CN115024365A - Application of fullerene to preparation of fullerene microcapsule powder and preparation method - Google Patents
Application of fullerene to preparation of fullerene microcapsule powder and preparation method Download PDFInfo
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- CN115024365A CN115024365A CN202210449776.6A CN202210449776A CN115024365A CN 115024365 A CN115024365 A CN 115024365A CN 202210449776 A CN202210449776 A CN 202210449776A CN 115024365 A CN115024365 A CN 115024365A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
- A23D7/04—Working-up
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/80—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in fisheries management
- Y02A40/81—Aquaculture, e.g. of fish
- Y02A40/818—Alternative feeds for fish, e.g. in aquacultures
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Abstract
The invention belongs to the field of feed, and discloses application of fullerene to preparation of fullerene micro-capsule powder and a preparation method thereof. Meanwhile, the food can be ingested in a food mode, and the taste and the ingestion mode are more flexible and diversified. The microcapsule powder prepared from the raw materials can greatly improve the application field of the microcapsule powder.
Description
The application is a divisional application, the application number of the original application is 201811365406.4, the application date is 2018, 11 and 16, and the name is fullerene livestock and poultry feed additive and a preparation method and feed thereof. Since the original application enjoys priority over application No. 201810259287.8, entitled "use of fullerene for preparation of fullerene microcapsule powder", filed on 27.3.2018, the present application enjoys priority over application No. 201810259287.8, entitled "use of fullerene for preparation of fullerene microcapsule powder", filed on 27.3.2018, and the entire contents of the patent application are incorporated herein by reference.
Technical Field
The invention belongs to the field of feeds, and particularly relates to application of fullerene to preparation of fullerene micro-capsule powder and a preparation method of the fullerene micro-capsule powder.
Background
Fullerene is a carbon atom cluster consisting of 60 carbon atoms, and is an allotrope of graphite and diamond. Can be compatible with free radicals, and has strong oxidation resistance. Due to the biological activities of antivirus, antioxidation, antibiosis and the like, the fullerene is widely applied to daily life and social production of people, such as cosmetics, drug carriers, medical diagnosis and other fields. An article published by the french Fathi Moussa research group on Biomaterials in 2011 published significant findings: when C60 was dispersed in olive oil and fed to mice, C60 was found to have no chronic toxicity and could extend the life of the mice by more than 90%. In studies on neurodegenerative diseases caused by the deposition of amyloid fibrils, such as senile dementia and Parkinson's disease, it has been found that fullerene is effective in preventing the formation of amyloid fibrils. In the research of liver cancer, the research shows that the injection of the fullerene water-soluble derivative into the abdominal cavity is compared with the anti-cancer drugs CTX and cissplatin, and the research shows that after the injection of the fullerene derivative, the tumor is greatly inhibited, the concentration increasing effect is improved, and the effect is equivalent to that of CTX when the amount of the fullerene water-soluble derivative is 1/500 of CTX; fullerene derivatives are much more effective than cissplatin.
The microcapsule technology is a technology in which a solid or liquid is coated with a film-forming material to form fine particles. The oil microcapsule powder is a food raw material which develops very rapidly in recent years, has the excellent characteristics of common oil, and can provide energy and improve the flavor and mouthfeel of food; in addition, the microcapsule powder can overcome the application defects of the traditional grease, such as the prevention of oxidation and deterioration of certain unstable food raw and auxiliary materials. In terms of storage stability, the oil particles are wrapped with a film formed of an embedding agent, and therefore, the oil particles have thermal stability against rancidity. Fullerene is insoluble in water, which limits its development and application. In the application of fullerene, the fullerene is mainly prepared into water-soluble derivatives, such as hydrated fullerene, fullerol, fullerene-vitamin C, metal fullerene and the like; has prominent expression in the treatment of liver cancer, kidney cancer, neurodegenerative diseases and the like. Therefore, the development of more suitable and flexible use of fullerene is urgently needed.
Fullerene (Fullerene) is the third allotrope found in elemental carbon. Any substance consisting of carbon, in a spherical, ellipsoidal or tubular structure, can be called fullerene, which refers to a class of substances. At present, the preparation method of fullerene mainly comprises an electric arc method, a thermal evaporation method, a combustion method, a chemical vapor deposition method and the like. C 60 The molecules have aromaticity, and are reddish brown when dissolved in benzene. C 60 The compound has scientific value and application prospect, and has certain significance in the fields of life science, medicine, celestial physics and the like. In the fullerene, C 60 And C 70 Is the most common, but also mass-producible fullerene.
For fullerene C 60 The research on the application of nano materials is always the most concerned focus of scientific researchers. Research shows that the fullerene C 60 The nano material has potential application value in the aspects of optics, electricity, material science and the like, and has very wide application prospect in the aspects of organic solar cells, catalysis, biomedicine and the like.
The fullerene has multiple excellent performances, contains various bioactive substances and functional factors, and has high medical and health-care values. The functional fullerene is applied to the cosmetic market by utilizing the performance of efficiently removing free radicals of the fullerene, and has a wide development prospect. At present, fullerene is used as a feed additive in the feeding of livestock and poultry and is matched with other components to be used as the feed additive, but no related technical report exists.
The feed additive can promote animal growth, improve animal product quality, improve livestock and poultry disease resistance, and increase animal husbandry profit. However, with the development of animal husbandry, the feed additive is abused in animal feed, which causes many problems of food quality safety and causes large-scale livestock and poultry diseases. With the continuous occurrence of food safety problems, people worry about potential safety hazards brought to human beings by using antibiotics, so that the research and development of novel, safe, non-toxic and side-effect and non-residual feed additives are particularly important.
Disclosure of Invention
The first purpose of the invention is to provide the application of fullerene used for preparing fullerene microcapsule powder and a preparation method thereof.
In order to achieve the purpose, the invention provides a use of fullerene used for preparing fullerene microcapsule powder.
Further, the fullerene comprises C60 and derivatives thereof, C70 and derivatives thereof, fullerene metal derivatives, and fullerene oil solution.
Further, the fullerene microcapsule powder contains fullerene, nutrient compound oil, an edible emulsifier and wall materials.
Furthermore, the weight consumption of the fullerene is 1-5 per mill.
Further, the weight amount of the nutrient compound oil is 50-70%;
optionally, the amount of the edible emulsifier is 4-6% of the weight content of fat in the nutritional compound oil; preferably, the edible emulsifier is used in an amount of 5% by weight of the fat content;
optionally, the weight amount of the wall material is 29-49%.
Further, the fat fatty acid proportion of the nutrient compound oil is that the saturated fatty acid: monounsaturated fatty acids: the polyunsaturated fatty acid is 1 (0.5-2) to (0.5-2), wherein the linoleic acid in the polyunsaturated fatty acid: linolenic acid is 1 (0.5-2);
preferably, the fat fatty acid proportion of the nutrient compound oil is that of saturated fatty acid: monounsaturated fatty acids: the polyunsaturated fatty acid is 1 (0.5-1.5) to (0.5-1.5), wherein the weight ratio of linoleic acid in the polyunsaturated fatty acid is as follows: linolenic acid is 1 (0.5-1.5);
more preferably, the fat fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acids: the polyunsaturated fatty acid is 1:1:1, wherein the ratio of linoleic acid in the polyunsaturated fatty acid: linolenic acid is 1: 1.
Further, the nutritional compound oil is a combination of more than two of linseed oil, safflower seed oil, perilla seed oil, camellia oleifera seed oil, sunflower seed oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, sea buckthorn fruit oil, sea buckthorn seed oil, peony seed oil, walnut oil, shinyleaf yellowhorn oil, sea buckthorn oil, hemp seed oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid and conjugated linoleic acid triglyceride.
