CN109096054A - A kind of biological extraction process of resveratrol - Google Patents
A kind of biological extraction process of resveratrol Download PDFInfo
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- CN109096054A CN109096054A CN201810917783.8A CN201810917783A CN109096054A CN 109096054 A CN109096054 A CN 109096054A CN 201810917783 A CN201810917783 A CN 201810917783A CN 109096054 A CN109096054 A CN 109096054A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
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Abstract
The invention discloses and a kind of resveratrol biological extraction process, be related to effective ingredients in plant extractive technique field.This technique is the following steps are included: crush, fermentation, precipitating, enzymatic hydrolysis, purifying；The precipitating reagent that the present invention is generated with tartaric acid, flavonols by esterification can precipitate the big molecular impurity in resveratrol, improve the purity of resveratrol；Precipitating reagent can prevent in purification process simultaneously, and resveratrol is destroyed by external environment, improve extraction efficiency；To the product of hydroxypropyl methyl cellulose, acrylic acid synthesis, effectively small molecular weight impurity, the pigment in resveratrol can be absorbed, significantly improve the purity of resveratrol；Present invention process is simple and environmentally-friendly, is suitble to industrial production, improves the utilization rate of resource.
Description
Technical field:
The present invention relates to effective ingredients in plant extractive technique fields, and in particular to a kind of biology extraction work of resveratrol
Skill.
Background technique:
Resveratrol is a kind of non-flavonoids polyphenolic substance with stilbene class formation, is primarily present in grape, peanut, mulberry
In the plants such as Shen and polygonum cuspidate, in field of medicaments for anticancer, anti-inflammatory and antiallergy, antirheumatic, prevention cardiovascular disease etc.；In beauty
Hold industry for lipid-loweringing beauty and weight-reducing natural health care to be made；Its anti-oxidant, free radical resisting characteristic is utilized in drinks,
Reduce the risk of alcoholism.
Resveratrol content in plant is lower, and the complicated component of plant extracts also contains mostly in addition to target component
There are flavonoids, phenolic acid.Therefore, the resveratrol that obtain high-purity needs to select suitable extracting method.Both at home and abroad
A large amount of research has been carried out to resveratrol, depending on sample type, extracting method has much the extracting method of resveratrol,
Such as infusion process, refluxing extraction.Occur ultrasonic wave assisted extraction, Microwave Extraction, Enzymatic Extraction, decompression boiling in recent years to extract
Etc. extracting methods.The classical process route of the resveratrol of domestic enterprise's production at present is: Rhizoma Polygoni Cuspidati-fermentation-alcohol concentrate
Active carbon decoloring-the crystallization of contracting-dry column column chromatography (silica gel or aluminium oxide)-and recrystallization.The final products of this process route are white
The yield of veratryl alcohol generally only has 0.3-0.5%, color slightly cream colour or canescence, the purity of resveratrol in 95-98%,
The resveratrol that its price and purity are 99% has biggish gap.
Summary of the invention:
Technical problem to be solved by the present invention lies in provide a kind of biological extraction process of high-purity resveratrol.
The following technical solution is employed for the technical problems to be solved by the invention to realize:
A kind of biological extraction process of resveratrol, comprising the following steps:
(1) it crushes: being 27- by fresh polygonum cuspidate drying to water content using vacuum and low temperature cold wind drier in 30-32 DEG C
30%, the raw material powder that partial size is 150-180 mesh is then ground into pulverizer；
(2) it ferments: being added 2-3 times into raw material powder and measure water infiltration 5-10h, then add cellulase, pectase, zymase
It is uniformly mixed, is sealed by fermentation 5-10 days, obtains fermentation liquid；By fermentation liquid ethyl alcohol, ethyl acetate mixture extraction 2-4 times, often
Secondary extraction 1-2h, Extracting temperature are 60-80 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220-260r/min；
(3) it precipitates: precipitating reagent being added into extracting solution and stirs evenly, places 2-3h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: it is 4.5-5.1 that sodium acetate is added into clarified solution and adjusts pH value, adds superoxide dismutase, β-
Glucuroide, carbohydrase are digested, and controlled at 43-58 DEG C, are digested 5-10h, are obtained enzymolysis liquid；
(5) it purifies: scarvenger being added into the enzymolysis liquid in step 4,80-90 DEG C of stirring 1-3h is filtered, and gained filtrate subtracts
Pressure is concentrated into solvent and recycles completely, is dried under vacuum to constant weight in 40-45 DEG C to get resveratrol finished product is arrived.
The cellulase, pectase, zymase mass ratio be 5-10:5-10:1-5.
