Analysis of Per- and Polyfluoroalkyl Substances (PFAS) Specified in EPA M8327 using the LCMS-8050 Triple Quadrupole Mass Spectrometer

Significance of the Topic

The widespread use and persistence of per- and polyfluoroalkyl substances (PFAS) in consumer and industrial applications have led to their global distribution in non-potable waters. Due to potential health effects including reproductive, hepatic, renal, and immunological impacts, sensitive and reliable monitoring of PFAS at low ng/L concentrations is essential for environmental protection and regulatory compliance.

Objectives and Study Overview

This study evaluates the performance of the Shimadzu LCMS-8050 triple quadrupole mass spectrometer for the direct analysis of 24 target PFAS and 19 isotope-labeled surrogates in groundwater, surface water, and wastewater according to draft EPA Method 8327.

• Demonstrate quantitation limits at or below 5 ppt for all analytes
• Verify linearity, accuracy, and precision across a 5–200 ppt calibration range
• Assess method robustness in diverse environmental matrices
• Confirm suitability for rapid, high-throughput workflows

Methodology and Instrumentation

Samples were diluted 1:1 with methanol containing 0.1% acetic acid, vortexed, and filtered prior to direct injection. Chromatographic separation employed a phenyl-hexyl analytical column with an in-line delay column to eliminate system PFAS contamination. A 21-minute gradient at 0.3 mL/min delivered baseline resolution of all analytes. MRM transitions were optimized by flow-injection analysis.

Used Instrumentation

• Shimadzu Nexera UHPLC coupled to LCMS-8050 triple quadrupole
• Shim-pack GIST Phenyl-Hexyl analytical column (2.1×100 mm, 3 µm)
• Shim-pack XR-ODS delay column (3×50 mm, 2.2 µm)
• Mobile phases: ammonium acetate in water/acetonitrile
• MRM acquisition with at least two transitions per compound

Main Results and Discussion

The method consistently achieved:

• Limits of quantitation ≤5 ppt for all target PFAS
• Calibration linearity (r2>0.99) with 1/x weighting
• Accuracy within 50–150% at the lowest level and 70–130% at higher levels
• Precision (RSD) ≤20% across all matrices
• Effective removal of system-derived PFAS by the delay column
• Maintained peak shape and resolution in groundwater, surface water, and wastewater

Benefits and Practical Applications of the Method

The direct injection approach eliminates extensive sample cleanup, supports high sample throughput with a 21-minute run time, and meets draft EPA Method 8327 criteria. Laboratories transitioning from ASTM D7979 workflows can readily adopt this protocol for routine PFAS surveillance in environmental monitoring, wastewater treatment, and regulatory testing.

Future Trends and Possibilities

• Implementation of isotopic dilution for enhanced quantitation
• Further reduction of detection limits through optimized source conditions
• Expansion to emerging PFAS and replacement chemistries
• Integration of online SPE or automated sample preparation
• Application of high-resolution MS for non-target screening
• Increased regulatory adoption and standardization of EPA Method 8327

Conclusion

The Shimadzu LCMS-8050 delivers precise, accurate, and sensitive quantitation of PFAS in challenging environmental matrices, exceeding the performance requirements of draft EPA Method 8327 and enabling rapid, high-throughput monitoring of persistent organic pollutants.

References

• 1. Environmental Science and Technology Polyfluorinated Compounds Past Present and Future
• 2. Agency for Toxic Substances and Disease Registry Per- and Polyfluoroalkyl Substances PFAS and Your Health
• 3. U.S. EPA Per- and Polyfluoroalkyl Substances PFAS
• 4. National Institute of Environmental Health Sciences Per-fluorinated Chemicals PFCs
• 5. U.S. EPA Basic Information about PFAS
• 6. U.S. EPA Drinking Water Health Advisories for PFOA and PFOS
• 7. ASTM D7979-17 Standard Test Method for Determination of PFAS in Water Sludge Influent Effluent and Wastewater by LC-MS/MS
• 8. ASTM D7979-17 Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water Sludge Influent Effluent and Wastewater by LC-MS/MS
• 9. Shimadzu Analysis of PFAS Specified in EPA M537.1 Using LCMS-8045 Brahm Prakash et al