CN113274331B

CN113274331B - Acne-removing anti-inflammatory composition and preparation method and application thereof

Info

Publication number: CN113274331B
Application number: CN202110692319.5A
Authority: CN
Inventors: 马艺宸; 周秋娜; 金荣熙; 陈欢; 尹锺赫; 金延埈
Original assignee: Cosmax China Cosmetics Co Ltd
Current assignee: Kesimeshi Guangzhou Cosmetics Co ltd; Cosmax China Cosmetics Co Ltd
Priority date: 2021-06-22
Filing date: 2021-06-22
Publication date: 2022-12-13
Anticipated expiration: 2041-06-22
Also published as: CN113274331A

Abstract

The invention discloses an acne-removing and anti-inflammatory composition and a preparation method and application thereof. The acne-removing anti-inflammatory composition comprises an extract of red clover, an extract of bakuchiol and scutellaria baicalensis and a solvent which is acceptable in the field of cosmetics. The red clover extract and the scutellaria baicalensis extract are ethanol extracts of bulk drugs of the red clover and the scutellaria baicalensis respectively; wherein the mass ratio of the bulk drugs of the red clover, the psoralen and the scutellaria baicalensis is (1-5) to (0.01-0.1) to (1-5); the cosmetically acceptable solvent includes polyhydric alcohols. The composition can effectively inhibit acne, improve sebum quality, reduce pores, and effectively improve sebum quality.

Description

Acne-removing anti-inflammatory composition and preparation method and application thereof

Technical Field

The invention belongs to the field of daily chemicals, and relates to an acne-removing anti-inflammatory composition, and a preparation method and application thereof.

Background

Acne is a common skin problem in people, is a series of inflammatory reactions caused by the fact that skin cannot normally excrete grease, is a chronic inflammatory skin symptom generated at the hair follicle sebaceous gland tissue part, and mainly occurs in areas with vigorous sebum secretion, such as faces, breasts, backs and the like.

The causes of acne are complex, usually the result of the combined action of multiple factors, and the main causes are abnormal control of sebaceous glands by androgen, abnormal keratinization of sebaceous gland ducts, excessive reproduction of propionibacterium acnes and inflammatory immune response.

The main component of sebum is squalene, which is a flowing liquid at normal temperature, and when oxidized, the sebum becomes a viscous liquid of linseed oil and is easy to remain in the mouth of a hair follicle to cause blockage. Causing abnormal keratinization of sebaceous gland duct, inducing inflammation, and forming comedo and acne

Acne can lead to decreased confidence, decreased quality of life, depression and even mental disorders in patients. In order to prevent acne and relieve symptoms, the acne patients are easy to have impatience and the patients are in urgent disorder to be hospitalized. For example, some unsafe and inappropriate acne removal products, which may contain keratolytic agents, glucocorticoids, etc., may compromise the integrity of the stratum corneum over time, inhibit stratum corneum lipid synthesis, and cause the skin barrier to be compromised.

The existing acne removing products on the market mainly aim at inhibiting excessive reproduction of propionibacterium acnes and inflammatory immune reaction, neglect improvement of sebum quality and prevention of keratinization abnormality, and have small improvement on the problems of large blackheads and pores and the like.

Disclosure of Invention

The invention aims to provide an acne-removing and anti-inflammatory composition, which solves the problems in the prior art. The acne-removing anti-inflammatory composition has the advantages of effectively inhibiting acne, improving the quality of sebum, reducing pores and further providing the application of the acne-removing anti-inflammatory composition in cosmetics. Through extensive and intensive research, the composition effectively inhibits acne and simultaneously improves the sebum quality, the pore is large and the like by selecting the red clover extract, the bakuchiol and the scutellaria baicalensis extract.

The invention provides an acne-removing and anti-inflammatory composition, which comprises an red clover extract, a psoralea phenol extract, a scutellaria extract and a solvent acceptable in the field of cosmetics; the red clover extract and the scutellaria baicalensis extract are ethanol extracts of bulk drugs of the red clover and the scutellaria baicalensis respectively; wherein the mass ratio of the bulk drugs of the red clover, the psoralen and the scutellaria baicalensis is (1-5) to (0.01-0.1) to (1-5); the cosmetically acceptable solvent includes polyhydric alcohols; the polyalcohol comprises one or more of 1, 3-butanediol, 1, 2-propylene glycol, dipropylene glycol and glycerol.

