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International Collaborative Exercises (Ice) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report BIOLOGICAL SPECIMENS 2013/2 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 Codes and Abbreviations Page 4 Sample 1 Analysis Page 5 Identified substances Page 5 Statement of findings Page 6 Identification methods Page 10 Summary Page 12 Z-Scores Page 13 Sample 2 Analysis Page 15 Identified substances Page 15 Statement of findings Page 16 Identification methods Page 20 Summary Page 22 Z-Scores Page 23 Sample 3 Analysis Page 25 Identified substances Page 25 Statement of findings Page 27 Identification methods Page 31 Summary Page 33 Z-Scores Page 34 Sample 4 Analysis Page 36 Identified substances Page 36 Statement of findings Page 38 Identification methods Page 42 Summary Page 44 Test Samples Information Samples Comments on samples Sample 1 To prepare BS-1, urine was spiked with 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) (1590 ng base/ml), as an ethanolic solution. The spiked urine was dispensed in 50ml aliquots and lyophilised Sample 2 To prepare BS-2, urine was spiked with Gammahydroxybutyrate (GHB) (14360 ng base/ml), as an aqueous solution. The spiked urine was dispensed in 50ml aliquots and lyophilised Sample 3 To prepare BS-3, urine was spiked with Amfetamine sulphate (1570ng/ml, 1150 ng base/ml) and Metamfetamine hydrochloride (4290 ng/ml, 3450 ng base/ml) as aqueous solutions. The spiked urine was dispensed in 50ml aliquots and lyophilised Sample 4 BS-4 was a blank test sample containing no substances in the ICE menu Samples Substances Concentrations Comments on substances Sample 1 4-Bromo-2,5-dimethoxyphenethylamine (2C- 1590 ng/ml B) Sample 2 gamma-Hydroxybutyric acid (GHB) 14360 ng/ml Sample 3 Metamfetamine 3450 ng/ml Amfetamine 1150 ng/ml Sample 4 [blank sample] This report contains the data received from laboratories participating in the current exercise. The results compiled in this report are not intended to be an overview of the quality of work and cannot be interpreted as such. These comments do not reflect the general state of the art within the profession. Participant results are reported using a randomly assigned "WebCode". This code maintains participant's anonymity, provides linking of the various report sections, and will change with every report. 2013/2-BS (2) Copyright (c) 2014 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Introduction An important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. Two rounds are offered per year with each round presenting participants with four different test samples for analysis. This report provides information on the analytical results of laboratories participating in the Biological Specimens (BS) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts, which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact. Comments from the International Panel of Forensic Experts Participation of laboratories Samples within both the Seized Materials (SM) and Biological Specimens (BS) test groups were sent to 165 laboratories in 59 countries. 63 laboratories participated in the BS test group and 62 (98%) laboratories submitted the results of their analysis in time for inclusion in the summary report, with 98% using the ICE portal for return of results. Qualitative and Quantitative Analysis of the biological specimens test samples Overall, the level of performance in identification of the test samples was good given the inherently higher level of difficulty in the analysis of biological specimens compared to seized materials. The complexity of the test samples in ICE 2013/2 was designed in order to challenge the participants and BS-1 contained 4-bromo-2,5-dimethoxyphenethylamine (2C-B) which was identified by 50% of participants. BS-2 contained gamma-hydroxybutyric acid (GHB), which was identified by 29% of participants. This represents an increase from the 22% of participants who identified this substance in the 2013/1 round of ICE. BS-3 contained a mixture of amphetamine and methamphetamine which were identified by 87% and 94% of participants respectively. BS-4 was a blank test samples containing no substances from the ICE menu. With regard to false positive results, there were a total of 13 throughout all the BS test samples in 2013/2 including a number of false positive results for the New Psychoactive Substances (NPS) pentedrone and 2C-D. As the ICE programme develops, UNODC will include further examples of representative NPS in the ICE menu to assist participants in their analysis and detection of emerging substances. ICE participants are encouraged to use the UNODC Early Warning Advisory on New Psychoactive Substances http://www.unodc.org/nps, to report NPS detected in their laboratories. This information will greatly assist UNODC to further target its technical assistance to ICE participants. A modified Z-score was used for the statistical examination of the quantitative results, as it is a robust method based on absolute deviations from the median of all participant values and is relatively insensitive to outliers. The results for quantitative analysis within the BS test group were excellent. For BS-1, 9 out of 11 (82%) laboratories quantified the 2C-B with acceptable Z-scores. Within BS-2, 11 of 11 (100%) laboratories quantified the GHB with acceptable Z-scores and within BS-3, 22 of 26 (85%) quantified the amphetamine and 21 of 27 (78%) quantified the methamphetamine with Z-scores ≤3.5. It is encouraging to note that of those laboratories who did carry out quantification, 85% performed quantification on at least two of the four substances in all test samples. The predominant analytical techniques used by participants for quantification within the BS test group were GC/MS (72%), followed by LC/MS (16%). Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. Also, laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. (3) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 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 reagent (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate 150 Thin Layer Chromatography 160 High/Ultra High Performance Liquid Chromatography 161 High Performance Liquid Chromatography with diode array detection 170 Gas Chromatography NPD 171 Gas Chromatography FID 172 Gas Chromatography ECD 180 Gas Chromatography/Mass Spectrometry 190 Fourier Transform Infrared Spectrometry 200 Spectrophotometry (visible, UV) 210 Others (specify) 211 NMR 220 Microcrystal test 230 Liquid chromatography/mass spectrometry 231 Liquid chromatography/tandem mass spectrometry 2013/2-BS (4) Copyright (c) 2014 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Sample 1 Analysis Identified substances for Test Sample 1 Code Identified Substances 0M000K 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 1141EE 2C-B 1QGKQ2 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE 1WETGW 2CB 2EBBHO 4-Bromo-2,5-dimethoxyphenethylamine 2KCYAI 2C-B 46IBBF 2CB 8DVTCL 4 bromo 2,5 dimethoxyphenethylamine (2C-B) 9XZBR7 4-Bromo-2,5- dimethoxyphenethylamine (2C-B) BLIJKY 2C-B D4DPHG 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) DT7ISD 2C-B EJ2CHZ 2C-B FBENZD 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) G77E4Y 4-Bromo-2,5-dimethoxyphenethylamine GDND33 4-Bromo-2,3-dimethoxyphenetylamine (2C-B) GGVBC9 2C-B H3JJHS no drugs IM1DVM 2C-B JEJOYK 2-CB LJFPOP 4-Bromo-2,5-dimethoxyphenethylamine LLJIXJ 2C-B LRZE2T 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) NNNNNT pentedrone, 2 CB OQD7DK METANFETAMINA QGLOM0 2C-B RWEVZ2 2 CB SYYXMI 2C-B UMKJAA 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) UNFSFL 2C-B, 6-Monoacetylmorphine V4Q444 none VOG5LQ 2C-B W7ETOR ephedrine YJJ4JB 2-CB Z4FFXF 2C-D 2013/2-BS (5) Copyright (c) 2014 UNODC INTERNATIONAL QUALITY ASSURANCE
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