Article(id=1206272757277454694, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-1039, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1723392000000, receivedDateStr=2024-08-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1765527436798, onlineDateStr=2025-12-12, pubDate=null, pubDateStr=null, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1765527436798, onlineIssueDateStr=2025-12-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1765527436798, creator=13701087609, updateTime=1765527436798, updator=13701087609, issue=Issue{id=1206272755658453329, tenantId=1146029695717560320, journalId=1205117023404326918, year='2025', volume='45', issue='5', pageStart='739', pageEnd='920', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=0, createTime=1765527436411, creator=13701087609, updateTime=1765531454840, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1206289610234196753, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1206289610234196754, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=821, endPage=832, ext={EN=ArticleExt(id=1206272757436838251, articleId=1206272757277454694, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Application of TRSDMC method for the determination of 5 components in Moslae Herba, columnId=1206272756333736276, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Ingredient Analysis, runingTitle=null, highlight=null, articleAbstract=

Objective: To establish a two reference substances for determination of multiple components (TRSDMC)method for the simultaneous determination of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in Moslae Herba, which was more economical and effective for the quality control of Moslae Herba. Methods: The retention times of the five components in Moslae Herba were determined using HPLC on 13 different C18 columns. The average retention time of each component under each column was then used as the standard retention time for that component.Rosmarinic acid (peak 2) and carvacrol (peak 4) were chosen as linear calibration standards. The chromatographic peaks were localized by using liner calibration with two reference substances (LCTRS). Rosmarinic acid was used as the control substance to determine the content of each component using a relative correction factor. And the results were compared with those obtained from the external standard method. Chemometric analysis was used to excavate the differential quality markers of Moslae Herba. Results: LCTRS had accurate prediction results for the measured components and enjoyed a wide range of column applications. The correction factors of scutellarin, negletein, carvacrol and thymol to rosmarinic acid were 0.853 3, 0.475 2, 3.034 7 and 2.738 6, respectively, and their relative standard deviations were below 2.0%.There was no significant difference between contents obtained by the two methods. The contents of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in 21 batches of Moslae Herba were 0.05-2.87 mg · g-1, 0.73-9.73 mg · g-1, 0.04-0.99 mg · g-1, 0.36-8.52 mg · g-1 and 0.61-10.2 7 mg · g-1, respectively. The 24 batches of samples could be clustered into three categories, and thymol, carvacrol and negletein ether could be used as differential quality markers. Conclusion: TSDMC method for the simultaneous determination of the contents of 5 components in Moslae Herba is stable and reliable, and provides a new idea for the overall quality control of Moslae Herba.

, correspAuthors=Lin-chun WAN, Feng WEI, 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=Li-qin LIU, Zai-ping XU, Wen-yan FU, Ming-ming YUAN, Wen ZHAO, Xin-kai YANG, Lin-chun WAN, Feng WEI), CN=ArticleExt(id=1206272758527357368, articleId=1206272757277454694, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=双标多测法在香薷5个成分含量测定中的应用*, columnId=1206272756476342615, journalTitle=药物分析杂志, columnName=成分分析, runingTitle=null, highlight=null, articleAbstract=

目的:建立双标多测(TRSDMC)法同时测定香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚5个成分的含量,更加经济有效地对香薷进行质量控制研究。方法:采用HPLC法,在13根不同型号的C18色谱柱上测定香薷5个成分的实际保留时间,以各成分在各色谱柱下的平均保留时间为各组分的标准保留时间。选取迷迭香酸(峰2)和香荆芥酚(峰4)作为双标化合物,使用双标线性校正(LCTRS)法进行色谱峰定位;以迷迭香酸为对照,用相对校正因子测定各成分含量,并与外标法(ESM)测定结果进行比较;采用化学计量学方法分析香薷差异性质量标志物。结果:LCTRS法对待测组分的预测结果准确且色谱柱适用范围广;野黄芩苷、黄芩素-7-甲醚、香荆芥酚和麝香草酚相对于迷迭香酸的校正因子分别为0.853 3、0.475 2、3.034 7、2.738 6,其RSD均在2.0%以内,2种方法计算的含量值无明显差异。24批香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆草酚、麝香草酚的含量分别为0.05~2.87、0.73~9.73、0.04~0.99、0.36~8.52、0.61~10.27 mg · g-1。24批香薷样品可以聚为3类,麝香草酚、香荆芥酚、黄芩素-7-甲醚为香薷的差异性质量标志物。结论:本文建立的同时测定香薷中5个成分含量的TRSDMC法稳定、可靠,可为香薷的整体质量控制提供新的思路。

, correspAuthors=万林春, 魏峰, authorNote=null, correspAuthorsNote=
** 万林春 Tel:(0791)86176095;E-mail:;
魏峰 Tel:(010)67095432;E-mail:
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刘丽琴 Tel:18857164578;E-mail:

徐载萍 Tel:13767494657;E-mail:

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刘丽琴 Tel:18857164578;E-mail:

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1. 野黄芩苷(scutellarin) 2. 迷迭香酸(rosmarinic acid) 3. 黄芩素-7-甲醚(negletein) 4. 香荆芥酚(carvacrol) 5. 麝香草酚(thymol)

, figureFileSmall=iU+PmWXGw5FFj3R+Ev8pjA==, figureFileBig=uHWsBuAoexqNGyt4CEfZ6w==, tableContent=null), ArticleFig(id=1206300931088511550, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Fig. 2, caption=HCA of 24 batches of Moslae Herba sample, figureFileSmall=BrA5Yc7c5q/qtz5SkETnCg==, figureFileBig=gNY8gx5AwoI2QMEArot2qg==, tableContent=null), ArticleFig(id=1206300931155620418, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=图2, caption=24批香薷样品HCA图, figureFileSmall=BrA5Yc7c5q/qtz5SkETnCg==, figureFileBig=gNY8gx5AwoI2QMEArot2qg==, tableContent=null), ArticleFig(id=1206300931247895111, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Fig. 3, caption=PCA score plot of 24 batches of Moslae Herba sample, figureFileSmall=l2qlwkEdrjeRtXRrTNWwvA==, figureFileBig=vHxiE6E9flDU1Dl1kZsffw==, tableContent=null), ArticleFig(id=1206300931331781201, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=图3, caption=24批香薷样品PCA得分图, figureFileSmall=l2qlwkEdrjeRtXRrTNWwvA==, figureFileBig=vHxiE6E9flDU1Dl1kZsffw==, tableContent=null), ArticleFig(id=1206300931428250198, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Fig. 4, caption=OPLS-DA score plot of 24 batches of Moslae Herba sample, figureFileSmall=NX9xJAfwILwbGH00NuxEJw==, figureFileBig=QZmyewpq8QfimFZQjr/ttw==, tableContent=null), ArticleFig(id=1206300931520524890, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=图4, caption=24批香薷样品OPLS-DA得分图, figureFileSmall=NX9xJAfwILwbGH00NuxEJw==, figureFileBig=QZmyewpq8QfimFZQjr/ttw==, tableContent=null), ArticleFig(id=1206300931658936927, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Fig. 5, caption=VIP score plot of 24 batches of Moslae Herba sample, figureFileSmall=k5I6D8huqUaqRst2GFwCKw==, figureFileBig=e+eTByY2CNLRrwySuWS1cg==, tableContent=null), ArticleFig(id=1206300931788960361, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=图5, caption=24批香薷样品VIP得分图, figureFileSmall=k5I6D8huqUaqRst2GFwCKw==, figureFileBig=e+eTByY2CNLRrwySuWS1cg==, tableContent=null), ArticleFig(id=1206300931898012269, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 1, caption=

