CN111184656A - Skin barrier repair micro-nano emulsion containing camellia oil and preparation method thereof - Google Patents

Abstract

The invention relates to the field of cosmetics, in particular to a skin barrier repair micro-nano emulsion containing camellia oil and a preparation method thereof. The ingredients are as follows: 10-50 wt% of camellia oil, 0.1-5 wt% of ceramide, 0.05-3 wt% of cholesterol, 0.03-2 wt% of fatty acid, 1-10 wt% of water, 1-10 wt% of phospholipid and the balance of glycerol; the preparation method comprises the following steps: mixing glycerol and water, adding phospholipid, and swelling to obtain phase A; mixing ceramide, cholesterol, fatty acid and camellia oil, and stirring until solute is dissolved to obtain a phase B; mixing and homogenizing the phase A and the phase B to obtain a pretreatment solution, carrying out high-pressure homogenization on the pretreatment solution, discharging and cooling to obtain the skin barrier repair micro-nano emulsion containing camellia oil. The nano emulsion prepared by the invention has good skin barrier repair effect and is repaired more quickly; the whole emulsion has good stability and water dispersibility, and is convenient to match and use with other components.

Description

Skin barrier repair micro-nano emulsion containing camellia oil and preparation method thereof

Technical Field

The invention relates to the field of cosmetics, in particular to a skin barrier repair micro-nano emulsion containing camellia oil and a preparation method thereof.

Background

Skin barrier function is one of the important functions of the skin, over-cleansing, makeup removal, and some sensitive skin, where the skin barrier is weakened. Wherein the lipids of the stratum corneum are of great importance for the proper functioning of the skin barrier. Skin problems such as dryness, roughness and the like are external manifestations of stratum corneum dysfunction, in which the dry state of the skin cannot be well changed if the skin is simply supplemented with water, and more importantly, restoration and maintenance of normal stratum corneum barrier function is achieved by supplementing the lipid components of the stratum corneum.

The lipid constituting the human skin barrier mainly comprises two parts: lipid membrane and stratum corneum intercellular lipids. The sebaceous membrane consists of lipids secreted by sebaceous glands and disintegrated by keratinocytes, mainly composed of squalene (12%), wax lipids (26%), triglycerides (57.5%), cholesterol esters (3.0%), cholesterol (1.5%). The main components of stratum corneum intercellular lipid are sphingomyelin, glucosyl ceramide, phospholipid, cholesterol and the like, and ceramide (50%), free fatty acid (15%) and cholesterol (25%) form a multilayer membrane of stratum corneum which fills the whole stratum corneum intercellular stroma.

The water-lipid film (Hydro-lipid film) covering the skin surface is also called skin lipid film, lipidation film, hydration film and the like, and is the outermost layer defense line of the skin barrier structure. The water is secreted from sweat gland and evaporated from epidermis, and the lipid is secreted from sebaceous gland, and also contains many epidermal metabolites, inorganic salts, etc. The lipids in sebum lubricate the skin and reduce the evaporation of water from the skin surface. Excessive washing removes sebum from the skin, disrupts the hydrated film barrier of the skin, causes dryness of the skin and increased loss of transdermal water, which is the basis of the onset of senile cutaneous pruritus.

Camellia oil is also called tea oil, camellia seed oil, etc. The camellia oil is composed of fatty acid, camellin, phospholipid, saponin, vitamin E, tannin and other components. The tea oil has rich unsaturated fatty acid content up to more than 85%, and the fatty acid composition of the tea oil is very similar to that of olive oil. The camellia oil also has good skin care and skin moistening effects. The camellia oil can effectively supplement triglyceride in the sebum membrane. The camellia oil not only can supplement components of a human body sebum membrane, but also has a promotion effect on percutaneous absorption of medicines, and the camellia oil is frequently used as an ointment matrix in the aspect of medicaments.

