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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISE (ICE)

Summary Report

SEIZED MATERIAL 2011/2 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE)

Table of contents

Introduction Page 4

Comments from the International Panel of Forensic Experts Page 4

Codes and Abbreviations Page 5

Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 9 Identification methods Page 16 Summary Page 19 Z-Scores Page 20

Sample 2 Analysis Page 22 Identified substances Page 22 Statement of findings Page 23 Identification methods Page 29 Summary Page 32 Z-Scores Page 33

Sample 3 Analysis Page 34 Identified substances Page 34 Statement of findings Page 37 Identification methods Page 44 Summary Page 47 Z-Scores Page 48

Sample 4 Analysis Page 50 Identified substances Page 50 Statement of findings Page 53 Identification methods Page 59 Summary Page 62 Z-Scores Page 63

Test Samples Information

Samples Comments on samples Sample 1 SM1 was prepared from a seizure containing 6.9% w/w cocaine base. The sample also contained caffeine, lidocaine and procaine.

Sample 2 SM2 was a blank test sample of glucose containing no substances in the ICE menu.

Sample 3 SM3 was prepared from a seizure containing 5.5% w/w amfetamine base. The sample also contained caffeine and creatinine. Sample 4 SM4 was prepared from a sample containing 4.7% w/w ketamine base in glucose.

Samples Substances Concentrations Comments on substances Sample 1 Caffeine 0 % Quantification not required. Cocaine 6.9 % Procaine 0 % Quantification not required. Lidocaine (Lignocaine) 0 % Quantification not required. Sample 2 [blank sample] Sample 3 Caffeine 0 % Quantification not required. Amfetamine 5.5 % Sample 4 Ketamine 4.7 %

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.

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 Seized Materials (SM) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”. These codes will change in every round. Two rounds are offered per year with each round presenting participants with four different test samples for analysis. 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. 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 133 laboratories in 50 countries. Within the SM test group, samples were sent to 103 laboratories in 43 countries and 97 laboratories (94%) submitted the results of their analysis in time for inclusion in the summary report, with 95 (98%) using the ICE portal for return of results. The almost universal usage of the ICE portal is a high endorsement of its utility. Some laboratories continue to have difficulty in obtaining import authorization and some delays in the preparation of test samples resulted in an extension of the deadline for submission of results.

Qualitative Analysis

The results for the qualitative identification of the controlled substances were excellent for SM-1, SM-3 and SM-4, with 98% correctly identifying cocaine in SM-1 and 93% of participants identifying amfetamine in SM-3 and ketamine in SM-4. Additionally, it is encouraging that a high percentage of laboratories identified the 3 additives: caffeine: 91%, lidocaine: 88% and procaine: 75% within SM-1. Within the blank test sample SM-2, there were no false positives for controlled substances on the ICE menu and 2 false positives for additives. Within SM-3 there were three false positive and 6 false negative results. Two false positives were reported for amfetamine in SM-4 and two additional false positive identifications were reported for substances not included in the ICE menu: methylphenidate (SM-3) and prazepam (SM-2), each of which was only reported once.

Quantitative Analysis

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 proportion of participants who carried out quantitative analysis, 72 (74%) for SM-1, 57 (59%) for SM-3 and 48 (50%) continues to be encouraging and some 91% of participants overall used GC-MS indicating the availability of a high level of technical expertise. Analysis of the Z-scores showed that 63 out of 72 (88%) of participants provided acceptable quantitative results with Z-scores within 3.5 for cocaine in SM-1, 50 out of 57 (88%) for amfetamine in SM-3 and 42 of 48 (88%) laboratories for ketamine in SM-4. Participants with Z-scores outside acceptable limits should review their quantification procedures. Overall, only 46% of participants carried out quantitation of all 3 samples, and encouragement should be given for those who do carry out quantitative analysis to do so on all samples as this allows them to get a better measure of their performance over time. 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 ICE also helps in monitoring the effect of corrective actions.

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 140 Colorimetric reactions 141 Marquis reagent (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate 150 Thin Layer Chromatography 160 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

Identified substances for Test Sample 1 Code Identified Substances 02RPHG Cocaïne 0H0JO1 caffeine, lidocaine, procaine, cocaine 1111NT Cocaine 1ZTSFT COCAINE 2JJ8HU cocaine 2XPJYP Cocaine 3TL3NN Cocaine 4FSWFF cocaïne 4GB444 Cocaine 4O1QQS Cocaine,Caffeine,Lidocaine and Procaine 4PBNK1 cocaine 4R4TLX cocaine 5IGXOG Cocaine Hydrochloride 666Q1T Cocaine, Lidocaine, Levamisol, Procaine, Caffeine 6GSCQF cocaine 6YRT1G Probably cocaine 73CCWP cocaine 76B77M cocaine 7WVOE5 cocaine 88XBE8 Cocaine 8GAURX cocaine hydrochloride 99V493 cocaine AOOEOD Cocaine AQADQV Cocaine AQZK6G Caffein, Cocaine, Lidocaine, Procaine B44PS4 Cocaine B4UUTU caffeine, cocaine and lidocaine BZCDP3 Cocaine CQSFOX Cocaine, lidocaine, procainamide CTMZ2M cocaine hidrochloride CTTOGT cocaine DL3VGI Cocaine (7%), Lidocaine(6%) DZ5DHD cocaine EAAA1A Cocaine EGILJI Cocaine, Procaine and Lidocaine F0XV9S Cocaine, Lidocaine, Procaine F2V4FT Procaïne et caféïne FFYCML Cocaine FGNTSP Cocaine FWFKFG Cocaine

Code Identified Substances GBEILS cocaine GKMY4V cocaine GMTGGC cocaine hydrochloride GUBCXC Cocaine HHAPY1 COCAINE HHQBHO Cocaine HNNIXK Cocaine ICKQLL cocaine IKO7ZK Cocaine, Lidocaine, Procaine IYIISS cocaine, lidocaine, caffeine IYZIN8 Cocaine JETQUT cocaine JJIJLJ COCAINE KBBJUV cocaïne KSKMBO cocain KUUG6K cocaine L5OSY0 Cocaine L9SN4N Cocaine LCG7ZT Cocain LKB44Q cocaine LOO8O7 Cocaine, Lidocaine, Caffeine LUXVKH i found caffeine, cocaine, procaine and lidocaine M0ADFO Cocaine HCl MCBSQR cocaine MJNCV8 Cocaine NJ9WNG Cocaine NU8JX5 cocaina O55RIG Cocaine PCPZLP COCAINE PDAKIA cocain hydrochloride Q0RDRB Cocaine,Lidocaine,Procaine and Caffeine QHSMH4 Cocaine QNPXNV Cocaine QQG9Q8 cocaine RSLNUR caffeine,lidocaine,cocaine,procaine SJCEJK Cocaine SQQQEU cocaine TWXYBN COCAINE UBUTUX cocaine/caffeine/lidocaine/procaine UP7176 Cocaine Hydrochloride V00WXT Cocaine, Caffeine and Lidocaine V9RPY9 cocaine clorhidrate W1WDNT cocaine, caffeine, procaine, lignocaine W71QCW cocaine, procaine, lidocaine, caffeine

Code Identified Substances WGIY0C Cocaine WH9EFB Caffeine -Lidocaine-Procaine-Cocaine- XWBWWE cocaine Y0JSL0 Cocaine and Lidocaine Y8DGCA cocaine YEFX2X Cocaine YJZY3Z Cocaine YNYYYW cocaine YPGEYE cocaine chlorhydrate ZQMAOY cocaine ZQR8JR Cocaine , Caffeine ZRXCZK cocaine

