双相识别HPLC法拆分普萘洛尔对映体  

The Resolution of Propranolol Enantiomers by HPLC with Two-Phase Discrimination

作　　者：李乃瑄[1] 肖如亭[1] 董迎[1] 高素华[1] 杨俊杰[1] 

机构地区：[1]天津理工学院生物与化学工程系,天津300191

出　　处：《应用化学》2003年第11期1084-1087,共4页Chinese Journal of Applied Chemistry

基　　金：天津市教委科技发展基金资助项目 ( 0 1 2 0 5 10 )

摘　　要：建立了一种手性固定相和手性流动相双相识别的HPLC拆分手性化合物对映体的新方法。在γ 氨丙基硅胶上涂覆质量分数为 1 5 %的纤维素 三苯甲酸酯 (CTB)作为手性固定相 ,流动相组成为V(正己烷 )∶V(乙醇 ) =85∶1 5 ,添加N 苄氧羰基 S 苯基 L 半胱胺酸 (BPC)为手性试剂 ,c(BPC) =0 40mmol/L ,流动相流速为 0 3mL/min ,检测波长为 2 5 4nm ,普萘洛尔对映体的分离选择性系数为 1 3 0 ,分离度为 1 5 6。BPC的辅助识别明显提高了CTB对普萘洛尔对映体的手性识别能力 ,可满足用高效液相制备色谱技术进行拆分的要求。结合热力学参数 ,探讨了双相识别HPLC的拆分机理。The resolution of propranolol enantiomers has been sucessfully carried out by HPLC using two phase discrimination:γ-amino propyl silica gel coated with 15%(mass fraction) of cellulose tribenzoate(CTB) as chiral stationary phase and hexane-alcohol(V∶V=85∶15) soltuion containing 0.40 mmol/L N-benzyloxycarbonyl-S-phenyl-L-cysteine(BPC) as chiral mobile phase. The chromatiographic method with flow rate of 0.3 mL/min and UV detection at 254 nm gave a separation selectivity of 1.30 and a separation degree of 1.56. The discrimination of CTB to propranolol enantiomers was apparently improved by the presence of BPC. The resolution mechanism of the two-phases discrimination has been discussed based on the thermodynamic parameters obtained.

关 键 词：双相识别 普萘洛尔 拆分 高效液相色谱 

分 类 号：O658[理学—分析化学]