PFAS Analysis in Food Packaging Using an Agilent 6495D Triple Quadrupole LC/MS

Significance of the Topic

Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants commonly found in food packaging. Their potential migration into food raises health concerns and drives tightening regulations. Sensitive, reliable analytical methods are essential to support compliance and protect consumers.

Objectives and Study Overview

This study aims to develop and validate a robust workflow for simultaneous quantification of 110 PFAS (73 native and 37 labeled compounds) in plastic food bag materials using an Agilent 6495D triple quadrupole LC/MS. Performance criteria include low detection limits, high linearity, and accurate recoveries across a broad PFAS range.

Methodology and Instrumentation

The workflow integrates a straightforward solvent extraction and dilute-and-shoot protocol:

• Sample Preparation: Plastic bag pieces (smaller than 5×5 mm) were spiked with native PFAS and a surrogate internal standard mix, then extracted with methanol at 60 °C using mechanical shaking and ultrasonication.
• Cleanup: Extracts were centrifuged and filtered through polypropylene syringe filters with nylon membranes.
• Dilution and Analysis: Filtered extracts were diluted 12.5-fold with water and an isotope performance standard before injection into the LC/TQ system.

Applied Instrumentation

• Agilent 1290 Infinity II LC with PFC-free conversion kit to minimize background contamination.
• Agilent Jet Stream ESI source on a 6495D triple quadrupole mass spectrometer operating in negative ion mode.
• ZORBAX RRHD Eclipse Plus C18 column (2.1×100 mm, 1.8 μm) and a 15-minute gradient with ammonium acetate in water and methanol.

Main Results and Discussion

The method achieved detection limits ≤0.2 μg/kg for all 73 native PFAS, with 45% of analytes reaching ≤0.05 μg/kg. Linearity exceeded R²=0.99 across calibration ranges (1–50,000 ng/L). Quality control samples spiked at 1, 10, and 50 μg/kg yielded recoveries of 65–135% for 95% of targets and precision (%RSD) ≤20%. Key PFAS (PFOA, PFOS, PFNA) demonstrated high reproducibility and clear chromatographic separation of isomers.

Benefits and Practical Applications

The streamlined extract-and-shoot approach eliminates time-consuming cleanup steps while maintaining sensitivity and reliability. The workflow supports routine high-throughput PFAS screening in food packaging, aiding manufacturers and regulators in compliance monitoring and risk assessment.

Future Trends and Applications

Emerging short-chain PFAS and novel fluorinated additives will require expanded target lists and improved high-resolution screening. Integration with non-targeted analysis and automated sample handling will further enhance throughput. Broader application to diverse food contact materials will support comprehensive exposure assessments.

Conclusion

The validated LC/TQ workflow on the Agilent 6495D system delivers robust, sensitive, and reproducible quantitation of a wide PFAS panel in food plastic bags. Its efficiency and performance enable effective monitoring under evolving regulatory frameworks and contribute to safer packaging practices.

References

• U.S. Environmental Protection Agency. PFAS Explained. 2024.
• National Institute of Environmental Health Sciences. Perfluoroalkyl and Polyfluoroalkyl Substances (PFAS). 2024.
• Consumer Reports. Dangerous PFAS Chemicals Are in Your Food Packaging. 2024.
• OECD. PFAS and Alternatives in Food Packaging. OECD Series on Risk Management No. 58; 2020.
• U.S. Food and Drug Administration. Market Phase-Out of PFAS Grease-Proofing Substances. 2024.
• Agilent Technologies. Consumables Ordering Guide, Application Note 5994-2357EN; 2024.
• Commission Regulation (EU) No 10/2011.
• Spring. Method Development and Screening of Extractable Organofluorine in Food Packaging; 2022.
• U.S. Environmental Protection Agency. EPA Method 1633; 2024.
• U.S. Environmental Protection Agency. Method Detection Limit Guidance; 2016.
• Wells G.; Prest H.; Russ W. C. Signal, Noise, and Detection Limits in Mass Spectrometry; Agilent Application Note 5990-7651EN; 2023.
• AOAC International. SMPR2023.003 for PFAS in Food and Feed; 2023.
• FDA Foods Program Compendium of Analytical Laboratory Methods: CAM.