CN110079571A - A kind of preparation process of high-quality fructose syrup - Google Patents
A kind of preparation process of high-quality fructose syrup Download PDFInfo
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- CN110079571A CN110079571A CN201910405063.8A CN201910405063A CN110079571A CN 110079571 A CN110079571 A CN 110079571A CN 201910405063 A CN201910405063 A CN 201910405063A CN 110079571 A CN110079571 A CN 110079571A
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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
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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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
- C12P19/24—Preparation of compounds containing saccharide radicals produced by the action of an isomerase, e.g. fructose
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Abstract
The invention discloses a kind of preparation process of high-quality fructose syrup, by rice in steep, grinding, liquefying-saccharifying, filtering decoloration, ion-exchange, isomery, finished product, then pass through chromatographic isolation, ion-exchange, purification, mixture, concentration are prepared into finished product fructose syrup;By the interaction between enzymes a variety of in liquid sugar melting process, collaboration improves the conversion ratio of glucose;Polygalacturonase can improve the Hyarogen-bonding of starch, reduce the influence of starch retrogradation phenomenon, calcium cyclamate can improve the cohesion performance of rice protein, so that albumen is efficiently separated with starch, the yield of fructose syrup is improved, and D-mannital can further destroy Secondary structure, and the activated centre of rice protein is exposed, so that calcium cyclamate is easier and the combination of protein is agglomerated, the yield of fructose syrup is further increased.
Description
Technical field
The present invention relates to the fabricating technology field of fructose syrup, in particular to a kind of preparation of high-quality fructose syrup
Technique.
Background technique
Fructose syrup is also referred to as high fructose syrup (FructoseComSyrups) or isomery syrup, industrial main use
Starch is raw material, through double enzyme solutions and saccharification, is hydrolyzed to glucose, then by the isomerization of glucolase, will be a part of
Phlorose is isomerized to α-fructose, obtains phlorose and α-fructose mixed liquor.Fructose syrup is a kind of new development
Starch sugar product, be widely used in food industry, especially soft-drink industry.Soft drink, that is, soft drink, mainly
Refer to soda, fruit wine, grape wine etc..At room temperature, fructose syrup is the liquid of a kind of colorless and odorless, good fluidity,
Show good sweet taste and metabolic characteristic.People more understand it, and application range is also increasingly wider.Due to its " collaboration
Synergy, cold sweet and tasty mouth " and there is close with sucrose or slightly above sucrose sugariness, there is cold sweet tea characteristic, sugariness at 40 DEG C or less
It reduces and increases with temperature.In recent years, it is remained high in environment in international sugared valence, the deep blueness by soft drink producer of fructose syrup
It looks at.
Currently, the method for most common starch industry conversion production fructose syrup is two enzymes method.The two enzymes method of starch sugaring
Technique includes three steps of starch gelization gelatinization, liquefaction and saccharification.During double-enzyme method sugar making, high temperature (100 DEG C or more) are used first
High steam to starch slurry handle the several seconds, expand starch granules rapidly, then pressure maintaining about 5 minutes, complete gelation operation with
Slurries are squeezed into reactor with extruder afterwards, a certain amount of α-amylase is added and carries out liquefaction processing, after the completion of liquefaction, liquid to be liquefied
When temperature is down to 55-65 DEG C, adjusts pH value to 4.5-5.0, add a certain amount of saccharification enzymatic treatment 48-92h, can finally generate DE value is
The glucose syrup of 97%-98%, glucose syrup are converted into fructose syrup using isomerization processing.
But there is also technical problems urgently to be solved for the two enzymes method in fructose syrup production process: 1, inversion rate of glucose
It is not high enough, since in the liquefaction process of high temperature retrogradation easily occurs for starch, so that making the conversion ratio of glucose reduces;2, double
Enzymatic conversion method production glucose during liquefy and be saccharified the two committed steps production cycle it is longer, energy consumption is larger, is not inconsistent
The policy requirements for developing low-carbon economy are closed, to limit the production capacity of glucose;3, it is converted and is given birth to using general two enzymes method
When malaga sugar, since the coherency of the impurity such as protein is poor, cause final filtering sugar solution poor, after influencing glucose even
The yield of sequence fructose syrup.
Therefore the technological means for effectively improving two enzymes method production inversion rate of glucose is found to fruit grape syrup energy conservation and environmental protection
Quantization production is of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation processes of high-quality fructose syrup, by more in liquid sugar melting process
Interaction between kind enzyme, collaboration improve the conversion ratio of glucose;The hydrogen bond that polygalacturonase can improve starch is made
Firmly, the influence of starch retrogradation phenomenon is reduced, calcium cyclamate can improve the cohesion performance of rice protein, so that albumen
It is efficiently separated with starch, improves the yield of fructose syrup, and D-mannital can further destroy the second level of protein
Structure enables the activated centre of rice protein to be exposed, so that calcium cyclamate is easier the knot with protein
Conjunction is agglomerated, and the yield of fructose syrup is further increased.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h wants repeated flushing multiple when rinsing, and except impurity such as dust, rice brans, immersion can make the abundant water swelling of rice, right
In the steeping tank of outdoor outdoor placement, the time of immersion, summer needed the time slightly shorter 1~3h impregnated, winter depending on season
Season slightly longer 4~6h.If steeping tank can be can control 40~50 DEG C of temperature, can be shortened soaking time with attemperation of steam;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) liquefying-saccharifying: being added α-amylase and carbohydrase in the starch slurry after sizing mixing, and is 110~118 DEG C with temperature
After injection liquefaction α-amylase and carbohydrase is added second in high-temperature steam injection, and starch slurry is pumped into liquefaction column and stops about 2~3h;
Adjust pH value be 4.0~4.5, saccharificatinn period for a period of time after, saccharification terminates, and obtains liquid glucose;
Under shear at high temperature power, starch granule is sufficiently opened, and complex enzyme is added second after injection liquefaction, starch slurry is pumped into
The column that liquefies stops about 2~3h.This process is cut using straight chain alpha-Isosorbide-5-Nitrae glycosidic bond of the Thermostable α-Amylase to starch
Cut, Thermostable α-Amylase be to the hydrolysis of starch it is random, this process can reduce rapidly the viscosity of starch milk, generate big
The dextrin of molecule and a small amount of glucose.After liquefaction, DE value is measured, and in the case where guaranteeing that iodine examination is qualified, to be controlled
Liquid glucose DE value is 14%~16%, first is that guarantee system viscosity reduces, long chained starch is hydrolyzed to short chain dextrin;Second is that control DE
Value, avoids short-chain amylose excessive hydrolysis, so that the enzyme in saccharification stage can play better effect.It needs to carry out after liquefaction
Simple filtering and removing slag, after liquefaction, into the saccharification stage, temperature control is at 60~65 DEG C, and pH value is 4.0~4.5, saccharification
30~40h of time.
(5) filtering decoloration: the liquid glucose for the end that is saccharified continues through the egg for being filtered to remove that saccharified rice residue and saccharification are precipitated
White, the equipment compared easily and economically is plate-frame filtering, and filtered fluid then passes through activated-charcoal column and decolourizes, and decoloration will remove fleshing
The visible impurity of eye, and some albumen of absorption and coloring matter.Final filter residue dry matter content reaches 55%~68%.
(6) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
Exchange, ion-exchange can also adsorb protein, organic matter etc. in liquid glucose.After ion-exchange can using be evaporated in vacuo to liquid glucose moisture into
Row removing, liquid glucose obtains to be concentrated to a certain extent.
(7) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose.In fructose preparation process, the development and utilization of immobilized isomerase are the important advances of fructose preparation, and isomerase is main
From microorganism, there are streptomycete, bacillus, actinoplanes and arthrobacterium etc..
(8) finished product: finished product fructose syrup is prepared by chromatographic isolation, ion-exchange, purification, mixture, concentration.
As a further improvement of the present invention, α-amylase is Thermostable α-Amylase, and the carbohydrase is glucoamylase
And Pullulanase.Thermostable α-Amylase, can straight chain alpha-Isosorbide-5-Nitrae glycosidic bond to starch cut, Thermostable α-Amylase pair
The hydrolysis of starch be it is random, this process can reduce rapidly the viscosity of starch milk, generate macromolecular dextrin and a small amount of Portugal
Grape sugar.There is good synergistic effect in the saccharification stage using both enzymes, combines and cuts to starch straight chain and branch, saccharification knot
Saccharified liquid DE value can be up to 95%~98% after beam.
As a further improvement of the present invention, raw material further includes 0.04~0.08 part of 1,4 beta-glucanase, the beta glucan
Enzyme is added together with α-amylase and carbohydrase in step (3).1,4 beta-glucanase is the same as Thermostable α-Amylase fast hydrolyzing one
Divide starch molecule, reduce liquefier viscosity, Thermostable α-Amylase molecule is preferably contacted with starch molecule, accelerates
Liquefaction reaction rate is conducive to effective progress of liquefaction reaction.
As a further improvement of the present invention, raw material further includes 0.01~0.05 part of polygalacturonase, described more
Polygalacturonase is added together with α-amylase and carbohydrase in step (3).Polygalacturonase and amylopectin
Molecule is had an effect, and the electron cloud answer to a riddle around starch molecule is reduced, and then chemical shift increases, while enhancing between starch
Hyarogen-bonding, reduce the retrogradation of starch, improve the conversion ratio of glucose.
As a further improvement of the present invention, raw material further includes 0.03~0.16 part of calcium cyclamate, the ring
Hexylamino sulfoacid calcium is added together with α-amylase and carbohydrase in step (3).The sulfonic group of calcium cyclamate with
The charge interaction on rice protein surface, agglomerates protein quickly, and can generate with the peptide bond nitrogen and oxygen of rice protein
Coordinate bond, forms the multicomponent complex with five-membered ring structure, further generates mixed complex reaction, and the two collective effect makes
Protein agglomerated product is more stable, improves the filterability of the final liquid glucose of postorder, improves the yield of fructose syrup.
As a further improvement of the present invention, raw material further includes 0.05~0.08 part of D-mannital, the D-MANNOSE
Alcohol is added together with α-amylase and carbohydrase in step (3).D-mannital can destroy egg rich in that can provide the hydroxyl of hydrogen bond
White intramolecular hydrogen bond, influences the secondary structure of rice protein, and the active group for keeping it internal is easier to be exposed, and weakens
The space steric effect of calcium cyclamate and protein improves the effect that calcium cyclamate acts on protein
Fruit plays synergistic effect.
As a further improvement of the present invention, in step (3), after liquefying-saccharifying, saccharified liquid DE value be 98.6%~
99.5%.
As a further improvement of the present invention, it is 55%~68% that final filter residue dry matter content, which reaches, in step (4).
As a further improvement of the present invention, step (3) saccharificatinn period is 30~40h, and saccharification temperature is 60~65 DEG C.?
It is saccharified at a temperature of 60~65 DEG C, effectively to avoid varied bacteria growing, and at this temperature, the activity of carbohydrase preferably, has the amount of money
Starch or short chain dextrin are further acted on conducive to carbohydrase.
As a further improvement of the present invention, 2~5 parts of stabilizer is added in step (7), the stabilizer is by carragheen
0.5~1 part, 1~5 part of butylated hydroxy anisole composition.Addition carragheen and butylated hydroxy anisole can effectively improve finished product fruit
The stability of glucose slurry, improves the product quality of fructose syrup.
The beneficial effects of the present invention are:
1. the present invention is liquefied and is saccharified using a variety of α-amylases and carbohydrase, the interaction between a variety of enzymes, association
With the conversion ratio for improving glucose, 1,4 beta-glucanase reduces liquid with a part of starch molecule of Thermostable α-Amylase fast hydrolyzing
Change liquid viscosity, Thermostable α-Amylase molecule is preferably contacted with starch molecule, accelerates liquefaction reaction rate, favorably
In effective progress of liquefaction reaction, polygalacturonase is had an effect with branched amylopectin molecules, is made around starch molecule
Electron cloud answer to a riddle reduces, and then chemical shift increases, while enhancing the Hyarogen-bonding between starch, and the retrogradation for reducing starch is existing
As improving the conversion ratio of glucose.
2. the present invention makes egg using the sulfonic group of calcium cyclamate and the charge interaction on rice protein surface
White matter is quickly agglomerated, and can generate coordinate bond with the peptide bond nitrogen and oxygen of rice protein, and being formed has the polynary of five-membered ring structure
Complex compound further generates mixed complex reaction, and the two collective effect keeps protein agglomerated product more stable, improves postorder
The filterability of final liquid glucose, improves the yield of fructose syrup.
3. after the liquefaction process of high temperature, rice protein deformation and structure compresses, the dextrin and rice protein of macromolecular
It is closely wound each other, forms secondary protein structure complexity, the steric hindrance between calcium cyclamate and protein is multiple
Miscellaneous, 1,4 beta-glucanase can hydrolyze the dextrin being wrapped in outside rice protein, discharge the action site of rice protein further to tie
It closes, cohesion, improves the cohesion removal rate of rice protein, further increase the yield of fructose syrup.
