An LC-MS-MS Method for the Determination of Perfluorinated Surfactants in Environmental Matrices

Recently, there has been increasing concern about perfluorinated surfactants, especially perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA) due to their persistence and chronic toxicity in the aquatic environment. Solid phase extraction (SPE) followed by liquid chromatography coupled with tandem mass spectrometry (LC-MS-MS) are widely applied to quantitatively identify PFOS and PFOA. However, the application of this powerful analytical technique is limited by matrix susceptibility. The co-eluting matrix components in the SPE extracts affect the ionization efficiency and lead to erroneous results. An efficient sample clean-up method was developed in this study to significantly remove co-eluting matrix components by applying the SPE extracts onto a silica cartridge. It was shown that matrix effect (ME%) increased to >70% for both PFOS and PFOA in the analysis of raw sewage. Internal standardization was used to further compensate for the matrix effect, which also proved to improve the signal reproducibility. The clean-up method described in this study was applied to different water samples (surface water and wastewater) to evaluate the efficiency of silica clean-up and the influence of sample origin on the matrix effect. ME% and recovery efficiency (RE%) were in the range of 91.9–98.3% and 89.2–98.0%, respectively. Results showed that the developed method is robust and can be applied to analyze PFOS and PFOA in different environmental matrices.