ results for Test Sample-2

Identified substances for Test Sample 2

Code Identified Substances

00EM0W ketamine and norketamine

14X0XQ Ketamine

1IH7T1 Ketamine, Norketamine

1WXG1M Ketamin,Norketamin

2ZHQMZ Ketamine, norketamine

33GBDB Ketamine and Norketamine

3AIJ73 Ketamine

3YZ7RO Ketamine and Norketamine

4MVDPF Ketamine and norketamine

4QOCQS KETAMINE, NORKETAMINE

6DFVYY NORKETAMINE-KETAMINE

700RJC Norketamine and Ketamine

7BA2IC ketamine and norketamine

7KX1K4 Ketamine and norketamine.

8T85GY Ketamine, norketamine

9L2893 ketamine

9X92FT ketamine, norketamine

AR2BHL Ketamine, Norketamine

BBBPDA Ketamine, Norketamine

BCKYTY Ketamine and Norketamine

BIQY5S Ketamine & Norketamine

CVDCCW Norketamine and Ketamine

CVDEWN Ketamine and Nor-Ketamine

D07DV8 Ketamine

D9SYSS ketamine

DZITOQ Ketamine and Norketamine

EYQYPG Ketamine, Norketamine

FAAKAX Ketamine, Norketamine

FJUGNL KETAMINE

FPKXPP Ketamine

FSYPJK Ketamine, Norketamine

GGGGLA KETAMINE,

GGGW8M Ketamine, Norketamine

GGHZVX none

GOUDX1 Norketamine and Ketamine

HLV08P Ketamine +Norketamine

HNCPVB Ketamine

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Code Identified Substances

IKQDOZ ketamine, norketamine

IVVPXY MDMA

J0Q014 KETAMINE

JBCBBB Ketamine

JGWJYI Ketamine, norketamine

JHHAXC KETAMINE

JVDIJJ Norketamine and Ketamine

K15R1P NORBUPRENORPHINE

KFCL1O Morphine

KHHBSB Ketamine and norketamine

KL7XB8 Ketamine/Norketamine

L0ZAGA Norketamine and Ketamine

LVFR11 Ketamine, norketamine

MMMLHE KETAMINE, NORKETAMINE

MRELLV Ketamine

N0N0VK norketamine

N4NRKA KETAMINE, norketamine

NCHVCR Ketamine / Norketamine

NSUYMO Ketemine and Norketamine

OLKLLL Ketamine and Norketamine

PBRKVK Ketamine

PEWPPB 6-MAM

PIPPUP keta AND norketa

PZKF1X caffeine, ketamine

QCYPRL Ketamine and norketamine

QDQIQG ketamine and norketamine

QSJNNV Ketamine, norketamine

RNZXZZ Ketamine, Norketamine

RREHHH Ketamine, Norketamine

S67HVA ketamine, norketamine

SS6REF METHYLECGONINE + KETAMINE + NORKETAMINE

T5552F Norketamine and Ketamine

U1LAJJ Ketamine, Norketamine

UDA9RR Others

UFDUCR Ketamine and Norketamine

UW5SKG Norketamine

V2TTTI None

VCNWXW Ketamine, Norketamine

VG8Y34 Norketamine and ketamine

VLAS0P Norketamine and Ketamine

VVVMVL kETAMINE AND NORKETAMINE

WFEBOC KETAMINE AND NORKETAMINE

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Code Identified Substances

WLNP5E Ketamine and Norketamine

X4J6QG Ketamine, norketamine

XN31XS ketamine, norketamine

Y4BXDJ Ketamine, Norketamine

YMMZBM Ketamine

YXARNC Ketamine and Norketamine

YXCAHN ketamine, norketamine

Z1X7PA ketamine, norketamine

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Statement of findings for Test Sample 2

Code Ketamine Norketamine

00EM0W + + Presence of ketamine and its metabolite norketamine

14X0XQ + - Toxicological examination revealed the presence of Ketamine

181PAR + + We found Ketamine and Norketamine as uncontrolled drugs

1HO1NR ANP ANP

1IH7T1 + + Sample 2019/2/BS/2 found to contain Ketamine and Norketamine

1WXG1M + + Ketamin,Norketamin

2ZHQMZ + +

33GBDB + + After completing the toxicological analyzes of the sample, using the Gas Chromatography/Mass Spectrometry (GC/MS) as screening thecnique and Gas Chromatography/Mass Spectrometry (GC/MS) as confirmation thecnique, were detected substances Ketamine and Norketamine in the urine sample 2019/2/BS-2.

3AIJ73 + ANP Ketamine was identified by GC-MS

3YZ7RO + + The sample contains Ketamine and Norketamine

4MVDPF + + drugs listed were detected

4QOCQS + + KETAMINE, NORKETAMINE

5U54R5 ANP ANP

6DFVYY + + Screening 161Tech

700RJC + + The presence of Norketamine in urine revealed the person is using hallucinogenic drug known as Ketamine since norketamine is biomarker metabolite for ketamine user

7BA2IC + +

7KX1K4 + + The sample contains ketamine and norketamine.

