新型脲氨基-β-环糊精衍生物键合毛细管电色谱开管柱的制备及评价

Preparation and evaluation of novel open-tubular column bonded urea-amino-β-cyclodextrin derivative for capillary electrochromatography

通过加成反应制备了新型脲氨基-β-环糊精衍生物(UB-β-CD)键合毛细管电色谱开管柱,并确定了最佳制柱条件:UB-β-CD用量0. 03 g,键合次数3次。采用红外光谱(FT-IR)和扫描电镜(SEM)对柱内固定相的结构和形貌进行表征。结果表明:类花状固定相与毛细管内壁紧密键合且分布均匀,固定相厚度约为1. 8μm。以硫脲为中性标记物,测得平均柱效在39138 plates/m以上,日内、日间及柱间柱效的相对标准偏差(RSDs)(n=5)分别为0. 31%,0. 61%和1. 4%。应用制备的开管柱对D,L-组氨酸和阿替洛尔对映体进行拆分,两者均达到基线分离。

A novel open-tubular column bonded urea-amino-β-cyclodextrin derivative(UB-β-CD)for capillary electrochromatography was prepared by addition reaction,and the optimal preparation conditions of the column were obtained:the dosage of UB-β-CD was 0.03 g and the bonding times was3.The structure and morphology of the stationary phase in the column were characterized by fourier infrared spectroscopy(FT-IR)and scanning electron microscopy(SEM).The results showed that the flower-like stationary phase was tightly and uniformly bonded to the inner wall of the capillary and its thickness was about 1.8μm.With thiourea as the neutral marker,the average column efficiency was above 39138 plates/m and the relative standard deviations(RSDs)(n=5)of intra-day,inter-day and column-to-column were 0.31%,0.61%and 1.4%,respectively.D,L-histidine and atenolol were separated by baseline using prepared open-tubular column.