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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Rapid and simple method for determination of cephradine in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS): Application to the bioequivalence study
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Rapid and simple method for determination of cephradine in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS): Application to the bioequivalence study

机译:液相色谱-串联质谱法(LC-MS / MS)快速简便地测定人血浆中头孢拉定的方法:在生物等效性研究中的应用

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A rapid and simple procedure was developed for the determination of cephradine in human plasma using liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). After trichloroacetic acid (TCA) precipitation of proteins from plasma samples, cephradine and cefaclor (the internal standard: IS) were eluted on a CN column. The isocratic mobile phase used consisted of acetonitrile-water-formic acid (25:75:0.1, v/v/v). Cephradine and the IS were both detected in multiple reaction monitoring (MRM) mode at the transitions: m/z 350.0 -> 90.8 for cephradine and m/z 368.1 -> 106.0 for the IS, respectively. The calibration curve was linear over the concentration range from 0.05 to 50 mu g/ml, and correlation coefficients were greater than 0.996. The coefficient of variation of assay precision was less than 9.36%, and its accuracy ranged from 87.92% to 111.16%. The chromatographic run time for each plasma sample was less than 3 min. The developed method was successfully applied to a bioequivalence study of cephradine in healthy male volunteers. (C) 2009 Elsevier B.V. All rights reserved.
机译:建立了一种快速,简单的程序,通过液相色谱与电喷雾电离串联质谱法(LC-ESI-MS / MS)一起测定人血浆中的头孢拉定。三氯乙酸(TCA)从血浆样品中沉淀出蛋白质后,头孢拉定和头孢克洛(内标:IS)在CN柱上洗脱。使用的等度流动相由乙腈-水-甲酸(25:75:0.1,v / v / v)组成。头孢拉定和IS都在多反应监测(MRM)模式下在以下转换中检测到:头孢拉定的m / z 350.0-> 90.8和IS的m / z 368.1-> 106.0。校准曲线在0.05至50μg / ml的浓度范围内呈线性,相关系数大于0.996。测定精度的变异系数小于9.36%,准确度范围为87.92%〜111.16%。每个血浆样品的色谱运行时间少于3分钟。所开发的方法已成功地应用于健康男性志愿者中头孢拉定的生物等效性研究。 (C)2009 Elsevier B.V.保留所有权利。

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