CN108103125A - A kind of industrialized production water-soluble dietary fiber preparation process and application - Google Patents
A kind of industrialized production water-soluble dietary fiber preparation process and application Download PDFInfo
- Publication number
- CN108103125A CN108103125A CN201711462244.1A CN201711462244A CN108103125A CN 108103125 A CN108103125 A CN 108103125A CN 201711462244 A CN201711462244 A CN 201711462244A CN 108103125 A CN108103125 A CN 108103125A
- Authority
- CN
- China
- Prior art keywords
- acid
- exchange resin
- reaction
- temperature
- enzyme
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C12P19/18—Preparation of compounds containing saccharide radicals produced by the action of a glycosyl transferase, e.g. alpha-, beta- or gamma-cyclodextrins
-
- 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
- C12P19/14—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
-
- 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
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/58—Aldonic, ketoaldonic or saccharic acids
Landscapes
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a kind of industrialized production water-soluble dietary fiber preparation process and applications.The technological reaction process is simple, reaction temperature is low, simultaneously glucose oxidase technique is used to make the glucose direct oxidation in enzymolysis process for gluconic acid, and oxidative decoloration is carried out to material using a small amount of hydrogen peroxide of its generation, the resistant dextrin produced is of light color, the degree of polymerization is low, is mass produced suitable for industrialization.
Description
Technical field
The invention belongs to food production processing technique field, a kind of industrialized production water-soluble dietary fiber preparation process and
Using.
Background technology
The dietary fiber that FAO (Food and Agriculture Organization of the United Nation) (FAO) and the World Health Organization (WHO) determined jointly in 1985 is determined
Justice：In the new water-soluble diet fiber product of low viscosity, it is can using that generally acknowledged quantitative approach measures, human digestive organ is intrinsic
The nonhydrolyzable edible animals and plants of digestive ferment constituent, be maintain human body health, cannot be by other materials institute's generation
A kind of nutrient replaced, people are referred to as after carbohydrate, fat, protein, vitamin, water, six big nutrition of minerals
Human body " the 7th nutrient " outside element.Wherein, resistant maltodextrin is as a kind of new water-soluble dietary fiber of low viscosity
Extensively using with the fields such as beverage, bakery, health products, can not only improve the mouthfeel of product, reduce product calorific value,
Product quality is improved, while intestinal flora can be adjusted, inhibits blood sugar concentration, reduces Serum lipid concentrations, once weight-reducing and Jiang Kuang
The functions such as prime element absorption, are modern functional food and the common functional food ingredient of health products.
Patent CN201410671093 uses sea sand as heat transfer medium, in high temperature using acid treated starch as raw material
Under the conditions of carry out pyrolytic reaction, obtain pyrodextrin crude product, pyrodextrin crude product obtains resistant dextrin product using refinement treatment.It should
Low energy consumption for method, and the time is short, and heat utilization efficiency is high, and starch is heated evenly, and the reaction time is short, and starch is not easy to be carbonized, concise in technology,
It is at low cost, but be complicated for operation the shortcomings that the technology, processing will be bad can have a great impact to equipment, and in saccharifying
Before also need to carry out sea sand separation.Song Gu chemical industry Co., Ltd. C N200580037471.9 contains the indigestibility of isomerized sugar
Property dextrin manufacturing method, by by the digestibility conversion in the pyrodextrin containing indigestible ingredient for after glucose,
Glucose isomerase is made to directly act on the indigestible dextrins containing glucose of generation, it can be with it be made to act on merely
Equal above efficiency makes a part for glucose be converted into fructose during glucose solution, so as to which efficiently manufacture contains isomerization
The indigestible dextrins of sugar.Patent CN201610700623 uses the acid adding into starch, the reaction of high-temperature vacuum dextrinization, Ran Houjia
Enter water and carry out acidolysis, resistant dextrin is prepared using enzymolysis.The technical disadvantages are easily to cause the anti-of generation using acid hemolysis process
Property dextrin with being not converted into the dextrin of resistant dextrin, being hydrolyzed together with starch, resistant dextrin yield is relatively low, and there is no essence
It is upper to solve the problems, such as that industrialization resistant dextrin reaction homogeneity is poor, color is deep, decoloration is difficult.Therefore, it is urgent to provide one kind to be suitable for work
The method that industry metaplasia produces resistant dextrin.
The content of the invention
In view of the above shortcomings of the prior art, inventor provides a kind of industrial metaplasia through long-term technology and practical exploration
The method for producing resistant dextrin, this method reaction process is simple, and reaction temperature is low, while makes enzymolysis using glucose oxidase technique
Glucose direct oxidation in the process is gluconic acid, and carries out oxidation to material using a small amount of hydrogen peroxide that it is generated and take off
Color, the resistant dextrin produced is of light color, and the degree of polymerization is low, is mass produced suitable for industrialization.
