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Vacuum pulse type method of preparing dihydromyricetin

A technology of dihydromyricetin and vacuum pulsation, which is applied in the production of bulk chemicals and organic chemistry, can solve the problems of high cost, long extraction time, and low efficiency, reduce equipment requirements, shorten extraction time, and improve application prospects broad effect

Inactive Publication Date: 2014-05-07
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Solvent method is mostly used to extract dihydromyricetin from Grape dentata, but it is difficult to guarantee high extraction efficiency by conventional solvent extraction methods. Therefore, ultrasonic-assisted, microwave-assisted, bionic extraction, dynamic countercurrent extraction and other methods have been developed. Extraction methods, although these methods have improved the extraction efficiency, due to the large investment in equipment, the production cost has not significantly decreased, and the prior art cannot meet the requirements for the extraction of dihydromyricetin
[0005] The reason why the extraction efficiency of the conventional solvent method is low is that the main components of the S. dentata grape are substances such as cellulose, pectin and lignin, and the penetrability of solvents to such substances is often poor, and dihydromyricetin is The plant cell tissue with cellulose, pectin and lignin as the main components is wrapped, so there is a large mass transfer resistance during the extraction process, it is difficult for the solvent to pass through the plant cell tissue to dissolve dihydromyricetin, and the dihydromyricetin is dissolved. The solution of hydromyricetin is also difficult to release, the extraction time is long and the efficiency is low, and the residual rate of dihydromyricetin is often high
[0006] On the other hand, the purification of dihydromyricetin mostly adopts relatively complicated methods such as resin adsorption and column chromatography, which are costly, troublesome to operate, and low in yield. Dihydromyricetin requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Treatment of raw medicinal materials: Dried and crushed the raw medicinal materials Ceratodon grape to 50 mesh.

[0018] (2) Extraction of dihydromyricetin: After placing the material in the extraction tank, vacuumize the tank to extract the air in the tank and plant cells, and then inhale ethanol with a mass fraction of 6% as a solvent to reflux the material. The volume-to-mass ratio of the inhaled solvent to the material is 5.5:1, the extraction time is 3.7 hours, and the operation is repeated twice. The combined extracts are concentrated, dried and pulverized to obtain the crude extract of Snake dentata grape, and the dihydromyrica rubra in the crude extract The mass fraction of prime is 61%. The unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and the vacuum pulse is used to enhance mass transfer.

[0019] (3) Purification of dihyd...

Embodiment 2

[0021] (1) Processing of raw medicinal materials: Dried and crushed the raw medicinal materials of Snaketodon grapes to 30 mesh.

[0022] (2) Extraction of dihydromyricetin: After placing the material in the extraction tank, vacuumize the tank, extract the air in the tank and plant cells, and then inhale ethanol with a mass fraction of 60% as a solvent to reflux the material. The volume-to-mass ratio of the inhaled solvent to the material is 8:1, the extraction time is 2.5 hours, and the operation is repeated twice. The combined extracts are concentrated, dried and pulverized to obtain the crude extract of Grape dentata, and the dihydromyrica rubra in the crude extract The mass fraction of prime is 53%. The unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and the vacuum pulse is used to enhance mass transfer.

[0023] (3) Purification of dihydrom...

Embodiment 3

[0025] (1) Processing of raw medicinal materials: Dried and crushed the raw medicinal materials of Snaketodon grapes to 70 mesh.

[0026] (2) Extraction of dihydromyricetin: After placing the material in the extraction tank, vacuumize it to extract the air in the tank and plant cells, and then inhale ethanol with a mass fraction of 90% as a solvent to carry out reflux extraction of the material. The volume-to-mass ratio of the inhaled solvent to the material is 14:1, the extraction time is 1.3 hours, and the operation is repeated twice, and the combined extracts are concentrated, dried and crushed to obtain the crude extract of Snakedon grape, and the dihydromyrica rubra in the crude extract The quality fraction of prime is 74%. The unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and the vacuum pulse is used to enhance mass transfer.

[0027] (3...

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PUM

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Abstract

The invention discloses a vacuum pulse type method of preparing dihydromyricetin. The method comprises the following steps: (1) drying and crushing a raw material medicinal material ampelopsis grossedentata to 20-80 meshes; (2) carrying out vacuum pulse type reflux extraction on the material by taking 5-95% of ethanol as a solvent, combining the extracting liquor, and concentrating, drying and crushing to obtain an ampelopsis grossedentata coarse extract; and (3) removing impurities with small polarity and strong lipid solubility of the ampelopsis grossedentata coarse extract by supercritical carbon dioxide, and crystallizing the extract twice by hot water to obtain an ampelopsis grossedentata refined extract. According to the method provided by the invention, under the condition of not using resin and column chromatography, the purity of dihydromyricetin reaches 92-98%, the product yield is improved by 10-15%, and the application range is wide.

Description

technical field [0001] The invention relates to a preparation method of dihydromyricetin, in particular to a method for extracting and purifying dihydromyricetin from Eperodendron grapes by means of vacuum pulsation extraction and supercritical carbon dioxide extraction. Background technique [0002] Snake-toothed grape is a plant of the genus Vitaceae in the family Vitis genus. It is sweet, light, and cool in nature. The Yao nationality in my country often collects its tender stems and leaves, kneads them after processing, and dries them to make health-care tea for drinking. It has a history of hundreds of years. [0003] Dihydromyricetin is a kind of polyphenol-based dihydroflavonol, also known as staphylophyllin, which belongs to flavonoid compounds and is the most important and most valuable active substance in Snake dentata grape. In recent years, with the flavonoid Dihydromyricetin, as one of the most important members, has attracted more and more attention from peopl...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
CPCC07D311/32C07D311/40Y02P20/54
Inventor 姚茂君
Owner JISHOU UNIVERSITY