8T85GY + + Positive for ketamine

9L2893 ANP ANP

9X92FT + +

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Code Ketamine Norketamine

AR2BHL + + Ketamine and Norketamine found.

BBBPDA + + Ketamine, Norketamine

BCKYTY + + Ketamine and Nor-Ketamine were identified by GC/MS and LC-MS/MS only, but not with immunoassay, sample BS-2

BIQY5S + + Ketamine and norketamine detected. Norketamine is a metabolite of ketamine.

CVDCCW + + Norketamine and Ketamine detected

CVDEWN + + It was detected the presence of Ketamine ans Nor-ketamine in the sample analysed.

D07DV8 + ANP Demonstrates prior ingestion of ketamine

D9SYSS + + In the biological sample were identified: ketamine and norketamine (metabolite ketamine), caffeine.

DUPOOO - - Negative

DZITOQ + + Firstly, in general screening, we use chemical immunoassay techniques, the result was negatif and after GCMS, HPLC analysis techniques we have fond two drugs: Ketamine and Norketamine.

EYQYPG + + Ketamine - Detected Norketamine - Detected

FAAKAX + + The coincidence between the relative retention time and mass -fragmentograms from a reference standard analysed at the same conditions that the biological sample, indicates the detection of Ketamine, Norketamine and Caffeine.

FJUGNL + ANP

FPKXPP + ANP Drug Result: Ketamine

FSYPJK + +

GGGGLA + +

GGGW8M + + Ketamine and Norketamine were identified in the sample.

GGHZVX - - no drugs found

GOUDX1 + +

HHJU84 - - Listed drugs could not be detected in sample 2019/2/BS-2.

HLV08P + + Sample 2019/2/BS-2 was found containing Ketamine and Norketamine

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Code Ketamine Norketamine

HNCPVB + ANP Consistent with use of Ketamine.

HPX5UF ANP ANP

HYMHGB + +

IKQDOZ + + positive

IVVPXY ANP ANP It was detected MDMA.

J0Q014 + + NORKETAMINE, CAFFEINE

JBCBBB + ANP Ketamine is detected in urine. Ketamine is a drug used for sedation and pain-relief and is used in anesthesia. Ketamine is also used as a recreational drug due to hallusinogenic effects.

JGWJYI + + Ketamine consumption

JHHAXC + + KETAMINE AND ITS METABOLITE NORKETAMINE

JVDIJJ + + In sample BS-2 the drugs ketamine and its metabolite norketamine were detected.

K15R1P - -

KFCL1O - -

KHHBSB + + Ketamine and norketamine was detected in the urnie sample considering LOD=25 ng/mL

KL7XB8 + + After chemical analysis was performed the sample contains Ketamine/Norketamine /caffeine

KWAGZD + ANP

L0ZAGA + + Norketamine and Ketamine were detected in sample 2019/2/BS-2.

LVFR11 + +

MMMLHE + +

MRELLV + ANP positive for ketamine

N0N0VK ANP + Sample 2019/2/BS-2 contain norketamine.

N4NRKA + + The presence of Ketamine and norketamine in the sample indicate consumption of ketamine.

NCHVCR + + recent intake of Ketamine

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Code Ketamine Norketamine

NHMXHX - ANP

NSUYMO + + In the sample was detected Ketamine and Norketamine, this finding indicates that Ketamine was consumed.

OLKLLL + + Positive to Ketamine and its metabolite Norketamine

PBRKVK + -

PEWPPB - -

PIPPUP + + kETA CONSUMPTION

PZKF1X + ANP

QCYPRL + + Ketamine is registered as a drug. It is a general anesthetic used for human or animal operations.Ketamine can cause a loss of feeling in the body and paralysis of the muscles. It can cause distorsion of reality. It is a dissociative anesthetic which can be diverted for recreational purposes or sometime used as a rape drug.Norketamine is the major active metabolite of ketamine

QDQIQG + + Sample positive for ketamine and norketamine

QNIWGB + +

QSJNNV + +

RNZXZZ + +

RREHHH + + -

S67HVA + + this person consumed ketamine

SS6REF + + In the 2019/2/BS-2 It was proved the presence of methylecgonine, ketamine and norketamine.

T5552F + +

TOVQID ANP ANP

U1LAJJ + + The laboratory identifed ketamine and norketamine in urine.

UDA9RR + - Ketamine

UFDUCR + + The Sample BS-2 was found to contain Ketamine and Norketamine

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Code Ketamine Norketamine

UW5SKG - + Norketamine was detected in BS-2 sample. Norketamine is a major active metabolite of Ketamine drug.

V2TTTI + ANP According to the cut off values established by the laboratory; Barbiturate 200 ng/ml, THC 50 ng/ml, Cocaine150 ng/ml, Benzodiacepine 200 ng/ml and Opiate 2000 ng/ml. None drug metabolite was detected. Amphetamin, hallucinogenic drugs and any other controlled drugs are not analyze by the laboratory.

