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Method for extracting and separating procyanidine

A technology for the separation of proanthocyanidins and peels, applied in the direction of organic chemistry, etc., can solve the problems of limited separation effect, loss of drug efficacy, increase in production cost, etc., and achieve the effects of increasing equipment efficiency, simple and easy process, and high production cost.

Inactive Publication Date: 2009-10-28
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Acidic water can degrade high-polymeric proanthocyanidins into dimers or trimers or even monomers, and then extract them. However, at the same time, it will degrade the oligomer proanthocyanidins of raw materials, and the antioxidant effect of proanthocyanidin monomers is far less than that of dimers. Body and trimer proanthocyanidins, resulting in loss of efficacy
Supercritical CO 2 And microwave-assisted means help to improve the extraction rate of proanthocyanidins, but the effect is limited, and often require harsh process conditions, which not only increases the production cost, but also causes the decomposition of some proanthocyanidins
[0005] The separation and purification of proanthocyanidins mainly contain resin adsorption or column chromatography (CN100384832C, CN 1923830A, CN 1253446C, CN 1169804C), countercurrent extraction (CN 1176919C) and membrane separation (CN 101100464A) and antisolvent method (CN1613854A), wherein Resin adsorption column chromatography and membrane separation are mainly used for some sugars in the extract, while countercurrent extraction uses the different distribution ratios of proanthocyanidins and impurities in two different solvents to achieve separation purposes. Due to different degrees of polymerization The distribution ratio of the proanthocyanidins in the two solvents is also not the same, so the separation effect is limited and the process yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) 100 grams of 10-mesh grape seed skins were mixed with NaHCO with a pH value of 9 3 1000ml of aqueous solution, extracted at 50°C for 10 hours, filtered; the filter cake was repeatedly extracted and filtered until the filtrate was nearly colorless.

[0025] (2) Combine the filtrates and concentrate to 100ml. The concentrated solution is extracted with n-butanol and separated to obtain an organic phase and an aqueous phase. After the aqueous phase is neutralized with hydrochloric acid, 100ml of methanol is added, stirred, left standing, and filtered.

[0026] (3) The filtrate was evaporated, washed with water, and dried to obtain 7 g of oligomeric proanthocyanidin product with a content of 88%. The filter cake was washed with water and dried to obtain 4 g of high poly proanthocyanidin with a content of 76%.

Embodiment 2

[0028] (1) 100 grams of 20-mesh seabuckthorn seed coats were extracted with 100 ml of NaOH-water-methanol (water:methanol=1:5, v / v) solution with a pH value of 14, extracted for 1 hour at 20° C., and filtered; The filter cake was repeatedly extracted and filtered until the filtrate was nearly colorless.

[0029] (2) Combine the filtrates and concentrate to 50ml. The concentrated solution is extracted with dichloromethane and separated to obtain an organic phase and an aqueous phase. The aqueous phase is neutralized with sulfuric acid, and 500ml of ethanol is added, stirred, left standing, and filtered.

[0030] (3) The filtrate was evaporated, washed with water and dried to obtain 7 g of oligomeric proanthocyanidin product with a content of 92%. The filter cake was washed with water and dried to obtain 8 g of high poly proanthocyanidin with a content of 72%.

Embodiment 3

[0032] (1) With 100 grams of 40 mesh grape seed skins, use Na with a pH value of 10 2 CO 3 -Water-ethanol (water:ethanol=1:0.1, v / v) solution 800ml, at 30°C, extract for 8 hours, filter; repeat the extraction and filtration of the filter cake until the filtrate is nearly colorless.

[0033] (2) Combine the filtrates and concentrate to 80ml. The concentrated solution is extracted with chloroform and separated to obtain an organic phase and an aqueous phase. The aqueous phase is neutralized with nitric acid, and 400ml of methanol is added, stirred, left standing, and filtered.

[0034] (3) The filtrate was evaporated, washed with water, and dried to obtain 6.5 g of oligomeric proanthocyanidins with a content of 86%. The filter cake was washed with water and dried to obtain 5 g of high-polymeric proanthocyanidins with a content of 80%.

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Abstract

A method for extracting and separating procyanidine comprises the steps of: separating the coat from the kernel of grape seeds or seabuckthorn seeds; crushing the seed coat into 10 meshes to 80 meshes; adding the crushed seed coat into alkali-water solution, alkali-alcohol-water solution or alkali-acetone-water solution with the pH value of 9 to 14 according to the solid-liquid ratio of 1g:1-10ml, conducting extraction for 1 hour to 10 hours at the temperature of 10 DEG C to 50 DEG C and then filtration; repeatedly extracting and filtering a filter cake until the filtrate is colorless or pale color; merging the filtrate and concentrating the filtrate till the weight of the filtrate is 0.5 time to 2 times of the weight of the seed coat raw materials; extracting the concentrated liquid with organic solvent and separating the liquid for obtaining an organic phase and a water phase; neutralizing the water phase with acid and adding methanol or ethanol with the volume of 1 time to 10 times, stirring, standing and filtrating; evaporating the filtrate, washing the obtained solid with water and then drying the solid for obtaining an oligomeric procyanidine product; and washing the filter cake with water and then drying the filter cake for obtaining the high-polymerization procyanidine. The invention has the advantages of less raw material input quantity, high product purity, high extraction rate, green environmental protection, simple process, and convenient industrial production.

Description

technical field [0001] The invention belongs to the field of natural product medicine and health care, and in particular relates to a method for separating and purifying proanthocyanidins. Background technique [0002] Oligomeric Proantho Cyanidins (OPC) is a bioflavonoid with a special molecular structure. It is currently internationally recognized as the most effective natural antioxidant for removing free radicals in the human body, and has very strong in vivo activity. Experiments have proved that OPC's ability to resist free radical oxidation is 50 times that of vitamin E and 20 times that of vitamin C, and it can be absorbed quickly and completely. It can reach the highest blood concentration in 20 minutes after oral administration, and its metabolic half-life is as long as 7 hours. Proanthocyanidins have the effects of improving blood circulation, treating diabetic retinopathy, reducing edema, whitening skin and inhibiting varicose veins. Anthocyanins have been used i...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 侯相林邓天昇齐永琴
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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