Specifically, the present invention relates to following technical schemes：
The first aspect of the invention, provides a kind of method of industrialized production resistant dextrin, and this method includes following
Step：
(1) into starch material add in acid, high-temperature vacuum dextrinization reaction, after reaction, adjust reaction solution I pH to
5.5~6.5, it adds in α-amylase and carries out pyroreaction；After reaction, reaction solution II pH to 4.2~4.8 are adjusted, add in saccharification
Enzyme, glucose oxidase and catalase carry out saccharification reaction, and after reaction, high temperature destroy the enzyme treatment obtains reaction solution III, institute
It states and contains resistant dextrin liquid glucose and gluconic acid in reaction solution III；
(2) reaction solution III made from step (1) is neutralized through alkali or basic anhydride, activated carbon decolorizing is condensed into 15-
30% liquid glucose；Contain resistant dextrin and gluconate in the liquid glucose；
(3) by made from step (2) liquid glucose carry out ion-exchange process, the ion-exchange process using highly acid sun from
Sub-exchange resin-weak-base anion-exchange resin-strong-base anion-exchange resin series system carries out, by ion exchange
Resistant dextrin finished product is made by being concentrated and dried in material after process, and ammonium hydroxide elution side is used to weak-base anion-exchange resin
Formula realizes the elution to gluconate, and gluconic acid finished product is made through deamination, desalination, concentration, crystallization；
Preferably, the starch material in the step (1) is selected from cornstarch, wheaten starch, tapioca, potato and forms sediment
One or more in powder or rice starch；It is further preferred that the starch material is cornstarch；
Preferably, the acid in the step (1) for hydrochloric acid, sulfuric acid, methanesulfonic acid, citric acid, lactic acid, one kind in acetic acid or
It is a variety of, it is further preferred that the acid is hydrochloric acid；The adding proportion of the acid is the 0.02~5% of starch material quality；
Preferably, step (1) the high temperature vacuum dextrinization reaction actual conditions is：Vacuum degree maintains -0.35~
0.8Mpa, 60~90 DEG C of 20~40min of heat preservation；Then heat to 140~180 DEG C of 40~60min of heat preservation；
Preferably, pH use in the step (1) to contain for 8.0~9.0 NaOH aqueous solutions adjusting reaction solution I to solid content
It is 5.5~6.5 to measure as 30~50%, pH；α-amylase pyroreaction condition reacts 15~20min, the liquid for 105~110 DEG C
Change enzyme is high temperature resistant α-amylase, and the U/g of 10,000 U of enzyme activity~200,000, adding proportion is the 0.02~1% of reaction solution I mass；
Preferably, enzyme pyroreaction to be liquefied terminates in the step (1), when temperature is reduced to 60 DEG C, adds in phosphoric acid tune
Reaction solution II pH to 4.2~4.8 are saved, carbohydrase, glucose oxidase and catalase is then added in and carries out saccharification reaction,
Reaction temperature is 60 DEG C, and the reaction time is 12~60h；The carbohydrase (enzyme activity is the U/g of 30,000 U~200,000), grape are glycoxidative
The adding proportion of enzyme (enzyme activity is the U/g of 10,000 U~100,000) and catalase (enzyme activity is the U/g of 100,000 U~800,000) is respectively
0.03~0.5%, 0.02~1.5% and the 0.02~1.5% of reaction solution II, further preferred glucose oxidase and peroxidating
Hydrogen enzyme mass ratio is 1:1；
Preferably, step (1) the high temperature enzyme-removal temperature is 80 DEG C, and the time is 30~40min (being preferably 30min)；
Preferably, alkali includes sodium hydroxide, potassium hydroxide, zinc hydroxide and calcium oxide in the step (2)；It is alkaline oxygenated
Object includes calcium oxide；
Preferably, step (3) intermediate ion exchanges process and is handed over for storng-acid cation exchange resin-weakly-basic anion
Resin-strong-base anion-exchange resin-storng-acid cation exchange resin is changed, is connected after strong-base anion-exchange resin
Storng-acid cation exchange resin is conducive to the adjusting of antagonism dextrin pH；
Preferably, weak-base anion-exchange resin sample introduction flow velocity is 0.3- in step (3) ion-exchange process
1.5ml/min, temperature are 25-50 DEG C, and pH is 1.0~2.0；
Preferably, step (3) the middle strong acidity cation exchange resin is exchanged including strongly acidic styrene's cation
Resin (001 × 7 resin), the weak-base anion-exchange resin include D301 resins or D318 resins, and the strong basicity is cloudy
Ion exchange resin includes 201 × 7 resins, D730 resins, D750 resins, D770 resins and 732 resins；
Preferably, specific method is concentrated and dried in the step (3) to be concentrated using quadruple effect, is spray-dried；It is furthermore preferred that
The spray drying actual conditions is that inlet air temperature is 150~350 DEG C, and temperature of outgoing air is 75~180 DEG C, pressure for -80~-
500Pa；
Preferably, in the step (3) ammonium hydroxide elution flow rate be 0.3-3.0ml/min, using electrodialysis to elution after
Gluconic acid carries out deamination, then gluconic acid finished product is made through quadruple effect condensing crystallizing in desalination；
The second aspect of the invention discloses resistant dextrin and gluconic acid that the above method is prepared；
The third aspect of the invention discloses application of the above method in resistant dextrin and gluconic acid is prepared.
Beneficial effects of the present invention：
(1) present invention is converted into grape by using the hydrolysate glucose of unconverted resistant dextrin in starch
Saccharic acid, and oxidative decoloration is carried out to material using hydrogen peroxide a small amount of after enzymolysis, then decomposed by catalase
Integrated technology, realize high-purity resistant dextrin and produced altogether with gluconic acid；
(2) present invention can realize grape by converting glucose into gluconic acid technology by ion-exchange process
The separation of sugar and resistant dextrin prepares high-purity resistant dextrin, and equipment investment cost is low, technology simple possible；
(3) present invention is handed over using storng-acid cation exchange resin-weak-base anion-exchange resin-strong alkalinity anion
Resin-storng-acid cation exchange resin purification process is changed, can not only realize the separation and elution of gluconic acid, but also can be with
The color of antagonism dextrin carries out maximum removing, while avoids conventional chromatogram separation or nanofiltration separation investment in machinery and equipment and energy
Consumption；
(4) by the way that acid adding, the vacuum degree of charging and temperature is controlled to realize the combination of nitration mixture and drying process, in reaction process
In by controlling vacuum degree, realize material and oxygen exposure level, while control heat radiation heat transfer caused by excessive vacuum slow etc.
