CN107823222B - Nano composite antibacterial agent and preparation method and application thereof - Google Patents

Nano composite antibacterial agent and preparation method and application thereof Download PDF

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CN107823222B
CN107823222B CN201711008670.8A CN201711008670A CN107823222B CN 107823222 B CN107823222 B CN 107823222B CN 201711008670 A CN201711008670 A CN 201711008670A CN 107823222 B CN107823222 B CN 107823222B
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nano
antibacterial agent
composite antibacterial
agent
nanocomposite
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CN107823222A (en
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韦勇
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Guizhou Prickly Pear Valley Health Industry Development Co ltd
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Guian New Area Ruicheng Bioengineering Co ltd
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Abstract

The invention provides a nano-composite antibacterial agent and a preparation method and application thereof, and relates to the technical field of antibacterial agents, wherein the nano-composite antibacterial agent mainly comprises raw materials such as nano-silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamins and the like, a liposome formed by the raw materials such as the protein, the phospholipid, the cholesterol and the like wraps functional substances such as the vitamins and the like, and the nano-silver, the graphene and the like are loaded in the liposome or on the surface after being compounded, so that the nano-composite antibacterial agent which is very similar to a cell structure is formed; the invention also provides a preparation method of the nano composite antibacterial agent, which can realize uniform mixing of all the raw materials, thereby being beneficial to improving the stability of the nano composite antibacterial agent.

Description

Nano composite antibacterial agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of antibacterial agents, and particularly relates to a nano composite antibacterial agent and a preparation method and application thereof.
Background
With the improvement of the living standard and health consciousness of people in China, the demand of antibacterial agents is greatly increased, and various antibacterial agents are continuously developed and applied. The antibacterial agent mainly comprises three major types of inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents. Although both organic antibacterial agents and natural antibacterial agents have a certain antibacterial ability, they have different problems. The organic antibacterial agent has poor heat resistance, is easy to hydrolyze, has short service life and low antibacterial effect, and may damage normal cells while killing pathogenic bacteria and viruses. The natural antibacterial agent is mainly limited by safety and processing conditions, and the large-scale market has certain problems. Compared with organic antibacterial agents and natural antibacterial agents, inorganic antibacterial agents have the characteristics of high temperature resistance, broad-spectrum antibacterial, safety, long-acting effect and the like, and have become important research points in the antibacterial field.
Among them, nano silver, as a novel inorganic antibacterial agent, has the characteristics of strong permeability, lasting antibacterial property, no drug resistance, safety and the like, and has been widely applied to the field of antibacterial products. The antibacterial principle of nano silver generally breaks through the cell wall and cell membrane barriers of bacteria, and an enzyme system in cytoplasm can be destroyed after the nano silver enters cytoplasm, so that the metabolism of the bacteria is interfered, or the nano silver enters nucleoplasm to destroy the DNA of the bacteria. Therefore, according to the antibacterial principle of nano silver, the nano silver needs to be matched with a carrier, passes through cell walls and cell membrane barriers of bacteria and plays an antibacterial role. The existing nano silver antibacterial agent formed by matching nano silver with a carrier generally has the problems of instability and further improvement of the antibacterial effect of an antibacterial material which is singly used.
In view of the above, the present invention is proposed to solve the above technical problems.
Disclosure of Invention
The first purpose of the invention is to provide a nano composite antibacterial agent, which is mainly prepared from base oil, nano silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamin, solubilizer, emulsifier, antioxidant, anti-polymerization agent, water and other raw materials, and the formed nano composite antibacterial agent has good antibacterial effect and stability through the synergistic cooperation of the raw materials.
The second purpose of the invention is to provide a preparation method of the nano composite antibacterial agent, the preparation method comprises the steps of mixing and homogenizing the raw materials, and then carrying out ultrahigh pressure micro-jet circulation treatment by adopting ultrahigh pressure micro-jet nano equipment to obtain the nano composite antibacterial agent, the preparation method is simple, the operation is easy, the whole production process is green and environment-friendly, and the nano composite antibacterial agent can be industrially produced in large batch. The nano composite antibacterial agent prepared by the method has uniform particles, high stability and good antibacterial effect.
The third purpose of the invention is to provide the application of the nano composite antibacterial agent.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a nano composite antibacterial agent, which is mainly prepared from the following raw materials: the nano silver anti-polymerization agent comprises base oil, nano silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamins, a solubilizer, an emulsifier, an antioxidant, an anti-polymerization agent and water.
Further, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 1-30% of base oil, 0.01-30% of nano-silver, 0.01-10% of graphene, 0.1-10% of protein, 1-15% of phospholipid, 0.1-10% of polysaccharide, 0.1-3% of cholesterol, 0.1-5% of vitamin, 1-30% of solubilizer, 1-10% of emulsifier, 0.1-1% of antioxidant, 0.5-10% of anti-polymerization agent and the balance of water to 100%.
