CN101830950A - Process for extracting anthocyanin from blueberries - Google Patents
Process for extracting anthocyanin from blueberries Download PDFInfo
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- CN101830950A CN101830950A CN201010182716A CN201010182716A CN101830950A CN 101830950 A CN101830950 A CN 101830950A CN 201010182716 A CN201010182716 A CN 201010182716A CN 201010182716 A CN201010182716 A CN 201010182716A CN 101830950 A CN101830950 A CN 101830950A
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Abstract
The invention relates to a process for extracting anthocyanin from blueberries. The process uses the blueberries as a raw material and comprises the following steps of: pulverizing the raw material and adding acid water with a pH of 1-3 for soaking and extracting; clarifying an obtained extract by using a precipitator; adsorbing by using macroporous resin; eluting by using a 70 percent alcohol solution; ultrafiltering an obtained eluent by using an ultrafiltration membrane and then concentrating by using a nanofiltration membrane; and spraying and drying an obtained concentrated solution to obtain a finished product. By adopting the process to produce the blueberry anthocyanin, the product yield has high cost value ratio, and the energy consumption is less. The process is easy for industrialization.
Description
Technical field:
The present invention relates to a kind of technology of from blueberry, extracting anthocyanogen, especially a kind of technology by macroporous resin separation and membrane concentration extraction anthocyanogen.
Background technology:
Blueberry (Blueberry), the formal name used at school blueberry belongs to Ericaceae genus vaccinium plant.
According to the analysis of U.S. Tufts university, in 40 kinds of vegetables and fruit with anti-oxidant effectiveness, the anthocyanidin content of blueberry ranks the first.The anthocyanidin that blueberry contained is that content is the highest among all fruit and vegetables, and the abundantest part of anthocyanidin of blueberry is exactly at its distinctive purple pericarp position.
Special nutrition compositions such as the contained anthocyanidin of blueberry, organic germanium, organoselenium, ursin, amino acid, tartaric acid are that any plant is all incomparable, especially the anthocyanidin of being made up of 16 kinds of Vitamin P complexs has than the more superior physiologically active of general plant anthocyanidin.Chokeberry more and more receives the concern of food, healthcare products circle in recent years, is because unique nourishing function of blue berry anthocyanogen.Contain abundant anthocyanogen (anthocyanidin) in the fruit of blueberry, mainly contain microbiotic effect, anti-radical action, anti-vision degeneration and arteriosclerosis and thrombotic effect.Cranberry juice can be used for extracting the red pigment of cowberry pigment, is widely used in food color and cosmonaut, student and cooks the healthcare products that prevent that eyesight from reducing and degenerating.
Anthocyanogen is by anthocyanogen aglucon (aglycon) and the class polyphenolic compound of sugar by the glycosidic link be combined into.The basic structure of natural pattern aglucon (anthocyanidin) is 3,5, and 7-trihydroxy--flavylium ion is muttered.Containing a large amount of anthocyanin class materials in the blackberry, blueberry fruit and have very strong anticancer, anti-oxidant, antimycotic, antimutagenic effect, is a kind of good natural food colour.
Anthocyanogen is a water-soluble substances, the mixing solutions that is soluble in methyl alcohol, ethanol, water and forms by them, be insoluble to non-polar solvents such as sherwood oil, ether, its color and stability are subjected to influence of various factors such as structure, temperature, illumination, pH value, auxilliary toner, and are subjected to the various factors effect widely different.
The existing technology of extracting anthocyanogen, there is acid alcohol to extract methods such as macroporous resin partition method, enzyme process extraction using alcohol, supercritical extraction, " progress of anthocyanogen extraction, separation and purification and evaluation " that Yu Dong etc. deliver, existing technology of the report that the document is detailed and relative merits.Patent (publication number 101012256) " a kind of method of extracting the natural pigment anthocyanogen from black rice ", the disclosed method of this patent is extraction using alcohol, concentrated spray drying.Patent (publication number 101434972) " a kind of technology of preparing Lonicera edulis anthocyanin by solid state biological reaction ", the method for this patent disclosure is solid state fermentation, extraction using alcohol, macroporous resin purification etc.Patent (publication number 101045741) " method of separating preparing anthocyan monomer from mulberry fruit ", the method for this patent disclosure are acidifying extraction using alcohol, resin cation (R.C.) absorption, adverse current chromatogram separation etc.
There is following shortcoming in existing in a word technology:
1. extraction using alcohol, solvent loss is big, the cost height.
2. the look price ratio is low, and content is low.
3. industrialization degree is low, and energy consumption is big.
Summary of the invention:
The objective of the invention is in order to provide a kind of energy consumption few, products obtained therefrom content height is easy to realize industrialized anthocyanogen extraction process.
