Validated method for determination of bromopride in human plasma by liquid chromatography--electrospray tandem mass spectrometry: application to the bioequivalence study |
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Authors: | Nazare P Massaroti P Duarte L F Campos D R Marchioretto M A M Bernasconi G Calafatti S Barros F A P Meurer E C Pedrazzoli J Moraes L A B |
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Affiliation: | 1. Clinical Pharmacology and Gastroenterology Unit, São Francisco University Medical School, Av. Sao Francisco de Assis 218, 12916-900, Bragança Paulista, SP, Brazil;2. Chemistry Department—FFCLRP-USP, Av. Dos Bandeirantes 3900, 114040-901, Ribeirão Preto, SP, Brazil |
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Abstract: | A simple, sensitive and specific liquid chromatography-tandem mass spectrometry method for the quantification of bromopride I in human plasma is presented. Sample preparation consisted of the addition of procainamide II as the internal standard, liquid-liquid extraction in alkaline conditions using hexane-ethyl acetate (1 : 1, v/v) as the extracting solvent, followed by centrifugation, evaporation of the solvent and sample reconstitution in acetonitrile. Both I and II (internal standard, IS) were analyzed using a C18 column and the mobile-phase acetonitrile-water (formic acid 0.1%). The eluted compounds were monitored using electrospray tandem mass spectrometry. The analyses were carried out by multiple reaction monitoring (MRM) using the parent-to-daughter combinations of m/z 344.20 > 271.00 and m/z 236.30 > 163.10. The areas of peaks from analyte and IS were used for quantification of I. The achieved limit of quantification was 1.0 ng/ml and the assay exhibited a linear dynamic range of 1-100.0 ng/ml and gave a correlation coefficient (r) of 0.995 or better. Validation results on linearity, specificity, accuracy, precision and stability, as well as application to the analysis of samples taken up to 24 h after oral administration of 10 mg of I in healthy volunteers demonstrated the applicability to bioequivalence studies. |
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Keywords: | mass spectrometry bioequivalence bromopride |
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