CN103396295A - Extraction method for resveratrol from giant knotweed rhizome - Google Patents
Extraction method for resveratrol from giant knotweed rhizome Download PDFInfo
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- 238000000605 extraction Methods 0.000 title abstract description 16
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 title abstract description 7
- 235000021283 resveratrol Nutrition 0.000 title abstract description 7
- 229940016667 resveratrol Drugs 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000002244 precipitate Substances 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000007787 solid Substances 0.000 claims abstract description 28
- 229920001661 Chitosan Polymers 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 24
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- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
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- RHMXXJGYXNZAPX-UHFFFAOYSA-N emodin Chemical compound C1=C(O)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O RHMXXJGYXNZAPX-UHFFFAOYSA-N 0.000 description 1
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- PKUBGLYEOAJPEG-UHFFFAOYSA-N physcion Natural products C1=C(C)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O PKUBGLYEOAJPEG-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides an extraction method for resveratrol from giant knotweed rhizome. Plants like giant knotweed rhizome, peanut rhizome, branches and leaves of grape and mulberry leaves having undergone enzymatic hydrolysis and fermentation can be used as raw materials. The extraction method comprises the following steps: adding superoxide dismutase according to the proportion of the raw materials and then adding an ethanol solvent with a concentration of 80% for extraction; combining obtained extracts, carrying out vacuum concentration and complete recovery of ethanol, adding a saturated chitosan solution into an obtained concentrate, and allowing an extract to be precipitated in a deposition manner; adding an ethanol solvent weighing 20 times of an obtained precipitate and having a concentration of 40% to dissolve the precipitate, then carrying out filtering, concentrating a filtrate, adding a chitosan solution into the concentrated filtrate and carrying out standing and centrifugation at normal temperature so as to obtain a solid precipitate; and adding an ethanol solvent weighing 20 times of the solid precipitate and having a concentration of 40% to dissolve the solid precipitate, then carrying out filtering, concentrating a filtrate, adding a chitosan solution into the concentrated filtrate, carrying out standing and centrifugation at normal temperature so as to obtain a solid precipitate and washing the solid precipitate with purified water until a washing liquid does not contain a pigment; and successively carrying out vacuum drying and crushing so as to obtain a product with purity of 50 to 60%. Compared with a conventional production method, the extraction method provided by the invention enables yield of resveratrol to be increased by more than 30%.
Description
One, technical field
The present invention relates to a kind of from giant knotweed, extracting the method for trans-resveratrol composition.Also be applicable to from the peanut rhizome, the branches and leaves of grape, the plants such as mulberry leaf are extracted trans-resveratrol as raw material.Belong to biological technical field.
Two, background technology
Trans-resveratrol is a kind of natural antioxidant; can reduce the viscosity of blood; suppress hematoblastic improper condensing; the impatient hard plug of prevention, cerebral embolism, hepar damnification; to ischemic heart, there are provide protection and arterial vascular diastole keep unobstructed blood and improve microcirculation; but the generation of preventing cancer and development; has atherosclerosis and coronary heart disease; immune system activity in ischemic heart disease, senile dementia, viral hepatitis, stomach ulcer and lifting wound treatment, and the effect of inhibition tumour.
The preparation of trans-resveratrol at present is divided into chemical synthesis, culture plant cell, microwave extraction, the five large classes such as ultrasonic extraction and solvent-extraction process; Chemical synthesis and culture plant cell method processing condition are harsh, complicated, and yield is low, is difficult to industrializing implementation; Though supersonic method and microwave method have the effect that increases yield, in this technique, because the singularity of product very easily becomes to produce the product oxidation, be not suitable for, also be difficult to carry out, the most widely used or plant extraction process.
Apply to now production method and mainly be divided into two kinds of techniques; A kind of is ethanol-extracted, ethyl acetate extraction then, then strip with alcohol, filtering and concentrating, drying obtains product.Another kind is directly to use ethyl acetate extraction, and then alcohol is stripped, filtering and concentrating, and drying obtains product.These existing technology exist all that man-hour is long, equipment used is more, solvent loss is large, yield is not high, produce and consume large, the common shortcoming of high in cost of production; The above method of what is more important can't be got rid of in (prevention) leaching process abundant because being heated, and makes to remain in the central low loss of zymin yield that accelerate decomposition causes of raw material.
Three, summary of the invention
The purpose of this invention is to provide a kind of method from extraction trans-resveratrol composition giant knotweed, it uses single-solvent extraction, and technique is simple, and is efficient, low cost, and Production Flow Chart is short, the production method that yield is high.
