核磁共振定量法测定恩曲他滨绝对含量  

Determination of Emtricitabine by Quantitative Nuclear Magnetic Resonance

作　　者：李宏伟[1] 张红芹 郝海军[3] LI Hong-wei;ZHANG Hong-qin;HAO Hai-jun(International School,Huanghe Science ＆ Technology College,Zhengzhou 450063,China;FuBiCheng（Shanghai）Pharmaceutical Technology Co.,Ltd.,Shanghai 201203,China;Shanghai Institute of Pharmaceutical Industry,Shanghai 201203,China)

机构地区：[1]黄河科技学院国际学院,河南郑州450063 [2]辅必成上海医药科技有限公司,上海201203 [3]上海医药工业研究院,上海201203

出　　处：《化学试剂》2018年第8期755-758,共4页Chemical Reagents

基　　金：河南省高等学校青年骨干教师培养计划资助项目(2017GGJS286)

摘　　要：分别采用氢核磁共振定量法和氟核磁共振定量法测定恩曲他滨绝对含量。氢核磁共振定量法以恩曲他滨δ8.32-8.40处质子峰和对苯二甲酸二甲酯δ8.12处为定量峰,在恒温27℃,采样时间4.01 s,弛豫延迟时间10s,扫描次数为64条件下采集氢谱。氟核磁共振定量法以4′-溴-2′-氟-乙酰苯胺为内标,在恒温27℃,谱宽为29 296.87 Hz,中心频率为-54 667.50 Hz下采集氟谱。结果显示,氢核磁共振定量法和氟核磁共振定量法测定结果基本与质量平衡法结果一致。因此,核磁共振法测定恩曲他滨绝对含量具有专属性高、准确、快速等优势。Proton nuclear magnetic resonance（ q HNMR） and fluorine nuclear magnetic resonance（ q FNMR） were employed to determine the content of emtricitabine.The1 HNMR spectra were collected at 27 ℃ with 4. 01 s acquisition time,10 s relaxation delay and 64 scanning times. Proton signal peaks at δ 8. 32 - 8. 40 of emtricitabine and δ 8. 12 of dimethyl terephthalate were served as quantitative peaks.The19 FNMR spectra were obtained at 27 ℃ with spectral width was 29 296. 87 Hz and transmitter frequency offset was-54 667. 50 Hz. 4′-Bromo-2′-fluoroacetanilide was employed as internal standard of q FNMR. The results of q HNMR and q FNMR were generally consistent with that of the mass balance method.Quantitative nuclear magnetic resonance was specific,rapid and accurate,and could be used for the quantitative determination of emtricitabine.

关 键 词：恩曲他滨 核磁共振法 氢核磁共振定量法 氟核磁共振定量法 

分 类 号：O652.1[理学—分析化学]