CN102718817A - Method for preparing anthocyanin extract from black bean peel - Google Patents
Method for preparing anthocyanin extract from black bean peel Download PDFInfo
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- CN102718817A CN102718817A CN2011100792280A CN201110079228A CN102718817A CN 102718817 A CN102718817 A CN 102718817A CN 2011100792280 A CN2011100792280 A CN 2011100792280A CN 201110079228 A CN201110079228 A CN 201110079228A CN 102718817 A CN102718817 A CN 102718817A
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- 238000000034 method Methods 0.000 title claims abstract description 22
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention relates to a method for preparing an anthocyanin extract from black bean peel and solves the problem that existing extracts have low effective component content and high protein content. The method comprises the following steps of: firstly extracting black bean peel by the use of an acidic solvent, condensing the extracted solution, removing the solvent, adding acidic protease for enzymolysis, absorbing the enzymolysis solution by the use of resin, carrying out desorption and elution on the adsorbent resin, condensing and drying the elution solution after desorption, so as to obtain the protein-free anthocyanin extract. In addition, studies show that the protein-free anthocyanin extract and a standard extract of Ginkgo biloba have antioxidant anti-aging synergy.
Description
Technical field
The invention belongs to the separation method field, be specifically related to a kind of method of from Testa sojae atricolor, extracting no protein anthocyanogen.
Background technology
Black soya bean is the black seed of pulse family soybean plants Glycine max (L.) Merr..Have another name called black beans, black soya bean, the sweet property of distinguishing the flavor of is flat.Black soya bean is a kind of of soybean, contains more rich protein, fat, glucide and Serlabo, VITMAIN B1, B2, nicotinic acid and robust fibre, calcium, and phosphorus, nutritive substances such as iron, and contain a spot of daidzin, estrogen-like effects is arranged.Testa sojae atricolor contains pectin, carbohydrate and multiple pigment.
The Compendium of Material Medica record: " beans have the five colors, each treating disorders in five ZANG-organs, and it is cold that the thought black soya bean belongs to water-based, can go into kidney.Harness the river, dissipate-swelling, the therapeutic method to keep the adverse qi flowing downward, control wind-heat and promoting blood circulation and detoxication, often edible black soya bean, but all kinds of diseases and ailments are not given birth to." " it is many that black soya bean is gone into the kidney merit, so can harness the river, the therapeutic method to keep the adverse qi flowing downward of subsiding a swelling.Control wind-heat and promoting blood circulation and detoxication." so traditional Chinese medicine think that the black soya bean sweet property of distinguishing the flavor of is flat, go into the spleen channel, kidney channel, be a kind of food that helps antidotal specific function.
Modern study finds that black bean extract (Black Soybean Hull Extract) has excellent anti-oxidation characteristics; Also have certain anticancer change, vascular protection, anti-inflammatory, obesity and anti-glycosuria effect (Bioavailability, antioxidant and biologicalproperties of the natural free-radical scavengers cyanidin and related glycosides.Ann Ist SuperSanita.2007; 43 (4): 382-93.).Therefore, black bean extract has been widely used as in protective foods and the makeup.And contained effective constituent is mainly Cyanidin (Cyanidin) and its anthocyanogen that derives--cyaniding 3-0-glucoside (Cyanidin-3-O-glucoside) in the cyanidin(e) in the black bean extract.
One Chinese patent application CN101250206 (application number is 200810052526.9) contains efficient part and the preparation method and the application of cyaniding 3-0-glucoside.Disclose a kind of efficient part and preparation method and application that contains cyaniding 3-0-glucoside, its preparation method is: with the Testa sojae atricolor is raw material, adds the water extract at room temperature, sieves, and must extract solution; Extract solution through macroporous resin adsorption, water and aqueous ethanolic solution gradient elution are collected the component that is rich in cyaniding 3-0-glucoside, and concentrating under reduced pressure gets enriched material; Enriched material carries out polyamide resin absorption, and water and aqueous ethanolic solution gradient elution are collected the component that is rich in cyaniding 3-0-glucoside, and with the elute soln concentrating under reduced pressure, drying obtains content greater than 50% cyaniding 3-0-glucoside product.
