WO2024032447A1 - 一种控油舒缓护肤组合物、化妆品及其制备方法和应用 - Google Patents

一种控油舒缓护肤组合物、化妆品及其制备方法和应用 Download PDF

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WO2024032447A1
WO2024032447A1 PCT/CN2023/110819 CN2023110819W WO2024032447A1 WO 2024032447 A1 WO2024032447 A1 WO 2024032447A1 CN 2023110819 W CN2023110819 W CN 2023110819W WO 2024032447 A1 WO2024032447 A1 WO 2024032447A1
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Prior art keywords
oil
soothing
skin
controlling
care cosmetics
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PCT/CN2023/110819
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English (en)
French (fr)
Inventor
杨素珍
王晓娜
郭海姣
徐佩佩
高春明
袁春颖
张辉
王倩
韩婷婷
郭芳钰
王兴凯
陈玉荣
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山东福瑞达生物股份有限公司
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Publication of WO2024032447A1 publication Critical patent/WO2024032447A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/008—Preparations for oily skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74—Biological properties of particular ingredients
    • A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782—Enzyme inhibitors; Enzyme antagonists
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Definitions

  • the invention belongs to the technical field of cosmetics, and specifically relates to an oil-controlling and soothing skin care composition, cosmetics and preparation methods and applications thereof.
  • Sebum is produced by sebaceous gland cells in the skin and then secreted to the surface of the skin.
  • the sebum film formed by sebum and sweat on the surface of the human body is one of the important components of the first barrier of the human body.
  • Normal sebum secretion is very important for maintaining the health of the skin. important.
  • Excessive sebum secretion in the skin will lead to undesirable skin appearance and uncomfortable touch.
  • Excessive sebum is distributed on the surface of the skin and is easily contaminated with dust, which has a certain impact on normal functions and brings problems to people's daily activities. A certain level of annoyance. Therefore, oil control is an important solution to treat such skin problems.
  • the conditioning of oily skin is also one of the problems that many consumers seek to improve.
  • DHT dihydrotestosterone
  • COX2 is the key rate-limiting enzyme in the synthesis of prostaglandins (PGs). COX2 catalyzes arachidonic acid to generate PGs, which is synthesized PGD2 and intermediate products are endogenous ligands of peroxide proliferator-activated receptor ⁇ (PPAR ⁇ ). The activation of PPAR ⁇ cooperates with the retinaldehyde receptor (RXR) to form a heterodimer and initiate the expression of a series of target genes. Stimulates sebocyte proliferation and increases sebum secretion.
  • RXR retinaldehyde receptor
  • Propionibacterium acnes grows, stimulating keratinocytes to produce pro-inflammatory factors IL-1 ⁇ , TNF- ⁇ , and inflammatory mediator PGE2, leading to duct rupture. When released, it will cause a strong local reaction of the innate immune system, resulting in varying degrees of itching, burning, stinging and even erythema.
  • the purpose of the present invention is to provide an oil-controlling and soothing skin care composition, cosmetics and preparation methods and applications thereof. It has been verified by experiments that the compositions and cosmetics provided by the present invention have strong ability to inhibit oil secretion and soothe skin. Therefore, It has good practical promotion and application value.
  • a first aspect of the present invention provides an oil-controlling and soothing skin care composition, which composition includes the following components in parts by mass:
  • the molecular weight of zinc hyaluronate is controlled to be 400,000-800,000 Da, and preferably, the molecular weight of zinc hyaluronate is 500,000-700,000 Da.
  • the wild sunflower fruit extract can be obtained commercially.
  • the wild sunflower fruit extract is prepared by the following method:
  • step S2 Distill and concentrate the wild sunflower fruit permeate obtained in step S1, and then add glycerol thereto to obtain the result.
  • the extract of the Radix Fronticifolia can also be obtained through commercial means.
  • the extract of the Radix Fronticifolia is prepared by the following method:
  • step S2 Concentrate the filtrate obtained in step S1 under reduced pressure, recover the ethanol until it has no alcohol smell, add butanediol, stir evenly, and filter.
  • a second aspect of the present invention provides the use of the above composition in the preparation of oil-controlling, soothing and skin-care cosmetics.
  • the present invention has verified through experiments that the above composition can inhibit the activity of COX2 by inhibiting 5 ⁇ -reductase activity, thereby effectively inhibiting oil secretion and controlling oil; at the same time, it can externally inhibit IL-1 ⁇ , TNF- ⁇ and PGE2 inflammatory factors. Its activity achieves excellent soothing effect; it is also safe and has no toxic side effects, so it can be used in cosmetics for oil control and soothing skin care.
  • the third aspect of the present invention provides a cosmetic for oil control, soothing and skin care, which cosmetic contains the above composition.
  • the oil-controlling and soothing skin care cosmetics may also contain other raw materials allowed to be added in any cosmetic field, including but not limited to emulsifiers, emollients, moisturizers, thickeners, etc.
  • the present invention can also prepare different cosmetic dosage forms, such as essence water, essence milk, essence cream, etc.
  • different cosmetic dosage forms such as essence water, essence milk, essence cream, etc.
  • the obtained cosmetic categories are further derived and prepared. It is obvious that All fall within the protection scope of this application.
  • a fourth aspect of the present invention provides a method for preparing the above-mentioned oil-controlling and soothing skin care cosmetics.
  • the preparation method includes the step of mixing the composition described in the above-mentioned first aspect and other raw material components.
  • the fifth aspect of the present invention provides the application of the above composition and/or cosmetics in oil control, soothing and skin care.
  • the oil-controlling and soothing skin care cosmetics obtained by the above technical solution have excellent oil-controlling and soothing effects; by inhibiting 5 ⁇ -reductase activity in vitro, inhibiting the activity of COX2, thereby effectively inhibiting oil secretion and controlling oil; by inhibiting IL-1 ⁇ , IL-1 ⁇ , The activity of TNF- ⁇ and PGE2 inflammatory factors achieves excellent soothing effect; further, through human efficacy experimental testing, the above cosmetic The product has good oil control and soothing functions and has remarkable effects.
  • the preparation method of the oil-controlling and soothing skin care cosmetic obtained by the above technical solution is simple and easy to implement, the raw materials are easy to obtain, and it is suitable for mass production, so it has good practical application value.
  • Figure 1 Effects of different test samples on 5 ⁇ -reductase activity (## means compared with the blank control, p ⁇ 0.01; ** means compared with the negative control, p ⁇ 0.01)
  • Figure 2 Histogram of synthetic Oil Red O staining results of lipid droplets of the test sample (## means compared with the blank control, p ⁇ 0.01; ** means compared with the negative control, p ⁇ 0.01; * means compared with the negative control ,0.01 ⁇ p ⁇ 0.05)
  • Figure 5 Comparison of skin soothing changes after using the product.
  • an oil-controlling and soothing skin care composition which composition includes the following components by mass:
  • Tests have proven that the combination of zinc hyaluronate, wild sunflower fruit extract and goldenrod extract has a very good oil control and soothing effect and can be used in cosmetics to improve oily skin problems.
  • the molecular weight of zinc hyaluronate is controlled to be 400,000-800,000 Da, and preferably, the molecular weight of zinc hyaluronate is 500,000-700,000 Da.
  • the wild sunflower fruit extract can be obtained commercially.
  • the wild sunflower fruit extract is prepared by the following method:
  • step S2 Distill and concentrate the wild sunflower fruit permeate obtained in step S1, and then add glycerol thereto to obtain the result.
  • a 60-100 mesh sieve is selected for the sieving process, such as 60, 70, 80, 90 or 100 mesh; in a specific embodiment of the present invention, an 80 mesh sieve is selected for the sifting process.
  • step S2 distillation and concentration are specifically performed by vacuum distillation at 55-65°C, and when the filtrate is evaporated until the remaining amount is 1/6-1/3 of the original filtrate (preferably 1/5), Add 1-1.5 times the amount of glycerol to the remaining concentrated solution, stir evenly and filter.
  • the extract of the Radix Fronticifolia can also be obtained through commercial means.
  • the extract of the Radix Fronticifolia is prepared by the following method:
  • step S2 Concentrate the filtrate obtained in step S1 under reduced pressure, recover the ethanol until it has no alcohol smell, add butanediol, stir evenly, and filter.
  • step S1 a 30-60 mesh sieve is used for the sieving process, such as 30, 40, 50 or 60 mesh; in a specific embodiment of the present invention, a 50 mesh sieve is used for the sieving process.
  • the ethanol is selected from 60% to 85% ethanol, the material-to-liquid ratio (w/w) is 1:8-1:10, and soaked for 10-30min (preferably 20min); the ultrasonic power during the ultrasonic extraction process is 100-300W (preferably (200W), ultrasonic treatment time is 30-40min;
  • the concentration under reduced pressure specifically involves performing a vacuum distillation process at 50-60°C, recovering the ethanol until it has no alcoholic taste to obtain a concentrated liquid of Radix Fronticifolia, and adding 2 to 2.5 times the mass of the Radix Fronticifolia concentrated liquid. of butanediol, stir evenly, and filter to obtain it.
  • the oil-controlling and soothing skin care composition consists of the following components by mass:
  • a second aspect of the present invention provides the use of the above composition in the preparation of oil-controlling, soothing and skin-care cosmetics.
  • the present invention has verified through experiments that the above composition can inhibit the activity of COX2 by inhibiting 5 ⁇ -reductase activity, thereby effectively inhibiting oil secretion and controlling oil; at the same time, it can externally inhibit IL-1 ⁇ , TNF- ⁇ and PGE2 inflammatory factors. Its activity achieves excellent soothing effect; it is also safe and has no toxic side effects, so it can be used in cosmetics for oil control and soothing skin care.
  • an oil-controlling, soothing and skin-care cosmetic is provided, which cosmetic contains the above composition.
  • the added amount of the oil-controlling and soothing skin-care composition is 0.5-40%, preferably 2-25%, such as 2%, 5 %, 10%, 15%, 20%, 25%, 30% or 40%.
  • the oil-controlling and soothing skin care cosmetics may also contain other raw materials allowed to be added in any cosmetic field, including but not limited to emulsifiers, emollients, moisturizers, thickeners, etc.
  • the added amount of the emulsifier is 1-6%, and the preferred added amount is 2-5%; the emollient The addition amount of the moisturizing agent is 6-25%, and the preferred addition amount is 8-20%; the addition amount of the moisturizing agent is 2-15%, and the preferred addition amount is 5-12%; the addition of the thickening agent The amount is 0.02-1.0%, and the preferred addition amount is 0.05-0.8%.
  • the emulsifier includes polyglyceryl-6 stearate, polyglyceryl-6 behenate, and polyglyceryl-6 distearate.
  • the emollient includes isononyl isononanoate, squalane, caprylic/capric triglyceride, and baobab seed oil. , Burr's Walnut Seed Oil, White Pond Flower Seed Oil, Dimethicone, Cyclopentamethicone, Isododecane, Glyceryl Tris(ethylhexanoate), Behenyl Alcohol, Any one or a combination of two or more of shea butter, dioctyl carbonate, and tocopheryl acetate.
  • the moisturizing agent includes glycerin, butylene glycol, 1,2-hexanediol, ethylhexylglycerin, sodium hyaluronate, and pantothenate. Any one or a combination of two or more of alcohol and trehalose.
  • the thickening agent includes sodium polyacrylate, carbomer, xanthan gum, hydroxyethyl cellulose, acryloyl dimethyl tau Any one or a combination of two or more of ammonium sulfonate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyltaurate copolymer, and polyacrylate cross-linked polymer-6.
  • the present invention can also prepare different cosmetic dosage forms, such as essence water, essence milk, essence cream, etc.
  • different cosmetic dosage forms such as essence water, essence milk, essence cream, etc.
  • the obtained cosmetic categories are further derived and prepared. It is obvious that All fall within the protection scope of this application.
  • a method for preparing the above-mentioned oil-controlling and soothing skin care cosmetics includes the step of mixing the composition described in the first aspect and other raw material components.
  • An oil-controlling and soothing skin care composition which is composed of zinc hyaluronate, wild sunflower fruit extract and Radix Paechinensis extract.
  • the molecular weight of zinc hyaluronate is 500,000 Da.
  • the method of obtaining wild sunflower fruit extract is:
  • step (2) Place the wild sunflower fruit percolation liquid obtained in step (1) into a rotary evaporator, evacuate, and distill under reduced pressure at 60°C. When the filtrate evaporates to one-fifth of the remaining amount, add 1.5% of the concentrated solution Double the mass of glycerol, stir evenly, and filter to obtain wild sunflower fruit extract.
  • the method for obtaining the extract of Pediculus chinensis is:
  • step (2) Place the filtrate obtained in step (1) in a rotary evaporator, evacuate, distill under reduced pressure at 60°C, recover the ethanol until it has no alcohol smell, add 2.5 times the mass of butylene glycol from the concentrated solution of Radix Scutellariae, Stir evenly and filter to obtain the extract of Phytophthora chinensis.
  • the above-mentioned oil-controlling and soothing skin care composition is used to prepare an essence water product containing the oil-controlling and soothing skin care composition, and the formula is shown in Table 2.
  • Comparative Example 5 The preparation method of Comparative Example 5 is the same as that of Example 4. The only difference is that Comparative Example 5 does not contain the oil-controlling and soothing skin-care composition. The amount occupied by the oil-controlling and soothing skin-care composition in Example 4 is filled with water.
  • the above-mentioned oil-controlling and soothing skin-care composition is used to prepare an essence milk product containing the oil-controlling and soothing skin-care composition.
  • the formula is shown in Table 3.
  • the above-mentioned oil-controlling and soothing skin-care composition is used to prepare an essence cream product containing the oil-controlling and soothing skin-care composition.
  • the formula is shown in Table 4.
  • Experimental method Use fertilized chicken embryos within 7 days of age and incubate them in an incubator at 37.6 ⁇ 0.5°C and 50% to 70% humidity for 9 days.
