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、碳谱、氟谱、异核单量子关系谱等。选择马来酸氟伏沙明在δ:-61.1×10^(-6)~-60.9×10^(-6)处的氟谱峰作为定量峰,氟化钠在δ:-122.8×10^(-6)~-121.9×10^(-6)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10.54~30.69 mg·mL^(-1),精密度和稳定性良好,平均回收率为99.69%。19F-qNMR测得马来酸氟伏沙明片的含量与HPLC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。
OBJECTIVE To qualitative and quantitative analyze the fluvoxamine maleate tablets by nuclear magnetic resonance(NMR).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 atδ:-61.1×10^(-6)--60.9×10^(-6) of fluvoxamine maleate andδ:-122.8×10^(-6)--121.9×10^(-6) 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 had characteristic of high specificity.There was a linear relationship for fluvoxamine maleate in the range of 10.54-30.69 mg·mL-1.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.CONCLUSION NMR method can be used for qualitative and quantitative of fluvoxamine maleate tablets simultaneously,which provide a rapid and accurate research method for production and clinical drug monitoring.
作者
冯顺丽
李振东
王会
刘莱莱
郑斌
FENG Shunli;LI Zhendong;WANG Hui;LIU Lailai;ZHENG Bin(Henan Vocational College of Applied Technology,Zhengzhou 450042,China;People's Hospital of Henan Province,Zhengzhou 450001,China;Shanghai Zhangjiang Yaogu Public Service Platform Co.,Ltd.,Shanghai 200120,China)
出处
《中国现代应用药学》
北大核心
2025年第13期2263-2269,共7页
Chinese Journal of Modern Applied Pharmacy
基金
河南省科技攻关项目(242102311150)
河南应用技术职业学院青年骨干教师资助项目(2024-GGJS-Y001)。
关键词
马来酸氟伏沙明
核磁共振法
氟化钠
定性
定量
fluvoxamine maleate tablets
nuclear magnetic resonance
NaF
qualitative
quantitative
