Abstract: 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,3 μm),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 R²=0.999 4.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.

Key words: liquid chromatography-mass spectrometry, erlotinic hydrochloride, 3-acetylene aniline, methodology validation