毛细管电泳-安培检测在雌酚类激素分析中的应用
本文选题:毛细管电泳 + 安培检测 ; 参考:《辽宁师范大学》2015年硕士论文
【摘要】:毛细管电泳(Capillary Electrophoresis,CE)是一种在毛细管中待测物溶液以高压电场为驱动力实现高效快速分离的分离技术。随着近年来的发展,其应用的范围更加广泛,已经应用在药物、食品、生物以及环境分析等各个领域。雌酚类激素因能够促进动物生长、增加乳产量等作用而被广泛应用于动物生产,这些激素通过食物链,进入人体内,有致癌等毒副作用,包括己烯雌酚、己烷雌酚和双烯雌酚。目前,单独检测己烯雌酚和检测己烯雌酚及其他雌激素的报道有很多,而同时检测己烯雌酚、己烷雌酚和双烯雌酚的报道还比较少见,同时检测分离这三种物质具有很大的意义。本论文基于毛细管电泳—安培检测技术独特的优点,从新缓冲体系的研究入手,定性定量雌酚类激素及其相关药物和鱼肉中的残留成分,使毛细管电泳-安培检测的应用范围更广泛。本文主要包括以下三个部分:第一章:绪论该章介绍了毛细管电泳概况,重点介绍了毛细管电泳样品预富集技术和在线样品富集技术,环糊精的结构和性质以及在分析化学中的应用,并简单的介绍了雌激素残留的主要途径及对环境和人类的影响,雌激素的研究进展,阐述了本文的选题意义。第二章:β-环糊精修饰胶束电动毛细管色谱法对雌酚类激素的检测本文建立了β-环糊精修饰胶束毛细管电泳-安培检测联用技术测定雌酚类激素己烷雌酚(HEX)、己烯雌酚(DES)和双烯雌酚(DE)残留的新方法。研究了一种毛细管电泳-电化学检测(CZE-AD)的新缓冲体系,此体系可在酸性条件下,运用β-环糊精和胶束SDS对样品进行检测。实验考察了缓冲体系的组成、浓度、分离电压、检测电位及进样时间等对实验结果的影响。DE、HEX与DES的分别在4×10-5-5×10-4 mol/L,1×10-5-5×10-4mol/L和1×10-5-5×10-4 mol/L范围内呈良好线性,相关系数(r2)分别为0.9819、0.9939、0.9867,检出限为10-6 mol/L。本方法选择性好,分析速度快,操作简单,能够在复杂混合物中测定各组分,并得出满意的结果。第三章:毛细管电泳-安培检测法测定动物组织中3种雌酚类激素的研究建立了毛细管区带电泳-安培检测法同时对三种雌酚类激素己烷雌酚(HEX)、己烯雌酚(DES)及双烯雌酚(DE)的残留量进行测定。研究了缓冲体系的组成、浓度、分离电压、检测电位以及进样时间等对实验结果的影响。本方法线性范围宽,目标组分在10-7-10-5mol/L范围内呈良好线性,检出限(LOD)低,达到10-9-10-8 mol/L,灵敏度比以往文献高,且在实际样品中也能很好的检测。
[Abstract]:Capillary Electrophoresis (CE) is a separation technique for high efficiency and rapid separation of the solution in a capillary with high pressure electric field as the driving force. With the development of recent years, its application has been widely used in various fields, such as drugs, food, raw materials and environmental analysis. It is widely used in animal production to promote animal growth and increase milk production. These hormones enter the human body through the food chain and have the toxic and side effects of carcinogenesis, including diethylstilbestrol, hexbestrol and dienethylstilbestrol. There are many reports of diethylstilbestrol and diethylstilbestrol and other estrogens at the same time. The reports of diethylstilbestrol, hexbestrol and dienethylstilbestrol are relatively rare, and the detection of these three substances is of great significance. Based on the unique advantages of capillary electrophoresis - ampere detection technology, this paper, starting with the study of the new buffer system, qualitatively and quantitatively quantified the residual components in the estradiol and related drugs and fish. The application scope of capillary electrophoresis - ampere detection is more extensive. This article mainly includes the following three parts: Chapter 1: introduction to introduction of the general situation of capillary electrophoresis, focusing on capillary electrophoresis sample preconcentration technology and on-line sample enrichment technology, structure and properties of cyclodextrin, and its application in analytical chemistry, and simple The main ways of estrogen residue and its influence on environment and human were introduced. The research progress of estrogen and the significance of this topic were expounded. The second chapter: beta cyclodextrin modified micellar electrokinetic capillary chromatography for the determination of estrin, the determination of female by beta cyclodextrin modified gel capillary electrophoresis and amperometric detection was established. A new method for the residue of hexenostrol (HEX), diethylstilbestrol (DES) and diethylstilbestrol (DE) of phenolic hormones. A new buffer system for capillary electrophoresis electrochemical detection (CZE-AD) was studied. The system can be detected by beta cyclodextrin and micellar SDS under acidic conditions. The composition, concentration and separation voltage of the buffer system are investigated experimentally. The effect of detection potential and sampling time on the experimental results.DE, HEX and DES are in good linearity in the range of 4 x 10-5-5 x 10-4 mol/L, 1 x 10-5-5 x 10-4mol/L and 1 x 10-5-5 x 10-4 mol/L, and the correlation coefficient (R2) is 0.9819,0.9939,0.9867, the detection limit is 10-6 mol/L. this method is selective, the analysis speed is fast, the operation is simple and can be used. The third chapter: the determination of 3 kinds of estradiol in animal tissues by capillary electrophoresis and amperometric detection established the capillary zone electrophoresis ampere detection method and the residue of three diethylstilbestrolestones (HEX), diethylstilbestrol (DES) and diethylstilbestrol (DE) The influence of the composition of the buffer system, the concentration, the separation voltage, the detection potential and the sampling time on the experimental results is studied. The linear range of the method is wide, the target component is in good linearity in the range of 10-7-10-5mol/L, the detection limit (LOD) is low, 10-9-10-8 mol/L is reached, and the sensitivity is higher than the previous literature, and it can also be good in the actual sample. Testing.
【学位授予单位】:辽宁师范大学
【学位级别】:硕士
【学位授予年份】:2015
【分类号】:O657
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