Further, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 5-30% of base oil, 0.01-25% of nano-silver, 0.1-10% of graphene, 0.1-8% of protein, 1-12% of phospholipid, 0.1-8% of polysaccharide, 0.3-3% of cholesterol, 0.5-5% of vitamin, 1-25% of solubilizer, 1-8% of emulsifier, 0.2-1% of antioxidant, 1-10% of anti-polymerization agent and the balance of water to 100%;
preferably, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 6-30% of base oil, 0.01-20% of nano-silver, 0.1-9% of graphene, 1-8% of protein, 2-10% of phospholipid, 1-8% of polysaccharide, 0.5-2.5% of cholesterol, 0.6-5% of vitamin, 2-25% of solubilizer, 2-8% of emulsifier, 0.4-1% of antioxidant, 1-8% of anti-polymerization agent and the balance of water to 100%.
Further, the nano composite antibacterial agent also comprises an adsorbent with the mass fraction of 0.01-2%, wherein the adsorbent comprises one or the combination of at least two of carbon nano tubes, silicon dioxide or zeolite;
preferably, the nano composite antibacterial agent further comprises a sustained release agent with the mass fraction of 0.01-2%, wherein the sustained release agent is selected from one or the combination of at least two of carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, fat or wax substances.
Further, the nano composite antibacterial agent also comprises a magnetic component with the mass fraction of 0.01-10%;
preferably, the magnetic component is ferroferric oxide.
Further, the nano composite antibacterial agent also comprises titanium dioxide with the mass fraction of 0.01-10%;
and/or, the nano composite antibacterial agent also comprises zinc oxide with the mass fraction of 0.01-10%.
The invention also provides a preparation method of the nano composite antibacterial agent, which comprises the following steps:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol, vitamins, solubilizer, emulsifier, antioxidant, anti-polymerization agent and part of water, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment to obtain liposome mixture;
(b) mixing nano silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment to obtain nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Further, in the step (a), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3 times;
preferably, the particle size of the liposome mixture is 1-20 nm.
Further, in the step (b), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3 times;
preferably, the nanoparticles in the nanoparticle solution have a particle size of 1 to 100 nm.
The invention also provides application of the nano composite antibacterial agent in daily necessities or medical products.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a nano composite antibacterial agent, which mainly comprises base oil, nano silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamin, solubilizer, emulsifier, antioxidant, anti-polymerization agent, water and other raw materials, wherein a liposome formed by the raw materials of the protein, the phospholipid, the cholesterol and the like wraps functional substances such as the vitamin, and the nano silver, the graphene and the like are loaded in or on the liposome after being compounded, so that the nano composite antibacterial agent which is very similar to a cell structure is formed, the composite antibacterial agent has high speed of entering microbial cells and can be aggregated around focuses to form a high-concentration drug effect, and the nano composite antibacterial agent can selectively adsorb, wrap, shield and kill pathogenic bacteria and viruses with negative charges on the surfaces due to positive charges on the surfaces of the nano composite antibacterial agent, has a strong antibacterial effect, and improves the common instability of the existing nano silver antibacterial agent formed by matching the nano silver and the carrier, and the antibacterial efficacy of the nano-silver antibacterial material is to be further improved.
(2) The invention provides a preparation method of a nano composite antibacterial agent, which is simple to operate, green and environment-friendly in production process and capable of realizing industrial mass production.
(3) The invention provides an application of a nano composite antibacterial agent, and the nano composite antibacterial agent can be widely applied to daily necessities or medical products in view of the advantages of the nano composite antibacterial agent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a human acne test wherein (a) is prior to the use of the nanocomposite antimicrobial of example 2; (b) 48 hours after the application of the nanocomposite antimicrobial of example 2;
FIG. 2 is a test of bacterial infection due to inflammation of hair follicles in human buttocks, wherein (a) is before the nanocomposite antibacterial agent of example 2 is used (pus discharge cleaning treatment is performed); (b) 48 hours after the application of the nanocomposite antimicrobial of example 2;
FIG. 3 is a human foot fungal infection test in which (a) is prior to use of the example 4 nanocomposite antimicrobial (3 years old); (b) 15 days after the application of the example 4 nanocomposite antimicrobial (daily continuous use);
FIG. 4 is a test of fungal infection in human hands, wherein (a) is prior to use of the nanocomposite antimicrobial of example 6 (with a 7 year history); (b) 20 days after the application of the nanocomposite antibacterial agent of example 6 (continuous use per day);
FIG. 5 is the psoriasis test 1 in humans, wherein (a) is prior to the use of the nanocomposite antimicrobial of example 8; (b) for 21 days after the application of the example 8 nanocomposite antibacterial agent (daily continuous use);
FIG. 6 is the psoriasis test 2 in humans, wherein (a) is prior to the use of the nanocomposite antimicrobial of example 1; (b) for 14 days (continuous use per day) after the use of the nanocomposite antibacterial agent of example 1.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
According to one aspect of the present invention, there is provided a nanocomposite antibacterial agent which is mainly prepared from the following raw materials: the nano silver anti-polymerization agent comprises base oil, nano silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamins, a solubilizer, an emulsifier, an antioxidant, an anti-polymerization agent and water.
