消癌平注射液中牛奶菜醇的NMR定量分析

波谱学杂志 ›› 2012, Vol. 29 ›› Issue (3): 410-418.

消癌平注射液中牛奶菜醇的NMR定量分析

高翔^1,2，陈东军³，马艳春²，朱丹妮²，余伯阳^1*

1. 中国药科大学现代中药教育部重点实验室，江苏南京 210009； 
2. 中国药科大学中药复方研究室，江苏南京 211198； 
3. 中国药科大学分析测试中心，江苏南京 210009

收稿日期:2011-10-19 修回日期:2012-03-26 出版日期:2012-09-05 发布日期:2012-09-05
通讯作者: 余伯阳，boyangyu@yahoo.com.cn E-mail:boyangyu@yahoo.com.cn；gaoxiang172@163.com
基金资助:
国家“重大新药创新”科技重大专项资助项目（2011ZX09201-201-02），江苏高校优势学科建设工程资助项目.

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

GAO Xiang^1,2, CHEN Dong-Jun³, MA Yan-Chun², ZHU Dan-Ni, YU Bo-Yang^1*

1. Key Laboratory of Modern Chinese Medicine (China Pharmaceutical University), Ministry of Education, Nanjing 210009, China;
2. Department of Complex Prescription of Traditional Chinese Medicine, China Pharmaceutical University, Nanjing 211198, China;
3. Centre for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, China

Received:2011-10-19 Revised:2012-03-26 Online:2012-09-05 Published:2012-09-05
Contact: YU Bo-Yang，boyangyu@yahoo.com.cn E-mail:boyangyu@yahoo.com.cn；gaoxiang172@163.com
Supported by:
国家“重大新药创新”科技重大专项资助项目（2011ZX09201-201-02），江苏高校优势学科建设工程资助项目.

摘要/Abstract

摘要：

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¹H NMR，¹³C NMR，DEPT，¹H-¹H 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δ 5.73，δ 6.73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（A_x/A_s，y）与注射液冻干粉与对苯二酚的质量比（W_x/W_s，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.

关键词: 核磁共振（NMR）, 定量分析, 消癌平注射液, 牛奶菜醇

Abstract:

In order to establish a quality control method for Xiaoaiping Injection, one-dimensional and two-dimensional NMR techniques used to measure the important chemical constituents, including condiritul, in the injection. An NMR method for quantitative analysis of condiritul using hydroquinone as the internal standard was presented. The proton signals of condiritul at δ 5.73 and those of hydroquinone at δ 6.73 were used for quantification. Linear regression of quantitative peak area ratio (A_x/A_s, y) of condiritul-hydroquinone versus mass ratio (W_x/W_s, 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 measurement of condiritul in Xiaoaiping Injection.

Key words: NMR, quantitative determination, Xiaoaiping Injection, condiritul

中图分类号:

O482.53

高翔, 陈东军, 马艳春, 朱丹妮, 余伯阳. 消癌平注射液中牛奶菜醇的NMR定量分析[J]. 波谱学杂志, 2012, 29(3): 410-418.

GAO Xiang, CHEN Dong-Jun, MA Yan-Chun, ZHU Dan-Ni, YU Bo-Yang. Identification and Determination of Condiritul in Xiaoaiping Injection by Nuclear Magnetic Resonance Spectrometry[J]. Chinese Journal of Magnetic Resonance, 2012, 29(3): 410-418.

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