冯玉飞, 马玲云, 刘睿, 关皓月, 刘倩, 杨东升, 牛剑钊. 用1H 定量核磁共振法同时确定成盐化合物的质量分数和各组分的比例[J]. 北京师范大学学报(自然科学版), 2023, 59(3): 396-400. DOI: 10.12202/j.0476-0301.2022263
引用本文: 冯玉飞, 马玲云, 刘睿, 关皓月, 刘倩, 杨东升, 牛剑钊. 用1H 定量核磁共振法同时确定成盐化合物的质量分数和各组分的比例[J]. 北京师范大学学报(自然科学版), 2023, 59(3): 396-400. DOI: 10.12202/j.0476-0301.2022263
FENG Yufei, MA Lingyun, LIU Rui, GUAN Haoyue, LIU Qian, YANG Dongsheng, NIU Jianzhao. Simultaneous determination of contents and ratio of salt-forming compounds by 1H qNMR[J]. Journal of Beijing Normal University(Natural Science), 2023, 59(3): 396-400. DOI: 10.12202/j.0476-0301.2022263
Citation: FENG Yufei, MA Lingyun, LIU Rui, GUAN Haoyue, LIU Qian, YANG Dongsheng, NIU Jianzhao. Simultaneous determination of contents and ratio of salt-forming compounds by 1H qNMR[J]. Journal of Beijing Normal University(Natural Science), 2023, 59(3): 396-400. DOI: 10.12202/j.0476-0301.2022263

1H 定量核磁共振法同时确定成盐化合物的质量分数和各组分的比例

Simultaneous determination of contents and ratio of salt-forming compounds by 1H qNMR

  • 摘要: 1H定量核磁共振(1H quantitative nuclear magnetic resonance,1H qNMR)方法具有操作简便、实验快速等优点.本文通过该方法可准确测定富马酸丙酚替诺福韦在样品中的含量,并给出丙酚替诺福韦和富马酸的比例,结果与其他分析测试所得结果相符.该方法以氘代二甲基亚砜(DMSO-d6)为溶剂,采集待测样品的核磁共振氢谱,对比丙酚替诺福韦定量峰、富马酸定量峰与内标物响应峰面积,分别计算丙酚替诺福韦和富马酸的质量分数.富马酸丙酚替诺福韦和富马酸与内标物的质量比值在 0.91~1.24范围内线性关系良好,1H qNMR法测得二者质量分数分别为100.06 %和10.90 %,与质量平衡法测得的结果基本一致.本研究建立的核磁共振定量方法不仅可准确、快速地测定丙酚替诺福韦和富马酸这2种成分的质量分数和比例,还为多组分、成盐的化学原料药的比例确定、绝对含量测定提供参考.

     

    Abstract: 1H quantitative nuclear magnetic resonance (1H qNMR) is an easy, fast analytical method.This method was used to simultaneously determine both contents and ratio of tenofovir alafenamide and fumarate in salt-forming drugs tenofovir alafenamide fumarate (TAF).1H NMR sample was prepared using deuterated dimethyl sulfoxide (DMSO-d6) as solvent.Content of TAF and fumarate were calculated after comparison of peak integrations of sample with internal standard.A linear relationship was found between TAF and fumarate in the range of 0.91-1.24.Content of TAF and fumarate from 1H qNMR was estimated to be 100.06 % and 10.90 %, respectively.These data were consistent with the mass balance method.This 1H qNMR method provides accurate and rapid determination of ratio and absolute content of multi-component, salt-forming API.

     

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