CN101704898A - Process for extracting amylose of blueberry - Google Patents
Process for extracting amylose of blueberry Download PDFInfo
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- CN101704898A CN101704898A CN200910035421A CN200910035421A CN101704898A CN 101704898 A CN101704898 A CN 101704898A CN 200910035421 A CN200910035421 A CN 200910035421A CN 200910035421 A CN200910035421 A CN 200910035421A CN 101704898 A CN101704898 A CN 101704898A
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- polysaccharide
- blueberry
- macroporous resin
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- nanofiltration membrane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a process for extracting amylose. Fresh blueberry fruits are used as a raw material and subject to zymohydrolysis, leaching, cold pressing, macroporous resin separation, film condensation, freezing and drying to prepare a finished product. The process adopted to produce the amylose has high yield, low energy consumption, low cost, and high output and high purity of the amylase; and the flavor of the amylose is reserved.
Description
Technical field:
The present invention relates to a kind of extraction polysaccharide process, especially a kind of method of from blueberry fresh fruit, extracting polysaccharide.
Background technology:
Blueberry (Blueberry) formal name used at school blueberry, another name have sincere this, pout have a liking for, all persimmon, pasture fruit etc., belong to Ericaceae genus vaccinium plant.It is blue that fruit is, and drape layer white fruit powder, the pulp exquisiteness, and fruity is sour-sweet, and unique flavor has salubrious pleasant fragrance, can eat raw, also can be processed into nectar and fruit wine.The fruits nutrition of blueberry is abundant, the blue berry real analysis measurement result of 14 kinds introducing from the U.S. is shown: contain protein, fat, carbohydrate the blueberry fresh fruit, V
A, V
E, superoxide-dismutase (SOD) etc., other VITAMIN all is higher than other fruit.In addition, the micronutrient levels of blueberry is also very high, calcic, phosphorus, magnesium, zinc, iron, germanium, copper etc. in the fresh fruit.Except that containing common nutritive ingredient, also contain special composition such as nicotinic acid, flavones in the blueberry fruit, nutritious, therefore, often be described as " king of berry ".
Since the eighties, scientists is to vegetable polysaccharides, particularly research has produced keen interest to the polysaccharide in the Chinese medicine, so far reported in succession that kind more than 100 has the herbal polysaccharide of immunomodulatory, multiple physiologically active such as antitumor, antiviral, anti-infective, hypoglycemic, have in clinical assisting therapy and the rehabilitation that is used for tumour, hepatitis, disease such as cardiovascular, wherein most important pharmacological action is when pushing away immunologic enhancement.Existing a large amount of pharmacology and clinical application show, the polysaccharide that these functions are definite, its crude drug in whole belong to help class Chinese medicine mostly.Recent pharmacological research and clinical application show that all it has significant immuno-potentiation, and its effective constituent is polysaccharide or glycoconjugate glycoconjugates, comprise that different its immunocompetent manifestation of glycopeptide such as glycopeptide protein-polysaccharide is also inequality, have to show as cellular immune function strong, have to show as humoral immune function strong, and have also have a significant lipoid peroxidization resistant, the structural analysis that suppresses these glycopeptide compounds of oxidation of LDL shows, their common feature is the polysaccharide content height, what have can be up to 90, the sugar structure has its general character, promptly all be terminal with Ara, but also each tool individual character, the main chain that has is that 1-6 links, have plenty of 1-4 and link, have also in conjunction with pigment.Pharmacological experiments shows also in these glycopeptide compounds that not only overall molecule has immunocompetence, and the polysaccharide chain in the molecule also has immunocompetence, and the effect of the ratio overall molecule that has also is eager to excel.Antitumour drug is because people are dissatisfied to current cancer chemotherapeutic drug as antitumour drug with polysaccharide.Though chemists have synthesized the numerous compound that cancer cells is had quite strong lethal effect, but injuring normal cell too in kill cancer cell, show a lot of side effects clinically, particularly chemotherapeutics causes damage to patient's immunity system, so Polysaccharide Immunoregulators is very attractive on tumor treatment.
