CN114736940A - Preparation method of amylose with different chain lengths - Google Patents
Preparation method of amylose with different chain lengths Download PDFInfo
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- 229920000856 Amylose Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 229920002472 Starch Polymers 0.000 claims abstract description 132
- 235000019698 starch Nutrition 0.000 claims abstract description 130
- 239000008107 starch Substances 0.000 claims abstract description 129
- 239000002244 precipitate Substances 0.000 claims abstract description 51
- 238000010008 shearing Methods 0.000 claims abstract description 36
- 238000011282 treatment Methods 0.000 claims abstract description 35
- 238000012216 screening Methods 0.000 claims abstract description 27
- 238000009826 distribution Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- 239000006185 dispersion Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000005119 centrifugation Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 108090000790 Enzymes Proteins 0.000 claims description 11
- 102000004190 Enzymes Human genes 0.000 claims description 11
- 230000003247 decreasing effect Effects 0.000 claims description 7
- 230000000750 progressive effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000013336 milk Nutrition 0.000 claims description 5
- 239000008267 milk Substances 0.000 claims description 5
- 210000004080 milk Anatomy 0.000 claims description 5
- 108090000637 alpha-Amylases Proteins 0.000 claims description 4
- 229920001592 potato starch Polymers 0.000 claims description 4
- 229920002261 Corn starch Polymers 0.000 claims description 2
- 239000008120 corn starch Substances 0.000 claims description 2
- 229940100445 wheat starch Drugs 0.000 claims description 2
- 235000013305 food Nutrition 0.000 abstract description 7
- 238000001556 precipitation Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 5
- 230000007704 transition Effects 0.000 description 13
- 238000006116 polymerization reaction Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
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- 238000011069 regeneration method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
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- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
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- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
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- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229940114079 arachidonic acid Drugs 0.000 description 1
- 235000021342 arachidonic acid Nutrition 0.000 description 1
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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Abstract
The invention belongs to the technical field of food processing, and discloses a preparation method of amylose with different chain lengths, which comprises the following steps: (1) carrying out debranching treatment on the gelatinized starch, cooling the debranched starch paste to fully regenerate, carrying out centrifugal treatment, and removing supernatant to obtain starch precipitate; (2) preparing 10-20% starch dispersion liquid from the starch precipitate, and performing thermal shearing treatment at 80-120 ℃; (3) and (3) carrying out thermal centrifugation treatment on the starch dispersion liquid subjected to thermal shearing treatment at the same thermal shearing temperature, and respectively collecting supernate and precipitate to obtain the amylose with the specific chain length distribution. The invention carries out screening and grading by a centrifugal mode at different temperatures to obtain the short straight chain starch components with different chain length distributions, and compresses the time consumed by the precipitation gradual grading method which is mainly used at present within several days to several hours.
Description
Technical Field
The invention relates to the fields of food processing technology, chemical industry and medicine, in particular to a method for preparing short straight chain starch with different chain lengths with simple operation and high efficiency.
Background
Starch is an abundant natural resource in China, is an important raw material for a plurality of industries such as food industry, pharmaceutical industry and the like, and how to utilize the starch resource is also an important subject of the food industry. Therefore, deep processing of starch is a key for optimizing the resource distribution efficiency of the starch, while short amylose as an enzymolysis product of starch has important application in food and medicine, but the short amylose has different property and functions due to different chain length distribution and wide molecular weight distribution after enzymolysis. Short amylose starch of a specific chain length possesses its superior spatial helical structure, can form a stable carrier with lipids to entrap drugs to improve the delivery efficiency of drugs, and the complexing ability with fatty acids depends on its chain length (Nuengphysical Klaochang, Chrurera Putten, Vilai Rungsang thong, et al. physiochemical and structural properties of debranned hydrolysis, waxy corn and waxy starch [ J ]. Food Hydrocolloids,2015, 45.). For example, the embedding efficiency of arachidonic acid by short amylose starch with an average DP of 34 is significantly better than that of short amylose starch with an average DP of 22 (Zhan Wei, Yuan Chao, Cui Bo, ethyl. effect of chain length on the structure and physical properties of active compounds/linear compositions [ J ]. Carbohydrate Polymers,2021,269.). Therefore, obtaining short straight chain starch with specific chain length distribution is a key common problem to be solved urgently in starch processing application.
