CN113350241B - Application of Terminalia catappa leaf extract, and allergy-relieving composition and application thereof - Google Patents

Application of Terminalia catappa leaf extract, and allergy-relieving composition and application thereof Download PDF

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CN113350241B
CN113350241B CN202110735904.9A CN202110735904A CN113350241B CN 113350241 B CN113350241 B CN 113350241B CN 202110735904 A CN202110735904 A CN 202110735904A CN 113350241 B CN113350241 B CN 113350241B
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terminalia catappa
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CN113350241A (en
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黄晓园
杨登亮
周雨叶
邓慧
李传茂
张伟杰
曾伟丹
张楚标
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Guangdong Danz Group Co Ltd
Guangzhou Keneng Cosmetic Research Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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Abstract

The application belongs to the field of daily chemicals, and particularly provides application of an Terminalia catappa leaf extract, a soothing and sensitizing composition and application thereof. The allergy-relieving composition for inhibiting the production of allergic dermatitis, which is provided by the application, consists of an extract containing Terminalia catappa leaves and an extract containing Morinda citrifolia leaves, and the mass ratio of the extracts is 1. The soothing and sensitizing composition disclosed by the application has a synergistic effect by matching the Terminalia catappa leaf extract and the Morinda citrifolia leaf extract, and can well inhibit allergic dermatitis. The skin care product can be applied to allergy-relieving skin care products, can inhibit mast cells from degranulation, has allergy-relieving effect, relieves pruritus and pain discomfort caused by dermatitis, can increase the moisture content of stratum corneum, and can prevent the moisture loss of deep layers of skin.

Description

Application of Terminalia catappa leaf extract, and allergy-relieving composition and application thereof
Technical Field
The invention relates to the field of daily chemicals, and particularly relates to an application of an Terminalia catappa leaf extract, a soothing and sensitizing composition and an application of the soothing and sensitizing composition.
Background
Allergic dermatitis is an allergic reaction caused by immune system disorder due to contact with an allergen, and is usually accompanied by skin barrier damage, often accompanied by allergen drugs, foods, dusts, cosmetics, microorganisms, and the like. The allergic reaction is caused by local or systemic reaction caused by the release of active mediators from mast cells and basophils mediated by antibody IgE generated by contacting with allergen, most of the allergic reaction is manifested by red, swollen, hot, painful, itching, blister and the like of the skin, and the allergic reaction brings facial anxiety to daily life of people.
The major routes of anti-allergy and skin care include the following, with respect to the route and influencing factors of skin allergy: the medicine composition is prepared from (1) histamine competing for H1 receptors on corresponding target cells, inhibiting telangiectasia caused by histamine, and increasing vascular permeability, (2) a mast cell stabilizer, stabilizing mast cell membranes, inhibiting mast cell lysis and degranulation, and preventing release of allergic mediators, (3) a calcium agent, increasing the compactness of capillary vessels, and reducing cellular permeability, thereby reducing exudation of inflammatory factors, and relieving or alleviating allergic symptoms, and (4) an immunosuppressant, and can inhibit proliferation and functions of cells (macrophages such as T cells and B cells and the like) related to immune reaction, and reduce antibody immune reaction.
In order to reduce uncomfortable feeling caused by allergic dermatitis, the components with the functions of relieving and resisting allergy in the skin care product mainly comprise the active spring water and various natural plant extracts. The skin care products on the market at present achieve the effect of relieving through inhibiting inflammatory factors generated by allergy, and active ingredients in the Terminalia catappa leaf extract can effectively inhibit mast cells from degranulating so as to achieve the effect of relieving dermatitis.
Disclosure of Invention
The invention aims to provide application of an extract of Terminalia catappa leaves in preparing a soothing and sensitizing skin care product.
The invention provides a allergy-relieving composition which can effectively relieve allergic dermatitis.
The soothing and sensitizing composition comprises an extract of Terminalia catappa leaves and other Chinese herbal medicine compound extracts; preferably, the Chinese herbal medicine compound extract is an extract of morinda citrifolia leaves.
In one aspect, the present application provides the use of an extract of terminalia catappa leaves for the preparation of a skin care product for inhibiting mast cell degranulation.
In one aspect, the present application provides a soothing composition for inhibiting the formation of allergic dermatitis, consisting of terminalia catappa leaf extract and morinda citrifolia leaf extract,
wherein the mass ratio of the Terminalia catappa leaf extract to the Morinda citrifolia leaf extract is 1.
In some embodiments, the weight ratio of the terminalia catappa leaf extract to the morinda citrifolia leaf extract may be: 1, 0.01-3; more preferably, from 1; more preferably 1.3 to 1.5.
The Terminalia catappa is native to peninsula malaysia, southeast Asia and Andaman Islands, is also cultivated in the south of China, is a perennial tree species, belongs to evergreen arbor, can be as high as 20 meters, is widely introduced into coastal habitats and coastal forests, and is used as an ornamental plant, a shading tree and a dune stabilizer. All parts of the Terminalia catappa can be used for medicine, wherein the leaves contain abundant flavonoids, can be used for treating diseases such as hepatitis, acute liver injury, rheumatoid disease and the like, also has antibacterial and antiviral effects, and can be prepared into tea for relieving, relaxing and tightening nerves.
