CN115350126B - Mild salicylic acid-containing composition with oil control and acne removal effects and application thereof - Google Patents
Mild salicylic acid-containing composition with oil control and acne removal effects and application thereof Download PDFInfo
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- CN115350126B CN115350126B CN202211014572.6A CN202211014572A CN115350126B CN 115350126 B CN115350126 B CN 115350126B CN 202211014572 A CN202211014572 A CN 202211014572A CN 115350126 B CN115350126 B CN 115350126B
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Abstract
The invention discloses a salicylic acid-containing mild composition with oil control and acne removal effects and application thereof, wherein the salicylic acid-containing mild composition comprises the following components in parts by weight: 5-15 parts of willow bark extract, 2-7 parts of radix sophorae flavescentis extract, 1-10 parts of wisense GSS, 1-8 parts of polyalcohol, 3-8 parts of persimmon leaf extract, 1-6 parts of thyme extract, 1-5 parts of rheum officinale extract, 1-7 parts of flaxseed extract and 2-8 parts of antimicrobial peptide freeze-dried powder. The invention aims to provide a composition which is mild and has synergistic ingredients and special effects on controlling oil and recovering damaged acne muscle skin barriers, and can be used for synergistic killing of gram-positive bacteria, especially killing of propionibacterium acnes and inhibition of reproduction of propionibacterium acnes.
Description
Technical Field
The invention belongs to the technical field of cosmetics, relates to a composition containing salicylic acid and having the effects of controlling oil and removing acnes, and further relates to application of the composition containing salicylic acid and having the effects of controlling oil and removing acnes in cosmetics.
Background
Modern women pay great attention to skin care, however, acne-like skin disorders are a major problem that has long plagued the general population. Acne, blackhead, whitehead, red pox, dark pox, acne and pigmentation, acne marks, acne pits, nodules, scars and the like generated by the acne, blackhead, whitehead, red pox, dark pox and acne seriously affect the psychological of a patient. The data show that the skin diseases of acnes are the most serious of the young and young sexual diseases, and cause psychological disorder to partial psychologically fragile people and have serious influence on later life, work and the like.
Acne is commonly called as acne, is a chronic inflammatory skin disease of a pilo-sebaceous gland unit, and can be suffered from various age groups, and the incidence rate of teenagers is high. The incidence rate of acne has three parts, firstly, the epidermis of the skin shows a vigorous state, and the oil absorption towel is used for wiping the surface of the skin, so that the oil absorption towel can clearly observe that a lot of grease is adsorbed; then, if left uncontrolled, the vigorous secretory state will continue and decrease gradually (in fact as a result of the occlusion of the follicle), with the appearance of sores or acne on the skin; if the interference is not carried out continuously, the acne is gradually developed into white, and the blackheads are further developed into various acnes along with the interference of external factors such as air sunlight and the like. At this time, microorganisms such as propionibacterium acnes can be detected at the acne sites without treatment, and finally, acne is developed thoroughly.
From the acne formation step, it can be seen that oil control is the first step of skin care on normal skin, especially oily skin or skin with vigorous secretion, and effectively terminates or controls skin oil secretion, which is the basis for maintaining normal physiological functions of skin. Second, the formation of acne or pimples is a result of the obstruction of the drainage of the follicular duct, which is an impermeable, blocked follicular duct, and tends to fail to prevent the formation of acne or comedones. The most critical step for normal skin not to form acne is not to block pores. Finally, once acne has formed, it is essential for symptomatic treatment, especially for the killing of microorganisms such as propionibacterium acnes.
The acne-removing cosmetics sold on the market at present mainly do so according to the mechanism: among them, salicylic acid is the most critical component in cosmetics for treating acne and the like, because salicylic acid has a definite medical effect of blocking follicular ducts through. Currently, salicylic acid is added to a formulation in mainly two forms, one in the form of salicylate and the other in the form of molecules. The pH of the formulation is generally above 5, while the optimal pH for salicylic acid treatment is below 4, and preferably 3. Salicylic acid is an oil-soluble substance that is hardly dissolved in water. Due to this property, salicylic acid molecules can penetrate the epidermis of the skin, rather than stay on the surface of the skin, thus acting accordingly. The form of salicylic acid molecules present in the aqueous solution is particularly important. That is, salicylic acid exists in molecular form in the formula to treat acne. The solvent is alcohol. Alcohol, in turn, has the following pain points during acne treatment: 1) When the formula containing alcohol is applied to the acne wound, the acne wound is more irritated, and the pain is obvious and intolerable; 2) Alcohol can stimulate skin hyperkeratinization, so that skin is easy to leave damage and tolerance symptoms such as pigmentation, acne marks, acne pits, nodules, scars and the like; 3) The optimal treatment time for acne is delayed. Therefore, it is very important and necessary to develop an effective composition for the skin of acne, which can remove acne and prevent the loss of the symptoms, for use in cosmetics.
Disclosure of Invention
The invention aims to provide a salicylic acid composition with the effects of controlling oil and removing acnes, which has the characteristics of water solubility, lower pH value and low temperature, can effectively control oil, permeate and block hair follicle ducts, does not leave damage to the capacitive symptoms and can kill microorganisms such as propionibacterium acnes.
The invention further aims to provide an application of the salicylic acid-containing mild composition with the effects of controlling oil and removing acnes in cosmetics, and the problems of excessive secretion of skin grease, hair follicle blockage, acne mark and acne are solved.
The invention adopts the technical scheme that the salicylic acid-containing mild composition with the effects of controlling oil and removing acne comprises the following components in parts by weight: 5-15 parts of willow bark extract, 2-7 parts of radix sophorae flavescentis extract, 1-10 parts of wisense GSS, 1-8 parts of polyalcohol, 3-8 parts of persimmon leaf extract and 1-6 parts of thyme extract.
