A Stability-indicating Assay HPLC Method of Ketoprofen

SHU-YING HSU, CHING-YIH SHAW AND BER-LIN CHANG

National Laboratories of Foods and Drugs, Department of Health,Executive Yuan

ABSTRACT

   The present official method for the assay and analysis of the ketoprofen related substances as described in the British Pharmacopeia is redox titration and thin layer chromatography. The assay method of ketoprofen preparation in the United States Pharmacopeia is an UV/VIS method. The National Laboratories of Foods and Drugs, ROC, require a rapid, sensitive and precise method for the analysis of large numbers of samples including those for ketoprofen. Since the existing official methods for ketoprofen are not all specific for ketoprofen, a specific HPLC method is then desirable. This report presents such an approach. The HPLC system consisted of a Zorbax ODS C18 (4.6 x 150mm) and a mobile phase of aqueous KH2P04 with glacial acetic acid in CH3CN (55/45, v/v) at pH 2.5. A flow rate of 1.2 ml/min, UV detection at 265nm and attenuation of 0.02 aufs were performed. The system suitability was established, and the statistical validation of the performance was carried out for linearity, accuracy and precision. Different chromatograms were observed for the acid, base and photo-degraded samples. The results suggest that different degradation reaction followed different mechanism. The major different degradation products resulting from acid, base and photo-degradation of ketoprofen were separated by this HPLC method.

Key words: Ketoprofen, HPLC, validation