Qualitatively Analysis of Gypenosides with UPLC-ESI-Orbitrap-MS

HE Yu-qi; LU Yan-liu; QIU Min; WANG Min; WANG Wei; YANG Li; WANG Zheng-tao

doi:10.13422/j.cnki.syfjx.2017190077

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Qualitatively Analysis of Gypenosides with UPLC-ESI-Orbitrap-MS

更新时间：2024-01-04

- Qualitatively Analysis of Gypenosides with UPLC-ESI-Orbitrap-MS
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 23, Issue 19, Pages: 77-81(2017)
- 作者机构：
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- DOI：10.13422/j.cnki.syfjx.2017190077
  CLC： O657.63;R284.1
- Published：2017
- 稿件说明：
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HE Yu-qi, LU Yan-liu, QIU Min, et al. Qualitatively Analysis of Gypenosides with UPLC-ESI-Orbitrap-MS[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(19): 77-81.
DOI：

HE Yu-qi, LU Yan-liu, QIU Min, et al. Qualitatively Analysis of Gypenosides with UPLC-ESI-Orbitrap-MS[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(19): 77-81. DOI： 10.13422/j.cnki.syfjx.2017190077.

摘要

目的：通过UPLC-ESI-Orbitrap-MS技术对绞股蓝总皂苷提取物的主要化学成分进行分析。方法：采用Thermo Q Exactive四极杆-静电场轨道阱高分辨质谱-色谱联用系统分析，以Hypersil Gold C18色谱柱（2.1 mm×150 mm，1.9 μm）为固定相，流动相0.1%甲酸水溶液（A）-乙腈（B）梯度洗脱（0~2 min，5% B；2~15 min，5%~95% B；15~17 min，95% B），流速0.3 mL ·min-1，柱温40℃；质谱条件采用电喷雾离子化（ESI）方式，在负离子模式下，以Full Scan/Targeted-ddMS2扫描模式检测，研究绞股蓝总皂苷提取物的主要皂苷类化学成分。结果：通过与对照品比对、结合参考文献，分析多级质谱数据，根据化学成分的质谱碎片，推测色谱峰对应的化学结构，共归属8种具有原人参二醇型母核结构的绞股蓝皂苷，分别是绞股蓝皂苷Ⅲ，Ⅳ，Ⅷ，Ⅻ，Rg3，Rb2，Rc，Rf。结论：该研究采用的方法简单、快速、灵敏，对绞股蓝总皂苷提取物中具有原人参二醇型母核结构的主要皂苷类进行了高分辨质谱分析，这一方法可以从定性分析的角度，对市售绞股蓝总皂苷提取物的质量进行初步快速鉴别。

Abstract

Objective: To analyze the main chemical components ingypenosidesextracts with UPLC-ESI-Orbitrap-MS technology. Method: Thermo Q Exactivequadrupolerod-electrostatic field orbitrap high resolution mass spectrometry-MS system was used and the chromatography separation was performed on Hypersil Gold C18 column (2.1 mm×150 mm

1.9 μm) with 0.1% formic acid solution (A)-acetonitrile (B) as the mobile phase for gradient elution (0-2 min

5%B; 2-15 min

5%-95%B; 15-17 min

95%B). The flow rate was set at 0.3 mL·min-1 and the column temperature was 40℃.Electrospray ionization (ESI) source was applied and operated in Full Scan/Targeted-dd MS2/negative ion mode. Result: Eight gypenosides were identified based on the reference compounds

high resolution mass number and comparison between experimental data and published data. These compounds included gypenoside Ⅲ

Ⅳ

Ⅷ

Ⅻ

Rg3

Rb2

and Rf. Conclusion: The established method would be used to qualitatively and rapidly compare the quality of extract from Gynostemma pentaphyllum on sale.

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