Method for preparing high-purity resveratrol from fresh giant knotweed rhizome

A resveratrol, high-purity technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult recovery of reagents, long cycle, low degree of industrialization, etc., to improve the efficiency of enzymatic hydrolysis and product content, reduce the loss of polydatin, and improve the effect of product yield

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the biological enzymatic hydrolysis uses Polygonum cuspidatum to break up and humidify, add biological enzymes, and place it for enzymatic hydrolysis. This process takes a long time
There is also alcohol extraction and enzymatic hydrolysis, and the recovery of reagents causes energy waste and high cost
There are also alkaline water extraction enzymatic hydrolysis and the application of microwave and ultrasonic auxiliary equipment, and the extraction rate is greatly improved. For example, "Chemical Industry and Engineering" published "Cellulase-Microwave Extraction of Resveratrol in Polygonum cuspidatum" in 2008-Volume 25, No. 5 In the literature, a large amount of polysaccharides are dissolved out during the extraction process using microwave extraction method, resulting in an increase in the amount of enzymes used and an increase in cost.
High-purity resveratrol is also mostly prepared by organic reagent extraction and column chromatography methods, such as Chinese Patent Authorization No. CN1090603C "A new method for extracting and purifying resveratrol from Polygonum cuspidatum". In the disclosed method, the Ethyl acetate extraction method; Another example is the Chinese patent authorization number CN1269831C "new preparation method of polydatin and resveratrol". In the disclosed method, procedures such as polyamide chromatography and activated carbon decolorization are used. These methods cause difficulties in reclaiming reagents, Long cycle, low yield, low degree of industrialization

Method used

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  • Method for preparing high-purity resveratrol from fresh giant knotweed rhizome
  • Method for preparing high-purity resveratrol from fresh giant knotweed rhizome

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Crush fresh Polygonum cuspidatum to 30 mesh, take 10kg (Polycoside content 2.48% resveratrol content 0.6%), add it to 40L saturated lime aqueous solution, heat to 80℃, keep for 1 hour, filter the extract, and repeat the extraction once. The combined extracts were adjusted to pH 7 with hydrochloric acid, filtered and added to an ultrafiltration membrane with a molecular weight cut-off of 1000-3000, and the permeate was collected. The permeate was then concentrated by a nanofiltration membrane with a molecular weight cut-off of 100-200 to collect 40L of concentrate. , Adjust the pH to 4.5 with hydrochloric acid, heat to 50°C, add 10 grams of β-glucosidase and stir evenly, keep warm for 9 hours, concentrate the enzymatic hydrolysate, filter and dry to obtain 280 grams of crude resveratrol content 70% . The crude resveratrol is saturated and dissolved in 90% ethanol reflux, placed at room temperature and added to a neutral alumina column to adsorb impurities, collect the col...

Embodiment 2

[0044] Crush fresh Polygonum cuspidatum to 40 mesh, take 10kg (Polycoside content 2.3% resveratrol content 0.4%), add it to 60L saturated lime aqueous solution, heat to 60℃, keep for 1 hour, filter the extract and repeat the extraction twice , The combined extract is adjusted to pH 8 with hydrochloric acid, filtered and added to an ultrafiltration membrane with a molecular weight cut-off of 1000-3000, and the permeate is collected. The permeate is then concentrated by a nanofiltration membrane with a molecular weight cut-off of 100-200 to collect 50L of the concentrated solution. . Adjust the pH to 5 with sulfuric acid, heat to 45°C, add 8 grams of cellulase and stir evenly, keep warm for 11 hours, concentrate the enzymatic hydrolysate, filter and dry to obtain 225 grams of crude resveratrol content 72%. The crude resveratrol is saturated and dissolved in 95% ethanol under reflux, placed at room temperature and added to a neutral alumina column to adsorb impurities, collect the ...

Embodiment 3

[0046] Crush fresh Polygonum cuspidatum to 60 mesh, take 10kg (Polycoside content 2.5% resveratrol content 0.7%), add it to 50L saturated lime aqueous solution, heat to 80℃, keep for 1.5 hours, filter the extract, and repeat the extraction once. The combined extracts were adjusted to pH 7.5 with sulfuric acid, filtered and added to an ultrafiltration membrane with a molecular weight cut-off of 1000 to 3000, the permeate was collected, and the permeate was concentrated by a nanofiltration membrane with a molecular weight cut-off of 100-200 to collect 50L of the concentrate. , Adjust the pH to 5 with hydrochloric acid, heat to 55°C, add 10 grams of amylase and stir evenly, keep the enzyme for 12 hours, concentrate the hydrolysate, filter and dry to obtain 288 grams of crude resveratrol content of 71%. The crude resveratrol is saturated and dissolved with 90% ethanol reflux, placed at room temperature and added to a neutral alumina column to adsorb impurities, collect the column li...

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Abstract

Then invention relates to a method for preparing resveratrol, which comprises: fresh giant knotweed rhizome is taken as the raw material; after being grinded, the fresh giant knotweed rhizome is heated and soaked by saturation lime water solution for extraction; the pH of extraction liquid can be adjusted; macromolecule purities are removed by adopting an ultra-filtration membrane; the solution is concentrated by adopting a nano-filtration membrane; biological enzyme is added into the concentrated solution for heat preservation and enzymolysis for 9-12h; the obtained crude product can be dissolved by ethanol; the impurities in the crude product are removed by adopting alumina resin; and then water can be added in the crude product for crystallization. The product prepared by adopting the method has the advantages of high content, high yield and low cost. The process is easy to be enlarged and industrialized.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity resveratrol from fresh Polygonum cuspidatum, in particular to a method for preparing resveratrol by adopting membrane separation, biological enzymatic hydrolysis, alumina adsorption and other procedures. Background technique: [0002] Resveratrol [0003] Alias: Polygonum cuspidatum [0004] Chemical name: (E)-5-[2-(4-hydroxyphenyl)-vinyl]-1,3-benzenediol; 3,5,4″-trihydroxystilbene; stilbene triphenol; Trans-3 -4′-trihydroxystilbene [0005] Molecular formula: C 14 H 12 O 3 [0006] Molecular weight: 228.25 [0007] Molecular Structure: [0008] [0009] Physical properties: odorless, white crystalline powder; insoluble in water, easily soluble in organic solvents such as ethanol and acetone. [0010] Resveratrol is a natural antioxidant that can reduce blood viscosity, inhibit platelet coagulation and vasodilation, keep blood flowing, prevent the occurrence and development of cancer, and has anti-atheros...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P7/22C07C39/21C07C37/82
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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