化学
色谱法
药代动力学
电喷雾电离
液相色谱-质谱法
蛋白质沉淀
选择性反应监测
质谱法
甲酸
串联质谱法
高效液相色谱法
电喷雾
生物分析
三级四极质谱仪
药理学
分析物
作者
Haiyan Zhou,Yang Zheng,Yanan Liu,Xiurong Hu,Guolan Wu,Jianzhong Shentu
摘要
Copen is a derivative obtained from the structural modification of osthole, which inhibits tumoral proliferation in many tumor cell lines. A rapid and sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was established for the quantification of copen in rat plasma. After a simple sample preparation procedure by one-step protein precipitation with methanol, copen and bicalutamide (internal standard, IS) were chromatographed on a Zorbax SB-C18 (4.6×100 mm, 1.8 µm) column with a mobile phase consisting of methanol–5 mm ammonium formate water with 0.1% formic acid (80:20, v/v). MS detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode with a positive eletrospray ionization source. The assay was validated in the concentration range of 51.58–20630 ng/mL, with a limit of quantitation (LOQ) of 51.58 ng/mL. The intra- and inter-day precisions (relative standard deviation) were ≤3.21 and ≤11.3%, respectively, with accuracy (%) in the range of 94.66–102.1%. The method was fully validated in a study of the pharmacokinetics of copen (25 mg/kg) after intragastric administration in rats. Copyright © 2014 John Wiley & Sons, Ltd.
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