Publisher： John Wiley & Sons Inc
E-ISSN： 1942-7611|7|4|290-299
ISSN： 1942-7603
Source： DRUG TESTING AND ANALYSIS, Vol.7, Iss.4, 2015-04, pp. : 290-299
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Abstract
A simple, precise, and rapid stable isotope dilution liquid chromatography‐tandem mass spectrometry method has been developed and validated for the quantification of rilpivirine, a non‐nucleoside reverse transcriptase inhibitor in human plasma. Rilpivirine and its deuterated analogue, rilpivirine‐d6, used as an internal standard (IS) were quantitatively extracted by liquid‐liquid extraction with methyl‐tert‐butyl ether and diethyl ether solvent mixture from 50 μL plasma. The chromatography was achieved on Gemini C18 (150 × 4.6 mm, 5 µm) analytical column in a run time of 2.2 min. The precursor → product ion transitions for rilpivirine (m/z 367.1 → 128.0) and IS (m/z 373.2 → 134.2) were monitored on a triple quadrupole mass spectrometer in the positive ionization mode. The linearity of the method was established in the concentration range of 0.5–200 ng/mL. The mean extraction recovery for rilpivirine (94.9%) and IS (99.9%) from spiked plasma samples was consistent and reproducible. The IS‐normalized matrix factors for rilpivirine ranged from 0.98 to 1.02 across three quality controls. Bench top, freeze‐thaw, wet extract, and long‐term stability of rilpivirine was examined in spiked plasma samples. The application of the method was demonstrated by a bioequivalence study with 25 mg rilpivirine tablet formulation in 40 healthy subjects. The assay reproducibility was shown by reanalysis of 200 study samples and the % change in the concentration of repeat values from the original values was within ±15%. Copyright © 2014 John Wiley & Sons, Ltd.
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