Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (5): 494-500.DOI: 10.3724/SP.J.1123.2014.12034

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Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

ZHU Pingping1,2, YUE Zhenfeng1, ZHENG Zongkun2, ZHANG Yi1, LI Wenyin1,2, ZHAO Fengjuan1, XIAO Chengui1, BAI Runye1,2, LIN Wei1,2   

  1. 1. Food Inspection and Quarantine Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau; Shenzhen Key Laboratory of Detection Technology R. & D. on Food Safety, Shenzhen 518045, China;
    2. College of Chemistry and Chemical Engineering, Shenzhen University, Shenzhen 518060, China
  • Received:2014-12-25 Revised:2015-03-18 Online:2015-05-08 Published:2015-04-23

Abstract:

A method was developed for the determination of 19 perfluoroalkyl acids (PFAs) in lamb liver by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile, and then cleaned-up by a mixture of N-propylethylenediamine (PSA), C18 and graphitized carbon black (GCB) sorbents. The 19 PFAs were analyzed by HPLC-MS/MS with a C18 chromatographic column, adopting the multiple reaction monitoring (MRM) mode with negative electrospray ionization. The effects of the dosages of hydrochloric acid and the sorbents on the recoveries of the 19 PFAs were studied. For accurate quantitative analysis, the isotope internal standard method was used. The calibration curves were linear with the correlation coefficients over 0.998 in the range of 0.05-20 μg/kg for the 19 PFAs. The limits of detection were 0.004-0.111 μg/kg. The limits of quantification were 0.012-0.370 μg/kg. The mean recoveries of the 19 PFAs at spiked levels of 0.5, 1.0, 2.0 μg/kg were in the range from 80% to 128% with the relative standard deviations of 0.31%-11.1%. The developed method is rapid, simple, accurate. It is suitable for the determination of the 19 PFAs in large quantities of lamb liver samples.

Key words: dispersive solid phase extraction, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), lamb liver, perfluoroalkyl acids

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