CN111041055A - Method for preparing arrowhead resistant starch by using ultrasound in cooperation with pullulanase - Google Patents
Method for preparing arrowhead resistant starch by using ultrasound in cooperation with pullulanase Download PDFInfo
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Abstract
The invention discloses a method for preparing arrowhead resistant starch by using ultrasound in cooperation with pullulanase, and belongs to the technical field of preparation of resistant starch. The method comprises the following steps: (1) cleaning and finishing arrowheads; (2) extracting arrowhead starch; (3) preparing resistant starch; (4) and (4) carrying out enzymolysis in an ultrasonic field, and freeze-drying to obtain the arrowhead resistant starch. The invention accelerates the movement of solvent molecules by the cavitation action and the mechanical vibration action of ultrasonic waves and improves the extraction rate of target products. In the preparation process of the arrowhead resistant starch by the pullulanase method, a multi-mode ultrasonic treatment technology is used. The enzymolysis of pullulanase is promoted by ultrasonic, so as to solve the problems of low enzymolysis reaction efficiency and the like in the process of preparing resistant starch by an enzyme method. The arrowhead resistant starch is prepared by taking arrowhead starch as a raw material, and the arrowhead resistant starch has multiple physiological functions and good food processing characteristics, so that the comprehensive utilization of the arrowhead is facilitated, and the additional value of the arrowhead is improved.
Description
Technical Field
The invention relates to the technical field of food processing, in particular to arrowhead resistant starch prepared by using arrowhead starch as a raw material and adopting ultrasonic synergistic pullulan enzymatic treatment.
Background
The arrowhead is a perennial root shallow water herbaceous plant of the genus arrowhead of the family alismatis, is an important aquatic vegetable in China, is planted in all parts of China, is mainly distributed in Yangtze river basin and south provinces thereof, and has a cultivation area of 20000hm every year2Left and right. Arrowhead, as a seasonal vegetable with high moisture content, is not easy to store. At present, the arrowhead is generally directly eaten as the vegetable, and the processing is little. The arrowhead has slight bitter taste and low market price, so the deep processing of the arrowhead plays an important role in improving the economic value and the market competitiveness of the arrowhead. Arrowhead is a low fat, high carbohydrate food product with a starch content of about 50% of dry matter in arrowhead. Wherein, the amylose starch accounts for 30.10 percent and is a good raw material for preparing resistant starch.
In recent years, health concerns have led to the development of resistant starch as a new research target. Resistant Starch (RS) is defined as a Starch that is not absorbed in the small intestine of a healthy human body, but is fermented in the large intestine by the microflora. Resistant starch has multiple physiological functions: the resistant starch is involved in blood sugar regulation, weight control, lipid metabolism, gastrointestinal diseases alleviation, mineral substance and vitamin absorption promotion, and the like. The resistant starch has good physicochemical properties for food processing. The resistant starch is white powder, has no peculiar smell, and does not influence the sensory evaluation of food after being added in a proper amount, so the resistant starch has wide application in the food industry. The resistant starch has good heat resistance and higher gelatinization temperature, and is convenient to popularize in food processing; the resistant starch has weak water holding capacity, is suitable for being added into low-humidity baked food, and is easy to control in production; the resistant starch can be used as a substrate for probiotic propagation and a thallus preservative, can promote the growth of probiotics and ensure proper quantity; the resistant starch has excellent physiological functions, is in health-care food, and is widely used for development of health-care food.
Resistant starches fall into four categories: physically embedded starch (RS1), resistant starch granules (RS2), retrograded starch (RS3) and chemically modified starch (RS 4). After RS1 and RS2 are heated and gelatinized, the structure is easy to break, so that the resistance to amylase disappears, and the amylase is difficult to be used in the actual production process. Both RS3 and RS4 can be prepared in large quantities by processing raw starch, but chemical reagents added during the preparation of RS4 will affect food safety. The retrogradation resistant starch RS3 is formed by recrystallization in the cooling process after starch gelatinization, and has the greatest development prospect because the food safety problem cannot be caused and the preparation process is easy to control.
The preparation method of RS3 mainly comprises a biochemical method and a physical method, the common biochemical method comprises an acid debranching method and an enzyme debranching method, the physical method comprises a heat treatment method, an extrusion treatment method, a microwave radiation method and an ultrasonic treatment, the chemical modification is rapid and simple, but not environment-friendly generally, and chemical residues are easily generated in products, the enzymes are sensitive to temperature, pressure, pH and salt ions, and the enzyme treatment is difficult to control generally, debranching by the enzyme method usually adopts debranching enzymes such as pullulanase and isoamylase, currently, pullulanase is commonly used as debranching enzyme, and is also one of isoamylase, and the debranching by the enzyme method can hydrolyze α -1 and 6 glycosidic bonds in pullulan, amylopectin and purple potato polysaccharide in an inscribed mode, but the enzymolysis time is long, the related research shows that the yield and the efficiency of resistant starch prepared by the enzyme method independently using the physical or biochemical method are low, the research on the yield and the yield of resistant starch prepared by the enzyme method is low, the research on the enzymatic hydrolysis of cassava starch prepared by a modern starch processing technology that the resistant starch is added to the yield of Bacillus amylovorans, the starch prepared by a modern enzymic processing technology that the resistant starch is the resistant starch treated by a proteinase, the guava starch, the resistant starch prepared by a modern enzymic method of a modern royal jelly, the resistant starch production technology that the resistant starch production of a modern royal jelly production and the resistant starch production of a modern royal jelly production technology that the resistant starch is increased to the resistant starch production of a sour potato production of a modern royal jelly production, the resistant starch production of a royal jelly production, the resistant starch.
