Article(id=1239973079988891651, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239973077845603299, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-0076, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1706803200000, receivedDateStr=2024-02-02, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773562219855, onlineDateStr=2026-03-15, pubDate=1730304000000, pubDateStr=2024-10-31, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773562219855, onlineIssueDateStr=2026-03-15, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773562219855, creator=13701087609, updateTime=1773562219855, updator=13701087609, issue=Issue{id=1239973077845603299, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='10', pageStart='1647', pageEnd='1826', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773562219344, creator=13701087609, updateTime=1773563041495, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239976526251356920, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239973077845603299, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239976526251356921, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239973077845603299, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1816, endPage=1826, ext={EN=ArticleExt(id=1239973080261521427, articleId=1239973079988891651, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Content determination and quality evaluation of 18 components in Fengshiantai tablets based on UPLC-MS/MS technology and chemometrics*, columnId=1206272758774821315, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Standard Deliberation, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish an UPLC-MS/MS method to measure the content of 18 characteristic components in Fengshiantai tablets,and conduct chemometric analysis on the measurement results to provide a basis for quality control.

Methods:

The components were separated on Waters BEH C18 (100 mm×2.1 mm,1.7 μm) column with methanol and 0.1% formic acid aqueous solution as the mobile phase by gradient elution at a flow rate of 0.2 mL·min-1. The column temperature was set at 40 ℃. The injection volume was 1 μL. The detection was carried out by electrospray ionization(ESI),and electron spray ionization source was adopted in positive ion detection with multiple reaction monitoring mode(MRM).

Results:

The established methods showed a good linear relationship in a certain range (r≥0.998 3),whose average recovery rates of samples were 90.2%-101.7% with the RSD of 1.1%-4.9%. The content of ephedrine(calculated as ephedrine hydrochloride),chlorogenic acid,syringin,strychnine,brucine,berberine(calculated as berberine hydrochloride),naringin,cinnamaldehyde,ginsenoside Re,ginsenoside Rg1,epimedin C,icariin,asperosaponin Ⅵ,glycyrrhizic acid(calculated as glycyrrhizic acid ammonium salt),ginsenoside Rb1,notopterol,isoimperatorin in 39 batches of samples were 20.23-141.75 μg per tablet,10.50-121.69 μg per tablet,215.24-697.34 μg per tablet,8.46-42.42 μg per tablet,135.24-363.32 μg per tablet,91.29-242.87 μg per tablet,19.65-80.31 μg per tablet,22.57-105.05 μg per tablet,4.69-86.88 μg per tablet,10.32-241.15 μg per tablet,3.36-65.07 μg per tablet,10.79-390.69 μg per tablet,6.51-86.29 μg per tablet,4.10-89.75 μg per tablet,195.55-566.37 μg per tablet,96.98-448.95 μg per tablet,0-132.41 μg per tablet,7.09-232.71 μg per tablet. The results of chemometrics showed that 39 batches of samples from 5 production enterprises were classify into three categories,and there were certain differeces in sample quality among different production enterprises,eight differential markers(naringin,glycyrrhizic acid,isoimperatorin,berberine,syringin,ephedrine,pseudoephedrine,strychnine) that caused quality differences were found.

Conclusion:

The established method is simple and feasible,combined with chemometric methods,and can be used for quality evaluation of Fengshiantai tablets.

, correspAuthors=Jian SU, 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, authorCompany=null, fund=null, authors=null, authorsList=Yuan-yuan ZHANG, Hui-zhu SUN, Xiao-lei WANG, Rong LEI, Xue-li LIU, Jian SU), CN=ArticleExt(id=1239973082761326693, articleId=1239973079988891651, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=基于UPLC-MS/MS技术与化学计量学相结合的风湿安泰片中18个成分含量测定及质量评价研究*, columnId=1206272758971953622, journalTitle=药物分析杂志, columnName=标准研讨, runingTitle=null, highlight=null, articleAbstract=
目的:

建立UPLC-MS/MS法,同时测定风湿安泰片中18个特征性成分含量,并对测定结果进行化学计量学分析,为其质量控制提供依据。

方法:

采用Waters BEH C18 (100 mm×2.1 mm,1.7 μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.2 mL·min-1,柱温40 ℃,进样量1 μL;质谱采用电喷雾离子源(ESI),正离子检测,多反应监测(MRM)模式。

结果:

所建方法在一定范围内线性关系良好(r≥0.998 6),平均加样回收率为90.2%~101.7%,RSD为1.1%~4.9%。39批次样品中麻黄碱(以盐酸麻黄碱计)、伪麻黄碱(以盐酸伪麻黄碱计)、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱(以盐酸小檗碱计)、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、人参皂苷Rb1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸(以甘草酸铵计)、羌活醇、异欧前胡素的含量范围分别为20.23~141.75、10.50~121.69、215.24~697.34、8.46~42.42、135.24~363.32、91.29~242.87、19.65~80.31、22.57~105.05、4.69~86.88、10.32~241.15、3.36~65.07、10.79~390.69、6.51~86.29、4.10~89.75、195.55~566.37、96.98~448.95、0~132.41、7.09~232.71 μg·片-1。化学计量学结果显示,5个生产企业39批样品聚为3类,不同生产企业样品质量存在一定差异,筛选出影响质量的8个差异性标志物(柚皮苷、甘草酸、异欧前胡素、小檗碱、紫丁香苷、麻黄碱、伪麻黄碱、士的宁)。

结论:

建立的方法简单、可行,结合化学计量学方法,可用于风湿安泰片的质量评价。

, correspAuthors=苏建, authorNote=null, correspAuthorsNote=
** Tel:(0311)69086155;E-mail:
, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=D5giv4BFO5vTCV8ISJrmrQ==, magXml=0RMgon3akBqmbYc3eQhLKA==, pdfUrl=null, pdf=cvsjL6XNeVoGJD5w80vLjQ==, pdfFileSize=4924243, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=uoy+kwoaQ8rl7nhLaBSmIw==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=zxkYnxcsJ6jPU/CR8b9uZg==, mapNumber=null, authorCompany=null, fund=null, authors=

Tel:(0311)69086155;E-mail:

, authorsList=张元元, 孙慧珠, 王晓蕾, 雷蓉, 刘雪莉, 苏建)}, authors=[Author(id=1239977430945943999, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=270856189@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239977431046607301, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977430945943999, language=EN, stringName=Yuan-yuan ZHANG, firstName=Yuan-yuan, middleName=null, lastName=ZHANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977431155659213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977430945943999, language=CN, stringName=张元元, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=河北省药品医疗器械检验研究院,石家庄 050227, bio={"content":"

Tel:(0311)69086155;E-mail:

"}, bioImg=null, bioContent=

Tel:(0311)69086155;E-mail:

