Chinese Journal of Chromatography

Chinese Journal of Chromatography

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Fast determination of polybrominated diphenyl ethers in human milk using gas chromatography-negative chemical ionization/mass spectrometry

LIU Yinping1,2, DAI Peng3, LI Jingguang1, ZHANG Lei1, ZHAO Yunfeng1, WU Yongning1, ZHU Lingyan2   

  1. 1.National Institute of Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China; 2.College of Environmental Science and Engineering, Nankai University, Tianjin 300071, China; 3.Shenyang Center for Disease Control and Prevention, Shenyang 110031, China
  • Received:2008-05-21 Revised:2008-08-21 Online:2008-11-30 Published:1983-06-25
  • Contact: LI Jingguang

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Abstract: A method for the quantitative determination of 8 polybrominated diphenyl ethers (PBDEs) in human milk was established using gas chromatography-negative chemical ionization/mass spectrometry (GC-NCI/MS). After extraction by Soxhlet extractor, the lipid in the extract was removed by acidic silica, and the analyte was further purified by the multilayer silica-alumina column. The concentrations of BDE28, BDE47, BDE99, BDE100, BDE153, BDE154, BDE183 and BDE209 in human milk were fast determined by GC-NCI/MS in selected ion monitoring (SIM) mode on a 7 m column. The quantitative analysis was performed by isotope dilution method for BDE209 and internal standard method for other PBDEs. The limits of detection (LODs) of PBDEs in the lipid ranged from 1.74 to 6.35 pg/g. The recoveries of the spiked PBDEs were between 61.5% and 108% and their relative standard deviations (RSDs) (n=6) were between 2.06% and 10.1%. The method was further validated by the analysis of the reference materials of human milk. It was demonstrated that it is a low cost, rapid and reliable alternative for the trace analysis of selected PBDEs, especially for BDE209 in human milk

Key words: human milk , polybrominated diphenyl ethers (PBDEs), selected ion monitoring mode, gas chromatography-negative chemical ionization/mass spectrometry (GC-NCI/MS)