目的 建立氫核磁共振定量法測(cè)定恩替卡韋含量的方法.方法 以氘代DMSO為溶劑,恩替卡韋為樣品,1,4-二硝基苯為內(nèi)標(biāo)測(cè)定氫核磁共振譜,通過(guò)比較樣品定量峰與內(nèi)標(biāo)物質(zhì)響應(yīng)峰面積,計(jì)算恩替卡韋的量.結(jié)果 同一樣品在相同條件下測(cè)定6次,定量峰與內(nèi)標(biāo)響應(yīng)峰比值的RSD值為1.1%;平行配制3份樣品,恩替卡韋質(zhì)量分?jǐn)?shù)93.8%,RSD值為0.70%,與質(zhì)量平衡法測(cè)定結(jié)果93.8%一致.結(jié)論 氫核磁共振定量法與質(zhì)量平衡法相比樣品用量少,不需要對(duì)照品,測(cè)定快速準(zhǔn)確,是一種有效地化學(xué)樣品含量測(cè)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.

"重大新藥創(chuàng)制"科技重大專項(xiàng)(2015ZX09303001);農(nóng)業(yè)部公益專項(xiàng)(201103027);中國(guó)食品藥品檢定研究院中青年基金(2014A6)