Validation of a stability-indicating HPLC method with diode array detection for the determination of beclomethasone dipropionate in aqueous suspension for nebulizer

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The aim of this study was to develop and validate a stability-indicating high performance liquid chromatographic method for the analysis of beclomethasone dipropionate in aqueous suspensions for nebulizer. This drug was submitted to accelerated degradation studies under acidic, alkaline and oxidation conditions, exposure to light and moisture and thermal stability. The separation of BD and its degradation products was achieved on Eclipse XDB Phenyl column (150 nn x 4.6 mm, i. d. 5 µm particle size) with an isocratic mobile phase containing methanol and water (80:20, v/v). The flow rate was 1.0 mL min-1 and detection wavelength was set at 240 nm, at 30 ºC. Different degradation products were formed in the stress conditions and the peak purity indexes of BD obtained by diode array detection were > 0.999, confirming the specificity of this method. The calibration curve was linear over the selected concentration range of 30.36 – 91.07 µg mL-1 with a correlation coefficient 0.99989. Recovery was within acceptable statistical limits and the limit of detection was 0.062 µg mL-1 . The intra-day repeatability and intermediate precision (RSD) amongst six sample preparations was 1.60 % and 1.43 %, respectively. In conclusion, the proposed method was found to be rapid and stability-indicating with adequate specificity, precision, accuracy and robustness and hence be suitable for monitoring the degradation process of BD during stability studies.