CN101586137B - Method for adding ethanol to enhance beta-cyclodextrin yield - Google Patents
Method for adding ethanol to enhance beta-cyclodextrin yield Download PDFInfo
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- CN101586137B CN101586137B CN2009100337226A CN200910033722A CN101586137B CN 101586137 B CN101586137 B CN 101586137B CN 2009100337226 A CN2009100337226 A CN 2009100337226A CN 200910033722 A CN200910033722 A CN 200910033722A CN 101586137 B CN101586137 B CN 101586137B
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Abstract
A method for adding ethanol to enhance the beta-cyclodextrin yield belongs to the cyclodextrin production technology field. The invention utilizes the cyclodextrin glycosyltransferase to catalyze the starch to transform and produce the beta-cyclodextrin, adds the ethanol in the reaction liquid to improve the beta-cyclodextrin yield. The method comprises: blending the starch milk with the mass concentration of 15-30%; stirring for 30-120 minutes at 80-90 DEG C, regulating the temperature to 50-60 DEG C, adding the cyclodextrin glycosyltransferase based on the concentration of 3-8 U in 1g starchand adding ethanol; completely reacting for 8-12 hours after the ethanol adding quantity achieves 0.1mL-0.5mL in 1g starch, regulating pH value to 6-9 in the transforming process, filtering, crystall izing and obtaining the beta-cyclodextrin products. The method has no process for recovering the organic solvent and greatly enhances the beta-cyclodextrin yield. The product beta-cyclodextrin has no organic solvent residues.
Description
Technical field
A kind of method of adding ethanol raising beta-cyclodextrin productive rate utilizes starch to add the method that ethanol improves the production Schardinger dextrins of beta-cyclodextrin productive rate as raw material and in reaction solution, belongs to the Schardinger dextrins production technical field.
Background technology
(cyclodextrin is that (cyclodextrin glycosyltransferase CGTase) acts on starch and one type of cyclic oligosaccharide producing to the cyclomaltodextrin glucanotransferase that produces of some bacterial classification by Bacillus (Bacillus) CD) to Schardinger dextrins.Schardinger dextrins has in outer hydrophilic, the ring of a ring hydrophobic and the three-dimensional chirality cavity of certain size is arranged, and this special construction makes it have many special physico-chemical properties.Its ring texture and cavity can the envelope different compounds; Like organic molecule, mineral compound etc.; Form inclusion compound, in fields such as food, medicine, chemical industry and environmental protection important purposes is arranged as the carrier of quality improver, stablizer, medicine and sorbent material etc.
The production technique of existing beta-cyclodextrin is following mostly:
Carry out starch according to the certain quality percentage concentration and size mixing, add cyclomaltodextrin glucanotransferase then, be warming up to 90 ℃~100 ℃ liquefaction behind the thorough mixing, be cooled to 50 ℃~60 ℃ again; Add cyclomaltodextrin glucanotransferase, regulate pH, add the organic solvent that Schardinger dextrins is had the complex-precipitation effect again, reacted 14~48 hours to the best use of conditioned response of enzyme 1~2 hour; Add AMS, adjusting pH is 6.0~6.5, is warming up to 80 ℃~85 ℃ and keeps 15~20min (the not reacted starch or the dextrin that extraction are had negative impact are removed in secondary liquefaction), continues to be warming up to 90 ℃~100 ℃ and fully reacts 8~10 hours; Reclaim organic solvent, crystallization obtains thick beta-cyclodextrin, and repeatedly clean then purifying makes the beta-cyclodextrin product.The shortcoming of this technology is to need secondary liquefaction in the production process and reclaim organic solvent, and repeatedly heating and cooling process is arranged, long reaction time, and energy consumption is big; The organic solvent that this process is used is generally toxic agent (hexanaphthene, toluene etc.), and residual organic solvent has limited the use range of Schardinger dextrins in the product, particularly in food and medicine, and brings certain influence to environment.Along with industrialized process, China has become a country that environmental pollution is comparatively serious, and this also is the negative impact that Economic development brought.Therefore when improving output, to pay attention to the protection of security of products and environment.
