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An inter‐laboratory cross‐validation study for the determination of perampanel in human plasma by liquid chromatography assays
Author(s) -
Mano Yuji
Publication year - 2016
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.3764
Subject(s) - perampanel , chromatography , chemistry , protein precipitation , extraction (chemistry) , mass spectrometry , human plasma , high performance liquid chromatography , sample preparation , detection limit , liquid chromatography–mass spectrometry , tandem mass spectrometry , pharmacology , medicine , adverse effect
Abstract For sample assay to support global clinical studies of perampanel, a novel AMPA receptor antagonist, six chromatographic assay methods in human plasma were developed and fully validated at each laboratory using liquid chromatography with tandem mass spectrometry (LC‐MS/MS) or LC with fluorescence detection (LC‐FL). In this study, samples fortified with known perampanel concentrations were assayed at six laboratories to find whether assay data are comparable. Perampanel was extracted by protein precipitation or liquid–liquid extraction, chromatographed on a reverse‐phase column then detected by MS/MS or FL to achieve the limit of quantification of 0.25 or 1 ng/mL. Cross‐validation samples at four concentrations prepared at a central laboratory were determined at six laboratories and the mean accuracy at each concentration was within ±15% except the low concentration at one laboratory (relative error −17.4%), suggesting that plasma concentrations of perampanel in clinical trials can be compared across laboratories.