  • CAM preparation Carry out photo-egg inspection, mark the position of the air chamber on the eggshell surface, use tweezers to peel off the marked eggshell part, and expose the white egg membrane. Care should be taken not to damage the integrity of the egg membrane. Add 0.5 mL of 0.9% NaCl solution dropwise to fully moisten the egg membrane, gently absorb the surface liquid with paper towels, and carefully remove the intima with tweezers to ensure that the vascular membrane is not damaged.
  • Reaction endpoint method Take 0.3 mL of the transparent test substance and evenly drop or apply it on the surface of the CAM. After 3 minutes of action, use 0.9% NaCl solution to wash away the test substance and observe the degree of change in each toxic effect of the CAM.
  • End point score method (end point score ES): For trials conducted using the reaction end point method, the end point score (ES) should be calculated, and the results should be retained to two decimal places.
  • the test results are shown in Table 6.
  • the oil-controlling and soothing skin care composition is non-irritating.
  • Test Example 2 In vitro inhibition of 5 ⁇ -reductase activity experiment
  • Testosterone is converted into dihydrotestosterone (DHT) by 5 ⁇ -reductase with the participation of NADPH.
  • DHT dihydrotestosterone
  • the expression of DHT affects the proliferation and differentiation of sebaceous gland cells. Therefore, by using an ultra-high performance liquid phase tandem mass spectrometry system (UPLC-MS) to measure the testosterone content of the substrate testosterone in the 5 ⁇ -reductase activity reaction system, the inhibitory effect of the test substance on 5 ⁇ -reductase can be evaluated.
  • UPLC-MS ultra-high performance liquid phase tandem mass spectrometry system
  • B represents the testosterone content of the blank control group
  • Q represents the testosterone content of the reaction group without inhibitor
  • R represents the testosterone content of the reaction group with the inhibitor to be tested added.
  • the original concentrations of each component in the enzyme reaction system are: buffer solution [Tris-HCl, pH 7.4]; NADPH concentration (10mmol/L, Sigma 93205); 5 ⁇ -reductase concentration is 10mg/mL; testosterone 4 ⁇ g/mL; Dutasteride concentrations were all 0.5mg/mL.
  • Example 1 Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4 all have significant in vitro inhibition of 5 ⁇ -reductase activity.
  • Example 1 The inhibition rate was 69.44%, the inhibition rate of Example 2 was 87.75%, the inhibition rate of Example 3 was 78.03%, the inhibition rate of Comparative Example 1 was 44.16%, the inhibition rate of Comparative Example 2 was 52.50%, and the inhibition rate of Comparative Example 3 was 54.68 %, while the inhibition rate of Comparative Example 4 was 5.22%.
  • the inhibitory effect of Example 2 is the most obvious, indicating that the oil-controlling and soothing skin care composition has a significant function of inhibiting 5 ⁇ -reductase activity, thereby achieving the oil-controlling effect.
  • Test Example 3 Activity experiment of inhibiting IL-1 ⁇ , TNF- ⁇ , COX2 and PGE2 factors in vitro
  • LPS bacterial lipopolysaccharide
  • Examples 1, 2, 3 and Comparative Examples 1, 2, 3, and 4 can significantly inhibit the activity of IL-1 ⁇ .
  • the inhibitory effect of Example 2 is the most significant, but Comparative Examples 1, 2 , the inhibition rates of 3 and 4 are all lower than those of Examples 1, 2, and 3, especially Comparative Example 1 is far lower than
  • Example 2 It shows that the oil-controlling and soothing skin care composition can significantly inhibit the activity of IL-1 ⁇ .
  • Examples 1, 2, 3 and Comparative Examples 1, 2, 3, and 4 can significantly inhibit the activity of TNF- ⁇ , but the inhibition rates of Comparative Examples 1, 2, 3, and 4 are all low. In Examples 1, 2, and 3, especially Comparative Example 1, the results are far lower than those in each Example. It shows that the oil-controlling and soothing skin care composition can significantly inhibit the activity of TNF- ⁇ .
  • Examples 1, 2, 3 and Comparative Examples 1, 2, 3, and 4 can significantly inhibit the activity of PGE2.
  • the inhibitory effect of Example 2 is the most significant, but Comparative Examples 1, 2, and 3
  • the inhibition rates of , 4 are all lower than those of Examples 1, 2, and 3, especially Comparative Example 1 is far lower than that of each Example. It shows that the oil-controlling and soothing skin care composition can significantly inhibit the activity of PGE2.
  • the oil-controlling and soothing skin care composition can significantly inhibit the activity of IL-1 ⁇ , TNF- ⁇ , COX2 and PGE2 factors, and has a certain oil-controlling and soothing effect.
  • Example 4 In vitro oil control experiment of Example 4
  • This experiment evaluates the oil control effect of the test substance by detecting the lipid droplet content of the sample acting on sebaceous gland cells SZ95.
  • Oil Red O staining Aspirate the old solution, wash the cells once with PBS, add 500 ⁇ L Oil Red O working solution (1 ⁇ g/mL) to each well, stain for 15 min in the dark (incubate at 37°C in an incubator), and wash twice with PBS.
  • the oil control ability was evaluated based on the OD value of the synthetic Oil Red O staining results of lipid droplets. The lower the OD value, the smaller the secreted oil content and the stronger the ability to control oil.
  • Inhibition rate calculation formula (NC group OD value - sample OD value)/NC group OD value * 100%
  • Example 4 The test results are shown in Figure 2.
  • the OD value of Example 4 is significantly lower than that of the negative control group (NC group), the inhibition rate is 12.63%, and it has significant oil control effect. Therefore, it shows that the product containing the oil control and soothing skin care composition has a certain oil control effect. ability.
  • Test Example 5 Effect of Example 4 on oil control on human skin
  • T0 means that the subject does not use the sample
  • T2 means that the subject uses the sample for a single time for 2 hours
  • T4 means that the subject uses the sample for a single time for 4 hours
  • T8 means that the subject uses the sample for a single time for 8 hours.
  • Comparative Example 5 was selected as the blank control group in this experiment.
  • sample area and blank area are randomly distributed on the left and right sides of the forehead to ensure that the positions of all sample areas and blank areas are statistically balanced;
  • test results are shown in Figures 3 and 4. After a single use of the sample for 2 hours, 4 hours, and 8 hours, the skin oil increase of the sample was significantly improved compared with the blank area of the control sample.
  • the inhibition rate after using the sample for two hours was 21.46%
  • the inhibition rate after using the sample for 4 hours was 22.55%
  • the inhibition rate after using the sample for 8 hours was 18.42%.
  • Example 4 The prepared essence aquatic product of Example 4 was tested for human skin efficacy, and 30 volunteers aged 18-40 years old (skin condition: sensitive skin (lactic acid stinging positive)) were sought for product testing.
  • VISIA skin tester CanField Company, USA.
  • This test collects pictures of the left, middle and right sides of the subject's face under three light sources: standard light 1, standard light 2 and cross-polarized light. and exported red zone images under cross-polarized light. Image analysis is performed on the red zone pictures to obtain the quantitative index red zone analysis a* value, which is used to evaluate the improvement of facial skin redness and sensitivity.
  • the red zone analysis a* value test results showed that compared with before use, after using the test sample for 4 weeks, the red zone analysis a* value was significantly reduced (0.01 ⁇ P ⁇ 0.05), indicating that products containing this oil-controlling and soothing skin care composition Has soothing properties.