Column information

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)色谱柱型号(column type)生产厂家(manufacturer)
col 1Symmetry C18(250 mm×4. 6 mm,5 μm)Waters
col 2Shimadzu Shim-pack C18(250 mm×4. 6 mm,5 μm)Shimadzu
col 3Zorbax SB C18(250 mm×4. 6 mm,5 μm)Agilent
col 4Intersil ODS-3C18(250 mm×4. 6 mm,5 μm)GL Sciences
col 5HALO C18(250 mm×4. 6 mm,5 μm)Advenced material technolgy
col 6XbridgeC18(250 mm×4. 6 mm,5 μm)Waters
col 7Phenomenex Luna C18(250 mm×4. 6 mm,5 μm)Phenomenex
col 8Titank C18(250 mm×4. 6 mm,5 μm)广州菲罗门科学仪器有限公司(Guangzhou FLM)
col 9Acclaimtm C18(250 mm×4. 6 mm,5 μm)Thermo
col 10capcell pak C18(250 mm×4. 6 mm,5 μm)Shiseido
col 11Eclipse plusC18(250 mm×4. 6 mm,5 μm)Agilent
col 12Eclipse XDB-C18(250 mm×4. 6 mm,5 μm)Agilent
col 13Acclaimtm C18(250 mm×4. 6 mm,5 μm)Thermo
col 14Agilent 5 HC C18(250 mm×4. 6 mm,5 μm)Agilent
), ArticleFig(id=1206300931990286963, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表1, caption=

色谱柱信息

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)色谱柱型号(column type)生产厂家(manufacturer)
col 1Symmetry C18(250 mm×4. 6 mm,5 μm)Waters
col 2Shimadzu Shim-pack C18(250 mm×4. 6 mm,5 μm)Shimadzu
col 3Zorbax SB C18(250 mm×4. 6 mm,5 μm)Agilent
col 4Intersil ODS-3C18(250 mm×4. 6 mm,5 μm)GL Sciences
col 5HALO C18(250 mm×4. 6 mm,5 μm)Advenced material technolgy
col 6XbridgeC18(250 mm×4. 6 mm,5 μm)Waters
col 7Phenomenex Luna C18(250 mm×4. 6 mm,5 μm)Phenomenex
col 8Titank C18(250 mm×4. 6 mm,5 μm)广州菲罗门科学仪器有限公司(Guangzhou FLM)
col 9Acclaimtm C18(250 mm×4. 6 mm,5 μm)Thermo
col 10capcell pak C18(250 mm×4. 6 mm,5 μm)Shiseido
col 11Eclipse plusC18(250 mm×4. 6 mm,5 μm)Agilent
col 12Eclipse XDB-C18(250 mm×4. 6 mm,5 μm)Agilent
col 13Acclaimtm C18(250 mm×4. 6 mm,5 μm)Thermo
col 14Agilent 5 HC C18(250 mm×4. 6 mm,5 μm)Agilent
), ArticleFig(id=1206300932065784440, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 2, caption=

Source information of 24 batches of Moslae Herba sample

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)产地(origin)批号(batch No.)
Y1江西余江(Yujiang,Jiangxi)20240301
Y2江西余江(Yujiang,Jiangxi)2310003
Y3江西余江(Yujiang,Jiangxi)2311003
Y4江西余江(Yujiang,Jiangxi)2312001
Y5江西新余(Xinyu,Jiangxi)2312002
Y6江西弋阳(Yiyang,Jiangxi)20240302
Y7江西弋阳(Yiyang,Jiangxi)2312003
Y8江西抚州(Fuzhou,Jiangxi)2312006
Y9江西上饶(Shangrao,Jiangxi)2312005
Y10江西鹰潭(Yingtan,Jiangxi)2401002
Y11湖北(Hubei)20240303
Y12浙江(Zhejiang)20240304
Y13湖南新宁(Xinning,Hunan)20240305
Y14湖南邵阳(Shaoyang,Hunan)2312004
Y15湖南邵阳(Shaoyang,Hunan)2311001
Y16江西余江(Yujiang,Jiangxi)20240601
Y17湖南邵阳(Shaotang,Hunan)20240602
Y18江西弋阳(Yiyang,Jiangxi)20240604
Y19江西(Jiangxi)20240501
Y20江西(Jiangxi)20240701
Y21湖北(Hubei)20240502
Y22湖北(Hubei)20240702
Y23湖南(Hunan)20240703
Y24四川(Sichuan)24240704
), ArticleFig(id=1206300932145476217, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表2, caption=

24批香薷样品来源信息

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)产地(origin)批号(batch No.)
Y1江西余江(Yujiang,Jiangxi)20240301
Y2江西余江(Yujiang,Jiangxi)2310003
Y3江西余江(Yujiang,Jiangxi)2311003
Y4江西余江(Yujiang,Jiangxi)2312001
Y5江西新余(Xinyu,Jiangxi)2312002
Y6江西弋阳(Yiyang,Jiangxi)20240302
Y7江西弋阳(Yiyang,Jiangxi)2312003
Y8江西抚州(Fuzhou,Jiangxi)2312006
Y9江西上饶(Shangrao,Jiangxi)2312005
Y10江西鹰潭(Yingtan,Jiangxi)2401002
Y11湖北(Hubei)20240303
Y12浙江(Zhejiang)20240304
Y13湖南新宁(Xinning,Hunan)20240305
Y14湖南邵阳(Shaoyang,Hunan)2312004
Y15湖南邵阳(Shaoyang,Hunan)2311001
Y16江西余江(Yujiang,Jiangxi)20240601
Y17湖南邵阳(Shaotang,Hunan)20240602
Y18江西弋阳(Yiyang,Jiangxi)20240604
Y19江西(Jiangxi)20240501
Y20江西(Jiangxi)20240701
Y21湖北(Hubei)20240502
Y22湖北(Hubei)20240702
Y23湖南(Hunan)20240703
Y24四川(Sichuan)24240704
), ArticleFig(id=1206300932309054078, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 3, caption=

