消癌平注射液中牛奶菜醇的NMR定量分析

Identification and Determination of Condiritul in Xiaoaiping Injection by Nuclear Magnetic Resonance Spectrometry

为了探索消癌平注射液中的重要化学成分及质量控制新方法,该文运用1 H NMR,13 C NMR,DEPT,1 H-1 H COSY,HSQC及HMBC技术,在消癌平注射液复杂化学成分体系中鉴别出牛奶菜醇,并以对苯二酚为定量内标,NMR内标法测定消癌平注射液中牛奶菜醇的绝对含量.以化学位移分别在δ5.73,δ6.73处的牛奶菜醇和对苯二酚的质子峰为定量特征峰,其峰面积比(Ax/As,y)与注射液冻干粉与对苯二酚的质量比(Wx/Ws,x)的线性回归方程为y=0.034 1 x+0.090 6,相关系数为0.999 6,精密度实验RSD为1.27%,重复性实验RSD为2.16%,稳定性实验RSD为0.13%.分析结果表明:该方法快速、准确、简便,为消癌平注射液的质量控制及质量标准的完善提供了新的方法.

In order to establish a quality control method for Xiaoaiping Injection, one-di- mensional and two-dimensional NMR techniques used to measure the important chemical constituents, including condiritul, in the injection. An NMR method for quantitative a- nalysis of condiritul using hydroquinone as the internal standard was presented. The proton signals of condiritul at 8 5.73 and those of hydroquinone at 8 6.73 were used for quantification. Linear regression of quantitative peak area ratio （Ax/As, y） of condirit-ul-hydroquinone versus mass ratio （Wx/Ws,x） yielded a regression equation of y = 0. 034 1 x＋0. 090 6 with a correlation coefficient of 0. 999 6. The precision relative standard deviation （RSD） was 1.27%, the reproducibility RSD 2.16% and the stability RSD 0. 13%. The results showed that ^1H NMR can be used for quantitative measure-ment of condiritul in Xiaoaiping Injection.