Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry
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,...
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Veröffentlicht in: | Journal of Zhejiang University. B. Science 2008-05, Vol.9 (5), p.385-390 |
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description | 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. |
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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.</description><identifier>ISSN: 1673-1581</identifier><identifier>EISSN: 1862-1783</identifier><identifier>DOI: 10.1631/jzus.B0820031</identifier><identifier>PMID: 18500778</identifier><language>eng</language><publisher>Heidelberg: SP Zhejiang University Press</publisher><subject>Biochemistry ; Biomedical and Life Sciences ; Biomedicine ; Chromatography ; Chromatography, High Pressure Liquid - methods ; Drug Contamination ; Lisinopril - analysis ; Magnetic Resonance Spectroscopy ; Mass spectrometry ; NMR ; Nuclear magnetic resonance ; Spectrometry, Mass, Electrospray Ionization - methods ; 质谱分析 ; 赖诺普利 ; 高性能液体色谱法</subject><ispartof>Journal of Zhejiang University. B. Science, 2008-05, Vol.9 (5), p.385-390</ispartof><rights>Zhejiang University 2008</rights><rights>Copyright © Wanfang Data Co. Ltd. All Rights Reserved.</rights><rights>Copyright © 2008, Journal of Zhejiang University Science 2008</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c544t-12b6789d96496535de1e1b4a739866b9e763d82fd8bb974803cb9ae177a07edc3</citedby><cites>FETCH-LOGICAL-c544t-12b6789d96496535de1e1b4a739866b9e763d82fd8bb974803cb9ae177a07edc3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Uhttp://image.cqvip.com/vip1000/qk/86281A/86281A.jpg</thumbnail><linktopdf>$$Uhttps://www.ncbi.nlm.nih.gov/pmc/articles/PMC2367377/pdf/$$EPDF$$P50$$Gpubmedcentral$$H</linktopdf><linktohtml>$$Uhttps://www.ncbi.nlm.nih.gov/pmc/articles/PMC2367377/$$EHTML$$P50$$Gpubmedcentral$$H</linktohtml><link.rule.ids>230,314,727,780,784,885,27922,27923,41486,42555,51317,53789,53791</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/18500778$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Zhu, Pei-xi</creatorcontrib><creatorcontrib>Wang, Dan-hua</creatorcontrib><creatorcontrib>Sun, Cui-rong</creatorcontrib><creatorcontrib>Shen, Zhi-quan</creatorcontrib><title>Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry</title><title>Journal of Zhejiang University. B. Science</title><addtitle>J. Zhejiang Univ. Sci. B</addtitle><addtitle>Journal of Zhejiang University Science</addtitle><description>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.</description><subject>Biochemistry</subject><subject>Biomedical and Life Sciences</subject><subject>Biomedicine</subject><subject>Chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Drug Contamination</subject><subject>Lisinopril - analysis</subject><subject>Magnetic Resonance Spectroscopy</subject><subject>Mass spectrometry</subject><subject>NMR</subject><subject>Nuclear magnetic resonance</subject><subject>Spectrometry, Mass, Electrospray Ionization - 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B. Science</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Zhu, Pei-xi</au><au>Wang, Dan-hua</au><au>Sun, Cui-rong</au><au>Shen, Zhi-quan</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry</atitle><jtitle>Journal of Zhejiang University. B. Science</jtitle><stitle>J. Zhejiang Univ. Sci. B</stitle><addtitle>Journal of Zhejiang University Science</addtitle><date>2008-05-01</date><risdate>2008</risdate><volume>9</volume><issue>5</issue><spage>385</spage><epage>390</epage><pages>385-390</pages><issn>1673-1581</issn><eissn>1862-1783</eissn><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 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.</abstract><cop>Heidelberg</cop><pub>SP Zhejiang University Press</pub><pmid>18500778</pmid><doi>10.1631/jzus.B0820031</doi><tpages>6</tpages><oa>free_for_read</oa></addata></record> |
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subjects | Biochemistry Biomedical and Life Sciences Biomedicine Chromatography Chromatography, High Pressure Liquid - methods Drug Contamination Lisinopril - analysis Magnetic Resonance Spectroscopy Mass spectrometry NMR Nuclear magnetic resonance Spectrometry, Mass, Electrospray Ionization - methods 质谱分析 赖诺普利 高性能液体色谱法 |
title | Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry |
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