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Article(id=1240688784442970245, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2023-0786, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=1718121600000, revisedDateStr=2024-06-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1773732857094, onlineDateStr=2026-03-17, pubDate=1727625600000, pubDateStr=2024-09-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773732857094, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773732857094, creator=13701087609, updateTime=1773732857094, updator=13701087609, issue=Issue{id=1240688783964819588, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='9', pageStart='1463', pageEnd='1645', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773732856979, creator=13701087609, updateTime=1773733032821, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240689521587712627, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240689521587712628, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1597, endPage=1603, ext={EN=ArticleExt(id=1240688784677851272, articleId=1240688784442970245, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Simultaneous determination of nine constituents in Tongshu Koushuang tablets by HPLC, columnId=1206272758774821315, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Standard Deliberation, runingTitle=null, highlight=null, articleAbstract=

Objective: To establish an HPLC method for simultaneous determination of loganic acid, gentiopicroside, hesperidin, paeonol, aloe-emodin, rhein, emodin, chrysophanol and physcion in Tongshu Koushuang tablets (Rhei Radix et Rhizoma, Aurantii Fructus Immaturus and Gentianae Macrophyllae Radix, etc.). Methods: The samples were extracted by refluxing with methanol and the separation was performed on a Thermo Acclaim-C18(250 mm×4.6 mm, 5 μm) column at 30 ℃, with mobile phase consisting of 0.15% phosphoric acid solution and acetonitrile with a gradient elution at a flow rate of 1.0 mL·min-1. The injection volume was 10 μL, and the detection wavelength was set at 236 nm (detecting loganic acid), 280 nm (detecting gentiopicroside, hesperidin and paeonol) and 254 nm (detecting aloe-emodin, rhein, emodin, chrysophanol and physcion). Results: Nine constituents (loganic acid, gentiopicroside, hesperidin, paeonol, aloe-emodin, rhein, emodin, chrysophanol and physcion) were in good linearity within their own ranges (r were 0.999 1-0.999 9), and the average recoveries were 99.6% (RSD=1.9%), 101.1% (RSD=2.0%), 103.0% (RSD=1.5%), 101.6% (RSD=0.51%), 99.8% (RSD=1.4%), 100.9% (RSD=1.4%), 100.8% (RSD=1.8%), 102.7% (RSD=1.2%) and 102.9% (RSD=0.86%), respectively. The content ranges of nine constituents were 1.871-3.517 mg·g-1, 6.274-12.55 mg·g-1, 2.140-3.946 mg·g-1, 1.393-2.018 mg·g-1, 0.394 8-0.807 2 mg·g-1, 0.657 5-1.246 mg·g-1, 0.484 7-0.915 8 mg·g-1, 0.839 8-1.429 mg·g-1 and 0.327 3-0.547 9 mg·g-1, respectively. Conclusion: This simple and accurate method can be used for the quality control and evaluation of Tongshu Koushuang tablets.

, correspAuthors=Yan HE, Li-bin HUANG, 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=Xiao-xiang HU, Yan HE, Qing-li KONG, Li-bin HUANG), CN=ArticleExt(id=1240688785378300047, articleId=1240688784442970245, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=HPLC法同时测定通舒口爽片中9个成分的含量, columnId=1206272758971953622, journalTitle=药物分析杂志, columnName=标准研讨, runingTitle=null, highlight=null, articleAbstract=

目的：采用高效液相色谱（HPLC）技术，建立同时测定通舒口爽片（大黄、枳实、秦艽等）中马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚9个成分的含量。方法：样品经甲醇回流提取后，分析采用Thermo Acclaim-C18（250 mm×4.6 mm，5 μm）色谱柱，流动相为0.15%磷酸(乙腈，梯度洗脱，流速1.0 mL·min-1，柱温30 ℃，进样量10 μL，检测波长为236 nm（检测马钱苷酸）、280 nm（检测龙胆苦苷、橙皮苷、丹皮酚）、254 nm（检测芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚）。结果：马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚在各自线性范围内呈良好的关系（r为0.999 1~0.999 9），平均加样回收率（RSD）分别为99.6%（RSD=1.9%）、101.1%（RSD=2.0%）、100.5%（RSD=1.5%）、101.6%（RSD=0.51%）、99.8%（RSD=1.4%）、100.9%（RSD=1.4%）、100.8%（RSD=1.8%）、102.7%（RSD=1.2%）、102.9%（RSD=0.86%），6批样品中9个成分的含量范围分别为1.871~3.517 mg·g-1、6.274~12.55 mg·g-1、2.140~3.946 mg·g-1、1.393~2.018 mg·g-1、0.394 8~0.807 2 mg·g-1、0.657 5~1.246 mg·g-1、0.484 7~0.915 8 mg·g-1、0.839 8~1.429 mg·g-1、0.327 3~0.547 9 mg·g-1。结论：所建立的方法简单准确，可用于通舒口爽片的质量控制与评价。

