LC-MS/MS方法测定Beagle犬血浆中比卡鲁胺的浓度

目的 建立灵敏的液相色谱-串联质谱法测定狗血浆中比卡鲁胺的浓度.方法 血浆样品采用乙腈蛋白沉淀方法,以0.2％甲酸-乙腈(35∶65,v/v)为流动相；采用Zorbax SB C18柱(150 mm×4.6mm,5 μm)分离,通过电喷雾电离源,以选择多反应监测(MRM)方式进行负离子检测,用于定量分析的离子反应分别为m/z428.9→254.7(比卡鲁胺)和m/z 269→169.6(内标,甲苯磺丁脲).结果 建立的体内比卡鲁胺测定方法线性范围为5～2 000 ng·mL-1,定量下限可达1 ng·mL-1.日内、日间精密度(RSD)均＜10％.结论 该方法预处理操作简洁、灵敏、专属性强,可方便用于比卡鲁胺药物的体内药动学研究.

LC-MS/MS determination of bicalutamide in Beagle plasma

Objective To develop a liquid chromatography-tandem mass spectrometric(LC-MS/ MS) method for the determination of bicalutamide in Beagle plasma.Methods Bicalutamide and the internal standard orinase were separated from the plasma by precipitation.Chromatographic separation was performed on a Zorbax SB C18 column(150 mm×4.6 mm,5 μm) with an isocratic mobile phase consisting of 0.2% formic acid-acetonitrile(35∶65,v/v).A tandem mass spectrometer equipped with electrospray ionization source was adopted as the detector.Multiple reaction monitoring transitions of m/z 428.9→254.7 and m/z 269→169.6 were measured in a positive mode for bicalutamide and the internal standard.Results The calibration curve of bicalutamide was linear at 5-2 000 ng·mL-1.The lower limit of quantification was 1 ng·mL-1.The intra-day and inter-day RSDs were less than 10%.Conclusion The method is sensitive and suitable for pharmacokinetic study of bicalutamide in vivo.