CN106755202A - A kind of preparation method of maltose beta cyclodextrin - Google Patents
A kind of preparation method of maltose beta cyclodextrin Download PDFInfo
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- CN106755202A CN106755202A CN201611063425.2A CN201611063425A CN106755202A CN 106755202 A CN106755202 A CN 106755202A CN 201611063425 A CN201611063425 A CN 201611063425A CN 106755202 A CN106755202 A CN 106755202A
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/16—Preparation of compounds containing saccharide radicals produced by the action of an alpha-1, 6-glucosidase, e.g. amylose, debranched amylopectin
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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Abstract
The present invention relates to cyclodextrin manufacture field, a kind of preparation method of maltose beta cyclodextrin is particularly disclosed.The preparation method of the maltose beta cyclodextrin, with beta cyclodextrin and maltose as raw material, it is characterized by：Beta cyclodextrin is added to the water dissolving, reaction solution is subsequently adding, 3/4 maltose and Pullulanase is added, reaction system is carried out ultrasonically treated, the maltose for adding remaining 1/4 continues to react；Mixed solution to terminating reaction heats the enzyme that goes out；Maltose beta cyclodextrin is isolated and purified, then it is concentrated, dry, obtain product.The present invention improves enzymatic activity, heat endurance and the enzyme efficiency of Pullulanase by way of metal ion activation, ultrasonic assistant, stream are with maltose, it is ensured that the completion catalytic reaction that it can be rapidly and efficiently, shortens the reaction time, improves product yield.
Description
（One）Technical field
The present invention relates to cyclodextrin manufacture field, more particularly to a kind of preparation method of maltose-beta cyclodextrin.
（Two）Background technology
Cyclodextrin is the cyclic oligosaccharide that α -1,4 glycosidic bonds produced by cyclodextrin glycosyl transferases effect starch are formed by connecting.
Cyclodextrin has unique cavity configuration, it is included by intermolecular interaction with many guest molecules, for example
Organic molecule, inorganic compound and rare gas etc., so as to form the compound of Subjective and Objective.Can be formed according to cyclodextrin
The property of host-guest complex, can be widely applied to the industries such as pharmacy, chemical industry, food.It is residual containing 6,7 and 8 glucose
The cyclodextrin of base be referred to as α-, β-and gamma-cyclodextrin.Beta-schardinger dextrin is strong because of its Binding ability, simple production process, cost
It is cheap, it is unique largely production and wide variety of product industrial at present.But the general dissolubility of beta-schardinger dextrin is smaller（25
DEG C, 1.8g/100mL H2O）, this just greatly limit its range of application.
Maltose-beta cyclodextrin is the derivative of cyclodextrin, and 1 is coupled on the 6th hydroxyl of carbon atom of beta cyclodextrin molecule
The branched cyclodextrin of individual malt saccharide residue, it is water-soluble（25 DEG C, 151g/100mL H2O）It is much higher than its corresponding β-ring paste
More than 100 times of essence, and can dissolve many oily substances.Biological safety and availability are high simultaneously.Therefore, maltosyl beta-cyclodextrin
Range of application is wider, with more application future, has a extensive future.Maltose-beta cyclodextrin synthesis mainly uses enzymatic clarification, for example
Maltodextrin transglucosidase, Pullulanase, immobilised enzymes.But at present due to being high temperature, high viscosity, half in reaction condition
Under solid-state, maltose-beta cyclodextrin synthesis is caused to remain the shortcoming that the reaction time is long, reaction efficiency is low.
（Three）The content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided the maltose-β rings paste that a kind of step is simple, product yield is high
The preparation method of essence.
The present invention is achieved through the following technical solutions：
A kind of preparation method of maltose-beta cyclodextrin, with beta-schardinger dextrin and maltose as raw material, comprises the following steps：
（1）Beta-schardinger dextrin is added to the water dissolving, reaction solution is subsequently adding, 3/4 maltose and Pullulanase is added,
The pH value for adjusting mixed solution is 4-5；
（2）At 70-75 DEG C, mixed solution is carried out every 0.5 hour ultrasonically treated 0.5 hour, reaction is carried out 8-10 hours, then
Remaining 1/4 maltose is added to continue to react, the pH that mixed solution is maintained in course of reaction is 4-5, whole course of reaction is 12-
16 hours；
（3）Mixed solution to terminating reaction heats the enzyme that goes out；
（4）Maltose-beta cyclodextrin is isolated and purified, then it is concentrated, dry, obtain product.
The present invention is acted on by the reverse reaction of Pullulanase, prepares branched cyclodextrin, by metal ion activation, ultrasound
Ripple auxiliary, stream improve the enzymatic activity and heat endurance of Pullulanase with the mode of maltose, it is ensured that it can be complete in high temperature, short time
Into catalytic reaction, shorten the reaction time, improve product yield.
More excellent technical scheme of the invention is：
Step（1）In, the weight proportion of each raw material is, maltose 40%, beta-schardinger dextrin 10-15%, reaction solution 30%, water 15-
20%, the addition of Pullulanase is 200-300U/g beta-schardinger dextrins.
