Validated HPLC Method for Determination of Sildenafil in Pharmaceutical Dosage Forms

Poposka, Zaklina and Shishovska, Maja and Starkoska, Katerina and Arsova-Sarafinovska, Zorica (2011) Validated HPLC Method for Determination of Sildenafil in Pharmaceutical Dosage Forms. In: 5th Congress of Pharmacy of Macedonia with International Participation, 21-25 Sept 2011, Ohrid, Republic of Macedonia.

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Abstract

Sildenafil is oral drug used primarily to treat male sexual function problems (impotence or erectile dysfunction) since becoming available in 1998. It is a potent and selective inhibitor of cGMP specific phosphodiesterase type 5 (PDE5) in the corpus cavernosum, where PDE5 is responsible for degradation of cGMP. Sildenafil has a peripheral site of action on erections. This substance has no direct relaxant effect on isolated human corpus cavernosum but potently enhances the relaxant effect of NO on this tissue. However, there is no analytical method for determination of this active compound in pharmaceutical preparations in the current European and US Pharmacopoeia. The aim of this study was to develop and validate HPLC method for sildenafil analysis in pharmaceutical dosage forms. HPLC analysis was performed using a Schimadzu LC-2010 chromatographic system (Schimadzu, Kyoto, Japan) consisting of a LC-20AT Prominence liquid chromatography pump with DGU-20A5 Prominence degasser, a SPD-M20A Prominence Diode Array Detector, RF 10AXI fluorescence detector and a SIL-20 AC Prominence auto sampler. Data analyses were done using Class VP 7.3 Software. The elution was carried out on a column Hypersil BDS-C18 (125 x 4 mm i.d., 5 mm), mobile phase consisted of phosphate buffer (20 mM, pH 2.8)-acetonitrile (71:29, V/V), flow rate 1.5 mL min-1, at controlled temperature (25oC) and auto sampler temperature at 4oC. Detection of sildenafil was carried out at 285 nm. Commercially available, film-coated tablets, containing 50 mg sildenafil as sildenafil citrate, were used in this study. The method was fully validated according to the ICH (International Conference on Harmonization) guidelines by determination of linearity, precision, accuracy, limit of detection and limit of quantification. Linearity of the method was tested in the range of: 2 – 100 mg mL-1 sildenafil. Experimental data showed high level of linearity which was proved with the value for the correlation coefficient (R2 = 0.9994). Limit of detection (LOD) and quantification (LOQ) of the method were tested in the range of: 20 – 200 ng mL-1 sildenafil. The results were: 0.23 ng and 0.68 ng for LOD and LOQ, respectively (9.2 ng mL-1 and 27.2 ng mL-1 for LOD and LOQ, respectively, obtained with 25 mL injected). Selectivity of the method was proved with the chromatographic peak resolution obtained between sildenafil and tadalafil (Rs = 10,5) Mean recovery for sildenafil was between 99,74% and 100,88% indicating that the developed method was accurate for determination of sildenafil in pharmaceutical formulation. The proposed method was successfully applied for determination of sildenafil in film-coated tablets, containing 50 mg sildenafil as sildenafil citrate. The results of the validation demonstrated that the proposed analytical procedure is accurate, precise and reproducible for sildenafil analysis in pharmaceutical dosage forms. Furthermore, this procedure is relatively inexpensive and simple and is particularly suitable for routine analyses when tandem mass spectrometric detection is not available. Additionally, it is important to mention that decreased consumption of organic solvent considerably reduces the laboratory expenses.

Item Type: Conference or Workshop Item (Poster)
Subjects: Natural sciences > Biological sciences
Natural sciences > Chemical sciences
Medical and Health Sciences > Clinical medicine
Medical and Health Sciences > Health sciences
Medical and Health Sciences > Other medical sciences
Divisions: Faculty of Medical Science
Depositing User: Zorica Arsova Sarafinovska
Date Deposited: 01 Jun 2015 09:49
Last Modified: 01 Jun 2015 09:49
URI: http://eprints.ugd.edu.mk/id/eprint/13226

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