, correspAuthors=何艳, 黄丽彬, authorNote=null, correspAuthorsNote=
** 何艳　Tel: (0735)2278323; E-mail: ;
黄丽彬　Tel: (0735)2116279; E-mail:
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Tel: 15873594256; E-mail:

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orderNo=2, keyword=高效液相色谱), Keyword(id=1240704454694072444, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=3, keyword=化学成分), Keyword(id=1240704454803124353, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=4, keyword=马钱苷酸), Keyword(id=1240704454907981962, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=5, keyword=龙胆苦苷), Keyword(id=1240704455004450954, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=6, keyword=橙皮苷), Keyword(id=1240704455117697168, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=7, keyword=丹皮酚), Keyword(id=1240704455189000339, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=8, keyword=芦荟大黄素), Keyword(id=1240704455302246552, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=9, keyword=大黄酸), Keyword(id=1240704455381938332, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=10, keyword=大黄素), Keyword(id=1240704455495184545, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=11, keyword=大黄酚), Keyword(id=1240704455595847851, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=12, keyword=大黄素甲醚), Keyword(id=1240704455683928237, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=13, keyword=含量测定), Keyword(id=1240704455767814320, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, orderNo=14, keyword=质量控制)], 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Chin Tradit Herb Drugs，2020，51(11)：2954, articleTitle=Study on law of quality value transmitting of Artemisiae Scopariae Herba standard decoction, refAbstract=null), Reference(id=1240704462877159792, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, doi=null, pmid=null, pmcid=null, year=2021, volume=39, issue=12, pageStart=124, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=30, authorNames=黄宽, 付鹏, 林艾和, journalName=中华中医药学刊, refType=null, unstructuredReference=黄宽，付鹏，林艾和，等. 不同产地夏枯草HPLC指纹图谱及化学模式识别研究[J]. 中华中医药学刊，2021，39(12)：124, articleTitle=不同产地夏枯草HPLC指纹图谱及化学模式识别研究, refAbstract=null), Reference(id=1240704462965240176, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, doi=null, pmid=null, pmcid=null, year=2021, volume=39, issue=12, pageStart=124, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=31, authorNames=HUANG K, FU P, LIN AH, journalName=Chin Arch Tradit Chin Med, refType=null, unstructuredReference=HUANG K，FU P，LIN AH，et al. Study on HPLC fingerprint and chemical pattern recognition of Xiakucao (Prunella vulgaris) from different producing areas[J]. Chin Arch Tradit Chin Med，2021，39(12)：124, articleTitle=Study on HPLC fingerprint and chemical pattern recognition of Xiakucao (Prunella vulgaris) from different producing areas, refAbstract=null), Reference(id=1240704463078486387, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, doi=null, pmid=null, pmcid=null, year=2021, volume=52, issue=7, pageStart=2082, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=32, authorNames=刘月新, 林艳, 谢菁琛, journalName=中草药, refType=null, unstructuredReference=刘月新，林艳，谢菁琛，等. 基于夏枯草不同生长发育时期化学成分的动态监测阐释“夏枯质优”的科学内涵[J]. 中草药，2021，52(7)：2082, articleTitle=基于夏枯草不同生长发育时期化学成分的动态监测阐释“夏枯质优”的科学内涵, refAbstract=null), Reference(id=1240704463170761078, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, doi=null, pmid=null, pmcid=null, year=2021, volume=52, issue=7, pageStart=2082, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=33, authorNames=LIU YX, LIN Y, XIE JK, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=LIU YX，LIN Y，XIE JK，et al. 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Chin Tradit Herb Drugs，2021，52(7)：2082, articleTitle=Scientific connotation of “summer withering with good quality” based on dynamic monitoring of chemical constituents at different growth and development stages of Prunella vulgaris, refAbstract=null)], funds=[Fund(id=1240704458187927785, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, awardId=2021JJ80023, language=CN, fundingSource=湖南省自然科学基金科药联合项目(2021JJ80023), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1240704449862235061, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, xref=1., ext=[AuthorCompanyExt(id=1240704449870623669, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704449862235061, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.Chenzhou Municipal Center for Food and Drug Control, Chenzhou 423000, China), AuthorCompanyExt(id=1240704449879012279, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704449862235061, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.郴州市食品药品检验检测中心，郴州　423000)]), AuthorCompany(id=1240704449967092673, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, xref=2., ext=[AuthorCompanyExt(id=1240704449975481282, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704449967092673, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.College of Pharmacy, Xiang Nan University, Chenzhou 423000, China), AuthorCompanyExt(id=1240704449979675587, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704449967092673, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.湘南学院药学院，郴州　423000)]), AuthorCompany(id=1240704450067755978, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, xref=3., ext=[AuthorCompanyExt(id=1240704450076144587, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704450067755978, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.Junhong Drug Company of Jilin, Tonghua 135100, China), AuthorCompanyExt(id=1240704450084533197, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, companyId=1240704450067755978, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.吉林省俊宏药业有限公司，通化　135100)])], figs=[ArticleFig(id=1240704455994306749, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=EN, label=Fig.1, caption=The HPLC chromatograms of Tongshu Koushuang tablets, figureFileSmall=wTYXSFg61ik3cRGxNDg5hA==, figureFileBig=R50F6K5NOq8oBwWLkdemCA==, tableContent=null), ArticleFig(id=1240704456094970050, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, label=图1, caption=通舒口爽片HPLC色谱图

