Quantitative proton nuclear magnetic resonance method for simultaneous analysis of fluticasone propionate and azelastine hydrochloride in nasal spray formulation

Abstract

A facile, rapid, accurate and selective quantitative proton nuclear magnetic resonance ( 1 H-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 1 H-qNMR analysis of the studied analytes was performed using inositol as the internal standard and dimethyl sulfoxide- d 6 (DMSO- d 6 ) 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 1 H-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 ( r 2 > 0.999), precision (% RSD < 1.5), stability, specificity and selectivity of the developed method.

Factorial design-assisted reverse phase HPLC–UV approach for the concurrent estimation of cetirizine and azelastine in aqueous humor

“…Different articles have been reported in the literature for the determination of AZE either in dosage form, human plasma or aqueous humor. These articles include: HPLC [27][28][29][30][31] , HPTLC 32,33 , capillary electrophoresis 34 , electrochemical analysis 35,36 , NMR 37 , spectrofluorimetry 22,[38][39][40] and spectrophotometry [41][42][43] .…”

Stability indicating eco-friendly quantitation of terbutaline and its pro-drug bambuterol using quantitative proton nuclear magnetic spectroscopy

“…Other drugs including: tadalafil [ 17 ], favipiravir [ 18 ] sofosbuvir, ledipasvir, and daclatasvir [ 19 ] were also determined. Additionally, research papers have reported the use of 1H-NMR in the determination of co-formulated drugs or related pharmaceutical compounds like an assay of aspirin, phenacetin and caffeine [ 20 ], an assay of levofloxacin, metronidazole and sulfamethoxazole [ 21 ] and analysis of fluticasone propionate and azelastine hydrochloride [ 22 ] in their combined pharmaceutical preparations. Subsequently, International Pharmacopoeias [ 4 , 5 ] reported qualitative NMR spectroscopy for identification purposes and quantitative NMR spectroscopy to evaluate the composition of polymers and impurities in drugs.…”

Simultaneous quantification of Fluticasone propionate and Olopatadine hydrochloride by High‐performance thin‐layer chromatography

“…Hence, FLU nasal spray is commonly used to treat antiallergic, anti-inflammatory, and antipruritic effects Fluticasone is official in Indian Pharmacopoeia [24], British Pharmacopeia [25], US Pharmacopoeia [26], and European Pharmacopeia [27]. From the literature review, it is observed that many analytical methods have been developed involving spectrophotometric [28], HPLC [29][30][31][32][33], UPLC-MS/MS [34], NMR [35], HPTLC [36], and stability indicating method [37][38][39] for the estimation of FLU in pharmaceutical formulations. The present manuscript describes a novel, cost-effective, and quick chromatographic separation method for the simultaneous estimation of OLO and FLU in pharmaceutical formulation.…”