The invention provides a nano composite antibacterial agent, which mainly comprises base oil, nano silver, graphene, protein, phospholipid, polysaccharide, cholesterol, vitamin, solubilizer, emulsifier, antioxidant, anti-polymerization agent, water and other raw materials, wherein a liposome formed by the raw materials of the protein, the phospholipid, the cholesterol and the like wraps functional substances such as the vitamin, and the nano silver, the graphene and the like are loaded in or on the liposome after being compounded, so that the nano composite antibacterial agent which is very similar to a cell structure is formed, the composite antibacterial agent has high speed of entering microbial cells and can be aggregated around focuses to form a high-concentration drug effect, and the nano composite antibacterial agent can selectively adsorb, wrap, shield and kill pathogenic bacteria and viruses with negative charges on the surfaces due to positive charges on the surfaces of the nano composite antibacterial agent, has a strong antibacterial effect, and improves the common instability of the existing nano silver antibacterial agent formed by matching the nano silver and the carrier, and the antibacterial efficacy of the nano-silver antibacterial material is to be further improved.
As a preferred embodiment of the invention, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 1-30% of base oil, 0.01-30% of nano-silver, 0.01-10% of graphene, 1-15% of phospholipid, 0.1-3% of cholesterol, 0.1-10% of polysaccharide, 0.1-10% of protein, 0.1-5% of vitamin, 1-30% of solubilizer, 1-10% of emulsifier, 0.1-1% of antioxidant, 0.5-10% of anti-polymerization agent and the balance of water to 100%.
In particular, the base oil belongs to lipid, and mainly acts to form emulsion, thereby being beneficial to keeping the stability of the system and being beneficial to intercellular fusion. The base oil is typically, but not limited to, selected from one or a combination of at least two of evening primrose oil, grape seed oil, jojoba oil, olive oil, wheat germ oil, almond oil, shea butter, peanut oil, avocado oil, rose hip oil, nut oil, safflower oil, sesame oil, soybean oil, rice bran oil, sunflower oil, castor oil, coconut oil, calendula oil, snake oil, ostrich oil or lanolin, preferably evening primrose oil.
Typical but non-limiting mass fractions of base oils are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 25%, 28% or 30%.
The nano silver is used as the main antibacterial component of the nano composite antibacterial agent and has the characteristics of strong permeability, lasting antibacterial property, no drug resistance, safety and the like.
The typical but non-limiting mass fraction of nanosilver is 0.01%, 0.05%, 0.1%, 0.25%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 25%, 28%, or 30%.
In the invention, the nano silver and the graphene are used in a composite way, so that the antibacterial effect is more obvious. Typical but not limiting mass fractions of graphene are 0.01%, 0.05%, 0.1%, 0.25%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
The phospholipid and the cholesterol jointly form the liposome, and the formed liposome has a structure similar to that of a biological cell, so that the liposome has good biocompatibility and can be fused with a human cell membrane, so that the nano silver, the graphene and nutrient components loaded by the liposome are delivered into the cell, the capability of breaking through the barrier of the human cell by antibacterial components is improved, the slow release stability of the nano silver and the graphene is improved, and the aim of effectively and durably resisting bacteria is fulfilled; and meanwhile, the nutrient substances wrapped by the liposome are transferred to cells to supplement cell energy, promote the growth of the cells and improve the self-repairing capability of the cells. In addition, the liposome can also prevent the nano silver from being oxidized, thereby improving the stability of the nano composite antibacterial agent.
Typical but not limiting mass fractions of phospholipids are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14% or 15%.
Typical but not limiting mass fractions of cholesterol are 0.1%, 0.5%, 1%, 2% or 3%.
The protein and polysaccharide can be used as nutrient substance, and coated or loaded on liposome. Typical but not limiting mass fractions of protein are 0.1%, 0.25%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%. Typical but not limiting mass fractions of polysaccharides are 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
Vitamins as nutrient substances of the nano composite antibacterial agent include but are not limited to one or more of vitamin A, vitamin B, vitamin C, vitamin D, vitamin E, vitamin K and derivatives, preferably vitamin E. Typical but not limiting mass fractions of vitamins are 0.1%, 0.5%, 1%, 2%, 3%, 4% or 5%. The liposome-encapsulated nutrient substances are transferred to cells while resisting bacteria, so that the cell energy is supplemented, the growth of the cells is promoted, and the self-repairing capability of the cells is improved.
