CN113383965A - Energy slow-release cereal-like microsphere and preparation method and application thereof - Google Patents
Energy slow-release cereal-like microsphere and preparation method and application thereof 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
- 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
-
- A—HUMAN NECESSITIES
- 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
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to the technical field of slowly digestible starch, and particularly provides energy slow-release cereal-like microspheres and a preparation method and application thereof. Sodium alginate and gellan gum with negative charges are combined with chitosan with positive charges through electrostatic interaction to form polyelectrolyte compound gel to wrap potato starch, and the energy slow-release grain-like starch microspheres are constructed. The gel microsphere has good energy slow release performance, reduces the digestion rate compared with the original starch, improves the content of slowly digestible starch, and is a low GI starch food. The microsphere prepared by the invention has good water absorption and expansibility, but the pH value of the soup of the microsphere is lower, and the dry matter quantity and the iodine blue value of the soup are obviously lower than those of rice and millet. The invention provides a new theoretical basis for constructing novel starch food with good energy slow release property and slowly digestible starch, is beneficial to promoting the development of starch processing industry, and provides a new thought and theoretical basis for the research and development of low GI (glycemic index) food.
Description
Technical Field
The invention belongs to the technical field of slowly digestible starch, and particularly provides energy slow-release cereal-like microspheres and a preparation method and application thereof.
Background
Starch can be classified into fast-digestible starch, slow-digestible starch and resistant starch according to the digestion rate of the starch in human body. The slowly digestible starch has the effects of improving human metabolism, preventing and treating diabetes, increasing satiety and providing durable and stable energy through experimental measurement. After glucose enters blood, the blood glucose value of a human body fluctuates. Currently, the results of studies on the reduction of digestibility of starch are not significant, and there are few studies on the preparation of microspheres having a slow digestibility using a method of preparing polyelectrolyte complexes.
Sodium alginate has good gel property, and the formed gel has good freeze-thaw stability, and is widely applied to the fields of edible films, drug-loaded systems, microcapsule wall materials, wound treatment and the like. Gellan gum, as a hydrocolloid, can form higher molecular weight complexes with starch, water, and the like. It has good properties and is widely used in the fields of food and medicine.
Chitosan, as the only cationic polysaccharide, and its derivatives, are widely used in medical and pharmaceutical applications due to their hemocompatibility and biodegradability. Besides being applied to medical and pharmaceutical fields, chitosan and derivatives thereof are also widely applied to the fields of food, cosmetics, bioengineering and the like. The modification of chitosan into composite materials is related to its low adsorption capacity in aqueous media, relating to its crystallinity and swellability, low porosity, low hydrophilicity, low specific surface area and instability in acidic media.
At present, the principle of synthesizing polyelectrolyte complexes is applied in many fields, but no research on applying polyelectrolyte complexes in the field of slowly digestible starch has been reported.
Disclosure of Invention
In order to solve the technical problems, the invention provides the energy slow-release cereal-like microsphere, and a preparation method and application thereof.
The invention is realized in such a way that a preparation method of energy slow-release cereal-like microspheres, which utilizes the combination of a sodium alginate solution with negative charges, a gellan gum solution and a chitosan solution with positive charges to form a polyelectrolyte compound to wrap starch, and specifically comprises the following steps:
1) uniformly mixing starch, a sodium alginate solution and a gellan gum solution with certain mass to form a mixed solution;
2) dripping the mixed solution into a chitosan solution, standing and soaking for a certain time to obtain a gel sphere;
3) filtering out the gel microspheres, and then adding the gel microspheres into a calcium chloride solution for fixing for a certain time;
4) and filtering out the fixed gel microspheres, and drying to obtain the energy slow-release cereal-like microspheres.
Preferably, in the step 1), the mass of the starch is 1g, the sodium alginate solution is 5mL, the gellan gum solution is 5mL, and the concentrations of the sodium alginate solution and the gellan gum solution are both 0.2% -1.2%.
Further preferably, in the step 1), the starch is potato starch or tapioca starch.
Further preferably, in the step 2), the concentration of the chitosan solution is 0.05% -0.25%.
Preferably, in the step 2), the mixed solution is dripped into the chitosan solution through a syringe needle by a constant flow pump, and the chitosan solution is kept stand and soaked for 1 hour.
