首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Selective method for the determination of cefdinir in human plasma using liquid chromatography electrospray ionization tandam mass spectrometry
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Selective method for the determination of cefdinir in human plasma using liquid chromatography electrospray ionization tandam mass spectrometry

机译:液相色谱电喷雾电离tandam质谱法测定人血浆中头孢地尼的选择方法

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A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed for the determination of cefdinir in human plasma. After a simple protein precipitation using trichloracetic acid, the post-treatment samples were applied to a prepacked RP18 Waters SymmetryShield column interfaced with a triple quadrupole tandem mass spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of methanol-water-formic acid (25:75:0.075, v/v/v). The analyte and I.S. cefaclor were both detected by the use of selected reaction monitoring mode. The method was linear in the concentration range of 5-2000 ng/ml. The lower limit of quantification was 5 ng/ml. The intra- and inter-day relative standard deviation across three validation runs over the entire concentration range was less than 4.3%. The accuracy determined at three concentrations (36, 360 and 1800 ng/ml for cefdinir) ranged from 99.6 to 106.7% in terms of recovery. The chromatographic run time for each plasma sample was less than 3 min. The method herein described was successfully applied for the evaluation of pharmacokinetic profiles of cefdinir capsule in 12 healthy volunteers. (c) 2006 Elsevier B.V. All rights reserved.
机译:建立了灵敏且选择性的液相色谱-串联质谱法(LC-MS / MS),用于测定人血浆中的头孢地尼。使用三氯乙酸对蛋白质进行简单沉淀后,将后处理样品应用于与三重四极串联质谱仪连接的预装RP18 Waters SymmetryShield色谱柱。正电喷雾电离用作电离源。流动相由甲醇-水-甲酸(25:75:0.075,v / v / v)组成。分析物和I.S.头孢克洛均通过选择的反应监测模式进行检测。该方法在5-2000 ng / ml的浓度范围内是线性的。定量下限为5 ng / ml。在整个浓度范围内进行的三次验证运行的日内和日间相对标准偏差均小于4.3%。在三种浓度下(头孢地尼的浓度分别为36、360和1800 ng / ml)测定的回收率在99.6%至106.7%之间。每个血浆样品的色谱运行时间少于3分钟。本文描述的方法已成功地用于评估12名健康志愿者中头孢地尼胶囊的药代动力学概况。 (c)2006 Elsevier B.V.保留所有权利。

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