凝胶渗透色谱柱去脂-气相色谱-质谱法测定人血清中新型卤系阻燃剂

引用本文: 何松洁, 李明圆, 金军, 王英, 何畅, 卜云洁, 田旸. 凝胶渗透色谱柱去脂-气相色谱-质谱法测定人血清中新型卤系阻燃剂[J]. 分析化学, 2012, 40(10): 1519-1523. doi: 10.3724/SP.J.1096.2012.20364 shu

Citation: HE Song-Jie, LI Ming-Yuan, JIN Jun, WANG Ying, HE Chang, BU Yun-Jie, TIAN Yang. Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(10): 1519-1523. doi: 10.3724/SP.J.1096.2012.20364 shu

凝胶渗透色谱柱去脂-气相色谱-质谱法测定人血清中新型卤系阻燃剂

通讯作者: 金军

基金项目:
本文受到教育部新世纪优秀人才支持计划(No.NCET-10-0106 ) (No.NCET-10-0106 )

中央民族大学985工程(No.MUC985-9) (No.MUC985-9)

中央高校基本科研业务费专项资金中央民族大学自主科研计划项目(No.0910KYQN50)支持 (No.0910KYQN50)

摘要: 建立了凝胶渗透色谱(GPC)去脂,气相色谱-负化学电离源-质谱(GC-NCI-MS)法测定人血清中2,2',4,4',5,5'-六溴联苯(BB-153)、1,2-二(2,4,6-三溴苯氧基)乙烷(BTBPE)和德克隆(Dechlorane plus,DP,包括syn-DP和anti-DP)的方法。人血清样本加入内标¹³C₁₂BB-153和¹³C₁₀syn-DP,经蛋白质变性、脂肪提取、GPC去脂、酸性硅胶柱净化后,利用气相色谱-负化学电离源-质谱法测定样品中BB-153, BTBPE, syn-DP和anti-DP,监测离子分别为m/z 627.5, 629.5,m/z 79, 81以及m/z 652, 654。结果表明,¹³C₁₂BB-153 和¹³C₁₀syn-DP 的血清加标回收率分别为91.5%±8.9%和92.3%±8.1%,检出限为0.6-1.2 ng/g脂肪。应用本方法对人血样品进行测定,BB-153和BTBPE在所有样本中均未检出,syn-DP和anti-DP的浓度范围分别是0.7-9.2 ng/g脂肪和0.6-2.0 ng/g脂肪。

关键词:

English

Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

1.
College of Life and Environmental Sciences, Minzu University of China, Beijing 100081, China

Corresponding author: 金军

Received Date: 06 April 2012
Fund Project:
本文受到教育部新世纪优秀人才支持计划(No.NCET-10-0106 )

中央民族大学985工程(No.MUC985-9)

中央高校基本科研业务费专项资金中央民族大学自主科研计划项目(No.0910KYQN50)支持

Abstract: A gel permeation chromatography-gas chromatography-negative chemical ionization-mass spectrometry method (GPC-GC-NCI-MS) was developed for the determination of 2,2',4,4',5,5'-hexabromobiphenyl (BB-153), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) and Dechlorane plus (DP) in human serum sample. The serum samples were spiked with ¹³C₁₂BB-153 and ¹³C₁₀syn-DP as surrogate internal standard before extracting, and the serum lipid was extracted and mostly removed by gel permeation chromatography. Samples were further cleaned up with a silica/sulfuric acid column. Identification and quantification of BB-153, BTBPE, syn-DP and anti-DP were performed by Gas chromatography-Negative chemical ionization-Mass spectrometry. The monitored ions were as follows: m/z 627.5 and 629.5 for BB-153; m/z 79 and 81 for BTBPE; m/z 652 and 654 for DP. The recoveries of ¹³C₁₂BB-153 and ¹³C₁₀syn-DP in serum samples were 91.5%±8.9% and 92.3%±8.1%, respectively. The limits of detection were from 0.6 to 1.2 ng/g lipid. BB-153 and BTBPE were not detected in all serum samples, and the concentrations of syn-DP and anti-DP were 0.7-9.2 ng/g lipid and 0.6-2.0 ng/g lipid, respectively.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

凝胶渗透色谱柱去脂-气相色谱-质谱法测定人血清中新型卤系阻燃剂

通讯作者: 金军

English

Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

Corresponding author: 金军

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

凝胶渗透色谱柱去脂-气相色谱-质谱法测定人血清中新型卤系阻燃剂

通讯作者: 金军

English

Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

Corresponding author: 金军

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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通讯作者: 陈斌, bchen63@163.com

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