Article(id=1239256893827371116, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239256891017195761, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024.06.17, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=1712678400000, revisedDateStr=2024-04-10, acceptedDate=null, acceptedDateStr=null, onlineDate=1773391467768, onlineDateStr=2026-03-13, pubDate=1719676800000, pubDateStr=2024-06-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773391467768, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773391467768, creator=13701087609, updateTime=1773391467768, updator=13701087609, issue=Issue{id=1239256891017195761, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='6', pageStart='921', pageEnd='1104', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773391467098, creator=13701087609, updateTime=1773391544580, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239257216084144253, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239256891017195761, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239257216084144254, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239256891017195761, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1055, endPage=1061, ext={EN=ArticleExt(id=1239256894045474936, articleId=1239256893827371116, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Quality evaluation of Hyssopus cuspidatu Boriss. based on characteristic chromatogram and chemical pattern recognition*, columnId=1239148841803501731, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Quality Control, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish an HPLC characteristic chromatogram for Hyssopus cuspidatu Boriss. and control quality and identity authentication for the herb.

Methods:

The HPLC method was used, and the mobile phases were acetonitrile (A) and 0.1% aqueous phosphoric acid (B) in gradient elution(0-15 min, 10% A; 15-30 min, 10% A→15% A; 30-40 min, 15% A→18% A; 40-60 min, 18% A→23% A; 60-70 min, 23% A→55% A; 70-85 min, 55% A→60% A; 85-85.1 min, 60% A→10% A; 85.1-90 min, 10% A). The column temperature was 30 ℃, the flow rate was 1.0 mL·min-1, the detection wavelength was 330 nm and the injection volume was 20 μL. Fifteen batches of Hyssopus cuspidatu Boriss. and its adulterants, notably Cynanchum officinale, were analyzed to construct characteristic chromatogram. The authenticity and quality of Hyssopus cuspidatu Boriss. were assessed through principal component analysis(PCA), cluster analysis, and similarity analysis.

Results:

Analysis of the characteristic chromatogram of ten Hyssopus cuspidatu Boriss. batches revealed fifteen distinct peaks, with six compounds identified as isodendrobioside, molluscoside, rosmarinic acid, salvianolic acid, geranylgeranyl, and trichothecenes. Cluster analysis segregated the Hyssopus cuspidatu Boriss. samples into three distinct groups, primarily influenced by geographical (latitude and longitude) and environmental (climate) factors. PCA results indicated that four principal components accounted for 92.914% of the variance. The similarities for the ten batches of Hyssopus cuspidatu Boriss. ranged from 0.896 to 0.997, with no significant difference observed between the wild and cultivated varieties in terms of overall HPLC profile and relative peak content. The overall profiles of the HPLC characteristic chromatogram and the contents of the main components of the Hyssopus cuspidatu Boriss. and the Nepeta bracteata Benth. were significantly different.

Conclusion:

The HPLC characteristic chromatogram method developed in this study is reproducible, stable, and practical for the quality control and authentication of Hyssopus cuspidatu Boriss. Moreover, it offers a reliable analytical technique for the quality evaluation and authentication of this herb, providing substantial data support.

, correspAuthors=Xiao-juan RONG, Lan-lan ZHANG, 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=Pan-pan WANG, Wotan AYIDANA, Xiao-juan RONG, Lan-lan ZHANG), CN=ArticleExt(id=1239256897056985335, articleId=1239256893827371116, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=基于特征图谱和化学模式识别的硬尖神香草质量评价*, columnId=1239148842025799861, journalTitle=药物分析杂志, columnName=质量分析, runingTitle=null, highlight=null, articleAbstract=
目的:

建立硬尖神香草HPLC特征图谱,利用该特征图谱把控硬尖神香草药材的质量及鉴别真伪。

方法:

采用HPLC法,流动相为乙腈(A)和0.1%磷酸水溶液(B)进行梯度洗脱(0~15 min,10% A;15~30 min,10% A→15% A;30~40 min,15% A→18% A;40~60 min,18% A→23% A;60~70 min,23% A→55% A;70~85 min,55% A→60% A;85~85.1 min,60% A→10% A;85.1~90 min,10% A),柱温为30 ℃,流速为1.0 mL·min-1,检测波长为330 nm,进样量20 μL。分别收集硬尖神香草10批次及其混伪品大苞荆芥5批次,建立HPLC特征图谱,结合主成分分析(PCA)、聚类分析和相似度分析法对硬尖神香草质量进行评价。

结果:

