CN113957107B - Preparation method of porous starch with high oil absorption rate - Google Patents
Preparation method of porous starch with high oil absorption rate Download PDFInfo
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- 229920002472 Starch Polymers 0.000 title claims abstract description 175
- 235000019698 starch Nutrition 0.000 title claims abstract description 170
- 239000008107 starch Substances 0.000 title claims abstract description 169
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 102000004190 Enzymes Human genes 0.000 claims abstract description 54
- 108090000790 Enzymes Proteins 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 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 claims abstract description 19
- 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 claims abstract description 19
- 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 claims abstract description 19
- 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 claims abstract description 19
- 102000004366 Glucosidases Human genes 0.000 claims abstract description 16
- 230000008961 swelling Effects 0.000 claims abstract description 16
- 108010056771 Glucosidases Proteins 0.000 claims abstract description 15
- 235000013336 milk Nutrition 0.000 claims description 48
- 239000008267 milk Substances 0.000 claims description 48
- 210000004080 milk Anatomy 0.000 claims description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229920002261 Corn starch Polymers 0.000 claims description 12
- 239000008120 corn starch Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229920001592 potato starch Polymers 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000009849 deactivation Effects 0.000 claims description 5
- 229940100445 wheat starch Drugs 0.000 claims description 5
- 238000006911 enzymatic reaction Methods 0.000 claims description 4
- 230000000977 initiatory effect Effects 0.000 claims description 3
- 239000012064 sodium phosphate buffer Substances 0.000 claims description 3
- 240000003183 Manihot esculenta Species 0.000 claims description 2
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 230000000415 inactivating effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000008057 potassium phosphate buffer Substances 0.000 claims description 2
- 229940088598 enzyme Drugs 0.000 abstract description 47
- 206010042674 Swelling Diseases 0.000 abstract description 15
- 108090000637 alpha-Amylases Proteins 0.000 abstract description 6
- 102000004139 alpha-Amylases Human genes 0.000 abstract description 5
- 229940024171 alpha-amylase Drugs 0.000 abstract description 5
- 239000003921 oil Substances 0.000 description 25
- 235000019198 oils Nutrition 0.000 description 25
- 230000009471 action Effects 0.000 description 18
- 239000008187 granular material Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 238000000053 physical method Methods 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 102000005744 Glycoside Hydrolases Human genes 0.000 description 6
- 108010031186 Glycoside Hydrolases Proteins 0.000 description 6
- 102000013142 Amylases Human genes 0.000 description 5
- 108010065511 Amylases Proteins 0.000 description 5
- 235000019418 amylase Nutrition 0.000 description 5
- 239000004382 Amylase Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 102000001746 Pancreatic alpha-Amylases Human genes 0.000 description 3
- 108010029785 Pancreatic alpha-Amylases Proteins 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000008363 phosphate buffer Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 229920000881 Modified starch Polymers 0.000 description 2
- 239000004368 Modified starch Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009088 enzymatic function Effects 0.000 description 2
- 235000019426 modified starch Nutrition 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241001467578 Microbacterium Species 0.000 description 1
- 241001467565 Microbacterium imperiale Species 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 108010028144 alpha-Glucosidases Proteins 0.000 description 1
- 229940025131 amylases Drugs 0.000 description 1
- 108010019077 beta-Amylase Proteins 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003778 fat substitute Substances 0.000 description 1
- 235000013341 fat substitute Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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- 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
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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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
- C12P19/14—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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Abstract
The invention provides a preparation method of porous starch with high oil absorption rate. The porous starch is prepared by combining swelling pretreatment with the co-action of a double enzyme method, the treatment is simple, and the product safety is high. The swelling temperature is controlled to be 5 ℃ above and below the gelatinization starting temperature, different temperature points are selected, short-time swelling treatment is carried out, and the oil absorption rate of the obtained porous starch is improved by 1.3-1.7 times; the invention adopts the combination of maltotriose, glucosidase and alpha-amylase, preferably optimizes the optimal reaction condition and the addition proportion, and proves that the porous starch can obtain better oil absorption performance only under the fixed addition sequence.
Description
Technical Field
The invention belongs to the technical field of modified starch, and particularly relates to a preparation method of high oil absorption porous starch.