In order to realize purpose of the present invention, the present invention implements by the following technical solutions:
(1), by through the good starting material of enzymolysis processing, adding raw material, weigh 1 ‰ superoxide-dismutase, add the alcohol solvent of 5 times of weight 80% concentration to extract, its temperature is controlled at 45-65 ℃ of degree, each 2 hours, extracts altogether 4 times;
(2), after extracting solution obtained above is merged, temperature is controlled at below 55--60 ℃, carry out vacuum concentration and reclaim ethanol fully, concentrated solution weighs 5% ratio according to raw material and adds the chitosan saturated solution, standing 8--12 hour, extract is separated out in the mode of precipitation at normal temperatures, after separating out fully, filters intercepting solid precipitation part;
(3), in solid sediment, the alcoholic degree that adds 20 times of precipitate weight is the alcohol solvent of 40--45%, precipitate is dissolved and filtration, insolubles discard, then the filtered liquid temperature is controlled under 55--60 ℃ of vacuum state, be concentrated into without after alcohol component, add the chitosan saturated solution that weighs 5% ratio in raw material, standing 8--12 hour under normal temperature, centrifugation obtains the precipitate of solid;
(4), again adding the alcoholic degree of 20 times of precipitate weight is the alcohol solvent of 40--45%, precipitate is dissolved and filtration, insolubles discard, then the filtered liquid temperature is controlled under 55--60 ℃ of vacuum state of heating, be concentrated into without after alcohol component, add raw material to weigh the chitosan saturated solution of 5% ratio, standing 8--12 hour under normal temperature, centrifugation obtains the precipitate of solid, and the precipitate that obtains solid is washed to washings non-pigment composition state with pure water;
(5), the precipitate after the washing is pulverized the product that both obtains 50%-65% after vacuum-drying.
Described a kind of from giant knotweed, extracting the method for trans-resveratrol composition, add raw material and weigh 1 ‰ superoxide-dismutase and stop in production process to be present in material plant be used to the enzyme that decomposes polidatin and lose activity and excessive enzyme no longer occurs decompose; Thereby protected the loss of trans-resveratrol composition in the leaching process
Described a kind of from giant knotweed, extracting the method for trans-resveratrol composition, adopt 5% chitosan saturated solution to guide fast separating out of product in concentrated solution.
The present invention is a kind of from giant knotweed, extracting the method for trans-resveratrol composition, and it amplifies actual measurement by technique; One, in extraction process, added the enzyme agent ' superoxide-dismutase ' of taking off that can suppress to continue enzyme digestion reaction and in leaching process, be present in material plant be used to the enzyme that decomposes polidatin and lose activity and excessive enzyme no longer occurs decompose; Thereby protected the more existing industry of loss (enterprise) of trans-resveratrol composition in the leaching process can improve yield more than 30%; Reduced simultaneously the content of the harmful free radical that produces because of enzymolysis in the product; Two, adopt the alcohol solvent of 40% content to coordinate chitosan solution to accelerate by precipitation in turbid solution, also to be separated out fully fast with solid form by the trans-resveratrol that the solvent item transfers in aqueous phase solution.The product link of naturally separating out of 2-4 days that changes in the traditional technology mode is to complete in 12 hours; Three, in the product emodin content less than 0.7% well below the company standard of industry 2.8%; The anthraquinone foreign matter content is less than 1/10 of traditional technology.
The present invention adds raw material and weighs 1 ‰ superoxide-dismutase and stop and protect the loss that the excessive decomposition in leaching process causes and the content that has reduced the harmful free radical that produces because of enzymolysis in the product; Adopt the chitosan saturated solution guiding concentrated solution of interpolation 5% to separate out fast.Superoxide-dismutase and chitosan all do not contain the toxicity composition and are added in technique and can cause unnecessary injury.
In the present invention, refer to the giant knotweed that contains the trans-resveratrol composition, the peanut rhizome, the branches and leaves of grape, the plants such as mulberry leaf, as raw material, are refered in particular to giant knotweed; The superoxide-dismutase that the present invention adds by raw material anharmonic ratio example is that form, the chitosan under dissolved state do not refer to the saturated solution in being dissolved in water.Due to the purity of industry product normally 50% content specification be not very high, comprise and account for half soluble impurity so process using of product and add chitosan solution and accelerated art production process corresponding shortening man-hour as the precipitation agent of guiding.
Provided by the invention a kind of from giant knotweed, extracting the method for trans-resveratrol composition, it is compared with existing production method, can improve yield more than 30%.
Five, embodiment
Below in conjunction with embodiment, come the present invention is done carefully to describe furtherly.
