Chalcone compounds and preparation method and application thereof.
A kind of compound, technology of chalcone, applied in the field of chalcone compound and preparation thereof
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[0026] Chalcone compound C of the present invention 20 h 20 o 5 The preparation method comprises extract extraction, silica gel column chromatography, high-pressure liquid chromatography separation steps, specifically comprises:
[0027] A. Extraction of extract: take a sample of the leech locust, crush it to 20-40 mesh, use 90-99% methanol to ultrasonically extract 3-5 times, each time for 30-60 min, combine the extracts, filter, and concentrate under reduced pressure to obtain extract;
[0028] B. Silica gel column chromatography: the extract is packed with 160~200 mesh silica gel dry method with a weight ratio of 2~3 times for silica gel column chromatography; chloroform-acetone solution with a volume ratio of 1:0~1:2 Perform gradient elution, pool the same fractions, collect and concentrate the eluate from each fraction;
[0029] C. High-pressure liquid chromatography separation: the 8:2 part of the eluent in step B is further separated and purified by high-pressure li...
Embodiment 1
[0038] The samples of leech leech came from Xishuangbanna, Yunnan. Sampling 2.2 kg of the leech locust was crushed to 30 mesh, extracted 3 times with 95% methanol by ultrasonic, 30 min each time, the extracts were combined, filtered, concentrated under reduced pressure to obtain an extract, 88.5 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 2.5 times, and then mixed with 120 g of 100-mesh crude silica gel, and 1.5 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 8 The chloroform-acetone elution part of :2 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 58% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) preparative column as stationary phase, Th...
Embodiment 2
[0040] The leech leech sample comes from Dehong, Yunnan. 3.5 kg of the leech leech was crushed to 40 meshes, extracted 5 times with 90% methanol by ultrasound, 45 min each time, the extracts were combined, filtered, and concentrated under reduced pressure into an extract, and 158 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 300 g of 80-mesh crude silica gel, and 1.5 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 8 The chloroform-acetone elution part of :2 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 58% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) preparative column as stationary phase, The flow rate was 2...
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