酰胺型手性固定相直接拆分克仑特罗对映体

Direct Resolution of Clenbuterol Enantiomers with Amide Derivative as Chiral Stationary Phase

将酰胺型手性固定相用于正相高效液相色谱直接拆分 β2 受体兴奋剂克仑特罗。讨论了三元流动相中正己烷、1,2 二氯乙烷和甲醇含量的变化以及柱温和流速对分离的影响 ;优化了实验条件 :流动相为V(正己烷 )∶V(二氯乙烷 )∶V(甲醇 ) =5 4∶38∶8,柱温为 17℃ ,流速为 1 0mL/min ;并对拆分的机理加以探讨。方法简单、快速。

A simple and rapid high performance liquid chromatographic method has been developed for the direct resolution of clenbuterol enantiomers. The method involved the use of an amide type chiral stationary phase(CSP) made of ( R )-1-naphthylglycine and 3,5-dinitrobenzoic acid known as the Chirex 3005 column. The effects of different contents of n -hexane, 1,2- dichloroethane and methanol in mobile phase on the chiral separation are discussed. The effects of column temperature and flow rate of mobile phase were also studied. The separation factor obtained was 1.32 and the resolution factor was 1.81 when using the optimized mobile phase composed of n -hexane-12-dichloroethane-methanol(54∶38∶8, volume ratio) at 17 ℃ and 1.0 mL/min. The mechanism of separation is also discussed.