4.D- mannitol can destroy the hydrogen bond inside protein molecular, influence rice egg rich in that can provide the hydroxyl of hydrogen bond
White secondary structure, the active group for keeping it internal are easier to be exposed, and weaken calcium cyclamate and protein
Space steric effect improves the effect that calcium cyclamate acts on protein, plays synergistic effect.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with specific embodiment.Obviously, described
Embodiment be only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to guarantor of the present invention
The range of shield.
One, embodiment
Embodiment 1
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, polygalacturonase, calcium cyclamate, D-mannital, the high temperature for being 110~118 DEG C with temperature
After injection liquefaction α-amylase and carbohydrase is added second in steam injection, and starch slurry is pumped into liquefaction column and stops about 2~3h;It adjusts
PH value is 4.0-4.5, and under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 80 parts of rice, 0.05 part of Thermostable α-Amylase, amylase and 0.08 part of Pullulanase, β-
0.04 part of dextranase, 0.01 part of polygalacturonase, 0.03 part of calcium cyclamate, D-mannital 0.05
Part.
Embodiment 2
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, polygalacturonase, calcium cyclamate, D-mannital, the high temperature for being 110~118 DEG C with temperature
After injection liquefaction α-amylase and carbohydrase is added second in steam injection, and starch slurry is pumped into liquefaction column and stops about 2~3h;It adjusts
PH value is 4.0-4.5, and under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 100 parts of rice, 0.6 part of Thermostable α-Amylase, amylase and 0.5 part of Pullulanase, β-Portugal
0.08 part of dextranase, 0.05 part of polygalacturonase, 0.16 part of calcium cyclamate, 0.08 part of D-mannital.
Embodiment 3
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, polygalacturonase, calcium cyclamate, D-mannital, the high temperature for being 110~118 DEG C with temperature
After injection liquefaction α-amylase and carbohydrase is added second in steam injection, and starch slurry is pumped into liquefaction column and stops about 2~3h;It adjusts
PH value is 4.0-4.5, and under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase, β-Portugal
0.06 part of dextranase, 0.02 part of polygalacturonase, 0.1 part of calcium cyclamate, 0.07 part of D-mannital.
Embodiment 4
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, poly liquefying-saccharifying: are added in the starch slurry after sizing mixing
Galacturonic acid enzyme, calcium cyclamate, D-mannital are sprayed, spray with the high-temperature steam that temperature is 110~118 DEG C
α-amylase and carbohydrase are added for the second time after penetrating liquefaction, starch slurry is pumped into liquefaction column and stops about 2~3h;Adjusting pH value is 4.0-
4.5, under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase, poly
0.02 part of galacturonic acid enzyme, 0.1 part of calcium cyclamate, 0.07 part of D-mannital.
Embodiment 5
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, calcium cyclamate, D-mannital are sprayed with the high-temperature steam that temperature is 110~118 DEG C, injection liquefaction
α-amylase and carbohydrase is added second afterwards, starch slurry is pumped into liquefaction column and stops about 2~3h;Adjusting pH value is 4.0-4.5,60
Under the conditions of~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase, β-Portugal
0.06 part of dextranase, 0.1 part of calcium cyclamate, 0.07 part of D-mannital.
Embodiment 6
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, polygalacturonase, D-mannital are sprayed with the high-temperature steam that temperature is 110~118 DEG C, injection liquefaction
α-amylase and carbohydrase is added second afterwards, starch slurry is pumped into liquefaction column and stops about 2~3h;Adjusting pH value is 4.0-4.5,60
Under the conditions of~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase, β-Portugal
0.06 part of dextranase, 0.02 part of polygalacturonase, 0.07 part of D-mannital.
Embodiment 7
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) Thermostable α-Amylase, amylase, Pullulanase, β-Portugal liquefying-saccharifying: are added in the starch slurry after sizing mixing
Dextranase, polygalacturonase, calcium cyclamate are sprayed, spray with the high-temperature steam that temperature is 110~118 DEG C
α-amylase and carbohydrase are added for the second time after penetrating liquefaction, starch slurry is pumped into liquefaction column and stops about 2~3h;Adjusting pH value is 4.0-
4.5, under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase, β-Portugal
0.06 part of dextranase, 0.02 part of polygalacturonase, 0.1 part of calcium cyclamate.
