A Study of Method Limit of Quantitation for 30 PFAS in Food

Importance of the Topic

The determination of trace levels of per- and polyfluoroalkyl substances (PFAS) in food has become critical for regulatory compliance and consumer safety. Recent European Union regulations and AOAC guidelines enforce stringent limits for PFAS in various food categories, demanding sensitive, reliable analytical methods.

Study Objectives and Overview

This study aimed to evaluate the method limit of quantitation (LOQ) for 30 PFAS in diverse food matrices. The approach combined QuEChERS extraction, Agilent Captiva EMR PFAS Food cartridge passthrough cleanup, and LC/MS/MS detection. Method performance was assessed against AOAC SMPR 2023.003 and EU Regulation 2023/915 requirements, and compared to the FDA C-010.03 method.

Methodology and Instrumentation

The key procedural steps included:

• Sample preparation by QuEChERS extraction to homogenize and extract PFAS from food.
• Enhanced matrix removal (EMR) via Captiva EMR PFAS Food cartridges for cleanup.
• Detection and quantitation using Agilent liquid chromatography tandem mass spectrometry (LC/MS/MS).
• LOQspiking determined as lowest spike yielding acceptable recovery and repeatability in 15 food matrices.
• LOQcal and method detection limit (MDL) calculated following 40 CFR Appendix B to Part 136 procedures.

Main Results and Discussion

LOQspiking values were established for each PFAS in 15 matrices, including infant formula, baby food, produce, dairy, seafood, meat, offal, and feed. Calculated LOQcal values met or exceeded AOAC and EU requirements for all but a few outliers caused by matrix background interference (e.g., 4:2 FTS in carrot, PFNA in beef). Comparison with FDA C-010.03 showed that the Agilent method achieved overall lower LOQcal levels across representative foods, attributed to the simplified cleanup, higher matrix removal efficiency, and allowance for larger sample sizes.

Benefits and Practical Applications

The validated method offers:

• Robust performance across a wide range of food matrices.
• Sensitivity meeting ultra-low EU regulatory targets.
• Reduced matrix effects leading to improved accuracy and precision.
• Streamlined workflow suitable for high-throughput food safety laboratories.

Future Trends and Potential Applications

Advances may include:

• Extension to novel or emerging PFAS analytes.
• Integration of high-resolution mass spectrometry (HRMS) for broader screening.
• Automation of sample preparation to increase throughput.
• Application in monitoring PFAS in environmental and biological samples.

Conclusion

The combination of QuEChERS, Captiva EMR PFAS cleanup, and LC/MS/MS provides a reliable, sensitive method for quantifying 30 PFAS in food. Method LOQspiking-A and LOQcal-A values satisfy AOAC SMPR 2023.003 and EU Regulation 2023/915, outperforming the FDA C-010.03 approach in sensitivity.

References

1. US Environmental Protection Agency. Definition and Procedure for the Determination of the Method Detection Limit, Revision 2, 40 CFR Appendix B to Part 136; December 2016.
2. AOAC International. Standard Method Performance Requirements (SMPR 2023.003) for Per- and Polyfluoroalkyl Substances (PFAS) in Produce, Beverages, Dairy Products, Eggs, Seafood, Meat Products, and Feed; 2023.
3. U.S. Food and Drug Administration. Chemical Analytical Manual, Compendium of Analytical Laboratory Methods, C-010.03 Determination of 30 Per- and Polyfluoroalkyl Substances (PFAS) in Food and Feed by LC-MS/MS; 2024.
4. European Commission. Commission Regulation (EU) 2023/915 of 25 April 2023 on Maximum Levels for Certain Contaminants in Food; 2023.
5. European Food Safety Authority. Guidance Document on Analytical Parameters for the Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Food and Feed, Version 1.2; May 2022.
6. Zhao L., Giardina M., Parry E. Determination of 30 Per- and Polyfluoroalkyl Substances in Infant Formula, Milk, and Eggs. Agilent Technologies Application Note; 2024.
7. Zhao L., Giardina M., Parry E. Determination of 30 Per- and Polyfluoroalkyl Substances in Baby Food. Agilent Technologies Application Note; 2024.
8. Zhao L., Giardina M., Parry E. Determination of 30 Per- and Polyfluoroalkyl Substances in Beef, Tuna, and Shrimp. Agilent Technologies Application Note; 2024.
9. Zhao L., Giardina M. Determination of 30 Per- and Polyfluoroalkyl Substances in Fruits, Vegetables, and Juices. Agilent Technologies Application Note; 2024.
10. Zhao L., Giardina M., Parry E. Determination of 30 Per- and Polyfluoroalkyl Substances in Bovine Kidney. Agilent Technologies Application Note; 2024.
11. Zhao L., Giardina M., Parry E. Determination of 30 Per- and Polyfluoroalkyl Substances in Dry Soybeans. Agilent Technologies Application Note; 2024.