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Solid phase microextraction and gas chromatography–mass spectrometry methods for residual solvent assessment in seized cocaine and heroin

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Abstract

A simple sample pre-treatment method based on solid phase microextraction (SPME) and gas chromatography–mass spectrometry (GC-MS) has been optimized and validated for the assessment of 15 residual solvents (2-propanol, 2-methylpentane, 3-methylpentane, acetone, ethyl acetate, benzene, hexane, methylcyclohexane, methylcyclopentane, m-xylene, propyl acetate, toluene, 1,2,4-trimethylbenzene, dichloromethane, and ethylbenzene) in seized illicit cocaine and heroin. DMSO and DMF as sample diluents were found to offer the best residual solvent transference to the head space for further adsorption onto the SPME fiber, and the developed method therefore showed high sensitivity and analytical recovery. Variables affecting SPME were fully evaluated by applying an experimental design approach. Best conditions were found when using an equilibration time of 5 min at 70 °C and headspace sampling of residual solvents at the same temperature for 15 min. Method validation, performed within the requirements of international guidelines, showed excellent sensitivity, as well as intra- and inter-day precision and accuracy. The proposed methodology was applied to 96 cocaine samples and 14 heroin samples seized in Galicia (northwestern Spain) within 2013 and 2014.

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Acknowledgments

The authors wish to thank the European Commission Directorate-General Justice (JUST/2011/ISEC/DRUGS/AG/3670) for support in this investigation.

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Authors and Affiliations

  1. Institute of Forensic Sciences, Faculty of Medicine, Universidade de Santiago de Compostela, Rúa San Francisco, s/n, 15782, Santiago de Compostela, Spain

    Pamela Cabarcos, Iván Álvarez-Freire, María Jesús Tabernero & Ana María Bermejo

  2. Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain

    Paloma Herbello-Hermelo, Antonio Moreda-Piñeiro & Pilar Bermejo-Barrera

Authors
  1. Pamela Cabarcos
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  2. Paloma Herbello-Hermelo
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  3. Iván Álvarez-Freire
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  4. Antonio Moreda-Piñeiro
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  5. María Jesús Tabernero
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  6. Ana María Bermejo
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  7. Pilar Bermejo-Barrera
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Correspondence to Ana María Bermejo.

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Cabarcos, P., Herbello-Hermelo, P., Álvarez-Freire, I. et al. Solid phase microextraction and gas chromatography–mass spectrometry methods for residual solvent assessment in seized cocaine and heroin. Anal Bioanal Chem 408, 6393–6402 (2016). https://doi.org/10.1007/s00216-016-9754-y

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  • DOI: https://doi.org/10.1007/s00216-016-9754-y

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