Drawback prepares acid adding, being charred in resistant dextrin technical process, adjusts so as to fulfill entire starch is completed in reaction vessel
Breast, liquefaction and etc. it is integrated；So as to greatly reduce equipment investment, so as to advantageously reduce production cost, it is more suitable for resistance paste
The industrialized production of essence and gluconic acid.
Description of the drawings
Fig. 1 is present invention industrialization synchronous production resistant dextrin and gluconic acid process flow chart.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.It is unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As background technology is introduced, soya-bean milk powder is prepared in the prior art and takes into full account soya-bean milk part beans raw meat and soybean milk powder
Stability problem；
In view of this, in an exemplary embodiment of the invention, a kind of method of industrialized production resistant dextrin is provided,
This method comprises the following steps：
(1) into starch material add in acid, high-temperature vacuum dextrinization reaction, after reaction, adjust reaction solution I pH to
5.5~6.5, it adds in α-amylase and carries out pyroreaction；After reaction, reaction solution II pH to 4.0~4.8 are adjusted, add in saccharification
Enzyme, glucose oxidase and catalase carry out saccharification reaction, and after reaction, high temperature destroy the enzyme treatment obtains reaction solution III, institute
It states and contains resistant dextrin liquid glucose and gluconic acid in reaction solution III；
(2) reaction solution III made from step (1) is neutralized through alkali or basic anhydride, activated carbon decolorizing is condensed into 15-
30% liquid glucose；Contain resistant dextrin and gluconate in the liquid glucose；
(3) by made from step (2) liquid glucose carry out ion-exchange process, the ion-exchange process using highly acid sun from
Sub-exchange resin-weak-base anion-exchange resin-strong-base anion-exchange resin series system carries out, by ion exchange
Resistant dextrin finished product is made by being concentrated and dried in material after process, and ammonium hydroxide elution side is used to weak-base anion-exchange resin
Formula realizes the elution to gluconate, and gluconic acid finished product is made through deamination, desalination, concentration, crystallization；
In the another exemplary embodiment of the present invention, the starch material in the step (1) is selected from cornstarch, wheat forms sediment
One or more in powder, tapioca, potato starch or rice starch；It is further preferred that the starch material is jade
Rice starch；
In the another exemplary embodiment of the present invention, the acid in the step (1) is hydrochloric acid, sulfuric acid, methanesulfonic acid, lemon
One or more in acid, lactic acid, acetic acid, it is further preferred that the acid is hydrochloric acid；The adding proportion of the acid is former for starch
Expect the 0.02~5% of quality；
In the another exemplary embodiment of the present invention, step (1) the high temperature vacuum dextrinization reaction actual conditions is：
Vacuum degree maintains -0.35~0.8Mpa, 60~90 DEG C of 20~40min of heat preservation；Then heat to 140~180 DEG C heat preservation 40~
60min；
Used in the another exemplary embodiment of the present invention, in the step (1) pH for 8.0~9.0 NaOH aqueous solutions
It is that 30~50%, pH is 5.5~6.5 that reaction solution I, which is adjusted, to solid content；α-amylase pyroreaction condition is 105~110 DEG C
15~20min is reacted, the adding proportion of the α-amylase is the 0.02~1% of reaction solution I mass；
In the another exemplary embodiment of the present invention, enzyme pyroreaction to be liquefied terminates in the step (1), and temperature reduces
During to 60 DEG C, add in phosphoric acid and adjust reaction solution II pH to 4.2~4.8, then add in carbohydrase, glucose oxidase and peroxide
Change hydrogen enzyme and carry out saccharification reaction, reaction temperature is 60 DEG C, and the reaction time is 12~60h；The carbohydrase, glucose oxidase and
The adding proportion of catalase is respectively 0.03~0.5%, 0.02~1.5% and the 0.02~1.5% of reaction solution II；Its
In, carbohydrase, glucose oxidase and catalase add or first add in together carbohydrase carry out saccharification reaction one section when
Between after add glucose oxidase and peroxidase；
Wherein, α-amylase is high temperature resistant α-amylase, the U/g of 10,000 U of enzyme activity~200,000；Glucoamylase enzyme vigor is 30,000 U~20
Ten thousand U/g, glucose oxidase enzyme activity are the U/g of 10,000 U~100,000, and catalase enzyme activity is the U/g of 100,000 U~800,000.
