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Preparation method of 2',4',6'-trihydroxychalcone

A technology of trihydroxychalcone and acetone, which is applied in the 2' field to achieve the effect of large processing capacity, short process flow and high separation efficiency

Inactive Publication Date: 2012-08-22
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching, there is no relevant research report on the extraction and separation of 2', 4', 6'-trihydroxychalcone from Hongguoshan pepper. Modern pharmacological studies have shown that 2', 4', 6'-trihydroxychalcone Has a variety of pharmacological effects, and the research prospect is very broad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 1 kg of the bark of Peppercorns chinensis, crush it, extract it by ethanol cold immersion, concentrate the extract under reduced pressure to obtain an extract, add 4 / 3 (V / V) acetone and appropriate amount of dipotassium hydrogen phosphate to the extract, mix well, The mass of dipotassium hydrogen phosphate in the formed aqueous two-phase extraction system accounted for 20% of the total volume of the liquid, and was allowed to stand at room temperature for 4 hours to be divided into upper and lower phases. The acetone phase rich in chalcone was taken out, mixed with 3% sodium chloride solution, then extracted with dichloromethane, the organic phase rich in chalcone was separated and concentrated under reduced pressure, and the concentrated extract was vacuum-dried to obtain 2 ', 4', 6'-trihydroxychalcone crude product, disperse the crude product with an appropriate amount of methanol, take 1 / 5 of the silica gel to mix the sample, evaporate the methanol, place the mix...

Embodiment 2

[0015] Take 1 kg of the bark of Peppercorns chinensis, crush it, extract it by ethanol cold immersion, concentrate the extract under reduced pressure to obtain an extract, add 1 / 3 (V / V) acetone and appropriate amount of dipotassium hydrogen phosphate to the extract, mix well, The mass of dipotassium hydrogen phosphate in the formed aqueous two-phase extraction system accounts for 10% of the total volume of the liquid, and it is allowed to stand at room temperature for 2 hours to be divided into upper and lower phases. The acetone phase rich in chalcone was taken out, mixed with 3% sodium chloride solution, then extracted with dichloromethane, the organic phase rich in chalcone was separated and concentrated under reduced pressure, and the concentrated extract was vacuum-dried to obtain 2 ', 4', 6'-trihydroxychalcone crude product, disperse the crude product with an appropriate amount of methanol, take 1 / 5 of the silica gel to mix the sample, evaporate the methanol, place the mi...

Embodiment 3

[0017] Take 10kg of the bark of Peppercorns hongguoshan, crush it, extract it by ethanol cold immersion, concentrate the extract under reduced pressure to obtain an extract, add 2 / 3 (V / V) acetone and appropriate amount of dipotassium hydrogen phosphate to the extract, mix well, The mass of dipotassium hydrogen phosphate in the formed aqueous two-phase extraction system accounted for 15% of the total volume of the liquid, and was allowed to stand at room temperature for 3 hours to be divided into upper and lower phases. The acetone phase rich in chalcone was taken out, mixed with 3% sodium chloride solution, then extracted with dichloromethane, the organic phase rich in chalcone was separated and concentrated under reduced pressure, and the concentrated extract was vacuum-dried to obtain 2 ', 4', 6'-trihydroxychalcone crude product, disperse the crude product with an appropriate amount of methanol, take 1 / 5 of the silica gel to mix the sample, evaporate the methanol, place the m...

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PUM

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Abstract

The invention relates to a preparation method of 2',4',6'-trihydroxychalcone, which is technically characterized by comprising the following steps: taking Lindera erythrocarpa bark, crushing, extracting by quenching with ethanol, concentrating the extracting solution to obtain an extract, proportionally adding an acetone-dipotassium hydrogen phosphate double-water-phase system, evenly mixing, dividing into an upper phase and a lower phase, taking out the chalcone-enriched acetone phase, adding an inorganic salt solution, evenly mixing, extracting with dichloromethane, separating the chalcone-enriched organic phase, concentrating under reduced pressure, carrying out vacuum drying on the concentrated extract to obtain a crude 2',4',6'-trihydroxychalcone product, passing the crude product through a silicagel column, eluting with dichloromethane-methanol ((65-80:(20-35)), concentrating and drying the eluate to obtain coarse crystals, and finally, recrystallizing with benzene to obtain the high-purity 2',4',6'-trihydroxychalcone. The invention has the advantages of high economy and high extraction rate, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a preparation method of 2', 4', 6'-trihydroxychalcone. Background technique [0002] Hongguoshan pepper, scientific name: Lindera erythrocarpa Makino, a plant of the genus Pepper in the family Lauraceae, is produced in Shaanxi, Henan, Shandong, Jiangsu, Anhui, Zhejiang, Jiangxi, Hubei, Hunan, Fujian, Taiwan, Guangdong, Guangxi, Sichuan and other provinces and regions, and is rich in resources. [0003] 2’,4’,6’-Trihydroxychalcone, CAS No.: 4197-97-1, yellow needle crystal, mp.176-178°C (benzene). Molecular formula: C 15 h 12 o 4 , molecular weight: 256.26, molecular structure formula: [0004] . [0005] At present, most of the research on Peppercorns hongguo focuses on the related research of its volatile oil. There are literatures that analyze the components of the volatile oils in the leaves and fruit parts of Peppercorns hongguo. After searching, there is no relevant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/835C07C45/78
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH