酸性外消旋联苯类药物在纤维素-三(3,5-二甲基苯基氨基甲酸酯)固定相上的直接拆分

 合成了纤维素 三 ( 3,5 二甲基苯基氨基甲酸酯 ) (CDMPC)衍生物 ,并将其涂敷于自制的球形硅胶上 ,制备出用于高效液相色谱手性拆分的固定相。在正相条件下 ,用该固定相对 5种酸性外消旋联苯类药物进行了直接拆分 ,并考察了流动相组成和样品结构对保留和拆分的影响 ,讨论了固定相对样品的作用模式。结果表明 ,在正己烷 /异丙醇流动相体系中加入少量三氟乙酸 ,可对外消旋羧酸类化合物进行有效的手性拆分。

Direct optical resolution of acidic biphenyl drugs by high performance liquid chromatography on tris(3,5-dimethylphenylcarbamate) of cellulose]

A chiral stationary phase was prepared by coating cellulose-tris(3, 5-dimethylphenylcarbamate) onto aminopropylated silica gel. A series of enantiomeric acidic biphenyl drugs were directly resolved on the chiral stationary phase (CSP) by normal-phase high performance liquid chromatography (HPLC). A hexane-2-propanol eluting system containing 1% of trifluoroacetic acid was used as mobile phase. Efficient optical resolution of the acidic biphenyl drugs has been attained. The factors that influence chiral discrimination such as structural characeristic of the samples and mobile phase were investigated. An interaction model between the stationary phase and the samples was discussed. The results showed that efficient optical resolution of racemic carboxylic acids could be attained by normal-phase HPLC on CSP using a hexane-2-propanol eluting system containing 1% of trifluoroacetic acid.