Stratum corneum intercellular lipids, also known as structural lipids, are important components that constitute the physical barrier structure of the skin. The brick wall model is used to describe the organization structure of the stratum corneum of the skin, and intercellular lipid is the mortar between bricks. Intercellular lipids are synthesized by the spine cells, distributed in the cytoplasm in the form of lamellar bodies or Orland bodies, which gradually move to the cell periphery during the upward migration and differentiation of the spine cells, fuse with the cell membrane, and finally are excreted in the interstitial space in the form of exocytosis, or become intercellular components connected to the protosomal body as the cells finally differentiate, cornify and collapse. From the biochemical composition, intercellular lipid is remarkably changed in the differentiation process from acanthocyte to keratinocyte, namely polar lipid is rapidly reduced, neutral lipid is gradually increased, particularly sphingolipid such as ceramide, and the latter has excellent water storage and moisture retention capacity and is a moisture retention raw material frequently used in cosmetics; from the structural characteristics, intercellular lipid has an obvious biomembrane bilayer structure, namely, a lipophilic group faces inwards, a hydrophilic group faces outwards, and a multi-layer sandwich structure with water and lipid phases is formed. This structure on the one hand retains the semi-permeable or selectively permeable nature of the biofilm, favouring the absorption and permeation of certain small-molecule nutrients, such as electrolytes, and on the other hand it binds a portion of the water molecules, so-called bound water, which is not lost even in the case of very dry conditions, to immobilize the latter. Research of dermatologists shows that the abnormity of intercellular lipid not only reduces the water storage and moisture retention functions of skin, but also directly influences the growth, differentiation and regulation of keratinocyte, and influences the formation of healthy stratum corneum.

Researchers are now increasingly focusing on the role of intercellular lipids in keratinocytes, particularly the use of ceramides. At present, many studies on the nano-level of ceramide mainly include that ceramide has physical and chemical properties such as high melting point and insolubility, can be dissolved in grease at high temperature, and is easy to crystallize and separate out after the ceramide is recovered to room temperature. In addition, ceramides are poorly water-soluble and tend to crystallize out in aqueous media. The following patents are all published documents for micro-nano coating of ceramide to provide a preparation with good stability and easy water solubility.

CN100536817C discloses a ceramide nano liposome preparation and a preparation method and application thereof. The preparation method is characterized in that 0.1-5 wt% of ceramide, 1-20 wt% of phospholipid, 10-70 wt% of glycerol and 25-80 wt% of water are discharged by a high-pressure homogenizer to obtain the ceramide nano liposome preparation with the average grain diameter of less than 100 nm. The liposome preparation has the characteristics of high stability, biological compatibility of a water dispersing agent and the like. CN103690391B discloses a ceramide nano-emulsion and a preparation method thereof, and the key points are as follows: mixing 10-67% of glycerol, 0.1-4% of cholesterol, 0.1-6% of ceramide, 0.1-3% of hydrogenated phospholipid and 1-12% of octyl dodecanol uniformly at 70-90 ℃, adding 1-25% of water by weight into the mixed solution, stirring uniformly, and treating by a high-pressure homogenizer to obtain the ceramide nanoemulsion with semitransparent or transparent appearance. The ceramide nanoemulsion has the characteristics of high stability, good water dispersibility, good biocompatibility, capability of being freely matched with a cosmetic formula at normal temperature and the like. CN104739658B discloses a ceramide nano-emulsion, which is characterized in that a Gemini surfactant with a special structure is used, so that the use amount of an emulsifier is remarkably reduced, and the content of ceramide in a formula is increased. Has good water dispersibility and biocompatibility, and can be freely matched with a cosmetic formula at normal temperature.

These inventions focus on the important role of intercellular lipid ceramide and solve the problem of compatibility to some extent. However, it has been shown that abnormalities in any of the lipid components of intercellular lipids directly affect the skin barrier structure, resulting in transdermal water loss.

In addition, studies have been reported to enhance the skin barrier both from intercellular lipids and the sebaceous membrane.

CN102579287B discloses a cosmetic composition for repairing skin stratum corneum, which comprises, by mass, 30-60% of camellia oil, 20-50% of ceramide, 5-35% of cholesterol, 2-30% of lecithin and 0.1-25% of vitamin and derivatives thereof. The camellia oil is used as the basic oil, so that the absorptivity and permeability of physiological lipid are improved to a certain extent, and the restoration of the barrier function of the damaged cuticle of the skin can be accelerated. However, the compatibility of ceramide is not sufficiently considered, and ceramide is likely to crystallize, and the skin permeability is limited.

CN107998046A discloses a moisturizing agent containing high molecular humectant, small molecular humectant, phytosterol, camellia oil, meadowfoam seed oil, isohexadecane, ceramide-1, hydrogenated lecithin, rosemary leaf extract, plant active extract, EDTA-2Na, L-glutamic acid and water. And a nanoemulsion spray composition was prepared. Although the formula adopts the nano emulsion as the emulsion, the composition is mild, fresh and moist, can effectively relieve the problems of dry and itching scalp and related inflammation of an allergic agent, and increases the barrier function of skin. The invention mainly solves the problem of the scalp. Although the camellia oil is matched with the ceramide and the phytosterol, the content of the camellia oil is low, the ceramide cannot be completely dissolved to achieve a good permeation promoting effect, and free fatty acid is not contained.

