WO2022199507A1 - Anti-irritation composition, preparation method therefor and application thereof - Google Patents

Anti-irritation composition, preparation method therefor and application thereof Download PDF

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Publication number
WO2022199507A1
WO2022199507A1 PCT/CN2022/081921 CN2022081921W WO2022199507A1 WO 2022199507 A1 WO2022199507 A1 WO 2022199507A1 CN 2022081921 W CN2022081921 W CN 2022081921W WO 2022199507 A1 WO2022199507 A1 WO 2022199507A1
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Prior art keywords
preparation
irritant composition
parts
irritation
irritant
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PCT/CN2022/081921
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French (fr)
Chinese (zh)
Inventor
刘有停
苏牧楠
吕永博
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北京东方淼森生物科技有限公司
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Priority to JP2023557286A priority Critical patent/JP2024510767A/en
Publication of WO2022199507A1 publication Critical patent/WO2022199507A1/en

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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
    • A61K8/96—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
    • A61Q19/10—Washing or bathing preparations
    • 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
    • A61K2800/75—Anti-irritant

Definitions

  • the present invention relates to an anti-irritant composition and its preparation method and application.
  • the patent discloses an anti-irritant composition and a preparation method thereof: (1) extracting peach gum and cactus with water to obtain an initial extract, preferably, the weight ratio of peach gum and cactus is 1:5 -15:1, preferably 1:10-10:1; (2) centrifuging the primary extract to obtain a supernatant; (3) subjecting the supernatant to microfiltration to obtain a microfiltrate.
  • the microfiltrate was mixed with the components described (dextrin, cyclodextrin, methylcyclodextrin, hydroxypropylcyclodextrin, trehalose, polyvinylpyrrolidone, methylcellulose, methylhydroxyethylcellulose, hydroxyethylcellulose propyl methyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose) are mixed to produce solids; (5) the solids produced after mixing in step (4) are dried. But it is only for skin irritation caused by surfactants in cosmetics.
  • an anti-irritant composition that alleviates the problem of skin irritation caused by cosmetic irritants in various ways, avoids the problem of limited use of formulation raw materials due to irritation, and reduces adverse reactions caused by cosmetics. is very necessary.
  • the present invention provides an anti-irritant composition, which has simple composition of raw materials, simple preparation process, interaction between components, and can effectively resist skin irritation caused by cosmetic raw materials.
  • the anti-stimulation composition of the invention can antagonize lactic acid stimulation, improve the inhibition rate of erythrocyte hemolysis caused by SDS, and reduce the stimulation of chick embryo chorioallantoic membrane caused by SDS.
  • the anti-irritant composition of the present invention can antagonize the effects of various irritants in cosmetics. When applied in cosmetics, it is expected to have anti-irritant effect, which can antagonize skin irritation caused by various irritants in cosmetics, such as acidic substances, surfactants, flavors and fragrances, and preservatives.
  • a first aspect of the present invention provides an anti-irritant composition.
  • the anti-irritant composition comprises the following components in parts by weight: 1-30 parts of peach gum, 0.1-10 parts of cactus, 0.1-10 parts of Centella asiatica, and 0.01-5 parts of psyllium.
  • the anti-irritant composition includes the following components in parts by weight: 1-5 parts of peach gum, 0.5-2 parts of cactus, 0.5-2 parts of Centella asiatica, 0.1-1 parts of psyllium share.
  • the anti-irritant composition further comprises component 5).
  • the component 5) is selected from one of dextrin, cyclodextrin, maltodextrin, hydroxypropyl- ⁇ -cyclodextrin, ⁇ -cyclodextrin, and resistant dextrin or several.
  • the plant composition is prepared by a preparation method comprising the following steps:
  • the weight ratio of the total weight of peach gum, cactus, Centella asiatica and psyllium to water is 1:10-1:80 (m/m).
  • the weight ratio of the total weight of peach gum, cactus, Centella asiatica and psyllium to water in step (1) may be 1:10 (m/m), 1:11 (m/m) ), 1: 12(m/m), 1: 13(m/m), 1: 14(m/m), 1: 15(m/m), 1: 16(m/m), 1: 17 (m/m), 1: 18 (m/m), 1: 20 (m/m), 1: 30 (m/m), 1: 40 (m/m), 1: 45 (m/m) , 1:50(m/m), 1:55(m/m), 1:60(m/m), 1:65(m/m), 1:70(m/m), 1:75( m/m), 1:80 (m/m), and point values between the above values.
  • the extraction temperature in step (1) of the preparation method is 50-100°C.
  • the extraction temperature in step (1) of the preparation method can be 50°C, 51°C, 52°C, 53°C, 54°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, 90°C, 95°C, 100°C, and points in between.
  • the extraction time in step (1) of the preparation method is 0.5-5h.
  • the extract is concentrated by 1-5 times.
  • the addition amount of component 5) is 1-30% based on the weight of the total feed liquid.
  • the amount of glycerol added is 10-50% based on the weight of the total feed liquid.
  • step (2) of the preparation method the amount of trehalose added is 1-30% based on the weight of the total feed liquid.
  • step (2) of the preparation method conventional cosmetic accessories include preservatives, chelating agents, and thickening agents.
  • the preservatives are hexanediol and pentanediol.
  • the chelating agent is disodium EDTA.
  • the thickening agent is xanthan gum.
  • the addition amount of hexanediol is 0.1-5%.
  • the addition amount of pentanediol is 0.1-5%.
  • the amount of disodium EDTA added is 0.01-5%.
  • the added amount of xanthan gum is 0.01-1%.
  • the sterilization method in step (3) of the preparation method is a conventional sterilization method in the field.
  • the sterilization method in step (3) of the preparation method is high temperature sterilization.
  • the sterilization temperature in step (3) of the preparation method is 70-100°C.
  • the sterilization time in step (3) of the preparation method is 20-60 min.
  • the second aspect of the present invention provides a method for preparing the anti-irritant composition of the first aspect of the present invention.
  • the preparation method of the anti-irritant composition comprises the following steps:
  • the initial extract is compounded with 1-30% component 5) (based on the weight of the total feed liquid, the same below), 10-50% glycerol, 1-30% trehalose, 1-30% component 5), 0.1-5% hexanediol, 0.1-5% pentanediol, 0.01-5% disodium EDTA, 0.01-1% xanthan gum;
  • the anti-irritant composition in step (1) of the preparation method includes the following components in parts by weight: 1-5 parts of peach gum, 0.5-2 parts of cactus, 0.5-2 parts of Centella asiatica, 0.1-1 servings of psyllium.
  • component 5) in step (2) of the preparation method is selected from dextrin, cyclodextrin, maltodextrin, hydroxypropyl- ⁇ -cyclodextrin, ⁇ -cyclodextrin, resistant dextrin one or more of them.
  • the sterilization method in step (3) of the preparation method is high temperature sterilization.
  • the sterilization temperature in step (3) of the preparation method is 70-100°C.
  • the sterilization time in step (3) of the preparation method is 20-60 min.
  • the third aspect of the present invention provides that the anti-irritant composition of the first aspect of the present invention and/or the anti-irritant composition prepared by the preparation method of the anti-irritant composition of the second aspect of the present invention can be used in cosmetics and/or skin care products. application.
  • the anti-irritant composition is used in the preparation of skin care products and/or cosmetics for anti-irritation and antagonism of irritation sources in cosmetics.
  • the cosmetics and/or types and dosage forms are not particularly limited, such as facial masks, creams, facial cleansers, essences or lotions and the like.
  • the anti-irritant composition of the invention comprises peach gum, cactus, centella asiatica and psyllium, has simple material composition, simple preparation process, and interaction between components, which can effectively resist skin irritation caused by cosmetic raw materials.
  • Efficacy evaluation experiments confirmed that the anti-irritant composition of the present invention can antagonize lactic acid stimulation, improve the inhibition rate of erythrocyte hemolysis caused by SDS, reduce the stimulation of chicken embryo chorioallantoic membrane caused by SDS, and antagonize various stimuli in cosmetics.
  • it is expected to have anti-irritant effects, which can antagonize skin irritation caused by various irritants in cosmetics, such as lactic acid, surfactants, flavors and fragrances, and preservatives.
  • the main raw material name of the present invention, supplier/manufacturer, place of origin are as shown in Table 1:
  • Peach gum 3g, cactus 2g, psyllium 0.1g, according to the total raw materials: water 1:40 (m/m), add water 204g, extraction temperature 80 °C, extract 2h, filter, concentrate 1 times; take the weight of the concentrate Total, 24% Glycerol, 9% Trehalose, 9% Hydroxypropyl- ⁇ -Cyclodextrin, 1% Hexylene Glycol, 2% Pentylene Glycol, 0.2% Disodium EDTA, 0.05% Xanthan Gum, 90 Sterilize at °C for 40 min to obtain the anti-irritant composition of Comparative Example 1.
  • Peach gum 0.1g, cactus 1g, Centella asiatica 1g, psyllium 0.1g, according to the total raw materials: water 1:40 (m/m), add water 88g, extraction temperature 80 °C, extract 2h, filter, concentrate 1 24% glycerol, 9% trehalose, 9% hydroxypropyl- ⁇ -cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05 % xanthan gum, sterilized at 90° C. for 40 min, to obtain the anti-irritant composition of Comparative Example 3.
  • peach gum 1g of Centella asiatica, 0.1g of Psyllium Liquid weight, compound 24% glycerin, 9% trehalose, 9% hydroxypropyl- ⁇ -cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum , sterilized at 90° C. for 40 min, to obtain the anti-irritant composition of Comparative Example 9.
  • Test Example 1 Antagonizing the stimulation of acidic substances
  • Test samples Examples 1-6, Comparative Examples 1-9;
  • Table 2 embodiment 1 lactic acid stimulation score summary table
  • Table 3 embodiment 2 lactic acid stimulation score summary table
  • Table 6 embodiment 5 lactic acid stimulation score summary table
  • Example 1-6 lactic acid stinging score difference and pruritus score difference are all higher, and it has a significant effect on skin stinging and itching caused by lactic acid.
  • the anti-irritant composition has a better effect of antagonizing lactic acid stimulation; compared with Comparative Examples 3-4, the difference between the lactic acid stinging score and the pruritus score difference in Examples 1-6 are higher, indicating that the present invention combines peach gum, The combination of Cactus, Centella asiatica and Psyllium chinensis produced an obvious synergistic effect in a certain proportion, and its effect was better than the combination of some components, and it had a better effect of antagonizing lactic acid stimulation.
  • the erythrocyte hemolysis coagulation test was used to investigate the antagonistic effects of Examples 1-6 and Comparative Examples 1-9 on the inhibition rate of erythrocyte hemolysis caused by SDS.
  • H50 the system concentration of SDS when the hemolysis rate is 50%.
  • the H50 is required to be in the range of 25.7-33.1mg/L.
  • test concentration is the test concentration
  • Erythrocyte hemolysis inhibition rate (%) (OD_negative control group-OD_sample group)/OD_negative control group ⁇ 100.
