title: Development and validation of a reversed phase liquid chromatographic method for analysis of griseofulvin and impurities.
abstract: A simple and robust reversed phase liquid chromatographic method was developed and validated for the quantitative determination of griseofulvin (GF) and its impurities in drug substances and drug products (tablets). Chromatographic separation was achieved on a Discovery C18 (250mm×4.6mm, 5μm) column kept at 30°C. The mobile phase consisted of a gradient mixture of mobile phase A (water-0.1% formic acid pH 4.5, 80:20, v/v) and B (ACN-water-0.1% formic acid pH 4.5, 65:15:20, v/v/v) pumped at a flow rate of 1.0mL/min. UV detection was performed at 290nm. The method was validated for its robustness, sensitivity, precision, accuracy and linearity based on ICH guidelines. The robustness study was performed by means of an experimental design and multivariate analysis. Satisfactory results were obtained from the validation studies. The use of volatile mobile phases allowed for the identification of three main impurities present above the identification threshold using mass spectrometry (MS). The developed LC method has been applied for the assay and impurity determination of GF drug substances and tablets. The method could be very useful for the quality control of GF and its impurities in bulk and formulated dosage forms.
authors.affiliation: Laboratorium voor Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, KU Leuven, O&N2, PB-923, Herestraat 49, B-3000 Leuven, Belgium.
authors.forename: Getu
authors.initials: G
authors.lastname: Kahsay
authors.forename: Aremu Olajire
authors.initials: AO
authors.lastname: Adegoke
authors.forename: Ann
authors.initials: A
authors.lastname: Van Schepdael
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D000935:Antifungal Agents / Q000032:analysis* / Q000737:chemistry; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004340:Drug Contamination; D006118:Griseofulvin / Q000032:analysis* / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods; D015999:Multivariate Analysis; D011786:Quality Control; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000935:Antifungal Agents; D006118:Griseofulvin