羧甲基-β-环糊精/SiO_2/TiO_2毛细管开管柱的制备及其应用于毛细管电色谱

Preparation of Carboxymethyl-β-Cyclodextrin/SiO_2/TiO_2 Hybrid Open Capillary Column and Its Application to Capillary Electrochromatography

以钛酸丁酯和正硅酸乙酯为无机体,以羧甲基-β-环糊精(CM-β-CD)为有机体,在有机相与无机相的质量比为4比3时,通过溶胶-凝胶法制备了CM-β-CD/SiO2/TiO2溶胶作为固定相,从而制成新型的环糊精基有机-无机杂化毛细管色谱开管柱。用扫描电镜及红外光谱法对此开管柱进行表征,证明了固定相与毛细管内壁均匀键合并紧密结合;羧基与Ti-O发生键合并形成了保留环糊精的新型配合物。应用此开管柱对氨基酸对映体、氨基酸混合物和手性药物进行分离,均达到基线分离。试验选用含30%(体积分数)乙腈的磷酸二氢钠缓冲溶液(pH 8.0)为流动相,分离电压15kV,检测波长200nm。此开管柱的最高柱效为每米塔板数(N)116 478;连续10次进样,其迁移时间的相对标准偏差为3.1%。

Using tetrabutyloxytitanate and tetraethyloxysilicane as inorganic matters,carboxymethyl-β-cyclodextrin(CM-β-CD)as organic matter,and keeping morg∶minorgas 4∶3,the sol of CM-β-CD/SiO2/TiO2was prepared by the sol-gel method;and a novel cyclodextrin-based organic-inorganic hybrid open capillary column with the sol material as stationary phase was prepared.The column prepared was characterized by SEM and IRS, showing that the stationary phase was bonded evenly with and bound tightly on the inner surface of the capillary column;that bonding between COO-and Ti-O was formed;and that a new coorrdination complex retaining the cyclodextrin molecule was formed.The open capillary column was applied to chiral separation of enantiomers of amino acid,mixture of amino acids and 2chiral drugs,satisfactory separation from base lines was attained.Buffer solution of NaH2PO4(pH 8.0)mixed with acetonitrile with volumic ratio of 7to 3was used as mobile phase, separation voltage of 15kV and detection wavelength of 200nm were adopted in the experiments.Maximum column efficiency and precision of migration time were tested,giving values of Nand RSD(n=10)of 116 478plates/m and 3.1%respectively.