Preparation method of mild and efficient blackhead exporting liquid as well as product and application of mild and efficient blackhead exporting liquid

The dual encapsulation of plant extracts and enzymes addresses the inefficiencies of existing blackhead removal methods by providing stable and effective blackhead removal with reduced skin irritation and long-term prevention.

CN120305190APending Publication Date: 2025-07-15GUANGDONG LIYAN BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510539280.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-27
Publication Date
2025-07-15

AI Technical Summary

Technical Problem

The existing blackhead removal products have chemical peeling methods that cause skin barrier damage and physical adsorption methods to not solve the problem in depth, and are prone to blackhead recurrence. It is urgent to develop mild and efficient blackhead removal products.

Method used

The dual embedding release technology is adopted to double-layer embedding treatment of plant extracts and biological enzymes to form a stable embedding structure, slowly release active ingredients to remove oil and blackheads, avoid inhibition of enzyme activity, and combine the use of polysaccharide carriers and calcium chloride solution to enhance stability and activity.

Benefits of technology

It has achieved high blackhead removal efficiency, safe and gentle skin and long-term protection, significantly reducing blackhead recurrence, and improved product stability and activity.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a preparation method of mild and efficient blackhead exporting liquid as well as a product and application thereof, the preparation method comprises the following steps: (1) mixing a plant extract, a polysaccharide carrier and a calcium chloride aqueous solution, carrying out primary embedding treatment, and freeze-drying to obtain a primary embedding structure; and (2) dissolving a biological enzyme in water, adjusting the pH value, adding the primary embedding structure, mixing, adding a polysaccharide carrier and a calcium chloride aqueous solution, mixing, carrying out secondary embedding treatment, and freeze-drying to obtain a dual embedding structure, namely the mild and efficient blackhead exporting liquid. According to the method, a double embedding and releasing technology is adopted, the product can firstly remove grease and blackheads and then minimize pores, and triple breakthrough of blackhead removing efficiency, skin safety and mildness and long-acting protection is achieved.
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Description

Technical Field

[0001] The present invention belongs to the technical field of cosmetics, and particularly relates to a preparation method, product and application of a mild and highly effective blackhead extractor fluid. Background Art

[0002] The formation of blackheads (open comedones) is the initial stage of acne pathogenesis. Its core pathological mechanism is that the pilosebaceous glands secrete excessive oil (mainly triglycerides and squalene), which is mixed with exfoliated keratinocytes (rich in keratin) to form a horny plug. After being oxidized by air, it forms a black lipid hard mass that blocks the pores. The existing blackhead care techniques mainly include chemical peeling and physical adsorption methods.

[0003] The chemical peeling method is to use fruit acid or salicylic acid to dissolve the horny plug in an acidic system. For example, CN119792108A discloses a composition with blackhead removal effect and its application in cosmetics. In this invention, mandelic acid and salicylic acid in it can penetrate deep into the pores to dissolve oil and keratin, thus playing a role in reducing the formation of blackheads. Tea tree essential oil can remove bacteria and dirt in the pores, and can also perform antibacterial and anti-inflammatory functions on the basis of removing blackheads. By adding carboxymethyl yeast glucan, it can reduce the stinging sensation of skin allergy and play a moisturizing role; Portulaca oleracea extract has anti-inflammatory, anti-allergic and skin immune function enhancing effects. When it is used in a composition with blackhead removal effect, it can play an effect of accelerating skin recovery. D-panthenol has the effect of quickly penetrating into the stratum corneum of the skin, and can stimulate the growth of epidermal cells to accelerate the repair of the skin barrier after removing blackheads. Combining with chitosan-based gel can reduce the probability of skin being stimulated and allergic.

[0004] The physical adsorption method is to remove the surface oil by tearing off a mud mask. For example, CN113208943A discloses a composition and its application in the preparation of blackhead removal cosmetics. The composition provided by this invention includes illite, capryloyl glycine and compound amino acids. This composition can achieve mild blackhead removal through physical adsorption, greatly reducing the irritation and burden on the skin of blackhead removal mud products. After gently removing the cutin and blackheads, this invention controls sebum secretion and moisturizes to prevent the recurrence of blackheads, achieving the purpose of long-term inhibition of blackhead recurrence.

