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 effi...

本研究首次开发了一种简便、快速、准确且具有选择性的定量质子核磁共振（1H-qNMR）方法，用于同时测定药用鼻喷剂中的丙酸氟替卡松与盐酸氮卓斯汀。该方法以肌醇（inositol）为内标，以氘代二甲基亚砜-d6（dimethyl sulfoxide-d6, DMSO-d6）为溶剂，对目标分析物开展1H-qNMR分析。丙酸氟替卡松的定量选择性质子信号为位于6.290、6.294、6.316及6.319 ppm处的双二重峰，而盐酸氮卓斯汀的定量选择性质子信号为位于8.292和8.310 ppm处的二重峰。内标物肌醇在3.70与3.71 ppm处产生二重峰信号。该方法对丙酸氟替卡松和盐酸氮卓斯汀的线性浓度范围分别为0.25~20.0 mg·mL⁻¹与0.2~15.0 mg·mL⁻¹。对目标分析物进行NMR分析时，无需进行标记或预处理步骤。所建立的1H-qNMR方法已通过方法学验证（原文后续内容未完整呈现）。