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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
Ist Teil von
Journal of pharmaceutical and biomedical analysis, 2012-11, Vol.70, p.529-533
Ort / Verlag
Amsterdam: Elsevier B.V
Erscheinungsjahr
2012
Link zum Volltext
Quelle
Elsevier ScienceDirect Journals
Beschreibungen/Notizen
► A new LC–ESI-ITMS method is established for the determination of PDE5 inhibitors. ► A sample treatment using HybridSPE-Precipitation cartridges is proposed. ► The method permits the determination of analytes in serum and brain tissue. ► The study has been the first to evaluate the rat brain levels of PDE5 inhibitors.
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.