WO2019184419A1 - Use of fullerene compound, fullerene microcapsule powder and preparation method and application thereof - Google Patents

Abstract

Provided are use of a fullerene compound, a fullerene microcapsule powder, a preparation method, and an application therefor. The fullerene microcapsule powder contains a fullerene, compounded nutritional oils, an edible emulsifier, and a wall material. The fullerene microcapsule powder may be used in preparation of a beverage, a food, a beauty product, a hangover product, or a medicament for the prevention and treatment of liver cancer, neurodegenerative disease, or tumors.

Description

Use of fullerene compound and fullerene microcapsule powder and preparation method and application thereof

This application claims priority from application No. 201810259287.8 filed on March 27, 2018, entitled "The use of fullerenes for the preparation of fullerene microcapsules", and is required to be enjoyed on September 26, 2018. Application No. 201811123023.6, entitled "Use of Fullerene Compounds, and Fullerene Microcapsule Powders, and Their Preparation Methods and Applications", the entire contents of which are incorporated herein by reference. .

Technical field

The invention belongs to the field of fullerenes, and particularly relates to the use of fullerene compounds and fullerene microcapsule powders and preparation methods and applications thereof.

Background technique

Fullerenes are the fourth crystalline form of carbon after diamond, graphite and linear carbon. Fullerenes include C ₆₀ , C ₇₀ and derivatives thereof. Among them, C ₆₀ is the most representative member of the fullerene family, its molecule is aromatic, soluble in benzene is sauce red. C ₆₀ can be obtained by a method of heating a graphite rod by electric resistance or evaporating graphite by an electric arc method. C ₆₀ is lubricious and may become a super lubricant. The metal C ₆₀ is superconducting and is a promising superconducting material.

Fullerene has a wide range of applications in daily life and social production, such as cosmetics, drug carriers, and medical diagnostics, because of its antiviral, anti-oxidant, antibacterial and other biological activities. In 2011, the article published by the French Fathi Moussa research team on Biomaterials published their major findings: After dispersing C ₆₀ into olive oil and feeding the mice, it was found that C ₆₀ has no chronic toxicity and can extend the life of mice by more than 90%. In the study of degenerative diseases caused by deposition of amyloid fibrils such as Alzheimer's disease and Parkinson's syndrome, it has also been found that fullerenes can effectively prevent the formation of amyloid fibers. In the study of liver cancer, it was found that by intraperitoneal injection of fullerene water-soluble derivatives compared with the anticancer drugs CTX and cisplatin, it was found that after the injection of fullerene derivatives, the tumor was greatly inhibited, and the effect of increasing the concentration was also improved. The effect is equivalent to CTX when the amount is 1/500 of CTX; the effect of fullerene derivatives is much better than that of the anticancer drug cisplatin.

Fullerene has poor solubility in most solvents, and usually needs to be dissolved in aromatic solvent toluene, chlorobenzene, or non-aromatic solvent carbon disulfide. The poor solubility of water under normal conditions restricts its application to the body. Various areas of application, especially in the health industry and modern agriculture. In addition, although the fullerene oil solution can be made into a capsule, it is easy to carry, but it is unstable due to its instability, the oil needs to be protected from light and stored at a low temperature, and the taste is not acceptable to the public. In addition, the insoluble nature of fullerenes also limits their development and application. In the application of fullerene, fullerene is mainly made into water-soluble derivatives such as hydrated fullerenes, fullerenes, fullerenes-vitamins C, metal fullerenes and the like. In view of the outstanding performance of fullerenes in the treatment of liver cancer, kidney cancer, and neurodegenerative diseases, in order to give full play to the above properties of fullerenes, it is urgent to find a way to improve the stability of fullerenes and enable them to be applied. A technical method suitable for various fields of the body application.

Summary of the invention

The object of the present invention is to provide a novel use of fullerene compounds and fullerene microcapsule powders and methods for their preparation and use.

In particular, the present invention provides the use of fullerene compounds for the preparation of fullerene microcapsule powders.

Preferably, the fullerene microcapsule powder contains a fullerene compound, a nutritive compound oil, an edible emulsifier, and a wall material.

Preferably, the total weight content of the fullerene compound and the nutritive compound oil is from 10% to 80% based on the total weight of the fullerene microcapsule powder and the weight of the fullerene compound The content of the edible emulsifier is from 0.01% to 5%, and the weight of the wall material is from 0.01% to 80%.

Preferably, the fullerene compound has a weight content of 1‰-5‰ based on the total weight of the fullerene microcapsule powder, and the nutritional compound oil has a weight content of 50%-70%. The weight content of the edible emulsifier is 4-6% by weight of the fat in the nutritional compound oil, and the weight content of the wall material is 29% to 49%.

Preferably, the fullerene compound may be C ₆₀ and its derivatives, C ₇₀ and its derivatives, fullerene metal derivatives, fullerene oxygenated derivatives, organic compound modified or encapsulated rich At least one of a olefin, a modified or encapsulated fullerene derivative. Wherein the oxygen atom in the fullerene oxygen-containing derivative is bonded to a carbon atom on the fullerene skeleton or to an alkylene chain. The organic compound in the fullerene and fullerene derivative modified or encapsulated by the organic compound may be any of various existing organic oligomers capable of forming inclusions or complexes, for example, cyclodextrin and / or crown ether.

The nutritional compound oil is selected from at least one of edible oils, 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 selected from the group consisting of soybean oil, rapeseed oil, palm oil, olive oil, sunflower oil, safflower oil, sea buckthorn seed oil, corn oil, safflower oil, perilla seed oil, tea seed oil, and camellia seed. Oil, cottonseed oil, coconut oil, sesame oil, linseed oil, pumpkin seed oil, peony seed oil, sea buckthorn oil, walnut oil, red pine nut oil, evening primrose oil, safflower seed oil, borage oil, hemp seed At least one of oil, salad oil, wheat germ oil, avocado oil, and sea buckthorn oil. The animal oil is preferably selected from at least one of lard, tallow, sheep oil, fish oil, horse oil and sea turtle oil. The hydrocarbons are preferably squalane and/or squalene. The fatty acid is preferably selected from at least one 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 triglycerides and/or linoleic acid glycerides. Most preferably, the nutritional compound oil is linseed oil, safflower seed oil, perilla seed oil, camellia seed oil, sunflower 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, celery oil, sea buckthorn oil, sesame oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid, conjugate A combination of two or more of linoleic acid triglycerides.

The edible emulsifier may be one which has hydrophilicity and lipophilicity in various molecular structures and has surface activity due to amphiphilicity, and may be an anionic surfactant, a cationic surfactant, or a non- An ionic surfactant or an amphoteric surfactant. Specific examples of the edible emulsifier include, but are not limited to, sucrose fatty acid esters, polyglycerin fatty acid esters, glycerin fatty acid esters, polyoxyethylene sorbitan fatty acid esters, sodium caseinate, lecithin, stearin Sodium, monoglyceride organic acid fatty acid ester, betaine, amino acid salt, glyceryl succinate fatty acid ester, sodium stearoyl lactylate, Tween-80, Span-80, polyglycerol ester, propylene glycol fatty acid ester and polysorbate At least one of fatty acid esters; or, the edible emulsifier is A, or a mixture of A and B, and A is one or both of oligofructose, resistant dextrin, skimmed milk powder, and B is cheese One of sodium acidate, mono-, diglycerin fatty acid ester, sodium starch octenyl succinate, ascorbic acid, sodium ascorbate, phospholipid, natural vitamin E, sodium tripolyphosphate, and ascorbyl palmitate.

