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New miniaturized clean-up procedure for hair samples by means of microextraction by packed sorbent: determination of cocaine and metabolites

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Abstract

Cocaine is still one of the most commonly used illicit substances worldwide, with an estimated 4 million users in Europe in the last year. Hair samples have been widely used for the determination of episodic or repeated consumption of this substance, but the use of miniaturized techniques for hair sample clean-up has been challenging due to the sample complexity. Despite hair’s complex matrix, MEPS provides a method that is fast, reduces the volume of extraction solvents used, and offers low-cost options (since extraction beds may be reused several times). Microextraction by packed sorbent using a mixed-mode sorbent was optimized for hair sample clean-up in order to determine cocaine, benzoylecgonine, ecgonine methyl ester, norcocaine, cocaethylene and anhydroecgonine methyl ester by gas chromatography coupled to tandem mass spectrometry. The method was fully validated according to internationally accepted criteria, presenting good linearity between the limits of quantification (0.01–0.15) and 5 ng/mg. Precision and accuracy resulted in coefficients of variation typically lower than 15%, with mean relative errors within ±15% for all compounds, except for the limit of quantification (±20%). The present work describes the first application of microextraction by packed sorbent for the concentration of cocaine and metabolites extracted from hair samples.

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Acknowledgements

The authors acknowledge all the staff of Casas de Santiago (Belmonte, Portugal). The authors wish further to thank Hernâni Marques and Marlene Mota for their laboratorial assistance.

Funding

This work was partially supported by CICS-UBI which is financed by National Funds from Fundação para a Ciência e a Tecnologia (FCT) and Community Funds (UIDB/00709/2020). T. Rosado acknowledges the Centro de Competências em Cloud Computing in the form of a fellowship (C4_WP2.6_M1 – Bioinformatics; Operação UBIMEDICAL – CENTRO-01-0145-FEDER-000019 – C4 – Centro de Competências em Cloud Computing), supported by Fundo Europeu de Desenvolvimento Regional (FEDER) through the Programa Operacional Regional Centro (Centro 2020).

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Authors and Affiliations

  1. Health Sciences Research Centre, Faculty of Health Sciences of the University of Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-556, Covilhã, Portugal

    Tiago Rosado & Eugenia Gallardo

  2. Pharmaco-Toxicology Laboratory-UBIMedical, University of Beira Interior, Estrada Municipal 506, 6200-284, Covilhã, Portugal

    Tiago Rosado & Eugenia Gallardo

  3. C4 - Cloud Computing Competence Centre, University of Beira Interior, 6201-001, Covilhã, Portugal

    Tiago Rosado

  4. Faculty of Medicine, University of Coimbra, 3000-548, Coimbra, Portugal

    Duarte N. Vieira

  5. Laboratory of Forensic Chemistry and Toxicology, National Institute of Legal Medicine and Forensic Sciences, South Branch, Rua Manuel Bento de Sousa, 3, 1169-201, Lisbon, Portugal

    Mário Barroso

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  1. Tiago Rosado
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Correspondence to Eugenia Gallardo.

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This study was conducted according to ethical standards and was approved by the ethics committee from Casas de Santiago. All analyses were carried out according to the ethical standards of the institution, and the analyzed samples were obtained from individuals who provided informed consent for their use (including the drug-free samples used in the validation experiments, provided by laboratory staff).

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Rosado, T., Gallardo, E., Vieira, D.N. et al. New miniaturized clean-up procedure for hair samples by means of microextraction by packed sorbent: determination of cocaine and metabolites. Anal Bioanal Chem 412, 7963–7976 (2020). https://doi.org/10.1007/s00216-020-02929-6

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