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Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food

Analytical and Bioanalytical Chemistry volume 404, pages 2193–2201 (2012)Cite this article

Abstract

A sensitive and accurate method was developed and validated for simultaneous analysis of perfluoroalkyl carboxylic acids, sulfonic acids, and phosphonic acids (PFPAs) at low picograms per gram concentrations in a variety of food matrices. The method employed extraction with acetonitrile/water and cleanup on a mixed-mode co-polymeric sorbent (C8 + quaternary amine) using solid-phase extraction. High-performance liquid chromatographic separation was achieved on a C18 column using a mobile phase gradient containing 5 mM 1-methyl piperidine for optimal chromatographic resolution of PFPAs. A quadrupole time-of-flight high-resolution mass spectrometer operating in negative ion mode was used as detector. Method detection limits were in the range of 0.002 to 0.02 ng g−1 for all analytes. Sample preparation (extraction and cleanup) recoveries at a spiking level of 0.1 ng g−1 to a baby food composite were in the range of 59 to 98 %. A strong matrix effect was observed in the analysis of PFPAs in food extracts, which was tentatively assigned to sorption of PFPAs to the injection vial in the solvent-based calibration standard. The method was successfully applied to a range of different food matrices including duplicate diet samples, vegetables, meat, and fish samples.

Extracted high-resolution mass chromatograms of a PFPAs spiked at 0.06 ng g –1 to baby food, b PFSAs spiked at 0.02 ng g –1 to baby food, and c PFCAs spiked at 0.02 ng g –1 to baby food

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Acknowledgments

The authors acknowledge the European Union for the financial support through the PERFOOD project (KBBE-227525). Dr. Hermann Fromme (Bavarian Health and Food Authority, Munich, Germany) and Dr. Martin Schlummer (Fraunhofer IVV, Freising, Germany) are acknowledged for providing the duplicate diet samples. The authors thank Anne-Sofie Kärsrud for preparing the food samples. Wellington is acknowledged for the donation of isotopically mass-labeled standards.

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Authors and Affiliations

  1. Department of Applied Environmental Science (ITM), Stockholm University, 106 91, Stockholm, Sweden

    Shahid Ullah, Tomas Alsberg, Robin Vestergren & Urs Berger

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  1. Shahid Ullah
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  2. Tomas Alsberg
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  3. Robin Vestergren
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  4. Urs Berger
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Correspondence to Urs Berger.

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Ullah, S., Alsberg, T., Vestergren, R. et al. Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food. Anal Bioanal Chem 404, 2193–2201 (2012). https://doi.org/10.1007/s00216-012-6374-z

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  • DOI: https://doi.org/10.1007/s00216-012-6374-z

Keywords

  • PFCAs
  • PFSAs
  • PFPAs
  • Food samples
  • HPLC
  • HRMS