Further preferably, in the step 3), the gel microspheres are filtered out through gauze, and then the gel microspheres are added into a calcium chloride solution for fixation for 1 hour, wherein the concentration of the calcium chloride solution is 0.5% -1.5%.
Further preferably, in the step 4), the immobilized gel microspheres are filtered out by gauze and dried in an oven.
The invention also provides the energy slow-release cereal-like microsphere prepared by the preparation method of the energy slow-release cereal-like microsphere prepared by the method.
The energy slow-release cereal-like microsphere provided by the invention is applied to the field of slowly digestible starch as a polyelectrolyte compound.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the polyelectrolyte complex technology is applied to the production of slowly digestible starch for the first time, and the starch gel microspheres are constructed according to the formation mechanism of the polyelectrolyte complex, so that the digestibility of the starch is reduced;
2. the microsphere provided by the invention has good water absorption and expansibility, has a complete spherical structure after being steamed for a long time, has similar steaming quality and texture characteristics to millet, and can be used as a pseudo-grain for daily eating;
3. the invention expands the application of the potato starch and can promote the development of the potato starch industry;
4. the invention can be used as a polyelectrolyte compound to be applied to the field of slowly digestible starch to develop novel low GI food.
Drawings
FIG. 1 is an appearance diagram of energy-releasing cereal-like microspheres prepared by the present invention;
FIG. 2 is an in vitro simulated digestion curve for examining the in vitro simulated digestibility of energy-extended pseudograin starch microspheres in comparison to natural grain rice and millet milled as compared to potato starch;
FIG. 3 is a graph showing the content of Rapidly Digestible Starch (RDS), Slowly Digestible Starch (SDS) and Resistant Starch (RS) in the energy-release pseudocereal Starch microspheres compared with natural cereal rice and millet after milling, using potato Starch as a control;
FIG. 4 shows the SDS content percentage of the energy-extended pseudo-cereal microspheres prepared according to the examples of the present invention
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Determination of simulated digestibility in vitro:
dissolving 0.4g of potato starch energy slow-release pseudograin microspheres in acetic acid buffer solution, gelatinizing in boiling water bath for 10min, and then keeping at 37 ℃ for 10 min. To the sample was added mixed hydrolase (1450U pancreatin a-amylase and 75U saccharifying enzyme) and the mixture was subjected to hydrolysis with shaking in a water bath at 37 ℃. And (3) adding anhydrous ethanol into samples which are hydrolyzed for 10min, 20min, 60 min and 120min respectively to inactivate enzyme, centrifuging, and measuring the glucose content in the supernatant according to a 3, 5-dinitrosalicylic acid (DNS) method. The digestibility of the samples was calculated as follows:
D＝G*0.9/M*100
d-digestibility of starch/%
G-amount of glucose produced by hydrolysis/mg
0.9 molar Mass conversion factor of glucose to starch
M-mass of starch in sample/mg
Measurement of cooking quality:
the cooking quality is divided into water absorption, expansion rate, pH of the soup, dry matter of the soup and iodine blue value of the soup. Taking two common grains of rice and millet as a contrast, accurately weighing 1g of rice, millet and energy slow-release pseudograin microspheres, placing the rice, the millet and the energy slow-release pseudograin microspheres in copper wire cages with known weights, placing the copper wire cages together in a beaker, adding 120mL of distilled water, placing the beaker on an electric furnace, heating and boiling for 30min, taking out the copper wire cages, placing the copper wire cages on the beaker until no soup drips, and cooling for 10 min.
The water absorption calculation formula is as follows:
the sample expansion volume calculation formula is:
measuring the pH value of the rice soup: the pH of the rice soup cooled to room temperature in the beaker was measured using a pH meter.
And (3) measuring the dry substance of the soup: the pH-measured broth was diluted to 100mL with distilled water, centrifuged at 8000rpm for 30min, and the supernatant was dried in an oven and weighed. The dry matter mass calculation formula of the soup is as follows:
and (3) measuring the iodine blue value of rice water: taking 1mL of the centrifuged soup, adding 50mL of distilled water, 1mL of 0.5mol/L HCL solution and 1mL of 0.2mol/L iodine reagent, and diluting to 100mL with distilled water. The absorbance was measured at 600nm with an ultraviolet spectrophotometer.
Comparative example
Dissolving 1g potato starch in acetic acid buffer solution, gelatinizing in boiling water bath for 10min, and maintaining at 37 deg.C for 10 min. The content of slowly digestible starch is 5.94% by adding mixed enzyme to carry out in-vitro digestion test.