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])]), Author(id=1239977431264711125, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=1, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239977431352791515, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431264711125, language=EN, stringName=Hui-zhu SUN, firstName=Hui-zhu, middleName=null, lastName=SUN, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977431457649123, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431264711125, language=CN, stringName=孙慧珠, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=河北省药品医疗器械检验研究院,石家庄 050227, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])]), Author(id=1239977431533146599, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=2, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239977431629615602, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431533146599, language=EN, stringName=Xiao-lei WANG, firstName=Xiao-lei, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977431713501685, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431533146599, language=CN, stringName=王晓蕾, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=河北省药品医疗器械检验研究院,石家庄 050227, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])]), Author(id=1239977431809970681, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=3, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239977431914828289, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431809970681, language=EN, stringName=Rong LEI, firstName=Rong, middleName=null, lastName=LEI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977431981937158, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977431809970681, language=CN, stringName=雷蓉, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=河北省药品医疗器械检验研究院,石家庄 050227, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])]), Author(id=1239977432086794763, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=4, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239977433588355601, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977432086794763, language=EN, stringName=Xue-li LIU, firstName=Xue-li, middleName=null, lastName=LIU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977433689018903, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977432086794763, language=CN, stringName=刘雪莉, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=河北省药品医疗器械检验研究院,石家庄 050227, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])]), Author(id=1239977435635175964, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, orderNo=5, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=1083937623@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1239977435735839261, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977435635175964, language=EN, stringName=Jian SU, firstName=Jian, middleName=null, lastName=SU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239977435798753828, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, authorId=1239977435635175964, language=CN, stringName=苏建, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=河北省药品医疗器械检验研究院,石家庄 050227, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])])], keywords=[Keyword(id=1239977435979108911, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=1, keyword=Fengshiantai tablets), Keyword(id=1239977436100743733, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=2, keyword=UPLC-MS/MS), Keyword(id=1239977436184629818, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=3, keyword=characteristic components), Keyword(id=1239977436276904511, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=4, keyword=content determination), Keyword(id=1239977436369179207, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=5, keyword=chemometrics), Keyword(id=1239977436448870990, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=6, keyword=risk assessment), Keyword(id=1239977436541145683, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, orderNo=7, keyword=quality evaluation), Keyword(id=1239977438013346389, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=1, keyword=风湿安泰片), Keyword(id=1239977438134981212, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=2, keyword=液质联用), Keyword(id=1239977438231450210, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=3, keyword=特征性成分), Keyword(id=1239977438348890727, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=4, keyword=含量测定), Keyword(id=1239977438474719854, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=5, keyword=化学计量学), Keyword(id=1239977438604743286, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=6, keyword=风险评估), Keyword(id=1239977438768321151, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, orderNo=7, keyword=质量评价)], refs=[Reference(id=1239977440911610585, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=23, issue=11, pageStart=1982, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=刘东升, 刘婷婷, 姚世霞, journalName=中国现代中药, refType=null, unstructuredReference=刘东升,刘婷婷,姚世霞,等. 风湿关节炎片的质量标准提升研究[J].中国现代中药202123(11):1982, articleTitle=风湿关节炎片的质量标准提升研究, refAbstract=null), Reference(id=1239977441020662492, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=23, issue=11, pageStart=1982, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=1, authorNames=LIU DS, LIU TT, YAO SX, journalName=Mod Chin Med, refType=null, unstructuredReference=LIU DSLIU TTYAO SX,et al. Improvement of quality standard for Fengshi Guanjieyan tablets[J]. Mod Chin Med202123(11):1982, articleTitle=Improvement of quality standard for Fengshi Guanjieyan tablets, refAbstract=null), Reference(id=1239977442526417632, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2017, volume=36, issue=3, pageStart=98, pageEnd=null, url=null, language=null, rfNumber=[2], rfOrder=2, authorNames=王伟, journalName=内蒙古中医药, refType=null, unstructuredReference=王伟. 马钱子的炮制质量研究[J].内蒙古中医药201736(3):98, articleTitle=马钱子的炮制质量研究, refAbstract=null), Reference(id=1239977442656441060, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2017, volume=36, issue=3, pageStart=98, pageEnd=null, url=null, language=null, rfNumber=[2], rfOrder=3, authorNames=WANG W, journalName=Inner Mongolia J Tradit Chin Med, refType=null, unstructuredReference=WANG W. Preparation research of Strychnos nux-vomica L.[J]. Inner Mongolia J Tradit Chin Med201736(3):98, articleTitle=Preparation research of Strychnos nux-vomica L., refAbstract=null), Reference(id=1239977442748715753, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=34, issue=4, pageStart=191, pageEnd=null, url=null, language=null, rfNumber=[3], rfOrder=4, authorNames=张莉, 李莉, 杜冠华, journalName=中药药理与临床, refType=null, unstructuredReference=张莉,李莉,杜冠华.中药马钱子毒的历史认识与现代研究[J].中药药理与临床201834(4):191, articleTitle=中药马钱子毒的历史认识与现代研究, refAbstract=null), Reference(id=1239977442874544878, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=34, issue=4, pageStart=191, pageEnd=null, url=null, language=null, rfNumber=[3], rfOrder=5, authorNames=ZHANG L, LI L, DU GH, journalName=Pharmacol Clin Chin Mater Med, refType=null, unstructuredReference=ZHANG LLI LDU GH. Historical understanding and modern research on the toxicity of traditional Chinese medicine Strychni Semen[J]. Pharmacol Clin Chin Mater Med201834(4):191, articleTitle=Historical understanding and modern research on the toxicity of traditional Chinese medicine Strychni Semen, refAbstract=null), Reference(id=1239977442962625265, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=38, issue=10, pageStart=1824, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=6, authorNames=王菲菲, 张聿梅, 郑笑为, journalName=药物分析杂志, refType=null, unstructuredReference=王菲菲,张聿梅,郑笑为,等. 骨刺片中士的宁和马钱子碱含量测定方法的研究[J].药物分析杂志201838(10):1824, articleTitle=骨刺片中士的宁和马钱子碱含量测定方法的研究, refAbstract=null), Reference(id=1239977443059094261, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=38, issue=10, pageStart=1824, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=7, authorNames=WANG FF, ZHANG YM, ZHENG XW, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=WANG FFZHANG YMZHENG XW,et al. Study on assay method of brucine and strychnine in Guci tablets[J]. Chin J Pharm Anal201838(10):1824, articleTitle=Study on assay method of brucine and strychnine in Guci tablets, refAbstract=null), Reference(id=1239977443172340476, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=25, issue=1, pageStart=9, pageEnd=null, url=null, language=null, rfNumber=[5], rfOrder=8, authorNames=刘静, 于健东, 朱嘉亮, journalName=中国现代中药, refType=null, unstructuredReference=刘静,于健东,朱嘉亮,等. 2008—2021年国家药品抽检中成药质量分析[J].中国现代中药202325(1):9, articleTitle=2008—2021年国家药品抽检中成药质量分析, refAbstract=null), Reference(id=1239977443302363901, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=25, issue=1, pageStart=9, pageEnd=null, url=null, language=null, rfNumber=[5], rfOrder=9, authorNames=LIU J, YU JD, ZHU JL, journalName=Mod Chin Med, refType=null, unstructuredReference=LIU JYU JDZHU JL,et al. Quality analysis of Chinese patent medicines based on 2008—2021 national drug sampling inspection[J]. Mod Chin Med202325(1):9, articleTitle=Quality analysis of Chinese patent medicines based on 2008—2021 national drug sampling inspection, refAbstract=null), Reference(id=1239977443449164547, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=1990, volume=null, issue=null, pageStart=64, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=10, authorNames=null, journalName=null, refType=null, unstructuredReference=卫生部药品标准.第二十册[S]. 1990:64, articleTitle=null, refAbstract=null), Reference(id=1239977443570799366, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=1990, volume=null, issue=null, pageStart=64, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=11, authorNames=null, journalName=null, refType=null, unstructuredReference=Drug Specifications Promulgated by the Ministry of Public Health. PR China. Vol 20[S]. 1990:64, articleTitle=null, refAbstract=null), Reference(id=1239977443658879753, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=43, issue=6, pageStart=1156, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=12, authorNames=王亚丹, 戴忠, 孙彩林, journalName=中国中药杂志, refType=null, unstructuredReference=王亚丹,戴忠,孙彩林,等. UPLC-ELSD指纹图谱结合化学计量学方法用于骨刺片的质量控制[J].中国中药杂志201843(6):1156, articleTitle=UPLC-ELSD指纹图谱结合化学计量学方法用于骨刺片的质量控制, refAbstract=null), Reference(id=1239977443776320269, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2018, volume=43, issue=6, pageStart=1156, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=13, authorNames=WANG YD, DAI Z, SUN CL, journalName=China J Chin Mater Med, refType=null, unstructuredReference=WANG YDDAI ZSUN CL,et al. Quality control of Guci tablets using UPLC-ELSD fingerprint analysis coupled with chemometrics[J]. China J Chin Mater Med201843(6):1156, articleTitle=Quality control of Guci tablets using UPLC-ELSD fingerprint analysis coupled with chemometrics, refAbstract=null), Reference(id=1239977443910538004, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2019, volume=39, issue=4, pageStart=595, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=14, authorNames=王亚丹, 戴忠, 何凤艳, journalName=药物分析杂志, refType=null, unstructuredReference=王亚丹,戴忠,何凤艳,等. RRLC-MS/MS法同时测定骨刺片中14个成分的含量[J].药物分析杂志201939(4):595, articleTitle=RRLC-MS/MS法同时测定骨刺片中14个成分的含量, refAbstract=null), Reference(id=1239977444141224729, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2019, volume=39, issue=4, pageStart=595, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=15, authorNames=WANG YD, DAI Z, HE FY, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=WANG YDDAI ZHE FY,et al. Simultaneous determination of 14 compounds in Guci tablets using RRLC-MS/MS method[J]. Chin J Pharm Anal201939(4):595, articleTitle=Simultaneous determination of 14 compounds in Guci tablets using RRLC-MS/MS method, refAbstract=null), Reference(id=1239977444262859549, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=43, issue=3, pageStart=596, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=16, authorNames=陈玉华, 卢松, journalName=中成药, refType=null, unstructuredReference=陈玉华,卢松. UPLC-QQQ-MS/MS法同时测定风湿安泰片中12种成分[J].中成药202143(3):596, articleTitle=UPLC-QQQ-MS/MS法同时测定风湿安泰片中12种成分, refAbstract=null), Reference(id=1239977444346745631, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=43, issue=3, pageStart=596, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=17, authorNames=CHENG YH, LU S, journalName=Chin Tradit Pat Med, refType=null, unstructuredReference=CHENG YHLU S. Simultaneous determination of twelve constituents in Fengshiantai tablets by UPLC-QQQ-MS/MS[J]. Chin Tradit Pat Med202143(3):596, articleTitle=Simultaneous determination of twelve constituents in Fengshiantai tablets by UPLC-QQQ-MS/MS, refAbstract=null), Reference(id=1239977444443214624, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=44, issue=6, pageStart=1441, pageEnd=null, url=null, language=null, rfNumber=[10], rfOrder=18, authorNames=张婷, 陈斌, 刘利萍, journalName=中药材, refType=null, unstructuredReference=张婷,陈斌,刘利萍,等. UHPLC-ESI-MS/MS法测定烫骨碎补-续断药对中10个成分的含量[J].中药材202144(6):1441, articleTitle=UHPLC-ESI-MS/MS法测定烫骨碎补-续断药对中10个成分的含量, refAbstract=null), Reference(id=1239977444543877922, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2021, volume=44, issue=6, pageStart=1441, pageEnd=null, url=null, language=null, rfNumber=[10], rfOrder=19, authorNames=ZHANG T, CHEN B, LIU LP, journalName=J Chin Med Mater, refType=null, unstructuredReference=ZHANG TCHEN BLIU LP,et al. Determination of the content of 10 components in the couplet medicines of burning Drynariae Rhizoma and Dipsaci Radix by UHPLC-ESI-MS/MS[J]. J Chin Med Mater202144(6):1441, articleTitle=Determination of the content of 10 components in the couplet medicines of burning Drynariae Rhizoma and Dipsaci Radix by UHPLC-ESI-MS/MS, refAbstract=null), Reference(id=1239977444623569701, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=43, issue=9, pageStart=1612, pageEnd=null, url=null, language=null, rfNumber=[11], rfOrder=20, authorNames=李沁, 张聪, 陈亮, journalName=药物分析杂志, refType=null, unstructuredReference=李沁,张聪,陈亮,等.基于超高效液相色谱指纹图谱、多指标成分定量及化学计量学的小儿感冒颗粒质量评价[J].药物分析杂志202343(9):1612, articleTitle=基于超高效液相色谱指纹图谱、多指标成分定量及化学计量学的小儿感冒颗粒质量评价, refAbstract=null), Reference(id=1239977444699067176, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=43, issue=9, pageStart=1612, pageEnd=null, url=null, language=null, rfNumber=[11], rfOrder=21, authorNames=LI Q, ZHANG C, CHEN L, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=LI QZHANG CCHEN L,et al. Quality evaluation of Xiao’er Ganmao granules based on UPLC fingerprint,multi-component determination,and chemometric analysis[J]. Chin J Pharm Anal202343(9):1612, articleTitle=Quality evaluation of Xiao’er Ganmao granules based on UPLC fingerprint,multi-component determination,and chemometric analysis, refAbstract=null), Reference(id=1239977444778758956, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=54, issue=21, pageStart=7034, pageEnd=null, url=null, language=null, rfNumber=[12], rfOrder=22, authorNames=曹春琪, 孙慧珠, 赵振霞, journalName=中草药, refType=null, unstructuredReference=曹春琪,孙慧珠,赵振霞,等.基于UHPLC-MS/MS技术的导赤丸中24个成分定量测定联合化学计量学质量评价[J].中草药202354(21):7034, articleTitle=基于UHPLC-MS/MS技术的导赤丸中24个成分定量测定联合化学计量学质量评价, refAbstract=null), Reference(id=1239977444850062129, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=54, issue=21, pageStart=7034, pageEnd=null, url=null, language=null, rfNumber=[12], rfOrder=23, authorNames=CAO CQ, SUN HZ, ZHAO ZX, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=CAO CQSUN HZZHAO ZX,et al. Quantitative determination of 24 components in Daochi pills based on UHPLC-MS/MS technology combined with chemometrics quality evaluation[J]. Chin Tradit Herb Drugs202354(21):7034, articleTitle=Quantitative determination of 24 components in Daochi pills based on UHPLC-MS/MS technology combined with chemometrics quality evaluation, refAbstract=null), Reference(id=1239977444925559604, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=54, issue=19, pageStart=6452, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=24, authorNames=任慧, 胡静, 崔小敏, journalName=中草药, refType=null, unstructuredReference=任慧,胡静,崔小敏,等.基于指纹图谱结合化学模式识别及多酚类成分含量测定的大盘龙七质量评价[J].中草药202354(19):6452, articleTitle=基于指纹图谱结合化学模式识别及多酚类成分含量测定的大盘龙七质量评价, refAbstract=null), Reference(id=1239977445013639988, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=54, issue=19, pageStart=6452, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=25, authorNames=REN H, HU J, CUI XM, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=REN HHU JCUI XM,et al. Quality evaluation of Bergeniae Scopulosae Rhizoma based on fingerprints combination with chemical pattern recognition and content determination of phenolic compounds[J]. Chin Tradit Herb Drugs202354(19):6452, articleTitle=Quality evaluation of Bergeniae Scopulosae Rhizoma based on fingerprints combination with chemical pattern recognition and content determination of phenolic compounds, refAbstract=null), Reference(id=1239977445105914681, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2024, volume=54, issue=2, pageStart=1, pageEnd=null, url=null, language=null, rfNumber=[14], rfOrder=26, authorNames=籍学伟, 陈备尧, 白妍, journalName=中草药, refType=null, unstructuredReference=籍学伟,陈备尧,白妍,等.基于HPLC指纹图谱和多成分含量测定结合化学计量学的暖宫七味丸质量评价研究[J].中草药202454(2):1, articleTitle=基于HPLC指纹图谱和多成分含量测定结合化学计量学的暖宫七味丸质量评价研究, refAbstract=null), Reference(id=1239977445210772285, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2024, volume=54, issue=2, pageStart=1, pageEnd=null, url=null, language=null, rfNumber=[14], rfOrder=27, authorNames=JI XW, CHEN BY, BAI Y, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=JI XWCHEN BYBAI Y,et al. Quality evaluation of Nuangong Qiwei pills by HPLC fingerprint and multi-component content determination combined with chemometrics[J]. Chin Tradit Herb Drugs202454(2):1, articleTitle=Quality evaluation of Nuangong Qiwei pills by HPLC fingerprint and multi-component content determination combined with chemometrics, refAbstract=null), Reference(id=1239977445294658368, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=45, issue=9, pageStart=2846, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=28, authorNames=于密密, 王安琪, 杜小伟, journalName=中成药, refType=null, unstructuredReference=于密密,王安琪,杜小伟,等.基于HPLC指纹图谱结合化学计量学的痢泻灵片质量评价[J].中成药202345(9):2846, articleTitle=基于HPLC指纹图谱结合化学计量学的痢泻灵片质量评价, refAbstract=null), Reference(id=1239977445386933058, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=45, issue=9, pageStart=2846, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=29, authorNames=YU MM, WANG AQ, DU XW, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=YU MMWANG AQDU XW,et al. Quality evaluation of Lixieling tablets based on combinative methods of HPLC fingerprint,quantitative analysis of multi-components and chemometrics analysis[J]. Chin Tradit Herb Drugs202345(9):2846, articleTitle=Quality evaluation of Lixieling tablets based on combinative methods of HPLC fingerprint,quantitative analysis of multi-components and chemometrics analysis, refAbstract=null), Reference(id=1239977445475013446, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2022, volume=12, issue=7, pageStart=1659, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=30, authorNames=RAMZAN M, GOURION-ARSIQUAUD S, HUSSAIN A, journalName=Drug Deliv Transl Res, refType=null, unstructuredReference=RAMZAN MGOURION-ARSIQUAUD SHUSSAIN A,et al. In vitro release,ex vivo penetration,and in vivo dermatokinetics of ketoconazole-loaded solid lipid nanoparticles for topical delivery[J]. Drug Deliv Transl Res202212(7):1659, articleTitle=In vitro release,ex vivo penetration,and in vivo dermatokinetics of ketoconazole-loaded solid lipid nanoparticles for topical delivery, refAbstract=null), Reference(id=1239977446968185674, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2022, volume=53, issue=10, pageStart=3000, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=31, authorNames=郭玉岩, 高滔, 李春城, journalName=中草药, refType=null, unstructuredReference=郭玉岩,高滔,李春城,等. 酸碱药对甘草-马钱子配伍汤液沉积相态解放特性研究[J].中草药202253(10):3000, articleTitle=酸碱药对甘草-马钱子配伍汤液沉积相态解放特性研究, refAbstract=null), Reference(id=1239977447039488844, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2022, volume=53, issue=10, pageStart=3000, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=32, authorNames=GUO YY, GAO T, LI CC, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=GUO YYGAO TLI CC,et al. Release characteristics of principal components of acid-base drug pair Glycyrrhizae Radix et Rhizoma-Strychni Semen compatibility decoction in sedimentary phase[J]. Chin Tradit Herb Drugs202253(10):3000, articleTitle=Release characteristics of principal components of acid-base drug pair Glycyrrhizae Radix et Rhizoma-Strychni Semen compatibility decoction in sedimentary phase, refAbstract=null), Reference(id=1239977447123374929, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=45, issue=8, pageStart=2718, pageEnd=null, url=null, language=null, rfNumber=[18], rfOrder=33, authorNames=马俊, 曼琼, 闫潇, journalName=中成药, refType=null, unstructuredReference=马俊,曼琼,闫潇,等. 野生与栽培甘草对马钱子致肝毒性的解毒作用[J].中成药202345(8):2718, articleTitle=野生与栽培甘草对马钱子致肝毒性的解毒作用, refAbstract=null), Reference(id=1239977447224038228, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, doi=null, pmid=null, pmcid=null, year=2023, volume=45, issue=8, pageStart=2718, pageEnd=null, url=null, language=null, rfNumber=[18], rfOrder=34, authorNames=MA J, MAN Q, YAN X, journalName=Chin Tradit Pat Med, refType=null, unstructuredReference=MA JMAN QYAN X,et al. Detoxification effect of wild and cultivated Glycyrrhizae Radix et Rhizoma on the hepatotoxicity caused by Strychni Semen[J]. Chin Tradit Pat Med202345(8):2718, articleTitle=Detoxification effect of wild and cultivated Glycyrrhizae Radix et Rhizoma on the hepatotoxicity caused by Strychni Semen, refAbstract=null)], funds=[Fund(id=1239977440710283985, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, awardId=2023ZC1018, language=CN, fundingSource=*河北省药品监督管理局科技计划项目(2023ZC1018), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239977430832697781, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, xref=null, ext=[AuthorCompanyExt(id=1239977430836892088, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1239977430845280695, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, companyId=1239977430832697781, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=河北省药品医疗器械检验研究院,石家庄 050227)])], figs=[ArticleFig(id=1239977439011590798, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Fig.1, caption=Extraction MRM chromatograms of negative sample(A),mixed reference substances(B) and sample(C), figureFileSmall=F7TMdISSB7K4L8Kh/KgfhA==, figureFileBig=4AFJaBaTzbI9TXmAD0bzPw==, tableContent=null), ArticleFig(id=1239977439099671186, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=图1, caption=阴性样品(A)、混合对照品(B)和样品(C)的MRM提取离子流图

