定量核磁共振法测定去水卫矛醇的含量

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，弛豫延迟时间为20 s，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-d₆）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(¹H 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 dianhydrogalactitol 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.

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