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目的:建立采用~1H NMR法测定奥沙西泮杂质Ⅰ的绝对含量。方法:以对苯二甲酸二甲酯基准试剂为内标,以氘代氯仿为溶剂,采用Bruker AvanceⅢ500型核磁共振谱仪,noesyigld1d脉冲序列在恒温25℃下获取~1H NMR谱,测定奥沙西泮杂质Ⅰ的含量,驰豫延迟时间为25 s。结果:以奥沙西泮杂质Ⅰ的峰(δ5.97)及对苯二甲酸二甲酯(δ8.10)峰作为定量峰,将样品与内标的NMR峰面积比对其质量比绘制标准曲线,奥沙西泮杂质Ⅰ的线性范围为8~24 mg,相关系数为0.999 9,精密度RSD为0.08%(n=5),重复性RSD为0.43%(n=6),定量限为0.338 mg;核磁共振法测得奥沙西泮杂质Ⅰ的含量为99.8%,与质量平衡法测得结果 99.6%基本一致。结论:采用核磁共振定量的方法可测定奥沙西泮杂质Ⅰ的绝对含量,此方法准确快捷,简单易行,是对标准物质绝对含量测定的一种良好的补充方法。
Objective: To establish the determination of the absolute content of oxazepam impurity Ⅰ using ~ 1H NMR. Methods: 1H NMR spectra were obtained at a constant temperature of 25 ° C using a Bruker Avance III 500 nuclear magnetic resonance spectrometer with a noesyigldld pulse sequence using deuterated chloroform as a solvent, using dimethyl terephthalate as a reference reagent. The content of pan impurity I, the relaxation delay time is 25 s. Results: The impurity peaks of otaxepam (δ5.97) and dimethyl terephthalate (δ8.10) peaks were quantified. The standard curve The linear range of oxazepam I was 8-24 mg, the correlation coefficient was 0.999 9, the precision RSD was 0.08% (n = 5), the repeatability RSD was 0.43% (n = 6), and the limit of quantification was 0.338 mg; the content of oxazepam impurity I measured by NMR is 99.8%, which is basically consistent with the result of 99.6% measured by mass balance method. Conclusion: The absolute content of oxazepam impurity I can be determined by NMR quantitative method. The method is accurate, rapid and easy to perform. It is a good supplement to determine the absolute content of standard substance.