CN112301076A - Method for preparing maltotriose by using starch as raw material - Google Patents
Method for preparing maltotriose by using starch as raw material Download PDFInfo
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- CN112301076A CN112301076A CN202011049181.9A CN202011049181A CN112301076A CN 112301076 A CN112301076 A CN 112301076A CN 202011049181 A CN202011049181 A CN 202011049181A CN 112301076 A CN112301076 A CN 112301076A
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- FYGDTMLNYKFZSV-BYLHFPJWSA-N β-1,4-galactotrioside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@H](CO)O[C@@H](O[C@@H]2[C@@H](O[C@@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-BYLHFPJWSA-N 0.000 title claims abstract description 72
- DBTMGCOVALSLOR-UHFFFAOYSA-N 32-alpha-galactosyl-3-alpha-galactosyl-galactose Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(OC2C(C(CO)OC(O)C2O)O)OC(CO)C1O DBTMGCOVALSLOR-UHFFFAOYSA-N 0.000 title claims abstract description 71
- RXVWSYJTUUKTEA-UHFFFAOYSA-N D-maltotriose Natural products OC1C(O)C(OC(C(O)CO)C(O)C(O)C=O)OC(CO)C1OC1C(O)C(O)C(O)C(CO)O1 RXVWSYJTUUKTEA-UHFFFAOYSA-N 0.000 title claims abstract description 71
- FYGDTMLNYKFZSV-UHFFFAOYSA-N mannotriose Natural products OC1C(O)C(O)C(CO)OC1OC1C(CO)OC(OC2C(OC(O)C(O)C2O)CO)C(O)C1O FYGDTMLNYKFZSV-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229920002472 Starch Polymers 0.000 title claims abstract description 48
- 235000019698 starch Nutrition 0.000 title claims abstract description 45
- 239000008107 starch Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002994 raw material Substances 0.000 title claims abstract description 18
- 108090000637 alpha-Amylases Proteins 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 102000004139 alpha-Amylases Human genes 0.000 claims abstract description 22
- 229940024171 alpha-amylase Drugs 0.000 claims abstract description 22
- 230000002538 fungal effect Effects 0.000 claims abstract description 20
- 238000013375 chromatographic separation Methods 0.000 claims abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000013336 milk Nutrition 0.000 claims abstract description 12
- 239000008267 milk Substances 0.000 claims abstract description 12
- 210000004080 milk Anatomy 0.000 claims abstract description 12
- 238000005342 ion exchange Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000006188 syrup Substances 0.000 claims description 15
- 235000020357 syrup Nutrition 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000004042 decolorization Methods 0.000 claims description 8
- 239000011552 falling film Substances 0.000 claims description 6
- 229920001592 potato starch Polymers 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 4
- 229920002261 Corn starch Polymers 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- 229940100445 wheat starch Drugs 0.000 claims description 3
- 244000017020 Ipomoea batatas Species 0.000 claims description 2
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 2
- 240000003183 Manihot esculenta Species 0.000 claims description 2
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 2
- 229940100486 rice starch Drugs 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 28
- 102000004190 Enzymes Human genes 0.000 abstract description 11
- 108090000790 Enzymes Proteins 0.000 abstract description 11
- 229940088598 enzyme Drugs 0.000 abstract description 11
- 230000009849 deactivation Effects 0.000 abstract description 3
- 229940079919 digestives enzyme preparation Drugs 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000002253 acid Substances 0.000 description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 8
- 239000003729 cation exchange resin Substances 0.000 description 8
- 150000001450 anions Chemical class 0.000 description 5
- 238000010612 desalination reaction Methods 0.000 description 5
- 239000003957 anion exchange resin Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229920001218 Pullulan Polymers 0.000 description 3
- 239000004373 Pullulan Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 235000019423 pullulan Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004382 Amylase Substances 0.000 description 2
- 102000013142 Amylases Human genes 0.000 description 2
- 108010065511 Amylases Proteins 0.000 description 2
- 235000019418 amylase Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 108060002716 Exonuclease Proteins 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- FYGDTMLNYKFZSV-DZOUCCHMSA-N alpha-D-Glcp-(1->4)-alpha-D-Glcp-(1->4)-D-Glcp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)O[C@H](O[C@@H]2[C@H](OC(O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-DZOUCCHMSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 102000013165 exonuclease Human genes 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229960004793 sucrose Drugs 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- -1 therefore Polymers 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/16—Preparation of compounds containing saccharide radicals produced by the action of an alpha-1, 6-glucosidase, e.g. amylose, debranched amylopectin
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
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- General Chemical & Material Sciences (AREA)
- Molecular Biology (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a method for preparing maltotriose by using starch as a raw material, which comprises the steps of preparing starch milk with the mass concentration of 3-5%, heating to 80-85 ℃, preserving heat for 5-20 minutes, cooling to 45-55 ℃, adjusting the pH value to 4.5-5.5 by using hydrochloric acid, adding fungal alpha-amylase to react for 1-3 hours, then adding pullulanase, continuing to react for 10-20 hours to obtain saccharified liquid, and obtaining a maltotriose product through vacuum concentration, activated carbon decoloration and filtration, ion exchange and chromatographic separation. The invention takes starch as raw material, adopts pullulanase to cooperate with fungal alpha-amylase to directly carry out liquefaction and saccharification on the starch emulsion, omits the previous high-temperature high-pressure enzyme deactivation process, and has the advantages that the pullulanase and the fungal alpha-amylase are both enzyme preparations which are easily obtained in the market, the reaction time is shortened, the operation method is simple, the cost is low, and the industrial production is easy.