Example 1
Mixing 1g of starch, 5 mL0.8% sodium alginate solution and 5mL of 1% gellan gum solution, dripping the mixed solution into 100 mL0.2% chitosan solution through a syringe needle by a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, drying the microspheres in an oven at 40 ℃, wherein the content of the slowly digestible starch of the microspheres is 49.12%. The sodium alginate, the gellan gum and the chitosan are added to form a polyelectrolyte compound gel membrane wall wrapping the starch, so that the starch is difficult to diffuse into the solution through the gel membrane. As a synthetic or natural macromolecule containing ionized groups, polyelectrolytes may form a macromolecular polyelectrolyte complex by establishing electrostatic interactions with oppositely charged polyelectrolytes. The formation of polyelectrolyte complex can be divided into three stages of primary polymerization, internal rearrangement and hydrophobic polymerization, and the formation process is mainly affected by molecular composition, ionic strength and pH. In the primary polymerization stage, polyelectrolytes with opposite charges are rapidly accumulated in the solution to form a primary compound; then undergoes a complex internal rearrangement process, in which the electrostatic bonds and polymer chains of the primary polyelectrolyte complex rearrange to form intermediate complexes, which generally lasts for 1-2 hours; finally, the intermediate polymers are mutually aggregated under the action of hydrophobic force to finally form the polyelectrolyte compound. And the polyelectrolyte compound is researched and found to have good energy slow release performance, so that the polyelectrolyte compound is widely applied to the field of medical energy. The gel microsphere is constructed by utilizing the starch and polyelectrolyte compound, so that the slow digestion effect of the starch is realized, the energy is slowly released, and the starch energy slow release microsphere with functional characteristics is formed. Therefore, the digestion rate of the starch is reduced, and the slow release effect is obvious.
Example 2
Mixing 1g of starch, 5 mL0.2% sodium alginate solution and 5mL of 1% gellan gum solution, dripping the mixed solution into 100 mL0.2% chitosan solution through a syringe needle by a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, drying the microspheres in an oven at 40 ℃, wherein the content of the slowly digestible starch of the microspheres is 34.15%. The sodium alginate has excellent gel characteristics, ion exchange is carried out in the presence of metal divalent cations, guluronic acid is folded and stacked to form a new hydrophilic space, the metal cations occupy the space and then have chelation with carboxyl oxygen, the stretched molecular chains are converted into an ordered belt-shaped structure, and finally the egg box gel with a three-dimensional network structure is presented. When the method is explained, the polyelectrolyte compound constructed by the sodium alginate-gellan gum-chitosan is more compact, and can more efficiently delay the digestion of starch. When the concentration of sodium alginate is lower, the gel structure of the formed polyelectrolyte compound is unstable, and each starch particle cannot be completely wrapped, so that the slowly digestible starch content is lower.
Example 3
Mixing 1g of starch with 5mL of 1% sodium alginate solution and 5mL of 0.6% gellan gum solution, dripping the mixed solution into 100mL of 0.2% chitosan solution through a syringe needle by using a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, and drying the microspheres in an oven at 40 ℃, wherein the content of the slowly digestible starch of the microspheres is 47.48%. Gellan gum is a type of extracellular episomal polysaccharide produced by pseudomonas aeruginosa. The product is nontoxic and harmless, has viscosity similar to food gum such as xanthan gum and carrageenan, and can be used as stabilizer and thickener in food processing industry such as fruit juice and meat paste. The gellan gum also has good gel characteristics, linear molecules can be automatically rearranged into a double-helix structure after the gellan gum dissolved by heating is cooled, and the linear molecules are further entangled to finally form the gel with a three-dimensional network structure. Under the condition that cations exist, the gel can shield the electrostatic repulsion action of carboxyl side chains and is combined with carboxyl, so that the intermolecular crosslinking action is accelerated, the gel with a net structure is easier to form, and the gel strength is related to the cooling speed, the gellan gum concentration, the ion type and other factors. Therefore, when the gellan gum concentration is reduced, the gel with a net structure is not easy to form, the gel strength is poor, the starch particles are not completely wrapped, the energy slow release effect of the starch microspheres is poor, and the content of slowly digestible starch is low. With the increase of the content of sodium alginate, the thickness and compactness of the formed polyelectrolyte compound gel membrane wall wrapping the starch are increased, so that the starch is difficult to diffuse into the solution through the gel membrane, the starch digestion rate is reduced, and the slow release effect is obvious. Therefore, sodium alginate can be used as a raw material for preparing polyelectrolyte complexes to reduce digestibility of starch.