Statement of findings for Test Sample 1

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) 02RPHG + + + + Levamisole + caffeine + lidocaïne + procaïne 0H0JO1 + + + + creatinine 1111NT + + + + Test sample 2011/2/SM-1 contains Cocaine, Lidocaine, Procaine and Caffeine 1ZTSFT + + + + Sample 2011/2/SM-1 was found to contain controlled substance COCAINE. Sample 2011/2/SM-1 was also found to contain LIDOCAINE, PROCAINE and CAFFEINE. 2JJ8HU + + + + The sample also contained caffeine, lidocaine and procaine. 2XPJYP + + + + Caffeine, Lidocaine, Procaine 3TL3NN - + - ANP The powder was analysed when it was found to contain Cocaine, a class A drug within the provisions of a National Drugu control act. 4FSWFF + + + + the sample contains cocaïne which is scheduled as illicit drug in this country. 4GB444 - + + - Analysis of the powder revealed the presence of cocaine 4O1QQS + + + + 1.Screening:We use color tests to find if the material may have controlled drugs. The material have negative results for the color tests of amphetamine type stimulants, cannabinoids, hallucinogenic drugs and opiates, but have positive result for the color test of cocaine.The detailed method is that we use three kind of reagents. Solution 1 is 2% cobalt thiocyanate-Co(CNS)2-dissolved in water and then diluted 1:1 with 96% glycerine(pharmacertical grade),Solution 2 is hydrochloric acid (concentrated);Solution 3 is chloroform. Put some test material in a test tube, 5 drop of solution 1 are added and the mixture is shaken, then the mixture become blue. Add one drop of solution 2 and shake,then the blue color disappear and a clear pink can be seen. Add 7 drops of solution 3 and shake, then the chloroform layer develop an intense blue color. So we think that the material may contain cocaine. 2.Confirmation:We take 10 mg test material, solved in 10 mL methanol, shake. Then we analysis the solution with GC and GC-MS.And we also analysis the reference materials of controlled drugs in the menu.Then we compare the retention time and mass spectrum of the test material and reference materials. If the relitive error of the retention time of the test material and reference material is below 2%, and the similarity of the mass spectrum of two materials is above 90%,then we think it contains the material. By this method we find that it contains cocaine, caffeine, lidocaine, procaine and creatine.Creatine is not in the drug menu. 4PBNK1 + + + + White powder containing 7.3% w/w of cocaine. The sample was also found to contain caffeine, lidocaine, procaine and lactose. 4R4TLX + + + -

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) 5IGXOG + + + + The powder contained an average of 7% Cocaine Hydrochloride, together with creatine, caffeine, lignocaine,levamisole and procaine. 666Q1T + + + + The sample contained Cocaine, Lidocaine, Levamisol, Procaine and Caffeine. 6GSCQF + + + + cocaine+lidocaine+caffeine+procaine 6YRT1G ANP ANP ANP ANP The sample does not have amfetamine type stimulants, heroin and morphine; however, it may contain cocaine which has to be confirmed applying confirmatory tests. At the moment, this laboratory is not able to do confirmatory tests for this substance since standard cocaine is not available for the lab. The analyses for finding other substances in the menu of ICE programme were not performed. 73CCWP + + + +

76B77M + + + + The sample was dissolved into a certain amount of a methanol:chloroform solution. The solution was analyzed by GC-MS and its mass spectrum was compared to the one collected on a 1 ppm fresh prepared solution of cocaine. 7WVOE5 ANP + - -

88XBE8 + + + - In the test sample 2011/2/SM-1 were detected cocaine, caffeine and lidocaine. 8DWWDM + + + +

8GAURX + + + + MS and FTIR spectra, sample contains caffeine procaine and lidocaine. FTIR points out on the presence of creatine. 99V493 + + + + caffeine, lidocaine and procaine was also detected. AOOEOD + + + - Sample SM1, a white, odourless powder, was found to contain Cocaine, a controlled substance under the Narcotics Codex. AQADQV + + + +

AQZK6G + + + + Sample SM-1 contains cocaine and fillers. B44PS4 + + + + sample contains 7.1 % cocaine

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) B4UUTU + + + - The substance was found to contain caffeine, lidocaine and cocaine. BZCDP3 + + + + The powder was analysed and found to contain cocaine. CQSFOX + + + - caffeine, quantification in GC-MS with an internal standard CTMZ2M + + + + Base Cocaine 6,48% ; caffeine; lidocaine; procaine; creatine CTTOGT - + + - mixture with lidocaine and dextrose DL3VGI + + + ANP Matrix has coffeine DZ5DHD + + + + The sample contains cocaine. EAAA1A - + - + The Test Sample 2011/2/SM-1 was analysed by colour tests and Thin Layer Chromatography (TLC) techniques and found to contain Cocaine and Procaine. EGILJI + + + + On analysis, i found the sample "2011/2/SM-1" to contains Cocaine, Procaine, Lidocaine and caffeine. F0XV9S + + + +

F2V4FT + - - + Following analysis the sample 2011/2/SM-1 was found to contain procaine and caffeine FFYCML + + - - We found cocaine and caffeine FGNTSP + + ANP ANP The white powder contained an average of 7% of cocaine. FWFKFG + + + + Sample 2011/2/SM-1 consists of white powder. Cocaine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. GBEILS + + + + The sample contains cocaine, caffeine, lidocaine and procaine. The percentage by weight of cocaine (as base) is 7.74%. GKMY4V + + + + Cocaine is present and identified by GC-MS analysis. It was quantified by GC-FID analysis upon a calibration curve performed with a certified reference material and a n-alkane as internal standard.

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) GMTGGC + + + + This sample contains cocaine hydrochloride (7.1 % as base) cut with caffeine (6.9 %), lidocaine (5.7 % as base), procaine (3.1 % as base) and creatine (not quantified). GUBCXC + + + + Cocaine clorhidrate 6.9% (base), Caffeine, Lidocaine, Procaine and Glucitol HHAPY1 + + + + White powder containing cocaine. Also detected caffeine, lidocaine and procaine. HHQBHO ANP + - - Colorimetric Reactions (CR) SCOTT Reagent and Thin Layer Chromatography (TCL) HNNIXK + + + + This sample contains cocaine wich is listed as a controlled drug, according to national law

ICKQLL + + + + The sample was found to contain 6.8% of cocaine (as base). IKO7ZK + + + + One glass bottle containing 0.22 grammes of a powder containing 0.01 grammes of cocaine. IYIISS + + + -

IYZIN8 + + + + Adulterants:Lidocaine, Procaine, caffeine JETQUT + + - + cocaine (12.29 %) + procaine (2.33 %) + caffeine (5.68%) JJIJLJ + + + - The sample contains cocaine,a narcotic substance contained in Annex I of the decree of 22 February 1990 as amended establishing the list of substances classified as narcotics. The amount of cocaine base is 7% KBBJUV . + + + + Products found : procaïne ; lidocaine : caffein KSKMBO + + + + Sample contains 7% cocain, 3% procain.HCl, 6% lidocain.HCl and 6% caffeïn. Cocain is controled by National Drug laws. Procain, lidocain and caffeïn are adulterants often found in cocain streetsamples, these are not controled by the drug law. KUUG6K + + + + The sample is cocaine. L5OSY0 + + + + White powder of total net weight 0.226 grams containing caffeine, lignocaine, procaine and 6% COCAINE.

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) L9SN4N - + + + We also found on analysis procaine, lidocaine and starch.- LCG7ZT + + - + screening colour test ( Cobalt thiocyanate )+ve Identification by TLC , Confirmation by GC.MS LKB44Q + + + + CR, TLC, FTIR, GC/FID LOO8O7 + + + - Presence of Cocaine, Lidocaine and Caffeine. The purity of Cocaine was 6.68%. LUXVKH + + + + the sample was confirmed by gc-ms M0ADFO + + + + SM1 is a mixture of Cocaine HCl, Caffeine, Lidocaine, Procaine and Creatinine with 7% Cocaine base MCBSQR + + + + the sample contains 12% cocaine (calculated as cocaine base) MJNCV8 + + + + The sample identified as 2011/2/SM-1 presents cocaine, lidocaine, procaine and caffeine; cocaine has a percentage by weight of 7.8% in the sample. NJ9WNG + + + + Cocaine, 7% as base, caffeine, procaine, lactose. NU8JX5 ANP + ANP ANP

O55RIG + + + + The sample contains cocaine, lidocaine, procaine, caffeine and creatine monohydrate. PCPZLP + + + + COCAINE, PROCAINE, LIDOCAINE AND CAFFEINE PDAKIA + + + + cafein 7 %, lidocaïn 6%, procaïn 3 %, creatin, mannitol

Q0RDRB + + + + Test Sample 2011/2/SM-1 was found to contain stimulant type drugs and cocaine type drugs QHSMH4 + + + + Cocaine existed in salt form. Besides, Procaine, lidocaine and caffeine were found in the sample QNPXNV + + + + Lidocaine, Procaine and Caffine

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) QQG9Q8 + + + - On analysis, I found the substance to contain 6.95% cocaine, lidocaine and caffeine RSLNUR + + + +

SJCEJK + + + + Caffeine, procaine (we had doubts for procainamide), lignocaine, cocaine. SQQQEU + + + + cocaine at 7.5 % w/w, caffeine, lidocaine and procaine TWXYBN + + + +

UBUTUX + + + + cocaineˣcaffeineˣlidocaine and procaine detected in SM-1.Cocaine content is 6.86%.