The ethyl alcohol, ethyl acetate volume ratio be 10:1-5.
The precipitating reagent the preparation method is as follows: prepare tartaric acid saturated solution using 20-25 DEG C of deionized water, and pass through
Sulfuric acid adjusts pH stable in 4-4.5, and flavonols and tetraethyl titanate is added, is heated to reflux state insulated and stirred 1-3h, institute
Mixture is obtained to be sent into freeze drier after cooled to room temperature, micro mist is made through micronizer in dry obtained solid,
Up to precipitating reagent.
The tartaric acid, flavonols, tetraethyl titanate mass ratio be 15-20:10-15:1-3.
The superoxide dismutase, beta-glucosidase, carbohydrase mass ratio be 5-10:1-5:1-5.
The scarvenger the preparation method is as follows: montmorillonite is add to deionized water, be heated to reflux state heat preservation
10-20min is stirred, undecyl imidazole quinoline is added and continues return stirring 10-30min, is then cooled to 40-50 DEG C, hydroxyl is added
Propyl methocel and tetraethyl titanate, 40-50 DEG C of stirring 20-30min, are subsequently added into acrylic acid, continue to stir 1-2h, mistake
Filter, gained precipitating deionized water and dehydrated alcohol wash away impurity, are sent into drying box, and drying to constant weight obtains scarvenger.
The montmorillonite, undecyl imidazole quinoline, hydroxypropyl methyl cellulose, tetraethyl titanate, acrylic acid mass ratio
For 10-15:1-5:15-30:1-3:10-20.
The molecular weight of the hydroxypropyl methyl cellulose is 50000-100000.
Reaction principle according to the present invention is as follows:
(1) tartaric acid, flavonols generate precipitating reagent by esterification, which can be by big point in resveratrol
Sub- contamination precipitation gets off, and achievees the purpose that preliminary purification, while precipitating reagent can protect resveratrol not by organic solvent, height
The destruction of the extraneous factors such as temperature；
(2) cation exchange reaction occurs for undecyl imidazole quinoline and montmorillonite, enters in montmorillonite, montmorillonite layer
Surface is covered by long alkyl chain, enhances montmorillonite to the compatibility of Organic Ingredients, while longer alkyl molecule chain is in lamella
Between arrange in some way, can make piece interlamellar spacing increase, be conducive to the intercalation of larger molecular organics；
(3) esterification, but reaction temperature mistake are occurred under the effect of the catalyst to hydroxypropyl methyl cellulose, acrylic acid
When low, reaction efficiency is too low, and when the temperature is excessively high, cellulose is easy to decompose, the same efficiency for influencing reaction；Illiteracy after modification is de-
Soil can play activation to above-mentioned esterification, make it that can react at conventional temperatures, and reaction is efficient；Quilt simultaneously
The direction that the montmorillonite layer structure qualification esterification of long alkyl chain covering carries out, make esterification products it is neat be adsorbed on illiteracy
In de- soil lamella, there is excellent adsorption effect to pigment, impurity, the recovery rate of resveratrol can be improved.
The beneficial effects of the present invention are:
(1) precipitating reagent that is generated with tartaric acid, flavonols by esterification of the present invention can tentatively will be in resveratrol
Big molecular impurity precipitate, improve the purity of resveratrol；Precipitating reagent can prevent in purification process simultaneously, white black false hellebore
Alcohol is destroyed by external environment, improves extraction efficiency；
(2) product of hydroxypropyl methyl cellulose, acrylic acid synthesis is distributed in the lamellar structure of montmorillonite, passes through illiteracy
Alternately stacked lamellar structure, can effectively absorb small molecular weight impurity, the pigment in resveratrol, significantly in de- soil
The purity for improving resveratrol；
(3) present invention process is simple and environmentally-friendly, at low cost, is suitble to industrial production, improves the utilization rate of resource.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,12g flavonols and 1g tetraethyl titanate is added, is heated to reflux state
Insulated and stirred 2h, gained mixture are sent into freeze drier after cooled to room temperature, and dry obtained solid is through Ultramicro-powder
Micro mist is made to get precipitating reagent is arrived in broken machine.
The preparation of scarvenger: 10g montmorillonite is add to deionized water, and is heated to reflux state insulated and stirred 10min,
2g undecyl imidazole quinoline is added and continues return stirring 15min, is then cooled to 40 DEG C, 20g hydroxypropyl methyl cellulose is added
With 2g tetraethyl titanate, 40 DEG C of stirring 20min, then plus 15g enters acrylic acid, continue stir 1h, filtering, gained precipitating spend from
Sub- water and dehydrated alcohol wash away impurity, are sent into drying box, and drying to constant weight obtains scarvenger.
