型态可调阳离子有机物的两种毛细管电泳柱上富集新机制的研究

发布时间：2018-06-16 00:12

本文选题：毛细管电泳柱上富集 + pH调制堆积　；参考：《河北大学》2016年硕士论文

【摘要】：高效毛细管电泳技术具有分析速度快、分离效率高等优点,为了进一步提高毛细管电泳方法的灵敏度,基于毛细管柱的柱上富集方法一直是毛细管电泳研究的热点之一,本文建立了型态可调阳离子有机物的两种毛细管电泳柱上富集的新机制,旨在提高其在毛细管电泳检测中的灵敏度,同时寻求一种简单快速、绿色环保的毛细管电泳柱上富集检测方法。本文共分3章,其主要内容如下:第1章:绪论。介绍了高效毛细管电泳分离的基本原理及分离的突出特点,详细综述了近年来高效毛细管电泳柱上富集的方法及其研究进展,在文献调研的基础上发现各个富集方法的优劣之处,对型态可调阳离子有机物毛细管电泳柱上富集的研究提供了思路和方法。第2章:本章建立了pH调制堆积技术检测型态可调阳离子有机物的新机制。该机制通过样品区带pH的变化,调节样品区带的电导率和型态可调阳离子有机物的带电状态,从而改变分析物迁移速率实现其柱上富集,该机制具有操作简单、快速,绿色环保等特点。在本工作中,以选择苯胺类和维生素B类物质作为型态可调阳离子有机物分析模型分子,进行了pH调制新机制的分析与检测:通过酸引入pH调制堆积对环境水样中的联苯胺和邻-甲基苯胺进行了富集分离,加标回收率在94.3-101.7%之间;通过碱引入pH调制堆积对人体尿样中的维生素B1和烟酰胺进行了富集分离,加标率在83.4-106.3%之间。第3章:本章建立了水凝胶半封闭毛细管柱抑制电渗流-瞬时等速电泳检测型态可调阳离子有机物的新机制。本文用水凝胶将毛细管柱的一端进行封闭,减弱了毛细管柱中液体的整体流动,抑制了电渗流。与高酸度条件下抑制电渗流的方法相比,水凝胶半封闭毛细管柱电渗流抑制法更容易在较高pH条件下,实现瞬时等速电泳柱上富集。与传统的毛细管柱壁改性修饰抑制电渗流法相比,水凝胶半封闭法达到电渗流抑制目的的实验操作更为简单。首先,选取二甲亚砜(DMSO)为中性标记物,以毛细管区带电泳为分离模式,对比了不同pH值下电泳分离过程中在毛细管柱阳极端使用或不使用水凝胶时,DMSO的出峰时间的变化,从而对半封闭毛细管抑制电泳中的电渗流方法的可靠性进行了验证。然后,以三聚氰胺作为型态可调阳离子有机物的分析物模型,电泳时使用水凝胶半封闭毛细管柱,在较高pH值下(pH5.6)通过瞬时等速电泳富集法检测了牛奶中的三聚氰胺。三聚氰胺在0.01-10 mg/L范围内峰面积与浓度具有良好的线性,实际牛奶样品的加标回收率在89.1-113.8%之间。
[Abstract]:High performance capillary electrophoresis (HPCE) has the advantages of fast analysis and high separation efficiency. In order to further improve the sensitivity of capillary electrophoresis, capillary column enrichment method has always been one of the hotspots in capillary electrophoresis. In this paper, two capillary electrophoresis columns with adjustable Yang separated organic compounds were enriched. The new mechanism is designed to improve its sensitivity in capillary electrophoresis detection and to seek a simple, fast, green and environmentally friendly capillary electrophoresis column enrichment detection method. This paper is divided into 3 chapters. The main contents are as follows: first chapter: introduction. The basic principle of high performance capillary electrophoresis separation and the outstanding characteristics of separation are introduced. The method and progress in the enrichment of high performance capillary electrophoresis (HPCE) on the column of high performance capillary electrophoresis (HPCE) have been found on the basis of literature research, and the advantages and disadvantages of the enrichment methods are found. The second chapter: this chapter has established the adjustable cation of pH modulation Accumulation Technology in this chapter. A new mechanism of organic matter. Through the change of pH in the sample area, the mechanism regulates the electrical conductivity of the sample zone and the electrified state of the cationic organic matter, thus changing the migration rate of the analyte to the enrichment of the column. This mechanism has the characteristics of simple operation, rapid and green environmental protection. In this work, the selection of aniline and vitamin B is selected. As a model molecule of adjustable cationic organic matter analysis model, a new mechanism of pH modulation was analyzed and detected. Through the introduction of acid into pH modulation accumulation, the concentration and separation of benzidine and O methylaniline in environmental water samples were enriched and the recovery rate was between 94.3-101.7%; pH modulation accumulation was introduced to the dimension of human urine by the alkali introduction. The concentration and separation of raw B1 and nicotinamide were concentrated and separated and the standard rate was between 83.4-106.3%. The third chapter: a new mechanism of adjustable cation organics was established by the hydrogel semi closed capillary column restraining the electroosmotic percolation transient isokinetic electrophoresis. The end of the capillary column was closed by the hydrogel, and the liquid whole in the capillary column was weakened. Compared with the method of suppressing the electroosmotic seepage under high acidity, the hydrogel semi closed capillary column electroosmotic seepage suppression method is more likely to be enriched in the instantaneous isokinetic electrophoresis column under the higher pH condition. Compared with the traditional capillary wall modified modified electroosmotic flow method, the hydrogel semi closed method achieves the electroosmotic flow suppression. The experimental operation of the purpose is more simple. First, two methyl sulfoxide (DMSO) is selected as neutral marker, and capillary zone electrophoresis is used as the separation mode. The variation of the peak time of the DMSO in the capillary positive or non use of hydrogels at the capillary column sun at different pH values is compared. The reliability of the electroosmotic method was verified. Then, using melamine as an analytical model of the adjustable cationic organic matter, a hydrogel semi closed capillary column was used for electrophoresis to detect melamine in milk at a high pH value (pH5.6) by instantaneous isokinetic electrophoresis enrichment. The peak of melamine in the range of 0.01-10 mg/L was detected. The area and concentration had good linearity, and the recovery rate of the actual milk samples was between 89.1-113.8%.
【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O658.9

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