CN104171800A - Isomaltooligosacharide-fructooligosaccharide composite particle and preparation method thereof - Google Patents

Isomaltooligosacharide-fructooligosaccharide composite particle and preparation method thereof Download PDF

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Publication number
CN104171800A
CN104171800A CN201410389991.7A CN201410389991A CN104171800A CN 104171800 A CN104171800 A CN 104171800A CN 201410389991 A CN201410389991 A CN 201410389991A CN 104171800 A CN104171800 A CN 104171800A
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fos
oligoisomaltose
liquid glucose
preparation
make
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邵先豹
干昭波
杨腾腾
窦光朋
张明站
张兴晶
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Shandong Bailong Chuangyuan Bio Tech Co Ltd
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Shandong Bailong Chuangyuan Bio Tech Co Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation 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
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/16Preparation of compounds containing saccharide radicals produced by the action of an alpha-1, 6-glucosidase, e.g. amylose, debranched amylopectin
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/22Preparation of compounds containing saccharide radicals produced by the action of a beta-amylase, e.g. maltose
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01001Alpha-amylase (3.2.1.1)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01002Beta-amylase (3.2.1.2)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01041Pullulanase (3.2.1.41)
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention relates to an iosomaltooligosacharide-fructooligosaccharide composite particle and a preparation method thereof. The iosomaltooligosacharide-fructooligosaccharide composite particle comprises the following components in percentage by weight: 51-99% of iosomaltooligosacharide and 1-49% of fructooligosaccharide. The invention also relates to the preparation method of the composite particle. By virtue of the preparation method of the composite particle, iosomaltooligosacharide is firstly mixed with fructooligosaccharide according to a ratio for preparing the particle; the prepared composite particle has the advantages of good fluidity, high dissolubility, no moisture absorption, long shelf life, good effect of increasing probiotics in the intestinal tracts of the human bodies and the like, and is low in production cost; the additional value of iosomaltooligosacharide is greatly enhanced.

Description

A kind of oligoisomaltose and FOS composite particles and preparation method thereof
Technical field
The present invention relates to a kind of oligoisomaltose and FOS composite particles and preparation method thereof, belong to functional sugar preparing technical field.
Technical background
Oligoisomaltose (Isomaltooligosacharide) claim again bifurcation oligose, refer to that glucosyl group is with α-1, the monose number that 6 glycosidic bonds are combined into, at 2~6 class compound sugar that do not wait, because molecular conformation is different, is called oligoisomaltose for being different from maltose.
Oligoisomaltose has good physicochemical property and physiological function, as low in sugariness, is 40%~50% of sucrose, and the soft U.S. of sweet taste, and mouthfeel is more refreshing; Be difficult to be digested by gastric enzyme, heat is low, does not substantially increase blood pressure and blood lipoid; Promote the propagation of Bifidobacterium in human body intestinal canal, can suppress the formation of the interior harmful bacteria of enteron aisle and corrupt substance.In addition, oligomeric different wheat sugar has the performance of anti-carious tooth etc.In view of characteristic and the health care of oligoisomaltose, its range of application is very extensive, can be applied to the industries such as food, medicine, feed, cosmetics.
The research and development of China's functional oligose start from the beginning of the nineties, what form at present suitability for industrialized production mainly contains oligoisomaltose, FOS, xylo-oligosaccharide, wherein the most cheap with oligoisomaltose price, occupation rate of market is the highest, the problem of puzzlement oligoisomaltose industry development mainly contains two at present: the one, and the hygroscopicity problem of oligoisomaltose itself, easily form caking, the application to it in downstream product has a negative impact; The 2nd, oligoisomaltose to the value-added effect of beneficial bacteria of intestinal tract compared with FOS and xylo-oligosaccharide a little less than, downstream product client more and more tends to use FOS and xylo-oligosaccharide and does not use oligoisomaltose.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of oligoisomaltose and FOS composite particles and preparation method thereof are provided, the oligoisomaltose of preparing by the present invention and FOS composite particles have good fluidity, soluble, nonhygroscopic, shelf life of products long, to advantages such as human body intestinal canal probio value-added effect are good, effectively solved two problems of above puzzlement oligoisomaltose industry development.
In order to realize object of the present invention, the present invention adopts following technical scheme:
A composite particles for oligoisomaltose and FOS, component is as follows, is all weight percentage:
Oligoisomaltose 51%~99%, FOS 1%~49%.