Background
Porous starch, also called microporous starch, is porous honeycomb particle type modified starch with a large amount of pore structure distributed or penetrating through the whole starch particles, has the characteristics of high porosity, high specific surface area, good loading performance and the like, and is widely focused on multiple fields of medicine, chemical industry, environmental protection, food and the like. The porous starch can be used as an adsorbent, a fat substitute, an active substance microcapsule, a flavor substance carrier and the like, and the starch raw material has wide sources, is safe and nontoxic, has extremely high biocompatibility, and therefore has extremely high application value.
Currently, the preparation methods of porous starch mainly comprise three methods, namely a physical method, a chemical method and a biological enzyme method. The physical method mainly means that the damage of the surface structure of the starch particles is realized by the external physical actions such as ultrasonic waves, spraying, mechanical impact or repeated freezing and thawing to increase the number and the volume of holes, but the physical method is numerous, but has the defects of low porosity, poor uniformity and adsorption performance, high equipment requirement, high energy consumption and high production cost, and has difficulty in realizing industrial production; the chemical method is to treat the starch particles with acid, ethanol or other chemical reagent to form pores on the surface of the starch particles and extend the starch particles from outside to inside. Compared with a physical method, the porous starch prepared by the chemical method has certain advantages, such as low equipment requirement, low energy consumption and low production cost, but has strong randomness, lower porosity, environmental protection problem and the like, so that the porous starch is limited in industrial production and application; the biological enzyme process is to treat starch with exoenzyme, such as saccharifying enzyme, and endoenzyme, such as alpha-amylase, to make the non-reducing end of starch cut and inscribed randomly to produce great amount of holes deep into the granule, and the product has great amount of deep holes, great specific surface area and high adsorption rate. The biological enzyme method is the mainstream technology of the current porous starch industrial production, but has the problems of enzyme limitation for production, long reaction time, uneven micropore distribution, low enzymolysis efficiency and the like.
In recent years, the cooperative preparation of porous starch by combining a physical method or a chemical method with a biological enzyme method has become the mainstream; the preparation method of the V-shaped granular porous starch (application number: 202011632449.1) comprises the following steps: the method comprises the steps of preparing V-shaped starch by a high Wen Chun method (100-150 ℃), adding alpha-amylase and saccharifying enzyme into an ethanol system to modify the starch, and preparing the V-shaped porous starch; a method for preparing modified porous starch using a pulsed electric field (20171076798. X): preparing porous starch with high adsorptivity, high transparency, high freeze thawing stability and high mechanical energy by using pulse starch under the condition of being lower than the gelatinization temperature of the starch; a method for preparing porous starch by an ultra-high pressure auxiliary enzyme method (201810004365. X): the method is characterized in that starch is used as a raw material, after ultrahigh pressure treatment, alpha-amylase and saccharifying enzyme are adopted to carry out enzymolysis treatment on the starch, so that porous starch is obtained, and the adsorption performance of the porous starch prepared by the method is enhanced, and the production period is shortened. The physical method or the chemical method is combined with the biological enzyme method, so that the enzymolysis efficiency can be improved better, the product performance is changed, but the problems that the physical method needs better equipment assistance, pollution exists in the chemical method and the like cannot be changed, and the limitation is still larger; meanwhile, the biological enzyme method is mainly focused on the application of one or a combination of alpha-amylase and glycosidase, while other enzymes such as beta-amylase, pullulanase and the like are reported, but the enzymolysis efficiency is lower, and the practical application is limited.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above-mentioned and conventional problems occurring in the prior art.