Ultrasound is a physical treatment at frequencies above the human hearing threshold. In recent years, ultrasound has attracted a wide interest in food-based research and commercial applications. Ultrasonic treatment has shown beneficial effects in food processing and preservation, including higher product yield, reduced processing time, reduced operating and maintenance costs, improved quality, reduced pathogens, and the like. Ultrasound not only improves the quality and safety of food products, but also provides opportunities for creating new products with unique properties. The application of ultrasonic waves in starch systems is mostly liquid-solid two-phase systems with water as a medium. The sonic energy of the ultrasonic waves is not absorbed by the molecules and is thus converted. Chemically usable forms are achieved by cavitation phenomena. Ultrasonic cavitation is generated in the solution by ultrasonic waves to generate micro-bubbles, and when the micro-bubbles are broken, high energy is released and converted into high pressure and high temperature to generate physical and chemical effects. Physical effects include intense microjets, shear forces and shock waves from bubble collapse, and acoustic streaming. The chemical effect is caused by radicals such as hydroxide (OH) and hydrogen (H) radicals generated by the decomposition of water molecules in cavitation caused by bubble collapse. Cavitation effects produce localized intense shear, high temperature, free radicals, reduce the viscosity of the starch paste and break the C-C bonds in the starch molecules.
The use of physical and biochemical methods has been to reduce the viscosity of gelatinized starch systems, increase the amylose ratio, and increase the concentration of starch chains with suitable chain length in the systems, therefore, in the actual production process, physical and biochemical methods are often combined to improve the production efficiency of resistant starch, studies have shown that ultrasonic wave combined enzymatic methods are more favorable for improving the yield of resistant starch than enzymatic methods for preparing resistant starch, and shorten the time for enzymatic hydrolysis, Hu finds that ultrasonic water bath and α -amylase simultaneously act on mung bean starch, and are easier for starch retrogradation (Hu AJ, Li Q, Zheng J, Yang Land Qin ZP, Study on structure of hydrolytic and tapioca starch slurry, center Oils 1: 13-15 (2012), Lu et al found that synergistic effect of blue enzyme and ultrasonic Debranching process produces synergistic effect, increase the linear and linear chain length in preparation, and increase the yield of starch produced by ultrasonic wave hydrolysis, SDS-3. the synergistic effect of ultrasonic wave hydrolysis of starch produced by biochemical method is reported by biochemical method, and the method for preparing starch hydrolysate starch.
The invention introduces an advanced multi-mode ultrasonic technology, hopes that the ultrasonic wave and pullulanase cooperate to carry out hydrolysis on arrowhead starch molecules, the starch molecules are degraded and enzymolyzed in the treatment process, the ultrasonic wave can promote the enzymolysis reaction while degrading the starch, so as to solve the problems of low enzymolysis reaction efficiency, long enzymolysis time, large enzyme consumption and the like in the process of preparing the resistant starch by the enzyme method and improve the yield of the arrowhead resistant starch.
Disclosure of Invention
In order to solve the problems, on the basis of preparing the arrowhead resistant starch by the pullulanase method, the arrowhead starch is processed by the ultrasonic synergistic enzyme method, and the influence on the yield of the arrowhead resistant starch is researched.
The method for preparing arrowhead resistant starch by using ultrasound and pullulanase provided by the invention comprises the following steps:
(1) cleaning fresh rhizoma Sagittariae Sagittifoliae, peeling, removing tail, cutting into blocks, and weighing. Adding distilled water with the same volume at 4 ℃, pulping in a juicer, sequentially filtering the beaten pulp through a sample sieve (200 mesh sieve → 300 mesh sieve), and removing fibers;
(2) standing the filtrate in a beaker overnight, removing supernatant, eluting precipitate with 0.2% NaOH solution to remove protein, adjusting pH to 7 with 0.1mol/L hydrochloric acid solution, centrifuging in a 250ml centrifuge cup, discarding supernatant, scraping off non-white impurities on the surface of the residual solid, and repeatedly washing with deionized water until all impurities are removed;
(3) oven drying at 50 deg.C, pulverizing, sieving with 100 mesh sieve to obtain arrowhead starch, packaging, and storing in a drier.
(4) Accurately weighing arrowhead starch in a conical flask to prepare a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(5) Placing in a 50 deg.C constant temperature water bath, adjusting pH to 5.0 with 0.05mol/L HCl solution, adding pullulanase, performing debranching treatment under ultrasonic treatment to obtain Sagittaria sagittifolia resistant starch, and performing enzymolysis in 50 deg.C water bath.
(6) Cooling to room temperature, pouring the sample into a culture dish, aging at 4 ℃ for 24h, freeze-drying for 48h, grinding, packaging, and storing in a dryer.
Wherein the pullulanase in the step (5) is added in an amount of 6npun/g (starch) -58npun/g (starch); the enzyme is preferably added in an amount of 32npun/g (starch).
Wherein the enzymolysis time of the pullulanase in the step (5) is 8-40 h; the enzymolysis time is preferably 24 h.