Further, the edible emulsifier is A or a mixture of A and B; wherein A is 1 or 2 of oligomeric maltose, maltodextrin, solid corn syrup, fructo-oligosaccharide, resistant dextrin, and skimmed milk powder; b is one of sodium caseinate, mono-diglycerol fatty acid ester, starch sodium octenylsuccinate, ascorbic acid, sodium ascorbate, gelatin, polydextrose, phospholipid, natural vitamin E, sodium tripolyphosphate, acacia and ascorbyl palmitate;
optionally, the wall material is formed by mixing 2 or more than 3 of soybean protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose and maltodextrin.
Further, the preparation method of the microcapsule powder comprises the following steps,
preparing an oil phase: preparing nutrient compound oil according to the proportion of fatty acid, and then dissolving fullerene into the nutrient compound oil after sterilizing to form a compound oil compound; dissolving an edible emulsifier into the compound oil compound to obtain an oil phase;
preparation of an aqueous phase: dissolving the wall material in hot water to obtain a water phase; preferably, the temperature of the hot water is 60-80 ℃; wherein the dissolution is incomplete at a temperature below 60 ℃, and the effective components are easily damaged at a temperature above 80 ℃;
mixing and sterilizing: mixing the obtained water phase and oil phase, stirring, and sterilizing;
homogenizing, spraying and drying: homogenizing, spraying, and drying to obtain fullerene microcapsule powder.
Furthermore, the microcapsule powder has the functions of improving the oxidation resistance, and/or improving the immunity, and/or preventing cancers, delaying neurodegenerative diseases, and/or relieving alcoholism.
Fullerene is not completely dissolved in the fat and oil, and the amount of fullerene added is not proportional to the solubility. If the dissolution is extremely small, the process is simple, the cost is low, but the amount of the ingested microcapsule powder is correspondingly increased, the amount of the ingested oil is correspondingly increased, and the requirement of human nutrition is not met; if the amount of the fullerene dissolved is high, the process is complicated, the technical difficulty is high, and the cost of the fullerene is increased greatly. Through hard labor, the applicant finds that when the addition amount of the fullerene is 1-5 per mill, the fullerene can be dissolved by a simple stirring mode; when the addition amount is more than 5 per mill, the fullerene is not completely dissolved by stirring, insoluble fullerene is obtained by centrifugal treatment, and the residual fullerene is not easy to clean. Meanwhile, through experiments on the effect, the remarkable antioxidant effect can be shown if the intake of the fullerene is 8 mg/day/person.
When the addition amount of the nutritional compound oil is less than 50%, the contained nutritional component oil is less, and the taste is poor; when the addition amount of the nutrient compound oil is more than 70%, the wall of the oil is easy to break, the embedding effect is poor, the brewing is influenced, and the produced microcapsule powder is easy to agglomerate and agglomerate.
The nutritional compound oil is prepared by compounding 2 or more than 3 of linseed oil, safflower seed oil, perilla seed oil, camellia seed oil, sunflower seed oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, sea buckthorn fruit oil, sea buckthorn seed oil, peony seed oil, walnut oil, shinyleaf yellowhorn oil, cannabis oil, linoleic acid, linolenic acid triglyceride, conjugated linoleic acid triglyceride and the like according to the proportion of fatty acid.
The wall material is prepared by mixing 2 or more than 3 of soybean protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose and maltodextrin.
The edible emulsifier is A or a mixture of A and B; wherein A is 1 or 2 of oligomeric maltose, maltodextrin, solid corn syrup, fructo-oligosaccharide, resistant dextrin, and skimmed milk powder; b is prepared from 2 or more than 3 of sodium caseinate, mono-diglycerol fatty acid ester, starch sodium octenylsuccinate, ascorbic acid, sodium ascorbate, polydextrose, phospholipid, natural vitamin E, sodium tripolyphosphate, acacia, and ascorbyl palmitate by mixing. The edible emulsifier is generally about 5% of the fat content, and the composite use can achieve the ideal effects of high stability, good water solubility, good loose property of the microcapsule powder, and difficult caking and agglomeration.
The fullerene is prepared into the microcapsule powder and then can be taken in a food mode, and the taste and the taking mode are more flexible and various. The microcapsule powder prepared from the raw materials can greatly improve the application field of the microcapsule powder. The fullerene microcapsule powder is prepared by adopting food raw materials as wrapping materials, is transformed into a nutritional beverage which is convenient to eat and has various flavors, can be taken for a short time or a long time, has the health-care effects of resisting aging and inhibiting cancers, and has extremely high popularization value.
The second purpose of the invention is to provide a novel fullerene livestock and poultry feed additive, a preparation method thereof and a feed.
The fullerene livestock and poultry feed additive comprises 20-90 wt% of fullerene microcapsule powder, 3-20 wt% of vitamins, 0.05-30 wt% of prebiotics and 0.5-30 wt% of shell powder, wherein the total weight of the fullerene livestock and poultry feed additive is taken as a reference.
Preferably, the fullerene microcapsule powder contains a fullerene compound, nutritional compound oil, an edible emulsifier and a wall material.
Preferably, the total weight content of the fullerene compound and the nutrient composite oil is 10-80 wt% and 0.1-5 wt% of the fullerene compound, the weight content of the edible emulsifier is 0.01-5 wt%, and the weight content of the wall material is 0.01-80 wt% based on the total weight of the fullerene microcapsule powder.
Preferably, the weight content of the fullerene compound is 1-5 wt%, the weight content of the nutritional compound oil is 50-70 wt%, the weight content of the edible emulsifier is 4-6 wt% of the weight content of fat in the nutritional compound oil, and the weight content of the wall material is 29-49 wt% based on the total weight of the fullerene microcapsule powder.
Preferably, the fullerene compound may be C 60 And derivatives thereof, C 70 And at least one of a derivative thereof, a fullerene metal derivative, a fullerene oxygen-containing derivative, a fullerene modified or included with an organic compound, and a fullerene derivative modified or included with an organic compound. Wherein the oxygen atom in the fullerene oxygen-containing derivative is connected with the carbon atom on the fullerene skeleton or bonded with the alkylene chain. The organic substance in the fullerene and fullerene derivative modified or included by the organic compound may be any of various organic oligomers capable of forming an inclusion or complex, such as cyclodextrin and/or crown ether.
The nutrient compound oil is at least one selected from edible oil, oil-soluble vitamins, hydrocarbons, fatty acids, higher alcohols and esters. Wherein the edible oil comprises vegetable oil and animal oil. The vegetable oil is preferably at least one selected from soybean oil, rapeseed oil, palm oil, olive oil, sunflower seed oil, shinyleaf yellowhorn oil, sea buckthorn seed oil, corn oil, safflower oil, perilla seed oil, tea seed oil, camellia seed oil, cottonseed oil, coconut oil, sesame oil, linseed oil, pumpkin seed oil, peony seed oil, sea buckthorn fruit oil, walnut oil, red pine kernel oil, evening primrose oil, safflower seed oil, borage oil, hemp seed oil, salad oil, wheat germ oil, avocado oil and sea buckthorn oil. The animal oil is preferably at least one selected from the group consisting of lard, tallow, mutton fat, fish oil, horse oil and turtle oil. The hydrocarbon is preferably squalane and/or squalene. The fatty acid is preferably at least one selected from the group consisting of oleic acid, linoleic acid, linolenic acid, conjugated linoleic acid, DHA, stearic acid, lauric acid, arachidonic acid, and EPA. The higher alcohol is preferably at least one selected from the group consisting of octyldodecanol, lauryl alcohol, phytosterol, cholesterol and stearyl alcohol. The esters are preferably conjugated linoleic acid triglyceride and/or linoleic acid glyceride. Most preferably, the nutritional compound oil is a combination of more than two of linseed oil, safflower seed oil, perilla seed oil, camellia oleifera seed oil, sunflower seed oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, sea buckthorn fruit oil, sea buckthorn seed oil, peony seed oil, walnut oil, shinyleaf yellowhorn oil, sea buckthorn oil, hemp seed oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid and conjugated linoleic acid triglyceride.
