注射用盐酸吉西他滨及其原辅料中丙酮、二氯甲烷、吡啶残留溶剂测定  

Determination of Acetone,Dichloromethane,Pyridine in Gemcitabine Hydrochloride for Injection and Its API and Ingredients

作　　者：熊欣 郭艳芳 钟振华 夏红英 刘贞 程奇珍 XIONG Xin;GUO Yanfang;ZHONG Zhenhua;XIA Hongying;LIU Zhen;CHENG Qizhen(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang Jiangxi 330029,China)

机构地区：[1]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,江西南昌330029

出　　处：《药品评价》2021年第16期969-972,共4页Drug Evaluation

摘　　要：目的:建立了气相色谱法测定注射用盐酸吉西他滨中丙酮、二氯甲烷、吡啶3种有机溶剂残留量的方法。方法:采用溶液直接进样法,在优化的气相色谱条件下,对收集到的58批次注射用盐酸吉西他滨、8批次盐酸吉西他滨原料及26批次辅料进行3种有机溶剂残留量的测定。结果:方法操作简便,3种残留溶剂均能有效分离,在考察浓度范围内,线性关系良好(r=0.9998),平均回收率90.5%~96.7%(n=9)。结论:该方法为制剂及原料药中残留溶剂的合理控制及其法定标准是否增订残留溶剂检查项提供数据依据。结合原料及制剂测定结果,建议制剂与原料生产企业优化生产工艺,严格控制内部工艺的稳定性,提高批间批内精密度。Objective:To establish a capillary GC method for the determination of acetone,dichloromethane,pyridine in gemcitabine hydrochloride for injection.Methods:The direct injection was used to determinate three residual organic solvents in 58 batches of gemcitabine hydrochloride for injection,8 batches of gemcitabine hydrochloride raw material and 26 batches of accessories at optimized chromatographic conditions.Results:The method was simple,the three residual organic solvents were separated well.Good linearities were obtained in the experimental concentration(correlation coefficient:r=0.9998).The average recoveries were in the range from 90.5%-96.7%(n=9).Conclusion:The method can provide data for rational control of residual solvents in preparations and APIs and provide gist for their statutory standards whether add a residual solvent item.Combined with the determination results of preparations and APIs, it is suggested that the manufacturers should optimize the manufacturing process, control the stability of internal process strictly, and improve with in-batch and batch-to-batch precision.

关 键 词：盐酸吉西他滨 丙酮 二氯甲烷 吡啶类 残留溶剂 气相色谱法 

分 类 号：R927[医药卫生—药学]