Article(id=1195816327345652659, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, articleNumber=1001-2494(2024)24-2322-08, orderNo=null, doi=10.11669/cpj.2024.24.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1711987200000, receivedDateStr=2024-04-02, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1763034429632, onlineDateStr=2025-11-13, pubDate=1734796800000, pubDateStr=2024-12-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763034429632, onlineIssueDateStr=2025-11-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763034429632, creator=13701087609, updateTime=1763034429632, updator=13701087609, issue=Issue{id=1195816324862624679, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='24', pageStart='2299', pageEnd='2406', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1763034429040, creator=13701087609, updateTime=1763034724390, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1195817563738390939, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1195817563738390940, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=2322, endPage=2329, ext={EN=ArticleExt(id=1195816328104821686, articleId=1195816327345652659, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Quality Evaluation of Pterospermum heterophyllum Based on Fingerprint Combined with Chemical Pattern Recognition, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To use fingerprint combined with hierarchical clustering analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) to identify chemical patterns. METHODS Chrom Core 120 C18 (4.6 mm×250 mm, 5 μm) chromatographic column, 0.1% phosphoric acid aqueous solution (A)-acetonitrile (B) as mobile phase for gradient elution, volume flow rate of 0.8 mL·min-1, detection wavelength of 280 nm, column temperature of 30 ℃ injection volume of 10 μL, HPLC method was used to establish the fingerprints of 30 batches of medicinal herbs from 12 origins, and similarity analysis, HCA, PCA and PLS-DA were used and other chemical pattern recognition technologies were used to screen and quantitatively analyze the differentially characteristic components. RESULTS The fingerprinting method established by the established fingerprint method met the methodological requirements, and 17 common peaks were indexed by HPLC fingerprint of 30 batches of Pterospermum chinensis, with a similarity of 0.863-0.975. HCA, PCA and PLS-DA were used to distinguish the PH from different origins, and combined with the previous experiments, three components, protocatechuic acid, proanthocyanidins B2 and epicatechins, were comprehensively analyzed and screened as the active ingredients of the PH, and the content ranges were 0.103-1.676, 0.141-5.556 and 0.144-3.381 mg·g-1, respectively. CONCLUSION The fingerprint of the medicinal materials and the determination of the contents of the three active ingredients established in this study are stable, reliable and reproducible, which provides a certain scientific basis for evaluating the quality of Pterospermum heterophyllum.

, correspAuthors=Chenggang HU, 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=Tongzhi TAI, Juan TANG, Jiazhen HU, Chenggang HU), CN=ArticleExt(id=1195816530903613769, articleId=1195816327345652659, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=于指纹图谱结合化学模式识别对翻白叶树的质量评价, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 采用指纹图谱结合聚类分析(hierarchical clustering analysis,HCA)、主成分分析(principal component analysis, PCA)和正交偏最小二乘-判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA)等进行化学模式识别,对翻白叶树药材指纹图谱数据进行分析,筛选特征性指标成分并以此建立翻白叶树有效成分的定量分析,为翻白叶树质量控制提供科学依据。方法 采用ChromCore 120 C18(4.6 mm×250 mm,5 μm)色谱柱,以0.1%磷酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,体积流量0.8 mL·min-1,检测波长为280 nm,柱温30 ℃,进样量10 μL,HPLC 法建立12个产地30批药材翻白叶树的指纹图谱,运用相似度分析、HCA、PCA 和 PLS-DA 等化学模式识别技术对差异性特征成分进行筛选,并定量分析。结果 建立的指纹图谱方法符合方法学要求,30批翻白叶树HPLC指纹图谱标定17个共有峰,相似度在0.863~0.975;通过聚类分析将不同产地翻白叶树分为3类,聚类分析与主成分分析结果一致;通过 HCA、PCA 和 PLS-DA 较好地区分各产地翻白叶树,结合前期实验,综合分析筛选原儿茶酸、原花青素B2及表儿茶素3个成分作为翻白叶树有效成分,含量范围分别为0.103~1.676、0.141~5.556、0.144~3.381 mg·g-1结论 该研究建立的翻白叶树药材指纹图谱及3个有效成分含量的测定方法稳定、可靠,重现性好,对评价翻白叶树的质量提供一定的科学依据。

, correspAuthors=胡成刚, authorNote=null, correspAuthorsNote=
* 胡成刚,男,硕士,教授,硕士生导师 研究方向:中药及民族药基础研究与开发 Tel:(0855)5353416
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邰通芝,女,硕士研究生 研究方向:中药及民族药基础研究与开发

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邰通芝,女,硕士研究生 研究方向:中药及民族药基础研究与开发

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邰通芝,女,硕士研究生 研究方向:中药及民族药基础研究与开发

