Chromone derivative from Cassia pumila and preparation method and application thereof
A kind of technology of stipitate lentils and derivatives, applied in the field of phytochemistry
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[0026] The preparation method of the chromone derivative 8-hydroxyl-2-(3-hydroxypropyl)-5-(isobutyryl)-4H-4-chromone of the present invention comprises crushing, extracting extract, silica gel column chromatography , high pressure liquid chromatography and gel column chromatography steps, specifically comprising:
[0027] A, extraction of extract: get the whole plant of lentil lentils, lentil lentils can be crushed or cut into small sections, and use high-concentration methanol (w%: 80% ~ 100%) or high-concentration ethanol (w%: 80%) %~100%) or high-concentration acetone (w%: 70%~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;
[0028]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 80 to 100 ...
Embodiment 1
[0034] The lentil lentils sample comes from Xinping County, Yunnan. 2.0 kg of the lentil lentils 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. 106g. The extractant is dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 120 g of 80 mesh thick silica gel, and 0.7 kg of 160 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 and merging the same fractions to obtain 6 fractions, among which the chloroform-methanol elution fraction with a volume ratio of 9:1 Separation by Shimadzu's LC-8A semi-preparative high-performance liquid chromatography, with 58% methanol as the mobile phase, Venusil MP C 18 (20×250mm, 5μm) The preparative column is a stationary phase, the flow rate is 20ml / min, the detection w...
Embodiment 2
[0036] The sample of Shandenshan lentils comes from Shuangjiang County, Yunnan Province. Take 4.0kg of Bandenshan lentils and chop them up, extract them with 95% ethanol for 4 times, each time for 48 hours, combine the extracts, filter, and concentrate under reduced pressure to form an extract. Obtain extractum 196g. After dissolving the extract with 2.0 times the amount of pure methanol by weight, mix the sample with 200g of 100-mesh silica gel, pack 1kg of 200-mesh silica gel into a column for silica gel column chromatography, and use a volume ratio of 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, wherein the chloroform-acetone elution part with a volume ratio of 9:1 was used Shimadzu's LC-8A semi-preparative high-performance liquid chromatography separation, with 58% methanol as the mobile phase, Venusil MP C 18 (20×250mm, 5μm) The preparative column is a stationary phase, the flow rate is ...
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