Abstract
A facile, rapid, accurate and selective quantitative proton nuclear magnetic resonance (1H-qNMR) method was developed for the simultaneous determination of fluticasone propionate (FLP) and azelastine hydrochloride (AZH) 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 FLP was doublet of doublet at 6.290, 6.294, 6.316 and 6.319 ppm, while that of AZH 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 and 0.2–15.0 mg ml−1 for FLP and AZH, respectively. No labelling 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 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.
Highlights
Allergic rhinitis is an inflammatory complication caused by seasonal or perennial aeroallergens
The results indicated that dimethyl sulfoxide-d6 (DMSO-d6) is the most appropriate deuterated solvent as it is non-volatile at room temperature, it allowed good solubility of the studied drugs, and its signal at 2.5 ppm did not overlap with the quantitative NMR signals of fluticasone propionate (FLP), azelastine hydrochloride (AZH) and inositol
The results indicated an adequate sensitivity of the proposed method (LOD ≤ 0.04 and limits of quantification (LOQ) ≤ 0.12 mg ml−1) that is suitable for the simultaneous estimation of FLP and AZH in their combined pharmaceutical dosage
Summary
Allergic rhinitis (hay fever) is an inflammatory complication caused by seasonal or perennial aeroallergens. Treatment of allergic rhinitis is mainly based on using intranasal glucocorticoids, oral and intranasal antihistamines, intranasal mast cell stabilizers, topical decongestant and leukotriene antagonist [1]. Fluticasone propionate is chemically named as (S)-(fluoromethyl)-6α,9-difluoro-11β, 17-dihydroxy-16αmethyl-3-oxoandrosta-1,4-diene-17β-carbothioate, 17-propanoate (figure 1). It is a synthetic potent trifluorinated corticosteroid with a powerful anti-inflammatory activity that acts by preventing the release of inflammatory mediators in the body [3]. Azelastine hydrochloride is chemically named as (RS)-4-[(4chlorophenyl) methyl]-2-(1-methylazepan-4-yl)-phthalazin-1-one (figure 1). It is a second-generation nonsedating antihistamine drug, which blocks H1-receptor. It possesses anti-inflammatory and mast cell stabilizing effects. It is used topically to relief allergic conditions such as rhinitis and conjunctivitis [4]
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