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复杂样品环境雌激素前处理技术及液相色谱分析方法研究

Development of Pretreatment Methods for Environmental Estrogens and Determination by High Performance Liquid Chromatography

【作者】 董祥芝

【导师】 郭广生; 林金明;

【作者基本信息】 北京化工大学 , 应用化学, 2009, 硕士

【摘要】 环境雌激素是广泛存在于环境中的内分泌干扰物,它们能够干扰人类和动物的内分泌系统,使人类和生物的持续生存与繁衍受到威胁。因此近年来,环境样品中雌激素的检测受到人们广泛的重视,研究和建立雌激素分析方法对于环境保护具有重要意义。样品前处理技术是制约环境分析化学发展的瓶颈,随着科技的发展,高灵敏性、高选择性、简便、经济实用的分析新方法的研究日益受到重视。复杂环境样品如天然水体、底泥、生物样品等,常常具有基质复杂、去除困难等特点。本文利用两种样品前处理技术对不同环境样品中的环境雌激素进行分离萃取,并联用高效液相色谱对目标物进行定量检测。主要工作如下:1、利用分散固相萃取技术对水生动物样品中的雌二醇、雌三醇、4-羟基雌二醇和2-甲氧基雌二醇等环境雌激素进行分离萃取,采用高效液相色谱进行定性定量分析。考察并优化了仪器的主要参数和实验条件。应用所建立的分散固相萃取-高效液相色谱法,实现了对实际样品中四种雌激素的测定,实验结果表明,本方法具有分离速度快、富集倍数大、回收率高、操作简便、成本低等优点,在环境水样及生物样品的环境雌激素的分析方面,具有很好的应用前景。2、利用免疫磁颗粒的磁性和抗原抗体反应的专一性,对环境水样中的雌二醇进行分离萃取,并使用高效液相色谱方法来定量分析。对实验进行优化后,具有高灵敏度、专一性、快速并且重现性好的优点。对基质特别复杂的水样,可以先经过固相萃取,再采用本方法。结果表明,本方法对雌二醇有很好的萃取检测作用,可以代替传统的分析方法。

【Abstract】 Environmental estrognes is a class of endocrine-disrupting compounds in environment.It may affect human and animals on their normal endocrines, which would pose a threat to the sustaind living and proliferation.For fast monitoring of the environmental estrogens,sensitive,rapid and simple analytical methods are necessary.Pretreatment methods are restricting the development of environmental analytical chemistry.Along with the technological development,study on high sensitivity,high selectivity,simple and economical pretreatment methods are get more and more attention.Complex environmental samples,such as natural water,sediments and biological samples,often with complicated and varied matrix.The present paper used two pretreatrnent methods to extraction estrogens from different environmental samples,and analyzed by high-performance liquid chromatography(HPLC).The main study is giving as follows:1.The 17β-Estradiol(E2),estriol(E3) and their estrogen metabolites 4-hydroxyestradiol(4-OHE2) and 2-methoxyestradiol(2-MeOE2) in aquatic animal samples were pretreatment by dispersive solid-phase extraction (dispersive-SPE) and analyzed by high-performance liquid chromatography (HPLC).In this paper,the parameters of dispersive-SPE were investigated in details,and the optimal conditions of dispersive-SPE were obtained.Under the optimal conditions,the four estrogens were extracted and analyzed from aquatic animal samples by dispersive-SPE coupled HPLC.2.A immunomagnetic beads(IMBs)-based immunoassay with HPLC analysis method with high sensitivity,specificity,rapidity,and reproducibility was proposed for the evaluation of E2 in water samples.The SPE process was successfully applied for the water sample pretreatment,which have complicated and varied matrix.And the method is promising to be a simple and effective method for the conventional analysis of E2 in clean water and other intricate matrixes.

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