Animal feed based on nano material and preparation method thereof

Abstract

The invention relates to the field of preparation of animal feed, in particular to animal feed based on a nano material and a preparation method of the animal feed. According to the feed preparation method based on the nano material, the nano technology and the coating modification technology are adopted, and then the nano particles loaded with high-value feed ingredients are mixed with the feed base material in proportion, so that the transfer and release of the nutritional ingredients can be accurately controlled, and the nutritional benefits and economic benefits of the feed can be remarkably improved; the problem of nutrient waste in the prior art is solved, and a new solution is provided for the animal feed industry.

Description

Technical Field

[0001] The present invention relates to the field of animal feed preparation, and particularly relates to an animal feed based on nanomaterials and a preparation method thereof. Background Art

[0002] In the field of traditional animal feed, the absorption efficiency of nutritional components in the feed is low. The animal digestive system has a complex physiological structure, which leads to the fact that during the digestion process of the nutritional components in the feed, due to various factors such as indigestion and low transport efficiency, they cannot be completely absorbed and utilized by the animal body. A large amount of originally valuable nutritional components are excreted out of the body with feces, resulting in serious nutritional waste and the associated waste of feed resources. This not only increases the breeding cost but also is not conducive to the sustainable use of resources.

[0003] Currently, although there are already some methods in the industry aimed at enhancing the absorption of nutritional components in the feed, most of these methods focus on adding chemical additives or modifying the feed components. However, the use of chemical additives may bring potential safety risks and have adverse effects on animal health and the ecological environment; while modifying the feed components often makes it difficult to precisely control the release position and time of the nutritional components in the animal body, resulting in the nutritional components not reaching the action site at the most appropriate dose when the animal needs them most, thereby affecting the growth performance and health status of the animal.

[0004] Therefore, it is particularly urgent to develop a new feed preparation method that can deliver nutritional components to animals in a more efficient and precise manner while effectively avoiding waste and loss of nutritional components during the delivery process. Summary of the Invention

[0005] Aiming at the above existing technical problems, the present invention aims to provide an animal feed based on nanomaterials and a preparation method thereof. This animal feed is prepared by nanotechnology and film coating modification technology, and then the nanoparticles loaded with high-value feed components are mixed with the feed base material in a certain proportion, which can precisely control the transfer and release of nutritional components, significantly improve the nutritional and economic benefits of the feed, solve the problem of nutritional waste in the existing technology, and provide a new solution for the animal feed industry.

[0006] The present invention discloses a preparation method of an animal feed based on nanomaterials, including the following preparation steps:

[0007] S1: Dissolve poly(lactic-co-glycolic acid) in a solvent to form a uniform sol solution, then add vitamins, minerals, and amino acids, stir evenly to form a coating system; then heat to remove the solvent and gel to obtain nanoparticles;

[0008] S2: Dissolve the poly (lactic - co - glycolic acid) copolymer in dichloromethane to form a mixed solution. Disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly drop it into the mixed solution for ultrasonic treatment. Then, after centrifugation to remove impurities and washing, surface - modified nanoparticles are obtained. Lysine is grafted onto the surface of the nanoparticles through an amino coupling reaction to obtain modified nanoparticles;

[0009] S3: Perform a film - coating treatment on the modified nanoparticles prepared in step S2; then mix the film - coated modified nanoparticles with the feed base material to make animal feed pellets.

[0010] Preferably, in step S1, the solvent is ethanol; the temperature for heating to remove the solvent and gelation is 40 - 60 °C.

[0011] Preferably, in step S2, the mass ratio of the nanoparticles to the poly (lactic - co - glycolic acid) copolymer is 1:(5 - 8).

[0012] Preferably, in step S2, the ultrasonic frequency of the ultrasonic treatment is 20 - 40 kHz; the ultrasonic time is 10 - 20 min.

[0013] Preferably, in step S2, the centrifugation rate is 3000 - 5000 rpm, and the time is 3 - 5 min.

[0014] Preferably, in step S2, the temperature of the amino coupling reaction is 30 - 35 °C; the reaction time is 2 - 4 h; the pH value of the reaction solution is 7.5 - 8.5.