The edible emulsifier can be a substance which has hydrophilicity and lipophilicity in various existing molecular structures and surface activity due to the amphiphilicity, and can be an anionic surfactant, a cationic surfactant, a nonionic surfactant or an amphoteric surfactant. Specific examples of the edible emulsifier include, but are not limited to: at least one of sucrose fatty acid ester, polyglycerol fatty acid ester, glycerol fatty acid ester, polyoxyethylene sorbitan fatty acid ester, sodium caseinate, lecithin, sodium stearate, monoglyceride organic acid fatty acid ester, betaine, amino acid salt, succinic acid glycerol fatty acid ester, sodium stearoyl lactylate, tween-80, span-80, polyglycerol ester, propylene glycol fatty acid ester and polysorbate fatty acid ester; or the edible emulsifier is A or a mixture of A and B, the A is one or two of fructo-oligosaccharide, resistant dextrin and skimmed milk powder, and the B is one of sodium caseinate, mono-diglycerol fatty acid ester, sodium starch octenyl succinate, ascorbic acid, sodium ascorbate, phospholipid, natural vitamin E, sodium tripolyphosphate and ascorbyl palmitate.
The wall material has the function of forming a film with certain strength and improving the microencapsulation efficiency. The wall material is preferably a water-soluble polymer material, and specifically may be selected from maltodextrin (DE18 or DE20), Soy Protein Isolate (SPI), acacia (GA), β -cyclodextrin, starch (corn starch, modified starch, porous starch, methylhydroxypropyl starch), Whey Protein Concentrate (WPC), dextrin, corn syrup, gelatin, sodium carboxymethylcellulose (CMC), xanthan gum, agar, carrageenan, chitosan, starch octenyl succinate, guar gum, algin, and alginate, at least one of milk protein, casein, mucedin, gliadin, cocoa butter replacer, caseinic acid (SC), vegetable protein, lactose, sucrose, maltose, methyl cellulose, ethyl cellulose, methylhydroxypropyl cellulose, carboxymethyl cellulose, hydroxymethyl cellulose, hydroxypropyl cellulose, crystalline cellulose, and water-soluble dietary fiber. Preferably, the wall material is formed by mixing two or more than three of soybean protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose and maltodextrin.
Preferably, the fat fatty acid ratio of the nutrient compound oil is that of saturated fatty acid: monounsaturated fatty acids: the weight ratio of the polyunsaturated fatty acid is 1 (0.5-2) to 0.5-2, wherein the weight ratio of linoleic acid in the polyunsaturated fatty acid is as follows: the weight ratio of linolenic acid is 1 (0.5-2).
Preferably, the fat fatty acid ratio of the nutrient compound oil is that of saturated fatty acid: monounsaturated fatty acids: the weight ratio of the polyunsaturated fatty acid is 1 (0.5-1.5) to (0.5-1.5), wherein the weight ratio of linoleic acid in the polyunsaturated fatty acid is as follows: the weight ratio of linolenic acid is 1 (0.5-1.5).
More preferably, the fat fatty acid ratio of the nutrient compound oil is saturated fatty acid: monounsaturated fatty acids: the weight ratio of the polyunsaturated fatty acid is 1:1:1, and the weight ratio of linoleic acid in the polyunsaturated fatty acid is as follows: the weight ratio of linolenic acid is 1: 1.
Preferably, the fullerene microcapsule powder further contains a stabilizer and/or a glidant.
Preferably, the weight content of the stabilizer is 0.01-20 wt% and the weight content of the glidant is 0.01-2 wt% based on the total weight of the fullerene microcapsule powder.
The stabilizer can be various substances which can stabilize the performance of the fullerene capsule, and can be organic acid with chelation or salt thereof, and specific examples thereof include but are not limited to: at least one of erythorbic acid and salts thereof, gallic acid and derivatives thereof, gluconic acid, sodium tripolyphosphate, composite phosphate, dipotassium hydrogen phosphate, sodium polyphosphate, sodium metaphosphate, sodium carboxymethylcellulose and agar.
The glidant can impart better flow to the fullerene capsule forming components to facilitate molding. Specific examples of said glidant include, but are not limited to: at least one of silicate, stearate, iron salt, phosphate, polysaccharide, talcum powder, calcium carbonate and zinc dioxide. Wherein the silicate may be at least one selected from the group consisting of silicon dioxide, calcium silicate, sodium aluminum silicate, magnesium silicate and sodium aluminosilicate. The stearate may be selected from at least one of sodium stearate, calcium stearate, aluminum stearate, and zinc stearate. The iron salt can be ammonium iron citrate and/or sodium ferrocyanide. The phosphate may be calcium phosphate and/or magnesium phosphate. The polysaccharide may be depolymerised starch and/or microcrystalline depolymerised cellulose.
Preferably, the particle size of the fullerene microcapsule powder is 5-500 mu m.
Preferably, the fullerene microcapsule powder is prepared by the following mode (1) or mode (2):
mode (1):
preparing an oil phase: preparing the nutrient compound oil according to the proportion of fatty acid, then sterilizing the fullerene compound, dissolving the fullerene compound into the nutrient compound oil to form a compound oil compound, and then dissolving the edible emulsifier into the compound oil compound to obtain an oil phase;
preparation of an aqueous phase: dissolving the wall material in hot water to obtain a water phase; preferably, the temperature of the hot water is 60-80 ℃;
mixing and sterilizing: mixing the obtained water phase and oil phase, stirring, and sterilizing;
homogenizing and spray drying: homogenizing, and spray drying to obtain fullerene microcapsule powder;
mode (2):
dissolving the fullerene compound in the nutrient compound oil to obtain a fullerene oil solution;
mixing, dissolving, dispersing and homogenizing the fullerene oil solution, the wall material, the edible emulsifier and the optional stabilizer and flow aid to prepare emulsion, homogenizing the obtained emulsion, and then spray-drying the homogenized emulsion.
Preferably, in the mode (1) and the mode (2), the mixing is performed under a shearing condition, and the mixing condition includes a temperature of 50 to 80 ℃, a shearing rate of 10000-.
Preferably, the homogenizing pressure is 30-35MPa, and the homogenizing times are 2-5 times.
Preferably, the conditions of the spray drying include that the air inlet temperature is 180-240 ℃ and the air outlet temperature is 75-85 ℃.
Preferably, the content of the fullerene micro-capsule powder is 30-80 wt%, more preferably 40-75 wt%, and most preferably 60-75 wt%, based on the total weight of the fullerene livestock and poultry feed additive.
Preferably, the vitamins comprise vitamin a, vitamin B2 and vitamin D; the content of the vitamin A is 3-10 wt%, preferably 4-8 wt%, more preferably 5-8 wt%, the content of the vitamin B2 is 0.01-5 wt%, preferably 0.1-5 wt%, more preferably 0.5-5 wt%, most preferably 0.5-2 wt%, and the content of the vitamin D is 1-8 wt%, preferably 3-8 wt%, more preferably 4.5-8 wt%, based on the total weight of the fullerene livestock and poultry feed additive.
