CN109265570A - A method of efficiently preparing nanometer starch crystal - Google Patents
A method of efficiently preparing nanometer starch crystal Download PDFInfo
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- CN109265570A CN109265570A CN201811175179.9A CN201811175179A CN109265570A CN 109265570 A CN109265570 A CN 109265570A CN 201811175179 A CN201811175179 A CN 201811175179A CN 109265570 A CN109265570 A CN 109265570A
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- linear dextrin
- polyethylene glycol
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/06—Drying; Forming
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- C08B30/04—Extraction or purification
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- 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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- 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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Abstract
A method of nanometer starch crystal efficiently being prepared, belongs to starch manufacture field.The method of the present invention combination waxy starch takes off branch and prepares linear dextrin, reduces linear dextrin molecular weight distribution by classification, accelerates linear dextrin to be self-assembly of the technologies such as nanometer starch crystal in conjunction with polyethylene glycol precipitation and prepares nanometer starch crystal.Key step includes: waxy starch gelatinization, and the de- branch of Pullulanase obtains linear dextrin solution, ethyl alcohol is slowly added to while stirring and makes linear dextrin solution and ethyl alcohol volume ratio for 3:1, continues to stir 10min, and in 4 DEG C of standing 1h, centrifugation removes precipitating；Continue to be slowly added to ethyl alcohol in supernatant, so that linear dextrin solution and ethyl alcohol volume ratio are 1:3, continue to stir 10min, in 4 DEG C of standing 1h, centrifugation obtains linear dextrin precipitating；Linear dextrin is dispersed in water, the linear dextrin solution that compound concentration is 4.0%~8.0%, polyethylene glycol is added with 40.0~50.0g polyethylene glycol/100mL linear dextrin solution ratio, heating, stirring to polyethylene glycol are completely dissolved, 4 DEG C are cooled to, and stands 1~2h at 4 DEG C, centrifugation is precipitated, with the polyethylene glycol of chloroform wash residual, forced air drying 5min obtains nanometer starch crystal at 40 DEG C.
Description
Technical field
A method of nanometer starch crystal efficiently being prepared, is related to ethyl alcohol fractional precipitation classification dextrin technology and polyethylene glycol adds
Fast linear dextrin recrystallizes rate technology, belongs to starch manufacture field.
Background technique
Nanometer starch crystal can be used as particle emulsifying agents, material filler etc., has in fields such as food, materials and widely answers
With.Traditional starch is nanocrystalline to be prepared by acid-hydrolysis method starch, but time-consuming for this method, and yield is low.In recent years, development uses straight chain
Dextrin recrystallization technology prepares nanometer starch crystal, i.e., by after starch gelatinization, carries out de- branch to starch and obtain linear dextrin, utilize
Linear dextrin is self-assembly of nanometer starch crystal.Compared with acid-hydrolysis method, this method shorten nanometer starch crystal preparation time,
Improve nanometer starch crystal yield.However, causing nanometer starch crystal to obtain since the linear dextrin molecular weight distribution that de- branch obtains is wide
Rate is low, crystallinity is low and particle diameter distribution is wide.
This research team discovery reduce linear dextrin molecular weight distribution, can be improved linear dextrin crystalline rate, crystallinity and
The particle diameter distribution for reducing nanometer starch crystal, it is found furthermore that polyethylene glycol can accelerate linear dextrin as the precipitating reagent of linear dextrin
Crystallization.Based on above-mentioned discovery, the present invention provides a kind of method for efficiently preparing nanometer starch crystal.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for efficiently preparing nanometer starch crystal, to expand starch application, mention
The surcharge of high starch.
The technical solution of the present invention is as follows:
Using waxy starch as raw material, de- branch method prepares linear dextrin, ethyl alcohol step-by-step precipitation method reduces linear dextrin molecular weight
Distribution, polyethylene glycol accelerate linear dextrin crystallization, and nanometer starch crystal is prepared.
Specific steps of the invention include:
(1) take off branch method prepare linear dextrin: disperse waxy starch in distilled water so that starch concentration be 6.0%~
8.0%, being placed in heating 30min in boiling water bath is gelatinized starch completely, is cooled to 55 DEG C；With acetate buffer adjust pH to
4.5, Pullulanase is added according to the ratio of 50U/g starch, reacts 2h, boiling water bath heats 5min and stops reaction；
(2) ethyl alcohol step-by-step precipitation method reduces linear dextrin molecular weight distribution: being added by peristaltic pump with the rate of 0.5mL/min
Enter ethyl alcohol in (1) resulting linear dextrin solution, so that dextrin solution and ethyl alcohol volume ratio are 3:1, continues to stir 10min, 4
DEG C stand 1h, centrifugation, remove precipitating；Continue to be slowly added to ethyl alcohol in supernatant, so that linear dextrin solution and ethyl alcohol volume ratio
For 1:3, continue to stir 10min, in 4 DEG C of standing 1h, centrifugation is precipitated, as target linear dextrin；
(3) polyethylene glycol accelerates linear dextrin crystallization to prepare nanometer starch crystal: dispersing water for the linear dextrin that (2) obtain
In, the linear dextrin solution that compound concentration is 4.0%~8.0% is molten with 40.0~50.0g polyethylene glycol/100mL linear dextrin
Polyethylene glycol is added in the ratio of liquid, and heating, stirring are completely dissolved to polyethylene glycol, is cooled to 4 DEG C, and 1~2h is stood at 4 DEG C,
Centrifugation is precipitated, and with the polyethylene glycol of chloroform wash residual, forced air drying 5min obtains nanometer starch crystal at 40 DEG C；
(4) its partial size the characterization of nanometer starch crystal property: is measured using nano particle size instrument；It is measured using x-ray diffractometer
Its crystallinity.
