Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry  

作　　者：Pei-xi ZHU Dan-hua WANG Cui-rong SUN Zhi-quan SHEN 

机构地区：[1]Department of Chemistry, Zhejiang University, Hangzhou 310027, China [2]Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027, China

出　　处：《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》2008年第5期385-390,共6页浙江大学学报（英文版）B辑（生物医学与生物技术）

基　　金：Project (No. 20772109) supported by the National Natural ScienceFoundation of China

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 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.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.

关 键 词：LISINOPRIL IMPURITIES High-performance liquid chromatography （HPLC） Multi-stage mass spectrometry （MS^n） 

分 类 号：R914[医药卫生—药物化学]