The prebiotics are substances that selectively stimulate the growth or activation of bacteria in the gastrointestinal tract of a host, promote the health of the host, and are digested by the gastrointestinal tract of the host. The prebiotics are preferably at least one selected from inulin, fructo-oligosaccharide, soy oligosaccharide, galacto-oligosaccharide, xylo-oligosaccharide, lactulose, isomalto-oligosaccharide, lactulose-oligosaccharide, gentiooligosaccharide, galacto-oligosaccharide and manno-oligosaccharide. In addition, the content of the prebiotics is preferably 6-12 wt% based on the total weight of the fullerene livestock and poultry feed additive.
Preferably, the content of the shell powder is 0.5-20 wt%, preferably 5-15 wt%, more preferably 8-15 wt%, and most preferably 10-15 wt%, based on the total weight of the fullerene livestock and poultry feed additive.
The preparation method of the fullerene livestock and poultry feed additive provided by the invention comprises the steps of uniformly mixing the fullerene micro-capsule powder, vitamins, prebiotics and shell powder, granulating, sieving, and obtaining the underflow, namely the fullerene livestock and poultry feed additive. Wherein, the mixing can be carried out by adopting a three-dimensional mixer, the mixing temperature can be room temperature, and the mixing time can be 10-15 min. The granulation may be carried out in a boiling granulator. The aperture of the screen mesh used for sieving can be 0.4-0.6 mm.
In addition, the invention also provides a feed, wherein the feed contains the fullerene livestock and poultry feed additive.
Preferably, the fullerene livestock and poultry feed additive accounts for 1-3 wt% of the total weight of the feed.
The fullerene livestock and poultry feed additive provided by the invention is rich and balanced in nutrition, can improve the taste of the feed, improve the palatability of the feed, and can enhance intestinal secretion of animals, promote digestion and absorption, improve the conversion efficiency of the feed, enhance the immunity of organisms, improve the disease resistance of the organisms, promote growth, improve the lean meat percentage and improve the quality of muscles.
Drawings
Fig. 1 is a schematic view of the microstructure of fullerene microcapsule powder provided by the present invention.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative of the invention and is not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1-1: preparation of fullerene microcapsule powder
Table 1-1 raw material usage (% by weight) table for examples
| Sterile fullerene | Emulsifier | Nutrient compound oil | Wall material | |
| Examples 1 to 1 | 1‰ | 3.0％ | 50％ | 46.90％ |
| Examples 1 to 2 | 5‰ | 3.5％ | 70％ | 26.00％ |
| Examples 1 to 3 | 2.5‰ | 2.5％ | 50％ | 47.25％ |
| Examples 1 to 4 | 3‰ | 3.0％ | 60％ | 36.70％ |
The preparation process of the fullerene microcapsule powder comprises the following steps:
(1) preparing nutrient compound oil according to the proportion of fatty acid;
(2) sterilizing fullerene, and dissolving the fullerene in the nutrient compound oil to form a compound oil compound;
(3) dissolving an edible emulsifier into the compound oil compound to obtain an oil phase;
(4) dissolving the wall material in hot water at 60-80 deg.C to obtain water phase;
(5) mixing the obtained water phase and oil phase, stirring, and sterilizing;
(6) homogenizing, spraying, and drying to obtain fullerene microcapsule powder.
The oxidation resistance of the prepared fullerene microcapsule powder is measured to be 125 times of that of vitamin C by an in vitro beta-carotene oxidation method.
Examples 1 to 2: preparation of fullerene microcapsule powder
Raw materials: see Table 1-1.
The procedure of preparation was the same as in example 1-1. The oxidation resistance of the prepared fullerene microcapsule powder is measured to be 125 times of that of vitamin C by an in vitro beta-carotene oxidation method.
Examples 1 to 3: preparation of fullerene microcapsule powder
Raw materials: see Table 1-1.
The procedure of preparation was the same as in example 1-1. The oxidation resistance of the prepared fullerene microcapsule powder is measured to be 125 times of that of vitamin C by an in vitro beta-carotene oxidation method.
Examples 1 to 4: preparation of fullerene microcapsule powder
Raw materials: see Table 1-1.
The procedure of preparation was the same as in example 1-1. The oxidation resistance of the prepared fullerene micro-capsule powder is measured by an in-vitro beta-carotene oxidation method to be 125 times of that of vitamin C.
Examples 1 to 5: effect experiment of fullerene microcapsule powder for improving immunity
5g of fullerene microcapsule powder obtained in any one of examples 1-1 to 1-4, 1g of anthocyanin and 500mg of vitamin C are made into powder or pressed into tablets, and the fullerene microcapsule powder has the function of improving immunity after being taken for a long time.
Examples 1 to 6: fullerene microcapsule powder for health care effect experiment
20g of fullerene microcapsule powder obtained in any one of examples 1-1 to 1-4. It can be taken orally once a day for a long time to prevent cancer and delay neurodegenerative diseases such as Parkinson and senile dementia. Meanwhile, the fullerene micro-capsule powder is more acceptable to patients in taste and eating way than pure fullerene olive oil.
Examples 1 to 7: hangover alleviating product containing fullerene microcapsule powder and effect verification experiment
2g of fullerene microcapsule powder obtained in any one of examples 1-1 to 1-4, 1g of kudzu root, 1g of hovenia dulcis thunb, 0.25g of poria cocos and 1g of honey, and the fullerene microcapsule powder is prepared into powder or solid particles and can relieve symptoms of hangover, headache and vomiting after drinking.
An anti-alcohol experiment:
the safety of the product is determined as follows:
taking 20 healthy and clean Kunming mice (with the weight of 18-22g) with half each female and half each male, randomly pairing the Kunming mice into two groups, 10 mice in each group, and administering the group: 0.33ml/20gBW (corresponding to 10 times of the dose of human body) (calculation method: 5.25g of human effective dose (converted into 65Kg of human body weight) and about 0.0165 of 10 times of the dose of 20g of mouse; 0.5g of the anti-hangover product is dissolved in 10ml of water, 0.33ml contains 0.0165g, that is, the required amount of mouse for gastric lavage is 0.33ml/20g), and control group: 0.33ml/20gBW equivalent of physiological saline was administered. Both groups were continuously fed for 7 days, and mice were observed for growth status, adverse reactions and death. Mice were sacrificed on day 8 and abnormal conditions of the organs were observed visually and under a microscope. The observation results show that: the mice have no adverse reaction, and the observation of all organs under a mirror shows no abnormal condition.
Pre-experiment:
referring to the literature, 6 groups of mice were individually subjected to intragastric gavage with 6 mice each group at 0.26ml/20g, 0.28ml/20g, 0.30ml/20g, 0.32ml/20g, 0.34ml/20g, 0.36ml/20g alcohol solution (56 degree red star Erguotou). The mice were observed for the amount of alcohol required to cause the elimination of the righting reflex without death of the mice. The results are shown in Table 2: the subsequent experiment was carried out by selecting a gavage 0.30ml/20g wine solution.
