CN113882024A - Method for preparing starch nanofiber by electrostatic spinning - Google Patents
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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Abstract
The invention discloses a method for preparing starch nanofibers through electrostatic spinning. The method takes a high amylose debranching solution as a raw material, forms a spinning solution after shearing and homogenizing, and prepares the starch nanofiber through electrostatic spinning. The method has simple process, uses water as a unique solvent, does not use an organic solvent, is green and environment-friendly, and the prepared starch nanofiber has a perfect non-beaded fiber shape and uniform fiber diameter distribution, has an average fiber diameter of 121-158 nm, and can be used as an adsorption material, a delivery carrier and a tissue scaffold to be applied to the fields of food, medicine, cosmetics and the like.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a method for preparing starch nano fibers by electrostatic spinning.
Background
The electrostatic spinning starch nanofiber has the characteristics of high porosity, extremely high specific surface area, good biocompatibility, biodegradability and the like, and has great application potential in the medical fields of drug delivery, wound dressing, tissue engineering and the like. The research of applying native starch to electrospinning began in 2012, and american scientists Ziegler et al reported that starch fibers were prepared by "wet" electrospinning using dimethyl sulfoxide as a solvent and ethanol as a precipitating agent for a coagulation bath (Kong & Ziegler, Biomacromolecules,2012,13(8): 2247-. Although starch nanofibers (-146 nm) can be obtained by high temperature gelatinization of high amylose starch and complex electrospinning with fatty acid salts and pullulan, problems such as too long drying time still remain (Wang & Ziegler, International Journal of Biological Macromolecules,2019,133: 1168-. Lanmuski et al first reported that "dry" electrospinning of formic acid as a solvent can yield starch nanofibers with diameters between 80-300nm, but the use of formic acid causes methylesterification of the starch molecules and degradation of their molecular weight, and the formic acid dissolves the starch for too long (> 24h) (Lanmuski et al, Biomacromolecules,2015,16(8): 2529-2536). At present, a large amount of organic solvents (dimethyl sulfoxide and formic acid) are needed to dissolve starch in the processes of preparing the starch fiber by the wet method and the dry method, so that potential safety hazards exist, and the application of the starch fiber in the fields of food, medicine and cosmetics is limited.
Disclosure of Invention
The invention aims to provide a method for preparing starch nanofibers by electrostatic spinning, which is simple in process and does not use an organic solvent.
The technical scheme for realizing the purpose of the invention is as follows:
the method for preparing the starch nanofiber by electrostatic spinning enhances the intermolecular entanglement degree of the high amylose debranching solution and increases the spinnability of the starch nanofiber by shearing and homogenizing, and comprises the following specific steps:
shearing and homogenizing 0.2-0.3G/mL high amylose debranching solution at 10000-20000 rpm for 1-2 min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10-20 mL needle tube injector, and connecting a spinning needle of 18-23G, wherein the electrostatic spinning parameters are as follows: the voltage is 10-20 kV, the spinning distance is 10-20 cm, the flow rate of the injector is 0.1-0.3 mL/h, the rotating speed of the roller is 5-20 rpm, and the starch nanofibers are obtained through electrostatic spinning.
Preferably, the electrostatic spinning time is 2-4 h.
Preferably, the preparation method of the high amylose debranching solution is as follows:
step (1), fully gelatinizing high amylose starch: dispersing high amylose starch in a buffer solution with the pH value of 4.5-6.0 according to 0.2-0.3 g/mL, heating in a boiling water bath for 1-2 h, placing in an autoclave, and treating at 121-142 ℃ for 20-60 min to obtain a fully gelatinized high amylose starch solution;
step (2), debranching enzymolysis: and (3) placing the high amylose starch solution in a water bath at 50-65 ℃, adding 20-40U/g debranching enzyme, performing enzymolysis for 12-24 hours, placing in an autoclave, and treating at 121-142 ℃ for 20-60 min to obtain the high amylose starch debranching solution.
Preferably, in the step (1), the high amylose starch is high amylose corn starch or high amylose rice starch, and the content of amylose is 65-80%; the buffer solution is phosphate, acetate or citrate buffer solution.
