纤维素三苯甲酸酯作为薄层色谱固定相拆分手性化合物

Tribenzoyl-cellulose as Stationary Phase for Chiral Separation of Optical Isomers

用超声的方法合成了纤维素三苯甲酸酯(CTB),并将得到的产物用红外光谱与元素分析进行了表征。将该种手性固定相(CSP)用于薄层色谱分离手性化合物,分别采用TEAA,乙腈∶TEAA=2∶1及乙酸乙酯∶水∶冰乙酸=6∶2∶1作为展开剂,使2-(9-蒽基)-2-甲氧基乙酸、2-(9-蒽基)-2-羟基乙酸及苯丙氨酸都获得了完全分离。

Tribenzoyl-cellulose was synthesized by homogeneous reaction of benzoyl chloride with microcrystalline cellulose in pyridine under ultrasonication at about 45℃. Elemental analysis and IR spectra indicated that almost all hydroxyl groups of the cellulose were converted to ester groups in the pure polymeric form. The prepared tribenzoyl-cellulose was used as chiral stationary phase of thin-layer chromatography to separate three chiral molecules, 2-（9-anththryl）-2-methoxyacetic acid, 2-（9-anthryl）- 2-hydroxyacetic acid and 2-amino-3-phenylpropanoic acid. The three chiral molecules were completely separated by using TEAA, acetonitrile-1 % TEAA （2 ： 1 ） and ethyl acetate-H2O-acetic acid （6 ： 2 ： 1） as developer, respectively.