Determination of Per- and Polyfluoroalkyl Substances in Food and Feed by Enhanced Matrix Removal LC-MS/MS Method,
Limian Zhao1, Matthew Giardina1, Emily Parry1
1Agilent Technologies Inc, 2850 Centerville Rd, Wilmington, DE 19808, USA.
Background:
AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR)® 2023.003 outlines method performance requirements for the determination of per- and polyfluoroalkyl substances (PFAS) across a broad range of food and feed matrixes.
Objective:
The objective of this study was to develop and validate the EMR LC-MS/MS method in accordance with AOAC INTERNATIONAL SMPR 2023.003 using a single-laboratory approach.
Methods:
The method features QuEChERS extraction followed by a novel enhanced matrix removal (EMR) mixed-mode passthrough cleanup, an online injection program, sensitive LC-MS/MS detection, and accurate, precise quantitation using neat calibration curves with isotopically labeled internal standards.
Results:
Method performance was evaluated for suitability and selectivity, calibration linearity, limit of quantitation (LOQ), recovery, and repeatability, and the method was successfully validated in a single-laboratory validation (SLV) across 16 diverse food matrixes, encompassing all 11 required food categories. Acceptable PFAS background cleanliness was demonstrated, supporting accurate and reliable quantitation in all food matrixes. Validated or calculated LOQs for all analytes across all food matrixes were equal or below the required LOQs, with an exception rate of <1%. Recovery and single-laboratory repeatability also satisfied the acceptance criteria specified in the AOAC SMPR guideline, again with an exception rate of <1%. Method selectivity was confirmed through baseline separation of cholic acid interferences from PFOS isomers and through secondary confirmation of PFBA and PFPeA using LC-QTOF analysis.
Conclusions:
The EMR LC-MS/MS method met all performance criteria, supporting its advancement as a First Action AOAC Official Method of AnalysisSM 2025.11.
Highlights:
A novel EMR LC-MS/MS method was developed and successfully validated for the determination of 30 PFAS analytes across a wide range of food and feed matrixes, fulfilling the requirements of AOAC SMPR 2023.003.
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