VCNWXW + + Ketamine and Norketamine were detected in BS-2

VG8Y34 + + In the urine sample labeled BS-2/2/2019 Norketamine and ketamine were found

VLAS0P + + Sample 2019/2/BS-2 contains Ketamine and Norketamine

VVVMVL + +

WFEBOC + + IN BS-2 IT WAS DETECTED KETAMINE AND NORKETAMINE

WLNP5E + + Ketamine is a dissociative anesthetic and norketamine is its metabolite. Ketamine is a schedule III substances in the United States.

X4J6QG + + in the analyzed urine sample it was detected and confirmed the prensence of Ketamine, norketamine

XAL8XE - -

XN31XS + + Use of ketamine.

Y4BXDJ + +

YCBZMP ANP ANP Test sample 2019/2/BS-2 does not contain controlled drugs, therefore Negative for Screening and Confirmatory analyses.

YMCYXY ANP ANP

YMMZBM + - Analytical Adverse Finding for ketamine

YXARNC + + Ketamine and Norketamine was detected in BS-2 sample.

YXCAHN + + use of ketamine

YXYYWO ANP ANP The sample has negative results for : AMFETAMINE TYPE STIMULANTS, BARBITURATES, BENZODIAZEPINES, CANNABINOIDS COCAINE and/or METABOLITES, OPIATES/OPIOIDS. HALLUCINOGENIC DRUGS not performed. Z1X7PA + + The presence of ketamine and its metabolite norketamine indicates the intake of ketamine.

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Code Ketamine Norketamine

Z6ATVN ANP ANP NO HUBO CONSUMO DE DROGAS

ZO0USM + +

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Identification methods for Test Sample 2

Analytical Technique Codes

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

00EM0W S SI I

14X0XQ S SI I

181PAR S I I

1HO1NR S I

1IH7T1 SI

1WXG1M S I

2ZHQMZ S I

33GBDB S I

3AIJ73 S I

3YZ7RO S I

4MVDPF I

4QOCQS I SI I

6DFVYY S SI SI

700RJC SI

7BA2IC S I SI I

7KX1K4 SI S Q-TOF LC-MS

8T85GY S I

9X92FT I I

AR2BHL S I I I

BBBPDA S SI SI

BCKYTY S I I

BIQY5S S I I

CVDCCW I

CVDEWN S I

D07DV8 SI I

D9SYSS I SI

DUPOOO S I I

DZITOQ I I S chimical immunoassay techniques

EYQYPG S I I

FAAKAX I

FJUGNL I

FPKXPP SI

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

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ICE 2019/2-BS

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

FSYPJK S I

GGGGLA I I Triage 8, CUP Alere

GGGW8M I S Multi-Drug Test Panel(urine)

GGHZVX S I I

GOUDX1 S I I

HHJU84 S SI

HLV08P S I

HNCPVB S SI SI

HPX5UF S I

HYMHGB S I I

IKQDOZ I SI SFC-MS/MS

IVVPXY S I

J0Q014 S I I

JBCBBB SI I SI QTOF

JGWJYI S I

JHHAXC S I

JVDIJJ SI SI

K15R1P SI

KFCL1O I S

KHHBSB I S Immunoassay

KL7XB8 S I I

KWAGZD S I I

L0ZAGA SI

LVFR11 S I SI

MMMLHE SI

MRELLV S I

N0N0VK S I I I S Randox biochip technology,ketamines N4NRKA I I S lateral flow

NCHVCR S I SI LC-MS²

NHMXHX SI I I

NSUYMO I S Lateral Flow Inmunnoassay

OLKLLL S SI

PBRKVK I I S cobas analyzer

PEWPPB I I

PIPPUP SI

PZKF1X S I

QCYPRL S I I

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Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

QDQIQG I S Chromatographic immunoassay

QNIWGB S I I

QSJNNV S I

RNZXZZ S I

RREHHH SI

S67HVA S I I

SS6REF SI

T5552F I I I Kinetic Interactions of Microparticles

TOVQID S I

U1LAJJ S I I

UDA9RR I SI Dipro Drug lab screen

UFDUCR S I I

UW5SKG S I I

V2TTTI S I HPLC MS-MS

VCNWXW S SI

VG8Y34 I

VLAS0P I

VVVMVL S I I LC-HR-MS-ORBITRAP

WFEBOC S I

WLNP5E I LC-QTOF

X4J6QG SI SI I

XAL8XE I I I

XN31XS I I S

Y4BXDJ S I LC/QTOF

YCBZMP I S DTK

YMCYXY SI I

YMMZBM SI SI

YXARNC S I

YXCAHN I

YXYYWO S

Z1X7PA S I SI

Z6ATVN S I I S randox

ZO0USM SI S doa L MultiGnost

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12. ANNEX 3: Participants’ results for Test Sample-3

Identified substances for Test Sample 3

Code Identified Substances

00EM0W morphine

14X0XQ Morphine

181PAR Morphine

1HO1NR morphine

1IH7T1 None

1WXG1M Morphine

2ZHQMZ Morphine

3AIJ73 Morphine

3YZ7RO Morphine

4MVDPF Morphine

4QOCQS MORPHINE

700RJC Morphine

7BA2IC morphine

7KX1K4 Morphine

8T85GY Morphine

9L2893 morphine

9X92FT morphine

AR2BHL Morphine

BBBPDA Morphine

BCKYTY Morphine and Hydromorphone

BIQY5S Morphine

CVDEWN Morphine

D07DV8 Morphine

D9SYSS morphine

DUPOOO Morphine

DZITOQ Morphine (Total)