[0005] Although the above-mentioned existing technologies all have the effect of removing blackheads, the chemical peeling method is likely to cause the thinning of the epidermal layer and damage the skin barrier due to the use of acids. After cleaning, the pores are temporarily expanded due to the softening of the cutin, and the subsequent blackhead recurrence is even more aggravated. The physical adsorption method cannot fundamentally solve the problem, and excessive tearing is likely to cause skin flushing and sensitivity. Therefore, there is an urgent need to develop a mild and highly effective blackhead removal product to meet the application requirements. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the present invention provides a method for preparing a mild and efficient blackhead removal liquid, a product and an application thereof. The method of the present invention adopts a double embedding and releasing technology, which enables the product to first remove grease and blackheads, and then tighten pores, achieving a triple breakthrough in blackhead removal efficiency, skin safety and mildness, and long-term protection.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a method for preparing a mild and efficient blackhead removal liquid, the preparation method comprising:

[0009] (1) mixing the plant extract, the polysaccharide carrier and the calcium chloride aqueous solution, performing a primary embedding treatment, and freeze-drying to obtain a primary embedding structure;

[0010] (2) The biological enzyme is dissolved in water, the pH is adjusted and then a primary embedding structure is added, a polysaccharide carrier and a calcium chloride aqueous solution are added after mixing, a secondary embedding treatment is performed after mixing, and a double embedding structure is obtained after freeze drying, which is the mild and efficient blackhead extraction solution.

[0011] The method of the present invention can provide a more stable environment for the embedded substance through the double-layer embedding structure, reduce the influence of external factors on the embedded substance, improve the stability and activity of the plant composition and the biological enzyme, and can continuously release the embedded substance for a long time through the embedding release technology to maintain its effective concentration at the site of action. Because most plant compositions contain a large amount of organic acid, the present invention can avoid the mutual reaction between the plant composition and the biological enzyme to cause the inhibition of enzyme activity through the double embedding treatment, thereby making the product more effective in removing oil and blackheads.

[0012] Preferably, the mass ratio of the plant extract, the polysaccharide carrier and the calcium chloride aqueous solution in step (1) is (1-2):(2-4):(2-5).

[0013] Wherein "1-2" can be 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8 or 1.9, etc.;

[0014] "2-4" can be 2.1, 2.3, 2.5, 2.7, 2.9, 3, 3.2, 3.5, 3.7 or 3.9, etc.;

[0015] “2-5” can mean 2.2, 2.5, 2.8, 3, 3.2, 3.5, 3.8, 4, 4.2, 4.5 or 4.8, etc.

[0016] Preferably, the concentration of the calcium chloride aqueous solution is 2-5%, for example, 2.5%, 3%, 3.5%, 4% or 4.5%.

[0017] Preferably, the plant extract in step (1) includes white willow bark extract and / or pancratium maritimum extract.

[0018] Preferably, the plant extract is white willow bark extract and pancratium maritimum extract.

[0019] Preferably, the mass ratio of the white willow bark extract to the pancratium maritimum extract is 1:(0.5 - 1.5), for example, it can be 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1, 1:1.1, 1:1.2, 1:1.3, or 1:1.4, etc.

[0020] In the present invention, the white willow bark extract can loosen the connection of keratinocytes, promote the shedding of the aged cutin layer, gently remove the old cutin cells on the skin surface, make the skin smoother, more delicate and shiny, and improve the problem of skin roughness. The pancratium maritimum extract can promote the metabolism of skin cells, accelerate the shedding of aged cutin, make the skin renewal more smooth, and has a good effect of astringing the skin. When the two are used in combination, they have a synergistic effect, and further make the product have a more significant effect of removing oil and blackheads.

[0021] Preferably, the polysaccharide carrier in step (1) includes chitosan and / or sodium alginate.

[0022] Preferably, the polysaccharide carrier is chitosan and sodium alginate.

[0023] Preferably, the mass ratio of the chitosan to the sodium alginate is 1:(1.5 - 4), for example, it can be 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.5, 1:2.8, 1:3, 1:3.2, 1:3.5, 1:3.7, or 1:3.9, etc.

[0024] Preferably, the primary embedding treatment is carried out in a manner of high-pressure homogenization.

[0025] Preferably, the high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 100 - 200 bar (for example, it can be 110 bar, 130 bar, 150 bar, 170 bar, or 190 bar, etc.), and the homogenization rate is 5 - 15 L / h (for example, it can be 6 L / h, 8 L / h, 10 L / h, 12 L / h, or 14 L / h, etc.).

[0026] Preferably, when freeze-drying in step (1), the temperature is -40°C to -10°C (for example, it can be -15°C, -20°C, -25°C, -30°C, or -35°C, etc.), the vacuum degree is 500 to 900 Pa (for example, it can be 600 Pa, 700 Pa, 800 Pa, or 850 Pa, etc.), and the time is 2 - 5 h (for example, it can be 2.5 h, 3 h, 3.5 h, 4 h, or 4.5 h, etc.).

[0027] Preferably, the bio-enzyme described in step (2) includes alkaline protease and / or alkaline lipase.

[0028] Preferably, the bio-enzyme is alkaline protease and alkaline lipase.

[0029] Preferably, the mass ratio of the alkaline protease to the alkaline lipase is 1:(1.5 - 3), and can be, for example, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.5, 1:2.7 or 1:2.9, etc.

[0030] As a preferred technical solution of the present invention, the bio-enzyme selected is alkaline protease and alkaline lipase. They not only have mild performance, but also have a better targeting effect on the main components of blackheads, triglyceride and keratin, when used in combination.

[0031] Preferably, the material-liquid ratio of the bio-enzyme to water is 5 - 10 g / mL, and can be, for example, 6 g / mL, 7 g / mL, 8 g / mL or 9 g / mL, etc.

[0032] Preferably, the pH in step (2) is adjusted to 10 - 11, and can be, for example, 10.1, 10.3, 10.5, 10.7 or 10.9, etc.

[0033] Preferably, arginine is used to adjust the pH in step (2).

[0034] In the present invention, using arginine to adjust the alkaline system can ensure that alkaline protease and alkaline lipase are in the best active state when released. Moreover, arginine has a mild effect and can enhance the skin barrier function.

[0035] Preferably, the mass ratio of the bio-enzyme to the first embedding structure is 1:(2 - 4), and can be, for example, 1:2.2, 1:2.5, 1:2.8, 1:3, 1:3.2, 1:3.5 or 1:3.8, etc.

[0036] Preferably, the mass ratio of the first embedding structure, the polysaccharide carrier and the calcium chloride aqueous solution in step (2) is (0.5 - 1):(2 - 4):(2 - 5).

[0037] Among them, "0.5 - 1" can be 0.55, 0.6, 0.65, 0.7, 0.75, 0.8, 0.85, 0.9 or 0.95, etc.;

[0038] "2 - 4" can be 2.1, 2.3, 2.5, 2.7, 2.9, 3, 3.2, 3.5, 3.7 or 3.9, etc.;

[0039] "2-5" can be 2.2, 2.5, 2.8, 3, 3.2, 3.5, 3.8, 4, 4.2, 4.5, 4.8, etc.

[0040] Preferably, the polysaccharide carrier in step (2) includes chitosan and / or sodium alginate.

[0041] Preferably, the polysaccharide carrier in step (2) is chitosan.

[0042] Preferably, the concentration of the calcium chloride aqueous solution in step (2) is 2-5%, and can be, for example, 2.5%, 3%, 3.5%, 4%, or 4.5%, etc.

[0043] Preferably, the secondary embedding treatment in step (2) is carried out by high-pressure homogenization;

[0044] Preferably, the high-pressure homogenization is carried out in a high-pressure homogenizer, the pressure of the homogenization is 100-200 bar (for example, it can be 110 bar, 130 bar, 150 bar, 170 bar, or 190 bar, etc.), and the homogenization rate is 5-15 L / h (for example, it can be 6 L / h, 8 L / h, 10 L / h, 12 L / h, or 14 L / h, etc.).

[0045] Preferably, when freeze-drying in step (2), the temperature is -40°C to -10°C (for example, it can be -15°C, -20°C, -25°C, -30°C, or -35°C, etc.), the vacuum degree is 500 to 900 Pa (for example, it can be 600 Pa, 700 Pa, 800 Pa, or 850 Pa, etc.), and the time is 2-5 h (for example, it can be 2.5 h, 3 h, 3.5 h, 4 h, or 4.5 h, etc.).

[0046] Specific point values within the above numerical ranges can all be selected, and will not be elaborated one by one here.

[0047] In a second aspect, the present invention provides a mild and highly efficient blackhead extractor liquid, and the mild and highly efficient blackhead extractor liquid is prepared by using the preparation method as described in the first aspect.

[0048] In a third aspect, the present invention provides an application of the mild and highly efficient blackhead extractor liquid as described in the second aspect in the preparation of cosmetics.