One Chinese patent application CN1844129 (application number is 200610013546.6) extracts the method for anthocyanogen from Testa sojae atricolor.Disclose a kind of method of from Testa sojae atricolor, extracting anthocyanogen, comprised as follows: in the Testa sojae atricolor raw material, add aqueous ethanolic solution or methanol aqueous solution, soaking and extracting is filtered, and the pH of solution is 1～4, and extracting solution is concentrated into does not have alcohol, leaves standstill, and abandons deposition, gets supernatant; Supernatant is adsorbed through styrene resin, and water or aqueous ethanolic solution or methanol aqueous solution wash-out begin when darkening to collect, with elute soln under≤70 ℃ of conditions, drying under reduced pressure, the anthocyanogen product.
The preparation technology of the natural Testa sojae atricolor pigment of one Chinese patent application CN101095504 (application number is 200710057844.X).A kind of extraction process of natural Testa sojae atricolor pigment is disclosed; It comprises step of preparation process such as selected black soya bean, machinery decortication, selection by winnowing skin of beancurd, drying, pulverizing, lixiviate, filtration, evaporation concentration, liquid grinding, drying, finished product, and has optimized Testa sojae atricolor from many-sides such as extraction solution and concentration thereof, pH value, thing liquor ratio, temperature, extraction times and extracted melanic technology.
One Chinese patent application CN101353362 (application number is 200810052747.6), the process for extracting of cyaniding 3-0-glucoside.Disclose a kind of process for extracting of cyaniding 3-0-glucoside, comprised the steps: that with Testa sojae atricolor etc. be raw material, added entry or aqueous acid to extract; Through macroporous resin adsorption, water and aqueous ethanolic solution gradient elution are collected the component that is rich in cyaniding 3-0-glucoside, concentrating under reduced pressure; Enriched material is dispersed to carries out polyamide resin absorption in the water, water and aqueous ethanolic solution gradient elution are collected the component that is rich in cyaniding 3-0-glucoside, concentrating under reduced pressure, drying; Carry out Toyopearl volume-exclusion chromatography column chromatography purification, obtain the different cyaniding 3-0-glucoside extracts of content＞20%.
The production technique of above-mentioned black bean extract all is merely from Testa sojae atricolor, to extract pigment, does not all carry out isolating protein at leaching process and handles, and protein contnt mostly＞5%.Therefore these extracts exist plant protein to cause the great risk of skin allergy when utilization in the time of particularly in adding makeup to.And do not see the relevant report for preparing the method for no albumen anthocyanogen red pigment from Testa sojae atricolor at present as yet.
Summary of the invention
The method that from Testa sojae atricolor, prepares the anthocyanogen extract that the purpose of this invention is to provide a kind of effective component content higher protein content trace.
The present invention is achieved in that
A kind of method that from Testa sojae atricolor, prepares the anthocyanogen extract of the present invention; At first Testa sojae atricolor is extracted with acid solvent; The extraction solution concentration desolventizes back adding aspartic protease and carries out enzymolysis; Enzymolysis solution carries out the desorption wash-out with resin absorption to polymeric adsorbent, and the elute soln concentrate drying must not have albumen anthocyanogen extract after the desorption.
Testa sojae atricolor is extracted as solvent with the Hydrocerol A ethanolic soln, wherein the content of Hydrocerol A is 0.1～0.3% (w/v), and the ethanol alcoholic degree is 70 °～90 °; Extracting temperature is 45～55 ℃; Solvent pH value is 2～3, and the Hydrocerol A ethanolic soln is 15: 1 with Testa sojae atricolor gross weight ratio, divides three extractions; Each solution and Testa sojae atricolor weight ratio are 5: 1, extract 2 hours.
Method extraction solution for vacuum concentrating under reduced pressure desolventizes back adding aspartic protease and carries out enzymolysis; Wherein vacuum decompression concentrates and will remain on below 60 ℃; Proportion is 1.03～1.05 when concentrating end; The enzyme amount that adds aspartic protease is 30～50u/ml, and the enzymolysis holding temperature is 40～60 ℃, and enzymolysis time is 4～6 hours.