从10批硬尖神香草特征图谱中共标定了15个共有色谱峰,指认了6个成分,分别为异槲皮苷、毛蕊花糖苷、迷迭香酸、丹酚酸B、香叶木素和三裂鼠尾草素。聚类分析将10批硬尖神香草样品聚为3类;主成分结果筛选出累计贡献率为92.914%的4个主成分;10批硬尖神香草的相似度为0.896~0.997,硬尖神香草野生品种与种植品种从整体轮廓以及特征峰相对含量无明显差异;硬尖神香草与大苞荆芥的HPLC特征图谱整体轮廓及主成分含量均有明显差别。

结论:

该研究建立的HPLC特征图谱方法重复性、稳定性好,具有可操作性,为硬尖神香草药材的质量控制及鉴别真伪提供了分析方法,为该类药材的质量评价提供了数据支持。

, correspAuthors=戎晓娟, 张兰兰, authorNote=null, correspAuthorsNote=
** 戎晓娟 Tel:18997562425;E-mail:;
张兰兰 Tel:18199127303;E-mail:
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Tel: 17834467995;E-mail:

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Chin J Pharm Anal202343(10):1784, articleTitle=Quality control study of four seasons sanhuang pills based on UPLC fingerprinting combined with chemical pattern recognition, refAbstract=null)], funds=[Fund(id=1239268360039486205, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, awardId=2022D01E65, language=CN, fundingSource=*新疆维吾尔自治区自然科学基金资助项目(2022D01E65), fundOrder=null, country=null), Fund(id=1239268360144343812, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, awardId=2023TSYCCX0065, language=CN, fundingSource=“天山英才”培养计划(2023TSYCCX0065), fundOrder=null, country=null), Fund(id=1239268360228229895, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, awardId=81960752, language=CN, fundingSource=国家自然科学基金项目(81960752), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239268351122395596, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, xref=1., ext=[AuthorCompanyExt(id=1239268351126589902, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351122395596, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.Xinjiang University, Urumqi 830046, China), AuthorCompanyExt(id=1239268351139172815, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351122395596, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.新疆大学,乌鲁木齐 830046)]), AuthorCompany(id=1239268351231447509, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, xref=2., ext=[AuthorCompanyExt(id=1239268351239836116, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351231447509, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.Xinjiang Uygur Autonomous Region Institute of Pharmaceutical Research, Urumqi 830004, China), AuthorCompanyExt(id=1239268351252419030, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351231447509, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.新疆维吾尔自治区药物研究所,乌鲁木齐 830004)]), AuthorCompany(id=1239268351348888029, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, xref=3., ext=[AuthorCompanyExt(id=1239268351365665246, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351348888029, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.Food and Drug Review and Verification Center of Xinjiang Production and Construction Corps, Urumqi 831400, China), AuthorCompanyExt(id=1239268351374053855, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, companyId=1239268351348888029, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.新疆生产建设兵团食品药品审评核查中心,乌鲁木齐 831400)])], figs=[ArticleFig(id=1239268355941651077, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.1, caption=HPLC characteristic chromatogram of Hyssopus cuspidatus Boriss., figureFileSmall=7nOCZDGR/5a7hXW0Zh2PUQ==, figureFileBig=wpEErP132mtrUsc3DOqtbw==, tableContent=null), ArticleFig(id=1239268356038120075, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图1, caption=硬尖神香草HPLC特征图谱

9.异槲皮苷(isodendrobioside) 10.毛蕊花糖苷(mullein glycoside) 12.迷迭香酸(rosmarinic acid) 13.丹酚酸B(salvinorin B) 14.香叶木素(geraniolin) 15.三裂鼠尾草素(geraniolin)

, figureFileSmall=7nOCZDGR/5a7hXW0Zh2PUQ==, figureFileBig=wpEErP132mtrUsc3DOqtbw==, tableContent=null), ArticleFig(id=1239268356193309332, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.2, caption=HPLC chromatogram of mixed reference standards, figureFileSmall=wFfEzI4FF8X3oI3vZDwrsg==, figureFileBig=Aa46zZw3Rwqe5JIjdS650A==, tableContent=null), ArticleFig(id=1239268356310749849, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图2, caption=混合对照品HPLC色谱图

1.异槲皮苷(isodendrobioside) 2.毛蕊花糖苷(mullein glycoside) 3.迷迭香酸(rosmarinic acid) 4.丹酚酸B(salvinorin B) 5.香叶木素(geranylgeranyl) 6.三裂鼠尾草素(trichothecenes)