EYQYPG Morphine

FAAKAX Morphine

FJUGNL MORPHINE

FPKXPP Morphine

FSYPJK Morphine

GGGGLA MORPHINE

GGGW8M Morphine

GGHZVX Methadone

GOUDX1 Morphine

HHJU84 Morphine

HLV08P Morphine

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Code Identified Substances

HNCPVB Morphine

IKQDOZ morphine

IVVPXY Temazepam

J0Q014 MORPHINE

JBCBBB Morphine

JGWJYI Morphine

JHHAXC MORPHINE

JVDIJJ Morphine

K15R1P MORPHINE

KFCL1O Benzoylecgonine

KHHBSB Morphine

KL7XB8 Morphine

LVFR11 Morphine

MMMLHE MORPHINE

MRELLV Morphine

N0N0VK morphine

N4NRKA MORPHINE

NCHVCR Morphine

NHMXHX Morphine

NSUYMO Morphine

OLKLLL Morphine

PBRKVK Morphine

PEWPPB Morphine

PIPPUP morphine

PZKF1X morphine

QCYPRL Morphine

QDQIQG morphine (total)

QSJNNV Morphine

RNZXZZ Morphine

RREHHH Morphine (Total)

S67HVA morphine

SS6REF MDMA

T5552F Morphine

TOVQID Opiaceos, Morfina

U1LAJJ Morphine

UDA9RR Opiates

UW5SKG Morphine

V2TTTI None

VCNWXW Morphine

VG8Y34 Morphine

VLAS0P No common basic drugs was detected in sample BS-3.

VVVMVL MORPHINE

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ICE 2019/2-BS

Code Identified Substances

WFEBOC MORPHINE

WLNP5E Morphine

X4J6QG Morphine

XN31XS morphine

Y4BXDJ Morphine

YMCYXY opiates

YMMZBM Morphine

YXARNC Morphine

YXCAHN morphine

YXYYWO OPIATES

Z1X7PA Morphine

Z6ATVN MORFINA

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Statement of findings for Test Sample 3

Code Morphine (Total)

00EM0W + Presence of morphine

14X0XQ + Toxicological examination revealed the presence of Morphine

181PAR + We found Morphine as narcotic substance based on INCB Yellow List Regulation

1HO1NR +

1IH7T1 ANP Sample 2019/2/BS/3 found not to contain any drugs

1WXG1M + Morphine

2ZHQMZ +

33GBDB ANP After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) as screening thecnique and Gas Chromatography/Mass Spectrometry (GC/MS) as screening thecnique, were not detected drugs in the urine sample 2019/2/BS-3.

3AIJ73 + Morphine was identified by GC-MS

3YZ7RO + The Sample contains Morphine and Caffeine

4MVDPF + drug was detected

4QOCQS + MORPHINE

5U54R5 ANP

6DFVYY ANP

700RJC + The presence of morphine in urine confirms either a person is a morphine abuser or obtained from medication.

7BA2IC +

7KX1K4 + The sample contains morphine.

8T85GY + Positive for morphine

9L2893 ANP Only free morphine was measured

9X92FT +

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Code Morphine (Total)

AR2BHL ANP Morphine found.

BBBPDA + Morphine (total)

BCKYTY + Opiates were identified by Immunoassay, GC/MS and LC-MS/MS . Differential opiates as Morphine and Hydro-Morphone were identified by GC/MS and LC-MS/MS in sample number BS-3

BIQY5S + Morphine detected.

CVDCCW - Drug not detected

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

D07DV8 + Demonstrates non-recent ingestion of heroin/morphine. However given the low indicated level of total morphine, cannot rule out the prior ingestion of a poppy seed based food product.

D9SYSS + In the biological sample was identified: morphine and caffeine.

DUPOOO + Morphine was detected using GC/MS which indicate use of controlled drug

DZITOQ + the drug tha was fond is Morphine (Total) , confirmed by HPLC and GC/MS.

EYQYPG + Morphine, Total Detected > 0.5mg/L

FAAKAX + The coincidence between the relative retention time and mass -fragmentograms from a reference standard analysed at the same conditions that the biological sample, indicates the detection of Morphine and Caffeine.

FJUGNL +

FPKXPP + Drug Result: Morphine. Please note that the presence of morphine in urine may occur as a result of the consumption of poppy seed products, medications containing codeine and/or morphine, or illicit drugs.

FSYPJK +

GGGGLA +

GGGW8M + Morphine was identified in the sample.

GGHZVX - Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with Methadone

GOUDX1 +

HHJU84 + Morphine was detected in sample 2019/2/BS-3.

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Code Morphine (Total)

HLV08P + Sample 2019/2/BS-3 was found containing Morphine

HNCPVB + Consistent with use of Morphine and/or heroin.

