CN112274462B - Composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects and preparation and application thereof - Google Patents

Abstract

The invention discloses a composite bacteriostatic agent with bacteriostatic and epidermis moisturizing effects, and a preparation method and an application thereof.

Description

Composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects and preparation and application thereof

Technical Field

The invention relates to the field of cosmetics, in particular to a composite bacteriostatic agent with bacteriostatic and epidermis moisturizing effects and preparation and application thereof.

Background

Along with the development of economy and the improvement of living standard of people, the frequency of using cosmetics is higher and higher, and the requirements of people on the safety and the quality of the cosmetics are higher and higher. Good bacteriostats are not only required to prevent and inhibit the growth of microorganisms such as bacteria and fungi, but also must be safe, mild, non-toxic and non-irritating to the human body, non-reactive with other chemical components of the formulation, and provide the desired bacteriostatic function during storage and use of the cosmetic.

Traditionally, the bacteriostatic agent used in cosmetics adopts one or more of 51 preservatives allowed by cosmetic rules, and is compounded to solve the problem of microbial growth of the cosmetics. Because traditional antiseptic itself is the restricted use material, solve cosmetics microorganism growth with a certain antiseptic alone, be difficult to guarantee the effect, and need improve the quantity, improve the quantity and can bring the product security problem. Therefore, there is a tendency that the use of conventional preservatives in cosmetics is less and less.

In view of the above, those skilled in the art have endeavored to develop new safe, mild, non-irritating bacteriostatic products.

Disclosure of Invention

The invention aims to provide a composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects, and preparation and application thereof.

In a first aspect of the invention, a composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects is provided, and comprises nano silver, a plant extract and a plant polysaccharide extract.

Preferably, the composite bacteriostatic agent comprises the following components in parts by weight:

0.0001 to 1 portion of nano silver

0.01-20 parts of plant extract; and

0.01-20 parts of plant polysaccharide extract.

Preferably, the composite bacteriostatic agent comprises the following components in parts by weight:

0.01 to 0.2 portion of nano silver

0.1-20 parts of plant extract; and

1-20 parts of plant polysaccharide extract.

Preferably, the plant extract is selected from one or more of the following group: neem extract, artemisia argyi plant extract, and rosemary plant extract.

Preferably, the plant polysaccharide extract is selected from one or more of the group consisting of: polysaccharide extract of Orchidaceae plant, and Tremella polysaccharide extract.

Preferably, the orchid family plant comprises one or more of cymbidium, cymbidium and cymbidium.

Preferably, the composite bacteriostatic agent further comprises saponin and/or glycyrrhetinic acid.

Preferably, the composite bacteriostatic agent comprises the following components in parts by weight:

in a second aspect of the invention, there is provided the use of the composite bacteriostatic agent of the first aspect of the invention in the preparation of a cosmetic.

Preferably, the cosmetics comprise skin-care lotion, skin-care emulsion, hand sanitizer and shower gel.

In a third aspect of the invention, a cosmetic is provided, which comprises the composite bacteriostatic agent of the first aspect of the invention.

Preferably, the cosmetics comprise skin-care lotion, skin-care emulsion, hand sanitizer and shower gel.

The fourth aspect of the invention provides a preparation method of a composite bacteriostatic agent, which comprises the following steps:

(1) Mixing the raw materials of the composite bacteriostatic agent, and stirring the mixture at 40-80 ℃ to form a uniform mixture;

(2) Adjusting the pH value of the mixture to 5.0-8.0;

(3) Filtering the mixture, and cooling to room temperature to obtain the composite bacteriostatic agent;

wherein, the raw materials of the composite bacteriostatic agent comprise nano silver, plant extracts and plant polysaccharide extracts.

Preferably, the raw materials of the composite bacteriostatic agent comprise the following components in parts by weight:

0.0001 to 1 portion of nano silver

0.01-20 parts of plant extract; and

0.01-20 parts of plant polysaccharide extract.

