IMPURITY PROFILING OF THE ROPINIROLE EXTENDED RELEASE FORMULATION, IDENTIFICATION AND CHARACTERIZATION OF POTENTIAL DEGRADANT

A novel gradient reversed-phase high-performance liquid chromatographic method has been developed for quantitative determination of Ropinirole hydrochloride and its six impurities in pharmaceutical dosage forms. Chromatographic separation has been achieved on an Inertsil ODS-3V (250mm x 4.6 mm) 5 mu m with buffered mobile phase consisting of solvent A (mixture of 0.1 molar (M) phosphate (pH 7.1) buffer and acetonitrile in the ratio 90:10 (v/v); respectively) and solvent B (mixture of 0.1 molar (M) phosphate (pH 7.1) buffer and acetonitrile in the ratio 60:40 (v/v); respectively) delivered at flow rate of 1.2mL min(-1) and the detection wavelength of 215 nm. Resolution of Ropinirole hydrochloride and all the six potential impurities has been achieved greater than 2.0 for all closely eluting impurities. This drug product was subjected to the stress conditions and stability studies were one degradant impurity was crossing reporting threshold those degradants were separated by preparative high performance liquid chromatography (HPLC) and structural elucidation was carried out by H nuclear magnetic resonance (NMR) and mass spectroscopy. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness.