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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/m L and successfully applied to a pharmacokinetic study of healthy rabbits.
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 the 0.1% formic acid: methanol (20:80, v / v) as the mobile phase. The parent-product ion transitions for the drug / 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 / m L and successfully applied to a pharmacokinetic study of healthy rabbits.