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A rapid method for the determination of perfluoroalkyl substances including structural isomers of perfluorooctane sulfonic acid in human serum using 96-well plates and column-switching ultra-high performance liquid chromatography tandem mass spectrometry

Salihovic, Samira, Kärrman, Anna, Lindström, Gunilla, Lind, P. Monica, Lind, Lars, van Bavel, Bert
Journal of chromatography 2013 v.1305 pp. 164-170
epidemiological studies, detection limit, blood serum, humans, acids, ultra-performance liquid chromatography, isomers, rapid methods, tandem mass spectrometry, sulfonic acids, perfluorocarbons
To facilitate high-throughput analysis suitable for large epidemiological studies we developed an automated column-switching ultra-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method for determination of perfluorocarboxylic acids (PFCAs; C₅, C₆, C₇, C₈, C₉, C₁₀, C₁₁, C₁₂, and C₁₃), perfluoroalkyl sulfonic acids (PFSAs; C₄, C₆, C₈, and C₁₀), perfluorooctane sulfonamide (PFOSA), and five groups of structural perfluorooctane sulfonic acid (PFOS) isomers in human serum or plasma. The analytical procedure involves rapid protein precipitation using 96-well plates followed by an automated sample clean-up using an on-line trap column removing many potentially interfering sample components while through the mobile phase gradient the target analytes are eluted onto the analytical column for further separation and subsequent mass detection. The method was linear (R²<0.995) at concentrations ranging from 0.01 to 60ngmL⁻¹ with method detection limits ranging between 0.01 and 0.17ngmL⁻¹ depending on the analyte. The developed method was precise, with repeatability (n=7) and reproducibility (n=103) coefficients of variation between 2% and 20% for most compounds including PFOS (2% and 8%) and its structural isomers (2–6% and 4–8%). The method was in conformity with a standard reference material. The column-switching HPLC–MS/MS method has been successfully applied for the determination of perfluoroalkyl substances including structural PFOS isomers in human plasma from an epidemiological study.