1.马钱苷酸（loganic acid）　2.龙胆苦苷（gentiopicroside）　3.橙皮苷（hesperidin）　4.丹皮酚（paeonol）　5.芦荟大黄素（aloe-emodin）　6.大黄酸（rhein）　7.大黄素（emodin）　8.大黄酚（chrysophanol）　9.大黄素甲醚（physcion）

, figureFileSmall=wTYXSFg61ik3cRGxNDg5hA==, figureFileBig=R50F6K5NOq8oBwWLkdemCA==, tableContent=null), ArticleFig(id=1240704456199827654, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=EN, label=Tab.1, caption=

The results of linearity investigation of nine constituents

, figureFileSmall=null, figureFileBig=null, tableContent=
成分（component）回归方程（regression equation）r线性范围（linear range）/（μg·mL-1）
马钱苷酸（loganic acid）Y=12.16X+26.140.999 17.855~78.55
龙胆苦苷（gentiopicroside）Y=12.18X+16.120.999 922.41~224.1
橙皮苷（hesperidin）Y=15.32X-0.561 10.999 96.275~62.75
丹皮酚（paeonol）Y=44.68X-6.9650.999 84.236~42.36
芦荟大黄素（aloe-emodin）Y=46.63X-2.0140.999 91.420~14.20
大黄酸（rhein）Y=33.81X-2.0710.999 91.932~19.32
大黄素（emodin）Y=33.60X-1.7780.999 82.114~21.14
大黄酚（chrysophanol）Y=48.72X-3.9910.999 92.417~24.17
大黄素甲醚（physcion）Y=31.99X-1.2740.999 91.119~11.19
), ArticleFig(id=1240704456296296652, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, label=表1, caption=

9个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）
马钱苷酸（loganic acid）Y=12.16X+26.140.999 17.855~78.55
龙胆苦苷（gentiopicroside）Y=12.18X+16.120.999 922.41~224.1
橙皮苷（hesperidin）Y=15.32X-0.561 10.999 96.275~62.75
丹皮酚（paeonol）Y=44.68X-6.9650.999 84.236~42.36
芦荟大黄素（aloe-emodin）Y=46.63X-2.0140.999 91.420~14.20
大黄酸（rhein）Y=33.81X-2.0710.999 91.932~19.32
大黄素（emodin）Y=33.60X-1.7780.999 82.114~21.14
大黄酚（chrysophanol）Y=48.72X-3.9910.999 92.417~24.17
大黄素甲醚（physcion）Y=31.99X-1.2740.999 91.119~11.19
), ArticleFig(id=1240704457701388497, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=EN, label=Tab.2, caption=

Results of recovery test for nine constituents

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		称样量
(mass)/g		样品量
(amount)/mg		加入量
(added)/mg		测得量
(detected)/mg		回收率
(recovery)/%		平均回收率
(average recovery)/%		RSD/%
马钱苷酸（loganic acid）0.351 21.2491.2682.535101.499.61.9
0.350 41.2461.2682.524100.8
0.351 11.2481.2682.524100.6
0.350 81.2471.2682.50599.2
0.351 61.2501.2682.50899.2
0.350 31.2451.2682.46596.2
龙胆苦苷（gentiopicro side）0.351 23.5443.5557.176102.2101.12.0
0.350 43.5363.5557.04598.7
0.351 13.5433.5557.110100.3
0.350 83.5403.5557.106100.3
0.351 63.5483.5557.120100.5
0.350 33.5353.5557.248104.4
橙皮苷(hesperidin）0.351 21.0291.0242.065101.2100.51.5
0.350 41.0261.0242.064101.4
0.351 11.0281.0242.071101.9
0.350 81.0271.0242.055100.4
0.351 61.0301.0242.058100.4
0.350 31.0261.0242.02597.6
丹皮酚（paeonol）0.351 20.638 80.656 31.304101.4101.60.51
0.350 40.637 40.656 31.305101.7
0.351 10.638 70.656 31.303101.2
0.350 80.638 10.656 31.306101.8
0.351 60.639 60.656 31.312102.5
0.350 30.637 20.656 31.300101.0
芦荟大黄素(aloe-emodin)0.351 20.177 00.184 60.360 099.199.81.4
0.350 40.176 60.184 60.358 298.4
0.351 10.176 90.184 60.359 498.86
0.350 80.176 80.184 60.361 399.9
0.351 60.177 20.184 60.365 8102.2
0.350 30.176 50.184 60.362 1100.5
大黄酸（rhein）0.351 20.282 60.300 20.592 1103.1100.91.4
0.350 40.281 90.300 20.586 4101.4
0.351 10.282 50.300 20.582 399.9
0.350 80.282 30.300 20.580 299.2
0.351 60.282 90.300 20.584 6100.5
0.350 30.281 90.300 20.586 0101.3
大黄素（emodin）0.351 20.218 80.231 20.452 8101.2100.81.8
0.350 40.218 30.231 20.446 698.8
0.351 10.218 80.231 20.451 5100.7
0.350 80.218 60.231 20.446 998.8
0.351 60.219 10.231 20.457 3103.0
0.350 30.218 30.231 20.455 3102.5
大黄酚（chrysopha nol）0.351 20.390 20.406 80.816 2104.7102.71.2
0.350 40.389 30.406 80.802 7101.6
0.351 10.390 10.406 80.804 9102.0
0.350 80.389 70.406 80.804 0101.8
0.351 60.390 60.406 80.808 1102.6
0.350 30.389 20.406 80.809 9103.4
大黄素甲醚（physcion）0.351 20.146 30.178 80.332 3104.0102.90.86
0.350 40.146 00.178 80.328 1101.9
0.351 10.146 30.178 80.329 0102.2
0.350 80.146 10.178 80.331 4103.6
0.351 60.146 50.178 80.329 6102.4
0.350 30.145 90.178 80.330 7103.4
), ArticleFig(id=1240704457814634712, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, label=表2, caption=