The inventor of the present invention found that the terminalia catappa leaf extract has an excellent inhibitory effect on mast cell degranulation, and the inhibitory rate gradually increases with the increase of the mass concentration of the terminalia catappa leaf extract.
Morinda citrifolia (Morinda citrifolia) is a perennial plant native to southeast Asia and has traditionally been used as a food and pharmaceutical. The Morinda citrifolia leaf extract contains a large amount of active substances, has the effects of resisting inflammation, allergy, bacteria and the like, wherein the active substances such as ursolic acid, rutin and the like play an important role in an antiallergic process, and has a remarkable effect in the process of inhibiting mast cell degranulation.
In some embodiments, the terminalia catappa leaf extract and the morinda citrifolia leaf extract are matched, so that the synergistic effect is achieved, and discomfort caused by allergic dermatitis can be well inhibited.
In some embodiments, the composition consists of 25 to 99% of the terminalia catappa leaf extract and 1 to 75% of the morinda citrifolia leaf extract by mass fraction.
In some embodiments, the preparation method of the terminalia catappa leaf extract comprises the steps of:
s1: pulverizing Terminalia catappa leaf raw material;
s2: adding the crushed Terminalia catappa leaf raw materials into an extraction tank, and extracting by using water and alcohol, wherein the mass ratio of the Terminalia catappa leaf raw materials to the water to the alcohol is 1:0.05 to 5:0.05 to 5 ℃, the extraction temperature is 50 to 80 ℃, the extraction is carried out for 1 to 5 times, the extraction time is 1 to 5 hours, and the coarse extract of the Terminalia catappa leaves is obtained;
s3: filtering the obtained crude extract of Terminalia catappa leaves, concentrating in an external circulation tank and a settling tank, freeze drying, and dissolving in 50% butanediol aqueous solution to obtain Terminalia catappa leaf extract.
In some embodiments, in the step S3, the prepared liquid component is concentrated, freeze-dried, sieved through a 80-100 mesh sieve, and dissolved in a 50% aqueous solution of butylene glycol to obtain the terminalia catappa leaf extract.
In some embodiments, the weight ratio of the terminalia catappa leaf raw material, water and alcohol in the step S2 is 1:0.05 to 5:0.05 to 5, preferably 1:0.1 to 4:0.1 to 4, more preferably 1:0.2 to 2:0.2 to 4. When the proportion of the Terminalia catappa leaf raw material, water and alcohol is 1:0.05 to 5: when the content is in the range of 0.05-5, the obtained Terminalia catappa leaf extract has high content of effective components, and can further effectively inhibit mast cell degranulation. The alcohol may be ethanol, ethylene glycol, propanol, etc.
By adopting the preparation method, the prepared terminalia catappa leaf extract is brown powder, and by mass, the ash content is below 10%, the moisture content is below 5%, the heavy metal content is below 10ppm, the lead content is below 2ppm, the arsenic content is below 3ppm, and the total number of bacteria is below 1000 CFU/g; the total amount of mould and yeast is below 100CFU/g, and no bacteria such as salmonella and Escherichia coli are existed.
In some embodiments, the temperature of the extraction is from 50 to 80 ℃, preferably from 60 to 70 ℃. The number of times of extraction is 1 to 5 times, preferably 2 to 4 times. The extraction time is 1 to 5 hours, preferably 2 to 4 hours.
On one hand, the invention provides a allergy-relieving skin care product, which comprises the allergy-relieving composition for inhibiting allergic dermatitis and a penetration enhancer, wherein the addition amount of the allergy-relieving composition for inhibiting allergic dermatitis is 0.01-10% by mass percent; the addition amount of the penetration enhancer is 0.01-10%, and the penetration enhancer is bis-diethoxy diglycol cyclohexane 1,4-dicarboxylic acid ester.
In some embodiments, the allergy-relieving composition for inhibiting allergic dermatitis is added in an amount of 0.01 to 10% by mass of the allergy-relieving skin care product, for example: the amount of the desensitizing composition added may be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 9%, etc. When the addition amount of the allergy-relieving composition is between 0.01 and 10 percent, the skin elasticity of the skin care product using the allergy-relieving composition is increased. When the addition amount of the allergy relieving composition is less than 0.01%, the improvement effect of skin allergy symptoms is not obvious, and the allergy relieving effect cannot be achieved; when the amount of the atopic dermatitis inhibitor composition added is more than 10%, the content of the composition is too high, the cost is too high, and the allergic effect cannot be further increased.
In some embodiments, the penetration enhancer is added in an amount of 0.01 to 10% by mass of the soothing skin care product, for example: 0.5%, 1%, 2%, 3%, 5%, 6%, 7%, 8%, etc. When the addition amount of the penetration enhancer is less than 0.01%, the penetration enhancing effect is not significant. When the addition amount of the penetration enhancer is more than 10%, the penetration enhancer cannot further function.
In some embodiments, at least one of a moisturizer, a thickener, a pH adjuster, an emulsifier, an oil, a skin conditioner, an antioxidant, a preservative, a whitening agent, and a fragrance is further included.