  • the anti-irritant compositions of the present invention 1-6 have higher inhibition rates of erythrocyte hemolysis caused by SDS than the anti-irritant compositions obtained in Comparative Example 1, Comparative Examples 6-7, and Comparative Examples 8-9 and
  • the inhibition rate of erythrocyte hemolysis caused by SDS by the single extract obtained in Example 2 and Comparative Example 5 shows that the anti-irritant composition of the present invention has more anti-inflammatory properties than any single extract and any combination of two or three raw materials.
  • the stimulating composition can better antagonize the inhibition rate of erythrocyte hemolysis caused by SDS, which shows that the combination of peach gum, cactus, Centella asiatica and psyllium in the present invention has produced obvious synergistic effect;
  • the inhibitory rate of the stimulatory composition to erythrocyte hemolysis caused by SDS reaches more than 75%, while the inhibition rate of the erythrocyte hemolysis caused by SDS to the comparative examples 3-4 is lower.
  • Different components have a mutually promoting effect, and have a better antagonistic effect on erythrocyte hemolysis caused by SDS.
  • 1Egg selection select SPF-grade Bailaihang chicken fertilized eggs (purchased by Beijing Melia Experimental Animal Co., Ltd.). The quality of eggs meets the requirements of relevant standards, and the supplier should have the qualification of "Designated Production Enterprise of SPF Chicken (Egg) for Veterinary Drug Production and Inspection" recognized by the agricultural department. Eggs should be fresh, clean and intact, with a mass of 50g-60g. When hatching to 4 days of age, the eggs should be checked, and the unfertilized chicken embryos should be discarded, and the broken or thin-shelled chicken embryos should not be used.
  • Incubation conditions Incubation temperature 37.5 ⁇ 0.5°C, relative humidity 55-70%, turntable frequency 3-6 times/h, turn the eggs for 3 days, and stop turning the eggs after opening the window on the 4th day.
  • 3CAM preparation When the chicken embryo hatched for 4 days, use an electric grinder to make holes in the small end of the egg, use a 10mL syringe to extract 2-3mL of egg white, and then use an electric grinder to open a 1cm ⁇ 1cm window in the middle of the egg slightly near the big end. , expose the CAM, and carefully remove the eggshell and eggshell membrane with tweezers to ensure that the embryonic allantoic membrane is not damaged. At this time, the structure of the vascular system and the growth of the chicken embryo should be observed. After sealing the hole at the small end and the small window in the middle with scotch tape, put it into the incubator to continue culturing.
  • test substance is a group, 6 chicken embryos are tested in each group, and 40 ⁇ l of the test substance is directly applied to the surface of the CAM in the Teflon ring. After 30min exposure at 37°C, the changes of chorioallantoic membrane toxicity index (such as: bleeding, vasolysis and coagulation, etc.) were observed, and combined to calculate the endpoint score (ES). The end point score of the test substance treatment group is compared with that of the negative control, and the lower the end point score of the sample, the stronger the anti-stimulation effect of the test substance is.
  • Test samples anti-irritant compositions prepared in Examples 1-6 and Comparative Examples 1-9.
  • Table 20 Summary table of chicken embryo chorioallantoic membrane stimulation scores
  • Example 1 Chicken embryo chorioallantoic membrane stimulation score (ES) stimulus level 0.1% SDS+5%
  • Example 1 8 mild stimulation 0.1% SDS + 5%
  • Example 2 9 mild stimulation 0.1% SDS + 5%
  • Example 3 6 mild stimulation 0.1% SDS + 5%
  • Example 4 7 mild stimulation 0.1% SDS + 5%
  • Example 5 4 mild stimulation 0.1% SDS + 5%
  • Example 6 6 mild stimulation 0.1% SDS+5% Comparative Example 1 12 Moderate stimulation 0.1% SDS+5% Comparative Example 2 13 Moderate stimulation 0.1% SDS+5% Comparative Example 3 14 Moderate stimulation 0.1% SDS+5% Comparative Example 4 14 Moderate stimulation 0.1% SDS+5% Comparative Example 5 14 Moderate stimulation 0.1% SDS+5% Comparative Example 6 14 Moderate stimulation 0.1% SDS+5% Comparative Example 7 13 Moderate stimulation 0.1% SDS+5% Comparative Example 8 13 Moderate stimulation 0.1% SDS+5% Comparative Example 9 14 Moderate stimulation 0.1% SDS 15 Moderate stimulation normal saline 0 No stimulation
  • the 0.1% SDS+5% anti-irritant compositions of Examples 1-6 of the present invention can stimulate the chicken embryo chorioallantoic membrane (ES) by SDS less than 10, while 0.1% SDS+5% of the present invention
  • the irritation scores (ES) of the chicken embryo chorioallantoic membrane caused by the anti-irritant compositions of Examples 1-6 were all greater than 12.
  • the fraction of the chicken embryo chorioallantoic membrane stimulation by the anti-irritant compositions of Examples 1-6 of the present invention caused by SDS is lower than that of the single extract obtained in Example 2, Comparative Example 5, and Comparative Examples 1, 6-7 and Comparative Examples 8-9
  • the obtained anti-irritant composition can stimulate the chicken embryo chorioallantoic membrane fraction caused by SDS.
  • the anti-irritant composition can better reduce the stimulation of the chick embryo chorioallantoic membrane caused by SDS, which shows that when the composition of the present invention is used in combination, it can antagonize the effect of SDS stimulation through a synergistic effect; compared with Comparative Examples 3-4,
  • the anti-irritant composition of the present invention has better antagonistic effect on the stimulation of the chick embryo chorioallantoic membrane caused by SDS, and by rationally compounding the components, a synergistic effect is produced, and the efficacy of the anti-irritant composition of the present invention to antagonize the stimulation of SDS is increased. .
  • phenoxyethanol can be used as a preservative irritant representative to verify the efficacy of anti-irritant compositions.
  • 1% phenoxyethanol as the stimulus source, 5 volunteers (aged 18-55, male or female, meeting volunteer standards) who were sensitive to phenoxyethanol stimulation were screened for the test.
  • 1% phenoxyethanol (stimulation group), 3% test sample + 1% phenoxyethanol (sample group) were applied to the two nasolabial folds of the volunteers respectively, 0.5min, 2.5min, 5min, 7.5min after application
  • the stinging and burning sensations were scored at 10 minutes on a scale of 0-3, with 0 representing no stinging and burning, 1 indicating mild stinging and burning, 2 indicating moderate stinging and burning, and 3 points.
  • Score difference mean stimulation score of stimulation group - mean stimulation score of sample group. The larger the score difference, the better the antagonistic effect of phenoxyethanol stimulation.
  • the difference in the stinging scores of eugenol in Examples 1-6 is higher than that in Comparative Examples 1-9, indicating that the anti-irritant composition of the present invention has a better effect of antagonizing eugenol stimulation
  • the eugenol stinging score difference of embodiment 1-6 is higher, and it has better inhibitory effect on the skin stinging caused by eugenol, The effect is better than that of each component used alone, and also better than the combination of some components, showing obvious synergistic effect, which shows that the synergistic effect of the four components of peach gum, cactus, Centella asiatica and psyllium , the anti-irritant composition of the present invention has a better effect of antagonizing the stimulation of eugenol; compared with the comparative examples 3-4, the difference between the stinging scores of eugenol in Examples 1-6
  • the anti-irritant composition of the present invention can effectively prevent, antagonize or restore the efficacy of various irritants in cosmetics by combining peach gum, cactus, Centella asiatica and psyllium in a specific ratio, and the components interact with each other.
  • various irritants such as acidic substances, surfactants, preservatives, spices, etc.
  • it is expected to have anti-irritant effects, which can antagonize skin irritation caused by various irritants in cosmetics.

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Abstract

Disclosed are an anti-irritation composition, a preparation method therefor and the application thereof. The anti-irritation composition comprises peach gum, cactus, Centella asiatica, and Semen plantaginis. The material composition is simple, the preparation process is simple, all the components interact with each other, and skin irritation caused by cosmetics raw materials can be effectively resisted. Efficacy evaluation experiments have proven that the anti-irritation composition of the present invention can antagonize lactic acid irritation, improve the rate of inhibition of red blood cell hemolysis caused by sodium dodecyl sulfate (SDS), reduce chick chorioallantoic membrane irritation caused by SDS, and antagonize various irritation sources in cosmetics. When the composition is applied to cosmetics, the composition is expected to have an anti-irritation efficacy and can antagonize skin irritation caused by various irritation sources, such as acidic substances, surfactants, flavors and fragrances, preservatives etc. in cosmetics raw materials.

Description

一种抗刺激组合物及其制备方法和应用A kind of anti-irritant composition and its preparation method and application 技术领域technical field
本发明涉及一种抗刺激组合物及其制备方法和应用。The present invention relates to an anti-irritant composition and its preparation method and application.
背景技术Background technique
随着生活水平的不断提高，人们对美容和护肤追求也越来越高。近年来，我国化妆品的生产量和消费量急剧增长，由此产生的皮肤不良反应问题日益增加，引起人们的广泛关注。化妆品皮肤不良反应已成为皮肤科一种常见病。在我国，2005-2014年共报告13534例化妆品不良反应患者，其中女性占95.40％，中青年患者(20-44岁)占80.85％，确诊病例5446例，病变类型以化妆品不良反应接触性皮炎为主(94.66％)，另有未包含在诊断标准中的其他病变类型132例，确诊病例共涉及14209个化妆品。由此看来，化妆品不良反应现象日益增多，无论是消费者还是化妆品企业，都需对其引起高度重视，化妆品不良反应问题亟待解决。因此，急切需要开发具有有效拮抗化妆品刺激的原料。With the continuous improvement of living standards, people's pursuit of beauty and skin care is also getting higher and higher. In recent years, the production and consumption of cosmetics in my country have increased sharply, and the resulting problems of adverse skin reactions have been increasing, causing widespread concern. Cosmetic skin adverse reactions have become a common disease in dermatology. In my country, from 2005 to 2014, a total of 13,534 patients with cosmetic adverse reactions were reported, of which women accounted for 95.40%, young and middle-aged patients (20-44 years old) accounted for 80.85%, and 5,446 confirmed cases. (94.66%), and 132 cases of other lesion types not included in the diagnostic criteria. A total of 14,209 cosmetic cases were involved in the confirmed cases. From this point of view, the phenomenon of adverse reactions to cosmetics is increasing day by day. Both consumers and cosmetics companies need to pay great attention to them. The problem of adverse reactions to cosmetics needs to be solved urgently. Therefore, there is an urgent need to develop a raw material having an effective antagonistic against cosmetic irritation.