The wall material functions to form a film having a certain strength and to improve the microencapsulation efficiency. The wall material is preferably a water-soluble polymer material, and may be specifically selected from the group consisting of maltodextrin (DE18 or DE20), soy protein isolate (SPI), gum arabic (GA), β-cyclodextrin, starch (corn starch, modified). Starch, porous starch, methyl hydroxypropyl starch), whey protein concentrate (WPC), dextrin, corn syrup, gelatin, sodium carboxymethyl cellulose (CMC), xanthan gum, agar, carrageenan, shell Glycan, octenyl succinate starch, guar gum, seaweed gum, alginate, milk protein, casein, gluten, gliadin, cocoa butter, casein acid (SC), vegetable protein , lactose, sucrose, maltose, methyl cellulose, ethyl cellulose, methyl hydroxypropyl cellulose, carboxymethyl cellulose, hydroxymethyl cellulose, hydroxypropyl cellulose, crystalline cellulose and water-soluble meal At least one of the fibers. Preferably, the wall material is a mixture of two or more of soy protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose, and maltodextrin.

Preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1: (0.5-2): (0.5-2), in the polyunsaturated fatty acid Linoleic acid: linolenic acid weight ratio is 1: (0.5-2).

Preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1: (0.5-1.5): (0.5-1.5), in the polyunsaturated fatty acid Linoleic acid: linolenic acid weight ratio is 1: (0.5-1.5).

More preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1:1:1, linoleic acid: linolenic acid weight in the polyunsaturated fatty acid The ratio is 1:1.

Preferably, the fullerene microcapsule powder further contains a stabilizer and/or a glidant.

Preferably, the stabilizer is present in an amount of from 0.01% to 20% by weight based on the total weight of the fullerene microcapsule powder, and the glidant is present in an amount of from 0.01% to 2% by weight.

The stabilizer may be any one of various substances capable of stabilizing the performance of the fullerene capsule, and may be an organic acid having a chelate or a salt thereof, and specific examples thereof include, but are not limited to, erythorbic acid and a salt thereof, gallic acid. And a derivative thereof, at least one of gluconic acid, sodium tripolyphosphate, complex phosphate, dipotassium hydrogen phosphate, sodium polyphosphate, sodium metaphosphate, sodium carboxymethylcellulose, and agar.

The glidant is capable of imparting better fluidity to the components forming the fullerene capsule for ease of molding. Specific examples of the glidant include, but are not limited to, at least one of a silicate, a stearate, an iron salt, a phosphate, a polysaccharide, a talc, calcium carbonate, and zinc dioxide. Wherein the silicate may be at least one selected from the group consisting of silica, 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 may be ammonium ammonium citrate and/or sodium ferric hydride. The phosphate may be calcium phosphate and/or magnesium phosphate. The polysaccharide may be a depolymerized starch and/or a microcrystalline depolymerized cellulose.

Preferably, the fullerene microcapsule powder is prepared in the following manner (1) or mode (2):

Mode (1):

Oil phase preparation: the nutrient compound oil is formulated according to a ratio of fatty acids, and then the fullerene compound is sterilized and dissolved in a nutrient compound oil to form a compound oil compound, and then the edible emulsifier is dissolved. Into the compound oil composite, an oil phase is obtained;

Aqueous phase preparation: dissolving the wall material in hot water to obtain an aqueous phase; preferably, the temperature of the hot water is 60-80 ° C;

Mixed sterilization: mixing the obtained aqueous phase with the oil phase, stirring uniformly, and then sterilizing;

Homogenization, spray drying: homogenization, spray drying to obtain fullerene microcapsule powder;

Mode (2):

Dissolving the fullerene compound in the nutrient compounding oil to obtain a fullerene oil solution;

Mixing, dissolving, dispersing, and homogenizing the fullerene oil solution, the wall material, the edible emulsifier, and the stabilizer and the glidant selectively contained, to form an emulsion, and homogenizing the obtained emulsion, and then The homogeneous emulsion is spray dried.

Preferably, in the modes (1) and (2), the mixing is performed under shearing conditions, and the mixing conditions include a temperature of 50-80 ° C, a shear rate of 10000-15000 rpm, and a time of 2 10min.

Preferably, the homogenous pressure is 30-35 MPa, and the number of times is 2-5 times.

Preferably, the conditions of the spray drying include an inlet air temperature of 180-240 ° C and an outlet air temperature of 75-85 ° C.

The present invention also provides a fullerene microcapsule powder, wherein the fullerene microcapsule powder contains a fullerene compound, a nutrient compound oil, an edible emulsifier, and a wall material.

Preferably, the total weight content of the fullerene compound and the nutritive compound oil is from 10% to 80% based on the total weight of the fullerene microcapsule powder and the weight of the fullerene compound The content of the edible emulsifier is from 0.01% to 5%, and the weight of the wall material is from 0.01% to 80%.

Preferably, the fullerene compound has a weight content of 1‰-5‰ based on the total weight of the fullerene microcapsule powder, and the nutritional compound oil has a weight content of 50%-70%. The weight content of the edible emulsifier is 4-6% by weight of the fat in the nutritional compound oil, and the weight content of the wall material is 29% to 49%.

Preferably, the fullerene microcapsule powder further contains a stabilizer and/or a glidant.

Preferably, the stabilizer is present in an amount of from 0.01% to 20% by weight based on the total weight of the fullerene microcapsule powder, and the glidant is present in an amount of from 0.01% to 2% by weight.

The types of the fullerene compound, the nutritional compound oil, the edible emulsifier, the wall material, the stabilizer, and the glidant have been described above, and will not be described herein.

Preferably, the fullerene microcapsule powder has a particle diameter of from 5 to 500 μm.

The preparation method of the fullerene microcapsule powder provided by the invention comprises:

Mode (1):

Oil phase preparation: the nutrient compound oil is formulated according to a ratio of fatty acids, and then the fullerene compound is sterilized and dissolved in a nutrient compound oil to form a compound oil compound, and then the edible emulsifier is dissolved. Into the compound oil composite, an oil phase is obtained;

Aqueous phase preparation: dissolving the wall material in hot water to obtain an aqueous phase; preferably, the temperature of the hot water is 60-80 ° C;

Mixed sterilization: mixing the obtained aqueous phase with the oil phase, stirring uniformly, and then sterilizing;

Homogenization, spray drying: homogenization, spray drying to obtain fullerene microcapsule powder;

Mode (2):

Dissolving the fullerene compound in the nutrient compounding oil to obtain a fullerene oil solution;

Mixing, dissolving, dispersing, and homogenizing the fullerene oil solution, the wall material, the edible emulsifier, and the stabilizer and the glidant selectively contained, to form an emulsion, and homogenizing the obtained emulsion, and then The homogeneous emulsion is spray dried.