In some embodiments, the humectant is added in an amount of 0.01 to 20% by mass of the allergy-relieving skin care product; the addition amount of the thickening agent is 0.02-1.5%; the addition amount of the pH regulator is 0.01-1%; the addition amount of the emulsifier is 0.01-2%; the addition amount of the grease is 1-8%; the addition amount of the skin conditioner is 0.01 to 10 percent; the addition amount of the antioxidant is 0.01-1%; the addition amount of the preservative is 0.01-1%; the addition amount of the sensitizer is 0.01-5%; the adding amount of the aromatic is 0.005-0.5%.
In some embodiments, the moisturizer may be added in an amount of 1 to 19%, may be 3 to 18%, may be 5 to 16%, may be 7 to 15%, may be 8 to 14%, and the like, by mass percentage of the soothing skin care product. When the content of the humectant is less than 0.01%, the moisturizing effect is not obvious; when the content of the humectant is more than 20%, the allergy-relieving skin care product has sticky feeling.
In some embodiments, the thickener may be added in an amount of 0.05 to 0.6%, may be 0.1 to 0.5%, etc., in terms of mass percentage of the soothing skin care product.
In some embodiments, the pH adjusting agent is added in an amount of 0.01 to 1% by mass of the soothing skin care product. The pH value of the allergy-relieving emulsion is more suitable for human skin by adding the pH regulator. The amount of the pH adjuster of the present invention to be added may be preferably 0.03 to 0.8%, 0.06 to 0.5%, 0.1 to 0.3%, or the like. When the addition amount of the pH regulator is more than 1% or less than 0.01%, the allergy-relieving skin care product with proper pH value cannot be obtained.
In some embodiments, the amount of the oil added is 5-20% by mass of the soothing skin care product, for example, the amount of the oil added may be 8%, 10%, 12%, 14%, 16%, 18%, and the like. By adding oil into the allergy-relieving emulsion, evaporation of water on the surface of the skin can be reduced, and skin chapping can be prevented. In addition, by adding oil or fat, a hydrophobic film can be formed on the skin surface to prevent the invasion of harmful substances from the outside. When the content of the oil is less than 5%, evaporation of moisture on the skin surface cannot be reduced, and intrusion of harmful substances cannot be effectively prevented; when the content of the oil is more than 20 percent, the allergy-relieving emulsion is too greasy, and the use feeling is reduced.
In some embodiments, the emulsifier is added in an amount of 0.01 to 5% by mass of the soothing skin care product, for example: may be 0.1 to 4.5%, may be 1 to 4%, etc. When the dosage of the emulsifier is less than 0.01%, the emulsification is insufficient, so that the system is unstable; when the dosage of the emulsifier is more than 5 percent, certain influence on the stability of the product can be caused.
In some embodiments, the emulsification systems of the present application are non-water-in-oil systems, and thus, when propylene glycol and bis-diethoxydiethylene glycol cyclohexane 1,4-dicarboxylate are used as permeation enhancers, their synergistic effect is not compromised, if not simultaneously added.
In some embodiments, the skin conditioning agent is added in an amount of 0.01 to 5% by mass of the soothing skin care product. The addition amount of the skin conditioner can be 0.1-4%, 0.15-3%, 0.2-2% and the like. When the addition amount of the skin conditioner is less than 0.01%, the corresponding effect cannot be achieved; when the skin conditioning agent is added in an amount of more than 5%, the cost is too high.
The allergy-relieving emulsion can also be added with a small amount of whitening agent. The addition amount of the skin whitening agent is 0.01-5%. The skin whitening agent may be added in an amount of 0.01 to 4%, 0.1 to 3%, 0.4 to 2%, etc. When the addition amount of the skin whitening agent is less than 0.01%, the content is too low to play a corresponding effect; when the amount of the skin whitening agent added is more than 5%, the cost is too high.
The skin whitening agent comprises one or more of nicotinamide, magnolia sieboldii extract, kojic acid and its derivatives, arbutin and its derivatives, and vitamin C and its derivatives.
In some embodiments, the added amount of the antioxidant is 0.01 to 1 percent by mass of the soothing skin care product. The invention can prevent the oily components of oil, wax, hydrocarbon and the like of the cosmetics from contacting with oxygen in the air to generate oxidation, generate peroxide, aldehyde, acid and the like, and lead the cosmetics to discolor, rancidity, quality reduction and the like by using the antioxidant. The antioxidant comprises one or more of butylated hydroxytoluene, lycopene, tocopherol and tocopherol acetate.
In addition, the skin care product for soothing the allergy also contains a preservative and a flavoring agent. The preservative in the skin care product is added in an amount of 0.01-1% and the aromatic is added in an amount of 0.01-0.5% in percentage by mass. The preservative can comprise one or the combination of more than two of phenoxyethanol, methyl hydroxybenzoate, propyl hydroxybenzoate, benzoic acid and salts thereof. The aromatic may be a perfume, etc.
In some embodiments, the humectant is selected from at least one of glycerin, dipropylene glycol, glyceryl polyether-26, sodium hyaluronate, panthenol, PEG/PPG-17/6 copolymer, butylene glycol, xylitol, betaine, glycerin polymethacrylate, propylene glycol, mannose, trehalose.