UP7176 + + + + The powder contained an average of 7% Cocaine Hydrochloride, together with creatine, caffeine, lignocaine, levamisole and procaine. V00WXT + + + ANP cocaine, caffeine and Lidocaine detected in sample SM-1 but quantitation not performed V9RPY9 + + + ANP The sample contains cocaine hydrocloride (with a purity of 6.39 % as base) W1WDNT + + + + On analysis the powder was found to contain cocaine. W71QCW + + + + color test : cobalt thiocyanate = blue TLC : TA and TE = cocaine , caffeine GC : cocaine bas 7.58%, procaine base 2.57%, lidocaine base 5.44%, caffeine 7.65% WGIY0C + + + - The percentage of cocaine found to be 7.6 % WH9EFB + + + + HPLC-DAD, GC-MASS XWBWWE + + + + The samples contains cocaine in a mixture with lidocaine, caffeine and creatine Cocaine is a substance contained in Annex I of the decree of 22 February 1990 as amended establishing the list of substances classified as narcotics.

Y0JSL0 + + + ANP We found Cocaine ( 8.4166 %) and Lidocaine (4.9974 %) as a controlled drugs in this sample and also we found caffeine as adulterant (uncontrolled drugs)

Code Lidocaine Caffeine Cocaine Procaine (Lignocaine) Y8DGCA + + + +

YEFX2X + + + +

YJZY3Z + + + +

YNYYYW + + + +

YPGEYE + + + + caféine, lidocaïne, lévamisole, procaïne, créatine ZQMAOY + + + + We found cocaine and lidcocaine,caffeine and procaine ZQR8JR + + - - The sample 2011/2/SM_1 gave the positive results with Cobalt Thiocyanate test it Indicate present of Cocaine and Caffeine, GC if compairing between the sample Cocaine and caffeine the peak come out the same time. ZRXCZK + + + + cocaine, lidocaine, procaine, caffeine

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 230 231 210 02RPHG S S I I SI 0H0JO1 I SI 1111NT S I I 1ZTSFT I S 2JJ8HU SI SI 2XPJYP I SI 3TL3NN S I S DMAB 4FSWFF S I 4GB444 SI I I 4O1QQS S S S I I I I 4PBNK1 I SI 4R4TLX S S S I I 5IGXOG S S I 666Q1T I SI HPTLC 6GSCQF SI SI SI SI I I 6YRT1G S I S I I 73CCWP SI I 76B77M I SI 7WVOE5 I SI 88XBE8 I I 8DWWD S I I M 8GAURX S S I I I 99V493 S SI I AOOEOD S S I I AQADQV I SI I CE AQZK6G SI I SI SI Immunoassay B44PS4 SI B4UUTU S I SI BZCDP3 S S I CQSFOX SI I CTMZ2M S S S I I I I XRD CTTOGT S I I I I DL3VGI SI I HPLC-UV/VIS DZ5DHD SI SI

Code 140 141 142 150 160 161 170 171 180 190 200 230 231 210 EAAA1A S S S I Ehrlich Reagent EGILJI S S I I I S Duquenois-Levine F0XV9S S S S I I F2V4FT S I FFYCML SI SI I FGNTSP S S I I FWFKFG S S I I I GBEILS SI GKMY4V I I I SI GMTGGC I I GUBCXC S I HHAPY1 S SI I I HHQBHO SI S S I HNNIXK I ICKQLL SI IKO7ZK S S I SI IYIISS SI I IYZIN8 I SI JETQUT SI I JJIJLJ S S I I KBBJUV I SI KSKMBO I KUUG6K S I I L5OSY0 S S I L9SN4N S I I LCG7ZT S S S I I I I LKB44Q S SI I I LOO8O7 S SI LUXVKH S I I M0ADFO SI I MCBSQR S S I MJNCV8 S S S I I I NJ9WNG I I I NU8JX5 SI O55RIG S I SI S PCPZLP I SI PDAKIA S S S S I Q0RDRB SI I QHSMH4 S I I

Code 140 141 142 150 160 161 170 171 180 190 200 230 231 210 QNPXNV S I SI QQG9Q8 S S S I I RSLNUR SI SJCEJK S S I S Duquenois-Levin SQQQEU SI TWXYBN I S UBUTUX I I S colloidal gold UP7176 S S I V00WXT S S SI V9RPY9 S S S I S Ehrlich W1WDNT I I W71QCW S S I I WGIY0C I S S S I SI I WH9EFB S S S SI I I XWBWW SI SI I E Y0JSL0 SI I I Y8DGCA S I I YEFX2X SI I YJZY3Z S S S I I YNYYYW I SI S YPGEYE SI ZQMAOY I SI ZQR8JR S S S I I ZRXCZK SI I I

Summary for SM-1

The response summary of all 97 laboratiories participating for identification of SM-1, frequency of use of screening and identification techniques and false positives and negatives:

Identification of SM-1: Caffeine: 88 Cocaine: 95 Lidocaine (Lignocaine): 85 Procaine: 73

False Positives for SM-1: no false positives found

False Negatives for SM-1: no false negatives found

Frequency of Use of Screening and Identification techniques:

Section 140 141 142 150 160 161 170 171 180 190 200 230 231 210 Screening 25 36 32 19 1 1 1 1 37 4 0 0 1 7 25.8% 37.1% 33.0% 19.6% 1.0% 1.0% 1.0% 1.0% 38.1% 4.1% 0.0% 0.0% 1.0% 7.2% Identification 3 2 1 32 5 14 4 24 87 15 2 3 4 6 3.1% 2.1% 1.0% 33.0% 5.2% 14.4% 4.1% 24.7% 89.7% 15.5% 2.1% 3.1% 4.1% 6.2% # labs using 26 37 32 39 5 14 4 25 87 19 2 3 4 11 this 26.8% 38.1% 33.0% 40.2% 5.2% 14.4% 4.1% 25.8% 89.7% 19.6% 2.1% 3.1% 4.1% 11.3% technique

