Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS

Xiao-na LI; Xin DONG; Na LI; Nan ZHANG; Jia-bao MAO; Bao-quan BAO; Ping ZHANG

doi:10.13422/j.cnki.syfjx.20200615

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Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS

Pharmacy Fundamentals | 更新时间：2021-02-09

- Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 26, Issue 6, Pages: 121-131(2020)
- 作者机构：
  
  1.内蒙古医科大学　药学院，呼和浩特　 010110
  2.内蒙古医科大学　第一临床医学院，呼和浩特　 010110
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20200615
  CLC： R284.2; R289; R22; R2-031
- Received：12 November 2019，
  
  Published Online：07 December 2019，
  
  Published：20 March 2020
- 稿件说明：
移动端阅览
Xiao-na LI, Xin DONG, Na LI, et al. Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2020, 26(6): 121-131.
DOI：

Xiao-na LI, Xin DONG, Na LI, et al. Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2020, 26(6): 121-131. DOI： 10.13422/j.cnki.syfjx.20200615.

摘要

目的：

运用高效液相色谱串联四极杆-静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS/MS)，快速表征和识别四味土木香散中的成分。

方法：

采用Agilent ZORBAX SB-Aq色谱柱(4.6 mm×150 mm，5 μm)，流动相5 mmol·L

-1

乙酸铵＋0.1%甲酸水溶液-乙腈梯度洗脱。依据ChemSpider和ChemicalBook数据库检索及化学成分分离与结构鉴定等方法，建立组方药材化学成分的分子式、相对分子质量、结构式以及二级质谱信息的本地数据库；建立HPLC-Q-Exactive-MS/MS分析方法，结合Xcalibur 3.0软件、对照品比对及裂解规律研究，对四味土木香散中的化学成分进行快速的结构鉴定。

结果：

利用HPLC-Q-Exactive-MS/MS技术从四味土木香散中共鉴定了110个成分，包括来源于土木香的倍半萜内脂3个，来源于苦参的生物碱16个及异戊二烯黄酮38个，来源于悬钩子木的三萜皂苷12个、儿茶素类1个及黄酮苷类4个，并总结了主要类型化合物的质谱裂解规律，其中31个成分为首次报道质谱信息。

结论：

该研究可系统、准确、快速鉴定四味土木香散中目标化合物及非目标化合物，为该复方的体内分析以及药代动力学研究奠定基础。

Abstract

Objective:

To rapidly characterize and identify the components of Siwei Tumuxiang San by using high performance liquid chromatography tandem quadrupole-electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q-Exactive-MS/MS).

Method:

Agilent ZORBAX SB-Aq column (4.6 mm×150 mm

5 μm) was adopted and 5 mmol·L

-1

ammonium acetate+ 0.1% formic acid aqueous solution-acetonitrile were used as mobile phase. According to the separation and structure identification results of chemical components based on the methods of ChemSpider and ChemicalBook database retrieval

a local database of molecular formula

molecular weight

structural formula and MS/MS spectrum information of chemical components in Siwei Tumuxiang San was established. An HPLC-Q-Exactive-MS/MS analysis method was established. The complex compounds of Siwei Tumuxiang San were identified rapidly by using Xcalibar 3.0 software

comparison of reference materials and studies on MS/MS fragment pathways.

Result:

A total of 110 compounds were identified from the Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS technology

including 3 sesquiterpene compounds from Inulae Radix

16 alkaloid compunds and 38 isoprene flavonoid compounds from Sophorae Radix flavescentis

12 triterpenoid saponin compounds

1 catechin compounds and 4 flavonoid glycoside compounds from

Rubus sachalinensis

. The fragment pathways of the main types of compounds were summarized. Among them

mass spectrometry information of 31 compounds was reported for the first time.

Conclusion:

This study can be used to identify the target compounds and non-target compounds in Siwei Tumuxiang San systematically

accurately and quickly

which will lay a foundation for the

in vivo

analysis and pharmacokinetic study of the formulation.

关键词

Keywords

references

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