Validated HPLC Method for Assay and Content Uniformity Testing of Roflumilast in Blend and Tablets

What is it about?

Roflumilast is a selective enzyme inhibitor of phosphodiesterase-4. This drug is recommended for treatment of patients suffering from chronic-obstructive-pulmonary-disease with chronic-bronchitis. Roflumilast is not official in pharmacopoeia and the reported methods are having high chromatographic run times. A short run time HPLC method was developed for assay and content uniformity testing to determine the roflumilast in blend and tablets. The mobile phase consists of 10 mM sodium dihydrogen phosphate monohydrate buffer and acetonitrile in the ratio of 45:55 v/v. The HPLC method was developed using accucore-C18 150 × 4.6 mm, 4 μm column with a flow rate of 1.0 mL min-1, 215 nm wavelength and 10 μL injection volume with run time of 5 min. The method linearity was proved between 5.02-40.17 μg mL-1 and obtained correlation-coefficient value is 1.0000. The mean recovery of roflumilast was 100.6%. The stability indicating nature was established and performed the validation by considering ICH Q2 (R1) recommendations.

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Why is it important?

A simple, specific, precise, good extraction and robust HPLC-PDA method was developed and validated for quantification of roflumilast in blend samples and tablets. The method development was done in HPLC with a fast and short chromatographic run time, which results in faster analysis in the present competitive pharma industry. Roflumilast peak was well separated from eight known impurities. Non-interference of blank, placebo and impurities upon chromatographic evaluation of forced-degradation samples revealed that the present quantification method is suitable for analysis of stability samples stored at accelerated and long term storage. The method was well demonstrated for ICH Q2 (R1) recommended validation parameters of linearity, specificity, precision-repeatability, accuracy, intermediate precision and robustness. In addition to roflumilast assay in bulk, blend and tablet formulations, the method can also be applied for testing of blend content uniformity, tablet content uniformity and estimation of drug released from a dosage form in vitro dissolution test.

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