2,6-二-O-苄基-β-环糊精键合硅胶固定相的合成与色谱性能

Preparation and Chromatographic Performances of 2,6-di-O- Benzyl-β-Cyclodextrin Bonded Silica Stationary Phase

为了提高环糊精键合固定相的立体选择性,以γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷为连接臂,合成了2,6-二-O-苄基-β-CD键合硅胶固定相(BCDS);利用傅里叶红外光谱、X射线光电子能谱、莫氏(Molisch)试验颜色反应进行了表征;以邻苯二甲酸二甲酯、甲苯和菲为测试溶质,评价了该键合固定相的色谱性能;考察了该固定相对位置异构体的分离效果,硝基苯胺、苯二酚等的位置异构体在新合成的键合固定相上得到了很好的分离.实验结果说明:通过把β-CD的2-,6-羟基用苄基取代,这种亲水性的变化改变了环糊精键合固定相的保留性能和立体选择性.

In order to improve the stereoselectivity of the native β-cyclodextrin boned-silica gel stationary phase, 2,6-di-O-benzyl-β-cyclodextrin bonded stationary phase (BCDS) was prepared via the spacer γ-glycidoxypropyltrimethoxy-silane. The bonded silica was characterized by three methods (Fourier transform infrared spectrogram, Molish color reaction, X-ray optical electrical energy spectrogram). The chromatographic performances of BCDS were appraised by using toluene, dimethyl phthalate and phenanthrene. The selectivity of the new bonded-silica gel stationary phase was investigated by isomers. Some of the isomers such as nitroaniline, diphenols etc. were separated successfully by 2,6-di-O-benzyl-β-cyclodextrin bonded silica stationary. The results show that the introduction of benzyl to β-cyclodextrin leads to change of the retention of solutes and the dimensional selectivity.