GC-MS法测定缬沙坦中的N-亚硝基二甲胺  

Determination of the contents of N-nitrosodimethylamine in valsartan by GC-MS

作　　者：吴兆伟[1] 杜凯[1] 王琳[1] 郑洁[1] 胡琴[1] 张喆[1] 吴斌[1] WU Zhao-wei;DU Kai;WANG Lin;ZHENG Jie;HU Qin;ZHANG Zhe;WU Bin(Beijing Institute for Drug Control,National Medical Products Administration Key Laboratory for Research and Evaluation of Generic Drugs,Beijing 102206,China)

机构地区：[1]北京市药品检验所国家药品监督管理局仿制药研究与评价重点实验室

出　　处：《中国新药杂志》2019年第20期2478-2481,共4页Chinese Journal of New Drugs

基　　金：国家“重大新药创制”科技重大专项资助项目(2017ZX09101001)

摘　　要：目的:建立气质联用法测定缬沙坦中N-亚硝基二甲胺(N-nitrosodimethylamine,NDMA)的含量,确保缬沙坦原料药的质量安全。方法:采用GC-MS方法,使用DB-WAX UI石英毛细管柱(30 m×0.25mm,0.25μm),按内标曲线法测定缬沙坦中NDMA的含量。结果:该方法线性范围3~300 ng·mL^-1,r=0.9999;平均回收率103.2%,RSD=2.5%;检出限为1 ng·mL^-1。用建立的方法测定了2家企业共9批缬沙坦样品,其中一家企业所有样品中均未检出NDMA,另一家企业样品中NDMA的含量为0.08~0.14 ppm。结论:该方法操作简单、灵敏、准确,适用于缬沙坦原料药中NDMA的检测。Objective:To establish a method for determination of N-nitrosodimethylamine(NDMA)in valsartan by GC-MS to meet the need of quality assurance and safety supervision.Methods:NDMA was determined by GC-MS using DB-WAX UI(30 m×0.25 mm,0.25μm)capillary column and internal standard curve method.Results:The linear calibration curve was obtained over the range of 3~300 ng·mL^-1(r=0.9999).The average recovery was 103.2%with RSD of 2.5%.The limit of detection was 1 ng·mL^-1.Nine batches of samples from two companies were tested.For the samples from one of the two companies,NMDA was not detected,while for the other one the content was 0.08~0.14 ppm.Conclusion:The method is simple,sensitive and accurate,and can be used for determination of NDMA in valsartan.

关 键 词：气相色谱质谱联用 N-亚硝基二甲胺 遗传毒性杂质 缬沙坦 

分 类 号：R917[医药卫生—药物分析学]