The technical proposal of the invention is also characterized in that,
also comprises 1 to 5 parts of rheum officinale extract and 1 to 7 parts of flaxseed extract.
Also comprises 2 to 8 parts of antibacterial peptide freeze-dried powder.
7-12 parts of willow bark extract, 3-6 parts of radix sophorae flavescentis extract, 4-8 parts of wisense GSS, 2-6 parts of polyalcohol, 4-7 parts of persimmon leaf extract and 2-5 parts of thyme extract.
8-11 parts of willow bark extract, 4-5 parts of radix sophorae flavescentis extract, 5-7 parts of wisense GSS, 3-5 parts of polyalcohol, 5-6 parts of persimmon leaf extract, 3-4 parts of thyme extract, 2-4 parts of rheum officinale extract and 3-6 parts of flaxseed extract.
8-11 parts of willow bark extract, 4-5 parts of radix sophorae flavescentis extract, 5-7 parts of wisense GSS, 3-5 parts of polyalcohol, 5-6 parts of persimmon leaf extract, 3-4 parts of thyme extract, 2-4 parts of rheum officinale extract, 3-6 parts of flaxseed extract and 4-7 parts of antibacterial peptide freeze-dried powder.
The Wisence GSS comprises the following components in percentage by mass: 40% of salicylic acid, 40% of PEG-15 cocoamine and 20% of stearamidopropyl dimethylamine.
The other technical scheme adopted by the invention is the application of the composition which is mild and has the effects of controlling oil and removing acne and contains salicylic acid in cosmetics.
The invention has the advantages that,
(1) The rheum officinale extract, the flaxseed extract and the willow bark extract, the kuh-seng extract, the wisense GSS, the polyalcohol, the persimmon leaf extract and the thyme extract are used together to realize synergistic effect, so that the retention time of the willow bark extract, the kuh-seng extract, the wisense GSS, the polyalcohol, the persimmon leaf extract and the thyme extract on skin delivery is prolonged, the composition has special effects of controlling oil, removing acnes, restoring damaged acne skin barriers and synergistic effect and killing gram positive bacteria, particularly has special effects of killing and inhibiting propionibacterium acnes and inhibiting reproduction of propionibacterium acnes, realizes the effect of 1+1 & gt2, can be used for treating I-III type acne, has no acne mark, has better effect on IV level and has lower irritation;
(2) The antibacterial peptide freeze-dried powder in the composition can neutralize acid stimulation of certain salicylic acid, and the addition of other extracts can increase the solubility of the antibacterial peptide in water under the condition of not changing the action mechanism of the antibacterial peptide freeze-dried powder, can play a role in sterilizing and inhibiting bacteria at extremely low concentration, can synergize and kill gram positive bacteria, has the effect of killing partial viruses, fungi, protozoa, cancer cells and the like, can even improve the immunity and accelerate the wound healing process, and is an indispensable step in anti-inflammatory, antibacterial and wound healing processes in the acne removing process, so that the antibacterial peptide freeze-dried powder is also an indispensable component in the components.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention provides a salicylic acid-containing mild composition with oil control and acne removal effects, which comprises the following components in parts by weight: 5-15 parts of willow bark extract, 2-7 parts of radix sophorae flavescentis extract, 1-10 parts of wisense GSS, 1-8 parts of polyalcohol, 3-8 parts of persimmon leaf extract and 1-6 parts of thyme extract.
Also comprises 1 to 5 parts of rheum officinale extract and 1 to 7 parts of flaxseed extract.
The antibacterial peptide freeze-dried powder also comprises 2-8 parts of antibacterial peptide freeze-dried powder, wherein the antibacterial peptide freeze-dried powder is an active antibacterial peptide, comprises small peptides such as lysozyme, nisin and the like, can neutralize certain acid stimulation of salicylic acid, and can increase the solubility of the antibacterial peptide in water under the condition of not changing the action mechanism of the antibacterial peptide freeze-dried powder, can play a role in sterilizing and inhibiting bacteria at extremely low concentration, and can synergize and kill gram-positive bacteria.
Further, the composite material comprises the following components in parts by weight: 7-12 parts of willow bark extract, 3-6 parts of radix sophorae flavescentis extract, 4-8 parts of wisense GSS, 2-6 parts of polyalcohol, 4-7 parts of persimmon leaf extract and 2-5 parts of thyme extract.
Further, the composite material comprises the following components in parts by weight: 8-11 parts of willow bark extract, 4-5 parts of radix sophorae flavescentis extract, 5-7 parts of wisense GSS, 3-5 parts of polyalcohol, 5-6 parts of persimmon leaf extract, 3-4 parts of thyme extract, 2-4 parts of rheum officinale extract and 3-6 parts of flaxseed extract.
Further, 8-11 parts of willow bark extract, 4-5 parts of radix sophorae flavescentis extract, 5-7 parts of wisense GSS, 3-5 parts of polyalcohol, 5-6 parts of persimmon leaf extract, 3-4 parts of thyme extract, 2-4 parts of rheum officinale extract, 3-6 parts of flaxseed extract and 4-7 parts of antibacterial peptide freeze-dried powder.
The components involved in the composition are purchased through commercial channels, wherein willow bark extract, thyme extract, kuh-seng extract and persimmon leaf extract are purchased from Huzhou Jiamei biochemical products limited, polyalcohol is purchased from Shanghai Zhen trade limited, rhubarb extract is purchased from Nanjing doffer biotechnology limited, antibacterial peptide freeze-dried powder is purchased from Shanxi Huikang biotechnology limited, wisence GSS and linseed extract are purchased from Shanghai Rui Rhinoceros trade limited.
The invention relates to a preparation method of a composition which contains salicylic acid and has the effects of controlling oil and removing acnes, which is prepared by weighing the components in parts by weight and stirring and mixing the components at normal temperature.
The invention provides an application of a composition which is mild and has the effects of controlling oil and removing acne and contains salicylic acid in cosmetics, wherein the addition amount of the composition is 0.5-8.0% of the total mass of the cosmetics.
The Wisence GSS in the composition of the invention comprises 40% salicylic acid, 40% PEG-15 cocoamine and 20% stearamidopropyl dimethylamine. The polyalcohol is polyhydroxy-containing alcohols, generally refers to water-soluble alcohols such as propylene glycol, 1, 3-propylene glycol, methyl propylene glycol, 1, 3-butanediol, 1, 2-butanediol, pentanediol, glycerol and the like, and the polyalcohol is synergistic with PEG-15 cocoamine and stearamidopropyl dimethylamine in the Wisence GSS to form intermolecular hydrogen bonds, so that hydration of salicylic acid in the Wisence GSS can be well increased, and dissolution of salicylic acid in water is enhanced; the main component of the willow bark extract is salicin, the salicin is a polymer of salicylic acid and glycosyl units, and can be slowly hydrolyzed into salicylic acid and saccharides in the presence of polyalcohol and Wisence GSS, and forms dynamic balance with the salicylic acid in the Wisence GSS. The three have obvious pharmacological effects, and the inhibition test result on propionibacterium acnes is as follows: the original bacterial count of 1×108, the bacterial count remained after 1h culture after 1.3×104 and 2.3×103 respectively after 1.0% and 2.0% of extract is added respectively, and the inhibition data show that it has powerful elimination performance on propionibacterium acnes and can be used for preventing and treating acnes. The kuh-seng extract has the functions of anti-inflammatory, bacteriostasis, nourishing and the like, which is very critical for treating acne. The kuh-seng extract has strong antibacterial activity, and the MIC (minimum inhibitory concentration) of the kuh-seng extract on gram-positive bacteria is 25-50 ng/mL (Propionibacterium acnes is the gram-positive bacteria). The matrine (prepared by extracting dried roots, plants and fruits of kuh-seng with organic solvents such as ethanol) has strong inhibition effect on acne bacteria, and the result shows that the matrine has a minimum inhibitory concentration of 10mg/L but has weak bactericidal effect. But can be significantly improved by the addition of persimmon leaf extract and thyme extract. This is because both activate the cathepsins (cathepsins are associated with inflammation of the skin, and low cathepsins indicate skin inflammation), thereby improving its bactericidal effect. The composition can provide skin balance and control grease secretion by cooperating with other components, condition the skin to a balance state, permeate and block follicular ducts, kill microorganisms such as propionibacterium acnes and the like, and leave no acne marks, thereby effectively realizing the effects of controlling oil, removing acnes and the like.
Example 1
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 5 parts of willow bark extract, 2 parts of radix sophorae flavescentis extract, 1 part of wisense GSS, 1 part of polyalcohol, 3 parts of persimmon leaf extract and 1 part of thyme extract.
The invention provides a preparation method of a salicylic acid-containing mild composition with oil control and acne removal effects, which comprises the following steps of weighing the components in parts by weight, and stirring and mixing at normal temperature.
Example 2
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 5 parts of willow bark extract, 2 parts of radix sophorae flavescentis extract, 1 part of wisense GSS, 1 part of polyalcohol, 3 parts of persimmon leaf extract and 1 part of thyme extract.
The preparation method according to this example is the same as that of example 1.
Example 3
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 9 parts of willow bark extract, 5 parts of radix sophorae flavescentis extract, 6 parts of wisense GSS, 5 parts of polyalcohol, 6 parts of persimmon leaf extract and 4 parts of thyme extract.
The preparation method according to this example is the same as that of example 1.
Example 4
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 12 parts of willow bark extract, 6 parts of radix sophorae flavescentis extract, 8 parts of wisense GSS, 6 parts of polyalcohol, 7 parts of persimmon leaf extract and 5 parts of thyme extract.
The preparation method according to this example is the same as that of example 1.
Example 5
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 15 parts of willow bark extract, 7 parts of radix sophorae flavescentis extract, 10 parts of wisense GSS, 8 parts of polyalcohol, 8 parts of persimmon leaf extract and 6 parts of thyme extract.
The preparation method according to this example is the same as that of example 1.
Example 6
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 5 parts of willow bark extract, 2 parts of radix sophorae flavescentis extract, 1 part of wisense GSS, 1 part of polyalcohol, 3 parts of persimmon leaf extract, 1 part of thyme extract, 1 part of rheum officinale extract and 1 part of flaxseed extract.
The preparation method according to this example is the same as that of example 1.
Example 7
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 8 parts of willow bark extract, 4 parts of radix sophorae flavescentis extract, 5 parts of wisense GSS, 3 parts of polyalcohol, 5 parts of persimmon leaf extract, 3 parts of thyme extract, 2 parts of rheum officinale extract and 3 parts of flaxseed extract.
The preparation method according to this example is the same as that of example 1.
Example 8
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 11 parts of willow bark extract, 5 parts of radix sophorae flavescentis extract, 7 parts of wisense GSS, 5 parts of polyalcohol, 6 parts of persimmon leaf extract, 4 parts of thyme extract, 4 parts of rheum officinale extract and 6 parts of flaxseed extract.
The preparation method according to this example is the same as that of example 1.
Example 9
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 15 parts of willow bark extract, 7 parts of radix sophorae flavescentis extract, 10 parts of wisense GSS, 8 parts of polyalcohol, 8 parts of persimmon leaf extract, 6 parts of thyme extract, 5 parts of rheum officinale extract and 7 parts of flaxseed extract.
The preparation method according to this example is the same as that of example 1.
Example 10
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 5 parts of willow bark extract, 2 parts of radix sophorae flavescentis extract, 1 part of wisense GSS, 1 part of polyalcohol, 3 parts of persimmon leaf extract, 1 part of thyme extract and 2 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 11
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 11 parts of willow bark extract, 5 parts of radix sophorae flavescentis extract, 7 parts of wisense GSS, 5 parts of polyalcohol, 8 parts of persimmon leaf extract, 4 parts of thyme extract and 7 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 12
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 15 parts of willow bark extract, 7 parts of radix sophorae flavescentis extract, 10 parts of wisense GSS, 8 parts of polyalcohol, 8 parts of persimmon leaf extract, 6 parts of thyme extract and 8 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 13
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 5 parts of willow bark extract, 2 parts of radix sophorae flavescentis extract, 1 part of wisense GSS, 1 part of polyalcohol, 3 parts of persimmon leaf extract, 1 part of thyme extract, 1 part of rheum officinale extract, 1 part of flaxseed extract and 2 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 14
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 8 parts of willow bark extract, 4 parts of radix sophorae flavescentis extract, 5 parts of wisense GSS, 3 parts of polyalcohol, 5 parts of persimmon leaf extract, 3 parts of thyme extract, 2 parts of rheum officinale extract, 3 parts of flaxseed extract and 4 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 15
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 11 parts of willow bark extract, 5 parts of radix sophorae flavescentis extract, 5 parts of wisense GSS, 7 parts of polyalcohol, 6 parts of persimmon leaf extract, 4 parts of thyme extract, 4 parts of rheum officinale extract, 6 parts of flaxseed extract and 7 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Example 16
The invention discloses a composition containing salicylic acid and having the effects of controlling oil and removing acnes, which comprises the following components in parts by weight: 15 parts of willow bark extract, 7 parts of radix sophorae flavescentis extract, 10 parts of wisense GSS, 8 parts of polyalcohol, 8 parts of persimmon leaf extract, 6 parts of thyme extract, 5 parts of rheum officinale extract, 7 parts of flaxseed extract and 8 parts of antibacterial peptide freeze-dried powder.
The preparation method according to this example is the same as that of example 1.
Comparative experiments were also performed in this application, the specific comparative examples are as follows:
comparative example 1
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 8 parts of willow bark extract, 5 parts of wisense GSS and 5 parts of persimmon leaf extract.
The comparative example involved the same preparation as in example 1.
Comparative example 2
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 4 parts of kuh-seng extract, 3 parts of polyalcohol and 3 parts of thyme extract.
The comparative example involved the same preparation as in example 1.
Comparative example 3
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 8 parts of willow bark extract, 5 parts of wisense GSS, 5 parts of persimmon leaf extract and 2 parts of rheum officinale extract.
The comparative example involved the same preparation as in example 1.
Comparative example 4
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 4 parts of kuh-seng extract, 3 parts of polyalcohol, 3 parts of thyme extract and 3 parts of flaxseed extract.
The comparative example involved the same preparation as in example 1.
Comparative example 5
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 8 parts of willow bark extract, 5 parts of wisense GSS, 5 parts of persimmon leaf extract, 2 parts of rheum officinale extract and 4 parts of antibacterial peptide freeze-dried powder.
The comparative example involved the same preparation as in example 1.
Comparative example 6
The composition containing salicylic acid and having the effects of controlling oil and removing acne comprises the following components in parts by weight: 4 parts of kuh-seng extract, 3 parts of polyalcohol, 3 parts of thyme extract, 3 parts of flaxseed extract and 4 parts of antibacterial peptide freeze-dried powder.
The comparative example involved the same preparation as in example 1.
To verify the beneficial effects of the present invention, experiments were conducted on examples 1 to 16 and comparative examples 1 to 6, and the experimental data are specifically as follows:
1. stability test
Cosmetics were prepared according to the composition of examples 1 to 16 and comparative examples 1 to 6, respectively, and their stability was examined, and the results are shown in tables 1.1, 1.2, 1.3 and 1.4.
TABLE 1.1 results of stability test (unit: wt%)
As can be seen from Table 1.1, the stability test results of examples 1 to 5 were all transparent and stable.
TABLE 1.2 stability test results (unit: wt%)
As can be seen from Table 1.2, the stability test results of examples 6-9 are all transparent and stable.
TABLE 1.3 stability test results (unit: wt%) for examples 10 to 16
As can be seen from Table 1.3, the stability test results of examples 10-16 are all transparent and stable.
TABLE 1.4 stability test results (unit: wt%)
As can be seen from Table 1.4, the stability test results of comparative examples 1,3 and 5 are transparent and unstable, and have precipitation phenomenon; the stability test results of comparative examples 2, 4, and 6 were all transparent and stable.
2. Oil control efficacy test (in vitro method):
reference test method: intracellular lipid content assay
(1) Test sample: the compositions of examples 1 to 16 and comparative examples 1 to 6 were added to a conventional emulsion external matrix to prepare test samples, and a blank control was the conventional emulsion external matrix. The test method in which the compositions of examples 1 to 16 and comparative examples 2, 4 and 6 of the present invention account for 5% of the total mass of the emulsion is an in vitro method, and is suitable for evaluating cosmetics which are said to achieve an oil control effect by reducing the lipid content in human sebaceous cells.
(2) The testing method comprises the following steps: intracellular lipid content assay: taking SZ95 cells, paving the SZ95 cells into a 96-well plate for culturing for 24 hours, replacing the SZ95 cells with a culture medium containing samples to be detected with different concentrations, and fixing the SZ95 cells with 4% paraformaldehyde for 30 minutes after culturing for 24 hours; OD490nm was then detected with the oil red O staining kit. The results are shown in Table 2.
TABLE 2 intracellular lipid content
From the results of the oil control tests in Table 2, it can be seen that the oil control effects of examples 1 to 16 and comparative examples 2, 4 and 6 are all more remarkable, but the effects of examples 1 to 5 are weaker than those of examples 6 to 16, the intracellular lipid content can be as low as 24%, and the oil control effects of all the examples are superior to those of all the comparative examples. These differences in effect are caused by the difference in component and the difference in the amount of component added. This also directly illustrates that the synergistic interaction between the components in the composition has a more effective and direct effect on oil control.
3. Acne efficacy test (in vitro method)
(1) Test sample: the compositions of examples 1 to 16, comparative examples 2, 4 and 6 were added to a conventional emulsion external-use matrix to prepare a test sample, the negative control was the conventional emulsion matrix, and the positive control was BPO gel (Sichuan Minxin pharmaceutical Co., ltd.). Wherein the compositions of examples 1 to 16 and comparative examples 2, 4 and 6 of the present invention account for 8% of the total mass of the emulsion. And meanwhile, the common emulsion external matrix is used as a control group.
(2) The testing method comprises the following steps: activating frozen Propionibacterium acnes, and diluting the bacterial liquid to 1.0X10 6 CFU/mL. Adding 100 mu L of diluted bacterial liquid into a 96-well plate, and simultaneously adding 100 mu L of each sample solution; the negative control was 100. Mu.L of the normal emulsion base solution and the positive control was added with 100. Mu.L of BPO gel solution. Placing the 96-well plate in an anaerobic box for 48h, taking out, and detecting by using an enzyme-labeled instrumentOD600 of each hole is used for obtaining the antibacterial rate of propionibacterium acnes. The results are shown in Table 3.
Table 3 sample antibacterial rate
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As can be seen from the acne-removing test results of Table 3, the acne-removing effects of examples 1 to 16 and comparative examples 2, 4 and 6 are all more remarkable, but the effects of examples 1 to 5 are weaker than those of examples 6 to 16, and the differences of the effects are caused by the differences of the formulas and the addition amounts of the components of the formulas. However, the acne-removing effect of examples 1 to 16 is better than that of all comparative examples. The highest antibacterial rate in the examples can reach 89%, while the highest antibacterial rate in the comparative examples is 45%, which is almost half of the effect of the examples. The combination of the individual components in the composition is illustrated, the bacteriostasis rate is far less than the bacteriostasis effect of the synergistic action of the components, and the invention has great advantages in bacteriostasis.
4. Human body safety inspection method
The method refers to a skin closed patch test tested by a human skin patch test method of section 2 of the seventh chapter of cosmetic safety technical Specification (2015 edition).
(1) Test sample: the compositions of examples 1 to 16, comparative examples 2, 4 and 6 were added to the conventional emulsion external-use matrix to prepare test samples, wherein the compositions of examples 1 to 16, comparative examples 2, 4 and 6 according to the present invention account for 0.5% of the total mass of the emulsion. And meanwhile, the common emulsion external matrix is used as a control group.
(2) The tester chooses: volunteers 18 to 60 years old, which meet the test requirements, were selected as subjects. The population with the following conditions could not be treated as a subject: antihistamines used in the last week or immunosuppressants used in the last month; any anti-inflammatory agent is applied to the tested part in the last two months; a subject suffering from a clinically unhealed inflammatory skin condition; insulin dependent diabetes mellitus patients; asthma or other chronic respiratory disease patients undergoing treatment; receiving an anticancer chemotherapeutic within approximately 6 months; patients with immunodeficiency or autoimmune disease; women in lactation or gestation; bilateral mastectomy and bilateral axillary lymphadenectomy; judging that the skin to be tested is affected by scars, pigments, atrophy, moles, or other flaws; participate in other clinical trial researchers; highly sensitive body constitution; non-volunteer participants or those who were unable to complete the prescribed content as required by the trial.
(3) The testing method comprises the following steps: 50 subjects were selected, 30 women, 20 men.
The selected area is not more than 50mm 2 A plaque test apparatus of about 1mm depth. The test sample was placed in a plaque laboratory at a level of about 0.020g to about 0.025g. The patch test with the test sample was applied to the lateral side of the forearm of the subject with hypoallergenic tape and gently pressed with the palm to apply it uniformly to the skin for 24 hours.
Skin reactions were observed according to the criteria of Table 3 for 30min (after disappearance of the indentation), 24h and 48h, respectively, after removal of the plaque tester of the test sample. And the observations were recorded, the results are shown in tables 4.1, 4.2.
TABLE 4.1 skin response grading Standard for skin closed Patch test
TABLE 4.2 Patch test score table
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As can be seen from the patch results of Table 4.2, examples 1 to 16 and comparative examples 2, 4 and 6 all had a certain irritation, examples 1 to 16 all had a level 1 weak reaction, and comparative examples 2, 4 and 6 all had a large range of level 2 reactions and a small number of level 3 reactions, which means that although all had irritation, the potential safety hazard of comparative examples was far greater than that of all examples, the number of reaction persons of examples was gradually decreased with the lapse of time, and the number of reaction persons of level 2 in comparative examples was gradually increased with the lapse of time, which may be caused by the difference in the compositions and proportions of comparative examples 2, 4 and 6. As can be seen from the combination of the efficacy test and the safety test results, the comparative examples 2, 4 and 6 show a certain effect in the oil control and acne removal efficacy test, but the effect is not significant, is far from that of the examples, has great hidden danger in human safety, and needs to be further perfected if the product is used as an acne removal product.
5. Human body oil control efficacy test
Reference is made to the test method for the efficacy of controlling oil of the T ZHCA 002-2018 cosmetic.
(1) Test sample: the compositions of examples 1 to 16 and comparative examples 2, 4 and 6 were added to a conventional emulsion external use matrix to prepare a test sample, and the control was the conventional emulsion external use matrix. Wherein the compositions of examples 1 to 16 and comparative examples 2, 4 and 6 of the present invention account for 5% of the total mass of the emulsion.
(2) Subject selection:
number of subjects: the effective subjects were 220 persons, 10 persons per group. The age is between 18 and 65 years.
Volunteers cleaned their faces with alkaline soap-based cleansing products, rinsed with clear water, blotted with chipless, dry paper towels, sat still in a standard-compliant test environment with forehead exposure, and remained relaxed, avoiding touching the forehead. Skin surface sebum amount of forehead was measured using skin surface sebum tester Sebumeter, volunteer forehead sebum amount exceeding 120 μg/cm in 8h 2 As a subject.
The following cannot be selected as the subject: use in the last month affects sebum secretion formulations; antihistamines used in the last week or immunosuppressants used in the last month; any anti-inflammatory agent is applied to the tested part in the last two months; a subject suffering from a clinically incurable inflammatory dermatological condition; insulin dependent diabetes mellitus patients; asthma or other chronic respiratory disease patients undergoing treatment; patients who received anti-cancer treatments in nearly six months; patients with immunodeficiency or autoimmune diseases; women in lactation or gestation; bilateral mastectomy and bilateral axillary lymphadenectomy; judging that the skin to be tested is affected by scars, pigments, atrophy, moles, or other flaws; participate in other clinical trial researchers; highly sensitive body constitution; non-volunteer participants or those who were unable to complete the prescribed content as required by the trial.
(3) Measurement procedure
Preparation before testing
The test site is the forehead. The sample smearing area and the control area are randomly distributed on the left and right sides of the forehead, the areas of the sample smearing area and the control area are consistent, the areas of the areas are at least 3cm multiplied by 3cm, the interval between the areas is at least 1cm, and the sample smearing area and the control area are ensured to be balanced statistically.
Before the formal test, the test should sit still in a room meeting the standard for at least 20min, water and beverage cannot be drunk, and the forehead of the subject is exposed and kept relaxed, so that the tested part is prevented from being touched.
Measurement
The test was performed according to the instructions of the skin surface sebum tester.
The measuring method comprises the following steps: under the management of a tester, the tested part of the subject is cleaned by an alkaline soap-based cleaning product, and is sucked by a chipless water-absorbing dry tissue after being washed clean by clean water. The skin surface sebum amounts of the sample application area and the control area were measured 3 times at different positions in each area within 3 minutes, respectively, and the measurement results were expressed as an average value of 3 measurements as an initial value.
The sample was measured at a concentration of (2.0.+ -. 0.1) mg/cm 2 The amount of the sample is smeared for a single time, quantitative sampling is carried out through a syringe or the equivalent, the sample is uniformly arranged in a specified area by using a latex fingerstall, and the actual sample coating amount is recorded; measuring 3 times at different positions in a sample smearing area and a control area at a set measurement time point to obtain the sebum amount of the skin surface of each area, wherein the measurement result is expressed as an average value of 3 times of measurement; set measurementThe time point interval should be not less than 1h, and the set time is 4h and 8h; when measuring at different measuring time points, avoiding the measured position; during the test, the forehead of the subject is exposed, so as to avoid touching the tested part; testing of the same subject must be accomplished by the same tester using the same instrument; when the cosmetics are tested, the control area is blank control; during sample use, such as adverse reactions to the skin of the subject, the test should be immediately discontinued and the subject treated appropriately. Adverse reactions were recorded.
(4) Calculation result
Descriptive statistics
Descriptive statistics were performed on measurements from the sample application area and the control area.
Differential analysis
Differences between the initial values of the sample application area and the control area and the measured values of the other time points are calculated respectively, and then differences between the sample application area and the control area at different measuring times are statistically analyzed by using the differences.
If the test data are normally distributed, adopting a t-test method to carry out statistical analysis; if the test data are non-normal distribution, adopting a rank sum test method to carry out statistical analysis
The statistical methods all adopt two-tail inspection, and the inspection level alpha=0.05
(5) Result determination
Positive results: compared with a control area, the difference value of sebum measured values of the sample smearing area is obviously less than 0.050, and the difference value represents that the tested product has an oil control effect;
negative results: compared with a control area, the difference value of sebum measurement values of the sample smearing area is not significantly different, namely, the difference value P is not less than 0.050, and the effect of no oil control of the tested product is shown;
the test results are shown in Table 5.
TABLE 5 skin lipid levels for samples at 0h, 4h, 8h
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The experimental results of table 5 were statistically analyzed to reduce the skin oil content of examples 1 to 16 by 4h and 8h compared with 0h, and the skin oil content was significantly different from the skin oil content of the control group, and P <0.001; the formulations of examples 1-16 demonstrate the inhibition of skin oil content by continued use of the emulsions prepared from the compositions of the present invention. The formulations of comparative examples 2, 4 and 6 have an inhibitory effect on the skin lipid content. The skin oil content of examples 1 to 16 was compared with comparative examples 2, 4 and 6 using 4 hours and 8 hours, and the oil control effect of examples 1 to 16 was superior to comparative examples 2, 4 and 6. The composition has the advantages of synergistic effect of all components and good oil control effect.
6. Human body acne removing efficacy test
Reference (T/TDCA 004-2021) method
(1) Test sample: the compositions of examples 1 to 16, comparative examples 2, 4 and 6 were added to a general emulsion external-use matrix to prepare test samples. Wherein the compositions of examples 1-16 and comparative examples 2, 4 and 6 of the present invention account for 8% of the total mass of the emulsion.
(2) Subject selection
Number of subjects: the effective subjects were 220 persons, 10 persons per group.
Control before and after use: selecting eligible subjects based on subject inclusion and exclusion criteria ensures that no less than 10 persons per group are ultimately completed in an effective number.
Criteria for inclusion
The age is between 18 and 40 years old, and healthy females or males; the facial skin has a certain number of powder prickers, and cannot be nodules, cysts and the like which are difficult to improve by clinical preparations; no allergic diseases, no allergic history of cosmetics and other external preparations; the skin of the face should not have the phenomena of fetal marks, scratches, white spots, pigmented nevi and the like which affect the test; the test procedure can be understood, voluntarily taking part in the test and signing a written informed consent.
Exclusion criteria
Women in the period of pregnancy or gestation or lactation and six months after delivery; patients with severe systemic disease, immunodeficiency or autoimmune disease; antihistamines used in the last week or immunosuppressants used in the last month; any anti-inflammatory drug is administered to the subject in the last two months; the tested parts participated in other clinical trial patients in the last three months; a patient suffering from a respiratory disease undergoing treatment; a population undergoing dermatological treatment; insulin dependent diabetes mellitus patients.
Subject restriction
During the test, the test and control products provided by the test institution must be used by the subject, and any other products with the effects of controlling oil and removing acne and mildness or influencing the test result cannot be used;
the subjects should maintain a regular life during the trial, taking care of a healthy diet.
(3) Test procedure
Test procedure
Self front-back comparison test flow
For the first visit, subjects were subjected to a test instruction and signed a written informed consent. The subject is asked a series of questions regarding disease history, health status, etc. based on inclusion and exclusion criteria, etc., and facial acne conditions are evaluated for compliance and recorded.
Qualified subjects cleaned their faces using an alkaline soap-based cleaning product under the direction of the staff, and after cleaning were wiped clean with a chipless absorbent dry paper towel. The user cannot drink water and drink during sitting still in the satisfactory room for at least 30 minutes.
The facial acne of the subject is counted by the dermatologist or laboratory researcher.
The standard image is photographed with the skin image photographing system. The image analysis software is used for analyzing the a-value of the skin of the tested part, and the smaller the a-value is, the lighter the acne inflammation is, and the heavier the acne inflammation is otherwise.
The staff distributes the test product to the subjects and provides the product using instructions, and the using method (comprising using parts, using modes, using amount each time, using frequency, notice matters and the like) of the product is defined, so that the subjects can be ensured to correctly and continuously use the product until the test period is finished.
The subjects returned to the laboratory at the set time points, evaluated and tested according to the steps under the same test conditions, and a plurality of test time points can be set according to the product evaluation requirement, and the whole test period is usually not more than 4 weeks.
At each return visit, the subject needs to bring the test product back, weigh and record the amount of test product used.
The test should be terminated immediately and the subject treated appropriately during the use of the product, such as an adverse reaction to the skin of the subject. Adverse reactions should be noted.
(4) Calculation result
And carrying out normal distribution inspection after carrying out statistical analysis on the data by using statistical analysis software, meeting the normal distribution requirement, comparing the data before and after the data by adopting paired t inspection, and otherwise adopting two related sample rank sum inspection.
Statistical methods all used a two-tailed test with a significance level of α=0.05.
(5) Result determination
The visual evaluation or image analysis of any visual point before and after the product shows that the test product has acne removing effect, or the test product is considered to have no acne removing effect, and the result is shown in Table 6.
TABLE 6 VISIA-CR vaccinia area ratio of test sample to D28 prior to use
Statistical analysis of the experimental results of Table 6 shows that the 28 day vaccinia area ratio of examples 1-16 was reduced compared to the pre-use base value, and that there was a significant difference, p <0.001, indicating that the formulations of examples 1-16, which were prepared using the compositions of the present invention, provided significant improvement in the skin vaccinia problem; the reduction rate of the acne area ratio of comparative examples 2, 4 and 6 is obviously lower than that of examples 1 to 16, which shows that the acne removing effect of examples 1 to 16 is better than that of comparative examples 2, 4 and 6. In conclusion, the components in the composition disclosed by the invention are synergistic, so that the composition has a good acne removing effect and achieves a lasting acne removing effect.
Table 7 shows comparison of a with D28 before use of the test sample
Statistical analysis of the experimental results of table 7, examples 1-16 show a significant difference in the reduction in the comparison of the 28 day facial red area a and the pre-use basal value, p <0.001, indicating that the formulations of examples 1-16, which were prepared with the compositions of the present invention, had a significant effect on the improvement of skin inflammation; comparative examples 2, 4, 6 show significantly lower changes in the values of the red areas a than examples 1-16, indicating that examples 1-16 have better facial inflammation ameliorating effects than comparative examples 2, 4, 6. In conclusion, the composition disclosed by the invention has the advantages of synergistic interaction of all the components and good anti-inflammatory and acne-removing effects.
7. Acne-removing print pigment deposition test
(1) Test sample
The compositions of examples 1 to 16, comparative examples 2, 4 and 6 were added to a general emulsion external-use matrix to prepare test samples. Wherein the compositions of examples 1-16 and comparative examples 2, 4 and 6 of the present invention account for 8% of the total mass of the emulsion.
(2) Application method
Test products were dispensed by the staff and the subjects were instructed to use according to instructions to ensure that the subjects were correctly and continuously using the products for 4 weeks.
(3) Selection of a subject
Qualified subjects were selected according to subject inclusion and exclusion criteria, ensuring that the effective subjects 220 were eventually completed, 10 per group.
Criteria for inclusion
18-60 years old, healthy female or male; at least one obvious acne mark is arranged on the tested part; no allergic diseases, no allergic history of cosmetics and other external preparations; no medicine affecting the light sensitivity is used in the recent history of no light-sensitive disease; the skin of the tested part should not have the phenomena of birthmarks, inflammations, scars, hair and the like; the test procedure can be understood, voluntarily taking part in the test and signing a written informed consent.
Exclusion criteria
Pregnant or lactating women, or those who have a pregnancy preparation plan recently; patients with skin history such as psoriasis, eczema, atopic dermatitis, severe acne, etc.; or suffering from other chronic systemic diseases; for the last 1 month, anti-inflammatory drugs such as corticosteroids, etc. are orally taken or externally used; for about 2 months, any skin color affecting product or drug (such as hydroquinone type preparation) such as percarboxylic acid, salicylic acid, etc.; the test part uses the vitamin A acid preparation or the medical and aesthetic therapist who carries out chemical stripping, laser, pulse light and the like within 3 months; unavoidable long-term sun exposure; other clinical trials were enrolled in the last 2 months; other clinical evaluations were considered unsuitable for the participants.
Subject restriction
The test product or control product provided by the test mechanism must be used at the test site during the test, and any other product with the effect of removing pigmentation or possibly influencing the test result cannot be used; no insolation is possible during the test and the test site should be well-protected from sunlight.
(4) Test site: a face.
(5) Instrument apparatus: skin melanin detector: there is an instrument for detecting skin MI values based on the principle of spectral absorption.
(6) Test procedure
The enrolled group of volunteer subjects were enrolled as required, and written informed consent was signed. Before the group is put into the group, the subjects are inquired about a series of problems about disease history, health condition and the like according to the inclusion and exclusion criteria and the like, and meanwhile, the skin conditions such as acne print pigment deposition and the like at the test part are subjected to consistency evaluation and screening and recorded.
Performing evaluation and test of skin basic values before product use on qualified subjects in a group, including visual evaluation, instrument test and standard image shooting, and recording; the same evaluation and testing was again performed 4 weeks after product use. At the visit time point, measuring the MI value of the skin of the acne-print pigment precipitation area of the test part of the test group by using a skin melanin tester, testing each test area for three times, and recording; the smaller the MI value of the test area, the lighter the skin color, and conversely, the darker the skin color.
(7) Calculation result
The statistical analysis software is applied to carry out statistical analysis of data and normal distribution inspection, the normal distribution requirement is met, the comparison before and after the statistical analysis software is matched with the paired t inspection, or else, the two related sample rank sum inspection is adopted; comparing the grade data before and after use, and adopting two related sample ranks and tests; comparison between test product and control group used independent sample t-test or rank-sum test. The above statistical analysis was a two-tailed test with a significance level of α=0.05.
The change results of any one of the relevant parameters of visual evaluation, instrument test or image analysis at any visit time before and after the use of the product are obviously different (P < 0.05), the test product is considered to have the acne-removing print pigment deposition efficacy, otherwise, the test product is considered to have no acne-removing print pigment deposition efficacy, and the results are shown in Table 8.
TABLE 8 MI value of test sample with D28 before use
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Statistical analysis of the experimental results of Table 8 shows that the comparison of the MI values of the faces of examples 1-16 with 28 days and the basic values before use are reduced, and the comparison has significant differences, p is less than 0.001, which indicates that the formulas of examples 1-16, which are prepared by continuously using the composition of the invention, have significant improvement effect on the acne-removing pigment deposition of the skin; the reduction rate of MI values of comparative examples 2, 4 and 6 was significantly lower than that of examples 1 to 16, indicating that examples 1 to 16 had better pigmentation improvement effect than comparative examples 1 to 6. The composition has the advantages of synergistic effect of all the components and good acne-removing and pigment-depositing effects.
In conclusion, the synergistic effect among the natural active substances of the willow bark extract, the kuh-sence extract, the wisense GSS, the polyalcohol, the persimmon leaf extract, the thyme extract, the rheum officinale extract, the flaxseed extract and the antimicrobial peptide freeze-dried powder is expected to be achieved through the results of the stability test, the oil control and the acne removal efficacy test, the acne removal and acne mark prevention can be more effectively and effectively achieved on the basis of no skin damage, and the synergistic effect of the composition provided by the invention is better than that of a comparative example and the original advantages are maintained, so that the salicylic acid self advantages are amplified and the defects of the salicylic acid are overcome.
Claims (3)
1. The composition containing salicylic acid and having the effects of controlling oil and removing acne is characterized by comprising the following components in parts by weight: 5-15 parts of willow bark extract, 2-7 parts of radix sophorae flavescentis extract, 1-10 parts of wisense GSS, 1-8 parts of polyalcohol, 3-8 parts of persimmon leaf extract and 1-6 parts of thyme extract; also comprises 1-5 parts of rheum officinale extract and 1-7 parts of flaxseed extract; 2-8 parts of antibacterial peptide freeze-dried powder;
the Wisence GSS comprises the following components in percentage by mass: 40% of salicylic acid, 40% of PEG-15 cocoamine and 20% of stearamidopropyl dimethylamine.
2. The salicylic acid-containing mild and oil-controlling acne-removing composition according to claim 1, wherein 8-11 parts of willow bark extract, 4-5 parts of radix sophorae flavescentis extract, 5-7 parts of wisense GSS, 3-5 parts of polyalcohol, 5-6 parts of persimmon leaf extract, 3-4 parts of thyme extract, 2-4 parts of rheum officinale extract, 3-6 parts of flaxseed extract and 4-7 parts of antimicrobial peptide freeze-dried powder.
3. Use of a composition according to any one of claims 1-2 in the preparation of a cosmetic, said composition being added in an amount of 0.5-8.0% of the total mass of the cosmetic.
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