专利(CN201911356697.5)公开了一种抗刺激组合物及其制备方法：(1)将桃胶和仙人掌用水进行提取，得到初提液，优选地，桃胶和仙人掌的重量比为1:5-15:1，优选为1:10-10:1；(2)将初提液进行离心，得到上清液；(3)将所述上清液进行微滤，得到微滤液。将微滤液与所述组分(糊精、环糊精、甲基环糊精、羟丙基环糊精、海藻糖、聚乙烯吡咯烷酮、甲基纤维素、甲基羟乙基纤维素、羟丙基甲基纤维素、羟乙基纤维素和羟丙基纤维素)进行混合，产生固体物；(5)将步骤(4)混合后产生的固体物进行干燥。但其仅针对化妆品中表面活性剂引起的皮肤刺激问题。The patent (CN201911356697.5) discloses an anti-irritant composition and a preparation method thereof: (1) extracting peach gum and cactus with water to obtain an initial extract, preferably, the weight ratio of peach gum and cactus is 1:5 -15:1, preferably 1:10-10:1; (2) centrifuging the primary extract to obtain a supernatant; (3) subjecting the supernatant to microfiltration to obtain a microfiltrate. The microfiltrate was mixed with the components described (dextrin, cyclodextrin, methylcyclodextrin, hydroxypropylcyclodextrin, trehalose, polyvinylpyrrolidone, methylcellulose, methylhydroxyethylcellulose, hydroxyethylcellulose propyl methyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose) are mixed to produce solids; (5) the solids produced after mixing in step (4) are dried. But it is only for skin irritation caused by surfactants in cosmetics.
因此，针对上述问题，开发一种从多种途径缓解化妆品刺激源引起皮肤刺激的问题，避免了配方原料因刺激性使用受限的问题，减少了化妆品引起皮肤刺激的不良反应的抗刺激组合物是十分必要的。Therefore, in view of the above problems, an anti-irritant composition is developed that alleviates the problem of skin irritation caused by cosmetic irritants in various ways, avoids the problem of limited use of formulation raw materials due to irritation, and reduces adverse reactions caused by cosmetics. is very necessary.
发明内容SUMMARY OF THE INVENTION
基于上述现有技术的缺陷，本发明提供了一种抗刺激组合物，该组合物原料组成简单，制备工艺简单，各组分之间相互作用，可有效抵御化妆品原料引起的皮肤刺激。Based on the above-mentioned defects of the prior art, the present invention provides an anti-irritant composition, which has simple composition of raw materials, simple preparation process, interaction between components, and can effectively resist skin irritation caused by cosmetic raw materials.
本发明的抗刺激组合物能够拮抗乳酸刺激、提高SDS引起的红细胞溶血抑制率，降低SDS引起鸡胚绒毛尿囊膜刺激。The anti-stimulation composition of the invention can antagonize lactic acid stimulation, improve the inhibition rate of erythrocyte hemolysis caused by SDS, and reduce the stimulation of chick embryo chorioallantoic membrane caused by SDS.
本发明的抗刺激组合物可拮抗化妆品中各种刺激源等功效。将其应用于化妆品中，预计具有抗刺激功效，可拮抗化妆品中各种刺激源如酸性物质、表面活性剂、香精香料、防腐剂等引起的皮肤刺激性。The anti-irritant composition of the present invention can antagonize the effects of various irritants in cosmetics. When applied in cosmetics, it is expected to have anti-irritant effect, which can antagonize skin irritation caused by various irritants in cosmetics, such as acidic substances, surfactants, flavors and fragrances, and preservatives.
本发明所要解决的技术问题是通过以下技术方案来实现的：The technical problem to be solved by this invention is realized through the following technical solutions:
本发明第一个方面提供了一种抗刺激组合物。A first aspect of the present invention provides an anti-irritant composition.
根据本发明，所述抗刺激组合物包括以下重量份数的组分：桃胶1-30份、仙人掌0.1-10份、积雪草0.1-10份、车前子0.01-5份。According to the present invention, the anti-irritant composition comprises the following components in parts by weight: 1-30 parts of peach gum, 0.1-10 parts of cactus, 0.1-10 parts of Centella asiatica, and 0.01-5 parts of psyllium.
根据本发明一些具体实施方式，所述抗刺激组合物包括以下重量份数的组分：桃 胶1-5份、仙人掌0.5-2份、积雪草0.5-2份、车前子0.1-1份。According to some specific embodiments of the present invention, the anti-irritant composition includes the following components in parts by weight: 1-5 parts of peach gum, 0.5-2 parts of cactus, 0.5-2 parts of Centella asiatica, 0.1-1 parts of psyllium share.
根据本发明，所述抗刺激组合物，所述抗刺激组合物还包括组分5)。According to the present invention, the anti-irritant composition further comprises component 5).
根据本发明一些具体实施方式，所述组分5)选自糊精、环糊精、麦芽糊精、羟丙基-β-环糊精、β-环糊精、抗性糊精的一种或几种。According to some specific embodiments of the present invention, the component 5) is selected from one of dextrin, cyclodextrin, maltodextrin, hydroxypropyl-β-cyclodextrin, β-cyclodextrin, and resistant dextrin or several.
根据本发明，所述植物组合物通过包括以下步骤的制备方法制备：According to the present invention, the plant composition is prepared by a preparation method comprising the following steps:
(1)将桃胶、仙人掌、积雪草和车前子提取，过滤，浓缩，得初提液；(1) extracting peach gum, cactus, Centella asiatica and psyllium, filtering, concentrating to obtain primary extract;
(2)将初提液复配组分5)、甘油、海藻糖和化妆品常规辅料；(2) compound component 5), glycerol, trehalose and cosmetic conventional auxiliary materials with the primary extract;
(3)灭菌，得抗刺激组合物。(3) Sterilization to obtain an anti-irritant composition.
根据本发明，所述制备方法步骤(1)中桃胶、仙人掌、积雪草和车前子总重量与水的重量比为1:10-1:80(m/m)。According to the present invention, in step (1) of the preparation method, the weight ratio of the total weight of peach gum, cactus, Centella asiatica and psyllium to water is 1:10-1:80 (m/m).
根据本发明的一些实施方式，步骤(1)中桃胶、仙人掌、积雪草和车前子总重量与水的重量比可以是1：10(m/m)、1：11(m/m)、1：12(m/m)、1：13(m/m)、1：14(m/m)、1：15(m/m)、1：16(m/m)、1：17(m/m)、1：18(m/m)、1：20(m/m)、1：30(m/m)、1：40(m/m)、1：45(m/m)、1：50(m/m)、1：55(m/m)、1：60(m/m)、1：65(m/m)、1：70(m/m)、1：75(m/m)、1：80(m/m)，以及上述数值之间的点值。According to some embodiments of the present invention, the weight ratio of the total weight of peach gum, cactus, Centella asiatica and psyllium to water in step (1) may be 1:10 (m/m), 1:11 (m/m) ), 1: 12(m/m), 1: 13(m/m), 1: 14(m/m), 1: 15(m/m), 1: 16(m/m), 1: 17 (m/m), 1: 18 (m/m), 1: 20 (m/m), 1: 30 (m/m), 1: 40 (m/m), 1: 45 (m/m) , 1:50(m/m), 1:55(m/m), 1:60(m/m), 1:65(m/m), 1:70(m/m), 1:75( m/m), 1:80 (m/m), and point values between the above values.
根据本发明，所述制备方法步骤(1)中提取温度为50-100℃。According to the present invention, the extraction temperature in step (1) of the preparation method is 50-100°C.
根据本发明，所述制备方法步骤(1)中提取温度可以是50℃、51℃、52℃、53℃、54℃、55℃、60℃、65℃、70℃、75℃、80℃、85℃、90℃、95℃、100℃，以及上述数值之间的点值。According to the present invention, the extraction temperature in step (1) of the preparation method can be 50°C, 51°C, 52°C, 53°C, 54°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, 90°C, 95°C, 100°C, and points in between.
根据本发明，所述制备方法步骤(1)中提取时间0.5-5h。According to the present invention, the extraction time in step (1) of the preparation method is 0.5-5h.
根据本发明，所述步骤(1)中提取液浓缩1-5倍。According to the present invention, in the step (1), the extract is concentrated by 1-5 times.
根据本发明，所述制备方法步骤(2)中以总料液重量计，组分5)添加量为1-30％。According to the present invention, in step (2) of the preparation method, the addition amount of component 5) is 1-30% based on the weight of the total feed liquid.
根据本发明，所述制备方法步骤(2)中以总料液重量计，甘油添加量为10-50％。According to the present invention, in step (2) of the preparation method, the amount of glycerol added is 10-50% based on the weight of the total feed liquid.
根据本发明，所述制备方法步骤(2)中以总料液重量计，海藻糖添加量为1-30％。According to the present invention, in step (2) of the preparation method, the amount of trehalose added is 1-30% based on the weight of the total feed liquid.
根据本发明，所述制备方法步骤(2)中化妆品常规辅料包括防腐剂、螯合剂、增稠剂。According to the present invention, in step (2) of the preparation method, conventional cosmetic accessories include preservatives, chelating agents, and thickening agents.
根据本发明一些具体实施方式，所述防腐剂为己二醇、戊二醇。According to some specific embodiments of the present invention, the preservatives are hexanediol and pentanediol.
根据本发明一些具体实施方式，所述螯合剂为EDTA二钠。According to some specific embodiments of the present invention, the chelating agent is disodium EDTA.
根据本发明一些具体实施方式，所述增稠剂为黄原胶。According to some embodiments of the present invention, the thickening agent is xanthan gum.
根据本发明一些具体实施方式，以总料液重量计，己二醇添加量为0.1-5％。According to some specific embodiments of the present invention, based on the weight of the total feed liquid, the addition amount of hexanediol is 0.1-5%.
根据本发明一些具体实施方式，以总料液重量计，戊二醇添加量为0.1-5％。According to some specific embodiments of the present invention, based on the weight of the total feed liquid, the addition amount of pentanediol is 0.1-5%.
根据本发明一些具体实施方式，以总料液重量计，EDTA二钠添加量为0.01-5％。According to some specific embodiments of the present invention, based on the weight of the total feed liquid, the amount of disodium EDTA added is 0.01-5%.
根据本发明一些具体实施方式，以总料液重量计，黄原胶添加量为0.01-1％。According to some specific embodiments of the present invention, based on the weight of the total feed liquid, the added amount of xanthan gum is 0.01-1%.
根据本发明，所述制备方法步骤(3)中灭菌方式为本领域常规灭菌方式。According to the present invention, the sterilization method in step (3) of the preparation method is a conventional sterilization method in the field.
根据本发明，所述制备方法步骤(3)中灭菌方式为高温灭菌。According to the present invention, the sterilization method in step (3) of the preparation method is high temperature sterilization.
根据本发明，所述制备方法步骤(3)中灭菌温度为70-100℃。According to the present invention, the sterilization temperature in step (3) of the preparation method is 70-100°C.
根据本发明，所述制备方法步骤(3)中灭菌时间为20-60min。According to the present invention, the sterilization time in step (3) of the preparation method is 20-60 min.
本发明第二个方面提供本发明第一方面所述抗刺激组合物的制备方法。The second aspect of the present invention provides a method for preparing the anti-irritant composition of the first aspect of the present invention.