The short amylose fractionation method at home and abroad mainly comprises exclusion chromatography and solvent precipitation stepwise fractionation. The chromatography is not only expensive in the filler and the separation device, but also difficult to be put into industrial production due to small treatment amount. The solvent precipitation stepwise fractionation method mainly comprises two precipitants, namely ethanol and polyethylene glycol: the former can cause low separation efficiency due to local coprecipitation phenomenon and grading temperature sensitivity, while the latter needs at least one day and a large amount of polyethylene glycol reagent for each grading when the separation is carried out successively, so that the disadvantages of long time consumption, large amount of organic reagent consumption and the like exist. Meanwhile, the solvent precipitation gradual classification method needs to remove the residual precipitant in the classified starch, thereby increasing the separation step and the operation difficulty, and causing complicated and inconvenient operation.
Disclosure of Invention
Aiming at the current situations that the existing method for preparing the short linear starch with different chain lengths has long grading time, low grading efficiency, large organic solvent consumption and complex operation and limits the large-scale production in the industrial field, the invention aims to provide the grading method for screening the short linear starch with different chain lengths, which is simple to operate and high-efficiency. The simple, energy-saving and efficient preparation of the short straight chain starch with different chain lengths is realized by the starch with different chain lengths under the conditions of different temperatures and centrifugal forces.
The purpose of the invention is realized by the following technical scheme:
a method for preparing amylose with different chain lengths comprises the following steps:
(1) debranching the gelatinized starch by using debranching enzyme, cooling the obtained debranched starch paste to fully regenerate, performing centrifugal treatment, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 10-20% (w/v) of starch dispersion liquid, and carrying out thermal shearing treatment at 80-120 ℃;
(3) and (3) carrying out thermal centrifugation treatment on the starch dispersion liquid subjected to thermal shearing treatment obtained in the step (2) at the same thermal shearing temperature, and respectively collecting supernatant and precipitate to obtain the amylose with the specific chain length distribution.
Preferably, the method further comprises the step (4) of screening I: and (3) repeating the thermal shearing and thermal centrifuging treatment of the step (2) and the step (3) at least once on the precipitate obtained in the step (3), and collecting the precipitate to further obtain the amylose with the specific chain length distribution.
Preferably, the method further comprises the step (4) of screening II: and (3) cooling the supernatant obtained in the step (3) to fully regenerate, repeating the thermal shearing and thermal centrifugation treatment of the steps (2) and (3) at least once, and collecting precipitates to further obtain the amylose with the specific chain length distribution.
Preferably, the thermal shearing temperature in step (3) and the progressive screening I is increased gradually, and the thermal shearing temperature in step (3) and the progressive screening II is decreased gradually.
Preferably, the thermal shearing treatment is to shear the starch milk at a rotating speed of 350 +/-50 r/min for 30 +/-10 min in a heating process.
Preferably, the centrifugal force of the centrifugal treatment in steps (1), (3) and (4) is gradually reduced.
Preferably, the centrifugal force of the centrifugation treatment in the steps (1) (3) (4) is 5000-.
Preferably, the starch paste in the step (1) and the supernatant in the step (4) of the step-by-step screening II are cooled to below 20 ℃ and regenerated for 1 h.
Preferably, the preparation of debranched starch paste of step (1): adding water into starch to prepare 5-20% starch milk, and heating for gelatinization; and then, reducing the temperature of the starch paste to an appropriate enzyme temperature, adjusting the pH value, and adding pullulanase for enzymolysis to obtain the debranched starch paste.
Preferably, the starch is potato starch, corn starch, soybean starch, wheat starch.
The heating shear temperature or centrifugation temperature according to the invention is preferably 80 to 120 ℃. The set temperature cannot be too high, and the disintegration of the starch aggregate is easy to happen at the too high temperature, so that the starch aggregate is centrifuged to supernatant; if the temperature is too low, there is no specificity in the screening for different chain lengths. In addition, the temperature should be increased or decreased stepwise for each screening. When the step-by-step screening I is carried out in the steps (1), (2), (3) and (4), the thermal shearing temperature is gradually increased along with the screening times, so that the starch aggregate with low phase transition temperature can be damaged, and the thermal stability and the average chain length of the starch aggregate with high phase transition temperature can be improved. Referring to example 5 and fig. 1, when the screening temperature is gradually increased, the branching degree of the obtained starch molecules is gradually reduced, and the amylose content and the average polymerization degree are gradually increased, so that the chain length in the classified starch can be remarkably increased, and the amylose with a longer chain length distribution can be obtained. And (3) when the step-by-step screening II is carried out in the steps (1), (2), (3) and (4), the thermal shearing temperature is gradually reduced along with the screening times, and the centrifugal force is gradually reduced to carry out centrifugal treatment, so that amylose with shorter chain length or amylopectin with small branch can be separated. And then the content and the branching degree of amylose in the graded starch can be controlled, and finally the amylose with different chain lengths is prepared. Referring to example 6 and FIG. 2, when the screening temperature is gradually decreased, the branching degree of the obtained starch molecules is gradually increased, and the amylose content and the average polymerization degree are gradually decreased, so that the amylose component with gradually decreased average chain length and gradually increased branching degree can be obtained.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention carries out screening and grading by a centrifugal mode at different temperatures to obtain the short straight chain starch components with different chain length distributions, and compresses the time consumed by the precipitation gradual grading method which is mainly used at present within several days to several hours.
