A kind of chromone derivative extracted from Cassia brevifolia and its preparation method and application
A technology of derivatives, chromones, applied in the field of phytochemistry
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[0027] The preparation method of chromone derivative 6-(2,2-dimethyl-2H-chromene)-2-isopropyl-8-methyl-4H-4-chromone of the present invention comprises pulverization, extract Extraction, silica gel column chromatography, high pressure liquid chromatography and gel column chromatography steps, specifically including:
[0028]A, extract extract: get the Cassia brevifolia plant of whole plant, and Cassia brevifolia can be pulverized or cut into small sections, with high-concentration methanol (w%: 85%~100%) or high-concentration ethanol (w%: 85%) %~100%) or high-concentration acetone (w%: 80%~100%) is the extraction solvent, extraction solvent: three tendons of hairy leaves (weight ratio)=2~4:1, soak for 24h~72h, extract 3~5 times, the extracts were combined, filtered and concentrated into an extract;
[0029] B. Silica gel column chromatography: the extract is dissolved with pure methanol or pure ethanol or pure acetone with a weight ratio of 1.5 to 3 times, and then mixed with...
Embodiment 1
[0035] The sample of Cassia brevifolia comes from Xishuangbanna, Yunnan. Crush 3.0 kg of the sample of Cassia brevifolia and extract it 4 times with 95% methanol for 48 hours each time. The extracts are combined, filtered, and concentrated under reduced pressure to obtain an extract 152 g . The extractant is dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 180 g of 80 mesh thick silica gel, and 0.75 kg of 160 mesh silica gel is packed into a column for silica gel column chromatography, and the volume ratio is 20:1, 9:1, 8:2, 7:3, 6:4, 5:5 chloroform-methanol gradient elution, TLC monitoring and merging the same fractions to obtain 6 fractions, among which the chloroform-methanol elution fraction with a volume ratio of 9:1 Use Agilent 1200 preparative high-performance liquid chromatography to separate, with 68% methanol as mobile phase, Zorbax SB-C18 (21.2 * 250mm, 5 μ m) preparative column is stationary phase, flow velocity is 20ml / min, and the ...
Embodiment 2
[0037] The sample of Cassia brevifolia comes from Mangshi, Yunnan. 2.0 kg of Cassia brevifolia sample is chopped and extracted 5 times with 95% ethanol for 24 hours each time. The extracts are combined, filtered, and concentrated under reduced pressure to obtain an extract. Extract 91g. The extractant is dissolved in pure methanol with a weight ratio of 2.0 times, and then the sample is mixed with 100 g of 100 mesh thick silica gel, and 0.5 kg of 200 mesh silica gel is packed for silica gel column chromatography, and the volume ratio is 20:1, 9:1, 8:2, 7:3, 6:4, 5:5 chloroform-methanol gradient elution, TLC monitoring Merge the same fractions to obtain 6 fractions, of which the volume ratio of 9:1 chloroform-acetone elution fraction Use Agilent 1200 preparative high-performance liquid chromatography to separate, with 68% methanol as mobile phase, Zorbax SB-C18 (21.2 * 250mm, 5 μ m) preparative column is stationary phase, flow velocity is 20ml / min, and the detection wavelength ...
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