摘要
建立了反门控去耦-定量核磁共振氢谱法测定氘代新药氢溴酸氘瑞米德韦(VV116)中非氘代化合物的含量。选择氘代甲醇为溶剂消除活泼氢干扰,采用noesyigld1d脉冲序列对^(13)C去耦消除卫星峰,以弛豫延迟时间15 s,扫描次数64次等实验条件采样测试;以非氘代物在δ7.53的特征^(1)H峰为定量峰,VV116和非氘代物在δ7.11的总芳香1H峰为参比峰,计算VV116中非氘代物的含量。结果表明,非氘代物在0.2~2.0 mg/mL范围内定量峰面积与质量浓度线性关系良好(r=0.9999),回收率为98.5%~101%,相对标准偏差(RSD)为0.27%,样品溶液24 h内稳定。5批商业化样品中非氘代物的测定结果为0.87%~1.54%。该方法准确灵敏,操作简便,无需精密称量,且无需任何标准物质,可用于VV116中非氘代物的测定与质量控制。
A quantitative proton nuclear magnetic resonance(1H qNMR)method with inverse-gated decoupling was established for the determination of the non-deuterium compound in deuremidevir hydrobromide(VV116),a new deuterated drug.CD3OD was used as the solvent to eliminate the interference of the active hydrogen,and the ^(13)C satellites were decoupled by the noesyigld1d pulse sequence.The ^(1)H qNMR experiment was conducted with the relaxation delay time of 15 s and 64 scanning times.The content of non-deuterium compound in VV116 was calculated using the characteristic proton peak atδ7.53 and the aromatic proton peak atδ7.11 as the quantitative and reference peak,respectively.The non-deuterium compound showed good linearity in the range of 0.2-2.0 mg/mL with the correlation coefficient of 0.9999.The recoveries were 98.5%-101%,and the relative standard deviation(RSD)was 0.27%.The sample solution was stable within 24 h.The testing results of samples from five commercial batches were 0.87%-1.54%.The method was accurate,sensitive,and independent of reference materials and accurate weighing,which could be applied to the quantification of the non-deuterium compound in VV116.
作者
黄逸文
陈蓉
鲁辉
任杰
吴杨
HUANG Yi-wen;CHEN Rong;LU Hui;REN Jie;WU Yang(Suzhou Institute for Drug Control,Suzhou 215104,China;Shanghai Center for Drug Evaluation and Inspection,Shanghai 200120,China)
出处
《分析测试学报》
北大核心
2025年第10期2198-2203,共6页
Journal of Instrumental Analysis
基金
江苏省市场监督管理局科技计划项目(KJ2024084)
苏州市科技计划项目(SKYD2023165)。
关键词
定量核磁共振氢谱
反门控去耦
氢溴酸氘瑞米德韦
非氘代化合物
氘代药物
quantitative proton nuclear magnetic resonance
inverse-gated decoupling
deuremidevir hydrobromide
non-deuterium compound
deuterated drug
