摘要
目的:建立定量核磁共振氢谱法(qHNMR)测定维莫非尼含量的方法。方法:首先采用质谱、核磁共振方法对维莫非尼结构进行确证,然后采用Bruker ANANCE NEO 600型核磁共振波谱仪测定一维定量氢谱,90°脉冲,弛豫时间(D1)15 s,扫描次数(NS)32次,测定温度25℃,以对苯二酚为内标,氘代二甲基亚砜(DMSO-d_(6))为溶剂,对维莫非尼进行定量研究。结果:对维莫非尼核磁共振氢谱和碳谱数据进行归属,利用qHNMR对维莫非尼进行定量分析,测得含量为98.78%,与质量平衡法测得的结果(98.91%)基本一致。结论:建立的qHNMR法操作简单、快速、准确,可用于维莫非尼含量测定。
Objective:To establish a quantitative proton nuclear magnetic resonance method for the determination of vemurafenib.Methods:The structure of vemurafenib was confirmed by MS and NMR.The spectra of proton nuclear magnetic resonance spectroscopy were obtained in dimethylsulfoxide-d_(6),by using Bruker ANANCE NE0600,the parameters of which were set up as follows:90°pulse sequences,the relaxation delay time was 15 s,the number for scanning was 32,the experiment temperature was controlled at 25℃,and hydroquinone were selected as internal standard.The quantitative study was conducted on vemurafenib.Results:The ^(1)H and ^(13)C NMR spectra of vemurafenib was assigned.The content of vemurafenib determined by qHNMR were 98.78%,which was basically consistent with the results of mass balance method(98.91%).Conclusion:The method is simple,rapid and accurate,and can be used for the determination of vemurafenib.
作者
陈忠兰
靳龙龙
徐翊雯
孙会敏
张雅军
吴先富
CHEN Zhong-lan;JIN Long-long;XU Yi-wen;SUN Hui-min;ZHANG Ya-jun;WU Xian-fu(National Institutes for Food and Drug Control,Beijing 102629,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2023年第7期747-751,共5页
Chinese Journal of New Drugs
关键词
定量核磁共振氢谱法
含量测定
维莫非尼
对苯二酚
质量平衡法
quantitative proton nuclear magnetic resonance method
determination of content
vemurafenib
hydroquinone
mass balance method