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Shanghai: Shanghai Science and Technology Press, 2006., articleTitle=null, refAbstract=null), Reference(id=1196125898828198429, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=2014, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=6, authorNames=WANG G Q, journalName=National Compilation of Chinese Herbal Medicine(全国中草药汇编), refType=null, unstructuredReference=WANG G Q. National Compilation of Chinese Herbal Medicine(全国中草药汇编)[M]. Beijing: People's Medical Publishing House, 2014., articleTitle=null, refAbstract=null), Reference(id=1196125898891112990, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=1999, volume=null, issue=null, pageStart=389, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=7, authorNames=Chinese Materia Medica Editorial Committee, State Administration of Traditional Chinese Medicine, journalName=Chinese Materia Medica(中药材). Volume Ⅴ, refType=null, unstructuredReference=Chinese Materia Medica Editorial Committee, State Administration of Traditional Chinese Medicine. Chinese Materia Medica(中药材). Volume Ⅴ[M]. Shanghai: Shanghai Science and Technology Press, 1999:389-390., articleTitle=null, refAbstract=null), Reference(id=1196125898949833247, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=1991, volume=null, issue=null, pageStart=299, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=8, authorNames=Jiangsu Provincial Institute of Botany, journalName=Xinhua Compendium of Materia Medica(新华本草纲要). Book 2, refType=null, unstructuredReference=Jiangsu Provincial Institute of Botany. Xinhua Compendium of Materia Medica(新华本草纲要). Book 2[M]. Shanghai: Shanghai Science and Technology Press, 1991:299., articleTitle=null, refAbstract=null), Reference(id=1196125899012747808, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=2023, volume=58, issue=12, pageStart=1123, pageEnd=1132, url=null, language=null, rfNumber=[10], rfOrder=9, authorNames=XIAO X J, LI M M, GU J F, journalName=Chin Pharm J(中国药学杂志), refType=null, unstructuredReference=XIAO X J, LI M M, GU J F, et al. Comprehensive evaluation of germplasm quality of Spatholobus suberectus Dunn based on combinative method of HPLC fingerprint, chemical pattern recognition and quantitative analysis of multicomponents[J]. Chin Pharm J(中国药学杂志), 2023, 58(12):1123-1132., articleTitle=Comprehensive evaluation of germplasm quality of Spatholobus suberectus Dunn based on combinative method of HPLC fingerprint, chemical pattern recognition and quantitative analysis of multicomponents, refAbstract=null), Reference(id=1196125899071468065, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=2017, volume=31, issue=7, pageStart=829, pageEnd=834, url=null, language=null, rfNumber=[11], rfOrder=10, authorNames=LU H X, WU F Y, JIANG M X, journalName=Nat Prod Res(天然产物研究), refType=null, unstructuredReference=LU H X, WU F Y, JIANG M X, et al. Tzumin A and B, two new lignan derivatives from the barks of Sassafras tzumu.[J]. Nat Prod Res(天然产物研究), 2017, 31(7):829-834., articleTitle=Tzumin A and B, two new lignan derivatives from the barks of Sassafras tzumu., refAbstract=null), Reference(id=1196125899155354146, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=2021, volume=268, issue=null, pageStart=118214, pageEnd=118214, url=null, language=null, rfNumber=[12], rfOrder=11, authorNames=SUN Y Q, HUO J X, ZHONG S, journalName=Carbohydrate Polymers(碳水化合物聚合物), refType=null, unstructuredReference=SUN Y Q, HUO J X, ZHONG S, et al. Chemical structure and anti-inflammatory activity of a branched polysaccharide isolated from Phellinus baumii[J]. Carbohydrate Polymers(碳水化合物聚合物), 2021, 268:118214-118214., articleTitle=Chemical structure and anti-inflammatory activity of a branched polysaccharide isolated from Phellinus baumii, refAbstract=null), Reference(id=1196125899230851619, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, doi=null, pmid=null, pmcid=null, year=2013, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=12, authorNames=CHEN J M, journalName=Study on chemical constituents of petroleum ether extract and fingerprint of root of Rhizome Aplakia L., refType=null, unstructuredReference=CHEN J M. Study on chemical constituents of petroleum ether extract and fingerprint of root of Rhizome Aplakia L.[D]. Guangzhou: Jinan University, 2013., articleTitle=null, refAbstract=null)], funds=[Fund(id=1196125898291327510, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, awardId=3052-052190023, language=CN, fundingSource=贵州省2019年中药资源普查项目(3052-052190023), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1196125892901646802, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, xref=null, ext=[AuthorCompanyExt(id=1196125892910035411, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, companyId=1196125892901646802, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Guizhou University of Chinese Medicine, Guiyang 550025, China), AuthorCompanyExt(id=1196125892918424020, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, companyId=1196125892901646802, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=贵州中医药大学, 贵阳 550025)])], figs=[ArticleFig(id=1196125895279817210, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Fig.1, caption=HPLC fingerprints of 30 batches of Pterospermum heterophyllum, figureFileSmall=iYIshAcLBQtCHigIUR9qGg==, figureFileBig=+X7Dmsh4NjY+glpReJYEYg==, tableContent=null), ArticleFig(id=1196125895346926075, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=图1, caption=30批翻白叶树药材HPLC指纹图谱, figureFileSmall=iYIshAcLBQtCHigIUR9qGg==, figureFileBig=+X7Dmsh4NjY+glpReJYEYg==, tableContent=null), ArticleFig(id=1196125895430812156, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Fig.2, caption=Chromatograms of sample (A) and reference (B)

1-protocatechuic acid; 4-catechin; 7-proanthocyanidin B2; 11-epicatechin.

, figureFileSmall=eSm3CStcUqu0UDx4equ9AA==, figureFileBig=C3DL7KIo5rS1RojfnK9cWQ==, tableContent=null), ArticleFig(id=1196125895506309629, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=图2, caption=混合对照品(A)和样品(B)色谱图

1-原儿茶酸; 4-儿茶素; 7-原花青素B2; 11-表儿茶素。

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Sources of 30 batches of Pterospermum heterophyllum

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Origin(in Chinese) Collection
time
No. Origin(in Chinese) Collection
time
S1 Kaili City, Guizhou Province(贵州省凯里市) 2020.11 S16 Hainan Shounanshan Ginseng Industry Co., Ltd.(海南省寿南山参业
有限公司)
2021.11
S2 Rongjiang County, Guizhou Province(贵州省榕江县) 2020.11 S17 Sichuan Lotus Pond Chinese Herbal Medicine Market 1(四川省荷花
池中药材市场1)
2020.11
S3 Jieyang City, Guangdong Province(广东省揭阳市) 2021.12 S18 Sichuan Lotus Pond Chinese Herbal Medicine Market 2(四川省荷花
池中药材市场2)
2020.11
S4 Hakka Baicao Direct Sales Center in Meizhou City, Guangdong
Province(广东省梅州市客家百草直营中心)
2021.11 S19 Hainan Province Haikou Rizhongtian Pharmaceutical Co., Ltd(海南
省海口市日中天制药有限公司)
2021.11
S5 Hongran Gu's Traditional Chinese Medicine Clinic in Guangzhou,
Guangdong Province(广东省广州市弘然古氏中医诊所)
2021.11 S20 Huaxin Haiyi Hall, Haikou City, Hainan Province(海南省海口市华
信海医堂)
2021.11
S6 Guangzhou City, Guangdong Province(广东省广州市) 2021.11 S21 Hainan Province Fuyitang Traditional Chinese Medicine Decoction
Piece Company(海南省福益堂中药饮片公司)
2021.11
S7 Shenzhen, Guangdong Province(广东省深圳市) 2021.12 S22 Huatuo Town, Bozhou City, Anhui Province(安徽省亳州市华佗镇) 2021.12
S8 Jianai Duoda Pharmacy in Guangzhou City, Guangdong Province
(广东省广州市健爱多大药房)
2021.11 S23 Anhui Province Bozhou City Kangguan Chinese Herbal Medicine
Trading Center(安徽省亳州市康关中药材交易中心)
2021.11
S9 Panlong District, Kunming City, Yunnan Province(云南省昆明市
盘龙区)
2021.11 S24 Zhang Jiliang Pharmacy, Huangshan City, Anhui Province(安徽省
黄山市张济良大药房)
2021.04
S10 Guandu District, Kunming City, Yunnan Province 1(云南省昆明
市官渡区1)
2021.11 S25 Wuyang County, Bozhou City, Anhui Province (安徽省亳州市
涡阳县)
2021.11
S11 Guandu District, Kunming City, Yunnan Province 2(云南省昆明
市官渡区2)
2021.11 S26 Luzhai County Hospital of Traditional Chinese Medicine, Liuzhou
City, Guangxi Province(广西壮族自治区柳州市鹿寨县中医院)
2021.04
S12 Jiujiang, Jiangxi Province(江西省九江市) 2021.11 S27 Anguo City, Baoding City, Hebei Province(河北省保定市安国市) 2021.12
S13 Jiangxi Peng's Chinese Medicine Tang Decoction Pieces Co., Ltd.
(江西彭氏国药堂饮片有限公司)
2021.11 S28 Shiyan City, Hubei Province(湖北省十堰市) 2021.12
S14 Guoxin Pharmacy, Yichun City, Jiangxi Province(江西省宜春市
国信大药房)
2021.11 S29 Xuchang City, Henan Province(河南省许昌市) 2021.12
S15 Chengdu, Sichuan(四川省成都市) 2021.11 S30 Lishui City, Zhejiang Province(浙江省丽水市) 2021.12
), ArticleFig(id=1196125897167254023, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表1, caption=

