INTERNATIONALCOLLABORATIVE EXERCISES

Drug Analysis2012

ICE

Ro

unds

201

1/2

and

2012

/1

Figure 1: Member States participating in the International Collaborative Exercises programme in 2011/2 and 2012/1. Note, the boundaries, names and delegations used do not imply official endorsement or acceptance by the United Nations. This document has not been formally edited.

Introduction

An important part of the UNODC International Quality Assur-ance Programme (IQAP) is the implementation of the Inter-national Collaborative Exercises (ICE). Participation in such exercises, inter-laboratory comparisons or proficiency tests is one of the essential elements for the implementation of a laboratory quality management system and ultimately ac-creditation. This is recognised by the International Organi-zation for Standardization in ISO/IEC 17025-2005: “General requirements for the competence of testing and calibration laboratories” as contributing to assuring the quality of test results.

The UNODC ICE programme allows drug testing laboratories from both developing and developed countries to continu-ously monitor their performance on a global scale. The op-tions available for participation are in the analysis of drugs in Seized Materials (SM) and in Biological Specimens (BS, spe-cifically urine). Two rounds are offered per year with each round presenting participants with four different test sam-ples for analysis in each test group.

Laboratories participating in the ICE programme can use an on-line portal for direct submission of results to UNODC. This enables participants to receive immediate confidential feed-back from UNODC on their performance and greatly facilli-tates the implementation of the programme. During the ICE rounds 2011/2 and 2012/1, the portal was used for submis-sion of results by 97% of laboratories in both the SM and BS test groups. This almost universal usage of the ICE portal by participants continues to be a high endorsement of its utility.

Upon completion of each ICE round, the analytical results are evaluated by UNODC and an International Panel of Forensic Experts which oversees the implementation of ICE and offers guidance and support in addressing relevant quality issues.

Following evaluation, summary reports of the performance

Figure 2: Laboratories actively participating in the ICE programme since 2010. 1 Data from January 2013.

of participating laboratories in both the SM and BS test groups are made available to participants through the ICE portal and the UNODC website. These summary reports al-low participants to evaluate their performance while main-taining confidentiality.

Participation

For the 2011/2 round of the ICE programme, 125 laborato-ries in 51 Member States submitted results. For the 2012/1 round, participation had increased to 140 laboratories in 53 Member States, representing a 12% increase in participation within the year.1 Figure 2 shows the participation of laborato-ries in the SM and BS test groups for all ICE rounds from 2010 up to the most recent 2012/1 round of the programme.

It is recognised that some participants continue to have difficulty with obtaining import authorization for the SM test samples and the reference samples for the SM and BS groups. This, in combination with some unforeseen delays with shipping the test samples to the laboratories, contrib-

85

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93

37

102

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115

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60

80

100

120

num

ber

of p

arti

cipa

nts

2010/1 2010/2 2011/1 2011/2 2012/1

ICE round

SM BS

Table 1: Composition of SM test samples, performance of participants and number of false positive and false negative results in ICE 2011/2 and 2012/1.

Test

Sam

ple

Cont

ents

(%

pur

ity)

Med

ian

Valu

e R

epor

ted

(%)

Corr

ect

Iden

tific

ation

(%)

Num

ber

of

Fals

e Po

siti

ves

Num

ber

of

Fals

e N

egati

ves

2011/2 SM-1 Cocaine (6.9) 7.0 98 0 1

2011/2 SM-2 Blank - - 0 -

2011/2 SM-3 Amfetamine (5.5) 5.6 93 2 6

2011/2 SM-4 Ketamine (4.7) 5.2 93 2 3

2012/1 SM-1 Amfetamine (25.3) 25 95 1 3

2012/1 SM-2 MDEA (81.0) 84.0 95 5 5

2012/1 SM-3 Cocaine (86.3) 90.1 100 1 0

2012/1 SM-4 Heroin (74.7) 76.1 98 11 1

Test

Sam

ple

Cont

ents

(n

g/m

l)

M

edia

n Va

lue

Repo

rted

(n

g/m

l)

Corr

ect

Iden

tific

ation

(%)