In some embodiments, the thickener is selected from at least one of carbomer, xanthan gum, sclerotium rolfsii, behenyl alcohol, ammonium acryloyldimethyltaurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyltaurate copolymer, acrylic acid/C10-30 alkanol acrylate crosspolymer, hydroxyethyl acrylate/sodium acryloyldimethyltaurate copolymer, and a complex of isohexadecane and polysorbate-60.
In some embodiments, the pH adjusting agent is selected from at least one of aminomethyl propanol, arginine, citric acid, sodium citrate, sodium hydroxide.
In some embodiments, the emulsifier is selected from at least one of PEG-20 methyl glucose sesquistearate, sorbitan isostearate, polyglyceryl-3 methyl glucose distearate, laureth-7, isosteareth-20.
In some embodiments, the oil or fat is selected from at least one of cyclopentadimethylsiloxane, cyclomethicone, a composite of dimethicone and dimethiconol, oleyl erucate, shea butter, ethylhexyl palmitate, hydrogenated polydecene, cyclohexasiloxane, hydrogenated polyisobutene, C20-24 alkyl dimethicone, C13-14 isoparaffin, C12-15 alcohol benzoate.
In some embodiments, the skin conditioning agent is selected from at least one of hydrolyzed collagen, avenin, ceramide 3, fucus extract, chlorella fermentation product, chlorella extract, brown algae extract, witch hazel water, bisabolol, allantoin, mistletoe ginkgo leaf extract, cogongrass rhizome extract, serine, kelp extract, beta-glucan, and cactus extract.
In some embodiments, the antioxidant is selected from at least one of vitamin E, tocopherol acetate, butylated hydroxytoluene, lycopene.
The allergy-relieving skin care product can be emulsion, cream or aqua and the like with allergy-relieving efficacy.
On one hand, the invention also provides a allergy-relieving emulsion which comprises the following components in percentage by weight:
phase A:
Figure GDA0003828202450000071
phase B:
0.1 to 5 percent of compound of cyclopentadimethylsiloxane and cyclohexasiloxane;
0.01 to 0.5 percent of tocopherol acetate;
and C phase:
Figure GDA0003828202450000072
Figure GDA0003828202450000081
phase D:
0.1 to 5 percent of glycerin polymethacrylate;
0.1 to 5 percent of C12-15 alcohol benzoate;
0.01 to 1 percent of aminomethyl propanol;
phase E:
Figure GDA0003828202450000082
Figure GDA0003828202450000091
in some embodiments, a soothing emulsion of the present application, method of making the same, comprises the steps of:
1) Adding the phase A raw material into an oil phase pot, stirring and heating to 75-85 ℃, and completely dissolving; before emulsification, adding the phase B raw material into an oil phase pot, and keeping the temperature at 75-85 ℃ for 5-20 min;
2) Adding the C-phase raw material into a water phase pot, stirring and dissolving completely, heating to 75-85 ℃, and keeping the temperature for 5-20 min;
3) Vacuumizing, preheating and drying the emulsifying pot, pumping the phase C, pumping the phase A/B mixed phase in vacuum, homogenizing for 1-10 minutes at the stirring speed of 1000-1500 rpm, and stirring for 20-40 minutes at the temperature of 75-85 ℃;
4) Cooling to 55-65 ℃, adding the phase D, stirring at 500-1000 r/min, and stirring uniformly;
5) Cooling to 40-50 ℃, adding the phase E and stirring uniformly;
6) Cooling to 30-40 ℃, discharging after passing the inspection, and standing for 12-48 hours;
7) And (5) inspecting, subpackaging, packaging, inspecting again, and warehousing finished products.
The invention has the beneficial effects that:
the Terminalia catappa leaf extract has an excellent inhibition effect on mast cell degranulation, and has wide application in allergy-relieving skin care products.
The allergy-relieving composition disclosed by the application has a synergistic effect by matching the terminalia catappa leaf extract and the morinda officinalis leaf extract, and can well inhibit discomfort caused by allergic dermatitis.
The allergy-relieving skin care product comprises the allergy-relieving composition and the penetration enhancer, can inhibit mast cells from degranulation and play a role in relieving allergy, and also has the effects of moisturizing, locking water, blocking water loss and creating a moisturizing barrier for skin. Meanwhile, the soothing and sensitizing emulsion disclosed by the invention has a repairing effect on skin and activates the function of the skin, and the preparation method is simple to operate and can be used for large-scale production.
Drawings
Fig. 1 is a graph of the sample concentration of the terminalia catappa leaf extract, which is the mass concentration of the terminalia catappa leaf extract, versus the cell viability in examples 1-5;
FIG. 2 is a graph of the effect of Terminalia catappa leaf extract on mast cell P815 degranulation test in examples 6-10;
FIG. 3 is a graph showing the measurement of histamine release from mast cells P815 by the Terminalia catappa leaf extract in examples 11-15;
FIG. 4 shows the relief of lactic acid prick test in application examples 2 to 6 and application comparative example 1 and application comparative example 7 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will understand that,
the following examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are commercially available, and are not indicated by manufacturers.