30批翻白叶树来源

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Origin(in Chinese) Collection
time
No. Origin(in Chinese) Collection
time
S1 Kaili City, Guizhou Province(贵州省凯里市) 2020.11 S16 Hainan Shounanshan Ginseng Industry Co., Ltd.(海南省寿南山参业
有限公司)
2021.11
S2 Rongjiang County, Guizhou Province(贵州省榕江县) 2020.11 S17 Sichuan Lotus Pond Chinese Herbal Medicine Market 1(四川省荷花
池中药材市场1)
2020.11
S3 Jieyang City, Guangdong Province(广东省揭阳市) 2021.12 S18 Sichuan Lotus Pond Chinese Herbal Medicine Market 2(四川省荷花
池中药材市场2)
2020.11
S4 Hakka Baicao Direct Sales Center in Meizhou City, Guangdong
Province(广东省梅州市客家百草直营中心)
2021.11 S19 Hainan Province Haikou Rizhongtian Pharmaceutical Co., Ltd(海南
省海口市日中天制药有限公司)
2021.11
S5 Hongran Gu's Traditional Chinese Medicine Clinic in Guangzhou,
Guangdong Province(广东省广州市弘然古氏中医诊所)
2021.11 S20 Huaxin Haiyi Hall, Haikou City, Hainan Province(海南省海口市华
信海医堂)
2021.11
S6 Guangzhou City, Guangdong Province(广东省广州市) 2021.11 S21 Hainan Province Fuyitang Traditional Chinese Medicine Decoction
Piece Company(海南省福益堂中药饮片公司)
2021.11
S7 Shenzhen, Guangdong Province(广东省深圳市) 2021.12 S22 Huatuo Town, Bozhou City, Anhui Province(安徽省亳州市华佗镇) 2021.12
S8 Jianai Duoda Pharmacy in Guangzhou City, Guangdong Province
(广东省广州市健爱多大药房)
2021.11 S23 Anhui Province Bozhou City Kangguan Chinese Herbal Medicine
Trading Center(安徽省亳州市康关中药材交易中心)
2021.11
S9 Panlong District, Kunming City, Yunnan Province(云南省昆明市
盘龙区)
2021.11 S24 Zhang Jiliang Pharmacy, Huangshan City, Anhui Province(安徽省
黄山市张济良大药房)
2021.04
S10 Guandu District, Kunming City, Yunnan Province 1(云南省昆明
市官渡区1)
2021.11 S25 Wuyang County, Bozhou City, Anhui Province (安徽省亳州市
涡阳县)
2021.11
S11 Guandu District, Kunming City, Yunnan Province 2(云南省昆明
市官渡区2)
2021.11 S26 Luzhai County Hospital of Traditional Chinese Medicine, Liuzhou
City, Guangxi Province(广西壮族自治区柳州市鹿寨县中医院)
2021.04
S12 Jiujiang, Jiangxi Province(江西省九江市) 2021.11 S27 Anguo City, Baoding City, Hebei Province(河北省保定市安国市) 2021.12
S13 Jiangxi Peng's Chinese Medicine Tang Decoction Pieces Co., Ltd.
(江西彭氏国药堂饮片有限公司)
2021.11 S28 Shiyan City, Hubei Province(湖北省十堰市) 2021.12
S14 Guoxin Pharmacy, Yichun City, Jiangxi Province(江西省宜春市
国信大药房)
2021.11 S29 Xuchang City, Henan Province(河南省许昌市) 2021.12
S15 Chengdu, Sichuan(四川省成都市) 2021.11 S30 Lishui City, Zhejiang Province(浙江省丽水市) 2021.12
), ArticleFig(id=1196125897242751496, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.2, caption=

Evaluation results of similarity of 30 batches of Pterospermum heterophyllum fingerprints

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Similarity No. Similarity No. Similarity
S1 0.863 S11 0.909 S21 0.957
S2 0.962 S12 0.907 S22 0.922
S3 0.925 S13 0.961 S23 0.961
S4 0.956 S14 0.947 S24 0.944
S5 0.949 S15 0.958 S25 0.926
S6 0.937 S16 0.937 S26 0.975
S7 0.974 S17 0.969 S27 0.955
S9 0.939 S19 0.911 S29 0.954
S10 0.913 S20 0.945 S30 0.872
), ArticleFig(id=1196125897318248969, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表2, caption=

30批翻白叶树指纹图谱相似度评价结果

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Similarity No. Similarity No. Similarity
S1 0.863 S11 0.909 S21 0.957
S2 0.962 S12 0.907 S22 0.922
S3 0.925 S13 0.961 S23 0.961
S4 0.956 S14 0.947 S24 0.944
S5 0.949 S15 0.958 S25 0.926
S6 0.937 S16 0.937 S26 0.975
S7 0.974 S17 0.969 S27 0.955
S9 0.939 S19 0.911 S29 0.954
S10 0.913 S20 0.945 S30 0.872
), ArticleFig(id=1196125897385357834, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.3, caption=

The eigenvalue and cumulative variance contribution rate of Pterospermum heterophyllum

, figureFileSmall=null, figureFileBig=null, tableContent=
Principal
component
Initial
eigenvalues
Variance
contribution rate/%
Cumulative variance
contribution rate/%
PC1 10.800 63.527 63.527
PC2 4.274 25.141 88.668
PC3 1.026 6.035 94.703
), ArticleFig(id=1196125897448272395, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表3, caption=