TABLE 1-2 influence on mortality from alcoholism in mice
| Group of | Total number n | Alcohol (ml/20g) | Death n (%) | Survival n (%) | Drunk n (%) |
| A | 10 | 0.26 | 0 | 100 | 30 |
| B | 10 | 0.28 | 0 | 100 | 50 |
| C | 10 | 0.30 | 0 | 100 | 100 |
| D | 10 | 0.32 | 20 | 80 | 100 |
| E | 10 | 0.34 | 60 | 40 | 100 |
| F | 10 | 0.36 | 90 | 10 | 100 |
The influence of the administration on the drunkenness time, the drunkenness dispelling time and the drunkenness rate of the acute alcoholism mouse is as follows:
the mice were randomly divided into 4 groups: the model group (drenched with equal volume of normal saline), the low dose group (drenched with 0.1ml/20g), the medium dose group (drenched with 0.2ml/20g), and the high dose group (drenched with 0.3ml/20g), each group containing 10 patients. Each group of mice was fasted for 12h and given one time. After 30min, the stomach of each group is filled with 15ml/kg (based on the pre-experimental data) of Beijing Erguotou wine with the weight of 56 ℃, the drunk time (the time from waking to disappearance of anti-normal reflex) of the mouse is observed and recorded, and the drunk rate within 24h is calculated. Whether the mouse is drunk or not is judged by taking whether the righting reflex disappears or not as a standard: and (3) after the mouse is drunk, putting the mouse in a squirrel cage lightly, and if the mouse keeps a posture of being back-down for more than 30s, determining that the righting reflection disappears, namely drunk. Mice were observed and recorded for time to sober (time from disappearance of righting reflex to waking) and mortality within 24h was calculated. The results are shown in tables 1-3 and tables 1-4: therefore, the invention has good effect of relieving alcoholism.
Table 1-3 dosage tables for different experimental groups
| Group of | Number of | Dosage (ml/20g) | Equivalent to human body weight (mg/kg) |
| |
20 | 0.1 | - |
| |
20 | 0.04 | 150 |
| |
20 | 0.08 | 300 |
| |
20 | 0.1 | 450 |
And starting the intragastric administration wine at 10 o' clock.
Note: ddH where control group administration was given 2 O。
TABLE 1-4 table of results after gavage in different groups
| Control group | Low dose group | Middle dose group | High dose group | |
| Drunk time | 10:30 | 11:00 | 11:20 | 12:00 |
| Time of sobering up | 15:30 | 15:00 | 15:00 | 15:30 |
| Length of drunk | 5h | 4h | 3h40min | 3h30min |
| Number of deaths within 24h | 0 | 0 | 0 | 0 |
As can be seen from tables 1 to 3 and tables 1 to 4, the time for getting drunk is significantly shortened in the low dose group, the medium dose group and the high dose group, and the time is reduced with the increase of the dose, which indicates that the anti-inebriation product containing the microcapsule powder has significant effect of relieving hangover.
Preparation example 1: preparation of fullerene oil solution
Accurately weighing 100g of nutritional compound oil (weight ratio of olive oil, linseed oil and shinyleaf yellowhorn oil is 5:3:2) and 0.3g of fullerene C 60 Pouring the raw materials into a ball milling tank for ball milling, transferring a ball-milled product into a centrifuge bottle for centrifugation for 1h at 8000r/min, performing degerming treatment on the centrifuged product through a filter device (0.5 mu m), and obtaining a product, namely the fullerene nutrient compound oil solution after degerming.
Preparation example 2: preparation of fullerene oil solution
Accurately weighing 100g of olive oil and 0.15g of fullerene C 60 Pouring the raw materials into a ball milling tank for ball milling, transferring a ball-milled product into a centrifuge bottle for 7000r/min centrifugation for 1.5h, performing sterilization treatment on the centrifuged product through a filter device (0.5 mu m), and performing sterilization to obtain a product, namely the fullerene olive oil solution.
Preparation example 3: preparation of fullerene oil solution
Accurately weighing 100g of oleum Hippophae and 0.12g of fullerene C 70 Pouring the raw materials into a ball milling tank for ball milling, transferring a ball-milled product into a centrifuge bottle for 6500r/min centrifugation for 2h, performing sterilization treatment on the centrifuged product through a filtering device (0.5 mu m), and performing sterilization to obtain the fullerene sea buckthorn oil solution.
Preparation example 4: preparation of fullerene oil solution
Accurately weighing 100g soybean oil and 0.08g fullerene C 70 Pouring the raw materials into a ball milling tank for ball milling, transferring a ball-milled product into a centrifuge bottle for 6000r/min for 2.5h, performing sterilization treatment on the centrifuged product through a filter device (0.5 mu m), and performing sterilization to obtain the fullerene soybean oil solution.
The formulations of fullerene microcapsule powders in examples 1-4 are shown in table 1:
TABLE 1 amount of each raw material (wt%) in examples 1 to 4
| Item | Fullerene oil solution | Wall material | Edible emulsifier | Stabilizer | Glidants |
| Example 1 | 50 | 46 | 2 | 1 | 1 |
| Example 2 | 33.3 | 62.7 | 2 | 1 | 1 |
| Example 3 | 25 | 71 | 2 | 1 | 1 |
| Example 4 | 50 | 47 | 1 | 0.5 | 1.5 |
Example 1: preparation of fullerene microcapsule powder
Raw materials: see Table 1
The preparation method comprises the following steps: at 60 ℃, 46 wt% of maltodextrin (wall material), 2 wt% of sodium caseinate (edible emulsifier), 1 wt% of dipotassium hydrogen phosphate (stabilizer) and 1 wt% of silicon dioxide (glidant) are mixed, stirred and dissolved with distilled water, and 50 wt% of fullerene nutrient complex oil solution (obtained from preparation example 1) is added to prepare emulsion. Shearing and emulsifying at 11200rpm for 5min at 60 deg.C. Immediately carrying out high-pressure homogenization on the sheared emulsion for 3 times by using a high-pressure homogenizer at the homogenization pressure of 30-35MPa, carrying out spray drying on the homogenized emulsion at the air inlet temperature of 200 ℃ and the air outlet temperature of 82 ℃ to obtain fullerene micro-capsule powder, wherein the micro-morphology of the fullerene micro-capsule powder is shown in a figure 1. From the results of fig. 1, it can be seen that the fullerene microcapsule powder has a particle size of 5 to 20 μm and a hollow spherical or elliptical interior, because bubbles are formed inside the particle when the shell of the product is rapidly formed, and the shell expands when the temperature of the particle exceeds the vaporization temperature of the ambient moisture and the vapor pressure inside the particle exceeds the pressure of the ambient environment. In addition, the fullerene microcapsule powder has a spherical or elliptical shape, a smooth, compact and crack-free surface, and the surfaces of some particles are slightly sunken and shrunk, which is unique to a spray drying processing technology.
Example 2: preparation of fullerene microcapsule powder
Raw materials: see Table 1
The preparation method comprises the following steps: 62.7 wt% of maltodextrin (wall material), 2 wt% of sodium caseinate (edible emulsifier), 1 wt% of dipotassium hydrogen phosphate (stabilizer) and 1 wt% of silicon dioxide (flow aid) are mixed with distilled water at 60 ℃ and stirred to be dissolved, and 33.3 wt% of fullerene olive oil solution (obtained from preparation example 2) is added to prepare an emulsion. Shearing and emulsifying at 11200rpm for 5min at 60 deg.C. Immediately carrying out high-pressure homogenization on the sheared emulsion for 3 times by using a high-pressure homogenizer, wherein the homogenization pressure is 30-35MPa, carrying out spray drying on the homogenized emulsion, and obtaining fullerene micro-capsule powder with the particle size of 100-200 mu m, wherein the air inlet temperature is 200 ℃ and the air outlet temperature is 82 ℃.
