Indian Journal of Advances in Chemical Science Volume: 6, Issue 3: , August 2018

ISSN No.: 2320-0898 (Print); 2320-0928 (Electronic)

DOI: 10.22607/IJACS.2018.603007

Research Article

Novel Validated Stability-indicating Ultra-performance Liquid Chromatography Method for the Determination of Roflumilast and its Degradation Products in Active Pharmaceutical Ingredient and in Pharmaceutical Dosage Forms

Varaprasad Jagadabi, P. Venkata Nagendra Kumar*, Srinivasu Pamidi, L. A. Ramaprasad, R. Ramakrishna

ABSTRACT

A novel stability-indicating reverse-phase ultra-performance liquid chromatographic method was developed for quantitative determination of roflumilast and its related impurities and degradation products. Chromatographic separation was achieved using a waters acquity ultra-performance liquid chromatography BEH C18 100 mm × 2.1 mm, 1.7 μ column with mobile phase containing a gradient mixture of mobile phase A and B at 60°C with a flow rate of 0.4 mL/min. The related compounds were monitored at 220 nm. The run time was 15 min within which roflumilast and its seven related impurities were well resolved. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision, and robustness. The calibration curves obtained for the seven impurities were linear over the range of 0.202–3.880 μg/mL. The relative standard deviations of intra- and inter-day experiments were <3.0%. The detection limits ranged from 0.070 to 0.085 μg/mL depending on the impurity.

Key words: Roflumilast, Method validation, Potential degradation products, Impurities, Stability indicating, Ultra-performance liquid chromatography.

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