Abstract
A forced degradation study on roflumilast drug substance was conducted under the conditions of hydrolysis, oxidation, thermal and photolysis. The method was developed and optimized by analyzing forcefully degraded samples. The best separation was achieved on a Zorbax SB C18 1.8 µm column with 0.005 M ammonium formate buffer pH 3.5 and acetonitrile as mobile phase in a 13 min run time. The proposed method was able to resolve all the possible degradation products formed during stress study. The drug was stable to neutral, thermal and photolytic conditions but unstable to acidic, alkaline and oxidative conditions at 80° for 24 h. The degradation products resulting from stress study did not interfere in assay and related substances of roflumilast and thus the method can be regarded as stability indicating. An alternate method was also developed on a conventional 250×4.6 mm, 5 µm column wherein runtime was 38 min. Thus rapid resolution high throughput column was able to reduce the run time from 38 min to 13 min.