Enzymolysis solution adsorbs with polar macroporous resin, and the absorption flow velocity is 1～3BV/h, after absorption finishes; Content with Hydrocerol A is 0.2% (w/v), and the ethanol alcoholic degree is that 10 ° solution carries out the removal of impurities washing to the polar macroporous resin after adsorbing, and wash volumes is 2～4BV; Content with Hydrocerol A is 0.2% (w/v) again; The ethanol alcoholic degree is that 50 °～70 ° solution carries out wash-out to polar macroporous resin, begins to collect from color burn, and elution volume is 2～4BV; Elution flow rate is 0.5～1.5BV/h, to must there not being albumen anthocyanogen extract behind the elute soln concentrate drying.
Technology letter of the present invention, with low cost, protein content＜0.1% greatly reduces the great risk that plant protein causes skin allergy.
Embodiment
1-9 embodiment of the present invention as solvent, adds the aspartic protease decomposing protein with Hydrocerol A ethanol in extracting enriching soln, enriching soln carries out the removal of impurities washing and conciliates absorb-elute after resin absorption.
Through following tabulation to processing condition so that 1-9 embodiment of the present invention to be described.
Following embodiment 1～9th extracts with the Hydrocerol A ethanolic soln 500g Testa sojae atricolor to Testa sojae atricolor.Then Testa sojae atricolor is extracted solution concentration to proportion 1.03～1.05, add aspartic protease, stir the insulation enzymolysis to extracting enriching soln.
Enzymolysis solution is adsorbed with polar macroporous resin, and after absorption finished, the Hydrocerol A ethanolic soln carried out the removal of impurities washing to the polar macroporous resin after adsorbing, and with the Hydrocerol A ethanolic soln polar macroporous resin is carried out wash-out again, began to collect from color burn.
Hydrocerol A ethanol elution solution concentrates with vacuum decompression, and temperature is below 70 °, and concentration ratio focuses on 1.03～1.05.After concentrating completion, be drying to obtain no protein anthocyanogen extract.
Wherein, alcohol concn (°), citric acid concentration (w/v), extract in temperature and pH value, the extract cyaniding 3-0-glucoside content (%) and see table 1.
Table 1
Extraction solution concentration proportion, interpolation aspartic protease enzyme amount, hydrolysis temperature, enzymolysis time are seen table 2 among the embodiment 1-9.
Table 2
The absorption flow velocity of embodiment 1-9, wash-out alcoholic degree, elution volume, elution flow rate are seen table 3.
Table 3
Embodiment 10
Testa sojae atricolor is extracted as solvent with phosphoric acid ethanol solution, wherein the content of phosphoric acid is 0.2% (w/v), and the ethanol alcoholic degree is 80 °; Extracting temperature is 50 ℃; Solvent pH value is 2～3, and phosphoric acid ethanol solution is 15: 1 with Testa sojae atricolor gross weight ratio, divides three extractions; Each solution and Testa sojae atricolor weight ratio are 5: 1, extract 2 hours.
Extract the aspartic protease that adds the production of Ningxia jade of the He family Bioisystech Co., Ltd after the solution for vacuum concentrating under reduced pressure desolventizes and carry out enzymolysis; Wherein vacuum decompression concentrates and will remain on below 60 ℃; Proportion is 1.03～1.05 when concentrating end; The enzyme amount that adds aspartic protease is 40u/ml, and the enzymolysis holding temperature is 50 ℃, and enzymolysis time is 5 hours.
Enzymolysis solution adsorbs with polar macroporous resin, and the absorption flow velocity is 2BV/h, after absorption finishes; Content with phosphoric acid is 0.2% (w/v), and the ethanol alcoholic degree is that 10 ° solution carries out the removal of impurities washing to the polar macroporous resin after adsorbing, and wash volumes is 3BV; Content with phosphoric acid is 0.2% (w/v) again; The ethanol alcoholic degree is that 60 ° solution carries out wash-out to polar macroporous resin, begins to collect from color burn, and elution volume is 3BV; Elution flow rate is 1BV/h, to must there not being albumen anthocyanogen extract behind the elute soln concentrate drying.Wherein cyaniding 3-0-glucoside content is 34.3%, and protein content is 0.07%.
Embodiment 11
Testa sojae atricolor is extracted as solvent with the acetate ethanolic soln, wherein the content of acetate is 0.2% (w/v), and the ethanol alcoholic degree is 80 °; Extracting temperature is 50 ℃; Solvent pH value is 2～3, and the acetate ethanolic soln is 15: 1 with Testa sojae atricolor gross weight ratio, divides three extractions; Each solution and Testa sojae atricolor weight ratio are 5: 1, extract 2 hours.