The reaction solution is the ethanol solution of the mass concentration 15-20% for being added with calcium chloride and magnesium chloride mixture, chlorine
The addition for changing calcium and magnesium chloride mixture is the 0.2-0.5% of ethanol solution quality, and the ratio of calcium chloride and magnesium chloride is 3-5:
1。
Beta-schardinger dextrin is added in 90 DEG C of water and is dissolved, after temperature is down to 70-75 DEG C, add reaction solution, used
Hydrochloric acid adjusts the pH value of mixed solution.
Step（2）In, sonification power is 3-5w/g.
Step（3）In, mixed solution is heated to 100 DEG C, and go out enzyme 15min.
Step（4）In, use molecular cut off tentatively to be divided maltose-beta cyclodextrin for the NF membrane of 200-400
From, then isolated and purified using sephadex G -15；Eluent concentration is the 1/8 of original volume, under 80 DEG C of vacuum conditions
Dry, dry to moisture and be less than 13%, obtain maltose-beta cyclodextrin product.
Maltose-beta cyclodextrin preparation method that the present invention is provided, has the advantages that the reaction time is short, and the reaction time is by general
40 hours or so of logical preparation method, shorten to 12-16 hour, also have the advantages that reaction efficiency is high, malt-base β-ring
Dextrin conversion ratio reaches 68%, and relatively common preparation method improves nearly 30%.
The present invention improves the enzyme activity of Pullulanase by way of metal ion activation, ultrasonic assistant, stream are with maltose
Property, heat endurance and enzyme efficiency, it is ensured that the completion catalytic reaction that it can be rapidly and efficiently, shorten the reaction time, improve product yield.
（Four）Specific embodiment
Embodiment 1：The preparation of maltose-beta cyclodextrin
（1）The preparation of reaction solution：15% ethanol solution is prepared, then again to adding CaCl in the ethanol solution2And MgCl2
Mixture, CaCl2And MgCl2The addition of mixture is 0.2%, CaCl of ethanol solution quality2And MgCl2Ratio be 3：1.
（2）Add raw material and enzyme：Beta-schardinger dextrin is added in 90 DEG C of water is in proportion dissolved, temperature is reduced to 70 DEG C, plus
Enter reaction solution, add 3/4 maltose, enzyme concentration is 200U/g beta-schardinger dextrins, using salt acid for adjusting pH to 4.
（3）Ultrasonic assistant reacts：Under the conditions of 70 DEG C, ultrasonically treated 0.5 is carried out to reaction system every 0.5 hour small
When, sonification power is 3w/g.Reaction is carried out 8 hours, and the maltose for adding remaining 1/4 continues to react, in course of reaction
PH4 is maintained, is that whole course of reaction was controlled at 12 hours.
（4）Terminate reaction：Reaction system is heated to 100 DEG C, 15 minutes enzymes that go out.
（5）Isolate and purify：Use molecular cut off carries out initial gross separation for 200 NF membrane to maltose-beta cyclodextrin,
Isolated and purified using SephadexG15.
（6）Concentrate drying：Eluent concentration is the 1/8 of original volume, is dried under 80 DEG C of vacuum conditions, dries to moisture and contains
Amount is less than 13%, obtains maltose-beta cyclodextrin product；After measured, maltosyl beta-cyclodextrin conversion ratio is 65%.
Embodiment 2：The preparation of maltose-beta cyclodextrin
（1）The preparation of reaction solution：20% ethanol solution is prepared, then again to adding CaCl in the ethanol solution2And MgCl2
Mixture, CaCl2And MgCl2The addition of mixture is 0.5%, CaCl of ethanol solution quality2And MgCl2Ratio be 5：1.
（2）Add raw material and enzyme：Beta-schardinger dextrin is added in 90 DEG C of water is in proportion dissolved, temperature is reduced to 75 DEG C, plus
Enter reaction solution, add 3/4 maltose, enzyme concentration is 300U/g beta cyclodextrins, using salt acid for adjusting pH to 5.
（3）Ultrasonic assistant reacts：Under the conditions of 75 DEG C, ultrasonically treated 0.5 is carried out to reaction system every 0.5 hour small
When, sonification power is 5w/g.Reaction is carried out 10 hours, and the maltose for adding remaining 1/4 continues to react, in course of reaction
PH5 is maintained, is that whole course of reaction was controlled at 16 hours.
（4）Terminate reaction：Reaction system is heated to 100 DEG C, 15 minutes enzymes that go out.
（5）Isolate and purify：Use molecular cut off carries out initial gross separation for 400 NF membrane to maltose-beta cyclodextrin,
Isolated and purified using SephadexG15.
（6）Concentrate drying：Eluent concentration is the 1/8 of original volume, is dried under 80 DEG C of vacuum conditions, dries to moisture and contains
Amount is less than 13%, obtains maltose-beta cyclodextrin product；After measured, maltosyl beta-cyclodextrin conversion ratio is 68%.
Embodiment 3：The preparation of maltose-beta cyclodextrin
（1）The preparation of reaction solution：18% ethanol solution is prepared, then again to adding CaCl in the ethanol solution2And MgCl2
Mixture, CaCl2And MgCl2The addition of mixture is 0.4%, CaCl of ethanol solution quality2And MgCl2Ratio be 4：1.