Therefore, the invention aims to provide a preparation method of porous starch with high oil absorption rate.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided: a preparation method of porous starch with high oil absorption rate comprises,
pretreatment: preparing starch raw materials into starch milk;
preheating: preheating to realize proper swelling of starch;
and (3) enzymolysis treatment: adjusting pH, adding enzyme reaction into the swelled starch milk, and inactivating enzyme of the starch milk after the enzymolysis reaction is finished;
post-treatment: regulating the pH of the starch milk after the enzymolysis treatment to 7.0 by using 1M hydrochloric acid, repeatedly washing for a plurality of times by using distilled water until the washing liquid is neutral, drying, grinding, crushing and sieving to obtain a porous starch product;
the sequential enzyme reaction is that 300U/g of glucosidase is added for 3 hours, the pH of starch milk is adjusted to 11 by 1MNaOH, and the reaction is carried out for 10 minutes, and enzyme is inactivated; adding 400U/g maltotriose to react for 3 hours, wherein the adding amount ratio of the glucosidase to the maltotriose is 3:4;
the preheating is performed for 10min at the gelatinization initiation temperature of + -5 ℃ of the starch raw material.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the starch raw material comprises one or more of corn starch, wheat starch, potato starch and tapioca starch.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the preparation of starch raw material into starch milk comprises the steps of,
dispersing starch material in a solution comprising 50mM sodium phosphate buffer or potassium phosphate buffer and 5mM CaCl 2 The dispersion having a pH of 6.0 was prepared as a starch milk having a mass concentration of 10 to 50%.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the pH of the enzymolysis treatment is adjusted by using 1M hydrochloric acid or NaOH to adjust the pH of the starch milk to the optimal pH of the required additive enzyme.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the enzyme deactivation comprises the steps of,
the pH of the starch milk is adjusted to 11 by 1MNaOH for 10min to stop the enzyme deactivation, and the enzyme deactivation time is 10min.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the drying is to dry at 30-50 ℃ until the moisture content of the starch milk is 8-12%.
As a preferable scheme of the preparation method of the Gao Xiyou porous starch, the preparation method comprises the following steps: the sieving is 100-200 mesh sieving.
The invention has the beneficial effects that:
the invention provides a method for moderately swelling and pretreating starch, which can avoid the problems of high requirement on most of the existing physical method equipment, high energy consumption, strong randomness of a chemical method, environmental protection and the like, screens swelling temperature, selects different temperature points above and below the gelatinization starting temperature by 5 ℃ and carries out short-time swelling treatment, and the oil absorption rate of the obtained porous starch is improved by 1.3-1.7 times.
The action modes of different amylase on starch granules are inconsistent, and the invention is compounded and used from maltotriose enzyme and glucosidase. In the preparation process, glycosidase needs to be added first to react to form holes, and then maltotriose is added. Experiments prove that only this feeding sequence can make the enzyme function better, which also indicates that the type of the enzyme and the feeding sequence play a decisive role in the oil absorption rate of the porous starch. The invention also provides an effective method for preparing the porous starch with high oil absorption rate by selecting the reaction conditions and the adding proportion.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a process flow of a porous starch preparation process;
FIG. 2 is a diagram of a scanning electron microscope of a common commercially available corn starch;
FIG. 3 is a scanning electron microscope image of the corn porous starch prepared in example 3.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The method for calculating the porous starch yield in the embodiment of the invention comprises the following steps:
after enzymolysis, the supernatant is poured out, and the precipitated porous starch is placed in a flat plate for drying and weighing.
Wherein m is the total mass of the starch sample and g; m is m 1 The mass of the plate is g; m is m 2 G is the total mass of the flat plate and the porous starch after drying.
The method for calculating the oil absorption rate of the porous starch in the embodiment of the invention comprises the following steps:
accurately weighing 1g of porous starch in a beaker, adding 10mL of peanut oil, placing on a magnetic stirrer for stirring for 30min, pouring the mixed solution into a sand core funnel for suction filtration until no oil drops drop, recording the front and rear mass of the sand core funnel, and calculating according to the following formula.
Wherein m is 3 G, the mass of the sand core funnel before suction filtration; m is m 4 G, the mass of the sand core funnel after suction filtration; m is m 5 The mass of the porous starch is weighed and g is measured.
The maltotriose enzyme used in the examples of the present invention was derived from Microbacterium moth (Microbacterium imperiale), and had a molecular weight of about 65kDa as determined by electrophoresis, and porcine pancreatic alpha amylase and glucosidase were purchased from Shanghai Sigma-Aldrich company.
Corn starch and potato starch used in the examples of the present invention were purchased from national starch industry (Shanghai) Inc., and wheat starch was supplied by Jiangsu Huashen flour Inc.
The corn starch used in the examples of the present invention was a common commercial corn starch with an initial gelatinization temperature of 63 ℃.
The sodium phosphate buffer used in the examples of the present invention is Na 2 HPO 4 And NaH 2 PO 4 Formulated at 50mM, providing a buffered pH condition for enzyme action; caCl used 2 5mM; hydrochloric acid 1M was used; the NaOH solution used was 1M.
Comparative example 1:
100g of common corn starch is taken and dispersed in phosphate buffer with pH of 6.0 and CaCl 2 In the moderating solution of (2), 10% starch milk was prepared, and stirred in a water bath at room temperature for 10min (not swollen).