翻白叶树样品特征值及累积方差贡献率

, figureFileSmall=null, figureFileBig=null, tableContent=
Principal
component
Initial
eigenvalues
Variance
contribution rate/%
Cumulative variance
contribution rate/%
PC1 10.800 63.527 63.527
PC2 4.274 25.141 88.668
PC3 1.026 6.035 94.703
), ArticleFig(id=1196125897511186956, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.4, caption=

Initial factor load matrix of the sample of Pterospermum heterophyllum

, figureFileSmall=null, figureFileBig=null, tableContent=
There are
common
peaks
Load
Principal
component 1
Principal
component 2
Principal
component 3
A1 -0.176 0.058 0.972
A2 0.49 0.839 -0.092
A3 0.056 0.965 0.088
A4 0.083 0.976 -0.124
A5 0.659 0.731 0.098
A6 0.212 0.936 0.054
A7 0.99 -0.083 0.031
A8 0.987 -0.046 0.01
A9 0.991 -0.099 0.038
A10 0.893 -0.111 -0.095
A11 0.917 0.16 -0.081
A12 0.979 -0.179 0.037
A13 0.972 -0.208 0.047
A14 0.967 -0.192 0.023
A15 0.899 -0.257 0.112
A16 0.936 -0.073 -0.018
A17 0.97 -0.182 0.041
), ArticleFig(id=1196125897599267341, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表4, caption=

翻白叶树样品初始因子载荷矩阵

, figureFileSmall=null, figureFileBig=null, tableContent=
There are
common
peaks
Load
Principal
component 1
Principal
component 2
Principal
component 3
A1 -0.176 0.058 0.972
A2 0.49 0.839 -0.092
A3 0.056 0.965 0.088
A4 0.083 0.976 -0.124
A5 0.659 0.731 0.098
A6 0.212 0.936 0.054
A7 0.99 -0.083 0.031
A8 0.987 -0.046 0.01
A9 0.991 -0.099 0.038
A10 0.893 -0.111 -0.095
A11 0.917 0.16 -0.081
A12 0.979 -0.179 0.037
A13 0.972 -0.208 0.047
A14 0.967 -0.192 0.023
A15 0.899 -0.257 0.112
A16 0.936 -0.073 -0.018
A17 0.97 -0.182 0.041
), ArticleFig(id=1196125897666376206, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.5, caption=

Linear equation, correlation coefficient and linear range of Pterospermum heterophyllum

, figureFileSmall=null, figureFileBig=null, tableContent=
Comparisons Regression equations r Linear range/μg·mL-1
Protocatechuic acid y=4 152.7x+359.3 0.999 4 1.4-42.0
Proanthocyanidins B2 y=9 708.5x+24 391 0.999 3 0.55-165.0
Epicatechin y=7 507.6x-44.48 0.999 6 2.9-87.0
), ArticleFig(id=1196125897720902159, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表5, caption=

翻白叶树样品的线性方程、相关系数和线性范围

, figureFileSmall=null, figureFileBig=null, tableContent=
Comparisons Regression equations r Linear range/μg·mL-1
Protocatechuic acid y=4 152.7x+359.3 0.999 4 1.4-42.0
Proanthocyanidins B2 y=9 708.5x+24 391 0.999 3 0.55-165.0
Epicatechin y=7 507.6x-44.48 0.999 6 2.9-87.0
), ArticleFig(id=1196125897788011024, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.6, caption=

The reproducibility of the control substance was examined by the experimental results. n=6

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Comparisons Weigh the sample size/g Peak area/mV·s Content/mg Average content/mg RSD/%
Protocatechuic acid 1.000 3 45 226 0.432
1.000 1 42 380 0.405
1.000 1 42 627 0.407 0.416 2.40
1.000 3 43 846 0.419
1.000 4 43 900 0.419
1.000 0 43 175 0.412
Proanthocyanidins B2 1.000 3 495 727 1.942
1.000 1 496 829 1.946
1.000 1 500 020 1.960 1.941 0.71
1.000 3 490 316 1.920
1.000 4 496 797 1.946
1.000 0 493 461 1.933
Epicatechin 1.000 3 186 373 0.993
1.000 1 179 876 0.959
1.000 1 189 137 1.008 0.977 2.23
1.000 3 180 247 0.961
1.000 4 185 071 0.986
1.000 0 179 080 0.954
), ArticleFig(id=1196125897850925585, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表6, caption=

对照品重现性考察实验结果。n=6

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Comparisons Weigh the sample size/g Peak area/mV·s Content/mg Average content/mg RSD/%
Protocatechuic acid 1.000 3 45 226 0.432
1.000 1 42 380 0.405
1.000 1 42 627 0.407 0.416 2.40
1.000 3 43 846 0.419
1.000 4 43 900 0.419
1.000 0 43 175 0.412
Proanthocyanidins B2 1.000 3 495 727 1.942
1.000 1 496 829 1.946
1.000 1 500 020 1.960 1.941 0.71
1.000 3 490 316 1.920
1.000 4 496 797 1.946
1.000 0 493 461 1.933
Epicatechin 1.000 3 186 373 0.993
1.000 1 179 876 0.959
1.000 1 189 137 1.008 0.977 2.23
1.000 3 180 247 0.961
1.000 4 185 071 0.986
1.000 0 179 080 0.954
), ArticleFig(id=1196125897913840146, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.7, caption=

Experimental results of sample recovery of Pterospermum heterophyllum. n=6

, figureFileSmall=null, figureFileBig=null, tableContent=
Comparisons m(Sample)
/g
m(Original)
/mg
m(Added)
/mg
m(Found)
/mg
Recovery
/%
Average
recovery/%
RSD
/%
Protocatechuic acid 0.501 7 0.208 0.210 0.414 99.043 97.09 1.80
0.502 5 0.208 0.210 0.400 95.694
0.500 9 0.208 0.210 0.396 94.737
0.503 6 0.208 0.210 0.409 97.847
0.505 2 0.208 0.210 0.413 98.804
0.504 1 0.208 0.210 0.403 96.411
Proanthocyanidins B2 0.501 7 0.971 0.970 1.905 98.145 98.36 0.86
0.502 5 0.971 0.970 1.911 98.454
0.500 9 0.971 0.970 1.879 96.806
0.503 6 0.971 0.970 1.917 98.764
0.505 2 0.971 0.970 1.927 99.279
0.504 1 0.971 0.970 1.916 98.712
Epicatechin 0.501 7 0.497 0.488 0.960 97.462 96.67 0.67
0.502 5 0.497 0.488 0.945 95.939
0.500 9 0.497 0.488 0.953 96.751
0.503 6 0.497 0.488 0.959 97.360
0.505 2 0.497 0.488 0.950 96.447
0.504 1 0.497 0.488 0.946 96.041
), ArticleFig(id=1196125897993531923, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表7, caption=

