Total Workflow for the Sensitive Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Fish, Meat, Edible Offal and Eggs

Importance of the Topic

Per- and polyfluoroalkyl substances (PFAS) are chemically stable compounds widely used in industrial and consumer products. Their persistence and potential health risks have led to increased scrutiny of dietary exposure. Monitoring PFAS in consumable matrices such as fish, meat, offal, and eggs is crucial to assess human intake and ensure food safety in line with EFSA and FDA guidelines.

Objectives and Study Overview

This study develops and evaluates a sensitive analytical workflow for the determination of 30 PFAS in complex food commodities: salmon, tilapia, ground beef, beef liver, beef kidney, and chicken eggs. The method aims to achieve reliable recoveries across diverse compound classes and meet regulatory criteria at trace concentration levels (0.1–5 ng/g).

Methodology and Sample Preparation

An alkaline digestion was followed by solid-phase extraction using a weak anion exchange sorbent to isolate PFAS from homogenized food samples. Samples were spiked at 0.1, 1.0, and 5 ng/g in quintuplicate to assess accuracy and precision. Isotopically labeled standards were added to evaluate recoveries. Alternative SPE using Oasis HLB was noted but found unsuitable for the full PFAS panel due to selectivity limitations.

Applied Instrumentation

• Liquid Chromatography: ACQUITY UPLC I-Class Plus with PFAS Kit
• Column: ACQUITY BEH C18, 2.1 × 100 mm, 1.7 μm; Temperature: 35 °C
• Mobile Phases: A) Water + 2 mM ammonium acetate; B) Methanol + 2 mM ammonium acetate
• Mass Spectrometry: Xevo TQ-XS triple quadrupole with electrospray ionization, positive mode; desolvation: 350 °C, 900 L/h; capillary voltage: 0.5 kV

Main Results and Discussion

Recovery rates for most PFAS fell within the FDA’s acceptable range (40–120%), with exceptions for neutral sulfonamides lost during the WAX SPE wash step and certain long-chain carboxylates in egg and fish extracts. Analysis of NIST SRM 1947 (Lake Michigan Fish Tissue) over eight replicates yielded results consistent with certified values for PFNA, PFDA, PFUnDA, and PFTriDA, confirming method accuracy. Real sample testing detected PFOS in beef liver (0.76 ng/g) and multiple short-chain PFAS (PFPeA, PFHxA, PFHpA, PFOA) in eggs at concentrations of 0.13–0.29 ng/g.

Benefits and Practical Applications

The proposed workflow offers a streamlined, robust approach for regulatory laboratories and research institutions to quantify a broad PFAS panel in food matrices. Its sensitivity supports compliance monitoring at low ng/g levels, aiding risk assessment and exposure studies.

Future Trends and Applications

Advances may include automation of sample preparation, expansion of compound coverage to emerging PFAS, and integration with high-resolution mass spectrometry for non-target screening. Miniaturized extraction formats and data-driven workflows will further enhance throughput and traceability.

Conclusion

A validated, comprehensive method enables reliable PFAS quantitation across diverse food commodities, meeting regulatory performance criteria. The approach demonstrates accuracy, sensitivity, and applicability for routine monitoring and exposure assessment.

Reference

1. EFSA CONTAM Panel. Risk to human health related to PFAS in food. EFSA Journal. 2020;18(9).
2. FDA. Analytical results of testing food for PFAS from environmental contamination. June 2021.