根据本发明，所述抗刺激组合物制备方法包括以下步骤：According to the present invention, the preparation method of the anti-irritant composition comprises the following steps:
(1)桃胶1-30份、仙人掌0.1-10份、积雪草0.1-10份、车前子0.01-5份，按照总原 料：水＝1:10-1:80(m/m)，提取温度50-100℃条件下提取0.5-5h，过滤，浓缩1-5倍，得初提液；(1) 1-30 parts of peach gum, 0.1-10 parts of cactus, 0.1-10 parts of Centella asiatica, 0.01-5 parts of plantain seeds, according to the total raw materials: water = 1:10-1:80 (m/m) , extract at 50-100℃ for 0.5-5h, filter, and concentrate 1-5 times to obtain the primary extract;
(2)初提液复配1-30％组分5)(按照总料液重量计，下同)，10-50％甘油，1-30％海藻糖，1-30％组分5)，0.1-5％己二醇，0.1-5％戊二醇，0.01-5％EDTA二钠，0.01-1％黄原胶；(2) The initial extract is compounded with 1-30% component 5) (based on the weight of the total feed liquid, the same below), 10-50% glycerol, 1-30% trehalose, 1-30% component 5), 0.1-5% hexanediol, 0.1-5% pentanediol, 0.01-5% disodium EDTA, 0.01-1% xanthan gum;
(3)灭菌，得抗刺激组合物。(3) Sterilization to obtain an anti-irritant composition.
根据本发明一些具体实施方式，所述制备方法步骤(1)抗刺激组合物包括以下重量份数的组分：桃胶1-5份、仙人掌0.5-2份、积雪草0.5-2份、车前子0.1-1份。According to some specific embodiments of the present invention, the anti-irritant composition in step (1) of the preparation method includes the following components in parts by weight: 1-5 parts of peach gum, 0.5-2 parts of cactus, 0.5-2 parts of Centella asiatica, 0.1-1 servings of psyllium.
根据本发明，所述制备方法步骤(2)中组分5)选自糊精、环糊精、麦芽糊精、羟丙基-β-环糊精、β-环糊精、抗性糊精的一种或几种。According to the present invention, component 5) in step (2) of the preparation method is selected from dextrin, cyclodextrin, maltodextrin, hydroxypropyl-β-cyclodextrin, β-cyclodextrin, resistant dextrin one or more of them.
根据本发明，所述制备方法步骤(3)灭菌方式为高温灭菌。According to the present invention, the sterilization method in step (3) of the preparation method is high temperature sterilization.
根据本发明，所述制备方法步骤(3)中灭菌温度为70-100℃。According to the present invention, the sterilization temperature in step (3) of the preparation method is 70-100°C.
根据本发明，所述制备方法步骤(3)中灭菌时间为20-60min。According to the present invention, the sterilization time in step (3) of the preparation method is 20-60 min.
本发明第三个方面提供本发明第一方面所述抗刺激组合物和/或本发明第二方面所述抗刺激组合物制备方法制备得到的抗刺激组合物在化妆品和/或护肤品中得应用。The third aspect of the present invention provides that the anti-irritant composition of the first aspect of the present invention and/or the anti-irritant composition prepared by the preparation method of the anti-irritant composition of the second aspect of the present invention can be used in cosmetics and/or skin care products. application.
根据本发明，所述抗刺激组合物在制备用于抗刺激、拮抗化妆品中刺激源的护肤品和/或化妆品中的应用。According to the present invention, the anti-irritant composition is used in the preparation of skin care products and/or cosmetics for anti-irritation and antagonism of irritation sources in cosmetics.
根据本发明，所述化妆品和/或种类、剂型没有特殊限制，例如面膜、膏霜、洗面奶、精华液或乳液等。According to the present invention, the cosmetics and/or types and dosage forms are not particularly limited, such as facial masks, creams, facial cleansers, essences or lotions and the like.
本发明有益效果:Beneficial effects of the present invention:
本发明抗刺激组合物包括桃胶、仙人掌、积雪草、车前子，物质组成简单，制备工艺简单，各组分之间相互作用，可有效抵御化妆品原料引起的皮肤刺激。功效评价实验证实，本发明的抗刺激组合物能够拮抗乳酸刺激、提高SDS引起的红细胞溶血抑制率，降低SDS引起鸡胚绒毛尿囊膜刺激，拮抗化妆品中各种刺激源等功效。将其应用于化妆品中，预计具有抗刺激功效，可拮抗化妆品中各种刺激源如乳酸、表面活性剂、香精香料、防腐剂等引起的皮肤刺激性。The anti-irritant composition of the invention comprises peach gum, cactus, centella asiatica and psyllium, has simple material composition, simple preparation process, and interaction between components, which can effectively resist skin irritation caused by cosmetic raw materials. Efficacy evaluation experiments confirmed that the anti-irritant composition of the present invention can antagonize lactic acid stimulation, improve the inhibition rate of erythrocyte hemolysis caused by SDS, reduce the stimulation of chicken embryo chorioallantoic membrane caused by SDS, and antagonize various stimuli in cosmetics. When applied in cosmetics, it is expected to have anti-irritant effects, which can antagonize skin irritation caused by various irritants in cosmetics, such as lactic acid, surfactants, flavors and fragrances, and preservatives.
具体实施方式Detailed ways
下面结合具体实例对本发明进行进一步阐述，但本发明并不局限于此。The present invention will be further described below with reference to specific examples, but the present invention is not limited thereto.
下面实施例所述的实验方法，如无特殊说明，均为常规方法；所述的实验材料和试剂，如无特殊说明，均可从商业途径获得。The experimental methods described in the following examples are conventional methods unless otherwise specified; the experimental materials and reagents described above can be obtained from commercial sources unless otherwise specified.
本发明主要原料名称、供应商/生产商、产地如表1所示：The main raw material name of the present invention, supplier/manufacturer, place of origin are as shown in Table 1:
表1原料及来源Table 1 Raw materials and sources
原料名称raw material name 供应商/生产商Supplier/Manufacturer 产地Origin
桃胶peach gum 襄阳天马众合商贸有限公司Xiangyang Tianma Zhonghe Trading Co., Ltd. 云南Yunnan
仙人掌cactus 郑州格贝进出口贸易有限公司Zhengzhou Gebei Import & Export Trading Co., Ltd. 河南Henan
积雪草Centella 西畴县香光药材有限公司Xichou County Xiangguang Medicinal Materials Co., Ltd. 云南Yunnan
车前子psyllium 河北金叶子药业有限公司Hebei Golden Leaf Pharmaceutical Co., Ltd. 河北Hebei
海藻糖trehalose 广州朋远化工有限公司Guangzhou Pengyuan Chemical Co., Ltd. 日本Japan
甘油glycerin 广州朋远化工有限公司Guangzhou Pengyuan Chemical Co., Ltd. 马来西亚Malaysia
已二醇Hexylene glycol 北京仁泰科技有限公司Beijing Rentai Technology Co., Ltd. 德国Germany
戊二醇Pentylene glycol 北京仁泰科技有限公司Beijing Rentai Technology Co., Ltd. 德国Germany
EDTA二钠Disodium EDTA 南通奥凯生物技术开发有限公司Nantong Okay Biotechnology Development Co., Ltd. 江苏Jiangsu
黄原胶Xanthan Gum 北京徽之克贸易有限公司Beijing Huizhike Trading Co., Ltd. 美国U.S.
实施例1Example 1
桃胶3g，仙人掌1g，积雪草1g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水204g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得实施例1抗刺激组合物。3g peach gum, 1g cactus, 1g centella asiatica, 0.1g psyllium, according to the total raw materials: water = 1:40 (m/m), add 204g water, extract at 80°C, extract for 2h, filter, and concentrate 1 times ;Based on the weight of concentrate, compound 24% glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% Xanthan gum was sterilized at 90° C. for 40 minutes to obtain the anti-irritant composition of Example 1.
实施例2Example 2
桃胶10g，仙人掌5g，积雪草5g，车前子1g，按照总原料：水＝1:30(m/m)，加入水630g，提取温度70℃，提取3h，过滤，浓缩2倍；以浓缩液重量计，复配20％甘油，8％海藻糖，5％β-环糊精，1.5％己二醇，1.5％戊二醇，0.5％EDTA二钠，0.1％黄原胶，100℃灭菌30min，即得实施例2抗刺激组合物。10g of peach gum, 5g of cactus, 5g of Centella asiatica, 1g of psyllium, according to the total raw materials: water = 1:30 (m/m), add 630g of water, extract at 70°C, extract for 3h, filter, and concentrate twice; Based on the weight of the concentrate, compound 20% glycerol, 8% trehalose, 5% β-cyclodextrin, 1.5% hexanediol, 1.5% pentanediol, 0.5% disodium EDTA, 0.1% xanthan gum, 100 Sterilize at ℃ for 30 min to obtain the anti-irritant composition of Example 2.
实施例3Example 3
桃胶15g，仙人掌7g，积雪草5g，车前子3g，按照总原料：水＝1:50(m/m)，加入水1500g，提取温度50℃，提取5h，过滤，浓缩3倍；以浓缩液重量计，复配10％甘油，20％海藻糖，20％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.5％EDTA二钠，0.1％黄原胶，100℃灭菌30min，即得实施例3抗刺激组合物。15g of peach gum, 7g of cactus, 5g of Centella asiatica, 3g of psyllium, according to the total raw materials: water = 1:50 (m/m), add 1500g of water, extract at 50°C, extract for 5h, filter, and concentrate 3 times; Based on the weight of the concentrate, compound 10% glycerol, 20% trehalose, 20% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.5% disodium EDTA, 0.1% yellow The original gum was sterilized at 100° C. for 30 minutes to obtain the anti-irritant composition of Example 3.
实施例4Example 4
桃胶25g，仙人掌8g，积雪草8g，车前子5g，按照总原料：水＝1:70(m/m)，加入水3220g，提取温度95℃，提取1h，过滤，浓缩4倍；以浓缩液重量计，复配30％甘油，30％海藻糖，10％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.5％EDTA二钠，0.1％黄原胶，100℃灭菌30min，即得实施例4抗刺激组合物。25g of peach gum, 8g of cactus, 8g of Centella asiatica, 5g of Plantain seeds, according to the total raw materials: water = 1:70 (m/m), add 3220g of water, extract at 95°C, extract for 1 hour, filter, and concentrate 4 times; Based on the weight of the concentrate, compound 30% glycerol, 30% trehalose, 10% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.5% disodium EDTA, 0.1% yellow The original gum was sterilized at 100° C. for 30 minutes to obtain the anti-irritant composition of Example 4.
实施例5Example 5
桃胶30g，仙人掌10g，积雪草10g，车前子5g，按照总原料：水＝1:40(m/m)，加入水2200g，提取温度85℃，提取1h，过滤，浓缩2倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得实施例5抗刺激组合物。30g of peach gum, 10g of cactus, 10g of Centella asiatica, 5g of plantain seeds, according to the total raw materials: water = 1:40 (m/m), add 2200g of water, extract at 85°C, extract for 1 hour, filter, and concentrate twice; Based on the weight of the concentrate, compound 24% glycerin, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% yellow The original gum was sterilized at 90° C. for 40 minutes to obtain the anti-irritant composition of Example 5.
实施例6Example 6
桃胶1g，仙人掌0.1g，积雪草0.1g，车前子0.01g，按照总原料：水＝1:40(m/m)，加入水48.4g，提取温度85℃，提取1h，过滤，浓缩2倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得实施例6抗刺激组合物。1 g of peach gum, 0.1 g of cactus, 0.1 g of Centella asiatica, 0.01 g of psyllium, according to the total raw materials: water = 1:40 (m/m), add 48.4 g of water, extract at 85°C, extract for 1 hour, filter, Concentrated 2 times; based on the weight of the concentrate, compound 24% glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA , 0.05% xanthan gum, and sterilized at 90° C. for 40 minutes to obtain the anti-irritant composition of Example 6.
对比例1Comparative Example 1
桃胶3g，仙人掌2g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水204g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例1抗刺 激组合物。Peach gum 3g, cactus 2g, psyllium 0.1g, according to the total raw materials: water = 1:40 (m/m), add water 204g, extraction temperature 80 ℃, extract 2h, filter, concentrate 1 times; take the weight of the concentrate Total, 24% Glycerol, 9% Trehalose, 9% Hydroxypropyl-β-Cyclodextrin, 1% Hexylene Glycol, 2% Pentylene Glycol, 0.2% Disodium EDTA, 0.05% Xanthan Gum, 90 Sterilize at ℃ for 40 min to obtain the anti-irritant composition of Comparative Example 1.
对比例2Comparative Example 2
积雪草5.1g，按照总原料：水＝1:40(m/m)，加入水204g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例2抗刺激组合物。Centella asiatica 5.1g, according to the total raw material: water = 1:40 (m/m), add 204g of water, extract at 80°C, extract for 2h, filter, concentrate 1 times; based on the weight of the concentrate, compound 24% glycerol , 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum, sterilized at 90°C for 40min, that is, Comparative Example 2 Anti-irritant composition.
对比例3Comparative Example 3
桃胶0.1g，仙人掌1g，积雪草1g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水88g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例3抗刺激组合物。Peach gum 0.1g, cactus 1g, Centella asiatica 1g, psyllium 0.1g, according to the total raw materials: water = 1:40 (m/m), add water 88g, extraction temperature 80 ℃, extract 2h, filter, concentrate 1 24% glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05 % xanthan gum, sterilized at 90° C. for 40 min, to obtain the anti-irritant composition of Comparative Example 3.
对比例4Comparative Example 4
桃胶3g，仙人掌0.05g，积雪草1g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水166g，提取温度80℃，提取2h，过滤，浓缩1倍，；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例4抗刺激组合物。3g peach gum, 0.05g cactus, 1g centella asiatica, 0.1g psyllium, according to the total raw materials: water = 1:40 (m/m), add 166g water, extract at 80°C, extract for 2h, filter, concentrate 1 24% glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, based on the weight of the concentrate, 0.05% xanthan gum, sterilized at 90° C. for 40 min, to obtain the anti-irritant composition of Comparative Example 4.
对比例5Comparative Example 5
车前子5.1g，按照总原料：水＝1:40(m/m)，加入水204g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例5抗刺激组合物。Plantago 5.1g, according to the total raw material: water = 1:40 (m/m), add 204g of water, extract at 80°C, extract for 2h, filter, and concentrate 1 times; based on the weight of the concentrate, compound 24% glycerol , 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum, sterilized at 90°C for 40min, that is, Comparative Example 5 Anti-irritant composition.
对比例6Comparative Example 6
仙人掌1g，积雪草1g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水88g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例6抗刺激组合物。Cactus 1g, Centella asiatica 1g, Plantago 0.1g, according to the total raw materials: water = 1:40 (m/m), add water 88g, extraction temperature 80 ℃, extract 2h, filter, concentrate 1 times; By weight, compounded 24% glycerol, 9% trehalose, 9% hydroxypropyl-beta-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum, Sterilize at 90° C. for 40 minutes to obtain the anti-irritant composition of Comparative Example 6.
对比例7Comparative Example 7
桃胶3g，仙人掌1g，积雪草1g，按照总原料：水＝1:40(m/m)，加入水200g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例7抗刺激组合物。3g of peach gum, 1g of cactus, 1g of Centella asiatica, according to the total raw materials: water = 1:40 (m/m), add 200g of water, extract at 80°C, extract for 2h, filter, and concentrate 1 times; based on the weight of the concentrate , 24% glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum, 90℃ Sterilize for 40min to obtain the anti-irritant composition of Comparative Example 7.
对比例8Comparative Example 8
桃胶3g，仙人掌1g，按照总原料：水＝1:40(m/m)，加入水200g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例8抗刺激组合物。3 g of peach gum, 1 g of cactus, according to the total raw materials: water = 1:40 (m/m), add 200 g of water, extract at 80 ° C, extract for 2 hours, filter, and concentrate 1 times; based on the weight of the concentrate, compound 24% Glycerol, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum, sterilized at 90°C for 40min, namely An anti-irritant composition of Comparative Example 8 was obtained.
对比例9Comparative Example 9
桃胶3g，积雪草1g，车前子0.1g，按照总原料：水＝1:40(m/m)，加入水204g，提取温度80℃，提取2h，过滤，浓缩1倍；以浓缩液重量计，复配24％甘油，9％海藻糖，9％羟丙基-β-环糊精，1％己二醇，2％戊二醇，0.2％EDTA二钠，0.05％黄原胶，90℃灭菌40min，即得对比例9抗刺激组合物。3g of peach gum, 1g of Centella asiatica, 0.1g of Psyllium Liquid weight, compound 24% glycerin, 9% trehalose, 9% hydroxypropyl-β-cyclodextrin, 1% hexanediol, 2% pentanediol, 0.2% disodium EDTA, 0.05% xanthan gum , sterilized at 90° C. for 40 min, to obtain the anti-irritant composition of Comparative Example 9.
试验例1拮抗酸性物质刺激Test Example 1 Antagonizing the stimulation of acidic substances
拮抗乳酸刺激效果评价Evaluation of the effect of antagonizing lactate stimulation
乳酸刺激试验Lactic acid stimulation test
测试样品：实施例1-6，对比例1-9；Test samples: Examples 1-6, Comparative Examples 1-9;
以10％乳酸为刺激源，筛选8名(18-55岁，男女不限，符合志愿者标准)对乳酸刺激敏感的志愿者进行试验。在志愿者两测鼻唇沟部位分别贴敷含10％乳酸(刺激组)、3％测试样品+10％乳酸(样品组)，涂抹后0.5min、2.5min、5min、7.5min、10min时对刺痛、瘙痒感觉进行打分，分数为0-3分，0分代表无刺痛、瘙痒，1分代表轻度刺痛、瘙痒，2分代表中度刺痛、瘙痒，3份代表强刺痛、瘙痒。分数差值＝刺激组刺激分数平均值-样品组刺激分数平均值。分数差值越大，说明对乳酸刺激的拮抗效果越好。Using 10% lactic acid as the stimulus source, 8 volunteers (aged 18-55, male or female, meeting the volunteer standards) who were sensitive to lactic acid stimulation were screened for the test. 10% lactic acid (stimulation group), 3% test sample + 10% lactic acid (sample group) were applied to the two nasolabial folds of the volunteers, respectively. The tingling and itching sensations were scored on a scale of 0-3, with 0 representing no tingling and itching, 1 representing mild tingling and itching, 2 representing moderate tingling and itching, and 3 representing strong tingling , itching. Score difference = mean stimulation score of stimulation group - mean stimulation score of sample group. The larger the score difference, the better the antagonistic effect on lactate stimulation.
表2实施例1乳酸刺激分数汇总表Table 2 embodiment 1 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000001
Figure PCTCN2022081921-appb-000001
表3实施例2乳酸刺激分数汇总表Table 3 embodiment 2 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000002
Figure PCTCN2022081921-appb-000002
表4实施例3乳酸刺激分数汇总表Table 4 embodiment 3 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000003
Figure PCTCN2022081921-appb-000003
表5实施例4乳酸刺激分数汇总表Table 5 embodiment 4 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000004
Figure PCTCN2022081921-appb-000004
表6实施例5乳酸刺激分数汇总表Table 6 embodiment 5 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000005
Figure PCTCN2022081921-appb-000005
表7实施例6乳酸刺激分数汇总表Table 7 embodiment 6 lactic acid stimulation score summary table
Figure PCTCN2022081921-appb-000006
Figure PCTCN2022081921-appb-000006
表8对比例1乳酸刺激分数汇总表Table 8 Comparative Example 1 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000007
Figure PCTCN2022081921-appb-000007
表9对比例2乳酸刺激分数汇总表Table 9 Comparative Example 2 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000008
Figure PCTCN2022081921-appb-000008
表10对比例3乳酸刺激分数汇总表Table 10 Comparative Example 3 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000009
Figure PCTCN2022081921-appb-000009
表11对比例4乳酸刺激分数汇总表Table 11 Comparative Example 4 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000010
Figure PCTCN2022081921-appb-000010
表12对比例5乳酸刺激分数汇总表Table 12 Comparative Example 5 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000011
Figure PCTCN2022081921-appb-000011
表13对比例6乳酸刺激分数汇总表Table 13 Comparative Example 6 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000012
Figure PCTCN2022081921-appb-000012
表14对比例7乳酸刺激分数汇总表Table 14 Comparative Example 7 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000013
Figure PCTCN2022081921-appb-000013
表15对比例8乳酸刺激分数汇总表Table 15 Comparative Example 8 Summary of Lactate Stimulation Scores
Figure PCTCN2022081921-appb-000014
Figure PCTCN2022081921-appb-000014
表16对比例9乳酸刺激分数汇总表Table 16 Comparative Example 9 Lactic Acid Stimulation Score Summary Table
Figure PCTCN2022081921-appb-000015
Figure PCTCN2022081921-appb-000015
表17乳酸刺激分数差值汇总表Table 17 Summary of differences in lactate stimulation scores
Figure PCTCN2022081921-appb-000016
Figure PCTCN2022081921-appb-000016
由表17可知，与对比例相比，实施例1-6乳酸刺痛分数差值、瘙痒分数差值均高于对比例1-9，说明本发明抗刺激组合物具有更好的拮抗乳酸刺激的功效；与对比例1-2、对比例5-9相比，实施例1-6乳酸刺痛分数差值、瘙痒分数差值均较高，其对乳酸引起的皮肤刺痛和瘙痒的具有更好的抑制效果，效果好于各组分单独使用，表现出明显的协同增效作用，由此说明通过桃胶、仙人掌、积雪草、车前子四种组分的协同作用，本发明抗刺激组合物具有更好的拮抗乳酸刺激的功效；与对比例3-4相比，实施例1-6乳酸刺痛分数差值、瘙痒分数差值均较高，说明本发明将桃胶、仙人掌、积雪草、车前子组合在一定比例下产生了明显的增效协同作用，其效果优于部分组分的组合，具有更好的拮抗乳酸刺激的功效。As can be seen from Table 17, compared with the comparative example, the difference of the lactic acid stinging score and the difference of the itching score of Examples 1-6 are higher than those of Comparative Examples 1-9, indicating that the anti-irritant composition of the present invention has better antagonistic lactic acid stimulation. Compared with Comparative Example 1-2 and Comparative Example 5-9, Example 1-6 lactic acid stinging score difference and pruritus score difference are all higher, and it has a significant effect on skin stinging and itching caused by lactic acid. Better inhibitory effect, the effect is better than that of each component used alone, showing obvious synergistic effect, which shows that through the synergistic effect of the four components of peach gum, cactus, Centella asiatica and psyllium, the present invention The anti-irritant composition has a better effect of antagonizing lactic acid stimulation; compared with Comparative Examples 3-4, the difference between the lactic acid stinging score and the pruritus score difference in Examples 1-6 are higher, indicating that the present invention combines peach gum, The combination of Cactus, Centella asiatica and Psyllium chinensis produced an obvious synergistic effect in a certain proportion, and its effect was better than the combination of some components, and it had a better effect of antagonizing lactic acid stimulation.
