经典名方清金化痰汤物质基准指纹图谱及多指标含量测定研究  

Quality Control of Classical Famous Prescriptions Qingjinhuatan decoction Based on HPLC Fingerprint and Simultaneous Determination of Multi-Components

作　　者：李莹曼 张林林[2,3] 朱强[4] 刘建庭 李翔宇[4] 张洪兵[2] 韩彦琪[2] 王权 许浚[2,3] 张铁军[2,3] Li Yingman;Zhang Linlin;Zhu Qiang;Liu Jianting;Li Xiangyu;Zhang Hongbing;Han Yanqi;Wang Quan;Xu Jun;Zhang Tiejun(Graduate School of Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;Tianjin Key Laboratory of Quality Indicators of Traditional Chinese Medicine,Tianjin Pharmaceutical Research Institute,Tianjin 300301,China;State Key Laboratory of Drug Release Technology and Pharmacokinetics,Tianjin Pharmaceutical Research Institute,Tianjin 300301,China;Anhui Jiren Pharmaceutical Co.,Ltd.Bozhou 236800,China)

机构地区：[1]天津中医药大学研究生院,天津301617 [2]天津药物研究院天津市中药质量标志物重点实验室,天津300301 [3]天津药物研究院释药技术与药代动力学国家重点实验室,天津300301 [4]安徽济人药业有限公司,亳州236800

出　　处：《世界科学技术-中医药现代化》2023年第1期163-174,共12页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：国家自然科学基金委员会重点项目(81830111):基于“成分构成-靶标网络-生物效应”多维整合的中药质量标志物发现与确认,负责人:许海玉;国家科学技术部国家重大新药创制计划课题(2018ZX09721004-006):基于中医典籍的肺系病经典名方清金化痰汤的新药研发,负责人:李文军。

摘　　要：目的建立清金化痰汤物质基准(QJHT)的高效液相色谱(HPLC)指纹图谱及栀子苷、芒果苷、橙皮苷、黄芩苷、汉黄芩苷的含量测定方法,为其质量控制提供参考。方法采用Agilent Eclipse XDB C_(18)色谱柱,以乙腈-0.1%磷酸水为流动相(梯度洗脱),流速设为1.0 mL·min^(-1),检测波长为230 nm,柱温为30℃,进样量为10μL。采用《中药色谱指纹图谱相似度评价系统》(2012版)绘制20批QJHT指纹图谱,明确共有峰,进行相似度分析。采用SPSS 26、MeV-4.9.0和SIMCA 14.1软件进行化学模式识别研究,筛选出影响其质量的关键性成分。采用Agilent ZORBAX Eclipse XDB C_(18)色谱柱,以乙腈-0.1%磷酸水为流动相(梯度洗脱),流速为1.0 mL·min^(-1),进样量为10μL,柱温为30℃,检测波长为240 nm(0-30 min),276 nm(30-60 min),建立含量测定方法。结果20批物质基准特征图谱的相似度均大于0.99,共指认了23个共有峰。聚类分析(CA)、主成分分析(PCA)和正交偏最小二乘法判别分析(OPLS-DA)均将物质基准分为3类,即S1-S6、S11-S16聚为一类,S7-S10、S17、S18、S20聚为一类,S19单独聚为一类。通过结合PCA和OPLS-DA,筛选出影响物质基准分类的化学成分,分别归属于黄芩、栀子、橘红、桑白皮和甘草。含量测定显示,栀子苷、芒果苷、橙皮苷、黄芩苷、汉黄芩苷分别在浓度为13.75-141.00、7.52-77.10、5.97-61.20、29.43-301.80、7.41-76.05μg·mL^(-1)范围内,线性关系良好;回收率分别为100.90%、100.11%、97.75%、102.93%、98.65%;含量分别为1.85%、0.21%、0.34%、3.76%、0.74%。结论本文建立的指纹图谱和多指标含量测定方法准确、稳定,为经典名方清金化痰汤的物质基准及相关制剂的质量控制提供依据。Objective The HPLC fingerprint of Qingjinhuatan decoction(QJHT) and the determination method of geniposide,mangiferin,hesperidin,baicalin and wogonoside were established to provide reference for its quality control.Methods The fingerprint was performed on Agilent Eclipse XDB C_(18) column with acetylene-0.1% phosphoric acid water as the mobile phase(gradient elution),the flow rate was set to 1.0 mL·min^(-1),the detection wavelength was 230 nm,the column temperature was 30 ℃,and the injection volume was 10 μL.The HPLC fingerprint of 20 batches of QJHT was drawn and the similaritiy evaluatin were carried out by using the Similarity Evaluation System of Chinese medicine Chromatographic Fingerprint(2012 edition),and the common peaks were also confirmed.Chemical pattern recognition studies were conducted using SPSS 26,MeV-4.9.0 and SIMCA 14.1 software to screen out key components that affect their quality.The content determination method was established by using Agilent ZORBAX Eclipse XDB C_(18) column with mobile phase consisted of acetylene-0.1% phosphoric acid water(gradient elution),the flow rate was 1.0 mL·min^(-1) and the injection volume was 10 μL,the column temperature was maintained at 30 ℃,the detection wavelength were set at 240 nm(0-30 min),276 nm(30-60 min).Results The similarities of the 20 batches of substance were greater than 0.99,and a total of 23 common peaks were identified.By cluster analysis(CA),principal component analysis(PCA),and orthogonal partial least squares discriminant analysis(OPLS-DA),the substance benchmarks were divided into three categories,S1-S6,S11-S16 were clustered into one category,S7-S10,S17,S18,S20 were clustered into one category,and S19 were clustered into one category.By combining PCA and OPLS-DA,the chemical constituents that determine the classification of QJHT were screened out,which belonged to Scutellariae Radix,Gardeniae Fructus,Citri Exocarpium Rubrum,Mori Cortex and Glycyrrhizae Radix,respectively.The content determination showed that geniposide,mangiferin,

关 键 词：经典名方 清金化痰汤 物质基准 指纹图谱 含量测定 聚类分析 主成分分析 正交偏最小二乘-判别分析 

分 类 号：R284.1[医药卫生—中药学]