基于UFLC-Triple-TOF-MS/MS技术的白虎加桂枝汤化学物质基础

郭敏群; 严曾豪; 吴灏; 林娜

doi:10.13422/j.cnki.syfjx.20190713

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基于UFLC-Triple-TOF-MS/MS技术的白虎加桂枝汤化学物质基础

资源与质量评价 | 更新时间：2021-02-09

- 基于UFLC-Triple-TOF-MS/MS技术的白虎加桂枝汤化学物质基础
- Chemical Material Basis of Extract of Baihu Jia Guizhi Tang by UFLC-Triple-TOF-MS/MS
- 中国实验方剂学杂志 2019年25卷第10期页码：134-141
- 作者机构：
  
  1.广州中医药大学，广州　 510006；
  2.中山大学　生命科学学院，广州　 510275；
  3.中国中医科学院　中药研究所，北京　 100700
- 作者简介：
  
  郭敏群，在读硕士，从事中药学研究，Tel: 010-64014411-2869，E-mail: guominqun66@163.com
  *林娜，博士，研究员，博士生导师，从事方剂的作用原理研究，Tel: 010-64014411-2869，E-mail: linna888@163.com
- 基金信息：
  
  国家自然科学基金重点项目(81630107)
- DOI：10.13422/j.cnki.syfjx.20190713
  中图分类号： R283.6; R289; R284.1; R2-031
- 收稿日期：2018-09-30，
  
  网络出版日期：2018-12-19，
  
  纸质出版日期：2019-05-20
- 稿件说明：
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郭敏群, 严曾豪, 吴灏, 等. 基于UFLC-Triple-TOF-MS/MS技术的白虎加桂枝汤化学物质基础[J]. 中国实验方剂学杂志, 2019,25(10):134-141.

Min-qun GUO, Zeng-hao YAN, Hao WU, et al. Chemical Material Basis of Extract of Baihu Jia Guizhi Tang by UFLC-Triple-TOF-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(10): 134-141.
郭敏群, 严曾豪, 吴灏, 等. 基于UFLC-Triple-TOF-MS/MS技术的白虎加桂枝汤化学物质基础[J]. 中国实验方剂学杂志, 2019,25(10):134-141. DOI： 10.13422/j.cnki.syfjx.20190713.

Min-qun GUO, Zeng-hao YAN, Hao WU, et al. Chemical Material Basis of Extract of Baihu Jia Guizhi Tang by UFLC-Triple-TOF-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(10): 134-141. DOI： 10.13422/j.cnki.syfjx.20190713.

摘要

目的：

采用超快速高效液相色谱串联四级飞行时间质谱(UFLC-Triple-TOF-MS/MS)对白虎加桂枝汤的化学成分进行研究。

方法：

采用Phenomenex C

色谱柱(3.0 mm×100 mm，2.6 μm)，以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相，梯度洗脱，柱温40 ℃，流速0.3 mL·min

－1

，进样量5 μL；采用高分辨三重四级杆飞行时间质谱，分别在正、负离子模式下进行检测；借助Peakview软件中Formula Finder功能计算化合物的元素组成，调用软件中IDA explore功能，获得该质量数的二级碎片离子，结合文献数据和对照品数据比对进行化合物结果鉴定。

结果：

通过精确相对分子质量的质谱裂解规律，定性白虎加桂枝汤的35个化合物，包括甾体皂苷类16个、三萜皂苷类6个、黄酮类7个、有机酸类4个和其他类2个，其中10个成分(知母皂苷AⅢ，知母皂苷Ⅰ，知母皂苷BⅢ，知母皂苷BⅡ，新芒果苷，芒果苷，芹糖甘草苷，甘草苷，甘草酸和肉桂酸)通过与对照品比对确认，并对化合物的药材来源进行归属。

结论：

UFLC-Triple-TOF-MS/MS可以简便、快速地对白虎加桂枝汤中化学成分进行定性。相关研究为该方的药效物质基础研究、质量控制以及作用原理阐释提供了参考。

Abstract

Objective:

To systematically identify the chemical constituents in extract of Baihu Jia Guizhi Tang (BHGZT) by ultra-fast liquid chromatography/triple time-of-flight tandem mass spectrometry (UFLC-Triple-TOF-MS/MS).

Method:

Phenomenex C

(3.0 mm×100 mm

2.6 μm) was eluted with acetonitrile (containing 0.1%formic acid) and 0.1%formic acid solution as the mobile phase in a gradient mode. The column temperature was set at 40 ℃

the flow rate was 0.3 mL·min

-1

and the injection volume was 5 μL. High-resolution triple quadrupole flight mass spectrometry was adopted to test in both positive and negative modes. Formula finder function in peakview software was used to calculate the element composition of the compounds

and IDA explore function in the software was invoked to obtain secondary fragmentation ions of this mass number. And the compounds were identified based on literature data and the reference substances.

Result:

On the basis of the mass fragmentation regularity of accurate molecular weight

35 compounds were identified in BHGZT

including 16 steroid saponins

6 triterpenoid saponins

7 flavonoids

and 4 organic acids and 2 others. Among them

10 components (timosaponin AⅢ

timosaponin I

timosaponin BⅢ

timosaponin BⅡ

new mangiferin

mangiferin

liquiritin apioside

liquiritin

glycyrrhizic acid and cinnamic acid) were confirmed by comparing with reference substances

and the sources of the compound were identified.

Conclusion:

UFLC-Triple-TOF-MS/MS can be used to characterize the chemical composition of BHGZT simply and quickly. Relevant researches provide references for the research of pharmacodynamic material basis

the quality control and the explanation of mechanism of action.

关键词

Keywords

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