摘要
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-C_(18)色谱柱(250 mm×4.6 mm, 5μm);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 9μg,各成分线性关系良好(R^(2)≥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。
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-C_(18)(250 mm×4.6 mm,5μm)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 C.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 0.1353~2.7060,0.1340~2.6800,0.0085~0.1705,0.0156~0.3128,0.0059~0.1189μg,respectively.The linear relationship of each component is good(R^(2)≥0.9990),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.
作者
马永犇
田宇柔
田伟
高乐
展佳琪
冯希雅
吴玲芳
牛丽颖
MA Yong-ben;TIAN Yu-rouu;TIAN Wei;GAO Le;ZHAN Jia-qi;FENG Xi-ya;WU Ling-fan;NIU Li-ying(Hebei University of Traditional Chinese Medicine,Shijiazhuang 050091,China;Hebei Traditional Chinese Medicine Formula Granule Engineering&Technology Innovate Center,Shjiazhuang 050091,China;Quality Evaluation&Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine,Shijiazhuang 050091,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2023年第9期961-968,共8页
Chinese Journal of New Drugs
基金
河北省中医药管理局科研计划项目(2023114)
河北省中医药管理局科研计划项目(2020130)
河北省高等学校科学技术研究资助项目(QN2019119)
河北中医学院博士基金资助项目(BZS2019001)。
关键词
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
Folium Photiniae
fingerprint
similarity evaluation
cluster analysis
principal component analysis
quality markers