The nanocomposite antimicrobial is a suspension that tends to aggregate, fuse, and potentially leak the entrapped drug during storage. In order to improve the stability, a solubilizer, an emulsifier, an antioxidant, an anti-polymerization agent and the like are required to be added.
The solubilizer is selected from one of ethanol, propylene glycol, 1-2 butanediol and 1-3 butanediol, preferably propylene glycol. Typical but non-limiting mass fractions of solubilizers are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 25%, 28% or 30%.
The emulsifier is selected from one or more of methyl glucoside sesquistearate, EG sodium polyacrylate copolymer, steareth, glyceryl stearate/PEG-100 stearate, cetearyl ether, sorbitan sesquioleate, monoglyceride, span 60, span 80, Tween 60, Tween 80, triglycerol diisostearate, peregal and quaternary ammonium salt ethanol, and is preferably one or more of glyceryl stearate, stearate copolymer or monoglyceride. Typical but not limiting mass fractions of emulsifiers are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
The antioxidant is selected from one or more of Butylated Hydroxyanisole (BHA), dibutyl hydroxy toluene (BHT), Propyl Gallate (PG) and tert-butyl hydroquinone (TBHQ), preferably dibutyl hydroxy toluene. Antioxidants are typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 0.10% by mass.
The anti-polymerization agent is selected from one or a combination of at least two of alkyl glucoside, hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, coconut oil fatty acid diethanol amine, dodecanoic acid, tetradecanoic acid, hexadecanoic acid, EDTA disodium salt, sodium lauroyl sarcosine, potassium lauryl alcohol ether phosphate, potassium monoalkyl ether ester, sodium cocoyl hydroxyethyl sulfonate or sodium cocoyl hydroxyethyl sulfonate, and preferably alkyl glucoside. Typical but non-limiting mass fractions of the anti-polymerization agent are 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
As a preferred embodiment of the invention, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 5-30% of base oil, 0.01-25% of nano-silver, 0.1-10% of graphene, 0.1-8% of protein, 1-12% of phospholipid, 0.1-8% of polysaccharide, 0.3-3% of cholesterol, 0.5-5% of vitamin, 1-25% of solubilizer, 1-8% of emulsifier, 0.2-1% of antioxidant, 1-10% of anti-polymerization agent and the balance of water to 100%;
preferably, the nano composite antibacterial agent is mainly prepared from the following raw materials in percentage by mass: 6-30% of base oil, 0.01-20% of nano-silver, 0.1-9% of graphene, 1-8% of protein, 2-10% of phospholipid, 1-8% of polysaccharide, 0.5-2.5% of cholesterol, 0.6-5% of vitamin, 2-25% of solubilizer, 2-8% of emulsifier, 0.4-1% of antioxidant, 1-8% of anti-polymerization agent and the balance of water to 100%.
The physical and chemical stability of the nano composite antibacterial agent relates to a plurality of factors, and all the factors are mutually restricted, so that the selection of the specific raw material composition and the proportion of the contents of the raw materials needs to control the plurality of factors to prepare the stable and effective nano composite antibacterial agent. By further optimizing the raw material composition of the nano composite antibacterial agent, the stronger the synergistic cooperation effect among the raw material compositions is, the better the stability is, the stronger the ability of penetrating cell membranes is, and the more remarkable the antibacterial ability is.
The phrase "made mainly of … …" as used herein means that it may include, in addition to the components, other components such as thickeners and the like which impart different properties to the nanocomposite antimicrobial agent. In addition, the invention described as "made primarily of … …" may be replaced with a closed "being" or "made of … …".
As a preferred embodiment of the present invention, the nanocomposite antibacterial agent further comprises a thickener in a mass fraction of 0.5 to 3%. The thickening agent can be used to adjust the consistency to meet the actual requirement. In the present invention, the thickener is selected from one or a combination of at least two of polyethylene glycol, carbomer, acrylic acid polymer, methyl glucoside polyoxyethylene, carbomer, polyvinylpyrrolidone, polyvinyl alcohol, alkyl polyammonium salt polymer, xanthan gum or sodium alginate, and is preferably xanthan gum or polyethylene glycol. Typical but not limiting mass fractions of thickeners are 0.5%, 1%, 1.5%, 2%, 2.5% or 3%.
As a preferred embodiment of the present invention, the nanocomposite antibacterial agent further comprises 0.01 to 2% by mass of an adsorbent. The adsorbent is added into the nano-composite antibacterial agent, so that pathogenic bacteria and viruses can be effectively adsorbed around the nano-composite antibacterial agent, and then the aim of killing the pathogenic bacteria and the viruses is fulfilled by utilizing the antibacterial components of the nano-composite antibacterial agent.
Typical but not limiting mass fractions of the adsorbent are 0.01%, 0.05%, 0.1%, 0.2%, 0.4%, 0.6%, 0.8%, 0.10%, 0.12%, 0.14%, 0.16%, 0.18% or 0.20%. The adsorbent comprises one or a combination of at least two of carbon nanotubes, silica or zeolite.
