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目的:采用19F核磁共振定量法(19F qNMR法)测定五氟利多的绝对含量。方法:以4-氟肉桂酸为内标,以二甲基亚砜为溶剂,采用Bruker AvanceⅢ400型核磁共振谱仪,脉冲序列zgfhigqn.2在恒温25℃下获取19F核磁共振谱(19F NMR谱),测定五氟利多的含量,驰豫延迟时间(D1)为10 s。结果:以五氟利多的峰(δ-117.4)及4-氟肉桂酸(δ-110.9)峰作为定量峰;同一样品连续测试5次,测得精密度RSD为0.34%;平行配制6份供试溶液,其结果的重复性RSD为0.38%;将样品与内标的NMR峰面积比对其质量比绘制标准曲线,五氟利多的线性范围为6.58~22.85 mg,相关系数为0.999 9;定量限为4.06mg。19F qNMR法测得样品的含量为99.89%,与质量平衡法结果 99.96%基本一致。结论:经方法学验证,19F qNMR法可用于测定五氟利多的绝对含量。
OBJECTIVE: To determine the absolute amount of pentaflumidol by 19F nuclear magnetic resonance (19F qNMR) method. Methods: The 19F NMR spectrum of 4F-MS was obtained by using 4-fluorocinnamic acid as internal standard, using dimethylsulfoxide as solvent, Bruker Avance III 400 nuclear magnetic resonance spectrometer and pulse sequence zgfhigqn.2 at 25 ℃. , Determination of pentafluoridin content relaxation delay time (D1) of 10 s. Results: The peak of pentafluoride (δ-117.4) and 4-fluorocinnamic acid (δ-110.9) peak were quantified. The same sample was tested 5 times in succession and the RSD of precision was 0.34%. Six samples were prepared in parallel The results showed that the RSD was 0.38%. The standard curve of the peak area ratio of the sample to the internal standard was plotted against the mass ratio. The linear range of pentafluoride was 6.58-22.85 mg with a correlation coefficient of 0.999 9. Is 4.06 mg. The content of the sample measured by 19F qNMR method was 99.89%, which was basically consistent with the mass balance method of 99.96%. Conclusion: The method of 19F qNMR can be used to determine the absolute content of pentafluidon by methodological validation.