硅胶整体柱的制备及其色谱功能的研究.pdfVIP

摘要 摘 要 整体柱是二十世纪九十年代迅速发展起来的一个新的技术领域 从它产生便 倍受关注 硅胶整体柱是近几年才出现的新型色谱柱 由于硅胶整体柱具有高速 低压 高效 适于极性和流速梯度洗脱 机械强度高 柱性能稳定 等诸多优势 这使其很适合高通量分析和快速分离 在分离领域中发挥着越来越重要的作用 本文结合本研究室的工作 对常规硅胶整体柱的制备方法 制备机理与结构 特性以及应用作一概述 本文采用改进的溶胶-凝胶技术 以四甲氧基硅烷和聚乙二醇为原料 通过研 究水域温度 反应溶液pH值对凝胶化过程的影响 探讨了不同的四甲氧基硅烷/ 聚乙二醇比例 不同制孔剂浓度对柱结构的影响 以及不同焙烧温度和酸活化处 理方法对柱体Si-OH含量和线性收缩率的影响 并建立了消除柱体开裂和变形弯 曲的方法及中孔的构建方法 由此确定最佳制备条件 由此得到的硅胶整体柱床 经包覆后 考察了流速对柱压降的影响 并在正相色谱模式下应用制备的硅胶整 体柱对苯取代化合物进行了分离 效果令人满意 此外 制备了 -CD 键合硅胶 整体柱 成功分离了硝酚异构体 关键词 硅胶整体柱 高效液相色谱 溶胶凝胶技术 正相色谱 Abstract Abstract Monolithic column is a new separation material which has attracted much attention of scientists since 1990s. Monolithic silica column is the new type column of chromatography which possessed high permeability low column back pressure, high mechanical strength and column efficiency. It is well suited for high speed and high efficiency separations and it will play more and more important role in analysis and separation. This paper consists of the following parts: monolithic silica column’s preparation, principle, characterization and application. First, a new approach of preparing monolithic silica column was developed by adopting an improved sol-gel technology with tetramethoxysiane and polyethylene glycol as the matrix materials in this paper. The effects of the misture pH value and temperature of water-bath in the process of gelation were investigated. The influences of different TMOS/PEG ratio and concentration of porogenic diluent on monolithic silica column, the change of Si-OH content of monolithic column with roasting temperature and the mesopore size on the skeleton with reaction conditions were also discussed. The problems of crack and deformation in preparing the column were solved by using N,N-dimethylformamide and a new heat treatment procedure. Second,