The pH of the starch milk is adjusted to 5.0 by 1M hydrochloric acid, 300U/g of glucosidase is added for 3 hours, the pH of the starch milk is adjusted to 11 by 1M NaOH, and the reaction is stopped after 10 minutes. The pH of the starch milk was adjusted to 6.5 with 1M hydrochloric acid, 400U/g maltotriose was added thereto for 3 hours, and the reaction was terminated by adjusting the pH of the starch milk to 11 with 1M NaOH for 10 minutes.
And (3) regulating the pH of the starch milk to 7.0 by using 1M hydrochloric acid, repeatedly washing with distilled water for a plurality of times to make the washing liquid neutral, drying the product until the water content reaches 10%, grinding and sieving with a 100-mesh sieve to obtain the porous starch (not swelled).
Example 1:
100g of common corn starch is taken and dispersed in phosphate buffer with pH of 6.0 and CaCl 2 In the moderating solution of (2), 10% of starch milk is prepared, heated and stirred at different temperatures, and then the temperature of the water bath kettle is reduced to 50 ℃.
The pH of the starch milk is adjusted to 5.0 by 1M hydrochloric acid, 300U/g of glucosidase is added for 3 hours, the pH of the starch milk is adjusted to 11 by 1M NaOH, the reaction is stopped after 10 minutes, the pH of the starch milk is adjusted to 6.5 by 1M hydrochloric acid, 400U/g of maltotriose is added for 3 hours, and the pH of the starch milk is adjusted to 11 by 1M NaOH for 10 minutes to stop the reaction.
And (3) regulating the pH of the starch milk to 7.0 by using 1M hydrochloric acid, repeatedly washing with distilled water for a plurality of times to make the washing liquid neutral, drying the product until the water content is below 10%, grinding and sieving with a 100-mesh sieve to obtain the porous starch.
TABLE 1 influence of different swelling temperatures and times on porous starch yield and oil absorption
From example 1, comparative example 1 and table 1, it is understood that the moderate swelling plays a certain role in improving the oil absorption of porous starch, and the more desirable the improving effect is as the gelatinization initiation temperature is approached. The swelling temperature and time are screened, and the swelling treatment is carried out for a short time at 5 ℃ above and below the gelatinization starting temperature, more preferably at 2 ℃ above and below the gelatinization starting temperature, so that the oil absorption rate of the obtained porous starch is improved by 1.3-1.7 times. The starch granules are moderately swelled in a short time near the initial temperature and are in an irreversible water absorption stage, so that the grain crystal structure of the starch granules cannot be changed obviously, the grain volume of the starch granules can be increased moderately, and meanwhile, the surface of the starch granules is swelled to be more favorable for the adhesion and action of amylase, so that the enzymolysis pore opening effect of the starch granules is improved. However, if the action time is too long, the starch particles are damaged to a certain extent under the action of stirring mechanical force, and the damage action is more remarkable when the gelatinization starting temperature is higher, so that the swelling lifting effect of the starch particles is reduced. Therefore, the starch is swelled for a short time near the gelatinization starting temperature, and the oil absorption rate of the porous starch can be remarkably improved.
Example 2:
100g of common corn starch is taken and dispersed in phosphate buffer with pH of 6.0 and CaCl 2 10% starch milk was prepared, heated and stirred at 63 ℃ for 10min, then the water bath temperature was reduced to 50 ℃, and different enzyme combinations were added according to table 2.
When the enzyme is maltotriose, 1MNaOH is used to adjust the pH of the starch milk to pH6.5, maltotriose is added for reaction for 3 hours, and then 1MNaOH is used to adjust the pH of the starch milk to 11 for reaction for 10 minutes to terminate the reaction.
When the enzyme is glucosidase, the pH of the starch milk is adjusted to 5.0 by 1M hydrochloric acid, the glucosidase is added for 3 hours, and the pH of the starch milk is adjusted to 11 by 1MNaOH for 10 minutes to terminate the reaction.
When the enzyme is porcine pancreatic alpha amylase, the pH of the starch milk is adjusted to 6.9 by 1MNaOH, the porcine pancreatic alpha amylase is added for 3 hours, and the pH of the starch milk is adjusted to 11 by 1MNaOH for 10 minutes to stop the reaction.