The processing step that the present invention adopts is to optimize gained by parallel test, and adopts vertical mode of amplifying to implement;
Embodiment 1:
learnt from else's experience enzymolysis by---detect Resveratrol content and be 1.4% giant knotweed raw material 1 kilogram (eliminating water ratio) and add 1 gram superoxide-dismutase and add simultaneously 5 liter of 80% concentration ethanol solvent, heating and temperature control was 50 ℃ of refluxing extraction 2 hours, after filtering out extracting solution, the extraction using alcohol 2 hours that adds again 5 liters, 4 times like this, the extracting solution merging control temperature that each batch obtains is carried out to vacuum concentration recovery ethanol at 60 ℃, extracting solution after concentrated weighs 5% ratio in raw material and adds the chitosan saturated solution, separated out at normal temperatures in standing 10 hours, after separating out fully, filter,
It is that 40% alcohol solvent carries out redissolve and filters the precipitate that obtains that the intercepting solid precipitation partly adds 20 times of mass concentrations to precipitate, insolubles discards, under 60 ℃ of vacuum states of filtered liquid heating and temperature control, be concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 2% ratio, under normal temperature, separated out in standing 10 hours.Centrifugation obtains the precipitate of solid;
The alcoholic degree that again adds 20 times of precipitate weight is that 40% alcohol solvent dissolves precipitate and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states of heating and is concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 5% ratio, under normal temperature standing 10 hours, centrifugation obtained the extract of solid and separates out.With pure water, wash to washings non-pigment composition state.
Precipitate after washing is pulverized to obtain 57% product 23 grams, yield 93.6% after vacuum-drying.
Embodiment 2:
getting fermentation is that 1.4% giant knotweed raw material 10 kilograms (eliminating water ratio) adds 10 gram superoxide-dismutases and adds simultaneously 50 liter of 80% concentration ethanol solvent by detecting Resveratrol content, heating and temperature control was 50 ℃ of refluxing extraction 2 hours, after filtering out extracting solution, the extraction using alcohol 2 hours that adds again 5 liters, 4 times like this, the extracting solution merging control temperature that each batch obtains is carried out to vacuum concentration recovery ethanol at 60 ℃, extracting solution after concentrated weighs 5% ratio in raw material and adds the chitosan saturated solution, separated out at normal temperatures in standing 12 hours, after separating out fully, filter.
It is that 40% alcohol solvent carries out redissolve and filters the precipitate that obtains that the intercepting solid precipitation partly adds 20 times of mass concentrations to precipitate, insolubles discards, under 60 ℃ of vacuum states of filtered liquid heating and temperature control, be concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 2% ratio, under normal temperature, separated out in standing 12 hours.Centrifugation obtains the precipitate of solid.
The alcoholic degree that again adds 20 times of precipitate weight is that 40% alcohol solvent dissolves precipitate and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states of heating and is concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 5% ratio, under normal temperature standing 12 hours, centrifugation obtained the extract of solid and separates out.With pure water, wash to washings non-pigment composition state.
Precipitate after washing is pulverized to obtain 55% product 238 grams, yield 93.5% after vacuum-drying.
Embodiment 3:
getting fermentation is that 1.4% giant knotweed raw material 100 kilograms (eliminating water ratio) adds 100 gram superoxide-dismutases and adds simultaneously 500 liter of 80% concentration ethanol solvent by detecting Resveratrol content, heating and temperature control was 50 ℃ of refluxing extraction 2 hours, after filtering out extracting solution, the extraction using alcohol 2 hours that adds again 5 liters, 4 times like this, the extracting solution merging control temperature that each batch obtains is carried out to vacuum concentration recovery ethanol at 60 ℃, extracting solution after concentrated weighs 5% ratio in raw material and adds the chitosan saturated solution, separated out at normal temperatures in standing 12 hours, after separating out fully, filter.
It is that 40% alcohol solvent carries out redissolve and filters the precipitate that obtains that the intercepting solid precipitation partly adds 20 times of mass concentrations to precipitate, insolubles discards, under 60 ℃ of vacuum states of filtered liquid heating and temperature control, be concentrated into without after alcohol component, adding raw material to weigh the poly-saturated sugar soln of shell of 2% ratio, under normal temperature, separated out in standing 12 hours.Centrifugation obtains the precipitate of solid.
The alcoholic degree that again adds 20 times of precipitate weight is that 40% alcohol solvent dissolves precipitate and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states of heating and is concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 5% ratio, under normal temperature standing 12 hours, centrifugation obtained the extract of solid and separates out.With pure water, wash to washings non-pigment composition state.
Precipitate after washing is pulverized to obtain 2.4 kilograms of 54% products, yield 92.5% after vacuum-drying.
