Sampling procedures heroin

Evaluation of a Sampling Procedure for Heroin Street Doses." journal cf Forensic Sciences, 43... 

In conclusion, methods have been presented for the comparison of heroin samples. These analytical procedures have been successfully used for both intelligence purposes and court testimony. 

Offidani et al. compared chemical hydrolysis with enzymatic hydrolysis utilizing hair samples obtained from heroin users. Hair samples were subjected to incubation in a solution of 1 M NaOH, then neutralized with hydrochloric acid and pH 7, 1 M phosphate buffer. Samples were also treated with a 1-mg/mL pronase solution in 0.05 M Tris buffer for 24 h at 39°C, followed by neutralization with pH 7, 1 M phosphate buffer. Both procedures yielded comparable results for morphine by RIA. 

Methods utilizing newer techniques including ITMS, CE, and GC/MS/MS have recently been developed. ITMS analysis by Curcuruto et al. ° and Traldi et al. readily demonstrated the presence of morphine in hair. Free zone CE with amperometric detection was sensitive and highly selective. A novel procedure by Polettini et al. describes the treatment of methanol-washed samples with a silylating solution, followed by injection into GC. The silylating reagent was prepared by mixing MSTFA with dithioerythritol and ammonium iodide. Analysis of heroin, 6-AM, acetylcodeine. 

Generally, the samples tested were head hair obtained from expertises or from subjects deceased from fatal heroin or cocaine overdose. Collection procedures have not been standardized, but hair is often collected from the area at the back of the head (vertex posterior), cut as close as possible to the scalp and stored in dry tubes. In this area, there is less variability in hair growth rate, the number of hairs in the growing phase is more constant, and the hair is less subject to age and sex-related influences. Occasionally, axiUaty or pubic hair have also been tested for cannabinoids. 

To avoid mistakes caused by contamination of the hair, the total strand is washed with water, petrolether, and methanol. Acute contamination should be excluded by examining the wash solutions. Blank and Kidwell described experiments concerning the contamination of hair with cocaine in the laboratory and found relevant drug concentration even after several washing procedures. Our experience with the hair of technical assistants who are handling heroin, cocaine, and hashish every day shows that these samples contain only traces of drugs. This is confirmed by the studies of Mieczkowski, who examined the hair of undercover narcotic officers. 

Nine samples of illicit heroin preparations were analyzed in duplicate by a gas chromatographic method. The samples can be assumed to have been drawn randomly from the same population. Pool the following data to establish an estimate of cr for the procedure. 

Cocaine can also be analyzed well by GC. Here again silylation can help to achieve good separation of majog minor, and trace components of the illicit cocaine samples and was therefore proposed as early as in 1973 by Moore. The sample preparation procedure used in our laboratory for the analysis of heroin and cocaine starts by dissolving the sample in chloroform. Then a mixture of MSTFA and pyridine is added and allowed to react at 80 C for 10 min. After that the solution is chromatographed directly. 

Quantitation of N-acetylnorheroin in heroin hydrochloride samples was by gas chromatography on a Perkin Elmer 900 Gas Chromatograph (column 6 ft. x 1/4 in.) temperature initial 180°C, final 270°C, program rate 4°C/min. Flame Ionization Detector, interfaced with Spectra-Physics Autolab System I Computing Integrator, measured peak areas in y volts Carrier gas nitrogen 60 ml/min. Authentic heroin hydrochloride samples were prepared by dissolving ca. 60 mg/ml in methanol. Standard N-acetylnorheroin (prepared by procedure described below) was 5.0 mg/ml. Sample... 

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