层层自组装高效液相色谱固定相制备及评价

发布时间：2018-04-23 13:37

本文选题：层层自组装技术 + 聚电解质多层膜　；参考：《河南工业大学》2017年硕士论文

【摘要】：功能膜材料的物理和化学特性是非常独特的,广泛应用与诸多领域,同时由于种种制备材料,导致多种制备方法。层层自组装(LBL)技术可以达到膜的组成、结构、层数的控制,而且具有成膜物质种类丰富、基材选择多,这是与其它制备方法比较下具有的优势,被广泛应用于光电器件、生物医用材料、药物缓释等诸多领域。本研究以聚(乙烯-alt-马来酸酐)和L-苯丙氨醇为原料通过酰胺化反应生成PEMAPHE聚阴离子电解质,分别与聚烯丙基胺盐酸盐(PAH)和壳聚糖(CHI)作一体系,另有壳聚糖和聚苯乙烯磺酸钠(PSS)体系,过层层自组装技术,将带有异种电荷的聚电解质通在活化色谱硅胶表面交替沉积构筑多层膜,制备高效液相色谱固定相,装填色谱柱。在反相色谱条件下,以多种化学物质(烷基苯、多环芳烃、酚类、胺类、对羟基苯甲酸及其酯类)作分析物,进行分离分析,评价其色谱性能。以多种分析物在色谱柱上的保留行为,探讨固定相的色谱性质。固定相在不同的流动相配比下,表现出不同的色谱性质。在高水相下,非极性化合物烷基苯和多环芳烃的保留随着有机相含量的升高而减弱,表现出反相液相色谱的性质,在一定比例后,保留缓慢增强;极性化合物胺类、酚类、对羟基苯甲酸及其酯类在有机相含量达到一定比例后,保留同样增强,表现出亲水色谱的性质,其容量因子随流动相变化的曲线成U型。对比不同的分析物,对色谱保留机制进行分析。结果表明,固定相上形成疏水性与亲水性相统一的过渡性质的固定相识别体系。对比不同的色谱柱,发现它们表现出的亲水性是针对某类物质。不同体系的多层膜固定相对不同类极性物质表现出的亲水性不一。结果表明,固定相上组装的聚电解质及所携带官能团的改变对分析物的识别能力产生明显影响。
[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.
【学位授予单位】：河南工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652.63;TB383.2

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