CN113289559A - Nano microcapsule embedding hydrophilic compound and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a nano microcapsule embedding a hydrophilic compound, a preparation method and application thereof. The hydrophilic compound nano microcapsule provided by the invention takes protein and polysaccharide as wall materials, the wall materials and the hydrophilic compound are mixed in water to form a mixed solution, and the pH of the mixed solution is adjusted to 3.4-4.5 while the mixed solution is treated by ultrasonic waves, so that the hydrophilic compound nano microcapsule is obtained. In the preparation method provided by the invention, the hydrophilic compound accounts for 0.5-7% of the total weight of dry matter of the wall material. The hydrophilic compound nano microcapsule provided by the invention has good dispersibility, can effectively embed hydrophilic compounds such as caffeine and the like to form a core-shell structure, and can further form the core-shell structure.
Description
Technical Field
The invention relates to the technical field of hydrophilic compound embedding, relates to a hydrophilic compound-embedded nano microcapsule, and a preparation method and application thereof, and particularly relates to a hydrophilic compound-embedded method of a protein and polysaccharide nano microcapsule and a product.
Background
The microcapsule technology can realize the targeted delivery and accurate release of active substances of foods and medicines, but hydrophilic compounds are easy to diffuse into the water phase, so that the embedding of the hydrophilic compounds is limited. There are a number of reports on the entrapment of hydrophobic components, however there is still a lack of an effective method for entrapping and delivering hydrophilic compounds. At present, the embedding methods of the hydrophilic compound mainly comprise methods of multilayer emulsion, liposome, hydrogel and the like, and the methods have the technical problems of thermal instability, low embedding rate, non-edible material and the like.
Among embedding materials for hydrophilic compounds, polysaccharides and proteins have attracted much attention due to their natural safety characteristics, and common natural polysaccharides include sodium alginate, chitosan, gum arabic, and the like, and natural proteins include whey protein, bovine serum albumin, casein, and the like. Some scholars embed hydrophilic drugs (doxorubicin hydrochloride) by sodium alginate gel beads, and mix and drop-add sodium alginate and hydrophilic compounds into a mixed solution of calcium chloride and chitosan to realize layer-by-layer self-assembly of the hydrophilic compounds, however, the larger particle size (about 100 μm) limits the application. Still others have used ultrasound emulsions to prepare microcapsules for hydrophilic compound delivery, however, with a maximum yield of 38.2% and a maximum entrapment of 54.6%.
Caffeine is a central nervous stimulant substance, has wide stimulating effect on central nervous system, can enhance the stimulation of cerebral cortex and cortex motor region, and is soluble in water and ethanol. Caffeine is widely present in tea, coffee, cocoa and other plants. The small dose of caffeine has effects of resisting oxidation, protecting heart blood vessel, promoting urination, relieving fatigue, and improving work efficiency. After the human body takes the caffeine, the peak value of blood concentration is reached about 40-50min, so that the sustained beneficial effect can be produced only by taking the caffeine for a plurality of times. However, large doses of caffeine can lead to adverse reactions such as symptoms of nervousness, palpitations, anxiety, tremors, muscle twitching, sleep disturbances, and the like. The action of caffeine can be delayed or prolonged by means of microcapsules, so that a continuous exciting effect is achieved.
Disclosure of Invention
In the prior art, when preparing the embedded hydrophilic compound nano microcapsule, the commonly used embedding methods mainly comprise methods such as multilayer emulsion, liposome, hydrogel and the like, and the methods have the technical problems of thermal instability, low embedding rate, non-edible material and the like. The invention firstly discovers that under the condition of proper proportion of wall material to core material, the core material (hydrophilic compound) can be successfully embedded in the wall material consisting of polysaccharide and protein by combining continuous ultrasonic and acidification treatments, so as to form the nano microcapsule with a core-shell or core-shell structure capable of embedding the hydrophilic compound.
