Shimadzu Journal Vol 11 (Issue 1)

Significance of the Topic

Per- and polyfluoroalkyl substances (PFAS) are a large family of synthetic chemicals renowned for their exceptional thermal, chemical, and water-repellent properties. Their resistance to degradation has led to global persistence in water, soil, biota, and human blood. Drinking water constitutes a major exposure pathway, and regulatory agencies worldwide are tightening limits for key PFAS such as PFOA, PFOS, and PFHxS to protect public health.

Objectives and Overview of the Study

This work presents advanced analytical strategies for comprehensive PFAS monitoring in water. We illustrate: 1) a highly sensitive on-line SPE-LC-MS/MS method for 44 PFAS (including all compounds in EU Directive 2020/2184) using the Shimadzu LCMS-8060NX; 2) an untargeted screening approach on the high-resolution Q-TOF LCMS-9030 (HRAM-DIA) to discover known and novel PFAS; 3) compliance analysis of 40 PFAS per EPA Draft Method 1633 on the triple-quad LCMS-8050; and 4) precise quantitation of PFOA, PFOS, and PFHxS at sub-ng/L levels in drinking water using the LCMS-8050.

Methodology and Instrumentation

• On-line SPE coupled to UHPLC-MS/MS: EVOLUTE® SPE cartridge, Shim-pack Scepter C18 analytical column, delay column to block PFAS background.
• Shimadzu LCMS platforms: LCMS-8060NX TQ, Nexera X3 UHPLC; LCMS-9030 Q-TOF for HRAM-DIA screening; LCMS-8050 TQ for targeted methods (EPA 1633, 537.1, 533).
• Data acquisition: MRM for quantitation, HRAM-DIA deconvolution for discovery, LabSolutions Insight Explore for formula filtering, MS/MS spectral matching, and structural elucidation.
• Calibration and QA/QC: isotope-dilution, 7-point curves, method detection limits at low ppt; performance checks with internal standards and surrogate spikes in reagent water and wastewater.

Main Results and Discussion

The on-line SPE-LCMS-8060NX method achieved linearity (R² ≥ 0.99) across 0.5–100 ng/L with LOQs down to 0.5 ng/L for most analytes and RSDs < 20 %. Untargeted HRAM-DIA screening on the Q-TOF identified 16 PFAS-like species in real water, with spectral matches to in-house and MS-DIAL libraries, plus structural assignment via ChemSpider. The LCMS-8050 met EPA 1633 QC criteria for all 40 PFAS, with IDLs from 0.01–1.9 ng/mL and recoveries of 80–116 %. Drinking water quantitation of PFOA, PFOS, and PFHxS at 0.2 ng/L exhibited 82–103 % recovery and < 4 % RSD.

Benefits and Practical Applications

This unified, single-vendor suite addresses both routine compliance testing and research-grade screening. On-line SPE eliminates manual sample prep, boosting throughput and reproducibility. HRAM-DIA expands coverage to unknown PFAS, supporting source identification and risk assessment. Robust triple-quad methods deliver reliable quantitation in drinking and wastewater monitoring labs under evolving regulations.

Future Trends and Possibilities

Future developments will focus on sub-ppt sensitivity, direct injection on-line SPE, expanded high-resolution suspect- and non-target workflows, machine-learning-driven spectral deconvolution, and portable field deployable MS platforms. Integration with IoT-enabled automatic samplers and cloud-based data analytics will further enhance real-time water quality surveillance.

Conclusion

Shimadzu’s advanced LC-MS/MS and Q-TOF technologies provide a comprehensive solution for PFAS analysis, from high-throughput regulatory testing to untargeted discovery of emerging contaminants. The methods described meet stringent detection limits, ensure data quality, and offer a scalable path toward next-generation environmental monitoring.

Reference

• DIRECTIVE (EU) 2020/2184 on drinking water quality
• EPA Draft Methods 537.1, 533, and 1633 for PFAS analysis