Num

ber

of

Fals

e Po

siti

ves

Num

ber

of

Fals

e N

egati

ves

2011/2 BS-1 Blank - - 3 -

2011/2 BS-2 Caffeine (11,510) 11,550 - 2 -

2011/2 BS-3 Methadone (2,300) 2,374 91 2 2

2011/2 BS-4 Metamfetamine (1,150) 1,060 91 2 3

2012/1 BS-1 Metamfetamine (1,720) 1,607 90 5 4

2012/1 BS-2 MDA (1,150) 1,139 71 5 11

2012/1 BS-2 MDMA (1,720) 1,658 90 5 4

2012/1 BS-3 Ketamine (1,380) 1,304 77 4 6

2012/1 BS-4 Nordazepam (2,300) 1,900

88 0 6

uted to delays in the submission of results from a small num-ber of laboratories. However it should be noted that easing of import requirements in a number of Member States has played a significant role in the increased participation within the programme during 2012. The increased participation in 2012/1 is also a result of focused quality assuance support through the Afghanistan and neighbouring countries regional programme as well as the increased recognition globally of the benefits of the ICE programme.

Test samples

Participating laboratories are requested to analyse four test samples in the SM group and/or four test samples in the BS group for the substances listed in the ICE menu. This menu covers the controlled substances and adulterants most com-monly encountered in drug seizures. The ICE menu for the BS test group covers common drugs of abuse, their metabolites and related compounds.

The test samples within the SM group are prepared in the Laboratory and Scientific Section of UNODC using donations of seized materials from Member States, while the BS test samples are prepared using controlled substances, their me-tabolites and related compounds in lyophilized urine. The composition of the test samples are designed to simulate ac-tual casework encountered by forensic laboratories.

Laboratories are asked to analyse the test samples using the screening and confirmatory tests they employ routinely in casework. These may range from simple techniques such as colour tests and Thin Layer Chromatography (TLC) to more advanced methods such as Gas Chromatography-Mass Spec-trometry (GC-MS). By recording the techniques they use, the laboratories are able to assess their performance against that of other laboratories of similar capabilities and to identify any limitations of their performance compared with that of dif-ferently equipped laboratories. Indeed, the ICE programme is specifically designed as such to enable participation of labo-ratories with differing capacities. Participants are requested to identify the substances in the test samples and in addition, are encouraged to report the purity or concentrations of the controlled drugs present in the test samples.

ICE results

Qualitative analysis

The data in Table 1 shows the composition of the SM test samples in rounds 2011/2 and 2012/1 and gives the percent-age of laboratories that correctly identified each test sample and the numbers of false positive and false negative results reported for controlled substances. Overall, the results for qualitative analysis within the SM test group in both rounds were very good, with 93% and above of laboratories correctly identifying the controlled substances in each round.

The number of false positive and false negative results re-ported through 2011/2 and 2012/1 was low in most test samples. Laboratories who do report false positive or nega-tive results should investigate the reasons for this and correc-tive actions should be taken in order to continuously improve performance.

The qualitative performance of laboratories in the BS test groups in 2011/2 and 2012/1 are shown in Table 2. Within the BS test group, the results were also good in both rounds (71% and above of participants correctly identified the drugs pres-ent), given the inherently higher level of difficulty in the analy-sis of the low concentrations of drugs in biological specimens and the complexity of the matrix. The relatively high number of false negative results for 2012/1 BS-2 could be attributed to the complexity of this test sample containing both MDMA as well as MDA.

Table 2: Composition of BS test samples, performance of participants and number of false positive and false negative results in ICE 2011/2 and 2012/1.

Table 3: Complete list of z-scores for participating laboratories (with their lab code) within the BS test group in 2011/2 and 2012/1. Asterisks indicate that quantification was not performed or that the laboratory did not participate in that particular round of ICE. Table 4: Complete list of z-scores for participating laboratories (with their

lab code) within the SM test group in 2011/2 and 2012/1. Asterisks indi-cate that quantification was not performed or that the laboratory did not participate in that particular round of ICE.

2 B. Iglewicz, and D. Hoaglin, How to detect and handle outliers, American Society for Quality Control, 1993, volume 16

Quantitative analysis

Tables 1 and 2 also give details of the percentage composition of each test sample and the median value reported by par-ticipants who performed quantification. The percentage of laboratories who quantified at least one of the test samples in the BS test group was 46% and within the SM test group this value was 73% during the ICE rounds 2011/2 and 2012/1.

