UPLC-MS/MS法测定依托度酸中的基因毒性杂质2-乙基苯肼  

Determination of the Genotoxic Impurity 2-Ethylphenyl Hydrazine in Etodolac by UPLC-MS/MS

作　　者：孙建合 侯继鹏 时晓燕 冯中 张贵民 SUN Jianhe;HOU Jipeng;SHI Xiaoyan;FENG Zhong;ZHANG Guimin(National Engineering Research Center of Chiral Drugs,Lunan Pharmaceutical Group,Linyi 273400;School of Pharmaceutical Science(Shenzhen),Sun Yat-sen University,Shenzhen 518107)

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 [2]中山大学药学院(深圳),广东深圳518107

出　　处：《中国医药工业杂志》2022年第4期564-566,571,共4页Chinese Journal of Pharmaceuticals

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法测定依托度酸(1)中的基因毒性杂质2-乙基苯肼(2)。色谱柱采用ACQUITY HSS T;柱(2.1 mm×100 mm,1.8 μm),以0.1%甲酸为流动相A,含0.1%甲酸的乙腈为流动相B,梯度洗脱。采用电喷雾电离源(ESI),正离子模式采集,选择反应监测模式(SRM)。选择m/z 137.14→108.13为定性离子对,m/z 137.14→120.05为定量离子对。结果显示,2在12.25~122.5 pg/ml内线性关系良好,检测限和定量限分别为3.68、12.25 pg/ml。平均回收率(n=9)为85.46%,RSD为3.56%,可为1中2的测定提供参考。A UPLC-MS/MS method was established for the determination of the genotoxic impurity 2-ethylphenyl hydrazine(2) in etodolac(1).The ACQUITY HSS T;column(2.1 mm×100 mm,1.8 μm) was used,and the analysis was carried out in the gradient elution mode with 0.1% formic acid as mobile phase A,and acetonitrile containing 0.1% formic acid as mobile phase B.Electron spray ionization(ESI),positive ion mode acquisition and selective reaction monitoring(SRM) mode was used.The m/z 137.14→108.13 was selected as qualifier transition,and m/z 137.14→120.05 was selected as quantifier transition.The results showed that it was linear for 2 in the range of 12.25-122.5 pg/ml,and the LOD and LOQ were 3.68 and 12.25 pg/ml,respectively.The average recovery(n=9) was 85.46%,with the RSD of 3.56%,which could provide a reference for the determination of 2 in 1.

关 键 词：依托度酸 基因毒性杂质 2-乙基苯肼 超高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]