大环抗生素手性固定相拆分盐酸马布特罗对映体

基于三种大环抗生素类手性固定相Chirobiotic V,T和R,利用高效液相色谱法对盐酸马布特罗对映体进行了拆分;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,对分离机制进行了探讨.结果表明,盐酸马布特罗对映体在Chirobiotic R手性固定相上不能实现分离,在Chirobiotic V和T手性固定相上均可实现较好的基线分离.最佳色谱条件为:新极性有机相模式,流动相甲醇-冰醋酸-三乙胺(100∶0.01∶0.01,V/V/V),流速1.0mL/min,柱温20℃;相应的分离度分别可达3.08和3.73.与此同时,盐酸马布特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.

Enantioseparation of mabuterol hydrochloride with macrocyclic antibiotic stationary phases

The enantiomeric separation of mabuterol hydrochloride by high performance liquid chromatography with three macrocyclic antibiotic chiral stationary phases （CSPs）, Chirobiotic V, T and R, was conducted. The factors affecting the enantioresolution, such as the elution mode, composition of mobile phase, and column temperature were investigated. The separation efficiency was compared, and the separation mechanisms were discussed. Results indicate that it was infeasible to acquire enantiomeric separation of mabuterol hydrochloride with Chirobiotic R CSP, while desired baseline enantiomeric separation of mabuterol hydrochloride is achieved with Chirobiotic V and T CSPs. The optimal chromatographic condition was suggested as polar organic phase mode, mobile phase methanol-acetic acid-triethylamine （100 ： 0.01 ： 0.01,V/V/ V）, flow rate of 1.0 mL/min and column temperature of 20 ℃. Corresponding resolution fac tors with Chirobiotic V and T CSPs under the optimal condition were 3.08 and 3.73, respectively. In the meantime, the ionic interaction between Chirobiotic V and T chiral stationary phases and mabuterol was confirmed to be the dramatic interaction responsible for the chiral separation.