Example 3: preparation of fullerene microcapsule powder
Raw materials: see Table 1
The preparation method comprises the following steps: at 60 ℃, 71 wt% of maltodextrin (wall material), 2 wt% of sodium caseinate (edible emulsifier), 1 wt% of dipotassium hydrogen phosphate (stabilizer) and 1 wt% of silicon dioxide (glidant) are mixed, stirred and dissolved with distilled water, and 25 wt% of fullerene sea buckthorn seed oil solution (obtained from preparation example 3) is added to prepare emulsion. Shearing and emulsifying at 11200rpm for 5min at 60 deg.C. Immediately carrying out high-pressure homogenization on the sheared emulsion for 3 times by using a high-pressure homogenizer, wherein the homogenization pressure is 30-35MPa, carrying out spray drying on the homogenized emulsion, and obtaining fullerene microcapsule powder with the particle size of 225-305 mu m, wherein the air inlet temperature is 200 ℃ and the air outlet temperature is 82 ℃.
Example 4: preparation of fullerene microcapsule powder
Raw materials: see Table 1
The preparation method comprises the following steps: dissolving 9.4 wt% of soybean protein isolate (wall material) with distilled water, treating with a temperature-controlled magnetic stirrer at 80 deg.C for 30min, and cooling; 0.5 wt% of sodium carboxymethylcellulose (stabilizer) and 1.5 wt% of silicon dioxide (glidant) were dissolved in distilled water, 37.6% of maltodextrin (wall material) was uniformly mixed with the above-mentioned soy protein isolate solution and the mixed solution of sodium carboxymethylcellulose and silicon dioxide, 1% of lecithin (edible emulsifier) was added to a 50 wt% fullerene soybean oil solution (obtained from preparation example 4), the lecithin was sufficiently dissolved by stirring with a glass rod, the above-mentioned feed solutions were mixed, and shear emulsification was performed at 11200rpm for 5 min. Immediately carrying out high-pressure homogenization on the sheared emulsion for 3 times by using a high-pressure homogenizer, wherein the homogenization pressure is 35MPa, carrying out spray drying on the homogenized emulsion, and obtaining fullerene micro-capsule powder with the particle size of 310-400 microns, wherein the air inlet temperature is 220 ℃ and the air outlet temperature is 80 ℃.
TABLE 2 Fullerene animal feed additive amount of each component (wt%)
| Item | Fullerene microcapsule powder | Vitamin A | Vitamin B2 | Vitamin D | Prebiotics | Shell powder |
| Example 5 | 60 | 6 | 2 | 5 | 12 | 15 |
| Example 6 | 65 | 8 | 1 | 8 | 8 | 10 |
| Example 7 | 70 | 5 | 0.5 | 4.5 | 8 | 12 |
| Example 8 | 75 | 5.5 | 1 | 4.5 | 6 | 8 |
Example 5: preparation of fullerene feed additive for livestock and poultry
The dosage of the formula is as follows: see Table 2
The preparation method comprises the following steps: weighing the components in proportion (the fullerene microcapsule powder used in the embodiment is prepared in the embodiment 1), and uniformly mixing by using a V-shaped mixer for 10 min; mixing, granulating with a boiling granulator to obtain powder with average particle size of 0.4mm, and sieving to obtain Fullerene feed additive (ST-1).
Example 6: preparation of fullerene feed additive for livestock and poultry
The dosage of the formula is as follows: see Table 2
The preparation method comprises the following steps: weighing the components in proportion (the fullerene microcapsule powder used in the embodiment is prepared in the embodiment 2), and uniformly mixing by using a V-shaped mixer for 15 min; mixing, granulating with a boiling granulator to obtain powder with average particle size of 0.5mm, and sieving to obtain Fullerene feed additive (ST-2).
Example 7: preparation of fullerene feed additive for livestock and poultry
The dosage of the formula is as follows: see Table 2
The preparation method comprises the following steps: weighing the components in proportion (the fullerene microcapsule powder used in the embodiment is prepared in the embodiment 3), and uniformly mixing by using a V-shaped mixer for 10 min; mixing, granulating by boiling granulator to obtain powder with average particle diameter of 0.6mm, and sieving to obtain fullerene feed additive, and recording as ST-3.
Example 8: preparation of fullerene feed additive for livestock and poultry
The dosage of the formula is as follows: see Table 2
The preparation method comprises the following steps: weighing the components in proportion (the fullerene microcapsule powder used in the embodiment is prepared in the embodiment 4), and uniformly mixing by using a V-shaped mixer for 15 min; mixing, granulating with a boiling granulator to obtain powder with average particle size of 0.5mm, and sieving to obtain Fullerene feed additive for livestock and fowl (ST-4).
Comparative example 1: preparation of reference livestock and poultry feed additive
The livestock and poultry feed additive is prepared according to the method in the embodiment 5, except that the fullerene micro-capsule powder is replaced by prebiotics in the same weight part, so as to obtain a reference livestock and poultry feed additive, which is recorded as DST-1.
Comparative example 2: preparation of reference livestock and poultry feed additive
The livestock and poultry feed additive is prepared according to the method in the embodiment 5, except that the shell powder is replaced by the prebiotics in the same weight part to obtain the reference livestock and poultry feed additive which is recorded as DST-2.
Effect test
1. Grouping of test animals
The test site is carried out on farmer farm families in the same-safety area of Xiamen city, specifically, 210 fattening middle pigs which are healthy, uniform in weight, consistent in male-female proportion and similar in age of days are selected and randomly divided into 20 groups, each group comprises 10 pigs, six test groups and a control group, the groups are repeated for 2 groups, feeding tests are carried out, and the results are averaged.
2. Test daily ration
The feed for the feeding test is provided by a farmer group pig farm, and the corn-soybean meal feed, the daily ration composition and the nutritional ingredients are in accordance with the pig nutritional requirements recommended by the American NRC (2012). Composition of the test diets: corn, soybean meal, bran, calcium hydrophosphate, stone powder, sodium chloride, copper sulfate, ferrous sulfate, zinc sulfate, manganese sulfate, vitamin A, vitamin D3, vitamin E, L-lysine hydrochloride, ethoxyquinoline and calcium propionate, wherein the specific nutrient components are shown in Table 3.
Table 3 test diet formula and nutritional levels (%)
| Nutrient substance | Content (wt.) |
| Digestive energy DM (Mcal/kg) | 14 |
| Crude protein | >14 |
| Calcium carbonate | 0.5～1.0 |
| Total phosphorus | 0.4～0.7 |
| Coarse fiber | ≦8.0 |
| Coarse ash content | ≦9.0 |
The control group selects the test daily ration to feed, the test group selects the fullerene livestock and poultry feed additives ST-1 to ST-4 prepared in the examples 5 to 8 and the reference livestock and poultry feed additives DST-1 to DST-2 prepared in the comparative examples 1 to 2 to feed on the basis of the control group, and the weight ratio of the test daily ration to the livestock and poultry feed additives is 100: 1.
3. Feeding management
The whole test period is 60 days, 180 test pigs are fed in the same pigsty, each group is fed in groups, and each group contains 10 pigs. The ventilation in the house is good, the air is dry, and the temperature is suitable. Periodically sterilizing and immunizing according to epidemic prevention program of pig farm, providing sufficient clean drinking water by nipple type drinking device, feeding twice (6:00 and 17:00) every day, and freely eating and drinking water. The pig feeding, drinking, excrement color and disease occurrence conditions in the pigsty are observed every day, the humidity and temperature (17-22 ℃ and 35-50% of humidity) in the pigsty every day are recorded, and other management is carried out according to normal management of a pig farm.
4. Data processing
After the Excel is adopted for sorting and preliminary calculation, the SPSS statistical software general linear model is used for carrying out single-factor variance analysis, and the Duncan's method is used for multiple comparison. The data are expressed as mean ± standard error, and P <0.05 is used as a difference significance determination criterion, and analyzed by regression analysis.
