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吸附固定相电色谱和动态改性电色谱的手性分离
引用本文:叶明亮,邹汉法,雷政登,吴仁安,倪坚毅.吸附固定相电色谱和动态改性电色谱的手性分离[J].分析化学,2001,29(3):299-302.
作者姓名:叶明亮  邹汉法  雷政登  吴仁安  倪坚毅
作者单位:中国科学院大连化学物理研究所,国家色谱研究与分析中心,
摘    要:对动态改性电色谱手性分离进行了研究。电色谱柱填充强阴离子交换固定相(SAX0,添加在流动相中的磺化β-环糊精(S-CD)动态地吸陵于SAX填料表面,形成一层准手性固定相。色氨酸、阿托品和异博定对映体在本体系获得了很好的分离,它们的分离分别为2.06,10.1和1.96,对映体峰的柱效价于85,000塔板数/米和412,000塔板数/米之间。连续运行17次,死时间和色氨酸对映体的电色谱保留因子的相对标准偏差分别为0.53%,0.62%和0.69%。此外,以吸附于SAX填料的牛血清白蛋白和S-CD为手性固定相进行了电色谱手性分离的研究。在这两种体系下分离色氨酸对映体的分离度分别为3.86和2.97。吸附S-CD柱电色谱和动态改性电谱的重现性进行子比较,发现动态改性电色谱有更好的重现性。

关 键 词:毛细管电色谱  动态改性  吸附固定相  手性分离  手性药物

Chiral Separation by Capillary Electrochromatography with PhysicallyAdsorbed Stationary Phase and Dynamically Modified Stationary Phase
Ye Minglian,ZOU Hanfa,Lei Zhengdeng,Wu Renan,Li Jianyi.Chiral Separation by Capillary Electrochromatography with PhysicallyAdsorbed Stationary Phase and Dynamically Modified Stationary Phase[J].Chinese Journal of Analytical Chemistry,2001,29(3):299-302.
Authors:Ye Minglian  ZOU Hanfa  Lei Zhengdeng  Wu Renan  Li Jianyi
Abstract:A novel mode of chiral separation in electrochromatography (CEC) with dynamically modified stationary phase (DMS-CEC) was presented. The capillary column was packed with strong anionic exchange stationary phase, the sulfated β-cyclodextrin (S-CD), which was added in the mobile phase, dynamically adsorbed to the packing surface and a new layer of chiral stationary phase was formed. The separation of enantiomer was based on their different interaction with the new stationary phase. The enantionmers of tryptophan, atropine and verapamil were successfully separated in this system with resolution of 2.06, 10.1 and 1.96, and the column effeciency for the enantiomers were varied from 85000 plates/m to 412000 plates/m. The relative standard deviation (RSD) of void time and the tryptophan enantiomers′ migration time for 17 consecutive runs were 0.5%, 0.6% and 0.7%, respectively. Enantiomer separation by capillary electrochromatography with adsorbed bovine serum albumin (BSA) and sulfated cyclodextrin (S-CD) as chiral stationary phases were also studied. The resolution for tryptophan enantiomers in the two systems were 3.86 and 2.97, respectively. It was found that the superiority of DMS-CEC over the adsorbed S-CD column CEC was that better repeatability could be obtained in DMS-CEC.
Keywords:Capillary electrochromatography  dynamical modification  adsorbed stationary phase  enantiomer separation
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