Preferred according to the present invention, component is as follows, is all weight percentage:
Oligoisomaltose 60%~80%, FOS 20%~40%.
The preparation method of the composite particles of above-mentioned oligoisomaltose and FOS, step is as follows:
(1) by oligoisomaltose liquid glucose through concentrated, make mass concentration and be 60~70% oligoisomaltose liquid,
(2) FOS liquid glucose warp is concentrated, dry, make FOS powder,
(3) the FOS powder that oligoisomaltose liquid step (1) being made and step (2) make adds in fluid bed granulator granulation in proportion, under 50~80 ℃ of temperature conditions, granulate, cross after 40~60 order vibratory sieves, make the composite particles of oligoisomaltose and FOS;
Or step is as follows:
(a) oligoisomaltose liquid glucose warp is concentrated, dry, make oligoisomaltose powder,
(b) by FOS liquid glucose through concentrated, make mass concentration and be 40~50% FOS liquid,
(c) the FOS liquid that oligoisomaltose powder step (a) being made and step (b) make adds in fluid bed granulator granulation in proportion; under 50~80 ℃ of temperature conditions, granulate; cross after 40~60 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
Preferred according to the present invention, described step (1) or (a) in the preparation method of oligoisomaltose liquid glucose as follows:
(I) regulating starch slurry concentration, after adjusting pH, add high temperature resistant AMS, is 20%~25% liquefier through liquefying, making DE value;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, carry out after saccharification react, then add phlorose to turn glycosides enzyme, proceed to turn glycosides reaction, the enzyme that then goes out is lived, and makes liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, after decolouring, with adverse current ion-exchange chromatography, carry out ion-exchange desalination, make desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, the eluent that collection contains isomaltose, panose and Isomaltotriose, makes the oligoisomaltose liquid glucose that isomaltose+panose in total reducing sugar+Isomaltotriose content is not less than 95wt%.
Further preferred according to the present invention, in described step (I), starch slurry concentration is 15~20 Baume degrees, and pH value is 4~6.5, and the addition of high-temperatureα-amylase is that starch material per ton adds 1.2 * 10 7~2.0 * 10 7u, condensing temperature is 110~141 ℃.More excellent, described liquefaction is steam ejection liquefaction, liquefaction number of times is twice.
Further preferred according to the present invention, in described step (II), the addition of described beta amylase is that starch material per ton adds 1.0 * 10 8~1.5 * 10 8the addition of U, Pullulanase is that starch material per ton adds 1.2 * 10 5~1.5 * 10 5the addition of ASPU, fungi alpha amylase is that starch material per ton adds 0.1 * 10 8~0.3 * 10 8u is saccharification react 2~5h under the condition of 50~60 ℃ in temperature; The addition that described phlorose turns glycosides enzyme is that starch material per ton adds 1.8 * 10 8~3.6 * 10 8u is under the condition of 55~60 ℃, to turn glycosides reaction 26~32h in temperature.
Further preferred according to the present invention, in described step (III), the addition of active carbon is 0.3~0.5wt%, bleaching time 1.5~2.0h; Light transmittance >=85% of described desalination liquid glucose after ion-exchange desalination.
Further preferred according to the present invention, in described step (IV), chromatographic isolation service condition is operating pressure 0.25~0.35MPa, 65~70 ℃ of temperature, water loss-rate 1:1.2~1:1.5, charging 1.5~1.7m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose that isomaltose+panose in total reducing sugar+Isomaltotriose content is not less than 95wt%.
Preferred according to the present invention, described step (2) or (b) in the preparation method of FOS liquid glucose as follows:
(i) sucrose solution that preparation mass concentration is 25%~60%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, after reaction, make the thick solution of FOS;
(iii) step (ii) is made the thick solution of FOS through decolouring, filter, from handing over, chromatographic isolation, make the FOS liquid glucose that FOS content in total reducing sugar is not less than 95wt%.
Further preferred according to the present invention, in described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 0.5 * 10 6~1.5 * 10 6u, 20~40 ℃ of reaction temperatures, the reaction time is 20~36h.It is CGMCC No.9449 that Aspergillus niger strain BLCY-02 is deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) preserving number, β-transfructosylase that this bacterial strain produces is ectoenzyme, after isolation technics separation, separated enzyme liquid enzyme work can reach 1000U/ml routinely.