翻白叶树样品加样回收率实验结果。n=6

, figureFileSmall=null, figureFileBig=null, tableContent=
Comparisons m(Sample)
/g
m(Original)
/mg
m(Added)
/mg
m(Found)
/mg
Recovery
/%
Average
recovery/%
RSD
/%
Protocatechuic acid 0.501 7 0.208 0.210 0.414 99.043 97.09 1.80
0.502 5 0.208 0.210 0.400 95.694
0.500 9 0.208 0.210 0.396 94.737
0.503 6 0.208 0.210 0.409 97.847
0.505 2 0.208 0.210 0.413 98.804
0.504 1 0.208 0.210 0.403 96.411
Proanthocyanidins B2 0.501 7 0.971 0.970 1.905 98.145 98.36 0.86
0.502 5 0.971 0.970 1.911 98.454
0.500 9 0.971 0.970 1.879 96.806
0.503 6 0.971 0.970 1.917 98.764
0.505 2 0.971 0.970 1.927 99.279
0.504 1 0.971 0.970 1.916 98.712
Epicatechin 0.501 7 0.497 0.488 0.960 97.462 96.67 0.67
0.502 5 0.497 0.488 0.945 95.939
0.500 9 0.497 0.488 0.953 96.751
0.503 6 0.497 0.488 0.959 97.360
0.505 2 0.497 0.488 0.950 96.447
0.504 1 0.497 0.488 0.946 96.041
), ArticleFig(id=1196125898090000916, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=EN, label=Tab.8, caption=

Content determination of three chemical components in 30 batches of Pterospermum heterophyllum

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Content/mg·g-1
Protocatechuic acid Proanthocyanidins B2 Epicatechin
S1 0.219 0.141 0.144
S2 0.117 1.434 0.811
S3 0.167 0.897 1.291
S4 0.625 1.221 1.093
S5 0.203 1.302 2.137
S6 0.103 0.277 0.52
S7 0.153 0.878 1.408
S8 0.249 0.747 1.293
S9 0.191 1.571 2.48
S10 0.179 1.419 2.276
S11 0.153 1.78 1.912
S12 0.58 0.413 0.809
S13 1.498 0.433 0.751
S14 0.627 0.351 0.713
S15 0.499 1.653 1.811
S16 0.763 0.98 1.457
S17 1.676 0.139 0.278
S18 0.664 0.272 0.477
S19 0.485 1.249 1.861
S21 0.265 0.979 1.492
S22 0.364 2.171 2.336
S23 0.401 0.409 0.746
S24 0.482 5.134 2.261
S25 0.349 0.612 0.86
S26 0.463 5.556 3.381
S27 0.297 4.419 2.501
S28 0.186 1.825 2.467
S29 0.443 0.363 0.71
S30 0.361 1.659 1.473
), ArticleFig(id=1196125898152915477, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816327345652659, language=CN, label=表8, caption=

30批翻白叶树3种指标性成分含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Content/mg·g-1
Protocatechuic acid Proanthocyanidins B2 Epicatechin
S1 0.219 0.141 0.144
S2 0.117 1.434 0.811
S3 0.167 0.897 1.291
S4 0.625 1.221 1.093
S5 0.203 1.302 2.137
S6 0.103 0.277 0.52
S7 0.153 0.878 1.408
S8 0.249 0.747 1.293
S9 0.191 1.571 2.48
S10 0.179 1.419 2.276
S11 0.153 1.78 1.912
S12 0.58 0.413 0.809
S13 1.498 0.433 0.751
S14 0.627 0.351 0.713
S15 0.499 1.653 1.811
S16 0.763 0.98 1.457
S17 1.676 0.139 0.278
S18 0.664 0.272 0.477
S19 0.485 1.249 1.861
S21 0.265 0.979 1.492
S22 0.364 2.171 2.336
S23 0.401 0.409 0.746
S24 0.482 5.134 2.261
S25 0.349 0.612 0.86
S26 0.463 5.556 3.381
S27 0.297 4.419 2.501
S28 0.186 1.825 2.467
S29 0.443 0.363 0.71
S30 0.361 1.659 1.473
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于指纹图谱结合化学模式识别对翻白叶树的质量评价
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邰通芝 , 唐娟 , 胡家震 , 胡成刚 *
中国药学杂志 | 论著 2024,59(24): 2322-2329
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中国药学杂志 | 论著 2024, 59(24): 2322-2329
于指纹图谱结合化学模式识别对翻白叶树的质量评价
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邰通芝, 唐娟, 胡家震, 胡成刚*
作者信息
  • 贵州中医药大学, 贵阳 550025
  • 邰通芝,女,硕士研究生 研究方向:中药及民族药基础研究与开发

通讯作者:

* 胡成刚,男,硕士,教授,硕士生导师 研究方向:中药及民族药基础研究与开发 Tel:(0855)5353416
Quality Evaluation of Pterospermum heterophyllum Based on Fingerprint Combined with Chemical Pattern Recognition
Tongzhi TAI, Juan TANG, Jiazhen HU, Chenggang HU*
Affiliations
  • Guizhou University of Chinese Medicine, Guiyang 550025, China
出版时间: 2024-12-22 doi: 10.11669/cpj.2024.24.004
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目的 采用指纹图谱结合聚类分析(hierarchical clustering analysis,HCA)、主成分分析(principal component analysis, PCA)和正交偏最小二乘-判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA)等进行化学模式识别,对翻白叶树药材指纹图谱数据进行分析,筛选特征性指标成分并以此建立翻白叶树有效成分的定量分析,为翻白叶树质量控制提供科学依据。方法 采用ChromCore 120 C18(4.6 mm×250 mm,5 μm)色谱柱,以0.1%磷酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,体积流量0.8 mL·min-1,检测波长为280 nm,柱温30 ℃,进样量10 μL,HPLC 法建立12个产地30批药材翻白叶树的指纹图谱,运用相似度分析、HCA、PCA 和 PLS-DA 等化学模式识别技术对差异性特征成分进行筛选,并定量分析。结果 建立的指纹图谱方法符合方法学要求,30批翻白叶树HPLC指纹图谱标定17个共有峰,相似度在0.863~0.975;通过聚类分析将不同产地翻白叶树分为3类,聚类分析与主成分分析结果一致;通过 HCA、PCA 和 PLS-DA 较好地区分各产地翻白叶树,结合前期实验,综合分析筛选原儿茶酸、原花青素B2及表儿茶素3个成分作为翻白叶树有效成分,含量范围分别为0.103~1.676、0.141~5.556、0.144~3.381 mg·g-1结论 该研究建立的翻白叶树药材指纹图谱及3个有效成分含量的测定方法稳定、可靠,重现性好,对评价翻白叶树的质量提供一定的科学依据。