5. Determination of growth Performance
The test compares the growth performance of each group of pigs according to the measurement of average net weight gain, daily consumption and feed-weight ratio of each group of pigs. And measuring the weights of the pigs in each group at the beginning stage and the ending stage of the test, making records, counting the total feed intake, diarrhea and morbidity of each test pig column, and then calculating the average daily feed intake, the average daily gain and the feed-weight ratio according to the recorded statistical data, wherein the obtained results are shown in a table 4.
Average Daily Gain (ADG) ═ average weight in the end column-average weight in the initial column/days tested;
average Daily Food Intake (ADFI) — total food intake per column/(test days × number of heads per column);
the material weight ratio is the average feed intake/average daily gain;
TABLE 4 Fullerene feed additives Effect on the growth behavior of Central Swine
Note: the same row of digital shoulders are marked with different capital English alphabets to show significant difference (P <0.01), different lower case alphabets to show significant difference (P <0.05), no capital or lower case alphabets to show insignificant difference (P >0.05), and the following are the same.
As can be seen from Table 4, the average daily gain of the test groups ST-1, ST-2, ST-3, ST-4 was increased by 33.23%, 36.56%, 34.69%, 37.07% compared to the control group, respectively, with a significant difference (P <0.01), while the average daily consumption of each test group was not significantly different (P > 0.05); the material weight ratios of the test groups ST-1, ST-2, ST-3 and ST-4 are respectively reduced by 23.61%, 23.26%, 25.00% and 21.22% compared with the control group, and the differences are obvious. The average daily gain of the reference group DST-1 is not obviously different from that of the control group, but the material weight is improved by 6.94 percent compared with that of the control group. Compared with a control group, the average daily gain of the DST-2 is improved by 20.82 percent, and the material-to-weight ratio is reduced by 8.30 percent.
Therefore, the fullerene livestock and poultry feed additive provided by the invention can promote growth of fattening pigs, reduce the feed-weight ratio, improve the feed conversion capacity and improve the weight gain of the fattening pigs.
6. Determination of the digestibility of the daily rations
Stool sample: during the middle of the trial, 3 test pigs from each test group that approached the average body weight of the group were selected for a continuous 5d digestion trial. During digestion testing, test pigs were driven to a modified digestion room after the original lactating sow litter to ensure individual feeding and contamination free of fecal material from each other. Randomly taking fresh manure samples at a time of 9:00 and 17:00 each day in a test period of 5d, taking about 100g of the fresh manure samples each day, dividing the fresh manure samples into 2 parts, taking about 30g of the fresh manure samples as nitrogen fixation samples for measuring crude protein, specifically, adding concentrated sulfuric acid aqueous solution with the weight of 1/4 fresh manure and the concentration of 10 wt% into the fresh manure samples each day, then gathering the fresh manure samples obtained in 5d by taking a test pig as a unit, uniformly mixing the fresh manure samples, and putting the fresh manure samples together into an oven at 70 ℃ for drying and sample preparation; and (3) taking another part of fresh excrement, drying the fresh excrement in a 70 ℃ drying oven in time on the same day, taking the fresh excrement at the 2 nd day, accumulating the fresh excrement and drying the fresh excrement together, finally collecting 5d excrement samples together, drying the excrement samples to constant weight at 70 ℃, dampening the excrement samples for 24 hours at room temperature, preparing air-dried samples which are sieved by a 40-mesh sieve after measuring the initial moisture, and storing the air-dried samples in a ground wide-mouth bottle for later use (for measuring other indexes). The results are shown in Table 5.
Crude protein: GB/T6432-1994 is adopted to determine the content of crude protein in the feed and the excrement;
coarse fiber: measuring the content of crude fiber in feed and excrement by GB/T6434-2006;
coarse ash content: measuring the content of coarse ash in the feed and the excrement by GB/T6438-2007;
calcium: GB/T6436-2002 is adopted to determine the content of calcium in the feed and the excrement;
phosphorus: measuring the content of total phosphorus in the feed and the excrement by GB/T6437-2002;
the digestion test is measured by adopting an endogenous indicator acid-insoluble ash (AIA) method, and the measuring method refers to the national standard (GB/T-23742-: (a) firstly weighing 5g of crushed dry feed or feces sample, placing the crushed dry feed or feces sample in a 250mL beaker, adding 25mL of distilled water, adding 25mL of 3mol/L dilute hydrochloric acid after the feed or feces sample is wetted completely by the distilled water, standing until the foam disappears, adding 50mL of 3mol/L dilute hydrochloric acid, standing until the foam disappears if the foam exists, heating the beaker in a micro-boiling water bath kettle for 30 minutes or more until all starch is completely hydrolyzed, and covering the beaker with a glass dish during heating to reduce the volatilization of water and acid; (b) filtering the solution with ash-free filter paper (quantitative filter paper), washing the filter paper and residues with 100mL of hot distilled water (85-100 ℃), washing hydrochloric acid, transferring the ash and the filter paper into a crucible with constant weight, placing the crucible into an oven for drying at 105 ℃, placing the crucible into a muffle furnace for firing at 550 ℃ for 3 hours, and carefully observing whether carbon particles exist in the ash; taking out the crucible if no carbon particles exist, placing the crucible in a dryer to cool to room temperature, and weighing; if there are carbon particles, the crucible is then placed in a muffle furnace and fired until the carbon particles disappear, and the percentage of acid insoluble ash (w) is calculated according to the following equation: w ═ m2-mc)/(m1-mc) × 100%, m2 is the total weight of crucible and acid insoluble ash (g), mc is the weight of crucible (g), m1 is the total weight of crucible and sample (g), all samples weighed accurately to 0.001 g. The determination formula of the nutrient digestibility is as follows: the percent digestibility of a nutrient is 100- [1- (a/B) × (C/D) ] × 100%, wherein: a represents a certain nutrient content in feces, B represents the nutrient content in the diet, C represents the acid-insoluble ash content in the diet, and D represents the acid-insoluble ash content in feces, and the results are shown in Table 5.
TABLE 5 Effect of digestibility (%)
As can be seen from Table 5, the apparent digestibility of crude protein and crude fiber in the test group is significantly improved compared with that in the control group (P <0.05), and the apparent digestibility of crude ash, calcium and phosphorus is not significantly different among the groups (P > 0.05). Crude protein: the test groups ST-1, ST-2, ST-3 and ST-4 are respectively improved by 37.62 percent, 36.70 percent, 34.29 percent and 37.67 percent compared with the control group, and the DST-2 of the reference group is improved by 21.30 percent compared with the control group, and the difference is very obvious (P is less than 0.01). Coarse fiber: the test groups ST-1, ST-2, ST-3 and ST-4 are respectively improved by 7.75 percent, 6.23 percent, 5.88 percent and 7.04 percent compared with the control group, the DST-2 of the reference group is improved by 4.60 percent compared with the control group, and the difference is very obvious (P is less than 0.01). And the DST-2 of the reference group has no significant difference compared with the control group (P > 0.05). This shows that the fullerene feed additive of the invention is helpful for digestion and absorption of feed nutrients in pigs.
7. Biochemical index of serum
After feeding, 3 pigs were randomly selected from each test group and control group, and 5mL of blood was collected in the anterior vena cava using a disposable syringe (3500r/min, centrifugation 5min, serum separation, supernatant collection in a disposable PE tube and storage at-20 ℃). The samples were sent to Wuhan Severe Biotech, Inc. and measured with a fully automatic biochemical instrument: total Protein (TP), Albumin (ALB), globulin (BLO), blood Glucose (GLU), Triglycerides (TG), urea nitrogen (BUN), total Cholesterol (CHO), glutamic-oxaloacetic transaminase (GOT), glutamic-pyruvic transaminase (GPT), alkaline phosphatase (ALP), immunoglobulin (IgA), immunoglobulin (IgG), immunoglobulin (IgM). In addition, total antioxidant capacity (T-AOC), superoxide dismutase (T-SOD) was determined and calculated according to the kit procedures. The results are shown in Table 6.
TABLE 6 Fullerene feed additive Effect on serum Biochemical indicators of growing pigs
As can be seen from Table 6, the differences among globulin, total antioxidant capacity, total SOD and glutamic-pyruvic transaminase were improved compared with the control group, but the differences were not significant (P > 0.05). TP Total protein: ST-1, ST-2, ST-3 and ST-4 of the test group are respectively improved by 22.82%, 23.05%, 23.19% and 23.42% compared with the control group, and the difference is very obvious (P is less than 0.01); and the DST-2 of the reference group is improved by 6.03 percent compared with the control group, and the difference is not significant (P is more than 0.05). ALB albumin: ST-1, ST-2, ST-3 and ST-4 in the test group are respectively improved by 26.57%, 26.08%, 27.45% and 26.26% compared with the control group, and the difference is very obvious (P is less than 0.01); and the DST-2 of the reference group is improved by 13.28 percent compared with the control group, and the difference is not significant (P is more than 0.05). ALP alkaline phosphatase: the ST-1, ST-2, ST-3 and ST-4 of the test group are respectively improved by 5.87%, 5.34%, 6.38% and 5.93% compared with the control group, and the DST-2 of the reference group is improved by 2.11% compared with the control group, and the difference is very obvious (P is less than 0.01). GPT glutamic-pyruvic transaminase: the ST-1, ST-2, ST-3 and ST-4 of the test group are respectively improved by 13.80 percent, 14.18 percent, 14.70 percent and 15.13 percent compared with the control group, the DST-2 of the reference group is improved by 7.18 percent compared with the control group, and the difference is very obvious (P is less than 0.01). TC total cholesterol: ST-1, ST-2, ST-3 and ST-4 in the test group are respectively reduced by 6.14%, 2.63%, 4.82% and 4.39% compared with the control group, and DST-2 in the reference group is reduced by 3.95% compared with the control group. The antibody in the serum is obviously improved, and the disease resistance of the organism is enhanced. The TP and ALB contents of pig serum reflect the absorption, synthesis and decomposition conditions of protein of the body and reflect the immune condition of the body. In the test, the albumin index test group is obviously increased compared with the control group, which shows that the fullerene feed additive has certain effects on albumin, glutamic-pyruvic transaminase and cholesterol, and can enhance the digestion and absorption capacity of animals on protein and the immunity of organisms.
In conclusion, the fullerene livestock and poultry feed additive provided by the invention can improve the overall disease prevention and disease resistance of livestock and poultry, balance and coordinate growth, and can replace popular antibiotics and chemical synthetic drug feed additives, so that safe and high-quality livestock and poultry meat quality products can be produced, and the economic effect is obvious.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the foregoing embodiments may be combined in any suitable manner without contradiction. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The fullerene microcapsule powder comprises fullerene, nutrient compound oil, an edible emulsifier and wall materials.
2. The fullerene microcapsule powder according to claim 1, wherein the fullerene comprises C60 and its derivatives, C70 and its derivatives, fullerene metal derivatives, fullerene oil solution.
3. The fullerene microcapsule powder according to claim 1, wherein the fullerene is used in an amount of 1 to 5% by weight.
4. The fullerene microcapsule powder according to claim 1, wherein the nutrient compound oil is used in an amount of 50 to 70% by weight;
optionally, the amount of the edible emulsifier is 4-6% of the weight content of fat in the nutritional compound oil; preferably, the amount of edible emulsifier is 5% of the weight content of fat;
optionally, the weight amount of the wall material is 29-49%.
5. The fullerene microcapsule powder according to claim 1, wherein the nutrient complex oil has a ratio of fatty acids of saturated fatty acids: monounsaturated fatty acids: the polyunsaturated fatty acid is 1 (0.5-2) to (0.5-2), wherein the linoleic acid in the polyunsaturated fatty acid: linolenic acid is 1 (0.5-2);
preferably, the fat fatty acid proportion of the nutrient compound oil is that of saturated fatty acid: monounsaturated fatty acids: the polyunsaturated fatty acid is 1 (0.5-1.5) to (0.5-1.5), wherein the weight ratio of linoleic acid in the polyunsaturated fatty acid is as follows: linolenic acid is 1 (0.5-1.5);
more preferably, the fat fatty acid ratio of the nutrient compound oil is saturated fatty acid: monounsaturated fatty acids: the polyunsaturated fatty acid is 1:1:1, wherein the ratio of linoleic acid in the polyunsaturated fatty acid: linolenic acid is 1: 1.
6. The fullerene microcapsule powder according to claim 1, wherein the nutritional compound oil is a combination of two or more of linseed oil, safflower seed oil, perilla seed oil, camellia oil, sunflower seed oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, seabuckthorn fruit oil, seabuckthorn seed oil, peony seed oil, walnut oil, shinyleaf yellowhorn oil, seabuckthorn oil, hemp oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid, and conjugated linoleic acid triglyceride.
7. The fullerene microcapsule powder according to claim 1, wherein the edible emulsifier is a or a mixture of a and B; wherein A is 1 or 2 of oligomeric maltose, maltodextrin, solid corn syrup, fructo-oligosaccharide, resistant dextrin, and skimmed milk powder; b is one of sodium caseinate, mono-diglycerol fatty acid ester, starch sodium octenylsuccinate, ascorbic acid, sodium ascorbate, gelatin, polydextrose, phospholipid, natural vitamin E, sodium tripolyphosphate, acacia and ascorbyl palmitate;
optionally, the wall material is formed by mixing 2 or more than 3 of soybean protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose and maltodextrin.
8. Use of fullerenes for the preparation of fullerenic microencapsule powder of any one of claims 1-7 above.
9. Use of fullerene microcapsule powder according to claim 8 for preparing fullerene microcapsule powder, wherein the microcapsule powder has the functions of improving oxidation resistance and/or immunity and/or preventing cancer, delaying neurodegenerative diseases and/or relieving alcoholism.
10. A method for producing fullerene microcapsule powder according to any one of claims 1 to 7, wherein the fullerene microcapsule powder is produced by,
preparing an oil phase: preparing nutrient compound oil according to the proportion of fatty acid, and then dissolving fullerene into the nutrient compound oil after sterilizing to form a compound oil compound; dissolving an edible emulsifier into the compound oil compound to obtain an oil phase;
preparation of an aqueous phase: dissolving the wall material in hot water of 60-80 deg.C to obtain water phase; preferably, the temperature of the hot water is 60-80 ℃;
mixing and sterilizing: mixing the obtained water phase and oil phase, stirring, and sterilizing;
homogenizing, spraying and drying: homogenizing, spraying, and drying to obtain fullerene microcapsule powder.
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| CN2018102592878 | 2018-03-27 | ||
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| CN201811123023.6A Pending CN110301483A (en) | 2018-03-27 | 2018-09-26 | The purposes of fullerene compound and fullerene microcapsule powder and its preparation method and application |
| CN201811365700.5A Pending CN109258934A (en) | 2018-03-27 | 2018-11-16 | Application of the fullerene microcapsule powder as feed addictive |
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| CN109258931A (en) | 2019-01-25 |
| CN109258933A (en) | 2019-01-25 |
| CN109258932A (en) | 2019-01-25 |
| CN108497099A (en) | 2018-09-07 |
| CN109258934A (en) | 2019-01-25 |
| CN110301483A (en) | 2019-10-08 |
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