Z-Scores for Test Sample 1

Cocaine Cocaine CODE MAD: 0.5 CODE MAD: 0.5 Conc. * AbsDev ZScore Conc. * AbsDev ZScore 02RPHG 6.3 0.7 0.9 L5OSY0 6.0 1.0 1.4 0H0JO1 6.8 0.3 0.3 L9SN4N 7.5 0.5 0.7 1ZTSFT 7.7 0.7 0.9 LKB44Q 7.1 0.1 0.2 2XPJYP 6.5 0.5 0.7 LOO8O7 6.7 0.3 0.4 4FSWFF 7.0 0.0 0.0 LUXVKH 9.0 2.0 2.7 4GB444 4.0 3.0 4.1 M0ADFO 7.0 0.0 0.0 4O1QQS 7.3 0.3 0.4 MCBSQR 12.0 5.0 6.8 4PBNK1 7.3 0.3 0.4 MJNCV8 7.8 0.8 1.1 5IGXOG 7.0 0.0 0.0 NJ9WNG 7.0 0.0 0.0 6GSCQF 6.0 1.0 1.4 O55RIG 6.8 0.2 0.3 73CCWP 7.5 0.5 0.7 PCPZLP 8.0 1.0 1.3 76B77M 7.9 0.9 1.2 PDAKIA 7.0 0.0 0.0 7WVOE5 8.2 1.2 1.6 Q0RDRB 5.1 1.9 2.6 88XBE8 6.5 0.5 0.7 QHSMH4 5.6 1.4 1.9 8GAURX 6.7 0.3 0.4 QNPXNV 7.0 0.0 0.0 AOOEOD 7.4 0.4 0.5 QQG9Q8 7.0 0.0 0.1 AQADQV 12.2 5.2 7.0 SJCEJK 7.5 0.5 0.6 AQZK6G 6.0 1.0 1.3 SQQQEU 7.5 0.5 0.7 B44PS4 7.1 0.1 0.1 TWXYBN 4.0 3.0 4.1 B4UUTU 6.8 0.3 0.3 UBUTUX 6.9 0.1 0.2 CQSFOX 6.1 0.9 1.2 UP7176 7.0 0.0 0.0 CTMZ2M 6.5 0.5 0.7 V9RPY9 6.4 0.6 0.8 CTTOGT 2.4 4.6 6.2 W71QCW 7.6 0.6 0.8 DL3VGI 7.0 0.0 0.0 WGIY0C 7.6 0.6 0.8 F0XV9S 20.4 13.4 18.1 XWBWWE 7.0 0.0 0.0 FGNTSP 7.0 0.0 0.0 Y0JSL0 8.4 1.4 1.9 GBEILS 7.7 0.7 1.0 YEFX2X 7.5 0.5 0.7 GKMY4V 6.8 0.2 0.3 YJZY3Z 12.2 5.2 7.0 GMTGGC 7.1 0.1 0.1 YNYYYW 6.5 0.5 0.7 GUBCXC 6.9 0.1 0.1 YPGEYE 7.9 0.9 1.2 HHAPY1 6.9 0.1 0.1 ZQMAOY 8.1 1.1 1.4 HNNIXK 7.0 0.0 0.0 *) Concentration: w/w % ICKQLL 6.8 0.2 0.3 Z-Score has been calculated as modified Z-Score as it is a IKO7ZK 6.2 0.8 1.1 robust method and therefore relatively insensitive to outliers. IYIISS 13.0 6.0 8.1 Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a IYZIN8 7.9 0.9 1.2 laboratory value and the median of all the laboratory values for the given drug; JETQUT 12.3 5.3 7.1 MAD = median absolute deviation about the median. JJIJLJ 7.0 0.0 0.0 Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. KBBJUV 6.6 0.4 0.5 KSKMBO 7.1 0.1 0.1 Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle KUUG6K 6.9 0.1 0.2 Outliers, American Society for Quality Control, Milwaukee, WI

Z-Score per Sample include results submitted after deadline: No

Round: 2011/2

Substance: SM-1/Cocaine Median = 7 MAD = 0.50

Sample 2 Analysis

Identified substances for Test Sample 2 Code Identified Substances 1111NT None 6GSCQF - B4UUTU Glucose DL3VGI - DZ5DHD - EAAA1A Glucose /Dextrose F2V4FT does not contain drugs FFYCML - ICKQLL none JETQUT drugs are not detected KUUG6K No LOO8O7 None LUXVKH the sample was negative for illicit drugs M0ADFO - Q0RDRB Lidocaine RSLNUR prazepam YNYYYW No

Statement of findings for Test Sample 2

Code [blank sample] 02RPHG Glucose

0H0JO1 glucosa

1111NT Test sample 2011/2/SM-2 contains Dextrose

1ZTSFT Sample 2011/2/SM-2 was not found to contain controlled substances.

2JJ8HU SM-2 was a blank test sample. This sample is not contain any subtances in the ICE menu.

2XPJYP

3TL3NN The powder was analysed for the presence of drugs controlled under the terms of the national drug control act with a negative result.

4FSWFF

4GB444 Analysis of the powder for controlled drugs yielded negative result

4O1QQS 1.Screening:We use color tests to find if the material may have controlled drugs. The material have negative results for the color tests of amphetamine type stimulants, cannabinoids, cocaine, hallucinogenic drugs and opiates. So we can not know whether the material may contain controlled drugs in the menu. 2.Confirmation:We take 10 mg test material, solved in 10 mL methanol, shake. Then we analysis the solution with GC and GC-MS.And we also analysis the reference materials of controlled drugs in the menu.Then we compare the retention time and mass spectrum of the test material and reference materials. If the relitive error of the retention time of the test material and reference material is below 2%, and the similarity of the mass spectrum of two materials is above 90%,then we think it contains the material. By this method we find that it does not contain any drugs in the menu. Then we solve 10 mg material in 1 mL water, and analysis the solution with HPLC with differential refractive index detector and LC-MS.And we also analysis the reference materials of glucose, lactose and galactose. Then we find the retention time of the test material and glucose are same, and the molecular weight of the test material tested in the LC-MS is same as glucose. So we think it contains glucose.But glucose is not in the controlled drug menu. 4PBNK1 White powder containing glucose but no illicit substances.

4R4TLX

5IGXOG No controlled drugs were detected in the powder which was identified as glucose.

Code [blank sample] 666Q1T The sample did not contain any controlled substances in quantities above our detection limits.

6GSCQF -

6YRT1G The sample does not contain amfetamine type stimulants, heroin, morphine and cocaine. The analyses for finding other substances in the menu of ICE programme were not performed.

73CCWP

76B77M

7WVOE5

88XBE8 In the test sample 2011/2/SM-2 were not detected drugs, was detected glucose.

8DWWDM

8GAURX

99V493

AOOEOD Sample SM2, a white, odourless powder, was not found to contain any substances controlled under the Narcotics Codex.

AQADQV

AQZK6G Sample SM-2 dose not have any illegal drug.

B44PS4 No drugs found

B4UUTU The substance was found to contain glucose.

BZCDP3 The powder was analysed for the presence of common controlled drugs with a negative result.

CQSFOX Dextrose

Code [blank sample] CTMZ2M Glucose

CTTOGT dextrose

DL3VGI -

DZ5DHD The sample does not contain drugs.

EAAA1A The Test Sample 2011/2/SM-2 was analysed by colour tests and Thin Layer Chromatography (TLC) techniques and not to found drugs included in the menu list but responded positive tests for carbohydrates and found to contain Glucose/Dextrose EGILJI On analysis, i found the sample "2011/2/SM-2" to contains glucose.

F0XV9S

F2V4FT The sample 2011/2/SM-2 does not contain drugs

FFYCML We found dextrose

FGNTSP The white powder was examined and no evidence was found for the presence of substances controlled under the provisions of the national misuse of Drugs Act. the white powder contained glucose. FWFKFG Sample 2011/2/SM-2 consists of white powder. No substances from the ICE menu are included.

GBEILS

GKMY4V this product is glucose, it doesn't contain controlled drugs

GMTGGC This sample only contains glucose.

GUBCXC Glucose

HHAPY1 White powder.

HHQBHO

Code [blank sample] HNNIXK

ICKQLL No common controlled drug was detected in the sample.

IKO7ZK One glass bottle containing 0.22 grammes of a powder which did not contain any controlled drugs.

IYIISS

IYZIN8

JETQUT probably maltose (FTIR-ATR)

JJIJLJ The test for narcotics was negative.

KBBJUV Glucose (IFTR)

KSKMBO No controled drugs were found in the sample with the techniques used. Sample contains sugar; mostly glucose.

KUUG6K The sample is glucose.

L5OSY0 White powder of total net weight 0.225 grams. No controlled drugs were detected.

L9SN4N On analysis we only found glucose

LCG7ZT

LKB44Q CR, TLC, FTIR, GC/FID

LOO8O7 No drugs found.

LUXVKH the sample was confirmed by gc-ms

M0ADFO SM2 contains Glucose

Code [blank sample] MCBSQR the sample doesn't contain narcotic/psycotropic drugs

MJNCV8 The sample identified as 2011/2/SM-2 does not contain controlled drugs.

NJ9WNG Glucose

NU8JX5

O55RIG The main component of the sample is glucose.

PCPZLP

PDAKIA Glucose

Q0RDRB Test Sample 2011/2/SM-2 was found to contain cocaine type drug lidocaine.

