STRESS DEGRADATION STUDIES AND DEVELOPMENT OF A VALIDATED RP-HPLC METHOD FOR DETERMINATION OF TIAGABINE IN PRESENCE OF ITS DEGRADATION PRODUCTS
Keywords:
Tiagabine, RP-HPLC, Stress degradation studies, ValidationAbstract
Objective: To develop a simple and rapid isocratic reversed-phase high-performance liquid chromatography (RP-HPLC) method and validate as per ICH and USP guidelines for analysis of tiagabine in the presence of its degradation products.
Methods: The chromatographic separation was achieved on a Vision HT C18 column (150 mm × 4.6 mm, 5 µm) with mobile phase comprising of 11.5 mM of sodium dihydrogen phosphate (adjusted to pH 2.0 with orthophosphoric acid):acetonitrile (50:50,v/v) at a flow rate of 1.0 ml/min and the UV detection wavelength set at 254 nm. Stress degradation studies were performed as stated in ICH guidelines on tiagabine bulk drug using acid, base, oxidation, heat and light.
Results: Tiagabine was found to degrade under acidic, photolytic, oxidative and thermal conditions, but stable under basic hydrolysis condition. The developed method was found to be linear in the concentration range of 50-150 µg/ml (r2= 0.9983) and the percentage recovery for the accuracy was 98.86%-99.35%. The LOD and LOQ obtained were 31.93 µg/ml and 96.76 µg/ml, respectively while the %RSD for precision, robustness, and stability studies were less than 2%. The degradation products formed from the stress study were well separated from tiagabine and hence the method could be regarded as stability indicating.
Conclusion: A simple and rapid RP-HPLC method was developed and validated for analysis of tiagabine in the presence of its degradation products and thus, the proposed method can be used in the analysis of tiagabine bulk drug and pharmaceutical formulation in quality control laboratories.
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