【摘要】：毛細管整體柱是一種用有機或無機聚合方法在色譜柱內(nèi)進行原位聚合的連續(xù)床固定相。與傳統(tǒng)的填充柱相比,毛細管整體柱具有制備簡單、無需燒結(jié)塞子、通透性好、低柱壓等優(yōu)點,已成為當(dāng)今色譜領(lǐng)域研究的熱點之一�；旌夏Ｊ缴V是指同時應(yīng)用多種作用力使溶質(zhì)和固定相進行保留和分離的色譜方法。相比于單一色譜模式,混合模式色譜具有高選擇性、高分離效率等優(yōu)勢,能夠滿足對復(fù)雜樣品的分離分析�；诖�,本文致力于發(fā)展兩種具有高效分離能力的混合模式的毛細管整體柱,系統(tǒng)地探討了這類整體柱的色譜保留行為及分離機理,并將其應(yīng)用于多肽和蛋白酶解物等的分離研究。本論文主要從以下三個方面進行闡述：第一章綜述微柱液相色譜的原理和分類,毛細管整體柱的制備、分類,混合模式色譜,并介紹了本論文的研究意義與研究內(nèi)容。第二章以3-[N,N-二甲基-[2-(2-甲基丙-2-烯酰氧基)乙基]銨]丙烷-1-磺酸內(nèi)鹽(SPE)為有機功能單體,季戊四醇三丙烯酸酯(PETA)為親水交聯(lián)劑,以環(huán)己醇和乙二醇為二元致孔劑,通過原位聚合制備了混合模式的poly(SPE-co-PETA)有機聚合物基質(zhì)整體柱。實驗考察了單體、交聯(lián)劑以及致孔劑的加入量以及它們的配比對整體柱表面形貌、滲透性、以及色譜性能的影響。詳細討論了poly(SPE-co-PETA)整體柱對苯系物、酰胺類、苯胺類和苯酚類化合物的選擇性,結(jié)果表明該整體柱具備疏水、親水和離子交換等色譜性能。利用該有機聚合整體柱可成功地實現(xiàn)苯酚類、核苷酸、堿基、多肽等的高效分離。第三章以谷胱甘肽(GSH)為有機功能單體,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)為前驅(qū)體,通過將巰基-烯點擊化學(xué)和“一鍋”法相結(jié)合,制備了一種新型的有機-無機雜化整體柱。系統(tǒng)地考察了TMOS/γ-MAPS配比、GSH以及致孔劑用量對整體柱骨架滲透性、孔徑和表面積以及色譜性能等影響。在最優(yōu)的合成條件下,該整體柱呈現(xiàn)致密、均一的網(wǎng)格結(jié)構(gòu),良好的滲透性以及高的比表面積。分別以烷基苯系物、酰胺類、苯胺類等為考察對象,評價該雜化整體柱的疏水、親水和離子交換等色譜性能。在0.47mm/s的線速度下分離苯系物時,柱效高達80,000～124,000 plates/m。該雜化整體柱可成功地應(yīng)用于核苷酸,多肽,蛋白酶解物的高效分離。
[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 (緯 -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/ 緯 -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.
【學(xué)位授予單位】：福州大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2014
【分類號】：R917;O657.7

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