A fully validated method for the determination of vardenafil in blood using gas chromatography/mass spectrometry

Abstract

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.

Validated spectrofluorimetric method for determination of two phosphodiesterase inhibitors tadalafil and vardenafil in pharmaceutical preparations and spiked human plasma

“…Regarding TAD, the following methods have been reported including: spectrophotometry , densitometry , high‐performance liquid chromatography (HPLC) , liquid chromatography‐tandem mass spectrometry (LC/MS/MS) , gas chromatography–mass spectrometry (GC‐MS) , using adsorptive stripping square wave voltammetry , and micellar electrokinetic capillary chromatography (MEKC) . Meanwhile, VAR was determined via different analytical procedures including: HPLC , LC/MS/MS , GC‐MS , electrochemical method , CE , and MEKC .…”

Voltammetric Determination of Vardenafil on Modified Electrodes Constructed by Graphite, Metal Oxides and Functionalized Multi-Walled Carbon Nanotubes

“…[3][4][5][6] The sensitivity and selectivity of the electrochemical quantification depend on various factors, but the most important and vital of them are the electrodes used. Up to now, several methods were recommended for the determination of vardenafil such as atomic emission spectroscopy, 7 liquid chromatography with UV detection, [8][9][10] fluorescence detection, 11 chemiluminescence detection, 12 tandem mass spectrometry, [13][14] gas chromatography/mass spectrometry 15 and voltammetry. [16][17][18] In voltammetric studies, researchers used glassy carbon electrode, 16 carbon paste electrode 17 and pencil graphite electrode 18 , respectively.…”

Utilitization of Charge Transfer Complexation Reaction for the Spectrophotometric Determination of Vardenafil HCl and Yohimbin HCl in Pharmaceutical Formulations

“…The chemical structure of the studied drugs There is no official method for the determination of VARD in its formulations. Few reports have been published on the determination of Vd, including chromatographic methods [5][6][7][8][9][10][11][12] , gas chromatography 13,14 , electrokinetic capillary chromatography 15,16 , electrochemical methods 17,18 and atomic emission spectrometry 19 .…”