As a preferred embodiment of the present invention, the nanocomposite antibacterial agent further comprises a sustained-release agent in a mass fraction of 0.01 to 2%. The slow release agent can further ensure that the slow release effect of the nano composite antibacterial agent in cells is more durable.
Typical but not limiting mass fractions of the sustained release agent are 0.01%, 0.05%, 0.1%, 0.2%, 0.4%, 0.6%, 0.8%, 0.10%, 0.12%, 0.14%, 0.16%, 0.18% or 0.20%. The slow release agent is selected from one or the combination of at least two of carboxymethyl cellulose, hydroxypropyl methyl cellulose or polyvinylpyrrolidone.
As a preferred embodiment of the present invention, the nanocomposite antibacterial agent further comprises a magnetic component in a mass fraction of 0.01 to 10%. The nano composite antibacterial agent is added with magnetic components, and a high-concentration drug effect is formed at a pathological part under the guidance of an external magnetic field.
Typical but non-limiting mass figures for the magnetic component are 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%. The magnetic component can be selected from magnetic materials which have magnetism and are harmless to human bodies. Preferably, the magnetic component is ferroferric oxide.
In order to further improve the antibacterial ability of the nano composite antibacterial agent, as a preferred embodiment of the invention, the nano composite antibacterial agent further comprises 0.01-10% by mass of titanium dioxide;
and/or, the nano composite antibacterial agent also comprises zinc oxide with the mass fraction of 0.01-10%.
The titanium dioxide and the zinc oxide both have certain antibacterial capacity, and are added into the nano composite antibacterial agent to be matched with the nano silver and the graphene together, so that the antibacterial agent with stronger antibacterial capacity is formed.
Typical but non-limiting mass figures for titanium dioxide are 0.01%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%. Typical but non-limiting mass figures for zinc oxide are 0.01%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
The nano composite antibacterial agent provided by the invention can self-identify, adsorb, shield and kill pathogenic bacteria with negative electricity, reject normal cells with positive electricity and maintain the ecological balance among cells to the maximum extent.
According to another aspect of the present invention, there is also provided a method for preparing a nanocomposite antibacterial agent, comprising the steps of:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol, vitamins, solubilizer, emulsifier, antioxidant, anti-polymerization agent and part of water, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment to obtain liposome mixture;
(b) mixing and homogenizing nano silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water according to the formula amount, and performing ultrahigh pressure micro-jet circulation treatment to prepare a nano particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
The preparation method of the nano composite antibacterial agent provided by the invention has the advantages of simple process, convenience in operation, green and environment-friendly whole production process and capability of industrial mass production. And the method can realize the uniform mixing of the raw materials, thereby being beneficial to the improvement of the stability of the prepared nano composite antibacterial agent.
Further, in the step (a), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3 times;
preferably, the particle size of the liposome mixture is 1-20 nm.
In order to further refine the grain diameter of the nano composite antibacterial agent, the raw material mixture is treated by adopting ultrahigh pressure micro-jet equipment. In the ultrahigh pressure micro-jet circulation treatment process, the circulation frequency is not too high, otherwise the phospholipid structure is damaged, and the medicine leakage is caused. The selection of the treatment pressure has great influence on the particle size and the shape of the final nano composite antibacterial agent, the treatment pressure is not too low, if the treatment pressure is too low, the particle size of the liposome mixture is larger, and larger aggregates exist; the treatment pressure should not be too high, otherwise the encapsulation efficiency of the liposome mixture against the antibacterial component is affected.
In the present invention, in step (a), the temperature of mixing is 50 ℃, 55 ℃, 60 ℃, 65 ℃, or 70 ℃. Typical but non-limiting processing pressures for the ultra-high pressure micro-jet cycle are 180MPa, 190MPa, 200MPa, 205MPa, 210MPa, 220MPa, 225MPa, 230MPa, 235MPa, 240MPa, 245MPa or 250 MPa. The number of cycles was 1, 2 or 3.
The particle size of the liposome mixture is 1nm, 5nm, 8nm, 10nm, 12nm, 15nm, 18nm or 20 nm.
Further, in the step (b), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3 times;
preferably, the nanoparticles in the nanoparticle solution have a particle size of 1 to 100 nm.
In the present invention, in the step (b), the temperature of mixing is 50 ℃, 55 ℃, 60 ℃, 65 ℃, or 70 ℃. Typical but non-limiting processing pressures for the ultra-high pressure micro-jet cycle are 180MPa, 190MPa, 200MPa, 205MPa, 210MPa, 220MPa, 225MPa, 230MPa, 235MPa, 240MPa, 245MPa or 250 MPa. The number of cycles was 1, 2 or 3.
The particle size of the nanoparticles in the nanoparticle solution is 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm or 100 nm.
Through the research on various parameters involved in the preparation method and the specific matching relationship among the parameters, the parameters are determined, and the prepared nano composite antibacterial agent has good quality and efficacy.
