键合型纤维素3,5-二甲基苯基氨基甲酸酯手性固定相的制备及分离性能研究  

Preparation and Evaluation of Immobilized Chiral Stationary Phases Based on Cellulose 3,5-Dimethylphenylcarbamate

作　　者：张超超[1] 唐守万[2] 潘富友[2] 高建荣[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310014 [2]台州学院医药化工学院,浙江台州318000

出　　处：《分析测试学报》2014年第1期68-72,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金青年科学基金资助项目(20905057)

摘　　要：将溶于N,N-二甲基乙酰胺-LiCl-吡啶的纤维素混合液直接涂敷于氨丙基硅胶上,分别以4,4'-二苯基甲烷二异氰酸酯和1,6-己二异氰酸酯为间隔臂将纤维素键合到硅胶上,并通过与过量的3,5-二甲基苯基异氰酸酯反应,制得2种键合型纤维素3,5-二甲基苯基氨基甲酸酯手性固定相。考察了固定相的分离性能。研究表明,所制备的手性固定相具有较高的手性识别能力和溶剂耐受性,相比于常规流动相(正己烷/异丙醇混合液),当流动相中含有三氯甲烷或四氢呋喃时,多数对映体得到了更好的分离,且二异氰酸酯的种类对手性固定相的手性识别能力影响较小。After cellulose was dissolved in a mixture of N,N-dimethylacetamide-LiC1-pyridine mixed solution,it was directly coated onto y-aminopropyl silica gel,then immobilized onto silica gel using 4,4＇-diphenylmethane diisocyanate and hexamethylene diisocyanate as the spacer,respectively,and finally reacted with an excess of 3,5-dimethylphenyl isocyanate.Thus,two immobilizedtype chiral stationary phases（CSPs） based on cellulose 3,5-dimethylphenylcarbamate were prepared and evaluated for HPLC enantioseparation.The results showed that the obtained CSPs exhibited high chiral recognition ability and solvent durability.Many of the tested racemates could be well resolved when using eluents containing chloroform or tetrabydrofuran instead of the conventional eluent （e.g.hexane-isopropanol mixture）.In addition,interfences on the chiral recognition of CSPs due to different diisocyanates could be negligible.

关 键 词：手性固定相 多糖衍生物 键合 手性识别 手性分离 

分 类 号：O657.7[理学—分析化学] TQ460.72[理学—化学]