节点文献
纤维素2,3-位和2,3,6-位苯基氨基甲酸酯手性固定相的选择性研究
Study on Enantioselectivity of Celluloses Derived by Phenylcarbamate at 2,3or 2,3,6-Positions
【摘要】 合成了纤维素-2,3,6-三苯基氨基甲酸酯、纤维素-2,3-二苯基氨基甲酸酯、纤维素-2,3,6-三(3,5-二甲基苯基氨基甲酸酯)和纤维素-2,3-二(3,5-二甲基苯基氨基甲酸酯)4种纤维素衍生物手性固定相,用正己烷-异丙醇(体积比为9∶1)混合液作流动相,对9种手性化合物进行了高效液相色谱拆分。实验结果表明:对所测的9个样品,纤维素-2,3-二苯基氨基甲酸酯的手性选择性大大好于纤维素-2,3,6-三苯基氨基甲酸酯;而纤维素-2,3-二(3,5-二甲基苯基氨基甲酸酯)与纤维素-2,3,6-三(3,5-二甲基苯基氨基甲酸酯)的分离因子针对不同的对映体各有优点,但前者通常具有更小的保留因子,可以缩短一定的分析时间。
【Abstract】 Cellulose-2,3,6-trisphenylcarbamate,cellulose-2,3-bisphenylcarbamate,cellulose-2,3,6-tris(3,5-dimethylphenylcarbamate) and cellulose-2,3-bis(3,5-dimethylphenylcarbamate) were synthesized and respectively coated on silica gel as chiral stationary phases for high performance liquid chromatography(HPLC).Nine pairs of enantiomers,which are(±)-phenyl-1,2-ethanediol,(±)2-phenyl-1-propanol,DL-alpha-methylbenzylamine,DL-mandelic acid,(±)-1-(1-naphthyl) ethanol,(±)-propranolol,(±)-3-benzyloxy-1,2-propanediol,DL-tyrosine and(±)-di-O,O-p-toluyl-D-tartaric acid,were separated using hexane-isopropanol as mobile phase on the columns packed with the chiral stationary phases.For comparative reasons,the ratio of hexane/isopropanol in the eluent was kept at 9∶1(v/v) in all experiments,and the chromatographic separations were performed at 30 ℃ with a flow rate of 0.5 mL/min.All the test solutes were detected at 254 nm.The results showed that enantioseparation of cellulose-2,3-bisphenylcarbamate was better than cellulose-2,3,6-trisphenylcarbamate for the test enantiomers,and cellulose-2,3-bis(3,5dimethylphenylcarbamate) had low retention factors and short analysis times for most enantiomers and good separation factors for some racemates compared to cellulose-2,3,6-tris(3,5-dimethylphenylcarbamate).
【Key words】 cellulose derivatives; chiral stationary phases; high performance liquid chromatography(HPLC);
- 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2007年02期
- 【分类号】O657.7
- 【被引频次】10
- 【下载频次】278