涂敷型手性固定相的制备及氯氟草醚乙酯对映体的高效液相分离

 在前人工作的基础上,以微晶纤维素和3,5 二甲基苯基异氰酸酯为原料合成了纤维素 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(APS)上,制备出纤维素 三(3,5 二甲基苯基氨基甲酸酯)涂敷型硅基手性固定相。通过元素分析、红外光谱对该固定相进行了表征。用正相高效液相法在该固定相上首次直接拆分了触杀型苗后除草剂氯氟草醚乙酯对映体。考察了流动相组成对对映体保留和拆分的影响,结果发现,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1 0%时,分离度已达3 95。

Preparation of Cellulose-Based Chiral Stationary Phase and Enantioseparation of Ethoxyfen-Ethyl by High Performance Liquid Chromatography

Cellulose-tris (3,5-dimethylphenylcarbamate) was prepared after a reported method, and was confirmed by infrared spectroscopy and elemental analysis. Then it was coated onto an amino-propylated mesopore spherical silica gel. The final product was used as the chiral stationary phase of high performance liquid chromatography for the enantioseparation of a novel herbicide ethoxyfen-ethyl. The enantioseparation of ethoxyfen-ethyl on this stationary phase has been achieved for the first time. Mixtures of hexane and isopropanol were used as mobile phases. The effects of isopropanol concentration in the mobile phase on the retention and resolution were investigated. With the decrease of the content of isopropanol in mobile phase, the resolution factors increased. When the isopropanol concentration decreased to one percent, the resolution factor was 3.95. The structural features of the solutes that influence chiral separation are also discussed.