9个成分加样回收率试验结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		称样量
(mass)/g		样品量
(amount)/mg		加入量
(added)/mg		测得量
(detected)/mg		回收率
(recovery)/%		平均回收率
(average recovery)/%		RSD/%
马钱苷酸（loganic acid）0.351 21.2491.2682.535101.499.61.9
0.350 41.2461.2682.524100.8
0.351 11.2481.2682.524100.6
0.350 81.2471.2682.50599.2
0.351 61.2501.2682.50899.2
0.350 31.2451.2682.46596.2
龙胆苦苷（gentiopicro side）0.351 23.5443.5557.176102.2101.12.0
0.350 43.5363.5557.04598.7
0.351 13.5433.5557.110100.3
0.350 83.5403.5557.106100.3
0.351 63.5483.5557.120100.5
0.350 33.5353.5557.248104.4
橙皮苷(hesperidin）0.351 21.0291.0242.065101.2100.51.5
0.350 41.0261.0242.064101.4
0.351 11.0281.0242.071101.9
0.350 81.0271.0242.055100.4
0.351 61.0301.0242.058100.4
0.350 31.0261.0242.02597.6
丹皮酚（paeonol）0.351 20.638 80.656 31.304101.4101.60.51
0.350 40.637 40.656 31.305101.7
0.351 10.638 70.656 31.303101.2
0.350 80.638 10.656 31.306101.8
0.351 60.639 60.656 31.312102.5
0.350 30.637 20.656 31.300101.0
芦荟大黄素(aloe-emodin)0.351 20.177 00.184 60.360 099.199.81.4
0.350 40.176 60.184 60.358 298.4
0.351 10.176 90.184 60.359 498.86
0.350 80.176 80.184 60.361 399.9
0.351 60.177 20.184 60.365 8102.2
0.350 30.176 50.184 60.362 1100.5
大黄酸（rhein）0.351 20.282 60.300 20.592 1103.1100.91.4
0.350 40.281 90.300 20.586 4101.4
0.351 10.282 50.300 20.582 399.9
0.350 80.282 30.300 20.580 299.2
0.351 60.282 90.300 20.584 6100.5
0.350 30.281 90.300 20.586 0101.3
大黄素（emodin）0.351 20.218 80.231 20.452 8101.2100.81.8
0.350 40.218 30.231 20.446 698.8
0.351 10.218 80.231 20.451 5100.7
0.350 80.218 60.231 20.446 998.8
0.351 60.219 10.231 20.457 3103.0
0.350 30.218 30.231 20.455 3102.5
大黄酚（chrysopha nol）0.351 20.390 20.406 80.816 2104.7102.71.2
0.350 40.389 30.406 80.802 7101.6
0.351 10.390 10.406 80.804 9102.0
0.350 80.389 70.406 80.804 0101.8
0.351 60.390 60.406 80.808 1102.6
0.350 30.389 20.406 80.809 9103.4
大黄素甲醚（physcion）0.351 20.146 30.178 80.332 3104.0102.90.86
0.350 40.146 00.178 80.328 1101.9
0.351 10.146 30.178 80.329 0102.2
0.350 80.146 10.178 80.331 4103.6
0.351 60.146 50.178 80.329 6102.4
0.350 30.145 90.178 80.330 7103.4
), ArticleFig(id=1240704457898520797, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=EN, label=Tab. 3, caption=

