摘要
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry(HPLC/MS) with a simple and sensitive method suitable for HPLC/MSn analysis. The frag-mentation behavior of lisinopril and the impurities was investigated,and two unknown impurities were elucidated as 2-(6-amino-1-(1-carboxyethylamino)-1-oxohexan-2-ylamino)-4-phenylbutanoic acid and 6-amino-2-(1-carboxy-3-phenylpro-pylamino)-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence. The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance(NMR) experiments after preparative isola-tion.
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry （HPLC/MS） with a simple and sensitive method suitable for HPLC/MSn analysis. The fragmentation behavior of lisinopfil and the impurities was investigated, and two unknown impurities were elucidated as 2-（6-amino- l-（l-carboxyethylamino）- l-oxohexan-2-ylamino）-4-phenylbutanoic acid and 6-amino-2-（l-carboxy-3-phenylpropylamino）-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence, The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance （NMR） experiments after preparative isolation.
基金
Project (No. 20772109) supported by the National Natural ScienceFoundation of China
关键词
赖诺普利
杂质
高性能液体色谱法
质谱分析
Lisinopril, Impurities, High-performance liquid chromatography （HPLC）, Multi-stage mass spectrometry （MS^n）
