Qualitative Analysis on Perilla frutescens Leaves and Stalks by UPLC-Q-Exactive-Orbitrap-MS

Qian-li KANG; Zhuang-zhuang LI; Shan-shan FAN; Rong RONG; Hai-qiang JIANG; Xiao-lin JIANG; Ji-qiu ZHANG; Li-li GONG

doi:10.13422/j.cnki.syfjx.20201512

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Qualitative Analysis on Perilla frutescens Leaves and Stalks by UPLC-Q-Exactive-Orbitrap-MS

Pharmacy Fundamentals | 更新时间：2020-08-11

- Qualitative Analysis on Perilla frutescens Leaves and Stalks by UPLC-Q-Exactive-Orbitrap-MS
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 26, Issue 13, Pages: 156-162(2020)
- 作者机构：
  
  山东中医药大学药学院，实验中心，济南 250355
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20201512
  CLC： R284.2;R289;R22;R2-031
- Published Online：14 April 2020，
  
  Published：05 July 2020
- 稿件说明：
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亢倩丽,李壮壮,范珊珊等.基于UPLC-Q-Exactive-Orbitrap-MS的紫苏叶与紫苏梗化学成分分析[J].中国实验方剂学杂志,2020,26(13):156-162.

KANG Qian-li,LI Zhuang-zhuang,FAN Shan-shan,et al.Qualitative Analysis on Perilla frutescens Leaves and Stalks by UPLC-Q-Exactive-Orbitrap-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(13):156-162.
亢倩丽,李壮壮,范珊珊等.基于UPLC-Q-Exactive-Orbitrap-MS的紫苏叶与紫苏梗化学成分分析[J].中国实验方剂学杂志,2020,26(13):156-162. DOI： 10.13422/j.cnki.syfjx.20201512.

KANG Qian-li,LI Zhuang-zhuang,FAN Shan-shan,et al.Qualitative Analysis on Perilla frutescens Leaves and Stalks by UPLC-Q-Exactive-Orbitrap-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(13):156-162. DOI： 10.13422/j.cnki.syfjx.20201512.

摘要

目的

建立液相色谱-质谱联用技术（LC-MS）对紫苏叶与紫苏梗成分定性分析的方法，探讨紫苏叶与紫苏梗药效差异的物质基础。

方法

80%甲醇超声提取紫苏叶与紫苏梗药材，利用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱（UPLC-Q-Exactive-Orbitrap-MS）技术对样品进行定性分析，采用Halo-C

色谱柱（2.1 mm×100 mm，2.7 μm），流动相0.05%甲酸水溶液-0.05%甲酸乙腈，梯度洗脱，流速0.3 mL·min

-1

，柱温40 ℃，进样量5 μL，采用正、负离子2种监测模式。

结果

根据对照品的保留时间，Xcalibur软件的精确相对分子质量、准分子离子峰、碎片离子，相关文献和Mass Frontier 7.0软件对紫苏中的化学成分进行识别和鉴定。共鉴定出4种氨基酸类，7种苯丙素类，10种黄酮类，12种三萜类，7种有机酸类，4种脂肪酸类成分，10个未知成分，其中算盘子酮等6种三萜酸首次在紫苏中鉴定出，共54种化合物，对其中5种不同特征的化合物进行了结构解析。紫苏叶中有45种成分，紫苏梗中有32种成分，二者有23种共有成分。

结论

LC-MS技术能够快速有效地对紫苏进行成分鉴定，该研究为紫苏不同部位的质量控制、开发利用提供重要的实验理论依据。

Abstract

Objective

To establish a method for qualitative analysis of components in

Perilla frutescens

leaves and stalks by liquid chromatography-mass spectrometry (LC-MS)，so as to explore the substance basis of pharmacodynamics differences between

P.frutescens

leaves and stalks.

Method

P. frutescens

leaves and stalks were extracted by 80% methanol-water ultrasound. The samples were analyzed by UPLC-Q-Exactive-Orbitrap-MS comprehensively. Halo-C

column (2.1 mm×100 mm，2.7 μm) was used for gradient elution with 0.05% formic acid aqueous-0.05% acetonitrile formate as mobile phase in positive and negative ion modes. The flow rate was 0.3 mL·min

-1

，the column temperature was 40 ℃，and the injection volume was 5 μL.

Result

The chemical compound in

P. frutescens

was deduced and identified based on the retention time of chromatography，and the exact molecular weight，excimer ion peaks，fragment ions and reference materials in Xcalibur software. The chemical composition of

P. frutescens

was identified by Mass Frontier 7.0 software. Totally 4 amino acids，7 phenylpropanoids，10 flavonoids，12 triterpenoids，7 organic acids，4 fatty acids，10 unknown compounds and 54 compounds were identified. Among them，6 triterpene acids

including glochidone

were identified in

P. frutescens

for the first time. The structures of five characteristic compounds were analyzed. There were 45 constituents in

P.frutescens

leaves and 32 constituents in

P. frutescens

stalks. They had 23 common constituents.

Conclusion

LC-MS can identify the components of

P. frutescens

rapidly and effectively. This study provides an important theoretical basis for the quality control of different parts of

P. frutescens

and the development and utilization of

P. frutescens

关键词

Keywords

references

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