HPX5UF ANP

HYMHGB +

IKQDOZ + positive

IVVPXY - It was detected Temazepam.

J0Q014 + CAFFEINE

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

JGWJYI + Morphine administration

JHHAXC +

JVDIJJ + In sample BS-3 the drug morphine was detected.

K15R1P +

KFCL1O -

KHHBSB + Morphine was detected in the urine sample considering LOD=25 ng/mL

KL7XB8 + After chemical analysis was performed the sample contains Morphine + Caffeine

KWAGZD +

L0ZAGA ANP No common drugs were detected in sample 2019/2/BS-3.

LVFR11 +

MMMLHE +

MRELLV + positive for morphine

N0N0VK + Sample 2019/2/BS-3 contain morphine.

N4NRKA + The presence of Morphine in the sample indicates consumption of the drug itself or another drug which metabolite is Morphine

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Code Morphine (Total)

NCHVCR + recent intake of Morphine

NHMXHX - This sample mostly contains morphine base total of 136 ng/L

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

OLKLLL + Positive to Morphine

PBRKVK +

PEWPPB +

PIPPUP + MORPHINE CONSUMPTION

PZKF1X +

QCYPRL + Morphine is a pain medication (analgesic effect) of the opiate family. Morphine is an alkaloid molecule extracted from opium. It acts directly on the central nervous system to decrease the feeling of pain

QDQIQG + sample positive for morphine

QNIWGB +

QSJNNV +

RNZXZZ +

RREHHH + -

S67HVA + this person consumed morphine

SS6REF - In the 2019/2/BS-3 It was proved the presence of 3,4-Methylenedioxymetamfetamine (MDMA)

T5552F +

TOVQID + Opiaceos positivo Morfina positivo

U1LAJJ + The laboratory identifed morphine in urine.

UDA9RR + Morphine, Morphine-3-O-glucuronide

UFDUCR ANP NO drugs were detected according to our screening panel

UW5SKG + Morphine was detected in BS-3 sample.

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Code Morphine (Total)

V2TTTI ANP According to the cut off values established by the laboratory; Barbiturate 200 ng/ml, THC 50 ng/ml, Cocaine150 ng/ml, Benzodiacepine 200 ng/ml and Opiate 2000 ng/ml. None drug metabolite was detected. Amphetamin, hallucinogenic drugs and any other controlled drugs are not analyze by the laboratory.

VCNWXW + Morphine was detected in BS-3

VG8Y34 + In the urine sample labeled BS-3/2/2019 morphine was found

VLAS0P ANP No common basic drugs was detected in sample BS-3.

VVVMVL +

WFEBOC + IN BS-3 IT WAS DETECTED MORPHINE

WLNP5E + Morphine is a narcotic analgesic found in the opium poppy. It is a schedule II substances in the United States.

X4J6QG + in the analyzed urine sample it was detected and confirmed the prensence of Morphine

XAL8XE -

XN31XS + Probable use of medcinal morphine.

Y4BXDJ +

YCBZMP ANP Test sample 2019/2/BS-3 does not contain controlled drugs, therefore Negative for Screening and Confirmatory analyses.

YMCYXY + MAM, morphine, Codeine

YMMZBM + Analytical Adverse Finding for morphine (Doping -> lower than the DL 1,3 µg/ml)).

YXARNC + Morphine was detected in BS-3 sample.

YXCAHN + use of morphine

YXYYWO ANP The sample has positive results for OPIATES. The Analytical Technique used is a semi-quatitative methode. A confirmatory test is requiered to identify and quantify the drug. The sample has negative results for : AMFETAMINE TYPE STIMULANTS, BARBITURATES, BENZODIAZEPINES, CANNABINOIDS COCAINE and/or METABOLITES. HALLUCINOGENIC DRUGS not performed. Z1X7PA + The presence of morphine indicates the intake of morphine or the past exposure to heroin.

Z6ATVN + HUBO CONSUMO DE MORFINA

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Code Morphine (Total)

ZO0USM +

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ICE 2019/2-BS

Identification methods for Test Sample 3

Analytical Technique Codes

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

00EM0W S SI I

14X0XQ S SI I

181PAR S I I

1HO1NR S I

1IH7T1 SI

1WXG1M S I

2ZHQMZ S I

33GBDB S I

3AIJ73 S I

3YZ7RO S I

4MVDPF I

4QOCQS I SI I

6DFVYY S SI SI

700RJC SI

7BA2IC S I SI I

7KX1K4 SI S Q-TOF LC-MS

8T85GY S I

9X92FT I I

AR2BHL S I I I

BBBPDA S SI SI

BCKYTY S I I

BIQY5S S I I

CVDCCW I

CVDEWN S I

D07DV8 SI I

D9SYSS I SI

DUPOOO S I I

DZITOQ I I S chimical immunoassay techniques

EYQYPG S I I

FAAKAX I

FJUGNL I

FPKXPP SI

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

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Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

FSYPJK S I

GGGGLA I I Triage 8, CUP Alere

GGGW8M I S Multi-Drug Test Panel(urine)

