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液相色谱-质谱联用法同时测定人血浆中人参皂苷Rb(1)和Rg(1)的含量

Simultaneous determination of ginsenoside Rb(1) and Rg(1) in human plasma by liquid chromatography-mass spectrometry.

作者信息

Ji Hye Young, Lee Hye Won, Kim Hae Kyoung, Kim Hui Hyun, Chang Seung Goo, Sohn Dong Hwan, Kim Jaebaek, Lee Hye Suk

机构信息

College of Pharmacy, Wonkwang University, Shinyongdong 344-2, Jeonbuk, Iksan 570749, South Korea.

出版信息

J Pharm Biomed Anal. 2004 Apr 1;35(1):207-12. doi: 10.1016/j.jpba.2003.12.020.

Abstract

A liquid chromatographic-mass spectrometric (LC/MS) method for the simultaneous determination of ginsenoside Rb(1) and Rg(1) in human plasma was developed. The method involved the protein precipitation followed by analysis of ginsenoside Rb(1) and Rg(1) in an Atlantis C(18) column with the gradient elution of acetonitrile and ammonium formate (10mM, pH 3.0) at a flow rate of 0.2 ml/min. The analytes were determined using electrospray negative ionization mass spectrometry in the selected ion monitoring mode. The standard curves for ginsenoside Rb(1) and Rg(1) were linear over the concentration range of 10.0-1000 ng/ml. The lower limit of quantification was 10.0 ng/ml using 100 microl plasma sample. The coefficient of variation of intra- and inter-day assays for ginsenoside Rb(1) and Rg(1) at three quality control levels ranged from 1.0 to 6.8% and 5.4 to 9.8%, respectively. Ginsenoside Rb(1) and Rg(1) were stable in blank human plasma at room temperature for 24h and following three freeze-thaw cycles.

摘要

建立了一种同时测定人血浆中人参皂苷Rb(1)和Rg(1)的液相色谱-质谱(LC/MS)方法。该方法包括蛋白质沉淀,然后在Atlantis C(18)柱上分析人参皂苷Rb(1)和Rg(1),以乙腈和甲酸铵(10mM,pH 3.0)梯度洗脱,流速为0.2 ml/min。采用电喷雾负离子质谱在选择离子监测模式下测定分析物。人参皂苷Rb(1)和Rg(1)的标准曲线在10.0-1000 ng/ml浓度范围内呈线性。使用100微升血浆样品时,定量下限为10.0 ng/ml。人参皂苷Rb(1)和Rg(1)在三个质量控制水平下日内和日间测定的变异系数分别为1.0%至6.8%和5.4%至9.8%。人参皂苷Rb(1)和Rg(1)在空白人血浆中于室温下24小时及经过三个冻融循环后均稳定。

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