Embodiment 8
A kind of preparation process of high-quality fructose syrup, comprising the following steps:
(1) rice in steep: by Raw Materials Rice carry out repeated flushing after, be placed in steeping tank at 40~50 DEG C impregnate 3~
6h;
(2) grind: soaked rice is milled to 20~100 mesh using milling apparatus progress defibrination, by the screen to filtrate,
Water is added to size mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) liquefying-saccharifying: Thermostable α-Amylase, amylase, Pullulanase are added in the starch slurry after sizing mixing, with temperature
The high-temperature steam that degree is 110~118 DEG C sprays, and second of addition α-amylase and carbohydrase, starch slurry are pumped into liquid after injection liquefaction
Change column and stops about 2~3h;Adjusting pH value is 4.0-4.5, under the conditions of 60~65 DEG C, after saccharificatinn period is 30~40h, and saccharification knot
Beam obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified, continue through be filtered to remove saccharified rice residue and liquefying-saccharifying cohesion it is big
Rice gluten, it is 55%~68% that final filter residue dry matter content, which reaches,;
(5) ion-exchange: the inorganic ion in liquid glucose is carried out using strong acid cation resin cooperation weak base anion resins
It exchanges, liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtain concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into
For fructose;
(7) finished product: by adding 2~5 parts of stabilizer in chromatographic isolation, ion-exchange, purification, mixture, the stabilizer is by card
0.5~1 part of glue, 1~5 part of butylated hydroxy anisole composition are drawn, then concentration is prepared into finished product fructose syrup.
The raw material includes: 90 parts of rice, 0.3 part of Thermostable α-Amylase, amylase and 0.2 part of Pullulanase.
Embodiment 1-7, comparative example are prepared into sample according to preparation process, after measuring liquefying-saccharifying according to standard method
DE value and glucose relative amount, the results are shown in Table 1.
The wherein measuring method of DE value: the reduced sugar in measurement solution.Before experiment starts, Standard glucose solution is instilled
In Fehling's solution, constant volume, experimental data are averaged three times for progress.After above-mentioned solution ratio is good, accurately drawn with instrument first
In 250ml conical flask, next is put into 20-30ml distilled water and 5 beades by Fehling first solution and Fehling second solution 10ml, into
The pre- titration experiments of row.It determines that experiment sample mark-experimental solutions 5ml fewer than pre- titration experiments are put into conical flask, sufficiently shakes up progress
Titration experiments after heating, until it is titrated to terminal, the liquor capacity V of reduction after record experiment.Each sample will be carried out
Parallel titration three times guarantees that error is less than 0.05ml, and experimental result takes arithmetic mean of instantaneous value three times.Measurement dissolution consolidating in the solution
Shape object.Rice starch solution after taking liquefaction carries out homogeneous operation, the pH value that acid solution adjusts product is added, to rice starch
α-amylase in solution is inactivated, and carries out cooling treatment later, and using digital display abbe's refractometer, successively measurement is dissolved as three times
Solid content in rice starch liquid takes arithmetic average to measurement result three times, and the result obtained is just dissolved in greatly
Solid content in rice starch liquid.
The calculation formula of DE value: DE=G × 100 × n ÷ (ρ × V × DMC)
Percentage % shared by DE-sample glucose quality;
ρ-samples taken concentration, g/ml;
Sample liquid consumes volume, ml when V-titration;
The quality that G -5ml glucose is compared, Fehling first and Fehling second solution and g;
Times after the more samples taken dilutions of n-number;
DMC-is dissolved in the solid content percentage in samples taken solution, %.
The wherein measuring method of glucose relative amount:
Glucose relative amount is measured using Shimadzu LC-20AT high performance liquid chromatograph, detector RID-10A
Differential refraction detector, chromatographic column are 5 μm of carbohydrate analysis column, 150mm × 3.9mm (i.d);Mobile phase second eyeball+water (70
+ 30) Isocratic clution;Flow velocity: 1.0mL/min;25 DEG C of column temperature;35 DEG C of detection cell temperature;10 μ L of sample volume.
The glucose standards solution of 1,2,4,6,8, the 10 μ g/ml of preparation configuration of glucose standard curve, selected
Liquid phase analysis is carried out under liquid phase chromatogram condition, using the target peak area of gained chromatogram as abscissa, concentration of glucose is vertical sits
Mark, is made glucose standard curve.
