目的 建立使用非氘代溶劑的氟核磁共振定量方法。方法 以氟化鈉為內(nèi)標(biāo)、恩曲他濱為樣品、去離子水為溶劑，測定氟核磁共振譜，進行線性關(guān)系考察、精密度試驗、穩(wěn)定性試驗、耐用性試驗；平行配制5份樣品，進樣測定，通過樣品響應(yīng)信號與內(nèi)標(biāo)響應(yīng)信號面積比值，計算恩曲他濱含量；同時利用質(zhì)量平衡法測定恩曲他濱的含量，兩種方法進行比較。結(jié)果 非氘代溶劑的氟核磁共振譜圖中氟化鈉與恩曲他濱響應(yīng)信號分離較遠，互不干擾；方法線性關(guān)系良好，精密度、穩(wěn)定性、耐用性均符合要求；氟核磁共振測定樣品中恩曲他濱平均質(zhì)量分數(shù)為100.1%，RSD值為0.57%，與質(zhì)量平衡法測定結(jié)果99.7%基本一致。結(jié)論 建立的氟核磁定量方法無需使用氘代溶劑，準(zhǔn)確快速，可以有效降低試驗成本及環(huán)境污染。

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.

十二五重大新藥創(chuàng)制專項（2015ZX09303001）；廣西特聘專家資助專項2016