美花筋骨草乙酸乙酯部位化学成分分析

Chemical Constituents of Ethyl Acetate Extract from Ajuga ovalifolia var. calantha

目的:研究美花筋骨草(Ajuga ovalifolia var. calantha)95%乙醇提取物的乙酸乙酯萃取部位的化学成分。方法:将美花筋骨草药材用95%乙醇渗漉,合并渗漉液减压浓缩得到浸膏,加水分散浸膏后用石油醚萃取,得到石油醚萃取部位和水层,再用乙酸乙酯对水层进行萃取,得到乙酸乙酯萃取部位。利用硅胶,LH-20型羟丙基葡聚糖凝胶(Sephadex LH-20),小孔树脂(MCI),ODS等色谱柱及半制备型高效液相色谱等方法对美花筋骨草的乙酸乙酯萃取部位分离纯化,并利用NMR,ESI-MS等波谱手段对化合物进行结构鉴定。结果:从美花筋骨草中分离得到17个已知化合物,分别鉴定为蜂斗菜内酯-E(1),黑麦草内酯(2),异黑麦草内酯(3),(E)-linalool-1-oic acid(4),伞形花内酯(5),连翘脂素(6),1-(4-hydroxyphenyl)-ethanol(7),(2E)-8-hydroxy-2,6-dimethyl-2-octenoic acid(8),1H-吲哚-3-羧酸(9),ajugarin I(10),ajugalactone(11),木犀草素(12),20-hydroxyecdysone-2-acetate(13),benzyl-4’-hydroxy-benzoyl-3’-O-β-D-glucopyranoside(14),harpagide(15),6-deoxy-8-acetylharpagide(16),acteoside(17)。结论:其中化合物1,3~4,6~9,14均为初次在该属植物中分离得到,化合物2,5,10,13,15~16均为初次在该植物中分离得到。

Objective: To investigate the chemical constituents from the ethyl acetate extract of 95%ethanol extract from Ajuga ovalifolia var. calantha. Method: A. ovalifolia var. calantha was percolated with95% ethanol,and the percolate was concentrated under reduced pressure to obtain the extract. The extract was then dispersed with water and extracted with petroleum ether to obtain the petroleum ether extract fraction and water layer. Then ethyl acetate was used to extract the water layer to obtain the ethyl acetate extract fraction. The Compounds from the ethyl acetate extract fraction were isolated and purified by silica gel,Sephadex LH-20,MCI column,ODS column chromatography and semi-preparative high performance liquid chromatography. Their structures were elucidated by interpretation of NMR,ESI-MS and other spectral evidence. Result: 17 Compounds were isolated and elucidated as bakkenolide-E(1),loliotide(2),isololiotide(3),(E)-linalool-1-oic acid(4),umbelliferone(5),phillygenin(6),1-(4-hydroxyphenyl)-ethanol(7),(2 E)-8-hydroxy-2,6-dimethyl-2-octenoic acid(8),1 H-indole-3-carboxylic acid(9),ajugarin I(10),ajugalactone(11),luteolin(12),20-hydroxyecdysone-2-acetate(13),benzyl-4’-hydroxy-benzoyl-3’-O-β-D-glucopyranoside(14),harpagide(15),6-deoxy-8-acetylharpagide(16),and acteoside(17). Conclusion: Compounds 1,3-4,6-9,14 were isolated from the plants of Ajuga for the first time,and compounds 2,5,10,13,15-16 were isolated from this plant for the first time.