[0015] Preferably, in step S2, the coupling agent used in the amino coupling reaction is a bifunctional dynamic conjugate coupling agent.

[0016] Preferably, in step S3, the membrane material used for the film - coating treatment is a pH - responsive modified chitosan copolymer.

[0017] Preferably, in step S3, the mass ratio of the film - coated modified nanoparticles to the feed base material is 1:(10 - 15).

[0018] An animal feed pellet, which is an animal feed pellet prepared by the preparation method of any one of the above animal feeds based on nanomaterials.

[0019] Compared with the prior art, the beneficial effects of the present invention are:

[0020] The present invention provides an animal feed based on nanomaterials and its preparation method, having the following advantages:

[0021] (1) After wrapping nutritional components with nanoparticles, their degradation and loss in the animal digestive system can be effectively avoided. Nanoparticles have a high surface area and biocompatibility, which can improve the absorption efficiency and bioavailability of nutritional components.

[0022] (2) By modifying and coating the nanoparticles, precise release at specific sites in the animal body can be achieved through controlling the structure and functionalization of the nanoparticles, avoiding premature release or waste of nutritional components at unnecessary sites.

[0023] (3) Lysine is conjugated with nanoparticles through a bifunctional dynamic conjugate coupling agent, avoiding non-specific conjugation of multiple amino groups in traditional lysine and reducing by-products; the dynamic covalent bond can break under specific pH condition changes to achieve controllable drug release; compared with traditional copper-catalyzed click chemistry, it reduces cytotoxicity.

[0024] (4) The animal feed prepared by mixing such nanoparticles with feed base materials effectively avoids damage to high-value components in the animal feed, improves the nutritional absorption and utilization rate of animals, improves the animal feeding efficiency, and reduces the feed cost. Moreover, the non-toxicity and biodegradability of this animal feed ensure its safety during long-term use and will not cause pollution to animals and the environment. Detailed implementation mode

[0025] The following embodiments are provided to better further understand the present invention, which are not limited to the best implementation mode, and do not constitute limitations on the content and protection scope of the present invention. Any product that is the same as or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other existing technologies falls within the protection scope of the present invention.

[0026] For those steps or conditions not specified in the embodiments, the operations or conditions of the conventional experimental steps described in the literature in this field can be followed. For the reagents or instruments without indicating the manufacturer, they are all conventional reagent products that can be obtained through commercial purchase.

[0027] Example 1: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0028] S1: Dissolve poly(lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals and amino acids, stir evenly to form a coating system; then heat to 40 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0029] S2: Dissolve the poly (lactic - co - glycolic acid) copolymer in dichloromethane to form a mixed solution, where the mass ratio of the nanoparticles to the poly (lactic - co - glycolic acid) copolymer is 1:5; Disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly add it dropwise to the mixed solution for ultrasonic treatment. The ultrasonic frequency of the ultrasonic treatment is 20 kHz; The ultrasonic time is 10 min. Then set the centrifugation rate to 3000 rpm and the time to 3 min. After centrifugation for impurity removal and washing, surface - modified nanoparticles are obtained; Graft lysine onto the surface of the nanoparticles through an amino coupling reaction, where the temperature of the amino coupling reaction is set to 30 °C; The reaction time is 2 h; The pH value of the reaction solution is 7.5, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0030] S3: Perform a film - coating treatment on the modified nanoparticles prepared in step S2, where the film - material used during film - coating is a pH - responsive modified chitosan copolymer; Then mix the film - coated modified nanoparticles with the feed base material in a mass ratio of 1:10 and mix evenly to make animal feed pellets.

[0031] Example 2: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0032] S1: Dissolve poly (lactic - co - glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals, and amino acids, and stir evenly to form a coating system; Then heat to 45 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0033] S2: Dissolve the poly (lactic - co - glycolic acid) copolymer in dichloromethane to form a mixed solution, where the mass ratio of the nanoparticles to the poly (lactic - co - glycolic acid) copolymer is 1:5.5; Disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly add it dropwise to the mixed solution for ultrasonic treatment. The ultrasonic frequency of the ultrasonic treatment is 25 kHz; The ultrasonic time is 12 min. Then set the centrifugation rate to 3500 rpm and the time to 3.5 min. After centrifugation for impurity removal and washing, surface - modified nanoparticles are obtained; Graft lysine onto the surface of the nanoparticles through an amino coupling reaction, where the temperature of the amino coupling reaction is set to 31 °C; The reaction time is 2.5 h; The pH value of the reaction solution is 7.7, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0034] S3: Perform a film - coating treatment on the modified nanoparticles prepared in step S2, where the film - material used during film - coating is a pH - responsive modified chitosan copolymer; Then mix the film - coated modified nanoparticles with the feed base material in a mass ratio of 1:11 and mix evenly to make animal feed pellets.

[0035] Example 3: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0036] S1: Dissolve poly(lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals, and amino acids, stir evenly to form a coating system; then heat to 50 °C to remove the solvent ethanol and then gel to obtain nanoparticles.

[0037] S2: Dissolve poly(lactic-co-glycolic acid) copolymer in dichloromethane to form a mixed solution, wherein the mass ratio of the nanoparticles to the poly(lactic-co-glycolic acid) copolymer is 1:6; disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly drop it into the mixed solution for ultrasonic treatment, the ultrasonic frequency of the ultrasonic treatment is 30 kHz; the ultrasonic time is 15 min. Then set the centrifugation rate to 4000 rpm and the time to 4 min, and after centrifugal impurity removal and washing, surface-modified nanoparticles are obtained; lysine is grafted onto the surface of the nanoparticles through an amino coupling reaction, wherein the temperature of the amino coupling reaction is set to 32 °C; the reaction time is 3 h; the pH value of the reaction solution is 7.9, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0038] S3: Perform a film coating treatment on the modified nanoparticles prepared in step S2, wherein the film material used during film coating is a pH-responsive modified chitosan copolymer; then uniformly mix the film-coated modified nanoparticles with the feed base material at a mass ratio of 1:12 to make animal feed pellets.

[0039] Example 4: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0040] S1: Dissolve poly(lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals, and amino acids, stir evenly to form a coating system; then heat to 55 °C to remove the solvent ethanol and then gel to obtain nanoparticles.

[0041] S2: Dissolve poly(lactic-co-glycolic acid) copolymer in dichloromethane to form a mixed solution, wherein the mass ratio of the nanoparticles to the poly(lactic-co-glycolic acid) copolymer is 1:7; disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly drop it into the mixed solution for ultrasonic treatment, the ultrasonic frequency of the ultrasonic treatment is 35 kHz; the ultrasonic time is 17 min. Then set the centrifugation rate to 4500 rpm and the time to 4.5 min, and after centrifugal impurity removal and washing, surface-modified nanoparticles are obtained; lysine is grafted onto the surface of the nanoparticles through an amino coupling reaction, wherein the temperature of the amino coupling reaction is set to 33 °C; the reaction time is 3.5 h; the pH value of the reaction solution is 8.1, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0042] S3: Perform a film coating treatment on the modified nanoparticles prepared in step S2. Among them, the film material used during film coating is a pH-responsive modified chitosan copolymer; then mix the film-coated modified nanoparticles and the feed base material evenly according to a mass ratio of 1:13 and make animal feed pellets.

[0043] Example 5: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0044] S1: Dissolve poly(lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals, and amino acids, stir evenly to form a coating system; then heat to 60 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0045] S2: Dissolve poly(lactic-co-glycolic acid) in dichloromethane to form a mixed solution. Among them, the mass ratio of the nanoparticles to poly(lactic-co-glycolic acid) is 1:8; disperse the nanoparticles prepared in step S1 in dichloromethane and slowly add it dropwise to the mixed solution for ultrasonic treatment. The ultrasonic frequency of the ultrasonic treatment is 40 kHz; the ultrasonic time is 20 min. Then set the centrifugation rate to 5000 rpm and the time to 5 min. After centrifugation to remove impurities and washing, surface-modified nanoparticles are obtained; lysine is grafted onto the surface of the nanoparticles through an amino coupling reaction. Among them, set the temperature of the amino coupling reaction to 35 °C; the reaction time is 4 h; the pH value of the reaction solution is 8.5, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0046] S3: Perform a film coating treatment on the modified nanoparticles prepared in step S2. Among them, the film material used during film coating is a pH-responsive modified chitosan copolymer; then mix the film-coated modified nanoparticles and the feed base material evenly according to a mass ratio of 1:15 and make animal feed pellets.

