Application of Mass Spectrometry in Rapid Analysis of Constituents in

WANG Yi-chen; WANG Huan-jun; ZHANG Ling; ZHOU Hong-lei; MA Yan-ni

doi:10.13422/j.cnki.syfjx.20181710

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Application of Mass Spectrometry in Rapid Analysis of Constituents in

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- Application of Mass Spectrometry in Rapid Analysis of Constituents in
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 24, Issue 17, Pages: 80-87(2018)
- 作者机构：
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20181710
  CLC： R284.1
- Published：2018
- 稿件说明：
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WANG Yi-chen, WANG Huan-jun, ZHANG Ling, et al. Application of Mass Spectrometry in Rapid Analysis of Constituents in [J]. Chinese journal of experimental traditional medical formulae, 2018, 24(17): 80-87.
DOI：

WANG Yi-chen, WANG Huan-jun, ZHANG Ling, et al. Application of Mass Spectrometry in Rapid Analysis of Constituents in [J]. Chinese journal of experimental traditional medical formulae, 2018, 24(17): 80-87. DOI： 10.13422/j.cnki.syfjx.20181710.

摘要

目的：建立大狼把草化学成分的液质联用定性表征方法并总结裂解规律。方法：按照化学成分数据库构建-液质数据采集-数据库检索-质谱数据解析的步骤，采用HALO C18色谱柱（2.1 mm×150 mm，2.7 μm）；0.1%甲酸水溶液（A）-乙腈（B）为流动相，梯度洗脱（0~10 min，5%~25% B；10~30 min，25%~45% B；30~35 min，45%~70% B；35~45 min，70%~90% B；45~60 min，90%~100% B；60~70 min，100% B）。柱温25℃，流速0.2 mL·min-1，进样量5 μL；质谱条件为采用ESI离子源，在正离子模式下进行检测，对大狼把草中的橙酮、查尔酮、苯丙素等进行分析。结果：从大狼把草的提取液中，鉴定出黄酮类22个，苯丙素类5个，有机酸2个，碳烯1个，发现在正离子模式下，绿原酸及其衍生物会有规律的断裂产生[奎尼酸+H-H2O]+，[咖啡酰基+H]+，多羟基酸会脱水裂解。黄酮类化合物，主要会丢失CO，H2O等碎片，橙酮类化合物会产生286，270，230等碎片离子。结论：采用高效液相-飞行时间液质联用法可以快速有效的对中药中已知化学成分进行定性分析，为大狼把草的物质基础表征提供质谱依据。

Abstract

Objective:To establish a characterization method of chemical composition from Bidens frondosa by HPLC-TOF-MS. Method:In accordance with the procedure of construction of chemical composition database-MS data acquisition-database retrieval-mass spectrometry data analysis

the separation was performed on a HALO column

with C18(2.1 mm×150 mm

2.7 μm) as stationary phase. And the mobile phase was water and 0.1% formic acid(A)-acetonitrile(B) for gradient elution. The method of gradient elution:0-10 min

5%-25%B;10-30 min

25%-45%B;30-35 min

45%-70%B;35-45 min

70%-90%B;45-60 min

90%-100%B;60-70 min

100%B. The temperature of column was 25℃

the flow rate was 0.2 mL·min-1

and the injection volume was 5 μL. The composition of B. frondosa was analyzed under positive ion mode. Result:The 24 flavonoid constituents

5 phenylpropanoids

2 organic acids were identified in extraction of B. frondosa. In positive ion mode

chlorogenic acid and its derivatives were ruptured regularly

and produced[quinic acid+H-H2O]+

[caffeoyl+H]+

polyhydroxy acids were dehydrocracked. Flavonoids lost CO

H2O and other fragment ion

and aurones produced the ions of 286

270

230. Conclusion:HPLC-TOF-MS method could be used for fast qualitative analysis of the chemical components in traditional Chinese medicine

and provide the material basis for the characterization of B. frondosa based on mass spectrometry.

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