新型高效液相色谱固定相的制备及其色谱性能的研究

发布时间：2018-07-05 18:48

本文选题：高效液相色谱 + 色谱柱填料的制备　；参考：《青岛大学》2016年硕士论文

【摘要】：高效液相色谱(High performance liquid chromatography,HPLC)作为一种重要的分离分析方法,已被广泛应用于石油化工、食品、化学、医药和生命科学等众多领域。色谱柱固定相作为色谱分离的核心,其性能直接关系到分离的效率以及检测结果的准确性,因此研究与开发高性能的新型色谱柱填料一直是色谱领域中的热门课题。色谱柱固定相一般按基质的不同可分为无机基质,有机基质和有机-无机复合基质三大类。无机基质固定相中二氧化硅(SiO2)微球因其具有机械强度高,生物相容性好,表面基团丰富等特点而成为目前应用最广泛的高效液相色谱基质填料;而有机基质固定相中又以苯乙烯-二乙烯基苯共聚物(PS-DVB)应用最为广泛。本论文结合无机与有机基质固定相各自的优点,分别对二氧化硅微球的功能化改性新方法以及多孔交联聚苯乙烯微球的制备方法进行了研究,并对制备的新型填料进行了分离检测,取得了较好的效果,主要工作如下:1.采用改进的溶胶-凝胶法(St?ber法),制得了平均粒径约为2.5μm的单分散二氧化硅微球。以自制硅球为基质,利用光交联的反应原理,用水溶性的感光高分子重氮树脂(DR)取代毒性较大的硅烷化试剂实现了对硅球的功能化改性。在紫外光的照射作用下,诱导重氮树脂的原位光交联反应,从而在二氧化硅微球表面引入共价键和的功能性基团。基于重氮树脂的化学结构以及流动相的改变,利用改性后的微球作为色谱柱固定相可实现两种不同的分离模式,并取得了较好的效果。2.采用改进的种子聚合法制备出了具有二元孔结构的单分散交联聚苯乙烯微球,将该微球作为色谱柱填料,不仅分别成功分离了苯类化合物以及富勒烯碳60和碳70,而且由于其优良的通透性,在较高的分离流速下柱压可以维持在较低的水平。本论文所研究的二氧化硅的功能化新技术综合了物理吸附和化学键合方法的诸多优点,通过光照交联即可实现对二氧化硅微球简单快捷的功能化改性,是一种高效,稳定,绿色环保的改性方法;制备出的二元多孔聚苯乙烯微球则有效降低了柱压,提高了分离效率。这些新型色谱柱填料的制备技术对进一步优化高效液相色谱柱填料的制备有一定的指导意义。
[Abstract]:High performance liquid chromatography (HPLC), as an important separation and analysis method, has been widely used in many fields, such as petrochemical, food, chemistry, medicine and life science. The chromatographic column fixed phase is the core of the chromatographic separation, its performance is directly related to the efficiency of separation and the accuracy of the detection results. Therefore, the research and development of high performance new chromatographic column filler has always been a hot topic in the field of chromatography. The stationary phase of chromatographic column can be divided into inorganic matrix, organic matrix and organic inorganic composite matrix according to the difference of matrix. The silica (SiO2) microspheres in the fixed phase of inorganic matrix have high mechanical strength and biological strength. Good compatibility and rich surface groups have become the most widely used matrix filler in high performance liquid chromatography, and the most widely used in organic matrix stationary phase is styrene two vinyl benzene copolymer (PS-DVB). This paper combines the advantages of both inorganic and organic matrix fixed phase, and the function of silica microspheres respectively. The new method of modification and the preparation of porous crosslinked polystyrene microspheres have been studied, and the new packing has been separated and detected. The main work is as follows: 1. the mono dispersed silica microspheres with an average particle size of about 2.5 u m were prepared by the improved sol-gel method (St? BER). Based on the reaction principle of light crosslinking, a water-soluble photoreceptor diazonium resin (DR) has been replaced by a highly toxic silane reagent for the functional modification of silicon spheres. In situ light crosslinking reaction of diazo resin is induced under UV irradiation, thus introducing covalent bonds and functions on the surface of silica microspheres. Based on the chemical structure of the diazo resin and the change of the liquid phase, two different separation modes can be achieved by using the modified microspheres as the stationary phase of the chromatographic column, and a better effect.2. is achieved by the improved seed polymerization method to prepare the monodisperse crosslinked polystyrene microspheres with a two element pore structure. The microspheres are used as the microspheres. The chromatographic column packing has not only successfully separated the benzene compounds, fullerene carbon 60 and carbon 70, but also the column pressure can be maintained at a lower level at a high separation flow rate. The new functional technology of silica has integrated the advantages of physical adsorption and chemical bonding methods. The simple and quick functional modification of silica microspheres can be achieved through cross-linking of light. It is a highly efficient, stable, green and environmental modification method. The prepared two element porous polystyrene microspheres can effectively reduce the column pressure and improve the separation efficiency. The preparation technology of these new chromatographic columns is used to optimize the high efficiency liquid phase color. The preparation of the column packing has some guiding significance.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.72

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