Blueberry has abundant polysaccharide content, and the about 6g/100g fresh weight of oligomeric polysaccharide wherein, and the about 4.6g/100g fresh weight of content of cellulose can be used as an important source of vegetable polysaccharides.Still there is not report but the method for extracting polysaccharide from blueberry is domestic.
Summary of the invention:
The objective of the invention is for a kind of product yield height is provided, energy consumption is few, and cost is low, and output is big, and purity of polysaccharide reaches more than 97%, keeps original local flavor, is easy to realize industrialized polysaccharide extracting process.
Preparation method proposed by the invention is as follows:
1) enzymolysis: get blueberry fresh fruit, the deionized water that adds the cellulase of 0.5 times of amount of its weight soaks 3～4h, makes its enzymolysis.
Both extract and the blueberry weave construction can be destroyed with cellulase, make that extraction is easier to be carried out, improve extraction efficiency, also can change into polysaccharide behind the cellulose hydrolysis simultaneously, therefore can improve the extraction yield of polysaccharide.
In the above-mentioned enzymolysis process, the content of cellulase in deionized water is 0.5～3.0%, and regulating pH with hydrochloric acid is 4, and temperature is controlled at 40～45 ℃.
2) squeezing: squeezing at normal temperatures.
Immersion and high-pressure compressing can extract the aqueous soluble active constituent in the blueberry more up hill and dale, destroy the blueberry weave construction by mechanical effect under normal temperature condition, but do not relate to the reaction except that hydrolysis, make things convenient for next step purification operations.
The technology of polysaccharide in the said extracted blueberry, its squeezing process condition is as follows: enzymolysis solution is colded pressing under normal temperature 80～100MPa, soak 0.5～1h with the liquid material than the deionized water that is 0.5, cold pressing under these conditions, collect pressed liquor twice.
3) macroporous resin removal of impurities: the pressed liquor after the merging is through the non-polar macroporous resin removal of impurities.
Non-polar macroporous resin can be adsorbed the unwanted small-molecule substance of this technology at normal temperatures and polysaccharide is passed through, and assurance small molecules effective constituent is separated under situation about not being destroyed, and point of penetration is provided for the upgrading of technology; This technology is to hold back small molecules, sees through required macromolecular polysaccharide, so operation can be shortened the production cycle continuously to a certain extent.
The technology of polysaccharide in the said extracted blueberry is characterized in that described non-polar macroporous resin post can use D101, PSD, HZ802 macroporous resin.
4) macroporous resin adsorption: see through liquid and polysaccharide is adsorbed, use the ethanol elution polysaccharide again with polar macroporous resin.
Polar macroporous resin can adsorb the polysaccharose substance of this arts demand at normal temperatures, can not introduce new impurity, and macroporous resin regeneration simultaneously is convenient, can reuse.
The technology of polysaccharide in the said extracted blueberry is characterized in that described polar macroporous resin can use LSA-5B, D4020, D201 macroporous resin.
The technology of polysaccharide in the said extracted blueberry is characterized in that after the described polar macroporous resin absorption 50～60% ethanol elutions with 3～4 times of amount column volumes.
5) membrane concentration: with the elutriant membrane concentration, must hold back concentrated solution with nanofiltration membrane.
The polysaccharide molecule that the nanofiltration membrane molecular weight cut-off is bigger is further removed small molecular weight impurity, separated from solvent and reach spissated purpose.Operation does not simultaneously relate to heating yet, can effectively keep the local flavor of polysaccharide in the blueberry.
The technology of polysaccharide in the said extracted blueberry is characterized in that described nanofiltration membrane adopts ESNA series nanofiltration membrane or HNF-4040 series nanofiltration membrane.
6) lyophilize: with the concentrated solution lyophilize, promptly.