In the embodiment of the present invention, the preparation method of the applied terminalia catappa leaf extract comprises: the method comprises the steps of crushing the terminalia catappa leaf raw materials, adding the crushed terminalia catappa leaf raw materials into an extraction tank, adding water and ethanol at the temperature of 70 ℃, boiling and extracting for 3 times, wherein the mass ratio of the terminalia catappa leaf raw materials to the water to the ethanol is 1. Then filtering the obtained terminalia catappa leaf extract, storing the terminalia catappa leaf extract in a storage tank, slowly flowing the filtrate in the storage tank into an external circulation tank and a settling tank for concentration to obtain liquid components and precipitates, performing spray drying on the liquid components, drying the precipitates, and sieving the dried precipitates with a 80-100-mesh sieve to obtain the terminalia catappa leaf extract, and then detecting the terminalia catappa leaf extract to obtain the terminalia catappa leaf extract with the ash content of 7% and the water content of 4%.
In the embodiment of the present invention, the method for preparing the extract of the morinda citrifolia leaf comprises: drying and crushing morinda citrifolia leaves at 60 ℃, sieving the crushed morinda citrifolia leaves with a 40-mesh sieve, adding the crushed morinda citrifolia leaves into an extraction tank, adding water and ethanol at the water bath temperature of 60 ℃, extracting for 2 times at a mass ratio of 1. Dissolving the ethanol primary extract of the morinda citrifolia with a certain volume of deionized water, filtering with macroporous resin, eluting with 3-5 BV of water, eluting with 4-6 BV of 65% ethanol solution, and collecting the ethanol eluate. Concentrating the eluent until the relative density is 1.05-1.1, spray-drying the supernatant, drying the precipitate under reduced pressure, mixing uniformly, and sieving with a 100-mesh sieve to obtain the morinda citrifolia leaf extract.
It should be noted that different batches of purchased extract will have a corresponding error, typically not exceeding 5%.
Keratinocyte activity assay:
the Terminalia catappa leaf extract was diluted with phosphate buffer to give 5 sets of test solutions of different concentrations (final concentration) and filtered using a 0.22 μm filter head. The mass concentration of the Terminalia catappa leaf extract when tested for cell viability is shown in Table 1 below.
(1) The test method comprises the following steps: using a Calcein-AM fluorescent probe to mark living cells for in-vitro keratinocyte activity detection;
(2) The testing steps are as follows: the keratinocytes were counted and diluted to 5X 10 4 one/mL, and 100. Mu.L of the suspension was inoculated into a black 96-well cell culture plate, and incubated at 37 ℃ in an incubator without light for 12 hours without addition of keratinocytes to the blank. After the culture medium is sucked and discarded, 100 mul of the Terminalia catappa leaf extract with different concentrations is added into the experimental group, 100 mul of the culture medium is added into the blank group and the control group, and the blank group and the control group are incubated for 2 to 4 hours in an incubator at 37 ℃ in the dark. Add 100 u L3 xCalcein-AM solution, at 37 degrees C incubator light protection were incubated for 30 minutes.After incubation is finished, fluorescence can be directly detected by a fluorescence microplate reader (excitation wavelength is 494nm, emission wavelength is 517 nm) and cell activity is calculated, wherein the cell activity is in direct proportion to fluorescence intensity.
(3) The keratinocyte activity rate is calculated according to the following formula:
keratinocyte activity rate = [ (OD experimental group-OD blank)/(OD control group-OD blank) ] × 100%
TABLE 1
Figure GDA0003828202450000111
Figure GDA0003828202450000121
Mast cell degranulation assay:
(1) The test method comprises the following steps: mast cell degranulation assay
(2) The testing steps are as follows: taking the logarithmic growth phase concentration as 5 multiplied by 10 4 mu.L of P815 cells per ml were seeded in 96-well plates at 37 ℃ in CO 2 The incubator was grown for 48h. The supernatant medium was aspirated and washed 3 times with Tyrode's solution. Adding 100 μ L of Terminalia catappa leaf extract into experimental group, adding 100 μ L of Tyrode solution into control group and blank group, respectively, repeating three wells, and adding CO at 37 deg.C 2 Incubate for 5 minutes. The experimental and control groups were stimulated with 50. Mu. L C48/80 (10. Mu.g/mL), and the blank group was treated with 50. Mu.L of Tyrode solution in a 37 ℃ water bath for 45 minutes. After the incubation, 0.5% neutral red dye solution was added, and the cells were stained for 3 minutes, observed with a fluorescence microscope, and the number of degranulated mast cells of 200 cells was counted. Normal mast cells are round, smooth in edges, non-pigmented in nuclei, and have uniformly distributed pomegranate red granules inside cells; when the mast cells were deformed, irregular edges, or colored nuclei, degranulation was judged.
(3) The degranulation rate of mast cells was calculated according to the following formula:
relative mast cell degranulation (%) = [ (number of degranulated cells in experimental group-number of degranulated cells in blank group)/(number of degranulated cells in control group-number of degranulated cells in blank group) ] × 100%.
