Biochemistry |
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Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry |
Pei-xi ZHU, Dan-hua WANG, Cui-rong SUN, Zhi-quan SHEN |
Department of Chemistry, Zhejiang University, Hangzhou 310027, China; Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027, China |
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Abstract 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 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-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.
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Received: 24 January 2008
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