Freeze-drying and dehydrating is thorough, and the physical structure and the molecule structure change of material are minimum, and local flavor obtains fine reservation, and is convenient to long time stored.
In sum, there is following advantage in the present invention:
1) enzymolysis step makes this technology to raw material utilization more fully arranged, and has improved the yield of product and the output under the same raw materials cost;
2) macroporous resin and membrane sepn all make the treatment condition milder, the intact reservation of glycocalix, and regeneration is simultaneously saved a large amount of energy consumptions and cost easily:
3) lyophilize step has not only improved the purity of finished product, has also guaranteed the original local flavor of polysaccharide.
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:
Get 100g blueberry fresh fruit (total sugar content 10.3%), be dissolved in the 50L deionized water, add the 2.5g cellulase, add hydrochloric acid and regulate pH to 4, after extracting 1h under 40 ℃ of temperature, under 80MPa, cold pressing, residue is used 50L deionized water extraction 1h again, cold pressing, merge pressed liquor, cross the D-101 type macroporous resin column removal of impurities of column volume 5L, must see through liquid, then by LSA-5B type macroporous resin column absorption polysaccharide molecule, then with 15L 50% ethanol elution polysaccharide, with ESNA2 nanofiltration membrane concentrate eluant, the concentrated solution lyophilize finally obtains 8.86g content and is 97.5% polysaccharide finished product.
Embodiment 2:
Get 150g blueberry fresh fruit (total sugar content 10.5%), be dissolved in the 75L deionized water, add the 4.1g cellulase, add hydrochloric acid and regulate pH to 4, after extracting 1h under 42 ℃ of temperature, under 90MPa, cold pressing, residue is used 75L deionized water extraction 1h again, cold pressing, merge pressed liquor, cross the PSD macroporous resin column of column volume 5L and carry out removal of impurities, must see through liquid, adsorb polysaccharide molecule by D4020 type macroporous resin column then, then with 15L 55% ethanol elution polysaccharide, with HNF40-4040 nanofiltration membrane concentrate eluant, the concentrated solution lyophilize finally obtains 12.49g content and is 98.1% polysaccharide finished product.
Embodiment 3:
Get 200g blueberry fresh fruit (total sugar content 10.4%), be dissolved in the 100L deionized water, add the 6.0g cellulase, add hydrochloric acid and regulate pH to 4, after extracting 1h under 45 ℃ of temperature, under 100MPa, cold pressing, residue is used 100L deionized water extraction 1h again, cold pressing, merge pressed liquor, cross the HZ802 macroporous resin column of column volume 5L and carry out removal of impurities, must see through liquid, adsorb polysaccharide molecule by D201 type macroporous resin column then, then with 15L 60% ethanol elution polysaccharide, with HNF70-4040 nanofiltration membrane concentrate eluant, the concentrated solution lyophilize finally obtains 16.27g content and is 97.6% polysaccharide finished product.
Claims (7)
1. a technology of extracting polysaccharide in the blueberry is characterized in that being made up of following steps: get blueberry fresh fruit, add the deionized water immersion 3～4h of the cellulase of 0.5 times of amount of its weight, make its enzymolysis; Squeezing at normal temperatures; Pressed liquor sees through the polar macroporous resin absorption of liquid through the non-polar macroporous resin removal of impurities, uses ethanol elution again; With the elutriant membrane concentration, must hold back concentrated solution with nanofiltration membrane; With the concentrated solution lyophilize, promptly.
2. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that in the described enzymolysis process that the content of cellulase in deionized water is 0.5～3.0%, regulating pH with hydrochloric acid is 4, and temperature is controlled at 40～45 ℃.
3. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that described squeezing process condition is as follows: enzymolysis solution is colded pressing under normal temperature 80～100MPa, soak 0.5～1h with the liquid material than the deionized water that is 0.5, cold pressing under these conditions, collect pressed liquor twice.
4. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that described non-polar macroporous resin post can use D101, PSD, HZ802 macroporous resin.
5. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that described polar macroporous resin can use LSA-5B, D4020, D201 macroporous resin.
6. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that after the described polar macroporous resin absorption 50～60% ethanol elutions with 3～4 times of amount column volumes.
7. according to the technology of polysaccharide in the described extraction blueberry of claim 1, it is characterized in that described nanofiltration membrane adopts ESNA series nanofiltration membrane or HNF-4040 series nanofiltration membrane.
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| CN200910035421A CN101704898A (en) | 2009-09-28 | 2009-09-28 | Process for extracting amylose of blueberry |
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| CN200910035421A CN101704898A (en) | 2009-09-28 | 2009-09-28 | Process for extracting amylose of blueberry |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337315A (en) * | 2011-10-08 | 2012-02-01 | 江苏世东野宝植物资源开发有限公司 | Method for preparing decolorized blueberry polysaccharide |
| CN103039885A (en) * | 2013-01-23 | 2013-04-17 | 贵阳学院 | Juicing method for increasing juice yield of blueberry juice and anthocyanin content in juice |
| CN104530253A (en) * | 2015-02-03 | 2015-04-22 | 上海中医药大学附属龙华医院 | Polygonatum sibiricum polysaccharide column chromatography separation method and extraction method |
| CN105037578A (en) * | 2015-08-24 | 2015-11-11 | 河南大学 | Anticoagulant blackberry seed polysaccharides, and extraction separation method and application thereof |
| CN105037577A (en) * | 2015-08-24 | 2015-11-11 | 河南大学 | Procoagulant blackberry seed polysaccharide, and extraction separation method and application thereof |
| CN110922505A (en) * | 2019-12-27 | 2020-03-27 | 华熙生物科技股份有限公司 | Preparation method of hyaluronic acid for eye drops |
| CN110981992A (en) * | 2019-12-27 | 2020-04-10 | 华熙生物科技股份有限公司 | Preparation method of hyaluronic acid for injection |
-
2009
- 2009-09-28 CN CN200910035421A patent/CN101704898A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337315A (en) * | 2011-10-08 | 2012-02-01 | 江苏世东野宝植物资源开发有限公司 | Method for preparing decolorized blueberry polysaccharide |
| CN103039885A (en) * | 2013-01-23 | 2013-04-17 | 贵阳学院 | Juicing method for increasing juice yield of blueberry juice and anthocyanin content in juice |
| CN104530253A (en) * | 2015-02-03 | 2015-04-22 | 上海中医药大学附属龙华医院 | Polygonatum sibiricum polysaccharide column chromatography separation method and extraction method |
| CN104530253B (en) * | 2015-02-03 | 2019-02-26 | 上海中医药大学附属龙华医院 | A kind of column chromatography separation method and extracting method of Siberian solomonseal rhizome polysaccharide |
| CN105037578A (en) * | 2015-08-24 | 2015-11-11 | 河南大学 | Anticoagulant blackberry seed polysaccharides, and extraction separation method and application thereof |
| CN105037577A (en) * | 2015-08-24 | 2015-11-11 | 河南大学 | Procoagulant blackberry seed polysaccharide, and extraction separation method and application thereof |
| CN105037578B (en) * | 2015-08-24 | 2017-03-29 | 河南大学 | A kind of anticoagulation blackberry seed polysaccharide and its extraction separation method, application |
| CN110922505A (en) * | 2019-12-27 | 2020-03-27 | 华熙生物科技股份有限公司 | Preparation method of hyaluronic acid for eye drops |
| CN110981992A (en) * | 2019-12-27 | 2020-04-10 | 华熙生物科技股份有限公司 | Preparation method of hyaluronic acid for injection |
| CN110981992B (en) * | 2019-12-27 | 2021-08-13 | 华熙生物科技股份有限公司 | Preparation method of hyaluronic acid for injection |
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Application publication date: 20100512 |