CN104480166A - Production of fructo-oligosaccharide by virtue of amylase method - Google Patents

Production of fructo-oligosaccharide by virtue of amylase method Download PDF

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CN104480166A
CN104480166A CN201410726333.2A CN201410726333A CN104480166A CN 104480166 A CN104480166 A CN 104480166A CN 201410726333 A CN201410726333 A CN 201410726333A CN 104480166 A CN104480166 A CN 104480166A
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starch
liquid
glucose
fructo
oligosaccharide
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CN104480166B (en
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张继红
窦宝德
窦光朋
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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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Abstract

The invention relates to production of fructo-oligosaccharide by virtue of an amylase method. The production comprises the following steps: (1) pulping and liquefying: adding 6-10U/g of alpha-amylase to each ton of starch raw materials, adding CaCl2, and continuing a liquefying reaction for 10min; (2) saccharifying: leading liquefied starch to a saccharifying tank, decreasing temperature to 60 DEG C and regulating pH to 4.5, and adding 250U/g of starch saccharifying enzyme; (3) refining saccharifying liquid; and (4) preparing fructo-oligosaccharide by virtue of an enzymic method: completely dissolving 20g of sucrose to 80.0ml of a phosphate buffer, adding fructosyltransferase and glucose isomerase, adding the phosphate buffer, and reacting at 50 DEG C so as to obtain the fructo-oligosaccharide. The production of the fructo-oligosaccharide disclosed by the invention is simple to operate, mild in action condition and easy to master; the fructo-oligosaccharide is high in purity which is more than 98%; the entire process can be completed within 100-160min; the production is a great innovation in high-purity fructo-oligosaccharide, and is worthy of popularizing.

Description

A kind of starch Production by Enzymes oligofructose
(1) technical field
The present invention relates to oligofructose, be specifically related to a kind of starch Production by Enzymes oligofructose.
(2) background technology
Oligofructose refers to that 2 ~ 5 fructosyls are chain link, the end group being chain with a glucosyl group, with fructosyl → fructose connecting key for main body framework links the carbohydrate formed.Namely refer to that 1 ~ 4 fructosyl is connected to the mixture of kestose (GF2), GF3 (GF3), GF4 (GF4) and sugarcane fruit six sugar (GF5) that the D-Fructose base of sucrose is formed with β-2,1 key.Commodity oligofructose is generally also containing a small amount of sucrose, fructose, glucose.Oligofructose is a kind of natural active matter, has regulating intestinal canal flora, propagation bifidus bacillus, promote the absorption of calcium, adjusting blood lipid, immunomodulatory, the novel sweetener of the nourishing functions such as anti-dental caries, is described as the additive of new generation of most potentiality after the microbiotic epoch---growth-promoting material; Oligofructose or a kind of water miscible food fibre, can reduce serum cholesterol and content of triglyceride, takes in oligofructose and glucose level can not be caused to fluctuate, can be used as the sweeting agent of hypertension, diabetes and obesity patient.
At present, the production method of oligofructose mainly contains two kinds: 1. sucrose inversion method, this method in 1982 at Japanese industry, with the sucrose solution of ferment treatment high density, obtain the solution of oligofructose contents on dry basis 55%, all the other 45% be fructose, glucose sugar and sucrose, obtain through separation and purification the oligofructose that purity is 95%.This method due to separating-purifying difficulty large, Chinese Enterprise can only produce the oligofructose product of 55% substantially.2. synanthrin hydrolysis method, this method is adopted in a large number by Europe at present.This method extracts synanthrin from witloof, be hydrolyzed through synanthrin restriction endonuclease, obtain the mixture of oligofructose, glucose, sucrose, oligofructose is obtained through separating-purifying, but because in enzymolysis product, the contents on dry basis of oligofructose also only has 55%, monose and sucrose content are too high, separation difficulty, can't produce the product that oligofructose content is greater than 95%.
There is same deficiency in above two kinds of technology, namely producing enzyme used only has few unit to produce, and as the then more difficult preparation of pure enzyme, use enzyme-squash techniqued oligofructose, cost is high, enzymolysis product be difficult to control, monose and sucrose content high, separating-purifying difficulty is large.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of starch Production by Enzymes oligofructose, easy to operate, and process is easy to control, and facilitate large-scale industrial to produce, oligofructose purity is high, can reach more than 98%.
The present invention is achieved through the following technical solutions:
A kind of starch Production by Enzymes oligofructose, its special character is: comprise the following steps:
(1) size mixing and liquefaction: starch water is modulated into the starch milk of dry matter content 30%-35%, adjusts pH6.0-6.5 with hydrochloric acid, starch material per ton adds ɑ-amylase consumption 6-10U/g starch, adds CaCl 2regulate Ca 2+concentration reaches 0.01mol/l, and powder stock pump enters Jet liquefier, is instantaneously warming up to 105-110 DEG C, pipeline liquefaction reaction 10-15min, feed liquid is delivered to liquefied pot, at 95-97 DEG C of temperature, add ɑ-amylase at twice, continue liquefaction reaction 10min, iodine colour response is qualified;
(2) saccharification: liquefied starch introduces saccharifying tank, is cooled to 60 DEG C of adjustment pH to 4.5, adds 250U/g diastatic enzyme, under gap is stirred, 60 DEG C of insulation 30min, saccharification is to DE > 95, heat to 90 DEG C, saccharifying enzyme is destroyed, saccharification react is stopped;
(3) saccharified liquid is refined: adopt the continuous filtration of diatomite precoating rotary drum filter, remove impurity and the jelly of non-solubility in saccharified liquid, use activated carbon decolorizing subsequently, the inorganic salt in spent ion exchange resin removing liquid glucose and organic impurity, improve purity further, colourless or the faint yellow sugar-containing concentration 24% of liquid glucose, specific conductivity < 50MS/cm, pH4.5-5.0, vacuum evaporation is to transmittance more than 90%, DE value 96-97, sugar concentration is 40%-45%;
(4) enzyme process prepares oligofructose: first by 20 grams of sucrose, be dissolved in 80.0ml phosphate buffered saline buffer completely, then fructosyl transferase and glucose isomerase is added, fructosyl transferase and glucose isomerase liquid glucose: the weight ratio of liquid glucose is 1:7, and wherein the enzyme activity ratio of fructosyl transferase and glucose isomerase is 2:1, be added in liquid glucose, reaction 5min, then add phosphate buffered saline buffer, liquid glucose: the volume ratio 100:1 of phosphate buffered saline buffer, in phosphate buffered saline buffer, KH 2pO 4with K 2hPO 4volume ratio is 2:1, and wherein both concentration is 0.05mol/L; Add incitant MgSO 47H 2o, ZnSO 4, Na 2seO 3as incitant, every glycemic liquid 4gMgSO 47H 2o, 1g ZnSO 4, 4g Na 2seO 3, in 50 °, reaction 20min, after 2min is boiled in sampling, is cooled to rapidly less than 40 DEG C, in the centrifugal 5min of 10000r/min, obtains oligofructose.
Beneficial effect of the present invention: the present invention is simple to operate for the production of oligofructose, action condition is gentle, easily grasp, oligofructose purity is high, can reach more than 98%, and whole process 100-160min can complete, be innovation great on high-purity fructo oligosaccharides, be worthy to be popularized.
(4) embodiment
Embodiment 1
The starch Production by Enzymes oligofructose of the present embodiment the steps include:
(1) size mixing and liquefaction: starch water is modulated into the starch milk of dry matter content 30%, adjusts pH6.0 with hydrochloric acid, starch material per ton adds ɑ-amylase consumption 6U/g starch, adds CaCl 2regulate Ca 2+concentration reaches 0.01mol/l, and powder stock pump enters Jet liquefier, is instantaneously warming up to 105 DEG C, pipeline liquefaction reaction 10min, and feed liquid is delivered to liquefied pot, at 95 DEG C of temperature, adds ɑ-amylase at twice, and continue liquefaction reaction 10min, iodine colour response is qualified;
(2) saccharification: liquefied starch introduces saccharifying tank, is cooled to 60 DEG C of adjustment pH to 4.5, adds 250U/g diastatic enzyme, under gap is stirred, 60 DEG C of insulation 30min, saccharification is to DE > 95, heat to 90 DEG C, saccharifying enzyme is destroyed, saccharification react is stopped;
(3) saccharified liquid is refined: adopt the continuous filtration of diatomite precoating rotary drum filter, remove impurity and the jelly of non-solubility in saccharified liquid, use activated carbon decolorizing subsequently, the inorganic salt in spent ion exchange resin removing liquid glucose and organic impurity, improve purity further, colourless or the faint yellow sugar-containing concentration 24% of liquid glucose, specific conductivity < 50MS/cm, pH4.5-5.0, vacuum evaporation is to transmittance more than 90%, DE value 96, sugar concentration is 40%%;
(4) enzyme process prepares oligofructose: first by 20 grams of sucrose, be dissolved in 80.0ml phosphate buffered saline buffer completely, then fructosyl transferase and glucose isomerase is added, fructosyl transferase and glucose isomerase liquid glucose: the weight ratio of liquid glucose is 1:7, and wherein the enzyme activity ratio of fructosyl transferase and glucose isomerase is 2:1, be added in liquid glucose, reaction 5min, then add phosphate buffered saline buffer, liquid glucose: the volume ratio 100:1 of phosphate buffered saline buffer, in phosphate buffered saline buffer, KH 2pO 4with K 2hPO 4volume ratio is 2:1, and wherein both concentration is 0.05mol/L; Add incitant MgSO 47H 2o, ZnSO 4, Na 2seO 3as incitant, every glycemic liquid 4gMgSO 47H 2o, 1g ZnSO 4, 4g Na 2seO 3, in 50 °, reaction 20min, after 2min is boiled in sampling, is cooled to rapidly less than 40 DEG C, in the centrifugal 5min of 10000r/min, obtains oligofructose.
Embodiment 2
The starch Production by Enzymes oligofructose of the present embodiment the steps include:
(1) size mixing and liquefaction: starch water is modulated into the starch milk of dry matter content 35%, adjusts pH6.5 with hydrochloric acid, starch material per ton adds ɑ-amylase consumption 10U/g starch, adds CaCl 2regulate Ca 2+concentration reaches 0.01mol/l, and powder stock pump enters Jet liquefier, is instantaneously warming up to 110 DEG C, pipeline liquefaction reaction 15min, and feed liquid is delivered to liquefied pot, at 97 DEG C of temperature, adds ɑ-amylase at twice, and continue liquefaction reaction 10min, iodine colour response is qualified;
(2) saccharification: liquefied starch introduces saccharifying tank, is cooled to 60 DEG C of adjustment pH to 4.5, adds 250U/g diastatic enzyme, under gap is stirred, 60 DEG C of insulation 30min, saccharification is to DE > 95, heat to 90 DEG C, saccharifying enzyme is destroyed, saccharification react is stopped;
(3) saccharified liquid is refined: adopt the continuous filtration of diatomite precoating rotary drum filter, remove impurity and the jelly of non-solubility in saccharified liquid, use activated carbon decolorizing subsequently, the inorganic salt in spent ion exchange resin removing liquid glucose and organic impurity, improve purity further, colourless or the faint yellow sugar-containing concentration 24% of liquid glucose, specific conductivity < 50MS/cm, pH4.5-5.0, vacuum evaporation is to transmittance more than 90%, DE value 96-97, sugar concentration is 40%-45%;
(4) enzyme process prepares oligofructose: first by 20 grams of sucrose, be dissolved in 80.0ml phosphate buffered saline buffer completely, then fructosyl transferase and glucose isomerase is added, fructosyl transferase and glucose isomerase liquid glucose: the weight ratio of liquid glucose is 1:7, and wherein the enzyme activity ratio of fructosyl transferase and glucose isomerase is 2:1, be added in liquid glucose, reaction 5min, then add phosphate buffered saline buffer, liquid glucose: the volume ratio 100:1 of phosphate buffered saline buffer, in phosphate buffered saline buffer, KH 2pO 4with K 2hPO 4volume ratio is 2:1, and wherein both concentration is 0.05mol/L; Add incitant MgSO 47H 2o, ZnSO 4, Na 2seO 3as incitant, every glycemic liquid 4gMgSO 47H 2o, 1g ZnSO 4, 4g Na 2seO 3, in 50 °, reaction 20min, after 2min is boiled in sampling, is cooled to rapidly less than 40 DEG C, in the centrifugal 5min of 10000r/min, obtains oligofructose.
Embodiment 3
The starch Production by Enzymes oligofructose of the present embodiment the steps include:
(1) size mixing and liquefaction: starch water is modulated into the starch milk of dry matter content 33%, adjusts pH6.0-6.5 with hydrochloric acid, starch material per ton adds ɑ-amylase consumption 8U/g starch, adds CaCl 2regulate Ca 2+concentration reaches 0.01mol/l, and powder stock pump enters Jet liquefier, is instantaneously warming up to 105-110 DEG C, pipeline liquefaction reaction 13min, feed liquid is delivered to liquefied pot, at 95-97 DEG C of temperature, add ɑ-amylase at twice, continue liquefaction reaction 10min, iodine colour response is qualified;
(2) saccharification: liquefied starch introduces saccharifying tank, is cooled to 60 DEG C of adjustment pH to 4.5, adds 250U/g diastatic enzyme, under gap is stirred, 60 DEG C of insulation 30min, saccharification is to DE > 95, heat to 90 DEG C, saccharifying enzyme is destroyed, saccharification react is stopped;
(3) saccharified liquid is refined: adopt the continuous filtration of diatomite precoating rotary drum filter, remove impurity and the jelly of non-solubility in saccharified liquid, use activated carbon decolorizing subsequently, the inorganic salt in spent ion exchange resin removing liquid glucose and organic impurity, improve purity further, colourless or the faint yellow sugar-containing concentration 24% of liquid glucose, specific conductivity < 50MS/cm, pH4.5-5.0, vacuum evaporation is to transmittance more than 90%, DE value 96-97, sugar concentration is 40%-45%;
(4) enzyme process prepares oligofructose: first by 20 grams of sucrose, be dissolved in 80.0ml phosphate buffered saline buffer completely, then fructosyl transferase and glucose isomerase is added, fructosyl transferase and glucose isomerase liquid glucose: the weight ratio of liquid glucose is 1:7, and wherein the enzyme activity ratio of fructosyl transferase and glucose isomerase is 2:1, be added in liquid glucose, reaction 5min, then add phosphate buffered saline buffer, liquid glucose: the volume ratio 100:1 of phosphate buffered saline buffer, in phosphate buffered saline buffer, KH 2pO 4with K 2hPO 4volume ratio is 2:1, and wherein both concentration is 0.05mol/L; Add incitant MgSO 47H 2o, ZnSO 4, Na 2seO 3as incitant, every glycemic liquid 4gMgSO 47H 2o, 1g ZnSO 4, 4g Na 2seO 3, in 50 °, reaction 20min, after 2min is boiled in sampling, is cooled to rapidly less than 40 DEG C, in the centrifugal 5min of 10000r/min, obtains oligofructose.

Claims (1)

1. a starch Production by Enzymes oligofructose, is characterized in that: comprise the following steps:
(1) size mixing and liquefaction: starch water is modulated into the starch milk of dry matter content 30%-35%, adjusts pH6.0-6.5 with hydrochloric acid, starch material per ton adds ɑ-amylase consumption 6-10U/g starch, adds CaCl 2regulate Ca 2+concentration reaches 0.01mol/l, and powder stock pump enters Jet liquefier, is instantaneously warming up to 105-110 DEG C, pipeline liquefaction reaction 10-15min, feed liquid is delivered to liquefied pot, at 95-97 DEG C of temperature, add ɑ-amylase at twice, continue liquefaction reaction 10min, iodine colour response is qualified;
(2) saccharification: liquefied starch introduces saccharifying tank, is cooled to 60 DEG C of adjustment pH to 4.5, adds 250U/g diastatic enzyme, under gap is stirred, 60 DEG C of insulation 30min, saccharification is to DE > 95, heat to 90 DEG C, saccharifying enzyme is destroyed, saccharification react is stopped;
(3) saccharified liquid is refined: adopt the continuous filtration of diatomite precoating rotary drum filter, remove impurity and the jelly of non-solubility in saccharified liquid, use activated carbon decolorizing subsequently, the inorganic salt in spent ion exchange resin removing liquid glucose and organic impurity, improve purity further, colourless or the faint yellow sugar-containing concentration 24% of liquid glucose, specific conductivity < 50MS/cm, pH4.5-5.0, vacuum evaporation is to transmittance more than 90%, DE value 96-97, sugar concentration is 40%-45%;
(4) enzyme process prepares oligofructose: first by 20 grams of sucrose, be dissolved in 80.0ml phosphate buffered saline buffer completely, then fructosyl transferase and glucose isomerase is added, fructosyl transferase and glucose isomerase liquid glucose: the weight ratio of liquid glucose is 1:7, and wherein the enzyme activity ratio of fructosyl transferase and glucose isomerase is 2:1, be added in liquid glucose, reaction 5min, then add phosphate buffered saline buffer, liquid glucose: the volume ratio 100:1 of phosphate buffered saline buffer, in phosphate buffered saline buffer, KH 2pO 4with K 2hPO 4volume ratio is 2:1, and wherein both concentration is 0.05mol/L; Add incitant MgSO 47H 2o, ZnSO 4, Na 2seO 3as incitant, every glycemic liquid 4gMgSO 47H 2o, 1g ZnSO 4, 4g Na 2seO 3, in 50 °, reaction 20min, after 2min is boiled in sampling, is cooled to rapidly less than 40 DEG C, in the centrifugal 5min of 10000r/min, obtains oligofructose.
CN201410726333.2A 2014-12-04 2014-12-04 A kind of starch Production by Enzymes FOS Active CN104480166B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105106043A (en) * 2015-07-16 2015-12-02 山东省分析测试中心 Peony flower-containing anti-inflammation and deodorization fragrant mouthwash and preparation method thereof
CN110106215A (en) * 2019-05-10 2019-08-09 武汉友谊兴泰科技有限公司 Saccharification, filtering technique and its equipment in a kind of fructose production process
CN115109810A (en) * 2022-07-22 2022-09-27 金建国 Fructo-oligosaccharide and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105106043A (en) * 2015-07-16 2015-12-02 山东省分析测试中心 Peony flower-containing anti-inflammation and deodorization fragrant mouthwash and preparation method thereof
CN105106043B (en) * 2015-07-16 2017-10-20 山东省分析测试中心 Fragrant mouthwash of a kind of peony anti-inflammatory deodorization and preparation method thereof
CN110106215A (en) * 2019-05-10 2019-08-09 武汉友谊兴泰科技有限公司 Saccharification, filtering technique and its equipment in a kind of fructose production process
CN115109810A (en) * 2022-07-22 2022-09-27 金建国 Fructo-oligosaccharide and preparation method thereof

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