[关键词]
[摘要]
目的 建立使用非氘代溶剂的氟核磁共振定量方法。方法 以氟化钠为内标、恩曲他滨为样品、去离子水为溶剂,测定氟核磁共振谱,进行线性关系考察、精密度试验、稳定性试验、耐用性试验;平行配制5份样品,进样测定,通过样品响应信号与内标响应信号面积比值,计算恩曲他滨含量;同时利用质量平衡法测定恩曲他滨的含量,两种方法进行比较。结果 非氘代溶剂的氟核磁共振谱图中氟化钠与恩曲他滨响应信号分离较远,互不干扰;方法线性关系良好,精密度、稳定性、耐用性均符合要求;氟核磁共振测定样品中恩曲他滨平均质量分数为100.1%,RSD值为0.57%,与质量平衡法测定结果99.7%基本一致。结论 建立的氟核磁定量方法无需使用氘代溶剂,准确快速,可以有效降低试验成本及环境污染。
[Key word]
[Abstract]
Objective To establish a 19F-quantitative nuclear magnetic resonance (qNMR) method using non-deuterated solvent. Methods Using sodium fluoride as an internal standard, emtricitabine as sample and de-ionized water as solvent, the 19F-qNMR of emtricitabine were analyzed. Linear relation test, precision test, stability test and durability test were carried out. Five samples were prepared in parallel for determination, the content of emtricitabine was calculated through response signal area ratios of sample and internal standard. Meanwhile, the mass balance method was used to determine the content of emtricitabine and the two methods were compared. Results In the non-deuterated solvent NMR spectra, NaF and emtricitabine response signal are far away from each other, and there was no interference between them. The method has a good linear relationship, and its precision, stability and durability all meet the requirements. The content of emtricitabine was calculated to be 100.1%, RSD was 0.57% in 19F-qNMR method. The results were consistent with assay calculated by mass balance method (99.7%). Conclusion The 19F-qNMR established in this paper does not require deuterated solvent and provides a effective way to reduce the test cost and environmental pollution.
[中图分类号]
[基金项目]
十二五重大新药创制专项(2015ZX09303001);广西特聘专家资助专项2016