磺丁基-β-环糊精氧化锆复合材料电色谱整体柱的制备及应用  

Preparation and application of electrochromatography monolithic column base on sulfobutyl ether-β-cyclodextrin zirconia composites

作　　者：李英杰[1] 王宁[1] 高立娣[1] 吕仁江[1] 刘树仁[1] 尹丽娟[1] 崔丽燕[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161006

出　　处：《分析试验室》2016年第12期1428-1431,共4页Chinese Journal of Analysis Laboratory

基　　金：黑龙江省自然科学基金项目(B2016009)资助

摘　　要：以四甲氧基硅烷(TMOS)为交联剂,氧氯化锆为原料,通过溶胶-凝胶技术制备磺丁基-β-环糊精氧化锆复合材料毛细管电色谱整体柱,并优化其实验条件。通过红外光谱(IR)、X射线衍射(XRD)及扫描电子显微镜(SEM)对整体柱固定相进行表征。整体柱内固定相分布均匀且与毛细管柱壁结合紧密,整体柱具有良好的通透性及稳定性。以硫脲为中性标记物,测定理论塔板数为7.9×104plates/m。以DL-组氨酸为考察物考察毛细管柱分离性能,其分离度为1.68。利用该整体柱对盐酸芬氟拉明对映体进行手性拆分,达到基线分离且分离度为1.51。Sulfobutyl ether- β -cyclodextrin zirconia composites capillary electrochromatography monolithic column was prepared through sol -gel technique, with TMOS as crosslinking agent and zirconium oxychloride as raw material, and the experimental conditions were optimized . The monolithic column stationary phase was characterized through infrared spectroscopy （IR）, X ray diffraction （XRD）, and scanning electron microscope （SEM）. Theinternal stationary phases of monolithic column are uniformly distributed and closely combine with capillary column wall. Moreover, the monolithic column has good permeability and stability. Meanwhile, the theoretical plate number was determined to be 7. 9 × 10^4 plates/m, with thiourea as neutral marker. The resolution of capillary column was examined to be 1.68 by taking DL - histidine as target. Chiral separation of fenfluramine hydrochloride enantiomers was conducted under the use of the monolithic column, and it achieved baseline separation and the resolution was 1.51.

关 键 词：磺丁基-β-环糊精 氧化锆 毛细管电色谱整体柱 盐酸芬氟拉明 

分 类 号：O657.7[理学—分析化学]