论文部分内容阅读
目的:考察氘代二甲基亚砜(DMSO-d6)和氘代甲醇(CD3OD)为测试溶剂对牡荆素鼠李糖苷核磁共振氢谱(1H-NMR)的影响,为利用1H-NMR波谱法对山楂叶总黄酮中牡荆素鼠李糖苷进行定量分析方法的建立提供基础研究数据。方法:HPLC法测定牡荆素鼠李糖苷对照品纯度;1H-NMR波谱法测定牡荆素鼠李糖苷对照品在不同溶剂中,以及在含有牡荆素鼠李糖苷的山楂叶总黄酮中加入不同内标物的波谱图。结果:牡荆素鼠李糖苷在DMSO-d6和CD3OD中的1H-NMR波谱峰形完全不同。以DMSO-d6为溶剂时,与HPLC得到的结论一样,即牡荆素鼠李糖苷几乎为纯品;而以CD3OD为溶剂时,牡荆素鼠李糖苷由2个化合物组成。含有牡荆素鼠李糖苷的山楂叶总黄酮加入二氯甲烷、3-三甲基甲硅烷基-2,2,3,3-四氘代丙酸钠(TSP)作内标时,2个化合物相对含量比不同。结论:1H-NMR波谱法对不太复杂混合物的定量分析,尤其对于利用HPLC法难以分离的同分异构体混合物的定量分析具有突出优势;由于1H-NMR波谱法对成分进行定量时不需要对照品,所以该法适用于没有对照品或难以获得对照品的药物定量分析;但该法的分析结果受溶剂、内标物的影响较大。
OBJECTIVE: To investigate the influence of deuterated dimethylsulfoxide (DMSO-d6) and deuterated methanol (CD3OD) on the rhamnosyl hydrogen nuclear magnetic resonance spectrum (1H-NMR) of vitertin. Law on hawthorn leaves flavonoids in the quantitative analysis of rhamnoside vitexin provide the basic research data. Methods: The HPLC method was used to determine the rhamnoside reference substance purity of vitexin. The rhamnoside reference substance of vitexin was determined by 1H-NMR spectroscopy in different solvents and the total flavonoids of hawthorn leaves containing vitexin rhamnoside Spectrum of different internal standards. Results: The results showed that the 1H-NMR spectra of rhamnoside in vitexin were completely different in DMSO-d6 and CD3OD. When DMSO-d6 was used as solvent, the rhamnoside of vitellin was almost pure, which was the same as that of HPLC. When CD3OD was used as a solvent, the rhamnoside of vitexin consisted of two compounds. When total flavonoids of hawthorn leaves containing vitexin rhamnoside were added into dichloromethane and 3-trimethylsilyl-2,2,3,3-tetradeuterated sodium propionate (TSP) was used as internal standard, 2 Compound relative content ratio is different. Conclusion: The quantitative analysis of less complex mixtures by 1H-NMR spectroscopy has outstanding advantages, especially for the quantitative analysis of mixtures of isomers which are difficult to separate by HPLC; it is not necessary to quantify the components by 1H-NMR spectroscopy Therefore, this method is applicable to the quantitative analysis of drugs without reference substance or difficult to obtain reference substance. However, the analysis results of this method are greatly affected by solvents and internal standard substances.