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目的:研究石草鞋乙醇提取物的化学成分,对石草鞋全草进行分离鉴定。方法:取石草鞋全草,用90%乙醇回流提取,经低压浓缩后得石草鞋浸膏。将上述浸膏加水超声溶解后依次用石油醚、二氯甲烷和正丁醇萃取。将所得正丁醇部分萃取物过硅胶色谱柱,以石油醚-丙酮-甲醇(80∶20∶0~0∶20∶80)系统梯度洗脱,经过结晶、重结晶、离心分离、过硅胶和LH-20羟丙基葡聚糖凝胶(Sephadex LH-20)纯化。将二氯甲烷萃取物以石油醚-丙酮-甲醇(50∶50∶0)系统梯度洗脱,合并相同组分,再经过离心分离、硅胶和葡聚糖Sephadex LH-20等反复分离、纯化。根据ESI-MS,~1H-NMR和~(13)C-NMR等波谱数据分析鉴定结构。结果:从石草鞋乙醇提取物正丁醇部分中鉴定了7化合物,二氯甲烷部分中鉴定了8化合物。分别鉴定为对羟基苯甲醛(1),3,5-二甲氧基4-羟基苯甲酸(2),苯甲酸(3),桂皮酸(4),丹皮酚(5),槲皮素(6),6,7-二羟基香豆素(7),阿魏酸(8),对羟基苯甲酸(9),2,3-二羟基苯甲酸(10),3,4-二羟基苯甲酸(11),齐墩果酸(12),金丝桃苷(13),没食子酸(14),β-谷甾醇(15)。结论:所有化合物均为首次从该植物中分离得到。
Objective: To study the chemical constituents of the ethanol extract of Shi Xie Xie and to isolate and identify the whole plant of Shi Shi Xie. Methods: Take the stone grass full of grass, with 90% ethanol reflux extraction, after concentration by low pressure Shishicaoxie extract. The above extract was dissolved in water ultrasonic followed by petroleum ether, dichloromethane and n-butanol extraction. The obtained n-butanol fraction was subjected to a silica gel column chromatography and eluted with a gradient of petroleum ether-acetone-methanol (80:20: 0 to 0:20:80) system. After crystallization, recrystallization, centrifugal separation, LH-20 hydroxypropyl dextran gel (Sephadex LH-20). The dichloromethane extract was eluted with a gradient system of petroleum ether-acetone-methanol (50:50: 0). The same fractions were combined and separated by centrifugation. Sephadex LH-20 and other fractions were purified by silica gel and Sephadex LH-20. The structure was identified by spectral data analysis, such as ESI-MS, ~ 1H-NMR and ~ (13) C-NMR. Results: Seven compounds were identified from the n-butanol fraction of the ethanol extract of Lithospermum, and eight compounds were identified in the methylene chloride fraction. Were identified as p-hydroxybenzaldehyde (1), 3,5-dimethoxybenzoic acid (2), benzoic acid (3), cinnamic acid (4), paeonol (6), 6,7-dihydroxycoumarin (7), ferulic acid (8), p-hydroxybenzoic acid (9), 2,3-dihydroxybenzoic acid Benzoic acid (11), oleanolic acid (12), hyperin (13), gallic acid (14) and β-sitosterol (15). Conclusion: All the compounds were isolated from this plant for the first time.