摘要
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 AvanceⅢ600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(δ6.76)及对苯二甲酸二甲酯(δ8.10)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 noesyigld1 d 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.
作者
周晓力
曾月林
南楠
陈华
ZHOU Xiao-li;ZENG Yue-lin;NAN Nan;CHEN Hua(National Institutes for Food and Drug Control,Beijing 102629,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第1期178-182,共5页
Chinese Journal of Pharmaceutical Analysis