1.麻黄碱(ephedrine) 2.伪麻黄碱(pseudoephedrine) 3.绿原酸(chlorogenic acid) 4.紫丁香苷(syringin) 5.士的宁(strychnine) 6.马钱子碱(brucin) 7.小檗碱(berberine) 8.柚皮苷(naringin) 9.桂皮醛(cinnamaldehyde) 10.人参皂苷Re(ginsenoside Re) 11.人参皂苷Rg1(ginsenoside Rg1) 12.朝藿定C(epimedin C) 13.淫羊藿苷(icariin) 14.川续断皂苷Ⅵ(asperosaponin Ⅵ) 15.甘草酸(glycyrrhizic acid) 16.人参皂苷Rb1(ginsenoside Rb1) 17.羌活醇(notopterol) 18.异欧前胡素(isoimperatorin)

, figureFileSmall=F7TMdISSB7K4L8Kh/KgfhA==, figureFileBig=4AFJaBaTzbI9TXmAD0bzPw==, tableContent=null), ArticleFig(id=1239977439200334487, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Fig.2, caption=HCA of 39 samples of Fengshiantai tablets, figureFileSmall=9Iwlv0ZldvYMjX22WaWRRg==, figureFileBig=tzLlhIC1LKSUT4Q6hAK4pQ==, tableContent=null), ArticleFig(id=1239977439275831962, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=图2, caption=39批风湿安泰片样品的HCA, figureFileSmall=9Iwlv0ZldvYMjX22WaWRRg==, figureFileBig=tzLlhIC1LKSUT4Q6hAK4pQ==, tableContent=null), ArticleFig(id=1239977439363912351, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Fig.3, caption=OPLS-DA scatter plot of 39 samples of Fengshiantai tablets, figureFileSmall=DTKoa2bMJktsYObDod/WRQ==, figureFileBig=2mHr7K41izTlPgUUjpUo/w==, tableContent=null), ArticleFig(id=1239977439447798437, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=图3, caption=39批风湿安泰片样品的OPLS-DA得分图, figureFileSmall=DTKoa2bMJktsYObDod/WRQ==, figureFileBig=2mHr7K41izTlPgUUjpUo/w==, tableContent=null), ArticleFig(id=1239977439514907304, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Fig.4, caption=VIP score plot of 18 components in Fengshiantai tablets, figureFileSmall=f1sszjzVhVjBIYFVf6fE8Q==, figureFileBig=Zkdd9c4IT+GpBRbzBFTIGw==, tableContent=null), ArticleFig(id=1239977439615570604, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=图4, caption=风湿安泰片中18个成分的VIP得分图, figureFileSmall=f1sszjzVhVjBIYFVf6fE8Q==, figureFileBig=Zkdd9c4IT+GpBRbzBFTIGw==, tableContent=null), ArticleFig(id=1239977439737205425, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Tab.1, caption=

MS parameters of 18 components in Fengshiantai tablets

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)
tR/min母离子
(parent ion)m/z
子离子
(daughter ion)m/z
锥孔电压
(cone voltage)/V
碰撞电压
(collision voltage)/V
麻黄碱(ephedrine)9.63166.5148.52015
伪麻黄碱(pseudoephedrine)10.13166.5148.52015
绿原酸(chlorogenic acid)11.42355.2163.52015
紫丁香苷(syringin)11.79395.4232.82020
士的宁(strychnine)11.87335.5223.42030
马钱子碱(brucin)12.18395.5324.52035
小檗碱(berberine)14.13335.9306.02025
柚皮苷(naringin)14.31581.5272.92030
桂皮醛(cinnamaldehyde)15.61133.155.12010
人参皂苷Re(ginsenoside Re)16.37969.8790.12045
人参皂苷Rg1(ginsenoside Rg116.48823.6203.12040
朝藿定C(epimedin C)16.87823.5369.92065
淫羊藿苷(icariin)16.88677.6369.02030
川续断皂苷Ⅵ(asperosaponin Ⅵ)18.25952.0259.52060
甘草酸(glycyrrhizic acid)18.99823.5453.32025
人参皂苷Rb1(ginsenoside Rb119.071131.7365.12030
羌活醇(notopterol)19.18377.1225.02020
异欧前胡素(isoimperatorin)19.32271.5147.42035
), ArticleFig(id=1239977439837868723, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=表1, caption=

