Comparison and validation of the QuEChERSER mega-method for determination of per- and polyfluoroalkyl substances in foods by liquid chromatography with high-resolution and triple quadrupole mass spectrometry

Instances of food contamination with per-and polyfluoroalkyl substances (PFAS) continue to occur globally, but sample preparation and analytical methods are quite limited and often monitor for a small percentage of known PFAS. This study aimed to evaluate, validate, and compare performance of two instruments with the recently developed quick, easy, cheap, effective, rugged, safe, efficient, and robust (QuEChERSER) sample preparation mega-method - a method developed to monitor chemicals over a broad range of physicochemical properties. Initial evaluation of the QuEChERSER mega-method for determination of PFAS in food demonstrated recoveries, matrix interferences, and co-extractive removal comparable to (or better than) US Food and Drug Administration (FDA) and USDA Food Safety and Inspection Service (FSIS) methods. Subsequent validation of QuEChERSER in beef, catfish, chicken, pork, liquid eggs, and powdered eggs on a high-resolution mass spectrometer achieved acceptable recoveries (70-120%) and precision (RSDs <= 20%) for all 33 target analytes at the 1 and 5 ng g(-1) levels and 67-88% of analytes at the 0.1 ng g(-1) level, depending on the matrix. Additional validation was performed by tandem mass spectrometry on a triple quadrupole instrument. This approach provided no non-detects and better recoveries at the 0.1 ng g(-1) level than the HRMS method but exhibited more variability at 1 and 5 ng g(-1) spiking levels. Analysis of NIST SRMs 1946 and 1947 gave accuracies of 70-117%. These results demonstrate the capability of combining PFAS analysis with a mega-method previously validated for 350 analytes, while collecting non-target data for future retrospective analysis of emerging alternatives with a high -resolution mass spectrometry method.

Automated summary

This study evaluated and compared the performance of two instruments for the determination of per- and polyfluoroalkyl substances (PFAS) using a newly developed sample preparation method. The results showed that the method had better recoveries, matrix interferences, and co-extractive removal compared to the FDA and FSIS methods. Validation of the method in different matrices achieved acceptable recoveries and precision for the target analytes at various levels. The study also demonstrated the potential for future analysis of emerging alternatives using high-resolution mass spectrometry.