Analysis of 28 EU Regulated and Recommended PFAS in Food via LC-MS/MS – Part 1: Vegetable, Fruit, and Baby Food

Importance of the Topic

Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants with potential adverse health effects. Their presence in agricultural products and processed foods has prompted stringent EU regulations. Sensitive, accurate monitoring of PFAS in fruits, vegetables, and baby food is essential to ensure food safety and regulatory compliance.

Study Objectives and Overview

This work aimed to develop and validate a single LC-MS/MS method capable of detecting and quantifying 28 EU-regulated and recommended PFAS in tomato, apple, and baby food matrices at ultra-trace levels. The method was designed to meet or exceed the criteria set forth in Commission Recommendation (EU) 2022/1431 and related regulatory guidance.

Methodology and Instrumentation

Samples were extracted using an alkaline methanolic solution and cleaned up with a novel bilayer SPE cartridge combining graphitized carbon black (GCB) and weak anion exchange (WAX) phases. Isotope-labeled extraction and injection internal standards were incorporated to correct for recovery, matrix effects, and instrumental variability. Liquid chromatography employed a short ACQUITY Premier UPLC BEH C18 column coupled with an isolator column to achieve baseline separation of linear and branched PFAS isomers. Detection was performed on a Xevo TQ Absolute tandem mass spectrometer in negative electrospray ionization mode.

Used Instrumentation

• ACQUITY PREMIER UPLC system with PFAS Analysis Kit
• ACQUITY Premier UPLC BEH C18, 2.1×50 mm, 1.7 µm column
• Atlantis Premier BEH C18 AX isolator column
• Xevo TQ Absolute mass spectrometer
• waters_connect software for data processing

Main Results and Discussion

• Instrument limits of detection as low as 0.0004 ng/mL; method LOQs down to 0.0005 µg/kg
• Recoveries ranged from 87 % to 116 % for mandatory PFAS and 65 % to 131 % for additional PFAS
• Repeatability (RSDr) ≤ 10 % across all matrices and fortification levels
• Excellent chromatographic separation of linear vs. branched isomers for accurate quantification
• Effective recovery of neutral PFAS (FOSA); low recoveries for capstone A/B due to zwitterionic properties; PFBA contamination in solvents requires further control

Benefits and Practical Applications

• Single-run method covering 28 PFAS conforms to EU regulatory requirements
• 50 % reduction in analysis time compared to previous UPLC workflows
• Robust SPE cleanup effectively handles both ionic and neutral PFAS
• High sensitivity enables monitoring of PFAS at ultra-trace concentrations in food

Future Trends and Applications

Part 2 of the study will extend the workflow to animal-derived food products. Further efforts will focus on mitigating PFBA contamination, enhancing capstone quantification, automating sample preparation, integrating high-resolution mass spectrometry, and expanding the PFAS analyte panel to address evolving regulatory requirements.

Conclusion

The optimized LC-MS/MS method combining bilayer GCB/WAX SPE cleanup and Xevo TQ Absolute detection delivers reliable, sensitive, and efficient analysis of 28 PFAS in vegetable, fruit, and baby food matrices. It meets current EU guidelines and provides a robust platform for routine regulatory monitoring. Future work will broaden its applicability to animal products.

References

1. Commission Regulation (EU) 2022/2388, amending Regulation (EC) No 1881/2006.
2. Commission Recommendation (EU) 2022/1431 on monitoring PFAS in food.
3. Commission Implementing Regulation (EU) 2022/1428 on sampling and analysis methods for PFAS.
4. EURL for halogenated POPs, Guidance Document on PFAS in Food and Feed (2022).
5. AOAC SMPR® 2023.003, PFAS in various food and feed matrices.
6. Dreolin N. et al., Waters White Paper 720007905 (2023).
7. Organtini K. et al., Waters Application Note 720007687 (2022).
8. Adams S. et al., Waters Application Note 720008108 (2023).
9. Magnusson B. and Örnemark U., Eurachem Guide (2nd ed., 2014).
10. Theurillat X. et al., Food Additives & Contaminants A, 40(7):862–877 (2023).