In the another exemplary embodiment of the present invention, step (1) the high temperature enzyme-removal temperature is 80 DEG C, the time for 30~
40min (being preferably 30min)；
In the another exemplary embodiment of the present invention, alkali includes sodium hydroxide, potassium hydroxide, hydrogen-oxygen in the step (2)
Change zinc and calcium oxide；Basic anhydride include calcium oxide；
In the another exemplary embodiment of the present invention, step (3) intermediate ion exchanges process and is handed over for highly acidic cation
Resin-weak-base anion-exchange resin-strong-base anion-exchange resin-storng-acid cation exchange resin is changed, in highly basic
It connects after property anion exchange resin storng-acid cation exchange resin, is conducive to the adjusting of antagonism dextrin pH；
In the another exemplary embodiment of the present invention, weakly-basic anion exchanges in step (3) ion-exchange process
Resin sample introduction flow velocity is 0.3-1.5ml/min, and temperature is 25-50 DEG C, and pH is 1.0~2.0；
In the another exemplary embodiment of the present invention, step (3) the middle strong acidity cation exchange resin includes strong acid
Property styrene type cation exchange resin (001 × 7 resin), the weak-base anion-exchange resin include D301 resins or
D318 resins, the strong-base anion-exchange resin include 201 × 7 resins, D730 resins, D750 resins, D770 resins and
732 resins；
It is dense using quadruple effect that specific method is concentrated and dried in the another exemplary embodiment of the present invention, in the step (3)
Contracting, spray drying；It is furthermore preferred that the spray drying actual conditions is that inlet air temperature is 150~350 DEG C, temperature of outgoing air 75
~180 DEG C, pressure is -80~-500Pa；
In the another exemplary embodiment of the present invention, ammonium hydroxide elution flow rate is 0.3-3.0ml/min in the step (3),
Deamination is carried out to the gluconic acid after elution using electrodialysis, then gluconic acid finished product is made through quadruple effect condensing crystallizing in desalination；
In the another exemplary embodiment of the present invention, resistant dextrin and glucose that the above method is prepared are provided
Acid；
In the another exemplary embodiment of the present invention, the above method is provided in resistant dextrin and gluconic acid is prepared
Using.
Explanation is further explained to the present invention by the following examples, but is not construed as limiting the invention.
Embodiment 1
5t reaction kettles are controlled vacuum degree in advance in advance, and up to -0.085~0.1MPa, temperature is adjusted to 90 DEG C, closes negative pressure
Maintenance system is opened maximum speed of agitator and is fed, into cornstarch 1t, since filling opening plus 1% hydrochloric acid, entirely
Process -0.05~0.08Mpa of vacuum degree control continues into starch 2t, 1% hydrochloric acid 60kg, when negative pressure is less than 0.05Mpa,
All feed inlets are closed, open negative pressure system, material mixing is carried out, negative pressure valve is closed when remaining charging, when opening negative pressure valve
Close material mouth.Treat that all materials into finishing, are started to warm up after -0.05Mpa80 DEG C of 20~40min of stirring of maintenance to 165 DEG C
60min is maintained, whole process maintains vacuum degree to reach -0.05~0.08MPa.
After reaction, by filling opening add in pH8.0~9.0 NaOH aqueous solutions size mixing to pH to continue after 6.5 plus
It is 50% that water, which adjusts solid content, adds in 1% α-amylase, and 105~110 DEG C of reaction 15min into saccharifying tank, add water by solid
Object adjusts to 35% and treats that temperature is reduced to 60 DEG C, and 0.3% carbohydrase, 0.02 Portugal are added in using phosphorus acid for adjusting pH to 4.2~4.8
Grape carbohydrate oxidase and 0.02% catalase are in 60 DEG C of saccharification 36h.Enzyme deactivation is carried out after saccharification, enzyme-removal temperature is 80 DEG C,
Time is 30min.It adds in calcium oxide at this time to be neutralized, activated carbon decolorizing.Resistant dextrin liquid glucose and gluconic acid after decoloration
Calcium compound is condensed into 15~30% liquid glucose, is directly entered ion-exchange process.
Wherein, α-amylase be high temperature resistant α-amylase, 10,000 U/g of enzyme activity；100,000 U/g of glucoamylase enzyme vigor, grape are glycoxidative
Enzyme enzyme activity is 100,000 U/g and catalase enzyme activity is 800,000 U/g.
Ion exchange process resin uses storng-acid cation exchange resin-weak-base anion-exchange resin-strong basicity
Anion exchange resin-storng-acid cation exchange resin series system carries out, and the material by after ion-exchange directly passes through concentration
Resistant dextrin is made in spray drying.Wherein storng-acid cation exchange resin is 001 × 7, and weak-base anion-exchange resin is
D318, strong-base anion-exchange resin are 201 × 7.Weak-base anion-exchange resin charging pH is 1.0-2.0, is fed
Temperature is 35 DEG C, flow velocity 0.3ml/min, after charging, by 2.0mol/L ammonium hydroxide to weak-base anion-exchange resin
Elution is carried out so as to which gluconate be eluted, elution flow rate 0.3ml/min；From weak-base anion-exchange resin tree
Fat discharging is directly entered strong-base anion-exchange resin selection 201 × 7.Then concentrated by quadruple effect, spray drying becomes anti-
Property dextrin finished product.Wherein, spray drying EAT is 160 DEG C, and temperature of outgoing air is 110 DEG C, and pressure is -80~-500Pa.It washes
The gluconate taken off using electrodialysis carry out deamination, desalination, then by quadruple effect condensing crystallizing obtain gluconic acid into
Product.
Using GB/T 22224-2008《The measure enzymatic gravimetric method of dietary fiber and enzymatic gravimetric method-liquid chromatogram in food
In method》Second method enzymatic gravimetric method --- liquid chromatography carries out resistant dextrin content detection, wherein resistant dextrin content
83.47%.
Embodiment 2
5t reaction kettles are controlled vacuum degree in advance in advance, and up to -0.1MPa, temperature is adjusted to 80 DEG C, is closed negative pressure and is maintained system
System is opened maximum speed of agitator and is fed, into cornstarch 0.5t, since filling opening plus 1% hydrochloric acid, whole process
Vacuum degree control -0.05~0.08Mpa continues into starch 2.5t, hydrochloric acid 450kg, when negative pressure is less than 0.05Mpa, closes
All feed inlets open negative pressure system, carry out material mixing, close negative pressure valve when remaining charging, closed when opening negative pressure valve
Material mouth.Treat that all materials into finishing, are started to warm up after 80 DEG C of stirring 40min of maintenance -0.05Mpa to 155 DEG C of maintenances
50min, whole process maintain vacuum degree to reach -0.05~0.08MPa.
After reaction, the NaOH aqueous solutions for pH8.0~9.0 being added in by filling opening are sized mixing and are continued plus water for 5.5 to pH
It is 30% to adjust solid content, adds in 0.02% α-amylase, and 105~110 DEG C of reaction 15min into saccharifying tank, add water by solid
Object adjusts to 35% and treats that temperature is reduced to 60 DEG C, using the carbohydrase of the additions of phosphoric acid condition pH to 4.2~4.8 0.5% at 60 DEG C
Saccharification adds in 1.5% glucose oxidase and 1.5% catalase in 60 DEG C of saccharification 36h afterwards for 24 hours.It goes out after saccharification
Enzyme, enzyme-removal temperature are 80 DEG C, time 30min.It adds in calcium oxide at this time to be neutralized, activated carbon decolorizing.Resistance after decoloration
Dextrin liquid glucose and gluconic acid calcium compound are condensed into 30% liquid glucose, are directly entered ion-exchange process.
Wherein α-amylase be high temperature resistant α-amylase, 200,000 U/g of enzyme activity；Glucoamylase enzyme vigor is 80,000 U/g, grape glycosyloxy
It is 400,000 U/g to change 40,000 U/g of enzyme and catalase enzyme activity.
Ion exchange process resin uses storng-acid cation exchange resin-weak-base anion-exchange resin-strong basicity
Anion exchange resin-storng-acid cation exchange resin series system carries out, and wherein storng-acid cation exchange resin is 001
× 7, weak-base anion-exchange resin D318, feeding temperature are 50 DEG C, and flow velocity 1.0ml/min, pH are 1.0~2.0；
Strong-base anion-exchange resin selects D770.Strong alkalinity anion is directly entered from weak-base anion-exchange resin discharging to hand over
Change Choice of Resin D770.Then concentrated by quadruple effect, spray drying becomes resistant dextrin finished product, and spray drying EAT is
150 DEG C, temperature of outgoing air is 75 DEG C, and pressure is -80~-500Pa.Weak-base anion-exchange resin is washed by 1.0mol/L ammonium hydroxide
The de- elution realized to gluconate, elution flow rate 1.0ml/min；Deamination is carried out using electrodialysis, then desalination is passed through
Quadruple effect condensing crystallizing obtains gluconic acid finished product.
Using GB/T 22224-2008《The measure enzymatic gravimetric method of dietary fiber and enzymatic gravimetric method-liquid chromatogram in food
In method》Second method enzymatic gravimetric method --- liquid chromatography carries out resistant dextrin content detection, wherein resistant dextrin content
89.94%.
Embodiment 3
5t reaction kettles are controlled vacuum degree in advance in advance, and up to -0.085~0.1MPa, temperature is adjusted to 90 DEG C, closes negative pressure
Maintenance system is opened maximum speed of agitator and is fed, into cornstarch 1t, since filling opening plus 2% hydrochloric acid, entirely
Process -0.05~0.08Mpa of vacuum degree control continues into starch 2t, 1% hydrochloric acid 300kg, when negative pressure is less than 0.05Mpa,
All feed inlets are closed, open negative pressure system, material mixing is carried out, negative pressure valve is closed when remaining charging, when opening negative pressure valve
Close material mouth.Treat that all materials into finishing, are started to warm up after -0.05Mpa80 DEG C of 20~40min of stirring of maintenance to 165 DEG C
60min is maintained, whole process maintains vacuum degree to reach -0.05~0.08MPa.
After reaction, by filling opening add in pH8.0~9.0 NaOH aqueous solutions size mixing to pH to continue after 6.5 plus
It is 50% that water, which adjusts solid content, adds in 0.2% α-amylase, and 105~110 DEG C of reaction 15min into saccharifying tank, add water solid
Shape object adjusts to 35% and treats that temperature is reduced to 60 DEG C, using phosphorus acid for adjusting pH to 4.2~4.8 add in 0.05% carbohydrase,
1.5% glucose oxidase and 1.5% catalase are in 60 DEG C of saccharification 36h.Enzyme deactivation is carried out after saccharification, enzyme-removal temperature is
80 DEG C, time 30min.It adds in calcium oxide at this time to be neutralized, activated carbon decolorizing.Resistant dextrin liquid glucose and grape after decoloration
Saccharic acid calcium compound is condensed into 15~30% liquid glucose, is directly entered ion-exchange process.
Wherein α-amylase is high temperature resistant α-amylase, and enzyme activity is the U/g of 10,000 U~200,000；Glucoamylase enzyme vigor for 200,000 U/g,
Glucose oxidase enzyme activity is 40,000 U/g and catalase enzyme activity is 400,000 U/g.