风湿安泰片中18个成分的质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)
tR/min母离子
(parent ion)m/z
子离子
(daughter ion)m/z
锥孔电压
(cone voltage)/V
碰撞电压
(collision voltage)/V
麻黄碱(ephedrine)9.63166.5148.52015
伪麻黄碱(pseudoephedrine)10.13166.5148.52015
绿原酸(chlorogenic acid)11.42355.2163.52015
紫丁香苷(syringin)11.79395.4232.82020
士的宁(strychnine)11.87335.5223.42030
马钱子碱(brucin)12.18395.5324.52035
小檗碱(berberine)14.13335.9306.02025
柚皮苷(naringin)14.31581.5272.92030
桂皮醛(cinnamaldehyde)15.61133.155.12010
人参皂苷Re(ginsenoside Re)16.37969.8790.12045
人参皂苷Rg1(ginsenoside Rg116.48823.6203.12040
朝藿定C(epimedin C)16.87823.5369.92065
淫羊藿苷(icariin)16.88677.6369.02030
川续断皂苷Ⅵ(asperosaponin Ⅵ)18.25952.0259.52060
甘草酸(glycyrrhizic acid)18.99823.5453.32025
人参皂苷Rb1(ginsenoside Rb119.071131.7365.12030
羌活醇(notopterol)19.18377.1225.02020
异欧前胡素(isoimperatorin)19.32271.5147.42035
), ArticleFig(id=1239977439946920628, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Tab.2, caption=

Results of linear regression of the investigated compounds

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/(μg·mL-1
麻黄碱(ephedrine)Y=5.605×109X-2.077×1040.999 60.025~2.591
伪麻黄碱(pseudoephedrine)Y=9.751×109X+2.592×1050.999 10.017~1.723
绿原酸(chlorogenic acid)Y=8.766×108X +2.921×1040.999 30.141~14.122
紫丁香苷(syringin)Y=1.830×108X+1.324×1040.999 30.008~0.835
士的宁(strychnine)Y=7.917×107X+1.667×1040.999 50.009~8.892
马钱子碱(brucin)Y=4.389×109X +8.945×1050.999 40.065~6.538
小檗碱(berberine)Y=1.210×1010X-1.584×1040.999 70.022~2.191
柚皮苷(naringin)Y=2.233×108X+111.6770.999 50.029~2.901
桂皮醛(cinnamaldehyde)Y=8.192×108X-4.798×1030.998 60.019~1.938
人参皂苷Re(ginsenoside Re)Y=3.721×108X-1.065×1040.999 70.040~4.047
人参皂苷Rg1(ginsenoside Rg1Y=1.088×109X+6.305×1030.999 20.008~0.856
朝藿定C(epimedin C)Y=3.201×107X-59.2890.999 70.023~2.281
淫羊藿苷(icariin)Y=9.033×109X+8.958×1050.999 10.020~2.072
川续断皂苷Ⅵ(asperosaponin Ⅵ)Y=9.646×107X+8.109×1030.999 70.093~9.283
甘草酸(glycyrrhizic acid)Y=6.069×108X+7.680×1040.999 80.089~8.855
人参皂苷Rb1(ginsenoside Rb1Y=1.493×107X-650.9260.999 80.059~5.961
羌活醇(notopterol)Y=1.642×109X+3.758×1040.999 60.010~1.078
异欧前胡素(isoimperatorin)Y=4.394×109X+3.893×1050.998 90.033~3.256
), ArticleFig(id=1239977440060166841, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=表2, caption=

各待测成分线性关系考察结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/(μg·mL-1
麻黄碱(ephedrine)Y=5.605×109X-2.077×1040.999 60.025~2.591
伪麻黄碱(pseudoephedrine)Y=9.751×109X+2.592×1050.999 10.017~1.723
绿原酸(chlorogenic acid)Y=8.766×108X +2.921×1040.999 30.141~14.122
紫丁香苷(syringin)Y=1.830×108X+1.324×1040.999 30.008~0.835
士的宁(strychnine)Y=7.917×107X+1.667×1040.999 50.009~8.892
马钱子碱(brucin)Y=4.389×109X +8.945×1050.999 40.065~6.538
小檗碱(berberine)Y=1.210×1010X-1.584×1040.999 70.022~2.191
柚皮苷(naringin)Y=2.233×108X+111.6770.999 50.029~2.901
桂皮醛(cinnamaldehyde)Y=8.192×108X-4.798×1030.998 60.019~1.938
人参皂苷Re(ginsenoside Re)Y=3.721×108X-1.065×1040.999 70.040~4.047
人参皂苷Rg1(ginsenoside Rg1Y=1.088×109X+6.305×1030.999 20.008~0.856
朝藿定C(epimedin C)Y=3.201×107X-59.2890.999 70.023~2.281
淫羊藿苷(icariin)Y=9.033×109X+8.958×1050.999 10.020~2.072
川续断皂苷Ⅵ(asperosaponin Ⅵ)Y=9.646×107X+8.109×1030.999 70.093~9.283
甘草酸(glycyrrhizic acid)Y=6.069×108X+7.680×1040.999 80.089~8.855
人参皂苷Rb1(ginsenoside Rb1Y=1.493×107X-650.9260.999 80.059~5.961
羌活醇(notopterol)Y=1.642×109X+3.758×1040.999 60.010~1.078
异欧前胡素(isoimperatorin)Y=4.394×109X+3.893×1050.998 90.033~3.256
), ArticleFig(id=1239977440135664317, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Tab.3, caption=

Contents of 18 components in Fengshiantai tablets(μg per tablet)

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
麻黄碱
(ephedrine)
伪麻黄碱
(pseudoephedrine)
绿原酸
(chlorogenic acid)
紫丁香苷
(syringin)
士的宁
(strychnine)
马钱子碱
(brucin)
小檗碱
(berberine)
柚皮苷
(naringin)
桂皮醛
(cinnamaldehyde)
S184.1559.78548.9936.78294.46226.5533.2386.508.74
S287.4161.84529.9638.52292.17230.2234.6386.807.61
S3102.4069.65543.7730.81296.96224.4151.01105.0517.16
S485.1460.71545.7235.56299.38229.1037.3197.746.21
S5103.8357.18665.3336.90305.01166.7934.3768.2619.27
S694.2264.04572.8133.51293.00226.1933.1778.637.55
S788.2966.92566.9132.06308.56236.8938.5837.456.72
S888.6060.25509.9028.43290.80230.6045.4361.648.99
S9113.5968.20610.7728.42285.86178.2342.0163.5916.19
S1066.0132.75487.8018.44273.11213.4865.2643.8715.86
S1175.7810.50448.538.85177.66197.3334.6438.0515.81
S12135.4164.28609.5129.86265.59242.8780.3170.3518.62
S1357.4932.51551.5217.07289.89219.3568.6443.8218.70
S1459.5237.81585.9410.50331.81183.2056.6538.075.74
S1546.5232.50555.5812.42338.94188.1140.4872.327.51
S1666.3350.40433.5918.34290.63199.4728.8422.577.62
S1759.3242.41603.4912.83363.32203.4540.1358.794.69
S1862.9643.04697.3413.15330.11222.2030.4040.484.75
S1953.8435.49599.9610.85315.91210.9851.2129.145.51
S2067.9637.63545.2418.32184.16211.1037.8345.7519.40
S2167.5639.15562.9216.10190.79207.1237.1149.2719.64
S2241.6132.21580.698.46328.46188.9638.1470.696.14
S2327.4125.05215.2411.41142.57104.1928.0248.8964.29
S2428.4126.94233.4213.60161.83116.3633.3347.8586.88
S2520.2320.04245.1714.85141.7391.2921.2837.9067.72
S2649.7550.63253.7820.23160.43106.9041.4454.8132.84
S2750.0251.75259.6219.74177.81117.3947.3359.0830.17
S2831.2931.05227.7417.89148.8696.8226.2930.6536.64
S2929.9931.27243.3119.04145.1493.2321.0329.6033.76
S3039.3238.37242.4719.73161.21106.4944.1748.7828.23
S3128.9429.72238.0516.74141.6592.3619.6529.9341.24
S32131.1865.82390.0742.42135.24194.0938.2744.887.49
S33100.5238.64359.9425.23136.54182.7333.9638.278.36
S34113.8658.47384.6040.32143.03198.6235.2140.397.56
S35122.90108.39417.8630.57214.12159.3542.3747.625.23
S36128.73114.61427.6133.07219.32157.6543.4353.125.45
S37116.4567.32402.3832.47176.14185.7335.3747.156.88
S38141.75121.69486.3727.27201.33161.0331.1948.796.13
S39118.2877.49410.4432.52143.10186.5921.4953.176.43
序号
(No.)
人参皂苷Rg1
(ginsenoside Rg1
人参皂苷Re
(ginsenoside Re)
朝藿定C
(epimedin C)
淫羊藿苷
(icariin)
川续断皂苷Ⅵ
(asperosaponin Ⅵ)
甘草酸
(glycyrrhizic acid)
羌活醇
(notopterol)
异欧前胡素
(isoimperatorin)
人参皂苷Rb1
(ginsenoside Rb1
S15.5414.7257.5585.38363.26411.671.6714.0019.94
S25.5016.8851.9186.43370.51412.432.6217.2926.74
S38.5861.4355.9485.33467.28322.753.6566.3570.56
S45.3910.3252.6683.85368.14448.951.8012.5413.59
S519.19171.4644.7876.76502.96323.713.1163.14188.73
S63.3628.0355.7180.95317.68269.671.9651.1738.25
S77.3713.9255.8586.71381.14283.872.2734.1910.79
S830.66147.9086.2974.42349.10335.5037.51111.90127.30
S930.05117.7344.0467.52407.82322.902.3763.47118.26
S1021.6721.1439.6069.89508.44367.609.4962.8933.45
S1117.0918.4046.8473.51387.94348.533.7068.8622.83
S1239.81112.3467.3089.75278.29365.96132.41108.3138.93
S1322.3523.0846.3469.29566.37347.479.7059.6319.68
S1441.6140.2072.1454.17295.94145.236.72205.74124.16
S1536.5438.4760.5739.80197.53163.287.08229.5999.80
S1635.5238.4950.1046.68309.43187.6026.34194.88102.00
S1736.8338.2866.2244.20195.55133.024.22231.63107.49
S1832.5338.3423.8635.56372.23136.755.17203.9679.49
S1931.0239.2964.3749.66322.69118.815.74221.1074.42
S2020.13120.7350.0341.02442.22157.845.12228.21390.69
S2120.05115.6246.0840.92459.80139.625.30232.71346.62
S2230.2238.9754.6138.79222.70127.507.29232.3266.07
S2332.24195.606.514.10380.6596.980.007.0975.87
S2442.07235.296.924.73379.77132.980.0012.52128.21
S2522.26117.716.899.54360.45196.080.0021.8370.04
S2654.76238.8511.329.26362.80246.860.0013.48232.89
S2760.41241.1513.2610.54328.28282.640.0013.83283.05
S2862.67198.929.8613.23344.32243.580.0010.68246.08
S2965.07229.5312.1011.07335.36228.280.0013.62304.85
S3059.08193.1110.3613.33236.17278.600.0024.26285.24
S3155.09167.067.109.90324.60244.040.0016.67266.93
S3213.9042.7053.9459.06422.89205.472.9813.4723.59
S339.6131.9038.9545.26331.53189.361.7411.1622.70
S3413.9441.4964.6458.01393.96252.232.7612.5937.14
S3512.7948.4120.0462.46374.79248.2714.1931.3848.51
S3613.9048.9520.0165.53386.37280.1315.0124.3756.84
S3713.9541.4948.6058.20385.64289.305.9815.8337.43
S389.6343.7114.1757.97359.44185.8111.4827.3338.93
S3912.4742.7941.2246.52290.57179.212.8643.0635.54
), ArticleFig(id=1239977440316019394, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=表3, caption=

