Titre du document / Document title

Determination of vardenafil in pharmaceutical formulation by HPLC using conventional C₁₈ and monolithic silica columns

Auteur(s) / Author(s)

ABOUL-ENEIN Hassan Y. ⁽¹⁾ ; GHANEM Ashraf ⁽¹⁾ ; HOENEN Hubert ⁽¹⁾ ;

Affiliation(s) du ou des auteurs / Author(s) Affiliation(s)

⁽¹⁾ Pharmaceutical Analysis Laboratory, Biological and Medical Research Department (MBC-03-65), King Faisal Specialist Hospital and Research Center, Riyadh, ARABIE SAOUDITE

Résumé / Abstract

A simple HPLC analysis for the identification and quantification of vardenafil in a pharmaceutical tablet formulation was performed on a conventional C₁₈ and Chromo-lith Performance RP-18e monolithic columns with acetonitrile-phosphate buffer mixtures as mobile phases. The effects of the proportion of organic solvent (from 20% to 90%), phosphate buffer pH (from 2 to 7.5) and flow rate (from 1 to 5 mL/min) were studied. The best chromatographic conditions were 20:80 (v/v) acetonitrile-10mM phosphate buffer, pH 3.0, as mobile phase at 1 mL/min flow rate for the C₁₈ column, whereas 30:70 (v/v) acetonitrile-10 mM phosphate buffer, pH 3.0, as mobile phase at 2 mL/min flow rate was best for the monolithic column. Methanol was found to be a suitable solvent for extraction of the active substance from tablets. For the C₁₈ and monolithic column, the calibration plots were linear (R²= 0.9996 and 0.9997, respectively) in the concentration range 10-1000μg/mL. Limit of detection (LOD) and limit of quantification (LOQ) values were 0.10 and 0.31 μg/mL for the C₁₈ and 0.11 mL and 0.32 μg/mL for the monolithic column. Intra-assay and inter-assay precision studies reflected a high level of reliability and reproducibility of the method. The proposed method is selective, precise (RSD = 0.45%), and accurate (recovery = 103-107%) in both columns used.

Revue / Journal Title

Journal of liquid chromatography & related technologies   ISSN 1082-6076   CODEN JLCTFC 

Source / Source

2005, vol. 28, n^o4, pp. 593-604 [12 page(s) (article)] (5 ref.)

Langue / Language

Anglais

Editeur / Publisher

Taylor & Francis, Colchester, ROYAUME-UNI  (1996) (Revue)

Mots-clés anglais / English Keywords

Calibration ; Validation ; Tablet ; Dosage form ; Piperazine derivatives ; Sulfonamide ; Lactam ; Bicyclic compound ; Angular nitrogen heterocycle ; Vardenafil ; Vasodilator agent ; Ultraviolet detector ; Reversed phase chromatography ; Monolithic column ; Bonded stationary phase ; HPLC chromatography ; Quantitative analysis ; Chemical analysis ;

Mots-clés français / French Keywords

Imidazotriazine ; Imidazo[5,1-f][1,2,4]triazin-4-one dérivé ; Etalonnage ; Validation ; Comprimé ; Forme pharmaceutique ; Pipérazine dérivé ; Sulfonamide ; Lactame ; Composé bicyclique ; Hétérocycle azote angulaire ; Vardénafil ; Vasodilatateur ; Détecteur UV ; Chromatographie phase inverse ; Colonne monolithique ; Phase stationnaire greffée ; Chromatographie HPLC ; Analyse quantitative ; Analyse chimique ;

Mots-clés espagnols / Spanish Keywords

Contraste ; Validación ; Tableta ; Forma farmacéutica ; Piperazina derivado ; Sulfonamida ; Lactamo ; Compuesto bicíclico ; Heterociclo nitrógeno angular ; Vardenafil ; Vasodilatador ; Detector UV ; Cromatografía fase inversa ; Columna monolítica ; Fase estationaria injertada ; Cromatografía HPLC ; Análisis cuantitativo ; Análisis químico ;

Mots-clés d'auteur / Author Keywords

Liquid chromatography ; monolithic column ; pharmaceutical preparation ; Vardenafil ;

Localisation / Location

INIST-CNRS, Cote INIST : 18068, 35400012674264.0090