多羟基化合物键合亲水色谱固定相的制备及其分离性能  

Preparation of multi-hydroxyl molecular-bonded stationary phase for hydrophilic interaction chromatography and its separation property

作　　者：张静[1] 王玲玲[1] 单联国[2] 卫引茂[2] 

机构地区：[1]陕西师范大学化学化工学院,陕西西安710062 [2]西北大学化学与材料科学学院,陕西西安710069

出　　处：《色谱》2012年第8期804-809,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(81173025;20975080)

摘　　要：用硅胶与氨丙基三甲氧基硅烷反应,再与δ-葡萄糖酸内酯反应,制备了一种多羟基化合物键合的新型亲水色谱固定相。以水-有机溶剂(乙醇、乙腈、四氢呋喃)为流动相,通过改变流动相中有机溶剂的种类及浓度、缓冲盐浓度和柱温,考察了该固定相对6种强极性中药组分的保留行为和保留机理。当水的比例在0～40%(v/v)范围时,溶质的保留随着流动相中水的比例的增大而减小,属于典型的亲水色谱分离模式;而当流动相中水的比例在0～100%(v/v)范围内变化时,溶质的保留随着水的比例变化呈"U"形曲线,属于亲水色谱和反相色谱的混合保留机理。缓冲盐的浓度和pH效应说明,所选用的中药组分与所制备的固定相间还存在弱的静电作用。该固定相对6种中药组分以及丹参注射液具有良好的分离性能,表明其在强极性中药有效成分的分离及其他强极性物质的分离分析中具有一定的应用前景。The surface of silica was modified by δ-gluconolactone,a multi-hydroxyl molecule,to prepare a new stationary phase for hydrophilic interaction chromatography（HILIC） of strongly polar compounds from traditional Chinese medicine.The separation properties and separation mechanisms of the stationary phase to six polar components were investigated by changing kinds of organic solvent（ethanol,acetonitrile and tetrahydrofuran） and concentration,salt concentration and column temperature.The retention times of the solutes decrease with increasing the concentration of water in mobile phase from 0 to 40%（v/v）,indicating a typical HILIC mode for the separation of the solutes,whilst the curves of the retention times of the six solutes exhibit ＂U＂ shape with the change in the concentration of the water from 0 to 100%（v/v）,indicating a mixed-mode of hydrophilic interaction and reversed-phase chromatography working on the separation of the solutes.The results of the salt concentration and pH affected the retention time show that there were weak electric interactions between the solutes and the prepared stationary phase.The fact that the strongly polar solutes and Danshen injections could be separated well indicated that the prepared stationary phase has a potential application in the separation of strongly polar components in traditional Chinese medicine and other strongly polar compounds.

关 键 词：亲水作用色谱 多羟基化合物固定相 强极性中药组分 色谱保留行为 

分 类 号：O658[理学—分析化学]