Abstract
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 (150 mm × 4.6 mm, 5 μm) 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 2.5 ng/mL and 2 to 5 ng/g in serum and brain tissue respectively, while limits of detection ranged from 0.3 to 0.9 ng/mL in serum and 0.6 to 1.9 ng/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 10 mg/kg of SDF, TDF or VDF.
Copyright © 2012 Elsevier B.V. All rights reserved.
Publication types
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Research Support, Non-U.S. Gov't
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Validation Study
MeSH terms
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Acetonitriles / chemistry
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Animals
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Biotransformation
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Brain / metabolism*
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Calibration
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Carbolines / blood
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Carbolines / pharmacokinetics
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Chromatography, Liquid* / standards
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Dealkylation
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Formates / chemistry
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Imidazoles / blood
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Imidazoles / pharmacokinetics
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Injections, Intraperitoneal
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Limit of Detection
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Male
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Phosphodiesterase 5 Inhibitors / administration & dosage
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Phosphodiesterase 5 Inhibitors / blood*
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Phosphodiesterase 5 Inhibitors / pharmacokinetics*
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Piperazines / blood
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Piperazines / pharmacokinetics
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Purines / blood
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Purines / pharmacokinetics
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Rats
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Rats, Sprague-Dawley
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Reference Standards
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Reproducibility of Results
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Sensitivity and Specificity
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Sildenafil Citrate
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Spectrometry, Mass, Electrospray Ionization* / standards
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Sulfones / blood
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Sulfones / pharmacokinetics
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Tadalafil
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Tandem Mass Spectrometry* / standards
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Triazines / blood
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Triazines / pharmacokinetics
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Vardenafil Dihydrochloride
Substances
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Acetonitriles
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Carbolines
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Formates
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Imidazoles
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Phosphodiesterase 5 Inhibitors
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Piperazines
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Purines
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Sulfones
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Triazines
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formic acid
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Vardenafil Dihydrochloride
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Tadalafil
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Sildenafil Citrate
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acetonitrile