Validation of the U.S. Food and Drug Administration’s Method for Detection of Per- and Polyfluoroalkyl Substances Analytes in Food and Feed: First Action 2025.06

Abstract Background The AOAC Stakeholder Panel on Strategic Food Analytical Methods approved AOAC INTERNATIONAL Standard Method Performance Requirements (SMPRs®) 2023.003 for per- and polyfluoroalkyl substances (PFAS) in produce, beverages, dairy products, eggs, seafood, meat products, and feed. The U.S. Food and Drug Administration’s (FDA’s) method is a single laboratory validated (SLV) method for determination of 30 PFAS in food and feed. Objective In response to a call for minimum method performance characteristics and analytical requirements, the FDA’s method for detection of PFAS in food and feed was validated in a single laboratory study with comparison to AOAC SMPR 2023.003. Methods Samples were extracted using (Quick, Easy, Cheap, Effective, Rugged, Safe) QuEChERS followed by solid phase extraction (SPE) clean-up and concentration using nitrogen. Analysis was performed using isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated for parameters such as limit of quantification, recovery, repeatability, system suitability, and reference materials were analyzed. Results A full validation was conducted in European Union (EU)-regulated matrixes (eggs, shrimp, clams, salmon, chicken, beef liver) and other matrixes (produce, milk, baby food, ground coffee, fish oil, protein powder, corn snaplage) with satisfactory performances both in terms of recovery and reproducibility. Recovery percentages at target limits of quantification (LOQ) and two additional levels for perfluorooctane sulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), and perfluorohexane sulfonic acid (PFHxS) were between 80-120% and repeatability (RSDr) results were ≤20% for EU-regulated matrixes. For other matrixes recovery percentages were between 65-135% and repeatability results were ≤25%. All were within acceptable ranges as per AOAC SMPR 2023.003. Conclusions The FDA’s method for detection of 30 PFAS in food and feed compares favorably with the requirements of AOAC SMPR 2023.003 and should be adopted as a First Action AOAC Official Method. Highlights The FDA’s single lab validated method for PFAS detection in food and feed meets the requirements of AOAC SMPR 2023.003.