Ion exchange process resin uses storng-acid cation exchange resin-weak-base anion-exchange resin-strong basicity
Anion exchange resin-storng-acid cation exchange resin series system carries out, and the material by after ion-exchange directly passes through concentration
Resistant dextrin is made in spray drying.Wherein storng-acid cation exchange resin is 001 × 7, and weak-base anion-exchange resin is
D318, strong-base anion-exchange resin are 201 × 7.Weak-base anion-exchange resin charging pH is 1.0-2.0, is fed
Temperature is 35 DEG C, flow velocity 0.3ml/min, after charging, by 0.5mol/L ammonium hydroxide to weak-base anion-exchange resin
Elution is carried out so as to which gluconate be eluted, elution flow rate 3.0ml/min；From weak-base anion-exchange resin tree
Fat discharging is directly entered strong-base anion-exchange resin selection 201 × 7.Then concentrated by quadruple effect, spray drying becomes anti-
Property dextrin finished product.Wherein, spray drying EAT is 160 DEG C, and temperature of outgoing air is 110 DEG C, and pressure is -80~-500Pa.It washes
The gluconate taken off using electrodialysis carry out deamination, desalination, then by quadruple effect condensing crystallizing obtain gluconic acid into
Product.
Using GB/T 22224-2008《The measure enzymatic gravimetric method of dietary fiber and enzymatic gravimetric method-liquid chromatogram in food
In method》Second method enzymatic gravimetric method --- liquid chromatography carries out resistant dextrin content detection, wherein resistant dextrin content
90.02%, but product color is apparently higher than embodiment 1 and embodiment 2.
Comparative example 1
5t reaction kettles are controlled vacuum degree in advance in advance, and up to -0.085~0.1MPa, temperature is adjusted to 90 DEG C, closes negative pressure
Maintenance system is opened maximum speed of agitator and is fed, into cornstarch 1t, since filling opening plus 1% hydrochloric acid, entirely
Process -0.05~0.08Mpa of vacuum degree control continues into starch 2t, hydrochloric acid 60kg, when negative pressure is less than 0.05Mpa, closes
All feed inlets open negative pressure system, carry out material mixing, close negative pressure valve when remaining charging, closed when opening negative pressure valve
Material mouth.Treat that all materials into finishing, are started to warm up after -0.05Mpa80 DEG C of 20~40min of stirring of maintenance to 165 DEG C of maintenances
60min, whole process maintain vacuum degree to reach -0.05~0.08MPa.
After reaction, it is 6.5 to be sized mixing by the NaOH aqueous solutions of filling opening addition pH8.0~9.0 to pH；Solid at this time
Object is 50%, adds in 1% α-amylase, and 105-110 DEG C of reaction 15min into saccharifying tank, adds water to adjust solid content to 35%
Treat that temperature is reduced to 60 DEG C, using the carbohydrase of the additions of phosphoric acid condition pH to 4.2 0.3% in 60 DEG C of saccharification 36h.After saccharification
Enzyme deactivation is carried out, enzyme-removal temperature is 80 DEG C, time 30min.It adds in calcium oxide at this time to be neutralized, activated carbon decolorizing.After decoloration
Resistant dextrin liquid glucose 30% liquid glucose, be directly entered ion-exchange process.
Wherein α-amylase is high temperature resistant α-amylase, and enzyme activity is the U/g of 10,000 U~200,000；Glucoamylase enzyme vigor is 100,000 U/g.
Ion exchange process resin is handed over using storng-acid cation exchange resin-strong-base anion-exchange resin-strong alkalinity anion
It changes resin-storng-acid cation exchange resin series system to carry out, wherein storng-acid cation exchange resin is 001 × 7, highly basic
Property anion exchange resin selection 201 × 7.Then concentrated by quadruple effect and sugar concentration is concentrated into 50%-60%；Spray drying
As resistant dextrin finished product.Spray drying EAT is 150 DEG C, and temperature of outgoing air is 75 DEG C, and pressure is -80~-500Pa.
Using GB/T 22224-2008《The measure enzymatic gravimetric method of dietary fiber and enzymatic gravimetric method-liquid chromatogram in food
In method》Second method enzymatic gravimetric method --- liquid chromatography carries out resistant dextrin content detection, and wherein resistant dextrin content is
55.47%.
The foregoing is merely the preferred embodiments of the application, are not limited to the application, for the skill of this field
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. method of industrialized production resistant dextrin, which is characterized in that the described method comprises the following steps：(1) acid is added in into starch material, high-temperature vacuum dextrinization is reacted, after reaction, adjusting reaction solution I pH to 5.5~ 6.5, it adds in α-amylase and carries out pyroreaction；After reaction, reaction solution II pH to 4.2~4.8 are adjusted, add in carbohydrase, Portugal Grape carbohydrate oxidase and catalase carry out saccharification reaction, and after reaction, high temperature destroy the enzyme treatment obtains reaction solution III, described anti- It answers and contains resistant dextrin and gluconic acid solution in liquid III；(2) reaction solution III made from step (1) is neutralized through alkali or basic anhydride, activated carbon decolorizing is condensed into 15-30% Liquid glucose；Contain resistant dextrin and gluconate in the liquid glucose；(3) liquid glucose made from step (2) is subjected to ion-exchange process, the ion-exchange process is handed over using highly acidic cation It changes resin-weak-base anion-exchange resin-strong-base anion-exchange resin series system to carry out, by ion-exchange process Resistant dextrin finished product is made by being concentrated and dried in material afterwards, real using ammonium hydroxide type of elution to weak-base anion-exchange resin Now to the elution of gluconate, gluconic acid finished product is made through deamination, desalination, concentration, crystallization.
