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

    • 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.

       

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