When the enzyme is added as the complex enzyme, the pH of the starch milk is adjusted to 5.5 by 1M hydrochloric acid, the complex enzyme is added for reaction for 3 hours, and then the pH of the starch milk is adjusted to 11 by 1MNaOH for reaction for 10 minutes to terminate the reaction.
And after the reaction is finished, regulating the pH of the starch milk to 7.0 by using 1M hydrochloric acid, repeatedly washing with distilled water for a plurality of times to make the washing liquid neutral, drying the product until the water content is less than 10%, and grinding and sieving the product with a 100-mesh sieve to obtain the porous starch.
TABLE 2 influence of different enzyme combinations on the oil absorption and yield of porous starch
The modes of action of different amylases on starch granules are not consistent, e.g. glucosidase tends to erode progressively from the outside to the inside of the starch granule, while maltotriose tends to act on the strong inside of the starch. The porous starch obtained by the glycosidase and the maltotriose has higher oil absorption rate mainly because of holes formed by the pre-action of the glycosidase, which is beneficial to the action of other enzymes. As can be seen from the table, the effect of the complex enzyme is weaker than that of the sequential enzyme. The main reasons for this are presumed to be three: firstly, the action pH of the complex enzyme is not the optimal action pH of the single enzyme, which is unfavorable for the action of two enzymes; secondly, the starch granules have limited sites suitable for enzyme action, and the possibility of competitive action exists when different enzymes act simultaneously, so that the action of the enzymes is weakened; finally, sequential enzyme action, especially glycosidase action, formed holes are beneficial to other amylase action in starch granules, so that the depth of the holes of the starch granules is increased by Kong Dianfen.
Experiments prove that only the combination of enzymes is added in sequence, the functions of the two enzymes can be fully exerted, and the obtained porous starch can obtain better oil absorption rate, which indicates that the combination method and the addition sequence of the enzymes play a decisive role in the quality of the porous starch. In particular, when the adding sequence is that 300U/g of glucosidase is added first and then 400U/g of maltotriose is added, the oil absorption rate of the obtained porous starch can reach 123.6%, and the yield can also reach 60.4%.
Example 3:
dispersing 100g of common starch in phosphate buffer solution with pH of 6.0 and CaCl 2 Preparing 10% starch milk, heating and stirring at different temperatures (corn starch 63 deg.C, potato starch 60 deg.C, wheat starch 50 deg.C, all set to gelatinization start temperature) for 10min, and then cooling to 50deg.C.
The pH of the starch milk is adjusted to 5.0 by 1M hydrochloric acid, the glucosidase is added for reaction for 3 hours, the pH of the starch milk is adjusted to 11 by 1M NaOH, the reaction is stopped after 10 minutes, the pH of the starch milk is adjusted to 6.5 by 1M hydrochloric acid, maltotriose is added for reaction for 3 hours, and the pH of the starch milk is adjusted to 11 by 1M NaOH for 10 minutes, and the reaction is stopped.
And (3) regulating the pH of the starch milk to 7.0 by using 1M hydrochloric acid, repeatedly washing with distilled water for a plurality of times to make the washing liquid neutral, drying the product until the water content reaches 10%, grinding and sieving with a 100-mesh sieve to obtain the porous starch.
TABLE 3 influence of different enzyme combinations on porous starch yield and oil absorption
As can be seen from example 3, the preparation process according to the invention is essentially suitable for common commercial starches. In corn starch, wheat starch and potato starch, the porous starch prepared by using the corn starch and the potato starch has higher oil absorption rate. In particular, when the ratio of the added amount of glucosidase to maltotriose is 3:4, the oil absorption rate reaches 123.6 percent. This is probably because the two are sequentially acted on the starch particles in different proportions, so that the pore diameter and the pore depth of the porous starch are suitable, and the starch structure is not broken due to the fact that the pore diameter and the pore depth are smaller or too large, so that the pore diameter oil absorption rate and the pore diameter oil absorption rate of the prepared porous starch are higher.
The invention provides a method for moderately swelling and pretreating starch, which can avoid the problems of high requirement on most of the existing physical method equipment, high energy consumption, strong randomness of a chemical method, environmental protection and the like, screens swelling temperature, selects different temperature points above and below the gelatinization starting temperature by 5 ℃ and carries out short-time swelling treatment, and the oil absorption rate of the obtained porous starch is improved by 1.3-1.7 times.