TABLE 2
Figure GDA0003828202450000122
Figure GDA0003828202450000131
Mast cell histamine content assay:
(1) The test method comprises the following steps: mast cell histamine content detection
(2) The testing steps are as follows: taking the logarithmic growth phase concentration as 5 multiplied by 10 4 100. Mu.L of P815 cells per ml were seeded in 96-well plates at 37 ℃ in CO 2 The incubator was grown for 48 hours. The supernatant medium was aspirated and discarded, and washed 3 times with Tyrode's solution. Adding 100 μ L of Terminalia catappa leaf extract with different concentrations into experimental group, adding 100 μ L of Pyrode solution into control group and blank group, respectively, repeating three wells, and placing in 37 deg.C CO 2 Incubate for 5 minutes. The experimental and control groups were stimulated with 50uL of C48/80 (10. Mu.g/mL), and the blank group was treated with 50. Mu.L of Pyrode solution in a 37 ℃ water bath for 45 minutes. After incubation, cell supernatants were removed and worked up according to mouse histamine kit instructions.
The method comprises the steps of coating a microporous plate with purified mouse Histamine (HIS) antibody to prepare a solid-phase antibody, sequentially adding the Histamine (HIS) into the microporous plate coated with a monoclonal antibody, combining with a Histamine (HIS) antibody marked by horseradish peroxidase to form an antibody-antigen-enzyme labeled antibody compound, and adding a substrate of tetramethylbenzidine for color development after thorough washing. Tetramethylbenzidine is converted to blue by the catalysis of horseradish peroxidase and to the final yellow by the action of an acid. The shade of the color was positively correlated with Histamine (HIS) in the sample. The absorbance was measured at a wavelength of 450nm with a microplate reader.
(3) Relative histamine concentration (%) = [ (OD experimental-OD blank)/(OD control-OD blank) ] × 100%
TABLE 3
Figure GDA0003828202450000132
Figure GDA0003828202450000141
Application examples and comparative application examples
The emulsions were prepared according to the following production process steps and with the contents (mass percentages) of the components in the emulsion formulations of application examples 2 to 6 and comparative application examples 1/7 in table 4 below.
TABLE 4
Figure GDA0003828202450000142
Figure GDA0003828202450000151
The production process comprises the following steps:
1. adding the phase A raw material into an oil phase pot, stirring and heating to 82 ℃, and completely dissolving; adding the phase B raw material into an oil phase pan before emulsification, and keeping the temperature at 82 ℃ for 10min;
2. adding the C-phase raw material into a water phase pot, stirring and dissolving completely, heating to 82 ℃, and keeping the temperature for 10min;
3. vacuumizing, preheating and drying the emulsifying pot, pumping the phase C, pumping the phase A/B mixed phase in vacuum, homogenizing for 5 minutes at the stirring speed of 1200 rpm, and keeping the temperature at 82 ℃ and stirring for 30 minutes;
4. cooling to 60 ℃, adding the phase D, stirring at the speed of 800 revolutions per minute, and stirring uniformly;
5. cooling to 45 ℃, adding the phase E and stirring uniformly;
6. cooling to 36 ℃, discharging after passing the inspection, and standing for 24 hours;
7. and (5) inspecting, subpackaging, packaging, inspecting again, and warehousing finished products.
Note: the A, B, C, D, E phases in the process are respectively:
phase A: polyglyceryl-3 methyl glucose distearate, glyceryl stearate, ethylhexyl palmitate, hydrogenated polydecene, oleyl erucate, shea butter, polydimethylsiloxane, methylparaben, butylated hydroxytoluene, ceramide 3, bisabolol;
phase B: a complex of cyclopentadimethylsiloxane and cyclohexasiloxane, tocopheryl acetate;
and C phase: water, glycerol, propylene glycol, butanediol, dipropylene glycol, allantoin, betaine, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, carbomer;
phase D: glycerol polymethacrylate, C12-15 alcohol benzoate, aminomethyl propanol;
phase E: terminalia catappa leaf extract, morinda citrifolia leaf extract, magnolia sieboldii extract, beta-glucan, phenoxyethanol, perfume, bis-diethoxydiol cyclohexane 1,4-dicarboxylate.
Wherein polyglycerol-3-methylglucidistearate is an emulsifier;
glyceryl stearate, glycerin, butanediol, propylene glycol, dipropylene glycol, betaine, and glyceryl polymethacrylate are moisturizers;
ethylhexyl palmitate, hydrogenated polydecene, oleyl erucate, shea butter, polydimethylsiloxane, a compound of cyclopentadimethylsiloxane and cyclohexasiloxane, and C12-15 alcohol benzoate are oils;
phenoxyethanol and methyl hydroxybenzoate as antiseptic; butylated hydroxytoluene and tocopherol acetate are antioxidants;
hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and carbomer are thickening agents;
aminomethyl propanol is a pH modifier; magnolia sieboldii extract is a whitening agent;
ceramide 3, allantoin, beta-glucan are skin conditioners; the essence is an aromatic.
Bis-diethoxydiethylene glycol cyclohexane 1,4-dicarboxylate is a penetration enhancer;
terminalia catappa leaf extract and Morinda citrifolia leaf extract are compositions for inhibiting allergic dermatitis.
