基于HPLC指纹图谱结合多成分含量测定和化学模式识别的大山楂丸质量评价  

Quality Evaluation of Dashanzha Pills Based on HPLC Fingerprint and Multi-Component Analysis Combined with Chemical Pattern Recognition

作　　者：李运 王苗 刘晓玲 许晓辉 马海棠 戚鹏飞 邱国玉 程显隆[4] LI Yun;WANG Miao;LIU Xiaoling;XU Xiaohui;MA Haitang;QI Pengfei;QIU Guoyu;CHENG Xianlong(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China;College of Pharmacy,Gansu University of Chinese Medicine,Lanzhou 730000,China;Gansu Pharmaceutical Group Science and Technology Innovation Research Institute Co.,Lid.Lanzhou 730000,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]兰州市食品药品检验检测研究院,兰州730050 [2]甘肃中医药大学药学院,兰州730000 [3]甘肃药业集团科技创新研究院有限公司,兰州730000 [4]中国食品药品检定研究院,北京100050

出　　处：《中国药学杂志》2024年第24期2372-2383,共12页Chinese Pharmaceutical Journal

基　　金：甘肃省药品科研项目资助(2022GSMPA0037);陇原青年创新创业人才项目资助(2023LQGR49);兰州市青年科技人才创新项目资助(2023-QN-144);兰州市科技计划项目资助(2022-2-2)。

摘　　要：目的建立大山楂丸(Dashanzha Pills,DSZP)的高效液相色谱(HPLC)指纹图谱及5种指标性成分的含量测定方法,并结合化学模式识别法对其质量进行评价。方法分析采用Eclipse Plus C18色谱柱(4.6 mm×250 mm,5μm),柱温30℃;以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,流速1.0 mL·min-1,检测波长250 nm,进样量10μL。基于51批次DSZP样本建立指纹图谱,指认了5种指标性成分,并对其进行了定量测定,结合聚类分析、主成分分析(principle component analysis,PCA)、正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等模式识别方法对DSZP进行综合分析。结果建立了DSZP指纹图谱,共标定了16个共有峰,并指认了5个化学成分,分别为绿原酸(5号峰)、香草酸(6号峰)、金丝桃苷(7号峰)、异绿原酸B(9号峰)、异绿原酸A(10号峰);含量测定5种指标性成分的线性关系良好(r>0.998),加标回收率在96.27%~109.35%,RSD在2.83%~4.07%。绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A的含量分别在0.0472~0.2270、0.0097~0.0362、0.0230~0.3702、0.0064~0.0632和0.0217~0.0645 mg·g-1之间。除厂家Q2外,其余厂家样品含量在各自均值的±30%,表明不同企业间的产品质量存在一定差异。化学模式识别结果提示,所有样品大致可分为两类,表明企业内的制备工艺较稳定,但企业间存在一定差异。筛选得到的样品差异标志物中包括指标成分绿原酸、金丝桃苷和异绿原酸B。结论该定量方法准确、快速,可行性较高,结合化学模式识别可为DSZP的质量进行综合评价。OBJECTIVE To establish the HPLC fingerprints and content determination method of five index components of Dashanzha pills(DSZP),and evaluate the quality combined with chemical pattern recognition.METHODS The analysis was performed on an Eclipse plus C_(18)column(4.6 mm×250 mm,5μm)at 30℃.Acetonitrile-0.1%formic acid aqueous solution was used as the mobile phase for gradient elution at flow rate of 1.0 mL·min~(-1).The detection wavelength was set at 250 nm,and the injection volume was 10μL.Based on 51 batches of DSZP samples,the fingerprint was established,and five index components were identified and quantitatively determined.Cluster analysis,principal component analysis and orthogonal partial least squares discriminant analysis were used to comprehensively analyze 51 batches of samples.RESULTS The fingerprints of DSZP were established,sixteen peaks were identified,and five chemical components were identified.They were chlorogenic acid(peak 5),vanillic acid(peak 6),hyperoside(peak 7),isochlorogenic acid B(peak 9),and isochlorogenic acid A(peak 10).The linear relationship of the five index components was good(r>0.998),and the recovery rate was 96.27%-109.35%,and the RSD was 2.83%-4.07%.The contents of chlorogenic acid,vanillicacid,hyperoside,isochlorogenic acid B,and isochlorogenic acid A were 0.0472-0.2270,0.0097-0.0362,0.0230-0.3702,0.0064-0.0632 and 0.0217-0.0645 mg·g~(-1),respectively.Except for manufacturer Q2,the contents of the products from the other manufacturers samples were maintained at(100±30)%of their respective average values,and the contents of the five components of manufacturer Q2 were mostly higher than 30%of the average value of all samples,indicating that there were great differences in product quality among different enterprises.The results of chemical pattern recognition showed that all samples could be roughly divided into two categories,indicating that the preparation process was relatively stable within the enterprise,but there were some differences between enterprises.The differen

关 键 词：大山楂丸 高效液相色谱指纹图谱 化学模式识别 质量控制 金丝桃苷 异绿原酸B 

分 类 号：R917[医药卫生—药物分析学]