The measurement of table 1 sample DE value and glucose relative amount
The liquid of the fructose syrup colorless and odorless of the embodiment of the present invention 1~8, good fluidity, shows mellow sweet taste
Property.
As shown in Table 1, using rice starch as raw material, without any processing (embodiment 8), glucose relative amount is lower,
And be added in the sample (Examples 1 to 7) of a variety of enzymes, pass through the interaction between enzymes a variety of in liquid sugar melting process, association
With the conversion ratio for improving glucose;Polygalacturonase can improve the Hyarogen-bonding of starch, reduce starch retrogradation phenomenon
Influence, calcium cyclamate can improve the cohesion performance of rice protein, so that albumen is efficiently separated with starch, mention
The yield of high fructose syrup, and D-mannital can further destroy Secondary structure, so that the work of rice protein
Property center can be exposed so that calcium cyclamate is easier to agglomerate with the combination of protein, further increase
The yield of fructose syrup, security and stability is high, meets the rank requirement of high-quality fructose syrup.
Claims (10)
1. a kind of preparation process of high-quality fructose syrup, which comprises the following steps:
(1) rice in steep: after Raw Materials Rice is carried out repeated flushing, 3~6h of immersion at 40~50 DEG C is placed in steeping tank;
(2) grind: soaked rice carries out defibrination using milling apparatus, is milled to 20~100 mesh, by the screen to filtrate, adds water
It sizes mixing, temperature is improved to 50~60 DEG C, makes starch gelatinization, obtains the rice starch cream of 18~22 ° of Baume degrees;
(3) liquefying-saccharifying: being added α-amylase and carbohydrase in the starch slurry after sizing mixing, the high temperature for being 110~118 DEG C with temperature
After injection liquefaction α-amylase and carbohydrase is added second in steam injection, and starch slurry is pumped into liquefaction column and stops about 2~3h;It adjusts
PH value is 4.0-4.5, saccharificatinn period for a period of time after, saccharification terminates, and obtains liquid glucose;
(4) filtering decoloration: the liquid glucose for the end that is saccharified continues through the rice egg for being filtered to remove saccharified rice residue and liquefying-saccharifying cohesion
It is white;
(5) ion-exchange: swapping the inorganic ion in liquid glucose using strong acid cation resin cooperation weak base anion resins,
Liquid glucose moisture is removed using vacuum evaporation after ion-exchange, obtains concentration liquid glucose;
(6) it isomery: will be packed into pillar after isomery enzyme immobilization, under the action of isomerase, glucose is converted into as fruit
Sugar;
(7) finished product: finished product fructose syrup is prepared by chromatographic isolation, ion-exchange, purification, mixture, concentration.
The raw material includes: 80~100 parts of rice, 0.05~0.6 part of α-amylase, 0.08~0.5 part of carbohydrase.
2. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that the α-amylase is high temperature resistant
Alpha-amylase, the carbohydrase are glucoamylase and Pullulanase.
3. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that the raw material further includes β-Portugal
0.04~0.08 part of dextranase, the 1,4 beta-glucanase is added together with α-amylase and carbohydrase in step (3).
4. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that the raw material further includes poly
0.01~0.05 part of galacturonic acid enzyme, the polygalacturonase is in step (3) together with α-amylase and carbohydrase
It is added.
5. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that the raw material further includes hexamethylene
0.03~0.16 part of base sulfamic acid calcium, the calcium cyclamate is in step (3) together with α-amylase and carbohydrase
It is added.
6. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that the raw material further includes D- sweet
0.05~0.08 part of sugar alcohol of dew, the D-mannital is added together with α-amylase and carbohydrase in step (3).
7. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that in the step (3), liquefaction
After saccharification, saccharified liquid DE value is 98.6%~99.5%.
8. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that final in the step (4)
It is 55%~68% that filter residue dry matter content, which reaches,.
9. the preparation process of high-quality fructose syrup as described in claim 1, which is characterized in that when the step (3) is saccharified
Between be 30~40h, saccharification temperature be 60~65 DEG C.
10. the preparation process of the high-quality fructose syrup as described in claim 1~9 is any, which is characterized in that the step
(7) stabilizer of 2~5 parts of addition, the stabilizer are made of 0.5~1 part of carragheen, 1~5 part of butylated hydroxy anisole in.
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