Among them, the conditions of the mixing, homogenization and spray drying have been described above and will not be described herein.

In addition, the present invention also provides the fullerene microcapsule powder for use in the preparation of beverages, foods, beauty products, hangover products, and for preventing and/or treating liver cancer, neurodegenerative diseases (such as Parkinson's disease, senile dementia). And the application of drugs in tumors.

The fullerene compound cannot be completely dissolved in the fat or oil, and the amount of addition is not proportional to the solubility. If the dissolution is particularly small, the process is simple and the cost is low, but the amount of microcapsule powder ingested will increase accordingly, and accordingly, the amount of oil to be ingested will also increase, which does not meet the requirements of human nutrition; High, complex, technically difficult, and the cost of fullerenes will increase a lot. When the fullerene is added in an amount of 0.1 ‰ to 5 Torr, it can be dissolved by a simple stirring method, but at this time, since the amount of fullerene added is too low, the oxidation resistance is not ideal; when the amount is more than 5 ‰ The stirring cannot be completely dissolved, the undissolved fullerene is treated by centrifugation, and the residual fullerene is not cleaned. The Applicant's inventors have discovered through hard work that when a fullerene compound is formulated with a nutrient compound oil, a wall material, an edible emulsifier, and optionally a stabilizer and a glidant, the microcapsule powder can be A good antioxidant effect is achieved at a lower amount of fullerene (0.1 ‰ -5 Torr). At the same time, through experiments on its effects, it was found that fullerene intake of 8mg / day / person, can show significant antioxidant effect, which is equivalent to the intake of fullerene microcapsule powder amount of 20g / day / people.

When the addition amount of the nutrient compounding oil is less than 50%, the nutrients contained in the nutrient component are less, and the mouthfeel is poor; when the amount of the nutrient compounding oil is more than 70%, the oil is easily broken, and the embedding effect is Not good, will affect the brewing, the microcapsule powder produced is easy to agglomerate and agglomerate. Therefore, preferably, the weight content of the nutritional compound oil in the fullerene microcapsule powder provided by the present invention is particularly preferably from 50% to 70%.

The fullerene is made into a microcapsule powder and can be ingested as a food, and is more flexible in terms of taste and intake. The use of fullerenes as microcapsules greatly enhances their field of application. The fullerene microcapsule powder of the invention adopts a food material as a wrapping material, and transforms it into a nutritious drink with convenient consumption and various flavors, and can be taken in a short-term or long-term manner, and has anti-aging and anti-cancer health effects, and has a high Promotion value.

The invention can effectively overcome the fact that the fullerene compound and the fullerene oil solution are difficult to preserve by using a fullerene compound, a nutrient compound oil, a wall material, an edible emulsifier, and an optional stabilizer and a glidant. It is easy to oxidize, accelerates discoloration or fading of pigments, easily hardens proteins, reduces digestibility, destroys vitamins, easily causes decomposition of nutrients, and produces toxic substances, which can significantly increase fullerene compounds. The stability is such that the fullerene compound can fully exert its activity. In addition, the fullerene microcapsule powder provided by the invention has the advantages of being soluble in water, high stability, convenient transportation, easy storage, and more flexible and diversified in taste and ingestion manner as a raw material of food or medicine.

The fullerene microcapsule powder provided by the invention overcomes the limitations of the prior art, and enables fullerenes and their derivatives to be applied in the field of body adaptability, and provides a new loading mode--microencapsulation.

The fullerene microcapsule powder provided by the invention can greatly broaden the application of fullerene compounds in various fields, for example, in the health industry, the fullerene microcapsule powder can be formulated into fullerene-containing micro-capsules. Solid beverages of sac powder, especially middle-aged and solid beverages, special medical foods containing fullerene microcapsule powder, cosmetic health products containing fullerene microcapsule powder, hangover products containing fullerene microcapsule powder; The medical application can be used for the preparation of a medicament for preventing and/or treating diseases such as liver cancer, neurodegenerative diseases (such as Parkinson's disease, senile dementia), and tumors.

DRAWINGS

1 is a schematic view showing the microstructure of a fullerene microcapsule powder provided by the present invention;

2 is a graph showing POV values of fullerene microcapsule powder and fullerene oil solution as a function of storage time;

Figure 3 is a graph showing the fullerene content in fullerene microcapsule powder and fullerene oil solution as a function of storage time.

detailed description

The embodiments of the present invention are described in detail below, and the examples of the embodiments are intended to explain the present invention and are not to be construed as limiting. Where specific techniques or conditions are not indicated in the examples, they are carried out according to the techniques or conditions described in the literature in the art or in accordance with the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are conventional products that can be obtained commercially.

Preparation Example 1: Preparation of fullerene oil solution

Accurately weigh 100g of nutritional compound oil (Olive oil, linseed oil, Wenguan fruit oil weight ratio of 5:3:2) and 0.3g fullerene C ₆₀ , pour the above raw materials into a ball mill tank for ball milling, ball milling The product was transferred to a centrifuge bottle and centrifuged at 8000 r/min for 1 h. The centrifuged product was sterilized by a filtering device (0.5 μm), and the product obtained after sterilization was a fullerene nutritional compound oil solution.

Preparation 2: Preparation of fullerene oil solution

Accurately weigh 100g of olive oil and 0.15g of fullerene C ₆₀ , pour the above raw materials into a ball mill tank for ball milling, transfer the ball milled product to a centrifuge bottle for centrifugation at 7000r/min for 1.5h, and pass the centrifuged product through filtration. The device (0.5 μm) was subjected to sterilization treatment, and the product obtained after sterilization was a fullerene olive oil solution.

Preparation 3: Preparation of fullerene oil solution

Accurately weigh 100g sea buckthorn seed oil and 0.12g fullerene C ₇₀ , pour the above raw materials into a ball mill tank for ball milling, transfer the ball milled product to a centrifuge bottle for 6h at 6500r/min, and pass the filtered product through filtration. The device (0.5 μm) was subjected to sterilization treatment, and the product obtained after sterilization was a fullerene sea buckthorn oil solution.

Preparation Example 4: Preparation of fullerene oil solution

Accurately weigh 100g soybean oil and 0.08g fullerene C ₇₀ , pour the above raw materials into a ball mill tank for ball milling, transfer the ball milled product to a centrifuge bottle for 6000h/min centrifugation for 2.5h, and pass the centrifuged product through filtration. The device (0.5 μm) was subjected to sterilization treatment, and the product obtained after sterilization was a fullerene soybean oil solution.