Disclosure of Invention

The invention provides a skin barrier repair micro-nano emulsion containing camellia oil and a preparation method thereof, aiming at solving the problems of uneven active ingredients, poor water solubility, easy precipitation and the like of the existing skin/stratum corneum barrier repair emulsion, poor compatibility, poor skin permeability and the like, or a series of problems of poor effect, limited functionality and the like although the active ingredients are stable and easy to permeate the skin. The invention aims to: firstly, the stability and the water solubility of the effective component ceramide in the emulsion are improved; secondly, the skin permeability of the lotion is improved, and the absorption of effective components of the lotion by a human body is further promoted; thirdly, a good skin water retention effect can be realized; and fourthly, improving the repair efficiency of the skin barrier while realizing a good skin barrier repair effect.

In order to achieve the purpose, the invention adopts the following technical scheme.

A skin barrier repair micro-nano emulsion containing camellia oil,

the skin barrier repair micro-nano emulsion containing camellia oil comprises the following components in percentage by weight:

10-50 wt% of camellia oil, 0.1-5 wt% of ceramide, 0.05-3 wt% of cholesterol, 0.03-2 wt% of fatty acid, 1-10 wt% of water, 1-10 wt% of phospholipid and the balance of glycerol.

In the technical scheme of the invention, the camellia oil is used as a good solvent while being used as a skin care component. The camellia oil contains various nutrient components such as unsaturated fatty acid, vitamin, mineral substance and the like which are effective to human skin, and the camellia oil is listed in Chinese pharmacopoeia as a medicine and has a long history of being used for treating skin diseases. In addition, the camellia oil also contains active substances such as tea polyphenol, squalene and the like, and has good oxidation resistance and skin barrier repairing capacity, so that the camellia oil has very excellent affinity to a human body and skin care effect on skin by taking the camellia oil as a main raw material.

In addition, the camellia oil can effectively dissolve the ceramide, compared with the technical scheme that glycerol is used as a solvent in CN100536817C, CN103690391B, CN104739658B and the like, the camellia oil is used as the solvent to dissolve the ceramide, and meanwhile, the camellia oil and the ceramide can achieve a good skin barrier repairing effect, and by reasonably controlling the using amounts of the camellia oil and the ceramide, a good compatibility effect can be achieved, and further a more excellent skin barrier repairing effect can be achieved.

The phospholipid is almost present in all organism cells, contains more phospholipid in important tissues of animals and plants, can be used as an emulsifier to form a lipid bilayer together with other molecules such as protein, glycolipid, cholesterol and the like, and the cholesterol is selected to realize the formation of the lipid bilayer, so that the skin moisturizing effect is good.

In addition, the phospholipid is preferably lecithin or hydrogenated lecithin, the lecithin and the hydrogenated lecithin have mature application in the field of food and medicine, are important components of human cell membranes, have excellent affinity with human skin, are very safe to human bodies, and can play roles in repairing skin barriers and moistening skin besides playing a good emulsification effect.

As a preference, the first and second liquid crystal compositions are,

the skin barrier repair micro-nano emulsion containing camellia oil comprises the following components in percentage by weight:

15-30 wt% of camellia oil, 0.5-3 wt% of ceramide, 0.2-1.8 wt% of cholesterol, 0.15-1.2 wt% of fatty acid, 2-8 wt% of water, 2-5 wt% of phospholipid and the balance of glycerol.

The proportion is better, the performance is more stable, compared with the dosage range of the components, the dosage range is more suitable for fine and high-quality production, the overall performance fluctuation is smaller, the difference is lower, and the effect is in a better range.

As a preference, the first and second liquid crystal compositions are,

the mass ratio of the camellia oil to the ceramide is more than or equal to 10: 1.

the dosage of the camellia oil can achieve the optimal dissolving effect of the ceramide by ten times or more than that of the ceramide, so that the ceramide can be uniformly dispersed in droplets of the camellia oil, and the problems that the ceramide is difficult to be absorbed by a human body due to precipitation, crystallization and precipitation in water and the like are avoided.

As a preference, the first and second liquid crystal compositions are,

the mass ratio of the ceramide to the cholesterol to the fatty acid is 1: (0.4-0.6): (0.3-0.4).

