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A fully validated method for the determination of vardenafil in blood using gas chromatography/mass spectrometry
Author(s) -
Papoutsis Ioannis,
Nikolaou Panagiota,
Athanaselis Sotirios,
Pistos Constantinos,
Maravelias Constantinos,
Spiliopoulou Chara
Publication year - 2011
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/jms.1868
Subject(s) - chromatography , chemistry , gas chromatography–mass spectrometry , derivatization , mass spectrometry , gas chromatography , analyte , vardenafil , detection limit , solid phase extraction , extraction (chemistry) , sample preparation , forensic toxicology , pharmacokinetics , quantitative analysis (chemistry) , calibration curve , sildenafil , tadalafil , pharmacology , medicine
Vardenafil (VDN) is one of the three commercially available phosphodiesterase type 5 inhibitors and it is mainly used in the treatment of erectile dysfunction. A sensitive and specific gas chromatography/mass spectrometry (GC/MS) method for the determination of VDN in blood has been developed and validated. Sample preparation included solid‐phase extraction and derivatization with N ‐methyl‐ N ‐ tert ‐butyldimethylsilyl‐trifluoroacetamide (MTBSTFA) and 1% tert ‐butyldimethylsilylchloride (TBDMSCl). Protriptyline was used as the internal standard for this assay. Limits of detection and quantification for VDN were 0.70 and 2.00 µg/l, respectively. The calibration curves were linear within the dynamic range 2.00–200.0 µg/l with a correlation coefficient higher than 0.991. Absolute recovery ranged from 88.6% to 95.7% for the analyte of interest at three quality control levels. Intra‐ and inter‐day accuracy was found to be between − 6.1% to 10.8% and − 9.3% to 11.6%, respectively, whereas intra‐ and inter‐day precision was < 7.8% and 9.7%, correspondingly. The proposed method is the first fully validated GC/MS method for the determination of VDN in blood samples and it can be used in routine every day analysis by clinical and forensic laboratories for pharmacokinetic studies, for therapeutic drug level monitoring or for the investigation of related forensic cases. A few blood samples analyzed using the developed method is reported herein to demonstrate the suitability of the method. Copyright © 2010 John Wiley & Sons, Ltd.