风湿安泰片中18种成分的含量(μg·片-1

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
麻黄碱
(ephedrine)
伪麻黄碱
(pseudoephedrine)
绿原酸
(chlorogenic acid)
紫丁香苷
(syringin)
士的宁
(strychnine)
马钱子碱
(brucin)
小檗碱
(berberine)
柚皮苷
(naringin)
桂皮醛
(cinnamaldehyde)
S184.1559.78548.9936.78294.46226.5533.2386.508.74
S287.4161.84529.9638.52292.17230.2234.6386.807.61
S3102.4069.65543.7730.81296.96224.4151.01105.0517.16
S485.1460.71545.7235.56299.38229.1037.3197.746.21
S5103.8357.18665.3336.90305.01166.7934.3768.2619.27
S694.2264.04572.8133.51293.00226.1933.1778.637.55
S788.2966.92566.9132.06308.56236.8938.5837.456.72
S888.6060.25509.9028.43290.80230.6045.4361.648.99
S9113.5968.20610.7728.42285.86178.2342.0163.5916.19
S1066.0132.75487.8018.44273.11213.4865.2643.8715.86
S1175.7810.50448.538.85177.66197.3334.6438.0515.81
S12135.4164.28609.5129.86265.59242.8780.3170.3518.62
S1357.4932.51551.5217.07289.89219.3568.6443.8218.70
S1459.5237.81585.9410.50331.81183.2056.6538.075.74
S1546.5232.50555.5812.42338.94188.1140.4872.327.51
S1666.3350.40433.5918.34290.63199.4728.8422.577.62
S1759.3242.41603.4912.83363.32203.4540.1358.794.69
S1862.9643.04697.3413.15330.11222.2030.4040.484.75
S1953.8435.49599.9610.85315.91210.9851.2129.145.51
S2067.9637.63545.2418.32184.16211.1037.8345.7519.40
S2167.5639.15562.9216.10190.79207.1237.1149.2719.64
S2241.6132.21580.698.46328.46188.9638.1470.696.14
S2327.4125.05215.2411.41142.57104.1928.0248.8964.29
S2428.4126.94233.4213.60161.83116.3633.3347.8586.88
S2520.2320.04245.1714.85141.7391.2921.2837.9067.72
S2649.7550.63253.7820.23160.43106.9041.4454.8132.84
S2750.0251.75259.6219.74177.81117.3947.3359.0830.17
S2831.2931.05227.7417.89148.8696.8226.2930.6536.64
S2929.9931.27243.3119.04145.1493.2321.0329.6033.76
S3039.3238.37242.4719.73161.21106.4944.1748.7828.23
S3128.9429.72238.0516.74141.6592.3619.6529.9341.24
S32131.1865.82390.0742.42135.24194.0938.2744.887.49
S33100.5238.64359.9425.23136.54182.7333.9638.278.36
S34113.8658.47384.6040.32143.03198.6235.2140.397.56
S35122.90108.39417.8630.57214.12159.3542.3747.625.23
S36128.73114.61427.6133.07219.32157.6543.4353.125.45
S37116.4567.32402.3832.47176.14185.7335.3747.156.88
S38141.75121.69486.3727.27201.33161.0331.1948.796.13
S39118.2877.49410.4432.52143.10186.5921.4953.176.43
序号
(No.)
人参皂苷Rg1
(ginsenoside Rg1
人参皂苷Re
(ginsenoside Re)
朝藿定C
(epimedin C)
淫羊藿苷
(icariin)
川续断皂苷Ⅵ
(asperosaponin Ⅵ)
甘草酸
(glycyrrhizic acid)
羌活醇
(notopterol)
异欧前胡素
(isoimperatorin)
人参皂苷Rb1
(ginsenoside Rb1
S15.5414.7257.5585.38363.26411.671.6714.0019.94
S25.5016.8851.9186.43370.51412.432.6217.2926.74
S38.5861.4355.9485.33467.28322.753.6566.3570.56
S45.3910.3252.6683.85368.14448.951.8012.5413.59
S519.19171.4644.7876.76502.96323.713.1163.14188.73
S63.3628.0355.7180.95317.68269.671.9651.1738.25
S77.3713.9255.8586.71381.14283.872.2734.1910.79
S830.66147.9086.2974.42349.10335.5037.51111.90127.30
S930.05117.7344.0467.52407.82322.902.3763.47118.26
S1021.6721.1439.6069.89508.44367.609.4962.8933.45
S1117.0918.4046.8473.51387.94348.533.7068.8622.83
S1239.81112.3467.3089.75278.29365.96132.41108.3138.93
S1322.3523.0846.3469.29566.37347.479.7059.6319.68
S1441.6140.2072.1454.17295.94145.236.72205.74124.16
S1536.5438.4760.5739.80197.53163.287.08229.5999.80
S1635.5238.4950.1046.68309.43187.6026.34194.88102.00
S1736.8338.2866.2244.20195.55133.024.22231.63107.49
S1832.5338.3423.8635.56372.23136.755.17203.9679.49
S1931.0239.2964.3749.66322.69118.815.74221.1074.42
S2020.13120.7350.0341.02442.22157.845.12228.21390.69
S2120.05115.6246.0840.92459.80139.625.30232.71346.62
S2230.2238.9754.6138.79222.70127.507.29232.3266.07
S2332.24195.606.514.10380.6596.980.007.0975.87
S2442.07235.296.924.73379.77132.980.0012.52128.21
S2522.26117.716.899.54360.45196.080.0021.8370.04
S2654.76238.8511.329.26362.80246.860.0013.48232.89
S2760.41241.1513.2610.54328.28282.640.0013.83283.05
S2862.67198.929.8613.23344.32243.580.0010.68246.08
S2965.07229.5312.1011.07335.36228.280.0013.62304.85
S3059.08193.1110.3613.33236.17278.600.0024.26285.24
S3155.09167.067.109.90324.60244.040.0016.67266.93
S3213.9042.7053.9459.06422.89205.472.9813.4723.59
S339.6131.9038.9545.26331.53189.361.7411.1622.70
S3413.9441.4964.6458.01393.96252.232.7612.5937.14
S3512.7948.4120.0462.46374.79248.2714.1931.3848.51
S3613.9048.9520.0165.53386.37280.1315.0124.3756.84
S3713.9541.4948.6058.20385.64289.305.9815.8337.43
S389.6343.7114.1757.97359.44185.8111.4827.3338.93
S3912.4742.7941.2246.52290.57179.212.8643.0635.54
), ArticleFig(id=1239977440412488391, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=EN, label=Tab.4, caption=

Initial eigenvalue and variance contribution rate of principal components

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
初始特征值
(initial eigenvalue)
方差贡献率
(variance conturbution rate)/%
累积贡献率
(cumulative variance contribution rate)/%
17.55241.95341.953
23.25618.08760.040
31.7169.53369.573
41.3417.45277.025
51.0755.97583.000
), ArticleFig(id=1239977440496374472, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239973079988891651, language=CN, label=表4, caption=