QHSMH4 Lactose only found in sample

QNPXNV Lactose

QQG9Q8 On analysis, I found the substance to contain caffeine.

RSLNUR

SJCEJK We couldn`t detect any substance with GC/MS.

SQQQEU found sugars

TWXYBN

UBUTUX Glucose detected in SM-2.

UP7176 No controlled drugs were detected in the powder which was identified as glucose.

Code [blank sample] V00WXT No drugs detected

V9RPY9 A controlled drug was not found

W1WDNT No controlled drugs were detected.

W71QCW FTIR = dextrose

WGIY0C Galactose was found

WH9EFB

XWBWWE The research for narcotics was negative.

Y0JSL0 no controlled drugs detected in this sample

Y8DGCA

YEFX2X

YJZY3Z

YNYYYW

YPGEYE glucose

ZQMAOY We found a sugar likely glucose

ZQR8JR

ZRXCZK

Identification methods for Test Sample 2

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

Summary for SM-2

The response summary of all 97 laboratiories participating for identification of SM-2, frequency of use of screening and identification techniques and false positives and negatives:

Identification of SM-2:

False Positives for SM-2: Code Name HNNIXK Caffeine Q0RDRB Lidocaine (Lignocaine) QQG9Q8 Caffeine RSLNUR Prazepam

False Negatives for SM-2:

no false negatives found

Frequency of Use of Screening and Identification techniques:

Z-Scores for Test Sample 2

Quantification is not required.

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

Sample 3 Analysis

Identified substances for Test Sample 3 Code Identified Substances 02RPHG amphetamine 0H0JO1 amfetamine, caffeine 1111NT Amphetamine 1ZTSFT AMPHETAMINE 2JJ8HU amfetamine 2XPJYP Amphetamine 3TL3NN Amphetamine 4FSWFF amfetamine 4GB444 Amphetamine 4O1QQS Amphetamine and Caffeine 4PBNK1 amphetamine 4R4TLX amphetamine 5IGXOG Amphetamine 666Q1T Amphetamine, Caffeine 6GSCQF amfetamine 73CCWP amphetamine 76B77M amphetamine 7WVOE5 amfetamine 88XBE8 Amfetamine 8GAURX amphetamine sulfate 99V493 amfetamine AOOEOD Amphetamine AQADQV Amphetamine AQZK6G Amphetamine, Methamphetaine, Caffeine B44PS4 Amfetamine B4UUTU amphetamine BZCDP3 Amphetamine CQSFOX amphetamine CTMZ2M Amphetamine sulphate CTTOGT amfetamine DL3VGI Amphetamine(5%) DZ5DHD amphetamine EAAA1A Amfetamine F0XV9S Amphetamine F2V4FT Caféïne FFYCML Amfetamine FGNTSP Amphetamine FWFKFG Amfetamine GBEILS amphetamine GKMY4V Amphetamine

Code Identified Substances GMTGGC amfetamine sulphate GUBCXC Amphetamine HHAPY1 AMPHETAMINE HHQBHO Amphetamine type Stimulants HNNIXK amfetamine ICKQLL amphetamine IKO7ZK Amphetamine IYIISS amfetamine, caffeine IYZIN8 Amphetamine JETQUT amfetamine JJIJLJ AMPHETAMINE KSKMBO amphetamine KUUG6K amphetamine L5OSY0 Amphetamine L9SN4N Amphetamine LCG7ZT Amphetamine LKB44Q Amphetamine HCl LOO8O7 Caffeine LUXVKH the sample contains caffeine and amphetamine M0ADFO Amphetamine Sulphate MCBSQR amphetamine MJNCV8 Amfetamine NJ9WNG Amphetamine NU8JX5 anphetamine O55RIG amphetamine PCPZLP AMPHETAMINE PDAKIA amphetamin sulfate Q0RDRB Caffeine QHSMH4 Amphetamine QNPXNV Amphetamine QQG9Q8 Amphetamine RSLNUR amphetamine SJCEJK amphetamine SQQQEU amphetamine TWXYBN AMFEMTAMINE UBUTUX amfetamine/caffeine UP7176 Amphetamine V00WXT Amphetamine and Caffeine V9RPY9 Amfetamine W1WDNT Amphetamine, caffeine W71QCW Amphetamine and caffeine WGIY0C Amfetamine WH9EFB Amphetamine-caffeine- XWBWWE amphetamine

Code Identified Substances Y0JSL0 Amphetamine Y8DGCA amfetamine YEFX2X Amphetamine YJZY3Z Amphetamine YNYYYW Amfetamine YPGEYE amfetamine sulfate ZQMAOY amfetamine ZQR8JR Methamphetamine Caffeine ZRXCZK amphetamine

Statement of findings for Test Sample 3

Code Amfetamine Caffeine 02RPHG + + caffeine 0H0JO1 + + creatinine 1111NT + + Test sample 2011/2/SM-3 contains Amphetamine and Caffeine 1ZTSFT + + Sample 2011/2/SM-3 was found to contain controlled substance Amphetamine. Sample 2011/2/SM-3 was also found to contain CAFFEINE. 2JJ8HU + + The sample also contained caffeine. 2XPJYP + + Caffeine 3TL3NN + - The powder was analysed when it was found to contain Amphetamine, a class B drug within the provisions of the National misuse of drugs act. 4FSWFF + + the sample contains amfetamine which is scheduled Nationally as an illicit drug. 4GB444 + - Analysis of the powder revealed the presence of amphetamine 4O1QQS + + 1.Screening:We use color tests to find if the material may have controlled drugs. The material have negative results for the color tests of cocaine, cannabinoids, hallucinogenic drugs and opiates, but have positive result for the color test of amphetamine.The detailed method is that we use two kind of reagents. Solution 1 is prepared in this way: add 10 drops of 37% formaldehyde solution in 10 mL of acetic acid,Solution 2 is concentrated sulfuric acid. Put some test material in a test tube, add one drop of solution 1, then add one drop of solution two, shake. The mixture become orange, and then slowly become brown. So we think that the material may contain amphetamine. 2.Confirmation:We take 10 mg test material, solved in 10 mL methanol, shake. Then we analysis the solution with HPLC with DAD and GC-MS.And we also analysis the reference materials of controlled drugs in the menu.Then we compare the retention time and mass spectrum of the test material and reference materials. If the relitive error of the retention time of the test material and reference material is below 2%, and the similarity of the mass spectrum of two materials is above 90%,then we think it contains the material. By this method we find that it contains amphetamine, caffeine and creatine.Creatine is not in the drug menu. 4PBNK1 + + White powder containing 6.1% w/w of amphetamine together with caffeine and lactose. 4R4TLX + +

5IGXOG + + The powder contained an average of 6% Amphetamine, together with creatine and caffeine

Code Amfetamine Caffeine 666Q1T + + The sample contained Amphetamine and Caffeine 6GSCQF + + amfetamine+caffeine 6YRT1G ANP ANP The sample does not contain amfetamine type stimulants, heroin, morphine and cocaine. The analyses for finding other substances in the menu of ICE programme were not performed. 73CCWP + +

76B77M + + The same test described for sample SM-1 was carried out, but using a 1 ppm fresh solution of D,L- amphetamine for comparison. 7WVOE5 + +

88XBE8 + + In the test sample 2011/2/SM-3 were detected amfetamine and caffeine. 8DWWDM + +

8GAURX + + sample contain also caffeine and creatine ( based on FTIR result) 99V493 + + caffeine was also detected AOOEOD + + Sample SM1, a off- white, odourless powder, was found to contain Amphetamine, a controlled substance under the Narcotics Codex. AQADQV + +

AQZK6G + + Sample no: SM-3 contains amphetamines and filler. B44PS4 + + Sample contains 5.4 % amfetamine

B4UUTU + + The substance was found to contain amphetamine. BZCDP3 + + The powder was analysed and found to contain amphetamine. CQSFOX + - with caffeine, quantification with gravimetric parameter and GC-MS %

