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High-purity resveratrol preparation method

A resveratrol, high-purity technology, applied in the field of preparation of high-purity resveratrol, can solve the problems of long production cycle, poor solvent penetration, long extraction time, etc., to reduce raw material processing costs, The effect of shortening the extraction time and increasing the extraction rate

Active Publication Date: 2014-04-02
江苏桂柳牧业集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been many reports on the process of extracting resveratrol from Polygonum cuspidatum. Since most of the resveratrol in Polygonum cuspidatum exists in the form of resveratrol glycosides, the existing resveratrol production process generally first passes Microbial fermentation converts resveratrol glycosides (also known as polydatin) into resveratrol and then extracts it. Since microorganisms convert resveratrol and produce more sugars, the viscosity of the material increases and the extraction During the process, the penetrability of the solvent becomes poor, resulting in low extraction rate and long extraction time; most of the purification after extraction of resveratrol requires the use of chloroform, and it is loaded on the column twice, and the resveratrol content is 20% and 50% of the two intermediate product links, so the product production cycle is long, the loss is large, the cost is high, and there is also the risk of toxic and harmful organic solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Treatment of raw medicinal materials: beat or pulverize the medicinal materials of Polygonum cuspidatum.

[0017] (2) Extraction and concentration of active ingredients: Use 35% ethanol as the solvent, and the volume-to-mass ratio of the solvent to the raw medicinal materials is 8:1 for dynamic countercurrent extraction in a tank group. The extraction time is 6.5 hours, and the extraction temperature is 45°C. The extraction is completed Afterwards, concentrate under reduced pressure until there is no alcohol smell, and set aside for later use. During the above extraction process, the extraction tank is vacuumed and broken intermittently, and the mass transfer is enhanced by vacuum pulsation.

[0018] (3) Enzymolysis: Add a compound enzyme preparation of 3 / 1000 of the medicinal material for enzymolysis. The enzymolysis time is 9 hours, the enzymolysis temperature is 45°C, and the enzymolysis process is continuously stirred. After the enzymolysis is completed, it is co...

Embodiment 2

[0021] (1) Treatment of raw medicinal materials: beat or pulverize the medicinal materials of Polygonum cuspidatum.

[0022] (2) Extraction and concentration of active ingredients: Use 82% ethanol as the solvent, and the volume-to-mass ratio of the solvent to the raw medicinal materials is 11:1 for dynamic countercurrent extraction in a tank group. The extraction time is 9.5 hours, and the extraction temperature is 72°C. The extraction is completed Afterwards, concentrate under reduced pressure until there is no alcohol smell, and set aside for later use. During the above extraction process, the extraction tank is vacuumed and broken intermittently, and the mass transfer is enhanced by vacuum pulsation.

[0023] (3) Enzymolysis: add a compound enzyme preparation of 7 / 1000 of the medicinal material for enzymolysis. The enzymolysis time is 6.2 hours, the enzymolysis temperature is 53°C, and the enzymolysis process is continuously stirred. After the enzymolysis is completed, it is...

Embodiment 3

[0026] (1) Treatment of raw medicinal materials: beat or pulverize the medicinal materials of Polygonum cuspidatum.

[0027] (2) Extraction and concentration of active ingredients: use 70% ethanol as the solvent, and the volume-to-mass ratio of the solvent to the raw medicinal material is 14:1 for dynamic countercurrent extraction in a tank group. The extraction time is 7.9 hours, and the extraction temperature is 60°C. The extraction is completed Afterwards, concentrate under reduced pressure until there is no alcohol smell, and set aside for later use. During the above extraction process, the extraction tank is vacuumed and broken intermittently, and the mass transfer is enhanced by vacuum pulsation.

[0028] (3) Enzymolysis: Add a compound enzyme preparation of 5 / 1000 of the medicinal material for enzymolysis. The enzymolysis time is 14 hours, the enzymolysis temperature is 38°C, and the enzymolysis process is continuously stirred. After the enzymolysis is completed, it is c...

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Abstract

The invention discloses a high-purity resveratrol preparation method which comprises (1) pulping or crushing a bulk drug polygonum cuspidatum; (2) taking 30%-90% ethyl alcohol as a solvent to conduct pot group type dynamic countercurrent extraction, conducting vacuum concentration after extraction until no alcohol flavor exists, and keeping the mixture for later use; (3) adding a complex enzyme preparation to conduct enzymolysis, and concentrating and filtering after enzymolysis to obtain a crude product; (4) extracting the obtained crude product by using methyl alcohol, drying the extract to obtain a by-product rheum emodin, and enabling the extract liquor to be subjected to alumina column alumina column chromatography, methyl alcohol analysis, concentration, gasoline washing, activated carbon decoloration, ethyl alcohol crystallization and drying to obtain the high-purity resveratrol. According to the invention, extraction and then enzymolysis are conducted to convert the polygonin, so that the conversion time is shortened, the adoption of the dynamic countercurrent and the combination of vacuum pulse improve the extraction rate, the environment protecting production of the resveratrol with short period, less steps and low loss is implemented, and the application prospect is wide.

Description

technical field [0001] The invention relates to a method for preparing high-purity resveratrol, in particular to a method for extracting and purifying resveratrol from Polygonum cuspidatum and obtaining by-product emodin. Background technique [0002] Polygonum cuspidatum is a perennial vine belonging to the family Polygonaceae, widely distributed in East China, Central South and Liaoning, Shaanxi, Gansu, Sichuan, Yunnan and other places. Scholars at home and abroad have done a lot of research on the chemical composition of Polygonum cuspidatum, and found that its rhizome contains a polyhydroxy stilbene compound——resveratrol, that is, 3,4,5-trihydroxystilbene, which belongs to tannin polyphenols. It has important regulatory effects on the human body such as lowering blood fat, antithrombotic, preventing arteriosclerosis, and enhancing immune function. It is widely used in pharmaceutical intermediates, food additives, health food and other fields. After decades of developmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P7/22C07C50/34C07C46/10
Inventor 李志平
Owner 江苏桂柳牧业集团有限公司
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