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出 处:《分析试验室》2014年第10期1194-1197,共4页Chinese Journal of Analysis Laboratory
基 金:山东省自然科学基金项目(ZR2012HL48)资助
摘 要:建立并优化了高效液相色谱手性固定相分离盐酸克伦特罗对映体的方法。使用两种Pirkle型手性固定相(α-Burke-2和Pirkle-1J)拆分了盐酸克伦特罗对映体,考察了缓冲盐添加剂,有机溶剂种类和浓度,以及柱温对保留行为和分离的影响。当流动相为二氯甲烷-乙醇(19:1,V/V)含5 mmol/L乙酸铵,流速2.0 mL/min,柱温20℃时,盐酸克伦特罗对映体在α-Burke-2色谱柱上能实现较好的分离,分离度可达1.85;在Pirkle-1J色谱柱上,分离度可达0.64。盐酸克伦特罗对映体与Pirkle型固定相之间的π-π主客体相互作用和氢键作用是实现对映体分离的最主要分离机制。方法可用于盐酸克伦特罗对映体的质量控制及立体选择性药代动力学的研究。The enantiomeric resolution of clenbuterol was achieved on two Pirkle-type (a-Burke -2 and Pirkle -1J ) by high performance liquid chromatography. chiral stationary phases Factors affecting the enantioresolution, such as the type and concentration of buffer solution, the type and content of organic modifier and temperature were investigated. The optimal separation conditions were as follows: dichloromethane-ethanol (19: 1, V/V) containing 5 mmol/L ammonium acetate as the mobile phase, at a flow rate of 2. 0 mL/min, column temperatureof 20 ℃. Under the above conditions, the enantiomers of clenbuterol were successfully separated on or-Burke -2 and Pirkle - 1J chiral stationary pahses with the resolution factors of 1.85 and 0. 64, respectively. The effeetive π - π donor-acceptor interaction and hydrogen bonding interaction between the two Pirkle-type ehiral stationary phases and clenbuterol were expected to be responsible for the chiral recognition. The method is simple and rapid for the quality control and stereoselective pharmacokinetics study of clenbuterol.
关 键 词:Pirkle型手性固定相 盐酸克伦特罗 对映体 手性拆分
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