Code Amfetamine Caffeine CTMZ2M + + Base amphetamine 6,40%, caffeine, creatine CTTOGT + + mixutre with caffeine DL3VGI + + Matrix has coffeine DZ5DHD + + The sample contains amphetamine. EAAA1A + + The Test Sample 2011/2/SM-3 was analysed by colour tests and Thin Layer Chromatography (TLC) techniques and found to contain Amfetamine and Caffeine. EGILJI - + On analysis, i found the sample "2011/2/SM-3" to contains caffeine. F0XV9S + +

F2V4FT - + Following analysis, sample 2011/2/SM-3 was found to contain caffeine FFYCML + + We found amfetamine and caffeine FGNTSP + + The white powder contained an average of 6% of amphetamine. FWFKFG + + Sample 2011/2/SM-3 consists of white powder. Amfetamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. GBEILS + + The sample contains amphetamine and caffeine. The percentage by weight of amphetamine (as base) is 5.58%. GKMY4V + + Amphetamine is present and identified by GC-MS analysis. It was quantified by HPLC-DAD analysis upon a calibration curve performed with a certified reference material. GMTGGC + + This sample contains amfetamine sulphate (5.4 % as base), cut with caffeine (30.0 %) and creatine (not quantified). GUBCXC + + Amphetamiene 4.78% and caffeine HHAPY1 + + White powder containing amphetamine. Also detected caffeine. HHQBHO + ANP Colorimetric Reactions (CR) MARQUIS Reagent

Code Amfetamine Caffeine HNNIXK + + This sample contains amfetamine wich is listed as a controlled drug, according to national law.

ICKQLL + + The sample was found to contain amphetamine. IKO7ZK + + One glass bottle containing 0.22 grammes of a powder containing 0.01 grammes of amphetamine. IYIISS + +

IYZIN8 + + adulterant:Caffeine JETQUT + + amfetamine (5.80 %) + caffeine (26.83 %) JJIJLJ + + The sample contains amphetamine, narcotic substance contained in Annex VI of the decree of 22 February 1990 as amended establishing the list of substances classified as drugs KBBJUV - + Caffein (CPS/MS) KSKMBO + + The sample contains 5% amphetamine and 28% caffein. Amphetamine is controled by KB from 2 december 1988, article 1. Caffein is an adulterant often found in amphetamine streetsamples. KUUG6K + + The sample is amphetamine. L5OSY0 + + Pale yellow powder of total net weight 0.227 grams containing caffeine and 5% AMPHETAMINE. L9SN4N + + We also found caffeine LCG7ZT + - screening colour test ( Marques )+ve Identification by TLC , Confirmation by GC.MS LKB44Q + + CR, TLC, FTIR, GC/FID LOO8O7 - + Present of Caffeine only. LUXVKH + + the sample was confirmed by gc-ms

Code Amfetamine Caffeine M0ADFO + + SM3 is a mixture of Amphetamine Sulphate, Caffeine and Creatinine with 5% Amphetamine base MCBSQR + + the sample contains 6.1% amphetamine (calculated as amphetamine base) MJNCV8 + + The sample identified as 2011/2/SM-3 presents amfetamine and caffeine; anfetamine has a percentage by weight of 19.74% in the sample. NJ9WNG + + Amphetamine 5,2% as base, caffeine. lactose. NU8JX5 + ANP

O55RIG + + The sample contains amphetamine, caffeine and creatine monohydrate. PCPZLP + + AMPHETAMINE AND CAFFEINE PDAKIA + + caféine, créatine Q0RDRB - + Test Sample 2011/2/SM-3 was found to contain stimulant type drug Caffeine QHSMH4 + + Amphetamine existed in base form. besides, Caffeine was found in the sample QNPXNV + + Caffeine, Methylphenidate (Ritalin) QQG9Q8 + + On analysis, I found the substance to contain 5.55% amphetamine and caffeine. RSLNUR + +

SJCEJK + + Caffeine, amphetamine SQQQEU + + amphetamine at 6.8% w/w and caffeine TWXYBN + +

UBUTUX + + Amfetamine and caffeine detected in SM-3.Amfetamine content is 5.78%.

Code Amfetamine Caffeine UP7176 + + The powder contained an average of 5% Amphetamine, together with creatine and caffeine. V00WXT + + Amphetamine and Caffeine detected in sample SM-3 but quantitation not performed V9RPY9 + + The sample contains a mixture of Amfetamine and caffeine W1WDNT + + On analysis the powder was found to contain amphetamine. W71QCW + + Color test : Marquis reagent = orange turning to brown, simon reagent = pink to cherry-red TLC : TA and TE = amphetamine and caffeine GC : Amphetamine base = 5.44% and caffeine 27.47% WGIY0C + + The percentage of amfetamine found to be 6.5 % WH9EFB + + TLC , HPLC-DAD , GC-MASS XWBWWE + + The sample contains amphetamine in a mixture with creatine and caffeine. Amphetamine is a narcotic substance contained in Annex III of the order of 22 February 1990, as amended, listing the substances classified as drugs. Y0JSL0 + + We found Amphetamine (6.8704 %) as a controlled drugs in this sample and also we found caffeine as adulterant (uncontrolled drugs) Y8DGCA + +

YEFX2X + +

YJZY3Z + +

YNYYYW + +

YPGEYE + + caféine, créatine ZQMAOY + + We found amfetamine and caffeine ZQR8JR - + The sample 2011/2/SM-3 gave the positive results with Maquist test it indicate present of Amphetamine type stimulants 2011/2/SM-3 the same as Methamphetamine , GC if we compairing between sample and Methamphetamine the peak come out the same time

Code Amfetamine Caffeine ZRXCZK + + amphetamine, caffeine

Identification methods for Test Sample 3

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

8GAURX S S I I I 99V493 S SI I AOOEOD S S I I AQADQV I SI I CE AQZK6G SI I SI SI Immunoassay B44PS4 SI B4UUTU S I SI BZCDP3 S S I CQSFOX SI I CTMZ2M S S S I I I I XRD CTTOGT S I I I I DL3VGI SI I HPLC-UV/VIS DZ5DHD SI SI

Y0JSL0 SI I I Y8DGCA S I I YEFX2X SI I YJZY3Z S S S I I YNYYYW I SI S YPGEYE SI ZQMAOY I SI ZQR8JR S S S I I ZRXCZK SI I I

Summary for SM-3

The response summary of all 97 laboratiories participating for identification of SM-3, frequency of use of screening and identification techniques and false positives and negatives:

Identification of SM-3: Amfetamine: 90 Caffeine: 90

False Positives for SM-3: Code Name AQZK6G Metamfetamine ZQR8JR Metamfetamine

False Negatives for SM-3:

Code: Q0RDRB, L00807, KBBJUV, F2V4FT, EGILJI, ZQR8JR

Frequency of Use of Screening and Identification techniques:

Z-Scores for Test Sample 3

Amfetamine Amfetamine CODE MAD: 0.5 CODE MAD: 0.5 Conc. * AbsDev ZScore Conc. * AbsDev ZScore 02RPHG 2.2 3.4 4.6 O55RIG 5.5 0.1 0.1 0H0JO1 5.5 0.1 0.1 PCPZLP 12.3 6.7 9.1 1ZTSFT 7.9 2.3 3.1 QHSMH4 1.5 4.1 5.5 2XPJYP 7.0 1.4 1.9 QNPXNV 5.4 0.2 0.3 4FSWFF 5.0 0.6 0.8 QQG9Q8 5.6 0.0 0.1 4O1QQS 5.6 0.0 0.0 SJCEJK 6.3 0.7 0.9 4PBNK1 6.1 0.5 0.7 SQQQEU 6.8 1.2 1.6 5IGXOG 6.0 0.4 0.5 UBUTUX 5.8 0.2 0.2 6GSCQF 4.0 1.6 2.2 UP7176 5.0 0.6 0.8 73CCWP 6.1 0.5 0.7 W71QCW 5.4 0.2 0.2 76B77M 6.4 0.8 1.1 WGIY0C 6.5 0.9 1.2 7WVOE5 5.8 0.2 0.3 Y0JSL0 6.9 1.3 1.7 88XBE8 6.0 0.4 0.5 YEFX2X 5.9 0.3 0.4 8GAURX 6.5 0.9 1.3 YJZY3Z 8.4 2.8 3.8 AOOEOD 5.6 0.0 0.0 YPGEYE 5.5 0.1 0.1 AQADQV 5.6 0.0 0.0 ZQMAOY 5.0 0.6 0.8 AQZK6G 11.3 5.7 7.6 *) Concentration: w/w % B44PS4 5.4 0.2 0.3 CQSFOX 4.5 1.1 1.5 Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. CTMZ2M 6.4 0.8 1.1 Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a CTTOGT 13.3 7.7 10.4 laboratory value and the median of all the laboratory values DL3VGI 5.0 0.6 0.8 for the given drug; MAD = median absolute deviation about the median. F0XV9S 5.5 0.1 0.2 Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. FGNTSP 6.0 0.4 0.5