Linear range of five components

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)
线性方程
(linear equation)
r线性范围
(linear range)/(μg · mL-1
野黄芩苷(scutellarin)Y=0.401 1 X-0.053 71.0002.118 2~84.729
迷迭香酸(rosmarinic acid)Y=0.351 5 X+0.099 61.0005.617 4~224.697 6
黄芩素-7-甲醚(negletein)Y=0.746 4 X-0.160 40.999 81.842 4~73.696
香荆芥酚(carvacrol)Y=0.115 9 X+0.102 30.999 63.622 6~144.906
麝香草酚(thymol)Y=0.127 8 X+0.058 71.000 14.967~588.680 7
), ArticleFig(id=1206300932405523073, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表3, caption=

5个成分线性范围

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)
线性方程
(linear equation)
r线性范围
(linear range)/(μg · mL-1
野黄芩苷(scutellarin)Y=0.401 1 X-0.053 71.0002.118 2~84.729
迷迭香酸(rosmarinic acid)Y=0.351 5 X+0.099 61.0005.617 4~224.697 6
黄芩素-7-甲醚(negletein)Y=0.746 4 X-0.160 40.999 81.842 4~73.696
香荆芥酚(carvacrol)Y=0.115 9 X+0.102 30.999 63.622 6~144.906
麝香草酚(thymol)Y=0.127 8 X+0.058 71.000 14.967~588.680 7
), ArticleFig(id=1206300932506186372, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 4, caption=

Relative correction factor

, figureFileSmall=null, figureFileBig=null, tableContent=
混合对照品溶液
(mixed reference substance solution)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
0.854 30.473 83.015 12.738 5
0.857 30.473 83.004 52.722 7
0.831 40.477 12.997 12.733 6
0.861 70.479 33.038 72.753 9
0.864 00.482 03.028 22.748 1
0.851 00.465 33.124 52.734 6
均值(mean)0.853 30.475 23.034 72.738 6
RSD/%1.41.21.50.41
), ArticleFig(id=1206300932669764234, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表4, caption=

相对校正因子

, figureFileSmall=null, figureFileBig=null, tableContent=
混合对照品溶液
(mixed reference substance solution)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
0.854 30.473 83.015 12.738 5
0.857 30.473 83.004 52.722 7
0.831 40.477 12.997 12.733 6
0.861 70.479 33.038 72.753 9
0.864 00.482 03.028 22.748 1
0.851 00.465 33.124 52.734 6
均值(mean)0.853 30.475 23.034 72.738 6
RSD/%1.41.21.50.41
), ArticleFig(id=1206300932736873102, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 5, caption=

Relative correction factor durability of different instruments and columns

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
(instrument)
色谱柱
(column)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarincacid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
Ultimate 3000col 10.844 11.0000.480 53.038 72.753 9
col 20.866 21.0000.472 53.041 92.727 3
col 30.869 01.0000.491 53.076 12.792 2
col 40.845 01.0000.483 02.994 42.755 7
col 50.845 61.0000.494 73.091 62.757 0
col 60.873 71.0000.496 93.055 72.778 3
col 70.831 61.0000.488 92.978 82.719 6
col 80.850 81.0000.487 53.051 32.787 0
col 90.847 11.0000.472 53.041 92.727 3
col 100.853 01.0000.468 03.007 52.792 2
col 110.848 61.0000.493 13.013 72.735 5
col 120.860 31.0000.483 22.886 62.725 8
col 130.852 21.0000.499 33.044 92.803 3
Agilent 1260 Infinity Ⅱcol 10.852 01.0000.494 33.057 72.709 8
col 20.857 01.0000.483 93.032 12.880 8
col 30.870 81.0000.478 02.942 52.675 4
col 40.876 41.0000.487 33.013 22.728 1
col 50.869 31.0000.485 92.938 72.720 0
col 60.844 71.0000.479 53.089 12.769 0
col 70.856 71.0000.497 93.037 72.694 7
col 80.867 41.0000.509 23.006 22.737 7
col 90.875 71.0000.497 03.083 22.576 9
col 100.856 91.0000.492 43.046 12.647 8
col 110.872 51.0000.476 93.080 82.708 7
col 120.876 91.0000.498 03.012 22.768 4
col 130.856 91.0000.484 93.141 62.710 5
LC-20ATcol 10.835 71.0000.496 83.049 12.745 7
col 20.848 41.0000.497 63.073 92.776 4
col 30.864 11.0000.504 32.971 32.774 4
col 40.869 51.0000.492 63.018 02.707 2
col 50.885 21.0000.490 22.935 22.753 5
col 60.859 01.0000.488 43.064 02.735 2
col 70.839 31.0000.491 32.906 42.743 2
col 80.865 81.0000.489 23.090 42.788 0
col 90.865 41.0000.480 22.948 42.738 0
col 100.863 91.0000.496 63.024 52.629 5
col 110.882 51.0000.496 83.036 62.766 6
col 120.873 71.0000.505 23.021 32.733 1
col 130.848 11.0000.500 53.075 52.762 2
均值(mean)0.861.000.493.032.74
RSD/%1.501.91.81.8
), ArticleFig(id=1206300932816564883, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表5, caption=

不同仪器和色谱柱的相对校正因子耐用性

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
(instrument)
色谱柱
(column)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarincacid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
Ultimate 3000col 10.844 11.0000.480 53.038 72.753 9
col 20.866 21.0000.472 53.041 92.727 3
col 30.869 01.0000.491 53.076 12.792 2
col 40.845 01.0000.483 02.994 42.755 7
col 50.845 61.0000.494 73.091 62.757 0
col 60.873 71.0000.496 93.055 72.778 3
col 70.831 61.0000.488 92.978 82.719 6
col 80.850 81.0000.487 53.051 32.787 0
col 90.847 11.0000.472 53.041 92.727 3
col 100.853 01.0000.468 03.007 52.792 2
col 110.848 61.0000.493 13.013 72.735 5
col 120.860 31.0000.483 22.886 62.725 8
col 130.852 21.0000.499 33.044 92.803 3
Agilent 1260 Infinity Ⅱcol 10.852 01.0000.494 33.057 72.709 8
col 20.857 01.0000.483 93.032 12.880 8
col 30.870 81.0000.478 02.942 52.675 4
col 40.876 41.0000.487 33.013 22.728 1
col 50.869 31.0000.485 92.938 72.720 0
col 60.844 71.0000.479 53.089 12.769 0
col 70.856 71.0000.497 93.037 72.694 7
col 80.867 41.0000.509 23.006 22.737 7
col 90.875 71.0000.497 03.083 22.576 9
col 100.856 91.0000.492 43.046 12.647 8
col 110.872 51.0000.476 93.080 82.708 7
col 120.876 91.0000.498 03.012 22.768 4
col 130.856 91.0000.484 93.141 62.710 5
LC-20ATcol 10.835 71.0000.496 83.049 12.745 7
col 20.848 41.0000.497 63.073 92.776 4
col 30.864 11.0000.504 32.971 32.774 4
col 40.869 51.0000.492 63.018 02.707 2
col 50.885 21.0000.490 22.935 22.753 5
col 60.859 01.0000.488 43.064 02.735 2
col 70.839 31.0000.491 32.906 42.743 2
col 80.865 81.0000.489 23.090 42.788 0
col 90.865 41.0000.480 22.948 42.738 0
col 100.863 91.0000.496 63.024 52.629 5
col 110.882 51.0000.496 83.036 62.766 6
col 120.873 71.0000.505 23.021 32.733 1
col 130.848 11.0000.500 53.075 52.762 2
均值(mean)0.861.000.493.032.74
RSD/%1.501.91.81.8
), ArticleFig(id=1206300934037107351, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 6, caption=

Influence of other factors on relative correction factor

, figureFileSmall=null, figureFileBig=null, tableContent=
实验条件
(experimental condition)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarinic acid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
流速(flow rate)/(mL · min-10.80.845 71.0000.497 53.030 22.761 0
10.845 31.0000.483 73.088 12.789 7
1.20.851 61.0000.490 93.094 02.756 1
柱温(column temperature)/℃280.849 11.0000.485 83.000 22.747 1
320.854 01.0000.481 12.934 32.736 5
波长(wavelength)/nm329、2740.851 61.0000.485 83.081 62.715 2
331、2760.866 71.0000.480 12.993 72.721 2
均值(mean)0.851.000.493.032.75
RSD/%0.8501.22.00.93
), ArticleFig(id=1206300934158742171, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表6, caption=

其他因素对相对校正因子的影响

, figureFileSmall=null, figureFileBig=null, tableContent=
实验条件
(experimental condition)
相对校正因子(relative correction factor)
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarinic acid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
流速(flow rate)/(mL · min-10.80.845 71.0000.497 53.030 22.761 0
10.845 31.0000.483 73.088 12.789 7
1.20.851 61.0000.490 93.094 02.756 1
柱温(column temperature)/℃280.849 11.0000.485 83.000 22.747 1
320.854 01.0000.481 12.934 32.736 5
波长(wavelength)/nm329、2740.851 61.0000.485 83.081 62.715 2
331、2760.866 71.0000.480 12.993 72.721 2
均值(mean)0.851.000.493.032.75
RSD/%0.8501.22.00.93
), ArticleFig(id=1206300934301348513, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 7, caption=

Linear equations of different chromatographic columns

, figureFileSmall=null, figureFileBig=null, tableContent=
色谱柱(column)线性方程(linear equation)r
col 1Y=1.001 9 X-0.195 10.999 8
col 2Y=1.032 9 X+0.143 60.999 1
col 3Y=0.954 4 X+0.907 30.999 4
col 4Y=0.988 3 X+0.674 60.999 2
col 5Y=1.008 4 X-0.497 20.999 7
col 6Y=0.996 6 X-0.568 90.999 6
col 7Y=0.961 4 X+2.725 10.999 7
col 8Y=0.988 9 X+0.594 60.999 3
col 9Y=1.005 3 X-0.176 90.999 0
col 10Y=0.925 X+3.893 70.999 5
col 11Y=0.967 7 X+1.983 50.999 3
col 12Y=0.985 9 X+0.191 40.999 2
col 13Y=1.002 7 X-1.931 40.999 3
), ArticleFig(id=1206300934402011811, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表7, caption=

不同色谱柱线性方程

, figureFileSmall=null, figureFileBig=null, tableContent=
色谱柱(column)线性方程(linear equation)r
col 1Y=1.001 9 X-0.195 10.999 8
col 2Y=1.032 9 X+0.143 60.999 1
col 3Y=0.954 4 X+0.907 30.999 4
col 4Y=0.988 3 X+0.674 60.999 2
col 5Y=1.008 4 X-0.497 20.999 7
col 6Y=0.996 6 X-0.568 90.999 6
col 7Y=0.961 4 X+2.725 10.999 7
col 8Y=0.988 9 X+0.594 60.999 3
col 9Y=1.005 3 X-0.176 90.999 0
col 10Y=0.925 X+3.893 70.999 5
col 11Y=0.967 7 X+1.983 50.999 3
col 12Y=0.985 9 X+0.191 40.999 2
col 13Y=1.002 7 X-1.931 40.999 3
), ArticleFig(id=1206300934519452329, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 8, caption=

Absolute deviation of predicted values by two methods

, figureFileSmall=null, figureFileBig=null, tableContent=
方法
(method)
色谱柱
(column)
绝对偏差(absolute deviation)/min
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarinic acid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
LCTRScol 10.134 8-0.356 3-0.445 2
col 20.138 0-0.368 9-0.465 6
col 30.099 1-0.342 5-0.429 9
col 40.142 7-0.350 4-0.450 8
col 50.132 2-0.323 2-0.449 9
col 60.128 4-0.299 2-0.422 9
col 70.148 1-0.358 7-0.447 7
col 80.142 3-0.332 8-0.480 6
col 90.131 2-0.336 3-0.416 4
col 100.148 0-0.381 4-0.469 4
col 110.149 2-0.366 0-0.474 0
col 120.135 7-0.354 7-0.463 6
col 130.120 5-0.302 3-0.429 3
相对保留时间法col 10.318 3-0.836 11.000 71.044 0
(relative retention time)col 20.325 8-0.865 50.991 41.091 7
col 30.234 9-0.803 80.971 61.008 3
col 40.336 8-0.822 31.001 21.057 0
col 50.312 2-0.758 70.996 61.054 9
col 60.303 4-0.702 70.994 80.991 9
col 70.349 4-0.841 81.016 21.049 8
col 80.335 9-0.781 31.006 80.819 5
col 90.309 9-0.789 31.014 81.044 8
col 100.349 2-0.894 70.992 81.032 3
col 110.352 0-0.858 81.008 91.043 0
col 120.320 6-0.832 40.982 11.001 6
col 130.284 9-0.709 90.975 20.989 7
), ArticleFig(id=1206300934624309933, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表8, caption=

