生物样品中甲磺基多氯联苯的测定及手性拆分  

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

作　　者：张荧[1,2] 吴江平[1] 罗孝俊[1] 佘雅哲[1,2] 麦碧娴[1] 

机构地区：[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

出　　处：《环境化学》2012年第8期1165-1170,共6页Environmental Chemistry

基　　金：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.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 · g^-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.

关 键 词：甲磺基多氯联苯 分析测定 弗罗里硅土柱 手性 Cyclosil-B手性柱 

分 类 号：X835[环境科学与工程—环境工程]