主成分的初始特征值和方差贡献率

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
初始特征值
(initial eigenvalue)
方差贡献率
(variance conturbution rate)/%
累积贡献率
(cumulative variance contribution rate)/%
17.55241.95341.953
23.25618.08760.040
31.7169.53369.573
41.3417.45277.025
51.0755.97583.000
)], attaches=null, journal=Journal(id=1205114436974182403, delFlag=0, nameCn=药物分析杂志, nameEn=Chinese Journal of Pharmaceutical Analysis, nameHistory1=null, nameHistory2=null, issn=0254-1793, eissn=, cn=11-2224/R, coden=null, periodic=月刊, language=CN, oaType=1, ccby=null, superviseOffice=null, ownerOffice=null, pubOffice=null, editorOffice=null, officeType=null, aims=null, clcCode=null, officeProv=null, officeCity=null, officeAddr=null, officeZip=null, officeEmail=, officePhone=, editDirector=null, officeDirector=null, officeDirectorPhone=null, officeStaffNum=null, officeEmpNum=null, coverPicUrl=E+iq5BU+frOtpo6YF6JpQQ==, journalPrice=null, startedYear=null, abbrevIsoEn=Chinese Journal of Pharmaceutical Analysis, journalRemark=null, publicationField=null, createdTime=1765251271721, updatedTime=1765252167692, createdBy=18614031015, updatedBy=13701087609, firstLetterCn=C, firstLetterEn=C, subjectCode=Life Sciences, subjectName=生命医学, subjectCodeEn=Life Sciences, subjectNameEn=null, picCn=E+iq5BU+frOtpo6YF6JpQQ==, picEn=n/3T/+AptjYTGmmMsE/a0Q==, jcr=null, cjcr=null, exts=[JournalExt(id=1205118195070906572, language=CN, name=药物分析杂志, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1765252167718, updatedTime=1765252167718, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionEditorUrl=https://ywfxeditor.manuscriptcloud.com/login, submissionReviewUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1205118195133821133, language=EN, name=Chinese Journal of Pharmaceutical Analysis, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1765252167733, updatedTime=1765252167733, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionEditorUrl=https://ywfxeditor.manuscriptcloud.com/login, submissionReviewUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1205117023404326918, websiteList=[Website(id=1205118568045195478, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1205117023404326918, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/ywfxzz/CN, language=CN, createTime=1765252256642, createBy=18614031015, updateTime=1765252521924, updateBy=18614031015, name=药物分析杂志-中文, tplId=1146099689490845704, title=药物分析杂志, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1205154326156128935, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=articleTextType, value=kx, createTime=1765260782040, updateTime=1765260782040, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326135157412, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=banner, value=null, createTime=1765260782035, updateTime=1765260782035, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326172906154, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=grayFlag, value=0, createTime=1765260782044, updateTime=1765260782044, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326126768803, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=logo, value=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/file/pic?fileId=5+7UKv7ckvsJ8AsWJeRI6g==, createTime=1765260782033, updateTime=1765260782033, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326181294764, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=minRunFlag, value=0, createTime=1765260782046, updateTime=1765260782046, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326147740326, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/file/pic, createTime=1765260782038, updateTime=1765260782038, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326177100459, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=silenceFlag, value=0, createTime=1765260782045, updateTime=1765260782045, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326143546021, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1765260782037, updateTime=1765260782037, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326160323240, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=themeColor, value=null, createTime=1765260782041, updateTime=1765260782041, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326164517545, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=themeStyle, value=null, createTime=1765260782042, updateTime=1765260782042, creator=18614031015, updator=18614031015)]), Website(id=1205118568124887259, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1205117023404326918, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/ywfxzz/EN, language=EN, createTime=1765252256661, createBy=18614031015, updateTime=1765252537379, updateBy=18614031015, name=药物分析杂志-英文, tplId=1146101810881728533, title=Chinese Journal of Pharmaceutical Analysis, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1205154361170174338, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=articleTextType, value=kx, createTime=1765260790388, updateTime=1765260790388, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361145008511, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=banner, value=null, createTime=1765260790382, updateTime=1765260790382, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361195340165, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=grayFlag, value=0, createTime=1765260790394, updateTime=1765260790394, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361132425598, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=logo, value=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/file/pic?fileId=5+7UKv7ckvsJ8AsWJeRI6g==, createTime=1765260790379, updateTime=1765260790379, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361207923079, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=minRunFlag, value=0, createTime=1765260790397, updateTime=1765260790397, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361157591425, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/file/pic, createTime=1765260790385, updateTime=1765260790385, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361199534470, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=silenceFlag, value=0, createTime=1765260790396, updateTime=1765260790396, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361149202816, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1765260790383, updateTime=1765260790383, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361174368643, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=themeColor, value=null, createTime=1765260790389, updateTime=1765260790389, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361186951556, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=themeStyle, value=null, createTime=1765260790392, updateTime=1765260790392, creator=18614031015, updator=18614031015)])], journalTitle=药物分析杂志, weixinUrl=null, journalUrl=null, iacademicId=null, status=1, seqNo=null, journalTitleEn=Chinese Journal of Pharmaceutical Analysis, journalPhotoCn=E+iq5BU+frOtpo6YF6JpQQ==, journalPhotoEn=n/3T/+AptjYTGmmMsE/a0Q==, journalFirstLetter=C, journalRecommend=null, journalNew=null, journalCollection=null, jcrJf=null, cjcrJf=null, jcrJfStr=null, cjcrJfStr=null, submissionFirstDecision=null, sciSubjectClassification=null, casSubjectClassification=null, citeScore=null, totalCitationFrequency=null, icpCode=null, psCode=null, advertisingLicenseCode=null, copyrightInformation=null, country=null, option=, provinceCode=null, provinceName=null, collectFlag=false), detailUrlCn=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/10.16155/j.0254-1793.2024-0076, detailUrlEn=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/10.16155/j.0254-1793.2024-0076, pdfUrlCn=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/PDF/10.16155/j.0254-1793.2024-0076, pdfUrlEn=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/PDF/10.16155/j.0254-1793.2024-0076, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, reference=null)
收藏切换
基于UPLC-MS/MS技术与化学计量学相结合的风湿安泰片中18个成分含量测定及质量评价研究*
收藏切换
PDF下载
张元元 , 孙慧珠 , 王晓蕾 , 雷蓉 , 刘雪莉 , 苏建 **
药物分析杂志 | 标准研讨 2024,44(10): 1816-1826
收起
收藏切换
药物分析杂志 | 标准研讨 2024, 44(10): 1816-1826
基于UPLC-MS/MS技术与化学计量学相结合的风湿安泰片中18个成分含量测定及质量评价研究*
全屏
张元元 , 孙慧珠, 王晓蕾, 雷蓉, 刘雪莉, 苏建**
作者信息
  • 河北省药品医疗器械检验研究院,石家庄 050227
  • Tel:(0311)69086155;E-mail:

通讯作者:

** Tel:(0311)69086155;E-mail:
Content determination and quality evaluation of 18 components in Fengshiantai tablets based on UPLC-MS/MS technology and chemometrics*
Yuan-yuan ZHANG , Hui-zhu SUN, Xiao-lei WANG, Rong LEI, Xue-li LIU, Jian SU**
Affiliations
  • Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China
出版时间: 2024-10-31 doi: 10.16155/j.0254-1793.2024-0076
文章导航
收藏切换
目的:

建立UPLC-MS/MS法,同时测定风湿安泰片中18个特征性成分含量,并对测定结果进行化学计量学分析,为其质量控制提供依据。

方法:

采用Waters BEH C18 (100 mm×2.1 mm,1.7 μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.2 mL·min-1,柱温40 ℃,进样量1 μL;质谱采用电喷雾离子源(ESI),正离子检测,多反应监测(MRM)模式。

结果:

所建方法在一定范围内线性关系良好(r≥0.998 6),平均加样回收率为90.2%~101.7%,RSD为1.1%~4.9%。39批次样品中麻黄碱(以盐酸麻黄碱计)、伪麻黄碱(以盐酸伪麻黄碱计)、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱(以盐酸小檗碱计)、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、人参皂苷Rb1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸(以甘草酸铵计)、羌活醇、异欧前胡素的含量范围分别为20.23~141.75、10.50~121.69、215.24~697.34、8.46~42.42、135.24~363.32、91.29~242.87、19.65~80.31、22.57~105.05、4.69~86.88、10.32~241.15、3.36~65.07、10.79~390.69、6.51~86.29、4.10~89.75、195.55~566.37、96.98~448.95、0~132.41、7.09~232.71 μg·片-1。化学计量学结果显示,5个生产企业39批样品聚为3类,不同生产企业样品质量存在一定差异,筛选出影响质量的8个差异性标志物(柚皮苷、甘草酸、异欧前胡素、小檗碱、紫丁香苷、麻黄碱、伪麻黄碱、士的宁)。

结论:

建立的方法简单、可行,结合化学计量学方法,可用于风湿安泰片的质量评价。

风湿安泰片  /  液质联用  /  特征性成分  /  含量测定  /  化学计量学  /  风险评估  /  质量评价
Objective:

To establish an UPLC-MS/MS method to measure the content of 18 characteristic components in Fengshiantai tablets,and conduct chemometric analysis on the measurement results to provide a basis for quality control.

Methods:

The components were separated on Waters BEH C18 (100 mm×2.1 mm,1.7 μm) column with methanol and 0.1% formic acid aqueous solution as the mobile phase by gradient elution at a flow rate of 0.2 mL·min-1. The column temperature was set at 40 ℃. The injection volume was 1 μL. The detection was carried out by electrospray ionization(ESI),and electron spray ionization source was adopted in positive ion detection with multiple reaction monitoring mode(MRM).

Results:

The established methods showed a good linear relationship in a certain range (r≥0.998 3),whose average recovery rates of samples were 90.2%-101.7% with the RSD of 1.1%-4.9%. The content of ephedrine(calculated as ephedrine hydrochloride),chlorogenic acid,syringin,strychnine,brucine,berberine(calculated as berberine hydrochloride),naringin,cinnamaldehyde,ginsenoside Re,ginsenoside Rg1,epimedin C,icariin,asperosaponin Ⅵ,glycyrrhizic acid(calculated as glycyrrhizic acid ammonium salt),ginsenoside Rb1,notopterol,isoimperatorin in 39 batches of samples were 20.23-141.75 μg per tablet,10.50-121.69 μg per tablet,215.24-697.34 μg per tablet,8.46-42.42 μg per tablet,135.24-363.32 μg per tablet,91.29-242.87 μg per tablet,19.65-80.31 μg per tablet,22.57-105.05 μg per tablet,4.69-86.88 μg per tablet,10.32-241.15 μg per tablet,3.36-65.07 μg per tablet,10.79-390.69 μg per tablet,6.51-86.29 μg per tablet,4.10-89.75 μg per tablet,195.55-566.37 μg per tablet,96.98-448.95 μg per tablet,0-132.41 μg per tablet,7.09-232.71 μg per tablet. The results of chemometrics showed that 39 batches of samples from 5 production enterprises were classify into three categories,and there were certain differeces in sample quality among different production enterprises,eight differential markers(naringin,glycyrrhizic acid,isoimperatorin,berberine,syringin,ephedrine,pseudoephedrine,strychnine) that caused quality differences were found.

Conclusion:

The established method is simple and feasible,combined with chemometric methods,and can be used for quality evaluation of Fengshiantai tablets.

