核磁共振法定量测定盐酸氨溴索杂质

目的: 建立以核磁共振(qNMR)技术测定盐酸氨溴索杂质含量的方法. 方法: 仪器为配备5 mm BBO探头的Bruker Ascend 500 MHz核磁共振仪,采集一维定量氢谱,延迟时间的 d₁为20 s,温度为25 ℃,采样次数为128次.分别以2,3,5-三碘苯甲酸、对苯二甲酸二甲酯和对硝基甲苯为内标,对5种盐酸氨溴索杂质(杂质A、B、C、D和E)进行定量研究. 结果: 5种盐酸氨溴索杂质(杂质A、B、C、D和E)qNMR法测定结果与对照品标定的质量平衡法定值结果基本一致,相差最大为0.4%. 结论: 采用核磁共振法测定盐酸氨溴索5种杂质的含量,是对标准物质量值测量的一种良好佐证.

Objective: To establish a quantitative nuclear magnetic resonance(qNMR)method for the determination of five ambroxol hydrochloride impurities. Methods: Proton nuclear magnetic resonance spectroscopy(¹H-NMR)spectra were collected at Bruker Ascend 500 spectrometer with 5 mm BBO probe.The internal standards were 2,3,5-triiodobenzoic acid,teraphthalic acid,bis-methyl ester,and 1,4-dinitrobenzene for the quantification of five ambroxol hydrochloride impurities.The parameters were set up as follows. d₁ for delay time was 20 s,the temperature was 25 ℃,the number for sampling was 128. Results: The qNMR results of five ambroxol hydrochloride impurities were generally consistent with the results by mass balance methods,the discrepancy was up to 0.4%. Conclusion: qNMR can be used for the quantitative determination of ambroxol hydrochloride impurities rapidly.It is a good supplementary quantitative method for determination of reference standard.