定量核磁共振法测定一清胶囊和三黄片中的黄芩黄酮总量  

Determination of flavones of Scutellariae radix in Yiqing capsule and Sanhuang tablet by quantitative nuclear magnetic resonance spectroscopy

作　　者：刘明珂 郭强胜[1] 禹珊 许旭[1] 

机构地区：[1]上海应用技术学院化学与环境工程学院,上海201418

出　　处：《分析试验室》2015年第11期1343-1347,共5页Chinese Journal of Analysis Laboratory

摘　　要：用定量NMR方法建立一清胶囊和三黄片两种中成药中黄芩黄酮总量的测定方法。选择内标为邻苯二甲酸氢钾,以其谱峰（δ8.20）为内标峰,待测物定量峰的化学位移在δ8.08处,溶剂为氘代DMSO。通过考察NMR实验条件的影响,选择采样次数NS为128次,延迟时间D1为1.0 s,脉冲宽度P1为3.0μs。通过对样品中主要中药成分的浸膏和辅料的NMR实验测定,显示这两种中成药中的其它中药成分和辅料不干扰定量峰的测定。用对照品评价的（样品/内标）质量比对NMR峰面积比的零截距标准曲线斜率与理论值非常接近,相关系数R=0.999998,显示可以用2010版中国药典的核磁共振绝对定量法计算两种中成药中黄芩黄酮的总含量。对一清胶囊样品中黄芩苷的加标回收率在99.7%~100.2%,溶液稳定。并实际测定了一清胶囊和三黄片两种复方中药的6个样品中黄芩苷类似物的总含量。本法可用于一清胶囊和三黄片两种中成药中黄芩黄酮总量的测定。A quantitative Nuclear Magnetic Resonance Spectroscopy（ q NMR） method was established for determining the flavones of Scutellariae Radix in Yiqing capsule and Sanhuang Tablet. Potassium hydrogen phthalate was chosen as internal standard and its NMR peak of δ 8. 20 as internal standard peak. Quantitative NMR peak of flavones of Scutellariae Radix was selected as δ 8. 08. The solvent was deuterated DMSO. By investigating their effects on NMR experiment,the experimental conditions was selected with number of sampling（ NS） as 128,delay time（ D1） as 1. 0 s,and pulse width（ P1） as 3. 0 μs. Other traditional Chinese medicinal materials and pharmaceutical excipients in these two kinds of Chinese patent medicines didn＇t interfere with the determination of flavones of Scutellariae Radix according to experimental study. The slope of quantitative standard curve of Y = 2. 18793 X is close to the theoretical value of 2. 18588 with the correlation coefficient r =0. 999998,which means absolute quantitative method can be used to calculate flavones of Scutellariae Radix in real two kinds of Chinese patent medicines without standard. The recoveries were 99. 7% ~ 100. 2%. The determined NMR sample solution was stable. The method has been applied to real sample determination. It can be used for the quality control of Yiqing capsule and Sanhuang tablet with its simple,accurate and reproducible features.

关 键 词：一清胶囊 三黄片 黄芩黄酮 定量核磁共振氢谱 

分 类 号：O657.61[理学—分析化学] R284.1[理学—化学]