Preferably, the mass ratio of the raw material medicines of the red clover, namely the bakuchiol to the raw material medicine of the scutellaria baicalensis is (1-3) to (0.01-0.05) to (1-3), and the mass ratio is preferably 3; the polyol is 1, 2-propylene glycol and 70% glycerol with the mass fraction of 30%.

In certain embodiments, the composition is extracted and prepared by the following steps:

1) Pulverizing herba Trifolii Pratentis and Scutellariae radix respectively, drying, sieving, weighing at a certain ratio, and mixing;

2) Adding ethanol, extracting for 1-3 times at 45-60 deg.C, and collecting extractive solution;

3) Cooling the extracting solution obtained in the step 2) to 20-30 ℃, and filtering to obtain primary filtrate;

4) Centrifuging the primary filtrate obtained in the step 3), and filtering to obtain secondary filtrate;

5) And (4) concentrating the secondary filtrate obtained in the step 4) under reduced pressure to obtain an extract. Adding bakuchiol according to a certain proportion, adding polyalcohol, mixing uniformly, and filtering to obtain the composition.

Preferably, the drying in step 1) is low-temperature drying, including but not limited to one or two of oven drying, freeze drying and vacuum drying.

Preferably, in the step 2, the mass ratio of the raw materials of the red clover and the scutellaria baicalensis to the ethanol is 1 to 10-1, and the extraction method is microwave and ultrasonic combined use; the microwave time is 5-10min, and the ultrasonic time is 30-50min.

Preferably, the centrifugation in the step 4) is carried out for 20-60min, and the rotating speed is 5000-10000rpm.

Preferably, in the step 5), the source of the bakuchiol is obtained by extracting traditional Chinese medicine fructus psoraleae or vernonia elm root, and the adding amount of the polyalcohol is 1-10 times of the mass of the extract.

The bakuchiol can be extracted by conventional method, or directly extracted from natural Chinese medicinal fructus Psoraleae or radix Ulmi Pumilae.

Preferably, the step 1) is carried out by sieving with a 60-mesh sieve; filtering by using gauze of 100-200 meshes in the step 3); filtering by using a microfiltration membrane with the diameter of 0.5 mu m in the step 4); filtering by using a 0.5 mu m microfiltration membrane in the step 5); the mass fraction of the ethanol is 30-70%, and more preferably 35%.

The present invention also provides a cosmetic comprising a composition according to any one of claims 1 to 8; the cosmetics include, but are not limited to, water aqua, emulsion, spray, cream, mask, foundation, facial cleanser, shampoo. The application has the following beneficial effects: the pratense, the bakuchiol and the scutellaria baicalensis are natural sources, can inhibit acne in multiple ways and improve acne muscles, are synergistic in components, green and safe, and can effectively inhibit acne and reduce lipid peroxidation, improve sebum quality, and cause coarse pores.

Drawings

FIG. 1 is a photograph of a part of a volunteer in Experimental example 5 before and after treatment;

FIG. 2 is a photograph showing a part of a volunteer in Experimental example 5 before and after treatment.

Detailed Description

Embodiments of the present application will be described in detail by examples, so that how to apply technical means to solve technical problems and achieve technical effects of the present application can be fully understood and implemented.

The raw materials and equipment used in the present application are all common raw materials and equipment in the field, and are all from commercially available products, unless otherwise specified. The methods used in this application are conventional in the art unless otherwise indicated.

There are many other possible implementations that may be made, which are not listed here, and the implementations that are claimed in the claims of this application may be made.

Examples

In the following examples and comparative examples of the present invention, the anti-itch soothing composition was prepared by the following procedure.

(1) Respectively crushing the plant raw material medicines, drying, sieving by a 60-mesh sieve, weighing according to the proportion, and uniformly mixing;

(2) Adding ethanol for extraction, wherein the mass ratio of the raw material medicines to the ethanol (35%) is 1;

(3) Cooling the extracting solution obtained in the step (2) to 25 ℃, and filtering with 200-mesh gauze to obtain primary filtrate;

(4) Centrifuging the primary filtrate obtained in the step (3) for 30min at the rotating speed of 6000rpm by using a microfiltration membrane with the pore diameter of 0.5 mu m, and collecting filtrate to obtain secondary filtrate;

(5) Concentrating the secondary filtrate obtained in the step (4) under reduced pressure to obtain extract, adding bakuchiol according to the proportion, adding polyalcohol, and stirring or ultrasonically mixing; filtering with a microfiltration membrane with the pore diameter of 0.5 mu m to obtain the composition.

In the secondary filtrate obtained in the step (5), the addition amount of the polyhydric alcohol is 5 times of the extract, the mass composition of the polyhydric alcohol is 30 percent of 1, 2-propylene glycol and 70 percent of glycerol, and the source of the bakuchiol is obtained by extracting the traditional Chinese medicine fructus psoraleae;

compositions 1-15 and comparative examples 1-3, the above-mentioned method was used to prepare each of the extract compositions 1-15 according to the proportions in Table 1, and the compositions obtained according to the proportions were tested for bacteriostasis, oxidation resistance, safety, etc. according to the following methods.

TABLE 1 compositions and comparative example formulations

The Chinese medicine red clover belongs to the plant of clover of leguminosae, is a herb plant grown for one year or more, is distributed all over the world, has wide coverage area, and is a famous covering plant in the world. The collagen protein has rich resources, mainly contains chemical components such as isoflavone, flavone, coumarins, saponin, stigmasterol and the like, can effectively remove superoxide anions and hydroxyl free radicals, protects DNA from oxidative damage, has good activity in the aspect of estrogen-like action of isoflavone substances, has the effects of preventing skin aging and wrinkles, and effectively reinforces collagen protein around hair.

Bakuchiol is a procylated phenol monoterpene compound extracted from fruit of Psoralea corylifolia of Leguminosae. Has various pharmacological effects including antioxidant, antibacterial, antiinflammatory, antiaging and estrogen-like effects. And can effectively slow down skin aging by preserving skin collagen.

Scutellaria baicalensis is a plant used as a perennial crude drug in Labiatae, contains effective components such as wogonin, wogonoside, baicalein and the like, and has good effects of resisting inflammation, resisting bacteria, resisting oxidation and the like. The research finds that the baicalin can weaken the activity of sebaceous glands by inhibiting the activity excitation and sebum secretion of the sebaceous glands, reducing the expression of androgen receptor mRNA of sebaceous gland cells and inhibiting the level of androgen. And can inhibit arachidonic acid pathway through different ways, inhibit NO, histamine and other molecules from forming, and has remarkable anti-allergic and anti-inflammatory effects.

The extracts are all natural herbal medicines, act on the skin through multiple paths, have synergistic effect of all the components, are green and safe, and can effectively inhibit acne, reduce lipid peroxidation, improve the quality of sebum, enlarge pores and the like through scientific proportioning

Experimental example 1

Bacteriostatic test

Detection of bacteriostatic effects

Selecting strains: staphylococcus aureus, escherichia coli, pseudomonas aeruginosa, propionibacterium acnes; the preparation of the bacterial liquid selects pseudomonas aeruginosa, staphylococcus aureus, escherichia coli and propionibacterium acnes as the listed strains. Preparation: the bacteria are diluted to about 1.0x105cfu/ml to 1.0x106cfu/ml by using sterile physiological saline. The prepared bacterial suspension can be used within 2h, or can be stored at 2-8 ℃ for no more than 24h.

And (3) detecting the antibacterial effect: the functional plant composition obtained in the step (5) of example was taken, and 20. Mu.L of a plant composition solution (10 mg/mL) at an actual use concentration was added dropwise to each of sterile dried filter paper sheets. Test bacterium inoculation: taking 1mL of each test bacterial suspension, and uniformly smearing the test bacterial suspension on the surface of a nutrient agar culture medium; the bacteriostatic test samples are attached, one bacterial staining flat plate is attached to each test, 4 filter paper sheets are attached to each dish, 3 filter paper sheets are test sample sheets, and 1 filter paper sheet is blank. And (3) sticking a sterile forceps sampling piece on the surface of the flat plate, placing the flat plate in a constant-temperature incubator at 36 +/-1 ℃, observing the result after culturing for 18 hours, and measuring the diameter of the antibacterial ring by using a vernier caliper. The results are the average of 3 measurements.

The experimental results are as follows: the results are shown in Table 2, and when compositions 1-15 are compared to comparative examples 1-3, it was found that:

1) The bacteriostatic activity of the plant compound combination is superior to that of a single plant;

2) The antibacterial activity of the plant compound combination is different according to different mass ratios, preferably, the antibacterial activity of the red clover is Bavacrol: scutellaria baicalensis = (1-3): (0.01-0.05): (1-3), more preferably, the antibacterial activity of the red clover is Bavacrol: scutellaria baicalensis = 3.

TABLE 2 compositions 1-15 and comparative examples 1-3 bacteriostatic effect

Experimental example 2 in vitro antioxidant assay

DPPH radical scavenging test

Precisely transferring 2.0mL of 50% ethanol DPPH solution (0.2 mmol/L), adding 2.0mL of test solution, mixing, shaking thoroughly, measuring absorbance A at 517nm after 30min, performing parallel measurement for 3 times, and taking the average value with vitamin C as positive control. The DPPH free radical clearance rate of each test solution is calculated according to the following formula:

DPPH clearance (%) = [1- (a) _i -A _j )/A ₀ ]*100％

In the formula: ai is the absorbance of the reaction after the test substance is added;

aj is the absorbance of the test solution;

a0 is a blank value without test solution.

OH free radical scavenging test

Hydroxyl radicals are generated by Fenton reaction. Adding 1.0mL of FeSO4 solution (9.0 mmol/L), 1.0mL of salicylic acid ethanol solution (9.0 mmol/L) and 1.0mL of test solution in sequence, mixing, shaking thoroughly, adding 1.0mL of H2O2 solution (8.8 mmol/L), reacting at 37 deg.C for 30min, measuring absorbance A at 510nm, parallel measuring for 3 times, taking the average value, and using vitamin C as positive control. The removal rate of OH free radicals by each test solution is calculated according to the following formula:

OH clearance (%) = (a) ₀ -A _X -A _X0 )/A ₀ *100％

In the formula: a0 is the absorbance of the blank control solution;

AX is the absorbance of the reaction after the test solution is added;

AX0 is the absorbance of the test substance without H2O 2.

3.O _2- Free radical scavenging test

4.0mL of Tris-HCl buffer (pH 8.2, 50.0 mmol/L) was added to 1.0mL of the test solution, and the mixture was incubated in a water bath at 25 ℃ for 10min. Adding 0.1mL pyrogallol solution (25.0 mmol/L), mixing, shaking thoroughly, keeping temperature for 5min, adding dropwise hydrochloric acid solution (10.0 mmol/L) to terminate reaction, measuring absorbance A at 325nm, and measuring for 3 times. Vitamin C was used as a positive control.

The clearance rate of each test solution to O2-free radicals is calculated according to the following formula:

O _2- clearance (%) = [ a ₀ -(A ₁ -A ₂ )]/A ₀ *100％

In the formula: a0 is the absorbance of the blank control solution;

a1 is the absorbance of the reaction after adding the test solution;

a2 is the absorbance of the test solution without pyrogallol.

The concentrations of vitamin C and each composition are the same and are 0.1mg/ml, five parallel experiments are carried out on data each time, the results are averaged, and three groups of test results are shown in a table 3.

Table 3: free radical scavenging experiments

The test results show that each composition treatment group has more excellent capability of scavenging DPPH free radicals, hydroxyl free radicals and superoxide anion free radicals compared with a vitamin C positive control group, and is better than a single-component test group, wherein the composition 7 group and the composition 13 group have the best effect.

EXAMPLE 3 safety Patch test

Dripping 20 mu L of liquid to be detected into the spot tester, wherein a blank control hole is used as a blank control (pure water); the spot tester with the tested object is attached to the bent side of the forearm of the tested person, and the tested person is lightly pressed by the palm to be uniformly attached to the skin for 24 hours; the skin irritation and sensitization were observed as in table 4 after 30min, 24 hours, and 48 hours, respectively, after removal of the test article plaque test device, and the observation results were recorded. Skin closed patch test skin response grading criteria are shown in table 4.

TABLE 4

The experimental results are as follows: compositions 7, 13 were formulated as 2% aqueous solutions for human skin patch testing and the results are shown in table 5. The result of the skin patch test of the human body shows that 20 people have no adverse reaction to the skin.

TABLE 5

Experimental example 4

40 vaccinia muscle volunteers were selected and randomly divided into four groups of 10 individuals each. The evaluation was performed using a normal moisturizing mask to which an active substance was added in an amount of 2% by mass, respectively.

The subject cleans the face every night, applies the face mask on the face, stays for 15-20min and then takes off.

The anti-acne effect of the product was evaluated by photographs taken at week 0, week 2, and week 4 using Antera 3D (Miravex, ireland) and self-rated.

The results of the self-evaluation are shown in Table 6, and photographs of a portion of composition 13 before and after treatment were obtained using Antera 3D, see in particular FIGS. 1 and 2.

FIGS. 1 and 2 are graphs showing the changes of the composition 13 in different parts of the same volunteer at 0w, 2w and 4w, respectively.

The composition provided by the application has a good long-term inhibition effect on the pox, and can smooth the skin and fade the pox marks.

Table 6:4w acne removing effect self-evaluation table

The content not described in detail in the specification of the present application belongs to the common general knowledge of those skilled in the art.

In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect.

It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrases "comprising one of \8230;" does not exclude the presence of additional like elements in an article or system comprising the element.

The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.

Claims

1. The acne-removing and anti-inflammatory composition is characterized by comprising an extract of red clover, an extract of psoralea fruit phenol, an extract of scutellaria baicalensis and a solvent acceptable in the field of cosmetics; the red clover extract and the scutellaria baicalensis extract are respectively ethanol extracts of the raw material medicines of the red clover and the scutellaria baicalensis; wherein, the mass ratio of the raw material medicines of the red clover, the bakuchiol and the raw material medicines of the scutellaria baicalensis is 3; the cosmetically acceptable solvent includes polyhydric alcohols; the polyol comprises 30 mass percent of 1, 2-propylene glycol and 70 mass percent of glycerol.

2. The composition of claim 1, which is extracted and prepared by the following steps:

5) Concentrating the secondary filtrate obtained in step 4) under reduced pressure to obtain extract, adding bakuchiol according to a proportion, adding polyalcohol, mixing well, and filtering to obtain the composition.

3. The composition of claim 2, wherein the drying of step 1) is a low temperature drying.

4. The composition of claim 2, wherein the drying of step 1) is selected from one or a combination of oven drying, freeze drying, and vacuum drying.

5. The composition of claim 2, wherein in the step 2), the mass ratio of the raw material medicines of the red clover and the scutellaria baicalensis to the ethanol is 1; the microwave time is 5-10min, and the ultrasonic time is 30-50min.

6. The composition of claim 2, wherein the centrifugation in step 4) is performed for 20 to 60min at 5000 to 10000rpm.

7. The composition of claim 2, wherein the source of bakuchiol in step 5) is obtained by extracting fructus Psoraleae or radix Ulmi Pumilae, and the amount of the polyalcohol is 1-10 times of the mass of the extract.

8. The composition of claim 2, wherein step 1) is performed with a 60 mesh screen; filtering by using gauze of 100-200 meshes in the step 3); filtering by using a 0.5 mu m microfiltration membrane in the step 4); filtering by using a 0.5 mu m microfiltration membrane in the step 5); the mass fraction of the ethanol is 30-70%.

9. The composition according to claim 8, wherein the ethanol is present in a mass fraction of 35%.

10. A cosmetic comprising a composition according to any one of claims 1 to 9.

11. The cosmetic of claim 10, wherein said cosmetic is selected from the group consisting of lotions, creams, sprays, creams, masks, foundations, facial washes, shampoos.