Technical scheme proposed by the invention is as follows:
A kind of technology of extracting anthocyanogen from blueberry is characterized in that being made up of following steps:
1) extracts: blueberry is pulverized, added 2-5 and doubly measure acidic aqueous solution immersion extraction in 2-4 hour 2-5 time, united extraction liquid;
2) resin column separates: said extracted liquid adds precipitation agent, precipitates 4-6 hour, gets supernatant liquor and adds macroporous resin column absorption, and deionized water is washed till sugar-free, with 6-7 times of 70% ethanolic soln wash-out, collects elutriant again;
3) membrane concentration: with above-mentioned elutriant, add the ultra-filtration membrane ultrafiltration, add nanofiltration membrane again through liquid and concentrate, the concentrated solution spraying drying promptly gets anthocyanogen.
Sour water is the sour water of PH1-3 in the step 1), sour optional mineral acid or organic acid.
Step 2) the optional ZTC straight juice of precipitation agent finings, consumption are the 1-5 ‰ of liquid.Preferred ZTC-III type fruit juice clarifier.
Step 2) macroporous resin column can be used non-polar macroporous resin such as X-5, AB-8, D101.
Step 3) membrane concentration condition: ultra-filtration membrane is that molecular weight cut-off is 3000 hollow composite hyperfiltration membrane, and nanofiltration membrane is that molecular weight cut-off is 200 hollow composite nanometer filtering film, and intake pressure is 0.3-0.4Mpa.
In sum, there is following advantage in the present invention:
1) anthocyanogen has better water solubility, is that solvent cost is lower with water
2) precipitation agent can improve extracting solution clarity, improves the macroporous resin adsorption amount.
3) membrane concentration can make the anthocyanogen structure of poor heat stability not be damaged, and has guaranteed yield, has also improved the content and the look price ratio of product.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Getting the 10kg blue berry pulverizes, drop into multi-function extractor, add the aqueous hydrochloric acid of 50Lph1, soaked 2 hours, suction filtration liquid, add the 30ph2L aqueous hydrochloric acid again and soaked 2 hours, behind the suction filtration liquid, continue to add 30L ph3 aqueous hydrochloric acid and soaked 2 hours, suction filtration liquid, merge No. three extracting solutions and add the ZTC-III fruit juice clarifier 320ml for preparing, mixed precipitation 4 hours, filter the absorption of adding 2LX-5 macroporous resin column, flow velocity 15L/h, adsorb saturated after, deionized water is washed till no fried sugar, uses 12L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collects to see through liquid to add molecular weight cut-off again be 200 concentrate, collect concentrated solution, spraying drying gets anthocyanogen product 65g, content 85%.
Embodiment 2:
Getting the 10kg blue berry pulverizes, drop into multi-function extractor, the aqueous citric acid solution that adds 50Lph2, soaked 4 hours, suction filtration liquid adds the 50Lph2L aqueous citric acid solution again and soaked suction filtration liquid 4 hours, united extraction liquid adds the ZTC-III fruit juice clarifier 300ml for preparing, and mixes precipitation 6 hours.Filter extracting solution and add the absorption of 2LD101 macroporous resin column, flow velocity 10L/h, adsorb saturated after, deionized water is washed till no fried sugar, use 14L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collect seeing through liquid, to add molecular weight cut-off again be that 200 hollow composite membrane nanofiltration concentrates, and collects concentrated solution, spraying drying, get anthocyanogen product 60g, content 82%.
Embodiment 3:
Getting the 10kg blue berry pulverizes, drop into multi-function extractor, the aqueous sulfuric acid that adds 50Lph2, soaked 4 hours, suction filtration liquid adds the ZTC-III fruit juice clarifier 100ml for preparing and mixed precipitation 4 hours, adding the 50Lph2L aqueous sulfuric acid in the extractor again soaked 4 hours, suction filtration liquid, add the ZTC-III fruit juice clarifier 80ml for preparing, mixed precipitation 4 hours, filter extracting solution and add the absorption of 2LX-5 macroporous resin column, flow velocity 10L/h, adsorb saturated after, deionized water is washed till no fried sugar, uses 14L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collects to see through liquid to add molecular weight cut-off again be that 200 hollow composite membrane nanofiltration concentrates, collect concentrated solution, spraying drying gets anthocyanogen product 62g, content 80%.
Embodiment 4:
Getting the 50kg blue berry pulverizes, drop into multi-function extractor, the aqueous citric acid solution that adds 250Lph2, soaked 4 hours, suction filtration liquid adds the ZTC-III fruit juice clarifier 250ml for preparing and mixed precipitation 6 hours, adding the 50Lph2L aqueous citric acid solution in the extractor again soaked 4 hours, suction filtration liquid, add the ZTC-III fruit juice clarifier 80ml for preparing, mixed precipitation 4 hours, filter extracting solution and add the absorption of 10LAB-8 macroporous resin column, flow velocity 60L/h, adsorb saturated after, deionized water is washed till no fried sugar, uses 60L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collects to see through liquid to add molecular weight cut-off again be that 200 hollow composite membrane nanofiltration concentrates, collect concentrated solution, spraying drying gets anthocyanogen product 300g, content 80%.