Cyclomaltodextrin glucanotransferase has the effect of catalytic cyclization, coupling and hydrolysis simultaneously; Cyclic action generates Schardinger dextrins; Coupling is the side reaction of cyclisation, and small molecular sugar is the substrate of coupled reaction, and hydrolytic action is meant that Schardinger dextrins can be hydrolyzed when cyclic action does not account for leading role; The existence of small molecular sugar suppresses cyclization and promotes coupling and hydrolysis reaction, thereby has influenced ultimate yield.
Summary of the invention
The purpose of this invention is to provide a kind of method that ethanol improves the beta-cyclodextrin productive rate of adding.
Technical scheme of the present invention: a kind of method that improves the beta-cyclodextrin productive rate; Utilize cyclomaltodextrin glucanotransferase catalysis starch to transform and produce beta-cyclodextrin; In reaction solution, add ethanol to improve the beta-cyclodextrin productive rate, technology is: modulation starch quality concentration is 15%~30% milk of starch, stirs 30~120 minutes down at 80~90 ℃; Again with temperature regulation to 50~60 ℃; The concentration that adds 3~8 enzymes unit alive according to every gram starch adds cyclomaltodextrin glucanotransferase, and add ethanol again: addition is after every gram starch adds the ethanol of 0.1mL~0.5mL, conversion reaction 8~12 hours; Regulate pH value 6~9 in the conversion process, filtrating adopts the crystalline means to obtain the beta-cyclodextrin product after filtering.
Used starch is selected the mixture of W-Gum, tapioca(flour), wheat starch, yam starch or different sorts starch for use.
The beta-cyclodextrin product that makes is applied in the strict no complexing agent hexanaphthene of the product quality requirement residual medicine and food service industry.
Beneficial effect of the present invention: compare with the production technique of existing beta-cyclodextrin; Improvements of the present invention are: the one, add ethanol in process of production; The coupling and the hydrolytic action that can suppress cyclomaltodextrin glucanotransferase in the production process to a certain extent, the productive rate of raising beta-cyclodextrin.The 2nd, the ethanol that is added in process of production is different from other organic solvents, and ethanol is volatile, and addition is less; Organic solvent ethanol is residual few in the product beta-cyclodextrin; And the process that reclaims organic solvent has been saved in the toxicological harmless spinoff of residual ethanol own, has saved energy consumption and time.The 3rd, compare with existing manufacturing technique; The productive rate of Schardinger dextrins improves greatly; The productive rate that does not add the mode of production beta-cyclodextrin of complexing agent is about 25%-30%; The productive rate that adds the mode of production beta-cyclodextrin of complexing agent is about 45%-50%, and adopts the productive rate of the beta-cyclodextrin that this technology produces can reach 55%-65%.The 4th, the prepared beta-cyclodextrin of the present invention does not have the organic solvent residual problem of toxic action, and its range of application can not be restricted, and can be used in the product quality requirement higher medicine and food service industry.
In a word, the reagent cost that enforcement of the present invention is added is low, and addition is few, and is simple to operate, and productive rate is high, and there is not the toxic substance residue problem in the product of producing, can be widely used in the industry to the product requirement strictness.This method can significantly improve the productive rate of beta-cyclodextrin with in process of production.
Embodiment
Embodiment 1
This instance provides the comparison of not adding ethanol, interpolation complexing agent hexanaphthene, adding ethanol gained beta-cyclodextrin productive rate respectively.
The corn starch milk mass concentration is 30g/100g, and pH 7.5,60 ℃ of enzymatic reaction temperature, and the cyclomaltodextrin glucanotransferase addition is 5 enzymes of every gram starch units alive, transformation time is 12 hours.
The comparison of table 1:3 kind working method beta-cyclodextrin productive rate
Method | 1 | 2 | 3 |
Productive rate | 29.67% | 50.87% | 60.21% |
Method 1 is not added alcoholic acid technology in the production process.
The technology that method 2 is added the complexing agent hexanaphthene for production process, complexing agent hexanaphthene addition is a 0.4mL/g starch.
Method 3 is to add the alcoholic acid novel process in the production process of the present invention, and the ethanol addition is a 0.4mL/g starch.
Embodiment 2
Configuration quality concentration is the corn starch milk of 15g/100g, stirs 60 minutes down 80 ℃ of high temperature, again with temperature regulation to 56 ℃; Concentration according to 6 enzymes of every gram starch unit alive adds cyclomaltodextrin glucanotransferase, adds ethanol 0.5mL/g starch again, fully reacts 12 hours; Regulate the pH value with usual manner in the conversion process; PH is controlled at 8, adopts the crystallization means to obtain beta-cyclodextrin after filtering, and the productive rate of final beta-cyclodextrin is 63.32%.
Claims (2)
1. method that improves the beta-cyclodextrin productive rate; It is characterized in that utilizing cyclomaltodextrin glucanotransferase catalysis starch to transform and produce beta-cyclodextrin; In reaction solution, add ethanol to improve the beta-cyclodextrin productive rate, technology is: modulation starch quality concentration is 15%~30% milk of starch, stirs 30~120 minutes down at 80~90 ℃; Again with temperature regulation to 50~60 ℃; The concentration that adds 3~8 enzymes unit alive according to every gram starch adds cyclomaltodextrin glucanotransferase, and add ethanol again: addition is after every gram starch adds the ethanol of 0.1mL~0.5mL, conversion reaction 8~12 hours; Regulate pH value 6~9 in the conversion process, filtrating adopts the crystalline means to obtain the beta-cyclodextrin product after filtering.
2. method according to claim 1 is characterized in that used starch selects the mixture of W-Gum, tapioca(flour), wheat starch, yam starch or different sorts starch for use.
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Cited By (1)
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CN102936607A (en) * | 2012-12-10 | 2013-02-20 | 广西高源淀粉有限公司 | Preparation method of Beta-cyclodextrin |
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CN102660608A (en) * | 2012-04-25 | 2012-09-12 | 云南师范大学 | Preparation method of beta-cyclodextrin |
CN102827900B (en) * | 2012-09-10 | 2015-09-23 | 江南大学 | A kind of biological process produces the production technique of γ-cyclodextrin |
CN104151451B (en) * | 2014-08-22 | 2016-04-20 | 淄博千汇生物科技有限公司 | A kind of preparation method of hydroxypropyl-beta-cyclodextrin |
CN104593453B (en) * | 2015-02-05 | 2018-04-06 | 江南大学 | A kind of method for improving enzyme process and preparing beta cyclodextrin yield |
CN111394406B (en) * | 2020-04-03 | 2022-05-31 | 淄博千汇生物科技有限公司 | Preparation method of gamma-cyclodextrin |
CN112048498B (en) * | 2020-09-14 | 2023-10-03 | 江苏省奥谷生物科技有限公司 | Preparation method for improving beta-cyclodextrin yield |
Citations (2)
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CN1850867A (en) * | 2006-05-26 | 2006-10-25 | 陕西省微生物研究所 | Method for directly preparing malt sugar group-beta-cyclodextrin using starch |
CN101319243A (en) * | 2008-07-02 | 2008-12-10 | 江南大学 | Process for preparing cyclodextrin |
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CN1850867A (en) * | 2006-05-26 | 2006-10-25 | 陕西省微生物研究所 | Method for directly preparing malt sugar group-beta-cyclodextrin using starch |
CN101319243A (en) * | 2008-07-02 | 2008-12-10 | 江南大学 | Process for preparing cyclodextrin |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102936607A (en) * | 2012-12-10 | 2013-02-20 | 广西高源淀粉有限公司 | Preparation method of Beta-cyclodextrin |
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