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指纹图谱结合一测多评法评价山楂叶质量
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李艳荣 ,段丽颖 ,魏 红 ,杜义龙 ,赵胜男 ,高 晗 ,潘海峰 (1.承德医学院中药研究所/河北省中药研究与
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开发重点实验室,河北 承德 067000;2.北京工业大学医院药剂科,北京 100124;3.神威药业集团有限公司,
石家庄 051430)
中图分类号 R917 文献标志码 A 文章编号 1001-0408(2023)22-2727-07
DOI 10.6039/j.issn.1001-0408.2023.22.07
摘 要 目的 建立不同产地山楂叶药材的指纹图谱和多成分含量测定方法,评价其质量并筛选差异标志物。方法 收集产自河
北省承德市、辽宁省葫芦岛市、山西省运城市、山东省临沂市的78批山楂叶药材,采用高效液相色谱(HPLC)法,利用《中药色谱指
纹图谱相似度评价系统(2012版)》绘制指纹图谱并进行相似度评价;采用SPSS 19.0、MetaboAnalyst 5.0工具、SIMCA 14.1软件等
进行灰色关联分析、聚类分析(CA)、主成分分析(PCA)和正交偏最小二乘判别分析(OPLS-DA),以变量重要性投影(VIP)值>1
且误差线不超过原点为标准筛选影响山楂叶质量的差异标志物。采用同一HPLC法结合一测多评(QAMS)法,以牡荆素鼠李糖
苷为内参物,测定 78 批山楂叶药材中绿原酸、牡荆素葡萄糖苷、金丝桃苷和异槲皮素的含量,并与外标法测定结果进行比较。
结果 4个产地的78批山楂叶药材指纹图谱中有8个共有峰被标定,有5种成分[绿原酸(峰1)、牡荆素葡萄糖苷(峰3)、牡荆素鼠李
糖苷(峰4)、金丝桃苷(峰7)和异槲皮素(峰8)]被指认,相似度为0.871~0.998。河北省承德市、辽宁省葫芦岛市、山西省运城市、
山东省临沂市样品的平均相对关联度分别为0.538、0.528、0.462、0.435;CA、PCA分析均显示,河北省承德市和辽宁省葫芦岛市样
品大致分为一类,山东省临沂市和山西省运城市样品大致分为一类;峰1、2、3、5的VIP值均大于1。QAMS法计算得绿原酸、牡荆
素葡萄糖苷、金丝桃苷、异槲皮素的平均相对校正因子分别为0.401、0.993、1.670、1.615(RSD<2%);与外标法结果比较,除2批样
品(S39、S41)中的异槲皮素外,其余批次样品中各成分的含量均无明显差异(相对偏差不高于5%)。结论 所建指纹图谱和QAMS
法操作简单,可用于评价山楂叶药材的质量;河北省承德市样品质量较优;绿原酸(峰1)、牡荆素葡萄糖苷(峰3)和峰2、5对应成分
可能是影响山楂叶药材质量的差异标志物。
关键词 山楂叶;指纹图谱;一测多评法;化学模式识别;差异标志物
Quality evaluation of Crataegus pinnatifida leaves by fingerprint combined with quantitative analysis of
multi-components by single-marker
LI Yanrong ,DUAN Liying ,WEI Hong ,DU Yilong ,ZHAO Shengnan ,GAO Han ,PAN Haifeng(1. Institute
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of Traditional Chinese Medicine/Key Laboratory of Traditional Chinese Medicine Research and Development of
Hebei Province, Chengde Medical University, Hebei Chengde 067000, China;2. Dept. of Pharmacy, Beijing
University of Technology Hospital, Beijing 100124, China;3. Shineway Pharmaceutical Group Ltd.,
Shijiazhuang 051430, China)
ABSTRACT OBJECTIVE To establish the fingerprint and multi-component content determination method of Crataegus
pinnatifida leaves from different producing areas, and to evaluate the quality of C. pinnatifida leaves and screen the differential
markers. METHODS Seventy-eight batches of C. pinnatifida leaves were collected from Chengde of Hebei Province, Huludao of
Liaoning Province, Yuncheng of Shanxi Province and Linyi of Shandong Province. High-performance liquid chromatography
(HPLC) and Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprints (2012 edition) were
used to draw the fingerprints and conduct similarity evaluation. Grey correlation analysis, cluster analysis (CA), principal
component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed by using SPSS
19.0, MetaboAnalyst 5.0 and SIMCA 14.1 software. The differential markers affecting the quality of C. pinnatifida leaves were
screened with variable importance in the projection (VIP) value greater than 1 and the error line not exceeding the origin as the
criterion. Using vitexin rhamnoside as an internal reference, the contents of chlorogenic acid, glucosylvitexin, hypericin and
isoquercetin in 78 batches of C. pinnatifida leaves were determined by the same HPLC combined with quantitative analysis of multi-
components by single-marker (QAMS), and the results were
Δ 基金项目 河北省重点研发计划项目(No.20372507D);河北省
compared with external standard method. RESULTS Eight
高校省级重点学科建设项目(No.冀教高〔2013〕4号)
* 第一作者 副 教 授 ,硕 士 。 研 究 方 向 :中 药 分 析 。 E-mail: common peaks were calibrated in the fingerprints for 78
liyanrong00001@163.com batches of C. pinnatifida leaves from 4 producing areas. Five
# 通信作者 教授,硕士生导师。研究方向:中药质量评价及中药 known components were identified, including chlorogenic acid
配方颗粒。电话:0314-2291186。E-mail:phf2301@163.com (peak 1), glucosylvitexin (peak 3), vitexin rhamnoside (peak
中国药房 2023年第34卷第22期 China Pharmacy 2023 Vol. 34 No. 22 · 2727 ·