According to a third aspect of the present invention, there is also provided a use of a nanocomposite antibacterial agent in a daily use article or a medical product.
The nano-composite antibacterial agent is formed by compounding nano-silver, graphene and other components, has lasting and long-term antibacterial effect, and can be prepared into a proper dosage form to be applied to the field of daily necessities or medicines.
The nano composite antibacterial agent has stable chemical properties, can be applied to the field of daily necessities, such as antibacterial and anti-inflammatory masks, emulsions, essences, face creams, foundations, disinfectants, hand sanitizers, foot lotions, face lotions, disinfectant soaps, laundry detergents, washing liquids, shampoos, shower gels, toothpaste, mouthwash, wet tissues, sanitary towels and the like, or can also be applied to the field of food preservatives and the like.
The nano-composite antibacterial agent has obvious curative effects on skin diseases such as acne, scabies, acne rosacea, eczema, burns, scalds, vaginal fungal infection and the like caused by infection of bacteria, fungi, spores, scabies and the like, so the nano-composite antibacterial agent can also be applied to the medical and sanitary fields such as medical antibacterial and anti-inflammatory ointment, medicinal powder, sterilizing and antibacterial dressing, instrument sterilization and the like; or applied to the field of medical inspection and quarantine, such as radioactive markers, targeted drug therapy and the like.
The present invention will be further described with reference to specific examples and comparative examples.
Example 1
The nano composite antibacterial agent provided by the embodiment is prepared from the following raw materials in percentage by mass: 1% of evening primrose oil, 0.01% of nano-silver, 0.1% of graphene, 0.1% of protein, 1% of phospholipid, 0.2% of chitosan, 2% of cholesterol, 0.2% of vitamin E, 2% of ethanol, 0.5% of monoglyceride, 0.2% of butylated hydroxytoluene, 1% of alkyl glucoside and the balance of water to 100%.
Example 2
The nano composite antibacterial agent provided by the embodiment is prepared from the following raw materials in percentage by mass: 11% of grape seed oil, 0.05% of nano-silver, 1% of graphene, 0.3% of protein, 3% of phospholipid, 0.3% of chitosan, 1% of cholesterol, 0.5% of vitamin C, 0.5% of vitamin E, 4% of propylene glycol, 1% of glyceryl stearate/PEG-100 stearate, 0.4% of tert-butyl hydroquinone, 0.8% of alkyl glucoside, 0.2% of sodium cocoyl isethionate, 0.5% of xanthan gum, 0.3% of polyethylene glycol, 0.2% of silicon dioxide and the balance of water to 100%.
Example 3
The nano composite antibacterial agent provided by the embodiment is prepared from the following raw materials in percentage by mass: 12% of evening primrose oil, 5% of nano-silver, 6% of graphene, 10% of protein, 7% of phospholipid, 10% of chitosan, 1% of cholesterol, 5% of vitamin C, 25% of ethanol, 8% of monoglyceride, 0.5% of dibutyl hydroxy toluene, 0.5% of alkyl glucoside, 0.2% of silicon dioxide and the balance of water to 100%.
Example 4
The nano composite antibacterial agent provided by the embodiment is prepared from the following raw materials in percentage by mass: 20% of evening primrose oil, 10% of nano-silver, 10% of graphene, 8% of protein, 12% of phospholipid, 1% of chitosan, 2% of cholesterol, 1% of vitamin E, 5% of ethanol, 2% of monoglyceride, 0.6% of dibutyl hydroxy toluene, 2% of alkyl glucoside and the balance of water to 100%.
Example 5
In this example, 0.2% by mass of silica and 1.5% by mass of a sustained-release agent were added to example 4, and the remaining raw materials and the amounts used were the same as in example 4.
Example 6
In this example, a nanocomposite antibacterial agent was prepared by adding 1% by mass of titanium dioxide and 2% by mass of zinc oxide to example 5, and the remaining raw materials and the amounts used were the same as in example 5.
Example 7
In the nano composite antibacterial agent provided by the embodiment, the ferroferric oxide with the mass fraction of 8% is added on the basis of the embodiment 6, and the rest raw materials and the using amount are the same as those in the embodiment 6.
Example 8
The nano composite antibacterial agent provided by the embodiment is prepared from the following raw materials in percentage by mass: 30% of evening primrose oil, 25% of nano-silver, 2% of graphene, 6% of protein, 15% of phospholipid, 5% of chitosan, 3% of cholesterol, 1% of vitamin B, 2% of vitamin E, 3% of ethanol, 1% of monoglyceride, 601% of tween, 0.8% of butylated hydroxyanisole, 1% of alkyl glucoside and the balance of water to 100%.