, figureFileSmall=wFfEzI4FF8X3oI3vZDwrsg==, figureFileBig=Aa46zZw3Rwqe5JIjdS650A==, tableContent=null), ArticleFig(id=1239268356394635933, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.3, caption=Overlay characteristic chromatograms of Hyssopus cuspidatus Boriss., figureFileSmall=tg1NBc9uysUo1CdijQgptg==, figureFileBig=xPSVMmkTVjEjQ52WkD6I/w==, tableContent=null), ArticleFig(id=1239268356495299234, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图3, caption=硬尖神香草药材特征图谱叠加图, figureFileSmall=tg1NBc9uysUo1CdijQgptg==, figureFileBig=xPSVMmkTVjEjQ52WkD6I/w==, tableContent=null), ArticleFig(id=1239268356595962533, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.4, caption=Difference in the contents of main components in Hyssopus cuspidatus Boriss., figureFileSmall=hL91udW0zDs+10dYc4fC+g==, figureFileBig=tOZiL1yQMH0y3ArOnaOZ7g==, tableContent=null), ArticleFig(id=1239268356700820139, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图4, caption=硬尖神香草药材主要成分含量差异, figureFileSmall=hL91udW0zDs+10dYc4fC+g==, figureFileBig=tOZiL1yQMH0y3ArOnaOZ7g==, tableContent=null), ArticleFig(id=1239268356805677743, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.5, caption=Systematic cluster analysis of Hyssopus cuspidatus Boriss., figureFileSmall=MhdY/I8BMCBroIkeNhltZA==, figureFileBig=A56lEoJnNvdyvHB8DEb7CA==, tableContent=null), ArticleFig(id=1239268356906341045, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图5, caption=硬尖神香草药材系统聚类分析图, figureFileSmall=MhdY/I8BMCBroIkeNhltZA==, figureFileBig=A56lEoJnNvdyvHB8DEb7CA==, tableContent=null), ArticleFig(id=1239268357007004347, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig. 6, caption=Overlay characteristic chromatogram of Nepeta bracteata Benth. superimposed on the map, figureFileSmall=uThQ/yr/tfqC/jTxnjDAqw==, figureFileBig=N+1u3XB49cbXf4dItgI/eA==, tableContent=null), ArticleFig(id=1239268357095084733, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图6, caption=大苞荆芥药材特征图谱叠加图, figureFileSmall=uThQ/yr/tfqC/jTxnjDAqw==, figureFileBig=N+1u3XB49cbXf4dItgI/eA==, tableContent=null), ArticleFig(id=1239268357250273986, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.7, caption=HPLC chromatogram of Hyssopus cuspidatus Boriss., figureFileSmall=f+vGSSx+Naz/ZtA+bWX5Hw==, figureFileBig=ahsN+r65dOFjzi50eOiHOw==, tableContent=null), ArticleFig(id=1239268357384491719, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图7, caption=硬尖神香草HPLC色谱图, figureFileSmall=f+vGSSx+Naz/ZtA+bWX5Hw==, figureFileBig=ahsN+r65dOFjzi50eOiHOw==, tableContent=null), ArticleFig(id=1239268357464183500, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Fig.8, caption=HPLC chromatogram of Nepeta bracteata Benth., figureFileSmall=14Vxs/PK0up9vYEnNr9ojA==, figureFileBig=yLRFAq9lNu2hSml1N7QK1w==, tableContent=null), ArticleFig(id=1239268357594206932, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=图8, caption=大苞荆芥HPLC色谱图, figureFileSmall=14Vxs/PK0up9vYEnNr9ojA==, figureFileBig=yLRFAq9lNu2hSml1N7QK1w==, tableContent=null), ArticleFig(id=1239268357728424668, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Tab.1, caption=

Information of 15 batches of herbs

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
药材
(herb)
批号
(batch No.)
来源
(source)
S1硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021001阿勒泰市汗德尕特乡(野生)[Khandagait Township,Altay City (wild)]
S2硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021002阿勒泰市汗德尕特乡(野生)[Khandagait Township,Altay City (wild)]
S3硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021003阿勒泰市克木乔乡(野生)[Kemujiao Township,Altay City (wild)]
S4硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021004布尔津阿盖贡担草原(野生)[Agongti Grassland,Burqin County,Altay City (wild)]
S5硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021005阿勒泰市红墩镇(野生)[Hongdun Town,Altay City (wild)]
S6硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021006阿勒泰市飞机场附近(野生)[Near the Altay City Airport (wild)]
S7大苞荆芥(Nepeta bracteata Benth.)W 2021007和田药材市场(Hotan Medicinal Herb Market)
S8硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021008阿勒泰市车管所西侧(野生)[West side of the Vehicle Administration Office,Altay City (wild)]
S9硬尖神香草(Hyssopus cuspidatus Boriss.)Z2021009阿勒泰市阿苇滩镇(种植)[Aweitan Town,Altay City (cultivated)]
S10硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021010阿勒泰市哈萨克医院(野生)[Kazakh Hospital,Altay City (wild)]
S11大苞荆芥(Nepeta bracteata Benth.)W2021011乌鲁木齐市维吾尔医院(Uighur Hospital,Urumqi City)
S12大苞荆芥(Nepeta bracteata Benth.)W2021012和田药材市场(Hotan Medicinal Herb Market)
S13大苞荆芥(Nepeta bracteata Benth.)W2021013喀什药材市场(Kashgar Medicinal Herb Market)
S14硬尖神香草(Hyssopus cuspidatus Boriss.)Z2021014阜康(种植)[Fukang City,Changji Hui Autonomous Prefecture (cultivated)]
S15大苞荆芥(Nepeta bracteata Benth.)W2021015乌鲁木齐市二道桥药材市场(Erdaoqiao Medicinal Herb Market,Urumqi City)
), ArticleFig(id=1239268357841670880, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=表1, caption=