Description
Technical Field
The invention belongs to the technical field of preparation of maltotriose, and particularly relates to a method for preparing maltotriose by taking starch as a raw material.
Background
Maltotriose is an important maltooligosaccharide, is formed by connecting three glucose units through alpha-1, 4-glycosidic bonds, has moderate sweet taste, high viscosity, low osmotic pressure, easy digestion and absorption, has energy slow release property, and can avoid the health problem caused by rapid rise of energy; the heat resistance and the acid resistance of the maltotriose are better than those of cane sugar and glucose, the maltotriose is stable under acidic and high-temperature conditions, Maillard reaction is not easy to occur, the color protection effect is achieved, meanwhile, the maltotriose is added into cakes, starch food can be prevented from aging, the food can be kept soft for a long time, and the maltotriose is an ideal health food raw material.
At present, the preparation methods of maltotriose are mainly divided into two types: one method is to use poly-maltotriose and pullulan as raw materials, decompose them with pullulanase to obtain maltotriose, or perform acetylhydrolysis reaction on pullulan by a chemical method to obtain fully acetylated maltotriose, and remove acetyl to obtain the target product maltotriose (such as Chinese patent CN 105713051A), but the production cost is higher by using pullulan as a raw material, and the cost for preparing maltotriose by using the method is higher. Another method is to use starch as raw material, liquefy starch milk with alpha-amylase first and then decompose with maltotriose amylase to obtain, for example, chinese patent CN1032153265A discloses a preparation method of high-purity maltotriose, first, liquefy starch liquid is saccharified with maltotriose amylase and pullulanase to generate maltotriose, only one-step saccharification reaction takes more than 30 hours, maltotriose enzyme is an exonuclease, hydrolysis of starch is blocked by alpha-1, 6-glycosidic bond in starch, therefore, starch debranching enzyme such as pullulanase is also needed to eliminate alpha-1, 6-glycosidic bond in starch, and the current market has less special enzyme for maltotriose, and the production cost is high; secondly, the alpha-amylase liquid used in the starch liquefaction process is high temperature resistant, and enzyme deactivation treatment needs to be carried out at high temperature and high pressure after liquefaction. Thus, the method is complicated to operate, time consuming and costly.
Chinese patent CN 103014097B discloses a preparation method of maltotriose by using starch as a raw material and a special fungal alpha-amylase (CCTCC NO: M2012440) thereof, various plant starches are used as raw materials, and the special fungal alpha-amylase Sfa is used for liquefaction and saccharification to obtain syrup with the maltotriose accounting for 46-55% of the total sugar proportion, but the fungal alpha-amylase Sfa is a special enzyme preparation and is not easy to obtain, and when a common fungal alpha-amylase is used, the content of the maltotriose in the prepared saccharification liquid is extremely low, so that the use requirement cannot be met.
In conclusion, the method which is low in cost, simple to operate and capable of obtaining high-purity maltotriose is significant.
