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采用中心切割 MDGC 同时对多氯联苯及其甲基砜代谢物进行对映体选择性分离:鱼油和牛肝样品中对映体分数的测定。

Simultaneous enantioselective separation of polychlorinated biphenyls and their methyl sulfone metabolites by heart-cut MDGC: determination of enantiomeric fractions in fish oils and cow liver samples.

机构信息

Department of Instrumental Analysis and Environmental Chemistry, Institute of General Organic Chemistry, CSIC, Madrid, Spain.

出版信息

Chirality. 2012 Jul;24(7):577-83. doi: 10.1002/chir.22062. Epub 2012 May 22.

DOI:10.1002/chir.22062
PMID:22615239
Abstract

The potential of three capillary columns based on β-cyclodextrin (i.e., Chirasil-Dex, BGB-172, and BGB-176SE) has been studied for the simultaneous enantiomeric separation of polychlorinated biphenyls (PCBs) and methylsulfonyl metabolites of PCBs (MeSO(2)-PCBs) employing a heart-cut multidimensional gas chromatographic system (heart-cut MDGC). Among the columns studied, the BGB-176SE capillary column provided the best results, allowing the simultaneous enantioselective resolution of six MeSO(2)-PCBs and six chiral PCBs; the Chirasil-Dex column did not resolve any of the studied MeSO(2)-PCBs; and a poor resolution was obtained for three MeSO(2)-PCBs when the BGB-172 column was employed. The developed method was successfully applied to two fish oil and one cow liver samples commercially available, which showed different enantioselective pattern. PCBs 91 and 176 presented a clear enrichment of the second eluted atropisomer in codfish oil, whereas in fish oil sample, slight enrichment of the first eluted atropisomer of CB45 and the second eluted atropisomer of CB136 were observed.

摘要

研究了基于β-环糊精的三种毛细管柱(Chirasil-Dex、BGB-172 和 BGB-176SE)在采用中心切割多维气相色谱系统(中心切割 MDGC)时对手性多氯联苯(PCBs)和 PCBs 的甲基磺酰基代谢物(MeSO(2)-PCBs)的同时对映体分离的潜力。在所研究的柱中,BGB-176SE 毛细管柱提供了最佳结果,允许同时对映选择性拆分六种 MeSO(2)-PCBs 和六种手性 PCB;Chirasil-Dex 柱不能拆分任何研究的 MeSO(2)-PCBs;而当使用 BGB-172 柱时,三种 MeSO(2)-PCBs 的分辨率很差。所开发的方法成功地应用于两种市售鱼油和一种牛肝样品,这些样品显示出不同的对映选择性模式。PCBs 91 和 176 在鳕鱼油中明显富集第二个出峰的对映异构体,而在鱼油样品中,观察到 CB45 的第一个出峰对映异构体和 CB136 的第二个出峰对映异构体略有富集。

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