本文選題：整體柱 + 點擊化學��； 參考：《西北大學》2017年碩士論文

【摘要】：整體柱是一種具有廣闊應用前景的新型色譜固定相,也是目前液相色譜領域研究的一個熱點�；趲�基的綠色點擊化學反應,具有反應條件溫和、產率高等特點,目前已經被廣泛應用于聚合物的制備以及材料表面修飾等方面。然而,目前鮮有文獻報道點擊化學反應直接制備整體柱的研究。本論文針對目前有機整體柱和雜化整體柱中存在的一些問題,本文發(fā)展了三種基于點擊反應制備整體柱的新技術:1.針對整體柱制備周期長的問題,采用巰基-丙烯酸酯(thiol-acrylate)點擊聚合反應快速制備有機整體柱。十八硫醇的引入有效地抑制傳統(tǒng)自由基聚合過程中的氧阻聚現(xiàn)象。此反應過程中既包含丙烯酸酯間的自聚反應,又存在丙烯酸酯與巰基間的共聚反應。所制備的有機整體柱對苯系物實現(xiàn)高效分離,最高柱效達75,000 N/m。對四種標準混合蛋白酶解液的分離效果與C-18填充柱結果相當。并且結合液質聯(lián)用(cLC-MS)技術首次將毛細管整體柱應用于長柄扁桃蛋白質的分離鑒定。2.針對整體柱表面性質較難調控的問題,采用“兩步”巰基-烯(thiol-ene)點擊聚合反應制備了一種多孔親水性雜化整體柱。通過與1-硫代甘油反應,疏水性單體八乙烯基倍半硅烷在致孔劑中的溶解性得到了顯著提高,然后將其作為前驅體成功制備了雜化整體柱。所制備的雜化整體柱具有連續(xù)均勻的網狀結構,在cLC應用中顯示出典型的HILIC保留機理,最高柱效達65,000 N/m。此外,本研究將肼功能化后的雜化整體材料成功應用于糖肽的富集。3.針對有機聚合物整體柱分離柱效低的問題,首次使用巰基-馬來酰亞胺(thiol-maleimide)點擊聚合反應直接合成兩種高交聯(lián)的有機聚合物整體柱。所制備的有機整體柱具有良好的熱穩(wěn)定性和機械強度。在5分鐘內實現(xiàn)對苯系物的高效分離,最高柱效可達180,500 N/m。此外,對苯酚類、堿性化合物、EPA 610、HeLa酶解液等樣品均展現(xiàn)出令人滿意的分離效果,為提高有機整體柱對小分子化合物分離柱效提供了一種新思路。
[Abstract]:Monolithic column is a new chromatographic stationary phase with broad application prospect, and it is also a hot spot in the field of liquid chromatography. The green click chemical reaction based on sulfhydryl group has been widely used in the preparation of polymers and the surface modification of materials because of its mild reaction conditions and high yield. However, there are few reports on the direct preparation of monolithic columns by clicking on chemical reactions. Aiming at some problems existing in organic monolithic column and hybrid monolithic column, this paper develops three new techniques for preparing monolithic column based on click-reaction: 1. In order to solve the problem of long preparation period of monolithic column, the organic monolithic column was rapidly prepared by mercapto-acrylic acid thiol-acrylate click-polymerization reaction. The introduction of octadecyl mercaptan can effectively inhibit the phenomenon of oxygen inhibition in the process of traditional free radical polymerization. The reaction includes both the self-polymerization of acrylate and the copolymerization of acrylic ester and sulfhydryl group. The organic monolithic column was used to separate benzene series with the highest column efficiency of 75000 N / m. The separation effect of four standard mixed proteolytic solutions was similar to that of C-18 packed column. The capillary monolithic column was applied to the separation and identification of almond protein for the first time. A porous hydrophilic hybrid monolithic column was prepared by "two-step" mercapto thiol-ene click-polymerization to solve the problem that it is difficult to control the surface properties of monolithic column. The solubility of hydrophobic monomer octavinyldisilane in pore-forming agent was significantly improved by reaction with 1-thioglycerol, and then the hybrid monolithic column was successfully prepared as a precursor. The hybrid monolithic column has a continuous and uniform reticular structure, which shows typical HILIC retention mechanism in the application of cLC. The maximum column efficiency is 65000 N / m. In addition, the hybrid monolithic material of hydrazine functionalized was successfully applied to the enrichment of glycopeptide. 3. In order to solve the problem of low column separation efficiency, two highly crosslinked organic polymer monolithic columns were synthesized by using mercapto-maleimide one-click polymerization for the first time. The prepared organic monolithic column has good thermal stability and mechanical strength. The highest column efficiency of 180500 N / m was achieved in 5 minutes. In addition, samples such as phenol, alkaline compound EPA 610N HeLa hydrolysate showed satisfactory separation effect, which provided a new way to improve the column efficiency of organic monolithic column for the separation of small molecular compounds.
【學位授予單位】：西北大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O652.6

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