大环抗生素手性固定相拆分克伦普罗对映体及分离机制研究  

Enantioseparation of Clenproperol on Macrocyclic Antibiotic Stationary Phases

作　　者：张丹丹[1] 张晓琳[1] 

机构地区：[1]青岛科技大学化工学院,山东青岛266042

出　　处：《分析科学学报》2015年第3期393-396,共4页Journal of Analytical Science

基　　金：山东省自然科学基金(No.ZR2012HL48)

摘　　要：应用三种大环抗生素类手性固定相Chirobiotic V、Chirobiotic T和Chirobiotic R,采用高效液相色谱法对盐酸克伦普罗对映体进行了拆分研究。实验考察了洗脱模式、流动相组成、柱温等因素对分离的影响,对分离结果进行了比较,并对其分离机制进行了探讨。结果表明,盐酸克伦普罗对映体在Chirobiotic R手性固定相上不能实现分离,在Chirobiotic V和Chirobiotic T手性固定相上,最佳色谱条件为:新极性有机相模式,流动相为甲醇-乙酸-三乙胺(100∶0.01∶0.01,V/V/V),流速:1.0mL/min,柱温:20℃,分离度可分别达到2.00和2.13。实验证明,盐酸克伦普罗对映体与大环抗生素类固定相之间的离子相互作用是实现对映体分离的最主要分离机制。The enantiomeric resolution of clenproperol was studied on three macrocyclic antibiotic chiral stationary phases（CSPs）：Chirobiotic V,T and R by high performance liquid chromatography.Factors affecting the enantioresolution,such as the separation mode,composition of mobile phase and temperature were investigated.No enantioresolution was achieved for clenproperol on Chirobiotic R CSP.On Chirobiotic V and T CSPs,the polar organic mode was proved to be the best,with methanol-acetic acid-triethylamine（100∶0.01∶0.01,V/V/V）as the mobile phase at a flow rate of 1.0mL/min and 20℃.Under the above conditions,the enantiomers of clenproperol were baseline separated with the maximum resolution factor of 2.00 and 2.13 on Chirobiotic V and T CSPs,respectively.The chiral recognition mechanism was discussed and ionic interaction between Chirobiotic V and T chiral stationary phases and clenproperol was confirmed to be the dramatic interaction responsible for the chiral discrimination.

关 键 词：大环抗生素手性固定相 盐酸克伦普罗 对映体 手性分离 高效液相色谱法 

分 类 号：O657.72[理学—分析化学]