Preferably, in the step (2), the debranching enzyme is pullulanase or isoamylase; the molecular weight of the high amylose debranching solution is 3-5 multiplied by 105g/mol。
The method takes the water-soluble high amylose debranching solution with good dispersibility as a raw material, enhances the intermolecular entanglement degree of the high amylose debranching solution by shearing and homogenizing, and greatly increases the spinnability of the starch nanofibers without using organic solvents. The starch nanofiber prepared by the method disclosed by the invention is in a perfect non-beaded fiber form, the fiber diameters are uniformly distributed, the average fiber diameter is 121-158 nm, the safety is good, and the starch nanofiber can be used as an adsorbing material, a delivery carrier and a tissue scaffold to be applied to related fields of food, medicine, cosmetics and the like.
Drawings
FIG. 1 is a scanning electron micrograph of an electrospun high amylose debranching solution of comparative example 1;
FIG. 2 is a scanning electron micrograph of an electrospun high amylose debranching solution of comparative example 4;
FIG. 3 is a scanning electron micrograph of an electrospun high amylose debranching solution of comparative example 6;
FIG. 4 is a scanning electron micrograph of electrospun starch nanofibers of example 1;
FIG. 5 is a fiber diameter distribution diagram of electrospun starch nanofibers of example 1;
FIG. 6 is a scanning electron micrograph of electrospun starch nanofibers of example 2;
FIG. 7 is a fiber diameter distribution diagram of electrospun starch nanofibers of example 2;
FIG. 8 is a scanning electron micrograph of electrospun starch nanofibers of example 3;
fig. 9 is a fiber diameter distribution diagram of electrospun starch nanofibers of example 3.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples and drawings, but the scope of the present invention is not limited to the examples.
The test methods described in the examples are as follows:
1) scanning electron microscope observation of samples
The sample was fixed on a metal stage with a conductive paste, and after spraying gold in vacuum for 90 seconds, the morphology of the sample was observed by a scanning electron microscope (S-4800 II, Hitachi, Japan) and observed and photographed at 20000 times.
2) Diameter analysis of samples
And analyzing the obtained scanning electron microscope pictures of the samples by ImageJ software, taking 5-10 pictures of each sample, taking points of each picture for 50-100 times, and calculating the average diameter after diameter data is obtained.
Comparative example 1
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: directly taking the high amylose corn starch debranching solution obtained in the step (2) as an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle head; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
It was tested that no fibrous structure was observed in the sem images of the electrospun high amylose debranching solution samples, exhibiting highly aggregated starch nanoparticles, as shown in fig. 1, indicating that the high amylose debranching solution, which was not shear homogenized, had insufficient intermolecular entanglement and was not spinnable.
Comparative example 2
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.35g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 10000rpm for 1min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
It was tested that electrospinning a high amylose corn starch debranching solution of 0.35g/mL did not yield a spun sample, which may prevent electrospinning by causing the solution viscosity to be too high due to the too high concentration of the spinning solution.
Comparative example 3
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.15g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 10000rpm for 1min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
It was tested that electrospinning a high amylose corn starch debranching solution of 0.15g/mL did not yield a spun sample, possibly due to the occurrence of electrostatic spraying due to too low a concentration of the spinning solution.
Comparative example 4
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 5000rpm for 1min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
Through tests, the scanning electron microscope image of the sample of the electrostatic spinning high amylose debranching solution shows the composite state of the nano-fibers and the 'beads' thereof, as shown in figure 2, the shearing homogenization can enhance the intermolecular entanglement degree of the spinning solution and improve the spinning effect, but when the shearing homogenization rotating speed is too low, the perfect (without 'beads') starch nano-fibers can not be obtained.
Comparative example 5
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 25000rpm for 1min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
Tests show that the high-amylose corn starch debranching solution subjected to shearing homogenization treatment at a high rotating speed cannot obtain a spinning sample. Although the shearing homogenization can improve the intermolecular entanglement degree of the spinning solution, the shearing homogenization at an excessively high rotation speed also causes the viscosity of the spinning solution to be greatly improved, and the electrostatic spinning is prevented.