The formulations of the fullerene microcapsule powders of Examples 1-4 are shown in Table 1:

Table 1 The amount of each raw material in Example 1-4 (wt%)

project	Fullerene oil solution	Wall material	Edible emulsifier	stabilizer	Glidant
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

Preparation method: 60% by weight of maltodextrin (wall material), 2% by weight of sodium caseinate (edible emulsifier), 1% by weight of dipotassium hydrogen phosphate (stabilizer) and 1% by weight of dioxide Silicon (glidant) and distilled water were mixed and dissolved, and a 50 wt% fullerene nutrient compound oil solution (obtained in Preparation Example 1) was added to prepare an emulsion. The emulsification was sheared at 11200 rpm for 5 min at 60 °C. The sheared emulsion was immediately homogenized three times by high pressure homogenizer, the homogenization pressure was 30-35 MPa, and the homogenized emulsion was spray-dried, the inlet air temperature was 200 ° C, and the outlet air temperature was 82 ° C. The fullerene microcapsule powder is obtained, and its microscopic morphology is shown in FIG. It can be seen from the results of Fig. 1 that the fullerene microcapsule powder has a particle diameter of 5-20 μm and a hollow spherical or elliptical shape inside, which is due to the occurrence of bubbles inside the particle when the outer shell of the product is rapidly formed. When the temperature of the particles exceeds the vaporization temperature of the surrounding moisture and the vapor pressure inside the particles exceeds the pressure of the surrounding environment, the outer casing expands. In addition, the fullerene microcapsule powder has a spherical or elliptical shape, and the surface is smooth, dense, and free of cracks, and some of the particles have a slight depression and shrinkage, which is unique to the spray drying process.

Example 2: Preparation of fullerene microcapsule powder

Raw materials: see Table 1

Preparation method: 60 ° C, 62.7 wt% maltodextrin (wall material), 2 wt% sodium caseinate (edible emulsifier), 1 wt% dipotassium hydrogen phosphate (stabilizer) and 1 wt% of two Silica (glidant) and distilled water were mixed and dissolved, and a 33.3 wt% fullerene olive oil solution (obtained in Preparation Example 2) was added to prepare an emulsion. The emulsification was sheared at 11200 rpm for 5 min at 60 °C. The sheared emulsion was immediately homogenized three times by high pressure homogenizer, the homogenization pressure was 30-35 MPa, and the homogenized emulsion was spray-dried, the inlet air temperature was 200 ° C, and the outlet air temperature was 82 ° C. A fullerene microcapsule powder having a particle diameter of 100 to 200 μm is obtained.

Example 3: Preparation of fullerene microcapsule powder

Raw materials: see Table 1

Preparation method: at 60 ° C, 71 wt% of maltodextrin (wall material), 2 wt% of sodium caseinate (edible emulsifier), 1 wt% of dipotassium hydrogen phosphate (stabilizer) and 1 wt% of dioxide Silicon (glidant) and distilled water were mixed and dissolved, and a 25 wt% fullerene sea buckthorn seed oil solution (obtained in Preparation Example 3) was added to prepare an emulsion. The emulsification was sheared at 11200 rpm for 5 min at 60 °C. The sheared emulsion was immediately homogenized three times by high pressure homogenizer, the homogenization pressure was 30-35 MPa, and the homogenized emulsion was spray-dried, the inlet air temperature was 200 ° C, and the outlet air temperature was 82 ° C. A fullerene microcapsule powder having a particle diameter of 225 to 305 μm is obtained.

Example 4: Preparation of fullerene microcapsule powder

Raw materials: see Table 1

Preparation method: 9.4 wt% soy protein isolate (wall material) was dissolved in distilled water, temperature-controlled magnetic stirrer treatment at 80 ° C for 30 min, cooling; 0.5 wt% sodium carboxymethyl cellulose (stabilizer) and 1.5 wt% Silica (glidant) is dissolved in distilled water, and then 37.6% of maltodextrin (wall material) is mixed with the above-mentioned soy protein isolate solution, sodium carboxymethylcellulose and silica, and mixed to 50% by weight. 1% lecithin (edible emulsifier) was added to the fullerene soybean oil solution (obtained in Preparation Example 4), and the lecithin was thoroughly dissolved by stirring with a glass rod, and the above materials were mixed and cut at 11200 rpm. Emulsified for 5 min. The sheared emulsion was immediately subjected to high pressure homogenization three times with a high pressure homogenizer, the homogenization pressure was 35 MPa, and the homogenized emulsion was spray dried, the inlet air temperature was 220 ° C, and the outlet air temperature was 80 ° C. Fullerene microcapsule powder having a particle size of 310-400 μm.

The formulations of the fullerene microcapsule powders of Examples 5-8 are shown in Table 2:

Table 2 The amount of each raw material in Examples 5-8 (wt%)

project	Sterile fullerene	Edible emulsifier	Nutritional compound oil	Wall material
Example 5	1‰	3.0%	50%	46.90%
Example 6	5‰	3.5%	70%	26.00%
Example 7	2.5‰	2.5%	50%	47.25%
Example 8	3‰	3.0%	60%	36.70%

Note: In the nutritional compound oil of Examples 5-8, the weight ratio of saturated fatty acid, monounsaturated fatty acid to polyunsaturated fatty acid is 1:1:1, and the weight ratio of linoleic acid to linolenic acid in polyunsaturated fatty acid It is 1:1.

Example 5: Preparation of fullerene microcapsule powder

Raw materials: See Table 2.

Preparation:

(1) preparing a nutritional compound oil according to the ratio of fatty acids;

(2) sterilizing the fullerene and dissolving it into a nutrient compounding oil to form a compound oil complex;

(3) dissolving the edible emulsifier into the compound oil composite to obtain an oil phase;

(4) dissolving the wall material in 60-80 ° C hot water to obtain an aqueous phase;

(5) mixing the obtained aqueous phase with the oil phase, stirring, and then sterilizing;

(6) homogenizing, spraying and drying to obtain fullerene microcapsule powder.

The prepared fullerene microcapsule powder has an antioxidant capacity of 125 times that of vitamin C as determined by an in vitro β-carotene oxidation method.

Example 6: Preparation of fullerene microcapsule powder

Raw materials: See Table 2.

The production process is the same as in the fifth embodiment. The prepared fullerene microcapsule powder has an antioxidant capacity of 125 times that of vitamin C as determined by an in vitro β-carotene oxidation method.

Example 7: Preparation of fullerene microcapsule powder

Raw materials: See Table 2.

The production process is the same as in the fifth embodiment. The prepared fullerene microcapsule powder has an antioxidant capacity of 125 times that of vitamin C as determined by an in vitro β-carotene oxidation method.

Example 8: Preparation of fullerene microcapsule powder

Raw materials: See Table 2.

The production process is the same as in the fifth embodiment. The prepared fullerene microcapsule powder has an antioxidant capacity of 125 times that of vitamin C as determined by an in vitro β-carotene oxidation method.

Test example 1

(1) Stability test

The Schaler oven method was used to test the oxidative stability of fullerene microcapsule powder and the fullerene content in fullerene microcapsule powder. Specifically, 12 dry and clean 50 mL screw bottles were added to each group, and 1 was added. The /2-volume fullerene microcapsule powder was stored in an oven at 60±2°C and 60% humidity for accelerated storage. A test bottle was taken every 5 days, and the POV value and fullerene content of the sample were measured. After 60 days, End the test.

Control test: The corresponding fullerene oil solution was tested for storage and stability using the above method.

A. Determination of POV value in fullerene microcapsule powder

Sample pretreatment: using toluene as solvent, using ultrasonic vibration to break the wall and extract the oil, weigh 5g sample in 50mL colorimetric tube, add 25mL toluene, put it in the ultrasonic cleaner water tank, ultrasonically shake for 30 minutes, take out, filter, and use The toluene was sufficiently washed, the filtrate was combined (the above operation was repeated twice), toluene was recovered by a rotary evaporator, heated in a water bath, toluene was fully exerted, and it was placed in a vacuum drying oven, and toluene was further removed at 50 ° C for use.