Wherein the specific parameters of the ultrasonic action in the step (5) are ultrasonic time of 5min-40min, preferably ultrasonic time of 10 min; the ultrasonic power is 60W-300W, and the preferable ultrasonic power is 240W; ultrasonic frequencies 20kHz, 40kHz, 60kHz, 20/60kHz, 40/60kHz, preferably ultrasonic frequencies 60 kHz; the ultrasonic intermittent ratio is 1:8 (ultrasonic 5-40s, intermittent 5 s); preferably, the ultrasonic pause ratio is 20s/5 s.
The invention has the beneficial effects that:
(1) the physical method used in the present invention is ultrasonic treatment. Ultrasonic treatment has shown beneficial effects in food processing and preservation, including higher product yield, shortened processing time, reduced operating and maintenance costs, etc., and is a novel physical method for starch modification.
(2) In the preparation process of the arrowhead resistant starch by the pullulanase method, a multi-mode ultrasonic treatment technology is used. The enzymolysis of pullulanase is promoted by ultrasonic, so as to solve the problems of low enzymolysis reaction efficiency and the like in the process of preparing resistant starch by an enzyme method.
(3) The arrowhead resistant starch is prepared by taking arrowhead starch as a raw material, and the arrowhead resistant starch has multiple physiological functions and good food processing characteristics, so that the comprehensive utilization of the arrowhead is facilitated, and the additional value of the arrowhead resistant starch is improved.
Drawings
FIG. 1 is a structural diagram of a multi-mode ultrasonic biological treatment device of the present invention, wherein 1, 2, 3 are ultrasonic vibration plates, 4 is a liquid container, 5 is a water bath, 6 is a temperature probe, 7 is a circulating pump, 8 is a computer program controller, and 9, 10, 11 are ultrasonic controllers.
Fig. 2 is an XRD diffraction pattern of arrowhead-resistant starch, in which X-ray diffraction patterns of three samples, namely, arrowhead-resistant starch (CS) prepared with ultrasonic assistance, arrowhead-resistant starch (WCS) prepared without ultrasonic assistance and native starch (YDF), are shown from top to bottom, respectively.
Fig. 3 is a scanning electron micrograph of three samples of native starch (YDF), arrowhead resistant starch (WCS) prepared without ultrasonic assistance, and arrowhead resistant starch (CS) prepared with ultrasonic assistance, a: YDF x 1000; b: YDF x 8000; c: WCS x 1000; d: WCSx 8000; e: CS x 1000; f: CS x 8000.
Detailed Description
Terms used in the present invention have meanings commonly understood by those of ordinary skill in the art unless otherwise specified. The present invention is described in further detail below with reference to specific examples and with reference to the data. It will be understood that these examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way.
FIG. 1 is a schematic diagram of a multi-mode ultrasonic biological treatment apparatus of the present invention, which is equipped with a computer program controller 8, and can set ultrasonic working parameters (ultrasonic power density, frequency, pulse working time, intermittent time and total treatment time) to control three ultrasonic controllers 9, 10 and 11, respectively, and connect three ultrasonic vibration plates 1, 2 and 3 with different frequencies, respectively, to realize single frequency/two frequencies/three frequencies ultrasonic treatment; putting the solution to be processed into the liquid container 4 for single-frequency/dual-frequency/multi-frequency ultrasonic processing, and starting the circulating pump 7 to circulate the solution. The automatic control of the solution temperature is realized through the water bath 5 and the temperature probe 6.
Experimental materials: arrowhead purchased from Kaiyuan tourist supermarket of Jiangsu university
Pullulanase was purchased from Sigma, USA (enzyme activity: 1000npun/ml)
The arrowhead starch is extracted from arrowheads and comprises the following components:
(1) fresh arrowheads were cleaned, peeled, tail removed and cut into pieces and weighed (ca. 5000 g). Adding distilled water with the same volume at 4 ℃, pulping in a juicer, sequentially filtering the beaten pulp through a sample sieve (200 mesh sieve → 300 mesh sieve), and removing fibers;
(2) standing the filtrate in a beaker overnight, removing supernatant, eluting precipitate with 0.2% NaOH solution to remove protein, adjusting pH to 7 with 0.1mol/L hydrochloric acid solution, centrifuging in a 250ml centrifuge cup, discarding supernatant, scraping off non-white impurities on the surface of the residual solid, and repeatedly washing with deionized water until all impurities are removed;
(3) drying at 50 deg.C, pulverizing, sieving with 100 mesh sieve to obtain arrowhead starch, packaging, and storing in a drier to obtain dried arrowhead starch 300g, which is native starch (YDF).
Example 1: screening of additive amount of pulullan enzyme for preparing arrowhead resistant starch by using pulullan enzyme method
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask to prepare a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 deg.C constant temperature water bath kettle, adjusting pH with 0.05mol/L HCl solution, adding pullulanase (the addition amount is shown in Table 1), and performing debranching treatment for 24 hr under 50 deg.C water bath condition.
(3) Cooling to room temperature, pouring the sample into a culture dish, aging at 4 ℃ for 24h, freeze-drying for 48h, grinding, packaging, and storing in a dryer. The content of the arrowhead resistant starch is determined by referring to the national standard NY-T2638-2014.
The yield of the arrowhead resistant starch is shown in table 1, the yield of the resistant starch shows a trend that the yield is increased firstly and then stabilized with the increase of the addition amount of the pullulanase, and when the addition amount of the pullulanase is 32npun/g (starch), the addition amount of the enzyme is continuously increased, the yield of the resistant starch is kept stable, and the change is not obvious. The enzyme addition was chosen to be 32npun/g (starch) and the yield of resistant starch was 21.36% (16% increase in resistant starch content compared to arrowhead starch) for subsequent screening of experimental conditions.
Table 1: influence of different enzyme addition amounts on yield of arrowhead resistant starch
| Enzyme addition (npun/g (starch)) | 0 | 6 | 19 | 32 | 45 | 58 |
| Resistant starch yield (%) | 5.36 | 16.42 | 20.32 | 21.36 | 21.47 | 22.24 |
Example 2: screening of enzymolysis time for preparing arrowhead resistant starch by pullulanase method
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask to prepare a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 ℃ constant temperature water bath kettle, adjusting the pH value with 0.05mol/L HCl solution, adding 32npun/g (starch) of pullulanase, and carrying out debranching treatment under the condition of 50 ℃ water bath, wherein the enzymolysis time is shown in Table 2.
(3) Cooling to room temperature, pouring the sample into a culture dish, aging at 4 ℃ for 24h, freeze-drying for 48h, grinding, packaging, and storing in a dryer. The content of the arrowhead resistant starch is determined by referring to the national standard NY-T2638-2014.
The yield of the arrowhead resistant starch is shown in table 2, the yield of the resistant starch tends to increase firstly and then stabilize with the increase of the enzymolysis time of the pullulanase, and the enzymolysis time is continuously increased when the pullulanase is subjected to enzymolysis for 24 hours, so that the yield of the resistant starch is kept stable and does not change remarkably. The enzymolysis time is 24h, the yield of the resistant starch is 21.29% (compared with arrowhead starch, the content of the resistant starch is improved by 15.93%) and the resistant starch is used for screening subsequent test conditions.
Table 2: influence of different enzymolysis time on yield of arrowhead resistant starch
| Time of enzymolysis (h) | 0 | 8 | 16 | 24 | 32 | 40 |
| Resistant starch yield (%) | 5.36 | 18.89 | 20.15 | 21.29 | 21.96 | 22.10 |
Example 3: screening of ultrasonic time for preparing arrowhead resistant starch by ultrasonic-pullulanase method
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask, preparing a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 deg.C constant temperature water bath kettle, adjusting pH to 5.0 with 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), debranching under the action of ultrasound, maintaining 50 deg.C water bath condition, and continuing enzymolysis for 24 hr. Wherein the ultrasonic frequency (60KHZ), the ultrasonic period is 30s/5s, the ultrasonic power is 180w, and the ultrasonic time is shown in Table 3.
(3) Cooling to room temperature, aging at 4 deg.C for 24 hr, freeze drying for 48 hr, grinding, packaging, and storing in desiccator. Determining the content of arrowhead resistant starch by referring to national standard NY-T2638-2014
The yield of the arrowhead resistant starch is shown in the table 3, and the yield of the resistant starch tends to increase and then decrease along with the increase of the ultrasonic time. When the ultrasonic time is 10min, the yield of the arrowhead resistant starch is up to 23.89% (compared with the pullulanase treatment, the content of the resistant starch is improved by 2.6%), and the ultrasonic time is 10min for screening the subsequent test conditions.
Table 3: effect of different sonication times on yield of arrowhead resistant starch
| Ultrasonic time (min) | 0 | 5 | 10 | 20 | 30 | 40 |
| Resistant starch yield (%) | 21.29 | 21.94 | 23.89 | 22.87 | 22.46 | 20.85 |
Example 4: screening of ultrasonic power for preparing arrowhead resistant starch by ultrasonic-pullulanase method
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask, preparing a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 deg.C constant temperature water bath kettle, adjusting pH to 5.0 with 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), debranching under the action of ultrasound, maintaining 50 deg.C water bath condition, and continuing enzymolysis for 24 hr. Wherein the ultrasonic frequency (60kHz), the ultrasonic period is 30s/5s, the ultrasonic time is 10min, and the ultrasonic power is shown in Table 3.
(3) Cooling to room temperature, aging at 4 deg.C for 24 hr, freeze drying for 48 hr, grinding, packaging, and storing in desiccator. Determining the content of arrowhead resistant starch by referring to national standard NY-T2638-2014
The yield of the arrowhead resistant starch is shown in the table 4, and the yield of the resistant starch tends to increase and then decrease with the increase of the ultrasonic power. When the ultrasonic power is 240W, the yield of the arrowhead resistant starch is 24.94% at most (compared with the pullulanase treatment, the content of the resistant starch is improved by 3.65%), and the ultrasonic power is 240W for screening subsequent test conditions.
Table 4: influence of different ultrasonic powers on yield of arrowhead resistant starch
| Ultrasonic power W | 0 | 60 | 120 | 180 | 240 | 300 |
| Yield of resistant starch% | 21.29 | 21.41 | 22.27 | 23.20 | 24.94 | 22.47 |
Example 5: ultrasonic frequency screening for preparing arrowhead resistant starch by ultrasonic-pullulanase method
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask, preparing a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Putting the mixture into a 50 ℃ constant-temperature water bath kettle, adjusting the pH value to 5.0 by using 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), carrying out debranching treatment under the action of ultrasonic waves, keeping the 50 ℃ water bath condition, and continuing enzymolysis for 24 hours, wherein the ultrasonic power (240w), the ultrasonic period is 30s/5s, the ultrasonic time is 10min, and the ultrasonic frequency is shown in a table 5.