15批药材信息

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
药材
(herb)
批号
(batch No.)
来源
(source)
S1硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021001阿勒泰市汗德尕特乡(野生)[Khandagait Township,Altay City (wild)]
S2硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021002阿勒泰市汗德尕特乡(野生)[Khandagait Township,Altay City (wild)]
S3硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021003阿勒泰市克木乔乡(野生)[Kemujiao Township,Altay City (wild)]
S4硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021004布尔津阿盖贡担草原(野生)[Agongti Grassland,Burqin County,Altay City (wild)]
S5硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021005阿勒泰市红墩镇(野生)[Hongdun Town,Altay City (wild)]
S6硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021006阿勒泰市飞机场附近(野生)[Near the Altay City Airport (wild)]
S7大苞荆芥(Nepeta bracteata Benth.)W 2021007和田药材市场(Hotan Medicinal Herb Market)
S8硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021008阿勒泰市车管所西侧(野生)[West side of the Vehicle Administration Office,Altay City (wild)]
S9硬尖神香草(Hyssopus cuspidatus Boriss.)Z2021009阿勒泰市阿苇滩镇(种植)[Aweitan Town,Altay City (cultivated)]
S10硬尖神香草(Hyssopus cuspidatus Boriss.)Y2021010阿勒泰市哈萨克医院(野生)[Kazakh Hospital,Altay City (wild)]
S11大苞荆芥(Nepeta bracteata Benth.)W2021011乌鲁木齐市维吾尔医院(Uighur Hospital,Urumqi City)
S12大苞荆芥(Nepeta bracteata Benth.)W2021012和田药材市场(Hotan Medicinal Herb Market)
S13大苞荆芥(Nepeta bracteata Benth.)W2021013喀什药材市场(Kashgar Medicinal Herb Market)
S14硬尖神香草(Hyssopus cuspidatus Boriss.)Z2021014阜康(种植)[Fukang City,Changji Hui Autonomous Prefecture (cultivated)]
S15大苞荆芥(Nepeta bracteata Benth.)W2021015乌鲁木齐市二道桥药材市场(Erdaoqiao Medicinal Herb Market,Urumqi City)
), ArticleFig(id=1239268357950722790, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Tab. 2, caption=

Peak areas per mass unit of the common peaks of the Hyssopus cuspidatus Boriss.

, figureFileSmall=null, figureFileBig=null, tableContent=
峰号
(peak No.)
峰面积(peak area)
S1S2S3S4S5S6S8S9S10S14
1746.9529.5795.5632.2562.71 060.7595.0312.5446.8394.0
21 284.81 413.81 098.81 762.92 085.7991.81 162.61 276.1550.61645.8
31 004.9640.6505.7755.1808.0606.5600.6411.4216.0383.6
41 867.61 332.71 556.51 891.61 923.02 317.01 727.81 233.0764.91 544.7
51 502.31 378.61 409.11 408.41 431.32 089.51 349.51 257.71 417.21 510.8
6738.0828.61 165.4649.7569.51 361.2763.5276.3842.4323.2
73 334.62 947.73 246.73 149.73 643.03 469.23 083.52 336.91 440.12 553.9
8164.0100.4148.0121.1136.7148.1220.752.7378.4103.8
9137.7132.6151.2134.8181.3169.6164.557.680.359.4
10234.9216.8247.1229.7268.6222.9247.3123.7143.2136.8
11467.4433.0317.3457.3300.8363.1352.9296.7245.6231.8
121 283.01 002.6954.51 211.01 154.11 643.61 174.4575.7688.8674.4
132 104.01 939.91 764.32 119.52 393.61 726.31 886.81 195.5791.51 430.2
1483.268.485.873.335.746.735.711.476.98.7
15439.8436.9647.3470.8532.5513.2807.0349.7488.6416.5
), ArticleFig(id=1239268358080746219, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=表2, caption=

