Objective:To develop the ultra performance liquid chromatography tandem mass spectrometry ( UPLC-MS/MS ) for the determination of perfluorocarboxylic acids ( PFCAs ) in fish.

Methods:The fish samples were extracted with tert-butyl methyl ether and purified by WAX columns. The WAX cartridges were rinsed with methanol and 25 mmol/L ammonium acetate, and the target compound residues were eluted with 0.5% ammonia methanol and then redissolved with 50% methanol aqueous solution after nitrogen blowing to nearly dry. Nine kinds of PFCAs were simultaneously quantified by UPLC-MS/MS with 1 mmol/L ammonium acetate-methanol solution as the mobile phase.

Results:The extraction was separated well in UPLC BEH C18 column. There were good linear correlations of nine kinds of PFCAs in the range of 1.0-200.0 ng/mL, with the coefficients all more than 0.99. The limits of detection and quantification were 0.06-0.19 μg/kg and 0.19-0.62 μg/kg, respectively. The recovery rates were 70.08%-117.24% at different spiked levels ( 5.0, 25.0, 50.0 μg/kg ), and the relative standard deviations were 2.31%-19.68%.

Conclusion:Through optimizing the pretreatment conditions, the mobile phase of liquid chromatography and the detection conditions of mass spectrometry, the UPLC-MS/MS could meet the monitoring requirements of PFCAs in fish.