Embodiment 5:
Getting the 100kg blue berry pulverizes, drop into multi-function extractor, the aqueous sulfuric acid that adds 500Lph2, soaked 4 hours, suction filtration liquid adds the ZTC-III fruit juice clarifier 1000ml for preparing and mixed precipitation 4 hours, adding the 500Lph2L aqueous sulfuric acid in the extractor again soaked 4 hours, suction filtration liquid, add the ZTC-III fruit juice clarifier 700ml for preparing, mixed precipitation 4 hours, filter extracting solution and add the absorption of 20LX-5 macroporous resin column, flow velocity 100L/h, adsorb saturated after, deionized water is washed till no fried sugar, uses 120L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collects to see through liquid to add molecular weight cut-off again be that 200 hollow composite membrane nanofiltration concentrates, collect concentrated solution, spraying drying gets anthocyanogen product 630g, content 83%.
Embodiment 6:
Getting the 100kg blue berry pulverizes, drop into multi-function extractor, the aqueous hydrochloric acid that adds 200Lph12, soaked 2 hours, suction filtration liquid extracts 5 times, and united extraction liquid adds the ZTC-III fruit juice clarifier 4L for preparing, mixed precipitation 3 hours, filter to add the absorption of 20LAB-8 macroporous resin column, flow velocity 100L/h, adsorb saturated after, deionized water is washed till no fried sugar, use 120L70% ethanolic soln wash-out again, collect elutriant, add the hollow composite membrane ultrafiltration of molecular weight cut-off 3000, intake pressure is controlled to be in the 0.3-0.4Mpa scope, collect seeing through liquid, to add molecular weight cut-off again be that 200 hollow composite membrane nanofiltration concentrates, and collects concentrated solution, spraying drying, get anthocyanogen product 700g, content 80%.
Claims (5)
1. technology of extracting anthocyanogen from blueberry is characterized in that being made up of following steps:
1) extracts: blueberry is pulverized, added 2-5 and doubly measure acidic aqueous solution immersion extraction in 2-4 hour 2-5 time, united extraction liquid;
2) resin column separates: said extracted liquid adds precipitation agent, precipitates 4-6 hour, gets supernatant liquor and adds macroporous resin column absorption, and deionized water is washed till sugar-free, with 6-7 times of 70% ethanolic soln wash-out, collects elutriant again;
3) membrane concentration: with above-mentioned elutriant, add the ultra-filtration membrane ultrafiltration, add nanofiltration membrane again through liquid and concentrate, the concentrated solution spraying drying promptly gets anthocyanogen.
2. according to the described technology of from blueberry, extracting anthocyanogen of claim 1, it is characterized in that sour water is the sour water of PH1-3 in the described step 1), sour optional mineral acid or organic acid.
3. according to the described technology of from blueberry, extracting anthocyanogen of claim 1, it is characterized in that described step 2) the optional ZTC straight juice of precipitation agent finings, consumption is the 1-5 ‰ of liquid.
4. according to the described technology of from blueberry, extracting anthocyanogen of claim 1, it is characterized in that described step 2) macroporous resin column can use non-polar macroporous resin such as X-5, AB-8, D101.
5. according to the described technology of from blueberry, extracting anthocyanogen of claim 1, it is characterized in that described step 3) membrane concentration condition: ultra-filtration membrane is that molecular weight cut-off is 3000 hollow composite hyperfiltration membrane, nanofiltration membrane is that molecular weight cut-off is 200 hollow composite nanometer filtering film, and intake pressure is 0.3-0.4Mpa.
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Cited By (21)
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CN102178325A (en) * | 2011-04-11 | 2011-09-14 | 浙江师范大学 | Preparation method of antioxidant in blueberry leaves |
CN102285953A (en) * | 2011-07-01 | 2011-12-21 | 湖南农业大学 | Method for separating and purifying blueberry anthocyanidin by using HP2MGL macroporous resin |
CN102443029A (en) * | 2010-10-01 | 2012-05-09 | 华中农业大学 | Column chromatography method for high-efficiency separation and purification of blood orange anthocyanins |
CN102690251A (en) * | 2012-06-17 | 2012-09-26 | 哈尔滨市海澳斯生物科技开发有限公司 | Extraction method of blueberry anthocyanin |
CN103113341A (en) * | 2013-02-01 | 2013-05-22 | 江苏万村爱农农业科技有限公司 | Process for extracting blueberry anthocyanin |
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CN103599164A (en) * | 2013-11-08 | 2014-02-26 | 天津大学 | Separation method of blueberry polyphenol |
CN103664856A (en) * | 2013-11-25 | 2014-03-26 | 宁波绿之健药业有限公司 | Cranberry extraction method |
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Application publication date: 20100915 |