β-环糊精基氧化钨毛细管电色谱整体柱的制备及应用  

Preparation and Application of Electrochromatographic Column Based on β-Cyclodextrin Derivatives and Tungsten Oxide

作　　者：李英杰[1] 张馨予[1] 高立娣[1] 吕仁江[1] 董艳丽[1] 陈男[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,黑龙江齐齐哈尔161006

出　　处：《化学试剂》2016年第4期297-300,共4页Chemical Reagents

基　　金：黑龙江省自然科学基金资助项目(B201218)

摘　　要：采用一步键合法合成了β-环糊精基氧化钨毛细管电色谱整体柱,考察了制备整体柱的主要影响因素,获得最佳制柱条件为:功能单体双(6-O-丁烯二酸单酯)-β-环糊精(CPD-β-CD)与EDMA物质的量比为0.12∶0.08,修饰纳米氧化钨的质量0.30 g,水浴温度40℃,聚合时间13 h。同时对整体柱进行了表征和评价,制备的整体柱有较均匀孔径的网状结构,固定相中修饰纳米氧化钨的含量达到16.6%,整体柱有良好的重现性和稳定性,同时具备较好的手性拆分能力。在最佳电色谱条件下,应用整体柱对美托洛尔、阿替洛尔和索他洛尔对映体进行拆分,均达到基线分离。In this work,the electrochromatography monolithic column of β-cyclodextrin derivatives and tungsten oxide was prepared by one-step reaction,at the same time,the main influencing factors of prepared column were investigated. The optimum conditions of prepared column were listed as follows： the molar ratio of CPD-β-CD and EDMA is 0. 12∶ 0. 08,the modified nanometer tungsten oxide of 0. 30 g,and the reaction time of 13 h at 40 ℃ water bath. Characterization and evaluation of the monolithic column were also carried out. The results show that the obtained monolithic column has a mesh structure with uniform pore size,and the content of tungsten oxide in stationary phase was about 16. 6%. The monolithic column has good reproducibility and stability,and the better ability of chiral separation. Under the optimum electrochromatographic conditions,the baseline separation of chiral drugs including metoprolol,atenolol and sotalol were obtained by the prepared monolithic column.

关 键 词：Β-环糊精衍生物 纳米氧化钨 电色谱整体柱 洛尔类药物 手性拆分 

分 类 号：O657.8[理学—分析化学]