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Multi-class method for biomonitoring of hair samples using gas chromatography-mass spectrometry

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Abstract

Currently, non-invasive biomonitoring of human exposure to organic pollutants bases upon the analysis mainly of urine and human breast milk. While mostly persistent organic pollutants are the center of interest, the aim of our study was to develop a method for the determination of different chemical classes of emerging pollutants (organophosphorus flame retardants, plastic additives such as phthalates, bisphenol A, insecticides, antimicrobials, preservatives and musk fragrances) in hair by gas chromatography–mass spectrometry. The preferred sample preparation included hydrolysis of the hair with trifluoroacetic acid in methanol followed by a liquid–liquid extraction using hexane/ethyl acetate. The validated method is characterized by recoveries higher than 77 % for most analytes, relative standard deviations below 16 % and limits of detection between 2 pg mg−1 (HHCB) and 292 pg mg−1 (propylparaben) using 50 mg of dry hair. After respective blank corrections, bis-(2-ethylhexyl)phthalate (DEHP) and the musk fragrance HHCB were the predominant compounds determined in all hair samples at concentrations between 32 and 59 ng mg−1 and 0.8–13 ng mg−1, respectively. The bactericide triclosan and the insect repellent N,N-diethyl-3-methylbenzamide (DEET) were detected in selected hair samples at 2 and 0.8 ng mg−1, respectively.

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Acknowledgments

The authors are grateful to the Escuela Politécnica Superior, University of Seville, Spain for supporting this work.

Conflict of interest

The authors declare that that there is no conflict of interest concerning the study presented.

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Authors and Affiliations

  1. Department of Analytical Chemistry, Escuela Politécnica Superior, University of Seville, C/ Virgen de África 7, 41011, Seville, Spain

    Julia Martín & Esteban Alonso

  2. Department of Analytical Chemistry, Helmholtz Centre for Environmental Research - UFZ, Permoserstraße 15, 04318, Leipzig, Germany

    Monika Möder & Thorsten Reemtsma

  3. Institute of Laboratory Medicine, University of Leipzig, Liebigstraße 27b, 04103, Leipzig, Germany

    Alexander Gaudl

Authors
  1. Julia Martín
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  2. Monika Möder
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  3. Alexander Gaudl
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  4. Esteban Alonso
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  5. Thorsten Reemtsma
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Corresponding author

Correspondence to Monika Möder.

Electronic supplementary material

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ESM 1

Electronic Supplementary Material. Table S1 Overview of procedures reported for the determination of different groups of organic pollutants in human hair. Fig. S1 Total ion chromatograms of GC-MS(SIM) analysis of hair extracts (non-spiked) a) treated with MeOH/TFA and extracted with ethyl acetate and b) treated with NaOH solution, then adjusted to pH 3 with acetic acid and extracted with ethyl acetate. Table S2 Blanks of the solvents used for the individual sample preparation steps and of the complete method without hair (n = 2). Values are given as amount per injection (PDF 453 kb)

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Martín, J., Möder, M., Gaudl, A. et al. Multi-class method for biomonitoring of hair samples using gas chromatography-mass spectrometry. Anal Bioanal Chem 407, 8725–8734 (2015). https://doi.org/10.1007/s00216-015-9026-2

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  • DOI: https://doi.org/10.1007/s00216-015-9026-2

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