分析测试学报2025,Vol.44Issue(10):2198-2203,6.DOI:10.12452/j.fxcsxb.241126555
定量核磁共振氢谱法结合反门控去耦测定氘代新药氢溴酸氘瑞米德韦中的非氘代物
Determination of Non-deuterium Compound in New Deuterated Drug Deuremidevir Hydrobromide by Quantitative Proton Nuclear Magnetic Resonance with Inverse-gated Decoupling
摘要
Abstract
A quantitative proton nuclear magnetic resonance(1 H qNMR)method with inverse-gated decoupling was established for the determination of the non-deuterium compound in deuremidevir hy-drobromide(VV116),a new deuterated drug.CD3 OD was used as the solvent to eliminate the inter-ference of the active hydrogen,and the 13 C satellites were decoupled by the noesyigld1d pulse se-quence.The 1 H qNMR experiment was conducted with the relaxation delay time of 15 s and 64 scan-ning times.The content of non-deuterium compound in VV116 was calculated using the characteristic proton peak at δ 7.53 and the aromatic proton peak at δ 7.11 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 0.999 9.The recoveries were 98.5%-101%,and the relative stan-dard 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 quanti-fication of the non-deuterium compound in VV116.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Key words
quantitative proton nuclear magnetic resonance/inverse-gated decoupling/deuremidevir hydrobromide/non-deuterium compound/deuterated drug分类
数理科学引用本文复制引用
黄逸文,陈蓉,鲁辉,任杰,吴杨..定量核磁共振氢谱法结合反门控去耦测定氘代新药氢溴酸氘瑞米德韦中的非氘代物[J].分析测试学报,2025,44(10):2198-2203,6.基金项目
江苏省市场监督管理局科技计划项目(KJ2024084) (KJ2024084)
苏州市科技计划项目(SKYD2023165) (SKYD2023165)