[0049] Preferably, the cosmetics are emulsion, essence, or facial mask;

[0050] Preferably, the addition amount of the mild and highly efficient blackhead extractor liquid in the cosmetics is 0.1-10%, such as 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, or 9%, etc.

[0051] Preferably, the raw material composition of the cosmetic further includes additives, and the additives include any one or a combination of at least two of solvents, emulsifiers, humectants, preservatives, or thickeners.

[0052] Specific point values within the above numerical ranges can all be selected, and will not be elaborated one by one here.

[0053] Compared with the prior art, the present invention has the following beneficial effects:

[0054] The method of the present invention can provide a more stable environment for the encapsulated substance through a double encapsulation structure, reduce its influence by external factors, improve the stability and activity of the plant composition and biological enzyme. Through the encapsulation release technology, the encapsulated substance can be continuously released for a long time to maintain its effective concentration at the action site. Since most plant compositions contain a large amount of organic acids, the present invention can avoid the reaction between the plant composition and the biological enzyme and the resulting inhibition of enzyme activity through double encapsulation treatment, thereby making the oil removal and blackhead removal effects of the product better. Specific Embodiments

[0055] The technical solution of the present invention will be further described below through specific embodiments. Those skilled in the art should understand that the embodiments are only for helping to understand the present invention and should not be regarded as specific limitations on the present invention.

[0056] The sources of some raw materials used in the examples or comparative examples of the present invention are as follows:

[0057] Name Source White willow bark extract Xi'an Weite Biotechnology Co., Ltd. Pancratium maritimum extract Shaanxi Xinkang Biotechnology Co., Ltd. Alkaline protease Nanning Dongheng Huadao Biotechnology Co., Ltd. Alkaline lipase Nanning Dongheng Huadao Biotechnology Co., Ltd.

[0058] The remaining raw materials can be used as long as they are purchased from regular distributors.

[0059] Example 1

[0060] This example provides a mild and highly effective blackhead extractor, and the preparation method of the mild and highly effective blackhead extractor is as follows:

[0061] (1) Mix the plant extract (white willow bark extract and pancratium maritimum extract with a mass ratio of 1:1) with the polysaccharide carrier (chitosan and sodium alginate with a mass ratio of 1:2) evenly, then add an aqueous calcium chloride solution (3% w / v), and mix evenly again. The mass ratio of the plant extract, polysaccharide carrier, and aqueous calcium chloride solution is 1:2:2. After mixing evenly, perform a primary encapsulation treatment on the mixture of white willow bark extract and pancratium maritimum extract in a high-pressure homogenizer. The homogenization pressure is 150 bar, and the homogenization rate is 10 L / h. Then, freeze-dry at -25°C and a vacuum degree of 700 Pa for 4 h, and grind and crush to obtain a primary encapsulation structure;

[0062] (2) Dissolve the bio-enzyme (alkaline protease and alkaline lipase with a mass ratio of 1:2) in water at a material-liquid ratio of 8 g / mL, adjust the pH value to 10.5 ± 0.2 with arginine, then add the primary embedding structure (the added mass is 3 times that of the bio-enzyme) and mix evenly. Then add chitosan and calcium chloride aqueous solution (3% w / v), and mix evenly again. The mass ratio of the primary embedding structure, chitosan and calcium chloride aqueous solution is 0.8:3:4. Uniformly carry out the embedding treatment by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 160 bar, and the homogenization rate is 12 L / h. Then freeze-dry at -20 °C and a vacuum degree of 600 Pa for 3 h. After grinding and pulverizing, a double embedding structure is obtained, that is, a mild and highly efficient blackhead extractor is prepared.

[0063] Example 2

[0064] This example provides a mild and highly efficient blackhead extractor. The preparation method of the mild and highly efficient blackhead extractor is as follows:

[0065] (1) Mix the plant extracts (white willow bark extract and pancratium maritimum extract with a mass ratio of 2:3) with the polysaccharide carrier (chitosan and sodium alginate with a mass ratio of 2:3) evenly, then add calcium chloride aqueous solution (2% w / v), and mix evenly again. The mass ratio of the plant extracts, polysaccharide carrier and calcium chloride aqueous solution is 2:2:5. After being uniform, carry out a primary embedding treatment on the mixture of white willow bark extract and pancratium maritimum extract by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 100 bar, and the homogenization rate is 15 L / h. Then freeze-dry at -15 °C and a vacuum degree of 900 Pa for 2 h. After grinding and pulverizing, a primary embedding structure is obtained;

