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生物样品中甲磺基多氯联苯的测定及手性拆分

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张荧, 吴江平, 罗孝俊, 佘雅哲, 麦碧娴. 生物样品中甲磺基多氯联苯的测定及手性拆分[J]. 环境化学, 2012, 31(8): 1165-1170.
引用本文: 张荧, 吴江平, 罗孝俊, 佘雅哲, 麦碧娴. 生物样品中甲磺基多氯联苯的测定及手性拆分[J]. 环境化学, 2012, 31(8): 1165-1170.
shu
ZHANG Ying, WU Jiangping, LUO Xiaojun, SHE Yazhe, MAI Bixian. Determination of methyl sulfonyl polychlorinated biphenyls and their chiral atropisomers in biota samples[J]. Environmental Chemistry, 2012, 31(8): 1165-1170.
Citation: ZHANG Ying, WU Jiangping, LUO Xiaojun, SHE Yazhe, MAI Bixian. Determination of methyl sulfonyl polychlorinated biphenyls and their chiral atropisomers in biota samples[J]. Environmental Chemistry, 2012, 31(8): 1165-1170.
shu

生物样品中甲磺基多氯联苯的测定及手性拆分

  • 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, 广州, 510640;

  • 2.

    中国科学院研究生院, 北京, 100049

  • 基金项目:

    国家自然科学基金项目(41073081,20890112)

    国家重点基础研究发展计划(973计划)项目(2009CB421604)资助.

Determination of methyl sulfonyl polychlorinated biphenyls and their chiral atropisomers in biota samples

  • 1.

    State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, 510640, China;

  • 2.

    Graduate School, Chinese Academy of Science, Beijing, 100049, China

  • Fund Project:

  • 摘要: 建立了一种生物样品中甲磺基多氯联苯(MeSO2-PCBs)及其手性对映体的分析测定方法. 本方法利用索氏抽提对鱼肉组织进行提取, 抽提液依次经凝胶渗透色谱柱、氧化铝硅胶复合柱和弗罗里硅土柱进行净化和分离, 气相色谱-质谱联用仪进行分析. 10个流程空白中, 所有目标化合物都低于仪器检出限; 17种MeSO2-PCBs在5个空白加标中的平均回收率在77.2%-98.2%之间; 样品平行样中目标化合物含量相对标准偏差均小于15%; 方法检测限为0.3-20.0 pg·g-1湿重. 采用Cyclosil-B手性柱拆分5种MeSO2-PCBs手性对映体, 分离度在0.671-2.543之间.
    Abstract: A method was developed for extraction, cleanup and separation in the determination of methyl sulfonyl polychlorinated biphenyls (MeSO2-PCBs) and their chiral atropisomers in biological samples. The target chemicals were Soxhlet extracted, cleaned up by gel permeation chromatography and multi-layer silica alumina, and were further fractioned using Florisil column. MeSO2-PCBs were identified and quantified by gas chromatography-mass spectrometry using electron capture negative ionization mode. No target compound was detected in the procedural blanks, and the average recoveries of the seventeen MeSO2-PCBs in the spiked blanks ranged from 77.2% to 98.2%. The relative standard deviations of the target compounds in duplicate samples were lower than 15%. The method detection limits ranged from 0.3 to 20.0 pg穏-1 wet weight, based on an average sample weight of 8 g. Using a Cyclosil-B chiral chromatography column, five chiral MeSO2-PCBs, i.e., 5'-and 4'-MeSO2-CB 132, 5-and 4-MeSO2-CB 149, and 5'-MeSO2-CB 174 were successfully separated, with the separation degree range of 0.671-2.543.
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  • [1] Routti H, Letcher R J, Arukwe A, et al. Biotransformation of PCBs in relation to phase Ⅰ and Ⅱ xenobiotic-metabolizing enzyme activities in ringed seals (Phoca hispida) from Svalbard and the Baltic Sea [J]. Environ Sci Technol, 2008, 42(23): 8952-8958
    [2] 王斌, 李德远. 细胞色素P450的结构与催化机理 [J]. 有机化学, 2009, 29(4): 658-662
    [3] Letcher R J, Klasson-Whehler E, Bergman . Methyl sulfone and hydroxylated metabolite of polychlorinated biphenyl//Paasivirta J. The handbook of Environmental Chemistry: New Type of Persistent halogenated Compounds. Vol. 3K. Berlin-Heidelberg: Springer-Verlag, 2000: 315-359
    [4] Norströ K, Eriksson J, Haglund J, et al. Enantioselective formation of methyl sulfone metabolites of 2,2',3,3',4,6'-hexachlorobiphenyl in rat [J]. Environ Sci Technol, 2006, 40(24): 7649-7655
    [5] Eljarrat E, Guerra P, Barceló D. Enantiomeric determination of chiral persistent organic pollutants and their metabolites [J]. Trends in Anal Chem, 2008, 27(10): 847-861
    [6] Norström K. Bis(4-chlorophenyl) sulfone and PCB methyl sulfone metabolites-Trends and chirality in the Baltic Sea environment. Sweden: Stockholm University, 2006
    [7] Johansson M, Nilsson S, Lund B O. Interactions between methylsulfonyl PCBs and the glucocorticoid receptor [J]. Environ Health Perspect, 1998, 106(12): 769-772
    [8] Kato Y, Haraguchi K, Shibahara T, et al. Reduction of thyroid hormone levels by methylsulfonyl metabolites of polychlorinated biphenyl congeners in rats [J]. Arch Toxicol, 1998, 72(8): 541-544
    [9] Letcher R J, Norström R J, Bergman . An integrated analytical method for determination of polychlorinated aryl methyl sulfone metabolites and polychlorinated hydrocarbon contaminants in biological matrixes [J]. Anal Chem, 1996, 67(22): 4155-4163
    [10] Wu J P, Luo X J, Zhang Y, et al. Bioaccumulation of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in wild aquatic species from an electronic waste (e-waste) recycling site in South China [J]. Environ Int, 2008, 34(8): 1109-1113
    [11] Zhang Y, Luo X J, Wu J P, et al. Contaminant pattern and bioaccumulation of legacy and emerging organhalogen pollutants in the aquatic biota from an E-waste recycling region in South China [J]. Environ Toxicol Chem, 2010, 29(4): 852-859
    [12] 张磊, 李敬光, 赵云峰, 等. 凝胶渗透色谱法在分析食品中多氯联苯的应用 [J]. 环境化学, 2007, 26(2): 197-201
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  • 收稿日期:  2011-10-21
张荧, 吴江平, 罗孝俊, 佘雅哲, 麦碧娴. 生物样品中甲磺基多氯联苯的测定及手性拆分[J]. 环境化学, 2012, 31(8): 1165-1170.
引用本文: 张荧, 吴江平, 罗孝俊, 佘雅哲, 麦碧娴. 生物样品中甲磺基多氯联苯的测定及手性拆分[J]. 环境化学, 2012, 31(8): 1165-1170.
shu
ZHANG Ying, WU Jiangping, LUO Xiaojun, SHE Yazhe, MAI Bixian. Determination of methyl sulfonyl polychlorinated biphenyls and their chiral atropisomers in biota samples[J]. Environmental Chemistry, 2012, 31(8): 1165-1170.
Citation: ZHANG Ying, WU Jiangping, LUO Xiaojun, SHE Yazhe, MAI Bixian. Determination of methyl sulfonyl polychlorinated biphenyls and their chiral atropisomers in biota samples[J]. Environmental Chemistry, 2012, 31(8): 1165-1170.
shu

生物样品中甲磺基多氯联苯的测定及手性拆分

  • 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, 广州, 510640;
  • 2.  中国科学院研究生院, 北京, 100049
  • 收稿日期:  2011-10-21
基金项目:

国家自然科学基金项目(41073081,20890112)

国家重点基础研究发展计划(973计划)项目(2009CB421604)资助.

摘要: 建立了一种生物样品中甲磺基多氯联苯(MeSO2-PCBs)及其手性对映体的分析测定方法. 本方法利用索氏抽提对鱼肉组织进行提取, 抽提液依次经凝胶渗透色谱柱、氧化铝硅胶复合柱和弗罗里硅土柱进行净化和分离, 气相色谱-质谱联用仪进行分析. 10个流程空白中, 所有目标化合物都低于仪器检出限; 17种MeSO2-PCBs在5个空白加标中的平均回收率在77.2%-98.2%之间; 样品平行样中目标化合物含量相对标准偏差均小于15%; 方法检测限为0.3-20.0 pg·g-1湿重. 采用Cyclosil-B手性柱拆分5种MeSO2-PCBs手性对映体, 分离度在0.671-2.543之间.

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