GGHZVX S I I

GOUDX1 S I I

HHJU84 S SI

HLV08P S I

HNCPVB S SI SI

HPX5UF S I

HYMHGB S I I

IKQDOZ I SI SFC-MS/MS

IVVPXY S I

J0Q014 S I I

JBCBBB SI I SI QTOF

JGWJYI S I

JHHAXC S I

JVDIJJ SI SI

K15R1P SI

KFCL1O I S

KHHBSB I S Immunoassay

KL7XB8 S I I

KWAGZD S I I

L0ZAGA SI

LVFR11 S I SI

MMMLHE SI

MRELLV S I

N0N0VK S I I I S Randox biochip technology,ketamines N4NRKA I I S lateral flow

NCHVCR S I SI LC-MS²

NHMXHX SI I I

NSUYMO I S Lateral Flow Inmunnoassay

OLKLLL S SI

PBRKVK I I S cobas analyzer

PEWPPB I I

PIPPUP SI

PZKF1X S I

QCYPRL S I I

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Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

QDQIQG I S Chromatographic immunoassay

QNIWGB S I I

QSJNNV S I

RNZXZZ S I

RREHHH SI

S67HVA S I I

SS6REF SI

T5552F I I I Kinetic Interactions of Microparticles

TOVQID S I

U1LAJJ S I I

UDA9RR I SI Dipro Drug lab screen

UFDUCR S I I

UW5SKG S I I

V2TTTI S I HPLC MS-MS

VCNWXW S SI

VG8Y34 I

VLAS0P I

VVVMVL S I I LC-HR-MS-ORBITRAP

WFEBOC S I

WLNP5E I LC-QTOF

X4J6QG SI SI I

XAL8XE I I I

XN31XS I I S

Y4BXDJ S I LC/QTOF

YCBZMP I S DTK

YMCYXY SI I

YMMZBM SI SI

YXARNC S I

YXCAHN I

YXYYWO S

Z1X7PA S I SI

Z6ATVN S I I S randox

ZO0USM SI S doa L MultiGnost

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13. ANNEX 4: Participants’ results for Test Sample-4

Identified substances for Test Sample 4

Code Identified Substances

00EM0W temazepam

14X0XQ Temazepam

181PAR Temazepam

1IH7T1 None

1WXG1M Temazepam

2ZHQMZ Temazepam, diazepam, acetaminophen

33GBDB Temazepam

3AIJ73 Temazepam

3YZ7RO Temazepam

4MVDPF Temazepam

4QOCQS TEMAZEPAM

6DFVYY TEMAZEPAM

700RJC Temazepam

7BA2IC temazepam

7KX1K4 Temazepam

8T85GY Temazepam

9L2893 temazepam

9X92FT temazepam

AR2BHL Temazepam

BBBPDA Temazepam

BCKYTY Temazepam and trace Diazepam

BIQY5S Temazepam

CVDCCW Temazepam

CVDEWN Temazepan

D07DV8 Temazepam

D9SYSS temazepam

DUPOOO Temazepam

DZITOQ Temazepam

EYQYPG Temazepam, Paracetamol

FAAKAX Temazapam

FPKXPP Temazepam

FSYPJK Temazepam

GGGGLA TEMAZEPAM

GGGW8M Temazepam

GGHZVX Nordazepam

GOUDX1 Temazepam

HHJU84 Temazepam

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Code Identified Substances

HLV08P Temazepam

HNCPVB Temazepam

IKQDOZ temazepam

J0Q014 DIAZEPAM

JBCBBB Temazepam

JGWJYI Temazepam

JHHAXC TEMAZEPAM

JVDIJJ Temazepam

K15R1P BENZODIAZEPINES

KFCL1O benzoylecgonine

KHHBSB Temazepam

KL7XB8 Temazepam

L0ZAGA Temazepam

LVFR11 temazepam

MMMLHE TEMAZEPAM

MRELLV Temazepan

N0N0VK nordazepam

N4NRKA TEMAZEPAM

NCHVCR Temazepam

OLKLLL Temazepam

PBRKVK temazepam

PEWPPB Nordazepam

PIPPUP temazepam

PZKF1X oxazepam

QCYPRL Temazepam

QDQIQG temazepam

QSJNNV Temazepam

RNZXZZ Temazepam

RREHHH Temazepam

S67HVA temazepam

T5552F Temazepam

TOVQID Benzodiacepinas (Zolpidem)

U1LAJJ Temazepam

UDA9RR Benzodiazepines

UFDUCR Benzodiazepines

UW5SKG Temazepam

V2TTTI Benzodiacepine

VCNWXW Temazepam

VG8Y34 Temazepam

VLAS0P Temazepam

VVVMVL TEMAZEPAM

WFEBOC TEMAZEPAM

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Code Identified Substances

WLNP5E Methamphetamine and Temazepam

X4J6QG Temazepam

XN31XS temazepam

Y4BXDJ Temazepam

YMCYXY benzodiazepines

YMMZBM Temazepam

YXARNC Temazepam

YXCAHN temazepam

YXYYWO BENZODIAZEPINES

Z1X7PA temazepam

Z6ATVN TEMAZEPAM

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Statement of findings for Test Sample 4