Comparative example 6
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 10000rpm for 0.5min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
Through testing, the scanning electron microscope image of the sample of the electrostatic spinning high amylose debranching solution shows the composite state of the nano-fibers and the 'beads' thereof, as shown in figure 3, which is similar to figure 2. The influence of too short shearing homogenizing time and too low shearing homogenizing rotating speed on starch electrostatic spinning is similar to that of the shearing homogenizing rotating speed, and the shearing homogenizing time and the shearing homogenizing rotating speed can both prove to enhance the intermolecular entanglement degree of the spinning solution and improve the spinning effect of the spinning solution, but the shearing homogenizing time is too short and the shearing homogenizing rotating speed is too low, so perfect (without 'beads') starch nanofibers cannot be obtained.
Comparative example 7
(1) Full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain a high amylose corn starch debranching solution (molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 10000rpm for 2.5min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm, wherein the flow rate of the injector is 0.1mL/h, the rotating speed of the roller is 5rpm, and thus obtaining a spinning sample.
Tests show that the high-amylose corn starch debranching solution subjected to shearing homogenization treatment at a high rotating speed cannot obtain a spinning sample. Although shearing homogenization can improve the intermolecular entanglement degree of the spinning solution, the viscosity of the spinning solution is greatly improved due to the excessive shearing homogenization, and electrostatic spinning is prevented.
Example 1
The method for preparing the starch nanofiber by electrostatic spinning comprises the following steps:
(1) full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 70%) in phosphate buffer solution with pH of 5.0 according to mass concentration of 0.25g/mL, heating in boiling water bath for 1h, and treating in autoclave at 142 deg.C for 20min to obtain fully gelatinized high amylose corn starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for processing at 121 ℃ for 20min to obtain the high amylose corn starch debranching solution (the molecular weight is 3 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 10000rpm for 1min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10mL needle tube injector, and connecting a 20G spinning needle; and (3) carrying out electrostatic spinning for 4 hours at an electrostatic spinning voltage of 15kV and a spinning distance of 15cm and a flow rate of 0.1mL/h and a roller rotation speed of 5rpm to obtain the starch nanofiber.
The resulting spun sample was tested to exhibit a perfect, beadless fiber morphology with a uniform distribution of fiber diameters (fig. 4) with an average fiber diameter of 121nm (fig. 5). Shear homogenization enhances the degree of intermolecular entanglement of the high amylose debranching solution compared to comparative example 1 (fig. 1), thereby greatly increasing the spinnability of electrospun starch nanofibers.
Example 2
The method for preparing the starch nanofiber by electrostatic spinning comprises the following steps:
(1) full gelatinization of high amylose rice starch: dispersing high amylose rice starch (amylose content 65%) in phosphate buffer solution with pH of 4.5 according to mass concentration of 0.3g/mL, heating in boiling water bath for 2h, and treating in autoclave at 121 deg.C for 60min to obtain fully gelatinized high amylose rice starch solution;
(2) debranching and enzymolysis: placing the high amylose rice starch solution obtained in the step (1) in a water bath at 60 ℃, adding 30U/g isoamylase, performing enzymolysis for 18h, and then placing in an autoclave for treatment at 142 ℃ for 30min to obtain the high amylose rice starch debranching solution (the molecular weight is 3.9 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high-amylose rice starch debranching solution obtained in the step (2) at 15000rpm for 2min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 20mL needle tube injector, and connecting with an 18G spinning needle; and (3) carrying out electrostatic spinning for 2 hours under the conditions that the electrostatic spinning voltage is 20kV, the spinning distance is 10cm, the flow rate of the injector is 0.3mL/h and the rotating speed of the roller is 20rpm, thus obtaining a spinning sample.
The resulting spun sample was tested to exhibit a perfect, beadless fiber morphology with a uniform distribution of fiber diameters (fig. 6), with an average fiber diameter of 131nm (fig. 7).
Example 3
The method for preparing the starch nanofiber by electrostatic spinning comprises the following steps:
(1) full gelatinization of high amylose corn starch: dispersing high amylose corn starch (amylose content 80%) in phosphate buffer solution with pH of 6.0 according to mass concentration of 0.2g/mL, heating in boiling water bath for 2h, and treating in autoclave at 135 deg.C for 60min to obtain fully gelatinized high amylose starch solution;
(2) debranching and enzymolysis: placing the high amylose corn starch solution obtained in the step (1) in a water bath at 55 ℃, adding 40U/g isoamylase, performing enzymolysis for 24h, and then placing in an autoclave for treatment at 141 ℃ for 20min to obtain the high amylose corn starch debranching solution (molecular weight is 5 multiplied by 10)5g/mol)；
(3) Preparing starch nanofiber by electrostatic spinning: shearing and homogenizing the high amylose corn starch debranching solution obtained in the step (2) at 20000rpm for 2min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 15mL needle tube injector, and connecting a 23G spinning needle; and electrostatic spinning voltage is 10kV, spinning distance is 20cm, the flow rate of the injector is 0.3mL/h, the rotating speed of the roller is 10rpm, and the spinning sample can be obtained after electrostatic spinning is carried out for 3 h.
