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[液相色谱-电喷雾质谱法定量测定银杏内酯]

[Quantitative determination of ginkgolides by liquid chromatography-electrospray mass spectrometry].

作者信息

Zhou Xin, Zhang Xue-Qin, Yuan Mu, Wang Dao-Ping

机构信息

The Key laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guiyang 550002, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2005 Dec;30(24):1915-8.

PMID:16494022
Abstract

OBJECTIVE

This paper reports a method based on liquid chromatography coupled with electrospray mass spectrometry for the analysis of terpenoids in ginkgo laminae.

METHOD

The analysis was performed on ZORBAX RX-C18 (2.1 mm x 150 mm) column with methanol-water(with gradient) as mobile phase at a flow rate of 0.25 mL x min(-1), and column temperature of 25 degrees C. Analyses were carried out in the selected ion monitoring (SIM) mode.

RESULT

Ginkgolides (GA, GB and GC) and bilobalide were quantitatively detected by external standardization with linear in the range of 4.04-1.012 x 10(2) ng, with coefficient and relative standard deviations being 0.993 7-0.999 8 and 2.50%-4.73%. LC-ESI-MS shows a greatly increased sensitivity compared with other methods. The detection limit of this method by SIM was 1.47 x 10(-3)-0.320 microg x mL(-1).

CONCLUSION

This method is specific, reproducible, rapidly and permits quantitative analyses of ginkgolides and bilobalide in different samples with simple pre-purification steps.

摘要

目的

本文报道一种基于液相色谱-电喷雾质谱联用的银杏叶片中萜类化合物分析方法。

方法

采用ZORBAX RX-C18(2.1 mm×150 mm)色谱柱,以甲醇-水(梯度洗脱)为流动相,流速为0.25 mL·min⁻¹,柱温25℃。分析在选择离子监测(SIM)模式下进行。

结果

通过外标法对银杏内酯(GA、GB和GC)及白果内酯进行定量检测,线性范围为4.04 - 1.012×10² ng,系数和相对标准偏差分别为0.993 7 - 0.999 8和2.50% - 4.73%。与其他方法相比,液相色谱-电喷雾质谱联用显示出更高的灵敏度。该方法在SIM模式下的检测限为1.47×10⁻³ - 0.320 μg·mL⁻¹。

结论

该方法特异性强、可重复、快速,且经过简单的预纯化步骤即可对不同样品中的银杏内酯和白果内酯进行定量分析。

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