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Method for extracting procyanidine from grape seeds

A proanthocyanidin and grape seed technology, applied in the direction of organic chemistry, can solve the problems of proanthocyanidin composition, many dissolved impurities, and long extraction time, so as to save the purification of macroporous adsorption resin, and the subsequent purification steps are simple and avoid Effects of prolonged exposure

Active Publication Date: 2015-04-22
内蒙古昶辉生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These extraction methods mainly have the following disadvantages: (1) the water extraction method uses water as the extraction agent, and the soaking time is long and the temperature is high, which easily causes the loss of proanthocyanidins. At the same time, the polarity of water is large and there are many dissolved impurities; Organic solvent extraction is time-consuming and costly, and has a great influence on the composition of proanthocyanidins; (3) Supercritical CO 2 The extraction method is costly and requires harsh operating conditions
[0004] Common methods for purifying proanthocyanidins crude products in this field include methods such as macroporous adsorption resin, HPLC, membrane filtration, recrystallization, etc., but the above-mentioned purification methods all consume a large amount of solvents

Method used

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  • Method for extracting procyanidine from grape seeds
  • Method for extracting procyanidine from grape seeds
  • Method for extracting procyanidine from grape seeds

Examples

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Effect test

Embodiment 1

[0023] The degreased grape seeds were crushed to 60 mesh, 100 g was weighed and 1200 g of ethyl acetate was added, and ultrasonic treatment was performed at a frequency of 80 kHz and a power of 250 W for 30 min. Grape seed particles are filtered out, the filtrate is concentrated under reduced pressure and ethyl acetate is recovered to obtain a crude extract , the crude extract Store at low temperature and avoid light; add 1000g of purified water to grape seed granules, add 8g of cellulase, enzymolyze at 45°C for 40min, and perform ultrasonic treatment for 5min every 10min, ultrasonic frequency 80kHz, power 250W; Add 1000 g of ethyl acetate to the solution, and extract with the same ultrasonic conditions as above for 30 min. Separate the ethyl acetate layer afterwards, concentrate under reduced pressure, reclaim ethyl acetate, the crude extract obtained Store at low temperature and avoid light; adjust the pH of the remaining aqueous solution containing grape seed particles...

Embodiment 2

[0025] The degreased grape seeds were crushed to 80 mesh, 200 g was weighed and 2000 g of ethyl acetate was added, and ultrasonic treatment was performed at a frequency of 80 kHz and a power of 250 W for 40 min. Grape seed particles are filtered out, the filtrate is concentrated under reduced pressure and ethyl acetate is recovered to obtain a crude extract , the crude extract Store at low temperature and avoid light; add 2000g of purified water to grape seed granules, add 12g of cellulase, enzymolyze at 40°C for 40min, and perform ultrasonic treatment for 5min every 10min, ultrasonic frequency 80kHz, power 250W; Add 2000 g of ethyl acetate to the solution, and extract for 40 min under the same ultrasonic conditions as above. Separate the ethyl acetate layer afterwards, concentrate under reduced pressure, reclaim ethyl acetate, the crude extract obtained Store at low temperature and avoid light; adjust the pH of the remaining aqueous solution containing grape seed particl...

Embodiment 3

[0027] The degreased grape seeds were crushed to 50 mesh, 100 g was weighed and added into a closed container and 1200 g of ethyl acetate was added, filled with nitrogen, and ultrasonically treated at a frequency of 80 kHz and a power of 250 W for 40 min. Grape seed particles are filtered out, the filtrate is concentrated under reduced pressure and ethyl acetate is recovered to obtain a crude extract , the crude extract Store at low temperature and avoid light; add 1000g of purified water and 10g of cellulase to the filtered grape seed particles, place in a closed container and fill with nitrogen, enzymatically hydrolyze at 45°C for 40min, and perform ultrasonic treatment for 5min every 10min. Ultrasonic frequency 80kHz, power 250W; add 1000g ethyl acetate to the solution after enzymatic hydrolysis, and extract under the same ultrasonic conditions for 40min. Separate the ethyl acetate layer afterwards, concentrate under reduced pressure, reclaim ethyl acetate, the crude ext...

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Abstract

The invention aims at providing a method for extracting oligomeric procyanidine from grape seeds. The method comprises the following steps: pulverizing defatted grape seeds, adding ethyl acetate and carrying out ultrasonic extraction to obtain a crude extract (shown in the specification), adding cellulose for enzymolysis, extracting twice with ethyl acetate to respectively obtain a crude extract (shown in the specification) and another crude extract (shown in the specification), mixing the crude extracts and purifying to obtain oligomeric procyanidine of which the purity is above 95%. According to the method, by many rounds of extraction and low-temperature preservation of extracts in a dark place, the long-term exposure of oligomeric procyanidine is avoided and thus the oxidation of oligomeric procyanidine and the degradation of excessive procyanidine into inactive monomers are decreased; the subsequent purification process steps of the method disclosed by the invention are simpler, the conventional steps of purifying with macroporous adsorption resin, HPLC refining and the like in the field are omitted, a large amount of solvents are saved and environment friendliness is achieved.

Description

technical field [0001] The application relates to a method for extracting proanthocyanidins from grape seeds. Background technique [0002] Proanthocyanidins are flavan-3-ol monomers connected by C4-C8 or C4-C6 to form a certain degree of polymerization. The basic units are mainly catechin, epicatechin and epicatechin gallate, etc. . According to the degree of polymerization, two to five polymers are usually referred to as oligomers (referred to as OPC), and more than pentamers are referred to as high polymers (referred to as PPC). This polyphenolic compound is widely found in grapes, blueberries, cherries, pine bark and other plants. Proanthocyanidin is a natural free radical scavenger and antioxidant. It has anti-aging, anti-tumor, prevention of cardiovascular and cerebrovascular diseases, prevention of atherosclerosis, and improvement of skin elasticity. It has been widely used in food, medicine and cosmetics, etc. field. [0003] At present, the methods for extractin...

Claims

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Application Information

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IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 马亚琼万润丽白易张成亮
Owner 内蒙古昶辉生物科技股份有限公司
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