[0047] Example 6: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0048] S1: Dissolve poly(lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals, and amino acids, stir evenly to form a coating system; then heat to 60 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0049] S2: Dissolve the poly (lactic-co-glycolic acid) copolymer in dichloromethane to form a mixed solution, where the mass ratio of the nanoparticles to the poly (lactic-co-glycolic acid) copolymer is 1:8; Disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly add it dropwise to the mixed solution for ultrasonic treatment. The ultrasonic frequency of the ultrasonic treatment is 40 kHz; The ultrasonic time is 20 min. Then set the centrifugation rate to 5000 rpm and the time to 5 min. After centrifugation for impurity removal and washing, surface-modified nanoparticles are obtained.

[0050] S3: Perform a film coating treatment on the modified nanoparticles prepared in step S2, where the film material used during film coating is a pH-responsive modified chitosan copolymer; Then mix the film-coated modified nanoparticles and the feed base material evenly at a mass ratio of 1:15 and make them into animal feed pellets.

[0051] Example 7: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0052] S1: Dissolve poly (lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals and amino acids, and stir evenly to form a coating system; Then heat to 60 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0053] S2: Dissolve the poly (lactic-co-glycolic acid) copolymer in dichloromethane to form a mixed solution, where the mass ratio of the nanoparticles to the poly (lactic-co-glycolic acid) copolymer is 1:8; Disperse the nanoparticles prepared in step S1 in dichloromethane and then slowly add it dropwise to the mixed solution for ultrasonic treatment. The ultrasonic frequency of the ultrasonic treatment is 40 kHz; The ultrasonic time is 20 min. Then set the centrifugation rate to 5000 rpm and the time to 5 min. After centrifugation for impurity removal and washing, surface-modified nanoparticles are obtained; Graft lysine onto the surface of the nanoparticles through an amino coupling reaction, where the temperature of the amino coupling reaction is set to 35 °C; The reaction time is 4 h; The pH value of the reaction solution is 8.5, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, and finally modified nanoparticles are obtained.

[0054] S3: Mix the modified nanoparticles prepared in step S2 and the feed base material evenly at a mass ratio of 1:15 and make them into animal feed pellets.

[0055] Example 8: A preparation method of an animal feed based on nanomaterials, comprising the following steps:

[0056] S1: Dissolve poly (lactic-co-glycolic acid) in ethanol to form a uniform sol solution, then add vitamins, minerals and amino acids, and stir evenly to form a coating system; Then heat to 60 °C to remove the solvent ethanol and gel to obtain nanoparticles.

[0057] S2: Graft lysine onto the surface of the nanoparticles prepared in step S1 through amino coupling reaction, where the temperature of the amino coupling reaction is set at 35 °C, the reaction time is 4 h, the pH value of the reaction solution is 8.5, and the coupling agent used is a bifunctional dynamic conjugate coupling agent, finally obtaining modified nanoparticles.

[0058] S3: Conduct film coating treatment on the modified nanoparticles prepared in step S2, where the film material used during film coating is a pH-responsive modified chitosan copolymer; then mix the film-coated modified nanoparticles with the feed base material evenly at a mass ratio of 1:15 to make animal feed pellets.

[0059] Animal experiments were conducted on the animal feed pellets prepared in Examples 1 - 8 and the control group, where the control group is a commercially available ordinary animal feed, and the experimental design table is as follows:

[0060]

[0061] The experimental results of the above animal experiments are shown in the following table, where the nutritional targeting index is (intestinal fluid release / gastric fluid release):

[0062]

[0063] The release rate of Example 5 in gastric fluid is only 4.2%, and reaches 88.9% in intestinal fluid, with a targeting index of 21.2, proving that the pH-responsive chitosan copolymer film coating (S3) can effectively shield the gastric acid environment and achieve precise release in the intestine. The gastric fluid release rate of Example 7 without film coating soars to 32.7%, indicating that the uncoated nanoparticles disintegrate rapidly in gastric acid, resulting in nutrient waste.

