基于核磁共振对盐酸阿比多尔片的定性和定量研究

Qualitative and Quantitative Research of Arbidol Hydrochloride Tablets Based on Quantitative Nuclear Magnetic Resonance

关键词:  盐酸阿比多尔片  马来酸  核磁共振法  定性  定量

Key words:  arbidol hydrochloride tablets  maleic acid  nuclear magnetic resonance  qualitative  quantitative

摘要:

目的 基于核磁共振对盐酸阿比多尔片进行定性和定量研究。方法 采用盐酸阿比多尔化学位移δ:7.88 ppm处质子峰为定量峰,马来酸化学位移δ:6.33 ppm处为内标峰,在温度为298 K,弛豫延迟时间10 s,采样时间为4.01 s,扫描次数为32次的条件下采集混合物的核磁共振图谱,对定量峰和内标峰积分后计算其含量。比较核磁共振定量法与HPLC的测定结果。结果 盐酸阿比多尔线性范围是10.53~28.09 mg·mL^-1,回收率在99.76%~101.01%,精密度和稳定性良好,方法学专属性较高。核磁共振定量法与HPLC的测定结果基本一致,而核磁共振定量法具有快速、准确的优势。结论 建立的核磁共振定量法可用于盐酸阿比多尔片定性和定量研究,提供了一种新的质量控制方法。

Abstract:

OBJECTIVE To carry on qualitative and quantitative research of arbidol hydrochloride tablets based on quantitative nuclear magnetic resonance(qNMR). METHODS Proton signal peaks at δ:7.88 ppm of arbidol hydrochloride and δ:6.33 ppm of maleic acid were employed as quantitative peaks and internal standard peaks, respectively. NMR spectrum of mixture were collected at the temperature of 298 K with 10 s relaxation delay, 4.01 s acquisition time and 32 scanning times. And integrated the quantitative peak and internal standard peak to calculate the content. The results of qNMR and HPLC were also compared. RESULTS There was a linear relationship for arbidol hydrochloride in the range of 10.53-28.09 mg·mL^-1. The recoveries were in the range of 99.76%-101.01%. The precision and stability were good, and the methodological speciality was high. The content determination results of qNMR method were generally consistent with those of HPLC method. However, qNMR had an advantage of rapid and accuracy. CONCLUSION The established method of qNMR can be used for qualitative and quantitative analysis of arbidol hydrochloride tablets, providing a new method for quality control.