翻白叶树  /  指纹图谱  /  相似度  /  化学模式识别  /  含量测定  /  原儿茶酸  /  原花青素B2  /  表儿茶素

OBJECTIVE To use fingerprint combined with hierarchical clustering analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) to identify chemical patterns. METHODS Chrom Core 120 C18 (4.6 mm×250 mm, 5 μm) chromatographic column, 0.1% phosphoric acid aqueous solution (A)-acetonitrile (B) as mobile phase for gradient elution, volume flow rate of 0.8 mL·min-1, detection wavelength of 280 nm, column temperature of 30 ℃ injection volume of 10 μL, HPLC method was used to establish the fingerprints of 30 batches of medicinal herbs from 12 origins, and similarity analysis, HCA, PCA and PLS-DA were used and other chemical pattern recognition technologies were used to screen and quantitatively analyze the differentially characteristic components. RESULTS The fingerprinting method established by the established fingerprint method met the methodological requirements, and 17 common peaks were indexed by HPLC fingerprint of 30 batches of Pterospermum chinensis, with a similarity of 0.863-0.975. HCA, PCA and PLS-DA were used to distinguish the PH from different origins, and combined with the previous experiments, three components, protocatechuic acid, proanthocyanidins B2 and epicatechins, were comprehensively analyzed and screened as the active ingredients of the PH, and the content ranges were 0.103-1.676, 0.141-5.556 and 0.144-3.381 mg·g-1, respectively. CONCLUSION The fingerprint of the medicinal materials and the determination of the contents of the three active ingredients established in this study are stable, reliable and reproducible, which provides a certain scientific basis for evaluating the quality of Pterospermum heterophyllum.