It should be noted that quantification is not compulsory within the ICE programme, though laboratories who do so are encouraged to quantify all test samples (depending on jurisdictional requirements) in order to get a better measure of their performance over time.

Within the ICE programme, the deviation of the individual re-sults from the assigned purity of a test sample are measured by a statistical parameter called the modified z-score. This approach uses the median value of all the reported results as the assigned value, and is relatively insensitive to the con-tribution from outliers.

Modified z-scores with an absolute value less than or equal to 3.5 are considered acceptable and those greater than 3.5 should be considered as outliers.2 Laboratories whose results are classified as outliers should investigate the cause and take appropriate corrective action, with support from UNODC if required.

A comprehensive list of the performance of all laboratories that performed quantitative analysis during ICE 2011/2 and 2012/1 is given in Tables 3 and 4.

ICE 2011/2 ICE 2012/1BS-3 BS-4 BS-1 BS-2 BS-3 BS-4

lab

code

Met

hado

ne

Met

amfe

tam

ine

Met

amfe

tam

ine

MD

MA

MD

A

Keta

min

e

Nor

daze

pam

110 * * 5.3 3.4 1.2 1.5 1.0321 2.6 0.6 0.7 0.2 0.3 0.6 1.4328 3.4 1.7 1.0 0.9 0.3 0.3 0.5330 1.5 0.5 0.4 2.4 1.4 0.9 0.7332 * 1.0 * * * * *348 0.1 0.5 4.5 0.7 0.4 * 0.1510 0.1 1.1 0.5 0.2 0.2 0.2 0.9529 0.7 0.8 0.7 0.3 0.7 0.4 0.1703 0.4 0.4 1.6 2.1 1.6 0.3 0.3751 0.1 0.8 0.0 0.7 1.2 0.6 0.0754 0.3 0.7 1.0 0.4 0.6 * 0.1761 * 0.7 0.0 0.0 0.2 0.2 *

8329 2.0 0.1 3.0 0.5 0.9 5.3 0.78369 0.0 0.1 1.3 0.7 0.3 * *8392 1.6 0.7 0.7 0.1 0.7 1.8 1.48396 0.5 0.8 0.1 0.5 0.3 1.6 0.98555 1.2 0.4 0.7 1.1 0.0 0.8 0.39193 0.1 0.9 0.1 22.4 6.6 4.4 0.69582 0.9 * * * * * *

11224 * * 2.1 2.1 1.8 1.1 2.311657 * 0.7 0.3 0.0 * * 0.111899 8.8 2.3 5.6 7.9 8.7 7.0 4.312563 0.1 0.3 2.7 2.6 * 0.2 0.8

