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
查看参考文献12篇
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文摘
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建立了一种生物样品中甲磺基多氯联苯(MeSO_2-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MeSO_2-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MeSO_2-PCBs手性对映体,分离度在0.671—2.543之间. |
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其他语种文摘
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A method was developed for extraction,cleanup and separation in the determination of methyl sulfonyl polychlorinated biphenyls(MeSO_2-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 MeSO_2-PCBs,i.e.,5′-and 4′-MeSO2-CB 132,5-and 4-MeSO2-CB 149,and 5′-MeSO_2-CB 174 were successfully separated,with the separation degree range of 0.671—2.543. |
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来源
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环境化学
,2012,31(8):1165-1170 【核心库】
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关键词
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甲磺基多氯联苯
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分析测定
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弗罗里硅土柱
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手性
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Cyclosil-B手性柱
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地址
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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
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语种
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中文 |
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ISSN
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0254-6108 |
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学科
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环境质量评价与环境监测 |
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基金
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国家973计划
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国家自然科学基金项目
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文献收藏号
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CSCD:4604692
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参考文献 共
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