Determination of 15 Perfluorinated Compounds in Eggs by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Filterable Solid Phase Extraction Column Purification

A method for the determination of 15 perfluorinated compounds, including perfluorobutyric acid, perfluoropentanoic acid, perfluorohexanoic acid, perfluoroheptanoic acid, perfluorooctanoic acid, perfluorononanoic acid, perfluorodecanoic acid, perfluoroundecanoic acid, perfluorododecanoic acid, perfluorotridecanoic acid, perfluorotetradecanoic acid, perfluorobutane sulfonate, perfluorohexane sulfonate, perfluoroheptane sulfonate and perfluorooctane sulfonate, in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry with filterable solid phase extraction column purification was proposed. The 0.1 mL of 20.0 μg·L^-1 the isotope standard mixed solution was added into 2 g of egg sample, and the mixture was extracted by oscillation and ultrasonic with 10 mL of 80% (volume fraction) acetonitrile solution. After centrifugation, 5 mL of the filtrate was taken and directly passed through Captive EMR-Lipid column for purification. The effluent was collected, and blown to nearly dryness by nitrogen. The residue was redissolved with 500 μL of methanol, and then determined after treatment by vortex and centrifugation. The separation was performed on Agilent Eclipse Plus C₁₈ RRHD column (100 mm×2.1 mm, 1.8 μm), and the mixed solutions composed of 2 mmol·L^-1 ammonium acetate solution and methanol at different volume radios was used for gradient elution. Multi-reaction monitoring mode was used for detection with scanning by electrospray ion source negative ion mode, and quantification by isotope internal standard method. It was shown that the linear ranges of standard curves for 15 perfluorinated compounds were found in the same range of 0.125-20.0 μg·L^-1, with lower limits of determination (10S/N) in the range of 0.05-0.16 μg·kg^-1. The recoveries of 15 targets were in the range of 78.0%-111% at spiked concentration levels of 0.500, 4.00, 16.0 μg·kg^-1, and RSDs (n=6) of the determined values range from 0.87% to 14%.