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Hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples

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Abstract

This study reports the development and validation of a method using hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC-MS/MS) for the analysis of cocaine and its metabolites benzoylecgonine (BE), ecgonine methyl ester (EME), and cocaethylene (CE) in hair samples. Decontamination was performed as follows: Firstly, the aliquot of hair was briefly rinsed with 2 mL dichloromethane, then was washed three times with 10 mL 0.01 M phosphate buffer, pH 6, for 15 min, followed by 2 mL 2-propanol for less than 2 min, and, finally, a last rinse with 2 mL dichloromethane was again done. Cocaine compounds were extracted from 10 mg of hair by incubation with 2 mL 0.1 M HCl at 50 °C for 12 h and purified by solid phase extraction with Oasis MCX cartridges. Analysis was performed by LC-MS/MS using an Atlantis HILIC silica chromatographic column. The method was fully validated. Linearity was established over the concentration range 0.020–10.0 ng/mg for cocaine (COC), 0.010–10.0 ng/mg for BE and CE, and 0.005–2.0 ng/mg for EME, and the correlation coefficients were all >0.99. Extraction efficiency was >70% for all analytes. Limits of detection were 0.0005 ng/mg for CE and 0.001 ng/mg for the other analytes (COC, BE, and EME). Lower limits of quantification were the lowest points of the calibration curves with acceptable accuracy and precision (coefficient of variation ≤20%). Intra- and inter-day imprecision ranged between 1.5% and 9.5% and 0.7% and 12.6%, respectively. Intra- and inter-day inaccuracy ranged from 0.5% to 12.3% and from 0.7% to 7.1%, respectively. With regard to matrix effects, suppression was <27.5% in all cases. The method was applied to the analysis of several samples derived from forensic cases.

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Acknowledgments

We gratefully acknowledge the support of the INCITE (Consellería de Innovación e Industria, Xunta de Galicia) by the Investigation Proyect INCITE08PXIB208090PR.

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Authors and Affiliations

  1. Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain

    Oscar Quintela, Elena Lendoiro, Angelines Cruz, Ana de Castro & Manuel López-Rivadulla

  2. National University of Córdoba, Córdoba, CP X5000JLN, Argentina

    Alfredo Quevedo

  3. National Institute of Toxicology and Forensic Sciences, 41009, Seville, Spain

    Carmen Jurado

Authors
  1. Oscar Quintela
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  2. Elena Lendoiro
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  3. Angelines Cruz
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  4. Ana de Castro
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  5. Alfredo Quevedo
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  6. Carmen Jurado
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  7. Manuel López-Rivadulla
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Correspondence to Oscar Quintela.

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Quintela, O., Lendoiro, E., Cruz, A. et al. Hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples. Anal Bioanal Chem 396, 1703–1712 (2010). https://doi.org/10.1007/s00216-009-3393-5

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  • DOI: https://doi.org/10.1007/s00216-009-3393-5

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