A sensitive, selective and high-throughput liquid chromatography–tandem mass spectrometry (LC–ESI–MS/MS) method was developed and validated for the quantitation of tolvaptan in rabbit plasma. Sample clean-up involved liquid–liquid extraction (LLE) and chromatography was performed on Zorbax SB C18 analytical column (50 mm ? 2.1 mm, 3.5 mm) using 0.1%formic acid:methanol (20:80, v/v) as the mobile phase. The parent-product ion transitions for the drug (m/z 449.2-252.1) and IS (m/z 456.2-259.2) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) and positive ion mode. The method was validated over the concentration range of 0.10–1000.00 ng/mL and successfully applied to a pharmacokinetic study of healthy rabbits.
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机译：开发了一种敏感，选择性和高通量的液相色谱 - 串联质谱（LC-ESI-MS / MS）方法并验证了兔血浆中托瓦氏菌的定量。样品清理所涉及的液 - 液萃取（LLE）和色谱法在ZORBAX SB C18分析柱（50mm→2.1mm，3.5mm）上使用0.1％甲酸：甲醇（20:80，v / v）作为流动阶段。在三重四极杆质谱仪上监测药物（M / Z 449.2-252.1）和是（M / Z 456.2-259.2）的母体产物离子转变，在多重反应监测（MRM）和正离子模式下操作。该方法验证在0.10-1000.00ng / ml的浓度范围内，并成功地应用于健康兔的药代动力学研究。
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