将硅烷偶联剂γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH560)先与十八醇反应,再键合到硅胶整体柱上,得到醚型十八烷基键合硅胶整体柱,并用红外光谱对其进行了表征。利用该固定相,在甲醇-水简单的二元流动相体系下,考察了该整体柱适用的pH范围,以及流速与柱压降和流速与柱效的关系,用该固定相对苯及其同系物进行了分离,并对尼群地平、硝苯地平和间尼索地平进行了分离。结果表明,该硅胶整体柱键合效果良好,具有较好的反相色谱性能,且在pH=2~8范围内稳定性好,柱压降、柱效受流速影响较小,可有效地用于化合物的快速分离分析。
An ether-bonded monolithic silica column for reversed-phase high performance liquid chromatography had been prepared by reacting octadecanol with γ-glycidoxypropyltrimethoxysilane firstly and then coupling it on to the monolithic silica column. Characterization of prepared ether-bonded monolithic silica column was performed with FTIR. Its chromatographic properties were evaluated by using benzene, toluene, naphthalene, phenanthrene and biphenyl as samples while methanol-water as the binary mobile phase. Column back-pressure, separation effect and the range of pH were also evaluated for fast separation. Moreover, separation of the nifedipine, nitrendipine and m-nisoldipine had achieved. The results showed that the stationary phase had fine chromatographic properties and existed good stability with the pH between 2 and 8. The column back-pressure and separation effect were weakly influenced by flow rate. Therefore, the resulted etherbonded monolithic silica column could be used for the fast-separation efficiently.