2015年版《中国药典》环磷酰胺有关物质检测方法的验证与改进  

Validation and Improvement of the Detection Method for Cyclophosphamide Related Substances in Chinese Pharmacopoeia(2015 Edition)

作　　者：雷成康 郭玲[2] 

机构地区：[1]西安市食品药品检验所,西安710054 [2]陕西师范大学生命科学学院,西安710119

出　　处：《中国药房》2016年第36期5122-5124,共3页China Pharmacy

基　　金：2014年国家药品计划抽验项目(No.111)

摘　　要：目的:改进环磷酰胺有关物质的检测方法。方法:对2015年版《中国药典》收载的环磷酰胺有关物质检测的薄层色谱法(TLC)进行验证,并对该方法进行改进,以环磷酰胺有关物质A、B、C、D对照品为对照,以二氯甲烷-冰乙酸-甲醇-水(50∶25∶15∶12,V/V/V/V)为展开剂,以茚三酮试液为显色剂,进行有关物质检测试验及方法学验证。结果:原TLC法不仅无法检测到环磷酰胺有关物质B、C、D,且操作过程烦琐,不够环保。改进后的TLC法对环磷酰胺有关物质A的检测限约为0.05μg,对有关物质B、C、D的检测限约为0.1μg;方法专属性试验结果表明,环磷酰胺与各有关物质之间互不干扰,分离度良好。结论:改进的TLC法具有简便、环保、灵敏度高的优点,可用于环磷酰胺及其制剂的质量控制。OBJECTIVE： To improve the detection method for the related substances of cyclophosphamide. METHODS： The TLC for the detection method of the cyclophosphamide related substances in Chinese Pharmacopoeia （2015 edition） was verified; the TLC was improved with references of compound A, B, C, D, the expanding agent of dichloromethane-acetic acid-metha- nol-water （50：25： 15： 12, V/V/V/V） and the chromogenic agent of ninhydrin solution, and the detection test and methodology valida- tion were conducted for the related substances. RESULTS： The original TLC can not detect the cyclophosphamide related compound B, C, D, and the operation process was cumbersome and not environmental protection. The detection limit of improved TLC for cyclophosphamide related compound A was 0.05 gg, and 0.1μg for related compound B, C, D; specificity method test results showed that cyclophosphamide and the related compounds did not interfere with each other with a good separation. CONCLU- SIONS ： Improved TLC has the advantages of simplicity, environmental protection and high sensitivity, which can be used for the quality control of cyclophosphamide and its preparations.

关 键 词：环磷酰胺 有关物质 薄层色谱法 改进 

分 类 号：R927[医药卫生—药学]