LC-MS法研究西司他丁钠中的有关物质  

LC-MS Studies on Related Substances in Cilastatin Sodium

作　　者：陆静[1] 李悦[1] 王慧敏[1] 杨明 

机构地区：[1]中国医药工业研究总院上海医药工业研究院,创新药物与制药工艺国家重点实验室,上海200040 [2]珠海联邦制药股份有限公司,广东珠海519041

出　　处：《中国医药工业杂志》2012年第11期938-942,共5页Chinese Journal of Pharmaceuticals

摘　　要：建立了液相色谱-质谱法检测并初步鉴定西司他丁钠原药中的有关物质,并考察了本法的专属性及有关物质的降解途径。采用Sepax HP C18色谱柱,以A:乙腈-0.1%甲酸水溶液(30︰70),B:0.1%甲酸水溶液为流动相进行梯度洗脱,0～30 min,15%～100%流动相A,30～45 min,100%流动相A。采用正离子模式采集数据。原药共检测出10个有关物质,推测分别为欧洲药典中收载的有关物质A、B、C,A的同分异构体,西司他丁酸降解产物,4个西司他丁同分异构体和1个西司他丁二聚物。A new LC-MS method was established for the determination of the related substances in cilastatin sodium. The specialization of the method and the degradation pathway of the related substances were also studied. A Sepax HP C18 column was used with the mobile phase of acetonitrile-0.1% formic acid aqueous solution （30 ： 70, A） and 0.1% formic acid aqueous solution （B） by gradient elution, which was operated at 15% - 100% A （0 - 30 rain） followed by 100 % A （30 - 45 min）. The data was acquired in positive ion mode. Ten related substances were detected in cilastatin sodium, including three compounds （impurity A, B and C） collected by European Pharmacopoeia, the isomer of impurity A, the acid hydrolysate of cilastatin, four isomeric compounds of cilastatin and a dipolymer.

关 键 词：西司他丁钠 有关物质 液相色谱-质谱 结构解析 

分 类 号：TQ463[化学工程—制药化工] TQ460.73