2种方法预测值的绝对偏差

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方法
(method)
色谱柱
(column)
绝对偏差(absolute deviation)/min
野黄芩苷
(scutellarin)
迷迭香酸
(rosmarinic acid)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
LCTRScol 10.134 8-0.356 3-0.445 2
col 20.138 0-0.368 9-0.465 6
col 30.099 1-0.342 5-0.429 9
col 40.142 7-0.350 4-0.450 8
col 50.132 2-0.323 2-0.449 9
col 60.128 4-0.299 2-0.422 9
col 70.148 1-0.358 7-0.447 7
col 80.142 3-0.332 8-0.480 6
col 90.131 2-0.336 3-0.416 4
col 100.148 0-0.381 4-0.469 4
col 110.149 2-0.366 0-0.474 0
col 120.135 7-0.354 7-0.463 6
col 130.120 5-0.302 3-0.429 3
相对保留时间法col 10.318 3-0.836 11.000 71.044 0
(relative retention time)col 20.325 8-0.865 50.991 41.091 7
col 30.234 9-0.803 80.971 61.008 3
col 40.336 8-0.822 31.001 21.057 0
col 50.312 2-0.758 70.996 61.054 9
col 60.303 4-0.702 70.994 80.991 9
col 70.349 4-0.841 81.016 21.049 8
col 80.335 9-0.781 31.006 80.819 5
col 90.309 9-0.789 31.014 81.044 8
col 100.349 2-0.894 70.992 81.032 3
col 110.352 0-0.858 81.008 91.043 0
col 120.320 6-0.832 40.982 11.001 6
col 130.284 9-0.709 90.975 20.989 7
), ArticleFig(id=1206300934737556146, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=EN, label=Tab. 9, caption=

Results of 24 batches of Moslae Herba sample obtained by ESM and TRSDMC method

, figureFileSmall=null, figureFileBig=null, tableContent=
编号
(No.)
含量(content)/(mg · g-1n=2)
野黄芩苷
(scutellarin)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
迷迭香酸
(rosmarinic acid)
ESMTRSDMCESMTRSDMCESMTRSDMCESMTRSDMCESM
Y10.820.830.160.160.590.591.811.839.73
Y22.872.930.991.011.531.5410.2710.386.68
Y30.110.110.070.071.281.282.382.391.46
Y40.600.610.160.171.230.231.891.915.02
Y50.650.660.180.183.163.173.543.588.95
Y61.391.410.870.891.381.397.457.533.57
Y70.170.180.240.240.580.585.065.120.99
Y82.852.910.140.151.141.150.610.629.2
Y90.320.410.10.12.582.571.391.364.59
Y103.023.070.850.878.528.542.462.489.42
Y110.930.950.310.321.281.291.261.296.47
Y121.851.880.800.810.870.884.294.343.97
Y130.981.000.570.581.051.068.118.154.74
Y140.070.070.040.040.560.561.531.540.73
Y152.172.210.840.853.763.779.329.413.72
Y160.540.550.680.692.382.396.396.455.38
Y170.840.860.390.390.650.657.988.078.13
Y180.490.500.550.561.811.814.894.946.32
Y190.650.660.480.480.650.664.124.194.98
Y200.800.810.300.311.061.072.632.735.27
Y210.130.130.330.330.700.713.573.654.17
Y220.800.810.280.290.520.522.222.265.01
Y230.530.540.310.320.360.373.293.364.25
Y240.050.060.100.110.470.323.653.744.19
), ArticleFig(id=1206300934842413749, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272757277454694, language=CN, label=表9, caption=

24批香薷样品ESM与TRSDMC法测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
编号
(No.)
含量(content)/(mg · g-1n=2)
野黄芩苷
(scutellarin)
黄芩素-7-甲醚
(negletein)
香荆芥酚
(carvacrol)
麝香草酚
(thymol)
迷迭香酸
(rosmarinic acid)
ESMTRSDMCESMTRSDMCESMTRSDMCESMTRSDMCESM
Y10.820.830.160.160.590.591.811.839.73
Y22.872.930.991.011.531.5410.2710.386.68
Y30.110.110.070.071.281.282.382.391.46
Y40.600.610.160.171.230.231.891.915.02
Y50.650.660.180.183.163.173.543.588.95
Y61.391.410.870.891.381.397.457.533.57
Y70.170.180.240.240.580.585.065.120.99
Y82.852.910.140.151.141.150.610.629.2
Y90.320.410.10.12.582.571.391.364.59
Y103.023.070.850.878.528.542.462.489.42
Y110.930.950.310.321.281.291.261.296.47
Y121.851.880.800.810.870.884.294.343.97
Y130.981.000.570.581.051.068.118.154.74
Y140.070.070.040.040.560.561.531.540.73
Y152.172.210.840.853.763.779.329.413.72
Y160.540.550.680.692.382.396.396.455.38
Y170.840.860.390.390.650.657.988.078.13
Y180.490.500.550.561.811.814.894.946.32
Y190.650.660.480.480.650.664.124.194.98
Y200.800.810.300.311.061.072.632.735.27
Y210.130.130.330.330.700.713.573.654.17
Y220.800.810.280.290.520.522.222.265.01
Y230.530.540.310.320.360.373.293.364.25
Y240.050.060.100.110.470.323.653.744.19
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双标多测法在香薷5个成分含量测定中的应用*
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刘丽琴 1 , 徐载萍 2 , 付文艳 3 , 袁铭铭 2 , 赵雯 2 , 杨莘锴 2 , 万林春 2, ** , 魏峰 4, **
药物分析杂志 | 成分分析 2025,45(5): 821-832
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药物分析杂志 | 成分分析 2025, 45(5): 821-832
双标多测法在香薷5个成分含量测定中的应用*
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刘丽琴1 , 徐载萍2 , 付文艳3, 袁铭铭2, 赵雯2, 杨莘锴2, 万林春2, ** , 魏峰4, **
作者信息
  • 1.杭州市红十字会医院,杭州 310015
  • 2.江西省药品检验检测研究院 国家药品监督管理局中成药质量评价重点实验室江西省药品与医疗器械质量工程技术研究中心,南昌 330029
  • 3.南昌大学第二附属医院,南昌 330006
  • 4.中国食品药品检定研究院,北京 102629
  • 刘丽琴 Tel:18857164578;E-mail:

