Fukinanolide compounds and pharmaceutical application thereof
A technology of butterbur lactone and compounds, applied in the field of chemical structure of four new butterbur lactone compounds
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Embodiment 1
[0076]35Kg of dried leaves of Butterbur was extracted three times with ethanol under reflux, and the amount of ethanol was 5 times, 2 times, and 1 times that of the rhizome, and the extraction time was 2 hours, 1 hour, and half an hour, respectively. The extract was concentrated under reduced pressure and dissolved in water to form a suspension, which was extracted with petroleum ether and ethyl acetate to obtain petroleum ether extract and ethyl acetate extract respectively. The ethyl acetate extract was subjected to silica gel column chromatography (chromatographic silica gel 200-300 mesh, Shandong Yantai Zhifu Huangwu Silica Gel Development and Test Factory), and washed with n-hexane-ethyl acetate (8:1 to 1:1) solvent system According to thin-layer chromatography monitoring, the eluates were combined into thirteen parts. The fourth part was subjected to silica gel column chromatography, eluted with n-hexane-ethyl acetate (20:1), and the eluate was concentrated and then subjecte...
Embodiment 2
[0079] 5 kg of dry rhizomes of hairy butterbur, add 10 liters of ethanol, infiltrate 3 times. Combine the percolates and concentrate under reduced pressure to a certain volume to obtain a crude extract of total butterbur lactone. Dissolve the crude butterbur lactone extract with water, and then pass the macroporous adsorption resin (D101 type, Tianjin Zhengtiancheng Clarification Technology Co., Ltd., or other brands, such as AB-8, D4020, 860021, HP20, SP825) Etc.), rinse with water or dilute ethanol, and then rinse with concentrated ethanol, and recover the concentrated ethanol to rinse part under reduced pressure to obtain the butterbur lactone mixture. The mixture was subjected to silica gel column chromatography and eluted with petroleum ether-acetone (50-5:1) to obtain Homofukinolide (7.9 mg), butterburide-Ia (29 mg) and butterburide-IIa ( 65mg), butterbur lactone-B (1.6g), butterbur lactone-IIIa (2.8g), butterbur lactone-IVa (2.9g), butterbur lactone-D (2.6g) .
Embodiment 3
[0081] The dry rhizome of butterbur was 5Kg, extracted three times with methanol reflux, the amount of methanol was 5 times, 2 times, and 1 times that of the rhizome, and the extraction time was 2 hours, 1 hour, and half an hour, respectively. The extract was concentrated under reduced pressure and dissolved in water to form a suspension, which was extracted with petroleum ether and ethyl acetate to obtain petroleum ether extract and ethyl acetate extract respectively. The petroleum ether extract was chromatographed on silica gel column (chromatographic silica gel 200-300 mesh, Shandong Yantai Zhifu Huangwu Silica Gel Development and Test Factory), and eluted with a gradient of n-hexane-ethyl acetate (20:1 to 1:1). The compounds butterburide A (6.1mg), Homofukinolide (6.9mg), butterburide-Ia (5mg) and butterburide-IIa (6.3mg), butterburide-Fa were sequentially obtained (6.2mg), butterbur lactone-Fb (26.9 mg), butterbur lactone-I (14.3 mg), butterbur lactone-J (7.2 mg), butterbur l...
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