Extended Evaluation of Method Performance for PFAS & Cyanotoxins Analysis Using a Single LC-MS/MS in Water

Importance of the Topic

Per- and polyfluoroalkyl substances (PFAS) and cyanotoxins are persistent environmental pollutants that threaten water safety and human health. Regulatory agencies worldwide have established stringent methods for their detection, driving the need for efficient, reliable, and high-throughput analytical solutions.

Study Objectives and Overview

This work evaluates the performance of a single Shimadzu LCMS-8060RX triple quadrupole mass spectrometer for simultaneous analysis of PFAS (EPA Method 533) and two sets of cyanotoxins (EPA Methods 544 and 545). The goal was to demonstrate seamless method switching, robust quantification, and operational stability over extended analytical runs.

Methodology

Standard preparation followed EPA protocols: PFAS standards (0.5–50 µg/L) in methanol/water; anatoxin-a (0.02–20 µg/L) and cylindrospermopsin (0.005–10 µg/L) with isotope-labeled internal standards; and microcystins plus nodularin (0.5–500 µg/L) in methanol/water. Chromatographic gradients were optimized for each method, and a five-minute automated rinse step prevented cross-contamination between PFAS and cyanotoxin analyses.

Used Instrumentation

• Shimadzu LCMS-8060RX triple quadrupole mass spectrometer
• Shimadzu LC-40 series liquid chromatography system
• Shim-pack GIST C18 analytical and delay columns
• Shim-pack Velox SP-C18 column for cyanotoxin separation

Main Results and Discussion

• Chromatographic separation: Baseline resolution achieved for most analytes within 8–15 minutes; overlapping peaks were resolved by distinct MRM transitions.
• Calibration performance: Linear curves (R² > 0.99) for all targets; injection accuracy ranged 80–120% with %RSD < 15%.
• System robustness: 294 injections over 54 hours confirmed stable accuracy at LLOQ, mid-range, and HLOQ levels, verifying effective rinsing and method switching.

Benefits and Practical Applications

• Single-system workflow reduces capital and maintenance costs.
• Automated method switching and rinsing minimize downtime and manual intervention.
• High-throughput capability supports timely response to harmful algal bloom events and routine monitoring.

Future Trends and Potential Applications

Further integration of additional contaminant classes, expanded automation for sample preparation, and real-time data processing will enhance laboratory efficiency. Adaptation of this multi-method platform to diverse environmental matrices and emerging regulatory methods is anticipated.

Conclusion

The Shimadzu LCMS-8060RX platform with automatic method switching delivers accurate, precise, and reliable quantification of PFAS and cyanotoxins in water using a single system. This streamlined approach offers a cost-effective, high-throughput solution for both routine compliance testing and rapid-response environmental analysis.

References

• ECHA. Progress update on the per- and polyfluoroalkyl substances (PFAS) restriction process. European Chemicals Agency; 2024.
• U.S. EPA. Method 537.1: Determination of Selected PFAS in Drinking Water by Solid Phase Extraction and LC-MS/MS; 2018.
• U.S. EPA. Method 533: Determination of Per- and Polyfluoroalkyl Substances in Drinking Water by Isotope Dilution Anion Exchange SPE and LC-MS/MS; 2019.
• U.S. EPA. Drinking Water Health Advisories for Cyanotoxins; 2021.
• U.S. EPA. Method 544: Determination of Microcystins and Nodularin in Drinking Water by SPE and LC-MS/MS; 2019.
• U.S. EPA. Method 545: Determination of Cylindrospermopsin and Anatoxin-a in Drinking Water by LC-ESI-MS/MS; 2017.
• Shimadzu Scientific Instruments, Inc. One System, Multiple Solutions: Analysis of PFAS & Cyanotoxins in Water adhering to EPA 537.1, 544, and 545; 2025.