    徐载萍 Tel:13767494657;E-mail:

通讯作者:

** 万林春 Tel:(0791)86176095;E-mail:;
魏峰 Tel:(010)67095432;E-mail:
Application of TRSDMC method for the determination of 5 components in Moslae Herba
Li-qin LIU1 , Zai-ping XU2 , Wen-yan FU3, Ming-ming YUAN2, Wen ZHAO2, Xin-kai YANG2, Lin-chun WAN2, ** , Feng WEI4, **
Affiliations
  • 1. Hangzhou Red Cross Hospital, Hangzhou 310015, China
  • 2. Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality, NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine, Jiangxi Institute for Drug Control, Nanchang 330029, China
  • 3. The Second Affiliated Hospital of Nanchang University,Nanchang 330006, China
  • 4. National Institutes for Food and Drug Control, Beijing 102629, China
doi: 10.16155/j.0254-1793.2024-1039
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目的:建立双标多测(TRSDMC)法同时测定香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚5个成分的含量,更加经济有效地对香薷进行质量控制研究。方法:采用HPLC法,在13根不同型号的C18色谱柱上测定香薷5个成分的实际保留时间,以各成分在各色谱柱下的平均保留时间为各组分的标准保留时间。选取迷迭香酸(峰2)和香荆芥酚(峰4)作为双标化合物,使用双标线性校正(LCTRS)法进行色谱峰定位;以迷迭香酸为对照,用相对校正因子测定各成分含量,并与外标法(ESM)测定结果进行比较;采用化学计量学方法分析香薷差异性质量标志物。结果:LCTRS法对待测组分的预测结果准确且色谱柱适用范围广;野黄芩苷、黄芩素-7-甲醚、香荆芥酚和麝香草酚相对于迷迭香酸的校正因子分别为0.853 3、0.475 2、3.034 7、2.738 6,其RSD均在2.0%以内,2种方法计算的含量值无明显差异。24批香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆草酚、麝香草酚的含量分别为0.05~2.87、0.73~9.73、0.04~0.99、0.36~8.52、0.61~10.27 mg · g-1。24批香薷样品可以聚为3类,麝香草酚、香荆芥酚、黄芩素-7-甲醚为香薷的差异性质量标志物。结论:本文建立的同时测定香薷中5个成分含量的TRSDMC法稳定、可靠,可为香薷的整体质量控制提供新的思路。

香薷  /  相对校正因子  /  双标多测法  /  双标线性校正法  /  含量测定

Objective: To establish a two reference substances for determination of multiple components (TRSDMC)method for the simultaneous determination of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in Moslae Herba, which was more economical and effective for the quality control of Moslae Herba. Methods: The retention times of the five components in Moslae Herba were determined using HPLC on 13 different C18 columns. The average retention time of each component under each column was then used as the standard retention time for that component.Rosmarinic acid (peak 2) and carvacrol (peak 4) were chosen as linear calibration standards. The chromatographic peaks were localized by using liner calibration with two reference substances (LCTRS). Rosmarinic acid was used as the control substance to determine the content of each component using a relative correction factor. And the results were compared with those obtained from the external standard method. Chemometric analysis was used to excavate the differential quality markers of Moslae Herba. Results: LCTRS had accurate prediction results for the measured components and enjoyed a wide range of column applications. The correction factors of scutellarin, negletein, carvacrol and thymol to rosmarinic acid were 0.853 3, 0.475 2, 3.034 7 and 2.738 6, respectively, and their relative standard deviations were below 2.0%.There was no significant difference between contents obtained by the two methods. The contents of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in 21 batches of Moslae Herba were 0.05-2.87 mg · g-1, 0.73-9.73 mg · g-1, 0.04-0.99 mg · g-1, 0.36-8.52 mg · g-1 and 0.61-10.2 7 mg · g-1, respectively. The 24 batches of samples could be clustered into three categories, and thymol, carvacrol and negletein ether could be used as differential quality markers. Conclusion: TSDMC method for the simultaneous determination of the contents of 5 components in Moslae Herba is stable and reliable, and provides a new idea for the overall quality control of Moslae Herba.

