Simultaneous Determination of Multiple Persistent Halogenated Compounds in Human Breast Milk

Abstract

Abstract A method was developed for simultaneous determination of multiple persistent organic pollutants (POPs) such as organochlorine pesticides (OCPs), hexabromocyclododecanes (HBCDs), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs), in human breast milk. The sample pretreatment procedure included liquid-liquid extraction, gel permeation chromatography (GPC), and solid-phase extraction (SPE) cleanup. Gas chromatography-mass spectrometry (GC-MS), liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) were applied in the analysis of target compounds. By using GPC to remove high-molecular-weight lipids and SPE for further cleanup and separation of target compounds, the interferences from the biological matrix could be greatly reduced. The developed sample pretreatment is suitable for multi-component analysis of very low concentrations of POPs in small volume of human samples. The developed method of simultaneous determination of PCBs and OCPs by GC-MS/MS exhibited excellent sensitivity and selectivity. Spiked 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, and limits of detection were 0.13–1.8 ng L −1 for PBDEs, 0.31–1.2 ng L −1 for HBCDs, 0.22–1.4 ng L −1 for PCBs, and 0.20–1.5 ng L −1 for OCPs. This method was applied to the analysis of POPs in 20 human breast milk samples from Weifang City. The result showed that the median concentrations of HBCDs, PBDEs, PCBs, and OCPs were 2.86, 7.76, 8.84 and 643 ng g −1 lipid weight, which were comparable to those in human breast milk samples from populations of other regions in China.