The ceramide, cholesterol and fatty acid in the proportion range are closer to the normal composition proportion of lipid among human keratinocytes, the lipid environment is easier to improve and regulate, and the effect of repairing skin barriers is realized.

As a preference, the first and second liquid crystal compositions are,

the ceramide is any one or mixture of ceramide 2 and ceramide 3.

As a preference, the first and second liquid crystal compositions are,

the content of phosphatidylcholine in the phospholipid is more than or equal to 75 wt%;

the fatty acid is any one or more of palmitic acid, stearic acid, oleic acid and linoleic acid.

Phosphatidylcholine is a phospholipid with a choline head group, and is a major component of biological membranes. The phospholipid and cholesterol form a lipid bilayer when being used in a compounding way, so that not only can the lipid environment between corneocytes be effectively and reasonably regulated, but also the coating and repair of damaged corneocytes can be further realized, and a good skin barrier repair effect is realized. The palmitic acid, the stearic acid, the oleic acid and the linoleic acid in the fatty acid have the property of being insoluble/insoluble in water, have good compatibility with camellia oil, and have certain effects of moistening skin, moisturizing and repairing skin barriers.

A method for preparing skin barrier repair micro-nano emulsion containing camellia oil,

the preparation method comprises the following preparation steps:

1-a) mixing glycerol and water, adding phospholipid, homogenizing until the phospholipid is uniformly swelled to be used as phase A;

1-B) mixing ceramide, cholesterol, fatty acid and camellia oil, and stirring until solute is completely dissolved to obtain a B phase;

2) mixing the phase A and the phase B, carrying out high-speed homogenization, obtaining a pretreatment solution after the high-speed homogenization, carrying out high-pressure homogenization on the pretreatment solution for a plurality of times, and then discharging and cooling to obtain the skin barrier repair micro-nano emulsion containing camellia oil.

In the method, firstly, water and glycerol are mixed to serve as an aqueous phase solvent, phospholipid is added to carry out homogenization, so that the phospholipid is swelled in the aqueous phase solvent to be in a uniform state, phase A is obtained, meanwhile, phase B preparation can be carried out simultaneously or sequentially, camellia oil serves as an oil phase solvent to dissolve ceramide, cholesterol and fatty acid, camellia oil serves as a main component, and after the ceramide, the cholesterol and the fatty acid are dissolved, the camellia oil can be well protected, and the problems of precipitation, crystallization and the like are avoided when the camellia oil is subsequently mixed with the aqueous phase.

In the step 2), when the phase A and the phase B are mixed, firstly, the phospholipid which is uniformly swelled and dispersed in the phase A wraps the active ingredient in the phase B, so that the problem that the active ingredient is separated out and precipitated when contacting water is avoided, the stability of the active ingredient is ensured, meanwhile, the emulsion droplets are primarily dispersed by high-speed homogenization, the emulsion droplets which are uniform and have larger particle size are formed after the high-speed homogenization, the emulsion droplets can be basically and uniformly dispersed in the pretreatment liquid, the high-pressure homogenization is further carried out, the nanocrystallization of the emulsion droplets can be realized, and the emulsion droplets with larger particle size are dispersed to form nano droplets with the particle size reaching the nano scale.

As a preference, the first and second liquid crystal compositions are,

homogenizing at 60-65 deg.c in step 1-a);

and (B) stirring at 75-80 ℃, cooling to 63-65 ℃ after the solute is completely dissolved, and preserving heat to obtain a phase B.

Under the condition of the 1-a), the swelling efficiency of the phospholipid in the aqueous phase solvent is higher, the effect is better, the preparation efficiency of the A phase can be effectively improved, and the swelling stability of the phospholipid is ensured. Under the condition of 1-b), the homogenization is faster, the uniform dissolution of each component can be promoted, and the heat preservation is carried out at 63-65 ℃, so that the problem that emulsion liquid drops are unstable due to overhigh temperature when the subsequent two phases are mixed is solved, and the problem that partial components are separated out, crystallized and precipitated due to the temperature reduction is solved.

As a preference, the first and second liquid crystal compositions are,

step 2), the high-speed homogenizing rotating speed is 5000-6000 rpm, and the high-speed homogenizing lasts for 5-10 min;

step 2), performing high-pressure homogenization by using a micro-jet high-pressure homogenizer at the homogenization pressure of 200-250 MPa for 3-8 times of circulation;

and 2) discharging and cooling to be less than or equal to 37 ℃ to obtain the skin barrier repair micro-nano emulsion containing camellia oil.

The preparation method can achieve a good primary homogenizing effect under the condition of the rotating speed, form uniform and dispersed emulsion droplets, basically achieve the preparation of nano droplets after secondary homogenization is carried out through a micro-jet high-pressure homogenizer, ensure that the droplets have high uniformity by repeatedly carrying out 3-8 times of circulation, and achieve that the average particle size reaches 150nm and below.

As a preference, the first and second liquid crystal compositions are,

the average particle size of the skin barrier repair micro-nano emulsion containing camellia oil is 80-150 nm.

The average particle size of the nano liquid drops in the skin barrier repair micro-nano emulsion containing camellia oil is in favor of absorption of human skin, if the particle size of the nano liquid drops is further reduced, the absorption effect is not obviously improved, but the cost is further greatly improved, so that the integral cost ratio is obviously reduced.

The invention has the beneficial effects that:

1) the prepared skin barrier repair micro-nano emulsion containing camellia oil has a good skin barrier repair effect;

2) the skin barrier repair efficiency is higher, and quick and effective repair can be realized;

3) the integral emulsion has good stability and water dispersibility, and is convenient to match and mix with other components;

4) the skin barrier repair micro-nano emulsion containing camellia oil further has a good water retention effect;

5) the whole skin has better permeability and is beneficial to the absorption of human body.

Drawings

FIG. 1 is a graph comparing the rate of skin barrier repair for group A and group B;

FIG. 2 is a graph comparing the skin barrier repair rates of group A and group C;

FIG. 3 is a graph comparing the skin barrier repair rates of group A and group D;

FIG. 4 is a graph comparing the skin barrier repair rates of group A and group E;

FIG. 5 is a graph comparing skin moisture levels of group A and group B;

FIG. 6 is a graph comparing skin moisture levels of group A and group C;

FIG. 7 is a graph comparing skin moisture content for group A and group D;

figure 8 is a graph comparing skin moisture content for group a and group E.

Detailed Description

The invention is described in further detail below with reference to specific embodiments and the attached drawing figures. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.

Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.

Example 1

Preparing 1kg of skin barrier repair micro-nano emulsion containing camellia oil;

the ingredients are as follows:

camellia oil (200g), ceramide 2(10g), cholesterol (6g), stearic acid (4g), water (20g), lecithin (30g) and glycerol (730 g);

the preparation method comprises the following steps:

1-a) mixing glycerol and water, adding lecithin, homogenizing at 63 +/-2 ℃ until the phospholipid is uniformly swelled to be used as phase A;

1-B) mixing ceramide 2, cholesterol, stearic acid and camellia oil, stirring at 78 +/-2 ℃ until the ceramide, the cholesterol and the fatty acid are completely dissolved to form a uniform oil phase, and then cooling to 64 +/-1 ℃ for storage as a phase B;

2) mixing the phase A and the phase B, homogenizing at 5000rpm for 5min at high speed to obtain a pretreatment solution, homogenizing the pretreatment solution at high pressure by a microfluid high-pressure homogenizer at the homogenizing pressure of 200MPa for 3 times, and discharging and cooling to a temperature of less than or equal to 37 ℃ to obtain the camellia oil-containing skin barrier repair micro-nano emulsion.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 91 nm.

Example 2

Preparing 1kg of skin barrier repair micro-nano emulsion containing camellia oil;

the ingredients are as follows:

camellia oil (250g), ceramide 3(25g), cholesterol (12.5g), oleic acid (7.5g), water (50g), hydrogenated lecithin (40g), glycerol (615 g);

the preparation method comprises the following steps:

1-a) mixing glycerol and water, adding hydrogenated lecithin, homogenizing at 63 +/-2 ℃ until the phospholipid is uniformly swelled to be used as phase A;

1-B) mixing ceramide 3, cholesterol, oleic acid and camellia oil, stirring at 78 +/-2 ℃ until the ceramide, the cholesterol and the fatty acid are completely dissolved to form a uniform oil phase, and then cooling to 64 +/-1 ℃ for storage as a phase B;

2) mixing the phase A and the phase B, homogenizing at 6000rpm for 8min at high speed to obtain a pretreatment solution, homogenizing the pretreatment solution at high pressure by a microfluid high-pressure homogenizer at the homogenizing pressure of 230MPa for 5 times, and discharging and cooling to a temperature of less than or equal to 37 ℃ to obtain the camellia oil-containing skin barrier repair micro-nano emulsion.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 108 nm.

Example 3

Preparing 1kg of skin barrier repair micro-nano emulsion containing camellia oil;

the ingredients are as follows:

camellia oil (400g), ceramide 3(20g), ceramide 2(20g), cholesterol (20g), palmitic acid (10g), linoleic acid (4g), water (100g), lecithin (50g), glycerol (376 g);

the preparation method comprises the following steps:

1-a) mixing glycerol and water, adding lecithin, homogenizing at 63 +/-2 ℃ until the phospholipid is uniformly swelled to be used as phase A;

1-B) mixing ceramide 2, ceramide 3, cholesterol, palmitic acid, linoleic acid and camellia oil, stirring at 78 +/-2 ℃ until the ceramide, the cholesterol and the fatty acid are completely dissolved to form a uniform oil phase, and then cooling to 64 +/-1 ℃ for storage as a phase B;

2) mixing the phase A and the phase B, homogenizing at 6000rpm for 10min at high speed to obtain a pretreatment solution, homogenizing the pretreatment solution at high pressure by a microfluid high-pressure homogenizer at the homogenizing pressure of 200MPa for 8 times, and discharging and cooling to a temperature of less than or equal to 37 ℃ to obtain the camellia oil-containing skin barrier repair micro-nano emulsion.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 125 nm.

Example 4

The specific preparation procedure was the same as in example 2, except that: the usage amount of camellia oil is 100g, the usage amount of ceramide 3 is 1g, the usage amount of cholesterol is 0.5g, the usage amount of oleic acid is 0.3g, the usage amount of water is 10g, the usage amount of hydrogenated lecithin is 10g, and the usage amount of glycerol is correspondingly adjusted to complement the total ingredient mass to 1 kg.

The average particle size of the nano droplets in the skin barrier repair micro-nano emulsion containing camellia oil prepared in the embodiment is 82 nm.

Example 5

The specific preparation procedure was the same as in example 2, except that: the usage amount of the camellia oil is 150g, the usage amount of the ceramide 3 is 5g, the usage amount of the cholesterol is 2g, the usage amount of the oleic acid is 1.5g, the usage amount of the water is 20g, the usage amount of the hydrogenated lecithin is 20g, and the usage amount of the glycerol is correspondingly adjusted to complement the total ingredient mass to 1 kg.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 86 nm.

Example 6

The specific preparation procedure was the same as in example 2, except that: 300g of camellia oil, 30g of ceramide 3, 18g of cholesterol, 12g of oleic acid, 80g of water, 50g of hydrogenated lecithin and 1kg of glycerol which is the total ingredient mass and is correspondingly adjusted.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 131 nm.

Example 7

The specific preparation procedure was the same as in example 2, except that: the using amount of the camellia oil is 500g, the using amount of the ceramide 3 is 50g, the using amount of the cholesterol is 30g, the using amount of the oleic acid is 20g, the using amount of the water is 100g, the using amount of the hydrogenated lecithin is 100g, and the using amount of the glycerol is correspondingly adjusted to complement the total ingredient mass to be 1 kg.

The average particle size of the nano droplets in the camellia oil-containing skin barrier repair micro-nano emulsion prepared in the embodiment is 146 nm.

Comparative examples 1 to 4

The formulations of comparative examples 1-4 are shown in Table 1 below.

Table 1: comparative examples 1-4 ingredient tables.

Ingredients	Comparative example 1	Comparative example 2	Comparative example 3	Comparative example 4
					Glycerol	656g	576g	496g	416g
Water (W)	100g	100g	100g	100g
					Lecithin	50g	50g	50g	50g
Ceramide 2	20g	20g	20g	20g
					Ceramide 3	20g	20g	20g	20g
Palmitic acid	10g	10g	10g	10g
					Linoleic acid	4g	4g	4g	4g
Cholesterol	20g	20g	20g	20g
					Camellia oil	120g	200g	280g	360g
Average particle diameter (nm)	1111	673	117	126

Comparative examples 1-4 the preparation method includes preparation steps consistent with example 3.

Comparative example 5

The ingredients were the same as in example 2, except that: high pressure homogenization was not performed.

The average particle size of the droplets in the emulsion prepared in this comparative example was 2380 nm.

Comparative examples 6 to 8

The ingredients of comparative examples 6-8 are shown in Table 2 below.

Table 2: and 6-8 in the table of ingredients of comparative examples.

Ingredients	Comparative example 6	Comparative example 7	Comparative example 8
				Glycerol	640g	627.5g	622.5g
Water (W)	50g	50g	50g
				Hydrogenated lecithin	40g	40g	40g
Ceramide 3	0g	25g	25g
				Cholesterol	12.5g	0g	12.5g
Oleic acid	7.5g	7.5g	0g
				Camellia oil	250g	250g	250g
Average particle diameter (nm)	98	103	105

Comparative examples 6-8 the preparation method includes preparation steps consistent with example 2.

Comparative example 9

The comparative example comprises the following ingredients:

caprylic capric acid glyceride (250g), ceramide 3(25g), cholesterol (12.5g), oleic acid (7.5g), water (50g), hydrogenated lecithin (40g), glycerol (615 g);

the preparation method of the comparative example is the same as that of example 2, and the camellia oil in the preparation process is replaced by caprylic capric glyceride.

Some of the above examples and comparative examples were tested and compared.

Stability testing and comparison:

the stability investigation method comprises the following steps: the samples were subjected to cold-hot cycling (continuously changing four temperature conditions) at-20 deg.C, 4 deg.C, 25 deg.C, 45 deg.C for 3 months, and the examination was stopped when there was instability.

Comparative test example 3 and comparative examples 1 to 4 the test results are shown in table 3 below.

Table 3: the test results of example 3 are shown in the comparative examples 1 to 4.

The results show that example 3 is superior to comparative examples 1-4 in stability, whereas in comparative example the stability becomes better as camellia oil increases, in comparative example 4 camellia oil: ceramide 9:1, with stratification occurring at 2 months, while camellia oil in example 3: ceramide 10:1 is stable for 3 months. The instability may be caused by ceramide precipitation, and the effect on the skin is weakened after the ceramide precipitation. Thus, to be more efficacious, camellia oil: ceramide is more than or equal to 10: 1.

Comparative test example 2 and comparative example 5 the results are shown in table 4 below.

Table 4: the results of the tests of example 2 and comparative example 5 are shown in the table.

	Example 2	Comparative example 5
			Prepared with an immediate appearance	Homogeneous liquid	Thickening of the discharged oil
Average particle diameter (nm)	108	2380
			Stability of	Is stable for 3 months	Delamination occurred in 7 days

Compared with the comparative example 5, the same proportion and different preparation processes lead to different particle sizes, larger difference of stability and better stability of the nano emulsion, and can be investigated by 3 months of stability. In addition, the lipid particle size is small, the skin permeability is good, and the effect of supplementing skin lipid is good.

The results of the human efficacy evaluation test are shown in table 5 below.

Table 5: and evaluating the test result of human body efficacy.

Sample A, B, C, D, E was prepared according to the above formulation for subsequent testing using example 5.2 for comparison and testing the difference in effect between example 2 and comparative examples 6-9

And (3) testing environment: temperature 20-22 ℃, relative humidity: 40 to 60 percent.

Testing an instrument: MPA4 skin tester, CK, Germany, equipped with a Coneometer and a Tewameter probe.

Testing the population: 18 to 22 years old men and women, 23 to 28 years old men and women, 29 to 36 years old men and women, 37 to 45 years old men and women, 5 46 to 60 years old men and women.

Testing indexes are as follows: skin moisture content MMV value; a transcutaneous water loss TEWL value; skin roughness was self-rated.

The specific test flow is as follows:

1) grouping: grouping according to age groups;

2) establishment of a damaged state: treating left and right forearm of the subject with 1% SDS plaque tester for 24 hr;

3) after removing the spot tester, the subject sits statically for 30min in a standard test environment, the TEWL value surrounding the center of each spot pasting area is measured, each area is measured once, and the measurement result is represented by the average value of the TEWL values of 3 spot pasting areas on a single arm and serves as an initial value;

4) after the initial value is tested, smearing samples on the patch areas, respectively testing different samples by each patch area, reserving one patch area for not testing, and testing TEWL values once in 1h, 4h and 7h respectively for comparison;

5) applying the skin test solution twice every day, testing skin TEWL values of 24h, 48h, 72h, 120h and 168h, flushing a testing area with clear water before each test, waiting for 30 minutes, testing, and scoring the roughness of the skin of a self-spot area by a test subject on the 7 th day;

6) at 168h (day 7), after TEWL was tested, the application of the sample was stopped and skin moisture content MMV values were tested on days 8, 10, 12, 14.

Wherein:

skin barrier repair rate ═ 1- (Tn (TEWL value) -T0(TEWL value))/(T1 (TEWL value) -T0(TEWL value)) in the formula: t0(TEWL value) -TEWL value of intact skin;

t1(TEWL value) -TEWL initial value after barrier disruption;

tn (TEWL value) -TEWL values at different measurement time points.

The results of the skin roughness self-evaluation are shown in table 6 below.

Table 6: skin roughness self-rated results.

As can be seen from table 6 above, the subject considered that the damaged skin became smooth after 7 days of use of sample a (example 2), which was more effective than the other comparative examples.

In addition, the skin barrier repair rate and the skin moisture content are shown in figures 1-8, wherein p is < 0.05 and p is < 0.01. As can be seen from FIGS. 1-4, the skin barrier repair using the composition of the present invention was significantly faster than the other comparative examples within 7 days of testing. As can be seen from FIGS. 5 to 8, the water content of the experimental group using the composition of the present invention is significantly higher than that of the other comparative examples within one week of stopping the use of the sample.

Claims (10)

1. A skin barrier repair micro-nano emulsion containing camellia oil is characterized in that,

the skin barrier repair micro-nano emulsion containing camellia oil comprises the following components in percentage by weight:

10-50 wt% of camellia oil, 0.1-5 wt% of ceramide, 0.05-3 wt% of cholesterol, 0.03-2 wt% of fatty acid, 1-10 wt% of water, 1-10 wt% of phospholipid and the balance of glycerol.

2. The skin barrier repair micro-nano emulsion containing camellia oil as claimed in claim 1,

the skin barrier repair micro-nano emulsion containing camellia oil comprises the following components in percentage by weight:

15-30 wt% of camellia oil, 0.5-3 wt% of ceramide, 0.2-1.8 wt% of cholesterol, 0.15-1.2 wt% of fatty acid, 2-8 wt% of water, 2-5 wt% of phospholipid and the balance of glycerol.

3. The skin barrier repair micro-nano emulsion containing camellia oil as claimed in claim 1 or 2, wherein the mass ratio of the camellia oil to the ceramide is not less than 10: 1.

4. the camellia oil-containing skin barrier repair micro-nano emulsion as claimed in claim 1 or 2, wherein the mass ratio of the ceramide, the cholesterol and the fatty acid is 1: (0.4-0.6): (0.3-0.4).

5. The camellia oil-containing skin barrier repair micro-nano emulsion as claimed in claim 1 or 2, wherein the ceramide is one or a mixture of ceramide 2 and ceramide 3.

6. The camellia oil-containing skin barrier repair micro-nano emulsion as claimed in claim 1 or 2, wherein the content of phosphatidylcholine in the phospholipid is more than or equal to 75 wt%;

the fatty acid is any one or more of palmitic acid, stearic acid, oleic acid and linoleic acid.

7. A method for preparing the skin barrier repair micro-nano emulsion containing camellia oil as claimed in any one of claims 1 to 6,

the preparation method comprises the following preparation steps:

1-a) mixing glycerol and water, adding phospholipid, homogenizing until the phospholipid is uniformly swelled to be used as phase A;

1-B) mixing ceramide, cholesterol, fatty acid and camellia oil, and stirring until solute is completely dissolved to obtain a B phase;

2) mixing the phase A and the phase B, carrying out high-speed homogenization, obtaining a pretreatment solution after the high-speed homogenization, carrying out high-pressure homogenization on the pretreatment solution for a plurality of times, and then discharging and cooling to obtain the skin barrier repair micro-nano emulsion containing camellia oil.

8. The method for preparing skin barrier repair micro-nano emulsion containing camellia oil according to claim 7,

homogenizing at 60-65 deg.c in step 1-a);

and (B) stirring at 75-80 ℃, cooling to 63-65 ℃ after the solute is completely dissolved, and preserving heat to obtain a phase B.

9. The method for preparing skin barrier repair micro-nano emulsion containing camellia oil according to claim 7,

step 2), the high-speed homogenizing rotating speed is 5000-6000 rpm, and the high-speed homogenizing lasts for 5-10 min;

step 2), performing high-pressure homogenization by using a micro-jet high-pressure homogenizer at the homogenization pressure of 200-250 MPa for 3-8 times of circulation;

and 2) discharging and cooling to be less than or equal to 37 ℃ to obtain the skin barrier repair micro-nano emulsion containing camellia oil.

10. The skin barrier repair micro-nano emulsion containing camellia oil as claimed in claim 7,

the average particle size of the skin barrier repair micro-nano emulsion containing camellia oil is 80-150 nm.

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