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Abstract

本发明属于化妆品技术领域，提供一种控油舒缓护肤组合物、化妆品及其制备方法和应用。所述控油舒缓护肤组合物，包含如下质量份数的组分：透明质酸锌0.1-1.0份，野葵果提取物1.0-20份，黄花前胡提取物1.0-20份。其通过抑制5α-还原酶及COX2因子活性，多通路作用达到控油功效，同时还通过抑制IL-1α、TNF-a及PGE2因子活性，达到舒缓功效。本发明控油舒缓护肤化妆品解决了现有的控油舒缓护肤化妆品控油舒缓效果不佳的问题，因此具有良好的实际推广和应用之价值。

Description

一种控油舒缓护肤组合物、化妆品及其制备方法和应用
本发明要求于2022年8月10日提交中国专利局、申请号为202210955687.9、发明名称为“一种控油舒缓护肤组合物、化妆品及其制备方法和应用”的中国专利申请的优先权，其全部内容通过引用结合在本发明中。
技术领域
本发明属于化妆品技术领域，具体涉及一种控油舒缓护肤组合物、化妆品及其制备方法和应用。
背景技术
公开该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。
皮脂是由皮肤里面的皮脂腺细胞生成，然后被分泌到皮肤表面，皮脂与汗液在人体表面形成的皮脂膜是人体第一道屏障重要组成之一，正常的皮脂分泌量对维持皮肤的健康状态非常重要。皮肤油脂分泌过多会导致皮肤不良的外观和不舒服的触感，过多的皮脂分布在皮肤表面，还容易沾污灰尘，对发挥正常的功能有一定的影响，给人在日常生活活动带来一定程度的烦恼。因此，控油是治疗此类皮肤问题的重要解决途径，同时，油性肌肤的调理也是很多消费者寻求改善的问题之一。
皮脂腺分泌异常通常是雄性激素过多导致的，睾酮和二氢睾酮(DHT)都属于雄性激素，DHT的活性是睾酮的5～10倍。5α-还原酶是睾酮转变为DHT的过程中直接的催化酶，DHT的表达会影响皮脂腺细胞的增殖和分化，从而导致皮脂腺分泌过多的油脂。
环境、UVB、激素等因素会诱导环氧合酶-2(COX2)的表达，COX2是前列腺素(PGs)合成过程关键限速酶，COX2催化花生四烯酸(arachidonic acid)生成PGs，合成的PGD2和中间产物均为过氧化物增殖激活受体γ(PPARγ)的内源性配体，PPARγ的激活协同视黄醛受体(RXR)形成异二聚体，启动一系列靶基因的表达，刺激皮脂细胞增殖、皮脂分泌增加。
油脂分泌过量会导致导管内压力增加，形成低氧环境，在低氧环境中痤疮丙酸杆菌生长，刺激角质形成细胞产生促炎因子IL-1α、TNF-α、炎性介质PGE2，在导管破裂时释放会引起先天免疫系统的强烈局部反应，产生不同程度的瘙痒感、灼烧感、刺痛感甚至红斑等。
发明人经研究发现，虽然现在市面上已有大量宣传具有控油舒缓效果的化妆品，但普遍存在控油舒缓效果不佳、生产制备工艺复杂、价格高昂等问题。
发明内容
针对现有技术中存在的不足，本发明目的在于提供一种控油舒缓护肤组合物、化妆品及其制备方法和应用。经试验验证，本发明提供的组合物及化妆品具有较强的抑制油脂分泌、舒缓肌肤的能力，因此 具有良好的实际推广和应用之价值。
为了实现上述技术目的，本发明提供的技术方案如下：
本发明的第一个方面，提供一种控油舒缓护肤组合物，所述组合物包含如下质量份数的组分：
透明质酸锌0.1-1.0份，野葵果提取物1-20份，黄花前胡提取物1-20份。
其中，透明质酸锌分子量控制为40万-80万Da，优选的，透明质酸锌分子量为50万-70万Da。
所述野葵果提取物可采用市售方式获得，在本发明的一个具体实施方式中，所述野葵果提取物，采用如下方法制备得到：
S1、将野葵果粉碎过筛，以乙醇为溶剂采用渗漉法获取野葵果渗漉液；
S2、将步骤S1得到的野葵果渗漉液进行蒸馏浓缩处理，然后向其中加入甘油即得。
所述黄花前胡提取物亦可通过市售方式获得，在本发明的一个具体实施方式中，所述黄花前胡提取物，采用如下方法制备得到：
S1、将黄花前胡粉碎过筛，粉碎后的黄花前胡浸于乙醇中进行超声提取，过滤，收集滤液，滤渣重复提取2-3次，合并所得滤液；
S2、将步骤S1制得滤液进行减压浓缩，回收乙醇至无醇味，加入丁二醇，搅拌均匀，过滤即得。
本发明的第二个方面，提供上述组合物在制备控油舒缓护肤的化妆品中的应用。本发明通过试验验证，上述组合物能够通过抑制5α-还原酶活性，抑制COX2的活性，从而达到有效抑制油脂分泌、控油的作用；同时，能够外抑制IL-1α、TNF-α及PGE2炎症因子的活性，达到优异的舒缓作用；同时安全无毒副作用，因此可应用于控油舒缓护肤的化妆品之中。
因此，本发明的第三个方面，提供一种控油舒缓护肤的化妆品，所述化妆品其包含上述组合物。
所述控油舒缓护肤化妆品还可以包含任意化妆品领域允许添加的其他原料成分，包括但不限于乳化剂、润肤剂、保湿剂和增稠剂等。
同时，本发明通过合理添加上述原料成分，也可以以此制备不同化妆品剂型，如精华水、精华乳、精华霜等，同时，基于上述基础化妆品品类，进一步衍生制备的获得的化妆品品类，其显然均属于本申请的保护范围之内。
本发明的第四个方面，提供上述控油舒缓护肤化妆品的制备方法，所述制备方法包括将包含上述第一方面所述的组合物以及其他各原料组分混合的步骤。
本发明的第五个方面，提供上述组合物和/或化妆品在控油舒缓护肤中的应用。
上述一个或多个技术方案的有益技术效果：
上述技术方案所获得控油舒缓护肤化妆品的控油能力及舒缓能力效果优异；通过体外抑制5α-还原酶活性，抑制COX2的活性，从而达到有效抑制油脂分泌、控油的作用；通过体外抑制IL-1α、TNF-α及PGE2炎症因子的活性，达到优异的舒缓作用；进一步的，通过人体功效实验测试，证明上述化妆 品具有很好的控油、舒缓功能，功效显著。
同时，上述技术方案所获得的控油舒缓护肤化妆品的制备方法简单易行，原料易于获取，适合大批量生产，因此具有良好的实际应用之价值。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。
图1：不同测试样品对5α-还原酶活性的影响(##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01)
图2：测试样品的脂滴合成油红O染色结果柱状图(##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01；*表示与阴性对照相比，0.01<p<0.05)
图3：使用产品后皮肤油脂含量检测结果(***，P<0.001)
图4：使用产品后皮肤油脂含量变化对比图(***，P<0.001)
图5：使用产品后皮肤舒缓变化对比图。
具体实施方式
应该指出，以下详细说明都是例示性的，旨在对本发明提供进一步的说明。除非另有指明，本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是，这里所使用的术语仅是为了描述具体实施方式，而非意图限制根据本申请的示例性实施方式。如在这里所使用的，除非上下文另外明确指出，否则单数形式也意图包括复数形式，此外，还应当理解的是，当在本说明书中使用术语“包含”和/或“包括”时，其指明存在特征、步骤、操作、器件、组件和/或它们的组合。
本发明的一个典型具体实施方式中，提供一种控油舒缓护肤组合物，所述组合物包含如下质量份数的组分：
