Analysis of Per- and Polyfluoroalkyl Substances (PFAS) Specified in EPA M537.1 Using the Triple Quadrupole LCMSTM-8045

Importance of the Topic

Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants used extensively in industrial and consumer products. Their chemical stability and widespread use have led to global detection in water supplies, raising public health concerns. Reliable quantitation of PFAS at low concentrations in drinking water is essential for regulatory compliance and risk assessment.

Study Objectives and Overview

This study evaluates the performance of the Shimadzu LCMS-8045 triple quadrupole mass spectrometer for quantifying 25 PFAS compounds according to EPA Method 537.1. The goal was to verify instrument sensitivity, accuracy, and precision while meeting all method quality criteria.

Methodology

A 250 mL sample volume was extracted and concentrated to 1 mL before injection. Ten calibration standards (1.25–100 ppb) were prepared, and multiple reaction monitoring (MRM) transitions were optimized by flow injection analysis. A delay column (Shim-pack XR-ODS) minimized PFAS background contamination. Chromatographic separation used a Shim-pack Velox C18 column with a gradient of 20 mM ammonium acetate (A) and methanol (B). The mobile phase flow rate was 0.25 mL/min at 40 °C.

Instrumentation Used

• Shimadzu LCMS-8045 triple quadrupole MS
• Nexera X2 UHPLC system
• Shim-pack XR-ODS (50 × 2 mm) delay column
• Shim-pack Velox C18 (2.1 × 150 mm, 2.7 µm)
• Electrospray ionization in negative mode

Main Results and Discussion

Calibration curves showed excellent linearity (R² > 0.99). Recoveries for all target PFAS ranged from 84 % to 112 % at low (80 ppt), mid (200 ppt), and high (400 ppt) levels. Method detection limits spanned 0.48–1.64 ppt, well below the 2 ppt requirement. Precision and accuracy studies at 40 ppt and 80 ppt achieved recoveries within ±15 % and %RSD < 20 %. Peak shapes for early eluters (PFBS, PFHxA) met asymmetry criteria.

Benefits and Practical Applications

The LCMS-8045 delivers rapid, reliable, and highly sensitive PFAS quantitation in drinking water, facilitating compliance with EPA Method 537.1. The lower injection volume (5 µL) compared to the official method reduces consumable usage and operational costs. Laboratories can upgrade easily to LCMS-8050 or LCMS-8060 for even lower detection limits.

Future Trends and Potential Applications

Advances in high-resolution MS and novel sample preparation will expand PFAS target lists and improve detection limits. Automation of sample cleanup and integration with data processing platforms will enhance throughput. Emerging regulations may drive analysis of additional PFAS classes in environmental, food, and biological matrices.

Conclusion

The Shimadzu LCMS-8045 exceeds EPA Method 537.1 requirements for sensitivity, accuracy, and precision in PFAS analysis. Its robust performance and low detection limits make it a practical solution for routine drinking water monitoring and environmental research.

References

1. US EPA. Method 537.1: Detections of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and LC-MS/MS, Version 1.0, November 2018.
2. Lindstrom, A. B., Strynar, M. J., & Libelo, E. L. Polyfluorinated Compounds: Past, Present, and Future. Environmental Science & Technology, 2011.
3. US EPA. Basic Information about Per- and Polyfluoroalkyl Substances (PFAS), 2020.
4. US EPA. Drinking Water Health Advisories for PFOA and PFOS, 2016.