试验例2拮抗表面活性剂刺激Test Example 2 Antagonizing Surfactant Stimulation
拮抗SDS引起的红细胞溶血抑制率效果评价Evaluation of the effect of antagonizing the inhibition rate of erythrocyte hemolysis induced by SDS
采用红细胞溶血凝血试验，考察实施例1-6和对比例1-9对SDS引起的红细胞溶血抑制率的拮抗效果。The erythrocyte hemolysis coagulation test was used to investigate the antagonistic effects of Examples 1-6 and Comparative Examples 1-9 on the inhibition rate of erythrocyte hemolysis caused by SDS.
红细胞溶血凝血试验red blood cell hemolysis coagulation test
①红细胞悬液处理：① Treatment of red blood cell suspension:
室温下，调整红细胞悬液中红细胞密度，在530nm波长下测定其吸光值，控制全溶血时红细胞OD值在1.3000-1.7000。At room temperature, adjust the density of erythrocytes in the erythrocyte suspension, measure the absorbance value at a wavelength of 530 nm, and control the OD value of erythrocytes at 1.3000-1.7000 during complete hemolysis.
②红细胞耐受性② red blood cell tolerance
分别用体系浓度为20mg/L、30mg/L、40mg/L的SDS水溶液作为样品，检测红细胞溶血抑制率，并计算H50(溶血率为50％时，SDS的体系浓度)。要求H50在25.7-33.1mg/L范围内。SDS aqueous solutions with system concentrations of 20 mg/L, 30 mg/L and 40 mg/L were used as samples to detect the inhibition rate of erythrocyte hemolysis and calculate H50 (the system concentration of SDS when the hemolysis rate is 50%). The H50 is required to be in the range of 25.7-33.1mg/L.
③检测受试物③Detect the test substance
A.取离心管，按照表4所示，依次加入受试样品(实施例1-6和对比例1-9)、PBS(磷酸盐缓冲溶液)、RBC悬液(红细胞悬液)、SDS(十二烷基硫酸钠)，并混合均匀，样品体系终浓度即为测试浓度；A. Take the centrifuge tube and add the test samples (Examples 1-6 and Comparative Examples 1-9), PBS (phosphate buffered solution), RBC suspension (erythrocyte suspension), SDS in turn as shown in Table 4 (sodium dodecyl sulfate), and mix well, the final concentration of the sample system is the test concentration;
B.置于摇床，孵育10min后离心；B. Place on a shaker, incubate for 10min and then centrifuge;
C.观察现象，并取上清液，测定OD530；C. observe the phenomenon, and take the supernatant to measure OD530;
D.计算溶血抑制率。D. Calculate hemolysis inhibition rate.
表18反应体系(μL)Table 18 Reaction system (μL)
添加试剂Add reagents 受试样品/μLTest sample/μL PBS/μLPBS/μL RBC悬液/μLRBC suspension/μL 0.14％SDS0.14% SDS
样品组+SDSSample set + SDS 200200 9090 100100 1010
阴性对照组(SDS)Negative control group (SDS) 00 290290 100100 1010
溶剂对照组solvent control 00 300300 100100 00
红细胞溶血抑制率的计算公式为：The formula for calculating the inhibition rate of erythrocyte hemolysis is:
红细胞溶血抑制率(％)＝(OD_阴性对照组-OD_样品组)/OD_阴性对照组×100。Erythrocyte hemolysis inhibition rate (%)=(OD_negative control group-OD_sample group)/OD_negative control group×100.
红细胞溶血抑制率越高，说明样品对SDS引起的红细胞溶血的拮抗效果越好。The higher the inhibition rate of erythrocyte hemolysis, the better the antagonistic effect of the sample on erythrocyte hemolysis caused by SDS.
表19红细胞溶血抑制率汇总表Table 19 Summary table of red blood cell hemolysis inhibition rate
样品名称sample name 红细胞溶血抑制率(％)Inhibition rate of red blood cell hemolysis (%)
0.0035％SDS+0.5％实施例10.0035% SDS+0.5% Example 1 8383
0.0035％SDS+0.5％实施例20.0035% SDS+0.5% Example 2 7878
0.0035％SDS+0.5％实施例30.0035% SDS+0.5% Example 3 7979
0.0035％SDS+0.5％实施例40.0035% SDS+0.5% Example 4 8585
0.0035％SDS+0.5％实施例50.0035% SDS+0.5% Example 5 8282
0.0035％SDS+0.5％实施例60.0035% SDS+0.5% Example 6 7575
0.0035％SDS+0.5％对比例10.0035% SDS+0.5% Comparative Example 1 4343
0.0035％SDS+0.5％对比例20.0035% SDS+0.5% Comparative Example 2 22twenty two
0.0035％SDS+0.5％对比例30.0035% SDS+0.5% Comparative Example 3 23twenty three
0.0035％SDS+0.5％对比例40.0035% SDS+0.5% Comparative Example 4 21twenty one
0.0035％SDS+0.5％对比例50.0035% SDS+0.5% Comparative Example 5 2525
0.0035％SDS+0.5％对比例60.0035% SDS+0.5% Comparative Example 6 3131
0.0035％SDS+0.5％对比例70.0035% SDS+0.5% Comparative Example 7 3535
0.0035％SDS+0.5％对比例80.0035% SDS+0.5% Comparative Example 8 3131
0.0035％SDS+0.5％对比例90.0035% SDS+0.5% Comparative Example 9 2929
由表19可知，本发明实施例1-6抗刺激组合物对SDS引起的红细胞溶血抑制率均高于对比例1、对比例6-7和对比例8-9得到的抗刺激组合物以及对比例2、对比例5得到的单一提取物对SDS引起的红细胞溶血抑制率，这说明本发明所述的抗刺激组合物具有比任何单一提取物以及任意其中两种或三种原料组合制备的抗刺激组合物都能更好的拮抗SDS引起的红细胞溶血抑制率，这表明本发明将桃胶、仙人掌、积雪草、车前子组合产生了明显的增效协同作用；实施例1-6抗刺激组合物对SDS引起的红细胞溶血抑制率达到75％以上，而对比例3-4对SDS引起的红细胞溶血抑制率较低，本发明通过合理复配各组分，产生协同增效作用，使不同组分产生互相促进的作用，对SDS引起的红细胞溶血的拮抗效果更好。It can be seen from Table 19 that the anti-irritant compositions of the present invention 1-6 have higher inhibition rates of erythrocyte hemolysis caused by SDS than the anti-irritant compositions obtained in Comparative Example 1, Comparative Examples 6-7, and Comparative Examples 8-9 and The inhibition rate of erythrocyte hemolysis caused by SDS by the single extract obtained in Example 2 and Comparative Example 5 shows that the anti-irritant composition of the present invention has more anti-inflammatory properties than any single extract and any combination of two or three raw materials. The stimulating composition can better antagonize the inhibition rate of erythrocyte hemolysis caused by SDS, which shows that the combination of peach gum, cactus, Centella asiatica and psyllium in the present invention has produced obvious synergistic effect; The inhibitory rate of the stimulatory composition to erythrocyte hemolysis caused by SDS reaches more than 75%, while the inhibition rate of the erythrocyte hemolysis caused by SDS to the comparative examples 3-4 is lower. Different components have a mutually promoting effect, and have a better antagonistic effect on erythrocyte hemolysis caused by SDS.
试验例3拮抗表面活性剂刺激Test Example 3 Antagonism to Surfactant Stimulation
鸡胚绒毛尿囊膜试验Chicken embryo chorioallantoic membrane test
①鸡蛋选择：选用SPF级白莱杭鸡受精鸡蛋(北京梅利亚试验动物有限公司购买)。鸡蛋质量符合相关标准的要求，供应商应具有农业部门认可的《兽药生产、检验用SPF鸡(蛋)定点生产企业》资格。鸡蛋应新鲜、干净、完好，质量50g-60g。孵化至4日龄时，应照蛋检查，弃去未受精的鸡胚，破壳或薄壳鸡胚也不能使用。①Egg selection: select SPF-grade Bailaihang chicken fertilized eggs (purchased by Beijing Melia Experimental Animal Co., Ltd.). The quality of eggs meets the requirements of relevant standards, and the supplier should have the qualification of "Designated Production Enterprise of SPF Chicken (Egg) for Veterinary Drug Production and Inspection" recognized by the agricultural department. Eggs should be fresh, clean and intact, with a mass of 50g-60g. When hatching to 4 days of age, the eggs should be checked, and the unfertilized chicken embryos should be discarded, and the broken or thin-shelled chicken embryos should not be used.
②孵化条件：孵化温度37.5±0.5℃，相对湿度55-70％，转盘频率3-6次/h，翻蛋孵化3天，第4天开窗后，停止翻蛋。②Incubation conditions: Incubation temperature 37.5±0.5℃, relative humidity 55-70%, turntable frequency 3-6 times/h, turn the eggs for 3 days, and stop turning the eggs after opening the window on the 4th day.
③CAM制备：在鸡胚孵化4天时，用电磨机在鸡蛋小头端打孔，用10mL注射器抽取2-3mL蛋清，再用电磨机在鸡蛋中部略微靠近大头段开一个1cm×1cm小窗，暴露CAM，小心用镊子去除蛋壳和蛋壳膜，保证鸡胚尿囊膜不受损。此时应观察血管系统的结构和鸡胚的生长情况。用透明胶带封住小头端的孔和中部的小窗后，放入孵化箱继续培养。每天需检查鸡胚的生长情况，及时弃去死胚。10日龄鸡胚用于试验。撕去封住小窗的透明胶带，用镊子扩大小窗面积，增大观察视野，应小心操作不破坏蛋膜完整性。此时应再次观察血管系统的结构，并对其完整性和是否适宜用于试验做出判断。将特氟龙环放在CAM上准备添加样品。③CAM preparation: When the chicken embryo hatched for 4 days, use an electric grinder to make holes in the small end of the egg, use a 10mL syringe to extract 2-3mL of egg white, and then use an electric grinder to open a 1cm×1cm window in the middle of the egg slightly near the big end. , expose the CAM, and carefully remove the eggshell and eggshell membrane with tweezers to ensure that the embryonic allantoic membrane is not damaged. At this time, the structure of the vascular system and the growth of the chicken embryo should be observed. After sealing the hole at the small end and the small window in the middle with scotch tape, put it into the incubator to continue culturing. The growth of chicken embryos should be checked every day, and dead embryos should be discarded in time. 10-day-old chicken embryos were used for the experiments. Tear off the scotch tape sealing the small window, and use tweezers to expand the area of the small window and increase the observation field. Care should be taken not to damage the integrity of the egg membrane. At this point, the structure of the vasculature should be revisited and a judgment made about its integrity and suitability for testing. Place the Teflon ring on the CAM in preparation for sample addition.