The aspartic protease that extraction solution for vacuum concentrating under reduced pressure desolventizes adding Shanghai, back pattern ocean Bioisystech Co., Ltd to be provided carries out enzymolysis; Wherein vacuum decompression concentrates and will remain on below 60 ℃; Proportion is 1.03～1.05 when concentrating end; The enzyme amount that adds aspartic protease is 40u/ml, and the enzymolysis holding temperature is 50 ℃, and enzymolysis time is 5 hours.
Enzymolysis solution adsorbs with polar macroporous resin, and the absorption flow velocity is 2BV/h, after absorption finishes; Content with acetate is 0.2% (w/v), and the ethanol alcoholic degree is that 10 ° solution carries out the removal of impurities washing to the polar macroporous resin after adsorbing, and wash volumes is 3BV; Content with acetate is 0.2% (w/v) again; The ethanol alcoholic degree is that 60 ° solution carries out wash-out to polar macroporous resin, begins to collect from color burn, and elution volume is 3BV; Elution flow rate is 1BV/h, to must there not being albumen anthocyanogen extract behind the elute soln concentrate drying.Wherein cyaniding 3-0-glucoside content is 32.6%, and protein content is 0.06%.
Embodiment 12
Testa sojae atricolor is extracted as solvent with the glycocoll ethanolic soln, wherein the content of glycocoll is 0.2% (w/v), and the ethanol alcoholic degree is 80 °; Extracting temperature is 50 ℃; Solvent pH value is 2～3, and the glycocoll ethanolic soln is 15: 1 with Testa sojae atricolor gross weight ratio, divides three extractions; Each solution and Testa sojae atricolor weight ratio are 5: 1, extract 2 hours.
Extract the aspartic protease that adds the production of the magnificent prosperous and powerful Bioisystech Co., Ltd in east, Beijing after the solution for vacuum concentrating under reduced pressure desolventizes and carry out enzymolysis; Wherein vacuum decompression concentrates and will remain on below 60 ℃; Proportion is 1.03～1.05 when concentrating end; The enzyme amount that adds aspartic protease is 40u/ml, and the enzymolysis holding temperature is 50 ℃, and enzymolysis time is 5 hours.
Enzymolysis solution adsorbs with polar macroporous resin, and the absorption flow velocity is 2BV/h, after absorption finishes; Content with acetate is 0.2% (w/v), and the ethanol alcoholic degree is that 10 ° solution carries out the removal of impurities washing to the polar macroporous resin after adsorbing, and wash volumes is 3BV; Content with acetate is 0.2% (w/v) again; The ethanol alcoholic degree is that 60 ° solution carries out wash-out to polar macroporous resin, begins to collect from color burn, and elution volume is 3BV; Elution flow rate is 1BV/h, to must there not being albumen anthocyanogen extract behind the elute soln concentrate drying.Wherein cyaniding 3-0-glucoside content is 36.5%, and protein content is 0.07%.
Embodiment 13
According to " modern medicine experiment skill pandect " (square Ford, combined publication society of China Concord Medical Science University of Beijing Medical University, 1995; 469) said method is separated mouse liver cell, and is that the mouse liver cell suspension of 5 * 106/ml divides to big ware every ware 14ml with density.It is listed that the protection group is pressed table 4, adds above no albumen anthocyanogen extract and Folium Ginkgo extract (Folium Ginkgo extract is a standard extract, contains flavones 24%, lactone 6%) respectively, and make that final concentration is respectively 0,0.05,0.10,0.15,0.20mg/ml.Control group and injured group add the PBS with volume; Establish 3 repetitions for every group, place 37 ℃ CO2 incubator to cultivate 2h altogether then, taking out back protection group and injured group accepting agent dose rate is the uviolizing 20min of 760 μ W/cm2; Control group is put the identical time under the fluorescent lamp; Adopt differential centrifugation to extract plastosome, analyze mitochondrial lipoperoxide content, relatively inhibiting rate.The mitochondrial protein assay is standard with the bovine serum albumin with examining Ma Shi light blue staining.The assay of lipoperoxide adopts the TBA colourimetry, is standard with the tetraethoxypropane, representes level of lipid peroxidation with mda (MDA) content.The inhibiting rate calculation formula that lipoperoxide forms is:
Inhibiting rate (%)=(injured group MDA-protection group MDA)/(injured group MDA-control group MDA) * 100%
The anti-oxidant synergy of table 4 no albumen anthocyanogen extract and Folium Ginkgo extract
Suppress counting rate meter (%)
Claims (6)
1. method that from Testa sojae atricolor, prepares the anthocyanogen extract; At first Testa sojae atricolor is extracted with acid solvent; The extraction solution concentration desolventizes back adding aspartic protease and carries out enzymolysis; Enzymolysis solution carries out the desorption wash-out with resin absorption to polymeric adsorbent, and the elute soln concentrate drying must not have albumen anthocyanogen extract after the desorption.