Further preferred according to the present invention, in described step (iii), decolour for activated carbon decolorizing, active carbon addition 0.1~0.3wt%, bleaching time 1~1.5h; Be filtered into plate-frame filtering; Through solution light transmittance >=85% after friendship.
Further preferred according to the present invention, in described step (iii), chromatographic isolation service condition is operating pressure 0.2~0.35MPa, 60~70 ℃ of temperature, water loss-rate 1:(1.2~1.5), charging 1.8~2.0m per hour 3, collect ketose, Nystose, GF4;
The high temperature resistant AMS that the present invention adopts act as and makes starch liquefaction and generate low molecule rapidly, so those skilled in the art can select corresponding high temperature resistant AMS according to actual needs, the high temperature resistant AMS of selling as Genencor Company.
The beta amylase that the present invention adopts act as from non reducing end successively take maltose as unit cut-out α-1,4-dextran chain, therefore those skilled in the art can select corresponding beta amylase according to actual needs, as the beta amylase of Shandong Anke Bioengineering Co., Ltd.'s sale.
The fungi alpha amylase that the present invention adopts is endo-amylase, can be hydrolyzed rapidly α-1 of gelatinized starch, amylose and amylopectin aqueous solution inside, 4 glucoside bonds, produce soluble dextrins and minority maltose and glucose, therefore those skilled in the art can select corresponding fungi alpha amylase according to actual needs, the fungi alpha amylase that as grand in Shandong mcroorganism Engineering Co., Ltd sells.
The Pullulanase that the present invention adopts act as selectivity and cuts α-1 in amylopectin branch point, 6 glycosidic bonds, cut whole branched structure, form amylose, therefore those skilled in the art can select corresponding Pullulanase according to actual needs, as the Pullulanase of Genencor Company's sale.
The alpha-glucosaccharase transferase that the present invention adopts act as α-1 of interrupting maltose, 4 glycosidic bonds, and by a free glucose residue with α-1, the form of 6 glycosidic bonds is connected on another glucose or maltose molecule, generate the non-fermentable carbohydrates such as isomaltose and panose, therefore those skilled in the art can select corresponding alpha-glucosaccharase transferase according to actual needs, the alpha-glucosaccharase transferase of selling as Japanese Tian Ye company.
Beneficial effect
The present invention is first in proportion by oligomeric maltose and FOS mixing granulation, prepared composite particles have good fluidity, soluble, nonhygroscopic, shelf life of products long, to advantages such as human body intestinal canal probio value-added effect are good, and production cost is low, greatly improved the added value of oligomeric maltose.
The specific embodiment:
Below in conjunction with embodiment, technical scheme of the present invention is further elaborated, but institute of the present invention protection domain is not limited to this.
Raw material sources
Aspergillus niger (Aspergillus niger) BLCY-02, within on 07 15th, 2014, be stored in China Committee for Culture Collection of Microorganisms's common micro-organisms center, preserving number CGMCC No.9449, address: No. 3, Yard 1, BeiChen xi Road, Chaoyang District, Beijing City Institute of Microorganism, Academia Sinica.
High temperature resistant AMS, Genencor Company is on sale, and enzyme is lived as 20000U/mL;
Beta amylase, Shandong Anke Bioengineering Co., Ltd. is on sale; Enzyme is lived as 100000U/g;
Fungal alpha-amylase, Shandong grand mcroorganism Engineering Co., Ltd is on sale; Enzyme is lived as 100000U/g;
Pullulanase, Genencor Company is on sale; Enzyme is lived as 1000ASPU/ml;
Alpha-glucosaccharase transferase, Japanese Tian Ye company is on sale; Enzyme is lived as 300000U/mL;
Embodiment 1
The preparation method of the composite particles of oligoisomaltose and FOS, step is as follows:
(1) by oligoisomaltose liquid glucose through concentrated, make mass concentration and be 60% oligoisomaltose liquid,
(2) FOS liquid glucose warp is concentrated, dry, make FOS powder,
(3) the FOS powder that oligoisomaltose liquid step (1) being made and step (2) make adds in fluid bed granulator granulation; under 50 ℃ of temperature conditions, granulate; cross after 40 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
The preparation method of described oligoisomaltose liquid glucose is as follows:
(I) regulating starch slurry concentration is 15 Baume degrees, after regulating pH to be 4, adds high temperature resistant AMS, and the addition of high-temperatureα-amylase is 0.6L/ ton dried starch, at 125 ℃, through secondary injection liquefaction, makes DE value and be 20% liquefier;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, the addition of beta amylase is that addition that starch material per ton adds 1.3kg, Pullulanase is that the addition that starch material per ton adds 0.12L, fungi alpha amylase is that starch material per ton adds 0.25kg, at 55 ℃, carry out saccharification react 5h, add again phlorose to turn glycosides enzyme, the addition that phlorose turns glycosides enzyme is that starch material per ton adds 0.8L, at 55 ℃, proceed to turn glycosides reaction 26h, at the 70 ℃ of enzymes that go out 5min alive, make liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, the addition of active carbon is 0.4wt%, after decolouring 2h, with adverse current ion-exchange chromatography, carries out ion-exchange desalination, makes light transmittance and be 90% desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, and chromatographic isolation service condition is operating pressure 0.25,65 ℃ of temperature, water loss-rate 1:1.3, charging 1.5m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose of isomaltose+panose in total reducing sugar+Isomaltotriose content 95wt%.
