溶剂、内标物对牡荆素鼠李糖苷1H—NMR波谱图变化的影响  

Effect of solvent and internal standard substance on rhamnosylvitexin 1H- NMR spectrograms

作　　者：臧雅丽[1] 王建农[1] 李林[2] 韩丁[1] 

机构地区：[1]中国中医科学院西苑医院,北京100091 [2]中国科学院化学研究所,北京100080

出　　处：《药物分析杂志》2010年第1期49-52,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：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：By contrasting 1H-NMR spectrograms of rhamnosylvitexin to examine the spectrogram differences when DMSO-d6 and CD3OD was used as solvent,with the help of this experiment,get some basic data when 1H-NMR was used to determine the quantity of rhamnosylvitexin in hawthorn leaves flavonoids（HLF）.Methods：By HPLC to determine the purity of rhamnosylvitexin;By NMR to obtain rhamnosylvitexin′s 1H-NMR spectrograms with different solvents and HLF′s 1H-NMR spectrograms with different internal standard substances.Results：1H-NMR spectrograms peaks′ shape and amount of rhamnosylvitexin were totally different between using DMSO-d6 and CD3OD as solvent.When DMSO-d6 was used as solvent,rhamnosylvitexin standard substance was nearly pure just as the result of HPLC,but when CD3OD was used as solvent,rhamnosylvitexin standard substance was composed of two compounds in fact.With dichlormethane and 3-trimethylsilyl-2,2,3,3-tetradeutero propionic acid（TSP） as internal standard substances,the ratio of relative quantity between two compounds of rhamnosylvitexin was different.Conclusions：1H-NMR spectrogram has a great preponderance in quantity analysis for those uncomplex mixture,especially for those mixture which can′t be separated by HPLC,but the analysis result is affected by solvent and internal-standard substance.

关 键 词：牡荆素鼠李糖苷 山楂叶总黄酮 内标物 核磁共振氢谱法 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]