Fengshiantai tablets  /  UPLC-MS/MS  /  characteristic components  /  content determination  /  chemometrics  /  risk assessment  /  quality evaluation
张元元, 孙慧珠, 王晓蕾, 雷蓉, 刘雪莉, 苏建. 基于UPLC-MS/MS技术与化学计量学相结合的风湿安泰片中18个成分含量测定及质量评价研究*. 药物分析杂志, 2024 , 44 (10) : 1816 -1826 . DOI: 10.16155/j.0254-1793.2024-0076
Yuan-yuan ZHANG, Hui-zhu SUN, Xiao-lei WANG, Rong LEI, Xue-li LIU, Jian SU. Content determination and quality evaluation of 18 components in Fengshiantai tablets based on UPLC-MS/MS technology and chemometrics*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (10) : 1816 -1826 . DOI: 10.16155/j.0254-1793.2024-0076
风湿安泰片由制马钱子、羌活、金银花、烫骨碎补、红参、黄柏、麻黄、甘草、槲寄生、淫羊藿、牛膝、桂枝、续断、五加皮等25味药组成,具有舒筋活血、祛风镇痛之功效,临床上用于治疗筋骨麻木、手足拘挛、腰腿疼痛、风湿性关节炎。处方中制马钱子既是君药,又属于毒性药材,所含主要成分士的宁和马钱子碱既为有效成分,又为毒性成分,且士的宁的治疗剂量和中毒剂量接近[1],成人口服5~10 mg就会出现中毒症状[2-5]。现行质量标准有《卫生部药品标准》中药成方制剂第二十册[6],WS3-B-3793-98-5等,但仅有WS3-B-3793-98-5对士的宁的含量限度进行了规定,其他厂家标准均未对士的宁和马钱子碱这2个毒性成分进行含量及限度规定,现行质量标准项目设置简单且不统一,覆盖药味较少,缺少对毒性药味的质量控制,无法实现标准可控和质量安全有效的目标。
由于该制剂中药味较多,成分复杂,且投药量较小,含毒性药材,传统HPLC法检测时干扰较多且分析时间过长,部分成分含量较低无法定量,因此采用专属性更强的UPLC-MS/MS法[7-10],对处方中麻黄、金银花、五加皮、槲寄生、制马钱子、黄柏、烫骨碎补、桂枝、红参、淫羊藿、续断、甘草、羌活13味药味中的特征性成分麻黄碱、伪麻黄碱、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱、柚皮苷、桂皮醛、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、淫羊藿苷、朝藿定C、川续断皂苷Ⅵ、甘草酸、羌活醇、异欧前胡素进行测定,并对测定结果进行化学计量学分析[11-15],以期从安全性和有效性2个方面为风湿安泰片的质量控制与评价提供参考。
Waters Acquity UPLC/XEVO TQ-S超高效液相色谱-三重四极杆质谱联用仪(Waters公司);XPE26型电子天平(0.001 mg)、XS105型电子天平(0.01 mg)均购于Mettler-Toledo公司;KQ-500DE型超声波清洗器(昆山超声仪器有限公司);Milli-Q型超纯水系统(Millipore公司)。
对照品盐酸麻黄碱(批号171241-201809,纯度100.0%)、盐酸伪麻黄碱(批号171237-200807,纯度99.9%)、绿原酸(批号110753-201817,纯度96.8%)、紫丁香苷(批号111574-202106,纯度94.3%)、士的宁(批号0705-200005,纯度100.0%)、马钱子碱(批号0706-200104,纯度100.0%)、盐酸小檗碱(批号110713-202015,纯度85.9%)、柚皮苷(批号110722-202116,纯度93.5%)、桂皮醛(批号110710-201821,纯度99.6%)、人参皂苷Re(批号110754-202129,纯度96.0%)、人参皂苷Rg1(批号110703-202034,纯度94.0%)、朝藿定C(批号111780-201804,纯度92.6%)、淫羊藿苷(批号110737-202017,纯度98.1%)、川续断皂苷Ⅵ(批号111685-201707,纯度90.9%)、甘草酸铵(批号110731-202021,纯度96.2%)、人参皂苷Rb1(批号110704-202028,纯度93.1%)、羌活醇(批号111820-201705,纯度99.9%)、异欧前胡素(批号110827-201410,纯度99.7%),均购于中国食品药品检定研究院。
甲醇、甲酸等均为色谱纯,水为超纯水。
39批风湿安泰片抽自全国各地经营、生产单位,涉及5家生产企业,其中A企业样品9批次(S1~S9)、B企业样品4批次(S10~S13)、C企业样品9批次(S14~S22)、D企业样品9批次(S23~S31)、E企业样品8批次(S32~S39)。
精密称取各待测成分对照品适量,分别加70%甲醇制成质量浓度均约为0.5 mg·mL-1的单一对照品储备液;精密量取上述单一对照品储备液适量,加70%甲醇配制成混合对照品储备溶液(每1 mL含盐酸麻黄碱5.18 μg、盐酸伪麻黄碱3.45 μg、绿原酸28.25 μg、紫丁香苷1.67 μg、士的宁17.78 μg、马钱子碱13.08 μg、盐酸小檗碱4.38 μg、柚皮苷5.80 μg、桂皮醛3.88 μg、人参皂苷Re 8.09 μg、人参皂苷Rg1 1.71 μg、朝藿定C 4.56 μg、淫羊藿苷4.14 μg、川续断皂苷Ⅵ 18.57 μg、甘草酸铵17.71 μg、人参皂苷Rb1 11.92 μg、羌活醇2.16 μg、异欧前胡素6.51 μg)。精密量取混合对照品储备溶液适量,加70%甲醇稀释10倍,即得混合对照品溶液。
取本品10片除去包衣,精密称定,研细,取约0.1 g,精密称定,置具塞锥形瓶中,精密加70%甲醇50 mL,称量,密塞,超声(功率250 W,频率40 kHz)处理30 min,取出,放冷,用70%甲醇补足减失的量,摇匀,滤过,取续滤液,经0.2 μm微孔滤膜滤过,即得。
采用Waters BEH C18 (100 mm×2.1 mm,1.7 μm)色谱柱,以甲醇(A)-0.1%甲酸(B)为流动相,梯度洗脱(0~7 min,5%A;7~16 min,5%A→67%A;16~20 min,67%A→87%A),体积流量0.2 mL·min-1,柱温40 ℃,进样量1 μL。
以三重四极杆串联质谱仪检测,电喷雾离子源(ESI),正离子检测,多反应监测模式(MRM),毛细管电压3 kV,锥孔电压20 kV,脱溶剂气温度450 ℃。各化合物质谱参数详见表1
按风湿安泰片处方比例和工艺,分别制备缺少麻黄、金银花和五加皮、槲寄生、制马钱子、黄柏、烫骨碎补、桂枝、红参、淫羊藿、续断、甘草、羌活药材的阴性样品,按照“2.1.2”项下方法制备阴性样品溶液,按照“2.2”项下条件对混合对照品溶液、供试品溶液、阴性样品溶液进样测定,结果供试品溶液中被测定成分与对照品的保留时间相对应,且分离效果与峰形良好,阴性样品溶液中无其他成分干扰测定,表明该方法专属性良好,色谱图见图1
精密量取“2.1.1”项混合对照品储备溶液适量,采用倍数稀释法,得到18个成分的系列浓度(6个浓度点)混合对照品溶液,在“2.2”项下条件下进行测定。以对照品质量浓度(X,μg·mL-1)为横坐标,峰面积积分值标(Y)为纵坐进行回归,结果见表2,可知各成分在各自范围内线性关系良好。
精密吸取“2.1.1”项下混合对照品溶液1 μL,按“2.2”项条件连续进样测定6次,测得麻黄碱、伪麻黄碱、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸、人参皂苷Rb1、羌活醇、异欧前胡素峰面积的RSD分别为1.0%、2.2%、0.77%、2.4%、0.85%、0.79%、0.74%、3.2%、1.4%、2.1%、1.4%、7.1%、0.29%、2.5%、3.3%、5.0%、1.7%、0.77%,表明仪器精密度良好。
取风湿安泰片样品(S8)10片,除去包衣,研细,精密称取0.1 g,共6份,分别按“2.1.2”项下方法制备供试品溶液,按“2.2”项条件进样测定,测得样品中麻黄碱(以盐酸麻黄碱计)、伪麻黄碱(以盐酸伪麻黄碱计)、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱(以盐酸小檗碱计)、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸(以甘草酸铵计)、人参皂苷Rb1、羌活醇、异欧前胡素含量的平均值分别为88.60、60.25、509.90、28.43、290.80、230.60、45.43、61.64、8.99、147.90、30.66、86.29、74.42、349.10、335.50、127.30、37.51、111.90 μg·片-1,其RSD分别为3.8%、2.4%、2.2%、0.96%、1.3%、1.3%、0.94%、2.9%、2.4%、2.8%、1.7%、7.4%、0.98%、2.6%、3.0%、2.8%、0.98%、1.3%,表明该方法重复性良好。
取“2.3.4”项下供试品溶液1份,于溶液制备后0、4、8、12、18、24 h按“2.2”项条件进样测定,测得麻黄碱、伪麻黄碱、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸、人参皂苷Rb1、羌活醇、异欧前胡素峰面积的RSD分别为1.1%、2.7%、3.4%、2.1%、1.4%、2.5%、2.0%、2.4%、2.3%、3.0%、2.7%、2.0%、0.82%、2.3%、2.6%、4.9%、2.1%、2.1%,表明供试品溶液在24 h内稳定性良好。
精密称取已测定含量的同一批风湿安泰片样品粉末(S8)约0.05 g,共6份,分别精密加入相当于样品中各待测成分含有量100%的混合对照品溶液,按“2.1.2”项下方法制备供试溶液,按“2.2”项条件进样测定,计算回收率。结果麻黄碱、伪麻黄碱、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸、人参皂苷Rb1、羌活醇、异欧前胡素的平均加样回收率分别为100.3%、96.2%、101.7%、98.0%、96.0%、101.7%、94.6%、97.3%、99.6%、97.4%、99.1%、90.2%、100.9%、96.7%、101.6%、101.5%、92.6%、95.6%,RSD分别为4.2%、3.2%、2.9%、3.7%、2.5%、1.3%、1.4%、4.4%、4.6%、4.3%、4.2%、4.9%、1.7%、3.5%、4.3%、4.2%、1.1%、4.3%,表明本方法各成分加样回收率良好。
取5个生产企业39批样品,分别按“2.1.2”项下方法制备供试品溶液,按“2.2”项条件进样测定,根据回归方程计算各成分含量,结果见表3
系统聚类分析(hierarchical cluster analysis,HCA)是一种非监督模式分析方法,可以更直观地展现样品批间化学组分的差异性,采用Simca 14.1软件对39批次样品中的18个成分含量进行HCA,结果见图2。39批样品按各生产企业聚为3类,A、B、E企业聚为一类,C、D企业各为一类,HCA结果表明同一生产企业的样品质量一致性较好,而不同生产企业样品质量存在一定差异。
采用SPSS 25.0软件对39批样品的18个成分含量数据进行主成分分析(principle component analysis,PCA),计算相关系数特征值和方差贡献率,结果见表4。以特征值>1为提取标准,得到前5个主成分,累积贡献率83.000%,表明前5个主成分可以代表风湿安泰片中18个成分83.000%的信息量,具有良好的代表性。
为进一步分析引起样品质量差异的原因,筛选出对差异贡献较大的成分,本研究基于HCA和PCA结果,采用Simca 14.1软件进行正交偏最小二乘判别分析(orthogonal least squares discriminant analysis,OPLS-DA),筛选差异成分,5个企业的39批样品按不同企业分类明显(图3),与HCA结果一致。在建立的模型中,累计解释能力参数R2XR2Y分别为0.821和1,预测能力参数Q2为0.778,均>0.5,表明所构建OPLS-DA模型稳定可靠,预测能力良好。
利用变量重要性投影(variable importance projection,VIP)值进行预测分析,以VIP值>1为标准,筛选出8个VIP值>1的差异性成分(图4),分别为柚皮苷、甘草酸、异欧前胡素、小檗碱、紫丁香苷、麻黄碱、伪麻黄碱、士的宁,分别归属于烫骨碎补、甘草、羌活、黄柏、槲寄生、麻黄、制马钱子,此8个成分对样品分类具有显著影响,是引起样品差异的主要标志物。由分析结果可知不同企业风湿安泰片样品中烫骨碎补、甘草、羌活、黄柏、槲寄生、麻黄、制马钱子质量差异明显,充分表明由于投料质量差异,不同企业间样品质量差异明显,提示企业应关注上述饮片质量。
风湿安泰片处方中药味较多,成分复杂,且投药量小,部分成分含量较低,无法定量,因此采用专属性更强的UPLC-MS/MS法,通过对目标化合物离子对的选定以及毛细管电压和碰撞电压的优化等,建立了同时测定13个药味中18个特征性成分含量的方法,覆盖药味较多,弥补现行标准控制药味较少,缺少对毒性药材质量控制项目的不足,可为全面评价制剂质量提供依据。处方中麻黄特征性成分麻黄碱和伪麻黄碱属于同分异构体,具有相同的定量离子对,可通过对照品定位进行有效定性。
对提取溶剂(30%甲醇、50%甲醇、70%甲醇、甲醇)、超声时间(20、30、50 min)、流动相洗脱系统(甲醇-水、乙腈-水、甲醇-0.1%甲酸溶液、乙腈-0.1%甲酸溶液、甲醇-0.1%乙酸溶液、乙腈-0.1%乙酸溶液、乙腈-10 mmol·L-1乙酸铵溶液)进行了考察,结果表明70%甲醇溶液超声30 min时,甲醇-0.1%甲酸溶液梯度洗脱,各成分均得到较好的提取,离子响应高,色谱峰分离效果和峰形均较好。
