基于多元活性成分同时测定结合多元统计分析评价不同产地金钱草药材的质量  

Quality evaluation of Lysimachiae Herba from different habitats based on simultaneous determination of multiple bioactive constituents combined with multivariate statistical analysis

作　　者：周永逸 陈海杰 薛佳 吴楠 袁嘉欢 刘训红[1,2] 邹立思 陈翠花[1] 蔡芷辰 杨薇[1] 程建明 ZHOU Yong-yi;CHEN Hai-jie'XUE Jjia;WU Nan;YUAN Jia-huan;LIU Xun-hong;ZOU Li-si;CHEN Cui-hua;CAI Zhi-chen;YANG Wei;CHENG Jian-ming(School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China;Jiangsu Province Engineering Research Center of Classical Prescription,Nanjing 210023,China)

机构地区：[1]南京中医药大学药学院,江苏南京210023 [2]江苏省经典名方工程研究中心,江苏南京210023

出　　处：《中国中药杂志》2023年第17期4663-4674,共12页China Journal of Chinese Materia Medica

基　　金：江苏高校品牌专业建设工程项目(PPZY2015A070)。

摘　　要：建立了超高效液相色谱-三重四极杆/线性离子阱质谱(UHPLC-QTRAP-MS/MS)同时测定金钱草中黄酮类、有机酸类、核苷类及氨基酸类共41种活性成分含量的方法,考察不同产地金钱草中多元活性成分含量的差异。采用Waters XBridge^(■)C18(4.6 mm×100 mm,3.5μm)色谱柱,以甲醇(A)和0.4%甲酸水(B)进行梯度洗脱,柱温30℃,流速0.8 mL·min^(-1),多反应监测模式检测(MRM);根据41种目标成分的含量,依次用聚类分析(HCA)、正交偏最小二乘法判别分析(OPLS-DA)以及灰色关联度分析(GRA)对不同产地金钱草药材进行综合评价。结果显示,41种目标成分在一定质量浓度范围内均呈良好的线性关系,相关系数(r)均大于0.9994;精密度、重复性和稳定性的相对标准偏差(RSD)均小于5.0%;平均加样回收率为98.06%~101.9%,RSD为0.62%~4.6%;HCA和OPLS-DA结果表明,48批不同产地金钱草药材样品分为3类,分别为川渝产区,江苏、浙江和江西产区以及贵州产区,3类产区样品中41种活性成分的含量差异显著;GRA结果显示,四川省南充市的金钱草样品综合质量较好。该研究所建立的多元活性成分同时测定结合多元统计分析评价体系准确、可靠,可用于金钱草药材内在质量的综合评价,同时为金钱草药材产地的优选提供基础资料。A method based on ultra-high performance liquid chromatography coupled with triple quadrupole linear ion trap-tandem mass spectrometry(UHPLC-QTRAP-MS/MS)was developed for the simultaneous determination of 41 bioactive constituents of flavonoids,organic acids,nucleosides,and amino acids in Lysimachiae Herba.The content of multiple bioactive constituents was compared among the samples from different habitats.The chromatographic separation was performed in a Waters XBridge^(■)C_(18)column(4.6 mm×100 mm,3.5μm)at 30℃.The gradient elution was performed with 0.4%methanol(A)-formic acid water(B)as the mobile phase at a flow rate of 0.8 mL·min^(-1),and the multiple-reaction monitoring(MRM)mode was adopted.According to the content of 41 constituents,hierarchical cluster analysis(HCA),orthogonal partial least squares discriminant analysis(OPLS-DA),and gray relational analysis(GRA)were perfomed to comprehensively evaluate the samples from different habitats.The results showed that the 41 constituents exhibited good linear relationship within the tested concentration ranges,with the correlation coefficients(r)greater than 0.9994.The method featured good precision,repeatability,and stability with the relative standard deviations(RSDs)less than 5.0%.The average recoveries of the 41 constituents ranged from 98.06%to 101.9%,with the RSDs of 0.62%-4.6%.HCA and OPLS-DA separated 48 batches of Lysimachiae Herba samples from different habitats into three categories:the producing areas in Sichuan and Chongqing,the producing areas in Jiangsu,Zhejiang,and Jiangxi,and the producing areas in Guizhou.The content of 41 constituents varied among the Lysimachiae Herba samples from different habitats.The GRA results revealed that the Lysimachiae Herba sample from Nanchong City,Sichuan Province had the best comprehensive quality.The method developed in this study was accurate and reliable and thus can be used for comprehensive evaluation of Lysimachiae Herba quality and provide basic information for the selection of habitats.

关 键 词：金钱草 不同产地 超高效液相色谱-三重四极杆/线性离子阱质谱 多元活性成分 多元统计分析 

分 类 号：R284.1[医药卫生—中药学]