【摘要】：色譜分離材料是色譜技術的核心,是各種色譜分離模式建立和發(fā)展的基礎。開發(fā)和研究具有優(yōu)良性能的新型色譜分離材料一直以來都是色譜研究領域的熱點之一。其中,以球形多孔硅膠為載體,在其表面進行化學鍵合與功能化修飾,制備得到不同類型基團的固定相,已成為現(xiàn)代色譜分離的主導填料。本研究基于以上研究背景,制備了三種液相色譜固定相分離材料,并對其進行了評價。主要研究內容如下:1.將2-甲基咪唑修飾在硅膠表面,制備了一種新型親水作用和陰離子交換混合色譜固定相。利用元素分析和紅外光譜技術對其進行了表征。通過分離8種堿基核苷、6種磺胺類化合物、5種水溶性維生素和5種糖類化合物,考察了其親水色譜性能;通過分離6種無機陰離子,考察了其陰離子交換色譜性能。通過改變流動相中乙腈含量、鹽濃度和pH值,考察不同色譜條件對堿基核苷在固定相上保留的影響,并與已被報道過的1-甲基咪唑鍵合硅膠固定相比較,發(fā)現(xiàn)2-甲基咪唑鍵合硅膠固定相展現(xiàn)出相似的、甚至更好的分離選擇性。2.利用新型綠色溶劑——低共熔溶劑作反應溶劑,通過表面自由基鏈轉移反應,將乙烯咪唑和丙烯酸分別通過單體聚合或共聚的方式修飾在硅膠表面,得到聚乙烯咪唑鍵合硅膠、聚丙烯酸鍵合硅膠、乙烯咪唑和丙烯酸共聚鍵合硅膠三種固定相材料。利用元素分析和紅外光譜技術對三種固定相材料進行了表征。通過分離9種堿基核苷、8種氨基酸和6種糖類化合物,考察其親水色譜性能。通過改變流動相中乙腈含量、鹽濃度、p H值和改變柱溫,考察不同色譜條件對堿基核苷在三種固定相上保留的變化。結果表明,低共熔溶劑可以作為制備聚合型硅膠固定相的反應溶劑。3.以2-甲基咪唑鍵合硅膠為前體,提出了一種制備ZIF-8@SiO_2核殼型微球材料的新方法。利用掃描電鏡法、X射線衍射法、紅外光譜法和元素分析法對其進行了表征。通過表征結果發(fā)現(xiàn)ZIF-8被成功地修飾在SiO_2的表面,其應用有待進一步拓展。
[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.
【學位授予單位】：新疆師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O652.6

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本文編號：2199551