Determination results of nine constituents in Tongshu Koushuang tablets

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
（lot number）		含量（contnet）/（mg·g-1）
马钱苷酸
（loganic acid）		龙胆苦苷
（gentiopicroside）		橙皮苷
（hesperidin）		丹皮酚
（paeonol）		芦荟大黄素
（aloe-emodin）		大黄酸
（rhein）		大黄素
（emodin）		大黄酚
（chrysophanol）		大黄素甲醚
（physcion）
202210011.8716.2742.1401.3930.498 10.768 30.571 81.2670.383 1
202211012.7259.0062.4242.0180.807 21.2460.915 81.4290.574 9
202201013.51710.212.9461.8910.497 30.811 50.607 91.1100.411 0
202202012.81010.223.5001.8280.443 80.675 40.507 00.854 40.341 9
202204012.88912.553.9121.7270.415 50.717 60.497 50.894 00.341 9
202204022.69211.563.3461.6280.394 80.657 50.484 70.839 80.327 3
), ArticleFig(id=1240704457990795486, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688784442970245, language=CN, label=表3, caption=

通舒口爽片中样品中9个成分含量结果（n=2）

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
（lot number）		含量（contnet）/（mg·g-1）
马钱苷酸
（loganic acid）		龙胆苦苷
（gentiopicroside）		橙皮苷
（hesperidin）		丹皮酚
（paeonol）		芦荟大黄素
（aloe-emodin）		大黄酸
（rhein）		大黄素
（emodin）		大黄酚
（chrysophanol）		大黄素甲醚
（physcion）
202210011.8716.2742.1401.3930.498 10.768 30.571 81.2670.383 1
202211012.7259.0062.4242.0180.807 21.2460.915 81.4290.574 9
202201013.51710.212.9461.8910.497 30.811 50.607 91.1100.411 0
202202012.81010.223.5001.8280.443 80.675 40.507 00.854 40.341 9
202204012.88912.553.9121.7270.415 50.717 60.497 50.894 00.341 9
202204022.69211.563.3461.6280.394 80.657 50.484 70.839 80.327 3
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HPLC法同时测定通舒口爽片中9个成分的含量
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胡小祥 1 , 何艳 2, ** , 孔庆丽 3 , 黄丽彬 1, **
药物分析杂志 | 标准研讨 2024,44(9): 1597-1603
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药物分析杂志 | 标准研讨 2024, 44(9): 1597-1603
HPLC法同时测定通舒口爽片中9个成分的含量
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胡小祥1 , 何艳2, ** , 孔庆丽3, 黄丽彬1, **
作者信息
  • 1.郴州市食品药品检验检测中心，郴州　423000
  • 2.湘南学院药学院，郴州　423000
  • 3.吉林省俊宏药业有限公司，通化　135100

    • Tel: 15873594256; E-mail:

通讯作者:

** 何艳　Tel: (0735)2278323; E-mail: ;
黄丽彬　Tel: (0735)2116279; E-mail:
Simultaneous determination of nine constituents in Tongshu Koushuang tablets by HPLC
Xiao-xiang HU1 , Yan HE2, ** , Qing-li KONG3, Li-bin HUANG1, **
Affiliations
  • 1.Chenzhou Municipal Center for Food and Drug Control, Chenzhou 423000, China
  • 2.College of Pharmacy, Xiang Nan University, Chenzhou 423000, China
  • 3.Junhong Drug Company of Jilin, Tonghua 135100, China
出版时间: 2024-09-30 doi: 10.16155/j.0254-1793.2023-0786
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摘要
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目的：采用高效液相色谱（HPLC）技术，建立同时测定通舒口爽片（大黄、枳实、秦艽等）中马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚9个成分的含量。方法：样品经甲醇回流提取后，分析采用Thermo Acclaim-C18（250 mm×4.6 mm，5 μm）色谱柱，流动相为0.15%磷酸(乙腈，梯度洗脱，流速1.0 mL·min-1，柱温30 ℃，进样量10 μL，检测波长为236 nm（检测马钱苷酸）、280 nm（检测龙胆苦苷、橙皮苷、丹皮酚）、254 nm（检测芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚）。结果：马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚在各自线性范围内呈良好的关系（r为0.999 1~0.999 9），平均加样回收率（RSD）分别为99.6%（RSD=1.9%）、101.1%（RSD=2.0%）、100.5%（RSD=1.5%）、101.6%（RSD=0.51%）、99.8%（RSD=1.4%）、100.9%（RSD=1.4%）、100.8%（RSD=1.8%）、102.7%（RSD=1.2%）、102.9%（RSD=0.86%），6批样品中9个成分的含量范围分别为1.871~3.517 mg·g-1、6.274~12.55 mg·g-1、2.140~3.946 mg·g-1、1.393~2.018 mg·g-1、0.394 8~0.807 2 mg·g-1、0.657 5~1.246 mg·g-1、0.484 7~0.915 8 mg·g-1、0.839 8~1.429 mg·g-1、0.327 3~0.547 9 mg·g-1。结论：所建立的方法简单准确，可用于通舒口爽片的质量控制与评价。

通舒口爽片  /  高效液相色谱  /  化学成分  /  马钱苷酸  /  龙胆苦苷  /  橙皮苷  /  丹皮酚  /  芦荟大黄素  /  大黄酸  /  大黄素  /  大黄酚  /  大黄素甲醚  /  含量测定  /  质量控制

