大粒径纤维素衍生物手性固定相合成及对普萘洛尔的手性拆分研究  

Synthesis of Large Particle Cellulose Derivative Chiral Stationary Phase and Chiral Separation of Propranolol

作　　者：杨沛[1,2] 王荣[1,2] 马骏[1] 谢华[1] 张军莉[1] 贾正平[1,2] 武晓玉[1] 王娟[1] 

机构地区：[1]兰州军区兰州总医院药理基地,兰州市730050 [2]兰州大学药学院,兰州市730000

出　　处：《中国药房》2011年第33期3133-3136,共4页China Pharmacy

摘　　要：目的:合成适合于手性药物制备分离的大粒径纤维素衍生物手性固定相并评价其性能。方法:以微晶纤维素和3,5-二甲基苯基异氰酸酯为原料,合成纤维素-三(3,5-二甲基苯基氨基甲酸酯)(CDMPC),并涂敷于大粒径(40～60μm)的氨丙基烷化硅胶上,制得了涂敷型CDMPC手性固定相;对CDMPC进行元素分析和红外光谱分析;采用高效液相色谱法,在正相条件下以普萘洛尔为对象评价了CDMPC的手性拆分性能。结果:元素分析和红外光谱分析结果表明CDMPC成功涂敷于手性固定相;普萘洛尔在此手性固定相上获得了手性分离,分离度达到1.67。结论:制备的大粒径纤维素衍生物手性固定相具有良好的手性拆分性能。OBJECTIVE： To synthesize large particle cellulose derivative chiral stationary phase （CSP） for the preparation and separation of chiral drugs, and to evaluate its performance. METHODS： Cellulose-tris （3, 5-dimethylphenylcarbamate） （CDMPC） was synthesized using microcrystalline cellulose and 3, 5-dimethylphenylisocyanate as raw material, This derivative was coated onto the large particle （40--60 um） aminopropyl silica by evaporation to prepare coated CDMPC chiral stationary phase. Elementary analysis and infrared spectrum analysis of CDMPC were carried out. The chiral separation performance of prepared CSP was evaluated by HPLC using propranolol as subject under positive condition. RESULTS： Results of elementary analysis and infrared spectrum analysis indicated that CDMPC was coated onto ehiral stationary phase successfully; chiral separation of propranolol was achieved with separation rate of 1.67. CONCLUSION： The prepared large particle cellulose derivative CSP has good capability of chiral separation.

关 键 词：纤维素-三(3 5-二甲基苯基氨基甲酸酯) 手性固定相 高效液相色谱法 手性拆分 

分 类 号：R917[医药卫生—药物分析学]