脲氨基-β-环糊精衍生物开管柱的制备及其手性拆分应用  

Preparation and enantioseparation application of urea amino-β-cyclodextrin derivative open-tubular column

作　　者：李雪[1] 李英杰[1] 秦世丽 高立娣[1] 唐艺旻 LI Xue;LI Ying-jie;QIN Shi-li;GAO Li-di;TANG Yi-min(College of Chemistry and Chemical Engineering,Qiqihar University,Qiqihar 161006,China)

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：《化学研究与应用》2022年第5期1099-1103,共5页Chemical Research and Application

基　　金：黑龙江省省属高等学校基本科研业务费资助项目(135409205)资助。

摘　　要：本文以新型脲氨基-β-环糊精衍生物(UB-β-CD)为单体制备键合毛细管电色谱开管柱并优化制备条件。通过红外光谱(FT-IR)和热重(TG)对UB-β-CD结构和热稳定性进行表征,扫描电子显微镜(SEM)对开管柱内壁形貌进行表征。结果表明固定相成功键合到毛细管内壁上,分布均匀,薄层厚度约为0.5μm。使用硫脲作为中性标记物测得开管柱平均柱效高于14400 plates·m^(-1),日内、日间及柱间柱效相对标准偏差(RSD)(n=5)分别为0.18%、0.56%和1.02%,且连续使用60天以上,仍有较好的柱效。应用制备的开管柱成功拆分了D,L-组氨酸和3种手性药物,均达到基线分离,说明制得的开管柱有良好的重现性,稳定性和较强的手性拆分能力。In this paper,the novel urea-amino-β-cyclodextrin derivative(UB-β-CD)was used as monomer to prepare the open-tubular column for capillary electrochromatography and the preparation conditions were optimized.The structure and thermal stability of UB-β-CD were characterized by infrared spectroscopy(FT-IR)and thermogravimetry(TG),and morphology of open-tubular column were characterized by scanning electron microscope(SEM).The results showed that the stationary phase was successfully bonded to the inner wall of the capillary with uniform distribution,and the thickness of the thin layer was about 0.5μm.With thiourea as the neutral marker,the average efficiency was above 14400 plates·m^(-1),and reproducibility values(RSD)(n=5)of run-to-run,day-to-day and column-to-column were 0.18%,0.56%and 1.02%,respectively.Meanwhile the prepared column was used continuously above 60 days and still had great efficiency.D,L-Histidine and three chiral drugs were separated and all achieved baseline separation using prepared open-tubular column.It could be seen that the open-tubular column had good reproducibility,stability and strong chiral separation ability.

关 键 词：脲氨基-β-环糊精衍生物 毛细管电色谱 开管柱 手性拆分 

分 类 号：O657.8[理学—分析化学]