Example 9
The preparation method of the nano composite antibacterial agent provided by the embodiment 1 comprises the following steps:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol and vitamins in formula amount, and respectively 1/2 solubilizer, emulsifier, antioxidant, anti-polymerization agent and water in formula amount, homogenizing at 55 deg.C, and performing ultrahigh pressure micro-jet circulation treatment under 200MPa for 2 times to obtain liposome mixture;
(b) mixing nano-silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water at 60 ℃, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment at 200MPa for 1 time to obtain a nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Example 10
The preparation method of the nano composite antibacterial agent provided by the embodiment 2 comprises the following steps:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol and vitamins in formula amount, and respectively 1/2 solubilizer, emulsifier, antioxidant, anti-polymerization agent and water in formula amount, homogenizing at 65 deg.C, and performing ultrahigh pressure micro-jet circulation treatment under 220MPa for 2 times to obtain liposome mixture;
(b) mixing nano-silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water at 65 ℃, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment at 220MPa for 2 times to obtain a nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Example 11
The preparation method of the nanocomposite antibacterial agent provided in example 3 includes the following steps:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol and vitamins in formula amount, and respectively 2/3 solubilizer, emulsifier, antioxidant, anti-polymerization agent and water in formula amount, homogenizing at 70 deg.C, and performing ultrahigh pressure micro-jet circulation treatment under 250MPa for 2 times to obtain liposome mixture;
(b) mixing nano-silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water at 50 ℃, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment at 250MPa for 1 time to obtain a nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Example 12
Examples 4-7 provide methods of preparing nanocomposite antimicrobial agents comprising the steps of:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol and vitamins in formula amount, and respectively 1/2 solubilizer, emulsifier, antioxidant, anti-polymerization agent and water in formula amount, homogenizing at 50 deg.C, and performing ultrahigh pressure micro-jet circulation treatment under 200MPa for 2 times to obtain liposome mixture;
(b) mixing nano-silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water at 70 ℃, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment at 250MPa for 3 times to obtain nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Example 13
The method of preparing a nanocomposite antimicrobial agent provided in example 8, comprising the steps of:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol and vitamins in formula amount, and respectively 1/2 solubilizer, emulsifier, antioxidant, anti-polymerization agent and water in formula amount, homogenizing at 50 deg.C, and performing ultrahigh pressure micro-jet circulation treatment under 180MPa for 3 times to obtain liposome mixture;
(b) mixing nano-silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water at 60 ℃, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment at 180MPa for 3 times to obtain nano-particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
Comparative example 1
This comparative example provides a nanocomposite antimicrobial agent, the raw materials and amounts and preparation method of which were the same as example 4, except that graphene was not added to the raw materials of example 4.
Comparative example 2
This comparative example provides a nanocomposite antimicrobial agent, the raw materials and amounts and preparation method were the same as in example 4, except that the antioxidant and the anti-polymerization agent were not added to the raw materials of example 4.
To verify the technical effects of the examples and comparative examples, the following experimental examples were specified.
Experimental example 1
Culture plates, the surfaces of which were uniformly coated with escherichia coli (8099), staphylococcus aureus (ATCC 6538), and candida albicans (ATCC 10331), were weighed, respectively, and test paper sheets carrying the nanocomposite antibacterial agents of the respective examples and comparative examples at the same concentration were gently placed on the middle positions of the bacterial culture plates. Then, the culture plate is placed in an incubator at 37 ℃, cultured for 48 hours and taken out to observe the size of the inhibition zone. The larger the inhibition zone is, the better the antibacterial effect is, and the specific detection results are shown in table 1.
TABLE 1 results of bacteriostatic tests of examples and comparative examples
Figure BDA0001444953540000171
Figure BDA0001444953540000181
As can be seen from Table 1, the nanocomposite antibacterial agent provided by the embodiments of the present invention has good antibacterial effects on Escherichia coli, Staphylococcus aureus and Candida albicans.
Examples 5 to 7 and comparative examples 1 to 2 were the control experiments of example 4. Compared with example 4, in example 5, the adsorbent and the sustained-release agent are added to the raw material of example 4, in example 6, the adsorbent, the sustained-release agent, titanium dioxide and zinc oxide are added to the raw material of example 4, and in example 6, the adsorbent, the sustained-release agent and the magnetic component are added to the raw material of example 4. As can be seen from the data in Table 1, the adsorbent, the sustained-release agent, the titanium dioxide, the zinc oxide and the magnetic component have certain improvement effect on the antibacterial performance of the nano composite antibacterial agent.
Comparative example 1 no graphene was added to the starting material of example 4. As can be seen from the data in the table, the antibacterial effect of comparative example 1 is much lower than that of example 4. This shows that the antibacterial effect of the graphene and nano-silver composite material can be significantly improved. Comparative example 2 no antioxidant and no anti-polymerization agent were added based on the raw material of example 4. The lack of antioxidant and anti-polymerization agent is not favorable for improving the stability of the nano composite antibacterial agent, thereby being not favorable for exerting the antibacterial effect.
