摘要
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氢谱定量分析方法。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400.123MHz、谱宽6410.3Hz、90°脉冲宽度6.450μs、采集时间4s和延迟时间18s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δ6.13ppm和δ8.45ppm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88.8477%、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盐酸小檗碱的含量测定和质量控制。
Objective To establish a rapid,specific and simple method for the quantitive determination of berberine hydrochloride.Methods Proton nuclear magnetic resonance spectroscopy（1H-NMR） spectra were obtained in CD3OD 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 CD30D revealed that the integration of signals at δ6.13 ppm of berberine hydrochloride and δ8.45 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%. Gonclusion 1H NMR can be used for the quantitative determination and quality control of berberine hydrochloride.
出处
《第三军医大学学报》
CAS
CSCD
北大核心
2009年第22期2217-2219,共3页
Journal of Third Military Medical University
基金
"十一五"国家科技支撑计划(2007BAI40B05)~~
关键词
核磁共振氢谱定量分析
内标法
盐酸小檗碱
quantitive proton nuclear magnetic resonance spectroscopy
internal standard method
berberine hydrochloride
