硅胶表面功能化修饰色谱分离材料的制备与评价
发布时间：2018-08-23 15:53
【摘要】：色谱分离材料是色谱技术的核心,是各种色谱分离模式建立和发展的基础。开发和研究具有优良性能的新型色谱分离材料一直以来都是色谱研究领域的热点之一。其中,以球形多孔硅胶为载体,在其表面进行化学键合与功能化修饰,制备得到不同类型基团的固定相,已成为现代色谱分离的主导填料。本研究基于以上研究背景,制备了三种液相色谱固定相分离材料,并对其进行了评价。主要研究内容如下:1.将2-甲基咪唑修饰在硅胶表面,制备了一种新型亲水作用和阴离子交换混合色谱固定相。利用元素分析和红外光谱技术对其进行了表征。通过分离8种碱基核苷、6种磺胺类化合物、5种水溶性维生素和5种糖类化合物,考察了其亲水色谱性能;通过分离6种无机阴离子,考察了其阴离子交换色谱性能。通过改变流动相中乙腈含量、盐浓度和pH值,考察不同色谱条件对碱基核苷在固定相上保留的影响,并与已被报道过的1-甲基咪唑键合硅胶固定相比较,发现2-甲基咪唑键合硅胶固定相展现出相似的、甚至更好的分离选择性。2.利用新型绿色溶剂——低共熔溶剂作反应溶剂,通过表面自由基链转移反应,将乙烯咪唑和丙烯酸分别通过单体聚合或共聚的方式修饰在硅胶表面,得到聚乙烯咪唑键合硅胶、聚丙烯酸键合硅胶、乙烯咪唑和丙烯酸共聚键合硅胶三种固定相材料。利用元素分析和红外光谱技术对三种固定相材料进行了表征。通过分离9种碱基核苷、8种氨基酸和6种糖类化合物,考察其亲水色谱性能。通过改变流动相中乙腈含量、盐浓度、p H值和改变柱温,考察不同色谱条件对碱基核苷在三种固定相上保留的变化。结果表明,低共熔溶剂可以作为制备聚合型硅胶固定相的反应溶剂。3.以2-甲基咪唑键合硅胶为前体,提出了一种制备ZIF-8@SiO_2核壳型微球材料的新方法。利用扫描电镜法、X射线衍射法、红外光谱法和元素分析法对其进行了表征。通过表征结果发现ZIF-8被成功地修饰在SiO_2的表面,其应用有待进一步拓展。
[Abstract]:Chromatographic separation materials are the core of chromatographic technology and the basis for the establishment and development of various chromatographic separation models. The development and research of new chromatographic separation materials with excellent performance has always been one of the hot spots in the field of chromatographic research. Among them, the spherical porous silica gel was used as the carrier, the surface was chemically bonded and functionalized, and the stationary phase with different groups was prepared, which has become the dominant packing for modern chromatographic separation. Based on the above research background, three kinds of stationary phase separation materials for liquid chromatography were prepared and evaluated. The main research contents are as follows: 1. A novel hydrophilic and anion exchange stationary phase was prepared by modifying 2-methylimidazole on silica gel. It was characterized by elemental analysis and infrared spectroscopy. The hydrophilic chromatographic properties of 8 base nucleoside compounds, 6 sulfonamides, 5 water soluble vitamins and 5 carbohydrates were studied, and the anion exchange chromatography was studied by separating 6 inorganic anions. By changing the acetonitrile content, salt concentration and pH value in the mobile phase, the effects of different chromatographic conditions on the retention of nucleoside on the stationary phase were investigated, and compared with the reported stationary phase of 1-methylimidazole-bonded silica gel. It was found that the stationary phase of 2-methylimidazole-bonded silica gel showed similar, even better separation selectivity. Using a new green solvent-low eutectic solvent as the reaction solvent, ethylene imidazole and acrylic acid were modified on the surface of silica gel by monomer polymerization or copolymerization respectively through the free radical chain transfer reaction on the surface, the polyvinylimidazole-bonded silica gel was obtained. Polyacrylic acid bonded silica gel, ethylene imidazole and acrylic acid copolymerization bonded silica gel three stationary phase materials. Three kinds of stationary phase materials were characterized by elemental analysis and infrared spectroscopy. The hydrophilic chromatographic properties of 9 nucleosides and 6 carbohydrates were studied by separating 9 kinds of nucleoside and 6 kinds of carbohydrates. By changing the acetonitrile content, salt concentration and column temperature in the mobile phase, the changes of nucleoside retention on the three stationary phases were investigated under different chromatographic conditions. The results show that the low eutectic solvent can be used as the reaction solvent for the preparation of polymeric silica gel stationary phase. A new method for preparing ZIF-8@SiO_2 core-shell microspheres was proposed using 2-methylimidazole-bonded silica gel as precursor. It was characterized by scanning electron microscopy (SEM), infrared spectroscopy (IR) and elemental analysis. The characterization results show that ZIF-8 is successfully modified on the surface of SiO_2, and its application needs further development.
【学位授予单位】：新疆师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652.6
[Abstract]:Chromatographic separation materials are the core of chromatographic technology and the basis for the establishment and development of various chromatographic separation models. The development and research of new chromatographic separation materials with excellent performance has always been one of the hot spots in the field of chromatographic research. Among them, the spherical porous silica gel was used as the carrier, the surface was chemically bonded and functionalized, and the stationary phase with different groups was prepared, which has become the dominant packing for modern chromatographic separation. Based on the above research background, three kinds of stationary phase separation materials for liquid chromatography were prepared and evaluated. The main research contents are as follows: 1. A novel hydrophilic and anion exchange stationary phase was prepared by modifying 2-methylimidazole on silica gel. It was characterized by elemental analysis and infrared spectroscopy. The hydrophilic chromatographic properties of 8 base nucleoside compounds, 6 sulfonamides, 5 water soluble vitamins and 5 carbohydrates were studied, and the anion exchange chromatography was studied by separating 6 inorganic anions. By changing the acetonitrile content, salt concentration and pH value in the mobile phase, the effects of different chromatographic conditions on the retention of nucleoside on the stationary phase were investigated, and compared with the reported stationary phase of 1-methylimidazole-bonded silica gel. It was found that the stationary phase of 2-methylimidazole-bonded silica gel showed similar, even better separation selectivity. Using a new green solvent-low eutectic solvent as the reaction solvent, ethylene imidazole and acrylic acid were modified on the surface of silica gel by monomer polymerization or copolymerization respectively through the free radical chain transfer reaction on the surface, the polyvinylimidazole-bonded silica gel was obtained. Polyacrylic acid bonded silica gel, ethylene imidazole and acrylic acid copolymerization bonded silica gel three stationary phase materials. Three kinds of stationary phase materials were characterized by elemental analysis and infrared spectroscopy. The hydrophilic chromatographic properties of 9 nucleosides and 6 carbohydrates were studied by separating 9 kinds of nucleoside and 6 kinds of carbohydrates. By changing the acetonitrile content, salt concentration and column temperature in the mobile phase, the changes of nucleoside retention on the three stationary phases were investigated under different chromatographic conditions. The results show that the low eutectic solvent can be used as the reaction solvent for the preparation of polymeric silica gel stationary phase. A new method for preparing ZIF-8@SiO_2 core-shell microspheres was proposed using 2-methylimidazole-bonded silica gel as precursor. It was characterized by scanning electron microscopy (SEM), infrared spectroscopy (IR) and elemental analysis. The characterization results show that ZIF-8 is successfully modified on the surface of SiO_2, and its application needs further development.
【学位授予单位】：新疆师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652.6
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