The POV value was determined according to the method specified in GB/T5538-2005 Determination of peroxide value of animal and vegetable oils.

2 is a graph showing the POV value of the fullerene microcapsule powder obtained in Example 1 and the corresponding fullerene oil solution as a function of storage time during high temperature storage. According to the hygienic standard of edible oils and fats per stipulated by the Codex Alimentarius Commission (≦10meq/kg), it can be seen from Figure 2 that the fullerene microcapsule powder is kept at an acceptable temperature within 60 °C. The time is 35d, while the fullerene oil solution under the same conditions can only be stored for 20d.

B, detection of fullerene content

Sample pretreatment: using toluene as solvent, using ultrasonic vibration to break the wall and extract the oil, weigh 5g sample in 50mL colorimetric tube, add 25mL toluene, put it in the ultrasonic cleaner water tank, ultrasonically shake for 30 minutes, take out, filter, and use The toluene was thoroughly washed, the filtrate was combined (the above operation was repeated twice), toluene was recovered by a rotary evaporator, heated in a water bath, and the mixture was placed in toluene, placed in a vacuum drying oven, and toluene was further removed at 50 ° C for use.

The fullerene microcapsule powder sample was pretreated and the fullerene oil solution and the control fullerene oil solution were filtered, and 1 mL was added to 3 mL of a toluene solution to dilute and dissolve. The column was analyzed by high performance liquid chromatography with a standard solution concentration of 0.3 mg/mL. Control peak area: 21296401 mAU*min.

Data: Concentration = A _-like * C _standard * 4 / A _standard

Where: A _-like - peak area of the sample mAU * min;

A _standard - the peak area of the standard mAU * min.

C _standard - the concentration of the standard product mg / mL.

High performance liquid chromatography detection conditions:

Column: 5Pye Waters 4.6*250mm

Wavelength: 320nm

Flow rate: 1mL/min

Column temperature: 30 ° C

Mobile phase: toluene

Detector: UV detector

Figure 3 is a graph showing the fullerene content of the fullerene microcapsule powder obtained in Example 1 and the corresponding fullerene oil solution as a function of storage time during high temperature storage. The results in Figure 3 show that the content of fullerenes in the experimental group and the control group remained unchanged over time. At the 10th day, the fullerene content in the fullerene oil solution began to decrease. The fullerene content in the fullerene microcapsules began to decrease on the 15th day. This indicates that the fullerene microcapsule powder can protect the fullerene and is not easily oxidized.

(2) Immunological performance test

Test animals and test group: 40 healthy pigs with uniform body weight, uniform male-female ratio and similar age were randomly divided into 4 groups, 10 in each group, one experimental group, one control group, and one repeat group. , carry out feeding experiments.

The experimental design: the test diet was divided into two groups, the control group and the experimental group, the control group added the basic diet, and the experimental group added 1wt% fullerene microcapsule powder on the basis of the control group. The test period is from March 30, 2018 to May 30, for a total of 60 days.

Feeding management: 60 days in the whole experiment, 40 pigs were kept in the same pig house, and each group was kept in 10 pigs per lap. It was well ventilated and the temperature was suitable. It was regularly disinfected according to the pig quarantine program, and nipple water was used. The device provides sufficient clean drinking water, and the test pigs are fed 3 times a day, free to eat and drink. Observe the pig's intake, drinking water, stool color and morbidity, and make daily records. Other management is carried out according to the normal management of the farm.

1. Determination of immunoglobulin: After the end of feeding, one pig with a body weight close to the average weight of the treatment was selected, and the anterior vena cava was collected. 5 mL of blood was collected by ordinary vacuum blood collection tube (3500 r/min, centrifuged for 5 min, serum was separated, and stored in -20 ° C refrigerator), used to determine the immunoglobulin in pig serum, immunoglobulin was determined by immunoturbidimetry.

2. Blood routine measurement: After the end of feeding, each pig with a weight close to the average weight of the treatment was selected, and the anterior vena cava was collected. The blood was quickly taken out and poured into an anticoagulant blood vessel with anticoagulant. The automatic animal blood cell analyzer measures the total number of red blood cells, total white blood cells, lymphocytes, intermediate cells and granulocytes in whole blood.

Data processing: After finishing and preliminary calculations using Excel, the general linear model of SPSS statistical software was used for one-way analysis of variance, and Duncan's method was used for multiple comparisons. Among them, the data were expressed as mean ± standard error, and P < 0.05 was used as the criterion for difference significance, and regression analysis was used for analysis.

Test results: The effect of the fullerene microcapsule powder obtained in Example 1 on serum physiological indexes in pigs is shown in Table 3. The results showed that compared with the control group, the experimental group significantly increased (P <0.05) the number of blood lymphocytes, and significantly increased (P <0.01) the number of granulocytes, but the total number of white blood cells, the number of intermediate cells, the total number of red blood cells and Hemoglobin had no significant effect (P>0.05).

The effect of the fullerene microcapsule powder obtained in Example 1 on immunoglobulin in pig serum is shown in Table 4. The results showed that the experimental group could significantly increase the serum IgM content (P<0.05), but had no significant effect on IgA and IgG (P>0.05).

This experimental study found that the addition of fullerene microcapsule powder significantly increased the number of lymphocytes and granulocytes in pig blood compared with no addition, but had no significant effect on other blood physiological indicators and immunoglobulin. In summary, fullerene microcapsule powder can promote the development of immune organs in pigs and promote the formation of lymphocytes and granulocytes, thereby improving immunity.

Table 3 Effect of fullerene microcapsule powder on physiological indexes of pig serum

Group	Control group	test group
White blood cell count, × 10 9 /L	18.10±0.69	20.16±1.20
Number of lymphocytes, ×10 9 /L	7.50 a ±1.35	8.65 ab ±1.24
Intermediate cell, ×10 9 /L	2.57±0.87	3.26±0.62
Granulocytes, ×10 9 /L	7.28 b ±1.03	11.16 a ±0.98
Red blood cells, ×10 9 /L	5.45±0.21	5.69±0.65
Hemoglobin, g/L	92.1±3.10	96.33±4.02

Table 4 Effect of fullerene microcapsule powder on immunoglobulin in pig serum

Group	Control group	test group
Immunoglobulin IgA	0.68±0.01	0.70±0.08
Immunoglobulin IgG	5.61±0.34	5.57±0.28
Immunoglobulin IgM	0.56 b ±0.05	0.78 a ±0.10

Test Example 2: Experiment of improving immunity by fullerene microcapsule powder

5 g of the fullerene microcapsule powder obtained in any of Examples 5-8, an anthocyanin 1 g, and a vitamin C 500 mg were prepared into a powder or compressed into tablets, and the long-term administration has an effect of improving immunity.

Test Example 3: Effect experiment of fullerene microcapsule powder for health care

20 g of the fullerene microcapsule powder obtained in any of Examples 5-8. Long-term consumption by one person once a day in the form of direct brewing can prevent cancer and delay neurodegenerative diseases such as Parkinson's and Alzheimer's disease. At the same time, the patient reflects that the fullerene microcapsule powder is more acceptable in taste and consumption than pure fullerene olive oil.

