A kind of ketone compound and its preparation method and application
A technology for koushan ketone and compound, which is applied in the field of koushan ketone compound and its preparation, and achieves the effects of simple extraction method, good antibacterial activity and easy industrial production.
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[0029] The preparation method of the mountain ketone compound described in the present invention is to use the black and purple swertia as raw material, through the steps of extraction from extract, silica gel column chromatography, and high pressure liquid chromatography, specifically:
[0030] A. Extraction of extract: use black purple water swert as raw material, crush black purple water swert or cut into small pieces, soak in organic solvent for 24 h to 72 h, extract 3 to 5 times, combine extracts, filter, reduce compressed and concentrated into extract;
[0031] B. Silica gel column chromatography: the extract is dry-packed with 160-300 mesh silica gel column with a weight ratio of 2 to 4 times for silica gel column chromatography; gradient elution is carried out with chloroform-acetone solution, and the same parts are combined and collected. Part of the eluate was concentrated;
[0032] C. Separation and purification by high-pressure liquid chromatography: the 7:3 part ...
Embodiment 1
[0044] Tobacco samples were from Lijiang, Yunnan. Sampling 2.0 kg of Swertia japonica was crushed and extracted 5 times with 95% methanol for 24 h each time. The extracts were combined, filtered, concentrated under reduced pressure to obtain an extract, and 105 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 120 g of 100-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 1:0, 20:1 , 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same parts to obtain 8 parts, wherein the volume ratio is 7 The chloroform-acetone eluted part of :3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 50% methanol as mobile phase, Zorbax SB-C18 (21.2×250 mm, 5 μ m ) The preparative column is a stationary phase, the flow rate is 20 ml / min, and ...
Embodiment 2
[0046] The sample of black and purple water swert came from Shangri-La, Yunnan. 3.5 kg of black and purple water swert was chopped and extracted four times with 95% ethanol for 48 hours each time. The extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract. , to obtain extract 250 g. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 250 g of 80-mesh crude silica gel, and 1.2 kg of 200-mesh silica gel was packed into a column for silica gel column chromatography, and the volume ratio was 1:0, 20:1 , 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same parts to obtain 8 parts, wherein the volume ratio is 7 The chloroform-acetone elution part of :3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) preparative column as stationary phase, The...
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