混合模式毛细管整体柱的制备以及色谱行为研究
发布时间：2018-08-23 12:08
【摘要】：毛细管整体柱是一种用有机或无机聚合方法在色谱柱内进行原位聚合的连续床固定相。与传统的填充柱相比,毛细管整体柱具有制备简单、无需烧结塞子、通透性好、低柱压等优点,已成为当今色谱领域研究的热点之一。混合模式色谱是指同时应用多种作用力使溶质和固定相进行保留和分离的色谱方法。相比于单一色谱模式,混合模式色谱具有高选择性、高分离效率等优势,能够满足对复杂样品的分离分析。基于此,本文致力于发展两种具有高效分离能力的混合模式的毛细管整体柱,系统地探讨了这类整体柱的色谱保留行为及分离机理,并将其应用于多肽和蛋白酶解物等的分离研究。本论文主要从以下三个方面进行阐述：第一章综述微柱液相色谱的原理和分类,毛细管整体柱的制备、分类,混合模式色谱,并介绍了本论文的研究意义与研究内容。第二章以3-[N,N-二甲基-[2-(2-甲基丙-2-烯酰氧基)乙基]铵]丙烷-1-磺酸内盐(SPE)为有机功能单体,季戊四醇三丙烯酸酯(PETA)为亲水交联剂,以环己醇和乙二醇为二元致孔剂,通过原位聚合制备了混合模式的poly(SPE-co-PETA)有机聚合物基质整体柱。实验考察了单体、交联剂以及致孔剂的加入量以及它们的配比对整体柱表面形貌、渗透性、以及色谱性能的影响。详细讨论了poly(SPE-co-PETA)整体柱对苯系物、酰胺类、苯胺类和苯酚类化合物的选择性,结果表明该整体柱具备疏水、亲水和离子交换等色谱性能。利用该有机聚合整体柱可成功地实现苯酚类、核苷酸、碱基、多肽等的高效分离。第三章以谷胱甘肽(GSH)为有机功能单体,以四甲氧基硅烷(TMOS)和3-(甲基丙烯酰氧)丙基三甲氧基硅烷(γ-MAPS)为前驱体,通过将巯基-烯点击化学和“一锅”法相结合,制备了一种新型的有机-无机杂化整体柱。系统地考察了TMOS/γ-MAPS配比、GSH以及致孔剂用量对整体柱骨架渗透性、孔径和表面积以及色谱性能等影响。在最优的合成条件下,该整体柱呈现致密、均一的网格结构,良好的渗透性以及高的比表面积。分别以烷基苯系物、酰胺类、苯胺类等为考察对象,评价该杂化整体柱的疏水、亲水和离子交换等色谱性能。在0.47mm/s的线速度下分离苯系物时,柱效高达80,000～124,000 plates/m。该杂化整体柱可成功地应用于核苷酸,多肽,蛋白酶解物的高效分离。
[Abstract]:Capillary monolithic column is a continuous bed stationary phase in which organic or inorganic polymerization is carried out in situ polymerization in chromatographic column. Compared with the traditional packed column, the capillary monolithic column has the advantages of simple preparation, no sintering plug, good permeability and low column pressure, and has become one of the hot spots in the field of chromatography. Mixed mode chromatography (MMC) is a chromatographic method by which solute and stationary phase can be retained and separated simultaneously by multiple forces. Compared with the single chromatographic mode, mixed mode chromatography has the advantages of high selectivity and high separation efficiency, and can be used for the separation and analysis of complex samples. Based on this, two kinds of capillary monolithic columns with high efficiency separation ability were developed, and the chromatographic retention behavior and separation mechanism of these monolithic columns were systematically discussed. It was applied to the separation of peptides and proteolytic compounds. In chapter 1, the principle and classification of microcolumn liquid chromatography, the preparation, classification and mixing mode chromatography of capillary monolithic column are reviewed. In chapter 2, 3- [N- N- dimethyl- [2- (2-methylallyl-2-allyloxy) ethyl] ammonium] propane-1-sulfonic acid (SPE) as organic functional monomer, pentaerythritol triacrylate (PETA) as hydrophilic crosslinking agent, cyclohexanol and ethylene glycol as binary porous agents, Poly (SPE-co-PETA) organic polymer matrix monolithic column with mixed mode was prepared by in situ polymerization. The effects of monomer, crosslinking agent and pore-forming agent on the surface morphology, permeability and chromatographic properties of the monolithic column were investigated. The selectivity of poly (SPE-co-PETA) monolithic column to benzenes, amides, anilines and phenols was discussed in detail. The results showed that the monolithic column had hydrophobic, hydrophilic and ion exchange properties. The separation of phenols, nucleotides, bases and polypeptides can be successfully achieved by using the organic polymerized monolithic column. In Chapter 3, using glutathione (GSH) as organic functional monomer and tetramethoxysilane (TMOS) and 3- (methacryloxy) propyltrimethoxysilane (纬 -MAPS) as precursors, mercapto-vinyl click-chemistry was combined with "one pot" method. A novel organic-inorganic hybrid monolithic column was prepared. The effects of TMOS/ 纬 -MAPS ratio and the amount of pore-forming agent on the permeability, pore size, surface area and chromatographic performance of monolithic column were systematically investigated. Under the optimal synthesis conditions, the monolithic column exhibits dense, uniform mesh structure, good permeability and high specific surface area. The hydrophobic, hydrophilic and ion-exchange chromatographic properties of the hybrid monolithic column were evaluated with alkyl benzene series, amides and anilines, respectively. The column efficiency of the separation of benzene series at the linear velocity of 0.47mm/s was as high as 800 000 plates / m. The hybrid monolithic column can be successfully applied to the separation of nucleotides, polypeptides and protease hydrolysates.
