Analytical and optimization data for determination of azelastine hydrochloride and fluticasone propionate by quantitative proton NMR

A facile, rapid, accurate, and selective quantitative proton nuclear magnetic resonance (1H-qNMR) method was developed for the simultaneous determination of fluticasone propionate and azelastine hydrochloride in pharmaceutical nasal spray for the first time. The 1H-qNMR analysis of the studied analytes was performed using inositol as the internal standard and dimethyl sulfoxide-d6 (DMSO-d6) as the solvent. The quantitative selective proton signal of fluticasone propionate was doublet of doublet at 6.290, 6.294, 6.316, and 6.319 ppm, while that of azelastine hydrochloride was doublet at 8.292 and 8.310 ppm. The internal standard (inositol) produced a doublet signal at 3.70 and 3.71 ppm. The method was rectilinear over the concentration ranges of 0.25–20.0 mg mL-1 and 0.2–15.0 mg mL-1 for fluticasone propionate and azelastine hydrochloride, respectively. No labeling or pretreatment steps were required for NMR analysis of the studied analytes. The proposed 1H-qNMR method was validated efficiently according to the International Council on Harmonisation (ICH) guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, specificity, and stability. Moreover, the method was applied to assay the analytes in their combined nasal spray formulation. The results ensured the linearity (r2 > 0.999), precision (% RSD < 1.5), stability, specificity, and selectivity of the developed method.