芫花根的~1H NMR指纹图谱解析  

Analysis for ~1H NMR fingerprint of Radix Daphne genkwa

作　　者：郑维发[1] 石枫[1] 

机构地区：[1]徐州师范大学江苏省药用植物生物技术重点实验室,江苏徐州221116

出　　处：《中成药》2005年第6期625-631,共7页Chinese Traditional Patent Medicine

基　　金：教育部科学技术研究重点项目(No.03049);江苏省高校自然科学基金重点项目(No02KJA360002);江苏省药用植物生物技术重点实室开放基金(No.KJS02114)

摘　　要：目的:建立芫花根的1HNMR指纹图谱,以揭示其次生代谢产物类别的组成,为芫花根有效成分脱毒提取工艺的研制提供检测手段。方法:以CDCl3/DMSO-d6为溶剂,在25°C测定芫花根石油醚丙酮甲醇提取物1HNMR图谱。各质子共振信号强度以相对积分面积表示。用1HNMR图谱考察石油醚→丙酮→甲醇和氯仿→乙醚→乙酸乙酯→甲醇两个分级系统芫花根的各级提取物化学组成的变化。结果:芫花根1HNMR指纹图谱出现了长链烃或二萜原酸酯的质子、芳环质子、吡喃糖基质子以及多个羟基共振信号,提示芫花根中存在二萜原酸酯或长链烃类、黄酮和香豆素等芳香族化合物。不同分级溶剂提取物的1HNMR有显著差异。随着分级提取溶剂的极性增加,高场区质子信号强度迅速减弱,低场区羟基信号、糖基质子信号强度迅速增加。结论:芫花根1HNMR指纹图谱具有特征性和专属性,可作为芫花根有效成分脱毒提取工艺研究提供简便可靠的检测方法。AIM: To establish ()~1H NMR fingerprint of Radix Daphne genkwa to disclose its chemical composition of the secondary metabolites and provide a quick and credible assay for the detoxicated extraction of the active constituents. METHODS: The ()~1H NMR spectrum of petrol-acetone-methanol extract from Radix Dephne genkwa was detected using CDCl_3/DMSO-d_6(1∶1) as the deuterium reagent. The resonance intensity of the proton in the spectrum was indicated in relative integral area of peaks referenced by the resonance intensity of methyl signal in DMSO. The ()~1H NMR of cascade extraction of Radix Dephne genkwa by the reagent in sequence of petrol→acetone→methanol or chloroform→aether→acetyl acetate→methanol was utilized for observing the variation on their chemical compositions. RESULTS: The ()~1H NMR of Radix Dephne genkwa clearly expressed the information of the protons from long chain aliphatics or genkwadaphnin derivatives, aromatic coumarins or flavonoids as well as glycosides with moiety(ies) of pyran saccharide, symbolizing the existence of aliphatics, genkwadaphnin derivatives, coumarins and flavonoids. Remarkable difference was observed in ()~1H NMR spectrum of the extract by different cascade reagent. As the increase in the polarity of reagent, the intensity of the proton signals in upper field was quickly reduced concomitantly with the rapid enhancement of active proton signals from hydroxyls and saccharides in glycosides in down field. CONCLUSION: The ()~1H NMR fingerprint of Radix Dephne genkwa possesses its own characteristics and can be used as a reliable assay for studying the extraction of active constituents with minimum content of toxic diterpenoids. (Key

关 键 词：芫花根 ^1H NMR指纹图谱 分级提取 

分 类 号：R284.1[医药卫生—中药学]