Analysis of 29 per- and polyfluorinated compounds in water, sediment, soil and sludge by liquid chromatography–tandem mass spectrometry

Abstract

ABSTRACTSeveral analytical methods were optimised for the analysis of 29 per- and polyfluoroalkyl substances (PFASs), including perfluorocarboxylic acids, perfluoroalkyl sulphonic acids and fluorotelomers (FTs), such as sulphonate, saturated carboxylic acid, unsaturated carboxylic acid, sulphonamide and sulphonamide betaine (FTAB), in environmental samples in order to assess pollution by PFASs around heavily contaminated sites. Non-filtered water samples were extracted, purified and pre-concentrated by a solid-phase extraction (SPE) procedure. Solid samples (sediments, soils and sludges) were extracted through solvent extraction under acidic conditions and thereafter purified and pre-concentrated using the same SPE procedure as for the water samples. An ultra-high performance liquid chromatography coupled to tandem mass spectrometry in negative electrospray ionisation mode was employed to separate and detect targeted compounds. Twelve labelled internal standards were used to provide an adequate correction compensating for matrix effects. The limits of quantification (LOQs) were between 4 and 10 ng/L in water depending on the analytes. For solid samples, the LOQs were 2 ng/g dry weight (dw) in sediments and soils, and 20 ng/g dw in sludges for all analytes. A surrogate parameter method based on the carboxylation of perfluoroalkyl acid precursors under basic pH conditions was furthermore implemented to estimate the occurrence of non-targeted PFAS compounds. In order to evaluate the reliability of these analytical methods, environmental samples collected around a training area in France, where aqueous fire-fighting foam is used, were analysed. Of all the compounds detected in these environmental samples, 6:2 FTAB was found in the highest concentrations.