Specifically, in order to solve the problems of unstable system heat, low embedding rate, non-edible material and the like in the prior art, the invention provides a specific scheme as follows:
according to the first aspect, the invention provides a preparation method of a nano microcapsule embedding a hydrophilic compound, which comprises the steps of taking protein and polysaccharide as wall materials, mixing the wall materials and the hydrophilic compound in water to form a mixed solution, and adjusting the pH value of the mixed solution to 3.4-4.5 in the process of treating the mixed solution with ultrasound to obtain the nano microcapsule with a core-shell structure and capable of embedding the hydrophilic compound.
The preparation method provided by the invention adopts food-grade wall materials and a physical treatment method, so that the process treatment difficulty is effectively reduced, and the pH of the mixed solution is changed while ultrasonic treatment is carried out, so that the polysaccharide and the protein serving as the wall materials form a compact nano microcapsule core-shell structure, and hydrophilic compounds dispersed in water are effectively embedded. The nano microcapsule prepared by the preparation method provided by the invention can be used in the fine processing fields of foods, medicines, health-care products and the like.
In the preparation method provided by the invention, the concentration of the protein is 0.3-10% and the concentration of the polysaccharide is 0.3-10% in percentage by mass and volume; the ultrasonic treatment is ultrasonic treatment at 100-750W for 1-5 min.
In the preparation method provided by the invention, the polysaccharide is carrageenin and/or chondroitin sulfate; the concentration of the polysaccharide is 1-3%.
In the preparation method provided by the invention, the protein is whey protein, bovine serum albumin, casein and/or egg white protein; the protein is whey protein; the concentration of the protein is 1-3%.
When the preparation method provided by the invention is used for preparing the hydrophilic compound nano-microcapsule, the hydrophilic compound accounts for 0.5-7% of the total weight of dry matter of the wall material, and a protein solution with the concentration of 1-3% is continuously added during the ultrasonic treatment process, so that the core-shell self-assembly hydrophilic compound nano-microcapsule can be formed.
In the preparation method provided by the invention, the hydrophilic compound is caffeine, coffee extract, anthocyanin, polysaccharide, oligopeptide, polypeptide, phycocyanin, cyclic nucleotide, cyclic adenosine monophosphate and/or terpenic acid compound.
In a second aspect, the present invention provides a nano-microcapsule for embedding hydrophilic compounds, which is prepared by the above preparation method.
In a third aspect, the present invention provides a hydrophilic compound nano-microcapsule prepared by the above method, wherein the particle size of the nano-microcapsule is 100-500nm, and the nano-microcapsule has a core-shell structure or a core-shell structure.
According to the understanding of the technical personnel in the field, the invention also claims the preparation method or the application of the nano microcapsule in the production of functional foods, functional health products or targeted therapeutic drugs.
Specifically, after sterilizing and canning the solution containing the nano-microcapsule, the beverage containing the hydrophilic compound nano-microcapsule is obtained;
or the solution containing the nano microcapsule is subjected to spray drying, and the air inlet temperature is as follows: 160 ℃ and 190 ℃, outlet temperature: collecting the bottom product at 70-90 deg.C to obtain hydrophilic compound nanometer microcapsule powder.
The invention also claims a method for preparing caffeine nano-microcapsule, which comprises the steps of putting whey protein, chondroitin sulfate and caffeine in water to form a mixed solution, wherein the concentration of the whey protein or the chondroitin sulfate is 0.3-3%; the caffeine accounts for 0.5-7% of the total weight of protein and polysaccharide dry matter; and (3) carrying out ultrasonic treatment on the mixed solution for 1-5min at the power of 100-750W, and adjusting the pH of the mixed solution to 4 to obtain the caffeine nano microcapsule.
In the preparation of the caffeine nano microcapsule, whey protein and chondroitin sulfate form a cavity under ultrasonic treatment, and the whey protein and the chondroitin sulfate are further crosslinked to form a nano capsule shell under an acidic environment, wherein the cavity of the nano capsule shell provides a space for embedding caffeine.
