36-3/Höld../Simultaneous Quantitation of Cocaine, Opiates, and...

Published: Journal of Chromatographic Science, Volume 36, Number 3, March 1998, pp. 125-130.

Simultaneous Quantitation of Cocaine, Opiates, and Their Metabolites in Human Hair by Positive Ion Chemical Ionization Gas Chromatography–Mass Spectrometry
K.M. Höld, D.G. Wilkins, D.E. Rollins, R.E. Joseph, Jr., and E.J. Cone

A sensitive method is developed for the combined extraction of cocaine (COC), cocaethylene (CE), benzoylecgonine (BE), ecgonine methyl ester (EME), norcocaine (NORCOC), 6-acetylmorphine (6-MAM), codeine (COD), norcodeine (NORCOD), morphine (MOR), and normorphine (NORMOR) from human head hair using an enzyme-based digestion technique (Protease VIII/DTT/Tris-buffer pH 6.5 at 22ÐC). After pH adjustment to 5.5, the digests are extracted with a solid-phase extraction procedure using Bond-Elut Certify columns. The extract residues are evaporated at 40ÐC, reconstituted in 20 µL of ethyl acetate, and derivatized with the reagents N-methyl-N-trimethylsilylheptafluorobutyramide (MSHFBA), N-methyl-bis-heptafluorobutyramide (MBHFBA), and N-trimethylsilylimidazole (TMSIM). Analyses are performed by positive ion chemical ionization gas chromatography–mass spectrometry using a DB-1 capillary column. Two injections are performed on each extract to optimize sensitivity for all analytes. The assay is capable of reliably quantitating 500 pg/mg of all compounds and is linear to 50 ng/mg, except for BE, which is linear to 25.0 ng/mg. The method was used to analyze human hair samples obtained from cocaine and heroin users. COC, BE, and EME are detectable in all samples, whereas NORCOC, CE, COD, 6-MAM, and MOR are detected in only some samples. Norcodeine and normorphine are not detected. The assay is currently being used to analyze hair samples from a study investigating the mechanisms of drug disposition in hair.

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