环糊精修饰中孔分子筛SBA15作为手性色谱固定相及其应用

Application of β-Cyclodextrin Modified Mseoporous Spherical Particles of Mesoporous Silicate as the Substrate for Chiral High Performance Liquid Chromatography

采用聚环氧乙烯醚-聚环氧丙烯醚-聚环氧乙烯醚(P123)为模板,正硅酸乙酯为硅源,在酸性介质中采用静置法合成出球形Φ4.3μm介孔氧化硅SBA15,通过γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH560)在无水条件下将β-环糊精键合到SBA15表面和孔道内部。利用X射线衍射(XRD)、比表面积测定仪、红外光谱(FT-IR)、扫描电镜(SEM)和差显量热仪进行了表征。该材料湿法装填成色谱柱后成功分离了手性药物布洛芬和Dns-Phe对映体,其分离度分为别为2.03和1.04,说明其在色谱填料和手性分离上都具有广泛的应用前景。

Spherical particles of mesoporous silicate （SBA15） with average pore size of 3.5 nm and particle size of 4.3 μm have been synthesized. Puronics P123 （EO20POToEO20） and cetyhrimethylammonium bromide （CTMAB） were used as surfactant and co-surfactant. β-Cyclodextrin was grafted within the channel of meso- porous silica SBA15 by means of KH560. SBA15 was characterized by XRD, FT-IR, SEM, Micromeritics ASAP and thermogravimetry-differential scanning catorimetry （TC-DSC）. The functionalized SBA15 was packed in a steel column and applied in chiral HPLC to separate chiral chemicals. Results show that Dns-Phe and chiral drugs Ibuprofen were successfully separated on the column packed with SBA15 fuctionalized with β-cyclodextrin.