Disclosure of Invention
Aiming at the problems of high cost and complex preparation process of a maltotriose raw material or an enzyme preparation in the prior art, the invention provides a method for preparing maltotriose by using starch as a raw material, the pullulanase assists the fungal alpha-amylase to act synergistically, the raw material and the enzyme preparation are simple and easy to obtain, and the cost is greatly reduced.
The invention is realized by the following technical scheme:
a method for preparing maltotriose by taking starch as a raw material specifically comprises the following steps: preparing 3-5% starch milk, heating to 80-85 ℃, preserving heat for 5-20 minutes, cooling to 45-55 ℃, adjusting the pH value to 4.5-5.5 by using hydrochloric acid, adding fungal alpha-amylase to react for 1-3 hours, then adding pullulanase, continuing to react for 10-20 hours to obtain a saccharified solution, and obtaining a maltotriose product through vacuum concentration, activated carbon decoloration and filtration, ion exchange and chromatographic separation.
Further, the starch is more than one of corn starch, wheat starch, cassava starch, rice starch, potato starch and sweet potato starch; the mass percentage concentration of the hydrochloric acid is 4%.
Furthermore, the mass percentage of the maltotriose in the maltotriose product is 70-80%.
Further, the addition amount of the fungal alpha-amylase is 2-6U/g of starch dry powder; the addition amount of the pullulanase is 0.4-0.8U/g starch dry powder.
Further, the operating pressure of the vacuum concentration is 0.1-0.5MPa, and the temperature is 70 ℃.
Furthermore, the adding amount of the active carbon in the active carbon decolorization filtration is 1 percent of the dry mass of the maltotriose, the temperature is 65-75 ℃, and the decolorization time is 30 minutes.
Further, the temperature of the ion exchange is 40-60 ℃ and the ion exchange is sequentially performed through an anode column, an anion column and an anode column, and the flow rate is 3 times of the column volume per hour.
Further, the chromatographic separation conditions comprise that the operating pressure is 0.1-0.5MPa and the temperature is 55-70 ℃;
further, the syrup subjected to chromatography is subjected to vacuum degree of 0.1-0.5MPa and temperature of 60-80 ℃ by adopting a four-effect falling film evaporator.
Advantageous effects
1. The starch is used as a raw material, the pullulanase and the fungal alpha-amylase are used for directly liquefying and saccharifying the starch emulsion, the conventional high-temperature and high-pressure enzyme deactivation process is omitted, and both the pullulanase and the fungal alpha-amylase are enzyme preparations which are easily obtained in the market, so that the cost is greatly reduced;
2. the method adopts starch as a raw material, and the fungal alpha-amylase and the pullulanase are used for preparing the maltotriose in a synergistic manner, so that the reaction time is shortened, the operation method is simple, and the industrial production is easy.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The fungal alpha-amylase used in the embodiment of the invention is commercially purchased from Shandong Longong great bioengineering Co., Ltd, and the enzyme activity is 20000U/ml; the pullulanase is commercially available from Shandong Longong bioengineering Co., Ltd, and the enzyme activity is 2000U/ml.
Example 1
1. Preparing potato starch milk (prepared by directly adding water) with mass concentration of 3%, and keeping the temperature at 85 deg.C for 10 min;
2. cooling the heat-preserved starch milk to 48 ℃, adjusting the pH to 4.5 by using hydrochloric acid with the mass fraction of 4%, adding fungal alpha-amylase 6U/g starch, reacting for 2 hours, adding pullulanase 0.8U/g starch, and continuing to react for 18 hours to obtain a saccharification liquid with the maltotriose accounting for 45% of the total sugar concentration;
3. vacuum concentrating the obtained saccharified liquid at the operating pressure of 0.3MPa and the temperature of 70 ℃ to obtain liquid maltotriose with the solid content of 44 percent by mass;
4. adding 1% (mass ratio of powdered activated carbon to maltotriose dry basis) of powdered activated carbon into the concentrated maltotriose saccharification liquid, uniformly stirring, keeping the temperature at 68 ℃ for 30min for decolorization, and then filtering by adopting a plate-and-frame filter press;
5. passing the decolorized and filtered maltotriose syrup through an anode column (D001 macroporous strong acid cation exchange resin) -an anion column (D301 macroporous adsorption anion exchange resin) -an anode column (D001 macroporous strong acid cation exchange resin) in sequence at 50 ℃ at the flow rate of 3 times of the column volume per hour for ion exchange desalination;
6. and (3) chromatographic separation: carrying out chromatographic separation on the exchanged and desalted maltotriose syrup, wherein the operating pressure is 0.3-0.4 MPa, the temperature is 60 ℃, and the mass percentage of maltotriose in the liquid after chromatographic separation is 72%;
7. concentrating the chromatographed syrup by adopting a four-effect falling film evaporator at the vacuum degree of 0.35MPa and the temperature of 70 ℃ until the concentration of the feed liquid is 78 percent, thus obtaining the maltotriose product.
