Flavonoid compound and preparation method and application thereof
A technology of flavonoids, compounds, applied in the field of phytochemistry
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[0027] The preparation method of the flavonoid compound of the present invention is based on Cassia brevifolia ( Cassia leschenaultiana DC.) as a raw material, prepared through extract extraction, silica gel column chromatography, high pressure liquid chromatography separation and gel column chromatography steps, specifically comprising the following steps:
[0028] A, extract extract: take raw material Cassia brevifolia ( Cassia leschenaultiana DC. ), using the whole plant as raw material or crushed and cut into small sections, adding 2 to 4 times the weight of the raw material in an organic solvent with a mass concentration of 70 to 100%, soaking and extracting for 24 to 72 hours, extracting for 3 to 5 times, combining the extracts, filtering Concentrate into an extract;
[0029] B. Silica gel column chromatography: use 150~200 mesh silica gel dry method packing 2~5 times the weight of the extract for silica gel column chromatography, and use chloroform-methanol solution...
Embodiment 1
[0040] The sample of Cassia brevifolia came from Yuanjiang, Yunnan. 2.0 kg of Cassia brevifolia sample was crushed and extracted 5 times with 95% methanol for 24 hours each time. The extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract 98 g. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 120 g of 80-mesh crude silica gel, and 0.6 kg of 160-mesh silica gel was packed into a column for silica gel column chromatography, and the volume ratio was 20:1, 9:1. , 8:2, 7:3, 6:4, 5:5 chloroform-methanol gradient elution, TLC monitoring and merging the same parts to obtain 6 parts, in which the volume ratio of 8:2 chloroform-methanol elution A part was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 60% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm ) The preparative column is a stationary phase, the flow rate is 20 ml / min, the detection wavel...
Embodiment 2
[0042] The sample of Cassia brevifolia comes from Lincang, Yunnan. A 4.0kg sample of Cassia brevifolia was chopped and extracted 4 times with 95% ethanol for 48 hours each time. The extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract. Extract 181 g. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 200 g of 100-mesh crude silica gel, and 1.0 kg of 200-mesh silica gel was packed into a column for silica gel column chromatography, and the volume ratio was 20:1, 9:1 , 8:2, 7:3, 6:4, 5:5 chloroform-methanol gradient elution, TLC monitoring and merging the same parts to obtain 6 parts, in which the volume ratio of 8:2 chloroform-acetone elution A part was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 60% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 mu m) The preparative column is a stationary phase, the flow rate is 20 ml / min, the detect...
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