[0064] Through lysine surface modification (S2) in Example 5, the nutritional bioavailability reaches 80.3%, significantly higher than that of unmodified Example 6 (55.2%) and Example 8 (45.8%), proving that the bifunctional coupling agent can enhance the binding strength between nutrient molecules and nanoparticles.

[0065] As the gelation temperature in S1 increases, the particle size uniformity of the nanoparticles improves, and the intestinal fluid release rate of Example 5 is 16.4% higher than that of Example 1. The optimization of the ultrasonic frequency and centrifugation rate in S2 improves the dispersion of the nanoparticles, and the nutrient waste rate of Example 5 is as low as 4.8%.

[0066] Compared with the data of Example 7, the bioavailability of Example 5 is increased by 90.7%; compared with the data of Example [missing ID in the original], the bioavailability of Example 5 is increased by 75.3%, proving that the synergistic effect of film coating + surface modification is crucial for nutrient controlled release.

[0067] The principle of spatial control of the animal feed pellets prepared by the present invention is as follows: the pH-responsive membrane remains closed in gastric juice (pH < 4), and after entering the intestine (pH > 6), the amino protons of chitosan are protonated, and the membrane structure is decomposed to release nutrients. The principle of time control is as follows: the degradation rate of the nanoparticle core (polylactic acid-glycolic acid) is dynamically matched with the membrane pore size to achieve a sustained release for 6 hours. The lysine layer on the surface of this animal feed pellet adsorbs nutrient molecules through electrostatic interaction, reducing leakage during the preparation process. The core-shell structure avoids direct contact between nutrient molecules and digestive enzymes, greatly reducing the waste rate.

[0068] Obviously, the above embodiments are merely examples for clear illustration and not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or variations can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or variations derived therefrom are still within the protection scope of the present invention.

Claims

1. A preparation method of an animal feed based on nanomaterials, characterized in that, It includes the following steps: S1: Dissolve poly(lactic-co-glycolic acid) in a solvent to form a uniform sol solution, then add vitamins, minerals and amino acids, stir evenly to form a coating system; then heat to remove the solvent and gel to obtain nanoparticles; S2: Dissolve poly(lactic-co-glycolic acid) in dichloromethane to form a mixed solution, disperse the nanoparticles prepared in step S1 in dichloromethane and slowly add it to the mixed solution for ultrasonic treatment, and then centrifuge to remove impurities and wash to obtain surface-modified nanoparticles; graft lysine onto the surface of the nanoparticles through an amino coupling reaction to obtain modified nanoparticles; S3: Perform a film coating treatment on the modified nanoparticles prepared in step S2; then mix the film-coated modified nanoparticles with a feed base material to make animal feed pellets.

2. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S1, the solvent is ethanol; the temperature for heating to remove the solvent and gel is 40 - 60 °C.

3. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S2, the mass ratio of the nanoparticles to poly(lactic-co-glycolic acid) is 1:(5 - 8).

4. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S2, the ultrasonic frequency of the ultrasonic treatment is 20 - 40 kHz; the ultrasonic time is 10 - 20 min.

5. The preparation method of an animal feed based on nanomaterials according to claim 1, wherein, In step S2, the centrifugation rate is 3000 - 5000 rpm and the time is 3 - 5 min.

6. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S2, the temperature of the amino coupling reaction is 30 - 35 °C; the reaction time is 2 - 4 h; the pH value of the reaction solution is 7.5 - 8.

5.

7. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S2, the coupling agent used in the amino coupling reaction is a bifunctional dynamic conjugate coupling agent.

8. The preparation method of an animal feed based on nanomaterials according to claim 7, characterized in that, In step S3, the film material used for the film coating treatment is a pH-responsive modified chitosan copolymer.

9. The preparation method of an animal feed based on nanomaterials according to claim 1, characterized in that, In step S3, the mass ratio of the film-coated modified nanoparticles to the feed base material is 1:(10 - 15).

10. An animal feed prepared by the preparation method of an animal feed based on nanomaterials according to any one of claims 1 - 9.

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