Test Example 4: Detoxification product containing fullerene microcapsule powder and effect verification experiment

2 g of fullerene microcapsule powder obtained in any of Examples 5-8, 1 g of puerarin, 1 g of medlar, 0.25 g of medlar, and 1 g of honey, which are made into powder or solid granules, and have a relief after drinking. Drunk, headache and vomiting symptoms.

The hangover experiment:

Product safety determination of the invention:

Twenty healthy Kunming mice (body weight 18-22g), male and female, were randomly divided into two groups, 10 in each group. The drug-administered group: 0.33ml/20gBW (equivalent to 10 times the amount taken by humans) (Calculation method: human effective dose 5.25g (calculated according to human body weight 65kg), converted into 20g mouse 10 times dose is about 0.0165; hangover product 0.5g dissolved in 10ml water, 0.33ml contains 0.0165g, ie mouse irrigation The amount required for the stomach was 0.33 ml/20 g), and the control group: 0.33 ml/20 g of BW was administered with the same amount of physiological saline. Both groups were fed continuously for 7 days, and the growth status, adverse reactions and death of the mice were observed. On the 8th day, the mice were sacrificed, and abnormalities of various organs were observed under the naked eye and under the microscope. The observation results showed that no adverse reactions occurred in the mice, and no abnormal findings were observed under the microscope.

Pre-test:

According to the relevant literature, 6 groups of mice were respectively treated with 0.26ml/20g, 0.28ml/20g, 0.30ml/20g, 0.32ml/20g, 0.34ml/20g, 0.36ml/20g wine solution (56 degree red star Erguotou). Stomach, 6 in each group. The amount of alcohol required to cause the disappearance of righting reflex in the mice without death of the mice was observed. The experimental results are shown in Table 5: The 0.30 ml/20 g wine solution was selected for subsequent experiments.

Table 5 Table of effects on mortality of alcoholism in mice

Group	Total 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

Effects of administration on drunkenness, hangover time and drunkenness in mice with acute alcoholism:

The mice were randomly divided into 4 groups: model group (administered volumetric saline), low-dose group (administered 0.1ml/20g), medium-dose group (administered 0.2ml/20g), high dose (administered 0.3ml) /20g), 10 per group. Each group of mice was fasted for 12 h and administered once. After 30 minutes, each group was given 15 ml/kg (based on pre-experiment data) and the weight of 56 °C Beijing Erguotou wine was intragastrically administered. The drunkenness time of the mice (from the time of waking to the disappearance of anyway reflex) was observed and the drunk rate within 24 hours was calculated. Whether the mice are drunk or not, whether the righting reflex disappears as the standard: after the mice are drunk, put them back down and gently put them into the squirrel cage. If the mouse is kept in a downward posture for more than 30 s, it is considered that the righting reflex Disappeared, that is drunk. Observe the time of waking up the mice (from the time of righting reflex to awake) and calculate the mortality within 24 hours. The results are shown in Tables 6-7. It can be seen that the fullerene microcapsule powder provided by the present invention has a good hangover effect.

Table 6 Dose tables for different experimental groups

Group	Quantity	Dosage amount (ml/20g)	Equivalent to human body (mg/kg)
Control group	20	0.1	-
Low dose group	20	0.04	150
Medium dose group	20	0.08	300
High dose group	20	0.1	450

Start drinking at 10 o'clock.

Note: The control group was administered dH ₂ O.

Table 7 Table of results after different groups of alcohol

project	Control group	Low dose group	Medium dose group	High dose group
Drunk time	10:30	11:00	11:20	12:00
Sobering time	15:30	15:00	15:00	15:30
Drunk time	5h	4h	3h40min	3h30min
Number of deaths within 24 hours	0	0	0	0

It can be seen from Table 6-7 that the low-dose group, the middle-dose group, and the high-dose group are significantly shorter than the control, and the duration of drunkenness is shortened, and the duration is shortened as the dose is increased, indicating that the hangover product containing the fullerene microcapsule powder is taken. With obvious hangover effect.

The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solutions of the present invention within the scope of the technical idea of the present invention. These simple variants All fall within the scope of protection of the present invention.

It should be further noted that the specific technical features described in the above specific embodiments may be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not be further described in various possible combinations.

In addition, any combination of various embodiments of the invention may be made as long as it does not deviate from the idea of the invention, and it should be regarded as the disclosure of the invention.

Claims (13)

1. The use of fullerene compounds for the preparation of fullerene microcapsule powders.
2. The use of the fullerene compound according to claim 1 for preparing a fullerene microcapsule powder, wherein the fullerene microcapsule powder contains a fullerene compound, a nutrient compound oil, Edible emulsifiers and wall materials;

   Preferably, the total weight content of the fullerene compound and the nutritive compound oil is from 10% to 80% based on the total weight of the fullerene microcapsule powder and the weight of the fullerene compound The content of the edible emulsifier is 0.01%-5%, the weight content of the wall material is 0.01%-80%;

   Preferably, the fullerene compound has a weight content of 1‰-5‰ based on the total weight of the fullerene microcapsule powder, and the nutritional compound oil has a weight content of 50%-70%. The weight content of the edible emulsifier is 4-6% by weight of the fat in the nutritional compound oil, and the weight content of the wall material is 29% to 49%.
3. The use of the fullerene compound according to claim 2 for the preparation of a fullerene microcapsule powder, characterized in that the fullerene compound is selected from the group consisting of C ₆₀ and its derivatives, C ₇₀ and derivatives thereof At least one of a compound, a fullerene metal derivative, a fullerene oxygen-containing derivative, a fullerene modified or encapsulated with an organic compound, or a fullerene derivative modified or encapsulated with an organic compound; preferably An oxygen atom in the fullerene oxygen-containing derivative is bonded to a carbon atom on a fullerene skeleton or bonded to an alkylene chain, and the organic compound is modified or encapsulated with fullerene and fullerene The organic compound in the derivative is a cyclodextrin and/or a crown ether;

   The nutritional compound oil is selected from at least one of an edible oil, an oil-soluble vitamin, a hydrocarbon, a fatty acid, a higher alcohol, and an ester; preferably, the edible oil includes a vegetable oil and an animal oil, and the vegetable oil is selected from the group consisting of vegetable oil and animal oil. Soybean oil, rapeseed oil, palm oil, olive oil, sunflower oil, celery 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 nut oil, evening primrose oil, safflower seed oil, borage oil, hemp seed oil, salad oil, wheat At least one of germ oil, avocado oil and sea buckthorn oil selected from at least one of lard, tallow, sheep oil, fish oil, horse oil and sea turtle oil; preferably, the hydrocarbon is Squalane and/or squalene; preferably, the fatty acid is selected from the group consisting of oleic acid, linoleic acid, linolenic acid, conjugated linoleic acid, DHA, stearic acid, lauric acid, arachidonic acid, and EPA At least one of; preferably, the higher alcohol is selected from the group consisting of octyldodecanol, lauryl alcohol, and At least one of sterol, cholesterol, and stearyl alcohol; preferably, the ester is conjugated linoleic acid triglyceride and/or linoleic acid glyceride; preferably, the nutritional compound oil is flax Seed oil, safflower seed oil, perilla seed oil, camellia seed oil, sunflower oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, sea buckthorn fruit oil, sea buckthorn seed oil, peony seeds Oil, walnut oil, celery oil, sea buckthorn oil, sesame oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid, conjugated linoleic acid triglyceride combination;