④样品测试：每个受试物为一组，每组试验6只鸡胚，取40μl的受试物直接作用于特氟龙环内CAM表面。37℃作用30min后，观察绒毛尿囊膜毒性效应指标(如：出血、血管溶解和凝血等)的变化，并进行组合计算终点评分(ES)。受试物处理组终点评分与阴性对照的终点评分进行比较，样品的终点评分越低，提示供试品抗刺激效果越强。④Sample test: Each test substance is a group, 6 chicken embryos are tested in each group, and 40 μl of the test substance is directly applied to the surface of the CAM in the Teflon ring. After 30min exposure at 37℃, the changes of chorioallantoic membrane toxicity index (such as: bleeding, vasolysis and coagulation, etc.) were observed, and combined to calculate the endpoint score (ES). The end point score of the test substance treatment group is compared with that of the negative control, and the lower the end point score of the sample, the stronger the anti-stimulation effect of the test substance is.
受试样品：实施例1-6和对比例1-9制备的抗刺激组合物。Test samples: anti-irritant compositions prepared in Examples 1-6 and Comparative Examples 1-9.
表20鸡胚绒毛尿囊膜刺激分数汇总表Table 20 Summary table of chicken embryo chorioallantoic membrane stimulation scores
样品名称sample name 鸡胚绒毛尿囊膜刺激分数(ES)Chicken embryo chorioallantoic membrane stimulation score (ES) 刺激等级stimulus level
0.1％SDS+5％实施例10.1% SDS+5% Example 1 88 轻度刺激mild stimulation
0.1％SDS+5％实施例20.1% SDS + 5% Example 2 99 轻度刺激mild stimulation
0.1％SDS+5％实施例30.1% SDS + 5% Example 3 66 轻度刺激mild stimulation
0.1％SDS+5％实施例40.1% SDS + 5% Example 4 77 轻度刺激mild stimulation
0.1％SDS+5％实施例50.1% SDS + 5% Example 5 44 轻度刺激mild stimulation
0.1％SDS+5％实施例60.1% SDS + 5% Example 6 66 轻度刺激mild stimulation
0.1％SDS+5％对比例10.1% SDS+5% Comparative Example 1 1212 中度刺激Moderate stimulation
0.1％SDS+5％对比例20.1% SDS+5% Comparative Example 2 1313 中度刺激Moderate stimulation
0.1％SDS+5％对比例30.1% SDS+5% Comparative Example 3 1414 中度刺激Moderate stimulation
0.1％SDS+5％对比例40.1% SDS+5% Comparative Example 4 1414 中度刺激Moderate stimulation
0.1％SDS+5％对比例50.1% SDS+5% Comparative Example 5 1414 中度刺激Moderate stimulation
0.1％SDS+5％对比例60.1% SDS+5% Comparative Example 6 1414 中度刺激Moderate stimulation
0.1％SDS+5％对比例70.1% SDS+5% Comparative Example 7 1313 中度刺激Moderate stimulation
0.1％SDS+5％对比例80.1% SDS+5% Comparative Example 8 1313 中度刺激Moderate stimulation
0.1％SDS+5％对比例90.1% SDS+5% Comparative Example 9 1414 中度刺激Moderate stimulation
0.1％SDS0.1% SDS 1515 中度刺激Moderate stimulation
生理盐水normal saline 00 无刺激No stimulation
由表19可知，0.1％SDS+5％本发明实施例1-6抗刺激组合物对SDS引起的鸡胚绒毛尿囊膜刺激分数(ES)均小于10，而0.1％SDS+5％本发明实施例1-6抗刺激组合物对SDS引起的鸡胚绒毛尿囊膜刺激分数(ES)均大于12。本发明实施例1-6抗刺激组合物对SDS引起的鸡胚绒毛尿囊膜刺激分数均低于比例2、对比例5得到的单一提取物以及对比例1、对比例6-7和对比例8-9得到的抗刺激组合物对SDS引起的鸡胚绒毛尿囊膜刺激分数，这说明本发明所述的抗刺激组合物比任何单一提取物以及任意其中两种或三种原料组合制备的抗刺激组合物能够更好的降低SDS引起的鸡胚绒毛尿囊膜刺激，这表明本发明组分组合复配使用时，通过协同作用拮抗SDS刺激的效果；与对比例3-4相比，本发明抗刺激组合物对SDS引起的鸡胚绒毛尿囊膜刺激的拮抗效果更优，通过合理复配各组分，产生协同增效作用，增加了本发明抗刺激组合物拮抗SDS刺激的功效。It can be seen from Table 19 that the 0.1% SDS+5% anti-irritant compositions of Examples 1-6 of the present invention can stimulate the chicken embryo chorioallantoic membrane (ES) by SDS less than 10, while 0.1% SDS+5% of the present invention The irritation scores (ES) of the chicken embryo chorioallantoic membrane caused by the anti-irritant compositions of Examples 1-6 were all greater than 12. The fraction of the chicken embryo chorioallantoic membrane stimulation by the anti-irritant compositions of Examples 1-6 of the present invention caused by SDS is lower than that of the single extract obtained in Example 2, Comparative Example 5, and Comparative Examples 1, 6-7 and Comparative Examples 8-9 The obtained anti-irritant composition can stimulate the chicken embryo chorioallantoic membrane fraction caused by SDS. The anti-irritant composition can better reduce the stimulation of the chick embryo chorioallantoic membrane caused by SDS, which shows that when the composition of the present invention is used in combination, it can antagonize the effect of SDS stimulation through a synergistic effect; compared with Comparative Examples 3-4, The anti-irritant composition of the present invention has better antagonistic effect on the stimulation of the chick embryo chorioallantoic membrane caused by SDS, and by rationally compounding the components, a synergistic effect is produced, and the efficacy of the anti-irritant composition of the present invention to antagonize the stimulation of SDS is increased. .
试验例4拮抗防腐剂刺激Test Example 4 Antagonism of Preservative Stimulation
苯氧乙醇刺激试验Phenoxyethanol stimulation test
苯氧乙醇作为目前化妆品最常用的防腐剂，可作为防腐剂刺激源代表验证抗刺激组合物的功效。以1％苯氧乙醇为刺激源，筛选5名(18-55岁，男女不限，符合志愿者标准)对苯氧乙醇刺激敏感的志愿者进行试验。在志愿者两测鼻唇沟部位分别贴敷含1％苯氧乙醇(刺激组)、3％测试样品+1％苯氧乙醇(样品组)，涂抹后0.5min、2.5min、5min、7.5min、10min时对刺痛、灼热感觉进行打分，分数为0-3分，0分代表无刺痛、灼热，1分代表轻度刺痛、灼热，2分代表中度刺痛、灼热，3份代表强刺痛、灼热。分数差值＝刺激组刺激分数平均值-样品组刺激分数平均值。分数差值越大，说明对苯氧乙醇刺激的拮抗效果越好。As the most commonly used preservative in cosmetics, phenoxyethanol can be used as a preservative irritant representative to verify the efficacy of anti-irritant compositions. With 1% phenoxyethanol as the stimulus source, 5 volunteers (aged 18-55, male or female, meeting volunteer standards) who were sensitive to phenoxyethanol stimulation were screened for the test. 1% phenoxyethanol (stimulation group), 3% test sample + 1% phenoxyethanol (sample group) were applied to the two nasolabial folds of the volunteers respectively, 0.5min, 2.5min, 5min, 7.5min after application The stinging and burning sensations were scored at 10 minutes on a scale of 0-3, with 0 representing no stinging and burning, 1 indicating mild stinging and burning, 2 indicating moderate stinging and burning, and 3 points. On behalf of strong stinging, burning. Score difference = mean stimulation score of stimulation group - mean stimulation score of sample group. The larger the score difference, the better the antagonistic effect of phenoxyethanol stimulation.
表21苯氧乙醇刺激分数差值汇总表Table 21 Summary table of differences in phenoxyethanol stimulation scores
Figure PCTCN2022081921-appb-000017
Figure PCTCN2022081921-appb-000017
由表21可知，与对比例相比，实施例1-6苯氧乙醇灼热分数差值、刺痛分数差值均高于对比例1-9，说明本发明抗刺激组合物具有更好的拮抗苯氧乙醇刺激的功效；与对比例1-2、对比例5-9相比，实施例1-6苯的氧乙醇刺痛分数差值、灼热分数差值均较高，其对苯氧乙醇引起的皮肤刺痛和灼热的具有更好的抑制效果，效果好于各组分单独使用，效果也优于部分组分的组合，表现出明显的协同增效作用，由此说明通过桃胶、仙人掌、积雪草、车前子四种组分的协同作用，本发明抗刺激组合物具有更好的拮抗苯氧乙醇刺激的功效；与对比例3-4相比，实施例1-6苯氧乙醇刺痛分数差值、灼热分数差值均较高，说明本发明将桃胶、仙人掌、积雪草、车前子组合在一定比例下产生了明显的增效协同作用，具有更好的拮抗苯氧乙醇刺激的功效。As can be seen from Table 21, compared with the comparative example, the difference between the phenoxyethanol burning score and the stinging score difference in Examples 1-6 are all higher than those in Comparative Examples 1-9, indicating that the anti-irritant composition of the present invention has better antagonism. The effect of phenoxyethanol stimulation; Compared with Comparative Example 1-2 and Comparative Example 5-9, the oxyethanol stinging score difference and the burning score difference of Example 1-6 benzene are all higher, and its phenoxyethanol The skin tingling and burning caused by the skin has better inhibitory effect, the effect is better than that of each component used alone, and the effect is also better than the combination of some components, showing obvious synergistic effect, which shows that through peach gum, The synergistic effect of the four components of cactus, centella asiatica and psyllium, the anti-irritant composition of the present invention has a better effect of antagonizing the stimulation of phenoxyethanol; The difference between the stinging score and the burning score of oxyethanol is relatively high, indicating that the combination of peach gum, cactus, Centella asiatica and psyllium in a certain proportion of the present invention has produced obvious synergistic effect, and has better synergistic effect. Antagonistic efficacy of phenoxyethanol stimulation.
