摘要
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 k Hz,脉冲宽度11.95μs,延迟时间6.50μs,采样温度27℃,采样次数32次。结果：以布洛芬中δ2.46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·m L-1,布洛芬质量浓度在1.0-8.0 mg·m L-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 an1H- 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 by1H- NMR. The pulse sequence,hydrogen spectral width,pulse width,delay time,temperature and number of scans were set to zg 30,6. 009 k Hz,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·m L- 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,the1H- NMR method could be applied to the measurement of ibuprofen in sustained release tablets and cream.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第3期548-552,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金资助项目(No.51173057)
关键词
核磁共振氢谱定量分析
布洛芬
乳膏
缓释片
非那西汀内标
含量测定
1H-NMR quantitative analysis
ibuprofen
cream
sustained release tablets
phenacetin internal standard
content determination
作者简介
第一作者Tel：15902792327；E—mail：luckyjm@mail．hust．edu．cn
通信作者Tel：15902792327；E—mail：2001020636@hust．edu．cn
