Mild acne-removing composition as well as preparation method and application thereof
Through the synergistic effects of colloidal sulfur, Huang Cen extract, encapsulated salicylic acid and quaternary ammonium salt-73 in the gentle acne removal composition, the problem of irritation of acne removal components in the prior art is solved, and gentle Quick and effective acne removal effect.
Patent Information
- Application Number
- CN202411910699.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-23
- Publication Date
- 2025-02-25
AI Technical Summary
In the prior art, the acne removal ingredients are highly irritating, leading to skin discomfort, and long-term use of antibiotics is prone to drug resistance, lacking complementary or alternative preparations with low side effects and accurate efficacy.
A gentle acne removal composition is provided, including colloidal sulfur, yellow cephala extract, encapsulated salicylic acid and quaternary ammonium salt-73, which can effectively eliminate acne through synergistic action and has a gentle and rapid effect.
This composition can significantly inhibit Propionibacterium acnes, reduce inflammatory response, improve skin texture, reduce skin aging risk, and is suitable for use in people of different skin types.
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Figure CN119499106A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of daily chemicals, and in particular to a mild acne-removing composition and a preparation method and application thereof. Background Art
[0002] Acne is a common chronic skin disease characterized by papules, pustules, cysts and even nodules. Acne usually begins to appear during adolescence. During adolescence, the body's androgen levels rise. Androgens stimulate the sebaceous glands to enlarge and increase sebum secretion. As adolescence progresses, hormone levels fluctuate and the symptoms of acne will also change. For example, factors such as high stress in life and bad living habits (such as staying up late for a long time and unhealthy diet) can also cause acne in adulthood or aggravate existing acne.
[0003] Currently, drugs for acne include retinoic acid drugs, benzoyl peroxide, antibiotics, etc., but these drugs all have side effects. Retinoic acid drugs may decompose when exposed to light, resulting in reduced efficacy. When first used, irritation reactions such as dry skin and desquamation may occur, and skin tolerance needs to be gradually established. Benzoyl peroxide may cause allergic reactions such as skin redness and itching in some people. Antibiotics are generally not recommended for long-term use alone to avoid drug resistance. Therefore, it is of great value to find complementary or alternative preparations with low side effects and definite efficacy, and to study safe, gentle and effective acne-removing ingredients. Summary of the invention
[0004] In view of this, the present invention provides a mild acne-removing composition and a preparation method and application thereof, aiming to solve the defect of the existing acne-removing ingredients having great irritation.
[0005] As a first aspect of the present invention, the present invention provides a mild acne-removing composition, comprising the following components by weight: 10-25 parts of colloidal sulfur; 70-90 parts of Scutellaria baicalensis extract; 0.01-5 parts of encapsulated salicylic acid; and 0.005-0.1 parts of quaternary ammonium salt-73.
[0006] In the anti-acne composition of the present invention, colloidal sulfur and quaternary ammonium salt-73 both have antibacterial and anti-inflammatory effects. Colloidal sulfur can inhibit harmful microorganisms such as Propionibacterium acnes on the skin surface, and quaternary ammonium salt-73 can further enhance the effect, and synergistically prevent and improve skin inflammation problems such as acne. Encapsulated salicylic acid can exfoliate, unclog pores, and improve skin texture. The Scutellaria baicalensis extract contains antioxidant and anti-inflammatory ingredients such as flavonoids. While salicylic acid improves the surface state of the skin, the Scutellaria baicalensis extract can reduce skin inflammation that may be caused by exfoliation, and its antioxidant effect can resist the damage of free radicals to the skin and reduce skin aging. The components in the composition work synergistically to achieve effective acne removal, and have a mild and rapid effect.
[0007] Colloidal sulfur
[0008] The present invention uses colloidal sulfur, which is a highly dispersed form of sulfur. It is a colloidal system formed by dispersing sulfur (S) in a medium in the form of extremely fine particles. The diameter of the colloidal particles is generally between 1 and 1000 nanometers, and the particle size of the colloidal sulfur is also within this range, so that it has some typical properties of colloids.
[0009] Compared with traditional sulfur products, such as sulfur soap, colloidal sulfur has reduced irritation after special treatment. It uses soothing ingredients to wrap small molecular sulfur, allowing it to slowly penetrate the skin and take effect. It is gentler on the skin and suitable for sensitive skin and delicate skin parts such as the face. In specific skin care products, colloidal sulfur can be better dispersed and has a good inhibitory effect on Propionibacterium acnes, scabies, some streptococci and Staphylococcus aureus. It can effectively reduce skin problems caused by these bacteria and mites, such as acne, blackheads, seborrheic dermatitis, etc., and has a significant effect on improving skin inflammation. Colloidal sulfur can also decompose keratin, promote the separation of the stratum corneum, help remove the aging cutin accumulated on the skin surface, make the skin smoother and more delicate, enhance the permeability of the skin, and facilitate the absorption of other skin care ingredients. It is safer.
[0010] Based on the weight of the mild anti-acne composition, the amount of colloidal sulfur added is 10-25 parts, for example, the amount of colloidal sulfur added can be 10 parts, 13 parts, 15 parts, 17 parts, 18 parts, 19 parts, 20 parts, 22 parts, 23 parts, 25 parts, etc.
[0011] Scutellaria baicalensis extract
[0012] The Scutellaria baicalensis extract in the mild acne-removing composition of the present invention contains flavonoids and has antibacterial, anti-inflammatory and antioxidant activities. Among them, antibacterial means that it has a certain inhibitory effect on various skin pathogens such as Propionibacterium acnes, and cooperates with other acne-removing ingredients to enhance the antibacterial spectrum and antibacterial effect of the composition. At the same time, the mild antibacterial method of the Scutellaria baicalensis extract helps to maintain the balance of skin microecology and avoid skin flora imbalance caused by excessive sterilization; anti-inflammatory properties mean that flavonoids can regulate the signal pathways related to inflammation in the body, reduce the inflammatory response caused by Propionibacterium acnes, and relieve symptoms such as skin redness, swelling, and pain. Antioxidation means that flavonoids can remove free radicals in the skin, reduce the damage of oxidative stress to skin cells, and prevent pigmentation and skin aging caused by acne inflammation.
[0013] Based on the weight of the mild anti-acne composition, the added amount of the Scutellaria baicalensis extract is 70-90 parts, such as 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, etc.
[0014] Salicylic Acid Encapsulation
[0015] The mild anti-acne composition also includes encapsulated salicylic acid, which is encapsulated using molecular complexation solubilization technology and is easily soluble in water. The encapsulated salicylic acid will be relatively gentle when it initially contacts the skin. As it is slowly released, the skin has time to gradually adapt to the effects of salicylic acid, thereby greatly reducing the chance of adverse reactions on the skin and enhancing the skin's tolerance to salicylic acid, making it more suitable for people with different skin types.
[0016] Based on the weight of the mild anti-acne composition, the amount of the encapsulated salicylic acid added is 0.01-5 parts, for example, 0.01 parts, 0.03 parts, 0.06 parts, 0.08 parts, 0.1 parts, 0.12 parts, 0.2 parts, 0.5 parts, 0.8 parts, 1 parts, 1.8 parts, 2.0 parts, 2.2 parts, 3 parts, 3.2 parts, 3.5 parts, 3.8 parts, 4 parts, 4.2 parts, 4.5 parts, 5 parts, etc.
[0017] Quaternary ammonium salt-73
[0018] Quaternary ammonium salt-73 is a highly effective antibacterial agent, and its chemical structure contains quaternary ammonium groups. Since quaternary ammonium salt-73 has a good inhibitory effect on acne-causing bacteria such as Propionibacterium acnes, it can help reduce the number of bacteria on the skin surface and reduce inflammatory reactions, thereby achieving the effect of preventing and treating acne.
[0019] Based on the weight of the mild anti-acne composition, the amount of quaternary ammonium salt-73 added is 0.005-0.1 parts, such as 0.005 parts, 0.01 parts, 0.03 parts, 0.05 parts, 0.08 parts, 0.1 parts, etc.
[0020] In one preferred embodiment of the first aspect of the present invention, the following components are included by weight: 15-25 parts of colloidal sulfur; 70-80 parts of Scutellaria baicalensis extract; 0.05-5 parts of encapsulated salicylic acid; and 0.05-0.1 parts of quaternary ammonium salt-73.
[0021] The mild acne-removing composition within the preferred range can significantly inhibit Propionibacterium acnes, improve the mildness of the colloidal sulfur composition, and has a mild and rapid acne-removing effect.
[0022] In one of the preferred embodiments of the first aspect of the present invention, the Scutellaria baicalensis extract is one or more extracts of the flowers, leaves and stems of Scutellaria baicalensis.
[0023] This patent prefers to extract active ingredients from the flowers, leaves and stems of alpine Scutellaria baicalensis. Compared with Scutellaria baicalensis root, the flowers, leaves and stems of alpine Scutellaria baicalensis are convenient for extraction and have a higher content of effective active ingredients. However, the extraction cost of Scutellaria baicalensis root is high and the content of active ingredients is relatively low, which is not convenient for mass production and preparation of subsequent products.
[0024] In one preferred embodiment, the colloidal sulfur is formed by microemulsion encapsulating nanosulfur, and the diameter of the colloidal sulfur is between 1 and 1000 nanometers. The colloidal sulfur is formed by encapsulating nanosulfur in microemulsion, which improves the dispersibility and permeability of the colloidal sulfur, making it more stable and efficient, and better exerting its efficacy.
[0025] In one preferred embodiment, the colloidal sulfur is prepared by the following steps:
[0026] S1: Weigh sulfur powder with a particle size of 20-100 um and water in a mass ratio of 1: (1.5-9), mix the sulfur powder and water, and stir and disperse to obtain a slurry;
[0027] Wherein, in this step, an emulsifier is used to disperse the sulfur powder and water, and the rotation speed of the emulsifier is 10000-28000rpm.
[0028] In other embodiments, it may also be an electric stirrer, a homogenizer, etc.
[0029] S2: Pour the slurry prepared in S1 into a ball mill, and add ball milling media and dispersant for dispersed ball milling;
[0030] The ball milling medium used is zirconium oxide, and its particle size is not more than 10mm. Its function is to break the sulfur particles into nanometer scale by collision and friction with the sulfur particles. The dispersant used is any one or a combination of propylene glycol and butylene glycol. The dispersant can reduce the surface energy of sulfur particles, prevent them from agglomerating, ensure that sulfur is evenly dispersed and refined to nanometer scale during the ball milling process, and improve its specific surface area and activity. In other embodiments, the dispersant can also be isomeric tridecanol polyoxyethylene ether sodium sulfate, etc. The amount of the ball milling medium added is 3-8 times the mass of the sulfur powder, and the amount of the dispersant added is 2-10% of the sulfur powder.
[0031] Specifically, the obtained slurry is added to a ball mill, and after adding ball milling media and dispersant, the ball mill is sealed, and the ball mill is placed on a ball mill with a rotation speed of 400-600 rpm for dispersion grinding, and the ball milling time is 5-10 hours.
[0032] S3: filtering the ball-milled sulfur slurry to remove particulate impurities that have not been dispersed, and obtaining nano-sulfur slurry with a particle size of 5nm-100nm;
[0033] The filtration step can ensure the purity and uniformity of the product and prevent large sulfur particles from irritating the skin or affecting the stability of the composition. Specifically, a vacuum suction filter with a filtration mesh of 800 mesh is used to remove particulate impurities in the sulfur slurry that cannot be dispersed after ball milling, thereby obtaining a nano-sulfur slurry with a small particle size.
[0034] S4: Take Tween60 and butylene glycol and add them to caprylic acid triglyceride, and stir to form an organic mixture of Tween60 / butylene glycol / caprylic acid triglyceride. Then slowly add the nano sulfur slurry of S3 and stir at a low speed to form colloidal sulfur.
[0035] In this step, the nano-sulfur slurry is encapsulated in microemulsion to reduce its irritation, while the organic mixture of Tween60 / butylene glycol / caprylic capric triglyceride is used as the encapsulation material, which has more soothing ingredients and is gentler on the skin.
[0036] Specifically, Tween60, as a surfactant, can reduce the oil-water interfacial tension, so that nano-sulfur can be stably dispersed in the organic phase to form a microemulsion encapsulation structure. Butanediol, as a co-surfactant, has moisturizing and solubilizing effects, which can improve the moisturizing properties of the composition and the compatibility of the various components. Caprylic / capric triglyceride, as an oil phase, provides a good carrier environment for the microemulsion, enhancing the stability and skin permeability of colloidal sulfur. This microemulsion-encapsulated nano-sulfur structure can, on the one hand, effectively control the release rate of sulfur, allowing it to continue to play an acne-removing role; on the other hand, it reduces the direct contact between sulfur and the skin, reduces irritation, and improves safety of use.
[0037] The mixing ratio of each component in the organic mixture of Tween60 / butylene glycol / caprylic acid capric acid triglyceride is 4:4:2. The ratio of the organic mixture to the nano sulfuric acid is 8:2.
[0038] In one preferred embodiment, the method for preparing the Scutellaria baicalensis extract is to use ionic liquid as an extractant to extract the Scutellaria baicalensis flowers / leaves / stems, followed by centrifugation, and the obtained supernatant is the Scutellaria baicalensis extract.
[0039] Ionic liquids have good solubility and selectivity, and can efficiently extract the active ingredients in Scutellaria baicalensis, such as baicalin, baicalein and other flavonoids. The extraction using ionic liquids is green and environmentally friendly, has strong stability, and can efficiently extract Scutellaria baicalensis flowers / leaves / stems, and is easy for subsequent purification and separation.
[0040] In the embodiment of the present invention, the ionic liquid used is 1-butyl-3-methylimidazolium bromide solution, and in other embodiments, it can be 1-ethyl-3-methylimidazolium acetate, 1-hexyl-3-methylimidazolium bromide, etc.
[0041] As a second aspect of the present invention, the present invention further claims a method for preparing a mild acne-removing composition, comprising the step of mixing the components of the mild acne-removing composition as described in any one of the first aspects of the present invention.
[0042] As a preferred embodiment of the second aspect of the present invention, the specific preparation method of the mild acne-removing composition comprises: placing the encapsulated salicylic acid, colloidal sulfur, scutellaria baicalensis extract, and quaternary ammonium salt-73 in a container in proportion, placing it in an ultrasonic instrument for ultrasonication, and then using a magnetic stirrer to fully stir at 55-60° C. to obtain the mild acne-removing composition after stirring.
[0043] Specifically, in a method for preparing a mild acne-removing composition, an ultrasonic instrument is used for mixing, and the cavitation effect of ultrasonic waves can be used to fully mix the components in a short time, break up possible agglomerates, and improve the uniformity and stability of the composition. After ultrasonication, a magnetic stirrer is used to fully stir at 55-60°C. Within this temperature range, on the one hand, the dissolution and mixing of the components can be further promoted, and on the other hand, it is conducive to the stability of some components (such as the microemulsion structure in colloidal sulfur), ensuring that a stable interaction relationship is formed between the components, and finally a mild acne-removing composition is obtained after stirring.
[0044] The ultrasonic time and stirring time are related to the amount of the mixture added. Specifically, in one embodiment, the ultrasonic time is 5-10 minutes, and the stirring time using a magnetic stirrer is 10-30 minutes.
[0045] The preparation method of the mild acne-removing composition of the present invention is simple and can stabilize the components, thus facilitating the subsequent production and use thereof.
[0046] As the third aspect of the present invention, the present invention also seeks to protect the use of any mild acne-removing composition described in the first aspect in skin care products / cosmetics.
[0047] Specifically, the third aspect of the present invention claims protection for the use of a mild acne-removing composition. The mild acne-removing composition of the present invention has a safe, mild and effective acne-removing effect, and has a wide range of application prospects in skin care products. The mild acne-removing composition of the present invention is applied to skin care products or cosmetics, so that the skin care products or cosmetics have the effect of removing acne, and the effect is mild and rapid. Specifically, the skin care products or cosmetics may include one or more of lotions, essences, sleeping masks, creams, moisturizing oils, and massage creams.
[0048] As a fourth aspect of the present invention, the present invention also seeks to protect a mild anti-acne skin care product, including any mild anti-acne composition described in the first aspect above.
[0049] Specifically, the corresponding mild acne-removing skin care product includes the mild acne-removing composition of the first aspect of the present invention, and also includes any other components of the skin care product, such as water, emulsifier, etc. The mild acne-removing skin care product having the mild acne-removing composition has a mild and effective acne-removing effect.
[0050] Beneficial Effects
[0051] The mild acne-removing composition provided by the present invention comprises mild and stable colloidal sulfur. The scutellaria baicalensis extract and the encapsulated salicylic acid are compounded and used in the colloidal sulfur, so that the composition has the effect of being milder and rapidly removing acne. The composition is then combined with quaternary ammonium salt-73 to remove acne from the root and reduce the recurrence of acne. The composition has a mild and effective acne-removing effect.
[0052] The preparation method of the mild acne-removing composition of the present invention is simple and easy to operate; the obtained mild acne-removing composition is stable, and is convenient for mass production and subsequent application.
[0053] The mild acne-removing composition of the present invention can be used in skin care products or cosmetics to prepare skin care products or cosmetics with mild acne-removing effects. The corresponding skin care products or cosmetics have the effect of removing acne and exert the effect mildly and quickly. BRIEF DESCRIPTION OF THE DRAWINGS
[0054] Figure 1 Schematic diagram of N0 release rate results.
[0055] Figure 2 It is a schematic diagram of the inhibition rate results of Staphylococcus aureus and Propionibacterium acnes;
[0056] Figure 3 Schematic diagram of VISIA skin redness a* value.
[0057] Figure 4 This is a diagram showing the average redness results of a single pimple measured by Antera 3D.
[0058] Figure 5 This is a schematic diagram of the Antera 3D single acne volume results. DETAILED DESCRIPTION
[0059] The embodiments of the present invention will be described in detail below in conjunction with the examples, but those skilled in the art will appreciate that the following examples are only used to illustrate the present invention and should not be considered to limit the scope of the present invention. If no specific conditions are specified in the examples, they are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be obtained commercially.
[0060] Aspect 1: Preparation of colloidal sulfur
[0061] The first aspect of the specific implementation of the present invention provides a method for preparing colloidal sulfur according to an embodiment of the present invention, wherein colloidal sulfur is formed by encapsulating nanosulfur with a novel microemulsion, and the method specifically comprises the following steps:
[0062] S10: Weigh sulfur powder with a particle size of 20-100 μm and water in a mass ratio of 1:(1.5-9), pour the sulfur powder and water into a container, and disperse them for 15-30 minutes using an emulsifier at a rotation speed of 10000-28000 rpm to obtain a slurry;
[0063] S20: pouring the slurry obtained in step S10 into a ball mill, adding ball milling medium and dispersant, the added amount of which is 3-8 times the mass of the sulfur powder, and the dispersant is 2-10%, and sealing the ball mill; wherein the ball milling medium is zirconium oxide, and the dispersant is a mixture of propylene glycol and butanediol;
[0064] S30: placing the ball mill jar on a ball mill with a rotation speed of 400-600 rpm for dispersion grinding, and the ball milling time is 5-10 hours;
[0065] S40: using a vacuum filter with a filter mesh of 800 mesh to remove and recover particulate impurities that have not been dispersed after ball milling in the sulfur slurry, to obtain a nano-sulfur slurry with a particle size of 5nm-100nm;
[0066] S50: adding Tween 60 and butylene glycol to caprylic acid triglyceride, stirring to form an organic mixture of Tween 60 / butylene glycol / caprylic acid triglyceride, and then slowly adding the nano sulfur slurry of step S40, stirring at a low speed to form colloidal sulfur.
[0067] The mixing ratio of each component in the organic mixture of Tween60 / butylene glycol / caprylic acid capric acid triglyceride is 4:4:2. The ratio of the organic mixture to the nano sulfuric acid is 8:2.
[0068] Second aspect: Preparation method of alpine scutellaria flower / leaf / stem extract
[0069] The second aspect of the specific implementation of the present invention provides a method for preparing the alpine Scutellaria baicalensis flower / leaf / stem extract in the embodiment of the present invention, and the specific method is as follows:
[0070] Accurately weigh 0.1g of alpine scutellaria flower / leaf / stem into a 10mL stoppered glass tube, use 1-butyl-3-methylimidazolium bromide solution as the extractant, the ionic liquid concentration is 50%, the solid-liquid ratio is 1:40g / mL, the extraction temperature is 30°C, the time is 10min, and centrifuge at 3000r / min for 5min. Take the supernatant to obtain the alpine scutellaria flower / leaf / stem extract.
[0071] The remaining components in the examples of the present invention are commercially available and are not described here.
[0072] The third aspect: mild acne-removing composition and its application verification
[0073] As the third aspect of the present invention, the efficacy of the mild acne-removing composition of the present invention and the corresponding skin care products are verified. The efficacy or effect of the acne-removing composition of the present invention and its application corresponding to the present invention will be described below in conjunction with specific examples.
[0074] Example 1
[0075] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 10% colloidal sulfur; 88.9% alpine scutellaria flower / leaf / stem extract; 1% encapsulated salicylic acid; 0.1% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 1 is obtained.
[0076] Example 2
[0077] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 15% colloidal sulfur; 83.95% alpine scutellaria flower / leaf / stem extract; 1% encapsulated salicylic acid; 0.05% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 2 is obtained.
[0078] Example 3
[0079] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 10% colloidal sulfur; 86.9% alpine scutellaria flower / leaf / stem extract; 3% encapsulated salicylic acid; 0.1% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 3 is obtained.
[0080] Example 4
[0081] In this embodiment, a mild acne-removing composition is prepared according to the following components and proportions. 20% colloidal sulfur; 78.9% alpine scutellaria flower / leaf / stem extract; 1% encapsulated salicylic acid; 0.1% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 4 is obtained.
[0082] Example 5
[0083] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 25% colloidal sulfur; 69.95% alpine scutellaria flower / leaf / stem extract; 5% encapsulated salicylic acid; 0.05% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 5 is obtained.
[0084] Example 6
[0085] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 15% colloidal sulfur; 84.495% alpine scutellaria flower / leaf / stem extract; 0.5% encapsulated salicylic acid; 0.005% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 6 is obtained.
[0086] Example 7
[0087] In this embodiment, a mild anti-acne composition is prepared according to the following components and proportions. 20% colloidal sulfur; 76.95% alpine scutellaria flower / leaf / stem extract; 3% encapsulated salicylic acid; 0.05% quaternary ammonium salt-73. Place in a suitable container according to a predetermined ratio, put into an ultrasonic instrument, ultrasonicate for 5-10 minutes, and then use a magnetic stirrer to fully stir at 55-60°C, and continue stirring for 10-30 minutes. Example 7 is obtained.
[0088] Example 8
[0089] A mild anti-acne composition was prepared according to the following components and proportions. 10% colloidal sulfur; 84.995% alpine scutellaria flower / leaf / stem extract; 5% encapsulated salicylic acid; 0.005% quaternary ammonium salt-73. The components were placed in a suitable container according to the predetermined proportion, placed in an ultrasonic instrument, ultrasonicated for 5-10 minutes, and then fully stirred at 55-60°C using a magnetic stirrer for 10-30 minutes. Example 8 was obtained.
[0090] Comparative Example 1
[0091] In Comparative Example 1, an anti-acne composition was prepared according to the following components and proportions: 75% alpine scutellaria flower / leaf / stem extract; 5% encapsulated salicylic acid; 0.1% quaternary ammonium salt-73. The components were placed in a suitable container according to a predetermined ratio, placed in an ultrasonic instrument, ultrasonicated for 5-10 minutes, and then fully stirred at 55-60°C using a magnetic stirrer for 10-30 minutes. Comparative Example 1 was obtained.
[0092] Comparative Example 2
[0093] In Comparative Example 2, an anti-acne composition was prepared according to the following components and proportions: 20% colloidal sulfur; 5% encapsulated salicylic acid; 0.1% quaternary ammonium salt-73. The components were placed in a suitable container according to a predetermined ratio, placed in an ultrasonic instrument, ultrasonicated for 5-10 minutes, and then fully stirred at 55-60° C. using a magnetic stirrer, and continued stirring for 10-30 minutes. Comparative Example 2 was obtained.
[0094] Comparative Example 3
[0095] In Comparative Example 3, a mild anti-acne composition was prepared according to the following components and proportions: 20% colloidal sulfur; 75% alpine scutellaria flower / leaf / stem extract; 5% encapsulated salicylic acid. The components were placed in a suitable container according to a predetermined ratio, placed in an ultrasonic instrument, ultrasonicated for 5-10 minutes, and then fully stirred at 55-60°C using a magnetic stirrer for 10-30 minutes. Comparative Example 3 was obtained.
[0096] Comparative Example 4
[0097] In Comparative Example 4, a mild anti-acne composition was prepared according to the following components and proportions: 20% colloidal sulfur; 75% alpine scutellaria flower / leaf / stem extract; 0.1% quaternary ammonium salt-73. The components were placed in a suitable container according to a predetermined ratio, placed in an ultrasonic instrument, ultrasonicated for 5-10 minutes, and then fully stirred at 55-60°C using a magnetic stirrer for 10-30 minutes. Comparative Example 4 was obtained.
[0098] The ratio of active ingredients in the above examples and comparative examples is shown in Table 1 below
[0099] Table 1, Examples and Comparative Examples
[0100]
[0101] Test 1: Effects of Examples and Comparative Examples on Nitric Oxide Concentration in LPS-Induced RAW 264.7 Cell Inflammation Model
[0102] AW264.7 cells were seeded in a 12-well plate at a density of 200,000 per well. After the cells adhered to the wall, different examples of acne-removing extract solutions containing 200 crude drug amounts were added and incubated for 1 hour. Then, 100 μL of culture medium was added to the blank group, and the remaining groups were added with an equal amount of 10 μg / mL lipopolysaccharide solution, and the supernatant was collected after continuing to incubate for 24 hours. The nitric oxide kit was operated according to the instructions of the nitric oxide kit, and the nitric oxide level was detected at a wavelength of 540 nm using an ELISA reader. The nitric oxide level in the cells treated with different concentrations of acne-removing extract was calculated according to the standard curve, and the nitric oxide release was calculated.
[0103] The results of nitric oxide release are shown in the attached figure. Figure 1 shown.
[0104] As attached Figure 1 As shown, the different embodiments and comparative examples in the experiment can inhibit the release of nitric oxide in the inflammatory response of RAW264.7 cells induced by lipopolysaccharide to a certain extent, and have anti-inflammatory effects. Compared with the embodiments and comparative examples, the mild acne-removing composition in the embodiments of the present invention is better than the comparative example, indicating that the mild acne-removing composition in the embodiments of the present invention has a synergistic anti-inflammatory effect.
[0105] Test 2: Determination of the antibacterial rate of the embodiments and comparative examples against Staphylococcus aureus and Propionibacterium acnes
[0106] The antibacterial rates of the compositions of the test examples and comparative examples against Staphylococcus aureus and Propionibacterium acnes were tested, and the corresponding antibacterial rates were obtained by a broth microdilution method experiment.
[0107] The specific steps of the experiment are:
[0108] ① Under sterile operating conditions, add 100 μL of nutrient broth medium (for Staphylococcus aureus culture) and immersion broth medium (for Propionibacterium acnes culture) to each well of a 96-well plate;
[0109] ② Add 100 μL of the anti-acne composition solution to the first well, mix it with the culture medium in the well by pipetting, then aspirate 100 μL of the suspension and add it to the second well, and repeat this process until the 11th well, then aspirate 100 μL of the suspension from the 11th well and discard it, and do not add the anti-acne composition solution to the 12th well as a positive control;
[0110] ③ Add 100 μL of diluted bacterial solution to each well and make the final concentration of bacterial solution in each well 1×10 6 CFU / mL, and a negative control was set up at the same time.
[0111] Among them, the results of the inhibition rate are shown in the attached Figure 2 shown.
[0112] From the attached Figure 2 It can be clearly seen that the anti-acne composition of the embodiment of the present invention has a significantly better inhibitory effect on Staphylococcus aureus and Propionibacterium acnes than the comparative example group. The inhibition rates of comparative examples 1-4 on the two bacteria are relatively low, and the inhibition rates are mostly around 70%, but there is still a certain inhibitory effect. All embodiments of embodiments 1-8 of the present invention have a high inhibition rate on Staphylococcus aureus and Propionibacterium acnes. The inhibition rates of embodiments 1 to 8 are mostly above 80%, and some are even close to 90%. Among them, embodiment 4 has the highest inhibition rate on Staphylococcus aureus, close to 90%, and embodiment 7 has the highest inhibition rate on Propionibacterium acnes, close to 90%.
[0113] It can be seen from Test 1 and Test 2 that the mild acne-removing composition of the embodiment of the present invention has a synergistic effect in anti-inflammatory and antibacterial properties, and has good effects in anti-inflammatory properties and inhibiting the growth of two types of bacteria.
[0114] Testing of skin care products
[0115] The invention prepares an anti-acne essence containing 1% of a mild anti-acne composition, wherein the mild anti-acne composition consists of the following components: 20% of colloidal sulfur, 78.9% of alpine scutellaria flower / leaf / stem extract, 0.1% of quaternary ammonium salt-73, and 1% of an anti-acne essence encapsulating salicylic acid.
[0116] The formula of the anti-acne essence is shown in Table 2 below:
[0117] The steps for preparing acne serum are as follows:
[0118] Add cetearyl alcohol, Tween 60, caprylic / capric triglyceride and glyceryl stearate in phase B into the clean oil phase pot in sequence and heat to 80°C, stir and dissolve evenly, and keep warm for 10 minutes;
[0119] Add the purified water, ammonium acryloyldimethyltaurate / VP copolymer, butylene glycol, xanthan gum and glycerin in phase A to the clean water phase pot in sequence, homogenize at high speed for 3 minutes, heat to 80°C, keep warm for 15 minutes, and stir thoroughly until completely dissolved;
[0120] Pump phase A and phase B into the emulsifier, homogenize at high speed for 5 minutes, and continue stirring for 8 minutes;
[0121] Use cooling water to cool the emulsifying pot to 45°C, and add phenoxyethanol, hexylene glycol and ethylhexylglycerin in phase C in sequence;
[0122] Finally, add the mild acne-removing composition in phase D;
[0123] After fully stirring, cool to 38°C, filter and obtain the anti-acne essence.
[0124] Table 2. Anti-acne essence formula ingredients
[0125]
[0126] Test 3 Essence Anti-Acne Efficacy Test
[0127] The acne-removing essence samples were prepared by the above method, and the acne-removing efficacy of the product was evaluated before and after use.
[0128] 33 subjects were enrolled, subjects numbered VT018 and VT033 withdrew from the test due to personal reasons, and finally 31 subjects were counted, including 8 males and 23 females, aged 21 to 40 years old, with an average age of 30.58±0.88 years old. Test product used: acne essence, usage: use after cleaning the skin, take an appropriate amount and apply evenly on the acne area, use 2-3 times a day, and clean the acne area before each use.
[0129] The judgment method is to use statistical analysis software to perform statistical analysis on the data to determine whether there is a significant difference.
[0130] Specific tests include but are not limited to: using VISIA skin detector to test the a* value of acne redness and the a* value of skin red area. Using skin imaging measuring instrument Antera3D to test the volume of a single acne and the uniformity of redness of a single acne.
[0131] Test 3.1: Facial Image Analyzer VISIA tests the area of acne red area and the a* value of acne redness
[0132] Specifically, the facial image analyzer VISIA was used to test the baseline value (D0), the test results 1 hour after using the test product (T1h), 8 hours after using the test product (T8h), and 14 days after using the test product (D14).
[0133] Among them, the VISIA acne red area test results are as follows: Table 3 and Table 4, VISIA skin redness a* value results are as follows: Figure 3 Shown
[0134] Table 3. VISIA acne red area detection results
[0135] Test products D0 T1h T8h D14 Anti-acne serum 21.93±1.80 18.61±1.51 18.44±1.62 14.96±1.42
[0136] Table 4. Improvement rate of VISIA acne red area
[0137]
[0138] Combined with Figure 3 , 1 hour after the subjects used the test product acne essence once, the VISIA skin redness a* value decreased significantly compared with the baseline value (p<0.001), and the decrease rate was 4.23%; 8 hours after the subjects used the test product acne essence once, the VISIA skin redness a* value decreased significantly compared with the baseline value (0.001≤p<0.01), and the decrease rate was 4.07%; the subjects used the test product acne essence continuously for 14 days, and the VISIA skin redness a* value decreased significantly compared with the baseline value (p<0.001), and the decrease rate was 6.84%.
[0139] Test 3.2: Antera 3D tests the average redness and volume of a single pimple
[0140] Specifically, using the anti-acne essence of the embodiment of the present invention, Antera 3D was used to capture acne images after using the anti-acne essence for 1 hour, 8 hours and 3 days, and the improvement rate of the volume of a single acne and the average redness of a single acne were determined. The results are shown in the attached figure. Figure 4 , Attachment Figure 5 As shown in Tables 5, 6 and 7 below.
[0141] Table 5. Antera 3D single acne redness average detection results
[0142] Test products Base value (D0) T1h T8h D3 Anti-acne serum 29.28±0.89 27.76±0.72 27.88±0.72 26.53±0.75
[0143] Table 6. Antera 3D single acne redness average improvement rate
[0144]
[0145] Table 7. Antera 3D single acne volume improvement rate test results
[0146]
[0147] One hour after the subjects used the test product acne essence once, the average redness of a single Antera 3D pimple decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 5.19%; 8 hours after the subjects used the test product acne essence once, the average redness of a single Antera 3D pimple decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 4.78%; the subjects used the test product acne essence continuously for 3 days, and the average redness of a single Antera 3D pimple decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 9.39%.
[0148] One hour after the subject used the test acne essence once, the volume of a single pimple of Antera 3D decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 14.34%; 8 hours after the subject used the soothing acne essence once, the volume of a single pimple of Antera 3D decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 19.12%; the subject used the test product acne essence for 3 consecutive days, and the volume of a single pimple of Antera 3D decreased significantly compared with the baseline value (p<0.001), with a decrease rate of 36.65%. The results show that the acne essence with the acne composition of the present invention can effectively reduce the volume of acne.
[0149] The above results show that the acne essence with the acne-removing composition of the present invention has acne-removing effect 8 hours after a single use of the test product acne essence, and continuous use of the test product acne essence for 3 days and 14 days. The test product has a soothing effect 1 hour and 8 hours after a single use of the test product acne essence, and continuous use of the test product acne essence for 14 days.
[0150] Test 3.3: Subject Evaluation
[0151] The subjects conducted self-assessment using a scoring system, with 1 being "strongly disagree", 2 being "disagree", 3 being "average", 4 being "agree", and 5 being "strongly agree". The subjects evaluated product satisfaction, acne removal, and mildness, and confirmed their approval rate. The evaluation table is shown in Table 8 below.
[0152] Table 8. Subject evaluation form
[0153]
[0154]
[0155] Significance marking method: "ns" indicates no statistical difference, p≥0.05; p<0.05 indicates a significant difference ("*" indicates 0.01≤p<0.05; "**" indicates 0.001≤p<0.01; "***" indicates p<0.001).
[0156] The self-evaluation results show that after using the test product acne essence for 14 consecutive days, 96.77% of the subjects believed that the skin's oil secretion was reduced, which balanced the skin's water and oil, and 100.00% of the subjects believed that the oiliness was reduced and had an oil-control effect; 100.00% of the subjects believed that the product was gentle (non-irritating) and safe, and 100.00% of the subjects felt that the product was suitable for sensitive skin; this shows that the test product of the present invention has an oil-control effect, and the test product is gentle and non-irritating and suitable for sensitive skin.
[0157] In summary, the skin care product comprising the anti-acne composition of the present invention has a mild, rapid and effective anti-acne effect.
[0158] The above embodiments are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the claims of the present invention.
Claims
1. A mild acne-removing composition, characterized in that: The invention comprises the following components by weight: 10-25 parts of colloidal sulfur; 70-90 parts of scutellaria baicalensis extract; 0.01-5 parts of encapsulated salicylic acid; and 0.005-0.1 parts of quaternary ammonium salt-73.
2. The mild anti-acne composition according to claim 1, characterized in that: The invention comprises the following components by weight: 15-25 parts of colloidal sulfur; 70-80 parts of Scutellaria baicalensis extract; Packing salicylic acid 0.05-5 parts; Quaternary ammonium salt-73 0.05-0.1 parts.
3. The mild anti-acne composition according to claim 1 or 2, characterized in that: The scutellaria extract is one or more extracts of the flower, leaf and stem of Scutellaria baicalensis.
4. The mild anti-acne composition according to claim 1 or 2, characterized in that: The colloidal sulfur is formed by microemulsion encapsulating nano-sulfur, and the diameter of the colloidal sulfur is between 1 and 1000 nanometers.
5. The mild anti-acne composition according to claim 4, characterized in that: The colloidal sulfur is prepared by the following steps: S1: Weigh sulfur powder with a particle size of 20-100 um and water in a mass ratio of 1: (1.5-9), mix the sulfur powder and water, and stir and disperse to obtain a slurry; S2: Pour the slurry prepared in S1 into a ball mill, and add ball milling media and dispersant for dispersed ball milling; S3: filtering the ball-milled sulfur slurry to remove particulate impurities that have not been dispersed, and obtaining nano-sulfur slurry with a particle size of 5nm-100nm; S4: Take Tween60 and butylene glycol and add them to caprylic acid triglyceride, and stir to form an organic mixture of Tween60 / butylene glycol / caprylic acid triglyceride. Then slowly add the nano sulfur slurry of S3 and stir at a low speed to form colloidal sulfur.
6. The mild anti-acne composition according to claim 3, characterized in that: The preparation method of the scutellaria baicalensis extract comprises: using ionic liquid as an extractant to extract the scutellaria baicalensis flower / leaves / stems, and then centrifuging to obtain the supernatant as the scutellaria baicalensis extract.
7. A method for preparing a mild anti-acne composition, comprising the step of mixing the components of the mild anti-acne composition according to any one of claims 1 to 6.
8. The method for preparing the mild anti-acne composition according to claim 7, characterized in that: The specific preparation method of the mild acne-removing composition comprises: placing the encapsulated salicylic acid, colloidal sulfur, scutellaria baicalensis extract, and quaternary ammonium salt-73 in a container in proportion, placing it in an ultrasonic instrument for ultrasonication, and then using a magnetic stirrer to fully stir at 55-60° C. to obtain the mild acne-removing composition after stirring.
9. Use of the mild anti-acne composition according to any one of claims 1 to 6 in skin care products / cosmetics.
10. A mild anti-acne skin care product, characterized in that: The invention comprises a mild acne-removing composition as described in any one of claims 1 to 6.