2. the described method of root a tree name claim 1 is characterized in that Testa sojae atricolor being extracted as solvent with the Hydrocerol A ethanolic soln, and wherein the content of Hydrocerol A is 0.1～0.3% (w/v); The ethanol alcoholic degree is 70 °～90 °, and extracting temperature is 45～55 ℃, and solvent pH value is 2～3; The Hydrocerol A ethanolic soln is 15: 1 with Testa sojae atricolor gross weight ratio; Divide and extract for three times, each solution and Testa sojae atricolor weight ratio are 5: 1, extract 2 hours.
3. the described method of root a tree name claim 1; It is characterized in that extracting the solution for vacuum concentrating under reduced pressure and carry out enzymolysis except that adding aspartic protease behind the organic solvent; Wherein vacuum decompression concentrates and will remain on below 60 ℃, and proportion is 1.03～1.05 when concentrating end, and the enzyme amount that adds aspartic protease is 30～50u/ml; The enzymolysis holding temperature is 40～60 ℃, and enzymolysis time is 4～6 hours.
4. the described method of root a tree name claim 1 is characterized in that enzymolysis solution adsorbs with polar macroporous resin, and the absorption flow velocity is 1～3BV/h; After absorption finishes, be 0.2% (w/v) with the content of Hydrocerol A, the ethanol alcoholic degree is that 10 ° the solution polar macroporous resin after to absorption carries out the removal of impurities washing; Wash volumes is 2-4BV, and the content with Hydrocerol A is 0.2% (w/v) again, and the ethanol alcoholic degree is that 50 °～70 ° solution carries out wash-out to polar macroporous resin; Begin to collect from color burn; Elution volume is 2～4BV, and elution flow rate is 0.5～1.5BV/h, to must there not being albumen anthocyanogen extract behind the elute soln concentrate drying.
5. the described method of root a tree name claim 1, the acid solvent that extracts Testa sojae atricolor also comprises phosphoric acid ethanol solution, acetate ethanolic soln, glycocoll ethanolic soln.
6. the described method gained of root a tree name claim 1 does not have albumen anthocyanogen extract, with the application in the oxidation-resisting and caducity medicine of standard silver Fructus Pruni extract.The concentration ratio that does not wherein have albumen anthocyanogen extract and standard silver Fructus Pruni extract is 4: 1～1: 4.
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| CN105670337A (en) * | 2016-03-15 | 2016-06-15 | 常州市阿曼特化工有限公司 | Technology method for extracting pigment from black soy bean peels |
| CN109337407A (en) * | 2018-11-29 | 2019-02-15 | 武汉职业技术学院 | A kind of extraction method of black bean skin natural dye and its application |
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| CN110548039A (en) * | 2019-09-23 | 2019-12-10 | 长春理工大学 | Weight-losing medicine for food-borne obesity and preparation method thereof |
| CN111838674A (en) * | 2020-07-30 | 2020-10-30 | 华中农业大学 | Composition with anti-sugar effect and application thereof |
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| CN116949118A (en) * | 2023-07-24 | 2023-10-27 | 暨南大学 | Black bean skin anthocyanin oleic acid acylation product and preparation method thereof |
| CN116949118B (en) * | 2023-07-24 | 2024-02-20 | 暨南大学 | Black bean skin anthocyanin oleic acid acylation product and preparation method thereof |
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