Embodiment 4:
getting fermentation is that 1.4% giant knotweed raw material 500 kilograms (eliminating water ratio) adds 0.5 kilogram of superoxide-dismutase and adds simultaneously 2500 liter of 80% concentration ethanol solvent by detecting Resveratrol content, heating and temperature control was 50 ℃ of refluxing extraction 2 hours, after filtering out extracting solution, the extraction using alcohol 2 hours that adds again 5 liters, 4 times like this, the extracting solution merging control temperature that each batch obtains is carried out to vacuum concentration recovery ethanol at 60 ℃, extracting solution after concentrated weighs 5% ratio in raw material and adds the chitosan saturated solution, separated out at normal temperatures in standing 12 hours, after separating out fully, filter.
It is that 40% alcohol solvent carries out redissolve and filters the precipitate that obtains that the intercepting solid precipitation partly adds 20 times of mass concentrations to precipitate, insolubles discards, under 60 ℃ of vacuum states of filtered liquid heating and temperature control, be concentrated into without after alcohol component, adding raw material to weigh the chitosan solution of 2% ratio, under normal temperature, separated out in standing 12 hours.Centrifugation obtains the precipitate of solid.
The alcoholic degree that again adds 20 times of precipitate weight is that 40% alcohol solvent dissolves precipitate and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states of heating and is concentrated into without after alcohol component, adding raw material to weigh the chitosan saturated solution of 5% ratio, under normal temperature standing 12 hours, centrifugation obtained the extract of solid and separates out.With pure water, wash to washings non-pigment composition state.
Precipitate after washing is pulverized to obtain 11.5 kilograms of 55% products, yield 90.4% after vacuum-drying.
Claims (3)
1. one kind from extracting the method for trans-resveratrol composition giant knotweed, it is characterized in that:
(1), by through the good starting material of enzymolysis processing, adding raw material, weigh 1 ‰ superoxide-dismutase, add the alcohol solvent of 5 times of weight 80% concentration to extract, its temperature is controlled at 45-65 ℃ of degree, each 2 hours, extracts altogether 4 times;
(2), after extracting solution obtained above is merged, temperature is controlled at below 60 ℃, carry out vacuum concentration and reclaim ethanol fully, concentrated solution weighs 5% ratio according to raw material and adds the chitosan saturated solution, standing 12 hours, extract is separated out in the mode of precipitation at normal temperatures, after separating out fully, filters intercepting solid precipitation part;
(3), in solid sediment, the alcoholic degree that adds 20 times of precipitate weight is 40% alcohol solvent, precipitate is dissolved and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states, be concentrated into without after alcohol component, add the chitosan saturated solution that weighs 5% ratio in raw material, under normal temperature standing 12 hours, centrifugation obtained the precipitate of solid;
(4), again adding the alcoholic degree of 20 times of precipitate weight is 40% alcohol solvent, precipitate is dissolved and filtration, insolubles discard, then the filtered liquid temperature is controlled under 60 ℃ of vacuum states of heating, be concentrated into without after alcohol component, add raw material to weigh the chitosan saturated solution of 5% ratio, under normal temperature standing 12 hours, centrifugation obtained the precipitate of solid, and the precipitate that obtains solid is washed to washings non-pigment composition state with pure water;
(5), the precipitate after the washing is pulverized the product that both obtains 50%-65% after vacuum-drying.
2. as claimed in claim 1 a kind of from giant knotweed, extracting the method for trans-resveratrol composition, it is characterized in that: add raw material and weigh 1 ‰ superoxide-dismutase and stop in production process to be present in material plant be used to the enzyme that decomposes polidatin and lose activity and excessive enzyme no longer occurs decompose; Thereby protected the loss of trans-resveratrol composition in the leaching process.
3. as claimed in claim 1 a kind of from giant knotweed, extracting the method for trans-resveratrol composition, it is characterized in that: adopt 5% chitosan saturated solution to guide fast separating out of product in concentrated solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111109511A (en) * | 2020-02-10 | 2020-05-08 | 广西壮族自治区农业科学院 | Rapid peeling method for food-grade walnut kernels |
| CN118325136A (en) * | 2024-06-11 | 2024-07-12 | 江苏中有信科技有限公司 | Chlamydomonas reinhardtii polysaccharide particles and preparation method thereof |
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| CN118325136A (en) * | 2024-06-11 | 2024-07-12 | 江苏中有信科技有限公司 | Chlamydomonas reinhardtii polysaccharide particles and preparation method thereof |
| CN118325136B (en) * | 2024-06-11 | 2024-10-01 | 江苏中有信科技有限公司 | Chlamydomonas reinhardtii polysaccharide particles and preparation method thereof |
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