5个生产企业39批次样品中,麻黄碱(以盐酸麻黄碱计)、伪麻黄碱(以盐酸伪麻黄碱计)、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱(以盐酸小檗碱计)、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、人参皂苷Rb1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸(以甘草酸铵计)、羌活醇、异欧前胡素的含量范围分别为20.23~141.75、10.50~121.69、215.24~697.34、8.46~42.42、135.24~363.32、91.29~242.87、19.65~80.31、22.57~105.05、4.69~86.88、10.32~241.15、3.36~65.07、10.79~390.69、6.51~86.29、4.10~89.75、195.55~566.37、96.98~448.95、0~132.41、7.09~232.71 μg·片-1。由直观分析和计量学结果可知同一生产企业的样品质量一致性较好,不同企业间样品质量差异明显。柚皮苷、甘草酸铵、异欧前胡素、小檗碱、紫丁香苷、麻黄碱、伪麻黄碱、士的宁8个成分是引起样品差异的主要标志物,分别归属于烫骨碎补、甘草、羌活、黄柏、槲寄生、麻黄、制马钱子,提示企业应关注上述饮片质量。
桂皮醛对热不稳定,样品中桂皮醛含量普遍偏低,推测可能是企业的制剂生产工艺中,干燥温度较高,使其分解或降低,导致整体含量较低。提示企业应关注生产工艺参数对不稳定成分的影响。
整体综合分析:A、B企业整体投料质量相对较好,D企业投料质量相对较差。
风湿安泰片中制马钱子为原粉入药,参照2020年版《中华人民共和国药典》药材标准规定限度,考虑到企业规模化生产的重现性问题并结合士的宁的不良反应及日服最大量应小于4.92 mg(士的宁为马钱子的主要毒性成分),以70%转移率计,每片制马钱子含士的宁(C21H22N2O2)计,应为160~440 μg,以马钱子碱(C23H26N2O4)计,不得少于110 μg。现方法测定的39批样品中士的宁、马钱子碱含量测定结果分别为135.24~363.32、91.29~242.87 μg·片-1,结果表明部分企业样品中士的宁和马钱子碱的含量偏低,提示部分企业应关注制马钱子饮片质量。
制马钱子所含士的宁和马钱子碱既为有效成分,又为毒性成分,且士的宁的治疗剂量和中毒剂量接近,成人口服5~10 mg就会出现中毒症状,过量时可过度兴奋延髓表现出神经系统毒性[16],甚至导致肝脏、肾毒性损伤。风湿安泰片的口服量为一次2片,一日2~3次,计算得1 d的口服马钱子中士的宁最大量为2.64 mg,低于允许日服最大量,理论中毒风险较低。处方中甘草为国老之药,可解众毒,有研究显示[17-18]甘草可解马钱子之毒,甘草配伍马钱子可减毒增效,因此该制剂整体安全性风险相对较低。
本文建立了UPLC-MS/MS法同时测定风湿安泰片中18个特征性成分,具有快速、准确及抗干扰强等优点。通过多指标成分含量测定结合化学计量学综合评价不同生产企业间风湿安泰片的整体质量,以期从安全性和有效性2个方面为风湿安泰片的质量控制与评价提供参考。
  • *河北省药品监督管理局科技计划项目(2023ZC1018)
参考文献 引证文献
排序方式:
[1]
刘东升,刘婷婷,姚世霞,等. 风湿关节炎片的质量标准提升研究[J].中国现代中药202123(11):1982
LIU DSLIU TTYAO SX,et al. Improvement of quality standard for Fengshi Guanjieyan tablets[J]. Mod Chin Med202123(11):1982
[2]
王伟. 马钱子的炮制质量研究[J].内蒙古中医药201736(3):98
WANG W. Preparation research of Strychnos nux-vomica L.[J]. Inner Mongolia J Tradit Chin Med201736(3):98
[3]
张莉,李莉,杜冠华.中药马钱子毒的历史认识与现代研究[J].中药药理与临床201834(4):191
ZHANG LLI LDU GH. Historical understanding and modern research on the toxicity of traditional Chinese medicine Strychni Semen[J]. Pharmacol Clin Chin Mater Med201834(4):191
[4]
王菲菲,张聿梅,郑笑为,等. 骨刺片中士的宁和马钱子碱含量测定方法的研究[J].药物分析杂志201838(10):1824
WANG FFZHANG YMZHENG XW,et al. Study on assay method of brucine and strychnine in Guci tablets[J]. Chin J Pharm Anal201838(10):1824
[5]
刘静,于健东,朱嘉亮,等. 2008—2021年国家药品抽检中成药质量分析[J].中国现代中药202325(1):9
LIU JYU JDZHU JL,et al. Quality analysis of Chinese patent medicines based on 2008—2021 national drug sampling inspection[J]. Mod Chin Med202325(1):9
[6]
卫生部药品标准.第二十册[S]. 1990:64
Drug Specifications Promulgated by the Ministry of Public Health. PR China. Vol 20[S]. 1990:64
[7]
王亚丹,戴忠,孙彩林,等. UPLC-ELSD指纹图谱结合化学计量学方法用于骨刺片的质量控制[J].中国中药杂志201843(6):1156
WANG YDDAI ZSUN CL,et al. Quality control of Guci tablets using UPLC-ELSD fingerprint analysis coupled with chemometrics[J]. China J Chin Mater Med201843(6):1156
[8]
王亚丹,戴忠,何凤艳,等. RRLC-MS/MS法同时测定骨刺片中14个成分的含量[J].药物分析杂志201939(4):595
WANG YDDAI ZHE FY,et al. Simultaneous determination of 14 compounds in Guci tablets using RRLC-MS/MS method[J]. Chin J Pharm Anal201939(4):595
[9]
陈玉华,卢松. UPLC-QQQ-MS/MS法同时测定风湿安泰片中12种成分[J].中成药202143(3):596
CHENG YHLU S. Simultaneous determination of twelve constituents in Fengshiantai tablets by UPLC-QQQ-MS/MS[J]. Chin Tradit Pat Med202143(3):596
[10]
张婷,陈斌,刘利萍,等. UHPLC-ESI-MS/MS法测定烫骨碎补-续断药对中10个成分的含量[J].中药材202144(6):1441
ZHANG TCHEN BLIU LP,et al. Determination of the content of 10 components in the couplet medicines of burning Drynariae Rhizoma and Dipsaci Radix by UHPLC-ESI-MS/MS[J]. J Chin Med Mater202144(6):1441
[11]
李沁,张聪,陈亮,等.基于超高效液相色谱指纹图谱、多指标成分定量及化学计量学的小儿感冒颗粒质量评价[J].药物分析杂志202343(9):1612
LI QZHANG CCHEN L,et al. Quality evaluation of Xiao’er Ganmao granules based on UPLC fingerprint,multi-component determination,and chemometric analysis[J]. Chin J Pharm Anal202343(9):1612
[12]
曹春琪,孙慧珠,赵振霞,等.基于UHPLC-MS/MS技术的导赤丸中24个成分定量测定联合化学计量学质量评价[J].中草药202354(21):7034
CAO CQSUN HZZHAO ZX,et al. Quantitative determination of 24 components in Daochi pills based on UHPLC-MS/MS technology combined with chemometrics quality evaluation[J]. Chin Tradit Herb Drugs202354(21):7034
[13]
任慧,胡静,崔小敏,等.基于指纹图谱结合化学模式识别及多酚类成分含量测定的大盘龙七质量评价[J].中草药202354(19):6452
REN HHU JCUI XM,et al. Quality evaluation of Bergeniae Scopulosae Rhizoma based on fingerprints combination with chemical pattern recognition and content determination of phenolic compounds[J]. Chin Tradit Herb Drugs202354(19):6452
[14]
籍学伟,陈备尧,白妍,等.基于HPLC指纹图谱和多成分含量测定结合化学计量学的暖宫七味丸质量评价研究[J].中草药202454(2):1
JI XWCHEN BYBAI Y,et al. Quality evaluation of Nuangong Qiwei pills by HPLC fingerprint and multi-component content determination combined with chemometrics[J]. Chin Tradit Herb Drugs202454(2):1
[15]
于密密,王安琪,杜小伟,等.基于HPLC指纹图谱结合化学计量学的痢泻灵片质量评价[J].中成药202345(9):2846
YU MMWANG AQDU XW,et al. Quality evaluation of Lixieling tablets based on combinative methods of HPLC fingerprint,quantitative analysis of multi-components and chemometrics analysis[J]. Chin Tradit Herb Drugs202345(9):2846
[16]
RAMZAN MGOURION-ARSIQUAUD SHUSSAIN A,et al. In vitro release,ex vivo penetration,and in vivo dermatokinetics of ketoconazole-loaded solid lipid nanoparticles for topical delivery[J]. Drug Deliv Transl Res202212(7):1659
[17]
郭玉岩,高滔,李春城,等. 酸碱药对甘草-马钱子配伍汤液沉积相态解放特性研究[J].中草药202253(10):3000
GUO YYGAO TLI CC,et al. Release characteristics of principal components of acid-base drug pair Glycyrrhizae Radix et Rhizoma-Strychni Semen compatibility decoction in sedimentary phase[J]. Chin Tradit Herb Drugs202253(10):3000
[18]
马俊,曼琼,闫潇,等. 野生与栽培甘草对马钱子致肝毒性的解毒作用[J].中成药202345(8):2718
MA JMAN QYAN X,et al. Detoxification effect of wild and cultivated Glycyrrhizae Radix et Rhizoma on the hepatotoxicity caused by Strychni Semen[J]. Chin Tradit Pat Med202345(8):2718
2024年第44卷第10期
PDF下载
85
36
引用本文
BibTeX
文章信息
doi: 10.16155/j.0254-1793.2024-0076
  • 接收时间:2024-02-02
  • 首发时间:2026-03-15
  • 出版时间:2024-10-31
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期:2024-02-02
基金
*河北省药品监督管理局科技计划项目(2023ZC1018)
作者信息
    河北省药品医疗器械检验研究院,石家庄 050227

通讯作者:

** Tel:(0311)69086155;E-mail:
参考文献
分享链接
https://castjournals.cast.org.cn/joweb/ywfxzz/CN/10.16155/j.0254-1793.2024-0076
分享至
全文二维码

扫描看全文

引用本文
BibTeX
本文的引用情况
2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
关闭全屏