硬尖神香草药材共有峰单位质量的峰面积

, figureFileSmall=null, figureFileBig=null, tableContent=
峰号
(peak No.)
峰面积(peak area)
S1S2S3S4S5S6S8S9S10S14
1746.9529.5795.5632.2562.71 060.7595.0312.5446.8394.0
21 284.81 413.81 098.81 762.92 085.7991.81 162.61 276.1550.61645.8
31 004.9640.6505.7755.1808.0606.5600.6411.4216.0383.6
41 867.61 332.71 556.51 891.61 923.02 317.01 727.81 233.0764.91 544.7
51 502.31 378.61 409.11 408.41 431.32 089.51 349.51 257.71 417.21 510.8
6738.0828.61 165.4649.7569.51 361.2763.5276.3842.4323.2
73 334.62 947.73 246.73 149.73 643.03 469.23 083.52 336.91 440.12 553.9
8164.0100.4148.0121.1136.7148.1220.752.7378.4103.8
9137.7132.6151.2134.8181.3169.6164.557.680.359.4
10234.9216.8247.1229.7268.6222.9247.3123.7143.2136.8
11467.4433.0317.3457.3300.8363.1352.9296.7245.6231.8
121 283.01 002.6954.51 211.01 154.11 643.61 174.4575.7688.8674.4
132 104.01 939.91 764.32 119.52 393.61 726.31 886.81 195.5791.51 430.2
1483.268.485.873.335.746.735.711.476.98.7
15439.8436.9647.3470.8532.5513.2807.0349.7488.6416.5
), ArticleFig(id=1239268359607472878, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=EN, label=Tab.3, caption=

Results of principal component eigenvalues and variance contribution of 10 batches of Hyssopus cuspidatus Boriss.

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
特征值
(eigenvalue)
方差贡献率
(variance contribution rate)/%
累积方差贡献率
(cumulative rate)/%
17.59450.62450.624
23.31322.08772.711
31.70511.36784.078
41.3258.83692.914
), ArticleFig(id=1239268359771050739, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239256893827371116, language=CN, label=表3, caption=

10批硬尖神香草药材的主成分特征值及方差贡献率结果

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
特征值
(eigenvalue)
方差贡献率
(variance contribution rate)/%
累积方差贡献率
(cumulative rate)/%
17.59450.62450.624
23.31322.08772.711
31.70511.36784.078
41.3258.83692.914
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基于特征图谱和化学模式识别的硬尖神香草质量评价*
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王盼盼 1 , 阿依达娜·沃坦 2 , 戎晓娟 2, ** , 张兰兰 3, **
药物分析杂志 | 质量分析 2024,44(6): 1055-1061
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药物分析杂志 | 质量分析 2024, 44(6): 1055-1061
基于特征图谱和化学模式识别的硬尖神香草质量评价*
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王盼盼1 , 阿依达娜·沃坦2, 戎晓娟2, ** , 张兰兰3, **
作者信息
  • 1.新疆大学,乌鲁木齐 830046
  • 2.新疆维吾尔自治区药物研究所,乌鲁木齐 830004
  • 3.新疆生产建设兵团食品药品审评核查中心,乌鲁木齐 831400
  • Tel: 17834467995;E-mail:

通讯作者:

** 戎晓娟 Tel:18997562425;E-mail:;
张兰兰 Tel:18199127303;E-mail:
Quality evaluation of Hyssopus cuspidatu Boriss. based on characteristic chromatogram and chemical pattern recognition*
Pan-pan WANG1 , Wotan AYIDANA2, Xiao-juan RONG2, ** , Lan-lan ZHANG3, **
Affiliations
  • 1.Xinjiang University, Urumqi 830046, China
  • 2.Xinjiang Uygur Autonomous Region Institute of Pharmaceutical Research, Urumqi 830004, China
  • 3.Food and Drug Review and Verification Center of Xinjiang Production and Construction Corps, Urumqi 831400, China
出版时间: 2024-06-30 doi: 10.16155/j.0254-1793.2024.06.17
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目的:

建立硬尖神香草HPLC特征图谱,利用该特征图谱把控硬尖神香草药材的质量及鉴别真伪。

方法:

采用HPLC法,流动相为乙腈(A)和0.1%磷酸水溶液(B)进行梯度洗脱(0~15 min,10% A;15~30 min,10% A→15% A;30~40 min,15% A→18% A;40~60 min,18% A→23% A;60~70 min,23% A→55% A;70~85 min,55% A→60% A;85~85.1 min,60% A→10% A;85.1~90 min,10% A),柱温为30 ℃,流速为1.0 mL·min-1,检测波长为330 nm,进样量20 μL。分别收集硬尖神香草10批次及其混伪品大苞荆芥5批次,建立HPLC特征图谱,结合主成分分析(PCA)、聚类分析和相似度分析法对硬尖神香草质量进行评价。

结果:

从10批硬尖神香草特征图谱中共标定了15个共有色谱峰,指认了6个成分,分别为异槲皮苷、毛蕊花糖苷、迷迭香酸、丹酚酸B、香叶木素和三裂鼠尾草素。聚类分析将10批硬尖神香草样品聚为3类;主成分结果筛选出累计贡献率为92.914%的4个主成分;10批硬尖神香草的相似度为0.896~0.997,硬尖神香草野生品种与种植品种从整体轮廓以及特征峰相对含量无明显差异;硬尖神香草与大苞荆芥的HPLC特征图谱整体轮廓及主成分含量均有明显差别。

结论:

该研究建立的HPLC特征图谱方法重复性、稳定性好,具有可操作性,为硬尖神香草药材的质量控制及鉴别真伪提供了分析方法,为该类药材的质量评价提供了数据支持。

硬尖神香草  /  大苞荆芥  /  特征图谱  /  化学模式识别  /  质量评价  /  真伪鉴别
Objective:

To establish an HPLC characteristic chromatogram for Hyssopus cuspidatu Boriss. and control quality and identity authentication for the herb.

Methods:

The HPLC method was used, and the mobile phases were acetonitrile (A) and 0.1% aqueous phosphoric acid (B) in gradient elution(0-15 min, 10% A; 15-30 min, 10% A→15% A; 30-40 min, 15% A→18% A; 40-60 min, 18% A→23% A; 60-70 min, 23% A→55% A; 70-85 min, 55% A→60% A; 85-85.1 min, 60% A→10% A; 85.1-90 min, 10% A). The column temperature was 30 ℃, the flow rate was 1.0 mL·min-1, the detection wavelength was 330 nm and the injection volume was 20 μL. Fifteen batches of Hyssopus cuspidatu Boriss. and its adulterants, notably Cynanchum officinale, were analyzed to construct characteristic chromatogram. The authenticity and quality of Hyssopus cuspidatu Boriss. were assessed through principal component analysis(PCA), cluster analysis, and similarity analysis.

Results:

Analysis of the characteristic chromatogram of ten Hyssopus cuspidatu Boriss. batches revealed fifteen distinct peaks, with six compounds identified as isodendrobioside, molluscoside, rosmarinic acid, salvianolic acid, geranylgeranyl, and trichothecenes. Cluster analysis segregated the Hyssopus cuspidatu Boriss. samples into three distinct groups, primarily influenced by geographical (latitude and longitude) and environmental (climate) factors. PCA results indicated that four principal components accounted for 92.914% of the variance. The similarities for the ten batches of Hyssopus cuspidatu Boriss. ranged from 0.896 to 0.997, with no significant difference observed between the wild and cultivated varieties in terms of overall HPLC profile and relative peak content. The overall profiles of the HPLC characteristic chromatogram and the contents of the main components of the Hyssopus cuspidatu Boriss. and the Nepeta bracteata Benth. were significantly different.

Conclusion:

The HPLC characteristic chromatogram method developed in this study is reproducible, stable, and practical for the quality control and authentication of Hyssopus cuspidatu Boriss. Moreover, it offers a reliable analytical technique for the quality evaluation and authentication of this herb, providing substantial data support.