Embodiment 2
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,12g flavonols and 1g tetraethyl titanate is added, is heated to reflux state
Insulated and stirred 2h, gained mixture are sent into freeze drier after cooled to room temperature, and dry obtained solid is through Ultramicro-powder
Micro mist is made to get precipitating reagent is arrived in broken machine.
The preparation of scarvenger: 10g montmorillonite is add to deionized water, and is heated to reflux state insulated and stirred 10min,
2g undecyl imidazole quinoline is added and continues return stirring 15min, is then cooled to 40 DEG C, 20g hydroxypropyl methyl cellulose is added
With 2g tetraethyl titanate, 40 DEG C of stirring 20min, then plus 15g enters acrylic acid, continue stir 1h, filtering, gained precipitating spend from
Sub- water and dehydrated alcohol wash away impurity, are sent into drying box, and drying to constant weight obtains scarvenger.
Reference examples 1
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,1g tetraethyl titanate is added, is heated to reflux state insulated and stirred 2h,
Gained mixture is sent into freeze drier after cooled to room temperature, and dry obtained solid is made micro- through micronizer
Powder to get arrive precipitating reagent.
The preparation of scarvenger: 10g montmorillonite is add to deionized water, and is heated to reflux state insulated and stirred 10min,
2g undecyl imidazole quinoline is added and continues return stirring 15min, is then cooled to 40 DEG C, 20g hydroxypropyl methyl cellulose is added
With 2g tetraethyl titanate, 40 DEG C of stirring 20min, then plus 15g enters acrylic acid, continue stir 1h, filtering, gained precipitating spend from
Sub- water and dehydrated alcohol wash away impurity, are sent into drying box, and drying to constant weight obtains scarvenger.
Reference examples 2
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,12g flavonols and 1g tetraethyl titanate is added, is heated to reflux state
Insulated and stirred 2h, gained mixture are sent into freeze drier after cooled to room temperature, and dry obtained solid is through Ultramicro-powder
Micro mist is made to get precipitating reagent is arrived in broken machine.
The preparation of scarvenger: 10g montmorillonite is add to deionized water, and is heated to reflux state insulated and stirred 25min,
Then it is cooled to 40 DEG C, is added 20g hydroxypropyl methyl cellulose and 2g tetraethyl titanate, 40 DEG C of stirring 20min, then plus 15g
Enter acrylic acid, continues to stir 1h, filtering, gained precipitating deionized water and dehydrated alcohol wash away impurity, are sent into drying box, do
It is dry to obtain scarvenger to constant weight.
Reference examples 3
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,12g flavonols and 1g tetraethyl titanate is added, is heated to reflux state
Insulated and stirred 2h, gained mixture are sent into freeze drier after cooled to room temperature, and dry obtained solid is through Ultramicro-powder
Micro mist is made to get precipitating reagent is arrived in broken machine.
The preparation of scarvenger: 10g montmorillonite is add to deionized water, and is heated to reflux state insulated and stirred 10min,
2g undecyl imidazole quinoline is added and continues return stirring 15min, is then cooled to 40 DEG C, filtering, gained precipitating uses deionized water
Impurity is washed away with dehydrated alcohol, is sent into drying box, drying to constant weight obtains scarvenger.
Reference examples 4
(1) it crushes: using vacuum and low temperature cold wind drier in 30-32 DEG C, 20kg fresh polygonum cuspidate is dry to water content
For 27-30%, the raw material powder that partial size is 150 mesh is then ground into pulverizer；
(2) it ferments: 2 times of amount water infiltration 10h being added into raw material powder, then add 5g cellulase, 5g pectase, 3g and make
Enzyme is uniformly mixed, and is sealed by fermentation 5 days, is obtained fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2 times, mentioned every time
1h is taken, Extracting temperature is 60 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220r/min；
(3) it precipitates: 10g precipitating reagent being added into extracting solution and stirs evenly, places 2h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: into clarified solution be added sodium acetate adjust pH value be 4.5-5.1, add 6g superoxide dismutase,
4g beta-glucosidase, 4g carbohydrase are digested, and controlled at 43 DEG C, are digested 5h, are obtained enzymolysis liquid；
(5) it purifies: 12g scarvenger, 80 DEG C of stirring 1h, filtering, gained filtrate decompression being added into the enzymolysis liquid in step 4
It is concentrated into solvent to recycle completely, is dried under vacuum to constant weight in 40 DEG C to get resveratrol finished product is arrived.