Objective: To establish an HPLC method for simultaneous determination of loganic acid, gentiopicroside, hesperidin, paeonol, aloe-emodin, rhein, emodin, chrysophanol and physcion in Tongshu Koushuang tablets (Rhei Radix et Rhizoma, Aurantii Fructus Immaturus and Gentianae Macrophyllae Radix, etc.). Methods: The samples were extracted by refluxing with methanol and the separation was performed on a Thermo Acclaim-C18(250 mm×4.6 mm, 5 μm) column at 30 ℃, with mobile phase consisting of 0.15% phosphoric acid solution and acetonitrile with a gradient elution at a flow rate of 1.0 mL·min-1. The injection volume was 10 μL, and the detection wavelength was set at 236 nm (detecting loganic acid), 280 nm (detecting gentiopicroside, hesperidin and paeonol) and 254 nm (detecting aloe-emodin, rhein, emodin, chrysophanol and physcion). Results: Nine constituents (loganic acid, gentiopicroside, hesperidin, paeonol, aloe-emodin, rhein, emodin, chrysophanol and physcion) were in good linearity within their own ranges (r were 0.999 1-0.999 9), and the average recoveries were 99.6% (RSD=1.9%), 101.1% (RSD=2.0%), 103.0% (RSD=1.5%), 101.6% (RSD=0.51%), 99.8% (RSD=1.4%), 100.9% (RSD=1.4%), 100.8% (RSD=1.8%), 102.7% (RSD=1.2%) and 102.9% (RSD=0.86%), respectively. The content ranges of nine constituents were 1.871-3.517 mg·g-1, 6.274-12.55 mg·g-1, 2.140-3.946 mg·g-1, 1.393-2.018 mg·g-1, 0.394 8-0.807 2 mg·g-1, 0.657 5-1.246 mg·g-1, 0.484 7-0.915 8 mg·g-1, 0.839 8-1.429 mg·g-1 and 0.327 3-0.547 9 mg·g-1, respectively. Conclusion: This simple and accurate method can be used for the quality control and evaluation of Tongshu Koushuang tablets.

