GC-MS法测定吉非替尼中的基因毒性杂质  

Determination of Genotoxic Impurities in Gefitinib by GC-MS

作　　者：丁兵 卢红华 孙建合 冯中 张贵民 DING Bing;LU Honghua;SUN Jianhe;FENG Zhong;ZHANG Guimin(National Chiral Pharmaceuticals Engineering and Technology Research Center,Lunan Pharmaceutical Group Co.,Ltd.,Linyi 273400)

机构地区：[1]鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂273400

出　　处：《中国医药工业杂志》2020年第11期1432-1434,共3页Chinese Journal of Pharmaceuticals

摘　　要：建立了气相色谱-质谱(GC-MS)法同时测定吉非替尼中遗传毒性杂质3,4-二氟硝基苯(3)、3-氯-4-氟硝基苯(4)和3,4-二氯硝基苯(5)。采用DB-624MS毛细管色谱柱,以选择离子监测(SIM)模式进行测定。结果显示,3、4、5在质量浓度12~72 ng/ml内线性关系良好,定量限分别为1.48、3.72、10.00 ng/ml,回收率分别为93.77%、99.27%和97.04%。A gas chromatography-mass spectrometry(GC-MS)method was established for the simultaneous determination of the genotoxic impurities including 3,4-difluoronitrobenzene(3),3-chloro-4-fluoronitrobenzene(4)and 3,4-dichloronitrobenzene(5)in gefitinib(1).The DB-624MS capillary column was used,and the measurement was performed in selected ion monitoring(SIM)mode.The results showed that it was linear for 3,4 and 5 in the range of 12-72 ng/ml.The limits of quantification were 1.48,3.72,10.00 ng/ml respectively,and the recoveries were 93.77%,99.27%,and 97.04%respectively.

关 键 词：气相色谱-质谱(GC-MS) 吉非替尼 3 4-二氟硝基苯 3-氯-4-氟硝基苯 3 4-二氯硝基苯 

分 类 号：O657.7[理学—分析化学]