本文選題：高效液相色譜 + 色譜柱填料的制備��； 參考：《青島大學(xué)》2016年碩士論文

【摘要】：高效液相色譜(High performance liquid chromatography,HPLC)作為一種重要的分離分析方法,已被廣泛應(yīng)用于石油化工、食品、化學(xué)、醫(yī)藥和生命科學(xué)等眾多領(lǐng)域。色譜柱固定相作為色譜分離的核心,其性能直接關(guān)系到分離的效率以及檢測(cè)結(jié)果的準(zhǔn)確性,因此研究與開發(fā)高性能的新型色譜柱填料一直是色譜領(lǐng)域中的熱門課題。色譜柱固定相一般按基質(zhì)的不同可分為無機(jī)基質(zhì),有機(jī)基質(zhì)和有機(jī)-無機(jī)復(fù)合基質(zhì)三大類。無機(jī)基質(zhì)固定相中二氧化硅(SiO2)微球因其具有機(jī)械強(qiáng)度高,生物相容性好,表面基團(tuán)豐富等特點(diǎn)而成為目前應(yīng)用最廣泛的高效液相色譜基質(zhì)填料;而有機(jī)基質(zhì)固定相中又以苯乙烯-二乙烯基苯共聚物(PS-DVB)應(yīng)用最為廣泛。本論文結(jié)合無機(jī)與有機(jī)基質(zhì)固定相各自的優(yōu)點(diǎn),分別對(duì)二氧化硅微球的功能化改性新方法以及多孔交聯(lián)聚苯乙烯微球的制備方法進(jìn)行了研究,并對(duì)制備的新型填料進(jìn)行了分離檢測(cè),取得了較好的效果,主要工作如下:1.采用改進(jìn)的溶膠-凝膠法(St?ber法),制得了平均粒徑約為2.5μm的單分散二氧化硅微球。以自制硅球?yàn)榛|(zhì),利用光交聯(lián)的反應(yīng)原理,用水溶性的感光高分子重氮樹脂(DR)取代毒性較大的硅烷化試劑實(shí)現(xiàn)了對(duì)硅球的功能化改性。在紫外光的照射作用下,誘導(dǎo)重氮樹脂的原位光交聯(lián)反應(yīng),從而在二氧化硅微球表面引入共價(jià)鍵和的功能性基團(tuán)。基于重氮樹脂的化學(xué)結(jié)構(gòu)以及流動(dòng)相的改變,利用改性后的微球作為色譜柱固定相可實(shí)現(xiàn)兩種不同的分離模式,并取得了較好的效果。2.采用改進(jìn)的種子聚合法制備出了具有二元孔結(jié)構(gòu)的單分散交聯(lián)聚苯乙烯微球,將該微球作為色譜柱填料,不僅分別成功分離了苯類化合物以及富勒烯碳60和碳70,而且由于其優(yōu)良的通透性,在較高的分離流速下柱壓可以維持在較低的水平。本論文所研究的二氧化硅的功能化新技術(shù)綜合了物理吸附和化學(xué)鍵合方法的諸多優(yōu)點(diǎn),通過光照交聯(lián)即可實(shí)現(xiàn)對(duì)二氧化硅微球簡(jiǎn)單快捷的功能化改性,是一種高效,穩(wěn)定,綠色環(huán)保的改性方法;制備出的二元多孔聚苯乙烯微球則有效降低了柱壓,提高了分離效率。這些新型色譜柱填料的制備技術(shù)對(duì)進(jìn)一步優(yōu)化高效液相色譜柱填料的制備有一定的指導(dǎo)意義。
[Abstract]:High performance liquid chromatography (HPLC), as an important separation and analysis method, has been widely used in many fields, such as petrochemical, food, chemistry, medicine and life science. The chromatographic column fixed phase is the core of the chromatographic separation, its performance is directly related to the efficiency of separation and the accuracy of the detection results. Therefore, the research and development of high performance new chromatographic column filler has always been a hot topic in the field of chromatography. The stationary phase of chromatographic column can be divided into inorganic matrix, organic matrix and organic inorganic composite matrix according to the difference of matrix. The silica (SiO2) microspheres in the fixed phase of inorganic matrix have high mechanical strength and biological strength. Good compatibility and rich surface groups have become the most widely used matrix filler in high performance liquid chromatography, and the most widely used in organic matrix stationary phase is styrene two vinyl benzene copolymer (PS-DVB). This paper combines the advantages of both inorganic and organic matrix fixed phase, and the function of silica microspheres respectively. The new method of modification and the preparation of porous crosslinked polystyrene microspheres have been studied, and the new packing has been separated and detected. The main work is as follows: 1. the mono dispersed silica microspheres with an average particle size of about 2.5 u m were prepared by the improved sol-gel method (St? BER). Based on the reaction principle of light crosslinking, a water-soluble photoreceptor diazonium resin (DR) has been replaced by a highly toxic silane reagent for the functional modification of silicon spheres. In situ light crosslinking reaction of diazo resin is induced under UV irradiation, thus introducing covalent bonds and functions on the surface of silica microspheres. Based on the chemical structure of the diazo resin and the change of the liquid phase, two different separation modes can be achieved by using the modified microspheres as the stationary phase of the chromatographic column, and a better effect.2. is achieved by the improved seed polymerization method to prepare the monodisperse crosslinked polystyrene microspheres with a two element pore structure. The microspheres are used as the microspheres. The chromatographic column packing has not only successfully separated the benzene compounds, fullerene carbon 60 and carbon 70, but also the column pressure can be maintained at a lower level at a high separation flow rate. The new functional technology of silica has integrated the advantages of physical adsorption and chemical bonding methods. The simple and quick functional modification of silica microspheres can be achieved through cross-linking of light. It is a highly efficient, stable, green and environmental modification method. The prepared two element porous polystyrene microspheres can effectively reduce the column pressure and improve the separation efficiency. The preparation technology of these new chromatographic columns is used to optimize the high efficiency liquid phase color. The preparation of the column packing has some guiding significance.
【學(xué)位授予單位】：青島大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.72

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