定量核磁共振法测定去水卫矛醇的含量  

Quantitative determination of dianhydrogalactitol by proton nuclear magnetic resonance

作　　者：吴先富[1] 张琪[1] 马玲云[1] 王昆[1] 刘明理[1] 李晓东[1] 肖新月[1] 

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2017年第1期181-184,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立定量核磁共振法(qNMR)测定去水卫矛醇的含量。方法:采用核磁共振仪测定一维定量氢谱,90°脉冲,谱宽7 500 Hz,驰豫延迟时间为20s,采样次数为64次测定温度25℃,以对苯二甲酸二甲酯为内标,氘代二甲基亚砜(DMSO-d_6)为溶剂,对去水卫矛醇进行定量研究。结果:qNMR法测定去水卫矛醇的含量为95.82%,与质量平衡法测定结果(96.22%)基本一致。结论:本文建立的qNMR法测定去水卫矛醇的含量准确可靠,简便快速,为该品种的质量控制和对照品赋值提供了新的测定方法。Objective： To establish a quantitative nuclear magnetic resonance （ qNMR ）method for the determination of dianhydrogalactitol. Methods： Proton nuclear magnetic resonance spectroscopy （ IH NMR ）spectra were obtained in DMSO-d6 with the internal standard dimethyl terephthalate by using a Bruker Ascend 500 spectrometer. The parameters of which were set up as follows ： 90~ pulse sequences, spectra width of 7 500 Hz, the relaxation delay time was 20 s, the number for scanning was 64, and the experiment temperature was controlled at 25℃. Results： The content of dianhydrogalaetitol determined by qNMR was 95.82%, which was basically consistent with the results of mass balance method （ 96.22% ）. Conclusion： The established qNMR method is accurate, reliable, simple, and rapid for the quantitative determination of dianhydrogalactitol. The study provides a new way for the quality control of dianhydrogalactitol and certification of its reference substance

关 键 词：去水卫矛醇 卫康醇 蜜花美登木 卫矛醇 定量核磁共振法 对苯二甲酸二甲酯 质量平衡法 

分 类 号：R917[医药卫生—药物分析学]