(3) Cooling to room temperature, aging at 4 deg.C for 24 hr, freeze drying for 48 hr, grinding, packaging, and storing in desiccator. Determining the content of arrowhead resistant starch by referring to national standard NY-T2638-2014
The yield of the arrowhead resistant starch is shown in the table 5, and the yield of the resistant starch tends to increase and then decrease along with the increase of the ultrasonic time. When the ultrasonic frequency is 60kHz, the yield of the arrowhead resistant starch is up to 23.89% (compared with the pullulanase treatment, the content of the resistant starch is improved by 2.2%), and the ultrasonic frequency is 60kHz and is used for screening subsequent test conditions.
Table 5: effect of different ultrasonic frequencies on the yield of arrowhead resistant starch
| Ultrasonic frequency (kHz) | 0 | 20 | 40 | 60 | 20/60 | 40/60 |
| Resistant starch yield (%) | 21.29 | 22.14 | 23.09 | 23.49 | 22.50 | 21.62 |
Example 6: screening of ultrasonic intermittent ratio for preparing arrowhead resistant starch by ultrasonic-synergistic pullulanase method
The ultrasonic pause ratio experimental parameters are shown in Table 6.
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask, preparing a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 ℃ constant temperature water bath kettle, adjusting the pH value to 5.0 by using 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), carrying out debranching treatment under the action of ultrasonic waves, keeping the 50 ℃ water bath condition, and continuing enzymolysis for 24 hours, wherein the ultrasonic power is 240W, the ultrasonic frequency is 60kHz, the ultrasonic time is 10min, and the ultrasonic intermittence ratio is shown in Table 6.
(3) Cooling to room temperature, aging at 4 deg.C for 24 hr, freeze drying for 48 hr, grinding, packaging, and storing in desiccator. Determining the content of arrowhead resistant starch by referring to national standard NY-T2638-2014
The yield of the arrowhead resistant starch is shown in the table 6, and the yield of the resistant starch tends to increase and then decrease along with the increase of the ultrasonic intermittent ratio. When the ultrasonic intermittent ratio is 20s/5s, the yield of the arrowhead resistant starch is 25.80% at most (compared with the pullulanase treatment, the content of the resistant starch is improved by 4.51%), and the ultrasonic frequency is 60kHz for screening subsequent test conditions.
Table 6: influence of different ultrasonic intermittent ratios on yield of arrowhead resistant starch
| Ultrasonic intermittent ratio (s/5s) | 0 | 5 | 10 | 20 | 30 | 40 |
| Resistant starch yield (%) | 21.29 | 21.88 | 22.93 | 25.80 | 22.62 | 21.95 |
Experimental example Structure characterization and characterization of Sagittaria sagittifolia resistant starch
A, sample preparation: arrowhead resistant starch (CS) prepared with ultrasound assistance
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask to prepare a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 ℃ constant-temperature water bath kettle, adjusting the pH value to 5.0 by using 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), carrying out debranching treatment under the action of ultrasound, keeping 50 ℃ water bath condition, and continuing enzymolysis for 24 hours, wherein the ultrasound-assisted enzymolysis condition is as follows: the ultrasonic time is 10min, the ultrasonic power is 240W, the ultrasonic frequency is 60KHZ, and the ultrasonic intermittent ratio is 20s/5 s.
(3) Cooling to room temperature, pouring the sample into a culture dish, aging at 4 ℃ for 24h, freeze-drying for 48h, grinding, packaging, and storing in a dryer. The content of the arrowhead resistant starch is determined by referring to the national standard NY-T2638-2014. The content of resistant starch was 25.8%. The sample was used for subsequent structural characterization and characterization.
B, sample preparation: arrowhead resistant starch (WCS) without ultrasound-assisted preparation
(1) Accurately weighing 2g of arrowhead starch in a 100ml conical flask to prepare a starch suspension (4 percent, m/m), and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min.
(2) Placing in a 50 deg.C constant temperature water bath kettle, adjusting pH to 5.0 with 0.05mol/LHCl solution, adding pullulanase 32npun/g (starch), maintaining 50 deg.C water bath condition, and performing enzymolysis for 24 hr. (without sonication)
(3) Cooling to room temperature, pouring the sample into a culture dish, aging at 4 ℃ for 24h, freeze-drying for 48h, grinding, packaging, and storing in a dryer. The content of the arrowhead resistant starch is determined by referring to the national standard NY-T2638-2014. The content of resistant starch was 21.29%. The sample was used for subsequent structural characterization and characterization.
Wherein the three samples of the arrowhead-resistant starch (CS) prepared with ultrasonic assistance, the arrowhead-resistant starch (WCS) prepared without ultrasonic assistance and the raw starch (YDF) in fig. 2-3 and in tables 7-8 refer to samples prepared by the different methods described above.