Moslae Herba  /  relative correction factor  /  two reference substances for determination of multiple components(TRSDMC) method  /  linear calibration using two-reference substances(LCTRS) method  /  content determination
刘丽琴, 徐载萍, 付文艳, 袁铭铭, 赵雯, 杨莘锴, 万林春, 魏峰. 双标多测法在香薷5个成分含量测定中的应用*. 药物分析杂志, 2025 , 45 (5) : 821 -832 . DOI: 10.16155/j.0254-1793.2024-1039
Li-qin LIU, Zai-ping XU, Wen-yan FU, Ming-ming YUAN, Wen ZHAO, Xin-kai YANG, Lin-chun WAN, Feng WEI. Application of TRSDMC method for the determination of 5 components in Moslae Herba[J]. Chinese Journal of Pharmaceutical Analysis, 2025 , 45 (5) : 821 -832 . DOI: 10.16155/j.0254-1793.2024-1039
香薷为唇形科植物石香薷Mosla chinensis Maxim.或江香薷Mosla chinensis ‘Jiangxiangru’的干燥地上部分,最早见于《名医别录》[1]。作为一种药食两用的中药材[2],香薷具有发汗解暑、行水散湿、利水消肿之功效,古代临床主要用于治疗暑湿症[3]。随着研究的深入,香薷中的化学成分不断被发现,目前已有研究证实香薷中富含挥发油类成分、黄酮类成分及酚酸类成分。其中香荆芥酚、麝香草酚作为香薷中挥发油成分[4],具有扩张血管、增强免疫力等功效[5-6];酚酸类成分迷迭香酸和黄酮类成分野黄芩苷、黄芩素-7-甲醚,具有抗菌、抗病毒、抗炎作用[7] 。不同成分从整体体现了香薷不同功效的物质基础,故本文以24批香薷为研究对象,对其进行质量控制评价。
2020年版《中华人民共和国药典》检识香薷的质量评价标准仅聚焦于2个关键指标性成分——麝香草酚与香荆芥酚[8-9]。近年来,中药的品质评价方法逐渐向整体化和多成分化方向发展,中药材、配方颗粒及中成药质量控制广泛采用了指纹图谱法和特征图谱法等方法。叶梦倩等[10]采用指纹图谱对不同基原香薷药材的质量控制提供研究基础;李文霞等[11]建立了特征图谱对江香薷饮片进行质量评价;张依欣等[12]采用HPLC法同时测定不同产地香薷药材中的7个化学成分。在追求实验经济性与效率的背景下,孙磊等[13-15]提出了一项创新技术——双标多测(TRSDMC)法。该技术在传统替代对照品法的基础上,增加1个对照品用于双重标准的线性校正,优化了色谱峰的定性分析过程。与文献[9-11]相比,本研究采用TRSDMC法测定香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚5个成分的含量。在一测多评的基础上,增加另外1种对照品定性,不仅提升了定性分析的精确度,而且增强了色谱柱的适用性,使保留时间预测更为精准;采用2种对照品测定5个成分的含量,可极大地节约检验成本。
Ultimate 3000液相色谱仪(戴安公司);Agilent 1260 Infinity Ⅱ型液相色谱仪(安捷伦科技有限公司);LC-20AT型液相色谱仪(岛津公司);ME204TE/02万分之一电子天平(梅特勒-托利多仪器有限公司);SECURA125-1CN十万分之一电子天平(赛多利斯公司);KQ-500DE超声波清洗器(昆山市超声仪器有限公司)。14根色谱柱信息见表1
对照品野黄芩苷(批号110842-202411,含量91.0%)、迷迭香酸(批号111871-202408,含量99.6%)、香荆芥酚(批号111691-201704,含量99.6%)、麝香草酚(批号100508-201603,含量99.9%)均购于中国食品药品检定研究院,对照品黄芩素-7-甲醚(批号29550-13-8,含量98.0%)购于上海诗丹德有限公司;乙腈、甲醇为色谱纯,水为超纯水;其余试剂均为分析纯。本次研究收集不同产地的24批次样品来源见表2,经江西药品检验检测研究院万林春副主任中药师鉴定为正品。
采用col 1~col 13色谱柱,以0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~20 min,15%B→20%B;20~20.1 min,20%B→25%B;20.1~40 min,25%B;40~40.1 min,25%B→45%B;40.1~65 min,45%B),流速1.0 mL · min-1,检测波长为330 nm(0~40 min)和275 nm(40~65 min),柱温30 ℃,进样量10 μL。
取野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚的对照品适量,精密称定,加甲醇制成质量浓度分别为 0.211 8、0.187 2、0.184 2、1.207 5、0.498 9 mg · mL-1的对照品储备液;分别精密吸取上述对照品储备液1、3、1、0.3、3 mL,置于同一10 mL量瓶中,加甲醇稀释,摇匀,即得。
取香薷粉末(过2号筛)约1 g,精密称定,置于具塞锥形瓶中,精密加入70%甲醇50 mL,称量,超声(功率250 W,频率 40 kHz)处理30 min,放冷后再次称量,用70%甲醇补足损失的量,摇匀,滤过,取续滤液,即得。
精密吸取混合对照品溶液和供试品溶液各10 μL,使用col 1色谱柱,按照“2.1”项下条件进样测定。结果(图1)表明,各成分峰均具有很好的分离,且不受溶剂的干扰。
取“2.2”项下混合对照品溶液,按“2.1”项下条件重复进样6次测定,计算野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚峰面积的RSD(n=6)为0.12%~0.62%。
精密吸取“2.2”项下混合对照品溶液1、2、5、10、20、40 μL,按“2.1”项下条件进样测定,以质量浓度X(μg · mL-1)为横坐标,峰面积Y为纵坐标进行线性回归,绘制标准曲线,结果见表3。在相应浓度范围内,各成分具有较好的线性关系。
取同一批(批号20240302)香薷样品,先按“2.3”项下方法配制供试品溶液,在“2.1”项色谱条件下进样测定,重复测定6次,按外标法(ESM)计算样品含量,结果香薷中野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚的平均含量分别为1.339 9、3.531 0、0.943 8、1.907 3、7.352 9 mg · g-1,RSD分别为1.2%、1.4%、0.62%、0.24%、0.17%,表明方法重复性良好。
取同一批(批号20240302)香薷样品,先按“2.3”项下方法配制供试品溶液,在“2.1”项色谱条件下,分别于 0、2、4、8、12、24 h进样测定,结果野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚的峰面积在24 h无明显变化,其RSD分别为0.63%、1.6%、1.1%、1.2%、0.74%,表明该方法稳定性好。
取同一批(批号20240302)香薷粉末9份,每份0.5 g,精密称定,置具塞锥形瓶中,按样品总量的80%、100%、120%加入对照品,按“2.3”项下方法配制溶液,照“2.1”项色谱条件进样测定,平行3次,考察回收率。结果野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚的平均回收率依次为102.0%、97.6%、95.6%、98.6%、96.9%,其RSD 分别为1. 7%、1.9%、2.0%、1.7%、1.1%,表明该方法的回收率良好。