- 2. method as described in claim 1, which is characterized in that the starch material in the step (1) is selected from cornstarch, wheat One or more in starch, tapioca, potato starch or rice starch；Preferably, the starch material forms sediment for corn Powder；Acid in the step (1) is hydrochloric acid, the one or more in sulfuric acid, methanesulfonic acid, citric acid, lactic acid, acetic acid, preferably , the acid is hydrochloric acid；The adding proportion of the acid is the 0.02~5% of starch material quality.
- 3. method as described in claim 1, which is characterized in that step (1) the high temperature vacuum dextrinization reacts actual conditions For：Vacuum degree maintains -0.35~0.8Mpa, 60~90 DEG C of 20~40min of heat preservation；Then heat to 140~180 DEG C of heat preservations 40 ~60min.
- 4. method as described in claim 1, which is characterized in that use pH water-soluble for 8.0~9.0 NaOH in the step (1) It is that 30~50%, pH is 5.5~6.5 that liquid, which adjusts reaction solution I to solid content,；α-amylase pyroreaction condition is 105~110 DEG C 15~20min of reaction, the adding proportion of the α-amylase is the 0.02~1% of reaction solution I mass.
- 5. method as described in claim 1, which is characterized in that enzyme pyroreaction to be liquefied terminates in the step (1), temperature drop During down to 60 DEG C, add in phosphoric acid and adjust reaction solution II pH to 4.2~4.8, then add in carbohydrase, glucose oxidase and mistake Hydrogen oxide enzyme carries out saccharification reaction, and reaction temperature is 60 DEG C, and the reaction time is 12~60h；The carbohydrase, glucose oxidase Adding proportion with catalase is respectively 0.03~0.5%, 0.02~1.5% and the 0.02~1.5% of reaction solution II；Wherein, α-amylase is high temperature resistant α-amylase, the U/g of 10,000 U of enzyme activity~200,000；Glucoamylase enzyme vigor is the U/ of 30,000 U~200,000 G, glucose oxidase enzyme activity is the U/g of 10,000 U~100,000 and catalase enzyme activity is the U/g of 100,000 U~800,000；Step (1) the high temperature enzyme-removal temperature is 80 DEG C, and the time is 30~40min (being preferably 30min).
- 6. method as described in claim 1, which is characterized in that alkali includes sodium hydroxide, potassium hydroxide, hydrogen in the step (2) Zinc oxide and calcium oxide；Basic anhydride include calcium oxide.
- 7. method as described in claim 1, which is characterized in that it is highly acidic cation that step (3) intermediate ion, which exchanges process, Exchanger resin-weak-base anion-exchange resin-strong-base anion-exchange resin-storng-acid cation exchange resin；In step (3) ion-exchange process weak-base anion-exchange resin sample introduction flow velocity be 0.3-1.5ml/min, temperature For 25-50 DEG C, pH is 1.0~2.0；Preferably, step (3) the middle strong acidity cation exchange resin includes strongly acidic styrene type cation exchange resin (001 × 7 resin), the weak-base anion-exchange resin include D301 resins or D318 resins, the strong alkalinity anion Exchanger resin includes 201 × 7 resins, D730 resins, D750 resins, D770 resins and 732 resins.
- 8. method as described in claim 1, which is characterized in that it is using quadruple effect that specific method is concentrated and dried in the step (3) Concentration, spray drying；It is furthermore preferred that the spray drying actual conditions is that inlet air temperature is 150~350 DEG C, temperature of outgoing air is 75~180 DEG C, pressure is -80~-500Pa.
- 9. method as described in claim 1, which is characterized in that ammonium hydroxide elution flow rate is 0.33.0ml/min in the step (3), Deamination is carried out to the gluconic acid after elution using electrodialysis, then gluconic acid finished product is made through quadruple effect condensing crystallizing in desalination.
