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

Authors: TAYLOR, RAEGYN - Oak Ridge Institute For Science And Education (ORISE); Sapozhnikova, Yelena

Submitted to: Analytica Chimica Acta
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 9/11/2022
Publication Date: 9/15/2022
Citation: Taylor, R., Sapozhnikova, Y.V. 2022. 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. Analytica Chimica Acta. 1230(16):340400. https://doi.org/10.1016/j.aca.2022.340400.
DOI: https://doi.org/10.1016/j.aca.2022.340400

Interpretive Summary: Per- and polyfluoroalkyl substances (PFAS) are known as "forever chemicals" for their persistence, ability to bioaccumulate, and potential adverse health effects. Diet has been considered a major source of PFAS exposure, however, efficient analytical methods for their measurement in foods are lacking. In this study, we extended and validated QuEChERSER mega-method for analysis of 34 PFAS in USDA Food Safety Inspection Service (FSIS) regulated foods: chicken, pork, beef, catfish and eggs. The developed method is fast and simple, and outperformed two official methods from the US Food and Drug Administration (FDA) and USDA FSIS. The validation results demonstrated the method's robustness, accuracy and precision. Using high resolution mass spectrometry analysis allows for data collection for future retrospective analysis of emerging PFAS alternatives. This method can easily be implemented in laboratories already analyzing environmental contaminants, mycotoxins, veterinary drugs, and pesticides.

Technical Abstract: 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 the 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 lipid 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 levels and 67 – 88% of analytes at the 0.1 ng/g level, depending on the matrix. Additional validation was also 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 level than the HRMS method but exhibited more variability at 1 and 5 ng/g 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.