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

BACKGROUND: The AOAC Stakeholder Panel on Strategic Food Analytical Methods approved AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR®) 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 SMPR 2023.003. METHODS: Samples were extracted using a Quick, Easy, Cheap, Effective, Rugged, Safe (QuEChERS) method followed by solid-phase extraction (SPE) cleanup 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 LOQ, recovery, repeatability, and system suitability, and reference materials were analyzed. RESULTS: A full validation was conducted in European Union (EU)-regulated matrixes (eggs, shrimp, clams, salmon, chicken, and beef liver) and other matrixes (produce, milk, baby food, ground coffee, fish oil, protein powder, and corn snaplage) with satisfactory performances both in terms of recovery and reproducibility. Recovery percentages at target LOQs and two additional levels for perfluorooctane sulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), and perfluorohexane sulfonic acid (PFHxS) were between 80 and 120% and repeatability (RSDr) results were ≤20% for EU-regulated matrixes. For other matrixes recovery percentages were between 65 and 135% and repeatability results were ≤25%. All were within acceptable ranges as per SMPR 2023.003. CONCLUSION: The FDA's method for detection of 30 PFAS in food and feed compares favorably with the requirements of SMPR 2023.003 and should be adopted as a First Action method. HIGHLIGHTS: The FDA's single-laboratory validated method for PFAS detection in food and feed meets the requirements of SMPR 2023.003.