摘要
目的建立盐酸雷尼替丁胶囊中N-亚硝基二甲胺(N-nitrosodimethylamine,NDMA)的含量,确保盐酸雷尼替丁胶囊的质量安全。方法采用液相色谱-大气压化学离子化-三重四极杆质谱联用法(LC-APCI-MS/MS)测定雷尼替丁中N-亚硝基二甲胺,色谱柱为ACE EXCEL 3 C_(18)-AR(4.6×150 mm×3μm),质谱采用正离子MRM扫描方式,结果表明:在1~500 ng·mL^(-1)范围内线性关系良好,回收率在99.7%~103.7%之间,平均回收率101.5%,RSD=1.8%。结果用建立的方法测定了2家企业共6批雷尼替丁胶囊样品,其中A企业样品中NDMA的含量为8.1~30.0 ppm,另一家企业样品中NDMA的含量为0.6 ppm。结论所建立的方法经方法学验证,该方法专属性强,可用于盐酸雷尼替丁胶囊中N-亚硝基二甲胺的含量测定,为雷尼替丁胶囊的质量控制及标准研究提供参考。
OBJECTIVE To establish a method for determination of NDMA in Ranitidine Hydrochloride Tablets by LC-APCI-MS/MS to meet the need of quality assurance and safety supervision.METHODS Identification of NDMA in Ranitidine Hydrochloride Tablets was established by LC-APCI-MS/MS using ACE EXCEL 3 C_(18)-AR(4.6×150 mm×3μm)Chromatographic column and the mass spectrum adopts positive ion MRM scanning mode.The linear calibration curve was obtained over the range of 1-500 ng·mL^(-1)(r=0.9994).The average recovery was 101.5%with RSD of 1.8%.RESULTS Six batches of samples from two companies were tested.For the samples from one of the two companies,the content of NDMA was 8.1-30.0 ppm,while for the other one the content was 0.6 ppm.CONCLUSION The method is simple,sensitive and accurate,and can be used for determination of NDMA in Ranitidine Hydrochloride Tablets.The method provides a scientific reference for the study of quality control method of NDMA in Ranitidine Hydrochloride Tablets.
作者
陈鸿玉
易必新
章为
刘雁鸣
李晓燕
李昌亮
王伟姣
CHEN Hong-yu;YI Bi-xin;ZHANG Wei;LIU Yan-ming;LI Xiao-yan;LI Chang-liang;WANG Wei-jiao(Hunan Institute for Drug Control,Changsha 410001,China;Hunan Pharmaceutical Quality Evaluation Engineering and Technology Research Center,Changsha 410001,China)
出处
《海峡药学》
2021年第2期70-73,共4页
Strait Pharmaceutical Journal
