An LC-MS/MS method for the quantitative determination of 57 per- and polyfluoroalkyl substances at ng/kg levels in different food matrices

Abstract

To enable the monitoring of a wide scope of per- and polyfluoroalkyl substances (PFAS) in the ng/kg level in foodstuffs, an LC-MS/MS method comprising 57 analytes was developed and validated in seven different matrices (milk powder, milk-based infant formula, meat-based baby food puree, fish and fish oil, fresh egg, and soluble coffee). The analytical approach was based on an acetonitrile:water extraction followed by solid phase extraction clean-up with subsequent quantification of the extracted analytes either by isotope dilution (55 compounds) or by standard addition (2 compounds) mass spectrometry. The validation criteria followed the guidance document for the analysis of PFAS issued by the European Union Reference Laboratory for Halogenated Persistent Organic Pollutants. The lowest limits of quantification (LOQs) for the four recently regulated compounds (L-PFOS, PFOA, PFNA, L-PFHxS) were set at 0.010 µg/kg in baby and infant foods (as sold) but also in dairy ingredients. Exception was for PFOA in milk powder due to too large variability in the repeatability. Applicability of the method was further demonstrated in 37 commodity check matrices. Overall validation data demonstrated the robustness of the method for most of the compounds and the LOQs achieved were low enough to ensure compliance with Commission Regulation EU 2022/2388 but also to support future collection of occurrence data in ng/kg level in food.

Keywords:

• Per- and polyfluoroalkyl substances
• PFAS
• food
• mass spectrometry
• LC-MS/MS

Author contributions

Xanthippe Theurillat: Conceptualisation, Methodology, Investigation, Validation, Formal analysis, Resources, Visualisation, Roles/Writing – original draft; Writing – review & editing. Claudia Mujahid: Conceptualisation, Methodology, Investigation, Validation, Formal analysis, Resources, Roles/Writing – original draft; Writing – review, Visualisation; Bjorn Eriksen: Conceptualisation, Methodology, Investigation, Validation, Formal analysis, Resources, Roles/Writing – original draft; Writing – review, Visualisation; Ashley Griffin: Methodology, Validation, Formal analysis, Resources, Writing – review & editing, Visualisation; Andrew Savage: Methodology, Validation, Formal analysis, Resources, Writing – review & editing, Visualisation; Thierry Delatour: Conceptualisation, Investigation, Resources, Writing – review & editing; Pascal Mottier: Conceptualisation, Investigation, Resources, Writing – review & editing, Project administration.

Disclosure statement

The authors are employees of the Société des Produits Nestlé SA – Nestlé Research Lausanne.