Simultaneous Quantification of 14 Bioactive Constituents in Forsythia Suspensa by Liquid Chromatography-Electrospray Ionisation-Mass Spectrometry
Simultaneous Quantification of 14 Bioactive Constituents in Forsythia Suspensa by Liquid Chromatography-Electrospray Ionisation-Mass Spectrometry
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DOI：
10.1002/pca.1194
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发表时间：
2010-05-01
影响因子：
3.3
通讯作者：
Zhang, Lantong
中科院分区：
文献类型：
--
作者：
Cui, Yang;Wang, Qiao;Zhang, Lantong
连翘是一种常用的中药，含有苯乙醇苷、木脂素、类黄酮、萜烯和挥发油。多组分定量分析对连翘药材质量控制具有重要意义。目的建立液相色谱-电喷雾-质谱联用法同时定量测定连翘不同产地、不同部位14种生物活性成分的方法。方法：采用Kromasil C-18色谱柱（150 × 4.6 mm, 5 μ m），甲醇、乙腈和0.1%甲酸梯度洗脱27 min，获得最佳色谱条件。通过多反应监测（MRM）模式监测前体-产物组合，在负电离模式下进行检测。方法的验证包括线性度、灵敏度、精密度、重复性、稳定性和准确度等试验。结果-所有校准曲线在测试范围内具有良好的线性回归（r为0.9990）。所建立的方法精密度和准确度较好，日内和日间总变化率分别为0.7 ~ 4.3和1.1 ~ 3.9%，总加样回收率为96.65 ~ 101.2%。结论-该方法可用于12份连翘样品中14种成分的定量分析。版权所有John Wiley & Sons， Ltd。
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 x 4.6 mm, 5 mu m) 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. Copyright (C) 2010 John Wiley & Sons, Ltd.