天然产物研究与开发 ›› 2015, Vol. 27 ›› Issue (1): 73-76.doi: 10.16333/j.1001-6880.2015.01.015

• 研究简报 • 上一篇    下一篇

UPLC-MRM-MS法测定头花蓼药材中7个指标成分

刘跃1,胡杰1,谢玉敏1,黄勇1,廖尚高2,郑林*   

  1. 1 贵阳医学院 药学院 贵州省药物制剂重点实验室;2 贵阳医学院 民族药与中药开发应用教育部工程研究中心,贵阳 550004
  • 出版日期:2015-01-31 发布日期:2015-02-12

Determination of Seven Components in Polygonum capitatum by UPLC-MRM-MS

LIU Yue1, HU Jie1, XIE Yu-min1, HUANG Yong1, LIAO Shang-gao2, ZHENG Lin1*   

  1. 1 Guizhou Provincial Key Laboratory of Pharmaceutics,School of Pharmacy,Guiyang Medical College; 2 Engineering Research Center for the Development and Application of Ethnic Medicine and TCM (Ministry of  Education),Guiyang Medical College,Guiyang 550004,China
  • Online:2015-01-31 Published:2015-02-12

摘要: 建立头花蓼药材中没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-(2″-没食子酰基)-鼠李糖苷及槲皮素的UPLC-MRM-MS检测方法。色谱采用Waters BEH C18(2.1 mm×50 mm,1.7 μm)色谱柱,以0.1%甲酸乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,质谱采用多反应离子监测(MRM)检测。没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-(2″-没食子酰基)-鼠李糖苷及槲皮素分别在0.136~32.965、0.031~7.481、0.022~5.300、0.076~18.433、0.085~20.737、0.017~4.147、0.128~31.029 μg/mL浓度范围线性关系良好,平均回收率为91.23%~105.33%,RSD<3%,精密度、重复性和稳定性良好。此方法操作简便,快速,灵敏度高,可用于头花蓼药材中主要活性成分的含量测定,并为头花蓼药材质量控制提供了新方法。

关键词: 头花蓼, UPLC-MRM-MS, 没食子酸, 原儿茶酸, 槲皮素, 含量测定

Abstract: To establish a UPLC-MRM-MS method for the determination of gallic acid,protocatechuic acid,que-3-O-β-D-Glc,quercitrin,catechin,que-3-O-(2″-O-galloyl)β-D-Glc and quercetin in Polygonum capitatum. The analysis was achieved by BEH C18 column with a mobile phase composed of 0.1% formic acid in acetonitrile and 0.1% formic acid in water using gradient elution.A TQD tandem mass spectrometry was used as detector and operated by multiple reaction monitoring (MRM) mode.Good linearity was achieved for these components in the range of 0.136-32.965,0.031-7.481,0.022-5.300,0.076-18.433,0.085-20.737,0.017-4.147,0.128-31.029 μg/mL,respectively.The average recoveries were 91.23%-105.33%,with RSD less than 3%.Precision,repeatability and stability were good.The developed method was simple,rapid,sensitive and suitable for the determination of the main active constituents in P.capitatum. It provided a new method for the quality control of P.capitatum.

Key words: Polygonum capitatum, UPLC-MRM-MS, gallic acid, protocatechuic acid, quercetin, content determination

中图分类号: 

R927.2