透明质酸锌0.1-1.0份，野葵果提取物1-20份，黄花前胡提取物1-20份。
经试验证明，透明质酸锌、野葵果提取物、黄花前胡提取物组合具有很好的控油舒缓效果，可以用于化妆品中改善油性肌肤问题。
其中，透明质酸锌分子量控制为40万-80万Da，优选的，透明质酸锌分子量为50万-70万Da。
所述野葵果提取物可采用市售方式获得，在本发明的一个具体实施方式中，所述野葵果提取物，采用如下方法制备得到：
S1、将野葵果粉碎过筛，以乙醇为溶剂采用渗漉法获取野葵果渗漉液；
S2、将步骤S1得到的野葵果渗漉液进行蒸馏浓缩处理，然后向其中加入甘油即得。
其中，
所述步骤S1中，过筛处理中选用60-100目筛，如60、70、80、90或100目；本发明的一个具体实施方式中，过筛处理选用80目筛。
以乙醇为溶剂采用渗漉法获取野葵果渗漉液具体方法为：
将粉碎过筛后的野葵果粉末置于渗漉筒中，加入3-8倍量(优选为5倍量)的30％-70％(优选为50％)乙醇浸泡6h～12h，以7-10mL/min的流速收集野葵果粉末10-20倍量(优选为15倍量)的渗漉提取液并过滤得滤液。
所述步骤S2中，蒸馏浓缩具体为在55-65℃条件下采用减压蒸馏处理，待滤液蒸发至剩余量为原有滤液的1/6-1/3时(优选为1/5)，加入剩余浓缩液1-1.5倍量的甘油，搅拌均匀过滤后即得。
所述黄花前胡提取物亦可通过市售方式获得，在本发明的一个具体实施方式中，所述黄花前胡提取物，采用如下方法制备得到：
S1、将黄花前胡粉碎过筛，粉碎后的黄花前胡浸于乙醇中进行超声提取，过滤，收集滤液，滤渣重复提取2-3次，合并所得滤液；
S2、将步骤S1制得滤液进行减压浓缩，回收乙醇至无醇味，加入丁二醇，搅拌均匀，过滤即得。
其中，
所述步骤S1中，过筛处理选用30-60目筛，如30、40、50或60目；本发明的一个具体实施方式中，过筛处理选用50目筛。
所述乙醇选用60％～85％乙醇，料液比(w/w)为1:8-1:10，浸泡10-30min(优选为20min)；超声提取过程中超声功率为100-300W(优选为200W)，超声处理时间为30-40min；
所述步骤S2中，减压浓缩具体为在50-60℃条件下进行减压蒸馏处理，回收乙醇至无醇味得黄花前胡浓缩液，加入所述黄花前胡浓缩液2～2.5倍质量的丁二醇，搅拌均匀，过滤后即得。
本发明的又一具体实施方式中，所述控油舒缓护肤组合物，由如下质量份数的组分组成：
透明质酸锌0.3份，野葵果提取物10份，黄花前胡提取物10份。
本发明的第二个方面，提供上述组合物在制备控油舒缓护肤的化妆品中的应用。本发明通过试验验证，上述组合物能够通过抑制5α-还原酶活性，抑制COX2的活性，从而达到有效抑制油脂分泌、控油的作用；同时，能够外抑制IL-1α、TNF-α及PGE2炎症因子的活性，达到优异的舒缓作用；同时安全无毒副作用，因此可应用于控油舒缓护肤的化妆品之中。
因此，本发明的又一具体实施方式中，提供一种控油舒缓护肤的化妆品，所述化妆品其包含上述组合物。
根据本发明的控油舒缓护肤化妆品，其中，以所述控油舒缓护肤化妆品的总质量计，所述控油舒缓护肤组合物的加入量为0.5-40％，优选2-25％，如2％、5％、10％、15％、20％、25％、30％或40％。
所述控油舒缓护肤化妆品还可以包含任意化妆品领域允许添加的其他原料成分，包括但不限于乳化剂、润肤剂、保湿剂和增稠剂等。
在本发明的又一具体实施方式中，以所述控油舒缓护肤化妆品的总质量计，所述乳化剂的加入量为1-6％，优选的加入量为2-5％；所述润肤剂的加入量为6-25％，优选的加入量为8-20％；所述保湿剂的加入量为2-15％，优选的加入量为5-12％；所述增稠剂的加入量为0.02-1.0％，优选的加入量为0.05-0.8％。
在本发明的又一具体实施方式中，根据本发明的控油舒缓护肤化妆品，所述乳化剂包括聚甘油-6硬脂酸酯、聚甘油-6山嵛酸酯、聚甘油-6二硬脂酸酯、聚甘油-3蜂蜡酸酯、C14-22醇、C12-20烷基葡糖苷、鲸蜡硬脂醇橄榄油酸酯、山梨坦橄榄油酸酯、氢化卵磷脂、菊粉月桂基氨基甲酸酯、二(月桂酰胺谷氨酰胺)赖氨酸钠、枯草菌脂肽钠中的任意一种或两种以上的组合。
在本发明的又一具体实施方式中，根据本发明的控油舒缓护肤化妆品，所述润肤剂包括异壬酸异壬酯、角鲨烷、辛酸/癸酸甘油三酯、猴面包树籽油、伯尔硬胡桃籽油、白池花籽油、聚二甲基硅氧烷、环五聚二甲基硅氧烷、异十二烷、甘油三(乙基己酸)酯、山嵛醇、乳木果油、碳酸二辛酯、生育酚乙酸酯中任意一种或两种以上的组合。
在本发明的又一具体实施方式中，根据本发明的控油舒缓护肤化妆品，所述保湿剂包括甘油、丁二醇、1，2-己二醇、乙基己基甘油、透明质酸钠、泛醇、海藻糖中任意一种或两种以上的组合。
在本发明的又一具体实施方式中，根据本发明的控油舒缓护肤化妆品，所述增稠剂包括聚丙烯酸钠、卡波姆、黄原胶、羟乙基纤维素、丙烯酰二甲基牛磺酸铵/VP共聚物、丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠共聚物、聚丙烯酸酯交联聚合物-6中的任意一种或两种以上的组合。
同时，本发明通过合理添加上述原料成分，也可以以此制备不同化妆品剂型，如精华水、精华乳、精华霜等，同时，基于上述基础化妆品品类，进一步衍生制备的获得的化妆品品类，其显然均属于本申请的保护范围之内。
本发明的又一具体实施方式中，提供上述控油舒缓护肤化妆品的制备方法，所述制备方法包括将包含上述第一方面所述的组合物以及其他各原料组分混合的步骤。
本发明的又一具体实施方式中，提供上述组合物和/或化妆品在控油舒缓护肤中的应用。
下面结合实施例对本发明进一步说明。下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围中。基于本发明中的实施例，本领域技术人员在没有作出创造性前提下，任何对本发明的变化都归属本发明的保护范围。同时，在本发明实施例中，若无特殊说明，所有制备原料均为本领域技术人员熟知的市售产品。
实施例
一种控油舒缓护肤组合物，其由透明质酸锌，野葵果提取物和黄花前胡提取物组成。
其中，透明质酸锌分子量为50万Da。
野葵果提取物的获得方法为：
(1)将干燥野葵果粉碎过80目筛，将野葵果粉末置于渗漉筒中，加入5倍量50％乙醇浸泡10h，以8mL/min的流速收集野葵果粉末15倍量的渗漉提取液，过滤。
(2)将步骤(1)得到的野葵果渗漉液置于旋转蒸发器中，抽真空，在60℃下减压蒸馏，待滤液蒸发至剩下五分之一时，加入浓缩液1.5倍质量的甘油，搅拌均匀，过滤，得到野葵果提取物。
黄花前胡提取物的获得方法为：
(1)将干燥的黄花前胡粉碎过50目筛，粉碎后的黄花前胡浸泡在70％乙醇中，质量比为1:9，浸泡20min，然后在超声功率为200W条件下提取30min，过滤，收集滤液，滤渣重复提取两次，合并三次滤液。
(2)将步骤(1)得到的滤液置于旋转蒸发器中，抽真空，在60℃下减压蒸馏，回收乙醇至无醇味，加入黄花前胡浓缩液2.5倍质量的丁二醇，搅拌均匀，过滤，得到黄花前胡提取物。
实施例1-3及对比例1-4制备方法：将透明质酸锌、野葵果提取物、黄花前胡提取物混合到一起，溶于纯化水中。具体方案如下表1所示，以质量比计算。
表1具体实施例及对比例成分列表
实施例4精华水
上述控油舒缓护肤组合物的应用，制备含有该控油舒缓的精华水产品，配方如表2所示。
表2精华水产品配方

