Determination of 30 Per- and Polyfluoroalkyl Substances in Infant Formula, Milk, and Eggs

Significance of the Topic

This work addresses the growing concern over per- and polyfluoroalkyl substances (PFAS) in infant formula, milk, and eggs. PFAS residues pose potential health risks and increasingly stringent regulations demand reliable methods for trace-level quantitation in complex food matrices.

Objectives and Study Overview

The study aimed to develop and validate a streamlined, multiresidue workflow for quantifying 30 PFAS in infant formula, milk, and eggs. Key goals included achieving low limits of quantitation (LOQs) in compliance with AOAC SMPR guidance and European regulatory requirements, while improving sample throughput and analytical robustness.

Methodology and Instrumentation Used

Sample preparation combined QuEChERS extraction with a novel Agilent Captiva EMR PFAS Food II passthrough cleanup cartridge, replacing time-consuming dispersive SPE and weak anion-exchange steps. LC/MS/MS analysis was performed on an Agilent 1290 Infinity II UHPLC coupled to a 6495D triple quadrupole mass spectrometer, using an InfinityLab PFC-free HPLC kit and a ZORBAX RRHD Eclipse Plus C18 column. Native PFAS standards and isotopically labeled internal standards were used for calibration.

Main Results and Discussion

The EMR mixed-mode cleanup delivered superior matrix removal, PFAS recovery (>80% for core targets), and >90% sample volume recovery, compared to traditional dSPE (<50%). Calibration curves spanned 20–10,000 ng/L with R² > 0.99 for all analytes. Validated LOQs met or exceeded SMPR requirements: ≤0.01 µg/kg for PFHxS, PFOA, PFNA, PFOS in infant formula and milk, and ≤0.3 µg/kg in eggs. Recoveries across three QC levels ranged 80–120% with relative standard deviations below 25%.

Benefits and Practical Applications of the Method

The simplified QuEChERS + EMR workflow reduces preparation time by two thirds, lowers solvent and consumable usage, and supports a single calibration set for multiple matrices. This approach enhances laboratory productivity and is readily adaptable for routine QA/QC and regulatory compliance testing of animal-origin foods.

Future Trends and Potential Applications

Emerging directions include extending the EMR cleanup to additional food and feed matrices, automation of cartridge-based workflows, and expansion to next-generation PFAS analytes. Integration with high-resolution MS platforms and miniaturized extraction techniques may further boost throughput and sensitivity.

Conclusion

The validated method employing Agilent Captiva EMR PFAS Food II passthrough cleanup with LC/MS/MS offers a rapid, sensitive, and robust solution for PFAS determination in infant formula, milk, and eggs. It meets stringent regulatory requirements while improving laboratory efficiency.

Reference

1. European Commission Regulation (EU) 2023/915 on PFAS maximum levels in foods.
2. AOAC SMPR 2023.003 for PFAS analysis in food and feed matrices.
3. U.S. EPA Method 533: LC-MS/MS analysis of PFAS in drinking water.
4. U.S. EPA Method 1633: LC-MS/MS determination of PFAS in environmental and tissue samples.
5. Genualdi, S. et al., Expandable PFAS method for food and feed, Anal. Bioanal. Chem. 2024.
6. Hwang, S. H. et al., QuEChERS and LC-MS/MS for PFAS in rice, Food Chemistry 2024.