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document
Reliable LC-MS/MS assay for the estimation of rilpivirine in human plasma : application to a bioequivalence study and incurred sample reanalysis . 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 % .
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Intervention_Pharmacological
LC-MS/MS assay
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Intervention_Pharmacological
rilpivirine-d6
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Outcome_Physical
estimation of rilpivirine
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Outcome_Physical
range of 0.5-200 ng/mL .
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Outcome_Other
consistent
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Outcome_Physical
and
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Outcome_Other
reproducible
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Outcome_Physical
. The IS-normalized
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Outcome_Other
across three quality controls .
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Participant_Condition
rilpivirine in human plasma :
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Participant_Condition
rilpivirine
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Participant_Condition
human plasma