The preparation method of described FOS liquid glucose is as follows:
(i) sucrose solution that preparation mass concentration is 45%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, β-transfructosylase addition is 0.5L/ ton sucrose, and reaction 20h, makes the thick solution of FOS;
(iii) step (ii) is made to the thick solution of FOS through activated carbon decolorizing, active carbon addition is 0.1wt%, bleaching time is 1.5h, then through plate-frame filtering, then through from friendship, obtain light transmittance and be 85% liquid glucose, through operating pressure 0.2MPa, temperature 60 C, water loss-rate 1:1.2, charging 1.8m per hour 3, collect ketose, Nystose, GF4, make the FOS liquid glucose that FOS content in total reducing sugar is not less than 95wt%.
In described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 0.5 * 10 6u, 20 ℃ of reaction temperatures, the reaction time is 36h.It is CGMCC No.9449 that Aspergillus niger strain BLCY-02 is deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) preserving number, β-transfructosylase that this bacterial strain produces is ectoenzyme, after isolation technics separation, separated enzyme liquid enzyme work can reach 1000U/ml routinely.
After testing, in the composite particles of oligoisomaltose and FOS, the mass percent of oligoisomaltose is 51%, and the mass percent of FOS is 49%.
Embodiment 2
The preparation method of the composite particles of oligoisomaltose and FOS, step is as follows:
(a) by oligoisomaltose liquid glucose, through being concentrated into mass concentration, be 70%, then dry, make oligoisomaltose powder,
(b) by FOS liquid glucose through concentrated, make mass concentration and be 50% FOS liquid,
(c) the FOS liquid that oligoisomaltose powder step (a) being made and step (b) make adds in fluid bed granulator granulation in proportion; under 60 temperature conditions, granulate; cross after 60 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
The preparation method of described oligoisomaltose liquid glucose is as follows:
(I) regulating starch slurry concentration is 17 Baume degrees, after regulating pH to be 6.5, adds high temperature resistant AMS, and the addition of high-temperatureα-amylase is that starch material per ton adds 1.0L, at 130 ℃, through secondary injection liquefaction, makes DE value and be 25% liquefier;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, the addition of beta amylase is that addition that starch material per ton adds 1.25kg, Pullulanase is that the addition that starch material per ton adds 0.13L, fungi alpha amylase is that starch material per ton adds 0.15kg, at 55 ℃, carry out saccharification react 5h, add again phlorose to turn glycosides enzyme, the addition that phlorose turns glycosides enzyme is that starch material per ton adds 1.2L, at 55 ℃, proceed to turn glycosides reaction 32h, at the 80 ℃ of enzymes that go out 5min alive, make liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, the addition of active carbon is 0.4wt%, after decolouring 1.7h, with adverse current ion-exchange chromatography, carries out ion-exchange desalination, makes light transmittance and be 90% desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, and chromatographic isolation service condition is operating pressure 0.3MPa, 68 ℃ of temperature, water loss-rate 1:1.4, charging 1.7m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose of isomaltose+panose in total reducing sugar+Isomaltotriose content 96wt%.