   The edible emulsifier is selected from the group consisting of sucrose fatty acid esters, polyglycerin fatty acid esters, glycerin fatty acid esters, polyoxyethylene sorbitan fatty acid esters, sodium caseinate, lecithin, sodium stearate, monoglycerin organic At least one of an acid fatty acid ester, a betaine, an amino acid salt, a glyceryl succinate fatty acid ester, a sodium stearoyl lactate, a Tween-80, a Span-80, a polyglycerol ester, a propylene glycol fatty acid ester, and a polysorbate fatty acid ester Or; the edible emulsifier is A, or a mixture of A and B, A is one or both of oligofructose, resistant dextrin, skim milk powder, B is sodium caseinate, single, a diglycerin fatty acid ester, sodium starch octenyl succinate, ascorbic acid, sodium ascorbate, phospholipids, natural vitamin E, sodium tripolyphosphate, and ascorbyl palmitate;

   The wall material is selected from the group consisting of maltodextrin, soy protein isolate, gum arabic, beta-cyclodextrin, starch, whey protein concentrate, dextrin, corn syrup, gelatin, sodium carboxymethylcellulose, xanthan gum, agar Carrageenan, chitosan, octenyl succinate starch, guar gum, seaweed gum, alginate, milk protein, casein, gluten, gliadin, cocoa butter, casein acid, Plant protein, lactose, sucrose, maltose, methylcellulose, ethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, crystalline cellulose and water soluble At least one of dietary fiber; preferably, the wall material is a mixture of two or more of soy protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose, maltodextrin .
4. The use of the fullerene compound according to claim 2 or 3 for preparing a fullerene microcapsule powder, characterized in that the nutrient compound oil has a fatty acid fatty acid ratio of a saturated fatty acid: monounsaturated fatty acid: The weight ratio of polyunsaturated fatty acid is 1: (0.5-2): (0.5-2), and the weight ratio of linoleic acid: linolenic acid in the polyunsaturated fatty acid is 1: (0.5-2);

   Preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1: (0.5-1.5): (0.5-1.5), in the polyunsaturated fatty acid Linoleic acid: linolenic acid weight ratio is 1: (0.5-1.5);

   More preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1:1:1, linoleic acid: linolenic acid weight in the polyunsaturated fatty acid The ratio is 1:1.
5. The use of the fullerene compound according to any one of claims 2 to 4 for producing a fullerene microcapsule powder, characterized in that the fullerene microcapsule powder further contains a stabilizer and/or Or a glidant;

   Preferably, the stabilizer has a weight content of 0.01%-20%, and the glidant has a weight content of 0.01%-2%, based on the total weight of the fullerene microcapsule powder;

   Preferably, the stabilizer is selected from the group consisting of erythorbic acid and its salts, gallic acid and its derivatives, gluconic acid, sodium tripolyphosphate, complex phosphate, dipotassium hydrogen phosphate, sodium polyphosphate, sodium metaphosphate, carboxymethyl At least one of cellulose sodium and agar;

   Preferably, the flow aid is at least one selected from the group consisting of silicates, stearates, iron salts, phosphates, polysaccharides, talc, calcium carbonate and zinc dioxide; preferably, the silicon The acid salt is selected from at least one of silica, calcium silicate, sodium aluminum silicate, magnesium silicate, and sodium aluminosilicate, the stearate being selected from the group consisting of sodium stearate, calcium stearate, and hard At least one of aluminum sulphate and zinc stearate, the iron salt being ammonium ammonium citrate and/or sodium ferric hydride, the phosphate being calcium phosphate and/or magnesium phosphate, the polysaccharide being a solution Poly starch and/or microcrystalline depolymerized cellulose.
6. The use of the fullerene compound according to any one of claims 1 to 5 for producing a fullerene microcapsule powder, characterized in that the fullerene microcapsule powder is in the following manner (1) or The method (2) is prepared:

   Mode (1):

   Oil phase preparation: the nutrient compound oil is formulated according to a ratio of fatty acids, and then the fullerene compound is sterilized and dissolved in a nutrient compound oil to form a compound oil compound, and then the edible emulsifier is dissolved. Into the compound oil composite, an oil phase is obtained;

   Aqueous phase preparation: dissolving the wall material in hot water to obtain an aqueous phase; preferably, the temperature of the hot water is 60-80 ° C;

   Mixed sterilization: mixing the obtained aqueous phase with the oil phase, stirring uniformly, and then sterilizing;

   Homogenization, spray drying: homogenization, spray drying to obtain fullerene microcapsule powder;

   Mode (2):

   Dissolving the fullerene compound in the nutrient compounding oil to obtain a fullerene oil solution;

   Mixing, dissolving, dispersing, and homogenizing the fullerene oil solution, the wall material, the edible emulsifier, and the stabilizer and the glidant selectively contained, to form an emulsion, and homogenizing the obtained emulsion, and then The homogeneous emulsion is spray dried;

   Preferably, in the modes (1) and (2), the mixing is performed under shearing conditions, and the mixing conditions include a temperature of 50-80 ° C, a shear rate of 10000-15000 rpm, and a time of 2 10 min; the homogenous pressure is 30-35 MPa, the number of times is 2-5 times; the spray drying conditions include an inlet air temperature of 180-240 ° C, and an outlet air temperature of 75-85 ° C.
7. A fullerene microcapsule powder, characterized in that the fullerene microcapsule powder contains a fullerene compound, a nutrient compound oil, an edible emulsifier and a wall material;

   Preferably, the total weight content of the fullerene compound and the nutritive compound oil is from 10% to 80% based on the total weight of the fullerene microcapsule powder and the weight of the fullerene compound The content of the edible emulsifier is 0.01%-5%, the weight content of the wall material is 0.01%-80%;

   Preferably, the fullerene compound has a weight content of 1‰-5‰ based on the total weight of the fullerene microcapsule powder, and the nutritional compound oil has a weight content of 50%-70%. The weight content of the edible emulsifier is 4-6% by weight of the fat in the nutritional compound oil, and the weight content of the wall material is 29% to 49%.
8. The fullerene microcapsule powder according to claim 7, wherein

   The fullerene compound includes C ₆₀ and its derivatives, C ₇₀ and its derivatives, fullerene metal derivatives, fullerene oxygenated derivatives, organic compounds modified or encapsulated fullerenes, At least one of the organic compound modified or encapsulated fullerene derivative; preferably, the oxygen atom in the fullerene oxygen-containing derivative is linked to a carbon atom on the fullerene skeleton or to an alkylene chain Bonding, the organic compound in the fullerene and fullerene derivative modified or encapsulated by the organic compound is a cyclodextrin and/or a crown ether;