The preparation of precipitating reagent: preparing tartaric acid saturated solution using 20-25 DEG C of deionized water, (quality of tartaric acid is
12g), and by sulfuric acid pH stable is adjusted in 4-4.5,12g flavonols and 1g tetraethyl titanate is added, is heated to reflux state
Insulated and stirred 2h, gained mixture are sent into freeze drier after cooled to room temperature, and dry obtained solid is through Ultramicro-powder
Micro mist is made to get precipitating reagent is arrived in broken machine.
Scarvenger: montmorillonite.
Embodiment 3
Based on embodiment 1, setting does not add the reference examples 1 of flavonols, does not add the control of undecyl imidazole quinoline
Example 2, only using modified montmorillonoid as the reference examples 3 of scarvenger, using montmorillonite as the reference examples 4 of scarvenger.
The extraction of resveratrol is carried out using embodiment 1-2, reference examples 1-4, the content and purity of gained resveratrol are such as
Shown in table 1.
The content and purity of 1 resveratrol of table
| Group | The content (g) of resveratrol | The purity (%) of resveratrol |
| Embodiment 1 | 898 | 99.8 |
| Embodiment 2 | 899 | 99.9 |
| Reference examples 1 | 845 | 96.3 |
| Reference examples 2 | 833 | 95.1 |
| Reference examples 3 | 809 | 89.6 |
| Reference examples 4 | 758 | 83.2 |
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of biological extraction process of resveratrol, which comprises the following steps:
(1) it crushes: being 27- by fresh polygonum cuspidate drying to water content using vacuum and low temperature cold wind drier in 30-32 DEG C
30%, the raw material powder that partial size is 150-180 mesh is then ground into pulverizer；
(2) it ferments: being added 2-3 times into raw material powder and measure water infiltration 5-10h, then add cellulase, pectase, zymase mixing
Uniformly, it is sealed by fermentation 5-10 days, obtains fermentation liquid；Fermentation liquid ethyl alcohol, ethyl acetate mixture are extracted 2-4 times, mentioned every time
1-2h is taken, Extracting temperature is 60-80 DEG C, and extracting solution is carried out centrifugal treating, revolving speed 220-260r/min；
(3) it precipitates: precipitating reagent being added into extracting solution and stirs evenly, places 2-3h, is filtered to remove precipitating, obtains clarified solution；
(4) digest: it is 4.5-5.1 that sodium acetate is added into clarified solution and adjusts pH value, adds superoxide dismutase, β-grape
Glycosidase, carbohydrase are digested, and controlled at 43-58 DEG C, are digested 5-10h, are obtained enzymolysis liquid；
(5) it purifies: scarvenger being added into the enzymolysis liquid in step 4,80-90 DEG C of stirring 1-3h is filtered, and gained filtrate decompression is dense
It is reduced to solvent to recycle completely, is dried under vacuum to constant weight in 40-45 DEG C to get resveratrol finished product is arrived.
2. the biological extraction process of resveratrol according to claim 1, it is characterised in that: the cellulase, pectin
Enzyme, zymase mass ratio be 5-10:5-10:1-5.
3. the biological extraction process of resveratrol according to claim 1, it is characterised in that: the ethyl alcohol, ethyl acetate
Volume ratio be 10:1-5.
4. the biological extraction process of resveratrol according to claim 1, it is characterised in that: the superoxide dismutase
Enzyme, beta-glucosidase, carbohydrase mass ratio be 5-10:1-5:1-5.
5. the biological extraction process of resveratrol according to claim 1, which is characterized in that the preparation side of the scarvenger
Method is as follows: montmorillonite being add to deionized water, reflux state insulated and stirred 10-20min is heated to, undecyl miaow is added
Oxazoline continues return stirring 10-30min, is then cooled to 40-50 DEG C, and hydroxypropyl methyl cellulose and tetraethyl titanate is added,
40-50 DEG C of stirring 20-30min, is subsequently added into acrylic acid, continues to stir 1-2h, filtering, gained precipitating deionized water and anhydrous
Ethyl alcohol washes away impurity, is sent into drying box, and drying to constant weight obtains scarvenger.
6. the biological extraction process of resveratrol according to claim 5, it is characterised in that: the montmorillonite, hendecane
Base imidazoline, hydroxypropyl methyl cellulose, tetraethyl titanate, acrylic acid mass ratio be 10-15:1-5:15-30:1-3:10-
20。
7. the biological extraction process of resveratrol according to claim 5, it is characterised in that: the hydroxypropyl methyl fiber
The molecular weight of element is 50000-100000.
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