Abstract

A VALIDATED STABILITY–INDICATING HPLC METHOD ESTIMATION OF KETOPROFEN IN THE PRESENCE OF PRESERVATIVE IN THE BULK DRUG AND FORMULATED GEL

Pallavi P. Sadanshio*, Sagar B Wankhede, Praveen D Chaudhari 

Abstract

A new stability-indicating high-performance liquid chromatographicmethod for simultaneous analysis of Ketoprofen, Methyl paraben andPropyl paraben in the bulk drug and Formulated Gel form wasdeveloped and validated. The chromatographic separation wasperformed on C18 Column (250mm × 4.6mm, 5μm particle size) usinga mobile phase Methanol: Water (50:50v/v)at a flow rate of 1.0 ml/minand 30°C column temperature with the detection wavelength at 233nmusing photodiode diode array detector. The retention times ofKetoprofen (RT 4.95 min) and Methyl paraben (RT 6.25 min) propylparben (RT 9.70 min). The linearity was performed in theconcentration range of 5 to 25 μg/mL 4 to 20 μg/mL and 2.5 to 12.5μg/mL for Ketoprofen, Methyl paraben and Propyl paraben respectively with a squaredcorrelation coefficient of 0.999, 0.999 and 0.9983 for MP, KETO and PP respectively. Thepercentage purity of Ketoprofen, Methyl paraben and Propyl paraben were found to be 99-101%. Precision (Inert-day) of the system was found to be 0.36% and 0.18%, 0.11% forKetoprofen, Methyl paraben and Propyl paraben respectively and all the method was foundto be specific and found to be within the limits of the acceptance criteria The limit ofdetection was 0.087 μg/mL and 0.037 μg/mL, 0.012 μg/mL for Ketoprofen, Methyl parabenand Propyl paraben respectively and limit of quantification were 0.77μg/mL and 0.34μg/mL, 0.13μg/mL for Ketoprofen, Methyl paraben and Propyl paraben respectively and the method was found to be specific. Forced degradation conditions of hydrolysis (neutral, acidic and alkaline), oxidation, photolysis and thermal stress, as suggested in the ICH guideline Q1A (R2). The drug showed instability in acid and oxide, while it remained stable in alkaline conditions. The method has proven specificity for stability indicating assay method.

Keywords: Ketoprofen, Methyl paraben. Propyl paraben, Validation, Force degradation studies