[0066] (2) Dissolve the bio-enzyme (alkaline protease and alkaline lipase with a mass ratio of 1:3) in water at a material-liquid ratio of 5 g / mL, adjust the pH value to 10.5 ± 0.2 with arginine, then add the primary embedding structure (the added mass is 2 times that of the bio-enzyme) and mix evenly. Then add sodium alginate and calcium chloride aqueous solution (5% w / v), and mix evenly again. The mass ratio of the primary embedding structure, sodium alginate and calcium chloride aqueous solution is 0.5:4:2. Uniformly carry out the embedding treatment by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 200 bar, and the homogenization rate is 5 L / h. Then freeze-dry at -40 °C and a vacuum degree of 500 Pa for 5 h. After grinding and pulverizing, a double embedding structure is obtained, that is, a mild and highly efficient blackhead extractor is prepared.

[0067] Example 3

[0068] This example provides a mild and highly efficient blackhead extractor. The preparation method of the mild and highly efficient blackhead extractor is as follows:

[0069] (1) Mix the plant extracts (white willow bark extract and pancratium maritimum extract with a mass ratio of 2:1) with the polysaccharide carrier (chitosan and sodium alginate with a mass ratio of 1:4) evenly, then add calcium chloride aqueous solution (5% w / v), and mix evenly again. The mass ratio of the plant extracts, the polysaccharide carrier and the calcium chloride aqueous solution is 1:4:2. After mixing evenly, perform a primary embedding treatment on the mixture of white willow bark extract and pancratium maritimum extract by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 200 bar, and the homogenization rate is 5 L / h. Then, freeze-dry at -40 °C and a vacuum degree of 500 Pa for 4 h, and grind and crush to obtain a primary embedding structure;

[0070] (2) Dissolve the bioenzymes (alkaline protease and alkaline lipase with a mass ratio of 2:3) in water at a material-liquid ratio of 10 g / mL, adjust the pH value to 10.5 ± 0.2 with arginine, then add the primary embedding structure (the added mass is 4 times that of the bioenzymes) and mix evenly. Then add chitosan and calcium chloride aqueous solution (2% w / v), and mix evenly again. The mass ratio of the primary embedding structure, chitosan and calcium chloride aqueous solution is 1:2:5. After mixing evenly, perform an embedding treatment by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 100 bar, and the homogenization rate is 15 L / h. Then, freeze-dry at -10 °C and a vacuum degree of 900 Pa for 2 h, and grind and crush to obtain a double embedding structure, that is, a mild and highly efficient blackhead extractor is prepared.

[0071] Example 4

[0072] This example provides a mild and highly efficient blackhead extractor, which is different from Example 1 only in that the plant extract in step (1) of the preparation method is only white willow bark extract, and the amount of the plant extract is kept unchanged, and the remaining steps and process parameters are the same as those in Example 1.

[0073] Example 5

[0074] This example provides a mild and highly efficient blackhead extractor, which is different from Example 1 only in that the plant extract in step (1) of the preparation method is only pancratium maritimum extract, and the amount of the plant extract is kept unchanged, and the remaining steps and process parameters are the same as those in Example 1.

[0075] Example 6

[0076] This example provides a mild and highly efficient blackhead extractor, which is different from Example 1 only in that the polysaccharide carrier in step (1) of the preparation method is only chitosan, and the amount of the polysaccharide carrier is kept unchanged, and the remaining steps and process parameters are the same as those in Example 1.

[0077] Example 7

[0078] This embodiment provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that the polysaccharide carrier in step (1) of the preparation method is only sodium alginate, and the dosage of the polysaccharide carrier remains unchanged, and the remaining steps and process parameters are the same as those of Embodiment 1.

[0079] Embodiment 8

[0080] This embodiment provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that the biological enzyme in step (2) of the preparation method is only alkaline protease, and the dosage of the biological enzyme remains unchanged, and the remaining steps and process parameters are the same as those of Embodiment 1.

[0081] Embodiment 9

[0082] This embodiment provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that the biological enzyme in step (2) of the preparation method is only alkaline lipase, and the dosage of the biological enzyme remains unchanged, and the remaining steps and process parameters are the same as those of Embodiment 1.

