Abstract

DEVELOPMENT AND VALIDATION OF A RAPID RP-HPLC METHOD FOR THE DETERMINATION OF CLIDINIUM BROMIDE, CHLORDIAZEPOXIDE AND PANTOPRAZOLE SODIUM IN THEIR COMBINED CAPSULE DOSAGE FORM

Dharati Rami* and Nehal J. Shah

ABSTRACT

Objectives: The current study was to develop a simple, accurate, precise and rapid reversed-phase HPLC method and subsequent validation using ICH suggested approach for the determination of Clidinium bromide (CLBr), Chlordiazepoxide(CDZ), and Pantoprazole sodium(PNT) in their combined capsule dosage forms. Methods: The chromatographic separation of CLBr, CDZ and PNT was achieved on a Sunshell_Coreshell C18 (100mm×4.6 mm; 2.6μm particle size) column using UV detection at 220 nm. The optimized mobile phase was consisted of TEA solution (0.4%)–methanol–acetonitrile pH 6 adjusted with Orthophosphoric Acid (50:30:20, v/v/v) as eluent, at a flow rate of 1.6 ml/min. The retention times were 1.343, 2.550 and 4.927 min for CLBr, CDZ and PNT, respectively. Results: The proposed method provided linear responses within the concentration ranges 10-30, 20-60 and 80-160 μg/ml with LOD values of 0.15, 0.070 and 0.092 μg/ml for CLBr, CDZ and PNT, respectively. Correlation coefficients(r) of the regression equations were greater than 0.996 in all cases. The precision of the method was demonstrated using intra- and inter-day assay C.V values which were less than 2% in all instances. Average % recovery was between 99.34 – 99.71%, 99.66 – 100.21% and 99.76-99.97% for CLBr, CDZ and PNT respectively. Conclusion: The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of CLBr, CDZ and PNT in their combined capsule dosage form.

Keywords: Clidinium Bromide; Chlordiazepoxide; Pantoprazole sodium; Reversed-phase HPLC; Validation.