试验例5拮抗香辛香料刺激Test Example 5 Antagonizing the stimulation of spices
丁子香酚刺激试验Eugenol stimulation test
以0.5％丁子香酚为刺激源，筛选5名(18-55岁，男女不限，符合志愿者标准)对丁子 香酚刺激敏感的志愿者进行试验。在志愿者两测鼻唇沟部位分别贴敷含0.5％丁子香酚(刺激组)、3％测试样品+0.5％丁子香酚(样品组)，涂抹后0.5min、2.5min、5min、7.5min、10min时对刺痛感觉进行打分，分数为0-3分，0分代表无刺痛，1分代表轻度刺痛，2分代表中度刺痛，3份代表强刺痛。分数差值＝刺激组刺激分数平均值-样品组刺激分数平均值。分数差值越大，说明对丁子香酚刺激的拮抗效果越好。With 0.5% eugenol as the stimulus source, 5 volunteers (18-55 years old, male or female, meeting volunteer standards) who are sensitive to eugenol stimulation were screened for the test. 0.5% eugenol (stimulation group), 3% test sample + 0.5% eugenol (sample group) were applied to the nasolabial folds of the volunteers for 0.5min, 2.5min, 5min, 7.5min after application. The tingling sensation was scored at 10 minutes on a scale of 0-3, with 0 representing no tingling, 1 representing mild tingling, 2 representing moderate tingling, and 3 representing strong tingling. Score difference = mean stimulation score of stimulation group - mean stimulation score of sample group. The larger the score difference, the better the antagonistic effect of eugenol stimulation.
表22样品丁子香酚刺激分数汇总表Table 22 Summary table of eugenol stimulation scores of samples
Figure PCTCN2022081921-appb-000018
Figure PCTCN2022081921-appb-000018
由表22可知，与对比例相比，实施例1-6丁子香酚刺痛分数差值高于对比例1-9，说明本发明抗刺激组合物具有更好的拮抗丁子香酚刺激的功效；与对比例1-2、对比例5-9相比，实施例1-6的丁子香酚刺痛分数差值较高，其对丁子香酚引起的皮肤刺痛具有更好的抑制效果，效果好于各组分单独使用，也优于部分组分的组合，表现出明显的协同增效作用，由此说明通过桃胶、仙人掌、积雪草、车前子四种组分的协同作用，本发明抗刺激组合物具有更好的拮抗丁子香酚刺激的功效；与对比例3-4相比，实施例1-6丁子香酚刺痛分数差值 较高，说明本发明将桃胶、仙人掌、积雪草、车前子组合在一定比例下产生了明显的增效协同作用，具有更好的拮抗丁子香酚刺激的功效。As can be seen from Table 22, compared with the comparative example, the difference in the stinging scores of eugenol in Examples 1-6 is higher than that in Comparative Examples 1-9, indicating that the anti-irritant composition of the present invention has a better effect of antagonizing eugenol stimulation Compared with Comparative Example 1-2 and Comparative Example 5-9, the eugenol stinging score difference of embodiment 1-6 is higher, and it has better inhibitory effect on the skin stinging caused by eugenol, The effect is better than that of each component used alone, and also better than the combination of some components, showing obvious synergistic effect, which shows that the synergistic effect of the four components of peach gum, cactus, Centella asiatica and psyllium , the anti-irritant composition of the present invention has a better effect of antagonizing the stimulation of eugenol; compared with the comparative examples 3-4, the difference between the stinging scores of eugenol in Examples 1-6 is higher, indicating that the present invention uses peach gum , Cactus, Centella asiatica, Psyllium combination in a certain proportion produced obvious synergy and synergy, and had better antagonizing effect of eugenol stimulation.
本发明抗刺激组合物通过将桃胶、仙人掌、积雪草、车前子，按特定比例组合，各组分之间相互作用，可有效预防、拮抗或修复化妆品中各种刺激源的功效，如酸性物质、表面活性剂、防腐剂、香辛香料等。将其应用于化妆品中，预计具有抗刺激功效，可拮抗化妆品中各种刺激源引起的皮肤刺激性。The anti-irritant composition of the present invention can effectively prevent, antagonize or restore the efficacy of various irritants in cosmetics by combining peach gum, cactus, Centella asiatica and psyllium in a specific ratio, and the components interact with each other. Such as acidic substances, surfactants, preservatives, spices, etc. When applied in cosmetics, it is expected to have anti-irritant effects, which can antagonize skin irritation caused by various irritants in cosmetics.
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。The above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, rather than limiting the embodiments of the present invention. For those of ordinary skill in the art, on the basis of the above descriptions, other Changes or changes in different forms cannot be exhaustively listed here, and all obvious changes or changes derived from the technical solutions of the present invention are still within the protection scope of the present invention.

Claims (10)

  1. 一种抗刺激组合物，其特征在于，所述抗刺激组合物包括以下重量份数的组分：桃胶1-30份、仙人掌0.1-10份、积雪草0.1-10份、车前子0.01-5份。An anti-irritant composition, characterized in that the anti-irritant composition comprises the following components by weight: 1-30 parts of peach gum, 0.1-10 parts of cactus, 0.1-10 parts of Centella asiatica, psyllium 0.01-5 servings.
  2. 根据权利要求1所述的抗刺激组合物，其特征在于，所述抗刺激组合物包括以下重量份数的组分：桃胶1-5份、仙人掌0.5-2份、积雪草0.5-2份、车前子0.1-1份。The anti-irritant composition according to claim 1, wherein the anti-irritant composition comprises the following components in parts by weight: 1-5 parts of peach gum, 0.5-2 parts of cactus, 0.5-2 parts of Centella asiatica portion, 0.1-1 portion of psyllium.
  3. 根据权利要求1或2所述的抗刺激组合物，其特征在于，所述抗刺激组合物还包括组分5)，所述组分5)选自糊精、环糊精、麦芽糊精、羟丙基-β-环糊精、β-环糊精、抗性糊精的一种或几种。The anti-irritant composition according to claim 1 or 2, characterized in that, the anti-irritant composition further comprises component 5), and the component 5) is selected from dextrin, cyclodextrin, maltodextrin, One or more of hydroxypropyl-β-cyclodextrin, β-cyclodextrin and resistant dextrin.
  4. 根据权利要求3所述的抗刺激组合物，其特征在于，所述植物组合物通过包括以下步骤的制备方法制备：The anti-irritant composition according to claim 3, wherein the plant composition is prepared by a preparation method comprising the following steps:
    (1)将桃胶、仙人掌、积雪草和车前子提取，过滤，浓缩，得初提液；(1) extracting peach gum, cactus, Centella asiatica and psyllium, filtering, concentrating to obtain primary extract;
    (2)将初提液复配组分5)、甘油、海藻糖和化妆品常规辅料；(2) compound component 5), glycerol, trehalose and cosmetic conventional auxiliary materials with the primary extract;
    (3)灭菌，得抗刺激组合物。(3) Sterilization to obtain an anti-irritant composition.
  5. 根据权利要求4所述的抗刺激组合物，其特征在于，所述制备方法步骤(1)中桃胶、仙人掌、积雪草和车前子总重量与水的重量比为1:10-1:80(m/m)。The anti-irritant composition according to claim 4, wherein in the preparation method step (1), the weight ratio of the total weight of peach gum, cactus, Centella asiatica and psyllium to water is 1:10-1 : 80(m/m).
  6. 根据权利要求4所述的抗刺激组合物，其特征在于，所述制备方法步骤(1)中提取温度为50-100℃，提取时间0.5-5h；所述制备方法步骤(1)中提取液浓缩1-5倍。The anti-irritant composition according to claim 4, characterized in that, in step (1) of the preparation method, the extraction temperature is 50-100° C., and the extraction time is 0.5-5h; the extraction solution in step (1) of the preparation method is Concentrate 1-5 times.
  7. 根据权利要求4所述的抗刺激组合物，其特征在于，所述制备方法步骤(2)中以总料液重量计，组分5)添加量为1-30％，甘油添加量为10-50％，海藻糖添加量为1-30％。The anti-irritant composition according to claim 4, characterized in that, in the preparation method step (2), based on the weight of the total feed liquid, the addition amount of component 5) is 1-30%, and the addition amount of glycerin is 10-30% 50%, trehalose addition is 1-30%.
  8. 根据权利要求4所述的抗刺激组合物，其特征在于，所述制备方法步骤(2)中化妆品常规辅料包括防腐剂、螯合剂、增稠剂；The anti-irritant composition according to claim 4, characterized in that, in step (2) of the preparation method, conventional cosmetic adjuvants include preservatives, chelating agents, and thickening agents;
    所述防腐剂为己二醇、戊二醇，和/或所述螯合剂为EDTA二钠，和/或所述增稠剂为黄原胶；The preservative is hexylene glycol, pentanediol, and/or the chelating agent is disodium EDTA, and/or the thickening agent is xanthan gum;
    以总料液重量计，所述制备方法步骤(2)中，己二醇添加量为0.1-5％、戊二醇添加量为0.1-5％、EDTA二钠添加量为0.01-5％、黄原胶添加量为0.01-1％。Based on the weight of the total feed liquid, in step (2) of the preparation method, the addition amount of hexanediol is 0.1-5%, the addition amount of pentanediol is 0.1-5%, the addition amount of disodium EDTA is 0.01-5%, The amount of xanthan gum added is 0.01-1%.
  9. 一种抗刺激组合物的制备方法，其特征在于，所述制备方法包括以下步骤：A preparation method of an anti-irritant composition, characterized in that the preparation method comprises the following steps:
    (1)桃胶1-30份、仙人掌0.1-10份、积雪草0.1-10份、车前子0.01-5份，按照总原料：水＝1:10-1:80(m/m)，在提取温度50-100℃条件下提取0.5-5h，过滤，浓缩1-5倍，得初提液；(1) 1-30 parts of peach gum, 0.1-10 parts of cactus, 0.1-10 parts of Centella asiatica, 0.01-5 parts of plantain seeds, according to the total raw materials: water = 1:10-1:80 (m/m) , extract 0.5-5h under the condition of extraction temperature 50-100℃, filter, concentrate 1-5 times to obtain primary extract;
    (2)初提液复配1-30％组分5)(按照总料液重量计，下同)，10-50％甘油，1-30％海藻糖，1-30％组分5)，0.1-5％己二醇，0.1-5％戊二醇，0.01-5％EDTA二钠，0.01-1％黄原胶；(2) The initial extract is compounded with 1-30% component 5) (according to the weight of the total feed liquid, the same below), 10-50% glycerol, 1-30% trehalose, 1-30% component 5), 0.1-5% hexanediol, 0.1-5% pentanediol, 0.01-5% disodium EDTA, 0.01-1% xanthan gum;
    (3)灭菌，得抗刺激组合物；(3) sterilization to obtain anti-irritant composition;
    所述组分5)选自糊精、环糊精、麦芽糊精、羟丙基-β-环糊精、β-环糊精、抗性糊精的一种或几种。The component 5) is selected from one or more of dextrin, cyclodextrin, maltodextrin, hydroxypropyl-β-cyclodextrin, β-cyclodextrin and resistant dextrin.
  10. 权利要求1-8任意一项所述抗刺激组合物或权利要求9所述制备方法制备得到的抗刺激组合物在制备用于抗刺激、拮抗化妆品中刺激源的护肤品和/或化妆品中的应用。The anti-irritant composition of any one of claims 1-8 or the anti-irritant composition prepared by the preparation method of claim 9 is used in the preparation of skin care products and/or cosmetics for anti-irritation and antagonism of irritants in cosmetics. application.
PCT/CN2022/081921 2021-03-26 2022-03-21 Anti-irritation composition, preparation method therefor and application thereof WO2022199507A1 (en)

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