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:

1. [1]
  1 ZHANG Ying, WU Jiang-Ping, YU Le-Huan, HE Ming-Jing, LUO Xiao-Jun, MAI Bi-Xian. Environ. Chem., 2011, 30(1): 34-431 ZHANG Ying, WU Jiang-Ping, YU Le-Huan, HE Ming-Jing, LUO Xiao-Jun, MAI Bi-Xian. Environ. Chem., 2011, 30(1): 34-43
2. [2]
  张荧, 吴江平, 余乐洹, 何明靖, 罗孝俊, 麦碧娴. 环境化学, 2011, 30(1): 34-43张荧, 吴江平, 余乐洹, 何明靖, 罗孝俊, 麦碧娴. 环境化学, 2011, 30(1): 34-43
3. [3]
  2 Qiu X H, Zhu T, Hu J X. Chemosphere, 2010, 80(10): 1207-12122 Qiu X H, Zhu T, Hu J X. Chemosphere, 2010, 80(10): 1207-1212
4. [4]
  3 de Wit CA. Chemosphere, 2002, 46(5): 583-6243 de Wit CA. Chemosphere, 2002, 46(5): 583-624
5. [5]
  4 Kohler M, Zennegg M, Bogdal C, Gerecke A C, Schmid P, Heeb N V, Sturm M, Vonmont H, Kohler H P, Giger W. Environ. Sci. Technol., 2008, 42(17): 6378-63844 Kohler M, Zennegg M, Bogdal C, Gerecke A C, Schmid P, Heeb N V, Sturm M, Vonmont H, Kohler H P, Giger W. Environ. Sci. Technol., 2008, 42(17): 6378-6384
6. [6]
  5 http://chm.pops.int/Programmes/NewPOPs/The9newPOPs/tabid/672/language/en-US/Default.aspx5 http://chm.pops.int/Programmes/NewPOPs/The9newPOPs/tabid/672/language/en-US/Default.aspx
7. [7]
  6 European Court of Justice. Cases C-14/06 and C-295/06, Judgement of the Court, 1 April 2008, Directive 2002/95/EC and Commission Decision 2005/717/EC;20086 European Court of Justice. Cases C-14/06 and C-295/06, Judgement of the Court, 1 April 2008, Directive 2002/95/EC and Commission Decision 2005/717/EC;2008
8. [8]
  7 Hoh E, Zhu L Y, Hites R A. Environ. Sci. Technol., 2005, 39(8): 2472-24777 Hoh E, Zhu L Y, Hites R A. Environ. Sci. Technol., 2005, 39(8): 2472-2477
9. [9]
  8 Law K, Halldorson T, Danell R, Stern G, Gewurtz S, Alaee M, Marvin C, Whittle M, Tomy G. Environ. Toxicol. Chem., 2006, 25(8): 2177-21868 Law K, Halldorson T, Danell R, Stern G, Gewurtz S, Alaee M, Marvin C, Whittle M, Tomy G. Environ. Toxicol. Chem., 2006, 25(8): 2177-2186
10. [10]
  9 Ren N, Sverko E, Li Y F, Zhang Z, Harner T, Wang D, Wan X, McCarry B E. Environ. Sci. Technol., 2008, 42(17): 6476-64809 Ren N, Sverko E, Li Y F, Zhang Z, Harner T, Wang D, Wan X, McCarry B E. Environ. Sci. Technol., 2008, 42(17): 6476-6480
11. [11]
  10 Hoh E, Zhu L, Hites R A. Environ. Sci. Technol., 2006, 40(4): 1184-118910 Hoh E, Zhu L, Hites R A. Environ. Sci. Technol., 2006, 40(4): 1184-1189
12. [12]
  11 de Wit C A, Herzke D, Vorkamp K.Sci. Total. Environ., 2010, 408(15): 2885-291811 de Wit C A, Herzke D, Vorkamp K.Sci. Total. Environ., 2010, 408(15): 2885-2918
13. [13]
  12 Xiao H, Hung H, Shen L, Wania F,Sverko E, Su Y S, Lei Y D, Reiner E, Kang S C, Barresi E, DeJong M. Proceedings of the BFR 2010 Conference, Kyoto, Japan, 7-9 April; 2010 www.bfr 2010.com/abstract-download/2010/90067.pdf12 Xiao H, Hung H, Shen L, Wania F,Sverko E, Su Y S, Lei Y D, Reiner E, Kang S C, Barresi E, DeJong M. Proceedings of the BFR 2010 Conference, Kyoto, Japan, 7-9 April; 2010 www.bfr 2010.com/abstract-download/2010/90067.pdf
14. [14]
  13 Moller A, Xie Z Y, Cai M H, Sturm R, Ebinghaus R. Environ. Sci. Technol., 2012, 46(6): 3141-314813 Moller A, Xie Z Y, Cai M H, Sturm R, Ebinghaus R. Environ. Sci. Technol., 2012, 46(6): 3141-3148
15. [15]
  14 Hovander L, Athanasiadou M, Asplund L, Jensen S, Wehler E K. J. Anal. Toxicol., 2000, 24(8): 696-70314 Hovander L, Athanasiadou M, Asplund L, Jensen S, Wehler E K. J. Anal. Toxicol., 2000, 24(8): 696-703
16. [16]
  15 REN Guo-Fa, LUO Xiang-Fan, MA Sheng-Tao, SUN Yan-Feng, YU Zhi-Qiang, SHENG Guo-Ying, FU Jia-Mo. Chinese J. Anal. Chem., 2011, 39(2): 235-23815 REN Guo-Fa, LUO Xiang-Fan, MA Sheng-Tao, SUN Yan-Feng, YU Zhi-Qiang, SHENG Guo-Ying, FU Jia-Mo. Chinese J. Anal. Chem., 2011, 39(2): 235-238
17. [17]
  任国发, 罗湘凡, 马盛韬, 孙延枫, 于志强, 盛国英, 傅家谟. 分析化学, 2011, 39(2): 235-238任国发, 罗湘凡, 马盛韬, 孙延枫, 于志强, 盛国英, 傅家谟. 分析化学, 2011, 39(2): 235-238

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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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