新型β-环糊精衍生物/硅基杂化手性固定相制备及评价

Preparation and evaluation of novel β-cyclodextrin derivatives/silicon-based hybrid chiral stationary phases

以脲氨基-β-环糊精硅基衍生物为手性单体,1,2-二(三乙氧基硅烷)乙烷(BTEE)为硅源,十六烷基三甲基溴化铵(CTAB)为模板,采用水热合成法制备脲氨基β-环糊精衍生物/硅基手性杂化材料(β-CD/PMOs)。以其为手性固定相制备一种新型毛细管电色谱开管柱,通过IR和SEM对固定相的结构和形貌进行表征。结果表明,固定相成功键合在毛细管内,并保留了固定相原有的球形结构。以硫脲为标记物,测得平均柱效在11698.4 plates/m以上,日内、日间及柱间柱效的相对标准偏差(RSD)(n=7)均≤1.31%,且成功拆分D,L-组氨酸,达到基线分离。可见,该开管柱具有良好的重现性、稳定性和手性拆分能力。

The new urea amino-β-cyclodextrin silicon-base chrial hybrid materials(β-CD/PMOs)was synthesized by hydrothermal processes using urea amino-β-cyclodextrin silicon-based derivative as chiral monomer,1,2-bis(triethoxysilyl)-ethane(BTEE)as silicon resources and cetyltriethyl-ammnonium bromide(CTAB)as template.And then a novel capillary electrochromatography open-tubular column was prepared usingβ-CD/PMOs as chiral stationary phase and characterized by IR and SEM.The results showed that the stationary phase was successfully bonded on the inner surface of the capillary and retained the original spherical structure.The average column efficiency was above 11698.4 plates/m and the relative standard deviation(RSD)(n=7)of run-to-run,day-to-day and column-to-column was≤1.31%,respectively when thiourea was used as a marker.Meanwhile the baseline chrial separation for D-histidine and L-histidine was obtained using the prepared open-tubular column.The above results can be seen that the prepared open-tubular column has good reproducibility,stability and better chiral separation performance.