(1) Analysis of thermal Properties
The experimental conditions are as follows: accurately weighing 2.5mg of starch sample in an aluminum sample plate by a ten-thousandth balance, adding 7.5 microliters of deionized water, sealing the sample plate, then balancing at room temperature for 1h, placing the sample plate in a sample seat in an instrument, and using a sealed empty aluminum box as a reference object. Scanning range: 30-150 ℃; scanning rate: 10 ℃/min; atmosphere: high purity nitrogen, flow: 40 mL/min; the scans were recorded and the start temperature To, peak temperature Tp, end temperature Tc and range temperature Tr on the endothermic curve were calculated.
Thermal Property (DSC) gelatinization parameters are determined by the molecular structure of amylopectin, the ratio of amylose to amylopectin,The ratio of crystalline to amorphous states or a combination thereof. This study measured DSC curves for three samples of native starch (YDF), arrowhead resistant starch (WCS) prepared without ultrasound assistance, and arrowhead resistant starch (CS) prepared with ultrasound assistance, where the T of the YDF, WCS and CS starches0(initial gelatinization temperature), TP(Peak gelatinization temperature), TC(temperature for terminating gelatinization), TC-T0The (transition temperature range) and Δ H (gelatinization enthalpy) are shown in table 7. The gelatinization temperature reflects the stability of the crystals. T is0The melting temperature of the weakest crystals in the starch granules, TCIt is associated with a melting temperature of high perfect crystallization. As can be seen from Table 7, for T0、TCChange of (YDF)>CS>And WCS. During the process of processing starch samples by WCS and CS, original crystallization is damaged, too short linear molecules are generated, and retrogradation forms a crystal structure with low stability. T of sonicated starch samplesC-T0At a minimum, WCS treated starch samples were inferior. The transition temperature is influenced by the molecular structure of the crystalline region. T isC-T0The value is reduced, the diversity of RS3 crystal is reduced, and the perfection of the helical ordered structure is improved. The reduction in the transition temperature range of the treated starch sample indicates an increase in its homogeneity and intact crystallites. This increased crystallite perfection is responsible for the increased resistance of the starch to digestion. The enthalpy of gelatinization (Δ H) reflects mainly the loss of the order of the double helix in the starch granule rather than the loss of crystallization. Starches containing high amounts of amylose require more energy to break the intermolecular bonds in the crystalline regions. In contrast, amylopectin is generally distributed in amorphous regions, and its crystals have a small size and are easily melted. Δ hmax for CS treated starch samples, next to WCS treated starch samples. In the WCS and CS sample processing process, the content of linear starch with proper chain length is increased, a double-helix structure is favorably formed, and delta H is increased. The increase in Δ H can be explained by the increased order and stability of the double helix structure through hydrogen bonding and other intermolecular forces. The phase transition temperature and the enthalpy of endotherm increase with increasing crystallinity and stability of the double helix structure. T of CS-treated sample0、TP、TCAnd increase in Δ H and TC-T0Compared to the WCS-treated sampleProduct, the perfection of the sample crystals treated with CS is higher.
TABLE 7 DSC parameters of arrowhead-resistant starch
(2) X-ray diffraction analysis
The experimental conditions are as follows: x-ray diffraction measurement conditions: selecting a Cu target as a characteristic ray; measuring the angle range of 5-30 degrees; the scanning speed is 5 DEG/min. The sample moisture content differences did not affect the X-ray diffraction pattern.
XRD is more sensitive to the long-term crystalline structure of starch granules consisting of repeating double helical units. The X-ray diffraction pattern may depend on the source of the starch as well as the environmental growth and processing conditions. According to XRD patterns, starch crystals can be currently classified into types A, B and C. Type A crystal structures are composed of short chains, usually present in cereal starches, while fruit and tuber starches are type B structures, composed of long chains. Type C crystal structures are a combination of type a and type B structures and are typically present in legume starches. The X-ray diffraction patterns and relative crystallinities of the three samples native starch (YDF), arrowhead resistant starch (WCS) prepared without ultrasound assistance and arrowhead resistant starch (CS) prepared with ultrasound assistance are shown in fig. 2 and table 8. The XRD diffractogram of YDF shows diffraction peaks at diffraction angles of 15 °, 17 °, 18 ° and 23 °, and is typical of a-type crystals. The WCS and CS treatments significantly changed the diffraction pattern of the sample, with diffraction peaks at diffraction angles 15, 17, 19, 22 and 24, and the crystal type changed from form A to form B. Glutinous rice starch paste (10%, w/w) was debranched with pullulanase and then retrograded at 25 ℃ to obtain short-chain amylose crystals having a B-type X-ray pattern. Differences in the crystallinity of the starch samples can be attributed to several aspects: crystal size, number of crystalline domains (influenced by amylopectin content and length of amylopectin), and orientation of the double helix within the crystalline domains. The degree of interaction of the double helix. The structure of starch molecules is divided into a microcrystalline region, a sub-crystalline region and an amorphous region. The relative crystallinity is defined as the ratio of the area of the crystalline region to the area of the crystalline region plus the microcrystalline region. The relative crystallinity reflects the proportion of dense crystalline regions. The crystalline region is difficult to hydrolyze by enzymes. Thus, the relative crystallinity can be used to measure the resistance of starch. The higher the relative crystallinity, the more resistant the starch is to enzymes. The relative crystallinity is the ratio of the crystalline area to the total diffraction area. As can be seen from the table, the relative crystallinities of the YDF, WCS and CS samples were 54.7%, 52.4% and 55.6%, respectively. The crystallinity of the WCS sample is reduced compared with that of the YDF sample, which shows that the interaction between double helices in the YDF crystallization area is stronger, and the experimental result is consistent with that reported in the literature, wherein the orientation of the crystal grains to the X-ray beam is better. The relative crystallinity of the CS samples was higher than the WCS and YDF samples, indicating that the double helix strands reoriented in a tighter manner, providing a more stable crystalline structure. The ultrasound and pullulanase act on arrowhead starch molecules, and the debranching degree of the arrowhead starch molecules is higher. Meanwhile, due to the cavitation effect of the ultrasonic waves, the broken chains are broken, the molecular chains are given higher arrangement and aggregation opportunities, and the molecular chains are recombined into double helix, so that a completely crystallized structure is formed. The increase in relative crystallinity may be due to increased bonding between starch chains and rearrangement of the disrupted double helix within the crystalline region, resulting in increased crystalline integrity or formation of new crystals. The level of crystallinity is consistently lower than that of the double helix, indicating that not all of the helically ordered starch molecules are arranged into crystals.
