关键词: 全氟辛基磺酸（PFOS）, 全氟辛酸（PFOA）, 沉积物, 固相萃取, 液相色谱-串联质谱, PFOS, PFOA, sediments, solid phase extraction(SPE), liquid chromatography-mass spectrometry(LC-MS)

Abstract: A method for simultaneous determination of PFOS and PFOA in environmental sediments samples was developed by ultra pressure liquid chromatography coupled with tandem mass spectrometry. Sediments sample was ultrasonic extraction with 15 mL methanol twice, then enriched and purified through a C18 SPE, and finally concentrated into 1.0 mL with an automated de-solvent device. Target analytes were separated on a Eclipse Plus-C18 column using methanol (containing 5.0 mmol/L NH4COOH) –water (containing 5.0 mmol/L NH4COOH) as mobile phase. The negative electrospray ionization (ESI-) and multiple reaction monitoring mode (MRM) was utilized. The recoveries (n=3) and relative standard deviations(RSD，n=7) were 82.5± 9.2% and 8.3% for PFOS at 0.5 ng/g, 2.0 ng/g and 5.0 ng/g spiking levels and 103.2± 9.2% and 9.1%for PFOA at 0.5 ng/g, 2.0 ng/g and 5.0 ng/g spiking levels，respectively. An internal standard calibration method was chosen to the quantitative analysis. The calibration curves of PFCs were linear in the range of 0.5-20 ng/g with correlation coefficients more than 0.999 0.The detection limits were 0.08 ng/g for PFOS and PFOA. The results showed that this method possessed efficiency and good selectivity，and can be used for the detection of PFOS and PFOA in marine sediments.