Determination of cocaine and metabolites in hair by column-switching LC-MS-MS analysis

被引:0
作者
Marcela Nogueira Rabelo Alves
Gabriele Zanchetti
Alberto Piccinotti
Silvia Tameni
Bruno Spinosa De Martinis
Aldo Polettini
机构
[1] Universidade de São Paulo,Faculdade de Ciências Farmacêuticas de Ribeirão Preto
[2] Synlab Italia Srl,Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto
[3] Universidade de São Paulo,Department of Public Health and Community Medicine
[4] University of Verona,undefined
来源
Analytical and Bioanalytical Chemistry | 2013年 / 405卷
关键词
Column switching; LC-MS-MS; Hair testing; Cocaine and metabolites; Drugs of abuse;
D O I
暂无
中图分类号
学科分类号
摘要
A method for rapid, selective, and robust determination of cocaine (CO) and metabolites in 5-mg hair samples was developed and fully validated using a column-switching liquid chromatography–tandem mass spectrometry system (LC-MS-MS). Hair samples were decontaminated, segmented, incubated overnight in diluted HCl, and centrifuged, and the diluted (1:10 with distilled water) extracts were analyzed in positive ionization mode monitoring two reactions per analyte. Quantifier transitions were: m/z 304.2→182.2 for CO, m/z 290.1→168.1 for benzoylecgonine (BE), and m/z 318.2→196.2 for cocaethylene (CE). The lower limit of quantification (LLOQ) was set at 0.05 ng/mg for CO and CE, and 0.012 ng/mg for BE. Imprecision and inaccuracy at LLOQ were lower than 20 % for all analytes. Linearity ranged between 0.05 and 50.0 ng/mg for CO and CE and 0.012 and 12.50 ng/mg for BE. Selectivity, matrix effect, process efficiency, recovery, carryover, cross talk, and autosampler stability were also evaluated during validation. Eighteen real hair samples and five samples from a commercial proficiency testing program were comparatively examined with the proposed multidimensional chromatography coupled with tandem mass spectrometry procedure and our reference gas chromatography coupled to mass spectrometry (GC-MS) method. Compared with our reference GC-MS method, column-switching technique and the high sensitivity of the tandem mass spectrometry detection system allowed to significantly reduce sample amount (×10) with increased sensitivity (×2) and sample throughput (×4), to simplify sample preparation, and to avoid that interfering compounds and ions impaired the ionization and detection of the analytes and deteriorate the performance of the ion source.
引用
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页码:6299 / 6306
页数:7
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