Development of an LCMS Methodology to Characterize and Quantitate Fluorinated Compounds in Consumer Products

Significance of the topic

Per- and polyfluorinated alkyl substances (PFAS) have been widely used since the 1940s in consumer goods for their water-, oil- and heat-resistant properties. However, their environmental persistence and potential health impacts have raised significant regulatory and public concerns over contamination and bioaccumulation.

Aims and study overview

This study aimed to develop and validate a standardized LC–MS/MS methodology for the quantitative analysis of 46 PFAS and 25 isotopically labeled surrogates across diverse consumer product matrices. Collaborative efforts between Shimadzu Scientific Instruments, RJ Lee Group, and ASTM sought to establish reproducible protocols for regulatory compliance and interlaboratory consistency.

Methodology

Solid samples (0.5 g) of plastics, non-stick foils, or Ottawa sand were spiked with surrogate solutions, vortexed, pH-adjusted (pH 9–10), tumbled for 2 h, and filtered through 0.2 µm syringe filters. Post-filtration, samples were acidified (pH 3–4), centrifuged, and directly injected without solid-phase extraction, streamlining the workflow.

Used Instrumentation

The analysis employed a Shimadzu LCMS-8060NX triple quadrupole system coupled to a Nexera UHPLC with a Shimadzu Nexcol PFAS Delay column (50 × 3 mm, 5 µm) and a Shim-pack Scepter C18-120 analytical column (2.1 × 100 mm, 3 µm). Mobile phases were ammonium acetate in water/acetonitrile (95/5) and acetonitrile, with a gradient elution at 0.45 mL/min and 40 µL injection. Negative ESI, optimized collision energies, and MS settings ensured sensitivity across a 100–4000 ng/kg reporting range.

Main results and discussion

Calibration curves for all analytes demonstrated excellent linearity (RF %RSD < 20 %). Surrogate recoveries in sand, plastic, and foil matrices ranged from 70 % to 130 % with %RSD < 15 %. The method eliminated the need for SPE, reducing analysis time and cost while maintaining robust repeatability and accuracy across matrices.

Benefits and practical applications

This approach provides a high-throughput, cost-effective solution for routine PFAS monitoring in consumer products, supporting quality control, regulatory compliance, and risk assessment. Coverage of a broad PFAS panel and simplified sample preparation enhances laboratory efficiency.

Future trends and potential applications

Anticipated advancements include expansion of target analyte lists, integration of high-resolution mass spectrometry for non-target screening, automation of sample handling, and adoption of green chemistry principles. Standardization via ASTM and other bodies will further harmonize PFAS analysis globally.

Conclusion

The developed LC–MS/MS method offers a validated, reproducible framework for quantifying a wide range of PFAS in diverse consumer product matrices. By streamlining sample preparation and ensuring reliable performance, it lays the groundwork for standardized testing protocols.

Reference

1. ATSDR. Per- and Polyfluoroalkyl Substances (PFAS) Toxicity Profile. Available at https://www.atsdr.cdc.gov/pfas/