十八烷基键合硅胶整体柱的制备及其色谱性能评价

Preparation of octadecyl-bonded monolithic silica column and evaluation of its chromatographic characteristics

选用十八烷基二甲基氯硅烷作为硅烷化试剂，制备十八烷基反相键合硅胶整体柱，并用元素分析进行了表征。以苯、甲苯、联苯、萘、菲混合物作为测试溶质，在以甲醇和水为二元流动相的反相色谱条件下评价了该键合整体柱的色谱性能，考察了该整体柱适用的pH范围，以及柱压降、柱效与流速的关系。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DH2～8之间稳定性好，柱压降、柱效受流速影响较小，对5种心血管系统用药可以达到快速、有效的分离。

An Octadecyl-bonded monolithic silica column for reversed-phase HPLC was synthesized by reacting with chlorodimethyloctadecylsilane onto monolithic silica column. Characterization of the prepared column was carried out with elemental analysis. The chromatographic properties of the packing were evaluated by using benzene, toluene, naphthalene, biphenyl and phenanthrene as samples and methanol-water as binary mobile phase. The column back- pressure and separation effect were also evaluated by fast separation. Several Cardiovascular drugs such as nifedipine, nitrendipine, nimodipine, nisoldipine and m-nisoldipine were also separated at different flow rates on the octadecyl- bonded monolithic silica column. The results show that the stationary phase has satisfactory chromatographic properties, and can resist hydrolysis between pH 2- 8, and it can be efficiently used for the fast-separation of solutes.