(2) The invention completely replaces the precipitant organic reagent consumed by the traditional method precipitation gradual grading method with clean resource water, solves the problem that the residual organic solvent in the starch needs to be cleaned and removed after each grading, improves the safety performance of starch screening, simplifies the operation steps of short straight chain starch screening, and can be widely used in the field of fine and further processing of starch resources.
Drawings
FIG. 1 is a graph of the thermal gelatinization profile of amylose of different chain lengths prepared in example 5.
FIG. 2 is a graph of the thermal gelatinization profile of amylose of different chain lengths prepared in example 6.
Detailed Description
In order that the invention may be better understood, the invention will now be further illustrated by way of example. There are many successful embodiments of the present invention, and 6 specific embodiments are listed below, which include 2 step-by-step screening embodiments, but the scope of the present invention is not limited to the embodiments presented.
Preparation of debranched starch pastes in the examples of the present invention reference is made to the method of Oluwaseun et al (Arijaje emulsion oilwaseun, WangYa-Jane. effects of chemical and enzymatic modifications on static-oleic acid complex formation [ J ]. Journal of agricultural and food chemistry,2015,63 (16)), where all raw materials such as potato starch, pullulanase, sodium hydroxide solution, etc. are materials commonly used by those skilled in the art, and the specific preparation of debranched starch pastes is as follows:
weighing 180g (dry basis) of potato starch, adding 1800mL of deionized water to prepare 10% starch milk, and gelatinizing in a water bath at 100 ℃ for 60 min; then, reducing the temperature of the starch paste to 55 ℃, adjusting the pH value to 5.0, and adding pullulanase of 150U/g starch for enzymolysis for 12 hours; adjusting pH to about 7.0 with sodium hydroxide water solution to stop reaction, and inactivating enzyme at 100 deg.C for 60min to obtain debranched starch paste.
Example 1
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated to 20 ℃ for sufficient regeneration for 1h, centrifuging at 5000 Xg for 10min, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 10% (w/v) starch dispersion, and performing thermal shearing treatment in a constant-temperature water bath at 85 ℃ and 350r/min rotation speed for 30 min;
(3) centrifuging the starch dispersion obtained in step (2) at 4500 Xg centrifugal force for 10min at the same thermal shearing temperature (85 ℃), discarding the supernatant, and collecting the precipitate, namely amylose with a specific chain length distribution.
And (3) carrying out thermodynamic analysis on the starch precipitate in the step (1) by adopting a differential scanning calorimeter, wherein the thermal gelatinization parameters are shown in table 1, and respectively carrying out analysis on the branching degree, the amylose content and the chain length distribution of the starch precipitate collected in the step (3) by adopting a superconducting nuclear magnetic resonance spectrometer, an iodine color development method and an ion chromatography. As can be seen from Table 1, the starch precipitate obtained in step (1) has three phase transition peaks, among which Peak I (phase transition range 84.46-94.90 ℃), Peak II (phase transition range 96.79-106.04 ℃) and Peak III (phase transition range 109.78-129.28 ℃) heat absorption peaks, indicating the presence of amylose aggregates with different thermal stabilities, so that setting the thermal shear and thermal centrifugation temperatures allows the starch aggregates with different phase transition temperatures to be separated, and the separated starch precipitate has a branching degree of 7.36%, an amylose content of 53.16% and an average polymerization degree of 23.85. This shows that amylose with a target average DP of 23.85 can be isolated by screening for aggregation behavior of starch short-term retrogradation and differences in aggregate thermal stability, and that thermal shear and thermal centrifugation temperature are key to the preparation of amylose with a specific chain length distribution.
