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Method for extracting and purifying procyanidine from waste grape seeds

A purification method and proanthocyanidin technology, applied in the direction of organic chemistry and the like, can solve problems such as the ineffective utilization of resources, and achieve the effects of low cost, good production safety and good yield

Inactive Publication Date: 2015-06-03
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some grape seeds are used for further processing to increase added value, and the rest are directly used as feed or fertilizer, and resources are not effectively used

Method used

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  • Method for extracting and purifying procyanidine from waste grape seeds
  • Method for extracting and purifying procyanidine from waste grape seeds
  • Method for extracting and purifying procyanidine from waste grape seeds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. After crushing the grape seeds, take 30g of grape seed powder and add 9 times the volume of 50% ethanol: 4% citric acid = 3:1 solvent, extract in a water bath at 40°C for 60 minutes, extract once, and cool and filter after extraction.

[0022] 2. Rotary steam at 40-50°C to the value of 1g of crude drug, ethanol precipitation with 95% ethanol, and refrigerate at 4°C for more than 12 hours;

[0023] 3. After filtering the alcohol precipitation solution, concentrate it to 1 / 8 of the filtrate, add 4 times of distilled water and mix evenly;

[0024] 4. Extract twice with n-butanol respectively, combine the extracts, and wash the extracts twice with saturated saline;

[0025] 5. Concentrate and dry the extract by rotation at 40-70° C. to obtain about 1.43 g of grape seed proanthocyanidin powder.

Embodiment 2

[0027] 1. After pulverizing the grape seeds, take 30g of grape seed powder and add 8 times the volume of 50% ethanol: 4% citric acid = 4:1 solvent, reflux extraction in a water bath at 50°C for 50min, extract once, and cool and filter after extraction.

[0028] 2. Rotary steam at 40-50°C to 1.5g crude drug value, ethanol precipitation with 95% ethanol, and refrigerate at 4°C for more than 12 hours;

[0029] 3. After filtering the alcohol precipitation solution, concentrate it to 1 / 4 of the filtrate, add 4 times of distilled water and mix evenly;

[0030] 4. Extract twice with n-butanol respectively, combine the extracts, and wash the extracts twice with saturated saline;

[0031] 5. Concentrate and dry the extract by rotating at 40-70° C. to obtain about 1.61 g of grape seed proanthocyanidin powder.

Embodiment 3

[0033] 1. After crushing the grape seeds, take 30g of grape seed powder and add 7 times the volume of 50% ethanol: 4% citric acid = 5:1 solvent, reflux extraction in a water bath at 60°C for 60min, extract once, and cool and filter after extraction.

[0034] 2. Rotary steam at 40-50°C to 1.5g crude drug value, ethanol precipitation with 95% ethanol, and refrigerate at 4°C for more than 12 hours;

[0035] 3. After filtering the alcohol precipitation solution, concentrate it to 1 / 8 of the filtrate, add 4 times of distilled water and mix evenly;

[0036] 4. Extract twice with n-butanol respectively, combine the extracts, and wash the extracts twice with saturated saline;

[0037] 5. Concentrate and dry the extract by rotating at 40-70° C. to obtain about 1.82 g of grape seed proanthocyanidin powder.

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Abstract

The invention provides a method for extracting and purifying procyanidine from waste grape seeds and discloses a process route with simpler and reasonable effects and low cost. The method comprises the following steps: carrying out water-bath reflux extraction on grape seed powder by using a solvent containing 50% alcohol and 4% citric acid at a ratio of (3:1)-(5:1) at a material-liquid ratio of (1:6)-(1:9) (m / v, the mass-volume rate), cooling, filtering, then carrying out rotary evaporation, and recovering alcohol; using the alcohol for alcohol precipitation, filtering alcohol-precipitation liquid, then concentrating, recovering alcohol, adding distilled water and uniformly mixing; extracting with normal butanol, combining extraction liquid, and cleaning the extraction liquid with saturated salt water; and carrying out rotary concentration and drying on the extraction liquid, and recovering normal butanol, thereby obtaining purpurin powder. The method provided by the invention has the following advantages that waste grape seeds in the wine brewing process are adopted as raw materials, so that not only are the wastes reasonably reutilized, but also the cost is low and the implementation benefit is obvious; alcohol is utilized for extraction, and normal butanol is utilized for extraction treatment, so that the production safety is good; alcohol and normal butanol are recovered, and are recycled, so that the cost is reduced; the product is high in purity and good in yield; and the process is simple and the industrialization is easy.

Description

technical field [0001] The invention relates to a method for extracting and purifying active ingredient proanthocyanidins from waste grape seeds, and belongs to the field of extraction and purification of plant effective ingredients. Background technique [0002] Grape seeds mainly come from the leftovers of wineries and beverage factories, accounting for 5% to 7% of the whole grape. my country is rich in grape resources. It is estimated that more than 100,000 tons of fresh grapes are used for winemaking and other industries every year. 5000-7000 tons of by-product grape seeds. Some grape seeds are used for further processing to increase added value, and the rest are directly used as feed or fertilizer, and the resources are not effectively used. [0003] Proanthocyanidins are composed of (+)-catechin, (-)-catechin and (-)-epicatechin gallate through C 4 -C 8 key or c 4 -C 6 Polyphenols with different degrees of polymerization formed by bonds are widely found in plants ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 韩静刘倩
Owner SHENYANG PHARMA UNIVERSITY
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