键合支链淀粉(3,5-二甲基苯基氨基甲酸酯)手性固定相的制备及手性拆分应用  

Preparation of bonded amylopectin(3,5-dimethylphenylcarbamate) chiral stationary phase and its application to chiral separation of racemic compounds

作　　者：韩小茜[1] 崔红[1] 李鸿瑜[1] 安丽丽[1] 常静[1] 

机构地区：[1]兰州交通大学化学与生物工程学院,兰州730070

出　　处：《分析仪器》2011年第2期21-26,共6页Analytical Instrumentation

基　　金：甘肃省科技攻关计划(2GS064-A52-036-06);兰州交通大学"青蓝"人才工程基金(QL-04-01A)

摘　　要：采用双官能团键合法,以六亚甲基异氰酸酯为键合试剂,自制了键合支链淀粉(3,5-二甲基苯基氨基甲酸酯)手性固定相。在所制得的固定相上,以正相、反相、极性有机相多种色谱分离模式对8种含苯环的手性化合物进行了拆分。实验结果发现,正相模式下,在流动相正己烷或正己烷/异丙醇中添加二氯甲烷、三氯甲烷、四氢呋喃有利于手性化合物的拆分。在反相和极性有机相色谱条件下,此固定相仍具有手性拆分能力;除样品7外,其余手性样品均获得不同程度的手性分离。A bonded amylopectin（3,5-dimethylphenylcarbamate） chiral stationary phase was prepared by double-functional group bonding method with hexamethylene diisocyanate as bonding agent.Eight racemic compounds with benzene ring were chirally separated using this stationary phase under normal-phase,reversed-phase and polar organic-phase chromatographic separation modes.Experimental results showed that under normal-phase mode,adding CH2CI2,CHCI3 and THF in mobile phase（hexence or hexene/isopropanol） was helpful for the separation of chiral compounds.Under reversed-phase（with methanol/water or CH3CN/water as mobite phase） and polar organic-phase（with methanol/isopropanol or CH3CN/isopropanol as mobile phase） modes,this stationary phase still has chiral separation ability.Except one sample,other seven chiral samples were all separated chirally with different degree.

关 键 词：键合型支链淀粉 3 5-二甲基苯基氨基甲酸酯 手性固定相 对映异构体 手性拆分 

分 类 号：O657.72[理学—分析化学]