CN104789616A - Method for preparing narrow-molecular-weight-distribution dextrin - Google Patents
Method for preparing narrow-molecular-weight-distribution dextrin Download PDFInfo
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- CN104789616A CN104789616A CN201510224774.7A CN201510224774A CN104789616A CN 104789616 A CN104789616 A CN 104789616A CN 201510224774 A CN201510224774 A CN 201510224774A CN 104789616 A CN104789616 A CN 104789616A
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Abstract
The invention relates to a method for preparing narrow-molecular-weight-distribution dextrin, which comprises the following steps: uniformly mixing starch and water, regulating the pH value to 5.8-6.0, and adding high-temperature alpha-amylase; uniformly stirring in a 99-DEG C water bath until the iodine test is light brown (acceptable); inactivating the enzyme; preparing a 1.5-10% (w/w) dextrin solution; adding ethanol into the dextrin solution until the ethanol concentration is 20% (v/v), synergically adding polyethyleneglycol and sodium chloride, standing, centrifuging, precipitating, washing, and drying to obtain a component 1; adding ethanol into the supernate until the end concentration is 30% (v/v), synergically adding polyethyleneglycol and sodium chloride, standing, centrifuging, precipitating, washing and drying to obtain a component 2; and repeating the process above until the ethanol concentration is 90% (v/v), wherein the components 1, 2 and the like are the narrow-molecular-weight-distribution dextrin of all stages. The technique provided by the invention is applicable to all the methods relating to organic solvent progressive or coordinated polyethyleneglycol and salt precipitation separation of starch or dextrin.
Description
Technical field
The present invention relates to food processing technology field, especially relate to a kind of method obtaining the dextrin of molecular weight narrow ditribution.
Background technology
Starch by a class can be produced when acidolysis or enzymatic treatment by glucose, maltose, a series of oligose such as trisaccharide maltose and polysaccharide composition dextrin solution; The index characterizing extent of starch hydrolysis adopts DE value usually.The maltodextrin of same DE value probably has distinct functional property, which reflects composition and the starch type of resultant in maltodextrin.At food processing field, the dextrin of different molecular weight distribution presents different character, thus presents different purposes, as can as blood substitute when hydroxyethylamyle molecular weight ranges is 40000 ~ 450000Da; Dextrin is a kind of extraordinary thickening material, and small-molecular-weight dextrin can affect food mouthfeel, and macromolecule dextrin is unstable.Based on this, separation prepares the dextrin of different molecular weight distribution for expansion dextrin range of application, improves starch deep processing added value significant; In addition character and then the announcement mechanism of action of studying relevant amylases is contributed to.
At present, the dextrin preparing different molecular weight distribution mainly adopts size exclusion chromatography, and this method filler is expensive, and chromatogram power system cost is high, and treatment capacity is little in addition, is difficult to realize suitability for industrialized production; Add polyoxyethylene glycol in starch degradation liquid step by step and can carry out simple classification roughing out to dextrin, but the longer and easy microbiological contamination of dextrin solution of classification cycle.The alcohol step by step alcohol precipitator method can be used widely in the separation being separated non-starch polysaccharide, but adopts alcohol deposition method separation different molecular weight dextrin to study rarely seen report.
Ethanol precipitation ultimate principle progressively adds alcohol in dextrin solution, is reduction of the specific inductivity of solution on the one hand, the electrostatic attraction between solute molecule is increased, and aggregate and precipitate occurs.On the other hand; The hydration of organic solvent itself reduces the concentration of free water, have compressed the thickness of solute molecule surface hydration layer, reduces its wetting ability and cohesion of dewatering.The polymkeric substance such as bibliographical information polyoxyethylene glycol and dextran have uncompatibility, change polymer solubility.
Summary of the invention
For the problems referred to above that prior art exists, the applicant provides a kind of method preparing molecular weight narrow ditribution dextrin.Allly to mention through organic solvent step by step or coordinate polyoxyethylene glycol and salt precipitate and separate starch or dextrin method, all applicable the technology of the present invention.
Technical scheme of the present invention is as follows:
Prepare a method for molecular weight narrow ditribution dextrin, comprise the following steps:
(1) starch mixes with the mass ratio of water according to 1:1.5 ~ 1:4, and regulate pH to 5.8 ~ 6.0 with 0.1mol/LNaOH, then add high-temperatureα-amylase, its addition is 10 ~ 30U/g starch, obtains mixed solution;
(2) step (1) mixed solution being placed in 99 DEG C of thermostatic water-circulator bath grooves (outfit magnetic stirring apparatus), stirring, is light brown and qualified through iodine examination; Regulate pH to 3.0, enzyme termination reaction of going out with 0.1mol/LHCI immediately, after balance 5min, with 0.1mol/LNaOH neutralization, regulate pH to neutral;
(3) liquefier dilution step (2) obtained, being configured to concentration is 1.5 ~ 10% (w/w) dextrin solution;
(4) in dextrin solution, slowly ethanol is added, be adjusted to ethanol final concentration 20% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, 4 DEG C of standing 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation, through the washing of this concentration ethanol, cryodrying obtains component 1;
(5) in supernatant liquor, slow interpolation ethanol, being adjusted to ethanol final concentration is 30% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, 4 DEG C of standing 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation, through the washing of this concentration ethanol, cryodrying obtains component 2;
(6) said process is repeated, to alcohol concn is 90% (v/v);
Described component 1, component 2 ... be described molecular weight narrow ditribution dextrin at different levels.
It is 2 ~ 8% (w/v) that step (4) ~ (6) all control Polyethylene glycol.
The number-average molecular weight of polyoxyethylene glycol is 4000Da, 6000Da or 8000Da.
It is 0.2 ~ 1.0% (w/v) that step (4) ~ (6) all control sodium chloride concentration.
Step (4) ~ (6) obtain dextrin component, through size exclusion chromatography to dextrin proximate analysis, calculate dextrin molecular weight and dispersion coefficient.
The technique effect that the present invention is useful is:
The present invention is based on polymeric hydrophilic group and charged situation and determine its solubleness in aqueous, certain density salt is added in aqueous solutions of polymers, solution ion strength can be changed and change polymer solubility, in starch hydrolyzate, improve alcohol concn collaborative interpolation polyoxyethylene glycol and sodium-chlor step by step, dextrin molecular weight is descending to be precipitated out step by step.The present invention compared with prior art has the following advantages:
(1) resolving power of the present invention is high, and solvent boiling point is low, and removing or recovery are conveniently, nontoxic.
(2) reaction conditions of the present invention is gentle, simple to operate, and treatment capacity is large, and production cost is low, is easy to suitability for industrialized production;
(3) molecular weight dextrins that prepared by the present invention presents narrow ditribution, can adapt to specific demand, and for lifting starch deep processing added value, development glucose industry, development of new functional oligose has positive promoter action.
Embodiment
Below in conjunction with embodiment, the present invention is specifically described.
Embodiment 1:
Take 50g W-Gum in beaker; Add 200mL deionized water (normal temperature) to mix, regulate pH to 5.8 ~ 6.0 with 0.1mol/LNaOH; Add high-temperatureα-amylase 1500U, stir.Be placed in 99 DEG C of thermostatic water-circulator bath grooves (outfit magnetic stirring apparatus), stir, iodine examination is qualified; Regulate pH to 3.0, enzyme termination reaction of going out with 0.1mol/LHCI immediately, after balance 5min, neutralize with 0.1mol/L NaOH, regulate pH to neutral.Starch hydrolyzate is diluted, is configured to the dextrin solution that mass concentration is 10% (w/w).
Get dextrin solution 100mL, slowly add ethanol, and constantly stir, be adjusted to ethanol final concentration 20% (v/v), collaborative interpolation polyoxyethylene glycol (6000Da) and sodium-chlor, control its concentration 2% (w/v), 0.2% (w/v) respectively, be placed in 4 DEG C of refrigerators and leave standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation is through respective concentration washing with alcohol, and cryodrying obtains component 1; In supernatant liquor, slowly interpolation ethanol is adjusted to ethanol final concentration is 30% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, control its concentration 2% (w/v) respectively, 0.2% (w/v) is collaborative adds polyoxyethylene glycol 2% (w/v), is placed in 4 DEG C of refrigerators and leaves standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitate through respective concentration washing with alcohol, cryodrying obtains component 2; Repetition aforesaid operations like this, being adjusted to ethanol final concentration is 90% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, control its concentration 2% (w/v) respectively, 0.2% (w/v), obtain 1 ~ 8 alcohol precipitation component respectively, measure different components molecular weight distribution through Size Exclusion Chromatograph SEC.
Based on size exclusion chromatography to dextrin proximate analysis, calculate dextrin molecular weight and dispersion coefficient, obtain 8 dextrin component molecular amount information as follows: dextrin 1 (i.e. component 1, lower same) weight-average molecular weight is 118.8kDa, and dispersion coefficient is 1.58; Dextrin 2 weight-average molecular weight is 27.9kDa, and dispersion coefficient is 1.23; Dextrin 3 weight-average molecular weight is 19.7kDa, and dispersion coefficient is 1.18; Dextrin 4 weight-average molecular weight is 12.1kDa, and dispersion coefficient is 1.41; Dextrin 5 weight-average molecular weight is 4.9kDa, and dispersion coefficient is 1.21; Dextrin 6 weight-average molecular weight is 4.2kDa, and dispersion coefficient is 1.08; Dextrin 7 weight-average molecular weight is 1.6kDa, and dispersion coefficient is 1.58; Dextrin 8 weight-average molecular weight is 1.1kDa, and dispersion coefficient is 1.23.
Embodiment 2:
Take 100g W-Gum in beaker; Add 250mL deionized water (normal temperature) to mix, regulate pH to 5.8 ~ 6.0 with 0.1mol/LNaOH; Add high-temperatureα-amylase 2000U, stir.Be placed in 99 DEG C of thermostatic water-circulator bath grooves (outfit magnetic stirring apparatus), stir, iodine examination is qualified; Regulate pH to 3.0, enzyme termination reaction of going out with 0.1mol/LHCI immediately, after balance 5min, with 0.1mol/LNaOH neutralization, regulate pH to neutral.Starch hydrolyzate is diluted, is configured to the dextrin solution that mass concentration is 5% (w/w).
Get dextrin solution 100mL, slowly add ethanol, and constantly stir, be adjusted to ethanol final concentration 20% (v/v), collaborative interpolation polyoxyethylene glycol (4000Da) and sodium-chlor, controlling its concentration is respectively 5% (w/v), 0.6% (w/v) is collaborative adds polyoxyethylene glycol 5% (w/v), be placed in 4 DEG C of refrigerators and leave standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation is through respective concentration washing with alcohol, and cryodrying obtains component 1; In supernatant liquor, it is 30% (v/v) that slow interpolation ethanol is adjusted to ethanol final concentration, collaborative interpolation polyoxyethylene glycol and sodium-chlor, controlling its concentration is respectively 5% (w/v), and 0.6% (w/v) is collaborative adds polyoxyethylene glycol 5% (w/v), be placed in 4 DEG C of refrigerators and leave standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation is through respective concentration washing with alcohol, and cryodrying obtains component 2; Repetition aforesaid operations like this, being adjusted to ethanol final concentration is 90% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, controlling its concentration is respectively 5% (w/v), 0.6% (w/v), obtain 1 ~ 8 dextrin component respectively, measure different components weight distributing characteristic through Size Exclusion Chromatograph SEC.
Based on size exclusion chromatography to dextrin proximate analysis, calculate dextrin molecular weight and dispersion coefficient, obtain 8 dextrin component molecular amount information as follows: dextrin 1 weight-average molecular weight is 121.3kDa, and dispersion coefficient is 1.42; Dextrin 2 weight-average molecular weight is 31.2kDa, and dispersion coefficient is 1.12; Dextrin 3 weight-average molecular weight is 21.3kDa, and dispersion coefficient is 1.08; Dextrin 4 weight-average molecular weight is 14.2kDa, and dispersion coefficient is 1.11; Dextrin 5 weight-average molecular weight is 5.2kDa, and dispersion coefficient is 1.15; Dextrin 6 weight-average molecular weight is 3.1kDa, and dispersion coefficient is 1.06; Dextrin 7 weight-average molecular weight is 2.3kDa, and dispersion coefficient is 1.09; Dextrin 8 weight-average molecular weight is 1.5kDa, and dispersion coefficient is 1.03.
Embodiment 3
Take 100g W-Gum in beaker; Add 150mL deionized water (normal temperature) to mix, regulate pH to 5.8 ~ 6.0 with 0.1mol/LNaOH; Add high-temperatureα-amylase 1000U, stir.Be placed in 99 DEG C of thermostatic water-circulator bath grooves (outfit magnetic stirring apparatus), stir, iodine examination is qualified; Regulate pH to 3.0, enzyme termination reaction of going out with 0.1mol/LHCI immediately, after balance 5min, with 0.1mol/LNaOH neutralization, regulate pH to neutral.Diluted by starch hydrolyzate, configuration quality concentration is the dextrin solution of 1.5% (w/w).
Get dextrin solution 100mL, slowly add ethanol, stir, be adjusted to ethanol final concentration 20% (v/v), collaborative interpolation polyoxyethylene glycol (8000Da) and sodium-chlor, controlling its concentration is respectively 8% (w/v), 1% (w/v), be placed in 4 DEG C of refrigerators and leave standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitation is through respective concentration washing with alcohol, and cryodrying obtains component 1; In supernatant liquor, it is 30% (v/v) that slow interpolation ethanol is adjusted to ethanol final concentration, collaborative interpolation polyoxyethylene glycol and sodium-chlor, and controlling its concentration is respectively 8% (w/v), 1% (w/v), collaborative interpolation polyoxyethylene glycol 8% (w/v), is placed in 4 DEG C of refrigerators and leaves standstill 24h, centrifugal (4 DEG C, 10000rpm, 20min), precipitate through respective concentration washing with alcohol, cryodrying obtains component 2; Repetition aforesaid operations like this, ethanol final concentration is regulated to be 90% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, controlling its concentration is respectively 8% (w/v), 1% (w/v), obtain 1 ~ 8 alcohol precipitation component respectively, measure different components molecular weight distribution through Size Exclusion Chromatograph SEC.
Based on size exclusion chromatography to dextrin proximate analysis, calculate dextrin molecular weight and dispersion coefficient, obtain 9 dextrin component molecular amount information as follows: dextrin 1 weight-average molecular weight is 106.3kDa, and dispersion coefficient is 1.24; Dextrin 2 weight-average molecular weight is 30.4kDa, and dispersion coefficient is 1.13; Dextrin 3 weight-average molecular weight is 23.1kDa, and dispersion coefficient is 1.03; Dextrin 4 weight-average molecular weight is 14.2kDa, and dispersion coefficient is 1.07; Dextrin 5 weight-average molecular weight is 5.3kDa, and dispersion coefficient is 1.11; Dextrin 6 weight-average molecular weight is 3.2kDa, and dispersion coefficient is 1.18; Dextrin 7 weight-average molecular weight is 1.7kDa, and dispersion coefficient is 1.21; Dextrin 8 weight-average molecular weight is 1.3kDa, and dispersion coefficient is 1.03.
The foregoing is only intersection example of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within the scope of protection of the invention.