Experimental example 2
In order to further verify the antibacterial effect of the nano-composite antibacterial agent provided by the invention, the nano-composite antibacterial agent is prepared into a medicament form and is smeared on the affected part, and the affected part is compared with the affected part before the nano-composite antibacterial agent is used, as shown in fig. 1-6.
As is apparent from fig. 1 to 6, the nano-composite antibacterial agent has a certain effect on alleviating facial acne, folliculitis, foot or hand fungal infection, psoriasis and the like of a human body, which shows that the nano-composite antibacterial agent provided by the invention has a good antibacterial effect.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (14)

1. The nano composite antibacterial agent is characterized by being mainly prepared from the following raw materials in percentage by mass: 1-30% of base oil, 0.01-30% of nano-silver, 0.01-10% of graphene, 0.1-10% of protein, 1-15% of phospholipid, 0.1-10% of polysaccharide, 0.1-3% of cholesterol, 0.1-5% of vitamin, 1-30% of solubilizer, 1-10% of emulsifier, 0.1-1% of antioxidant, 0.5-10% of anti-polymerization agent and the balance of water to 100%.
2. The nanocomposite antibacterial agent according to claim 1, characterized by being mainly prepared from the following raw materials in mass fraction: 5-30% of base oil, 0.01-25% of nano-silver, 0.1-10% of graphene, 0.1-8% of protein, 1-12% of phospholipid, 0.1-8% of polysaccharide, 0.3-3% of cholesterol, 0.5-5% of vitamin, 1-25% of solubilizer, 1-8% of emulsifier, 0.2-1% of antioxidant, 1-10% of anti-polymerization agent and the balance of water to 100%.
3. The nanocomposite antibacterial agent according to claim 1, characterized by being mainly prepared from the following raw materials in mass fraction: 6-30% of base oil, 0.01-20% of nano-silver, 0.1-9% of graphene, 1-8% of protein, 2-10% of phospholipid, 1-8% of polysaccharide, 0.5-2.5% of cholesterol, 0.6-5% of vitamin, 2-25% of solubilizer, 2-8% of emulsifier, 0.4-1% of antioxidant, 1-8% of anti-polymerization agent and the balance of water to 100%.
4. The nanocomposite antimicrobial agent according to any one of claims 1 to 3, further comprising 0.01 to 2 mass% of an adsorbent comprising one or a combination of at least two of carbon nanotubes, silica or zeolite.
5. The nanocomposite antibacterial agent according to any one of claims 1 to 3, further comprising a sustained release agent selected from one or a combination of at least two of carboxymethyl cellulose, hydroxypropyl methyl cellulose or polyvinylpyrrolidone in a mass fraction of 0.01 to 2%.
6. The nanocomposite antibacterial agent according to any one of claims 1 to 3, further comprising a magnetic component in a mass fraction of 0.01 to 10%.
7. The nanocomposite antimicrobial agent of claim 6, wherein the magnetic component is ferroferric oxide.
8. The nanocomposite antibacterial agent according to any one of claims 1 to 3, further comprising 0.01 to 10 mass% of titanium dioxide;
and/or, the nano composite antibacterial agent also comprises zinc oxide with the mass fraction of 0.01-10%.
9. A method for preparing a nanocomposite antibacterial agent according to any one of claims 1 to 8, characterized by comprising the steps of:
(a) mixing base oil, protein, phospholipid, polysaccharide, cholesterol, vitamins, solubilizer, emulsifier, antioxidant, anti-polymerization agent and part of water, homogenizing, and performing ultrahigh pressure micro-jet circulation treatment to obtain liposome mixture;
(b) mixing and homogenizing nano silver and graphene, optional adsorbent, slow release agent, magnetic component, titanium dioxide and zinc oxide, and residual solubilizer, emulsifier, antioxidant, anti-polymerization agent and water according to the formula amount, and performing ultrahigh pressure micro-jet circulation treatment to prepare a nano particle solution;
(c) and (b) mixing the liposome mixture obtained in the step (a) and the nano-particle solution obtained in the step (b), and performing ultrahigh pressure micro-jet circulation treatment to obtain the nano-composite antibacterial agent.
10. The method for preparing a nano-composite antibacterial agent according to claim 9, wherein in the step (a), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3.
11. The method of claim 9, wherein the liposome mixture has a particle size of 1-20 nm.
12. The method for preparing a nano-composite antibacterial agent according to claim 9, wherein in the step (b), the mixing temperature is 50-70 ℃, the pressure of the ultrahigh pressure micro-jet circulation treatment is 180-250MPa, and the circulation treatment times are 1-3.
13. The method of claim 9, wherein the nanoparticles in the nanoparticle solution have a particle size of 1 to 100 nm.
14. Use of the nanocomposite antibacterial agent of any one of claims 1 to 8 in daily necessities or in the preparation of medical products.
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