ICE 2011/2 ICE 2012/1SM-1 SM-3 SM-4 SM-1 SM-2 SM-3 SM-4

lab

code

Coca

ine

Am

feta

min

e

Keta

min

e

Am

feta

min

e

MD

EA

Coca

ine

Her

oin

101 0.7 1.1 * 0.5 * 0.7 0.2104 0.0 * * * 0.0 0.5 0.2108 0.5 * 0.3 * * * *110 0.8 0.2 1.0 8.7 0.5 1.1 0.4113 6.8 0.6 0.7 0.4 0.3 0.4 0.5139 0.1 * * * * 0.6 0.4140 0.5 0.0 * 8.8 0.8 1.7 7.4141 0.3 0.1 0.4 0.5 0.2 0.1 0.1149 0.0 0.8 1.4 0.0 0.2 0.2 1.3151 * * * 0.5 0.2 0.7 0.2152 * * * 0.5 0.2 1.4 0.7157 0.0 0.3 * 1.7 * 0.8 0.2158 0.4 4.3 3.5 6.8 11.0 0.2 0.9161 4.1 * * * * 2.9 *179 2.6 * * * * * *181 0.2 0.1 0.5 0.9 0.5 0.3186 0.2 0.4 0.8 2.7 0.6 0.4 2.4187 6.2 10.4 5.7 13.5 0.3 2.0 0.1188 1.4 2.2 0.7 4.6 0.9 0.4202 * * * * * 1.6 *204 * * * 0.7 * 1.5 1.1211 0.0 0.8 1.4 0.0 1.2 1.6 0.2212 * * * 0.0 0.3 0.4 0.2215 0.0 0.8 * 0.0 0.6 0.0 0.7506 * * * 0.0 0.8 0.6 1.1510 * * * 8.1 8.9 3.6 1.3515 2.8 1.2 0.3 2.1 0.2 0.6 0.0517 7.0 0.0 0.1 * * * *518 1.9 5.5 2.4 7.3 10.3 18.5 2.4521 18.1 0.2 0.5 1.0 9.1 1.0 0.1522 * * * * * 19.7 16.5524 0.1 0.5 0.6 * * * *527 * * * 0.5 7.7 1.6 1.2529 0.0 0.8 0.8 3.6 1.9 0.1 1.6533 0.8 * * * * 0.4 1.9560 0.3 0.8 0.3 * * * *701 0.7 1.2 0.6 * * * *703 0.1 0.1 2.2 0.2 * 0.3 1.1713 1.1 0.1 0.7 0.1 1.1 0.7 0.1714 0.3 * 0.4 * 0.1 0.3 0.5754 1.2 0.1 0.1 0.0 0.1 0.3 2.5

8100 0.1 0.3 1.0 0.6 0.3 1.0 0.88120 2.7 * * * * 2.0 *8122 1.2 1.5 2.9 6.1 0.3 0.2 2.28123 0.3 0.1 0.8 1.4 0.5 0.6 0.08221 1.2 0.1 * 1.0 0.5 1.6 5.08222 0.0 0.5 0.2 0.0 0.9 1.1 1.58223 0.0 0.5 * 0.0 0.9 0.5 0.78224 0.0 0.8 * 0.7 0.9 1.1 0.08227 0.7 1.9 1.8 0.0 0.9 0.2 0.78292 0.0 * * * * 0.8 0.48555 0.9 4.6 * 1.0 * * 0.99155 * * * * * 1.6 3.59174 4.1 * * * * * *9175 0.7 * * 0.3 0.1 0.0 0.29177 1.6 0.3 57.5 0.5 0.7 0.7 0.39178 0.0 * * * * * *9193 1.1 19.1 0.7 * * * *9194 1.4 0.8 * 1.4 * 0.5 2.69249 1.3 9.1 0.2 * * * *9251 0.6 0.9 * 2.8 1.1 0.3 2.19282 0.1 0.3 4.1 * * * *9563 * 3.4 * * * *9564 0.3 * 0.6 * * * 0.39579 * * * * * 1.8 3.4

10232 1.0 0.0 0.2 * * * *10242 0.3 0.7 0.2 0.9 0.1 0.2 0.710252 0.4 0.7 8.7 0.1 * 0.1 0.110262 0.7 1.6 0.1 2.8 0.9 3.0 1.310267 0.4 1.3 0.8 * * * *10282 1.4 0.8 1.1 4.2 0.1 1.6 0.210297 1.2 1.1 1.3 4.1 0.6 0.4 1.210411 0.1 1.1 * 0.0 0.1 1.0 0.510413 * * * 3.7 3.9 0.2 0.510466 7.1 0.3 0.1 2.5 0.3 0.1 2.410497 8.1 * * * * * *10531 0.4 * 75.2 0.5 3.2 7.6 3.010551 1.9 1.7 0.2 0.2 3.2 1.4 2.510581 0.9 3.1 0.7 5.5 1.4 1.7 1.911159 0.2 0.2 0.3 * * * *11224 * * * 14.9 3.4 7.1 15.911474 0.7 0.7 0.4 0.3 1.6 1.6 0.411544 0.7 0.4 0.1 * * *11635 0.4 0.0 0.1 0.2 1.9 0.6 0.011662 1.3 7.6 * * * * *11723 0.8 1.2 1.3 7.3 1.7 1.6 4.311887 7.0 3.8 6.4 1.5 2.1 0.3 0.111899 0.7 0.5 0.6 0.0 0.0 0.2 0.911915 0.0 0.5 0.4 0.7 0.0 0.4 0.212176 * * * 1.2 0.3 2.0 0.812252 * * * * * 0.7 *12288 * * * 0.3 * 0.6 2.212323 * * * * 11.1 16.1 11.612366 * * * * * 1.5 2.512456 * * * 2.5 2.7 0.6 0.612481 * * * 4.4 0.4 0.2 1.012563 1.5 2.2 0.4 1.1 0.5 0.2 0.412611 * * * * * * 3.912662 * * * 7.0 3.4 1.2 0.912791 * * * 0.3 0.4 0.9 0.612913 * * * * * 0.1 *

