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Application of capillary zone electrophoresis withof f-line solid-phase extraction to in i vitro metabolism studies of antifungals

Título : Application of capillary zone electrophoresis withof f-line solid-phase extraction to in i vitro metabolism studies of antifungals
Autor : Crego, Antonio L.
Gómez, Jesús
Marina, María Luisa
Lavandera Díaz, José Luis
Materias: Compuestos heterocíclicos.AntifungalsSolid-phase extractionCapillary zone electrophoresisin vitro metabolism
Resumen : A simple and robust solid-phase extraction (SPE) procedure for the cleanup and sample preconcentration of antifungals (ketoconazole, clotrimazole, itraconazole, fluconazole, and voriconazole) and their metabolites after incubation with human liver microsomes, as well as a simplified capillary zone electrophoresis (CZE) method for their rapid analysis, have been developed to determine the stability of these compounds in in vitro samples. Three different sample pretreatment procedures using SPE with reversed-phase sorbents (100 mg C8, 100 mg C18, and 30 mg Oasis-HLB) were studied. The highest and most reproducible recoveries were obtained using a 30mg Oasis- HLB sorbent and methanol containing2% acetic acid as eluent. Enrichment by a factor of about four times was achieved by reconstituting the final SPE eluates to a small volume. For the CZE separation, good separations without interfering peaks due to the in vitro matrix were obtained with a simple running electrolyte using a fused-silica capillary. The best separation for all components originated by each tested drug after incubation with human liver microsomes (unmetabolized parent drug and its metabolites) was obtained using a 0.05 M phosphate running buffer (pH 2.2) without additives. The effect of the injection volume was also investigated in order to obtain the best sensitivity. Performance levels in terms of precision, linearity, limits of detection, and robustness were determined.
Descripción : Artículo en colaboración con : Antonio L. Crego, Jesús Gómez y M. Luisa Marina
En: Electrophoresis. ISSN 0173-0835. v. 22, 2001, págs 2503-2511
URI : http://hdl.handle.net/10637/5537
Derechos: http://creativecommons.org/licenses/by-nc-nd/4.0/deed.es
Fecha de publicación : 1-nov-2001
Centro : Universidad San Pablo-CEU
Aparece en las colecciones: Medicina





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