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  • Author or Editor: D. Sangeetha x
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The objective of the current research is to understand the degradation behavior of avanafil under different stress conditions and to develop a stability-indicating high-performance liquid chromatography (HPLC) method for simultaneous determination of degradants observed during degradation. Avanafil tablets were exposed to acid, base, water, oxidative, thermal, and photolytic degradation conditions. In acid, oxidative, thermal, and humidity degradation, significant degradation was observed. All the degradants observed during degradation were separated from known impurities of avanafil by using reverse-phase (RP)-HPLC. Mobile phase A, 0.1% trifluoro acetic acid and triethylamine in water, and mobile phase B, water and acetonitrile in the ratio of 20:80 (v/v), were used at a flow rate of 1.2 mL/min in gradient elution mode. Separation was achieved by using Inertsil ODS 3 column (3 μm, 4.6 mm × 250 mm) at 45 °C. Peak responses were recorded at 245 nm. Method capability for detecting and quantifying the degradants, which can form during stability, was proved by demonstrating the peak purity of avanafil peak in all the stressed samples. Mass balance was established by performing the assay of stressed sample against reference standard. Mass balance was found >97% for all the stress conditions. The developed analytical method was validated as per International Conference on Harmonization (ICH) guidelines. The method was found specific, linear, accurate, precise, rugged, and robust.

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Summary

A simple, selective, and stability-indicating reverse phase liquid chromatographic method has been developed and validated for the simultaneous determination of impurities and forced degradation products of quetiapine fumarate. The chromatographic separation was achieved on Inertsil-3 C8, 150 mm × 4.6 mm, 5 μm column at 35°C with UV detection at 217 nm using gradient mobile phase at a flow rate of 1.0 mL/min. Mobile phase A contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 80:20 (v/v), respectively, and mobile phase B contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 20:80 (v/v), respectively. The drug product was subjected to the stress conditions of oxidative, hydrolysis (acid and base), hydrolytic, thermal, and photolytic degradation. Quetiapine fumarate was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from main peak and its impurities. The mass balance was found to be in the range of 96.6–102.2% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

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