The action modes of different amylase on starch granules are inconsistent, and the invention is compounded and used from maltotriose enzyme and glucosidase. In the preparation process, glycosidase needs to be added first to react to form holes, and then maltotriose is added. Experiments prove that only this feeding sequence can make the enzyme function better, which also indicates that the type of the enzyme and the feeding sequence play a decisive role in the oil absorption rate of the porous starch. The invention also provides an effective method for preparing the porous starch with high oil absorption rate by selecting the reaction conditions and the adding proportion.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (7)
1. A preparation method of porous starch with high oil absorption rate is characterized by comprising the following steps: comprising the steps of (a) a step of,
pretreatment: preparing starch raw materials into starch milk;
preheating: preheating to realize proper swelling of starch;
and (3) enzymolysis treatment: adjusting pH, adding sequential enzyme reaction into the swelled starch milk, and inactivating enzyme of the starch milk after the enzymolysis reaction is finished;
post-treatment: regulating the pH of the starch milk after the enzymolysis treatment to 7.0 by using 1M hydrochloric acid, repeatedly washing for a plurality of times by using distilled water until the washing liquid is neutral, drying, grinding, crushing and sieving to obtain a porous starch product;
the sequential enzyme reaction is that 300U/g glucosidase is added for 3h, 1M NaOH is used for adjusting the pH of starch milk to 11, and the reaction is carried out for 10min, and enzyme is inactivated; adding 400U/g maltotriose enzyme to react with 3h, wherein the adding amount ratio of the glucosidase to the maltotriose enzyme is 3:4;
the preheating is performed for 10min at the gelatinization initiation temperature of + -5 ℃ of the starch raw material.
2. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: the starch raw material comprises one or more of corn starch, wheat starch, potato starch and tapioca starch.
3. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: the preparation of starch raw material into starch milk comprises the steps of,
dispersing starch material into a solution comprising 50. 50mM sodium phosphate buffer or potassium phosphate buffer and 5mM CaCl 2 The dispersion having a pH of 6.0 is prepared as a starch milk having a mass concentration of 10 to 50%.
4. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: the pH of the enzymolysis treatment is adjusted by using 1M hydrochloric acid or NaOH to adjust the pH of the starch milk to the optimal pH of the required additive enzyme.
5. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: the enzyme deactivation comprises the steps of,
the pH of the starch milk is adjusted to 11 by using 1M NaOH to react for 10min, the reaction is stopped, and the enzyme deactivation time is 10min.
6. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: and the drying is performed at 30-50 ℃ until the moisture content of the starch milk is 8-12%.
7. The method for preparing the Gao Xiyou porous starch according to claim 1, wherein the method comprises the following steps: the sieving is 100-200 mesh sieving.
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| CN1661028A (en) * | 2004-12-22 | 2005-08-31 | 华南理工大学 | Method for preparing porous starch through enzyme method in high temperature |
| CN101608195A (en) * | 2008-06-19 | 2009-12-23 | 陕西北美基因股份有限公司 | A kind of method for preparing high specific surface micro-pore starch with the sequential acid-enzyme solution |
| CN102533908A (en) * | 2012-01-04 | 2012-07-04 | 江南大学 | Method for preparing porous starch with high oil absorption rate through preprocessing starch |
| CN103060400A (en) * | 2012-12-19 | 2013-04-24 | 华南理工大学 | Porous starch and joint preparation method for liquid glucose used for fermentation thereof |
| CN108018322A (en) * | 2018-01-24 | 2018-05-11 | 浙江树人学院 | A kind of preparation method of corn porous starch |
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| CN1661028A (en) * | 2004-12-22 | 2005-08-31 | 华南理工大学 | Method for preparing porous starch through enzyme method in high temperature |
| CN101608195A (en) * | 2008-06-19 | 2009-12-23 | 陕西北美基因股份有限公司 | A kind of method for preparing high specific surface micro-pore starch with the sequential acid-enzyme solution |
| CN102533908A (en) * | 2012-01-04 | 2012-07-04 | 江南大学 | Method for preparing porous starch with high oil absorption rate through preprocessing starch |
| CN103060400A (en) * | 2012-12-19 | 2013-04-24 | 华南理工大学 | Porous starch and joint preparation method for liquid glucose used for fermentation thereof |
| CN108018322A (en) * | 2018-01-24 | 2018-05-11 | 浙江树人学院 | A kind of preparation method of corn porous starch |
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