（2）Add raw material and enzyme：Beta-schardinger dextrin is added in 90 DEG C of water is in proportion dissolved, temperature is reduced to 72 DEG C, plus
Enter reaction solution, add 3/4 maltose, enzyme concentration is 250U/g beta cyclodextrins, using salt acid for adjusting pH to 4.5.
（3）Ultrasonic assistant reacts：Under the conditions of 72 DEG C, ultrasonically treated 0.5 is carried out to reaction system every 0.5 hour small
When, sonification power is 4w/g.Reaction is carried out 9 hours, and the maltose for adding remaining 1/4 continues to react, in course of reaction
PH4.5 is maintained, is that whole course of reaction was controlled at 14 hours.
（4）Terminate reaction：Reaction system is heated to 100 DEG C, 15 minutes enzymes that go out.
（5）Isolate and purify：Use molecular cut off carries out initial gross separation for 300 NF membrane to maltose-beta cyclodextrin,
Isolated and purified using SephadexG15.
（6）Concentrate drying：Eluent concentration is the 1/8 of original volume, is dried under 80 DEG C of vacuum conditions, dries to moisture and contains
Amount is less than 13%, obtains maltose-beta cyclodextrin product；After measured, maltosyl beta-cyclodextrin conversion ratio is 66%.
Claims (7)
1. a kind of preparation method of maltose-beta cyclodextrin, with beta-schardinger dextrin and maltose as raw material, it is characterized by, including it is as follows
Step：（1）Beta-schardinger dextrin is added to the water dissolving, reaction solution is subsequently adding, 3/4 maltose and Propiram is added
Enzyme, the pH value for adjusting mixed solution is 4-5；（2）At 70-75 DEG C, ultrasonically treated 0.5 is carried out to mixed solution every 0.5 hour
Hour, reaction is carried out 8-10 hours, and the maltose for adding remaining 1/4 continues to react, and mixed solution is maintained in course of reaction
PH is 4-5, and whole course of reaction is 12-16 hours；（3）Mixed solution to terminating reaction heats the enzyme that goes out；（4）To maltose-β
Cyclodextrin is isolated and purified, then concentrated, dry, obtains product.
2. the preparation method of maltose-beta cyclodextrin according to claim 1, it is characterised in that：Step（1）In, each raw material
Weight proportion be, maltose 40%, beta-schardinger dextrin 10-15%, reaction solution 30%, water 15-20%, the addition of Pullulanase is
200-300U/g beta-schardinger dextrins.
3. the preparation method of maltose-beta cyclodextrin according to claim 1 and 2, it is characterised in that：Step（1）In, institute
State the ethanol solution that reaction solution is the mass concentration 15-20% for being added with calcium chloride and magnesium chloride mixture, calcium chloride and chlorination
The addition of magnesium compound is the 0.2-0.5% of ethanol solution quality, and the ratio of calcium chloride and magnesium chloride is 3-5:1.
4. the preparation method of maltose-beta cyclodextrin according to claim 1 and 2, it is characterised in that：Step（1）In, will
Beta-schardinger dextrin dissolves in being added to 90 DEG C of water, after temperature is down to 70-75 DEG C, adds reaction solution, mixed using hydrochloric acid regulation
Close the pH value of solution.
5. the preparation method of maltose-beta cyclodextrin according to claim 1, it is characterised in that：Step（2）In, at ultrasound
Reason power is 3-5w/g.
6. the preparation method of maltose-beta cyclodextrin according to claim 1, it is characterised in that：Step（3）In, mix molten
Liquid is heated to 100 DEG C, and go out enzyme 15min.
7. the preparation method of maltose-beta cyclodextrin according to claim 1, it is characterised in that：Step（4）In, using cut
The NF membrane for staying molecular weight to be 200-400 carries out initial gross separation to maltose-beta cyclodextrin, then is entered using sephadex G -15
Row is isolated and purified；Eluent concentration is the 1/8 of original volume, is dried under 80 DEG C of vacuum conditions, dries to moisture and is less than
13%, obtain maltose-beta cyclodextrin product.
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| CN201611063425.2A CN106755202A (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of maltose beta cyclodextrin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107262664A (en) * | 2017-08-21 | 2017-10-20 | 马鞍山市三川机械制造有限公司 | A kind of Automobile flywheel shell moulding sand for casting |
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| CN1974604A (en) * | 2006-12-08 | 2007-06-06 | 江南大学 | Prepn process of branched cyclodextrin |
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2016
- 2016-11-28 CN CN201611063425.2A patent/CN106755202A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974604A (en) * | 2006-12-08 | 2007-06-06 | 江南大学 | Prepn process of branched cyclodextrin |
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| 于博: "普鲁兰酶的反向合成特性及应用研究", 《中国优秀博士学位论文全文数据库工程科技I辑》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107262664A (en) * | 2017-08-21 | 2017-10-20 | 马鞍山市三川机械制造有限公司 | A kind of Automobile flywheel shell moulding sand for casting |
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Application publication date: 20170531 |