不同载体涂敷的纤维素酯手性固定相的制备及性能

Preparation and Evaluation of Several Cellulose Ester-Coated Chiral Stationary Phases with Different Supports

微晶纤维素和3，5-二甲基苯基氨基甲酸酯为原料，合成了纤维素一三（3，5-二甲基苯基氨基甲酸酯）（CDMPC），将其分别涂敷于小孔硅胶（SG）、氨丙基化小孔硅胶（APS—SG）和介孔SBA-15微球上，制得3种手性固定相：SG@CDMPC（CSP1）、APS-SG@CDMPC（CSP2）及SBA．15@CDMPC（CSP3），正相条件下考察了12种中性或酸性手性化合物在自制手性固定相上的拆分效果，并与商品柱Chiralcel OD—H的拆分性能进行了对比。6个手性化合物在CSPl上获得比在商品柱上更高的柱效，其中2个手性化合物获得比在商品柱上更高的分离因子和分离度，而CSP2和CSP3的拆分效果总体较CSP1和商品柱的差。探讨了自制手性固定相对华法令的拆分和定量测定，华法令在CSPl上的检测限为10μg／L，在0．05—5g／L范围内线性关系良好。

Cellulose tris （ 3,5-dimethylphenylcarbamate ） （ CDMPC ） was prepared from cellulose and 3,5- dimethylphenyl isocyanate. Then the product was coated onto three supports, i.e. small-pore silica gel（ SG）, aminopropylsilylated silica gel （APS-SG）, and mesoporous silica SBA-15. The obtained chiral stationary phases（CSPs） were denoted as SG@ CDMPC （ CSP1 ）, APS-SG@ CDMPC （ CSP2）, and SBA-15@ CDMPC （CSP3）. Twelve neutral or acidic compounds were enantioseparated with these three homemade CSPs in the normal phase mode. The results were compared with enantioseparation using the commercial CSP, Chiralcel OD-H. Six compounds are obtained with a better column efficiency on CSP1 than that on Chiraleel OD-H, and two of them are obtained with a better enantioseparation. The enantioseparation ability is poorer on CSP2 and CSP3 than those on CSP1 and the commercial column in general. Enantioseparation and quantitative determination of warfarin were performed on the homemade CSPs. The limit of detection（LOD） is 10μg/L for warfarin on CSP1. The linear calibration curve is obtained in the concentration range of 0. 05 - 5.0 g/L.