核磁共振波谱法测定片剂中盐酸巴马汀含量

Determination on Content of Hydrochloride Palmatine in Tablets by Proton Nuclear Magnetic Resonance

以氘代甲醇为溶剂,马来酸为内标,通过比较马来酸内标峰与盐酸巴马汀定量峰的峰面积,采用核磁共振法测定了黄藤素片中盐酸巴马汀的含量。结果显示,该方法的线性范围为1. 00～10. 00 g/L,相关系数(r)为0. 999 3,定量下限为25. 0 mg/L,检出限为8. 5 mg/L,回收率为98. 5%～104%。测定结果与高效液相色谱法基本一致。该方法操作简便、测定结果准确,且与结构鉴定同步完成,适用于黄藤素片的质量控制。

A method of proton nuclear magnetic resonance was developed for the determination of hydrochloride palmatinein in tablets.CD 3OD was employed as solvent and maleic acid as an internal standard,the 1H NMR spectra were obtained with a Bruker AVANCEⅢ400 spectrometer.The content of hydrochloride palmatinein in tablets was determined by comparing the response signal areas of the internal standard(maleic acid,A r)and hydrochloride palmatine(A s).Results showed that there was a linear relationship for hydrochloride palmatine in the range of 1.00-10.00 gL with its correlation coefficient of 0.999 3.The limit of quantitation(LOQ)was 25.0 mgL and the limit of detection(LOD)was 8.5 mgL.The recoveries were in the range of 98.5%-104%.The content of hydrochloride bamatine in tablets was determined by high performance liquid chromatography(HPLC)and proton nuclear magnetic resonance(qNMR),respectively.Results indicated that the two methods had no difference.The qNMR method was easy and simple to handle,and the analysis results was accurate.Furthermore,the structure of the analyte could be identified at the same time.Therefore,qNMR could be used for the quality control of Huangtengsu tablet.