苯并咪唑衍生物对映体的高效液相色谱手性分离

Separation of Enantiomers of a Benzimidazole Derivative by High Performance Liquid Chromatography

在参照文献的基础上 ,合成了纤维素三 (3,5 -二甲基苯基氨基甲酸酯 ) ,并将其涂敷于小粒径的氨丙基化硅胶上 ,制备出涂敷型手性固定相。通过元素分析、红外光谱对该固定相进行了表征。正相高效液相色谱条件下 ,在该固定相上首次直接拆分了具有杀菌活性的 2 - (1-羟基乙基 ) - 1H -苯并咪唑对映体。并考察了流动相组成对对映体保留和拆分的影响。随着异丙醇体积分数的减小 ,对映体的分离度逐渐增大 ,在异丙醇的体积分数为 10 %时 ,分离度达 2 .2

Cellulose tris (3,5 dimethylphenylcarbamate) was prepared according to a reported method, and the structure was confirmed by infrared spectroscopy and elemental Analysis. It was coated onto an aminopropylated mesopore spherical silica gel, and the final product was used as a chiral stationary phase of high performance liquid chromatography for the enantioseparation of 2 (1 hydroxyethyl) 1 H benzimidazole, which is effective against Candida tropicalis with contact action. The first enantioseparation of this compound has been achieved. Mixtures of hexane and 2 propanol were used as mobile phases. The effects of 2 propanol concentration in the mobile phase on the retention and resolution were investigated. While the concentration of 2 propanol in mobile phase was decreasing, the resolution factor was increased. When the 2 propanol concentration comes down to 10%, the resolution factor is 2.23.