The analysis of perfluoroalkyl substances at ppt level in milk and egg using UHPLC-MS/MS

ABSTRACT

Per- and poly-fluorinated substances (PFASs) are man-made chemicals that have been used for a variety of applications and can end up in the food chain. New opinions on the risk assessment were recently published by the European Food Safety Authority, emphasising the need for more sensitive methods. From this, minimum required LOQs for the analytical method for analysis of milk and egg have been calculated for perfluorooctanoic acid (PFOA) and GenX (hexafluoropropylene oxide dimer acid, HFPO-DA). A fully validated method is described for analysis of 13 PFASs, including PFOA and HFPO-DA, in milk and egg. All compounds, except perfluorodecane sulphonate (PFDS), can be quantitatively determined in these matrices with a trueness ranging from 87% to 119% and a relative within-laboratory reproducibility between 12% and 41%. Also the method proved suitable for confirmation of the identity of the individual PFASs. The LOQ for HFPO-DA in milk and egg is 0.05 ng g⁻¹, well below the calculated required LOQ. For PFOA in egg the determined LOQ is 0.025 ng g⁻¹, nicely below the required level of 0.03 ng g⁻¹. In milk the required LOQ was not achieved: 0.005 instead of 0.003 ng g⁻¹. However, on six out of eight days an LOQ of 0.0025 ng g⁻¹ was demonstrated. It is concluded that the required LOQs are achievable when instrument performance is optimal. The current method can be expanded with long chain PFASs by using a cellulose filter instead of the PTFE filter vials. The presented method was applied for a small-scale study in The Netherlands.

GRAPHICAL ABSTRACT

KEYWORDS:

• Perfluoroalkyl substances
• PFAS
• milk
• egg
• validation
• LC-MS/MS
• GenX
• PFOA
• PFDS

Acknowledgments

The work presented was funded by the Dutch Ministry of Economic affairs (project WOT-02-001-011 and 017). We thank our colleagues from the WFSR quality department for critically assessing the validation plan and report.

Disclosure statement

No financial interest or benefit has arisen from the direct applications of the presented research.

Additional information

Funding

This work was supported by the Dutch Ministry of agriculture, nature and food quality [WOT-02-001-011 and 017].