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HPLC-MS/MS method for the determination of perfluoroalkyl substances in breast milk by combining salt-assisted and dispersive liquid-liquid microextraction

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Abstract

The widespread use of perfluoroalkyl substances has resulted in the universal exposure of humans to these endocrine-disrupting chemicals, including the exposure of neonates through breastfeeding. The objective of this study was to develop a method to determine 10 perfluoroalkyl substances in breast milk (1-mL aliquot) by combining salt-assisted liquid-liquid extraction with dispersive liquid-liquid microextraction and using high-performance liquid chromatography-tandem mass spectrometry. Chemometric strategies were applied to optimize experimental parameters. The limit of quantification was 20 pg mL−1 for all analytes, and inter-day variability (evaluated as relative standard deviation) ranged from 8.2 to 13.8%. The method was validated by a recovery assay with spiked samples. Percentage recoveries ranged from 85.9 to 110.8%. The method was satisfactorily applied to assess target compounds in 20 breast milk samples from donors. Perfluorooctanoic acid, perfluorooctane sulfonate, and perfluorohexanoic acid were the most frequently detected analytes. This analytical procedure can provide useful information on newborn’s exposure to these xenobiotics.

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Acknowledgements

The authors gratefully acknowledge editorial assistance provided by Richard Davies.

Funding

This study was supported in part by research grants from the European Union Commission (H2020-EJP-HBM4EU), Biomedical Research Networking Center-CIBER de Epidemiología y Salud Pública (CIBERESP), and the Instituto de Salud Carlos III (ISCIII) (FIS-PI16/01820 and FIS-PI16/01858). The authors are also grateful to the ISCIII and the “Fondo Europeo de Desarrollo Regional” (ISCIII/FEDER) for the Sara Borrell postdoctoral research contract granted to F. Vela-Soria (grant no. CD17/00212) and the Miguel Servet Type I Program granted to C. Freire (grant no. MS16/00085).

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Authors and Affiliations

  1. Instituto de Investigación Biosanitaria (ibs.GRANADA), 18012, Granada, Spain

    Fernando Vela-Soria, Nicolas Olea & Carmen Freire

  2. Unidad de Neonatología, Hospital Universitario Virgen de las Nieves, 18012, Granada, Spain

    Laura Serrano-López

  3. Unidad de Gestión Clínica de Laboratorios, Hospital Universitario Clínico San Cecilio, 18016, Granada, Spain

    Javier García-Villanova & Tomás de Haro

  4. CIBER de Epidemiología y Salud Pública (CIBERESP), Madrid, Spain

    Nicolas Olea & Carmen Freire

  5. Centro de Investigación Biomédica (CIBM), Universidad de Granada, 18100, Granada, Spain

    Nicolas Olea & Carmen Freire

  6. Departamento de Radiología y Medicina Física, Universidad de Granada, 18071, Granada, Spain

    Nicolas Olea

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  1. Fernando Vela-Soria
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  2. Laura Serrano-López
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  3. Javier García-Villanova
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Correspondence to Fernando Vela-Soria.

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All women signed their informed consent, and the study was approved by the Research Ethics Committee of the hospital.

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Vela-Soria, F., Serrano-López, L., García-Villanova, J. et al. HPLC-MS/MS method for the determination of perfluoroalkyl substances in breast milk by combining salt-assisted and dispersive liquid-liquid microextraction. Anal Bioanal Chem 412, 7913–7923 (2020). https://doi.org/10.1007/s00216-020-02924-x

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