Compared with prior art, the invention has the following advantages:
(1) by ethyl alcohol gradually the precipitation method reduce linear dextrin molecular weight distribution, to reduce the grain of nanometer starch crystal
Diameter distribution；
(2) accelerate linear dextrin crystallization so as to shorten the preparation time of nanometer starch crystal by polyethylene glycol precipitation.
In conclusion the method production time is short, high, the prepared nanometer starch crystal crystallinity of the yield of nanometer starch crystal
Height, particle diameter distribution are uniform.
Specific embodiment
Embodiment 1
It disperses Waxy Rice Starch in distilled water, so that starch concentration is 6.0%, stirring is placed in boiling water bath and adds
Hot 30min is gelatinized starch completely, is cooled to 55 DEG C, pH to 4.5 is adjusted with acetate buffer, according to the ratio of 50U/g starch
Example addition Pullulanase reacts 2h, and boiling water bath heats 5min and stops reaction, is cooled to room temperature, and stirs straight chain with the rate of 50rpm
Dextrin solution is added ethyl alcohol by peristaltic pump with the rate of 0.5mL/min and makes linear dextrin solution and ethyl alcohol volume ratio for 3:
1, continue to stir 10min, in 4 DEG C of standing 1h, 5min is centrifuged with 10000 × g rate at 4 DEG C, discards precipitating；Continue in supernatant
Ethyl alcohol is added with the rate of 0.5mL/min, so that linear dextrin solution and ethyl alcohol volume ratio are 1:3, continues to stir 10min, 4
DEG C 1h is stood, 5min is centrifuged with 10000 × g rate, discards supernatant liquid, gained precipitating is dispersed in water, and is prepared 100mL concentration and is
4.0% linear dextrin solution, is added the polyethylene glycol that 50.0g molecular weight is 4000, and heating, stirring are completely molten to polyethylene glycol
Solution, is cooled to 4 DEG C, and stand 1h at 4 DEG C, is centrifuged 5min with 10000 × g rate, is washed with chloroform remaining in precipitating
Polyethylene glycol, precipitating, which is placed in forced air drying 5min at 40 DEG C, can obtain nanometer starch crystal, and particle diameter distribution is 20~30nm, knot
Brilliant degree is 46.8%.
Embodiment 2
It disperses waxy corn starch in distilled water, so that starch concentration is 8.0%, stirring is placed in boiling water bath and adds
Hot 30min is gelatinized starch completely, is cooled to 55 DEG C, pH to 4.5 is adjusted with acetate buffer, according to the ratio of 50U/g starch
Example addition Pullulanase reacts 2h, and boiling water bath heats 5min and stops reaction, is cooled to room temperature, and stirs straight chain with the rate of 50rpm
Dextrin solution is added ethyl alcohol by peristaltic pump with the rate of 0.5mL/min and makes linear dextrin solution and ethyl alcohol volume ratio for 3:
1, continue to stir 10min, in 4 DEG C of standing 1h, 5min is centrifuged with 10000 × g rate at 4 DEG C, discards precipitating；Continue in supernatant
Ethyl alcohol is added with the rate of 0.5mL/min, so that linear dextrin solution and ethyl alcohol volume ratio are 1:3, continues to stir 10min, 4
DEG C 1h is stood, 5min is centrifuged with 10000 × g rate, discards supernatant liquid, gained precipitating is dispersed in water, and is prepared 100mL concentration and is
8.0% linear dextrin solution, is added the polyethylene glycol that 40.0g molecular weight is 8000, and heating, stirring are completely molten to polyethylene glycol
Solution, is cooled to 4 DEG C, and stand 2h at 4 DEG C, is centrifuged 5min with 10000 × g rate, is washed with chloroform remaining in precipitating
Polyethylene glycol, precipitating, which is placed in forced air drying 5min at 40 DEG C, can obtain nanometer starch crystal, and particle diameter distribution is 25~40nm, knot
Brilliant degree is 51.8%.