Preferably, the raw materials of the composite bacteriostatic agent comprise the following components in parts by weight:

0.01 to 0.2 portion of nano-silver

0.1-20 parts of plant extract; and

1-20 parts of plant polysaccharide extract.

Preferably, the plant extract is neem tree extract.

Preferably, the plant polysaccharide extract is an orchid polysaccharide extract.

Preferably, the orchidaceae plant is gymnadenia conopsea.

Preferably, the raw materials of the composite bacteriostatic agent also comprise saponin and/or glycyrrhetinic acid.

Preferably, the raw materials of the composite bacteriostatic agent comprise the following components in parts by weight:

it is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.

Drawings

FIG. 1 is a diagram of a finished product prepared in example 1 of the present invention;

FIG. 2 is a schematic view of the antibacterial test method in example 2 of the present invention.

Detailed Description

The inventor obtains a composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects through extensive and intensive research, wherein the composite bacteriostatic agent comprises nano silver, a plant extract and a plant polysaccharide extract, can effectively inhibit the growth of microorganisms in cosmetics, has an excellent skin epidermal moisturizing effect, and has the characteristics of safety, mildness and no irritation.

Before the present invention is described, it is to be understood that this invention is not limited to the particular methodology and experimental conditions described, as such methods and conditions may vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting, since the scope of the present invention will be limited only by the appended claims.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. As used herein, the term "about" when used in reference to a specifically recited value means that the value may vary by no more than 1% from the recited value. For example, as used herein, the expression "about 100" includes 99 and 101 and all values in between (e.g., 99.1, 99.2, 99.3, 99.4, etc.).

Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are now exemplified.

In a preferred embodiment of the invention, the invention provides a composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects, which consists of nano-silver, a plant extract and a plant polysaccharide extract.

In a preferred embodiment, the composite bacteriostatic agent comprises the following components in parts by weight:

about 0.001 to 1 portion of nano silver

About 0.01-20 parts of plant extract; and

about 0.01-20 parts of plant polysaccharide extract.

In a preferred embodiment, the composite bacteriostatic agent comprises the following components in parts by weight:

as described in the present invention, the term "Nano Silver" (Nano Silver) is a metallic Silver simple substance with a Nano-scale particle size, and is a novel inorganic antibacterial material having stable physical, chemical and biological properties and an antibacterial effect which is not comparable to that of the conventional inorganic antibacterial material. The nano silver has high safety and lasting effect, and is a long-acting antibacterial agent. The inventor finds that if the skin care product containing nano silver is applied on the skin, the bacteriostatic effect of the nano silver is obviously reduced along with the evaporation of water. After the plant polysaccharide extract with the strong water locking function is added, the bacteriostatic effect of the nano-silver can be remarkably improved.

As used herein, the term "plant extract" refers to a substance extracted or processed from a plant (whole or a part of a plant) using a suitable solvent or method, and can be used in the pharmaceutical industry, food industry, health industry, cosmetic industry, and other industries.

The plant extract of the present invention is preferably neem tree extract. Melia azedarach L.is an arbor of the Meliaceae family, the genus Melia, deciduous trees, up to 10 meters in height; the bark is gray brown, the branches are wide and spread, the leaves are 2-3 times odd feathery compound leaves, the small She Duisheng, the leaves are oval, elliptical or scaly, and the apical side is slightly larger.

As used herein, the term "plant polysaccharide extract" is a substance extracted from a plant and having a polysaccharide as a main component. The polysaccharide is a general name of a polymer formed by connecting monosaccharides through glycosidic bonds, and a large number of hydrophilic hydroxyl groups enable many polysaccharides to show some excellent physicochemical properties, such as strong water absorption and good film forming property. The pure natural plant polysaccharide not only has excellent moisturizing performance, but also meets the requirements of people on safety and environmental protection. The plant polysaccharide extract forms a water-containing film on the surface of the skin to lock water, so that the nano-silver can be ensured to be in a water-containing environment for a long time, and the bacteriostatic effect of the nano-silver can be exerted to the greatest extent.

The plant polysaccharide extract in the present invention is preferably an orchid polysaccharide extract, and most preferably an extract of Gymnadenia conopsea (l.) r.br.).

