^(19)F qNMR法测定盐酸氟西汀常规固体口服制剂的含量  

Quantitative determination of fluoxetine hydrochloride in conventional solid oral formulations using ^(19)F qNMR method

作　　者：李增鑫 周晓力[1] 刘万卉[2] 尹利辉[1] LI Zeng-xin;ZHOU Xiao-li;LIU Wan-hui;YIN Li-hui(National Institutes for Food and Drug Control,Beijing 102629,China;Yantai University,Yantai 264003,China)

机构地区：[1]中国食品药品检定研究院,北京102629 [2]烟台大学,烟台264003

出　　处：《中国新药杂志》2025年第1期89-93,共5页Chinese Journal of New Drugs

基　　金：中国食品药品检定研究院关键技术研究基金资助项目(GJJS-20224-2)。

摘　　要：目的:建立^(19)F核磁共振定量法(^(19)F quantitative nuclear magnetic resonance,^(19)F qNMR)测定盐酸氟西汀常规固体口服制剂的含量。方法:以4-氟肉桂酸为内标,二甲基亚砜为溶剂,采用Bruker AvanceⅢHD 500 MHz核磁共振波谱仪,脉冲序列zgfhigqn.2,恒温25℃采集^(19)F核磁共振谱(^(19)F NMR),弛豫时间(D1)为10 s,测定盐酸氟西汀多种常规固体口服制剂的绝对含量。结果:以盐酸氟西汀δ-60 ppm处的信号及4-氟肉桂酸δ-110.44 ppm处的信号作为定量信号;平行配制6份供试品溶液,重复性RSD均<2.0%;以样品峰面积对其质量绘制标准曲线,盐酸氟西汀的线性范围为2.5~7.5 mg,相关系数为0.999 6;回收率结果均在98%~102%之间;60 h稳定性及精密度RSD均<1.2%。^(19)F qNMR定量结果与HPLC含量测定结果基本保持一致。结论:经方法学验证,^(19)F qNMR法可用于测定盐酸氟西汀常规固体口服制剂的绝对含量。Objective:To establish a ^(19)F qNMR quantitative method for determining the content of fluoxetine hydrochloride in conventional solid oral formulations.Methods:4-Fluorocinnamic acid was used as the internal standard and dimethyl sulfoxide as the solvent.The Bruker Avance III HD 500 MHz nuclear magnetic resonance spectrometer was applied using a pulse sequence of zgfhigqn.2.The ^(19)F nuclear magnetic resonance spectra(^(19)F NMR spectrum)were collected at a constant temperature of 25℃,and a relaxation delay time(D1)of 10 seconds.The absolute contents of fluoxetine hydrochloride in conventional solid oral formulations were determined.Result:Quantitative signals were obtained from the signals atδ-60 ppm of fluoxetine hydrochloride andδ-110.44 ppm of 4-fluorocinnamic acid.In parallel configuration of 6 test sample solutions,the RSD for repeatability is less than 2%.A standard curve for the mass of the sample based on its peak area was plotted.The linear range of fluoxetine hydrochloride is 2.5 mg to 7.5 mg,with a correlation coefficient of 0.9996.The recovery rate results are all between 98%and 102%.The RSD for stability and precision within 60 hours is less than 1.2%.The quantitative results of ^(19)F qNMR are basically consistent with the HPLC content determination results.Conclusion:According to the certification of traditional Chinese medicine,the ^(19)F qNMR method can be used to determine the absolute content of fluoxetine hydrochloridec in onventional solid oral formulations.

关 键 词：盐酸氟西汀 4-氟肉桂酸 绝对含量测定 ^(19)F NMR法 多种固体制剂 

分 类 号：R917[医药卫生—药物分析学]