title: Simultaneous quantitation of cocaine and its major metabolites in human hair by gas chromatography/chemical ionization mass spectrometry.
abstract: A sensitive method for the simultaneous analysis of cocaine, benzoylecgonine (BE), and ecgonine methyl ester (EME) in human hair by gas chromatography/chemical ionization mass spectroscopy (GC/CIMS) is described. Hair samples are cut into 1-cm sections, washed with 1% sodium dodecylsulfate, rinsed with deionized water and methanol, and then digested overnight in a solution containing Tris buffer, sodium dodecylsulfate, Proteinase K, and dithiothreitol. Digested hair samples are extracted with Bond Elut Certify solid-phase extraction columns, derivatized with N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA), and analyzed by GC/CIMS using isobutane as reagent gas. This method is quantitative, does not cause degradation of cocaine, and requires as little as 5 mg of hair. Analysis is performed on a Finnigan ITS-40 ion trap mass spectrometer interfaced with a Varian 3400 gas chromatograph equipped with a Model 1075 split/splitless injector and a J&W DB-5 capillary column. Full scan spectra are used for identification of cocaine and its metabolites. Quantitation is based on peak area ratios of the MH+ ions, as follows: 304 for cocaine, 404 for BE-TBDMS, 314 for EME-TBDMS, and 340 for the internal standard, difluorococaine. This method can be used to quantitate cocaine at concentrations of 0.1 to 100 ng/mg hair. The coefficients of variation (%CV) at a drug concentration of 1 ng/mg hair are 10.3, 16.3, and 27.7% for cocaine, BE, and EME, respectively.
authors.affiliation: Department of Medical Pharmacology and Toxicology, School of Medicine, University of California, Davis 95616.
authors.forename: M R
authors.initials: MR
authors.lastname: Harkey
authors.forename: G L
authors.initials: GL
authors.lastname: Henderson
authors.forename: C
authors.initials: C
authors.lastname: Zhou
mesh_terms: D003042:Cocaine / Q000031:analogs & derivatives* / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006197:Hair / Q000737:chemistry*; D006801:Humans
chemical_list: C005618:benzoylecgonine; D003042:Cocaine; C034524:ecgonine methyl ester