垂盆草的化学成分分离鉴定

Chemical Constituents of Sedi Herba

摘要:

目的：对景天科植物垂盆草Sedum sarmentosum全草的化学成分进行分离并对分离得到的单体化合物进行结构鉴定。方法：取干燥垂盆草全草15 kg，加10倍量70%乙醇加热回流提取3次，每次2 h，合并滤液，浓缩得浸膏。经200~300目硅胶拌样后上硅胶柱，用石油醚-乙酸乙酯（100：1~98：2~9：1~7：3），二氯甲烷-甲醇（100：0~95：5~9：1~8：2~7：3~6：4）顺序进行梯度洗脱，得到10个部位。采用反复硅胶柱色谱，羟丙基葡聚糖凝胶柱色谱、反相ODS柱色谱、制备薄层色谱及重结晶的手段对石油醚-乙酸乙酯（98：2）部位、石油醚-乙酸乙酯（9：1）部位、二氯甲烷-甲醇（95：5）部位、二氯甲烷-甲醇（9：1）部位、二氯甲烷-甲醇（8：2）部位进行分离纯化，结合化合物理化常数和波谱数据分析来鉴定化合物结构。结果：从垂盆草中分离并鉴定出12个化合物，分别为δ-香树脂醇（1），δ-香树脂酮（2），3-表-δ-香树脂醇（3），β-谷甾醇（4），木犀草素（5），α-香树脂醇（6），山柰素（7），金丝桃苷（8），芹菜素（9），香草酸（10），槲皮苷（11），胡萝卜苷（12）。结论：化合物9，10为首次从该属中分离得到，化合物6，7为首次从垂盆草中分离得到。

Abstract:

Objective: To isolate the chemical constituents from Sedi Herba and identify the structure of the monomer compounds. Method: The 15 grams of the whole dry Sedi Herba was heated by 10 times the amount of 70% ethanol for 3 times(2 hours for each time) and the filtrate was combined to get the extracts.The extracts was mixed by 200-300 mesh silica gel and the elution was using petroleum ether-ethyl acetate(100:1-98:2-9:1-7:3) and dichloromethane-methanol(100:0-95:5-9:1-8:2-7:3-6:4) to get 10 sites.Silica gel,Sephadex LH-20,ODS,PTLC and recrystallization were used for the isolation and purification of chemical constituents of 5 sites. Their structures were identified on the basis of physico-chemical properties and spectral analysis. Result: Twelve compounds were isolated and their structures were identified as follows:δ-amyrin (1), δ-amyrione (2), 3-epi-δ-amyrin (3), β-sitosterol (4), luteolin (5), α-amyrin (6), kaempferide (7), hyperoside (8), apigenin (9), vanillic acid (10), quercitrin (11), daucosterol (12). Conclusion: Compounds 9 and 10 were isolated from this genus for the first time,compounds 6 and 7 were isolated from Sedi Herba for the first time.