孔道中杂合-β-环糊精的有机-无机手性固定相的制备及手性分离性能

制备了β-环糊精-6-单取代氨乙基氨丙基三甲氧基硅烷手性单体(β-CD siloxane)，以该手性单体和1,2-双(三乙氧基硅基)乙烷(BTEE)为硅源，十六烷基三甲基溴化铵(CTAB)为模板，采用水热合成法直接制得孔道中含有环糊精的手性介孔材料。 再对该产物进行苯基异氰酸酯化得到杂合β-环糊精的有机-无机介孔分离材料(β-CD PMOs)。 在正相HPLC及反相HPLC条件下，分别考察该填料柱对常见含氮碱性药物对映体的拆分效果。 结果表明，不管在反相或正相分离模式下，采用常见的流动相在pH=4.15条件实现了11个碱性药物的手性分离，手性选择因子(α)最高可达2.42。 孔道中直接杂合β-环糊精的手性固定相制备方法简便、快速和成本低，进一步优化成孔条件后有一定应用前景。

Preparation and Enantioseparation Performance of Organo-inorganic Silica Composite Chiral Stationary Phase Modified by β-Cyclodextrin

β-CD-mono-6-(N-aminoethyl)-3-aminopropyltrimethoxy silane was synthesized and used together with 1,2-bis(triethoxysilyl)-ethane(BTEE) as silica resources templated by cetyltriethyl-ammnonium bromide(CTAB) for preparing mesoporous chiral materials via hydrothermal processes.After phenylcarbamated with phenyl isocyanate an organo-inorganic chiral silica composite(β-CD PMOs) was obtained,in which β-CD was incorporated to the wall of the channels while ethyl groups were located in the framework.The periodic mesporous organosilicas(PMOs) was utilized as chiral stationary phase(CSP) for enantioseparartion of some alkaline medicines containing nitrogen under reverse-phase high-performance liquid chromatography(RP-HPLC) and normal-phase high-performance liquid chromatography(NP-HPLC) conditions.The results showed that the enantioseparartion of these medicines could be effectively achieved by β-CD PMOs using common mobile phases at the similar pH value(pH=4.15).The maximal enantioseparartion selectivity factor(α) was 2.42.In addition,excellent permeability and reproducibility facilitate the establishment of a new enantioseparation method for chiral medicines.The chromatographic data indicated that β-CD PMOs are promising for the enantioseparation of medicines.