The invention has the beneficial effects that:
(1) the hydrophilic compound nano microcapsule prepared by the invention adopts food-grade materials as wall materials, and the protein and polysaccharide serving as the wall materials have high safety and good edible value;
(2) the particle size of the hydrophilic compound nano microcapsule prepared by the invention is 100-500nm, and the nano microcapsule has good dispersibility;
(3) by adopting the preparation method provided by the invention, hydrophilic compounds such as caffeine and the like can be effectively embedded to form a core-shell structure, and further the core-shell structure can be formed;
(4) the preparation method provided by the invention has a wide application range, and can be used for preparing water-soluble compound nano microcapsules such as anthocyanin, polysaccharide, functional oligosaccharide (oligosaccharide), polypeptide, protein, cyclic nucleotide, cyclic adenosine monophosphate, terpene acid compounds and the like in food.
Drawings
Fig. 1 is a scanning electron micrograph (left) and a projection electron micrograph (right) of the hydrophilic compound nano-microcapsule according to example 1 of the present invention.
FIG. 2 is a diagram of the effect of the hydrophilic compound nano-microcapsule prepared by the present invention.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention. It is intended that all modifications or alterations to the methods, procedures or conditions of the present invention be made without departing from the spirit and substance of the invention.
Unless otherwise specified, test materials, reagents, instruments and the like used in the examples of the present invention are commercially available; all technical measures in the examples of the present invention are conventional measures well known to those skilled in the art, unless otherwise specified.
Example 1
The embodiment provides a preparation method of caffeine nano-microcapsules, which comprises the following steps:
(1) preparation of nano-microcapsules
Dissolving protein, polysaccharide and caffeine in water, wherein the concentration of protein is 0.8%, the concentration of polysaccharide is 1.2%, and the content of caffeine is 1% of the total weight of protein and polysaccharide dry matter.
The polysaccharide is chondroitin sulfate; the protein is whey protein; coffee is an extract of coffee.
Immersing an ultrasonic probe into the mixed solution or ultrasonically treating the mixed solution for 3min under the condition of 500W by adopting an ultrasonic device;
and in the ultrasonic process, the pH value of the system is adjusted to 3.5 by adopting a 1% citric acid solution to obtain the nano microcapsule.
(2) Layer-by-layer self-assembly nano microcapsule
In order to further enhance the slow release effect of the nano-microcapsules, the protein solution can be continuously added in the continuous ultrasonic process of the solution to form the core-shell self-assembled nano-microcapsules, and the electron microscope scanning image of the prepared nano-microcapsules is shown in fig. 1. The caffeine mixed solution prepared in this example is shown in fig. 2.
The embedding rate of the finally obtained core-shell structured nano microcapsule is 81.5 percent, and the embedding rate of the core-shell structured nano microcapsule is 70.2 percent.
Example 2
The embodiment provides a preparation method of caffeine nano-microcapsules, which comprises the following steps:
(1) preparation of nano-microcapsules
Dissolving protein, polysaccharide and caffeine in water, wherein the concentration of protein is 0.3%, the concentration of polysaccharide is 0.5%, and the content of caffeine is 1% of the total weight of protein and polysaccharide dry matter.
The polysaccharide is chondroitin sulfate; the protein is whey protein.
Immersing an ultrasonic probe into the mixed solution or ultrasonically treating the mixed solution for 3min under the condition of 100W by adopting an ultrasonic device;
and in the ultrasonic process, the pH value of the system is adjusted to 3.5 by adopting a 1% citric acid solution to obtain the nano microcapsule.
(2) Layer-by-layer self-assembly nano microcapsule
In order to further enhance the slow release effect of the nano-microcapsules, the protein solution can be continuously added in the continuous ultrasonic process of the solution to form the core-shell self-assembled nano-microcapsules.
The embedding rate of the finally obtained core-shell structured nano microcapsule is 66.8 percent, and the embedding rate of the core-shell structured nano microcapsule is 60.3 percent.
