Preparation of Carboxymethyl-β-Cyclodextrin/SiO2/TiO2 Hybrid Open Capillary Column and Its Application to Capillary Electrochromatography
摘 要
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15 kV,检测波长200 nm。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%。
Abstract
Using tetrabutyloxytitanate and tetraethyloxysilicane as inorganic matters, carboxymethyl-β-cyclodextrin (CM-β-CD) as organic matter, and keeping morg∶minorg as 4∶3, the sol of CM-β-CD/SiO2/TiO2 was 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 2 chiral drugs, satisfactory separation from base lines was attained. Buffer solution of NaH2PO4 (pH 8.0) mixed with acetonitrile with volumic ratio of 7 to 3 was used as mobile phase, separation voltage of 15 kV and detection wavelength of 200 nm were adopted in the experiments. Maximum column efficiency and precision of migration time were tested, giving values of N and RSD (n=10) of 116 478 plates/m and 3.1% respectively.
中图分类号 O657.8
所属栏目 试验与研究
基金项目 黑龙江省自然科学基金(B201218)
收稿日期 2013/1/24
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联系人作者李英杰(lyj310@163.com)
备注李英杰(1961-),男,黑龙江齐齐哈尔人,教授,博士,研究方向为电色谱分析。
引用该论文: LI Ying-jie,WU Jing,Lv Ren-jiang,DING Li,WANG Li-na,ZHANG Fu-xiang. Preparation of Carboxymethyl-β-Cyclodextrin/SiO2/TiO2 Hybrid Open Capillary Column and Its Application to Capillary Electrochromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(2): 161~165
李英杰,吴婧,吕仁江,丁莉,王立娜,张福祥. 羧甲基-β-环糊精/SiO2/TiO2毛细管开管柱的制备及其应用于毛细管电色谱[J]. 理化检验-化学分册, 2014, 50(2): 161~165
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【3】胡佳薇,申烨华,秦伟捷,等.多层开管毛细管酶反应器的制备及在蛋白质酶切中的应用[J].高等学校化学学报,2012,33(2):268-275.
【4】曾玉香,王超,王炳强.手性固定相毛细管电色谱在手性药物分离中的应用研究进展[J].理化检验-化学分册, 2009,45(4):485-490.
【5】NIELSEN A L, MADSEN F, LARSEN K L. Cyclodextrin modified hydrogels of PVP/PEG for sustained drug release[J]. Drug Delivery, 2009,16(2):92-101.
【6】金征宇,徐学明,陈寒青,等.环糊精化学制备与应用[M].北京:化学工业出版社, 2009:1-30.
【7】CHANG Y S, KO T H, HSU T J, et al. Synthesis of an imprinted hybrid organic-inorganic polymeric sol-gel matrix toward the specific binding and isotherm kinetics investigation of creatinine[J]. Anal Chem, 2009,81:2098-2105.
【8】XU L, LEE H K. Preparation,characterization and analytical application of a hybrid organic-inorganic silica-based monolith[J]. J Chromatogr A, 2008,1195:78-84.
【9】李英杰,郝秀菊,张春雨,等.甲基丙烯酸丁酯/SiO2/TiO2有机-无机杂化毛细管整体主的制备及其应用[J].应用化学, 2010,27(12):1457-1461.
【10】王艳霞.羧甲基环糊精合成新方法及其手性药物分离应用[D].河北:河北大学硕士学位论文, 2010:8-10.
【11】王园朝.β-环糊精溶胶-凝胶法电色谱开管柱的制备及评价[J].咸宁师专学报, 2000,20(3):71-74.
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