精华水的制备方法：
S1：分别加入A相中原料，加热至85℃搅拌溶解；
S2：溶解完全后，开始降温，降至45℃时分别加入B相中成分，搅拌溶解分散均匀；
S3：当温度降至40℃时，依次加入C相成分，搅拌溶解分散均匀，即得精华水产品。
对比例5的制备方法同实施例4，区别仅在于对比例5不含有控油舒缓护肤组合物，实施例4中控油舒缓护肤组合物所占用量加水补齐。
实施例5精华乳
上述控油舒缓护肤组合物的应用，制备含有该控油舒缓护肤组合物的精华乳产品，配方如表3所示。
表3精华乳产品配方
精华乳的制备方法：
S1：水相的制备：分别加入A相中原料，加热至85℃搅拌溶解；
S2：油相的制备：分别加入B相中原料，加热至80℃熔解；
S3：将A相与B相合相，开启均质(3000rpm)，均质12min；
S4：均质完毕后，加入C相，搅拌均匀，开始降温；
S5：当温度降至70℃时加入D相，搅拌溶解，溶解完毕后继续降温；
S6：当温度降至45℃时，依次加入E相成分，搅拌溶解分散均匀，即得精华乳产品。
实施例6精华霜
上述控油舒缓护肤组合物的应用，制备含有该控油舒缓护肤组合物的精华霜产品，配方如表4所示。
表4精华霜产品配方
精华霜的制备方法：
S1：水相的制备：分别加入A相中原料，加热至85℃搅拌溶解；
S2：油相的制备：分别加入B相中原料，加热至80℃熔解；
S3：将A相与B相合相，开启均质(3000r/min)，均质12min；
S4：均质完毕后，开始降温，当温度降至70℃时加入C相，搅拌溶解，溶解完毕后继续降温；
S5：当温度降至45℃时，依次加入D相成分，搅拌溶解分散均匀，即得精华霜产品。
试验例1：安全性测试实验
参照SN/T 2329-2009《化妆品眼刺激性/鸡胚绒毛尿囊膜试验》，对产品进行眼刺激测试即安全性测试。
实验方法：采用7日龄以内的受精鸡胚，在37.6±0.5℃﹑50％～70％湿度的孵育箱中孵育9日。
CAM制备：进行照蛋检查，在蛋壳表面标记气室位置，用镊子剥去带标记的蛋壳部分，暴露白色蛋膜，应小心操作不破坏蛋膜完整性。滴加0.5mL 0.9％NaCl溶液使蛋膜充分湿润，用纸巾轻轻吸干表面液体，并用镊子小心去除内膜，保证血管膜不受损。
反应终点法：取透明受试物0.3mL均匀滴加或涂抹于CAM表面，作用3min后使用0.9％NaCl溶液洗去受试物，观察CAM每种毒性效应变化的程度。
终点评分法(end point score ES)：采用反应终点法进行的试验，应计算终点评分(ES)，结果保留小数点后两位。每只鸡胚记分＝每只鸡胚观察到的出血、凝血和血管融解程度的和，ES＝6只鸡胚得分的数学总和。根据ES值按表5对受试物眼刺激性进行分类。
表5反应终点法结果判定标准
试验结果如表6所示该控油舒缓护肤组合物无刺激性。
表6刺激性实验结果统计表
试验例2：体外抑制5α-还原酶活性实验
睾酮在NADPH的参与下被5α-还原酶作用下转化为二氢睾酮(DHT)，DHT的表达会影响皮脂腺细胞的增殖和分化。因此，通过采用超高效液相串联质谱系统(UPLC-MS)对睾酮含量进行测定5α-还原酶活反应体系中底物睾酮含量变化，可以评估待测物对5α-还原酶抑制作用。
抑制率计算按照公式：I(％)＝[(B-Q)-(B-R)]/(B-Q)×100。B表示空白对照组睾酮含量，Q表示未加抑制剂的反应组睾酮含量，R表示加入待测抑制剂的反应组睾酮含量。
酶反应体系中各组分的原始浓度分别为：缓冲溶液[Tris-HCl,pH 7.4]；NADPH浓度(10mmol/L，Sigma 93205)；5α-还原酶浓度为10mg/mL；睾酮4μg/mL；度他雄胺浓度均0.5mg/mL。
表7反应体系加液表