Embodiment 3
It disperses Waxy Rice Starch in distilled water, so that starch concentration is 7.0%, stirring is placed in boiling water bath and adds
Hot 30min is gelatinized starch completely, is cooled to 55 DEG C, pH to 4.5 is adjusted with acetate buffer, according to the ratio of 50U/g starch
Example addition Pullulanase reacts 2h, and boiling water bath heats 5min and stops reaction, is cooled to room temperature, and stirs straight chain with the rate of 50rpm
Dextrin solution is added ethyl alcohol by peristaltic pump with the rate of 0.5mL/min and makes linear dextrin solution and ethyl alcohol volume ratio for 3:
1, continue to stir 10min, in 4 DEG C of standing 1h, 5min is centrifuged with 10000 × g rate at 4 DEG C, discards precipitating；Continue in supernatant
Ethyl alcohol is added with the rate of 0.5mL/min, so that linear dextrin solution and ethyl alcohol volume ratio are 1:3, continues to stir 10min, 4
DEG C 1h is stood, 5min is centrifuged with 10000 × g rate, discards supernatant liquid, gained precipitating is dispersed in water, and is prepared 100mL concentration and is
5.0% linear dextrin solution, is added the polyethylene glycol that 45.0g molecular weight is 6000, and heating, stirring are completely molten to polyethylene glycol
Solution, is cooled to 4 DEG C, and stand 2h at 4 DEG C, is centrifuged 5min with 10000 × g rate, is washed with chloroform remaining in precipitating
Polyethylene glycol, precipitating, which is placed in forced air drying 5min at 40 DEG C, can obtain nanometer starch crystal, and particle diameter distribution is 30~40nm, knot
Brilliant degree is 46.6%.
Claims (2)
1. a kind of method for efficiently preparing nanometer starch crystal, including prepare linear dextrin solution, linear dextrin self assembly preparation is received
Meter Jing, it is characterised in that linear dextrin molecular weight distribution is reduced using ethyl alcohol step-by-step precipitation method, straight chain is accelerated using polyethylene glycol
Dextrin is self-assembly of nanocrystalline, the specific steps are as follows: linear dextrin solution is stirred with the rate of 50rpm, by peristaltic pump with
Ethyl alcohol is added in the rate of 0.5mL/min, so that linear dextrin solution and ethyl alcohol volume ratio are 3:1, continues to stir 10min, at 4 DEG C
1h is stood, centrifugation removes precipitating；Continue to be slowly added to ethyl alcohol in supernatant, so that linear dextrin solution is with ethyl alcohol volume ratio
1:3 continues to stir 10min, and in 4 DEG C of standing 1h, centrifugation obtains linear dextrin precipitating；Linear dextrin is dispersed in water, is prepared
The linear dextrin solution that concentration is 4.0%~8.0%, with 40.0~50.0g polyethylene glycol/100mL linear dextrin solution ratio
Polyethylene glycol is added in example, and heating, stirring are completely dissolved to polyethylene glycol, is cooled to 4 DEG C, and stand 1~2h at 4 DEG C, is centrifuged
To precipitating, with the polyethylene glycol of chloroform wash residual, forced air drying 5min obtains nanometer starch crystal at 40 DEG C.
2. a kind of method for efficiently preparing nanometer starch crystal according to claim 1, it is characterised in that poly- second two used
The molecular weight of alcohol is 4000,6000 or 8000Da.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154818A (en) * | 2020-01-17 | 2020-05-15 | 江南大学 | Preparation method of straight-chain dextrin |
| CN111961262A (en) * | 2020-09-01 | 2020-11-20 | 郑州工业应用技术学院 | Production method of V-shaped amylose n-octanol compound |
| CN113087811A (en) * | 2021-04-16 | 2021-07-09 | 齐鲁工业大学 | Preparation method and application of linear dextrin nanoparticles |
| CN114736940A (en) * | 2022-04-22 | 2022-07-12 | 华南理工大学 | Preparation method of amylose with different chain lengths |
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| CN104198668A (en) * | 2014-09-17 | 2014-12-10 | 江南大学 | Dextrin grading method |
| CN104789616A (en) * | 2015-05-05 | 2015-07-22 | 江南大学 | Method for preparing narrow-molecular-weight-distribution dextrin |
| CN104804200A (en) * | 2015-04-09 | 2015-07-29 | 青岛农业大学 | Process for moderate-temperature self-assembly preparation of nano starch from enzymolysis short amylose |
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| CN104804200A (en) * | 2015-04-09 | 2015-07-29 | 青岛农业大学 | Process for moderate-temperature self-assembly preparation of nano starch from enzymolysis short amylose |
| CN104789616A (en) * | 2015-05-05 | 2015-07-22 | 江南大学 | Method for preparing narrow-molecular-weight-distribution dextrin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154818A (en) * | 2020-01-17 | 2020-05-15 | 江南大学 | Preparation method of straight-chain dextrin |
| CN111154818B (en) * | 2020-01-17 | 2022-03-15 | 江南大学 | Preparation method of straight-chain dextrin |
| CN111961262A (en) * | 2020-09-01 | 2020-11-20 | 郑州工业应用技术学院 | Production method of V-shaped amylose n-octanol compound |
| CN111961262B (en) * | 2020-09-01 | 2022-03-11 | 郑州工业应用技术学院 | Production method of V-shaped amylose n-octanol compound |
| CN113087811A (en) * | 2021-04-16 | 2021-07-09 | 齐鲁工业大学 | Preparation method and application of linear dextrin nanoparticles |
| CN114736940A (en) * | 2022-04-22 | 2022-07-12 | 华南理工大学 | Preparation method of amylose with different chain lengths |
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