Τίτλος:
Development and validation of a GC/MS method for the determination of tadalafil in whole blood
Γλώσσες Τεκμηρίου:
Αγγλικά
Περίληψη:
Tadalafil is a phosphodiesterase type 5 (PDE-5) inhibitor and it is used in the treatment of pulmonary arterial hypertension and erectile dysfunction. A sensitive and specific method is described for the determination of tadalafil in whole blood. Tadalafil and its internal standard (protriptyline) were isolated from the matrix by solid phase extraction, and were analyzed by gas chromatography/mass spectrometry (GC/MS) after derivatization by N,O-bis(trimethylsilyl)-trifluoracetamide (BSTFA) with 1% trimethylchlorsilane (TMCS). Limits of detection and quantification for tadalafil were 0.70 and 2.00. μg/L, respectively. The calibration curve was linear between 2.00 and 500.0. μg/L, with a correlation coefficient higher than 0.991. The values obtained for intra- and inter-day accuracy was found to be between -10.5 to 8.5% and -4.2 to 4.5%, respectively, while intra- and inter-day precision were less than 8.4 and 11.2%, correspondingly. Absolute recovery was determined at three concentration levels and ranged from 92.1 to 98.9%. The proposed method is the first fully validated GC/MS method for the determination of tadalafil in whole blood and it can be routinely applied by toxicological laboratories, for pharmacokinetic studies, for therapeutic drug level monitoring or for the investigation of related forensic cases. © 2011 Elsevier B.V.
Συγγραφείς:
Nikolaou, P.
Papoutsis, I.
Athanaselis, S.
Alevisopoulos, G.
Khraiwesh, A.
Pistos, C.
Spiliopoulou, C.
Περιοδικό:
Journal of Pharmaceutical and Biomedical Analysis
Λέξεις-κλειδιά:
tadalafil, accuracy; article; blood; blood sampling; drug blood level; drug determination; human; human tissue; liquid liquid extraction; mass fragmentography; priority journal; solid phase extraction, Blood Chemical Analysis; Calibration; Carbolines; Drug Monitoring; Gas Chromatography-Mass Spectrometry; Humans; Phosphodiesterase 5 Inhibitors; Reference Standards; Reproducibility of Results; Sensitivity and Specificity; Solid Phase Extraction
DOI:
10.1016/j.jpba.2011.05.036