Example 3
The embodiment provides a preparation method of caffeine nano-microcapsules, which comprises the following steps:
(1) preparation of nano-microcapsules
Dissolving protein, polysaccharide and caffeine in water, wherein the concentration of protein is 2%, the concentration of polysaccharide is 3%, and the content of caffeine is 0.5% of the total weight of protein and polysaccharide dry matter.
The polysaccharide is chondroitin sulfate; the protein is bovine serum albumin.
Immersing an ultrasonic probe into the mixed solution or ultrasonically treating the mixed solution for 4min under the condition of 750W by adopting an ultrasonic device;
and in the ultrasonic process, the pH value of the system is adjusted to 4.5 by adopting a 1% citric acid solution to obtain the nano microcapsule.
(2) Layer-by-layer self-assembly nano microcapsule
In order to further enhance the slow release effect of the nano-microcapsules, the protein solution can be continuously added in the continuous ultrasonic process of the solution to form the core-shell self-assembled nano-microcapsules.
The embedding rate of the finally obtained core-shell structured nano microcapsule is 89.5 percent, and the embedding rate of the core-shell structured nano microcapsule is 79.2 percent.
Example 4 anthocyanidin nanocapsules, phycocyanin nanocapsules
The present example provides anthocyanidin and phycocyanin as core materials to prepare nano-microcapsules. The solution preparation and nano-microcapsule preparation of this example are the same as those of example 1, except that the core material used in this example is anthocyanidin and phycocyanin.
The mixed solution of anthocyanins and phycocyanins prepared in this example is shown in fig. 2. It can be seen from fig. 2 that all three core materials exhibit a uniform and stable state, and fig. 2 demonstrates that the present invention as a general system achieves entrapment of hydrophilic compounds in foods or medicines. This example demonstrates the general applicability of the preparation method provided by the present invention to prepare embedded hydrophilic compound nano-microcapsules. The preparation method provided by the invention can be used for preparing the nano microcapsule embedding water-soluble compounds such as anthocyanin, polysaccharide, phycocyanin, functional oligosaccharide (oligosaccharide), polypeptide, protein, cyclic nucleotide, cyclic adenosine monophosphate, terpene acid compounds and the like in food.
EXAMPLE 5 Nannocapsule product
Sterilizing and canning the solution of the nano-microcapsules prepared in the embodiment 1 to obtain the caffeine-embedded beverage of the protein and polysaccharide nano-microcapsules; carrying out spray drying on the solution containing the nano microcapsule, wherein the air inlet temperature is as follows: 180 ℃, outlet temperature: and finally, collecting the bottom product at 80 ℃ to obtain the powder of the caffeine nano microcapsule.
Comparative example 1 different wall materials
In the comparative example, while acacia gum and whey protein were used as wall materials, and the caffeine nanocapsules were prepared in the same manner as in example 2, it was found that the microcapsules with caffeine successfully embedded could not be obtained, and the test showed that acacia gum could not form a shell of the microcapsules with caffeine embedded with whey protein.
Comparative example 2 different core and wall material ratios
The present comparative example provides a preparation method of a caffeine nano-microcapsule, which is the same as that of example 1 except that the concentration of protein in the mixed solution of the present comparative example is 2.7%, the concentration of polysaccharide is 0.3%, and the content of caffeine accounts for 8% of the total weight of protein and polysaccharide dry matter. The whole system can not be maintained uniformly and stably, and a large amount of precipitate is generated.
Comparative example 3 different ultrasound frequencies
The present comparative example provides a method for preparing caffeine nano-microcapsules, which is the same as in example 1, except that in the present comparative example, after the solutions are mixed, an ultrasonic probe is immersed in the mixed solution or an ultrasonic device is used to ultrasonically treat the mixed solution for 3min under the condition of 800W.