- 10. resistant dextrin and gluconic acid that any one of claim 1-9 the method is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711462244.1A CN108103125B (en) | 2017-12-28 | 2017-12-28 | Preparation process and application for industrially producing water-soluble dietary fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711462244.1A CN108103125B (en) | 2017-12-28 | 2017-12-28 | Preparation process and application for industrially producing water-soluble dietary fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108103125A true CN108103125A (en) | 2018-06-01 |
| CN108103125B CN108103125B (en) | 2022-03-22 |
Family
ID=62214126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711462244.1A Active CN108103125B (en) | 2017-12-28 | 2017-12-28 | Preparation process and application for industrially producing water-soluble dietary fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108103125B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826408A (en) * | 2020-07-27 | 2020-10-27 | 江苏省奥谷生物科技有限公司 | Preparation process of beta-cyclodextrin |
| CN114990170A (en) * | 2022-07-04 | 2022-09-02 | 青岛龙鼎生物技术有限公司 | Method for co-producing fructose and gluconic acid or gluconate by enzyme catalysis of glucose |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908017A (en) * | 2006-08-18 | 2007-02-07 | 广东省食品工业研究所 | Preparation technique of resistant maltodextrin |
| CN101870991A (en) * | 2010-06-08 | 2010-10-27 | 保龄宝生物股份有限公司 | Method for preparing novel anti-peptic dextrin |
| CN105996061A (en) * | 2016-05-12 | 2016-10-12 | 河南泰利杰生物科技有限公司 | Preparation process of dextrin difficult to digest |
| CN106244647A (en) * | 2016-08-24 | 2016-12-21 | 山东福洋生物科技有限公司 | A kind of method simultaneously preparing trehalose and gluconic acid lactone |
| CN106318991A (en) * | 2016-08-19 | 2017-01-11 | 山东百龙创园生物科技有限公司 | Resistant dextrin and preparation method thereof |
| CN106755203A (en) * | 2016-11-28 | 2017-05-31 | 保龄宝生物股份有限公司 | A kind of preparation method of resistant dextrin |
-
2017
- 2017-12-28 CN CN201711462244.1A patent/CN108103125B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908017A (en) * | 2006-08-18 | 2007-02-07 | 广东省食品工业研究所 | Preparation technique of resistant maltodextrin |
| CN101870991A (en) * | 2010-06-08 | 2010-10-27 | 保龄宝生物股份有限公司 | Method for preparing novel anti-peptic dextrin |
| CN105996061A (en) * | 2016-05-12 | 2016-10-12 | 河南泰利杰生物科技有限公司 | Preparation process of dextrin difficult to digest |
| CN106318991A (en) * | 2016-08-19 | 2017-01-11 | 山东百龙创园生物科技有限公司 | Resistant dextrin and preparation method thereof |
| CN106244647A (en) * | 2016-08-24 | 2016-12-21 | 山东福洋生物科技有限公司 | A kind of method simultaneously preparing trehalose and gluconic acid lactone |
| CN106755203A (en) * | 2016-11-28 | 2017-05-31 | 保龄宝生物股份有限公司 | A kind of preparation method of resistant dextrin |
Non-Patent Citations (5)
| Title |
|---|
| M. BLANCO等: "《On-line monitoring of starch enzymatic hydrolysis by near- infrared spectroscopy》", 《THE ANALYST》 * |
| 姜锡瑞等: "《全酶法生产葡萄糖酸钠》", 《2015中国生物发酵产业系列专题论坛论文集》 * |
| 张颖: "《抗性糊精的纯化及应用特性研究》", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
| 王博彦等: "《发酵有机酸生产与应用手册》", 30 September 2000 * |
| 郭峰: "《不同酶水解对抗性糊精消化性的影响研究》", 《食品工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826408A (en) * | 2020-07-27 | 2020-10-27 | 江苏省奥谷生物科技有限公司 | Preparation process of beta-cyclodextrin |
| CN114990170A (en) * | 2022-07-04 | 2022-09-02 | 青岛龙鼎生物技术有限公司 | Method for co-producing fructose and gluconic acid or gluconate by enzyme catalysis of glucose |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108103125B (en) | 2022-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105543311B (en) | A kind of processing method of resistant dextrin | |
| CN101455398B (en) | Soya-dregs water soluble diet fiber preparation method using nano filtration and spray-drying method | |
| CN106318991A (en) | Resistant dextrin and preparation method thereof | |
| CN101643795A (en) | Method for preparing xylose and xylitol by using bamboo | |
| CN108103125A (en) | A kind of industrialized production water-soluble dietary fiber preparation process and application | |
| CN105996061A (en) | Preparation process of dextrin difficult to digest | |
| CN108265091A (en) | A kind of technique for preparing fructose syrup using rice | |
| CN101787385B (en) | Preparation method for medical glucose with ultrahigh purity | |
| CN103404764A (en) | Resistant malt dextrin and preparation method thereof | |
| CN103798893B (en) | A kind of pumpkin Composite vinegar beverage and preparation method thereof | |
| CN112226474A (en) | Preparation method of D-psicose crystal | |
| CN103125807A (en) | Method for preparing alum-free vermicelli based on modified starch | |
| CN105613940A (en) | Method for extracting Chinese chestnut peptide | |
| CN101824097B (en) | Method for producing polyglucose | |
| CN105624235A (en) | Method for preparing xylose by utilizing eucalyptus pulp waste liquid | |
| CN105586368B (en) | A kind of method of the processing method and fermentation production of citric acid of sorghum seed | |
| CN105968226B (en) | A kind of preparation method of high-purity hydrogenation polydextrose | |
| CN109234336A (en) | A kind of method of dextrase enzymolysis inulin production oligofructose | |
| CN108902667A (en) | A kind of preparation method of caramel colorant | |
| CN107287258A (en) | A kind of preparation method of the resistant dextrin containing oligoisomaltose | |
| CN103665182A (en) | Acid degradation preparation method of konjac glucomannan | |
| CN109402198B (en) | Preparation method of special syrup for crunchy candy | |
| CN101880298A (en) | Method for preparing food-grade xylooligosaccharide | |
| CN1396175A (en) | Process for extracting both active embryonic peptide and natural corn oil from embryo bud of corn | |
| CN105919050B (en) | A kind of anti-digest carbohydrate and its processing method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220225 Address after: 251200 Yucheng national high tech Industrial Development Zone, De Zhou City, Shandong Province Applicant after: SHANDONG LONGLIVE BIO-TECHNOLOGY Co.,Ltd. Address before: 251200 Yucheng hi tech Development Zone, Dezhou City, Shandong Province Applicant before: SHANDONG LONGLIVE BIO-TECHNOLOGY Co.,Ltd. Applicant before: Heilongjiang Longli Biotechnology Co., Ltd |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |