基于核磁共振法对马来酸氟伏沙明片定性及定量分析

Qualitative and quantitative analysis of fluvoxamine maleate tablets based on nuclear magnetic resonance

关键词:  马来酸氟伏沙明  核磁共振法  定性  氟化钠  定量

Key words:  fluvoxamine maleate tablets  nuclear magnetic resonance  NaF  qualitative  quantitative

摘要:

目的 采用核磁共振法对马来酸氟伏沙明片进行定性及定量分析。方法 采用CDCl3提取马来酸氟伏沙明片成分,分别测试核磁共振氢谱(1H NMR)、碳谱(13C NMR)、氟谱(19F NMR)、异核单量子相关谱(HSQC)等。选择马来酸氟伏沙明在δ: -61.1～-60.9 ppm处的氟谱峰作为定量峰,氟化钠在δ: -122.8～-121.9 ppm处的氟谱峰作为内标峰,采集混合物的定量核磁共振氟谱(19F qNMR),通过比较两者信号峰面积计算马来酸氟伏沙明片含量,并进行方法学验证。结果 马来酸氟伏沙明片提取成分的核磁共振结构信息与马来酸氟伏沙明结构式一致。建立的19F qNMR方法专属性高,马来酸氟伏沙明线性范围为2.52～30.85 mg/mL,精密度和稳定性良好,平均回收率为99.69%。19F qNMR法测得马来酸氟伏沙明片的含量与HPLC法测定结果一致。结论 核磁共振法可实现对马来酸氟伏沙明片定性分析及含量测定,为生产及临床用药监控提供了一种快速、准确的研究方法。

Abstract:

Objective Nuclear magnetic resonance (NMR) was used for qualitative and quantitative of fluvoxamine maleate tablets. Methods The ingredients of fluvoxamine maleate tablets were extracted by CDCl3, spectra of 1H NMR, 13C NMR, 19F NMR and HSQC were determined. Fluorine spectrum peak at δ: -61.1～-60.9 ppm of fluvoxamine maleate and δ: -122.8～-121.9 ppm of NaF were employed as quantitative peaks and internal standard peaks, respectively. Quantitative 19F NMR spectra (19F qNMR) of the mixture were collected, and then calculated the content of fluvoxamine maleate tablets by comparing area of the two signal peaks. Method validation of 19F qNMR was also accomplished. Results Nuclear magnetic resonance information of the extracted ingredients from fluvoxamine maleate tablets was the same as the structure of fluvoxamine maleate. The established 19F qNMR method has characteristic of high specificity. There was a linear relationship for fluvoxamine maleate in the range of 2.52～30.85 mg/mL. Its precision and stability were good, and the average recovery was 99.69%. Determination results of 19F qNMR method were consistent with those of HPLC method. Conclusion NMR method could be used for qualitative and quantitative of fluvoxamine maleate tablets simultaneously, which provided a rapid and accurate research method for production and clinical drug monitoring.