母乳中多种含卤持久性有机污染物的联合检测方法

引用本文: 黄晓梅, 马盛韬, 崔君涛, 李佩, 曾祥英, 于志强. 母乳中多种含卤持久性有机污染物的联合检测方法[J]. 分析化学, 2017, 45(4): 593-600. doi: 10.11895/j.issn.0253-3820.160735 shu

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 shu

母乳中多种含卤持久性有机污染物的联合检测方法

1.
中国科学院广州地球化学研究所, 有机地球化学国家重点实验室, 广东省环境资源利用与保护重点实验室, 广州 510640;
2.
中国科学院大学, 北京 100049
基金项目:
2017-01-11接收本文系国家杰出青年科学基金（No.41225013）和中国科学院战略性先导科技专项（B类）（No.XDB14010202）资助

摘要: 建立了母乳中多种含卤持久性有机污染物（POPs）的联合检测方法，目标化合物主要包括六溴环十二烷（HBCDs）、多溴联苯醚（PBDEs）、多氯联苯（PCBs）和有机氯农药（OCPs）等。样品的前处理采用液液萃取、凝胶渗透色谱（GPC）净化和固相萃取（SPE）等技术，目标化合物经气相色谱-质谱联用仪（GC-MS）、液相色谱-三重四极杆串联质谱联用仪（LC-MS/MS）和气相色谱-三重四极杆串联质谱联用仪（GC-MS/MS）等进行检测。样品通过GPC除去脂肪，然后经SPE柱进一步净化并进行多组分分离，极大程度地减小了生物样品中复杂基质的干扰，适合样品量相对较小的人体样本中多种超痕量POPs的分析。应用灵敏度高、选择性更好的GC-MS/MS对样品中的PCBs和OCPs等进行分析，进一步降低基质的干扰。方法经过小牛血清加标实验验证，稳定可靠。POPs的加标回收率分别为88.7%~98.8%（PBDEs），88.5%~92.5%（HBCDs），67.9%~82.3%（PCBs）和81.7%~116.1%（OCPs），方法检出限分别为0.13~1.8 pg/mL（PBDEs），0.31~1.2 pg/mL（HBCDs），0.22~1.4 pg/mL（PCBs）和0.20~1.5 pg/mL（OCPs）。采用本方法对潍坊地区20例母乳样品进行分析，结果显示，潍坊市母乳中HBCDs、PBDEs、PCBs、HCHs和DDTs的中值浓度分别为2.86、7.76、8.84、140和503 ng/g 脂重，此浓度水平与国内其它地区人群相当。

关键词:

English

Simultaneous Determination of Multiple Persistent Halogenated Compounds in Human Breast Milk

1.
State Key Laboratory of Organic Geochemistry, Guangdong Provincial Key Laboratory of Utilization and Protection of Environmental Resources, Guangzhou Institute of Geochemistry Chinese Academy of Sciences, Guangzhou 510640, China;
2.
University of Chinese Academy of Sciences, Beijing 100049, China
Received Date: 30 September 2016
Revised Date: 11 January 2017
Fund Project:
This work was supported by the National Science Foundation for Distinguished Young Scholars of China (No. 41225013) and the strategic priority Research Program of the Chinese Academy of Sciences (No. XDB14010202)

Abstract: 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.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

母乳中多种含卤持久性有机污染物的联合检测方法

English

Simultaneous Determination of Multiple Persistent Halogenated Compounds in Human Breast Milk

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

母乳中多种含卤持久性有机污染物的联合检测方法

English

Simultaneous Determination of Multiple Persistent Halogenated Compounds in Human Breast Milk

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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