/代表不加相应物质
测试结果如图1所示，实施例1、实施例2、实施例3、对比例1、对比例2、对比例3和对比例4均具有显著的体外抑制5α-还原酶活性，实施例1抑制率为69.44％、实施例2抑制率为87.75％、实施例3抑制率为78.03％、对比例1抑制率为44.16％、对比例2抑制率为52.50％，对比例3的抑制率为54.68％，而对比例4的抑制率为5.22％。以实施例2的抑制效果最为明显，说明该控油舒缓护肤组合物具有显著的抑制5α-还原酶活性功能，从而达到控油功效。
试验例3：体外抑制IL-1α、TNF-α、COX2及PGE2因子的活性实验
采用LPS(细菌脂多糖)诱导小鼠巨噬细胞Raw264.7，通过ELISA方法检测IL-1α、TNF-α、COX2及PGE2表达量，来评价受试物抑制相关细胞通路因子表达的能力。见表8测试方案。
表8测试方案

测试结果如表9-表12所示。
表9 IL-1α含量结果汇总表

(注：##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01；*表示与阴性对照相比，
0.01<p<0.05。)
从表9中可以看出，实施例1，2，3及对比例1，2，3，4均能显著抑制IL-1α的活性，实施例2的抑制效果最为显著，但对比例1，2，3，4的抑制率均低于实施例1，2，3，尤其对比例1远远低于
实施例2。表明该控油舒缓护肤组合物能显著抑制IL-1α的活性。
表10 TNF-α含量结果汇总表

(注：##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01；*表示与阴性对照相比，
0.01<p<0.05。)
从表10中可以看出，实施例1，2，3及对比例1，2，3，4均能显著抑制TNF-α的活性，但对比例1，2，3，4的抑制率均低于实施例1，2，3，尤其对比例1远远低于各实施例。表明该控油舒缓护肤组合物能显著抑制TNF-α的活性。
表11 PGE2含量结果汇总表

(注：##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01；*表示与阴性对照相比，
0.01<p<0.05。)
从表11中可以看出，实施例1，2，3及对比例1，2，3，4均能显著抑制PGE2的活性，实施例2的抑制效果最为显著，但对比例1，2，3，4的抑制率均低于实施例1，2，3，尤其对比例1远远低于各实施例。表明该控油舒缓护肤组合物能显著抑制PGE2的活性。
表12 COX2含量结果汇总表

(注：##表示与空白对照相比，p<0.01；**表示与阴性对照相比，p<0.01；*表示与阴性对照相比，
0.01<p<0.05。)
从表12中可以看出，实施例1，2，3及对比例1，2和3均能显著抑制COX2的活性，实施例2的抑制效果最显著，但对比例4无显著抑制能力，对比例1，2和3远低于各实施例。表明该控油舒缓护肤组合物能显著抑制COX2的活性。
从以上结果可以看出该控油舒缓护肤组合物能显著抑制IL-1α、TNF-α、COX2及PGE2因子的活性，具有一定的控油舒缓功效。
试验例4：实施例4的体外控油实验
本实验通过检测样品作用于皮脂腺细胞SZ95的脂滴含量，来评价受试物的控油功效。
根据表13测试方案，待24孔板中细胞铺板率达到40％～50％时，进行分组给药，每孔加样1mL，每组设3个复孔。给药完成后将24孔板放置在培养箱(37℃、5％CO2)中培养24h。
油红O染色：吸弃旧液，用PBS清洗细胞1次，每孔加入500μL油红O工作液(1μg/mL)，避光染色15min(孵育箱37℃孵育)，PBS洗涤2次。
根据脂滴合成油红O染色结果的OD值来评价控油能力。OD值越低表明分泌油脂含量越少，控油能力越强。
抑制率计算公式＝(NC组OD值-样品OD值)/NC组OD值*100％
表13测试方案设计
测试结果如图2所示，实施例4的OD值显著低于阴性对照组(NC组)，抑制率为12.63％，具有显著控油功效，因此说明含有该控油舒缓护肤组合物产品具有一定的控油能力。
试验例5：实施例4在人皮肤上控油中的效果
根据实施例4中的精华水产品，评价其在人体皮肤上的控油效果。
方法参考：T/ZHCA 002-2018《化妆品控油功效测试方法》。
选取年龄在18-50岁的30名健康女性/男性志愿者，其皮肤油脂含量Sebum≥120(μg/cm2)。
测试项目
其中T0是指受试者没有使用样品，T2是指受试者单次使用样品2小时，T4是指受试者单次使用样品4小时，T8是指受试者单次使用样品8小时。
本实验空白对照组选择对比例5。
检测方法：
1)样品区和空白区随机分布在前额左、右侧，确保所有样品区和空白区位置在统计学上达到平衡；
2)取测试样品0.5g涂抹于测量区域，不需要清洗，空白区涂抹对照样品；
3)按皮肤油脂测定仪进行样品区和空白区的测量，每个区域平行测定3次。先测量各测试区域的初始值(样品使用前)，然后在使用样品2h、4h、8h后测定样品区和空白区的皮肤油脂含量；
4)同一受试者的测试必须使用同一仪器由同一个测量人员完成；
样品使用期间如志愿者皮肤出现不良反应，应立即终止测试，并对志愿者进行适当医治，对不良反应予以记录。
油脂抑制率计算公式：(空白区增值-样品区增值)/空白区增值*100％
测试结果：
测试结果如图3和图4所示，单次使用样品2小时、4小时、8小时后，与对照样品空白区相比，样品皮肤油脂增量显著改善。使用样品两小时后抑制率为21.46％，使用样品4小时后抑制率为22.55％，使用样品8小时后抑制率为18.42％，
通过以上结果表明：实施例4的精华水产品能够改善皮肤油脂分泌，具有8小时控油效果，说明含有该控油舒缓护肤组合物的精华水产品具有显著的控油效果。
试验例6：实施例4在人皮肤上舒缓中的效果
制备的实施例4精华水产品进行人体皮肤功效测试，寻求18-40岁的志愿者30人(皮肤状态：肌肤敏感(乳酸刺痛阳性))进行产品测试。
检测时间：试用产品14天、28天；
检测设备：VISIA皮肤检测仪(美国CanField公司)。
本次测试采集受试者面部左、中、右三面标准光1、标准光2和交叉偏振光3种光源下的图片 并在交叉偏振光下导出的红区图片。对红区图片进行图像分析，得到量化指标红区分析a*值，用于评估面部皮肤发红、敏感状态的改善情况。
测试结果：
如图5中示例2名受试者使用样品前后面部红区变化的图片。
表14-1红区分析a*值描述性统计结果(n＝30)
表14-2红区分析a*值统计分析结果(n＝30)

统计分析结果：“-”：差异无统计学意义(P≥0.05)；“*”：差异有统计学意义(0.01≤P<
0.05)；“**”：差异有统计学意义(0.001≤P<0.01)；“***”：差异有统计学意义(P<0.001)。
红区分析a*值测试结果显示，与使用前相比，在使用测试样品4周后，红区分析a*值显著降低(0.01≤P<0.05)，说明含有该控油舒缓护肤组合物的产品具有舒缓功效。
通过以上结果表明：含有控油舒缓护肤组合物的产品能够达到控油舒缓皮肤的功效，用于护肤品中具有显著的效果。
应注意的是，以上实例仅用于说明本发明的技术方案而非对其进行限制。尽管参照所给出的实例对本发明进行了详细说明，但是本领域的普通技术人员可根据需要对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围。

Claims (18)

  1. 一种控油舒缓护肤组合物，其特征在于，所述组合物包含如下质量份数的组分：
    透明质酸锌0.1-1.0份，野葵果提取物1-20份，黄花前胡提取物1-20份；
    透明质酸锌分子量控制为40万-80万Da；
    所述野葵果提取物采用如下方法制备得到：
    S1、将野葵果粉碎过筛，以乙醇为溶剂采用渗漉法获取野葵果渗漉液；
    S2、将步骤S1得到的野葵果渗漉液进行蒸馏浓缩处理，然后向其中加入甘油即得；
    所述步骤S1中，过筛处理中选用60-100目筛；
    以乙醇为溶剂采用渗漉法获取野葵果渗漉液具体方法为：
    将粉碎过筛后的野葵果粉末置于渗漉筒中，加入3-8倍量的30％-70％乙醇浸泡6h～12h，以7-10mL/min的流速收集野葵果粉末10-20倍量的渗漉提取液并过滤得滤液；
    所述步骤S2中，蒸馏浓缩具体为在55-65℃条件下采用减压蒸馏处理，待滤液蒸发至剩余量为原有滤液的1/6-1/3时，加入剩余浓缩液1-1.5倍量的甘油，搅拌均匀过滤后即得；
    所述黄花前胡提取物采用如下方法制备得到：
    S1、将黄花前胡粉碎过筛，粉碎后的黄花前胡浸于乙醇中进行超声提取，过滤，收集滤液，滤渣重复提取2-3次，合并所得滤液；
    S2、将步骤S1制得滤液进行减压浓缩，回收乙醇至无醇味，加入丁二醇，搅拌均匀，过滤即得；
    所述步骤S1中，过筛处理选用30-60目筛；
    所述乙醇选用60％～85％乙醇，料液比为1:8-1:10，浸泡10-30min；超声提取过程中超声功率为100-300W，超声处理时间为30-40min；
    所述步骤S2中，减压浓缩具体为在50-60℃条件下进行减压蒸馏处理，回收乙醇至无醇味得黄花前胡浓缩液，加入所述黄花前胡浓缩液2～2.5倍质量的丁二醇，搅拌均匀，过滤后即得。
  2. 如权利要求1所述的控油舒缓护肤组合物，其特征在于，所述透明质酸锌分子量为50万-70万Da。
  3. 如权利要求1所述的控油舒缓护肤组合物，其特征在于，所述野葵果提取物的制备方法中，步骤S1过筛处理选用80目筛；
    以乙醇为溶剂采用渗漉法获取野葵果渗漉液具体方法为：
    将粉碎过筛后的野葵果粉末置于渗漉筒中，加入为5倍量的50％乙醇浸泡6h～12h，以7-10mL/min的流速收集野葵果粉末15倍量的渗漉提取液并过滤得滤液；
    步骤S2中，蒸馏浓缩具体为在55-65℃条件下采用减压蒸馏处理，待滤液蒸发至剩余量为原有滤液的1/5时，加入剩余浓缩液1-1.5倍量的甘油，搅拌均匀过滤后即得。
  4. 如权利要求1所述的控油舒缓护肤组合物，其特征在于，所述黄花前胡提取物的制备方法中，步骤S1中过筛处理选用50目筛；乙醇浸泡时间为20min；超声提取过程中超声功率为200W。
  5. 权利要求1-4任一项所述组合物在制备控油舒缓护肤的化妆品中的应用。
  6. 一种控油舒缓护肤的化妆品，其特征在于，所述化妆品其包含权利要求1-4任一项所述组合物。
  7. 如权利要求6所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述控油舒缓护肤组合物的加入量为0.5-40％。
  8. 如权利要求7所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述控油舒缓护肤组合物的加入量为2-25％。
  9. 如权利要求6所述的控油舒缓护肤的化妆品，其特征在于，所述控油舒缓护肤化妆品还包含括乳化剂、润肤剂、保湿剂和增稠剂。
  10. 如权利要求9所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述乳化剂的加入量为1-6％。
  11. 如权利要求10所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述乳化剂的加入量为2-5％。
  12. 如权利要求9所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述润肤剂的加入量为6-25％。
  13. 如权利要求12所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述润肤剂的加入量为8-20％。
  14. 如权利要求9所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述保湿剂的加入量为2-15％。
  15. 如权利要求14所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述保湿剂的加入量为5-12％。
  16. 如权利要求9所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述增稠剂的加入量为0.02-1.0％。
  17. 如权利要求16所述的控油舒缓护肤的化妆品，其特征在于，以所述控油舒缓护肤化妆品的总质量计，所述增稠剂的加入量为0.05-0.8％。
  18. 权利要求6-17任一项所述控油舒缓护肤的化妆品的制备方法，其特征在于，所述制备方法包括将各原料组分混合的步骤。
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