Article(id=1322246453880275242, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1322246421869346895, articleNumber=null, orderNo=null, doi=null, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=1617033600000, acceptedDateStr=2021-03-30, onlineDate=1793177720756, onlineDateStr=2026-10-28, pubDate=1624982400000, pubDateStr=2021-06-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793177720756, onlineIssueDateStr=2026-10-28, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793177720756, creator=13701087609, updateTime=1793177720756, updator=13701087609, issue=Issue{id=1322246421869346895, tenantId=1146029695717560320, journalId=1235980733773295621, year='2021', volume='30', issue='12', pageStart='1057', pageEnd='1152', issueExtLink='null', onlineDate='null', pubDate='1624982400000', pubDateStr='2021-06-30', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793177713123, creator='13701087609', updateTime=1793178158604, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322248290402414824, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1322246421869346895, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322248290402414825, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1322246421869346895, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1110, endPage=1116, ext={EN=ArticleExt(id=1322246454249373995, articleId=1322246453880275242, tenantId=1146029695717560320, journalId=1235980733773295621, language=EN, title=Identification of related substances in mesaconine by ultra-high performance liquid chromatography tandem mass spectrometry, columnId=null, journalTitle=Chinese Journal of New Drugs, columnName=null, runingTitle=null, highlight=null, articleAbstract=
Objective: To identify the related substances in mesaconine.
Methods: An HPLC-ELSD method was established using Gemini C18 column (150 mm×4.6 mm, 5 μm) with mobile phase composed of methanol-0.1% trifluoroacetic acid to separate the impurities. Forced degradation tests were designed and performed on mesaconine to specify the impurities. Ultra-high performance liquid chromatography tandem time-of-flight mass spectrometry (UPLC-TOF/MS) and triple quadrupole mass spectrometry (UPLC-MS/MS) were used for determination of exact mass and product ions of impurities. The structures of impurities and fragmentation regularity were then figured out.
Results: A total of four impurities were detected and identified in mesaconine, including three impurities derived from synthesis process and a degradation product.
Conclusion: UPLC-MS/MS technology can effectively separate and identify the impurities in mesaconine, and the results provide a valuable reference for the manufacturing process and quality control of mesaconine.
, authors=Xue-ting WU, Xiu-xiu LIU, Guang-sheng QIAN, Ruo-bing CHAO, authorsList=Xue-ting WU, Xiu-xiu LIU, Guang-sheng QIAN, Ruo-bing CHAO, authorCompany=null, correspAuthors=Xiu-xiu LIU, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1322246455004348716, articleId=1322246453880275242, tenantId=1146029695717560320, journalId=1235980733773295621, language=CN, title=UPLC-MS/MS法鉴定中乌宁的有关物质, columnId=1236330556003242277, journalTitle=中国新药杂志, columnName=实验研究, runingTitle=null, highlight=null, articleAbstract=
方法: 采用Gemini C18柱(150 mm×4.6 mm,5 μm),以甲醇-0.1%三氟乙酸水溶液(20∶80,v/v)为流动相,用蒸发光散射检测器(ELSD)进行有关物质检查;对中乌宁进行强制降解试验,归属杂质来源;采用超高效液相色谱-飞行时间质谱(UPLC-TOF/MS)测定各杂质的精确分子量,并应用三重四极杆串联质谱(UPLC-MS/MS)测定各杂质碎片离子的质荷比,推测其化学结构和裂解规律。
结果: 在中乌宁中共检出并鉴定了4个杂质,包括3个工艺杂质和1个降解杂质。
结论: 液相色谱-质谱联用技术能有效地分离、鉴定中乌宁的有关物质,鉴定结果为其质量控制和工艺优化提供参考。
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