GBEILS 5.6 0.0 0.0 Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle GKMY4V 5.1 0.5 0.7 Outliers, American Society for Quality Control, Milwaukee, WI GMTGGC 5.4 0.2 0.3 GUBCXC 4.8 0.8 1.1 HNNIXK 5.0 0.6 0.8 IKO7ZK 5.5 0.1 0.1 IYZIN8 5.7 0.1 0.1 JETQUT 5.8 0.2 0.3 KSKMBO 5.2 0.4 0.5 KUUG6K 5.7 0.1 0.1 L5OSY0 5.0 0.6 0.8 L9SN4N 4.7 0.9 1.2 LKB44Q 5.9 0.3 0.4 M0ADFO 5.0 0.6 0.8 MCBSQR 6.1 0.5 0.6 MJNCV8 19.7 14.1 19.1 NJ9WNG 5.2 0.4 0.5

Z-Score per Sample include results submitted after deadline: No Round: 2011/2

Substance: SM-3/Amfetamine Median = 5.6 MAD = 0.50

Sample 4 Analysis

Identified substances for Test Sample 4 Code Identified Substances 02RPHG Ketamine 0H0JO1 ketamine 1111NT Ketamine 1ZTSFT KETAMINE 2JJ8HU ketamine 2XPJYP Ketamine 3TL3NN Ketamine 4FSWFF ketamine 4GB444 ketamine 4O1QQS Ketamine 4PBNK1 Ketamine 4R4TLX ketamine 5IGXOG Ketamine 666Q1T Ketamine 6GSCQF ketamine 73CCWP ketamine 76B77M ketamine 7WVOE5 ketamine 88XBE8 Ketamine 8GAURX ketamine hydrochloride 99V493 ketamine AOOEOD Ketamine AQADQV Ketamine AQZK6G Ketamine B44PS4 Ketamine B4UUTU ketamine BZCDP3 Ketamine CQSFOX Ketamine CTMZ2M ketamine CTTOGT ketamine DL3VGI Ketamine (4.5%) DZ5DHD ketamine EAAA1A Glucose/Dextrose EGILJI Ketamine F0XV9S Ketamine F2V4FT Amphétamine FFYCML Ketamine FGNTSP Ketamine Hydrochloride FWFKFG Ketamine GBEILS ketamine

Code Identified Substances GKMY4V Ketamine GMTGGC ketamine hydrochloride GUBCXC Ketamine HHAPY1 KETAMINE HNNIXK ketamine ICKQLL ketamine IKO7ZK Ketamine IYIISS ketamine IYZIN8 Ketamine JETQUT ketamine JJIJLJ KETAMINE HCl KBBJUV ketamine KSKMBO ketamine KUUG6K ketamine L5OSY0 Ketamine L9SN4N Ketamine LCG7ZT Ketamine LKB44Q Ketamine LOO8O7 Ketamine LUXVKH the sample contains ketamine M0ADFO Ketamine HCl MCBSQR ketamine MJNCV8 Ketamine NJ9WNG Ketamine O55RIG Ketamine PCPZLP KETAMINE PDAKIA kétamin hydrochloride Q0RDRB No sample Was recieved QHSMH4 ketamine QQG9Q8 Ketamine RSLNUR ketamine SQQQEU ketamine TWXYBN KETAMINE UBUTUX ketamine UP7176 Ketamine V00WXT Ketamine W1WDNT ketamine W71QCW Ketamine WGIY0C Ketamine WH9EFB Ketamine XWBWWE kétamine Y0JSL0 Ketamine Y8DGCA ketamine YEFX2X Ketamine

Code Identified Substances YJZY3Z Ketamine YNYYYW Ketamine YPGEYE kétamine ZQMAOY Ketamine ZRXCZK ketamine

Statement of findings for Test Sample 4

Code Ketamine 02RPHG + Glucose 0H0JO1 + glucosa 1111NT + Test sample 2011/2/SM-4 contains Ketamine and Dextrose 1ZTSFT + Sample 2011/2/SM-4 was found to contain controlled substance Ketamine. 2JJ8HU +

2XPJYP +

3TL3NN + The powder was analysed when it was found to contain Ketamine, a class C drug within the provisions of the National Misuse of Drugs Act. 4FSWFF + the sample contains ketamine which is scheduled nationally as an illicit drug. 4GB444 + Analysis of the powder revealed the presence of ketamine 4O1QQS + 1.Screening:We use color tests to find if the material may have controlled drugs. The material have negative results for the color tests of amphetamine type stimulants, cannabinoids, cocaine, hallucinogenic drugs and opiates. So we can not know whether the material may contain controlled drugs in the menu. 2.Confirmation:We take 10 mg test material, solved in 10 mL methanol, shake. Then we analysis the solution with HPLC with DAD and GC-MS.And we also analysis the reference materials of controlled drugs in the menu.Then we compare the retention time and mass spectrum of the test material and reference materials. If the relitive error of the retention time of the test material and reference material is below 2%, and the similarity of the mass spectrum of two materials is above 90%,then we think it contains the material. By this method we find that it contains ketamine.But the content is not high. So we solve some material in water and analysis the solution with LC-MS.Then we find it contains something whose retention time and molecular weight are same as glucose.So we think it contains glucose.But glucose is not in the controlled drug menu. 4PBNK1 + White powder containing 12.2% w/w of Ketamine 4R4TLX +

5IGXOG + The powder contained an average of 5% Ketamine, together with glucose.

Code Ketamine 666Q1T + The sample contained Ketamine. 6GSCQF + ketamine 6YRT1G ANP The sample does not contain amfetamine type stimulants, heroin, morphine and cocaine. The analyses for finding other substances in the menu of ICE programme were not performed. 73CCWP +

76B77M + The same test described for sample SM-1 was carried out, but using a 1 ppm fresh solution of ketamine for comparison. 7WVOE5 +

88XBE8 + In the test sample 2011/2/SM-4 was detected ketamine. 8DWWDM +

8GAURX + based on the MS and IR results. The IR results point out that sample 2011/2/SM-4 contain the same sugar derivative as sample 2011/2/SM-2 99V493 +

AOOEOD + Sample SM4, a white, sticky, odourless powder, was found to contain Ketamine, a controlled substance under the Narcotics Codex. AQADQV +

AQZK6G + Sample SM-4 contains hallucinogenic drug (Ketamine). B44PS4 + sample contains 8.5 % ketamine B4UUTU + The substance was found to contain amphetamine. BZCDP3 + The powder was analysed and found to contain ketamine. CQSFOX + Glucose, quantification with gravimetric parameter and GC-MS %

Code Ketamine CTMZ2M + ketamine; glucose CTTOGT + mixture with dextrose DL3VGI + - DZ5DHD + The sample contains ketamine. EAAA1A - The Test Sample 2011/2/SM-4 was analysed by colour tests and Thin Layer Chromatography (TLC) techniques and not to contain drugs included in the menu but responded positive tests for carbohydrates and found to contain Glucose/Dextrose. EGILJI + On analysis, i found the sample "2011/2/SM-4" to contains ketamine. F0XV9S +