The embedding rate of the finally obtained core-shell structured nano microcapsule is 52.6 percent, and the embedding rate of the core-shell structured nano microcapsule is 46.1 percent. This comparative example demonstrates that ultra-high power sonication can cause microcapsule rupture, which is detrimental to the formation of caffeine nanocapsules.
Comparative example 4
The comparative example provides a preparation method of caffeine nano-microcapsule, which is the same as that of example 1, except that in the comparative example, after the solution is mixed, magnetic stirring is performed for 3min, and the pH value is adjusted during the magnetic stirring process. The test can not obtain the nanometer microcapsule with the core-shell or core-shell structure. This comparative example demonstrates that ultrasound produces cavitation, forming the spherical structure of the nanocapsule.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a nano microcapsule embedding a hydrophilic compound is characterized in that protein and polysaccharide are used as wall materials, the wall materials and the hydrophilic compound are mixed in water to form a mixed solution, and in the process of ultrasonic treatment of the mixed solution, the pH value of the mixed solution is adjusted to be 3.4-4.5, so that the nano microcapsule with a core-shell structure for embedding the hydrophilic compound is obtained.
2. The method according to claim 1, wherein the protein is present at a concentration of 0.3 to 10% and the polysaccharide is present at a concentration of 0.3 to 10% in mass volume percent; the ultrasonic treatment is ultrasonic treatment at 100-750W for 1-5 min.
3. The method according to claim 2, wherein the polysaccharide is carrageenan and/or chondroitin sulfate; the concentration of the polysaccharide is 1-3%;
the protein is whey protein, bovine serum albumin, casein and/or egg white protein; the concentration of the protein is 1-3%;
preferably, the protein is whey protein.
4. The preparation method according to any one of claims 1 to 3, wherein the hydrophilic compound accounts for 0.5 to 7 percent of the total dry weight of the wall material, and the protein solution with the concentration of 1 to 3 percent is continuously added during the ultrasonic treatment process to form the core-shell self-assembly hydrophilic compound nano-microcapsule.
5. The method according to claim 4, wherein the hydrophilic compound is caffeine, coffee extract, anthocyanin, polysaccharide, oligopeptide, polypeptide, phycocyanin, cyclic nucleotide, cyclic adenosine monophosphate, and/or terpenic acid compound.
6. A nano-microcapsule useful for entrapping a hydrophilic compound, which is prepared by the production method according to any one of claims 1 to 3.
7. Hydrophilic compound nano-microcapsules, characterized in that they are prepared by the preparation method of any one of claims 1-5, and have a particle size of 100-500nm and exhibit a core-shell structure or a core-shell structure.
8. Use of the preparation process according to any of claims 1 to 5 or of the nanocapsules according to claim 6 or of the hydrophilic compound nanocapsules according to claim 7 for the production of functional foods, functional health products or targeted therapeutic drugs.
9. Use according to claim 8, characterized in that a solution containing hydrophilic compound nanocapsules according to claim 7 is sterilized and canned to obtain a beverage containing hydrophilic compound nanocapsules;
or spray-drying the solution containing the hydrophilic compound nano-microcapsules of claim 7, the air inlet temperature: 160 ℃ and 190 ℃, outlet temperature: collecting the bottom product at 70-90 deg.C to obtain hydrophilic compound nanometer microcapsule powder.
10. A method for preparing caffeine nano-microcapsule is characterized in that whey protein, chondroitin sulfate and caffeine are put in water to form a mixed solution, wherein the concentration of the whey protein or the chondroitin sulfate is 1-3%; the caffeine accounts for 0.5-7% of the total weight of protein and polysaccharide dry matter; and (3) adjusting the pH of the mixed solution to 4 in the process of carrying out ultrasonic treatment on the mixed solution for 1-5min at the power of 100-750W to obtain the caffeine nano microcapsule.
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| PCT/CN2022/085851 WO2022252818A1 (en) | 2021-06-04 | 2022-04-08 | Hydrophilic compound-embedded nano microcapsule, and preparation method therefor and application thereof |
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