支链淀粉-三(苯基氨基甲酸酯)手性固定相的制备及对外消旋环酮和环醇的直接拆分  被引量:4

Direct Enantiomeric Resolution of Cyclic Ketones and Cyclic Alcohol Using Amylopectin Tris(Phenylcarbamate) Chiral Stationary Phase

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作  者:周志强[1] 侯经国[1] 蒋生祥[1] 陈立仁[1] 

机构地区:[1]中国科学院兰州化学物理研究所,兰州730000

出  处:《分析化学》1997年第12期1423-1425,共3页Chinese Journal of Analytical Chemistry

基  金:中国科学院重点项目基金

摘  要:在参照文献基础上,合成并制备了支链淀粉-三(苯基氨基甲酸酯)手性固定相,以此手性固定相为基础,利用高效液相色谱首次直接拆分了3种外消旋环酮和一种外消旋环醇,并考察了流动相中异丙醇含量对拆分的影响。In the present study, we have synthesized amylopectin tris(phenylcarbamate) and used it as chiral stationary phase. This stationary phase offers a practically useful chiral column with a high enantiomer-separability. Amylopectin was allowed to react with an excess of phenylisocyanate in pyridine for 48 h. The carbamates obtained was dissolved and adsorbed on silica gel which had been treated with 3-aminopropyltriethoxysilane. The weight ratio of the carbamate to the silica gel was 0. 45/2. 55. Three cyclic ketones and one cyclic alcohol were resolved on amylopectin tris(phenylcarbamate) chiral stationary phase with a he-cane/2-propanol mixture at a flow rate of 0. 5 mL/min at room temperature. The effects of 2-propanol concentration on the retention and resolution have been investigated.

关 键 词:支链淀粉 手性固定相 外消旋化合物 拆分 HPLC 

分 类 号:O657.720.3[理学—分析化学]

 

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