基于¹H-NMR的布洛芬缓释片和乳膏含量测定方法研究

目的: 以基准物非那西汀为内标,建立布洛芬缓释片和布洛芬乳膏中布洛芬含量的核磁共振氢谱(¹H-NMR)测定方法. 方法: 选定¹H-NMR的脉冲程序zg 30,氢谱宽度6.009 kHz,脉冲宽度11.95 μs,延迟时间6.50 μs,采样温度27℃,采样次数32次. 结果: 以布洛芬中δ 2.46的峰为定量峰,非那西汀δ2.16的峰为内标峰,内标物非那西汀浓度为4.02 mg·mL^-1,布洛芬质量浓度在1.0~8.0 mg·mL^-1范围内具良好的线性关系Y=6.433X-0.181 3(r=0.999 6);缓释片和乳膏的平均加样回收率及其RSD分别为99.4%、0.88%(n=9)和100.2%、1.9%(n=9),测定布洛芬乳膏和布洛芬缓释片含量分别为95.1%、101.6%,与标示量相符. 结论: 该法经方法学验证可用于布洛芬制剂的含量测定.

Objective: To develop an ¹H-NMR method to measure ibuprofen in sustained release tablets and cream with the primary standard substance phenacetin as the internal standard. Methods: Ibuprofen samples and phenacetin(used as internal standard)were resolved in deuterated chloroform and then analyzed by ¹H-NMR.The pulse sequence,hydrogen spectral width,p ulse width,delay time,temperature and number of scans were set to zg 30,6.009 kHz,11.95 μs,6.50 μs,27℃ and 32,respectively. Results: The peak of δ 2.46 of the ibuprofen and the peak of δ 2.16 of phenacetin were selected as quantitative peak and internal standard peak,respectively.In the range of 1.0-8.0 mg·mL^-1,a good linear relationship was established with a regression equation as Y=6.433X-0.181 3(r=0.999 6)for ibuprofen.The average recovery rate and the relative standard deviation for ibuprofen sustained release tablets and cream measurement were 99.4%,0.88%(n=9),and 100.2%,1.9%(n=9),respectively.The content of ibuprofen in cream and sustained release tablets were 95.1% and 101.6%,respectively,in consistence with the labelled amount. Conclusion: With the methodology validation,the ¹H-NMR method could be applied to the measurement of ibuprofen in sustained release tablets and cream.