Chinese Journal of Chromatography

Chinese Journal of Chromatography

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Determination of dioxin like polychlorinated biphenyl residues in milk using isotope dilution gas chromatography-ion trap tandem mass spectrometry

DING Gangdou1,2, LI Xiang1, LIU Hanxia1, ZHONG Weike1,
HE Yinfeng2, ZHANG Yao1, SUN Yizhi1   

  1. 1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China;
    2.Department of Food Science, Inner Mongolia Agricultural University, Huhhot 010018, China
  • Received:2007-07-10 Revised:2007-10-23 Online:2008-01-30 Published:1984-09-25

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Abstract:

A method for the determination of dioxin like polychlorinated biphenyl (DL-PCB) residues in milk has been developed using high resolution gas chromatography coupled with ion trap mass spectrometry (GC-MS/MS-IT). Analytical procedure consisted of accelerate solvent extraction (ASE), lipid removal with acidic silica and clean-up using anthropogenic isolation column packed with multilayer silica. The analytes were separated on a DB-5 capillary column, detected with multiple reaction monitor mode (MRM) and quantified using internal standard calibration curve of isotope dilution technique. The correlation coefficients of calibration standard solution were above 0.9999 for all the DL-PCBs. The recoveries and relative standard deviations of labeled compound solution were in the oranges from 39% to 129% and from 5% to 22%, respectively. The detection limits in the range from 3 to 11 pg/g (fat) were established for the 12 DL-PCBs.

Key words: isotope dilution, milk , polychlorinated biphenyl residues, gas chromatography-ion trap tandem mass spectrometry (GC-MS/MS-IT)