Development of a rapid and sensitive LC-MS/MS assay for the determination of sorafenib in human plasma
Development of a rapid and sensitive LC-MS/MS assay for the determination of sorafenib in human plasma
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DOI：
10.1016/j.jpba.2007.10.027
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发表时间：
2008-01-22
影响因子：
3.4
通讯作者：
Figg, William D.
中科院分区：
文献类型：
--
作者：
Jain, Lokesh;Gardner, Erin R.;Figg, William D.
建立了测定人血浆中索拉非尼浓度的高效液相色谱-串联质谱仪(LC/MS/MS)方法。样品前处理包括简单的蛋白质沉淀，在50亩L血浆样品体积中加入含有内标([H-2(3)，N-15]索拉非尼)的乙腈0.5mL。色谱柱为Waters SymmetryShield RP8(2.1 mm×50 mm，3.5µm)，流动相为乙腈/0.1%甲酸：65/35(v/v)，流速为0.25 m L/min，柱温为室温。通过监测m/z 464.9->；252.0(索拉非尼)和m/z 469.0->；259.0(内标)的离子跃迁，在正离子多反应监测模式下使用电喷雾电离进行检测。浓度在5~2000 ng/mL范围内线性关系良好。对三组不同的质控样品在6个不同的天进行五次分析，其准确度和精密度分别为92.86%~99.88%和1.19%~4.53%。(C)-2007爱思唯尔B.V.保留所有权利。
A rapid and sensitive liquid chromatography/tandem mass spectrometric (LC/MS/MS) assay was developed for the quantitative determination of sorafenib in human plasma. Sample pretreatment involved simple protein precipitation by the addition of 0.5 mL acetonitrile, containing internal standard ([H-2(3), N-15] sorafenib), to 50 mu L of plasma sample volume. Separation was achieved on a Waters SymmetryShield RP8 (2.1 mm x 50 mm, 3.5 mu m) column at room temperature using an isocratic elution method with acetonitrile/0.1% formic acid in water: 65/35 (v/v) at a flow rate of 0.25 mL/min. Detection was per-formed using electrospray ionization in positive ion multiple reaction monitoring (MRM) mode by monitoring the ion transitions from m/z 464.9 --> 252.0 (sorafenib) and m/z 469.0 --> 259.0 (internal standard). Calibration curves were linear in the concentration range of 5-2000 ng/mL. The accuracy and precision values, calculated from three different sets of quality control samples analyzed in quintuplicate on six different days, ranged from 92.86% to 99.88% and from 1.19% to 4.53%, respectively. (C)- 2007 Elsevier B.V. All rights reserved.