纤维素-三(苯基氨基甲酸酯)涂敷氧化锆固定相的制备及硒代缩水甘油醚的拆分

Preparation of Cellulose-Tris (phenylcarbamate) Coated Zirconia and Its Direct Apllication on Enantioseparation of Glycidyl Selenides by High Performance Liquid Chromatography

制备并表征了纤维素 三(苯基氨基甲酸酯)涂敷氧化锆手性固定相,并用该固定相直接拆分了3种硒代缩水甘油醚。考察了固定相涂敷量、流动相组成等对手性拆分的影响。讨论了硒代缩水甘油醚分子结构与保留因子、选择性因子和分离因子的关系。结果表明,固定相的羰基和氨基是手性分离的主要部位,固定相的手性空穴是对映体分离产生立体差异的关键,对映体手性碳上连接的基团的立体效应是影响拆分的主要因素。实验结果表明:纤维素 三(苯基氨基甲酸酯)是性能稳定、有很好的手性拆分能力的固定相。

Cellulosetris (phenylcarbamate) coated zirconia chiral stationary phase (CTPC coated ZrO2 CSP) was prepared for high performance liquid chromatography. The chiral stationary phase exhibits good chiral recognition for racemic glycidyl selenides under normal conditions. The relationships between the separation parameters, such as retention factor, enantioselectivity and resolution, and the structures of glycidyl selenides were investigated. The influences of the loading of stationary phase and the solvent polarity of mobile phase on chromatographic behavior and chiral separation of the analytes were observed. The chiral recognition mechanism of the chiral stationary phase is also discussed.