NP-HPLC法分离测定阿普斯特及其中间体的对映异构体  

Determination of the Enantiomer of Apremilast and Its Intermediate by NP-HPLC

作　　者：王慧君[1] 黄生军[2] 潘红娟[1] 

机构地区：[1]中国医药工业研究总院上海医药工业研究院,分析测试中心,上海201203 [2]上海现代制药股份有限公司,上海200137

出　　处：《中国医药工业杂志》2016年第10期1284-1288,共5页Chinese Journal of Pharmaceuticals

摘　　要：建立了正相高效液相色谱法测定阿普斯特（1）中的对映异构体（2）。采用Daicel Chiralpak IF柱,流动相为正己烷∶无水乙醇∶异丙醇∶二乙胺（30∶40∶30∶0.1）,检测波长232 nm。2在1.0-10μg/ml范围内线性关系良好,检测限为0.084μg/ml;平均回收率为99.1%,RSD为1.59%。同时建立了正相高效液相色谱法测定阿普斯特中间体（3）中的对映异构体（4）。采用Daicel Chiralpak IF柱,流动相为正己烷∶异丙醇∶二乙胺（50∶50∶0.1）,检测波长232 nm。4在2.0-10μg/ml范围内线性关系良好,检测限为1.012μg/ml;平均回收率为98.9%,RSD为3.20%。A NP-HPLC method was established for the chiral separation and determination of the enantiomer （2） of apremilast （1）. A Daicel Chiralpak IF column was used, with the mobile phase of hexane∶ethanol∶isopropanol∶ diethylamine （30∶40∶30∶0.1） at the detection wavelength of 232 nm. It was linear for 2 in the range of 1.0—10 μg/ml. Its LOD was 0.084 μg/ml, and average recovery was 99.1%, with RSD of 1.59%. In addition, a NP-HPLC method was established for the chiral separation and determination of the intermediate of the enantiomer （4） in apremilast （3）. A Daicel Chiralpak IF column was used, with the mobile phase of hexane∶isopropanol∶diethylamine （50∶50∶0.1） at the detection wavelength of 232 nm. It was linear for 4 in the range of 2.0—10 μg/ml. The LOD was 1.012 μg/ml. Its average recovery was 98.9%, with RSD of 3.20%.

关 键 词：阿普斯特 中间体 对映异构体 高效液相色谱 手性拆分 含量测定 

分 类 号：TQ465.72[化学工程—制药化工] O657.72[理学—分析化学]