Hyssopus cuspidatus Boriss.  /  Nepeta bracteata Benth.  /  characteristic chromatogram  /  chemical pattern recognition  /  quality evaluation  /  authenticity
王盼盼, 阿依达娜·沃坦, 戎晓娟, 张兰兰. 基于特征图谱和化学模式识别的硬尖神香草质量评价*. 药物分析杂志, 2024 , 44 (6) : 1055 -1061 . DOI: 10.16155/j.0254-1793.2024.06.17
Pan-pan WANG, Wotan AYIDANA, Xiao-juan RONG, Lan-lan ZHANG. Quality evaluation of Hyssopus cuspidatu Boriss. based on characteristic chromatogram and chemical pattern recognition*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (6) : 1055 -1061 . DOI: 10.16155/j.0254-1793.2024.06.17
神香草为唇形科 (Labiatae) 神香草属 (Hys-sopus) 硬尖神香草Hyssopus cuspidatus Boriss.的地上干燥部分[1],富含挥发油、三萜、黄酮、酚酸、多糖等成分,被广泛应用于维药、哈萨克医药中。临床上,硬尖神香草多为感冒、咳嗽药方中的主药或辅药,还被制成祛痰剂、发汗剂等[2-5]。《维吾尔药志》记载其“性二级热,味苦、辛,气芳香,具有温肺平喘、祛寒止咳、燥湿祛痰、发汗解毒、消炎退肿的功效,用于湿寒性和黏液质性呼吸病[6-9]”。目前主要以野生为主,种植较少。在我国广泛分布于新疆天山、阿尔泰山、准噶尔西部山地、帕米尔高原和昆仑山的山地草原[10-12]。通过市场调研了解到“同名异物”大苞荆芥(维吾尔名为“祖发”)常被当作硬尖神香草(维吾尔名同为“祖发”)使用,市场应用较为混乱,再加上采收、加工、储藏等环节的不规范性,导致市场上的硬尖神香草药材质量差异较大,且常掺杂有其他植物干燥根及根茎,有时难以识别。因此有必要建立硬尖神香草综合质量评价方法,更好筛选出优质药材从而保证中成药的优质优效。
近年来,国内外学者对硬尖神香草开展了较为广泛的研究,但多集中在化学成分和药理活性[13-15],对于其全面质量评价研究较少。中华人民共和国卫生部《药品标准》维吾尔药分册收载了硬尖神香草,但仅有简单的性状描述及显微鉴别[16],目前虽有研究者做了部分检查和单指标含量测定相关研究,但仍难以全面控制和评价药材的质量。中药特征图谱是运用一定综合性的分析方法,通过特征性图谱对中药化学成分进行整体表征,是当前最高效的中药整体质量评价技术手段[17-18]。本研究以不同产地、种植/野生硬尖神香草和大苞荆芥为研究对象,通过HPLC特征图谱对硬尖神香草主要化学成分进行宏观整体表征,并结合化学模式识别对其质量及真伪进行分析,为硬尖神香草药材的质量控制及真伪鉴别提供科学依据。
Agilent 1260高效液相色谱仪(1260 Infinity Agilent Techeologies);电子天平TE212-L(赛多利斯科学仪器有限公司,0.01 g);PA225 D型电子天平(赛多利斯科学仪器有限公司,0.01 mg);KQ-500VDV型超声清洗仪(昆山市超声仪器有限公司,昆山)。
乙腈(Fisher Scientific公司)、甲酸(天津市北联精细化学品开发有限公司,)为色谱纯,甲醇为分析纯,水为娃哈哈纯净水。对照品香叶木素(批号PS010395,含量100%)、三裂鼠尾草素(批号PS010371,含量98.0%)、丹酚酸B(批号PS000278,含量98.0%)、毛蕊花糖苷(批号PS011528,含量100%)、异槲皮苷(批号PS001042,含量98.0%)均来自成都普思生物科技股份有限公司。对照品迷迭香酸(批号111871-202007,含量98.1%)来自中国食品药品检定研究院。15批药材具体信息见表1
采用COSMOSIL C18色谱柱(250 mm×4.6 mm,5 μm),流动相A为乙腈,流动相B为0.1%磷酸水溶液,梯度洗脱(0~15 min,10% A;15~30 min,10% A→15% A;30~40 min,15% A→18% A;40~60 min,18% A→23% A;60~70 min,23% A→55% A;70~85 min,55% A→60% A;85~85.1 min,60% A→10% A;85.1~90 min,10% A),柱温为30 ℃,流速为1.0 mL·min-1,检测波长为330 nm,进样量为 20 μL。
取香叶木素、三裂鼠尾草素、丹酚酸B、毛蕊花糖苷、异槲皮苷、迷迭香酸的对照品适量,精密称定,加50%甲醇制成0.1 mg·mL-1的混合对照品溶液。
分别取15批次的药材(批号S1-S15)约2 g,精密称定,置具塞锥形瓶中,加50%甲醇溶液40 mL,称量,超声(功率300 W,频率45 kHz)处理40 min,放冷,再称量,用50%甲醇水溶液补足减失的量,摇匀,0.45 μm微孔滤膜滤过,取滤液,即得。
取10批硬尖神香草药材,按“2.3”项下方法制备供试品溶液,分别按“2.1”项下确定的色谱条件进行测定,记录各样品的色谱图,并导出色谱图的AIA 格式,采用国家药典委员会推荐的“中药色谱指纹图谱相似度评价系统(2012,130723版本)”进行结果分析,选择其共有峰,再以7号峰为参照峰(即S峰),选择其中相对保留时间和相对峰面积较为稳定的共有峰作为特征峰,见图1