Manufacturer of the compound of cyclopentadimethylsiloxane and cyclohexasiloxane: the trade mark is as follows: a DC345; purchased from: dow Corning, USA.
Lactic acid sting test:
the Lactic acid tingling test (LAST) is essential in the development links of most anti-allergy cosmetic raw materials and products, and is the most effective method for evaluating sensitive skin. The method is simple, convenient, effective and high in repeatability, and is widely applied to clinical detection and experimental research. The lactic acid sting test was conducted as follows: at room temperature, 50. Mu.L of a 10% lactic acid aqueous solution was applied to one nasolabial fold, and the subjective symptoms of the subjects were asked at 2.5min and 5min, respectively, and scored by 4 points (0 point no stinging sensation, 1 point mild stinging, 2 point moderate stinging, and 3 point severe stinging). And then adding the two fractions to obtain the lactic acid stabbing pain score. Meanwhile, the skin barrier repair effect of the allergy-free lotion is evaluated by comparing the scores of the skin lactic acid sting test before and after the allergy-free lotion is used.
The number of subjects was 48, the experimental period was 4 weeks, 6 subjects were selected as one group, and the operation was performed according to 7 application embodiments and a control group shown in table 4, wherein the control group was ultrapure water, allergy-relieving emulsion (ultrapure water was used for the control group) was applied to the nasolabial sulcus on the same side every morning and evening, and the skin of the test area before the experiment (Day 1) and 28 days (Day 28) was measured and subjected to the lactic acid sting test and scored, respectively, and the results of the alleviation of the lactic acid sting test before and after the experiment are shown in fig. 4. Lactic acid sting relief value = lactic acid sting score before experiment (Day 1) -lactic acid sting score after experiment (Day 28).
As can be seen from FIG. 1, the concentration of the Terminalia catappa leaf extract is between 0.25 mg/ml and 5mg/ml, and the activity rate on keratinocytes is more than 90%, thus demonstrating that damage to skin keratinocytes in the extract concentration interval can be ignored.
From fig. 2, it can be seen that the concentration of the Terminalia catappa leaf extract is between 0.25 mg/ml and 5mg/ml, the Terminalia catappa leaf has an inhibitory effect on mast cell degranulation, and the inhibitory rate increases with the increase of the concentration; from fig. 3, it can be seen that the extract concentration is between 0.25 mg/ml and 5mg/ml, the Terminalia catappa leaf extract can inhibit histamine release, and the inhibition effect is increased along with the increase of the concentration, thus proving that the extract has the effect of inhibiting the generation of allergic dermatitis.
In fig. 4, it is understood that the application examples and the comparative application examples have the effect of relieving the atopic dermatitis by comparing the application examples 1 to 7 with the control group, while the application examples 2 to 6 having both the terminalia catappa leaf extract and the morinda citrifolia leaf extract have the synergistic effect, the corresponding effect is better than the application examples 1 and 7, and the effect of relieving the atopic dermatitis is the best when the formulation of example 5 is applied.
It should be understood that the above embodiments are only for illustrating the technical solutions of the present invention, and not for limiting the same, and those skilled in the art can modify the technical solutions described in the above embodiments, or make equivalent substitutions for some technical features; and all such modifications and alterations are intended to fall within the scope of the appended claims.

Claims (8)

1. The application of the Terminalia catappa leaf extract in preparing a skin care product for inhibiting the generation of allergic dermatitis comprises the following steps:
s1: pulverizing Terminalia catappa leaf raw material;
s2: adding the crushed Terminalia catappa leaf raw materials into an extraction tank, and extracting by using water and alcohol, wherein the mass ratio of the Terminalia catappa leaf raw materials to the water to the alcohol is 1:0.05 to 5:0.05 to 5, extracting for 1~5 times at the extraction temperature of 50 to 80 ℃ for 1~5 hours to obtain a coarse extract of the terminalia catappa leaves;
s3: filtering the obtained crude extract of Terminalia catappa leaves, concentrating in an external circulation tank and a settling tank, freeze drying, and dissolving in 50% butanediol aqueous solution to obtain Terminalia catappa leaf extract.
2. A soothing composition for inhibiting the formation of allergic dermatitis is characterized by comprising an extract of Terminalia catappa leaves and an extract of Morinda citrifolia leaves,
the weight ratio of the Terminalia catappa leaf extract to the Morinda citrifolia leaf extract is 1.01 to 3, and the preparation method of the Terminalia catappa leaf extract comprises the following steps:
s1: pulverizing Terminalia catappa leaf raw material;
s2: adding the crushed Terminalia catappa leaf raw materials into an extraction tank, and extracting by using water and alcohol, wherein the mass ratio of the Terminalia catappa leaf raw materials to the water to the alcohol is 1:0.05 to 5: extracting 1~5 times at 50-80 deg.C for 1~5 hr for 0.05-5 to obtain coarse extract of Terminalia catappa leaves;
s3: filtering the obtained crude extract of Terminalia catappa leaves, concentrating in an external circulation tank and a settling tank, freeze drying, and dissolving in 50% butanediol aqueous solution to obtain Terminalia catappa leaf extract.
3. The soothing composition of claim 2, wherein the mass ratio of the Terminalia catappa leaf extract to the Morinda citrifolia leaf extract is 1.