   The nutritional compound oil is selected from at least one of an edible oil, an oil-soluble vitamin, a hydrocarbon, a fatty acid, a higher alcohol, and an ester; preferably, the edible oil includes a vegetable oil and an animal oil, and the vegetable oil is selected from the group consisting of vegetable oil and animal oil. Soybean oil, rapeseed oil, palm oil, olive oil, sunflower oil, celery 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 nut oil, evening primrose oil, safflower seed oil, borage oil, hemp seed oil, salad oil, wheat At least one of germ oil, avocado oil and sea buckthorn oil selected from at least one of lard, tallow, sheep oil, fish oil, horse oil and sea turtle oil; preferably, the hydrocarbon is Squalane and/or squalene; preferably, the fatty acid is selected from the group consisting of oleic acid, linoleic acid, linolenic acid, conjugated linoleic acid, DHA, stearic acid, lauric acid, arachidonic acid, and EPA At least one of; preferably, the higher alcohol is selected from the group consisting of octyldodecanol, lauryl alcohol, and At least one of sterol, cholesterol, and stearyl alcohol; preferably, the ester is conjugated linoleic acid triglyceride and/or linoleic acid glyceride; preferably, the nutritional compound oil is flax Seed oil, safflower seed oil, perilla seed oil, camellia seed oil, sunflower oil, soybean oil, olive oil, pumpkin seed oil, evening primrose oil, borage oil, sea buckthorn fruit oil, sea buckthorn seed oil, peony seeds Oil, walnut oil, celery oil, sea buckthorn oil, sesame oil, linoleic acid, linolenic acid, linoleic acid triglyceride, conjugated linoleic acid, conjugated linoleic acid triglyceride combination;

   The edible emulsifier is selected from the group consisting of sucrose fatty acid esters, polyglycerin fatty acid esters, glycerin fatty acid esters, polyoxyethylene sorbitan fatty acid esters, sodium caseinate, lecithin, sodium stearate, monoglycerin organic At least one of an acid fatty acid ester, a betaine, an amino acid salt, a glyceryl succinate fatty acid ester, a sodium stearoyl lactate, a Tween-80, a Span-80, a polyglycerol ester, a propylene glycol fatty acid ester, and a polysorbate fatty acid ester Or; the edible emulsifier is A, or a mixture of A and B, A is one or both of oligofructose, resistant dextrin, skim milk powder, B is sodium caseinate, single, a diglycerin fatty acid ester, sodium starch octenyl succinate, ascorbic acid, sodium ascorbate, phospholipids, natural vitamin E, sodium tripolyphosphate, and ascorbyl palmitate;

   The wall material is selected from the group consisting of maltodextrin, soy protein isolate, gum arabic, beta-cyclodextrin, starch, whey protein concentrate, dextrin, corn syrup, gelatin, sodium carboxymethylcellulose, xanthan gum, agar Carrageenan, chitosan, octenyl succinate starch, guar gum, seaweed gum, alginate, milk protein, casein, gluten, gliadin, cocoa butter, casein acid, Plant protein, lactose, sucrose, maltose, methylcellulose, ethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, crystalline cellulose and water soluble At least one of dietary fiber; preferably, the wall material is a mixture of two or more of soy protein isolate, xanthan gum, modified starch, gelatin, carboxymethyl cellulose, maltodextrin .
9. The fullerene microcapsule powder according to claim 7 or 8, wherein the nutrient-mixing oil has a ratio of fatty acid to fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid in a weight ratio of 1: (0.5) -2): (0.5-2), the weight ratio of linoleic acid: linolenic acid in the polyunsaturated fatty acid is 1: (0.5-2);

   Preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1: (0.5-1.5): (0.5-1.5), in the polyunsaturated fatty acid Linoleic acid: linolenic acid weight ratio is 1: (0.5-1.5);

   More preferably, the nutritional fatty acid ratio of the nutritional compound oil is saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid weight ratio is 1:1:1, linoleic acid: linolenic acid weight in the polyunsaturated fatty acid The ratio is 1:1.
10. The fullerene microcapsule powder according to any one of claims 7-9, wherein the fullerene microcapsule powder further contains a stabilizer and/or a glidant;

    Preferably, the stabilizer has a weight content of 0.01%-20%, and the glidant has a weight content of 0.01%-2%, based on the total weight of the fullerene microcapsule powder;

    Preferably, the stabilizer is selected from the group consisting of erythorbic acid and its salts, gallic acid and its derivatives, gluconic acid, sodium tripolyphosphate, complex phosphate, dipotassium hydrogen phosphate, sodium polyphosphate, sodium metaphosphate, carboxymethyl At least one of cellulose sodium and agar;

    Preferably, the flow aid is at least one selected from the group consisting of silicates, stearates, iron salts, phosphates, polysaccharides, talc, calcium carbonate and zinc dioxide; preferably, the silicon The acid salt is selected from at least one of silica, calcium silicate, sodium aluminum silicate, magnesium silicate, and sodium aluminosilicate, the stearate being selected from the group consisting of sodium stearate, calcium stearate, and hard At least one of aluminum sulphate and zinc stearate, the iron salt being ammonium ammonium citrate and/or sodium ferric hydride, the phosphate being calcium phosphate and/or magnesium phosphate, the polysaccharide being a solution Poly starch and/or microcrystalline depolymerized cellulose.
11. The fullerene microcapsule powder according to any one of claims 7 to 10, wherein the fullerene microcapsule powder has a particle diameter of 5 to 500 μm.
12. The method for preparing a fullerene microcapsule powder according to any one of claims 7-11, wherein the method comprises:

    Mode (1):

    Oil phase preparation: the nutrient compound oil is formulated according to a ratio of fatty acids, and then the fullerene compound is sterilized and dissolved in a nutrient compound oil to form a compound oil compound, and then the edible emulsifier is dissolved. Into the compound oil composite, an oil phase is obtained;

    Aqueous phase preparation: dissolving the wall material in hot water to obtain an aqueous phase; preferably, the temperature of the hot water is 60-80 ° C;

    Mixed sterilization: mixing the obtained aqueous phase with the oil phase, stirring uniformly, and then sterilizing;

    Homogenization, spray drying: homogenization, spray drying to obtain fullerene microcapsule powder;

    Mode (2):

    Dissolving the fullerene compound in the nutrient compounding oil to obtain a fullerene oil solution;

    Mixing, dissolving, dispersing, and homogenizing the fullerene oil solution, the wall material, the edible emulsifier, and the stabilizer and the glidant selectively contained, to form an emulsion, and homogenizing the obtained emulsion, and then The homogeneous emulsion is spray dried;

    Preferably, in the modes (1) and (2), the mixing is performed under shearing conditions, and the mixing conditions include a temperature of 50-80 ° C, a shear rate of 10000-15000 rpm, and a time of 2 10 min; the homogenous pressure is 30-35 MPa, the number of times is 2-5 times; the spray drying conditions include an inlet air temperature of 180-240 ° C, and an outlet air temperature of 75-85 ° C.
13. The fullerene microcapsule powder according to any one of claims 7 to 11 for use in the preparation of a beverage, a food, a cosmetic product, a hangover product, and a medicament for preventing and/or treating liver cancer, a neurodegenerative disease and a tumor Application in .

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