柠檬酸-β-环糊精/SiO_2-TiO_2开管柱的制备及评价  

Preparation and evaluation of a citric acid-β-cyclodextrin/SiO_2-TiO_2 open tubular column

作　　者：李英杰[1] 徐红梅[1] 吕仁江[1] 高立娣[1] 于春杰[1] 王珊珊[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161006

出　　处：《分析试验室》2015年第3期292-295,共4页Chinese Journal of Analysis Laboratory

基　　金：黑龙江省自然科学基金(41465500-7-12042)资助

摘　　要：制备一种新型的环糊精衍生物有机-无机杂化材料固定相开管柱,通过毛细管电色谱-质谱(CEC-MS)对其进行评价。以正硅酸乙酯和钛酸丁酯为无机前驱体,柠檬酸-β-环糊精(CA-β-CD)为有机体,通过溶胶-凝胶法制备CA-β-CD/SiO2-TiO2有机-无机杂化毛细管电色谱开管柱,并对其制备条件进行优化。采用扫描电子显微镜和红外光谱对开管柱的形貌和杂化材料的结构进行表征。利用制备的杂化开管柱在CEC-MS上对酪氨酸和色氨酸对映体混合物进行定性分析评价。A new type of open tubular column with cyclodextrin derivative organic-inorganic hybrid material stationary phase is prepared,and evaluated by capillary electrochromatography-mass spectrometry（ CEC-MS）.Silicate（ TEOS） and titanate（ TBOT） acted as inorganic precursors and citric acid-β-cyclodextrin（ CA-β-CD）as organic groups,a CA-β-CD / Si O2-Ti O2organic-inorganic hybrid capillary electrochromatography open tubular column was prepared by sol-gel method,moreover,the preparation conditions of the hybrid open tubular column were also optimized. The morphology of the open tubular column and the microstructure of hybrid materials were characterized by scanning electron microscopy（ SEM） and infrared spectroscopy（ IR）. By using capillary electrochromatography-mass spectrometry（ CEC-MS）,the enantiomeric mixture of tyrosine and tryptophanthe was qualitatively analysized to evaluate the prepared hybrid open column. The results show that the prepared novel hybrid open tubular column has good ability of chiral separation.

关 键 词：有机-无机杂化 开管柱 毛细管电色谱-质谱联用 柠檬酸-β-环糊精 

分 类 号：O657.8[理学—分析化学] O656.2[理学—化学]