Reliable LC-MS/MS assay for the estimation of rilpivirine in human plasma: application to a bioequivalence study and incurred sample reanalysis.

摘要: A simple, precise, and rapid stable isotope dilution liquid chromatography-tandem mass spectrometry method has been developed validated for the quantification of rilpivirine, a non-nucleoside reverse transcriptase inhibitor in human plasma. Rilpivirine its deuterated analogue, rilpivirine-d6, used as an internal standard (IS) were quantitatively extracted by liquid-liquid extraction with methyl-tert-butyl ether diethyl solvent mixture from 50 μL The chromatography was achieved on Gemini C18 (150 × 4.6 mm, 5 µm) analytical column run time 2.2 min. precursor  product ion transitions rilpivirine (m/z 367.1  128.0) IS 373.2  134.2) monitored triple quadrupole spectrometer positive ionization mode. linearity established concentration range 0.5–200 ng/mL. mean recovery (94.9%) (99.9%) spiked plasma samples consistent reproducible. IS-normalized matrix factors ranged 0.98 to 1.02 across three quality controls. Bench top, freeze-thaw, wet extract, long-term stability examined samples. application demonstrated bioequivalence study 25 mg tablet formulation 40 healthy subjects. assay reproducibility shown reanalysis 200 % change repeat values original within ±15%. Copyright © 2014 John Wiley & Sons, Ltd.