Citation: HUANG Xiao-Mei, MA Sheng-Tao, CUI Jun-Tao, LI Pei, ZENG Xiang-Ying, YU Zhi-Qiang. Simultaneous Determination of Multiple Persistent Halogenated Compounds in Human Breast Milk[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(4): 593-600. doi: 10.11895/j.issn.0253-3820.160735
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A method was developed for simultaneous determination of multiple persistent organic pollutants (POPs) such as hexabromocyclododecanes (HBCDs), polybrominateddiphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs), and organochlorine pesticides (OCPs) in human breast milk. The sample pretreatment procedures included liquid-liquid extraction, gel permeation chromatography (GPC), and solid-phase extraction (SPE) clean-up. Gas chromatography coupled with mass spectrometry (GC-MS), liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS), and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) were applied in analysis of the target compounds. By using GPC to remove high-molecular mass lipids and SPE for further clean-up and separation of target compounds, the interferences of biological matrix were greatly reduced. The developed sample pretreatment procedure was suitable for the multi-component analysis of POPs in human samples which had very lower POPs concentrations and smaller sample volumes. The simultaneous determination of PCBs and OCPs by GC-MS/MS exhibited excellent sensitivity and selectivity. The method recoveries were tested by spiked target compounds into fetal bovine serum samples. The recoveries were 88.7%-98.8% for PBDEs, 88.5%-92.5% for HBCDs, 67.9%-82.3% for PCBs, and 81.7%-116.1% for OCPs, respectively. Limits of detection of the method were in the range of 0.13-1.8 ng/L for PBDEs, 0.31-1.2 ng/L for HBCDs, 0.22-1.4 ng/L for PCBs, and 0.20-1.5 ng/L for OCPs, respectively. Finally, the developed method was applied in POPs analysis of 20 human breast milk samples from Weifang city. The results showed that the median concentrations of HBCDs, PBDEs, PCB, HCHS and DDTs were 2.86, 7.76, 8.84, 140 and 503 ng/g lipid weight, respectively. Levels of the target compounds were comparable to those reported in human breast milk for general population from other regions in China.
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