Code Temazepam

00EM0W + Presence of temezepam

14X0XQ + Toxicological examination revealed the presence of Temazepam

181PAR + we found Temazepam as psychotropic substance based on INCB Green List Regulation

1HO1NR ANP

1IH7T1 ANP Sample 2019/2/BS/4 found not to contain any drugs

1WXG1M + Temazepam

2ZHQMZ +

33GBDB + After completing the toxicological analyzes of the sample, using the Enzyme Immunoassay Techiques (EIA) as screening thecnique and Gas Chromatography/Mass Spectrometry (GC/MS) as confirmation thecnique, was detected substance Temazepam in the urine sample 2019/2/BS-4.

3AIJ73 + Temazepam was identified by GC-MS

3YZ7RO + The sample contains Temazepam and Caffeine

4MVDPF + drug was detected

4QOCQS + TEMAZEPAM

5U54R5 ANP

6DFVYY + Screening 161Tech

700RJC + The presence of Temazepam in urine revealed that urine come from Diazepam user.

7BA2IC + sample contains also paracetamol

7KX1K4 + The sample contains temazepam.

8T85GY + Positive for benzodiazepine

9L2893 ANP

9X92FT +

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Code Temazepam

AR2BHL + Temazepam found

BBBPDA + Temazepam

BCKYTY + Benzodiazepines as a class were identified in sample BS-4 by immunoassay . GC/MS confirmed the benzodiazepine type in the sample to be Temazepam. LC-MS/MS identified the benzodiazepine type as Temazepam as well with trace amounts of Diazepam

BIQY5S + Temazepam detected.

CVDCCW + Temazepam detected

CVDEWN + It was detected the presence of Temazepan in the sample analysed.

D07DV8 + Demonstrates the prior ingestion of temazepam

D9SYSS + In the biological sample was identified: temazepam, paracetamol and caffeine. Temazepam belongs to a class of drugs called benzodiazepines

DUPOOO + Temazepam was detected using LC/MS/MS which indicate use of controlled drug

DZITOQ + the drug tha was fond is Temazepam, confirmed by HPLC and GC/MS.

EYQYPG + Temazepam ~0.8mg/L Paracetamol Detected

FAAKAX + The coincidence between the relative retention time and mass -fragmentograms from a reference standard analysed at the same conditions that the biological sample, indicates the detection of Temazepam and Caffeine.

FJUGNL ANP

FPKXPP + Drug result: Temazepam. Indicative of benzodiazepine consumption.

FSYPJK +

GGGGLA +

GGGW8M + Temazepam was identified in the sample

GGHZVX - Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with Nordazepam

GOUDX1 +

HHJU84 + Temazepam was detected in sample 2019/2/BS-4.

HLV08P + Sample 2019/2/BS-4 was found containing Temazepam

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Code Temazepam

HNCPVB + Consistent with use of Temazepam.

HPX5UF ANP

HYMHGB +

IKQDOZ + positive

IVVPXY + Not detected.

J0Q014 + TEMAZEPAM, CAFFEINE, ACETOMINOPHEN

JBCBBB + Temazepam is detected in urine. Temazepam is a metabolite of diazepam and can be explained by intake of diazepam, or an intake of temazepam as an individual drug can not be ruled out.

JGWJYI + Temazepam admnistration

JHHAXC +

JVDIJJ + In sample BS-4 the drug temazepam was detected.

K15R1P +

KFCL1O -

KHHBSB + Temazepam was detected in the urine sample considering LOD=25 ng/mL

KL7XB8 + After chemical analysis was performed the sample contains Temazepam + Caffeine + acetaminophen

KWAGZD +

L0ZAGA + Temazepam was detected in sample 2019/2/BS-4.

LVFR11 +

MMMLHE +

MRELLV + positive for temazepan

N0N0VK ANP Sample 2019/2/BS-4 contain nordazepam.

N4NRKA + The presence of Temazepam in the sample indicates consumption of the drug itself or another drug which metabolite is Temazepam

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Code Temazepam

NCHVCR + intake of Temazepam or other Benzodiazepines metabolized to Temazepam

NHMXHX -

NSUYMO ANP

OLKLLL + Positivo to Temazepam

PBRKVK +

PEWPPB -

PIPPUP + TEMAZEPAM CONSUMPTION

PZKF1X ANP

QCYPRL + Temazepam is a benzodiazepine used for its hypnotics properties in case of insomnia. It is no longer sold in France as a drug but is one of the metabolite of diazepam, another benzodiazepine drug (anxiolytic).

QDQIQG + sample positive for temazepam

QNIWGB +

QSJNNV +

RNZXZZ +

RREHHH + -

S67HVA + this person consumed temazepam

SS6REF -

T5552F +

TOVQID ANP Zolpidem positivo

U1LAJJ + The laboratory identifed temazepam in urine.

UDA9RR + Temazepam

UFDUCR ANP The Sample BS-4 was Screened Positive for Benzodiazepines

UW5SKG + Temazepam was detected in BS-4 sample.