TABLE 8 XRD diffraction Pattern parameters of arrowhead resistant starch
(3) Scanning electron microscope
Scanning electron microscope analysis: fixing the double-sided adhesive tape on an objective table of a scanning electron microscope, dipping a little starch sample by using a toothpick, uniformly smearing the starch sample on the double-sided adhesive, and lightly pressing. Blowing off excessive starch by an ear washing ball, placing the objective table in a gold plating instrument, plating a gold film on a starch sample by an ion sputtering coating instrument, taking out the objective table after 20min, placing the objective table in a scanning electron microscope, and observing the granular form of the starch under different magnifications (1000 times and 8000 times).
Morphological characteristics of three samples, namely raw starch (YDF), arrowhead resistant starch (WCS) prepared without ultrasonic assistance and arrowhead resistant starch (CS) prepared with ultrasonic assistance, were observed through a Scanning Electron Microscope (SEM), and morphological characteristics of arrowhead starch samples of different treatment modes were analyzed, and the results are shown in FIG. 3. Scanning electron microscope images show the shape and surface microstructure of different samples. Scanning electron microscopy of YDF samples showed small particles of varying sizes, oval or irregular, smooth surfaces with some protrusions and depressions, possibly due to partial damage of the starch during the starch extraction and drying process. The morphology of the particles of the WCS and CS samples changed significantly. The granular structure of YDF is damaged, and the crystal grains are rough and irregular in appearance, dense in structure and different in size. The WCS, CS samples exhibited bulk, dense structures with increased particle size compared to YDF. Some debris was observed on the surface of the WCS, CS samples. The WCS sample surface had some shallow, layered stripes and grooves. The CS sample has a plurality of deep-layer-shaped strips and holes on the surface, and the strips and holes are in an irregular structure. The formation of voids of non-uniform size may be due to cavitation by ultrasound. The changes in surface structure due to the ultrasound action can be attributed to the formation of local hot spots when bubbles collapse, and to the shear forces created by micro-streaming and shock waves. The dense and rigid structure of starch has a high resistance to enzymes. Irregular sheet-like shapes may be formed by leaching of amylose, disruption of amylopectin crystalline regions, and rearrangement of starch chains. The apparent structure of the pea starch regenerated by autoclaving is similar to an irregular flaky cohesive structure, and the pea starch is uneven in size. Retrogradation after debranching and/or degradation of starch results in the conversion of disordered linear starch molecules into a double helix structure, rearrangement of the double helix which enhances the interaction between starch chains and dissociation, and arrangement of three-dimensional cohesive networks, with changes in short-and long-range ordered structures. This compact structure and large particle size may have low sensitivity to digestive enzymes.
Claims (4)
1. The method for preparing arrowhead resistant starch by using ultrasound and pullulanase is characterized by comprising the following steps of:
(1) cleaning fresh arrowheads, peeling, removing tails, cutting into blocks, and weighing; adding distilled water with the same volume, pulping in a juicer, and filtering the beaten pulp through a sample sieve in sequence to remove fibers;
(2) standing the filtrate in a beaker overnight, removing supernatant, eluting and precipitating with 0.2% NaOH solution to remove protein, adjusting pH to 7 with 0.1mol/L hydrochloric acid solution, centrifuging in a 250ml centrifuge, discarding supernatant, scraping off non-white impurities on the surface of the residual solid, and repeatedly cleaning with deionized water until all impurities are removed;
(3) oven drying at 50 deg.C, pulverizing, sieving with 100 mesh sieve to obtain arrowhead starch, packaging, and storing in a drier;
(4) accurately weighing arrowhead starch in a conical flask to prepare starch suspension with the mass concentration of 4%, and placing the starch suspension in an autoclave for high-temperature treatment at 121 ℃ for 20 min;
(5) placing in a 50 ℃ constant-temperature water bath kettle, adjusting pH value to 5.0 with 0.05mol/L HCl solution, adding pullulanase, performing debranching treatment under ultrasonic treatment to prepare arrowhead resistant starch, and performing enzymolysis under 50 ℃ water bath condition;
(6) cooling to room temperature, and drying to obtain the arrowhead resistant starch.
