UPLC-QTRAP-MS分析不同产地茯苓药材中8个三萜酸类成分  

Analysis of 8 triterpene acids in Poria from different habitats based on UPLC-QTRAP-MS

作　　者：赵秋龙 张丽[1] 卞晓坤 钱大玮[1] 郭盛[1] 严辉[1] 王团结[2] 陈志鹏[1] 段金廒[1] ZHAO Qiu-long;ZHANG Li;BIAN Xiao-kun;QIAN Da-wei;GUO Sheng;YAN Hui;WANG Tuan-jie;CHEN Zhi-peng;DUAN Jin-ao(Collaborative Innovation Center of Chinese Medicinal Resources Industrialization,Nanjing 210023,China;Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China)

机构地区：[1]南京中医药大学江苏省中药资源产业化过程协同创新中心,南京210023 [2]江苏康缘药业股份有限公司,连云港222001

出　　处：《药物分析杂志》2020年第7期1169-1177,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家中药标准化项目(ZYBZH-C-JS-28)。

摘　　要：目的:建立超高效液相色谱-串联四极杆/线性离子阱质谱法(UPLC-QTRAP-MS法)同时测定不同产地茯苓药材中8个三萜酸类成分(茯苓新酸B、去氢土莫酸、茯苓新酸A、猪苓酸C、去氢茯苓酸、茯苓酸、松苓新酸、去氢齿孔酸)的含量,并比较其差异。方法:采用Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸水-乙腈,梯度洗脱,流速0.4 mL·min-1,柱温25℃,以多反应监测(MRM)方法进行质谱扫描,并利用偏最小二乘判别分析(PLS-DA)绘制得分图。结果:8个化合物线性范围良好,相关系数(r2)均大于0.9969,平均加样回收率在98.1%~101.1%范围内,RSD≤3.2%,经PLS-DA分析,茯苓样品按产地被聚集为3组,并通过变量权重重要性排序(VIP值)图发现茯苓新酸A、去氢土莫酸、去氢茯苓酸、猪苓酸C为3个产地茯苓样品间的主要差异成分。结论:所建立的茯苓药材UPLC-QTRAP-MS质量评价方法可用于茯苓药材的多成分的快速测定及质量控制。Objective:To establish an ulter-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry(UPLC-QTRAP-MS)method to simultaneously determine eight triterpenic acids(poricoic acid B,dehydrotumulosic acid,poricoic acid A,polyporenic acid C,dehydropachymic acid,pachymic acid,dehydrotrametenolic acid and dehydroeburicoic acid)in Poria from different habitats and compare the differences.Methods:The determination was performed on a Waters UPLC BEH C18 column(2.1 mm×100 mm,1.7μm),with gradient elution of water(0.1%formic acid)and acetonitrile at a flow rate of 0.4 mL·min-1.The column temperature was 25℃.The target compounds were analyzed by multiple reaction monitoring(MRM)mode.And the score plot was obtained by partial least squares discriminant analysis(PLS-DA).Results:The linear ranges of the 8 compounds were good,the correlation coefficients(r2)were all above 0.9969,and the average recoveries were between 98.1%and 101.1%with RSDs≤3.2%.All samples were divided into 3 groups according to habitats.Poricoic acid A,dehydrotumulosic acid,dehydropachymic acid and polyporenic acid C were found to be the main differential components in the samples from different habitats based on VIP value map.Conclusion:The established UPLC-QTRAP-MS quality evaluation method can be used for rapid determination and quality control of multi-components in Poria.

关 键 词：茯苓 三萜酸类成分 茯苓新酸 去氢土莫酸 猪苓酸 去氢茯苓酸 茯苓酸 松苓新酸 去氢齿孔酸 超高效液相色谱-串联四极杆/线性离子阱质谱法 含量测定 最小二乘判别分析 质量评价 

分 类 号：R917[医药卫生—药物分析学]