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Methods for impurity profiling 31 Sample preparation: All glassware is silylated. Add 200 mg of the heroin sample to 4 ml of 1M sulphuric acid and 4 ml of a 3:2 mixture of diethyl ether and dichloromethane, mix thoroughly. Centrifuge to separate phases and transfer 3 ml of the organic phase into a clean reaction vial. Dry under dry nitrogen at 60° C.* Add 300 µl of the derivatization solution and 60 µl of the internal standard. Seal the reaction vial tightly, mix thoroughly and heat at 70° C for 30 min. If method retention times shift more than 0.2 min, the instrument is recalibrated and/or the retention time of the internal standard is adjusted by adjusting the carrier gas flow. Rationale for use: The method allows a total impurity profile of all alkaloidal trace impurities. Several modifications of the above method are in use worldwide. This version should provide the sensitivity and the specificity necessary for the analysis of highly refined heroin samples, that is, highly refined hydrochloride samples from South-East Asia. Outcome: Indication of general source region (South-East Asia, South-West Asia, Mexico, South America). Sample comparisons for discrimination and evaluation of samples for case-to-case evidential purposes (linkage determinations). Provides additional information required to confirm links between samples, that is, the method should be used in conjunction with a major component analysis. *In this form, a tightly capped reaction vial can be stored for up to a week at -5° C prior to further analysis. 4. Residual solvent analysis Method B5: Dynamic headspace (thermal desorption) gas chromatography (Conventional GC instrument) Source: J. Cartier, O. Guéniat and M. D. Cole, “Headspace analysis of solvents in cocaine and heroin samples”, Science and Justice, vol. 37, No. 3 (1997), pp. 175-181. Operating conditions: Detector: FID, at 45 ml/min hydrogen and 450 ml/min air Column: DB-1 or equivalent , 60 m x 0.33 mm x 3.0 µm Carrier gas: Helium at 0.7 ml/min (column pressure 17 psig) Injection technique: 1 µl; split, 30:1 Temperatures: Injector: 280° C Detector: 280° C Oven: 35° C for 14 min, to 100° C at 5° C/min, to 245° C at 7° C/min, no final hold (if petrol/gasoline was detected, the temperature of the column was held at 245° C for 10 min)
32 Methods for impurity profiling of heroin and cocaine Internal standard: None Sample preparation:* Weigh 250-300 mg of the powdered heroin sample into a 2-ml GC derivatization vial. Add a 0.25-ml insert, containing approximately 100 mg of activated carbon (charcoal strip). After sealing the vial, heat the contents for 60 min at 80° C and allow to cool. Extract the activated carbon with 50 µl of carbon disulphide and inject 1 µl of this solution** into the GC. Rationale for use: The method provides for the detection of 12 solvents in heroin samples, at detection limits between 2-15 parts per million (ppm) for 250-300 mg powder samples. No special injector device is required; the method uses a conventional GC instrument. Solvent analyses may be carried out on samples up to two years old. Outcome: Provides additional information and an independent means of confirming links from organic impurity and inorganic ion determinations. *Preparation of headspace samples must be performed under clean laboratory conditions to avoid solvent cross-contamination. **The remainder of this sample can be reused for ICP-MS analysis. Method B6: Static headspace-GC/MS (Special injector device required) Source: Modified from D. R. Morello and R. P. Meyers, “Qualitative and quantitative determination of residual solvents in illicit cocaine HCl and heroin HCl”, Journal of Forensic Sciences, vol. 40, No. 6 (1995), pp. 957-963. Operating conditions: Detector: Mass spectrometer, 70eV EI, 20-220 amu, 0.5 sec scan cycle Column: DB-1, 60 m x 25 mm x 1.0 µm Carrier gas: Helium, constant velocity approx. 30 cm/s Injector technique: Split 38:1, Tekmar 7000/7050 headspace autosampler 22 ml vials Equilibration: 14 min at 85° C 2-ml loop; injection time: 0.3 min Temperatures: Loop: 175° C Injector: 190° C Injector transfer line: 175° C MS transfer line: 190° C Oven: 35° C to 150° C at 6° C/min to 180° C at 15° C/min, hold for 10 min
Page 1 and 2: METHODS FOR IMPURITY PROFILING OF H
Page 3 and 4: Note Operating and experimental con
Page 6 and 7: Contents page I. Introduction. . .
Page 8 and 9: I. INTRODUCTION A. Background In or
Page 10 and 11: Introduction 3 on the detection and
Page 12 and 13: II. ASPECTS OF DRUG CHARACTERIZATIO
Page 14 and 15: Aspects of drug characterization an
Page 20 and 21: III. METHODS FOR IMPURITY PROFILING
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Page 24 and 25: Methods for impurity profiling 17 M
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Page 30 and 31: Methods for impurity profiling 23 I
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Page 54 and 55: IV. DATA HANDLING, INTERPRETATION O
Page 56 and 57: Data handling, interpretation of re
Page 58 and 59: References 1. “Report of an exper
Page 60 and 61: References 53 31. H. Neumann and G.
Page 62: ANNEX I SUPPLEMENTARY INFORMATION (
Page 65 and 66: 58 Methods for impurity profiling o
Page 70 and 71: ANNEX III REFERENCE CHROMATOGRAMS A
Page 72 and 73: Annex III 65 Table 1. Relative migr
Page 74 and 75: Annex III 67 Table 2. Relative migr
Page 76 and 77: Annex III 69 Table 3. Identificatio
Page 78 and 79: Annex III 71 Table 4: Retention tim
Page 80: Annex III 73 Figure VII. Expanded
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*0583802* Printed in Austria V.05-8
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