基于多元活性成分同时测定结合多元统计分析评价不同干燥加工三叶青药材的质量  

Quality Evaluation of Tetrastigmae Radix under Different Drying Methods Based on Simultaneous Determination of Multiple Bioactive Constituents Combined with Multivariate Statistical Analysis

作　　者：陈海杰 周永逸 薛佳 邹立思[1] 吴楠 袁嘉欢 刘训红[1,2] 杨薇 程建明 CHEN Hai-jie;ZHOU Yong-yi;XUE Jia;ZOU Li-si;WU Nan;YUAN Jia-huan;LIU Xun-hong;YANG Wei;CHENG Jian-ming(School of Pharmacy,Nanjing University of Traditional Chinese Medicine,Nanjing 210023,China;Engineering Research Center for Classical Recipes of Jiangsu Province,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：《分析测试学报》2023年第3期251-263,共13页Journal of Instrumental Analysis

基　　金：江苏高校品牌专业建设工程资助项目(PPZY2015A070)。

摘　　要：建立了一种超快速液相色谱-三重四极杆-线性离子阱质谱(UFLC-QTRAP-MS/MS)同时测定三叶青中黄酮类、鞣质类、酚酸类、核苷类、多酚类和氨基酸类等60种活性成分的快速分析方法,并结合多元统计分析,评价不同干燥加工三叶青的质量。采用XBridge^(®)C_(18)柱(4.6 mm×100 mm,3.5μm)以0.4%甲酸-甲醇为流动相进行梯度分离,以多反应监测模式在电喷雾正、负离子模式下进行质谱检测。基于各目标成分的质量浓度,用方差分析(ANOVA)、熵权TOPSIS法及灰色关联度分析(GRA)对不同干燥加工三叶青样品进行综合评价。结果显示,各目标成分在一定质量浓度范围内的线性关系良好,相关系数均不低于0.9990,检出限为0.03~13.59 ng/mL,定量下限为0.09~45.30 ng/mL,平均加标回收率为96.1%~102%,相对标准偏差均小于5%;不同干燥方式对三叶青的多种活性成分有影响,与传统的干燥方式相比,现代的干燥方式能明显保留三叶青的活性成分。综合分析,真空干燥的三叶青样品的综合质量较好。该研究构建的方法可为三叶青的合理干燥和加工提供实验依据,同时也为三叶青质量的综合评价和整体控制提供新的方法参考。An ultra-fast liquid chromatography-triple quadrupole-linear ion trap mass spectrometry(UFLC-QTRAP-MS/MS)was developed for the rapid and simultaneous analysis of 60 active constituents including flavonoids,tannins,phenolic acids,nucleosides,polyphenols and amino acids in Tetrastigmae Radix,which was combined with multivariate statistical analysis to evaluate the quality of Tetrastigmae Radix dried or processed by different methods.The gradient separation was performed on an XBridge^(®)C_(18) column(4.6 mm×100 mm,3.5μm)with 0.4%formic acidmethanol as mobile phase,and the mass spectrometric detection was carried out in electrospray positive or negative ion mode under multiple reaction monitoring(MRM)mode.The samples of differently dried and processed Tetrastigmae Radix were comprehensively evaluated by entropy weight TOPSIS,analysis of variance(ANOVA)method and gray correlation analysis(GRA)according to the contents of 60 target constituents.The results showed that there were good linear relationships for 60 target constituents in a certain mass concentration range,with their correlation coefficients(r2)not less than 0.9990.The limits of detection(LODs)and the limits of quantitation(LOQs)were in the range of 0.03-13.59 ng/mL and 0.09-45.30 ng/mL,respectively.The average spiked recoveries for the samples ranged from 96.1%to 102%,with relative standard deviations(RSDs)less than 5%.Different drying methods have certain effects on the multiple active constituents in Tetrastigmae Radix,and modern drying methods could significantly retain the active constituents in Tetrastigmae Radix compared with the traditional drying methods.The ANOVA showed that the low temperature drying treatment had a good retention effect on flavonoids,tannins,and polyphenols.The loss of nucleosides and phenolic acids in Tetrastigmae Radix was low under vacuum drying conditions.Sun-drying or shade-drying treatment tends to cause the loss of amino acids in Tetrastigmae Radix.The results of GRA and TOPSIS analyses were the same,and the quality r

关 键 词：三叶青 不同干燥方式 多元活性成分 多元统计分析 超快速液相色谱-三重四极杆-线性离子阱质谱(UFLC-QTRAP-MS/MS) 

分 类 号：O657.63[理学—分析化学] R282.4[理学—化学]