Claims (4)
1. prepare a method for molecular weight narrow ditribution dextrin, it is characterized in that comprising the following steps:
(1) starch mixes with the mass ratio of water according to 1:1.5 ~ 1:4, and regulate pH to 5.8 ~ 6.0 with 0.1mol/LNaOH, then add high-temperatureα-amylase, its addition is 10 ~ 30U/g starch, obtains mixed solution;
(2) mixed solution that step (1) obtains is placed in 99 DEG C of thermostatic water-circulator bath grooves, stirs, be light brown and qualified through iodine examination, obtain liquefier, then carry out going out enzyme;
(3) liquefier dilution step (2) obtained, being configured to concentration is 1.5 ~ 10% (w/w) dextrin solution;
(4) in dextrin solution, slowly add ethanol, be adjusted to ethanol final concentration 20% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, 4 DEG C of standing 24h, centrifugal, precipitation, through the washing of this concentration ethanol, cryodrying obtains component 1;
(5) in supernatant liquor, slowly add ethanol, being adjusted to ethanol final concentration is 30% (v/v), collaborative interpolation polyoxyethylene glycol and sodium-chlor, and 4 DEG C of standing 24h are centrifugal, precipitation, and through the washing of this concentration ethanol, cryodrying obtains component 2;
(6) said process is repeated, to alcohol concn is 90% (v/v);
Described component 1, component 2 ... be described molecular weight narrow ditribution dextrin at different levels.
2. method according to claim 1, it is characterized in that step (4) ~ (6) all control Polyethylene glycol is 2 ~ 8% (w/v).
3. method according to claim 1, is characterized in that the number-average molecular weight of polyoxyethylene glycol is 4000Da, 6000Da or 8000Da.
4. method according to claim 1, it is characterized in that step (4) ~ (6) all control sodium chloride concentration is 0.2 ~ 1.0% (w/v).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105060762A (en) * | 2015-09-14 | 2015-11-18 | 江苏苏博特新材料股份有限公司 | Starch-based hydration heat regulation material preparation method |
| CN109265570A (en) * | 2018-10-10 | 2019-01-25 | 南昌大学 | A method of efficiently preparing nanometer starch crystal |
| CN113621084A (en) * | 2021-07-15 | 2021-11-09 | 南昌大学 | Method for grading dextrin |
-
2015
- 2015-05-05 CN CN201510224774.7A patent/CN104789616B/en active Active
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105060762A (en) * | 2015-09-14 | 2015-11-18 | 江苏苏博特新材料股份有限公司 | Starch-based hydration heat regulation material preparation method |
| CN109265570A (en) * | 2018-10-10 | 2019-01-25 | 南昌大学 | A method of efficiently preparing nanometer starch crystal |
| CN113621084A (en) * | 2021-07-15 | 2021-11-09 | 南昌大学 | Method for grading dextrin |
| CN113621084B (en) * | 2021-07-15 | 2022-10-11 | 南昌大学 | Method for grading dextrin |
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Effective date of registration: 20151208 Address after: No. 1800 road 214122 Jiangsu Lihu Binhu District City of Wuxi Province Applicant after: Jiangnan University Applicant after: Joint limited energy company of Jiangsu China Telecom Address before: No. 1800 road 214122 Jiangsu Lihu Binhu District City of Wuxi Province Applicant before: Jiangnan University |
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Inventor after: Shi Guiyang Inventor after: Ding Zhongyang Inventor after: Li Ying Inventor after: Gu Zhenghua Inventor after: Chen Jian Inventor after: Wang Baoshi Inventor after: Hu Zhijie Inventor after: Jiang Xiaodong Inventor after: Sun Fuxin Inventor after: Zhang Jie Inventor after: Li Youran Inventor after: Zhang Liang Inventor before: Shi Guiyang Inventor before: Li Ying Inventor before: Gu Zhenghua Inventor before: Wang Baoshi Inventor before: Hu Zhijie Inventor before: Jiang Xiaodong Inventor before: Sun Fuxin Inventor before: Zhang Jie Inventor before: Li Youran Inventor before: Zhang Liang Inventor before: Ding Zhongyang |
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