Tongshu Koushuang tablets  /  HPLC  /  chemical constituents  /  loganic acid  /  gentiopicroside  /  hesperidin  /  paeonol  /  aloe-emodin  /  rhein  /  emodin  /  chrysophanol  /  physcion  /  content determination  /  quality control
胡小祥, 何艳, 孔庆丽, 黄丽彬. HPLC法同时测定通舒口爽片中9个成分的含量. 药物分析杂志, 2024 , 44 (9) : 1597 -1603 . DOI: 10.16155/j.0254-1793.2023-0786
Xiao-xiang HU, Yan HE, Qing-li KONG, Li-bin HUANG. Simultaneous determination of nine constituents in Tongshu Koushuang tablets by HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (9) : 1597 -1603 . DOI: 10.16155/j.0254-1793.2023-0786
正文
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通舒口爽片由大黄、牡丹皮、当归、枳实、秦艽、夏枯草、茵陈、木贼8味药组成，具有清热除湿、化浊通便的作用，临床上用于口臭、牙龈肿痛、大肠湿热所致的便秘[1]，疗效显著。中药复方制剂成分复杂，成分间相互协同、相互作用，质量和疗效强调整体性；同时其质量评价指标应首选君药所含有效成分，同时兼顾臣、佐、使药有效成分[2-3]。通舒口爽片现行质量标准中仅对大黄中大黄素和大黄酚进行质量控制，尚未有关通舒口爽片质量控制的文献报道，难以全面控制和评价该制剂的质量。方中大黄清热解泻火、攻逐通便，主要活性成分有芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚等蒽醌类成分[4-5]，枳实破气消积、疏通决泄，主要活性成分为橙皮苷、辛弗林[6-7]，二者合为君药；秦艽祛风湿、清湿热，为臣药，主要活性成分为马钱苷酸、龙胆苦苷[8-9]，为臣药；牡丹皮清热凉血、活血散瘀，为佐药，主要活性成分为丹皮酚[10-11]。因此，本实验采用HPLC同时测定该制剂中马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚9个成分的含量，以期为了更加全面控制和评价通舒口爽片内在质量，从而确保临床疗效的稳定。
1　仪器与试药
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1.1　仪器
Agilent 1260型高效液相色谱仪（配有二极管阵列检测器、自动进样器、四元泵、柱温箱，Agilent公司）；XSE-205Du十万分之一电子天平（梅特勒托利多公司）；电热恒温水浴锅（北京市永光明医疗仪器有限公司）；KQ-500VDE超声清洗器（昆山超声仪器有限公司）。
1.2　试药
对照品马钱苷酸（批号111865-20202005，含量97.5%）、龙胆苦苷（批号110770-201918，含量97.1%）、橙皮苷（批号110721-202220，含量97.2%）、丹皮酚（批号110708-201908，含量99.8%）、芦荟大黄素（批号110795-201710，含量98.3%）、大黄酸（批号110757-201607，含量99.3%）、大黄素（批号110756-201913，含量96.0%）、大黄酚（批号110796-201922，含量99.4%）、大黄素甲醚（批号110758-201817，含量99.2%）购自中国食品药品检定研究院。甲酸、乙酸、磷酸（分析纯、国药集团化学试剂有限公司）；甲醇、乙腈（色谱纯，Merck公司）；水为屈臣氏纯净水。通舒口爽片（批号20221001、20221101、20220101、20220201、20220401、20220402，吉林省俊宏药业有限公司，有效期3年）。
2　方法与结果
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2.1　色谱条件
采用Thermo Acclaim-C18（250 mm×4.6 mm，5 μm）色谱柱，以0.15%磷酸为流动相A，乙腈为流动相B，梯度洗脱（0~10 min，8% B；10~20 min，8% B→15% B；20~35 min，15% B→25% B；35~50 min，25% B→40% B；50~65 min，40% B→70% B；65~70 min，70% B→80% B；70~80 min，80% B；再运行6 min），流速1.0 mL·min-1，柱温30 ℃，进样量10 μL，检测波长236 nm（检测马钱苷酸）、280 nm（检测龙胆苦苷、橙皮苷、丹皮酚）、254 nm（检测大黄素甲醚、大黄酚、大黄素、大黄酸、芦荟大黄素）。
2.2　溶液的制备
2.2.1　供试品溶液
取通舒口爽片样品20片（0.350 2 g·片-1），除去薄膜衣，研细，精密取称粉末0.7 g，置锥形瓶中，精密加入甲醇50 mL，称量，加热回流60 min，放冷，再称量，用甲醇补足减失的量，摇匀，滤过，滤液过0.45 μm微孔滤膜，即得。
2.2.2　阴性样品溶液
按照处方中各药味比例，分别取除秦艽、枳实、牡丹皮、大黄的其他药味，按照工艺制得各阴性样品，并按“2.2.1”项下方法制成缺秦艽、缺枳实、缺牡丹皮、缺大黄的阴性样品溶液。
2.2.3　混合对照品溶液
精密称取马钱苷酸、橙皮苷、丹皮酚、芦荟大黄素、大黄素、大黄酚对照品10.07、8.07、10.61、6.02、6.88、7.60 mg分别置25 mL量瓶中，精密称取大黄酸、大黄素甲醚对照品6.08、5.64 mg分别置50 mL量瓶中，加甲醇溶解并定容，得各单一对照品储备液。精密称取龙胆苦苷对照品5.77 mg置25 mL量瓶中，再分别往该量瓶中加入各单一对照品储备液：马钱苷酸5 mL、橙皮苷5 mL、丹皮酚2.5 mL、芦荟大黄素1.5 mL、大黄素4 mL、大黄素2 mL、大黄酚2 mL、大黄素甲醚2.5 mL，加甲醇定容至刻度，得混合对照品储备液（含马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚分别为78.55、224.1、62.75、42.36、14.20、19.32、21.14、24.17、11.19 μg·mL-1）。
2.3　专属性试验考察
取供试品溶液、4种阴性样品溶液、混合对照品储备液各适量，经0.45 μm微孔滤膜滤过，分别注入高效液相色谱仪，按“2.1”项色谱条件进样测定，记录各色谱图（见图1）。结果供试品色谱图中9个成分色谱峰保留时间与混合对照品一致，且与相邻杂质峰的分离度均大于1.9，阴性样品相应保留时间位置上无色谱峰出现，方法专属性良好。
2.4　线性关系考察
