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Type: Artigo de periódico
Title: Quantification Of Dapaconazole In Human Plasma Using High-performance Liquid Chromatography Coupled To Tandem Mass Spectrometry: Application To A Phase I Study
Author: de Moraes F.C.
Bittencourt S.F.
Perissutti E.
Frencentese F.
Arruda A.M.M.
Chen L.S.
Babadopulos T.
De Nucci G.
Abstract: A simple, selective and sensitive method based on high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) has been developed for the determination of dapaconazole in human plasma using tioconazole as internal standard. The drugs were extracted from plasma by liquid-liquid extraction with ether/hexane (80/20, v/v). The chromatography separation was performed on a Genesis® C18 reversed phase analytical column 4μm (100×2.1mm i.d.) with a mobile phase of methanol/acetonitrile/water (80/10/10, v/v/v)+ammonium acetate (0.5mM). Dapaconazole was quantified using a mass spectrometer with an electrospray source in the ESI positive mode (ES+) configured for multiple reaction monitoring (MRM) to monitor the transitions 415.1>159.2 and 387.0>131.0 for dapaconazole and tioconazole, respectively. The method had a chromatography run time of 3.8min and a linear calibration curve over the range 0.2-100ng/mL (r=0.9998). The lower limit of quantification (LLOQ) was 0.2ng/mL. The precision and accuracy values of the assay were within ±10%. The stability tests indicate no significant degradation under the conditions of the experiment. This method was used for a phase I study of topical administration of dapaconazole tosylate in healthy human male volunteers. © 2014 Elsevier B.V.
Editor: Elsevier
Rights: fechado
Identifier DOI: 10.1016/j.jchromb.2014.01.053
Date Issue: 2014
Appears in Collections:Unicamp - Artigos e Outros Documentos

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