Figure 5: New psychoactive substances reported by participating laboratories using the portal for the ICE rounds in 2011 and 2012.

Figure 4: Modified Z-score plot for ICE 2012/1, BS-1 (1720ng/ml Metamfet-amine). Each Bar represent the z-score of a laboratory who performed quan-titation and the line indicates the level below which z-scores are considered acceptable.

Figure 3: Modified Z-score plot for ICE 2012/1 SM-4 (74.7% Heroin). Each Bar represents the z-score of a laboratory who performed quantitation and the line indicates the level below which z-scores are considered acceptable.

This information enables laboratories to compare their indi-vidual quantitative performance with all other participants. Z-score plots are also provided to all participants in the summary report after each ICE round. Typical plots for ICE 2012/1 SM-4 (74.7% Heroin) and 2012/1 BS-1 (1720ng/ml Metamfetamine) are shown in Figures 3 and 4 respectively. The lines indicated (at Z = 3.5) show that the overwhelm-ing majority of participants who performed quantita-tion, in both the SM example (Figure 3) and the BS exam-ple (Figure 4), provided results with acceptable Z-scores.

New Emerging drugs

As well as facilitating the submission of test results, the ICE portal can also be used by participants to report emerging drug trends. This allows UNODC to compile important infor-mation on new drugs, in particular new psychoactive sub-stances that have recently appeared in seizures around the world. The new drugs reported through the ICE portal can be classified into five main groups, namely, synthetic cannabi-noids, cathinones, phenethylamines, piperazines, and trypt-amines. Substances not easily classified were grouped to-gether as miscellaneous. The number of observations of each group during 2011-2012 are shown in Figure 5.

UNODC would like to thank ICE participants for reporting their data on emerging substances. The information was used as part of a comprehensive survey with Member States on new psychoactive substances and a report on their global emer-gence will be presented at the 56th Session of the Commis-sion on Narcotic Drugs in March 2013.

The facility to report new emerging substances using the ICE portal will also form the basis for the creation of a UNODC early warning advisory currently under development in col-laboration with the UNODC Global SMART programme. The advisory, will allow Member States to report new substances, and search globally for where substances have emerged. The advisory will also provide resources where Member States can find information such as methods of analysis and refer-ence data for new psychoactive substances.

Acknowledgments

This report was produced by UNODC Laboratory and Scientific Section (LSS) under the supervision of Dr. Justice Tettey. The contributions of the UNODC International Panel of Forensic Experts (Drs Pirjo Lillsunde, Angeline Yap Tiong Whei and Mr. Marvin Salas), Dr. Iphigenia Naidis and the core ICE team (Dr. Conor Crean, Mr Antony Madhavapallil, Dr. Mee-Jung Park and Ms. Fernanda Rossi Iriondo) are gratefully acknowledged.

UNODC would like to acknowledge the financial and/or mate-rial support from the Governments of Canada, Denmark, Fin-land, Japan, Pakistan, and the United Kingdom to the UNODC drug analysis laboratory.

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2010-2 2011-1 2011-2 2012-1cathinones synthetic cannabinoids tryptaminesphenethylamines piperazines miscellaneous

Additional informationIf you have comments or questions related to this report, please e-mail us at UNODC-ICE@unodc.org or Lab@unodc.org. Additional information on the ICE programme and other UNODC Laboratory and Scientific Section programmes can be found via the internet at www.unodc.org, or by writing to UNODC at the Vienna International Centre, P.O. Box 500, A-1400 Vienna, Austria. Tel.: (+43-1) 26060-0, Fax: (+43-1) 26060-5866. February 2013