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Code Temazepam

V2TTTI ANP By utilizing EIA it was detected Benzodiazepine, only identifying the functional group. Without detecting which benzodiazepine belongs to.

VCNWXW + Urine in Item # BS-4 contains 752 ng/mL Temazepam

VG8Y34 + In the urine sample labeled BS-4/2/2019 temazepam was found

VLAS0P + Sample 2019/2/BS-4 contains Temazepam.

VVVMVL +

WFEBOC + IN BS-4 IT WAS DETECTED TEMAZEPAM

WLNP5E + Methamphetamine is a stimulant. Temazepam is a benzodiazepine and also a metabolite of diazepam. Methamphetamine is a schedule II substance and Temazepam is a schedule IV substance in the United States.

X4J6QG + in the analyzed urine sample it was detected and confirmed the prensence of Temazepam

XAL8XE -

XN31XS + Use of temazepam.

Y4BXDJ +

YCBZMP ANP Test sample 2019/2/BS-4 does not contain controlled drugs, therefore Negative for Screening and Confirmatory analyses.

YMCYXY + nordiazepam

YMMZBM + Analytical Adverse Finding for temazepam (+ diazepam)

YXARNC + Temazepam was detected in BS-4 sample.

YXCAHN + use of temazepam

YXYYWO ANP The sample has positive results for BENZODIAZEPINES. A confirmatory test is requiered to identify and quantify the drug. The sample has negative results for : AMFETAMINE TYPE STIMULANTS, BARBITURATES, CANNABINOIDS COCAINE and/or METABOLITES, OPIATES/OPIOIDS. HALLUCINOGENIC DRUGS not performed. Z1X7PA + The presence of temazepam indicates the intake of temazepam.or is a metabolite of diazepam, although other metabolites should also be present.

Z6ATVN + HUBO CONSUMO DE BENZODIAZEPINAS

ZO0USM +

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Identification methods for Test Sample 4

Analytical Technique Codes

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

00EM0W S SI I

14X0XQ S SI I

181PAR S I I

1HO1NR S I

1IH7T1 SI

1WXG1M S I

2ZHQMZ S I

33GBDB S I

3AIJ73 S I

3YZ7RO S I

4MVDPF I

4QOCQS I SI I

6DFVYY S SI SI

700RJC SI

7BA2IC S I SI I

7KX1K4 SI S Q-TOF LC-MS

8T85GY S I

9X92FT I I

AR2BHL S I I I

BBBPDA S SI SI

BCKYTY S I I

BIQY5S S I I

CVDCCW I

CVDEWN S I

D07DV8 SI I

D9SYSS I SI

DUPOOO S I I

DZITOQ I I S chimical immunoassay techniques

EYQYPG S I I

FAAKAX I

FJUGNL I

FPKXPP SI

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

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Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

FSYPJK S I

GGGGLA I I Triage 8, CUP Alere

GGGW8M I S Multi-Drug Test Panel(urine)

GGHZVX S I I

GOUDX1 S I I

HHJU84 S SI

HLV08P S I

HNCPVB S SI SI

HPX5UF S I

HYMHGB S I I

IKQDOZ I SI SFC-MS/MS

IVVPXY S I

J0Q014 S I I

JBCBBB SI I SI QTOF

JGWJYI S I

JHHAXC S I

JVDIJJ SI SI

K15R1P SI

KFCL1O I S

KHHBSB I S Immunoassay

KL7XB8 S I I

KWAGZD S I I

L0ZAGA SI

LVFR11 S I SI

MMMLHE SI

MRELLV S I

N0N0VK S I I I S Randox biochip technology,ketamines N4NRKA I I S lateral flow

NCHVCR S I SI LC-MS²

NHMXHX SI I I

NSUYMO I S Lateral Flow Inmunnoassay

OLKLLL S SI

PBRKVK I I S cobas analyzer

PEWPPB I I

PIPPUP SI

PZKF1X S I

QCYPRL S I I

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ICE 2019/2-BS

Code 100 110 120 130 140 150 161 170 172 180 190 230 231 210

QDQIQG I S Chromatographic immunoassay

QNIWGB S I I

QSJNNV S I

RNZXZZ S I

RREHHH SI

S67HVA S I I

SS6REF SI

T5552F I I I Kinetic Interactions of Microparticles

TOVQID S I

U1LAJJ S I I

UDA9RR I SI Dipro Drug lab screen

UFDUCR S I I

UW5SKG S I I

V2TTTI S I HPLC MS-MS

VCNWXW S SI

VG8Y34 I

VLAS0P I

VVVMVL S I I LC-HR-MS-ORBITRAP

WFEBOC S I

WLNP5E I LC-QTOF

X4J6QG SI SI I

XAL8XE I I I

XN31XS I I S

Y4BXDJ S I LC/QTOF

YCBZMP I S DTK

YMCYXY SI I

YMMZBM SI SI

YXARNC S I

YXCAHN I

YXYYWO S

Z1X7PA S I SI

Z6ATVN S I I S randox

ZO0USM SI S doa L MultiGnost

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