CN113412903A - Ultrasonic preparation method of arrowhead RS5 type resistant starch and application of functional food - Google Patents
Ultrasonic preparation method of arrowhead RS5 type resistant starch and application of functional food Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
- A23L33/12—Fatty acids or derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/04—Extraction or purification
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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Abstract
The invention discloses an ultrasonic preparation method of arrowhead RS5 type resistant starch and application of functional food, belonging to the technical field of resistant starch preparation. The invention researches the influence of ultrasonic frequency on the performance and the structure of the arrowhead starch-linoleic acid compound and also researches the influence of ultrasonic time on the performance and the structure of the arrowhead starch-stearic acid compound. Measuring the large complexation index of the arrowhead starch-lipid complex and in-vitro digestion to observe the influence of ultrasound on the stability and the digestibility of the arrowhead RS5 type resistant starch; the particle morphology and the crystal structure type of the arrowhead RS5 resistant starch are observed by a scanning electron microscope, X-ray diffraction and Fourier transform infrared spectroscopy. The method provides a green physical processing mode for the preparation of the starch-lipid complex, has simple process and advanced technology, and has good prospect in the aspects of food processing and functional food application.
Description
Technical Field
The invention belongs to the technical field of preparation of resistant starch, and particularly relates to a preparation method of an arrowhead starch-lipid compound by ultrasonic waves.
Background
Sagittaria sagittifolia L, Sagittaria sagittifolia and castanea alba belong to the family Alismaceae herbaceous plants. The arrowhead is rich in carbohydrate, protein, fat, mineral and other nutrient substances. Has various medicinal values, and can cool blood, stop bleeding, relieve cough, treat stranguria, dissipate stagnation, detoxify and the like. Arrowhead starch is the main nutrient component in arrowhead, and accounts for about 50% of the dry weight of arrowhead, and the amylose content accounts for 30% of the starch. Therefore, the arrowhead can be used as a starch raw material for development and utilization.
The resistant starch is also called as resistant starch, which can not be digested and absorbed by stomach and small intestine of human body, but can be fermented into multiple Short Chain Fatty Acids (SCFAs) in colon by probiotics, has physiological functions similar to dietary fiber, and has effects of improving intestinal metabolism, preventing colon cancer, improving insulin resistance, reducing blood lipid, etc. Resistant starches can be divided into: RS1 (physically embedded starch), RS2 (resistant starch granules), RS3 (retrograded starch), RS4 (chemically modified starch), RS5 (starch-lipid complex). RS5 resistant starch is a complex of starch and fatty acid or fatty alcohol, and has very high thermal stability and is not easily digested in vivo. The preparation method of RS5 type resistant starch is generally divided into chemical method, physical method and genetic engineering method. Chemical methods include DMSO dispersion method, KOH/HCl solution method, enzymatic method, etc.; physical methods generally include heating methods, ultra-high pressure methods, extrusion cooking methods, and the like. Although the chemical method has high recombination rate, the waste liquid generated in the production process pollutes the environment. The heat treatment preparation method for Zhang Jiayan is used for researching that the RS5 type resistant starch formed by compounding different lipid and rice starch has different stability (the influence of the lipid type on the properties of a starch-lipid complex, Liuzhou institute of technology, journal literature, 2021). Although the heating method in the physical method has simple process and no pollution, the compounding rate is low, so the invention introduces a green physical processing mode to improve the compounding rate and stability of the starch-lipid compound.
Ultrasound is a physical process with frequencies above the human hearing threshold. In recent years, the application of ultrasound in food processing has a remarkable effect, and the application of ultrasound in a starch system is wider. Ultrasonic waves, as a physical processing mode for starch modification, can produce cavitation effects and mechanical effects. Ultrasound may cause the gelatinized starch molecules to be released, promoting amylose and then the complexation of amylose with lipids. Although the ultrasonic technology is widely applied to the field of starch modification, no report about the ultrasonic preparation method of arrowhead starch RS5 type resistant starch is found. The invention aims to provide a green physical processing mode to prepare arrowhead RS5 type resistant starch, study the in-vitro digestion performance of the arrowhead RS5 type resistant starch and provide a preparation method of arrowhead RS5 type resistant starch with high digestibility and high complexing degree.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing an arrowhead starch-linoleic acid compound by utilizing multimode ultrasonic waves, and researches the influence of ultrasonic frequency on the performance and the structure of the arrowhead starch-linoleic acid compound. The invention also discloses a preparation method for preparing the arrowhead starch-stearic acid compound by using ultrasonic, and the influence of ultrasonic time on the performance and the structure of the arrowhead starch-stearic acid compound is researched.
The first purpose of the invention is to provide a method for preparing arrowhead starch-linoleic acid compound by ultrasound, which takes arrowhead starch as raw material, takes lipid as linoleic acid, and prepares starch-lipid compound under different ultrasound frequencies.
In one embodiment of the present invention, a method for preparing an arrowhead starch-linoleic acid compound by ultrasonic waves comprises the following steps:
(1) dissolving a small amount of linoleic acid in absolute ethyl alcohol, adding into 10% (m/v) arrowhead starch solution, stirring at 90 deg.C for 30min, cooling to room temperature, and packaging into high pressure resistant plastic sealing bag;
(2) transferring the mixture to a multi-mode ultrasonic device for ultrasonic treatment, wherein the ultrasonic time is 30min, the ultrasonic intermittence ratio is 10s/4s, the ultrasonic power density is 300W/L, and the treatment temperature is 25 ℃;
(3) centrifuging the mixture after ultrasonic treatment for 10min (4000rpm), washing with 50% ethanol solution, and centrifuging for three times to obtain precipitate;
(4) drying the precipitate in an oven at 40 deg.C for 24 hr to obtain arrowhead starch-lipid complex.
The mass ratio of arrowhead starch to linoleic acid in the step (1) is 1: 20.
the ultrasonic frequency in the step (2) is single frequency (20kHz, 40kHz and 60kHz), double frequency (20kHz/40kHz, 20kHz/60kHz and 40kHz/60kHz), and triple frequency (20kHz/40kHz/60kHz), preferably ultrasonic frequency 40kHz and triple frequency 20kHz/40kHz/60 kHz.
The second purpose of the invention is to provide a method for preparing arrowhead starch-stearic acid compound by ultrasound, which takes arrowhead starch as a raw material, takes lipid as stearic acid, and prepares the starch-lipid compound under different ultrasound time.
In another embodiment of the present invention, a method for preparing arrowhead starch-stearic acid compound by ultrasonic wave comprises the following steps:
(1) stirring arrowhead starch and stearic acid at 90 ℃ for 20min, and then putting into a high-pressure-resistant plastic bag;
(2) carrying out ultrasonic treatment under the conditions of ultrasonic frequency of 20/40kHz, ultrasonic power density of 300W/L, ultrasonic time of 20-60 min and ultrasonic intermittence ratio of 10s/4 s;
(3) centrifuging the sample prepared in the step (2) at 4000rpm for 10min, washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(4) and (3) drying the precipitate obtained in the step (3) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-stearic acid compound prepared by ultrasonic.
The mass ratio of arrowhead starch to stearic acid in the step (1) is 1: 10.
the ultrasonic treatment time in the step (2) is preferably 40 min.
The preparation method of the arrowhead starch in the step (1) comprises the following steps:
(1) soaking rhizoma Sagittariae Sagittifoliae in 4L distilled water at 4 deg.C for 12 hr;
(2) peeling rhizoma Sagittariae Sagittifoliae, cutting into pieces, and pulverizing for 5min with a blender;
(3) diluting the slurry to 10 times by using distilled water, and then adjusting the pH to 10.0 by using a NaOH solution;
(4) stirring the diluted slurry by magnetic force for 1h, and filtering by a 75-mesh sieve to remove fibers;
(5) centrifuging the filtrate for 30min (3000 Xg), discarding supernatant, and oven drying the white precipitate in a 40 deg.C oven to obtain arrowhead starch.
The application of the arrowhead starch-lipid complex as a functional food can be prepared into the functional food for stabilizing postprandial blood sugar, controlling body weight and regulating lipid metabolism.
The invention has the beneficial effects that:
(1) the invention uses ultrasonic waves in the process of preparing the arrowhead starch-lipid compound, promotes the formation of the compound by means of the cavitation effect of the ultrasonic waves and the like, and provides a green physical processing method for improving the stability of the compound. The ultrasonic wave can obviously improve the complexation index of the arrowhead starch-lipid compound, and the complexation index of the arrowhead starch-linoleic acid compound is the highest (84.47%) under the action of 20kHz/40kHz/60 kHz; the arrowhead starch-stearic acid complexation index was highest at 40min on sonication (78.51%).
(2) The arrowhead starch-lipid complex prepared by using the ultrasonic waves has low content of rapidly digested starch (SDS) and high content of Resistant Starch (RS), and the anti-digestibility of the arrowhead starch-lipid complex has good application prospect in the aspect of food processing.
(3) The ultrasonic preparation method of the arrowhead starch-lipid complex has simple process operation, can be used as functional food, and expands the application of ultrasonic waves in RS 5.
Drawings
FIG. 1 is a structural diagram of a multi-mode ultrasonic apparatus, in which 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 a swelling capacity measurement of prepared arrowhead starch;
FIG. 3 is a determination of the complexation index of the arrowhead starch-linoleic acid complexes of comparative example 1 and example 1;
FIG. 4 is a scanning electron micrograph of arrowhead starch, comparative example 1 and example 1 (ultrasound frequencies 40kHz and 20kHz/40kHz/60kHz) arrowhead starch-linoleic acid complexes;
FIG. 5 is an X-ray diffraction pattern of arrowhead starch, comparative example 1 and example 1 (ultrasound frequencies of 40kHz and 20kHz/40kHz/60kHz) arrowhead starch-linoleic acid complex;
FIG. 6 is a Fourier transform infrared spectrum of arrowhead starch, comparative example 1 and example 1 (ultrasound frequencies 40kHz and 20kHz/40kHz/60kHz) arrowhead starch-linoleic acid complex;
FIG. 7 is a complexation index determination for the arrowhead starch-stearic acid complexes of comparative example 2 and example 2;
figure 8 is the in vitro digestibility of arrowhead starch, the arrowhead starch-stearic acid complexes of comparative example 2 and example 2;
fig. 9 is a scanning electron micrograph of arrowhead starch-stearic acid complexes of comparative example 2 and example 2;
FIG. 10 is an X-ray diffraction pattern of arrowhead starch, arrowhead starch of comparative example 2 and example 2, and arrowhead starch-stearic acid complex;
figure 11 is a fourier transform infrared spectrum of arrowhead starch, arrowhead starch of comparative example 2 and example 2, and arrowhead starch-stearic acid complex.
Detailed Description
Terms used in the present invention have generally meanings as commonly understood by one 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 diagram of a multi-mode ultrasonic apparatus of the present invention, which is equipped with a computer program controller for setting ultrasonic working parameters (ultrasonic power density, frequency, pulse working time, pause time and total processing time) to control three ultrasonic controllers respectively, and connecting three ultrasonic vibration plates with different frequencies respectively, so as to realize single frequency/two frequency/three frequency ultrasonic processing; putting a sample to be processed into a liquid container for single-frequency/dual-frequency/multi-frequency ultrasonic processing, and starting a circulating pump to circulate the solution. The automatic control of the solution temperature is realized through the water bath and the temperature probe.
The swelling capacity determination method and the calculation formula of the arrowhead starch prepared in the embodiment of the invention are as follows: preparing 1% (w/v) starch suspension from rhizoma Sagittariae Sagittifoliae starch, and performing water bath at 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, and 90 deg.C for 30min, and performing vortex oscillation every 5 min. After cooling the sample to room temperature, it was centrifuged for 15min (6200 Xg). After separation of the supernatant, the swollen starch precipitate was weighed. Soluble Starch (SS) is the ratio of total carbohydrate in the supernatant to the weight of starch (based on Dry Weight (DW)). The swelling force (SP, g/g) was calculated according to the following formula:
SP ═ precipitate weight × 100/[ dry substance starch weight × (100-SS%) ]
The method for determining and calculating the complexation index of the arrowhead starch-lipid complex prepared in the embodiment of the invention comprises the following steps: weighing 2g of arrowhead starch-lipid complex prepared at different ultrasonic frequencies into 20mL of distilled water, and treating at 95 deg.C for 30min to gelatinize the arrowhead starch-lipid complex. 5g of the gelatinized and cooled sample is weighed, and then transferred to a 50mL centrifuge tube with 25mL of distilled water, vortexed for 2min, and centrifuged for 15min (1000 Xg). 500 μ L of the supernatant was taken, and then 2mL of iodine solution (2.0 gKI, 1.3 gI) was added with 15mL of distilled water2Prepared with 100mL of distilled water), mixed well, and the absorbance (A) was measured at 690nms). Absorbance (A) of gelatinized starch samples without linoleic acid0) As a control. The Complexation Index (CI) is calculated as follows:
CI(％)＝(A0-As)×100/A0
in-vitro digestibility determination and calculation methods of the arrowhead starch and the arrowhead starch-lipid complex prepared in the embodiment of the invention comprise the following steps: 100mg of the sample was weighed and dispersed in 25mL of an acetic acid buffer (0.1M, pH 5.2). The solution was boiled in water for 30 min. The cooled starch suspension was then mixed with 5mL of an enzyme solution containing porcine pancreatic alpha-amylase (solution (280U/mL) and amyloglucosidase (2500U/mL). the mixture was incubated at 37 ℃ with constant stirring (180rpm) for 120 min. an aliquot (1mL) of the hydrolysate was removed at 20min and 120min and mixed with 8mL of 80% ethanol to stop further digestion. after which the sample was centrifuged at 4000rpm for 10min and the hydrolyzed glucose concentration in the supernatant was determined by the 3, 5-dinitrosalicylic acid (DNS) method.three analyses were performed for each sample and the glucose content at 20min and 120min was labeled G20, G120.RDS, SDS, RS, respectively, as follows.
RDS＝G20×0.9/TS×100％
SDS＝(G120-G20)×0.9/TS×100％
RS＝TS-(RDS+SDS)/TS×100％
Where TS refers to the Total Starch (TS) content of the complex used for digestibility determination. Here, TS equals 100 mg.
The arrowhead starch and the arrowhead starch-lipid compound scanning electron microscope determination method comprises the following steps: a proper amount of samples are respectively and uniformly fixed on a sample table by conductive adhesive in a dispersed manner, gold is sprayed on the surfaces of the samples, and then microscopic morphology observation (500X-10000X) is carried out under the accelerating voltage of 5 kV.
The method for measuring the arrowhead starch and the arrowhead starch-lipid complex by X-ray diffraction comprises the following steps: the sample is spread and placed in a sample cell, and is placed on an X-ray diffractometer, copper target Ka radiation (lambda is 0.15418nm) is selected, the tube pressure is measured to be 45kV, the tube flow is 40mA, the scanning range is 4-40 degrees (2 theta), and the scanning speed is 5 degrees/min.
The arrowhead starch and arrowhead starch-lipid complex Fourier transform infrared spectrum determination method comprises the following steps: the dried sample of 2mg and kbr of 100mg were fully ground and mixed in an agate mortar, pressed into tablets and then measured by an infrared spectrometer. Taking a tablet of KBr as a background blank and measuring the thickness of the tablet at 4000-400 cm-1In the wavelength range of 4cm-1Resolution, accumulated 32 scans.
The preparation method of the arrowhead starch comprises the following steps:
(1) soaking rhizoma Sagittariae Sagittifoliae in 4L distilled water at 4 deg.C for 12 hr;
(2) peeling rhizoma Sagittariae Sagittifoliae, cutting into pieces, and pulverizing for 5min with a blender;
(3) diluting the slurry to 10 times by using distilled water, and then adjusting the pH to 10.0 by using a NaOH solution;
(4) stirring the diluted slurry by magnetic force for 1h, and filtering by a 75-mesh sieve to remove fibers;
(5) centrifuging the filtrate for 30min (3000 Xg), discarding supernatant, oven drying the white precipitate in a 40 deg.C oven to obtain arrowhead starch, and packaging;
(6) and (4) measuring the swelling capacity of the arrowhead starch prepared in the step (5).
Determination of arrowhead starch swelling capacity: the swelling force results for arrowhead starch are shown in figure 2. The solubility and swelling power of the water-soluble polyurethane resin tend to increase in the temperature range of 50-90 ℃. The swelling force also increases with increasing temperature. At elevated temperatures, the reactivity of the water increases, leading to increased diffusion of water into the amorphous regions of the starch granules, thereby increasing the swelling power.
Comparative example 1: preparing arrowhead starch-linoleic acid compound:
(1) dissolving 0.3mL of linoleic acid in 40mL of absolute ethanol, adding into 10% (m/v) of arrowhead starch solution (6g of arrowhead starch dispersed in 60mL of distilled water), stirring at 90 deg.C for 30min, and cooling the obtained starch paste to room temperature;
(2) centrifuging the mixture obtained in the step (1) for 10min (4000rpm), washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-linoleic acid compound.
Example 1: preparation of arrowhead starch-linoleic acid complexes at different ultrasonic frequencies:
(1) dissolving 0.3mL of linoleic acid in 40mL of absolute ethanol, adding into 10% (m/v) of arrowhead starch solution (6g of arrowhead starch dispersed in 60mL of distilled water), stirring at 90 deg.C for 30min, cooling to room temperature, and packaging in a high pressure resistant plastic sealed bag;
(2) transferring the mixture obtained in the step (1) into a multi-frequency power ultrasonic device for cold water bath ultrasonic treatment, wherein the ultrasonic time is 30min, the ultrasonic power density is 300W/L, the ultrasonic frequency (20kHz, 40kHz, 60kHz, 20kHz/40kHz, 20kHz/60kHz, 40kHz/60kHz, 20kHz/40kHz/60kHz) is adopted, and the ultrasonic intermittent ratio is 10s/4 s;
(3) centrifuging the mixture obtained in the step (2) at 4000rpm for 10min, washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(4) and (3) drying the precipitate obtained in the step (3) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-linoleic acid compound prepared by ultrasonic.
Comparative example 2: preparation of arrowhead starch-stearic acid complexes
(1) Stirring starch and stearic acid (10%, dry starch base) at 90 deg.C for 20min, and cooling the obtained starch paste to room temperature;
(2) centrifuging the sample prepared in the step (1) at 4000rpm for 10min, washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (3) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-stearic acid compound prepared by ultrasonic.
Example 2: preparation of arrowhead starch-stearic acid compound at different ultrasonic times
(1) Stirring starch and stearic acid (10%, dry starch base) at 90 deg.C for 20min, and packaging into high pressure resistant plastic bag;
(2) carrying out cold water bath ultrasonic treatment on the mixture prepared in the step (1) under the conditions of ultrasonic frequency of 20/40kHz, ultrasonic power density of 300W/L, ultrasonic time of 20, 40 and 60min and ultrasonic intermittence ratio of 10s/4 s;
(3) centrifuging the sample prepared in the step (2) at 4000rpm for 10min, washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(4) and (3) drying the precipitate obtained in the step (3) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-stearic acid compound prepared by ultrasonic.
Experimental example 1: complexation Index (CI) determination of sagittaria sagittifolia starch-linoleic acid complex
The preparation of the arrowhead starch-linoleic acid complex in this experiment was carried out according to the procedure of comparative example 1 and example 1 described above, and then the complex index was measured.
The complexation index for sonicated and non-sonicated arrowhead starch-linoleic acid complexes is shown in figure 3. Among the sonicated arrowhead starch-linoleic acid complexes, the CI value was highest at 20kHz/40kHz/60kHz (84.47%), followed by a CI value of 40kHz (83.9%), which was lower than that of the un-sonicated samples (72.45%). The increase in CI indicates that the interaction of the starch molecules with linoleic acid reduces the formation of amylose complexes and high V-type complexes. The increase in CI value after sonication may also be associated with cavitation-induced disintegration of swollen starch granules, which results in enhanced mass transfer of amylose molecules from the interior of the starch matrix.
Experimental example 2: in vitro digestibility determination of arrowhead starch and arrowhead starch-linoleic acid complex
The preparation method of arrowhead starch of this example was performed according to the above steps; a method for preparing non-sonicated arrowhead starch-linoleic acid complex, comprising the steps of comparative example 1; a method of preparing sonicated arrowhead starch-linoleic acid complex, performed according to the procedure of example 1.
The in vitro digestibility of arrowhead starch, sonicated arrowhead starch-linoleic acid complex and un-sonicated arrowhead starch-linoleic acid complex was determined and the results are shown in table 1. Arrowhead starch has the highest RDS (61.55%), the lowest SDS (15.07%) and the lowest RS (23.38%). Compared with non-ultrasonic-treated arrowhead starch-linoleic acid compound, the ultrasonic-treated arrowhead starch-linoleic acid compound has lower RDS and SDS content and higher RS content. The RS values were highest at 20kHz, 40kHz and 20kHz/40kHz/60kHz with 44.79%, 41.79% and 42.08% respectively. The SDS was lowest (19.9%) and RS highest (40.92%) at 20/40kHz with double frequency ultrasound. This may be due to structural changes in the starch granule configuration caused by sound waves.
TABLE 1 in vitro digestibility determination of arrowhead starch and arrowhead starch-linoleic acid complexes
Experimental example 3: structural characterization and analysis of arrowhead starch and arrowhead starch-linoleic acid complexes
The preparation method of arrowhead starch of this example was performed according to the above steps; a method for preparing non-sonicated arrowhead starch-linoleic acid complex, comprising the steps of comparative example 1; a process for preparing an ultrasonically treated arrowhead starch-linoleic acid complex was carried out as in example 1, except that the ultrasonic frequencies were selected to be 40kHz and 20kHz/40kHz/60 kHz.
(1) Analysis by scanning Electron microscope
FIG. 4 is a scanning electron micrograph of arrowhead starch and arrowhead starch-linoleic acid complexes, with the arrowhead starch (FIGS. 4A1, A2) showing the most pronounced starch granule shape and size, ranging from spherical, ovoid to smooth surfaced granules; but few particles have a rough surface. The un-sonicated arrowhead starch-linoleic acid complexes (fig. 4B1, B2) were rough in surface morphology, possibly containing multiple irregular protrusions and high tips, indicating the presence of branched polysaccharide molecules and their entanglement with each other. The sonicated arrowhead starch-linoleic acid complex showed clearly visible cracks in the porous surface, indicating the high pressure caused by cavitation and fragmentation near the starch granules. In addition, the curled morphology with small particles and non-uniform pore sizes is also exhibited due to ultrasound-induced complexation. In addition, the formation of V-type complexes may limit the degradation of amylose. This may be due to ultrasound-induced disaggregation, degradation and rearrangement effects of the arrowhead starch-linoleic acid complex.
(2) X-ray diffraction analysis
Fig. 5 is an X-ray diffraction pattern of arrowhead starch and arrowhead starch-linoleic acid complex, and the diffraction pattern and relative crystallinity of the samples were analyzed. As can be seen from fig. 5, arrowhead starch shows distinct peaks of the a-type crystal structure at 11 °, 15 °, 17 ° and 23 °. The sonicated arrowhead starch-linoleic acid complexes at 40kHz and 20kHz/40kHz/60kHz had characteristic peaks at 7.5 °, 13.3 °, and 20.15 °, indicating that the sonicated arrowhead starch-linoleic acid complexes were converted to V-shaped structures. The diffraction intensity of un-sonicated arrowhead starch-linoleic acid complexes was weaker than that of sonicated arrowhead starch-linoleic acid complexes, indicating a tendency for the number of complexes to increase after variable frequency sonication, consistent with the complexation index results. It is found from the relative crystallinity of the sample that the relative crystallinity of the sonicated arrowhead starch-linoleic acid complex is significantly increased and the cavitation effect of the surface sonication induces a higher relative crystallinity compared to the un-sonicated arrowhead starch-linoleic acid complex.
(3) Fourier transform infrared spectroscopy
Figure 6 is a fourier transform infrared spectrum of arrowhead starch and arrowhead starch-linoleic acid complex. The Fourier transform infrared spectrum is 1200-800cm-1Shows a sensitivity to short-range structural changes of the starch molecule. All samples were 1710 and 2850cm-1All show carbonyl (-C ═ O) stretching resonance in the infrared spectrum region, and can be carbonyl and asymmetric CH of arrowhead starch alkyl chain2、CH3And (5) stretching and vibrating. This demonstrates the feasibility of complex formation by interaction of starch with linoleic acid after multi-frequency sonication. The sonicated arrowhead starch-linoleic acid complexes were 1380 and 1425cm in comparison to arrowhead starch-1Bone vibration with no aromatic nuclei present nearby. This indicates that the sagittaria sagittifolia starch-linoleic acid complex is formed by incorporating the aromatic core of linoleic acid into the amylose helix. From Table 2, it can be seen that the multi-frequency ultrasonic wave is 1046cm-1And 1022cm-1Has a significant effect on the relative intensity of the infrared spectral band (p)<0.05), indicating that the ultrasound induced disruption of the crystal structure of the arrowhead flour particles. The ratio of the infrared spectra appearing in the absorption region of the spectrum at R1022/995 indicates the short-term crystallinity of the filling of the double helix in the internal structure of the particle. The results show that the absorbance of the composite decreased significantly with increasing ultrasonic frequency, indicating that the amorphous property of the composite increased and the crystallinity decreased due to the ultrasonic-induced cavitation phenomenon. The reason for this destruction may be that the structural configuration of the alpha-1, 4-glycosidic bond of the backbone of the wafer and non-wafer is disturbed, which also proves to be 930cm-1The IR region of (a) is less crystalline and this region is sensitive to C-O-C vibrations.
TABLE 2 Ipomoea batatas starch and Ipomoea batatas starch-linoleic acid Complex IR values
Experimental example 4: complexation Index (CI) determination of sagittaria sagittifolia starch-stearic acid complexes
The preparation of the arrowhead starch-stearic acid complexes in this experiment was carried out according to the procedure of comparative example 2 and example 2 above, and then the complexation index was determined.
The CI values of the starch-stearic acid complexes under different sonication conditions are shown in figure 7. The CI values of the arrowhead starch and the arrowhead starch-stearic acid compound are both more than 65%, wherein the CI value of the arrowhead starch-stearic acid compound treated by ultrasonic treatment for 40min is the highest and is 78.51%. This means that 40min of sonication makes it easier for stearic acid and starch molecules to form complexes. The increase in CI is due to the cavitation effect of ultrasound, which disintegrates the swollen starch granules, releasing more amylose from its internal matrix, thereby improving the feasibility of amylose binding to lipids.
Experimental example 5: in vitro digestibility determination of arrowhead starch and arrowhead starch-stearic acid complex
The preparation method of arrowhead starch of this example was performed according to the above steps; a method of preparing non-sonicated arrowhead starch-stearic acid complex, carried out according to the procedure of comparative example 2; a method of preparing an ultrasonically-treated arrowhead starch-stearic acid complex, was performed according to the procedure of example 2.
Determination of in vitro digestibility of arrowhead starch, un-sonicated arrowhead starch-stearic acid complexes and sonicated arrowhead starch-stearic acid complexes is shown in figure 8. The content of Rapidly Digestible Starch (RDS), Slowly Digestible Starch (SDS) and Resistant Starch (RS) of arrowhead starch was 59.29%, 18.55% and 22.16%, respectively. The Resistant Starch (RS) content was increased for all the sonicated complexes compared to arrowhead starch, while the content of fast digesting starch (RDS) was decreased, indicating that the V-type complexes showed a stronger resistance to digestion than the arrowhead starch. The highest RS content (32.3%) was obtained at 40min of sonication. The sonication time increased from 20min to 40min, and the SDS content of the arrowhead starch-stearic acid complex increased from 24.47% to 27.28%, thus suggesting that the sonication time may result in digestibility of the complex.
Experimental example 6: structural characterization and analysis of arrowhead starch and arrowhead starch-stearic acid complexes
The preparation method of arrowhead starch of this example was performed according to the above steps; a method for preparing non-sonicated arrowhead starch-linoleic acid complex, comprising the steps of comparative example 2; a method of preparing sonicated arrowhead starch-linoleic acid complex, performed according to the procedure of example 2.
(1) Analysis by scanning Electron microscope
Fig. 9 is a scanning electron micrograph of an arrowhead starch-stearic acid complex. As can be seen from the figure, the particle size of the composite is significantly increased, and the composite further exhibits a reorientation and crystallization phenomenon. In addition, the compound has a sheet structure, irregular shape and rough surface.
(2) X-ray diffraction analysis
Fig. 10 is an X-ray diffraction pattern of arrowhead starch and arrowhead starch-stearic acid complexes, and the samples were analyzed for diffraction pattern and relative crystallinity. As can be seen in fig. 10, all arrowhead starch-stearic acid complexes have characteristic peaks at both 13.0 ° and 20.0 °, indicating the formation of a V-shaped crystal structure. The arrowhead starch has characteristic peaks at 11.5 degrees, 15.0 degrees, 17.0 degrees and 23.0 degrees, which indicates that the arrowhead starch has an A-type crystal structure. The Relative Crystallinity (RC) of the arrowhead starch-stearic acid complexes ranged from 29.07% to 33.01%, with increasing sonication time increasing and then decreasing. The relative crystallinity of the complex was highest at 40min of sonication. It was shown that the ultrasonic treatment increased the leaching of amylose and allowed it to combine with stearic acid, while degrading amylopectin content. However, after 60min of sonication of the complex, the bubbles formed by sonication were so large that their collapse time was insufficient to break down the starch molecules. Furthermore, complexes with ultrasound effect show a better structural order, resulting in a stronger interaction between arrowhead starch and stearic acid, which may reduce the susceptibility of the complex to enzymatic digestion. Thus, from the in vitro digestibility results, it was shown that the RS content of all the sonicated complexes was increasing and the RDS content was decreasing compared to sagittaria sagittifolia starch. This indicates that the sonicated arrowhead starch-stearic acid complex exhibits a potentially higher resistance to digestion than does arrowhead starch.
(3) Fourier transform infrared spectroscopy
Figure 11 is a fourier transform infrared spectrum of arrowhead starch and arrowhead starch-stearic acid complex. Comparing with arrowhead starch, the arrowhead starch-stearic acid compound is at 2850cm-1And 1716cm-1Two characteristic peaks appear. The arrowhead starch is 3354cm-1Has a characteristic peak due to stretching vibration of O-H group, and the characteristic peak of O-H group corresponding to arrowhead starch-stearic acid compound is 3420cm-1To (3). Both the band intensity of the arrowhead starch-stearic acid complexes decreased compared to arrowhead starch, and the absorbance decreased with increasing sonication time, probably due to the increased hydrophobicity of the lipids caused by ultrasound. At 1200 and 800cm-1Within the range, the short range ordered structure of arrowhead starch and arrowhead starch-stearic acid complex was analyzed, 1045cm-1And 1022cm-1Correspond to the ordered crystalline and amorphous regions of starch, respectively. 1045/1022cm passing through Table 3-1And 1022/995cm-1The IR absorption ratio of (A) was found to be 1045/1022cm for all arrowhead starch-stearic acid complexes relative to arrowhead starch-1All increase in IR value of (A) and 1022/995cm-1The IR value of (a) decreases. The arrowhead starch-stearic acid compound shows higher short-range molecular order degree, which is consistent with the result of XRD.
TABLE 3 Ipomoea batatas starch and Ipomoea batatas starch-stearic acid complex IR values
Claims (9)
1. A method for preparing arrowhead starch-linoleic acid compound by ultrasonic waves is characterized by comprising the following steps:
(1) dissolving a small amount of linoleic acid in absolute ethyl alcohol, adding into 10% (m/v) arrowhead starch solution, stirring at 90 deg.C for 30min, cooling to room temperature, and packaging into high pressure resistant plastic sealing bag;
(2) transferring the mixture to a multi-mode ultrasonic device for ultrasonic treatment, wherein the ultrasonic time is 30min, the ultrasonic intermittence ratio is 10s/4s, the ultrasonic power density is 300W/L, and the treatment temperature is 25 ℃;
(3) centrifuging the mixture after ultrasonic treatment for 10min (4000rpm), washing with 50% ethanol solution, and centrifuging for three times to obtain precipitate;
(4) drying the precipitate in an oven at 40 deg.C for 24 hr to obtain arrowhead starch-lipid complex.
2. The method for preparing arrowhead starch-linoleic acid compound by ultrasonic wave as claimed in claim 1, wherein the ratio of arrowhead starch to linoleic acid in the step (1) is 1: 20.
3. the method for preparing arrowhead starch-linoleic acid complex by ultrasonic wave as claimed in claim 1, wherein the ultrasonic frequency in the step (2) is 20kHz, 40kHz, 60kHz, 20kHz/40kHz, 20kHz/60kHz, 40kHz/60kHz, 20kHz/40kHz/60 kHz.
4. The method for preparing arrowhead starch-linoleic acid complex by ultrasonic wave as claimed in claim 3, wherein the ultrasonic frequency in the step (2) is 40kHz, 20kHz/40kHz/60 kHz.
5. A method for preparing arrowhead starch-stearic acid compound by ultrasonic waves is characterized by comprising the following steps:
(1) stirring arrowhead starch and stearic acid at 90 ℃ for 20min, and then putting into a high-pressure-resistant plastic bag;
(2) carrying out ultrasonic treatment under the conditions of ultrasonic frequency of 20/40kHz, ultrasonic power density of 300W/L, ultrasonic time of 20-60 min and ultrasonic intermittence ratio of 10s/4 s;
(3) centrifuging the sample prepared in the step (2) at 4000rpm for 10min, washing with a 50% ethanol solution, and centrifuging three times to obtain a precipitate;
(4) and (3) drying the precipitate obtained in the step (3) in an oven at 40 ℃ for 24 hours to obtain the arrowhead starch-stearic acid compound prepared by ultrasonic.
6. The method for preparing arrowhead starch-stearic acid compound by ultrasonic wave as claimed in claim 5, wherein the ratio of arrowhead starch to stearic acid in the step (1) is 1: 20.
7. the method for preparing arrowhead starch-stearic acid compound by ultrasonic wave as claimed in claim 5, wherein the ultrasonic time in the step (2) is preferably 40 min.
8. The method for preparing an arrowhead starch-linoleic acid complex by ultrasonic waves as claimed in claim 1 or the method for preparing an arrowhead starch-stearic acid complex by ultrasonic waves as claimed in claim 5, wherein the preparation of the arrowhead starch in the step (1) is performed according to the following steps:
(1) soaking rhizoma Sagittariae Sagittifoliae in 4L distilled water at 4 deg.C for 12 hr;
(2) peeling rhizoma Sagittariae Sagittifoliae, cutting into pieces, and pulverizing for 5min with a blender;
(3) diluting the slurry to 10 times by using distilled water, and then adjusting the pH to 10.0 by using a NaOH solution;
(4) stirring the diluted slurry by magnetic force for 1h, and filtering by a 75-mesh sieve to remove fibers;
(5) centrifuging the filtrate for 30min (3000 Xg), discarding supernatant, and oven drying the white precipitate in a 40 deg.C oven to obtain arrowhead starch.
9. Use of the arrowhead starch-lipid complex prepared according to claims 1-8 as a functional food, which can be prepared to stabilize postprandial blood glucose, control body weight, regulate lipid metabolism.
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| CN110292166A (en) * | 2019-05-23 | 2019-10-01 | 江苏大学 | A method of resistant starch is prepared based on frequency sweep ultrasonic wave technology |
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