1H核磁共振定量法测定氢溴酸右美沙芬片含量

Determination of Content of Dextromethorphan Hydrobromide Tablets Based on Quantitative Proton Nuclear Magnetic Resonance

关键词:  氢溴酸右美沙芬片  苯甲酸苄酯  ¹H核磁共振定量法

Key words:  dextromethorphan hydrobromide tablets  benzyl benzoate  quantitative proton nuclear magnetic resonance

摘要:

目的 采用¹H核磁共振定量法（quantitative proton nuclear magnetic resonance，qHNMR）测定氢溴酸右美沙芬片中氢溴酸右美沙芬含量。方法 qHNMR以氢溴酸右美沙芬化学位移δ 7.05~7.15 ppm处质子峰为定量峰，苯甲酸苄酯δ 5.38 ppm处为内标峰，在温度为300 K，采样时间为4.01 s，弛豫延迟时间10 s，扫描次数为32次条件下采集混合物qHNMR图谱。比较qHNMR与HPLC的含量测定结果。结果 qHNMR专属性较高，线性范围5.88~23.08 mg·mL^-1，回收率为98.4%~99.7%，定量限为0.45 mg·mL^-1，检测限为0.10 mg·mL^-1。qHNMR含量测定结果与HPLC的测定结果基本一致。结论 qHNMR可用于氢溴酸右美沙芬片中氢溴酸右美沙芬的含量测定。

Abstract:

OBJECTIVE to determine the content of dextromethorphan hydrobromide tablets based on quantitative proton nuclear magnetic resonance(qHNMR). METHODS Proton signal peaks at δ 7.05-7.15 ppm of dextromethorphan hydrobromide and δ 5.38 ppm of benzyl benzoate were served as quantitative peaks and internal standard peaks, respectively. The spectra of the mixture were collected at 300 K with 4.01 s acquisition time, 10 s relaxation delay and 32 scanning times. The results of qHNMR and HPLC were also been compared. RESULTS The speciality of qHNMR was very high. There was a linear relationship for dextromethorphan hydrobromide in the range of 5.88-23.08 mg·mL^-1. The recoveries were in the range of 98.4%-99.7%. The limit of quantitation was 0.45 mg·mL^-1 and the limit of detection was 0.10 mg·mL^-1. The content determination results of qHNMR were generally consistent with those of HPLC. CONCLUSION The qHNMR can be used for the quantitative determination of dextromethorphan hydrobromide tablets.