精密量取混合对照品储备溶液0.5、1、2、3、4、5 mL各置5 mL量瓶中，加甲醇至刻度，得系列标准曲线工作液。取适量，用0.45 μm微孔滤膜滤过，分别按“2.1”项色谱条件进样测定，记录各待测成分的峰面积。以各待测成分质量浓度（X，μg·mL-1）为横坐标，峰面积Y为纵坐标进行线性回归，得回归方程（见表1）。结果各组分在试验范围内线性关系良好。
2.5　仪器精密度试验
取混合对照品储备液，用甲醇稀释2倍，用0.45 μm微孔滤膜滤过，照“2.1”项下色谱条件连续进样6 次测定各成分的峰面积。结果马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚峰面积的RSD分别为0.50%、0.15%、0.61%、0.19%、0.23%、0.20%、0.42%、0.17%、0.44%，表明仪器精密度良好。
2.6　稳定性试验
取同一供试品溶液（批号20220101），按“2.1”项色谱条件，于0、6、12、18、24、36 h进样测定，马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚峰面积的RSD依次为0.57%、0.55%、0.73%、0.66%、0.58%、0.93%、1.7%、0.55%、0.58%，供试品溶液在36 h内测定稳定性良好。
2.7　重复性试验
取同一批样品(批号20220101)，精密称取6份，按“2.2.1”项下的方法平行制备供试品溶液，再按“2.1”项色谱条件测定马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的峰面积，代入标准曲线，计算9个成分的含量。结果9个成分平均含量依次为3.555、10.09、2.929、1.819、0.503 9、0.804 6、0.623 1、1.111、0.416 6 mg·g-1，RSD为0.94%、1.0%、1.7%、2.0%、1.9%、1.9%、1.2%、1.8%、1.4%，该方法的重复性良好。
2.8　加样回收率试验
取含量已知的通舒口爽片（批号20220101）样品，精密称取0.35 g，共6份，分别置具塞锥形瓶中，每份按相当于样品中各成分含量的100%分别加入各对照品溶液（0.422 8 mg·mL-1马钱苷酸3 mL、0.355 5 mg·mL-1龙胆苦苷10 mL、0.204 mg·mL-1橙皮苷5 mL、0.437 5 mg·mL-1丹皮酚 1.5 mL、0.184 6 mg·mL-1芦荟大黄素1 mL、0.150 1 mg·mL-1大黄酸2 mL、0.231 2 mg·mL-1大黄素1 mL、0.271 2 mg·mL-1大黄酚1.5 mL、0.119 2 mg·mL-1大黄素甲醚1.5 mL），加甲醇补足至50 mL，再按“2.1”项色谱条件进样测定马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚峰面积，代入相应标准曲线，计算9个成分的加样回收率，结果见表2。
2.9　样品含量测定
通舒口爽片样品6批，每批次称取2份，分别按“2.2.1”项下方法制备供试品溶液，进样测定，分别代入标准曲线计算其含量（见表3）。
3　讨论
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3.1　检测成分的考察
为了对通舒口爽片质量进行更全面的评价，预实验还对当归中活性成分阿魏酸[12-13]、茵陈主要活性成分绿原酸[14-15]、夏枯草主要活性成分迷迭香酸[16-17]进行测定。发现阿魏酸和绿原酸含量较低，迷迭香酸色谱峰存在干扰，尝试多次未实现有效分离。故最终选择马钱苷酸、龙胆苦苷、橙皮苷、丹皮酚、大黄素甲醚、大黄酚、大黄素、大黄酸、芦荟大黄素作为含量测定的指标成分。
3.2　供试品制备条件的考察
以9个成分各色谱峰的峰形、峰面积、分离度（大于1.5）为评价指标，课题组前期考察了甲醇、70%甲醇、乙醇、70%乙醇等提取溶剂，发现以甲醇提取溶剂时各色谱峰峰形为最好，峰面积为最大，且分离度满足要求。以甲醇为溶剂考察了超声提取（30、45、60 min）和回流提取（30、45、60、90 min），在现回流提取条件下，大黄素等5个蒽醌类成分提取更为完全，且回流提取60 min基本上提取完全。故供试品制备方法最终确定为加50 mL甲醇回流提取60 min。
3.3　色谱条件的优化
在“2.1”项色谱条件下，对9个成分进行扫描（200~400 nm）。结果马钱苷酸在236 nm处有最大吸收，龙胆苦苷、橙皮苷、丹皮酚在280 nm处有较大吸收，大黄素甲醚、大黄酚、大黄素、大黄酸、芦荟大黄素在254 nm处有较大吸收。故本实验采用波长切换技术，选择236、280、254 nm作为检测波长。
预实验分别考察了乙腈-水、甲醇-水运行时9个成分的峰形及分离情况，发现乙腈-水系统压力较低，且各成分分离效果优于甲醇-水系统，但马钱苷酸和龙胆苦苷峰形不佳。进而比较了乙腈-0.1%乙酸、乙腈-0.1%甲酸、乙腈-0.1%磷酸等流动相系统对9个成分的峰形及分离的影响，以乙腈-0.1%磷酸流动相系统效果最佳，最后对磷酸的浓度（0.05%、0.1%、0.15%、0.2%）进行了筛选，以0.15%磷酸为最佳，故最终选择乙腈-0.15%磷酸为流动相梯度洗脱对通舒口爽片中9种成分进行测定。
3.4　小结
本实验采用高效液相色谱法建立了同时测定通舒口爽片中9个成分含量的方法，能较全面的反映和评价该制剂的内在质量，6批含量测定结果显示各成分含量范围波动较小，质量较为稳定，但所收集的样本量偏少，尚不能制定各成分含量的限度值，后续将继续收集样本，以期制定各成分的限量值。
基金
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  • 湖南省自然科学基金科药联合项目(2021JJ80023)
文献
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2024年第44卷第9期
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doi: 10.16155/j.0254-1793.2023-0786
  • 首发时间：2026-03-17
  • 出版时间：2024-09-30
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  • 修回日期：2024-06-12
基金
湖南省自然科学基金科药联合项目(2021JJ80023)
作者信息
    1.郴州市食品药品检验检测中心，郴州　423000
    2.湘南学院药学院，郴州　423000
    3.吉林省俊宏药业有限公司，通化　135100

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** 何艳　Tel: (0735)2278323; E-mail: ;
黄丽彬　Tel: (0735)2116279; E-mail:
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
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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