As used herein, the term "saponin" is a glycoside whose aglycone is a triterpene or spirostane compound, and is mainly distributed in plants such as terrestrial plateau and is present in a small amount in marine organisms such as starfish and sea cucumber. The main effective components of many Chinese herbal medicines such as ginseng, polygala root, platycodon root, liquorice, rhizoma anemarrhenae, radix bupleuri and the like contain saponin. Some saponins also have antibacterial activity or antipyretic, sedative, and anticancer activities. The saponin is preferably the gleditschia horrida saponin, and is an extract derived from the fruit of the gleditschia horrida.

As used herein, the term "glycyrrhetic acid" is formed by hydrolysis of glycyrrhetic acid to remove sugar acid chains, has a sweetness of 250 times that of sucrose, is an active ingredient of licorice, and is extracted from licorice root.

The main advantages of the invention are:

(1) The composite bacteriostatic agent adopts the following raw materials except 51 preservatives allowed by 3 cosmetic laws: the nano-silver, the plant extract and the plant polysaccharide extract are safer, milder and have no stimulation.

(2) The composite bacteriostatic agent disclosed by the invention is prepared by compounding the nano-silver, the chinaberry tree extract and the plant polysaccharide extract, so that the problem that the nano-silver is easy to aggregate and precipitate is solved, and the nano-silver can be more conveniently used in cosmetics.

(3) Because the nano silver can release silver ions with strong charges, and the plant polysaccharide extract contains a large amount of polysaccharide and protein substances, the charge balance is easily damaged by the silver ions to cause flocculent precipitate.

(4) According to the composite bacteriostatic agent, the nano-silver, the chinaberry extract and the plant polysaccharide extract are compounded, so that the bacteriostatic ability is remarkably improved, and a synergistic technical effect is achieved among the components.

(5) The composite bacteriostatic agent disclosed by the invention is prepared by compounding nano-silver, a chinaberry tree extract and a plant polysaccharide extract, so that the long-time moisturizing capability is obviously improved.

The present invention will be described in further detail with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Experimental procedures for conditions not specified in detail in the following examples are generally carried out under conventional conditions such as those described in molecular cloning, A laboratory Manual (Huang Peitang, eds., beijing: scientific Press, 2002, USA, sambrook, et al, USA, or under conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by weight. The test materials and reagents used in the following examples are commercially available without specific reference.

Specifically, the nano-silver of the present invention is available from heter international (shanghai) limited. Gymnadenia conopsea extract (water extract of gymnadenia conopsea root tuber 50). Neem tree EXTRACT (water EXTRACT of neem domimeticum EXTRACT, neem seed 30. Saponins (water extract of Gleditsia sinensis fruit 50. Glycyrrhetinic acid was obtained from Tanshan pharmaceutical Co.

EXAMPLE 1 Complex bacteriostatic Components proportioning Screen

In the research, the nano silver is directly added into the cosmetics, and is easy to aggregate and precipitate. In addition, the nano silver can release silver ions with strong charges, and the plant polysaccharide extract contains a large amount of polysaccharide and protein substances, so that the silver ions can easily destroy the charge balance to cause flocculent precipitation. Therefore, the present invention has conducted a number of screening tests in order to obtain a stable formulation system.

Some of the test data are listed below.

The preparation method of each composition comprises the following steps:

1) Putting the raw materials into an emulsifying pot, mixing the raw materials together, and stirring the mixture into a uniform mixture at the temperature of between 40 and 80 ℃;

2) Adjusting the pH of the mixture to 5.0-8.0

3) Filtering the mixture in the emulsifying pot, cooling the filtered mixture to room temperature, standing for 7d, and observing.

The contents of the components in the following table are the mass percentage contents added in the traditional cosmetic water. The conventional lotion is composed of 5% of glycerin, 0.1% of 1% hyaluronic acid aqueous solution, and 94.9% water.

TABLE 1

Experimental results show that a stable system with good dispersion can be obtained by compounding the nano-silver and the conic gymnadenia rhizome extract. The nano silver, the conic gymnadenia rhizome extract and the chinaberry tree extract are compounded, a stable system with good dispersion can be obtained, and the appearance of the product is shown in figure 1.

Example 2 moisturizing test

1. The lotions of experimental groups 1 to 4 were prepared according to the raw materials and weight percentage ratios of table 2, wherein the conventional lotion consisted of 5% glycerol, 0.1% hyaluronic acid aqueous solution, and 94.9% water.

TABLE 2

The preparation method comprises the following steps:

1) Putting the raw materials into an emulsifying pot, mixing the raw materials together, and stirring the mixture into a uniform mixture at the temperature of between 40 and 80 ℃;

2) Adjusting the pH of the mixture to 5.0-8.0

3) And filtering the mixture in the emulsifying pot, and cooling the filtered mixture to room temperature to obtain a finished product.

2. Cleaning the arm, air-drying for half an hour, respectively taking five square areas of 2 multiplied by 2cm on the forearm of the arm, detecting the water content of the stratum corneum of the skin, respectively smearing five samples of the toning lotion of experimental groups 1-4 and the water of a blank control group in different areas, taking 0.1ml of each sample, detecting once every 2 minutes after smearing and complete absorption, then detecting once every half an hour for 4 times, wherein the detection data is the water content of the stratum corneum of the skin. The results are shown in Table 3. Blank is 100% deionized water.

TABLE 3

Numbering	0min	2min	30min	60min	90min
						Experimental group 1	31.28％	50.22％	46.04％	44.22％	44.44％
Experimental group 2	32.81％	58.22％	57.76％	53.02％	50.32％
						Experimental group 3	33.62％	56.32％	57.63％	53.52％	53.46％
Experimental group 4	36.52％	43.40％	42.00％	42.12％	41.14％
						Experimental group 5	33.38％	56.06％	55.18％	52.46％	51.82％
Blank group	34.76％	42.68％	41.40％	41.08％	41.02％

According to the results in table 3, the experimental groups 2 and 3 can greatly improve the water content of the stratum corneum of the skin and have strong water replenishing and moisturizing capabilities compared with other samples. Proves that the skin epidermis moisturizing effect of the product can be obviously improved when the sample contains the arethusa extract (the gymnadenia conopsea extract). The moisture content of the stratum corneum of the experimental group 3 was maintained at a relatively high level for a period of time, and did not decrease continuously with time, as compared to the moisture content of the stratum corneum of the experimental group 2, so that the sample of the experimental group 3, which contained nano-silver, the gymnadenia conopsea extract, and the neem tree extract at the same time, had the best moisturizing effect.

Example 3 antimicrobial test

1. Lotions were prepared according to the raw materials and weight percentages in table 4.

TABLE 4

2. Test medium and strain

Culture medium:

TSB culture medium tryptone soya broth

YM Medium Yeast malt extract Medium

Letheen broth culture medium USP special culture medium for cosmetic preservation test

Lecithin Tween culture medium

Monglara red medium

Strain:

3. experimental method referring to the microorganism inspection method in chapter V of technical Specification for safety of cosmetics (2015), the concrete steps are shown in FIG. 2, the strains are divided into bacteria and fungi for experiment, and 10 inoculating bacteria and fungi are inoculated into culture medium on day 0 ⁶ cfu/ml bacteria and fungi, and observing the growth state of the bacteria and fungi by taking 1ml of culture medium at 25 ℃ under the environment of 60% humidity on the 7 th day, 14 th day, 21 th day and 28 th day of culture.

The experimental results are shown in table 3, and the judgment criteria of the results are: the total number of colonies of the bacteria is reduced by 99.9% at the 7 th day, and no increase is generated at the 28 th day; the fungus is judged to be preserved if the fungus is reduced by 99.0% at the 14 th day and does not grow until 28 days, otherwise, the fungus is not preserved.

