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 <ul style="display: flex;"><li style="flex:1">Introduction </li><li style="flex:1">Page </li><li style="flex:1">3</li></ul>Comments from the International Panel of Forensic Experts Codes and Abbreviations Page Page 34 Sample 1 Analysis Identified substances Statement of findings Identification methods Summary Page Page Page Page Page Page 55610 12 <ul style="display: flex;"><li style="flex:1">13 </li><li style="flex:1">Z-Scores </li></ul>Sample 2 Analysis Identified substances Statement of findings Identification methods Summary Page Page Page Page Page Page 15 15 16 20 22 <ul style="display: flex;"><li style="flex:1">23 </li><li style="flex:1">Z-Scores </li></ul>Sample 3 Analysis Identified substances Statement of findings Identification methods Summary Page Page Page Page Page Page 25 25 27 31 33 <ul style="display: flex;"><li style="flex:1">34 </li><li style="flex:1">Z-Scores </li></ul>Sample 4 Analysis Identified substances Statement of findings Identification methods Summary Page Page Page Page Page 36 36 38 42 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 <ul style="display: flex;"><li style="flex:1">Samples Substances </li><li style="flex:1">Concentrations Comments on substances </li></ul>Sample 1 4-Bromo-2,5-dimethoxyphenethylamine (2C- B) 1590 ng/ml Sample 2 gamma-Hydroxybutyric acid (GHB) Sample 3 Metamfetamine Amfetamine 14360 ng/ml 3450 ng/ml 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. <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(2) 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 <a href="/goto?url=http://www.unodc.org/nps" target="_blank">http://www.unodc.org/nps</a><a href="/goto?url=http://www.unodc.org/nps" target="_blank">, </a>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. <ul style="display: flex;"><li style="flex:1">(ANP): </li><li style="flex:1">Analysis not performed. </li></ul>Tech Code 100 110 120 130 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Name Agglutination Techniques Enzyme Immunoassay Techniques Fluorescence Polarization Immunoassay Radioimmunoassay Colorimetric reactions Marquis reagent (sulphuric acid, formaldehyde) Cobalt thiocyanate Thin Layer Chromatography High/Ultra High Performance Liquid Chromatography High Performance Liquid Chromatography with diode array detection Gas Chromatography NPD Gas Chromatography FID Gas Chromatography ECD Gas Chromatography/Mass Spectrometry Fourier Transform Infrared Spectrometry Spectrophotometry (visible, UV) Others (specify) NMR Microcrystal test Liquid chromatography/mass spectrometry Liquid chromatography/tandem mass spectrometry <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(4) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Sample 1 Analysis Identified substances for Test Sample 1 <ul style="display: flex;"><li style="flex:1">Code </li><li style="flex:1">Identified Substances </li></ul>0M000K 1141EE 1QGKQ2 1WETGW 2EBBHO 2KCYAI 46IBBF 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 2C-B 4-BROMO-2,5-DIMETHOXYPHENETHYLAMINE 2CB 4-Bromo-2,5-dimethoxyphenethylamine 2C-B 2CB 8DVTCL 9XZBR7 BLIJKY 4 bromo 2,5 dimethoxyphenethylamine (2C-B) 4-Bromo-2,5- dimethoxyphenethylamine (2C-B) 2C-B D4DPHG DT7ISD EJ2CHZ FBENZD G77E4Y GDND33 GGVBC9 H3JJHS IM1DVM JEJOYK LJFPOP LLJIXJ 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 2C-B 2C-B 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 4-Bromo-2,5-dimethoxyphenethylamine 4-Bromo-2,3-dimethoxyphenetylamine (2C-B) 2C-B no drugs 2C-B 2-CB 4-Bromo-2,5-dimethoxyphenethylamine 2C-B LRZE2T NNNNNT OQD7DK QGLOM0 RWEVZ2 SYYXMI UMKJAA UNFSFL V4Q444 VOG5LQ W7ETOR YJJ4JB 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) pentedrone, 2 CB METANFETAMINA 2C-B 2 CB 2C-B 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 2C-B, 6-Monoacetylmorphine none 2C-B ephedrine 2-CB <ul style="display: flex;"><li style="flex:1">Z4FFXF </li><li style="flex:1">2C-D </li></ul><ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(5) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Statement of findings for Test Sample 1 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) Code 0M000K +The sample contains 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) 0VK4JU 0X49WT 1141EE 1QGKQ2 1WETGW 2EBBHO 2KCYAI 2LL22V ANP -+Sample containing 2C-B ++2Cb is a controlled narcotic (illegal). +DPR 309/90 +2C-B was detected, this indicate that 2C-B was consumed ANP 3SSSXP 46IBBF ANP +Analytical Adverse Finding for 2CB in the sample. 