【学位授予单位】：福州大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R917;O657.7
[Abstract]:Capillary monolithic column is a continuous bed stationary phase in which organic or inorganic polymerization is carried out in situ polymerization in chromatographic column. Compared with the traditional packed column, the capillary monolithic column has the advantages of simple preparation, no sintering plug, good permeability and low column pressure, and has become one of the hot spots in the field of chromatography. Mixed mode chromatography (MMC) is a chromatographic method by which solute and stationary phase can be retained and separated simultaneously by multiple forces. Compared with the single chromatographic mode, mixed mode chromatography has the advantages of high selectivity and high separation efficiency, and can be used for the separation and analysis of complex samples. Based on this, two kinds of capillary monolithic columns with high efficiency separation ability were developed, and the chromatographic retention behavior and separation mechanism of these monolithic columns were systematically discussed. It was applied to the separation of peptides and proteolytic compounds. In chapter 1, the principle and classification of microcolumn liquid chromatography, the preparation, classification and mixing mode chromatography of capillary monolithic column are reviewed. In chapter 2, 3- [N- N- dimethyl- [2- (2-methylallyl-2-allyloxy) ethyl] ammonium] propane-1-sulfonic acid (SPE) as organic functional monomer, pentaerythritol triacrylate (PETA) as hydrophilic crosslinking agent, cyclohexanol and ethylene glycol as binary porous agents, Poly (SPE-co-PETA) organic polymer matrix monolithic column with mixed mode was prepared by in situ polymerization. The effects of monomer, crosslinking agent and pore-forming agent on the surface morphology, permeability and chromatographic properties of the monolithic column were investigated. The selectivity of poly (SPE-co-PETA) monolithic column to benzenes, amides, anilines and phenols was discussed in detail. The results showed that the monolithic column had hydrophobic, hydrophilic and ion exchange properties. The separation of phenols, nucleotides, bases and polypeptides can be successfully achieved by using the organic polymerized monolithic column. In Chapter 3, using glutathione (GSH) as organic functional monomer and tetramethoxysilane (TMOS) and 3- (methacryloxy) propyltrimethoxysilane (纬 -MAPS) as precursors, mercapto-vinyl click-chemistry was combined with "one pot" method. A novel organic-inorganic hybrid monolithic column was prepared. The effects of TMOS/ 纬 -MAPS ratio and the amount of pore-forming agent on the permeability, pore size, surface area and chromatographic performance of monolithic column were systematically investigated. Under the optimal synthesis conditions, the monolithic column exhibits dense, uniform mesh structure, good permeability and high specific surface area. The hydrophobic, hydrophilic and ion-exchange chromatographic properties of the hybrid monolithic column were evaluated with alkyl benzene series, amides and anilines, respectively. The column efficiency of the separation of benzene series at the linear velocity of 0.47mm/s was as high as 800 000 plates / m. The hybrid monolithic column can be successfully applied to the separation of nucleotides, polypeptides and protease hydrolysates.
【学位授予单位】：福州大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R917;O657.7
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