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采用高效液相色谱-电喷雾串联质谱法快速测定筋骨草中 20 种成分

Rapid method for simultaneous determination of 20 components in Isodon nervosa by high-performance liquid chromatography-electrospray ionisation tandem mass spectrometry.

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang 050017, China.

出版信息

Phytochem Anal. 2010 Sep-Oct;21(5):416-27. doi: 10.1002/pca.1212.

Abstract

INTRODUCTION

Isodon nervosa is a commonly used traditional Chinese medicine including diterpenoids, phenolic acids, triterpenoids and volatile oil. Qualitative and quantitative analysis of multi-components is important for its quality control.

OBJECTIVE

To establish a liquid chromatography-electrospray ionisation-mass spectrometry method for simultaneous analysis of 20 bioactive constituents of Isodon nervosa in different places of China and different parts of this herb.

METHODOLOGY

The optimal chromatographic conditions were achieved on a C(18) column (250 × 4.6 mm, 5 µm) with with linear gradient elution with 0.1% aqueous formic acid : methanol containing 0.1% formic acid at a flow-rate of 0.7 mL/min in 15 min. The identification and quantification of those analytes were achieved on a hybrid quadrupole linear ion trap mass spectrometer. Multiple-reaction monitoring scanning was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. Full validation of the method was carried out (linearity, precision, accuracy, limit of detection and limit of quantification).

RESULTS

The results indicated that the method was simple, rapid, specific and reliable. The proposed method was successfully applied for the qualitative and quantitative analysis of 20 chemical compositions in Isodon nervosa samples.

CONCLUSION

Twenty chemical compositions in 21 batches of wild and cultivated Isodon nervosa samples from different sources had great variation in the contents.

摘要

简介

冬凌草是一种常用的中药,包含二萜类、酚酸类、三萜类和挥发油。对其多成分进行定性和定量分析对其质量控制非常重要。

目的

建立一种液相色谱-电喷雾离子化-质谱联用同时分析中国不同产地和不同部位冬凌草中 20 种生物活性成分的方法。

方法

采用 C(18)柱(250×4.6mm,5μm),以 0.1%甲酸水溶液-甲醇(含 0.1%甲酸)为流动相,在 15min 内采用线性梯度洗脱,流速为 0.7mL/min,优化了色谱条件。采用混合四极杆线性离子阱质谱仪,在单次运行中切换电喷雾离子源的正、负模式进行多反应监测扫描,实现了对这些分析物的鉴定和定量。对该方法进行了全面验证(线性、精密度、准确度、检测限和定量限)。

结果

该方法简单、快速、特异、可靠。该方法成功应用于 21 批不同来源的野生和栽培冬凌草样品中 20 种化学成分的定性和定量分析。

结论

21 批来自不同来源的野生和栽培冬凌草样品中的 20 种化学成分含量差异较大。

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