2. The method for preparing arrowhead-resistant starch by using the ultrasonic synergy pullulanase according to claim 1, wherein the pullulanase in the step (5) is added in an amount of 6npun/g (starch) to 58npun/g (starch); the enzyme is preferably added in an amount of 32npun/g (starch).
3. The method for preparing arrowhead-resistant starch by using the ultrasound and pullulanase of claim 1, wherein the pullulanase of the step (5) has an enzymolysis time of 8-40 h; the enzymolysis time is preferably 24 h.
4. The method for preparing arrowhead-resistant starch by using the ultrasound and pullulanase of claim 1, wherein the specific parameters of the ultrasound action in the step (5) are 5-40 min ultrasound time, preferably 10min ultrasound time; the ultrasonic power is 60W-300W, and the preferable ultrasonic power is 240W; ultrasonic frequencies 20kHz, 40kHz, 60kHz, 20/60kHz, 40/60kHz, preferably ultrasonic frequencies 60 kHz; the ultrasonic intermittent ratio is 1:8 (ultrasonic 5-40s, intermittent 5 s); preferably, the ultrasonic pause ratio is 20s/5 s.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112806574A (en) * | 2021-02-04 | 2021-05-18 | 齐鲁工业大学 | Preparation method of pea starch-emulsifier compound with high complexation index |
| CN112931853A (en) * | 2021-03-08 | 2021-06-11 | 徐州工程学院 | Edible fungus puffed food and preparation method thereof |
| WO2021114694A1 (en) * | 2019-12-12 | 2021-06-17 | 江苏大学 | Method for preparing arrowhead resistant starch by ultrasound synergistic pullulanase |
| CN113845600A (en) * | 2021-09-30 | 2021-12-28 | 上海理工大学 | Preparation method of high-amylose mung bean resistant starch |
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Families Citing this family (2)
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|---|---|---|---|---|
| JP7071582B2 (en) * | 2018-04-05 | 2022-05-19 | ペヒナッツ・トルステン | Freeze-drying system and methods for it |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2537542A1 (en) * | 2003-09-08 | 2005-03-24 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Resistant starch with cooking properties similar to untreated starch |
| CN102640903A (en) * | 2012-04-24 | 2012-08-22 | 江苏食品职业技术学院 | Production method of colored nutritional Sagittaria sagittifolia vermicelli |
| CN105001343A (en) * | 2015-07-24 | 2015-10-28 | 中国农业科学院农产品加工研究所 | High resistant starch (RS3) content product prepared through autoclaving treatment and enzymatic debranching and preparation method thereof |
| CN106418054A (en) * | 2016-11-30 | 2017-02-22 | 江苏大学 | Method for preparing natural arrowhead juice by frequency-sweeping pulsed ultrasound assisted bienzyme hydrolysis |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110923282A (en) * | 2019-12-12 | 2020-03-27 | 江苏大学 | Method for preparing resistant starch by using ultrasonic-assisted amylase |
| CN111041055A (en) * | 2019-12-12 | 2020-04-21 | 江苏大学 | Method for preparing arrowhead resistant starch by using ultrasound in cooperation with pullulanase |
| CN111235195A (en) * | 2020-01-20 | 2020-06-05 | 江苏大学 | Preparation method of ultrasonic wave synergistic biological enzyme of lotus root resistant starch |
-
2019
- 2019-12-12 CN CN201911271258.4A patent/CN111041055A/en active Pending
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2537542A1 (en) * | 2003-09-08 | 2005-03-24 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Resistant starch with cooking properties similar to untreated starch |
| CN102640903A (en) * | 2012-04-24 | 2012-08-22 | 江苏食品职业技术学院 | Production method of colored nutritional Sagittaria sagittifolia vermicelli |
| CN105001343A (en) * | 2015-07-24 | 2015-10-28 | 中国农业科学院农产品加工研究所 | High resistant starch (RS3) content product prepared through autoclaving treatment and enzymatic debranching and preparation method thereof |
| CN106418054A (en) * | 2016-11-30 | 2017-02-22 | 江苏大学 | Method for preparing natural arrowhead juice by frequency-sweeping pulsed ultrasound assisted bienzyme hydrolysis |
Non-Patent Citations (1)
| Title |
|---|
| 姚慧等: "响应面法优化板栗抗性淀粉制备工艺", 《中国粮油学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021114694A1 (en) * | 2019-12-12 | 2021-06-17 | 江苏大学 | Method for preparing arrowhead resistant starch by ultrasound synergistic pullulanase |
| CN112806574A (en) * | 2021-02-04 | 2021-05-18 | 齐鲁工业大学 | Preparation method of pea starch-emulsifier compound with high complexation index |
| CN112931853A (en) * | 2021-03-08 | 2021-06-11 | 徐州工程学院 | Edible fungus puffed food and preparation method thereof |
| CN113845600A (en) * | 2021-09-30 | 2021-12-28 | 上海理工大学 | Preparation method of high-amylose mung bean resistant starch |
| CN115462520A (en) * | 2022-08-29 | 2022-12-13 | 江苏大学 | Ultrasonic preparation of lotus root starch pickering emulsion and application of lotus root starch pickering emulsion as functional food |
| CN115462520B (en) * | 2022-08-29 | 2023-08-18 | 江苏大学 | Ultrasonic preparation of lotus root starch pickering emulsion and application of lotus root starch pickering emulsion as functional food |
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