Method development and evaluation for the determination of perfluoroalkyl and polyfluoroalkyl substances in multiple...

A method for the determination of 21 perfluorinated and 10 polyfluorinated alkyl substances (PFAS) was developed for application in different food matrices. Acetonitrile was used as the extraction solvent with solid phase extraction weak anion-exchange (SPE-WAX) clean up, with LC-MS/MS analysis using both surrogate and performance standards to correct for losses during sample preparation and matrix effects. The method has been evaluated in four different matrices (fish, pizza, chicken nuggets and spinach). Originally, the focus was to develop a method for foods commonly thought to be a source of PFASs (e.g. fish). It was expanded to include foods where PFAS exposure would be possible through their presence in grease-proof food packaging (e.g. pizza, chicken nuggets). Vegetables (lettuce) and fruit (tomato) have recently been considered as part of proficiency testing programmes, so the inclusion of some testing in a vegetable matrix (i.e. spinach) was also added to the testing. Limits of quantification ranged from 0.018 ng g^-1 (L-PFDS) to 5.28 ng g^-1 (FHEA), although method quantification limits for PFBA (12.4 ng g^-1), 6:2 PAP (8.96 ng g^-1) and 8:2 PAP (3.49 ng g^-1) were elevated above instrumental limits owing to their consistent detection in reagent blank samples. PFAS analyses were strongly impacted by matrix, therefore the use of isotopically labelled internal standards was critical to the development of accurate results. The accuracy of the method using numerous proficiency testing schemes or interlaboratory comparison studies has shown the developed method to be successful with z-scores for all concerned analytes in all test matrices remaining within ±2.0, with the exception of PFBA in wheat flour which was -2.4.