F2V4FT - Following analysis, the sample 2011/2/SM-4 was found to contain amphetamine. FFYCML + We found Ketamine FGNTSP + The white powder contained Ketamine Hydrochloride. FWFKFG + Sample 2011/2/SM-4 consists of white powder. Ketamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. GBEILS + The sample contains ketamine. The percentage by weight of ketamine is 5.30%. GKMY4V + Ketamine is present and identified by GC-MS analysis. It was quantified by GC-FID analysis upon a calibration curve performed with a certified reference material and a n-alkane as internal standard. GMTGGC + This sample contains ketamine hydrochloride (6.0 as base) cut with glucose. GUBCXC + Ketamine and Glucose HHAPY1 + White powder containing ketamine. HHQBHO ANP

Code Ketamine HNNIXK + This sample contains ketamine wich is listed as a controlled drug, according to the national order, appendix IV of February 22nd 1990 ICKQLL + The sample was found to contain 4.8% of ketamine (as base). IKO7ZK + One glass bottle containing 0.21 grammes of a powder containing 0.01 grammes of ketamine. IYIISS +

IYZIN8 +

JETQUT + ketamine (5.09 %) + probably maltose (FTIR-ATR) JJIJLJ + The sample was found to contain ketamine, narcotic substance contained in Annex III of the order of 22 February 1990 as amended establishing the list of substances classified as drugs. KBBJUV + glucose (found by IFTR in insol. of CHCl3) KSKMBO + The sample contains 5% ketamine. Ketamine is controled by by national drug law (KB ...) KUUG6K + The sample is ketamine. L5OSY0 + White powder of total net weight 0.225 grams containing KETAMINE. L9SN4N + We also found on analysis, glucose LCG7ZT + Identification by TLC , Confirmation by GC.MS, Not under international control. LKB44Q + TLC, FTIR, GC/FID LOO8O7 + Presence of Ketamine with a purity of 66.46%. LUXVKH + the sample was confirmed by gc-ms M0ADFO + SM4 contains Ketamine HCl and Glucose with 4% Ketamine base

Code Ketamine MCBSQR + the sample contains 5,7% ketamine (calculated as ketamine base) MJNCV8 + The sample identified as 2011/2/SM-4 presents Ketamine. Ketamine has a percentage by weight of 5.70% in the sample. NJ9WNG + Ketamine 4,8% as base, glucose. NU8JX5 ANP

O55RIG + The sample contains ketamine and glucose. PCPZLP + KETAMINE PDAKIA + Glucose Q0RDRB ANP No analysis was done QHSMH4 + Ketamine existed in salt form. We also found lactose in the sample QNPXNV + Ketamine, Lactose QQG9Q8 + On analysis, I found the substance to contain 6.91% ketamine. RSLNUR +

SJCEJK + ketamine SQQQEU + ketamine at 5.2% w/w TWXYBN +

UBUTUX + Ketamine and Glucose detected in SM-4.Ketamine content is 5.43%.

UP7176 + The powder contained Ketamine, together with glucose.

Code Ketamine V00WXT + 7.9% of Ketamine detected in sample SM-4. Measurement Uncertainty +/- 0.21 V9RPY9 + The ketamine is not a controlled drug in this country. W1WDNT + On analysis the powder was found to contain ketamine. W71QCW + TLC : TA and TE = ketamine GC : ketamine base = 4.33% GC/MS = ketamine WGIY0C + The percentage of ketamine found to be 6.2 % WH9EFB + HPLC-DAD , GC-MASS XWBWWE + The sample contained ketamine in a mixture with glucose. The sample contains the narcotic ketamine, given in Annex IV of the order of 22 February 1990, as amended, listing the substances classified as anarcotic. Y0JSL0 + We found Ketamine (5.0006 %) in this sample. Ketamine is not under controlled by National Narcotics Regulation Y8DGCA +

YEFX2X +

YJZY3Z +

YNYYYW +

YPGEYE + glucose ZQMAOY + We found ketamine and in addition a sugar,but not lactose, likely glucose ZQR8JR -

ZRXCZK + ketamine

Identification methods for Test Sample 4

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

Summary for SM-4

The response summary of all 97 laboratiories participating for identification of SM-4, frequency of use of screening and identification techniques and false positives and negatives:

Identification of SM-4: Ketamine: 90

False Positives for SM-4: Code Name F2V4FT Amfetamine B4UUTU Amfetamine

False Negatives for SM-4:

no false negatives found

Frequency of Use of Screening and Identification techniques: Section 140 141 142 150 160 161 170 171 180 190 200 230 231 210 Screening 25 36 32 19 1 1 1 1 37 4 0 0 1 7 25.8% 37.1% 33.0% 19.6% 1.0% 1.0% 1.0% 1.0% 38.1% 4.1% 0.0% 0.0% 1.0% 7.2% Identification 3 2 1 32 5 14 4 24 87 15 2 3 4 6 3.1% 2.1% 1.0% 33.0% 5.2% 14.4% 4.1% 24.7% 89.7% 15.5% 2.1% 3.1% 4.1% 6.2% # labs using 26 37 32 39 5 14 4 25 87 19 2 3 4 11 this 26.8% 38.1% 33.0% 40.2% 5.2% 14.4% 4.1% 25.8% 89.7% 19.6% 2.1% 3.1% 4.1% 11.3% technique

Z-Scores for Test Sample 4

Ketamine Ketamine CODE MAD: 0.6 CODE MAD: 0.6 Conc. * AbsDev ZScore Conc. * AbsDev ZScore 0H0JO1 4.5 0.7 0.8 V00WXT 7.9 2.8 3.4 1ZTSFT 4.6 0.6 0.7 W71QCW 4.3 0.8 1.0 2XPJYP 3.7 1.5 1.8 WGIY0C 6.2 1.1 1.3 4O1QQS 5.3 0.1 0.1 Y0JSL0 5.0 0.2 0.2 4PBNK1 12.2 7.1 8.7 YEFX2X 5.1 0.1 0.1 5IGXOG 5.0 0.2 0.2 YJZY3Z 10.4 5.2 6.4 73CCWP 5.5 0.4 0.4 ZQMAOY 6.1 0.9 1.1 76B77M 6.2 1.1 1.3 *) Concentration: w/w % 7WVOE5 52.0 46.9 57.5 4.7 0.5 0.6 88XBE8 Z-Score has been calculated as modified Z-Score as it is a 8GAURX 5.8 0.6 0.8 robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AQADQV 5.3 0.1 0.1 AbsDev = Absolute value of the difference between a B44PS4 8.5 3.4 4.1 laboratory value and the median of all the laboratory values for the given drug; B4UUTU 4.6 0.5 0.6 MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 CQSFOX 2.8 2.4 2.9 should be considered as potential outliers. CTTOGT 0.5 4.7 5.7 Reference: DL3VGI 4.5 0.7 0.8 Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle F0XV9S 5.6 0.4 0.5 Outliers, American Society for Quality Control, Milwaukee, WI GBEILS 5.3 0.1 0.2 GKMY4V 5.3 0.1 0.2 GMTGGC 6.0 0.9 1.0 HNNIXK 4.0 1.2 1.4 ICKQLL 4.8 0.4 0.4 IKO7ZK 4.6 0.6 0.7 IYZIN8 5.2 0.0 0.1 JETQUT 5.1 0.1 0.1 KBBJUV 4.9 0.3 0.3 KSKMBO 4.7 0.5 0.6 L9SN4N 5.6 0.4 0.6 LKB44Q 4.5 0.7 0.8 LOO8O7 66.5 61.3 75.2 M0ADFO 4.0 1.2 1.4 MCBSQR 5.7 0.6 0.7 MJNCV8 5.7 0.6 0.7 NJ9WNG 4.8 0.4 0.4 O55RIG 4.8 0.3 0.4 PCPZLP 5.0 0.2 0.2 QHSMH4 3.2 2.0 2.4 QQG9Q8 6.9 1.8 2.2 SQQQEU 5.2 0.0 0.1 UBUTUX 5.4 0.3 0.3

Z-Score per Sample include results submitted after deadline: No

Round: 2011/2

Substance: SM-4/Ketamine Median = 5.15 MAD = 0.55

The Laboratory and Scientific Section UNODC, International Centre Wagramer Strasse 5, P.O. Box 500 A-1400, Vienna, AUSTRIA Email: [email protected]