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Article(id=1236346465778462795, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346464578891843, articleNumber=null, orderNo=null, doi=null, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=1662566400000, acceptedDateStr=2022-09-08, onlineDate=1772697567647, onlineDateStr=2026-03-05, pubDate=1684080000000, pubDateStr=2023-05-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772697567647, onlineIssueDateStr=2026-03-05, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772697567647, creator=13701087609, updateTime=1772697567647, updator=13701087609, issue=Issue{id=1236346464578891843, tenantId=1146029695717560320, journalId=1235980733773295621, year='2023', volume='32', issue='9', pageStart='865', pageEnd='968', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1772697567361, creator=13701087609, updateTime=1772697682369, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1236346947028701631, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346464578891843, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1236346947028701632, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346464578891843, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=961, endPage=968, ext={EN=ArticleExt(id=1236346466025926734, articleId=1236346465778462795, tenantId=1146029695717560320, journalId=1235980733773295621, language=EN, title=Screening and determination of quality markers of Folium Photiniae based on HPLC fingerprint and chemometrics, columnId=null, journalTitle=Chinese Journal of New Drugs, columnName=null, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish the HPLC-PDA fingerprint of Folium Photiniae combined with chemometrics to identify and screen the quality markers of Folium Photiniae, in order to provide a scientific basis for the quality of Folium Photiniae.

Methods:

The fingerprint was obtained by an Agilent Eclipse XDB-C18 (250 mm×4.6 mm,5 μm) chromatographic column with a mobile phase of acetonitrile (A)-0.1% formic acid aqueous solution (B) in a gradient elution. The volume flow rate was set at 1.0 mL·min-1, the wavelength was 350 nm and the column temperature was 35 ℃. The fingerprints of 15 batches of Folium Photiniae were established using the developed method and the similarity was evaluated. The common peaks were analyzed by chemical identification pattern to distinguish Folium Photiniae from different origins, and the quality markers of Folium Photiniae were screened.

Results:

The similarity of the 15 batches of Folium Photiniae were all above 0.996, and a total of 10 common peaks were calibrated. Cluster analysis, principal component analysis and partial least squares analysis screened out chromatographic peak No.1 (neochlorogenic acid), No.2 (chlorogenic acid), No.4 (rutin), No.5 (hyricoside), and No.6 (isoquercitrin) as the quality markers of Folium Photiniae. The contents of neochlorogenic acid and chlorogenic acid is positively correlated with the quality of Folium Photiniae. The contents of rutin, hypericin and isoquercitrin may be negatively correlated with the quality of Folium Photiniae, indicating that the contents of these three components in Folium Photiniae should be limited at a low level. Further quantitative analysis of the above five components indicated the linear ranges of 0.135 3~2.706 0, 0.134 0~2.680 0, 0.008 5~0.170 5, 0.015 6~0.312 8, 0.005 9~0.118 9 μg, respectively. The linear relationship of each component is good (R2≥0.999 0), and the average recovery rate is 99.30% to 101.90%.

Conclusion:

The established HPLC fingerprint and multi-component determination method are proved to be stable and reliable, which can provide a basis for the quality evaluation of Folium Photiniae.

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目的：

建立石楠叶药材HPLC-PDA指纹图谱，结合化学计量学识别和筛选石楠叶药材的质量标志物，为石楠叶的质量提供科学依据。

方法：

采用Agilent Eclipse XDB-C18色谱柱（250 mm×4.6 mm，5 μm）；以乙腈（A）-0.1%甲酸水溶液（B）为流动相，梯度洗脱，体积流量1.0 mL·min-1，检测波长350 nm，柱温35 ℃；建立15批石楠叶药材指纹图谱并进行相似度评价，对共有峰进行化学识别模式分析区分不同产地的石楠叶药材，筛选石楠叶的质量标志物。

结果：

15批石楠叶药材的相似度均在0.996以上，共标定了10个共有峰，聚类分析、主成分分析和偏最小二乘分析筛选出1号色谱峰（新绿原酸）、2号色谱峰（绿原酸）、4号色谱峰（芦丁）、5号色谱峰（金丝桃苷）、6号色谱峰（异槲皮苷）为石楠叶的质量标志性成分，其中新绿原酸、绿原酸的含量与药材的优质性呈正相关，芦丁、金丝桃苷和异槲皮苷的含量可能与药材质量呈负相关，说明这3种成分在药材中含量不宜太高。进一步对以上5个成分进行定量分析，线性范围分别为：0.135 3~2.706 0，0.134 0~2.680 0，0.008 5~0.170 5，0.015 6~0.312 8，0.005 9~0.118 9 μg，各成分线性关系良好（R2≥0.999 0），平均回收率在99.30%~101.90%。

结论：

建立的HPLC指纹图谱及多成分含量测定方法稳定、可靠，可为石楠叶药材的质量评价提供依据。

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吴玲芳，女，副教授，主要从事中药药效物质研究。联系电话：(0311)89926890，E-mail: 。
牛丽颖，女，博士生导师，教授，主要从事中药分析及药效物质基础研究。联系电话：(0311)89926890，E-mail: 。
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马永犇，男，硕士研究生，主要从事中药药效物质研究。E-mail: 。

, authorsList=马永犇, 田宇柔, 田伟, 高乐, 展佳琪, 冯希雅, 吴玲芳, 牛丽颖)}, authors=[Author(id=1236346466881564800, tenantId=1146029695717560320, journalId=1235980733773295621, articleId=1236346465778462795, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=Mayongben@hebcm.edu.cn, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1236346466957062279, tenantId=1146029695717560320, journalId=1235980733773295621, articleId=1236346465778462795, authorId=1236346466881564800, language=EN, stringName=Yong-ben MA, firstName=Yong-ben, middleName=null, lastName=MA, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1Hebei University of Traditional Chinese Medicine, Shijiazhuang 050091, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1236346467074502797, tenantId=1146029695717560320, journalId=1235980733773295621, articleId=1236346465778462795, authorId=1236346466881564800, language=CN, stringName=马永犇, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1河北中医学院，石家庄 050091, bio={"content":"

马永犇，男，硕士研究生，主要从事中药药效物质研究。E-mail: 。

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马永犇，男，硕士研究生，主要从事中药药效物质研究。E-mail: 。

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基于HPLC指纹图谱及化学计量学筛选石楠叶质量标志物及其含量测定研究
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马永犇 1 , 田宇柔 1, 2, 3 , 田伟 1, 2, 3 , 高乐 1, 2, 3 , 展佳琪 1 , 冯希雅 1 , 吴玲芳 1, 2, 3 , 牛丽颖 1, 2, 3
中国新药杂志 | 实验研究 2023,32(9): 961-968
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中国新药杂志 | 实验研究 2023, 32(9): 961-968
基于HPLC指纹图谱及化学计量学筛选石楠叶质量标志物及其含量测定研究
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马永犇1 , 田宇柔1, 2, 3, 田伟1, 2, 3, 高乐1, 2, 3, 展佳琪1, 冯希雅1, 吴玲芳1, 2, 3 , 牛丽颖1, 2, 3
作者信息
  • 1河北中医学院，石家庄 050091
  • 2河北省中药配方颗粒技术创新中心，石家庄 050091
  • 3中药材品质评价与标准化河北省工程研究中心，石家庄 050091

    • 马永犇，男，硕士研究生，主要从事中药药效物质研究。E-mail: 。

通讯作者:

吴玲芳，女，副教授，主要从事中药药效物质研究。联系电话：(0311)89926890，E-mail: 。
牛丽颖，女，博士生导师，教授，主要从事中药分析及药效物质基础研究。联系电话：(0311)89926890，E-mail: 。
Screening and determination of quality markers of Folium Photiniae based on HPLC fingerprint and chemometrics
Yong-ben MA1 , Yu-rou TIAN1, 2, 3, Wei TIAN1, 2, 3, Le GAO1, 2, 3, Jia-qi ZHAN1, Xi-ya FENG1, Ling-fang WU1, 2, 3 , Li-ying NIU1, 2, 3
Affiliations
  • 1Hebei University of Traditional Chinese Medicine, Shijiazhuang 050091, China
  • 2Hebei Traditional Chinese Medicine Formula Granule Engineering & Technology Innovate Center, Shijiazhuang 050091, China
  • 3Quality Evaluation & Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine, Shijiazhuang 050091, China
出版时间: 2023-05-15
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摘要
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目的：

建立石楠叶药材HPLC-PDA指纹图谱，结合化学计量学识别和筛选石楠叶药材的质量标志物，为石楠叶的质量提供科学依据。

方法：

采用Agilent Eclipse XDB-C18色谱柱（250 mm×4.6 mm，5 μm）；以乙腈（A）-0.1%甲酸水溶液（B）为流动相，梯度洗脱，体积流量1.0 mL·min-1，检测波长350 nm，柱温35 ℃；建立15批石楠叶药材指纹图谱并进行相似度评价，对共有峰进行化学识别模式分析区分不同产地的石楠叶药材，筛选石楠叶的质量标志物。

结果：

15批石楠叶药材的相似度均在0.996以上，共标定了10个共有峰，聚类分析、主成分分析和偏最小二乘分析筛选出1号色谱峰（新绿原酸）、2号色谱峰（绿原酸）、4号色谱峰（芦丁）、5号色谱峰（金丝桃苷）、6号色谱峰（异槲皮苷）为石楠叶的质量标志性成分，其中新绿原酸、绿原酸的含量与药材的优质性呈正相关，芦丁、金丝桃苷和异槲皮苷的含量可能与药材质量呈负相关，说明这3种成分在药材中含量不宜太高。进一步对以上5个成分进行定量分析，线性范围分别为：0.135 3~2.706 0，0.134 0~2.680 0，0.008 5~0.170 5，0.015 6~0.312 8，0.005 9~0.118 9 μg，各成分线性关系良好（R2≥0.999 0），平均回收率在99.30%~101.90%。

结论：

建立的HPLC指纹图谱及多成分含量测定方法稳定、可靠，可为石楠叶药材的质量评价提供依据。

石楠叶  /  指纹图谱  /  相似度评价  /  聚类分析  /  主成分分析  /  质量标志物
Objective:

To establish the HPLC-PDA fingerprint of Folium Photiniae combined with chemometrics to identify and screen the quality markers of Folium Photiniae, in order to provide a scientific basis for the quality of Folium Photiniae.

Methods:

The fingerprint was obtained by an Agilent Eclipse XDB-C18 (250 mm×4.6 mm,5 μm) chromatographic column with a mobile phase of acetonitrile (A)-0.1% formic acid aqueous solution (B) in a gradient elution. The volume flow rate was set at 1.0 mL·min-1, the wavelength was 350 nm and the column temperature was 35 ℃. The fingerprints of 15 batches of Folium Photiniae were established using the developed method and the similarity was evaluated. The common peaks were analyzed by chemical identification pattern to distinguish Folium Photiniae from different origins, and the quality markers of Folium Photiniae were screened.

Results:

The similarity of the 15 batches of Folium Photiniae were all above 0.996, and a total of 10 common peaks were calibrated. Cluster analysis, principal component analysis and partial least squares analysis screened out chromatographic peak No.1 (neochlorogenic acid), No.2 (chlorogenic acid), No.4 (rutin), No.5 (hyricoside), and No.6 (isoquercitrin) as the quality markers of Folium Photiniae. The contents of neochlorogenic acid and chlorogenic acid is positively correlated with the quality of Folium Photiniae. The contents of rutin, hypericin and isoquercitrin may be negatively correlated with the quality of Folium Photiniae, indicating that the contents of these three components in Folium Photiniae should be limited at a low level. Further quantitative analysis of the above five components indicated the linear ranges of 0.135 3~2.706 0, 0.134 0~2.680 0, 0.008 5~0.170 5, 0.015 6~0.312 8, 0.005 9~0.118 9 μg, respectively. The linear relationship of each component is good (R2≥0.999 0), and the average recovery rate is 99.30% to 101.90%.

Conclusion:

The established HPLC fingerprint and multi-component determination method are proved to be stable and reliable, which can provide a basis for the quality evaluation of Folium Photiniae.

Folium Photiniae  /  fingerprint  /  similarity evaluation  /  cluster analysis  /  principal component analysis  /  quality markers
马永犇, 田宇柔, 田伟, 高乐, 展佳琪, 冯希雅, 吴玲芳, 牛丽颖. 基于HPLC指纹图谱及化学计量学筛选石楠叶质量标志物及其含量测定研究. 中国新药杂志, 2023 , 32 (9) : 961 -968 .
Yong-ben MA, Yu-rou TIAN, Wei TIAN, Le GAO, Jia-qi ZHAN, Xi-ya FENG, Ling-fang WU, Li-ying NIU. Screening and determination of quality markers of Folium Photiniae based on HPLC fingerprint and chemometrics[J]. Chinese Journal of New Drugs, 2023 , 32 (9) : 961 -968 .
基金
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  • 河北省中医药管理局科研计划项目(2023114)
  • 河北省高等学校科学技术研究资助项目(QN2019119)
  • 河北省中医药管理局科研计划项目(2020130)
  • 河北中医学院博士基金资助项目(BZS2019001)
2023年第32卷第9期
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  • 首发时间：2026-03-05
  • 出版时间：2023-05-15
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出版历史
  • 录用日期：2022-09-08
基金
河北省中医药管理局科研计划项目(2023114)
河北省高等学校科学技术研究资助项目(QN2019119)
河北省中医药管理局科研计划项目(2020130)
河北中医学院博士基金资助项目(BZS2019001)
作者信息
    1河北中医学院，石家庄 050091
    2河北省中药配方颗粒技术创新中心，石家庄 050091
    3中药材品质评价与标准化河北省工程研究中心，石家庄 050091

通讯作者:

吴玲芳，女，副教授，主要从事中药药效物质研究。联系电话：(0311)89926890，E-mail: 。
牛丽颖，女，博士生导师，教授，主要从事中药分析及药效物质基础研究。联系电话：(0311)89926890，E-mail: 。
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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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