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液相色谱-串联质谱法测定大鼠血浆中蒙花苷的含量。

Liquid chromatography-tandem mass spectrometry for the determination of jaceosidin in rat plasma.

作者信息

Song Won Young, Kim Nam Jin, Kim Sung Yeon, Lee Hye Suk

机构信息

Drug Metabolism & Bioanalysis Laboratory, Wonkwang University, Iksan 570-749, Republic of Korea.

出版信息

J Pharm Biomed Anal. 2009 Feb 20;49(2):381-6. doi: 10.1016/j.jpba.2008.10.021. Epub 2008 Oct 28.

DOI:10.1016/j.jpba.2008.10.021
PMID:19070985
Abstract

Jaceosidin (4',5,7-trihydroxy-3',6-dimethoxyflavone), isolated from Artemisia species as well as Eupatorium species, has antiallergic, anticancer, anti-inflammatory and antioxidant activity. A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the quantification of jaceosidin in rat plasma was developed to characterize the pharmacokinetics of jaceosidin. Jaceosidin and the internal standard, linezolid, were extracted from rat plasma with ethyl acetate at acidic pH and analyzed on a Luna phenyl-hexyl column using the mixture of acetonitrile and 0.1% formic acid (45:55, v/v) as a mobile phase. The analytes were determined using an electrospray ionization tandem mass spectrometry in the multiple-reaction-monitoring mode. The calibration curve was linear (r(2)=0.9973) over the concentration range of 2.00-500ng/ml. The lower limit of quantification for jaceosidin was 2.0ng/ml using 50 microl of plasma sample. The coefficients of variation of intra- and inter-assay at four QC levels were 2.4-9.6% and the relative errors were -9.1 to 10.0%. The matrix effects for jaceosidin and linezolid were practically absent. The recoveries of jaceosidin and linezolid were 87.0 and 87.7%, respectively. This method was successfully applied to the pharmacokinetic study of jaceosidin in rats.

摘要

从蒿属植物以及泽兰属植物中分离得到的香叶木素(4',5,7 - 三羟基 - 3',6 - 二甲氧基黄酮)具有抗过敏、抗癌、抗炎和抗氧化活性。为了表征香叶木素的药代动力学特征,开发了一种快速、灵敏且选择性的液相色谱 - 串联质谱(LC/MS/MS)方法用于定量大鼠血浆中的香叶木素。香叶木素和内标利奈唑胺在酸性pH条件下用乙酸乙酯从大鼠血浆中提取,并在Luna苯基 - 己基柱上进行分析,以乙腈和0.1%甲酸(45:55,v/v)的混合物作为流动相。使用电喷雾电离串联质谱在多反应监测模式下测定分析物。校准曲线在2.00 - 500ng/ml的浓度范围内呈线性(r(2)=0.9973)。使用50微升血浆样品时,香叶木素的定量下限为2.0ng/ml。四个质量控制水平下的批内和批间变异系数分别为2.4 - 9.6%,相对误差为 - 9.1至10.0%。香叶木素和利奈唑胺几乎不存在基质效应。香叶木素和利奈唑胺的回收率分别为87.0%和87.7%。该方法成功应用于大鼠体内香叶木素的药代动力学研究。

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