[0083] Embodiment 10

[0084] This embodiment provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that sodium bicarbonate is used to adjust the pH to 10.5 ± 0.2 in step (2) of the preparation method, and the remaining steps and process parameters are the same as those of Embodiment 1.

[0085] Comparative Example 1

[0086] This comparative example provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that step (2) is not included in the preparation method, that is, the primary embedding structure is a mild and highly efficient blackhead extractor.

[0087] Comparative Example 2

[0088] This comparative example provides a mild and highly efficient blackhead extractor, which is different from that of Embodiment 1 only in that step (1) is not included in the preparation method, and the method is as follows:

[0089] Dissolve the bio-enzyme (alkaline protease and alkaline lipase with a mass ratio of 1:2) in water at a material-liquid ratio of 8 g / mL, adjust the pH value to 10.5 ± 0.2 with arginine, add a plant extract (white willow bark extract and pancratium maritimum extract with a mass ratio of 1:1) that is 3 times the mass of the bio-enzyme, mix well, then add chitosan and calcium chloride aqueous solution (3% w / v), and mix well again. The mass ratio of the plant extract, chitosan, and calcium chloride aqueous solution is 0.8:3:4, and the mixture is uniformly embedded by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 160 bar, and the homogenization rate is 12 L / h. Then, freeze-dry at -20 °C and a vacuum degree of 600 Pa for 3 h, grind and crush to obtain an embedded structure, that is, a mild and highly efficient blackhead extractor is prepared.

[0090] Comparative Example 3

[0091] This comparative example provides a mild and highly efficient blackhead extractor, and its preparation method is as follows:

[0092] Dissolve the bio-enzyme (alkaline protease and alkaline lipase with a mass ratio of 1:3) in water at a material-liquid ratio of 5 g / mL, adjust the pH value to 10.5 ± 0.2 with arginine, then add sodium alginate and calcium chloride aqueous solution (5% w / v), and mix well again. The mass ratio of the bio-enzyme, sodium alginate, and calcium chloride aqueous solution is 1:2:2, and the mixture is uniformly embedded by high-pressure homogenization. The high-pressure homogenization is carried out in a high-pressure homogenizer. The pressure of the homogenization is 200 bar, and the homogenization rate is 5 L / h. Then, freeze-dry at -40 °C and a vacuum degree of 500 Pa for 5 h, grind and crush to obtain a double-embedded structure, that is, a mild and highly efficient blackhead extractor is prepared.

[0093] Test Example 1 Skin Oil Content Test

[0094] Experimental principle: The oil test is based on the photometer principle. A special extinction tape with a thickness of 0.1 mm is selected, which can quickly absorb the oil on the human skin. Due to the effect of the oil, the extinction tape becomes semi-transparent. The more oil is absorbed, the greater the light transmittance. The light transmittance is measured with a photometer, and the skin oil content can be measured according to the change in the light transmittance before and after the extinction tape.

[0095] Test instrument: Sebumeter, a grease test probe of cuotometer MPA580 manufactured by Courage + Khazaka GmbH (German CK company).

[0096] Test method: 130 volunteers aged 20-30 with many blackheads on the nose were randomly divided into 13 groups, each with 10 people, in a test room with a temperature of 25±1°C and a relative humidity of 50±5%. Each group took the samples in Examples 1-10 and Comparative Examples 1-3 to wipe the nose and massage in circles for 5 circles. The test site was tested 3 times using a skin oil test probe, and the average value was taken. The measured values were statistically analyzed, and the mean method was used to analyze the change pattern and persistence of nose skin oil secretion.

[0097] The results of the oil content of the nose skin before use and 10 minutes and 30 minutes after use are shown in Table 1:

[0098] Table 1

[0099]

[0100]

[0101] Test Example 2 Blackhead Removal Effect Test

[0102] Test instrument: Visia-cr test instrument.

[0103] Test method: 130 volunteers aged 20-30 with many blackheads on the nose (the same group of volunteers as in Test Example 1) were selected and randomly divided into 13 groups, with 10 people in each group, in a test room with a temperature of 25±1°C and a relative humidity of 50±5%. Visia-CR was used in standard light mode to take macroscopic images of the target targets on the front faces of the subjects, analyze the number of blackheads in the target area, and record the initial value. Then each group tried to wipe the nose with the samples in Examples 1-10 and Comparative Examples 1-3, massaged in circles for 5 circles, and tested the number of blackheads in the target area after 10 minutes and 30 minutes, respectively, and used SPSS statistical software to analyze and calculate the rate of change.

[0104] Blackhead number change rate = (blackhead number after using the sample for x minutes - initial blackhead number) / initial blackhead number × 100%.

[0105] The change rate of the number of blackheads is shown in Table 2:

[0106] Table 2

[0107]

[0108]

[0109] Note: "-" in the table indicates that the number of blackheads decreased, and the observed difference was statistically significant (p < 0.05).

[0110] Test Example 3: Evaluation of blackhead removal effect

[0111] Test method: Select 130 volunteers aged 20 - 30 with more blackheads on the nose tip (the same batch of volunteers as in Test Example 1). In a test chamber with a temperature of 25 ± 1°C and a relative humidity of 50 ± 5%, randomly divide them into 13 groups, with 10 people in each group. For each group, take the samples in Examples 1 - 10 and Comparative Examples 1 - 3 and wipe the nose tip area, massage in circles for 5 rounds, use once a week for 4 consecutive weeks, test the blackhead removal effect, score on a ten-point scale, and take the average value of the test results (retain two decimal places). The higher the score, the more significant the blackhead removal effect. See Table 3.

[0112] Table 3

[0113]

[0114]

[0115] From the data in Tables 1 - 3, it can be seen that: The mild and highly efficient blackhead extract obtained by the method of the present invention in Examples 1 - 3 adopts a double embedding and release technology, which can remove oil, clear blackheads, and shrink pores, achieving a high blackhead removal efficiency.

[0116] From Examples 4 - 5, it can be seen that the synergistic cooperation of the salix alba bark extract and the pancratium maritimum extract can better promote the shedding of the aging cutin layer, and thus the product has better oil removal and blackhead removal effects.

[0117] From Examples 6 - 7, it can be seen that only when chitosan and sodium alginate are used in the primary embedding treatment can the plant extract be better isolated from the biological enzyme, and thus the two will not react with each other to affect the effect of the product.

[0118] From Examples 8 - 9, it can be seen that only the combined use of alkaline protease and alkaline lipase can target triglyceride and keratin, the main components of blackheads.

[0119] From Example 10, it can be seen that arginine can protect the biological enzyme to make it in the best active state, and thus improve the blackhead removal effect of the product.

[0120] From Comparative Examples 1 and 3, it can be seen that the plant extract and the biological enzyme can better improve the blackhead removal efficacy of the product when used in combination with double embedding.

[0121] From Comparative Example 2, it can be seen that when the plant extract and the biological enzyme are not double-embedded, they will have an inhibitory effect on each other, thus affecting the performance of the product.

[0122] Test Example 4: Irritation test

[0123] Select 30 volunteers aged 18 - 35, and each subject tries the products in Examples 1 - 10 for a skin patch test.

[0124] Test method: Select a qualified patch tester. Using the closed patch test method, add approximately 0.020 mL - 0.025 mL of the test sample to the patch tester, and apply it to the flexor side of the subject's forearm with a special external tape. After 24 hours, remove the test substance. Observe the skin reaction at 30 minutes, 24 hours, and 48 hours after removal respectively, and record the results according to the skin reaction grading standard (Table 4) in the "Technical Specifications for Cosmetics Safety" (2015 Edition).

[0125] Table 4 Skin reaction grading standard for skin closed patch test

[0126]

[0127] The patch test results are shown in Table 5 as follows:

[0128] Table 5 Skin patch test results

[0129] Sample Grade 0 Grade 1 Grade 2 Grade 3 Grade 4 Example 1 30 people 0 people 0 people 0 people 0 people Example 2 30 people 0 people 0 people 0 people 0 people Example 3 30 people 0 people 0 people 0 people 0 people Example 4 30 people 0 people 0 people 0 people 0 people Example 5 30 people 0 people 0 people 0 people 0 people Example 6 30 people 0 people 0 people 0 people 0 people Example 7 30 people 0 people 0 people 0 people 0 people Example 8 30 people 0 people 0 people 0 people 0 people Example 9 30 people 0 people 0 people 0 people 0 people Example 10 30 people 0 people 0 people 0 people 0 people

[0130] As can be seen from the data in Table 5, the mild and highly efficient blackhead extract provided in Examples 1 - 10 of the present invention is safe and non - irritating, indicating that the product provided by the present invention is milder in use and will not cause harm to the skin.