Example 2
1. Preparing corn starch milk with the mass concentration of 4%, and preserving heat for 15min at 80 ℃;
2. cooling the heat-preserved starch milk to 50 ℃, adjusting the pH to 4.9 by using hydrochloric acid with the mass fraction of 4%, adding fungal alpha-amylase 6U/g starch, reacting for 1h, adding pullulanase 0.8U/g starch, and continuing to react for 12h to obtain a saccharification liquid with the maltotriose accounting for 43% of the total sugar concentration;
3. vacuum concentrating the obtained saccharified liquid at the operating pressure of 0.4MPa and the temperature of 70 ℃ to obtain liquid maltotriose with the solid content of 44 percent by mass;
4. adding 1% (mass ratio of powdered activated carbon to maltotriose dry basis) of powdered activated carbon into the concentrated maltotriose saccharification liquid, uniformly stirring, keeping the temperature at 68 ℃ for 30min for decolorization, and then filtering by adopting a plate-and-frame filter press;
5. passing the decolorized and filtered maltotriose syrup through an anode column (D001 macroporous strong acid cation exchange resin) -an anion column (D301 macroporous adsorption anion exchange resin) -an anode column (D001 macroporous strong acid cation exchange resin) in sequence at 50 ℃ at the flow rate of 3 times of the column volume per hour for ion exchange desalination;
6. and (3) chromatographic separation: carrying out chromatographic separation on the exchanged and desalted maltotriose syrup, wherein the operating pressure is 0.3-0.4 MPa, the temperature is 60 ℃, and the mass percentage of maltotriose in the liquid after chromatographic separation is 71%;
7. concentrating the chromatographed syrup by adopting a four-effect falling film evaporator at the vacuum degree of 0.3MPa and the temperature of 70 ℃ until the concentration of the feed liquid is 75 percent, thus obtaining the maltotriose product.
Example 3
1. Preparing 3% wheat starch milk (prepared by directly adding water), and keeping the temperature at 85 deg.C for 10 min;
2. cooling the heat-preserved starch milk to 45 ℃, adjusting the pH to 5.2 by using hydrochloric acid with the mass fraction of 4%, adding fungal alpha-amylase 6U/g starch, reacting for 2 hours, adding pullulanase 0.6U/g starch, and continuing to react for 18 hours to obtain a saccharification liquid with the maltotriose accounting for 42% of the total sugar concentration;
3. vacuum concentrating the obtained saccharified liquid at the operating pressure of 0.3MPa and the temperature of 70 ℃ to obtain liquid maltotriose with the solid content of 41 percent by mass;
4. adding 1% (mass ratio of powdered activated carbon to maltotriose dry basis) of powdered activated carbon into the concentrated maltotriose saccharification liquid, uniformly stirring, keeping the temperature at 68 ℃ for 30min for decolorization, and then filtering by adopting a plate-and-frame filter press;
5. passing the decolorized and filtered maltotriose syrup through an anode column (D001 macroporous strong acid cation exchange resin) -an anion column (D301 macroporous adsorption anion exchange resin) -an anode column (D001 macroporous strong acid cation exchange resin) in sequence at 50 ℃ at the flow rate of 3 times of the column volume per hour for ion exchange desalination;
6. and (3) chromatographic separation: carrying out chromatographic separation on the exchanged and desalted maltotriose syrup, wherein the operating pressure is 0.5MPa, the temperature is 55 ℃, and the mass percentage of the maltotriose in the liquid after the chromatographic separation is 71%;
7. concentrating the chromatographed syrup by adopting a four-effect falling film evaporator at the vacuum degree of 0.35MPa and the temperature of 70 ℃ until the concentration of the feed liquid is 75 percent, thus obtaining the maltotriose product.
