PubMed · 11612302
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H Schott. 1982. [Not Available].. https://pubmed.ncbi.nlm.nih.gov/11612302/
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Volatility and thermal stability are necessary physical-chemical properties for analysing a substance by gas chromatography. A derivatization step is required before gas chromatography of benzoylecgonine (the main metabolite of cocaine). In the literature, reactions such as silylation, perfluoroalkylation or alkylation are the most frequently used to derivatize benzoylecgonine. However, they allow the formation of products sensitive to moisture or require a purification step. So, a procedure to derivatize benzoylecgonine with diazomethane before gas chromatographic analysis was evaluated. A study was performed to evaluate the efficiency of conversion of benzoylecgonine in cocaine, the necessary time for reaction and the stability of ethereal solution of diazomethane. The reaction was shown to be very fast in mild conditions and there was no need for a further purification step. When benzoylecgonine was extracted from urine by solid-phase extraction and derivatized with diazomethane, concentrations as low as 25 ng/ml could be detected using GC-MS in the full scan mode.
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The analysis of solvent residues trapped into crystals of illicit drugs provides useful evidence for monitoring current use trend in the chemical underground, and is also a suitable tool to achieve the complete chemical characterisation of street drugs for comparative examination of separate specimens. This paper describes a method developed in order to perform simultaneous qualitative and quantitative analysis of solvent residues in cocaine samples. The method is based on GC-MS analysis of solvents after their extraction/concentration from drug matrices accomplished by solid-phase microextraction (SPME) in static head space. The proposed method has been used to detect residues of solvents in 47 illicit street cocaine samples. Quantitative analyses were carried out only for the solvents identified at concentration values higher than 1 ppm. Statistical evaluation of our results allowed us to group the illicit samples into various classes according to different kinds of residual solvent, in connection with different clandestine manufacturing processes used to prepare illicit cocaine.