摘要
建立了一种液相色谱-质谱联用法对盐酸厄洛替尼片中基因毒性杂质3-乙炔苯胺含量的测定方法。采用ESI离子源正离子多反应监测(MRM)模式,选择离子对118→75、118→91进行测定。色谱柱为Thermo Hypersil GOLD C8(100 mm×4.6 mm,3μm),流动相为甲醇和水,梯度洗脱,流速为0.4 mL/min,柱温为35℃。结果表明:该方法中3-乙炔苯胺的检测质量浓度在1.0~20 ng/mL的范围内呈良好的线性关系,R^2=0.9994;精密度实验的相对标准偏差(n=6)为1.13%,低、中、高浓度的加标回收率(n=3)为90.1%~106.1%。该方法灵敏度高、专属性好、精密度高,满足盐酸厄洛替尼片中基因毒性杂质3-乙炔苯胺含量的测定要求。
A method was established for the determination of genotoxic impurity.in erlotinib hydrochloride(3-ethynylaniline)using liquid chromatography-mass spectrometry.Using the ESI ion source positive ion multireaction monitoring(MRM)mode,the ion pairs 118→75 and 118→91 were selected and measured.The chromatographic column was Thermo Hyperiil GOLD C8(100 mm×4.6 mm,3μm),the mobile phase was methanol and waterfor gradient elution,the flow rate was 0.4 mL/min,and the column temperature is 35℃.Results showed that the detection mass concentration of 3-ethynylaniline in this method had a good linear relationship in the range of 1.0 to 20 ng/mL,with R^2=0.9994.The relative standard deviation(n=6)of the precision experiment was 1.13%,and the recoveries of standard additions(n=3)at low,medium,and high concentrations were between 90.1%and 106.1%.The method exhibited high sensitivity,specificity,and precision,and it met the requirement for the determination of 3-acetyleniline,a genotoxic impurity in erlotinib hydrochloride tablets.
作者
刘兰畦
赵燕芳
谢含仪
王珊珊
陈相峰
LIU Lan-qi;ZHAO Yan-fang;XIE Han-yi;WANG Shan-shan;CHEN Xiang-feng(Shandong Analysis and Test Center,Qilu University of Technology(Shandong Academy of Sciences),Jinan 250014,China)
出处
《山东科学》
CAS
2020年第2期121-125,共5页
Shandong Science
基金
山东省重点研究发展计划(2019GSF111001)
山东省科学院青年博士基金(2019QN009)。
关键词
液相色谱-质谱联用法
盐酸厄洛替尼片
3-乙炔苯胺
方法学验证
liquid chromatography-mass spectrometry
erlotinic hydrochloride
3-acetylene aniline
methodology validation