精密吸取“2.2”项下混合对照品溶液1、2、5、10、20、40 μL,采用col 1色谱柱,按“2.1”项色谱条件进样测定。分别计算野黄芩苷、黄芩素-7-甲醚、香荆芥酚、麝香草酚相对于迷迭香酸的相对校正因子,结果见表4
考察3台仪器及13根色谱柱,野黄芩苷、迷迭香酸、黄芩素-7-甲醚、香荆芥酚、麝香草酚相对校正因子的RSD均<2.0%,表明在不同仪器及色谱柱上无显著差异,适用性良好(表5)。
在相同的条件下,采用Ultimate 3000液相色谱仪与col 1色谱柱,对流速(0.8、1.0、1.2 mL · min-1)、柱温(28、30、32 ℃)和波长(329、274、331、276 nm)等色谱条件进行考察。结果(表6)显示,相对校正因子的RSD均<2.0%。
本试验的色谱峰定性采用双标线性校正(LCTRS)法,具体原理和方法见文献[16-18]。通过测定对照品的实际保留时间定位色谱峰,得到所有待测成分的实际保留时间。以5个成分在不同色谱柱及不同仪器上的平均保留时间为标准保留时间,结果野黄芩苷、迷迭香酸、黄芩素-7甲醚、香荆芥酚、麝香草酚的标准保留时间依次为18.779、26.866、48.641、58.811、61.375 min。以5个成分的标准保留时间X为横坐标,实际保留时间Y为纵坐标,计算采用各色谱柱的线性方程和相关系数,见表7,可知各成分在不同色谱柱的保留时间呈良好的线性关系。
以col 14色谱柱进行验证。分别精密吸取双标对照品溶液和供试品溶液,进样测定,以迷迭香酸、香荆芥酚标准保留时间(26.866、58.811 min)为横坐标,迷迭香酸、香荆芥酚实际保留时间(26.434、58.183 min)为纵坐标,得到2点线性方程:Y=0.993 9X-0.267 2。再分别将野黄芩苷、黄芩素-7-甲醚、麝香草酚的标准保留时间(18.779、48.641、61.375 min)代入方程,得到相应成分的预测保留时间分别为18.397、48.077、60.733 min,与上述成分的实际保留时间(18.253、48.417、61.183 min)相比较,误差分别为-0.14、0.34、0.45 min。满足预测保留时间与实际保留时间误差应不超过0.5 min的要求[19],表明该方法切实可行。
LCTRS法以迷迭香酸和香荆芥酚作为双标化合物,相对保留时间法以迷迭香酸作为参照物。对得到的保留时间预测值和实际值进行统计,结果见表8。LCTRS法预测值的绝对偏差≤0.5 min,相对保留时间法预测值的绝对偏差≤1.1 min,由此可见,LCTRS法绝对偏差更小,准确度优,具有明显优势。
精密称取24批香薷饮片粉末各1 g,按“2. 3”项下方法制备供试品溶液,按“2. 1”项色谱条件,分别用ESM和TRSDMC法对香薷进行多成分含量测定,并对结果进行比较。2种方法测定的样品含量无显著性差异(RSD均<2.0%),见表9
将24批香薷中5个成分的含量测定结果导入SPSS 26.0软件,以样品编号为个案、各成分含量为变量进行系统聚类分析(HCA),算法采用组间联接法,测度选择平方欧式距离,得到HCA图,见图2。由图2可知,当分类距离为10时,样品大致可以分为3类:Y1、Y3-Y5、Y9、Y11-Y12、Y14、Y19-Y24为第1类,Y2、Y6、Y13、Y15-Y18为第2类,Y10为第3类。从HCA结果结合各个批次的产地归属,发现产地的样品不具备明显的地域性差异,说明不同产地香薷存在着较大的亲缘关系,种植的香薷质量接近。
采用SIMCA 14.1软件对24批香薷中的5个化学成分进行主成分分析(PCA),模型结果见图3。第一主成分的贡献率为50%,第二主成分的贡献率为26.30%,第三主成分的贡献率为14.80%,累计达91.90%,说明这些成分可代表香薷的绝大部分信息;PCA与HCA结果一致,同时所有检测数据无异常(所有数据点均在95%置信区间内),但各散点离散度较大,这可能与24批香薷的有效成分含量存在一定差异有关。为了进一步分析不同批次香薷之间化学成分的差异,采用SIMCA 14.1软件进行正交偏最小二乘判别分析(OPLS-DA),由图4可知,24批样品可分为3类,与PCA和HCA结果一致。再进行变量投影重要度分析(VIP),结果见图5。根据VIP值大小排序,依次为香荆芥酚(1.118 7)、麝香草酚(1.100 4)、黄芩素-7-甲醚(1.081 5)、野黄芩苷(0.907 0)、迷迭香酸(0.738 4),其中,香荆芥酚、麝香草酚和黄芩素-7-甲醚的VIP值均>1,说明这3个组分对香薷整体质量影响较大,后续在香薷质量控制过程中可重点关注,科学合理地进行质量监测。
本试验以香薷为研究对象,对其化学成分进行定性、定量分析。在定性上,采用LCTRS法,实现了对香薷多成分的准确定位。实验结果表明,采用LCTRS法可以更精确地预测各组分在样品中的保留时间,拓宽了色谱柱的使用范围,从而提高了分析的效率。在定量上,采用迷迭香酸对照,用相对校正因子法对指标性成分进行含量测定,并与ESM进行比较,结果发现2种方法的测量值无显著差异。TRSDMC法在香薷的多指标成分定性与定量分析中具有独特的优势,在节约对照品的同时降低检验成本,为香薷的质量控制提供了新思路。TRSDMC法在中药多成分分析方面有较好的应用前景,可进一步将其推广到国家药品抽检、省级药品抽检和药品标准研究等领域,并将其推广到更多的中药品种的质控中,对其进行替代检测方法的研究,以期更好地解决对照品的供求矛盾,更加全面地评价中药的品质,从而全面地保障中药材的品质。
本试验考察了乙腈、甲醇及不同种类、浓度的酸对样品分离的影响,结果发现,乙腈-0.1%磷酸溶液作为流动相时,分离程度最佳,保留时间符合要求。通过紫外吸收光谱进行全波长扫描,发现香薷中各种化学成分对紫外的吸收作用各不相同,其中野黄芩苷、迷迭香酸均在330 nm左右处有最大吸收,黄芩素-7-甲醚、香荆芥酚、麝香草酚在278 nm左右处有最大吸收。因此,在采用LCTRS法对化合物进行定性时,最终确定用280 nm和330 nm双波长进行含量测定。
本试验测定了24批药材,发现不同产地香薷在成分比例上与地域没有呈现明显的相关,香薷总体质量较为稳定。研究中发现同一产地不同批次的野黄芩苷、迷迭香酸、黄芩素-7-甲醚、麝香草酚及香荆芥酚5个成分的含量存在一定的差异,考虑可能与香薷的采收、加工方式贮存等因素有关。本试验采用TRSDMC法,不仅实现了香薷多组分含量的同步检测,而且为香薷的质量控制提供了更加科学、经济、稳定的方法。后续将进一步以药效为导向,深入研究5个主要成分与其内在质量的相关性和贡献度,更为科学合理地选择质控指标。
  • *江西省重点研发计划“揭榜挂帅”项目-江西省中药饮片炮制规范及我省道地药材饮片品质提升研究(20223BBG71001)
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doi: 10.16155/j.0254-1793.2024-1039
  • 接收时间:2024-08-12
  • 首发时间:2025-12-12
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*江西省重点研发计划“揭榜挂帅”项目-江西省中药饮片炮制规范及我省道地药材饮片品质提升研究(20223BBG71001)
作者信息
    1.杭州市红十字会医院,杭州 310015
    2.江西省药品检验检测研究院 国家药品监督管理局中成药质量评价重点实验室江西省药品与医疗器械质量工程技术研究中心,南昌 330029
    3.南昌大学第二附属医院,南昌 330006
    4.中国食品药品检定研究院,北京 102629

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** 万林春 Tel:(0791)86176095;E-mail:;
魏峰 Tel:(010)67095432;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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