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采用液相色谱-电喷雾电离-质谱法同时定量分析连翘中的 14 种生物活性成分。

Simultaneous quantification of 14 bioactive constituents in Forsythia suspensa by liquid chromatography-electrospray ionisation-mass spectrometry.

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang, 050017, People's Republic of China.

出版信息

Phytochem Anal. 2010 May-Jun;21(3):253-60. doi: 10.1002/pca.1194.

Abstract

INTRODUCTION

Forsythia suspensa is a commonly used traditional Chinese medicine including phenylethanoid glycosides, lignans, flavonoids, terpenes and volatile oils. Quantification of multi-components is important for the quality control of Forsythia suspensa.

OBJECTIVE

To establish a liquid chromatography-electrospray ionisation-mass spectrometry method for simultaneous quantification of 14 bioactive constituents of Forsythia suspensa in different places of China and different parts of this herb.

METHODOLOGY

The optimal chromatographic conditions were achieved on a Kromasil C(18) column (150 yen 4.6 mm, 5 microm) with gradient elution of methanol, acetonitrile and 0.1% formic acid in 27 min. Detection was performed in negative ionisation mode by monitoring the precursor-product combination in multiple reaction monitoring (MRM) mode. The validation of the method included tests of linearity, sensitivity, precision, repeatability, stability and accuracy.

RESULTS

All calibration curves showed good linear regression (r > 0.9990) within test ranges. The established method showed good precision and accuracy with overall intra-day and inter-day variations of 0.7-4.3 and 1.1-3.9% respectively, and overall recoveries of 96.65-101.2% for the compounds analysed.

CONCLUSION

The proposed method was successfully applied for the quantitative analysis of 14 constituents in 12 Forsythia suspensa samples.

摘要

简介

连翘是一种常用的中药,包括苯乙醇苷类、木脂素类、黄酮类、萜类和挥发油类。多成分定量分析对于连翘的质量控制非常重要。

目的

建立一种同时测定中国不同产地和不同部位连翘中 14 种生物活性成分的液相色谱-电喷雾离子化-质谱联用方法。

方法

采用 Kromasil C(18)柱(150mm×4.6mm,5μm),在 27min 内,以甲醇、乙腈和 0.1%甲酸为流动相进行梯度洗脱。采用负离子化模式,通过监测多反应监测(MRM)模式下的前体-产物组合进行检测。该方法的验证包括线性、灵敏度、精密度、重复性、稳定性和准确度的测试。

结果

所有校准曲线均呈良好的线性回归(r>0.9990)。该方法具有良好的精密度和准确度,日内和日间总变异分别为 0.7-4.3%和 1.1-3.9%,分析物的总回收率为 96.65-101.2%。

结论

该方法成功应用于 12 个连翘样品中 14 种成分的定量分析。

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