核磁共振氢谱内标法测定盐酸小檗碱的含量-第三军医大学学报.doc

核磁共振氢谱内标法测定盐酸小檗碱的含量 陈玉兰1，陶凌晖2，侯 华2，张 艺1*，周向东2 （1成都中医药大学民族医药学院，成都 611137；2第三军医大学药学院药物化学教研室，重庆 400038Varian 公司Mercury Plus 400MHz核磁共振仪，在25℃下、以氘代甲醇为溶剂、2，4-DNT400.123MHz、谱宽6410.3 Hz、90°脉冲宽度6.450 μs、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δ 6.130 ppm 和δ 8.450 ppm 盐酸小檗碱单峰和2,4-DNT的作为定量峰，含量测定重复性实验的RSD为1.785% (n =6)88.8477%、88.3803%、88.6587%。结论 在没有对照品的情况下，核磁共振氢谱内标法可用于的含量测定和质量控制。 核磁共振氢谱内标法A Determination quantitation of berberine hydrochloride by proton nuclear magnetic resonance spectroscopy with internal standard method CHEN Yu-Lan1, TAO Ling-Hui2,HOU Hua2, ZHANG Yi1,ZHOU Xiang-Dong2 (1Cheng Du University of Chinese Traditional Medicine, Cheng Du 611137; 2Department of Medicinal Chemistry, College of Pharmacy, Third Military Medical University, Chongqing 400038，China ) Abstract: Objective A rapid, specific and simple method was established for the quantitation of the Berberine Hydrochloride. Methods 1H-NMR spectra were obtained in CD3OD with a Varian Mercury Plus 400MHz spectromerter at 25℃. For each sample, 64 scans were recorded with the following parameters: observing frequency, 400.123MHz; spectra width, 6410.3 Hz; 90° pulses width, 6. 450μs; acquisition time, 4s; and delay time, 18s. Results The analysis of 1H NMR spectrum of Berberine Hydrochloride mixed with 2, 4-dinitrotoluene (2, 4-DNT) as internal standard in CD3OD revealed that the integration of signals at δ6.130 ppm of Berberine Hydrochloride and δ8.450ppm of 2, 4-DNT could be used for the quantitation. The precision RSD is 1.785% ( n = 6). The results of the contents are 88.8477%、88.3803%、88.6587%. Conclusion The results showed that 1H NMR can be used for the quantitative determination and quality control of Berberine Hydrochloride. Key words: quantitive proton nuclear magnetic resonance spectroscopy (q-1H NMR) ;internal standard method; berberine hydrochloride 基金项目：国家“十一五”科技支撑计划（2007BAI40B05） Supported by the National Eleventh Five-Year Technology Plan to support（2007BAI40B05） 作者简介：陈玉兰，女，四川省泸州市人，硕士研