目的 建立氢核磁共振定量法测定恩替卡韦含量的方法.方法 以氘代DMSO为溶剂,恩替卡韦为样品,1,4-二硝基苯为内标测定氢核磁共振谱,通过比较样品定量峰与内标物质响应峰面积,计算恩替卡韦的量.结果 同一样品在相同条件下测定6次,定量峰与内标响应峰比值的RSD值为1.1%;平行配制3份样品,恩替卡韦质量分数93.8%,RSD值为0.70%,与质量平衡法测定结果93.8%一致.结论 氢核磁共振定量法与质量平衡法相比样品用量少,不需要对照品,测定快速准确,是一种有效地化学样品含量测定手段.

Objective To establish a qNMR method to determine the content of entecavir. Methods Using DMSO-d₆ as solvent, entecavir as a sample, and 1,4-dinitrobenzene as an internal standard, the ¹H-NMR data of entecavir were characterized, calculate the assay of entecavir by comparing the response signal area of sample (As) and internal standard (Ar). Results One sample solution was determined under the same NMR conditions for six times, the RSD value of As/Ar was 1.1%; When prepared and characterized three samples, the content of entecavir calculated was 93.8%, RSD was 0.70%. The results were consistent with that using mass balance method (93.8%). Conclusion Using qNMR to characterize the assay of entecavir can avoid the use of reference substance. This is a precise, rapid, and effective method to characterize the contents of chemical samples.

"重大新药创制"科技重大专项(2015ZX09303001);农业部公益专项(201103027);中国食品药品检定研究院中青年基金(2014A6)