Document Detail


Validation of an LC-ESI-MS/MS method for the quantitation of phosphodiesterase-5 inhibitors and their main metabolites in rat serum and brain tissue samples.
MedLine Citation:
PMID:  22647499     Owner:  NLM     Status:  Publisher    
Abstract/OtherAbstract:
This work proposes a liquid chromatography-electrospray ionization ion trap mass spectrometry (LC-ESI-ITMS) method, for the quantification of sildenafil (SDF), tadalafil (TDF) and vardenafil (VDF) and their metabolites N-desmethylSDF, O-desethylSDF and N-desethylVDF, preceded by a sample preparation step based on protein and phospholipid elimination. A C8 column (150mm×4.6mm, 5μm) with ammonium formate (20mM) and acetonitrile as the mobile phase components have been used. This method has been validated, obtaining limits of quantification ranged from 1 to 2.5ng/mL and 2 to 5ng/g in serum and brain tissue respectively, while limits of detection ranged from 0.3 to 0.9ng/mL in serum and 0.6 to 1.9ng/g in brain tissue. Assay recoveries for low level QC samples were higher than 83% and the matrix effect ranged between 91% and 108% in serum and between 98% and 107% in brain tissue. The method has been applied to the quantification of these compounds in the serum and brain tissue of rats treated intraperitoneally with 10mg/kg of SDF, TDF or VDF.
Authors:
Nora Unceta; Leire Echeazarra; Mario Montaña; Joan Sallés; Alberto Gómez-Caballero; M Aránzazu Goicolea; Ramón J Barrio
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2012-5-10
Journal Detail:
Title:  Journal of pharmaceutical and biomedical analysis     Volume:  -     ISSN:  1873-264X     ISO Abbreviation:  -     Publication Date:  2012 May 
Date Detail:
Created Date:  2012-5-31     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  8309336     Medline TA:  J Pharm Biomed Anal     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
Copyright Information:
Copyright © 2012 Elsevier B.V. All rights reserved.
Affiliation:
Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country (UPV/EHU), Vitoria-Gasteiz, Spain.
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