Comparative example 1
1. Preparing potato starch milk (prepared by directly adding water) with mass concentration of 3%, and keeping the temperature at 85 deg.C for 10 min;
2. cooling the heat-preserved starch milk to 48 ℃, adjusting the pH to 4.5, adding 6U/g starch of fungal alpha-amylase, and reacting for 20 hours to obtain a saccharification liquid with maltotriose accounting for 26% of the total sugar concentration;
3. vacuum concentrating the obtained saccharified liquid at the operating pressure of 0.3MPa and the temperature of 70 ℃ to obtain liquid maltotriose with the solid content of 25 percent by mass;
4. adding 1% (mass ratio of powdered activated carbon to maltotriose dry basis) of powdered activated carbon into the concentrated maltotriose saccharification liquid, uniformly stirring, keeping the temperature at 68 ℃ for 30min for decolorization, and then filtering by adopting a plate-and-frame filter press;
5. passing the decolorized and filtered maltotriose syrup through an anode column (D001 macroporous strong acid cation exchange resin) -an anion column (D301 macroporous adsorption anion exchange resin) -an anode column (D001 macroporous strong acid cation exchange resin) in sequence at 50 ℃ at the flow rate of 3 times of the column volume per hour for ion exchange desalination;
6. and (3) chromatographic separation: carrying out chromatographic separation on the maltotriose syrup subjected to the ion exchange and desalination, wherein the operating pressure is 0.4MPa, the temperature is 60 ℃, and the mass percentage of the maltotriose in the liquid subjected to the chromatographic separation is 45%;
7. concentrating the chromatographed syrup by adopting a four-effect falling film evaporator at the vacuum degree of 0.35MPa and the temperature of 70 ℃ until the concentration of the feed liquid is 71 percent, thus obtaining the maltotriose product.
Claims (9)
1. A method for preparing maltotriose by taking starch as a raw material is characterized by comprising the following steps: preparing 3-5% starch milk, heating to 80-85 ℃, preserving heat for 5-20 minutes, cooling to 45-55 ℃, adjusting the pH value to 4.5-5.5 by using hydrochloric acid, adding fungal alpha-amylase to react for 1-3 hours, then adding pullulanase, continuing to react for 10-20 hours to obtain a saccharified solution, and obtaining a maltotriose product through vacuum concentration, activated carbon decoloration and filtration, ion exchange and chromatographic separation.
2. The method of claim 1, wherein the starch is one or more of corn starch, wheat starch, tapioca starch, rice starch, potato starch and sweet potato starch; the mass percentage concentration of the hydrochloric acid is 4%.
3. The method of claim 1, wherein the maltotriose product contains maltotriose in an amount of 70 to 80% by mass.
4. The method according to claim 1, wherein the fungal alpha-amylase is added in an amount of 2-6U/g dry starch powder; the addition amount of the pullulanase is 0.4-0.8U/g starch dry powder.
5. The method of claim 1, wherein the vacuum concentration is performed at a pressure of 0.1 to 0.5MPa and a temperature of 70 ℃.
6. The process according to claim 1, wherein the amount of activated carbon added in the decolorization filtration with activated carbon is 1% by weight of maltotriose on a dry basis, the temperature is 65 to 75 ℃, and the time for decolorization is 30 minutes.
7. The method of claim 1, wherein the ion exchange is performed at a temperature of 40 to 60 ℃ and at a flow rate of 3 column volumes per hour sequentially through the positive column, the negative column and the positive column.
8. The method according to claim 1, wherein the chromatographic separation conditions are an operating pressure of 0.1 to 0.5MPa and a temperature of 55 to 70 ℃.
9. The preparation method according to claim 1, wherein the chromatographed syrup is prepared by adopting a four-effect falling film evaporator under the conditions that the vacuum degree is 0.1-0.5MPa and the temperature is 60-80 ℃.
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| WO2014099415A1 (en) * | 2012-12-20 | 2014-06-26 | Danisco Us Inc. | Method of using alpha-amylase from aspergillus terreus and pullulanase for saccharification |
| US20140227744A1 (en) * | 2013-02-12 | 2014-08-14 | Nasir Ahmed | Single step liquefaction and saccharification of corn starch using an acidophilic, calcium independent and hyperthermophilic pullulanase |
| CN109182417A (en) * | 2018-09-18 | 2019-01-11 | 山东百龙创园生物科技股份有限公司 | A kind of preparation method of reproducibility resistant dextrin |
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