TABLE 5

According to the results in the table, the control groups 1, 2 and 3 respectively contain one or more of nano silver and chinaberry plant extracts, and the preservation challenge tests of the control groups all fail, and the control groups do not have the preservation effect. And meanwhile, the experiment group containing the nano silver, the chinaberry extract and the conic gymnadenia rhizome extract has successful anticorrosion challenge test and has anticorrosion effect. It is stated that in the composition, in order to achieve the desired bacteriostatic effect, the nano-silver, the chinaberry extract and the orchidaceae plant extract must be contained at the same time.

Example 4 safety test

1. Laboratory animal

Healthy male SPF-grade mice 6-8 weeks old, with a body weight of (25 + -2) g. Raising at 25 + -2 deg.C and humidity of 40 + -10%.

2. Establishment, grouping and administration of animal models

Mice were randomly grouped, 6 mice per group. The back side of the shaved and cleaned mouse was divided into two areas (2.5 cm. Times.2.5 cm), 0.5g of skin care lotion of each formulation group was applied to the left side, and a blank control was applied to the right side, which was covered with gauze and fixed with adhesive tape, and skin reactions at the applied site were observed after 1h, 24h, and 48 h.

After 14 consecutive days of application, the skin reaction at the site of application was observed and recorded. The skin was evaluated for irritation response and irritation intensity with reference to "evaluation procedure and method for cosmetic safety".

The result shows that although the skin care lotion containing the composite bacteriostatic agent has strong bacteriostatic and moisturizing capabilities, after the skin care lotion is continuously applied for 14 days, 2 mice in an experimental group have slight erythema phenomenon; 1 only a slight edema phenomenon appeared. The skin care lotion containing the composite bacteriostatic agent of the invention is shown to have slight inflammation in the using process. In order to solve the problem, the invention further optimizes the composite bacteriostatic agent.

The inventor respectively compounds more than 20 active ingredients from plants with the composite bacteriostatic agent, screens out 8 active ingredients which can be stably compounded with the composite bacteriostatic agent, and then tests the skin irritation experiment, and the result shows that the skin irritation defect can be eliminated by adding 0.1% of saponin and 0.01% of glycyrrhetinic acid into the composite bacteriostatic agent. By using the optimized formula, the skin of each mouse in 6 mice in the experimental group has no edema and erythema compared with the skin without the skin care lotion, and the skin care lotion after optimization is proved to have no irritation to the skin.

The finally optimized compound bacteriostatic agent comprises the following components in parts by weight:

0.02-0.20 weight part of nano silver;

0.10-10 parts by weight of chinaberry extract;

5-20 parts of gymnadenia conopsea extract;

0.05 to 0.20 weight portion of saponin;

0.01-0.02 weight part of glycyrrhetinic acid.

Example 5 moisturizing and antibacterial testing of skin emulsions

The skin care emulsion was prepared in the following manner, wherein the conventional skin care emulsion is a general product commercially available.

1. Preparing the raw materials

Taking 0.10g of nano-silver, 0.30g of chinaberry plant extract, 10.00g of gymnadenia conopsea extract, 0.1g of saponin and 0.01g of glycyrrhetinic acid, and adding traditional skin care lotion to 100g.

2. Mixing and stirring

The raw materials obtained in the first step are put into an emulsifying pot, mixed together and stirred into a uniform mixture at the temperature of 40 ℃.

3. Adjusting the pH of the mixture

The pH of the mixture obtained in step 2 was adjusted to 7.5.

4. Filtering, cooling to obtain the final product

Filtering the mixture in the emulsifying pot at 30-45 ℃, and cooling the filtered mixture to room temperature to obtain a finished product.

The prepared skin care emulsion was subjected to a moisturizing test according to the method of example 2, and the test results were: the skin care emulsion prepared by the invention can greatly improve the water content of the skin cuticle and has strong water replenishing and moisturizing capabilities.

The prepared skin care emulsion was subjected to an antibacterial test according to the method of example 3, and the test results were: the skin care emulsion prepared by the invention has antibacterial activity.

The prepared skin care emulsion was subjected to a safety test according to the method of example 4, and the test results were: the skin care emulsion prepared by the invention has good safety.

Example 4 moisturizing and antibacterial tests of hand lotions

The hand sanitizer was prepared as follows, wherein the conventional hand sanitizer is a common product on the market.

1. Preparing the raw materials

Taking 0.07g of nano-silver, 0.6g of chinaberry plant extract, 15g of gymnadenia conopsea extract, 0.15g of saponin and 0.02g of glycyrrhetinic acid, and adding the traditional hand sanitizer to 100g.

2. Mixing and stirring

The raw materials obtained in the first step are put into an emulsifying pot, mixed together and stirred into a uniform mixture at 40 ℃.

3. Adjusting the pH of the mixture

The pH of the mixture obtained in the second step was adjusted to 7.5.

4. Filtering, cooling to obtain the final product

Filtering the mixture in the emulsifying pot at 30-45 ℃, and cooling the filtered mixture to room temperature to obtain a finished product.

The prepared hand sanitizer is subjected to a moisturizing test according to the method in example 2, and the test result is as follows: the hand sanitizer prepared by the invention can greatly improve the water content of the skin cuticle and has strong water replenishing and moisturizing capabilities.

The prepared hand sanitizer is subjected to an antibacterial test according to the method of example 3, and the test result is as follows: the hand sanitizer prepared by the invention has antibacterial activity.

The prepared hand sanitizer is subjected to a safety test according to the method of example 4, and the test result is as follows: the hand sanitizer prepared by the invention has good safety.

Example 5 moisturizing and antibacterial tests of body wash

The hand sanitizer was prepared as follows, with a conventional body wash being a common product on the market.

1. Preparing the raw materials

Taking 0.05g of nano-silver, 1.0g of chinaberry plant extract and 12g of conic gymnadenia rhizome extract, and adding traditional shower gel to 100g.

2. Mixing and stirring

The raw materials obtained in the first step are put into an emulsifying pot, mixed together and stirred into a uniform mixture at the temperature of 40 ℃.

3. Adjusting the pH of the mixture

The pH of the mixture obtained in the second step was adjusted to 7.5.

4. Filtering, cooling to obtain the final product

Filtering the mixture in the emulsifying pot at 30-45 ℃, and cooling the filtered mixture to room temperature to obtain a finished product.

The prepared hand sanitizer is subjected to a moisturizing test according to the method of example 2, and the test result is as follows: the hand sanitizer prepared by the invention can greatly improve the water content of the skin cuticle and has strong water replenishing and moisturizing capabilities.

The prepared hand sanitizer is subjected to an antibacterial test according to the method of example 3, and the test result is as follows: the hand sanitizer prepared by the invention has antibacterial activity.

The prepared hand sanitizer is subjected to a safety test according to the method of example 4, and the test result is as follows: the hand sanitizer prepared by the invention has good safety.

All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.

Claims (10)

1. The composite bacteriostatic agent with bacteriostatic and epidermal moisturizing effects is characterized by comprising the following components in parts by weight:

2. the composite bacteriostatic agent according to claim 1, which comprises the following components in parts by weight:

3. use of the composite bacteriostatic agent according to claim 1 in the preparation of cosmetics.

4. The use according to claim 3, wherein the cosmetic comprises skin lotion, hand wash and body wash.

5. Use according to claim 3, wherein the cosmetic product is a skin care emulsion.

6. A cosmetic comprising the complex bacteriostatic agent of claim 1.

7. The cosmetic of claim 6, wherein the cosmetic comprises skin lotion, hand cleanser and body wash.

8. The cosmetic of claim 6, wherein the cosmetic is a skin care lotion.

9. The preparation method of the composite bacteriostatic agent is characterized by comprising the following steps of:

(1) Mixing the raw materials of the composite bacteriostatic agent, and stirring the mixture at 40-80 ℃ to form a uniform mixture;

(2) Adjusting the pH value of the mixture to 5.0-8.0;

(3) Filtering the mixture, and cooling to room temperature to obtain the composite bacteriostatic agent;

the composite bacteriostatic agent comprises the following raw materials in parts by weight:

10. the method of claim 9, wherein the composite bacteriostatic agent raw material comprises the following components in parts by weight:

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