TABLE 1
Example 2
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated to 20 ℃ for sufficient regeneration for 1h, centrifuging at 5000 Xg for 10min, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 15% (w/v) starch dispersion, and performing thermal shearing treatment for 30min at the rotating speed of 350r/min at 95 ℃ in a constant-temperature water bath kettle;
(3) centrifuging the starch dispersion obtained in the step (2) at the same thermal shearing temperature (95 ℃) under the centrifugal force of 4500 Xg for 10min, discarding the supernatant, and collecting the precipitate, namely the short straight chain starch with the specific chain length distribution. The heat gelatinization parameters of the obtained starch precipitate are shown in Table 2, and the starch precipitate has two heat absorption peaks, Peak I (phase transition range of 76.42-98.54 ℃) and Peak II (phase transition range of 105.87-129.38 ℃) which are known to exist. The degree of branching of the separated starch precipitate was 5.63%, the amylose content was 59.43%, and the average degree of polymerization was 26.23.
TABLE 2
Example 3
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated for 1 hour at 20 ℃, centrifuging for 10min at 5000 Xg, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 15% (w/v) starch dispersion liquid, and carrying out thermal shearing treatment for 30min in a constant-temperature water bath at the rotating speed of 350r/min and the temperature of 105 ℃;
(3) centrifuging the starch dispersion liquid obtained in the step (2) at the same thermal shearing temperature under the centrifugal force of 4500 Xg for 10min, discarding the supernatant, and collecting the precipitate, namely the short straight chain starch with specific chain length distribution. The heat gelatinization parameters of the obtained starch precipitate are shown in Table 3, and the starch precipitate has two heat absorption peaks, namely Peak I (phase transition range 73.35-81.46 ℃) and Peak II (phase transition range 109.92-137.34 ℃). The degree of branching of the separated starch precipitate was 4.64%, the amylose content was 61.03%, and the average degree of polymerization was 28.12.
TABLE 3
Example 4
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated to 20 ℃ for sufficient regeneration for 1h, centrifuging at 5000 Xg for 10min, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 20% (w/v) starch dispersion liquid, and carrying out thermal shearing treatment for 30min in a constant-temperature water bath at the rotating speed of 350r/min at 115 ℃;
(3) centrifuging the starch dispersion liquid obtained in the step (2) at the same thermal shearing temperature under the centrifugal force of 4500 Xg for 10min, discarding the supernatant, and collecting the precipitate, namely the short straight chain starch with specific chain length distribution. The obtained starch precipitate thermal gelatinization parameters are shown in Table 4, and the starch precipitate has two heat absorption peaks, namely Peak I (phase transition range of 62.68-75.66 ℃) and Peak II (phase transition range of 108.68-139.83 ℃) and has the separated starch precipitate branching degree of 4.49%, amylose content of 62.15% and average polymerization degree of 29.12.
TABLE 4
Example 5
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated to 20 ℃ for sufficient regeneration for 1h, centrifuging at 5000 Xg for 10min, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 15% (w/v) starch dispersion liquid, and performing thermal shearing treatment in a constant-temperature water bath at 90 ℃ and 350r/min rotation speed for 30 min;
(3) and (3) centrifuging the starch dispersion liquid obtained in the step (2) for 10min at the same thermal shearing temperature under a centrifugal force of 4390 Xg, and collecting precipitates, namely the short straight chain starch with specific chain length distribution.
(4) And (3) reconfiguring the precipitate obtained in the step (3) into a starch dispersion liquid, and repeating the thermal shearing and thermal centrifuging treatment of the steps (2) and (3) for three times, wherein the temperature is 100 ℃, 110 ℃ and 120 ℃ in sequence, and the corresponding centrifugal force is 2809 Xg, 1580 Xg and 702 Xg in sequence. Amylose having a specific chain length distribution can be further obtained. The four groups of starch precipitates separated have branching degrees of 7.12%, 4.83%, 4.39% and 4.29% in sequence, amylose contents of 52.11%, 61.13%, 62.23% and 63.37% in sequence, and average polymerization degrees of 24.94, 28.17, 29.62 and 30.81 in sequence. This shows that the screening can be carried out by the aggregation behavior of the short-term retrogradation of starch and the difference of the thermal stability of the aggregates, and the branching degree is gradually reduced and the amylose content and the average polymerization degree are gradually increased with the gradual increase of the treatment temperature. Thus, thermal shear and thermal centrifugation temperatures are key to the preparation of short amylose starches of a specific chain length distribution, thereby selecting amylose components with progressively increasing average chain length.