依据上述方法,确定供试品色谱中应呈现15个特征峰,并利用对照品的指认,确定硬尖神香草的特征峰归属:其中峰9为异槲皮苷,峰10为毛蕊花糖苷,峰12为迷迭香酸,峰13为丹酚酸B,峰14为香叶木素,峰15为三裂鼠尾草素,见图2
称取硬尖神香草药材(S10),按“2.3”项方法制备供试品溶液,按“2.1” 项色谱条件进行测定,连续进样6次,结果以7号峰为参照峰S,各特征峰与S峰的相对保留时间RSD在0.070%~0.14%范围内,由结果可知仪器精密度良好。
称取硬尖神香草药材(S10)6份,按“2.3”项方法制备供试品溶液,按“2.1” 项色谱条件进行测定,结果以7号峰为参照峰S,各特征峰与S峰的相对保留时间RSD在0.13%~0.57%,表明方法重复性较好。
同一份硬尖神香草(S10)供试品溶液,分别在0、3、6、9、12、24 h进行分析,结果显示12 h内药材特征图谱共有峰的峰面积RSD均小于5%,因此供试品溶液室温放置12 h稳定。
分别考察了柱温为32、30、28 ℃和流速为0.9、1.0、1.1 mL·min-1时的样品分离效果,结果表明各特征峰与S峰的相对保留时间RSD小于5.0%,较小的柱温和流速变动能满足系统适用性要求,耐用性较好。
分别将得到的10批硬尖神香草药材色谱数据以AIA格式导入“中药色谱指纹图谱相似度评价系统(2012,130723版本)”软件,以中位数法计算,经多点校正和自动匹配后生成对照特征图谱,以生成的对照特征图谱为标准,计算10批硬尖神香草药材的相似度,相似度范围是0.896~0.997,结果见图3
按10批硬尖神香草特征图谱中共有峰的单位质量峰面积计算,以15个主要成分的累积峰面积评价,结果显示S9、S10、S14共有峰的单位质量峰面积总和相对较低,其余批次主成分累计含量相近。结果见表2图4
以10批硬尖神香草15个共有峰的单位质量的峰面积为变量,导入SPSS 25.0统计软件,选择组间联接、平方欧式距离法进行系统聚类分析,当平方欧氏距离为10时,硬尖神香草药材可聚为3类,S10为1类,S9、S14为1类,其他为1类,该结果与药材主成分累积含量比较结果一致,结果见图5
以10批硬尖神香草药材15个共有峰的单位质量的峰面积为变量,采用 SPSS 25.0软件对10批硬尖神香草药材进行主成分分析,设定主成分特征值>1为提取标准,提取得到4个主成分,其累计贡献率为92.914%,结果见表3
照“2.1”色谱条件,5批大苞荆芥药材各峰分离均良好,如图6所示。硬尖神香草和大苞荆芥的色谱图整体轮廓存在较大差异,可明显区分硬尖神香草药材与大苞荆芥药材。如图78所示。主成分含量差异明显,硬尖神香草药材中异槲皮苷(0.008%)、毛蕊花糖苷(0.013%)、迷迭香酸(0.036%)、丹酚酸B(0.151%)、香叶木素(0.001%)、三裂鼠尾草素(0.021%)。“同名异物”大苞荆芥药材中异槲皮苷(0.112%)、毛蕊花糖苷(0.159%)、迷迭香酸(0.032%)、丹酚酸B(0.012%),无香叶木素和三裂鼠尾草素。
本实验建立硬尖神香草药材特征图谱方法,主要色谱峰的分离度良好,330 nm处吸收较好,基线平稳,峰个数多且峰形较好,因此选择330 nm作为检测波长;流动相分别选用甲醇、乙腈与0.2%甲酸水、0.1%磷酸水配比,结果乙腈-0.1%磷酸水作为流动相色谱峰峰形尖锐且分离良好,基线平稳,故确定有机相为乙腈,水相为0.1%磷酸水。优化梯度洗脱条件,在此色谱条件下硬尖神香草与大苞荆芥均有良好分离。
10批硬尖神香草药材色谱图中呈现15个共有峰,通过与对照品峰保留时间及紫外吸收情况比对,指认出6个峰,其他峰的指认尚需继续进行。特征图谱结合多种化学模式识别方法[19-20],进行了深入的数据分析,首先,硬尖神香草的野生品种与种植品种从整体轮廓到特征峰相对含量无明显差异,接下来将结合药效进行综合评价,这一结果可为硬尖神香草的种植提供一定的数据支持。其次,硬尖神香草与其“同名异物”大苞荆芥在此色谱条件下均有良好分离,二者成分存在较大差异,望能为临床应用提供指导。
综上所述,建立的硬尖神香草药材特征图谱方法重复性、稳定性好,具有可操作性。不仅为硬尖神香草的质量控制提供了更全面的信息,并为硬尖神香草药材的真伪鉴别,种质资源优选,种植替代野生及合理开发利用提供了实验数据。
  • *新疆维吾尔自治区自然科学基金资助项目(2022D01E65)
  • “天山英才”培养计划(2023TSYCCX0065)
  • 国家自然科学基金项目(81960752)
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doi: 10.16155/j.0254-1793.2024.06.17
  • 首发时间:2026-03-13
  • 出版时间:2024-06-30
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基金
*新疆维吾尔自治区自然科学基金资助项目(2022D01E65)
“天山英才”培养计划(2023TSYCCX0065)
国家自然科学基金项目(81960752)
作者信息
    1.新疆大学,乌鲁木齐 830046
    2.新疆维吾尔自治区药物研究所,乌鲁木齐 830004
    3.新疆生产建设兵团食品药品审评核查中心,乌鲁木齐 831400

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张兰兰 Tel:18199127303;E-mail:
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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
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