The preparation method of described FOS liquid glucose is as follows:
(i) sucrose solution that preparation mass concentration is 60%%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, β-transfructosylase addition is 1.5L/ ton sucrose, and reaction 36h, makes the thick solution of FOS;
(iii) step (ii) is made to the thick solution of FOS through activated carbon decolorizing, active carbon addition is 0.2wt%, bleaching time is 1.5h, then through plate-frame filtering, then through from friendship, obtain light transmittance and be 87% liquid glucose, through operating pressure 0.35MPa, temperature 70 C, water loss-rate 1:1.5, charging 2.0m per hour 3, collect under ketose, Nystose, GF4 condition and carry out chromatographic isolation, make the FOS liquid glucose of FOS content 97wt% in total reducing sugar.
In described step (ii), β-transfructosylase can be with reference to < < Preparation of fructosyltransferasefrom from Aspergillus niger VVTP 84 > > (Zheng Shi Jin Yun etc., the 22nd the 1st phase of volume of the journal > > of < < Wuxi Light Industry Univ., in January, 2003) the record preparation in a literary composition.
After testing, in the composite particles of oligoisomaltose and FOS, the mass percent of oligoisomaltose is 99%, and the mass percent of FOS is 1%.
Embodiment 3
The preparation method of the composite particles of oligoisomaltose and FOS, step is as follows:
(a) by oligoisomaltose liquid glucose, through being concentrated into mass concentration, be 65%, then dry, make oligoisomaltose powder,
(b) by FOS liquid glucose through concentrated, make mass concentration and be 45% FOS liquid,
(c) the FOS liquid that oligoisomaltose powder step (a) being made and step (b) make adds in fluid bed granulator granulation in proportion; under 80 ℃ of temperature conditions, granulate; cross after 50 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
The preparation method of described oligoisomaltose liquid glucose is as follows:
(I) regulating starch slurry concentration is 20 Baume degrees, after regulating pH to be 5.5, adds high temperature resistant AMS, and the addition of high-temperatureα-amylase is that starch material per ton adds 0.8L, at 141 ℃, through secondary injection liquefaction, makes DE value and be 22% liquefier;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, the addition of beta amylase is that addition that starch material per ton adds 1.5kg, Pullulanase is that the addition that starch material per ton adds 0.13L, fungi alpha amylase is that starch material per ton adds 0.3kg, at 60 ℃, carry out saccharification react 4h, add again phlorose to turn glycosides enzyme, the addition that phlorose turns glycosides enzyme is that starch material per ton adds 0.8L, at 58 ℃, proceed to turn glycosides reaction 28h, at the 75 ℃ of enzymes that go out 10min alive, make liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, the addition of active carbon is 0.5wt%, after decolouring 2h, with adverse current ion-exchange chromatography, carries out ion-exchange desalination, makes light transmittance and be 90% desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, and chromatographic isolation service condition is operating pressure 0.35MPa, temperature 70 C, water loss-rate 1:1.4, charging 1.65m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose of isomaltose+panose in total reducing sugar+Isomaltotriose content 96wt%.
The preparation method of described FOS liquid glucose is as follows:
(i) sucrose solution that preparation mass concentration is 30%%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, β-transfructosylase addition is 1.25L/ ton sucrose, and reaction 28h, makes the thick solution of FOS;
(iii) step (ii) is made to the thick solution of FOS through activated carbon decolorizing, active carbon addition is 0.3wt%, bleaching time is 1.5h, then through plate-frame filtering, then through from friendship, obtain light transmittance and be 90% liquid glucose, condition is operating pressure 0.35MPa, 65 ℃ of temperature, water loss-rate 1:1.45, charging 1.9m per hour 3, collection ketose, Nystose, GF4 make the FOS liquid glucose of FOS content 96wt% in total reducing sugar.
In described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 1.5 * 10 6u, 40 ℃ of reaction temperatures, the reaction time is 20h.It is CGMCC No.9449 that Aspergillus niger strain BLCY-02 is deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) preserving number, β-transfructosylase that this bacterial strain produces is ectoenzyme, after isolation technics separation, separated enzyme liquid enzyme work can reach 1000U/ml routinely.
After testing, in the composite particles of oligoisomaltose and FOS, the mass percent of oligoisomaltose is 75%, and the mass percent of FOS is 25%.
Embodiment 4
The preparation method of the composite particles of oligoisomaltose and FOS, step is as follows:
(1) by oligoisomaltose liquid glucose through concentrated, make mass concentration and be 70% oligoisomaltose liquid,
(2) FOS liquid glucose warp is concentrated, dry, make FOS powder,
(3) the FOS powder that oligoisomaltose liquid step (1) being made and step (2) make adds in fluid bed granulator granulation; under 60 ℃ of temperature conditions, granulate; cross after 40 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
The preparation method of described oligoisomaltose liquid glucose is as follows:
(I) regulating starch slurry concentration is 17 Baume degrees, after regulating pH to be 5, adds high temperature resistant AMS, and the addition of high-temperatureα-amylase is that starch material per ton adds 0.8L, at 135 ℃, through secondary injection liquefaction, makes DE value and be 22% liquefier;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, the addition of beta amylase is that addition that starch material per ton adds 0.1L, Pullulanase is that the addition that starch material per ton adds 0.12L, fungi alpha amylase is that starch material per ton adds 0.1L, at 50 ℃, carry out saccharification react 5h, add again phlorose to turn glycosides enzyme, the addition that phlorose turns glycosides enzyme is that starch material per ton adds 0.6L, at 55 ℃, proceed to turn glycosides reaction 26h, at the 70 ℃ of enzymes that go out 5min alive, make liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, the addition of active carbon is 0.3wt%, after decolouring 2h, with adverse current ion-exchange chromatography, carries out ion-exchange desalination, makes light transmittance and be 85% desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, and chromatographic isolation service condition is operating pressure 0.25,65 ℃ of temperature, water loss-rate 1:1.2, charging 1.5m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose of isomaltose+panose in total reducing sugar+Isomaltotriose content 95wt%.
The preparation method of described FOS liquid glucose is as follows:
(i) sucrose solution that preparation mass concentration is 25%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, β-transfructosylase addition is 1L/ ton sucrose, and reaction 20h, makes the thick solution of FOS;
(iii) step (ii) is made to the thick solution of FOS through activated carbon decolorizing, active carbon addition is 0.1wt%, bleaching time is 1.5h, then through plate-frame filtering, then through from friendship, obtain light transmittance and be 85% liquid glucose, through operating pressure 0.2MPa, temperature 60 C, water loss-rate 1:1.3, charging 1.8m per hour 3, collect ketose, Nystose, GF4, make the FOS liquid glucose that FOS content in total reducing sugar is not less than 95wt%.
In described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 1.0 * 10 6u, 30 ℃ of reaction temperatures, the reaction time is 30h.It is CGMCC No.9449 that Aspergillus niger strain BLCY-02 is deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) preserving number, β-transfructosylase that this bacterial strain produces is ectoenzyme, after isolation technics separation, separated enzyme liquid enzyme work can reach 1000U/ml routinely.
After testing, in the composite particles of oligoisomaltose and FOS, the mass percent of oligoisomaltose is 60%, and the mass percent of FOS is 40%.
Embodiment 5
The preparation method of the composite particles of oligoisomaltose and FOS, step is as follows:
(a) by oligoisomaltose liquid glucose, through being concentrated into mass concentration, be 66%, then dry, make oligoisomaltose powder,
(b) by FOS liquid glucose through concentrated, make mass concentration and be 46% FOS liquid,
(c) the FOS liquid that oligoisomaltose powder step (a) being made and step (b) make adds in fluid bed granulator granulation in proportion; under 75 ℃ of temperature conditions, granulate; cross after 50 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
The preparation method of described oligoisomaltose liquid glucose is as follows:
(I) regulating starch slurry concentration is 19 Baume degrees, after regulating pH to be 5.5, adds high temperature resistant AMS, and the addition of high-temperatureα-amylase is that starch material per ton adds 0.9L, at 141 ℃, through secondary injection liquefaction, makes DE value and be 25% liquefier;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, the addition of beta amylase is that addition that starch material per ton adds 1.4kg, Pullulanase is that the addition that starch material per ton adds 0.13L, fungi alpha amylase is that starch material per ton adds 0.25kg, at 55 ℃, carry out saccharification react 5h, add again phlorose to turn glycosides enzyme, the addition that phlorose turns glycosides enzyme is that starch material per ton adds 1.0L, at 60 ℃, proceed to turn glycosides reaction 30h, at the 75 ℃ of enzymes that go out 10min alive, make liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, the addition of active carbon is 0.5wt%, after decolouring 2h, with adverse current ion-exchange chromatography, carries out ion-exchange desalination, makes light transmittance and be 90% desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, and chromatographic isolation service condition is operating pressure 0.35MPa, temperature 70 C, water loss-rate 1:1.4, charging 1.65m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose of isomaltose+panose in total reducing sugar+Isomaltotriose content 95wt%.
The preparation method of described FOS liquid glucose is as follows:
(i) sucrose solution that preparation mass concentration is 50%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, β-transfructosylase addition is 1.5L/ ton sucrose, and reaction 30h, makes the thick solution of FOS;
(iii) step (ii) is made to the thick solution of FOS through activated carbon decolorizing, active carbon addition is 0.2wt%, bleaching time is 1.0h, then through plate-frame filtering, then through from friendship, obtain the liquid glucose of light transmittance 90%, condition is operating pressure 0.3MPa, 65 ℃ of temperature, water loss-rate 1:1.3, charging 2.0m per hour 3, collection ketose, Nystose, GF4 make the FOS liquid glucose of FOS content 95wt% in total reducing sugar.
In described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 0.8 * 10 6u, 25 ℃ of reaction temperatures, the reaction time is 33h.It is CGMCC No.9449 that Aspergillus niger strain BLCY-02 is deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) preserving number, β-transfructosylase that this bacterial strain produces is ectoenzyme, after isolation technics separation, separated enzyme liquid enzyme work can reach 1000U/ml routinely.
After testing, in the composite particles of oligoisomaltose and FOS, the mass percent of oligoisomaltose is 80%, and the mass percent of FOS is 20%.
Test example
The product of embodiment 1-5 and oligoisomaltose Icing Sugar (isomaltose+panose in total reducing sugar+Isomaltotriose content reaches 96wt%) are contrasted, product mobility adopts angle of repose index to carry out comparative evaluation, angle of repose refers to that powder or particle packing become the hypotenuse of steepest heap and the angle between horizontal plane, mobility often represents with angle of repose, angle of repose small flow is good, otherwise contrary.
Moisture absorption (hydroscopicity) is calculated as follows:
Hydroscopicity=(sample quality-absolute dried sample quality after moisture absorption)/absolute dried sample quality
After testing, testing result is as shown in table 1:
Table 1
Human body intestinal canal probio value-added effect detects according to the method for GB < < GB4789.35-2010 food security national standard food microbiological analysis lactic acid bacteria check > > regulation and carries out bacterial classification Identification and detection, as shown in table 2 to human body intestinal canal probio value-added effect comparative test result:
Table 2

Claims (10)

1. a composite particles for oligoisomaltose and FOS, is characterized in that, component is as follows, is all weight percentage:
Oligoisomaltose 51%~99%, FOS 1%~49%.
2. composite particles as claimed in claim 1, is characterized in that, component is as follows, is all weight percentage:
Oligoisomaltose 60%~80%, FOS 20%~40%.
3. the preparation method of the composite particles of oligoisomaltose and FOS described in claim 1, is characterized in that, step is as follows:
(1) by oligoisomaltose liquid glucose through concentrated, make mass concentration and be 60~70% oligoisomaltose liquid,
(2) FOS liquid glucose warp is concentrated, dry, make FOS powder,
(3) the FOS powder that oligoisomaltose liquid step (1) being made and step (2) make adds in fluid bed granulator granulation in proportion, under 50~80 ℃ of temperature conditions, granulate, cross after 40~60 order vibratory sieves, make the composite particles of oligoisomaltose and FOS;
Or step is as follows:
(a) oligoisomaltose liquid glucose warp is concentrated, dry, make oligoisomaltose powder,
(b) by FOS liquid glucose through concentrated, make mass concentration and be 40~50% FOS liquid,
(c) the FOS liquid that oligoisomaltose powder step (a) being made and step (b) make adds in fluid bed granulator granulation in proportion; under 50~80 ℃ of temperature conditions, granulate; cross after 40~60 order vibratory sieves, make the composite particles of oligoisomaltose and FOS.
4. preparation method as claimed in claim 3, is characterized in that, described step (1) or (a) in the preparation method of oligoisomaltose liquid glucose as follows:
(I) regulating starch slurry concentration, after adjusting pH, add high temperature resistant AMS, is 20%~25% liquefier through liquefying, making DE value;
(II) in the liquefier making to step (I), add beta amylase, Pullulanase, fungi alpha amylase, carry out after saccharification react, then add phlorose to turn glycosides enzyme, proceed to turn glycosides reaction, the enzyme that then goes out is lived, and makes liquid glucose;
(III) in the liquid glucose making to step (II), add active carbon, after decolouring, with adverse current ion-exchange chromatography, carry out ion-exchange desalination, make desalination liquid glucose;
(IV) desalination liquid glucose step (III) being made is through chromatographic isolation, the eluent that collection contains isomaltose, panose and Isomaltotriose, makes the oligoisomaltose liquid glucose that isomaltose+panose in total reducing sugar+Isomaltotriose content is not less than 95wt%.
5. preparation method as claimed in claim 4, is characterized in that, in described step (I), starch slurry concentration is 15~20 Baume degrees, and pH value is 4~6.5, and the addition of high-temperatureα-amylase is that starch material per ton adds 1.2 * 10 7~2.0 * 10 7u, condensing temperature is 110~141 ℃; More excellent, described liquefaction is steam ejection liquefaction, liquefaction number of times is twice.
6. preparation method as claimed in claim 4, is characterized in that, in described step (II), the addition of described beta amylase is that starch material per ton adds 1.0 * 10 8~1.5 * 10 8the addition of U, Pullulanase is that starch material per ton adds 1.2 * 10 5~1.5 * 10 5the addition of ASPU, fungi alpha amylase is that starch material per ton adds 0.1 * 10 8~0.3 * 10 8u is saccharification react 2~5h under the condition of 50~60 ℃ in temperature; The addition that described phlorose turns glycosides enzyme is that starch material per ton adds 1.8 * 10 8~3.6 * 10 8u is under the condition of 55~60 ℃, to turn glycosides reaction 26~32h in temperature.
7. preparation method as claimed in claim 4, is characterized in that, in described step (III), the addition of active carbon is 0.3~0.5wt%, bleaching time 1.5~2.0h; Light transmittance >=85% of described desalination liquid glucose after ion-exchange desalination.
8. preparation method as claimed in claim 4, is characterized in that, in described step (IV), chromatographic isolation service condition is operating pressure 0.25~0.35MPa, 65~70 ℃ of temperature, water loss-rate 1:1.2~1:1.5, charging 1.5~1.7m per hour 3, collect the eluent that contains isomaltose, panose and Isomaltotriose, make the oligoisomaltose liquid glucose that isomaltose+panose in total reducing sugar+Isomaltotriose content is not less than 95wt%.
9. preparation method as claimed in claim 3, is characterized in that, described step (2) or (b) in the preparation method of FOS liquid glucose as follows:
(i) sucrose solution that preparation mass concentration is 25%~60%;
(ii) in the sucrose solution making to step (i), add β-transfructosylase, after reaction, make the thick solution of FOS;
(iii) step (ii) is made the thick solution of FOS through decolouring, filter, from handing over, chromatographic isolation, make the FOS liquid glucose that FOS content in total reducing sugar is not less than 95wt%.
10. preparation method as claimed in claim 9, is characterized in that, in described step (ii), β-transfructosylase originates from Aspergillus niger strain BLCY-02, and the addition of this enzyme is that sucrose per ton adds 0.5 * 10 6~1.5 * 10 6u, 20~40 ℃ of reaction temperatures, the reaction time is 20~36h;
Further preferred according to the present invention, in described step (iii), decolour for activated carbon decolorizing, active carbon addition 0.1~0.3wt%, bleaching time 1~1.5h; Be filtered into plate-frame filtering; Through solution light transmittance >=85% after friendship;
Further preferred according to the present invention, in described step (iii), chromatographic isolation service condition is operating pressure 0.2~0.35MPa, 60~70 ℃ of temperature, water loss-rate 1:(1.2~1.5), charging 1.8~2.0m per hour 3, collect ketose, Nystose, GF4.
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CN106222216A (en) * 2016-07-25 2016-12-14 山东百龙创园生物科技有限公司 A kind of novel DP4 oligomeric isomaltose and preparation method thereof
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CN112111538A (en) * 2020-09-21 2020-12-22 江南大学 Functional sugar capable of adjusting positioning release of incretins and preparation method thereof
CN112111538B (en) * 2020-09-21 2022-05-10 江南大学 Functional sugar capable of adjusting positioning release of incretins and preparation method thereof
CN114032262A (en) * 2021-11-09 2022-02-11 山东星光首创生物科技有限公司 Method for producing sucrose tetrasaccharide

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