Example 4
Mixing 1g of starch with 5mL of 1% sodium alginate solution and 5mL of 0.8% gellan gum solution, dripping the mixed solution into 100mL of 0.2% chitosan solution through a syringe needle by using a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, and drying the microspheres in an oven at 40 ℃, wherein the content of digestible starch of the microspheres is 49.66%. The increase of the gellan gum enhances the slow release performance of the polyelectrolyte compound gel film, and the content of slowly digestible starch is positively correlated with the concentration of the solution thereof. On one hand, the compactness and the slow release effect of the polyelectrolyte compound are improved by adding the gellan gum, on the other hand, the gellan gum has good gelling property, after the microspheres are cooked, heated and cooled, the unreacted gellan gum in the microspheres can be automatically gathered to form stable gel, the mechanical strength of a gel skeleton in the microspheres is further enhanced, and the slow release effect is improved.
Example 5
Mixing 1g of starch with 5mL of 1% sodium alginate solution and 5mL of 1% gellan gum solution, dripping the mixed solution into 100 mL0.20% chitosan solution through a syringe needle by using a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, adding CaCl2Fixing the solution, filtering out the microspheres by using gauze, and drying the microspheres in an oven at 40 ℃ to obtain the microspheres with the slowly digestible starch content of 55.35%. Chitosan is the only cationic polysaccharide in the nature, the content of chitosan is second to cellulose, the chitosan can be degraded into amino sugar in the human body, and the chitosan has good biocompatibility. Because chitosan has positive charge under acidic condition, chitosan and its derivatives have blood compatibility and biodegradability and are widely used in medical medicine, food, cosmetics, bioengineering, etc. The chitosan in the organic acid dilute solution is influenced by the solubility, distribution, ionic strength and the degree of intramolecular hydrogen bonds of the organic acid. Sodium alginate and gellan gum are polyelectrolytes with negative charges, chitosan has positive charges, and under the condition that the electrolyte content of the negative charges in a solution is not changed, the reduction of the polyelectrolytes with the positive charges can lead to the unstable gel structure of the formed polyelectrolyte compound, the constructed gel starch microspheres are reduced, and a part of starch particles are not wrapped, so that the content of slowly digestible starch in the formed compound is reduced, and the energy slow release performance is weakened. The content of slowly digestible starch increases with increasing gellan gum concentration.
Example 6
Mixing 1g of starch with 5mL of 1% sodium alginate solution and 5mL of 1% gellan gum solution, dripping the mixed solution into 100 mL0.25% chitosan solution through a syringe needle by using a constant flow pump, standing and soaking for 1h to ensure that the mixed solution droplets and the chitosan fully react to form a gel sphere structure, then filtering the chitosan solution by using gauze, adding CaCl2Fixing the solution, filtering out microspheres with gauze, oven drying the microspheres in an oven at 40 deg.C to obtain microspheresThe slowly digestible starch content was 54.13%. As the concentration of the chitosan is increased, the structure of the formed gel becomes more stable, and the slow release effect is enhanced. However, the excessive concentration of chitosan can cause the excessive viscosity of the solution, which is not favorable for the dispersion of liquid drops in the solution and influences the spherical structure of the microspheres.
Referring to fig. 1, the energy-release cereal-like starch microspheres prepared by the present invention have an appearance similar to that of cereals, and for further research on edibility as a cereal-like product, the cooking quality and texture characteristics were compared and evaluated by using common staple cereals, rice and millet, as controls, and the cooking quality evaluation is shown in table 1. According to the data in the table, the water absorption rate and the expansion rate of the energy slow-release cereal-like starch microspheres are obviously higher (p <0.05) than those of rice and millet, which is probably caused by the high swelling rate of the polyelectrolyte complex. The microspheres have a low broth pH, which may be a difference caused by the composition of the microspheres. The dry matter quantity and iodine blue value of the soup of the microspheres are also obviously lower than those of rice and millet, which indicates that the starch dissolving amount in the soup of the microspheres is lower. However, in general, the difference between each index of the microspheres and the grain is within an acceptable range, and the microspheres can still keep a complete spherical structure under hydrothermal treatment, and have better cooking quality and certain grain quality characteristics.
TABLE 1
Fig. 2 is a graph that examines the simulated digestibility of energy-extended pseudograin starch microspheres in vitro, in comparison to the naturally-occurring milled rice and millet, using potato starch PS as a control. FIG. 2 shows an in vitro simulated digestion curve, in the fast digestion stage of starch, the starch hydrolysis rates are, from large to small: PS > rice flour ≈ millet flour > energy slow-release pseudo-grain starch microspheres; the overall trend of the starch hydrolysis rate in the slow digestion stage is unchanged; in the whole digestion process, the energy slow-release cereal-like starch microsphere shows excellent glucose slow-release effect, and can maintain the original anti-digestion property of starch.
FIG. 3 further analyzes the RDS, SDS and RS content of the samples, and the results show that: the amount of RDS in the energy slow-release quasi-cereal starch microspheres is greatly reduced, the numerical value of the RDS is far lower than that of natural cereal powder, and the rapid release of glucose at the initial stage of starch hydrolysis is relieved; the SDS content in the energy slow-release grain-like starch microspheres is increased by 6 times compared with the control, and the energy slow release control of the starch is realized.
FIG. 4 shows the SDS content of the microspheres prepared in each example. As shown in the figure, the starch microspheres which are constructed by utilizing sodium alginate, gellan gum and chitosan to wrap starch can slowly release energy and have certain grain quality characteristics can effectively control the rapid hydrolysis of starch at the early stage of digestion, the content of slowly digested starch is obviously improved, the smooth rise of postprandial blood sugar can be realized from the perspective of in vitro digestion, the risk of blood sugar fluctuation caused by eating starch or high starch food by hyperglycemic people can be reduced, and the negative influence of hypoglycemia after the peak value of blood sugar can be prevented.
Finally, it should be noted that the above-mentioned embodiments are only specific embodiments of the present invention, and obviously, the present invention is not limited to the above-mentioned embodiments, and many variations are possible. All modifications directly or indirectly obvious to those skilled in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (9)
1. A preparation method of energy slow-release cereal-like microspheres is characterized in that a sodium alginate solution with negative charges, a gellan gum solution and a chitosan solution with positive charges are combined to form a polyelectrolyte compound to wrap starch, and the preparation method specifically comprises the following steps:
1) uniformly mixing starch, a sodium alginate solution and a gellan gum solution with certain mass to form a mixed solution;
2) dripping the mixed solution into a chitosan solution, standing and soaking for a certain time to obtain a gel sphere;
3) filtering out the gel microspheres, and then adding the gel microspheres into a calcium chloride solution for fixing for a certain time;
4) and filtering out the fixed gel microspheres, and drying to obtain the energy slow-release cereal-like microspheres.
2. The preparation method of the energy slow-release cereal-like microsphere as claimed in claim 1, wherein in the step 1), the mass of the starch is 1g, the sodium alginate solution is 5mL, the gellan gum solution is 5mL, and the concentrations of the sodium alginate solution and the gellan gum solution are both 0.2% -1.2%.
3. The method for preparing energy-extended cereal-like microspheres according to claim 1, wherein in step 1), the starch is potato starch or tapioca starch.
4. The method for preparing energy-extended cereal-like microspheres according to claim 1, wherein in step 2), the concentration of the chitosan solution is 0.05-0.25%.
5. The preparation method of the energy slow-release cereal-like microsphere as claimed in claim 1, wherein in the step 2), the mixed solution is dripped into the chitosan solution through a syringe needle by a constant flow pump, and the chitosan solution is left to stand and soak for 1 hour.
6. The method for preparing energy-release cereal-like microspheres according to claim 1, wherein in the step 3), the gel microspheres are filtered out by gauze and then added into a calcium chloride solution for fixation for 1 hour, wherein the concentration of the calcium chloride solution is 0.5-1.5%.
7. The method for preparing energy-releasing cereal-like microspheres according to claim 1, wherein in step 4), the immobilized gel microspheres are filtered out by gauze and dried in an oven.
8. The energy-extended release cereal-like microspheres prepared by the method for preparing energy-extended release cereal-like microspheres according to claim 1, 2, 3, 4, 5, 6, 7 or 8.
9. The use of energy-extended release cereal-like microspheres according to claim 8, wherein the energy-extended release cereal-like microspheres are used in the field of slowly digestible starch as polyelectrolyte complexes.
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