Matrix Effect-Free Analytical Methods for Determination of Perfluorinated Carboxylic Acids in Environmental Matrixes

Abstract

Perfluorocarboxylic acids (PFCAs) are persistent chemicals that have been found widely in the environment. Their accurate determination in environmental matrixes, particularly soil, sediment, and sludge, at low levels presents significant analytical challenges. The commercialization of electrospray interfaces for liquid chromatography−mass spectrometric analysis facilitated analysis of PFCAs at low levels, but issues with quantitative analysis due to matrix suppression or enhancement still persist. The methods described in this study utilize simple and rapid sample purification procedures to remove matrix components sufficiently so that errors due to coeluting matrix peaks are negligible and recoveries of PFCAs are consistently and reproducibly quantitative. Extracts from solid samples (soil and sediment) and liquid bacterial sludge are purified using dispersive solid-phase extraction. Recovery values generally are in the 70−120% range, with limits of quantitation of 1 ppb. The method utilizes an extraction solvent previously shown to release and recover aged residues of PFCAs. A confirmatory method using two precursor to product ions is also provided and demonstrated.