4NPU45 8DVTCL ANP +2C-B is a psychedelic phenethylamine of the 2C family. 2C-B is sold as a white powder sometimes pressed in tablet or gel caps. The drug is usually taken orally but can also be insufflated or vaporized. 2 C-B is a controlled narcotic in France 9XZBR7 BHOY6O BLIJKY +Urine sample was positive in 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) ANP +-<ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(6) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) Code BLSRL6 -no drugs found BT0LUQ D4DPHG DT7ISD E72F2D EJ2CHZ F7F96F FBENZD G77E4Y GAISIJ ANP +4-Bromo-2,5-dimethoxyphenethylamine (2C-B) was detected. +++This person consumed 2C-B. ANP On analysis, no drug was found in the sample 2013/2/BS-1 +Sample is positive for 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) +4-Bromo-2,5-dimethoxyphenethylamine ANP No se detectó GDND33 GGVBC9 GH06SE H3JJHS IM1DVM JEJOYK JG8ZIW +As analytical standard was not available, quantification was not performed. +Consumption of 2C-B. ANP caffeine ANP ++BS1 positive for 2-CB ANP None detected for controlled substances <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(7) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) Code JU0000 ANP ANP ANP +KVSKNU KZ1811 LJFPOP LLJIXJ non è stata quantificata perché non abbiamo standard +LRZE2T MPEEAM NNNNNT OO55M5 OQD7DK PP8BHL Q8883N QGLOM0 QPMKNP RU1E3P +ANP +controlled substances ANP Negative -LA MUESTRA DE ORINA LIOFILIZADA CONTIENE METANFETAMINA ANP ANP No hubo consumo de las drogas analizadas en cantidades detectables por las tecnicas empleadas. +ANP No drugs detected in BS1 ANP Analysis of test sample B2013/2/BS-1 utilizing an eight (8) panel presumptive immunochemical technique did not indicate the presence of drugs. RWEVZ2 SYYXMI +Absorption of 2 CB Comment : In BS1, presence of a physiologic concentration of GHB (412 ng/ml) +screening and confirm by GC-MS: positive <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(8) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 4-Bromo-2,5- dimethoxyphenethy lamine (2C-B) Code TEYUEO ANP Test sample 2013/2/BS-1 does not contain controlled drugs for the tests performed, therefore Negative. TF2GTH U8WWWW UMKJAA UNFSFL V4Q444 VDXO2T VOG5LQ W7ETOR XJJRJO YJJ4JB ANP ANP +Urine sample positive for 4-Bromo-2,5-dimethoxyphenethylamine (2C-B) +-none -+ANP Ephedrine ANP No drug was detected in sample +It indicates the intake of 2-CB Z4FFXF ANP <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(9) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Identification methods for Test Sample 1 Legend: <ul style="display: flex;"><li style="flex:1">S ... used for Screening </li><li style="flex:1">I ... used for Identification </li></ul>SI ... used for both Analytical Technique Codes 100 110 120 140 150 161 170 180 230 231 210 Code <ul style="display: flex;"><li style="flex:1">0M000K </li><li style="flex:1">SI </li><li style="flex:1">I</li><li style="flex:1">Multi-Drug Screen Test </li></ul>Panel 0VK4JU 0X49WT 1141EE 1QGKQ2 1WETGW 2EBBHO 2KCYAI 2LL22V 3SSSXP 46IBBF I<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">SI </li></ul>SI II SI <ul style="display: flex;"><li style="flex:1">SI </li><li style="flex:1">I</li></ul>I SI S II<ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">I</li><li style="flex:1">S Lateral Flow Immunoassay </li></ul><ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">I</li></ul>ISI I SI 4NPU45 8DVTCL 9XZBR7 BHOY6O BLIJKY SSS<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li></ul>SI <ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">S</li></ul>S