title: An inter-laboratory cross-validation study for the determination of perampanel in human plasma by liquid chromatography assays.
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.
authors.affiliation: Drug Metabolism and Pharmacokinetics, Biopharmaceutical Assessment Core Function Unit, Eisai Co. Ltd, 1-3, 5-chome, Tokodai, Tsukuba-shi, Ibaraki, 300-2635, Japan.
authors.forename: Yuji
authors.initials: Y
authors.lastname: Mano
mesh_terms: D056148:Chromatography, Reverse-Phase / Q000379:methods*; D006801:Humans; D007753:Laboratories; D009570:Nitriles; D011728:Pyridones / Q000097:blood*; D011786:Quality Control; D018091:Receptors, AMPA / Q000819:agonists*; D013050:Spectrometry, Fluorescence
chemical_list: D009570:Nitriles; D011728:Pyridones; D018091:Receptors, AMPA; C551441:perampanel
keywords: chromatographic assay; cross-validation; perampanel; plasma