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采用液相色谱-电喷雾电离质谱法测定人血浆中甘草次酸的含量。

Determination of glycyrrhetic acid in human plasma by LC-ESI-MS.

作者信息

Ding Li, Huang Xin, Yang Jin, Bian Xiaojie, Zhang Zhengxing, Liu Guangyu

机构信息

Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.

出版信息

J Pharm Biomed Anal. 2006 Feb 24;40(3):758-62. doi: 10.1016/j.jpba.2005.10.047. Epub 2005 Dec 7.

Abstract

A sensitive liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for determination of glycyrrhetic acid, the active metabolite of glycyrrhizin, in human plasma using ursolic acid as the internal standard (IS) was established. Plasma was extracted with ethyl acetate and separated on a C18 column with a mobile phase of 10 mmol/l ammonium acetate-acetonitrile (10:90). Glycyrrhetic acid was determined using electrospray ionization in a single quadrupole mass spectrometer. HPLC-ESI-MS was performed in the selected ion monitoring (SIM) mode using target ions at m/z 469.5 for glycyrrhetic acid and m/z 455.5 for IS. Calibration curve was linear over the range of 0.1-400 ng/ml. The limit of quantitation for glycyrrhetic acid in plasma was 0.1 ng/ml. The mean plasma extraction recovery of glycyrrhetic acid was 94.51 +/- 3.82%. The method has been successfully applied to study the pharmacokinetics of glycyrrhetic acid in healthy male Chinese volunteers. The assay was proved to be sensitive, accurate and convenient.

摘要

建立了一种灵敏的液相色谱 - 电喷雾电离 - 质谱(LC - ESI - MS)法,以熊果酸为内标(IS)测定人血浆中甘草酸(甘草甜素的活性代谢产物)。血浆用乙酸乙酯萃取,在C18柱上分离,流动相为10 mmol/l乙酸铵 - 乙腈(10:90)。甘草酸在单四极杆质谱仪中用电喷雾电离法测定。HPLC - ESI - MS在选择离子监测(SIM)模式下进行,甘草酸的目标离子为m/z 469.5,内标的目标离子为m/z 455.5。校准曲线在0.1 - 400 ng/ml范围内呈线性。血浆中甘草酸的定量限为0.1 ng/ml。甘草酸的平均血浆萃取回收率为94.51±3.82%。该方法已成功应用于研究健康中国男性志愿者体内甘草酸的药代动力学。该测定方法灵敏、准确且方便。

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