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

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An Erratum to this article was published on 13 July 2013

Abstract

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.

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Authors and Affiliations

  1. Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, Av. do Café, Ribeirão Preto, 14040-903, São Paulo, Brazil

    Marcela Nogueira Rabelo Alves

  2. Synlab Italia Srl, Via Orzinuovi, 111-25125, Brescia, Italy

    Gabriele Zanchetti, Alberto Piccinotti & Silvia Tameni

  3. Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Av. Bandeirantes, 3900, Ribeirão Preto, 14040-901, São Paulo, Brazil

    Bruno Spinosa De Martinis

  4. Department of Public Health and Community Medicine, University of Verona, P.le Scuro 10, 37134, Verona, Italy

    Aldo Polettini

Authors
  1. Marcela Nogueira Rabelo Alves
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  2. Gabriele Zanchetti
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  3. Alberto Piccinotti
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  4. Silvia Tameni
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  5. Bruno Spinosa De Martinis
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  6. Aldo Polettini
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Correspondence to Aldo Polettini.

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Alves, M.N.R., Zanchetti, G., Piccinotti, A. et al. Determination of cocaine and metabolites in hair by column-switching LC-MS-MS analysis. Anal Bioanal Chem 405, 6299–6306 (2013). https://doi.org/10.1007/s00216-013-7046-3

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  • DOI: https://doi.org/10.1007/s00216-013-7046-3

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