SI <ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">BLSRL6 </li></ul>BT0LUQ D4DPHG DT7ISD E72F2D EJ2CHZ F7F96F FBENZD G77E4Y S I SI<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li><li style="flex:1">Q-TOF </li></ul>SSS<ul style="display: flex;"><li style="flex:1">SI </li><li style="flex:1">I</li></ul>II II I SS<ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">I</li><li style="flex:1">I</li></ul><ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li><li style="flex:1">SI Kinetics Interactions of </li></ul>Microparticles <ul style="display: flex;"><li style="flex:1">GAISIJ </li><li style="flex:1">S</li></ul>GDND33 GGVBC9 GH06SE H3JJHS IM1DVM JEJOYK JG8ZIW <ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">I</li></ul>IIII SSI S II I SSS I SI <ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(10) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 100 110 120 140 150 161 170 180 230 231 210 Code <ul style="display: flex;"><li style="flex:1">JU0000 </li><li style="flex:1">SI </li></ul><ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">KVSKNU </li></ul>KZ1811 LJFPOP LLJIXJ I<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">S</li><li style="flex:1">I</li></ul>SS II LRZE2T MPEEAM NNNNNT OO55M5 OQD7DK PP8BHL Q8883N QGLOM0 QPMKNP RU1E3P RWEVZ2 SYYXMI TEYUEO TF2GTH SI SI <ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li><li style="flex:1">I</li></ul>ISI <ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">S</li></ul>SS II<ul style="display: flex;"><li style="flex:1">SI </li><li style="flex:1">S Randox </li></ul><ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">SI </li></ul>I SI SSS<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li></ul>SI <ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">I</li><li style="flex:1">S Drug Test Kit </li></ul>SS I U8WWW W I UMKJAA UNFSFL V4Q444 VDXO2T VOG5LQ W7ETOR XJJRJO YJJ4JB <ul style="display: flex;"><li style="flex:1">S</li><li style="flex:1">SI </li></ul><ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">S</li></ul>SS II II I II I<ul style="display: flex;"><li style="flex:1">SI </li><li style="flex:1">SI </li></ul>S DIPRO DRUGLAB SCREEN SS I<ul style="display: flex;"><li style="flex:1">I</li><li style="flex:1">SI </li></ul><ul style="display: flex;"><li style="flex:1">2013/2-BS </li><li style="flex:1">Copyright (c) 2014 UNODC </li></ul>(11) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary for BS-1 The response summary of all 62 participating laboratories for the identification of BS-1, frequency of use of screening and identification techniques and false positives and negatives: Identification of BS-1: Response Summary Participants: 62 4-Bromo-2,5-dimethoxyphenethylamine (2C-B): 31 False positives for Test Sample 1 Code Name Technique NNNNNT Pentedrone 180 <ul style="display: flex;"><li style="flex:1">RWEVZ2 </li><li style="flex:1">GHB </li><li style="flex:1">161/180 </li></ul>Z4FFXF OQD7DK UNFSFL <ul style="display: flex;"><li style="flex:1">2C-D </li><li style="flex:1">180 </li></ul>180 RMetamfetamine s: 6-Monoacetylmorphine (6-MAM) 180/231 <ul style="display: flex;"><li style="flex:1">W7ETOR Ephedrine </li><li style="flex:1">150 </li></ul>False negatives for BS-1 (techinque(s) used) Code - OX49WT (161/180), BLSRL6 (110/180),OQD7DK (110/180) V4Q444 (150/180), VDXO2T (161/180) There were 25 false negative results where analysis for 2C-B was not performed Frequency of use of screening and identification techniques: Response Summary Response Summary Response Summary Participants: 54 Participants: 62 Participants: 61 <ul style="display: flex;"><li style="flex:1">100 </li><li style="flex:1">110 </li></ul>110 120 120 <ul style="display: flex;"><li style="flex:1">140 </li><li style="flex:1">150 </li><li style="flex:1">161 </li><li style="flex:1">170 </li><li style="flex:1">180 </li><li style="flex:1">230 </li><li style="flex:1">231 </li></ul>231 210

International Collaborative Exercises (Ice)

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