Multi-channel high-efficiency oil-control acne-removal composition and application of multi-channel high-efficiency oil-control acne-removal composition in cosmetics

Abstract

The invention relates to the field of cosmetics, in particular to a multi-channel efficient oil-control acne-removal composition and application thereof in cosmetics. The oil-controlling and acne-removing composition is prepared from the following components in parts by weight: 1 to 5 parts of capryloyl salicylic acid, 0.5 to 2 parts of magnolol and 0.5 to 10 parts of white willow bark extract. Capryloyl salicylic acid, magnolol and white willow bark extract are compounded to achieve a synergistic effect, so that the oil-control acne-removing composition has remarkable oil-control acne-removing effects and can be applied to cosmetics of different dosage forms. In addition, the invention also discovers that after the white willow bark extract is subjected to enzyme modification, the oil control and acne removal effects of the white willow bark extract can be further improved.

Description

Technical Field

[0001] The invention relates to the field of cosmetics, and in particular to a multi-channel high-efficiency oil-controlling and acne-removing composition and application thereof in cosmetics. Background Art

[0002] Excessive facial oil secretion is basically seborrhea. Seborrhea is mainly caused by overactive facial sebaceous glands, which leads to a large amount of sebum secretion. Areas with large pores are more likely to secrete excess oil, which may cause oily facial symptoms. The main reason for overactive sebaceous glands is the stimulation of dihydrotestosterone, which happens to be a component of male hormones. The formation of these male hormones is caused by genetic factors, or by the body staying up late and not getting enough sleep, and often eating spicy and irritating foods, which leads to excessive secretion of male hormones, especially dihydrotestosterone, which stimulates the sebaceous glands to form too much sebum. Excessive sebum secretion will then cause more skin diseases, which are common in the formation of open comedones, which further deteriorate to form acne.

[0003] According to a survey, 75-90% of adolescents and young adults suffer from acne, nearly 10-20% of people aged 25-35 still have acne, and 5% of men and women still have acne until the age of 45. The appearance of acne brings great distress to people and will bring a variety of complications.

[0004] Many oil-control and acne-removing products contain strong cleansing ingredients, such as alcohol and benzoic acid. Although they can effectively remove oil, long-term use may cause dryness and dehydration of the skin. When the skin is dry, it will secrete more oil to protect itself, which may form a vicious cycle of more oil and more oil. Many oil-control and acne-removing products can only temporarily relieve symptoms, but cannot fundamentally solve the problem. Once discontinued, acne and oiliness may reappear, which is only a temporary solution. Summary of the invention

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide an oil-controlling and acne-removing composition, which has a significant oil-controlling and acne-removing effect and can be applied to cosmetics.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] In a first aspect, the present invention provides an oil-controlling and anti-acne composition, comprising the following components in parts by weight: 1-5 parts of octanoylsalicylic acid, 0.5-2 parts of magnolol, and 0.5-10 parts of white willow bark extract.

[0008] Capryloyl salicylic acid has the effects of exfoliation, anti-inflammatory, and regulating oil secretion. It can penetrate deep into the pores, help remove dead skin cells, reduce the formation of acne and blackheads; reduce redness and inflammation, which is beneficial to acne skin; control excessive oil secretion and prevent pores from being blocked. Magnolia phenol has antibacterial and antiviral, antioxidant, anti-inflammatory and sedative effects, has a strong antibacterial effect, and helps inhibit the growth of microorganisms that cause skin infections; can remove free radicals and protect the skin from damage by environmental stress; relieve skin irritation and discomfort. White willow bark extract is a natural source of salicylic acid, contains rich salicylic acid derivatives, and has anti-inflammatory and antipyretic effects similar to aspirin; it also has anti-inflammatory and analgesic effects: it has a significant effect on relieving skin inflammation and pain. The present invention compounds the three components, synergistically, can comprehensively exert the effects of the components, has a significant oil control and acne removal effect, and can effectively improve or treat skin problems.

[0009] Preferably, the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0010] Preferably, the willow bark extract comprises unmodified willow bark extract and / or enzyme-modified willow bark extract; and the enzyme comprises at least one of β-glucosidase, β-glucanase and xylanase.

[0011] White willow is a plant species recognized in the art as having potential for food, medicine and cosmetics. There have been many studies on the properties of its bark extract. In order to improve the repair effect of white willow bark extract, the present invention performs ultrasonic extraction and enzyme modification on it, and it is found that enzyme modification has a positive effect on the efficacy of white willow bark extract.

[0012] More preferably, the white willow bark extract is obtained by modification with β-glucosidase.

[0013] β-glucosidase is an important component of cellulase, exists in many plants, and is related to the relaxation or reinforcement of cell walls during the growth and development of plant cells, and is also related to the signal recognition of plant cells and the production of some signal molecules. The present invention uses β-glucosidase to modify the white willow bark extract. Under the action of the enzyme, many precursor substances in the white willow bark, such as salicylic acid glycosides and active ingredients in bonded volatile substances, can be better released, so that the white willow bark extract can better exert its efficacy.

[0014] Preferably, the preparation method of the unmodified willow bark extract comprises the following steps: adding water to willow bark to obtain a willow bark water extract, concentrating, adding isochorismate synthase to assist, stirring and adding ethanol, sealing and standing, filtering and recovering ethanol, and drying to obtain a powder which is the willow bark extract.

[0015] Preferably, the preparation method of the unmodified willow bark extract specifically comprises the following steps:

[0016] Add five times the mass of deionized water to the crushed white willow bark for extraction, control the temperature between 50-60°C, and stir for 10-20 minutes; let it stand for 180-240 minutes, perform ultrasonic treatment for 10 minutes every 20 minutes during this period to help separate the effective components, obtain the white willow bark water extract, concentrate it to 1: (1-2) (mL: g), add 0.2% isochorismate synthase (ICS1) for assistance, cool it, slowly add ethanol while stirring to reach the specified alcohol content (more than 75%), seal it and refrigerate it for 24-48 hours, filter it, recover ethanol from the filtrate to obtain a refined solution, dry it, and the obtained powder is the white willow bark extract.

[0017] Preferably, the preparation method of the enzyme-modified willow bark extract comprises the following steps: (1) adding water to willow bark to obtain a willow bark water extract, concentrating it, adding isochorismate synthase to assist, stirring and adding ethanol, sealing and standing it, filtering and recovering the ethanol, drying to obtain a powder, and adding water to prepare an aqueous solution; (2) adding enzyme modification treatment to the aqueous solution obtained in step (1), concentrating it, and freeze-drying it to obtain the willow bark extract.

[0018] The present invention uses white willow widely cultivated in Xinjiang, China as raw material, uses water extraction and alcohol precipitation method to extract the white willow (SALIXALBA) bark water extract, which is prepared by the applicant of the present invention, adds 0.2% isochorismate synthase (ICS1) to assist in the extraction, uses microwave drying technology, and the dried water extract is brown or grayish white fine powder. The content of salicylic acid glycoside in the white willow bark water extract powder is greater than 18%.

[0019] Preferably, the concentration of the aqueous solution is 8-12% w / v.

[0020] 8-12 g of the obtained powder is dissolved in water to prepare an aqueous solution with a concentration of 8-12% w / v.

[0021] Preferably, in step (2), the enzyme concentration is 500-800 U / mL.

[0022] More preferably, in step (2), the enzyme concentration is 700 U / mL.

[0023] Preferably, in step (2), the conditions for enzyme treatment are: adjusting the pH to 5.0-6.0 and treating at 50-60° C. for 1-3 h.

[0024] The present invention has been found through research that within a certain pH range, the enzymatic reaction rate of plant enzymes increases with the increase of pH; but when the pH increases to a certain limit, the enzymatic reaction rate not only stops accelerating but decreases with the increase of pH. The present invention has found that the enzyme activity is optimal when the pH is 5.0-6.0, which is the optimal pH range for the enzyme reaction.

[0025] More preferably, in step (2), the conditions for enzyme treatment are: adjusting the pH to 5.5 and treating at 55° C. for 2 h.

[0026] Preferably, in step (2), the enzyme treatment is followed by treatment at 90° C. for 3-6 minutes to inactivate the enzyme.

[0027] In a second aspect, the present invention provides use of the above-mentioned oil-controlling and acne-removing composition in cosmetics.

[0028] In a third aspect, the present invention provides a cosmetic comprising the above-mentioned oil-controlling and acne-removing composition.

[0029] Preferably, the cosmetics also include auxiliary materials required for daily chemical products.

[0030] Preferably, the auxiliary materials include emulsifiers, skin conditioners, moisturizers, antioxidants, thickeners, emollients, and pH regulators.

[0031] Preferably, the emulsifier includes PEG-80 sorbitan laurate; the skin conditioner includes Centella asiatica extract; the moisturizer includes at least one of butylene glycol, 1,2-hexanediol, and glycerol; the antioxidant includes parahydroxyacetophenone; the thickener includes at least one of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, sodium polyacryloyldimethyl taurate, and Caesalpinia spinosa gum; the emollient includes polydimethylsiloxane and caprylic / capric triglyceride; the pH adjuster includes sodium hydroxide.

[0032] The beneficial effects of the present invention are:

[0033] After the present invention compounds capryloyl salicylic acid, magnolol and white willow bark extract, the three components can act synergistically, have significant oil control and acne removal effects, and can be applied to cosmetics of different dosage forms. In addition, the present invention also finds that after the white willow bark extract is enzyme-modified, its oil control and acne removal effects can be further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 Effects of unmodified / enzyme-modified white willow bark extract on the survival rate of SZ95 cells.

[0035] Figure 2Effect of unmodified / enzyme-modified white willow bark extract on the inhibition rate of Staphylococcus aureus.

[0036] Figure 3 Effects of unmodified / enzyme-modified white willow bark extract on the inhibition rate of Propionibacterium acnes. DETAILED DESCRIPTION

[0037] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0038] Unless otherwise specified, the raw materials used in the present invention can be purchased from the market.

[0039] Isochorismate synthase (ICS1), β-glucosidase, β-glucanase, and xylanase were purchased from Shanghai Yuanye, Wuhan Huaxiang Kejie and other manufacturers, all of which were food grade.

[0040] The raw materials of the cosmetics used in the present invention are cosmetic grade.

[0041] The raw material of Salix Alba bark extract is Salix Alba widely cultivated in Xinjiang, China. The extraction method is to use water extraction and alcohol precipitation method, and 0.2% isochorismate synthase (ICS1) is added to assist in the extraction. The content of salicylic acid glycoside in the extract is>18%. Capryloyl salicylic acid was purchased from Shanghai Bilai Chemical Technology Co., Ltd., and magnolol was purchased from Hunan Heguang Biotechnology Co., Ltd.

[0042] Embodiment 1:

[0043] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0044] The white willow bark extract is obtained by water extraction and alcohol precipitation.

[0045] The preparation method of the white willow bark extract (using water extraction and alcohol precipitation method, with enzyme assistance) comprises the following steps:

[0046] Add five times the mass of deionized water to the crushed white willow bark for extraction, control the temperature between 50-60°C, and stir for 10-20 minutes; let it stand for 180-240 minutes, perform ultrasonic treatment for 10 minutes every 20 minutes during this period to help separate the effective components, obtain the white willow bark water extract, concentrate it to 1: (1-2) (mL: g), add 0.2% isochorismate synthase (ICS1) for assistance, cool it, slowly add ethanol while stirring to reach the specified alcohol content (more than 75%), seal it and refrigerate it for 24-48 hours, filter it, recover ethanol from the filtrate to obtain a refined solution, and dry the obtained powder to obtain the white willow bark extract.

[0047] Embodiment 2:

[0048] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0049] The white willow bark extract is obtained by modification with beta-glucosidase.

[0050] The preparation method of the white willow bark extract comprises the following steps: (1) adding five times the mass of deionized water to the crushed white willow bark for extraction, controlling the temperature between 50-60° C., and stirring for 10-20 minutes; standing for 180-240 minutes, performing ultrasonic treatment for 10 minutes every 20 minutes to help separate the effective components, obtaining a white willow bark water extract, concentrating to 1: (1-2) (mL: g), adding 0.2% isochorismate synthase (ICS1 ) assisted by a mixing device, after cooling, slowly adding ethanol while stirring to reach a specified alcohol content (75% or more), sealing and refrigerating for 24-48 hours, filtering, recovering ethanol from the filtrate to obtain a refined solution, drying to obtain a powder, adding water to prepare a 10% w / v aqueous solution; (2) adding 700 U / mL of β-glucosidase to the aqueous solution in step (1), adjusting the pH to 5.5, treating at 55°C for 2 hours, then treating at 90°C for 5 minutes to inactivate the enzyme, concentrating, and freeze-drying to obtain the white willow bark extract.

[0051] Embodiment 3:

[0052] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0053] The white willow bark extract is obtained by modifying with beta-glucanase.

[0054] The preparation method of the white willow bark extract comprises the following steps: (1) adding five times the mass of deionized water to the crushed white willow bark for extraction, controlling the temperature between 50-60° C., and stirring for 10-20 minutes; standing for 180-240 minutes, performing ultrasonic treatment for 10 minutes every 20 minutes to help separate the effective components, obtaining a white willow bark water extract, concentrating to 1: (1-2) (mL: g), adding 0.2% isochorismate synthase (ICS) 1) after cooling, slowly adding ethanol while stirring to reach a specified alcohol content (75% or more), sealing and refrigerating for 24-48 hours, filtering, recovering ethanol from the filtrate to obtain a refined solution, drying to obtain a powder, adding water to prepare a 10% w / v aqueous solution; (2) adding 700 U / mL of β-glucanase to the aqueous solution in step (1), adjusting the pH to 5.5, treating at 55° C. for 2 hours, then treating at 90° C. for 5 minutes to inactivate the enzyme, concentrating, and freeze-drying to obtain the white willow bark extract.

[0055] Embodiment 4:

[0056] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0057] The white willow bark extract is obtained by modifying with xylanase.

[0058] The preparation method of the white willow bark extract comprises the following steps: (1) adding five times the mass of deionized water to the crushed white willow bark for extraction, controlling the temperature between 50-60° C., and stirring for 10-20 minutes; standing for 180-240 minutes, performing ultrasonic treatment for 10 minutes every 20 minutes to help separate the effective components, obtaining a white willow bark water extract, concentrating to 1: (1-2) (mL: g), adding 0.2% isochorismate synthase (IC S1) after cooling, slowly adding ethanol while stirring to reach a specified alcohol content (75% or more), sealing and refrigerating for 24-48 hours, filtering, recovering ethanol from the filtrate to obtain a refined liquid, drying to obtain a powder, adding water to prepare a 10% w / v aqueous solution; (2) adding 700 U / mL of xylanase to the aqueous solution in step (1), adjusting the pH to 5.5, treating at 55° C. for 2 hours, then treating at 90° C. for 5 minutes to inactivate the enzyme, concentrating, and freeze-drying to obtain the white willow bark extract.

[0059] Embodiment 5:

[0060] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol, and 1.2 parts of white willow bark extract.

[0061] The white willow bark extract is a conventional commercially available product purchased from Bozhou Xier Chinese Herbal Medicine Co., Ltd. and is prepared using only a water extraction and alcohol precipitation method.

[0062] Embodiment 6:

[0063] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 1 part of octanoylsalicylic acid, 0.5 parts of magnolol, and 10 parts of white willow bark extract.

[0064] The white willow bark extract is obtained by modification with beta-glucosidase.

[0065] The preparation of the willow bark extract is the same as in Example 2.

[0066] Embodiment 7:

[0067] An embodiment of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 5 parts of octanoylsalicylic acid, 2 parts of magnolol, and 0.5 parts of white willow bark extract.

[0068] The white willow bark extract is obtained by modification with beta-glucosidase.

[0069] The preparation of the willow bark extract is the same as in Example 2.

[0070] Comparative Example 1:

[0071] A comparative example of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition comprises the following components in parts by weight: 6 parts of octanoylsalicylic acid, 3 parts of magnolol, and 12 parts of white willow bark extract.

[0072] The white willow bark extract is obtained by modification with beta-glucosidase.

[0073] The preparation of the willow bark extract is the same as in Example 2.

[0074] Comparative Example 2:

[0075] A comparative example of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition of this comparative example is different from that of Example 2 only in that: this comparative example does not add magnolol, but replaces it with an equal weight portion of water.

[0076] Comparative Example 3:

[0077] A comparative example of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition of this comparative example is different from that of Example 2 only in that: this comparative example does not add white willow bark extract, but replaces it with an equal weight portion of water.

[0078] Comparative Example 4:

[0079] A comparative example of the oil-controlling and anti-acne composition of the present invention; the oil-controlling and anti-acne composition of this comparative example is different from that of Example 2 only in that capryloyl salicylic acid is not added in this comparative example, and is replaced by an equal weight portion of water.

[0080] Application Example 1:

[0081] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0082] The cosmetic comprises the following components in percentage by weight: 0.5% of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 0.4% of sodium polyacryloyldimethyl taurate, 0.2% of caesalpinia spirosa gum, 9% of glycerin, 5% of butylene glycol, 0.5% of polydimethylsiloxane, 0.8% of caprylic / capric triglyceride, 0.1% of sodium hydroxide, 0.45% of p-hydroxyacetophenone, 0.5% of 1,2-hexanediol, 10% of an oil-controlling and anti-acne composition pre-phase, and the balance being water.

[0083] The pre-phase of the oil-control and anti-acne composition comprises the following components in percentage by weight: 4.2% of the oil-control and anti-acne composition of Example 1, 1.5% of PEG-80 sorbitan laurate, 1.2% of Centella asiatica extract, 5% of butylene glycol, 0.45% of p-hydroxyacetophenone, 5% of 1,2-hexanediol, 10% of glycerol, and the balance is water.

[0084] The preparation method of the oil-controlling and anti-acne cosmetic comprises the following steps:

[0085] (1) Preparation of a preformed phase of an oil-controlling and anti-acne composition: ① The oil-controlling and anti-acne composition, PEG-80 sorbitan laurate, and butylene glycol are mixed and heated to completely dissolve; ② Centella asiatica extract, p-hydroxyacetophenone, 1,2-hexanediol, glycerin, and water are added, and the mixture is stirred at 80-85° C. to uniformly disperse the mixture, and the mixture is stirred to return to room temperature to obtain the preformed phase of the oil-controlling and anti-acne composition.

[0086] (2) Preparation process of essence: ① Mix and stir acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, sodium polyacryloyl dimethyl taurate, caesalpinia spirosa gum and glycerin to obtain mixture A; ② Add butylene glycol, p-hydroxyacetophenone, 1,2-hexanediol and water to mixture A, heat to 80-85° C., homogenize and disperse to obtain mixture B; ③ Add polydimethylsiloxane and caprylic / capric triglyceride to mixture B, homogenize and emulsify to obtain mixture C, stir and cool to obtain mixture C; ④ Cool to 50-55° C., add sodium hydroxide to mixture C, stir and disperse to obtain mixture C, continue to stir and cool; cool to 30-40° C., add the oil control and anti-acne composition pre-phase obtained in step (1), stir and disperse to obtain mixture B, discharge to obtain the oil control and anti-acne cosmetic (essence).

[0087] Application Example 2:

[0088] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0089] The difference between this application example and application example 1 is that the oil-controlling and anti-acne composition of application example 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of application example 2, and the remaining components and contents are the same as those of application example 1. Application example 3:

[0090] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0091] The difference between this application example and application example 1 is that the oil-controlling and anti-acne composition of embodiment 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of embodiment 3, and the remaining components and contents are the same as those of application example 1. Application example 4:

[0092] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0093] The difference between this application example and application example 1 is that the oil-controlling and anti-acne composition of embodiment 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of embodiment 4, and the remaining components and contents are the same as those of application example 1. Application example 5:

[0094] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0095] The difference between this application example and application example 1 is that the oil-controlling and anti-acne composition of embodiment 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of embodiment 5, and the remaining components and contents are the same as those of application example 1. Application example 6:

[0096] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0097] The only difference between this application example and application example 1 is that 4.2% of the oil-controlling and anti-acne composition of embodiment 1 is replaced by 11.5% of the oil-controlling and anti-acne composition of embodiment 6, and the remaining components and contents are the same as those in application example 1.

[0098] Application Example 7:

[0099] An application embodiment of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0100] The only difference between this application example and application example 1 is that 4.2% of the oil-controlling and anti-acne composition of embodiment 1 is replaced by 7.5% of the oil-controlling and anti-acne composition of embodiment 7, and the remaining components and contents are the same as those in application example 1.

[0101] Application Comparative Example 1:

[0102] A comparative application example of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0103] The difference between this application comparative example and application example 1 is only that 4.2% of the oil-controlling and anti-acne composition of example 1 is replaced by 21% of the oil-controlling and anti-acne composition of comparative example 1, and the remaining components and contents are the same as those of application example 1.

[0104] Application Comparative Example 2:

[0105] A comparative application example of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0106] The difference between this comparative example and application example 1 is that the oil-controlling and anti-acne composition of example 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of comparative example 2, and the remaining components and contents are the same as those of application example 1. Application comparative example 3:

[0107] A comparative application example of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0108] The difference between this comparative application example and application example 1 is that the oil-controlling and anti-acne composition of example 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of comparative example 3, and the remaining components and contents are the same as those of application example 1. Application comparative example 4:

[0109] A comparative application example of the cosmetics of the present invention; the cosmetics is specifically an essence.

[0110] The difference between this comparative example and Example 1 is that the oil-controlling and anti-acne composition of Example 1 is replaced with an equal amount of the oil-controlling and anti-acne composition of Comparative Example 4, and the remaining components and contents are the same as those of Example 1. Test Example 1: Performance Evaluation of Salix alba Bark Extract

[0111] Test sample: unmodified / enzyme-modified white willow bark extract in the oil-controlling and anti-acne composition described in Examples 1-4.

[0112] 1. After obtaining the white willow bark extract, use HPLC for verification.

[0113] (1.1) Instruments and reagents

[0114] Agilent infinite 1260Ⅱ with diode array detector, Agilent ZORBAX SB-C18 (150mm×4.6mm, 5μm), KQ-250 ultrasonic cleaner (Jiangsu Kunshan Ultrasonic Instrument Factory). Salicin reference substance (content 99%, provided by Sigma, USA) white willow bark extract (produced by Xi'an Haotian Bioengineering Technology Co., Ltd.), acetonitrile of analytical grade, water of double distilled water.

[0115] (1.2) Methods and Results

[0116] (1.2.1) Chromatographic conditions:

[0117] Chromatographic column: Inertsil ODS-3 (150 mm × 4.6 mm, 5 μm);

[0118] Mobile phase: acetonitrile-water (5:95); flow rate: 1.0 mL / min; detection wavelength: 269 nm; column temperature: 25°C.

[0119] (1.2.2) Preparation of reference solution: Accurately weigh about 5 mg of salicin reference substance into a 25 mL volumetric flask, add water to dissolve and add to the scale to obtain the reference solution.

[0120] (1.2.3) Preparation of test solution: Accurately weigh about 60 mg of white willow bark extract sample into 50 mL, add about 40 mL of water, ultrasonically vibrate for 30 minutes, let stand at room temperature, add water to the scale, and filter with a 0.45 μm microporous membrane to obtain the test solution.

[0121] (1.2.4) Regression curve and linear range: Weigh the salicin reference substance and add water to prepare a 0.20 mg / mL reference substance stock solution. Accurately pipette the stock solution and prepare it into 0.04, 0.10, 0.20, 0.30, and 0.40 mg / mL in sequence. Pipet 10L of each solution and perform the determination according to the above chromatographic conditions. Draw a standard curve with the peak area as the ordinate and the salicin concentration as the abscissa. Salicin has a good linear relationship in the range of 0.04 to 0.4 mg / mL, and the linear regression equation is Y=1.6798X-1.2923, r=0.9996.

[0122] (1.2.5) Precision test: The salicin reference solution was accurately pipetted and injected 5 times in succession, with 10 μL injected each time. The peak area was measured and the RSD was calculated to be 0.24% (n=5).

[0123] (1.2.6) Reproducibility test: Accurately weigh an appropriate amount of willow bark extract sample of the same batch number to prepare the test solution, inject the sample, and measure 5 portions. The results showed that the average content of salicin was 19.88% and the RSD was 0.25%.

[0124] (1.2.7) Stability test: The white willow bark extract test solution was accurately aspirated and sampled once every 1 hour with a sample volume of 10 μL. The peak area was measured and the RSD of the salicin peak area was 0.36% (n=9). The results showed that the test solution was basically stable within 8 hours.

[0125] (1.2.8) Recovery test: Accurately weigh a sample of willow bark extract with a salicin content of 19.50%, and accurately add 0.15, 0.25, 0.35, 0.45, and 0.55 mg of salicin reference substance, respectively, to prepare the test solution, inject the sample, and measure the results. The average recovery of salicin was 99.35%, and the RSD was 0.39% (n=5).

[0126] (1.2.9) Quantify the content of salicylic acid in the white willow bark extract for subsequent testing. The test method refers to Zhao Yongqiang et al.'s "Determination of salicin content in white willow bark by UPLC method".

[0127] Sample determination: Weigh the white willow bark extract sample accurately, prepare the test solution, inject the sample, and determine it. The results showed that the content of salicylic acid in the unmodified white willow bark extract was 20.54%, with an RSD of 0.24%; the content of salicylic acid in the white willow bark extract modified by β-glucosidase was 25.84%, with an RSD of 0.24%; the content of salicylic acid in the white willow bark extract modified by β-glucanase was 22.17%, with an RSD of 0.24%; the content of salicylic acid in the white willow bark extract modified by xylanase was 20.98%, with an RSD of 0.24%.

[0128] 2. Effect of white willow bark extract on the survival rate of SZ95 cells

[0129] Human sebaceous gland cells SZ95 were provided by Shanghai Dermatology Hospital, and the culture medium used was a culture medium containing 10% CCK-8 reagent (Dojin Chemical Research Institute, Japan). The cells frozen in liquid nitrogen were revived, digested, and then subcultured normally for experimental use.

[0130] SZ95 cells were seeded at a density of 20,000 per well on a 96-well plate and incubated in a cell culture incubator for 24 hours. Then, the test solution containing 25, 50, 100, and 200 μg / mL of the herbal drug (salicin) was added and incubated for another 24 hours. The culture medium was removed and washed with phosphate buffered saline (PBS), and then a culture medium containing 10% CCK-8 reagent was added and incubated for 30 minutes. Finally, the optical density (OD) of each well at a wavelength of 450 nm was detected using an ELISA reader (Molecular Devices, USA), and the cell survival rate was calculated according to formula (1).

[0131] Cell survival rate (%) = (OD 450 - PBS well OD 450 ) / (blank group OD 450 - PBS well OD 450 )×100%——Formula (1)

[0132] The results are as follows Figure 1 As shown. The white willow bark extracts without modification (Example 1), modified with β-glucosidase (Example 2), modified with β-glucanase (Example 3), and modified with xylanase (Example 4) can promote the growth of SZ95 cells (P < 0.05, all with significant differences), and the promotion effect tends to increase with the increase of the concentration of the test solution, indicating that the white willow bark extracts have no cytotoxicity to SZ95 cells.

[0133] 3. Effect of white willow bark extract on neutral lipid synthesis in SZ95 cells

[0134] SZ95 cells were inoculated at a density of 10,000 per well on BeyoGold black transparent bottom 96-well cell culture plates (Biyuntian Biotechnology Co., Ltd.). The next day, the test solution containing 200 μg / mL of crude drug (salicin) was added and incubated in a cell culture incubator at 37°C and 5% carbon dioxide for 24 hours. After the supernatant was removed and washed with PBS, 10 μg / mL of Nile red solution was added to each well for staining and incubated at 37°C in the dark for 10 minutes. After washing with PBS, the fluorescence intensity of Nile red was detected by an ELISA instrument at an excitation wavelength of 485 nm / emission wavelength of 565 nm. The relative lipid content in SZ95 cells was expressed as the ratio (percentage) of the fluorescence intensity of the treatment group to the control group.

[0135] The results are shown in Table 1.

[0136] Table 1

[0137] White Willow Bark Extract Relative content of neutral lipids (%) β-Glucosidase modification 60.63 β-Glucanase Modification 73.55 Xylanase modification 82.82 Unmodified 84.66

[0138] The results showed that enzyme-modified white willow bark extract, especially modified with β-glucosidase, significantly increased the inhibition of neutral lipid synthesis in SZ95 cells (P < 0.001, with significant difference), which would provide a good basis for oil control in the long run.

[0139] 4. Determination of the antibacterial effect of white willow bark extract on Staphylococcus aureus and Propionibacterium acnes

[0140] The antibacterial rate of white willow bark extract against Staphylococcus aureus and Propionibacterium acnes was tested by microbroth dilution experiment.

[0141] The specific operation steps of the experiment are as follows: ① Under sterile operation conditions, 100 μL of nutrient broth medium (purchased from Qingdao Haibo Biotechnology Co., Ltd., for Staphylococcus aureus culture) or brain heart infusion broth medium (purchased from Qingdao Haibo Biotechnology Co., Ltd., for Propionibacterium acnes culture) was added to each well of the 96-well plate; ② 100 μL of the test solution with a volume fraction of 1% was added to the first well, and after mixing with the culture medium in the well, 100 μL of the suspension was aspirated and added to the second well, and this operation was continued until the 11th well, and then 100 μL of the suspension was aspirated from the 11th well and discarded, and the test solution was not added to the 12th well as a positive control; ③ 100 μL of the diluted bacterial solution was added to each well so that the final concentration of the bacterial solution in each well was 1×10 6 CFU / mL, and set up negative controls (containing only the test solution and culture medium at different dilution multiples to remove the background OD of the test sample) 630 );④Detect OD after 24h incubation 630 , and calculate the bacterial survival rate and inhibition rate according to formula (2) and (3).

[0142] Bacterial survival rate (%) = (OD 630 - Negative control well OD 630 ) / (OD of positive control well 630

[0143] - Negative control well OD 630 )×100%——Formula (2)

[0144] Bacterial inhibition rate (%) = 1 - bacterial survival rate (%) - Formula (3)

[0145] The willow bark extract was diluted 4-64 times to observe its inhibitory effect on Staphylococcus aureus. Figure 2 It can be seen that the willow bark extracts of each example have good antibacterial effects, among which the willow bark extract modified by β-glucosidase has the best antibacterial rate against Staphylococcus aureus.

[0146] The white willow bark extract was diluted 4-64 times to observe its inhibitory effect on Propionibacterium acnes. Figure 3 It can be seen that the white willow bark extracts of each example have good antibacterial effects, among which the white willow bark extract modified by β-glucosidase (Example 2) has the best antibacterial rate against Propionibacterium acnes.

[0147] Test Example 2: Oil control and acne removal effect test

[0148] Test samples: cosmetics (essence) prepared in Application Examples 1-7 and Comparative Examples 1-4.

[0149] 1. Select volunteers to conduct product testing and evaluation

[0150] All enrolled subjects met the following inclusion and exclusion criteria:

[0151] (1.1) Subject inclusion criteria:

[0152] (1.1.1) 18 to 65 years old, healthy women or men;

[0153] (1.1.2) Facial skin has problems such as excessive oiliness, redness, and acne;

[0154] (1.1.3) People with sensitive skin (through sensitive skin questionnaire and lactic acid stinging score ≥ 3 points);

[0155] (1.1.4) Have not participated in other clinical studies in the past two months, and the test site has not received any skin treatment, cosmetic treatment, or other tests that may affect the test results;

[0156] (1.1.5) Those who can understand the trial process, voluntarily participate in the trial and sign the written informed consent.

[0157] (1.2) Subject exclusion criteria:

[0158] (1.2.1) Pregnant or breastfeeding women or those who are planning to get pregnant in the near future;

[0159] (1.2.2) Those with a history of skin diseases such as psoriasis, eczema, atopic dermatitis, severe acne, or other chronic systemic diseases;

[0160] (1.2.3) Those who have taken oral or topical corticosteroids or other anti-inflammatory drugs in the past month;

[0161] (1.2.4) Those with highly allergic constitution;

[0162] (1.2.5) Those who have used retinoic acid preparations or undergone chemical peels, laser, pulsed light or other medical aesthetic treatments on the test area within the past three months;

[0163] (1.2.6) Those who cannot avoid prolonged exposure to sunlight;

[0164] (1.2.7) Participated in other clinical trials within the past 2 months;

[0165] (1.2.8) Other persons deemed unsuitable for trial participation by clinical assessment.

[0166] (1.3) The subject information selected for this test case is shown in Table 2.

[0167] Table 2 Subject information

[0168] Human body machine test Total number of people male female Subjects (total number) 32 0 32 Subjects (effective number) 32 0 32

[0169] 2. Test instruments and materials

[0170] VISIA7 (PIMIA analysis system), Mexameter MX18, Tewameter TM HEX, Corneometer CM825, Primos CR.

[0171] 3. Test location and environment

[0172] Test address: Efficacy Evaluation Laboratory of Guangzhou Zhongkejian Technology Testing Co., Ltd.

[0173] Test environment: temperature 21±1℃; humidity 50±10%.

[0174] 4. Test methods

[0175] (4.1) The test items are shown in Table 3:

[0176] Table 3 Test items

[0177]

[0178]

[0179] (4.2) Basic principles

[0180] Before human testing of cosmetics, necessary toxicology tests must be completed and written certificates must be issued. Samples that fail toxicology tests will not be tested on humans. According to the Declaration of Helsinki, the selection of subjects follows the medical and ethical standards for human testing. All subjects must be tested voluntarily and sign informed consent forms before testing. Before subjects sign informed consent forms, testers need to inform them of the purpose of the test, possible benefits, potential risks and problems, and related rights and obligations.

[0181] (4.3) Testing process

[0182] (4.3.1) Product usage and frequency

[0183] After cleansing in the morning and evening, take an appropriate amount of this product and apply it on acne areas.

[0184] (4.3.2) Test steps

[0185] Subjects were recruited as required and signed written informed consent. Before enrollment, subjects were asked a series of questions about their medical history and health status according to the inclusion and exclusion criteria, and then lactic acid sting test (see 4.3.2.1 for the specific testing process) was performed to screen subjects who met the criteria to participate in this test project.

[0186] The subjects in the group cleaned their faces with facial cleanser, rinsed with water, and dried their faces with non-chip absorbent tissues. After cleaning their faces, they entered the constant temperature and humidity chamber and waited for 30 minutes. During the stabilization period, they were forbidden to eat or drink, their foreheads were exposed, and they were relaxed and avoided touching the test area.

[0187] After the rest, test the skin basal value, complete the skin testing process (see 4.3.2.2 for the specific testing process) and VISIA shooting testing process (see 4.3.2.3 for the specific testing process). The tested area is the acne area on the face. Inform the subjects to use the test samples according to the sample usage instructions.

[0188] (4.3.2.1) Lactic acid sting test

[0189] The lactic acid stinging test is used to assess whether the subject has sensitive skin. Take 50μL of 10% lactic acid solution and drop it on a 1*1cm filter paper. Apply the filter paper to the nasolabial groove on either side of the subject, and use saline as a control on the other side. The tester asks the subject about the stinging sensation at 0.5min, 2.5min, and 5min, and scores it according to the "4-point method" in the table below. Those with a cumulative stinging sensation of ≥3 points on the lactic acid side relative to the saline side can be judged as sensitive skin. The lactic acid stinging score is shown in Table 4:

[0190] Table 4

[0191] Level score Rating Basis 0 points No stinging sensation 1 point Mild tingling: Mildly noticeable 2 points Moderate stinging sensation: obviously tolerable 3 points Severe stinging pain: Very stinging, unbearable

[0192] (4.3.2.2) Skin testing process

[0193] Skin moisture content, transepidermal water loss (TEWL) and skin hemoglobin were measured by skin detector at 0h, 48h and 7 days respectively. The test area was 3cm×3cm, and the data were recorded for statistical analysis.

[0194] (4.3.2.3)VISIA Shooting and Testing Process

[0195] The VISIA instrument was used to measure the acne erythema area, skin pore density, and skin acne area at 0h, 48h, and 7 days, and the data were recorded and analyzed statistically.

[0196] (4.4) Data analysis

[0197] Statistical analysis software was used for statistical analysis of the data. Measurement data were expressed as mean ± standard deviation, and normal distribution test was performed. If the data met the normal distribution requirements, the paired t test was used for comparison before and after the data, otherwise the two related sample rank sum test was used; the comparison of the rank data before and after the data was used was the two related sample rank sum test; the comparison between the experimental sample and the control group was the independent sample t test or rank sum test. The above statistical analyses were all two-tailed tests, and the significance level was α = 0.05.

[0198] (4.5) Basis for test conclusion

[0199] (4.5.1) Claims of acne-removing efficacy: Using self-control before and after, observe the skin erythema area, Pillsbury grading score, skin pore density, acne volume, and transepidermal water loss rate. If at any visit time point after using the sample, the test values ​​of three or more parameters are better than the baseline values ​​before use, and the results are significantly different (P<0.05), then the test sample is considered to have acne-removing efficacy.

[0200] ① Skin erythema area: At each visit point, the skin erythema area was collected using the VISIA instrument. The smaller the measured value, the smaller the skin erythema area.

[0201] ② Pillsbury grading score: At each visit point, professionals will score the comedones, inflammatory papules, and pustules on the acne lesions on the subjects' faces.

[0202] Grade 1 (mild): a small amount of acne and papules, no inflammation;

[0203] Grade 2 (moderate): more comedones and papules, with a small number of inflammatory papules or pustules;

[0204] Grade 3 (moderate to severe): more inflammatory papules and pustules, possibly with a small number of nodules;

[0205] Grade 4 (severe): numerous inflammatory papules, pustules and nodules, possibly with cysts.

[0206] ③Skin pore density measurement: At each visit point, the VISIA instrument was used to collect and analyze the skin pore density. The smaller the measured value, the lower the skin pore density.

[0207] ④Acne volume: At each visit point, the Primos CR instrument was used to collect the acne volume. The smaller the measured value, the smaller the acne volume.

[0208] ⑤ Measurement of transepidermal water loss rate: At each visit point, the transepidermal water loss rate was collected and analyzed using the Tewameter TM HEX instrument. The smaller the measured value, the better the skin barrier.

[0209] (4.5.2) Soothing effect claim: Using self-control before and after, observe the skin erythema area, skin TEWL, and skin hemoglobin. The smaller the measured values ​​of the three, the smaller the skin erythema area, the better the skin barrier, and the weaker the redness. If at any visit time point after using the sample, the test value of any of the two is better than the baseline value before use, and the results are significantly different (P<0.05), then the test sample is considered to have a soothing effect.

[0210] (4.5.3) Claimed repairing effects: Using self-control before and after, observe that the smaller the skin TEWL and hemoglobin measurement values, the less transepidermal water loss and the less redness of the skin, respectively. If the test values ​​of the two are better than the baseline values ​​before use at any visit time point after using the sample, and the results are significantly different (P<0.05), then the test sample is considered to have the effect of improving pores.

[0211] (4.5.4) Claims of mild and non-irritating effects: Using self-control before and after, observe the skin erythema area and skin hemoglobin. The smaller the measured values, the smaller the skin erythema area and the weaker the redness. If at any visit time point after using the sample, the two test values ​​are better than the baseline value before use, and the results are significantly different (P<0.05), then the test sample is considered to have a mild and non-irritating effect.

[0212] The actual use effect of the product is shown in Table 5-6.

[0213] Table 5 7-day efficacy test data for human body is as follows:

[0214]

[0215]

[0216]

[0217]

[0218] Table 6 Statistics of adverse skin reactions

[0219]

[0220] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. An oil-controlling and acne-removing composition, characterized in that: The invention comprises the following components in parts by weight: 1-5 parts of octanoyl salicylic acid, 0.5-2 parts of magnolol and 0.5-10 parts of white willow bark extract.

2. The oil-controlling and anti-acne composition according to claim 1, characterized in that: The invention comprises the following components in parts by weight: 2 parts of octanoylsalicylic acid, 1 part of magnolol and 1.2 parts of white willow bark extract.

3. The oil-controlling and anti-acne composition according to claim 1, characterized in that: The white willow bark extract includes unmodified white willow bark extract and / or enzyme-modified white willow bark extract; the enzyme includes at least one of β-glucosidase, β-glucanase and xylanase.

4. The oil-controlling and anti-acne composition according to claim 3, characterized in that: The white willow bark extract is obtained by modification with beta-glucosidase.

5. The oil-controlling and anti-acne composition according to claim 3, characterized in that: The preparation method of the unmodified willow bark extract comprises the following steps: adding water to willow bark to obtain a willow bark water extract, concentrating, adding isochorismate synthase as an auxiliary, stirring and adding ethanol, sealing and standing, filtering and recovering ethanol, and drying to obtain a powder, which is the willow bark extract.

6. The oil-controlling and anti-acne composition according to claim 3, characterized in that: The preparation method of the enzyme-modified white willow bark extract comprises the following steps: (1) adding water to white willow bark to obtain a white willow bark water extract, concentrating, adding isochorismate synthase as an auxiliary, stirring and adding ethanol, sealing and standing, filtering and recovering ethanol, drying to obtain powder, and adding water to prepare an aqueous solution; (2) adding enzyme modification treatment to the aqueous solution obtained in step (1), concentrating, and freeze-drying to obtain the white willow bark extract.

7. The oil-controlling and anti-acne composition according to claim 6, characterized in that: In the step (2), the enzyme concentration is 500-800 U / mL.

8. The oil-controlling and anti-acne composition according to claim 6, characterized in that: In the step (2), the conditions for the enzyme modification treatment are: adjusting the pH to 5.0-6.0 and treating at 50-60° C. for 1-3 hours.

9. Use of the oil-controlling and anti-acne composition according to any one of claims 1 to 8 in cosmetics.

10. A cosmetic, characterized in that: The cosmetic comprises the oil-controlling and anti-acne composition according to any one of claims 1 to 8.

Images