¹H_qNMR定量测定二乙酰吗啡对照品的含量

目的：建立二乙酰吗啡含量的¹H定量核磁共振（¹H qNMR）测定方法。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 600型核磁共振谱仪，noesyigld1d脉冲序列在恒温25℃下获取¹H NMR谱，测定二乙酰吗啡的含量，驰豫延迟时间为25 s。结果：以二乙酰吗啡的峰（δ 6.76）及对苯二甲酸二甲酯（δ 8.10）峰作为定量峰，测得精密度RSD（n=5）为0.22%，重复性RSD（n=5）为0.43%。¹H qNMR测得二乙酰吗啡的含量为98.7%，与质量平衡法结果98.7%（HPLC）、98.3%（GC）以及DSC法结果98.4%基本一致。结论：建立的¹H qNMR可测定二乙酰吗啡的含量。此方法准确快捷，简单易行，是对标准物质含量测定的一种良好的补充方法。

Objective:To establish a ¹H quantitative nuclear magnetic resonance(¹H qNMR)method for the determination of diacetylmorphine. Methods:¹H qNMR spectra were obtained in chloroform-d by using an Avance Ⅲ 600 spectrometer with noesyigld1d pulse sequence at 25℃,the internal standard was dimethyl terephthalate(DMT),the relaxation delay time was 25 s. Results:The peaks at δ 6.76 of diacetylmorphine and δ 8.10 of DMT were used for quantitation;the precision RSD(n=5)was 0.22%,the repeatability RSD(n=5)was 0.74%. The result determined by the method(98.7%)was consistent with the results by mass balance method(98.7% by HPLC and 98.3% by GC)and DSC method(98.4%). Conclusion:The ¹H qNMR method can be used for the quantitative determination of diacetylmorphine. It is indicated that ¹H qNMR is effective and reliable as a good complementarity for the determination of the reference standards.

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