1H_NMR法定量测定奥沙西泮杂质Ⅰ对照品的含量
Determination of impurity Ⅰ reference substance of oxazepam by 1H NMR
分类号：
出版年·卷·期（页码）：2016,36 (9):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要：-------------------------------------------------------------------------------------------
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 Avance Ⅲ 500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（δ 5.97）及对苯二甲酸二甲酯（δ 8.10）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。
-----英文摘要：---------------------------------------------------------------------------------------
Objective: To develop a proton-nuclear magnetic resonance (1H NMR) approach for the determination of impurityⅠof oxazepam.Methods: 1H NMR spectra were obtained in chloroform-d by using an Avance Ⅲ 500 spectrometer with noesyigld1d pulse sequence at 25 ℃,the internal standard was dimethyl terephthalate (DMT),and the relaxation delay time was 25 s.Results: The peak at δ 5.97 of impurityⅠof oxazepam and δ 8.10 of DMT were used for quantitation.The linear relationship between peak area ratio and weight ratio of sample (δ 5.97) to inner standard DMT (δ 8.10) was obtained ranged from 8 mg to 24 mg,with correlative coefficient of 0.999 9.The precision RSD was 0.08%(n=5),and the repeatability RSD was 0.43%(n=6).The LOQ was 0.338 mg.The result determined by the method (99.8%) was consistent with the result by mass balance method (99.6%).Conclusion: The established quantitative nuclear magnetic resonance (QNMR) method can be used for the quantitative determination of impurityⅠof oxazepam,which is effective and reliable as a good complementarity for the determination of the reference standards.
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