Example 6
(1) Cooling debranched starch paste which is debranched by debranching enzyme and inactivated to 20 ℃ for sufficient regeneration for 1h, centrifuging at 5000 Xg for 10min, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 15% (w/v) starch dispersion liquid, and carrying out thermal shearing treatment for 30min in a constant-temperature water bath at the rotating speed of 350r/min and at the temperature of 110 ℃;
(3) centrifuging the starch dispersion liquid obtained in the step (2) at the same thermal shearing temperature under a centrifugal force of 4390 Xg for 10min, and collecting supernatant and precipitate, wherein the precipitate is short straight chain starch with a specific chain length distribution.
(4) And (3) cooling the supernatant obtained in the step (3) to 20 ℃, fully regenerating for 1h, reconfiguring into a starch dispersion liquid, and repeating the thermal shearing and thermal centrifuging treatments in the steps (2) and (3) three times, wherein the temperature is 100 ℃, 90 ℃ and 80 ℃ in sequence, and the corresponding centrifugal force is 2809 Xg, 1580 Xg and 702 Xg in sequence. Collecting the precipitate to obtain starch component with specific chain length distribution.
The four groups of starch precipitates separated had a branching degree of 7.56%, 9.23%, 10.56% and 12.68% in this order, an amylose content of 41.17%, 36.03%, 28.53% and 18.32% in this order, and an average degree of polymerization of 24.15, 22.87, 20.13 and 19.51 in this order. This indicates that the screening can be carried out by the aggregation behavior of the short-term retrogradation of starch and the difference of the thermal stability of the aggregates, and the branching degree is gradually increased and the amylose content and the average polymerization degree are gradually decreased with the gradual decrease of the treatment temperature. Therefore, the thermal shear and the thermal centrifugation temperature are key to the preparation of short amylose starch with a specific chain length distribution, thereby screening amylose components with gradually reduced average chain length and gradually increased branching degree.
It should be understood that the above-described embodiments of the present invention are only examples for clearly illustrating the present invention, and are not to be construed as limiting the present invention; any modification, replacement, combination, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method for preparing amylose with different chain lengths is characterized by comprising the following steps:
(1) debranching the gelatinized starch by using debranching enzyme, cooling the obtained debranched starch paste to fully regenerate, performing centrifugal treatment, and removing supernatant to obtain starch precipitate;
(2) preparing the starch precipitate obtained in the step (1) into 10-20% (w/v) of starch dispersion liquid, and carrying out thermal shearing treatment at 80-120 ℃;
(3) and (3) carrying out thermal centrifugation treatment on the starch dispersion liquid subjected to thermal shearing treatment obtained in the step (2) at the same thermal shearing temperature, and respectively collecting supernatant and precipitate to obtain the amylose with the specific chain length distribution.
2. The method of claim 1, further comprising the step (4) of progressive screening i: and (3) repeating the thermal shearing and thermal centrifuging treatment of the step (2) and the step (3) at least once on the precipitate obtained in the step (3), and collecting the precipitate, namely further obtaining the amylose with the specific chain length distribution.
3. The method of claim 1, further comprising the step (4) of progressive screening ii: and (3) cooling the supernatant obtained in the step (3) to sufficiently regenerate, repeating the thermal shearing and thermal centrifuging treatment of the steps (2) and (3) at least once, and collecting precipitates, namely further obtaining the amylose with the specific chain length distribution.
4. The method according to any one of claims 1 to 3, wherein the thermal shearing temperature in step (3) and the progressive screening I is increased successively, and the thermal shearing temperature in step (3) and the progressive screening II is decreased successively.
5. The method according to claim 4, wherein the thermal shearing treatment is a shearing treatment of the starch milk with a heating process at a rotation speed of 350 ± 50r/min for 30 ± 10 min.
6. The method according to any one of claims 1 to 3, wherein the centrifugal force of the centrifugal treatment in the steps (1), (3) and (4) is gradually reduced.
7. The method as claimed in claim 6, wherein the centrifugal force of the centrifugation in steps (1) (3) (4) is 5000-500 Xg, and the centrifugation time is 10 + -5 min.
8. A method according to any one of claims 1 to 3, wherein the starch paste of step (1) and the supernatant of step (4) and step II are cooled to below 20 ℃ for 1 hour.
9. The method according to any one of claims 1 to 3, wherein the debranched starch paste of step (1) is prepared by: adding water into starch to prepare 5-20% starch milk, and heating for gelatinization; and then, reducing the temperature of the starch paste to an appropriate enzyme temperature, adjusting the pH value, and adding pullulanase for enzymolysis to obtain the debranched starch paste.
10. The method of claim 9, wherein the starch is potato starch, corn starch, soy starch, wheat starch.
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