Pterospermum heterophyllum  /  fingerprinting  /  similarity  /  chemical pattern recognition  /  content determination  /  protocatechuic acid  /  proanthocyanidins B2  /  epicatechin
邰通芝, 唐娟, 胡家震, 胡成刚. 于指纹图谱结合化学模式识别对翻白叶树的质量评价. 中国药学杂志, 2024 , 59 (24) : 2322 -2329 . DOI: 10.11669/cpj.2024.24.004
Tongzhi TAI, Juan TANG, Jiazhen HU, Chenggang HU. Quality Evaluation of Pterospermum heterophyllum Based on Fingerprint Combined with Chemical Pattern Recognition[J]. Chinese Pharmaceutical Journal, 2024 , 59 (24) : 2322 -2329 . DOI: 10.11669/cpj.2024.24.004
翻白叶树(Pterospermum heterophyllum Hance) 为梧桐科翅子树属植物,又名异叶翅子树、红半枫荷、斗枫荷、番张麻、阴阳叶等,以根入药,分布于江西、广东、广西、海南和贵州等地。查阅各个地区典籍与地方药材质量标准中半枫荷药材来源可知,多省收载品种为翻白叶树[1-7],药用部位多为根,具有祛风除湿、活血通络的功能,主要用于治疗风湿痹痛、手足麻木、腰肌劳损、跌打损伤等疾病[8-9]
目前,翻白叶树质量控制相关报道较少,作为半枫荷药材的主要来源之一,有必要进一步优化翻白叶树的指纹图谱。基于课题组前期体外抗炎活性部位筛选和乙酸乙酯部位分离,本实验通过高效液相色谱(HPLC)指纹图谱结合化学模式识别技术整合分析指纹图谱中提取共有峰的面积数据,得到不同产地的特征化学成分并对其进行含量测定,以此反映不同批次药材之间的一致性、差异性,提升翻白叶树的质量控制水平。
LC-2030C岛津高效液相色谱仪(日本岛津公司);ChromCore 120 C18色谱柱(纳谱分析技术有限公司);KQ5200DB型超声波清洗仪(昆山市超声仪器有限公司);JCS-31001C型电子分析天平(哈尔滨众汇衡器有限公司);98-1-B型电子调温电热套(天津市泰斯特仪器有限公司)。
对照品原儿茶酸(批号C100822,贵州迪大科技有限公司);表儿茶素(批号110878-201703,中国食品药品检定研究院);原花青素B2(批号29106-49-8,成都埃法生物科技有限公司,质量分数≥98%);乙腈(批号:AS1122-801,美国TEDIA公司);磷酸、甲酸、冰醋酸均为色谱纯,水为纯净水(怡宝)。
翻白叶树药材采自贵州、广东、广西、海南、云南等地,共30批次。经贵州中医药大学胡成刚教授鉴定为梧桐科翅子树属翻白叶树(Pterospermum heterophyllum)的干燥根。翻白叶树药材来源见表1
ChromCore 120 C18(4.6 mm×250 mm,5 μm)色谱柱,流动相为0.1%磷酸水溶液(A)-乙腈(B),梯度洗脱,0~35 min,9%~11% B;35~50 min,11%~12%B;50~110 min,12%~16% B;110~115 min,16%~100% B;体积流量0.8 mL·min-1;检测波长为280 nm;柱温30 ℃;进样量10 μL。
精密称取半枫荷药材粉末(过3号筛)1.0 g,置具塞锥形瓶中,加入体积分数75%甲醇20 mL,超声提取30 min,0.45 μm的微孔滤膜滤过,取续滤液,即得。
分别取表儿茶素2.00 mg、儿茶素2.00 mg、原花青素B21.80 mg、原儿茶酸4.23 mg对照品,精密称定,置量瓶中,加入体积分数75%甲醇制成含表儿茶素0.133 mg·mL-1、儿茶素0.133 mg·mL-1、原花青素0.121 mg·mL-1、原儿茶酸0.141 mg·mL-1的混合对照品溶液。
取同一翻白叶树供试品(S1),按 “2.2.1”项下方法制备供试品溶液1份,按“2.1”项下色谱条件连续进样6次,以11号峰(表儿茶素)为参照峰(S),计算各共有峰的相对保留时间与相对峰面积。各共有峰的相对保留时间相对标准偏差(RSD)值分别为0.226%、0.312%、0.178%、0.125%、0.197%、0.106%、0.046%、0.047%、0.081%、0.058%、0.000%、0.085%、0.096%、0.125%、0.123%、0.123%和0.182%(n=6),各共有峰的相对保留峰面积RSD值分别为2.908%、2.548%、2.097%、2.206%、1.568%、2.836%、2.364%、0.980%、2.566%、2.745%、0.000%、2.324%、2.136%、2.261%、2.871%、2.581%和2.482%(n=6),均小于3%,表明仪器精密度良好。
取同一翻白叶树供试品(S1),按 “2.2.1”项下方法制备供试品溶液1份,按“2.1”项下色谱条件分别于0,4,8,12,18,24 h进样,以11号峰(表儿茶素)为参照峰(S),计算各共有峰的相对保留时间与相对峰面积。各共有峰的相对保留时间 RSD 值分别为0.441%、0.180%、0.165%、0.116%、0.232%、0.114%、0.049%、0.209%、0.285%、0.257%、0.000%、0.074%、0.187%、0.276%、0.279%、0.280%和0.756%(n=6),各共有峰的相对保留峰面积RSD值分别为0.543%、0.401%、0.598%、1.486%、1.269%、2.388%、1.122%、1.126%、0.647%、1.243%、0.000%、1.150%、1.014%、2.701%、2.771%、2.390%和1.211%(n=6),均小于3%,表明供试品溶液的稳定性良好。
取同一翻白叶树供试品(S1),按 “2.2.1”项下方法制备6份供试品溶液,按“2.1”项下色谱条件进样,以11号峰(表儿茶素)为参照峰(S),计算各共有峰的相对保留时间与相对峰面积。各共有峰的相对保留时间 RSD 值分别为0.174%、0.247%、0.199%、0.115%、0.136%、0.063%、0.052%、0.039%、0.042%、0.039%、0.000%、0.112%、0.163%、0.172%、0.183%、0.215%和0.304%(n=6),各共有峰的相对保留峰面积RSD值分别为2.801%、2.281%、1.254%、2.572%、1.814%、1.960%、2.720%、1.328%、2.721%、2.481%、0.791%、1.521%、2.646%、2.870%、2.452%、2.454%和2.804%(n=6),均小于3%,表明方法的稳定性良好。
取30批不同产地翻白叶树药材按“2.2.1”项下方法制备供试品溶液,按“2.1”项下色谱条件进样并记录色谱数据,将所得的30批翻白叶树色谱图以 AIA格式导入“中药色谱指纹图谱相似度评价系统(2012.1 版本)”,设S14为参照峰、平均数为对照图谱生成方法、0.5为时间窗宽度,多点校正以及峰匹配得到翻白叶树药材的指纹图谱和对照指纹图谱,并进行相似度分析。见图1
30批翻白叶树药材有17个共有峰,通过对照品图谱对比,指认其中4个色谱峰,见图2
对30批翻白叶树药材的指纹图谱进行相似度计算分析,30批翻白叶树药材色谱图与对照指纹图谱的相似度在0.863~0.975,表明各个产地翻白叶树相似度较高。相似度结果见表2
利用SPSS 26.0软件以翻白叶树指纹图谱标定的17个共有峰峰面积为变量,对30批翻白叶树药材数据进行聚类分析,使用组间连接聚类方法,以余弦离作为药材间的距离公式,结果见图3。当类间距离为5时,30批翻白叶树药材被分为3类,其中S2(贵州省榕江县)、S27(河北省保定市安国市)聚为一类,S24(安徽省黄山市张济良大药房)和S26(广西壮族自治区柳州市鹿寨县中医院)聚为一类,其余贵州产地、广东产地、云南产地、海南产地、四川产地、安徽产地、湖北产地、河南产地和浙江产地聚为一类。
