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Method for rapidly extracting high-purity dihydromyricetin in ampelopsis grossedentata leaves

A technology for dihydromyricetin from grape leaves and dihydromyricetin, which is applied in the field of efficient extraction of dihydromyricetin, can solve the problems of high cost, many organic solvents, and many soluble impurities, and achieve the reduction of soluble impurities, convenient operation, and high process efficiency. simple effect

Inactive Publication Date: 2014-02-05
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature and patent documents mostly use hydrothermal extraction and alcohol-water extraction methods, combined with crystallization, column chromatography and other impurity removal processes, first extraction and then purification, with relatively many steps, and the soluble impurities (polysaccharides, protein, amino acid, etc.), which need to be removed by chromatography, which consumes a lot of organic solvents and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for rapidly extracting high-purity dihydromyricetin from the leaves of Snake-dentatum grape, which comprises the following steps:

[0026] (1) Take the dried leaves of Grape dentatus and crush them to 10-20 meshes;

[0027] (2) Take 1.0 g of the prepared crushed leaves, wrap them with filter paper, put them into 100 mL of water, and soak them at room temperature for 6 hours;

[0028] (3) Take out the material bag, drain, add water at a mass-volume ratio of 1:25 (g / mL), extract at 95°C for 60 minutes, and separate the extract while it is hot;

[0029] (4) Cool the extract to promote crystallization, and filter to obtain 254 mg of crude product;

[0030] (5) Add boiling water until the crude product is completely dissolved, cool to crystallize, filter off the mother liquor, and obtain 144 mg of the product.

[0031] The above-mentioned filter paper is a medium-speed analysis filter paper, and the above-mentioned dried leaves are detected by HPLC, and the conten...

Embodiment 2

[0035] A method for rapidly extracting high-purity dihydromyricetin from the leaves of Snake-dentatum grape, which comprises the following steps:

[0036] (1) Take the fresh leaves of Snake-toothed Grape and cut them into 1-2mm pieces;

[0037] (2) Take 100g of the prepared crushed leaves and put them into 8L of water, soak at room temperature for 6 hours;

[0038] (3) Filter out the washing solution, add 2.5L water to extract at 95°C for 60 minutes, and separate the extract while it is hot;

[0039] (4) Cool the extract to promote crystallization, and filter to obtain 9.14 g of crude product;

[0040] (5) Add boiling water until the crude product is completely dissolved, cool to crystallize, filter off the mother liquor, and obtain 4.71g of the product.

[0041] The above-mentioned fresh leaves are leaves or young leaves in the vegetative stage with no more than two days of picking and no loss of too much water; the soaking solution can also be used for soaking in step (2),...

Embodiment 3

[0046] A method for rapidly extracting high-purity dihydromyricetin from the leaves of Snake-dentatum grape, which comprises the following steps:

[0047] (1) Take the dried leaves of Grape dentatus and crush them to 10-20 meshes;

[0048] (2) Put 100g of crushed leaves into 10L of water and soak for 6 hours at room temperature;

[0049] (3) Filter out the washing solution, add 2.5L solvent to extract at 95°C for 60 minutes, and separate the extract while it is hot;

[0050] (4) Cool the extract to promote crystallization, and filter to obtain 26.155 g of crude product;

[0051] (5) Add boiling water until the crude product is completely dissolved, cool to crystallize, filter off the mother liquor, and obtain 13.097g of the product.

[0052] The above-mentioned soaking solution can also be used for soaking in step (2), and the mother liquor can also be used for recrystallization in step (5); the above-mentioned dried leaves are detected by HPLC, and the content of dihydromyric...

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Abstract

The invention discloses a method for rapidly extracting high-purity dihydromyricetin in ampelopsis grossedentata leaves. The method comprises the following steps of (1) smashing dried leaves into 10-20 mesh; (2) immersion cleaning: putting into water and steeping for 6 hours at normal temperature, wherein the massic volume ratio of the material and liquid is 1:100(g / mL); (3) extracting: adding water again, extracting for 60 minutes at 95 DEG C, and separating the heat extracting solution, wherein the massic volume ratio of the material and the liquid is 1:25(g / mL); (4) crystallizing: cooling the extracting solution through refrigeration or at room temperature, promoting crystallization at 4-10 DEG C, filtering, thus obtaining crude product; and (5) recrystallizing: adding boiling water till the crude product is dissolved completely, recrystallizing, filtering mother liquid, thus obtaining the product. In step (1), if the raw material is fresh leaves, the fresh leaves need to be cut into pieces of 1-2mm, in step(2), the massic volume ratio of material and liquid for immersion cleaning is 1:80(g / mL). According to the method, the requirement on rapid preparation of high-purity dihydromyricetin product can be met through steps of immersion cleaning for once, extracting for once, and recrystallizing for once.

Description

technical field [0001] The invention belongs to a method for extracting components of traditional Chinese medicines, in particular to a method for efficiently extracting dihydromyricetin from Eperodendron grapes. [0002] Background technique [0003] Snake Grape ( Ampelopsis grossedentata (Hand.-Mazz.) W. T. Wang) belongs to the genus Vitaceae, mainly distributed in the mountainous areas of South China at an altitude of 200-1000 meters, and widely distributed in Fujian, Jiangxi, Hunan, Guangdong, Guangxi, Hubei, Guizhou and other provinces. The stem is slightly cylindrical, with a diameter of 0.5-3mm, the surface is yellow-green to yellow-brown, with longitudinal ribs, brittle, and the section is slightly fibrous; the leaves are oblong, narrowly rhomboid, rhombic-ovate or lanceolate, long 2 to 5 cm, 1 to 2 cm wide, with serrated edges and cuneate base. Folk drinking practice and scientific research results show that the snake grape has the functions of clearing away hea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40C07D311/32
CPCC07D311/32C07D311/40
Inventor 余正文王家胜张妮何磊磊玉秋萍孔琪
Owner GUIZHOU NORMAL UNIVERSITY
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