層層自組裝高效液相色譜固定相制備及評價
發(fā)布時間:2018-04-23 13:37
本文選題:層層自組裝技術(shù) + 聚電解質(zhì)多層膜; 參考:《河南工業(yè)大學(xué)》2017年碩士論文
【摘要】:功能膜材料的物理和化學(xué)特性是非常獨特的,廣泛應(yīng)用與諸多領(lǐng)域,同時由于種種制備材料,導(dǎo)致多種制備方法。層層自組裝(LBL)技術(shù)可以達(dá)到膜的組成、結(jié)構(gòu)、層數(shù)的控制,而且具有成膜物質(zhì)種類豐富、基材選擇多,這是與其它制備方法比較下具有的優(yōu)勢,被廣泛應(yīng)用于光電器件、生物醫(yī)用材料、藥物緩釋等諸多領(lǐng)域。本研究以聚(乙烯-alt-馬來酸酐)和L-苯丙氨醇為原料通過酰胺化反應(yīng)生成PEMAPHE聚陰離子電解質(zhì),分別與聚烯丙基胺鹽酸鹽(PAH)和殼聚糖(CHI)作一體系,另有殼聚糖和聚苯乙烯磺酸鈉(PSS)體系,過層層自組裝技術(shù),將帶有異種電荷的聚電解質(zhì)通在活化色譜硅膠表面交替沉積構(gòu)筑多層膜,制備高效液相色譜固定相,裝填色譜柱。在反相色譜條件下,以多種化學(xué)物質(zhì)(烷基苯、多環(huán)芳烴、酚類、胺類、對羥基苯甲酸及其酯類)作分析物,進(jìn)行分離分析,評價其色譜性能。以多種分析物在色譜柱上的保留行為,探討固定相的色譜性質(zhì)。固定相在不同的流動相配比下,表現(xiàn)出不同的色譜性質(zhì)。在高水相下,非極性化合物烷基苯和多環(huán)芳烴的保留隨著有機(jī)相含量的升高而減弱,表現(xiàn)出反相液相色譜的性質(zhì),在一定比例后,保留緩慢增強(qiáng);極性化合物胺類、酚類、對羥基苯甲酸及其酯類在有機(jī)相含量達(dá)到一定比例后,保留同樣增強(qiáng),表現(xiàn)出親水色譜的性質(zhì),其容量因子隨流動相變化的曲線成U型。對比不同的分析物,對色譜保留機(jī)制進(jìn)行分析。結(jié)果表明,固定相上形成疏水性與親水性相統(tǒng)一的過渡性質(zhì)的固定相識別體系。對比不同的色譜柱,發(fā)現(xiàn)它們表現(xiàn)出的親水性是針對某類物質(zhì)。不同體系的多層膜固定相對不同類極性物質(zhì)表現(xiàn)出的親水性不一。結(jié)果表明,固定相上組裝的聚電解質(zhì)及所攜帶官能團(tuán)的改變對分析物的識別能力產(chǎn)生明顯影響。
[Abstract]:The physical and chemical properties of functional membrane materials are very unique, widely used in many fields, at the same time, due to various preparation materials, lead to a variety of preparation methods. The layer by layer self-assembly (LBL) technique can control the composition, structure and number of layers of films, and it has the advantages of rich kinds of film-forming materials and more choice of substrate, which is the advantage compared with other preparation methods, and has been widely used in optoelectronic devices. Biomedical materials, drug release and many other fields. PEMAPHE polyanionic electrolytes were synthesized by amidation of poly (ethylene altmaleic anhydride) and L-phenylalanine, respectively, in the system of polyallylamine hydrochloride (PAH) and chitosan (CHI). On the other hand, chitosan and sodium polystyrene sulfonate (PSS) system were prepared by layer by layer self-assembly technique. The polyelectrolyte with dissimilar charge was alternately deposited on the silica gel surface of activation chromatography to form multilayer films. The stationary phase was prepared by high performance liquid chromatography (HPLC) and the chromatographic column was filled. The chromatographic properties of various chemical substances (alkylbenzene, polycyclic aromatic hydrocarbons, phenols, amines, p-hydroxybenzoic acid and their esters) were analyzed by reversed phase chromatography. The chromatographic properties of stationary phase were studied by the retention behavior of several analytes on chromatographic columns. The stationary phase shows different chromatographic properties under different mobile phase ratios. In high aqueous phase, the retention of nonpolar alkylbenzene and polycyclic aromatic hydrocarbons decreases with the increase of organic phase content, showing the properties of reversed phase liquid chromatography, and the retention increases slowly after a certain proportion. When the content of p-hydroxybenzoic acid and its esters reaches a certain proportion, the retention of p-hydroxybenzoic acid and its esters increases as well, showing the characteristics of hydrophilic chromatography. The curve of the volume factor of p-hydroxybenzoic acid and its esters varies with the mobile phase is U-shaped. The retention mechanism of chromatography was analyzed by comparing different analytes. The results show that a transition phase recognition system with hydrophobicity and hydrophilicity is formed on the stationary phase. By comparing different chromatographic columns, it is found that their hydrophilicity is specific to certain substances. The hydrophilicity of different polar substances is different from that of multilayer membrane fixation in different systems. The results show that the changes of polyelectrolytes and functional groups on the stationary phase have a significant effect on the recognition ability of the analytes.
【學(xué)位授予單位】:河南工業(yè)大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:O652.63;TB383.2
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