山东产忍冬藤乙酸乙酯部位化学成分分离鉴定

Chemical Constituents from Ethyl Acetate Extract of Lonicerae Japonicae Caulis

摘要:

目的：对山东道地药材忍冬藤的乙酸乙酯部位进行系统的化学成分研究。方法：将山东产忍冬藤药材50 kg粉碎成粗粉，加70%乙醇室温提取3次，合并提取液，滤过，将滤液减压浓缩得到忍冬藤浸膏，将浸膏加水分散，通过石油醚、乙酸乙酯、正丁醇分步萃取，得到其石油醚部位、乙酸乙酯部位和正丁醇部位。对其乙酸乙酯部分通过反复硅胶柱色谱，MCI-gel树脂柱色谱，Sephadex LH-20柱色谱等多种柱色谱技术进行化学成分的分离纯化，应用TLC，HPLC跟踪检测，结合重结晶技术，分离得到单体化合物。依据各化合物的理化性质和谱学数据鉴定其化学结构。结果：从山东产忍冬藤的乙酸乙酯部位中共分离得到并鉴定了10种化合物，分别为丁香酸（1），乌苏酸（2），松脂素（3），齐墩果酸（4），香叶木素（5），β-谷甾醇（6），肉桂酸（7），芹菜素（8），木犀草素（9），槲皮素（10）。结论：化合物1~3系首次从忍冬植物中分离得到，化合物4~5系首次从忍冬藤中分离得到。

Abstract:

Objective: To study the chemical constituents of the ethyl acetate extract of Lonicerae Japonicae Caulis made in Shandong. Method: Lonicerae Japonicae Caulis made in Shandong was crushed into coarse powder, extracted by 70% ethanol, concentrated under reduced pressure, and then its ethyl acetate extract was gained by fractional extraction. Chemical compounds were isolated and purified by using repeated column chromatographies such as silica gel, MCI-gel resin, and Sephadex LH-20.Their structures were elucidated by spectral data and physicochemical properties. Result: Ten compounds were obtained and identified as syringic acid (1), ursolic acid (2), pinoresinol (3),oleanolic acid (4), diosmetin (5), β-sitosterol (6), cinnamic acid (7), apigenin (8), luteolin (9), and quercetin (10). Conclusion: Compounds 1-3 were isolated from Lonicera for the first time, and compounds 4-5 were isolated from Lonicerae Japonicae Caulis for the first time.