核磁共振氢谱内标法测定盐酸小檗碱的含量

目的 建立用内标法快速、专属、简单的测定盐酸小檗碱含量的核磁共振氧谱定量分析方法 .方法 用Varian公司Mercury Plus 400 MHz核磁共振仪,在25℃下,以氘代甲醇为溶剂,2,4-二硝基甲苯(2,4-DNT)为内标,观察在频率400.123 MHz、谱宽6 410.3 Hz、90°脉冲宽度6.450μs、采集时间4 s和延迟时间18 s的条件下采集盐酸小檗碱试样的氢谱.结果 以化学位移分别在8 6.13 ppm和8 8.45 ppm盐酸小檗碱单峰和2,4-DNT的双二重峰作为定量峰,含量测定重复性实验的RSD为1.785%(n=6),测得3批盐酸小檗碱含量分别为88.847 7%、88.380 3%、88.658 7%.结论 在没有对照品的情况下,核磁共振氧谱内标法可用于盐酸小檗碱的含量测定和质量控制.

Quantitive determination of berberine hydrochloride by proton nuclear magnetic resonance spectroscopy with internal standard method

Objective To establish a rapid, specific and simple method for the quantitive determination of berberine hydroehloride. Methods Proton nuclear magnetic resonance spectroscopy (~1H-NMR) spectra were obtained in CD_3OD with a Varian Mercury Plus 400 MHz spectrometer at 25℃. For each sample, 64 scans were recorded with the following parameters: observing frequency (400.123 MHz), spectra width (6 410.3 Hz),90° pulses width (6.450 μs), acquisition time (4 s) and delay time (18 s). Results The analysis of ~1H-NMR spectrum of berberine hydrochloride mixed with 2,4-dinitrotoluene (2,4-DNT) as internal standard in CD_3 OD revealed that the integration of signals at 86.13 ppm of berberine hydrochloride and 88.45 ppm of 2,4-DNT could be used for the quantitation. The precision RSD was 1.785% (n =6). The results of the contents were 88.847 7%,88.380 3% and 88.658 7%. Conclusion ~1H NMR can be used for the quantitative deter-mination and quality control of berberine hydrochloride.