Simultaneous determination of legacy and emerging per- and polyfluoroalkyl substances in fish by QuEChERS coupled with ultrahigh performance liquid chromatography tandem mass spectrometry

Abstract

In this study, a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was developed for simultaneous determination of 30 legacy and emerging per- and polyfluoroalkyl substances (PFASs) in fish by UHPLC-MS/MS. Primary and secondary amine (PSA), octadecylsilane (C18), Florisil and Envi-carb were applied in this method. The method detection limits (MDLs) ranged from 2 to 10 pg g⁻¹ except for PFBA (60 pg g⁻¹). Recoveries obtained with fortified samples were in the range of 84.6% to 107%. The intra-day RSDs and inter-day RSDs ranged from 0.25% to 9.95% and 0.30% to 12.3%, respectively. Matrix effect (ME) factors were in the range of 0.79 to 1.31. ME factors increased with the increase of acetonitrile proportions in the mobile phase. The developed method was applied for PFAS detection in 40 marine fish samples. 16 PFASs were detected with ∑PFAS concentrations in the range of 120 to 4488 pg g⁻¹. Perfluorooctanoic acid (PFOA) was the predominant PFAS followed by perfluorooctanesulfonate (PFOS). The newly emerging 6:2 chlorinated polyfluoroalkyl ether sulfonate (6:2Cl-PFAES) was detected in 85% of the samples, which warranted further investigation. The developed method was time-saving, efficient and accurate for determination of legacy and emerging PFASs in fish.