The resulting spun sample was tested to exhibit a perfect, beadless fiber morphology with a uniform distribution of fiber diameters (fig. 8) with an average fiber diameter of 158nm (fig. 9).
The invention adopts high amylose debranching solution as raw material. In the preparation process of the high amylose debranching solution, high amylose is treated at high temperature by a boiling water bath and an autoclave to be fully gelatinized, and a double helix structure in the starch is completely opened; and then debranching enzymolysis is carried out to obtain debranched starch solution to improve the water solubility of the debranched starch solution, but too long enzymolysis process can cause recrystallization of partial amylose, so that the helical structure of the partially recrystallized amylose is opened by adopting high-temperature treatment of an autoclave, and the high-amylose debranching solution with good dispersibility is obtained. The high-amylose enzymolysis efficiency and the water solubility are greatly increased through the high-temperature treatment and the debranching enzymolysis of the autoclave, and the use of organic solvents such as dimethyl sulfoxide, formic acid and the like is avoided. In addition, the shearing homogenization treatment enhances the intermolecular entanglement degree of the high amylose debranching solution, and greatly increases the spinnability of the electrospun starch nanofiber.
Claims (8)
1. The method for preparing the starch nanofiber by electrostatic spinning is characterized by comprising the following specific steps:
shearing and homogenizing 0.2-0.3G/mL high amylose debranching solution at 10000-20000 rpm for 1-2 min to obtain an electrostatic spinning solution, filling the electrostatic spinning solution into a 10-20 mL needle tube injector, and connecting a spinning needle of 18-23G, wherein the electrostatic spinning parameters are as follows: the voltage is 10-20 kV, the spinning distance is 10-20 cm, the flow rate of the injector is 0.1-0.3 mL/h, the rotating speed of the roller is 5-20 rpm, and the starch nanofibers are obtained through electrostatic spinning.
2. The method according to claim 1, wherein the electrospinning time is 2 to 4 hours.
3. The method of claim 1, wherein the high amylose debranching solution is prepared by:
step (1), fully gelatinizing high amylose starch: dispersing high amylose starch in a buffer solution with the pH value of 4.5-6.0 according to 0.2-0.3 g/mL, heating in a boiling water bath for 1-2 h, placing in an autoclave, and treating at 121-142 ℃ for 20-60 min to obtain a fully gelatinized high amylose starch solution;
step (2), debranching enzymolysis: and (3) placing the high amylose starch solution in a water bath at 50-65 ℃, adding 20-40U/g debranching enzyme, performing enzymolysis for 12-24 hours, placing in an autoclave, and treating at 121-142 ℃ for 20-60 min to obtain the high amylose starch debranching solution.
4. The method of claim 3, wherein in step (1), the high amylose starch is high amylose corn starch or high amylose rice starch.
5. The method according to claim 3, wherein in step (1), the high amylose content is 65 to 80%.
6. The method according to claim 3, wherein in step (1), the buffer solution is a phosphate, acetate or citrate buffer solution.
7. The method according to claim 3, wherein in the step (2), the debranching enzyme is pullulanase or isoamylase.
8. The method according to claim 3, wherein in step (2), the high amylose debranching solution has a molecular weight of 3 to 5 x 105g/mol。
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| CN115211521A (en) * | 2022-07-14 | 2022-10-21 | 集美大学 | Starch nanofiber membrane, preparation method thereof and method for removing oyster peptide fishy smell |
| WO2023071416A1 (en) * | 2021-10-27 | 2023-05-04 | 扬州大学 | Method for preparing starch nanofiber by electrostatic spinning |
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| CN113882024B (en) | 2022-10-14 |
| WO2023071416A1 (en) | 2023-05-04 |
| JP2023553734A (en) | 2023-12-25 |
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