Simultaneous Determination of 12 Components in Pudilan Xiaoyan Oral Liquid by Ultra-high Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

Wen-ya GAO; Xin-ru GU; Li-juan ZHAO; Yan-yan ZHOU; Bao-lin BIAN; Hai-yu ZHAO

doi:10.13422/j.cnki.syfjx.20191415

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Simultaneous Determination of 12 Components in Pudilan Xiaoyan Oral Liquid by Ultra-high Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

Resource and Quality Evaluation | 更新时间：2021-02-09

- Simultaneous Determination of 12 Components in Pudilan Xiaoyan Oral Liquid by Ultra-high Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 25, Issue 18, Pages: 150-154(2019)
- 作者机构：
  
  中国中医科学院　中药研究所，北京　 100700
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20191415
  CLC： R284.1; R289; R22; R2-031
- Published：20 September 2019，
  
  Published Online：04 April 2019，
  
  Received：16 December 2018，
- 稿件说明：
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Wen-ya GAO, Xin-ru GU, Li-juan ZHAO, et al. Simultaneous Determination of 12 Components in Pudilan Xiaoyan Oral Liquid by Ultra-high Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry. [J]. Chinese Journal of Experimental Traditional Medical Formulae 25(18):150-154(2019)
DOI：

Wen-ya GAO, Xin-ru GU, Li-juan ZHAO, et al. Simultaneous Determination of 12 Components in Pudilan Xiaoyan Oral Liquid by Ultra-high Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry. [J]. Chinese Journal of Experimental Traditional Medical Formulae 25(18):150-154(2019) DOI： 10.13422/j.cnki.syfjx.20191415.

摘要

目的：

建立超高效液相色谱串联三重四级杆质谱法同时测定蒲地蓝消炎口服液中汉黄芩苷、黄芩苷、汉黄芩素、白杨素、木犀草素、咖啡酸、乙酰紫堇灵、紫堇灵、原阿片碱、水杨酸、尿嘧啶、腺苷的含量测定方法。

方法：

采用Agilent Extend C

色谱柱(3.0 mm×150 mm，3.5 μm)；流动相甲醇-水(0.1%甲酸)，梯度洗脱；流速0.3 mL·min

－1

。采用三重四极杆质谱检测器，电喷雾离子化源(ESI)，动态多反应监测(DMRM)模式，正、负离子交替模式检测。

结果：

12种对照品峰型良好具有良好专属性，汉黄芩苷、黄芩苷、汉黄芩素、白杨素、木犀草素、咖啡酸、乙酰紫堇灵、紫堇灵、原阿片碱、水杨酸、尿嘧啶、腺苷分别在0.062 24～16.24，33.95～530.4，0.013 64～3.558，0.001 157～0.302 4，0.001 199～0.313 0，0.014 64～3.821，0.000 739 5～0.038 59，0.060 83～3.174，0.002 443～0.637 4，0.021 80～1.138，0.022 99～6.000，0.006 046～1.578 μg·L

－1

线性关系良好，精密度、稳定性、重复性良好。汉黄芩苷、黄芩苷、汉黄芩素、白杨素、木犀草素、咖啡酸、乙酰紫堇灵、紫堇灵、原阿片碱、水杨酸、尿嘧啶、腺苷平均加样回收率分别为98.9%，100.2%，106.9%，100.8%，101.7%，99.3%，94.6%，100.0%，100.5%，103.4%，96.8%，98.1%。

结论：

该方法样品处理简便，专属性强，灵敏度高，检测结果可靠，为蒲地蓝消炎口服液的质量提升奠定了基础。

Abstract

Objective:

To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ MS) method for the simultaneous determination of twelve components (wogonoside

baicalin

wogonin

chrysin

uteolin

caffeic acid

acetylcorynoline

corynoline

protopine

salicylic acid

uracil and adenosine) in Pudilan Xiaoyan oral liquid.

Method:

The analysis was performed on an Agilent Extend C

column(3.0 mm×150 mm

3.5 μm)

with a gradient elution by using the mobile phase of methanol-water(0.1%formic acid). The flow rate was 0.3 mL·min

-1

. Triple quadrupole mass spectrometry

electrospray ionization source (ESI)

DMRM mode

and positive and negative ions alternate mode were adopted.

Result:

The 12 reference substances had a good specificity. Wogonoside

baicalin

wogonin

chrysin

uteolin

caffeic acid

acetylcorynoline

corynoline

protopine

salicylic acid

uracil and adenosine showed good linear relationships within the range of 0.062 24-16.24

33.95-530.4

0.013 64-3.558

0.001 157-0.302 4

0.001 199-0.313 0

0.014 64-3.821

0.000 739 5-0.038 59

0.060 83-3.174

0.002 443-0.637 4

0.021 80-1.138

0.022 99-6.000

0.006 046-1.578 μg·L

-1

with a good precision

stability and repeatability. And the average recoveries were 98.9%

100.2%

106.9%

100.8%

101.7%

99.3%

94.6%

100.0%

100.5%

103.4%

96.8%

98.1%.

Conclusion:

This method was simple

sensitive and reliable. It laid a foundation to promote the quality control standard of Pudilan Xiaoyan oral liquid.

关键词

蒲地蓝消炎口服液超高液相色谱串联三重四级杆质谱质量控制

Keywords

Pudilan Xiaoyan oral liquidUHPLC-QqQ-MSquality control

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