为了进一步区分各不同产地翻白叶树,将30批药材指纹图谱的17个共有峰峰面积为原始数据导入SPSS 软件进行处理,进行PCA分析。首先,进行降维因子分析,结果显示,KMO值为0.684,大于0.5,表明各变量相关性较好,设置特征值大于1,提取得到3个主成分,其累计贡献率达到94.703%,结果见表3,能基本反映药材共有峰的信息,以主成分因子变量绘制公因子碎石图,结果显示特征值较高的3个主成分因子的斜率更大,说明所提取的 3 个主成分可以最大程度地代表翻白叶树药材的整体质量特征,前3个主成分评价翻白叶树质量具有一定的可行性,见图4。初始因子载荷矩阵见表4,将其进行正交旋转,旋转后得到的17个共有峰成分在3个主成分中的旋转矩阵,反映了各变量对主成分的贡献大小,其绝对值越大对该成分在决定药材区分中的作用越大。载荷矩阵结果表明,第1主成分对应载荷量较大的峰为峰9、峰7(原花青素B2)、峰8、峰12、峰13、峰17、峰14、峰16、峰11(表儿茶素)、峰15、峰10、峰5,表明其对第1主成分的影响较大,可为翻白叶树的质量评价提供参考依据。第2主成分对应载荷量较大的峰为峰4(儿茶素)、峰3、峰6、峰5,表明其对第2主成分存在一定程度的影响。第3主成分对应峰1(原儿茶酸)。
利用SIMCA 14.1软件,用OPLS-DA对17个共有峰的峰面积进行分析,结果见图5,药材被显著的聚为3类,其结果与聚类分析结果一致。为了判断特征峰对翻白叶树的重要程度,提取OPLS-DA模型中17个变量的VIP值并从大到小排序,见图6,结合 OPLS-DA 模型中变量重要性投影值(variable importance in the projection,VIP)进行分析,以 VIP>1 为条件筛选出差异标志物,筛选出4个差异标志物,对翻白叶树药材的影响程度依次为峰7(原花青素B2)> 峰11(表儿茶素)>峰12(未知)>峰13(新绿原酸),以上化学成分可能导致泛白叶树质量产生差异的因素,并且可看出原花青素B2及表儿茶素在各批次中含量较高,因此,能够为后续含量测定指标的选择提供参考。
采用指纹图谱结合 CA、PCA 及 PLS-DA 对不同批次的翻白叶树药材进行研究分析,通过 PCA 可知峰9、峰7(原花青素B2)、峰8、峰12、峰13、峰17、峰14、峰16、峰11(表儿茶素)、峰15、峰10、峰5、峰4(儿茶素)、峰3、峰6、峰5以及峰1(原儿茶酸)是影响不同批次翻白叶树药材质量的特征化学成分。由 PLS-DA 结果可知,VIP>1 的有峰7(原花青素B2)、峰11(表儿茶素)、峰12(未知)及峰13(新绿原酸),表明不同批次间的含量差异较大,是翻白叶树的差异性特征成分。
通过前期对翻白叶树不同极性部位进行体外抗炎作用筛选,经查阅文献,从乙酸乙酯部位得到化合物圣草酚、儿茶素、表儿茶素、原花青素B2均有一定的抗炎作用,且表儿茶素与原花青素含量较高。考虑到中药材多成分、多靶点的协同作用,在地方药材质量标准中原儿茶酸的基础上,加上表儿茶素、原花青素B2这两个具有抗炎活性的主成分,综上,本实验以原儿茶酸、原花青素B2、表儿茶素作为翻白叶树差异特征成分进行含量测定。
精密称取对照品原儿茶酸、表儿茶素、原花青素B2 各2.8、1.1、5.8 mg分别至20 mL,然后制成0.14、0.055、0.29 mg·mL-1的混合对照品溶液,分别取0.1、0.5、1.0、1.5、2.0、2.5、3.0 mL加甲醇定容至10 mL,按“2.1”项下方法测定色谱峰面积,以进样浓度(μg·mL-1)为横坐标x,色谱峰面积为纵坐标y绘制标准曲线,计算线性回归方程和相关系数(r),结果见表5
取同一翻白叶树供试品(S1),按 “2.2.1”项下方法制备6份供试品溶液,按“2.1”项下色谱条件进样,测得原儿茶酸、表儿茶素、原花青素B2含量的RSD值分别为2.40%、0.71%和2.23%(n=6),结果表明,本方法重现性良好。结果见表6
精密称取已知含量的翻白叶树药材粉末0.5 g,共6份,精密称定,分别加入混合对照品溶液1 mL,按“2.2.1”项下方法制备供试品溶液,按“2.1”项下色谱条件测定峰面积,测得原儿茶酸、表儿茶素、原花青素B2加样回收率分别为97.09%、98.36%和96.67%,RSD值分别为1.80%、0.86%和0.67%。结果见表7
精密称取不同批次翻白叶树药材粉末(过3号筛)各1.0 g,按“2.2.1”项下方法制备供试液。按“2.1”项下色谱条件进样,测定原儿茶酸、表儿茶素、原花青素B2含量。结果见表8
本实验考察了不同提取方法(超声、回流)、不同提取溶剂(体积分数50%甲醇、75%甲醇、100%甲醇、50%乙醇、75%乙醇、100%乙醇)、不同提取时间(30、45、60 min)、不同料液比(1∶10、1∶20、1∶30、1∶40)对翻白叶树药材指纹图谱色谱图及含量测定的影响,结果发现:提取方法、提取时间及料液比对翻白叶树指纹图谱色谱图及含量测定无明显改变,而体积分数75%甲醇提取主峰面积较大,峰数量较多。料液比为1∶20,体积分数75%甲醇超声提取30 min为最佳提取方法。通过全波长扫描发现,原儿茶酸、原花青素B2、表儿茶素均在230、280 nm处有最大吸收,在280 nm下目标峰分离度高,基线平稳,故选280 nm为测定波长;考察了乙腈-0.1%冰醋酸水、乙腈-0.1%磷酸水及乙腈-0.1%甲酸水3种流动相体系,结果显示,乙腈-0.1%磷酸水系统下各峰分离效果好,故选择乙腈-0.1%磷酸水作为流动相。
为了更好地区分产地对质量的影响,本实验运用相似度评价、聚类分析、PCA 分析和 PLS-DA的化学计量学方法对不同产地翻白叶树进行质量评价研究。相似度评价可知,30批翻白叶树药材色谱图与对照指纹图谱的相似度在0.863~0.975,而对于Chen等[13]建立的翻白叶树指纹图谱,不同批次之间相似度在0.444~0.904之间,相比之下,本研究各个产地翻白叶树相似度较高。聚类分析可知,30批翻白叶树药材被分为3类,其中S2(贵州省榕江县)、S27(河北省保定市安国市)聚为一类,S24(安徽省黄山市张济良大药房)和S26(广西壮族自治区柳州市鹿寨县中医院)聚为一类,其余贵州产地、广东产地、云南产地、海南产地、四川产地、安徽产地、湖北产地、河南产地和浙江产地聚为一类。说明产地的生态环境、气候条件等因素相关造成不同的差异性。PCA和OPLS-DA与CA结果一致,表明30批翻白叶树药材化学成分既有相似性又有差异性,采用 OPLS-DA 模型 VIP 值筛选出原花青素B2、表儿茶素、新绿原酸是翻白叶树的差异性特征成分。通过前期对翻白叶树不同极性部位进行体外抗炎作用筛选,从乙酸乙酯部位得到的儿茶素、表儿茶素、原花青素B2均有一定的抗炎作用,且表儿茶素与原花青素含量较高。因此本实验以原儿茶酸、原花青素B2、表儿茶素作为翻白叶树差异特征成分进行含量测定。
由含量测定结果可知,这30批泛白叶树药材中大多数药材中原花青素B2和表儿茶素的含量均高于原儿茶酸,S13、S14、S17、S18中原儿茶酸高于原花青素B2和表儿茶素,分别产自贵州、江西、海南、海南;S24、S26、S27为广西产地,这3个批次原花青素B2及表儿茶素含量远高于其他批次;其中原儿茶酸含量最高的批次S17是原儿茶素含量最低的S6的16倍,原花青素B2含量最高的批次S26是原花青素B2含量最低的批次S1的39倍,表儿茶素含量最高的批次S26是表儿茶素含量最低的批次S1的23倍,各批药材含量差异较大,且没有明显规律,说明市场上流通的翻白叶树药材质量差异大,而造成这种因素的原因包括生长环境(海拔、土壤、水源、光照等)、采收时间、气候、产地、贮藏时间、加工方法、炮制方法等。
本实验首次建立了翻白叶树药材中3种成分原儿茶酸、原花青素B2及表儿茶素的HPLC含量测定方法,为进一步完善翻白叶树的质量控制提供科学依据。
  • 贵州省2019年中药资源普查项目(3052-052190023)
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2024年第59卷第24期
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doi: 10.11669/cpj.2024.24.004
  • 接收时间:2024-04-02
  • 首发时间:2025-11-13
  • 出版时间:2024-12-22
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  • 收稿日期:2024-04-02
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贵州省2019年中药资源普查项目(3052-052190023)
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    贵州中医药大学, 贵阳 550025

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* 胡成刚,男,硕士,教授,硕士生导师 研究方向:中药及民族药基础研究与开发 Tel:(0855)5353416
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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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