[0131] The applicant declares that the present invention uses the above - mentioned examples to illustrate a preparation method, its product and application of a mild and highly efficient blackhead extract of the present invention. However, the present invention is not limited to the above - mentioned examples, that is, it does not mean that the present invention must rely on the above - mentioned examples to be implemented. Those skilled in the art should understand that any improvement of the present invention, the equivalent substitution of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and the disclosure scope of the present invention.

[0132] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above - mentioned embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0133] In addition, it should be noted that in the various specific technical features described in the above - mentioned specific embodiments, they can be combined in any appropriate way without contradiction. To avoid unnecessary repetition, the present invention will not separately describe various possible combination methods.

Claims

1. A preparation method of a mild and highly efficient blackhead extractor, characterized in that The preparation method includes: (1) Mix the plant extract, polysaccharide carrier and calcium chloride aqueous solution, conduct a primary embedding treatment, and obtain a primary embedded structure after freeze-drying; (2) Dissolve the bio-enzyme in water, adjust the pH, add the primary embedded structure, add the polysaccharide carrier and calcium chloride aqueous solution after mixing, conduct a secondary embedding treatment after mixing, and obtain a double-embedded structure after freeze-drying, which is the mild and highly efficient blackhead removing liquid.

2. The preparation method according to claim 1, characterized in that, In step (1), the mass ratio of the plant extract, polysaccharide carrier and calcium chloride aqueous solution is (1-2):(2-4):(2-5); Preferably, the concentration of the calcium chloride aqueous solution is 2-5%.

3. The preparation method according to claim 1 or 2, characterized in that The plant extract in step (1) includes white willow bark extract and / or pancratium maritimum extract; Preferably, the plant extract is white willow bark extract and pancratium maritimum extract; Preferably, the mass ratio of the white willow bark extract to the pancratium maritimum extract is 1:(0.5-1.5).

4. The preparation method according to any one of claims 1-3, characterized in that, The polysaccharide carrier in step (1) includes chitosan and / or sodium alginate; Preferably, the polysaccharide carrier is chitosan and sodium alginate; Preferably, the mass ratio of chitosan to sodium alginate is 1:(1.5-4).

5. The preparation method according to any one of claims 1-4, characterized in that, The primary embedding treatment is carried out in a high-pressure homogenization manner; Preferably, the high-pressure homogenization is carried out in a high-pressure homogenizer, the homogenization pressure is 100-200 bar, and the homogenization rate is 5-15 L / h; Preferably, during the freeze-drying, the temperature is -40°C to -10°C, the vacuum degree is 500 to 900 Pa, and the time is 2-5 h.

6. The preparation method according to any one of claims 1-5, characterized in that, The bio-enzyme in step (2) includes alkaline protease and / or alkaline lipase; Preferably, the bio-enzyme is alkaline protease and alkaline lipase; Preferably, the mass ratio of the alkaline protease to the alkaline lipase is 1:(1.5-3); Preferably, the material-liquid ratio of the bio-enzyme to water is 5-10 g / mL.

7. The preparation method according to any one of claims 1-6, characterized in that, In step (2), the pH is adjusted to 10-11; Preferably, in step (2), arginine is used to adjust the pH; Preferably, the mass ratio of the bio-enzyme to the primary embedded structure is 1:(2-4).

8. The preparation method according to any one of claims 1-7, characterized in that, In step (2), the mass ratio of the primary embedded structure, polysaccharide carrier and calcium chloride aqueous solution is (0.5-1):(2-4):(2-5); Preferably, the polysaccharide carrier in step (2) includes chitosan and / or sodium alginate; Preferably, the concentration of the calcium chloride aqueous solution in step (2) is 2-5%; Preferably, the secondary embedding treatment in step (2) is carried out in a high-pressure homogenization manner; Preferably, the high-pressure homogenization is carried out in a high-pressure homogenizer, the homogenization pressure is 100-200 bar, and the homogenization rate is 5-15 L / h; Preferably, during the freeze-drying in step (2), the temperature is -40°C to -10°C, the vacuum degree is 500 to 900 Pa, and the time is 2-5 h.

9. A mild and highly efficient blackhead extractor, characterized in that, The mild and highly efficient blackhead removing liquid is prepared by using the preparation method described in any one of claims 1-8.

10. Use of a mild and highly efficient blackhead removing liquid as described in claim 9 in the preparation of cosmetics.

Citation Information

Patent Citations

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