4. A allergy-relieving skin care product, which is characterized by comprising the allergy-relieving composition for inhibiting the generation of allergic dermatitis according to any one of claims 2~3 and a penetration enhancer, wherein the addition amount of the allergy-relieving composition is 0.01-10% by mass of the allergy-relieving skin care product; the addition amount of the penetration enhancer is 0.01-10%, and the penetration enhancer is bis-diethoxydiethylene diglycol cyclohexane 1,4-dicarboxylic ester.
5. The soothing skin care product of claim 4, further comprising at least one of a humectant, a thickener, a pH adjuster, an emulsifier, a grease, a skin conditioner, an antioxidant, a preservative, a whitening agent, and a fragrance;
the adding amount of the humectant is 0.01 to 20 percent by mass of the allergy-relieving skin care product; the addition amount of the thickening agent is 0.02 to 1.5 percent; the addition amount of the pH regulator is 0.01 to 1 percent; the addition amount of the emulsifier is 0.01 to 5 percent; the addition amount of the grease is 5 to 20 percent; the addition amount of the skin conditioner is 0.01 to 10 percent; the addition amount of the antioxidant is 0.01 to 1 percent; the addition amount of the preservative is 0.01 to 1 percent; the addition amount of the whitening agent is 0.01 to 5 percent; the addition amount of the aromatic is 0.005 to 0.5 percent.
6. The soothing skin care product of claim 5, wherein the moisturizer is selected from at least one of glycerin, dipropylene glycol, glyceryl polyether-26, sodium hyaluronate, panthenol, PEG/PPG-17/6 copolymer, butylene glycol, xylitol, betaine, glyceryl polymethacrylate, propylene glycol, mannose, trehalose;
the thickening agent is selected from at least one of carbomer, xanthan gum, sclerotium rolfsii, behenyl alcohol, acryloyl dimethyl taurate/VP copolymer, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer and a compound of isohexadecane and polysorbate-60;
the emulsifier is at least one selected from PEG-20 methyl glucose sesquistearate, sorbitan isostearate, polyglycerol-3 methyl glucose distearate, laureth-7 and isosteareth-20;
the grease is selected from at least one of cyclopentadimethylsiloxane, cyclomethicone, a compound of dimethicone and dimethiconol, oleyl erucate, shea butter, ethylhexyl palmitate, hydrogenated polydecene, cyclohexasiloxane, hydrogenated polyisobutene, C20-24 alkyl dimethicone, C13-14 isoparaffin, C12-15 alcohol benzoate;
the skin conditioning agent is selected from at least one of hydrolyzed collagen, oat peptide, ceramide 3, fucus vesiculosus extract, chlorella fermentation product, chlorella extract, brown algae extract, hamamelis virginiana water, bisabolol, allantoin, folium Ginkgo Viscum album extract, lalang grass rhizome extract, serine, macrocystis grandiflora extract, beta-glucan, and radix et caulis Opuntiae Dillenii extract;
the antioxidant is at least one selected from vitamin E, tocopherol acetate, butylated hydroxytoluene and lycopene;
the whitening agent is selected from one or more of niacinamide, magnolia sieboldii extract, kojic acid and its derivatives, arbutin and its derivatives, and vitamin C and its derivatives.
7. The allergy-relieving emulsion is characterized by comprising the following components in percentage by weight:
phase A:
0.1 to 3 percent of hydrogenated polydecene;
0.5 to 5 percent of polydimethylsiloxane;
0.1 to 4 percent of polyglycerol-3-methylglucose distearate;
0.5 to 8 percent of ethylhexyl palmitate;
0.1 to 2 percent of shea butter;
0.1 to 8 percent of glycerol stearate;
0.01 to 2 percent of oleyl erucate;
ceramide 3.05 to 1 percent;
0.05 to 0.4 percent of methylparaben;
butylated hydroxytoluene 0.001 to 0.5 percent;
phase B:
0.1 to 5 percent of compound of cyclopentadimethylsiloxane and cyclohexasiloxane;
0.01 to 0.5 percent of tocopherol acetate;
and C phase:
the balance of water is 100%;
0.1 to 5 percent of propylene glycol;
0.1 to 5 percent of glycerin;
0.1 to 7 percent of butanediol;
0.5 to 10 percent of dipropylene glycol;
0.1 to 5 percent of betaine;
0.02 to 0.8 percent of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer;
0.01 to 2 percent of allantoin;
0.01 to 1.5 percent of carbomer;
phase D:
0.1 to 5 percent of glycerin polymethacrylate;
0.1 to 5 percent of C12-15 alcohol benzoate;
0.01 to 1 percent of aminomethyl propanol;
phase E:
0.01 to 1 percent of beta-glucan;
bis-diethoxydiol cyclohexane 1,4-dicarboxylic ester 0.01 to 10%;
0.1 to 1 percent of phenoxyethanol;
0.01 to 5 percent of magnolia sieboldii extract
0.005 to 0.5 percent of essence;
0.1 to 5 percent of the extract of the terminalia catappa leaves;
0.1 to 10 percent of Morinda citrifolia leaf extract,
the preparation method of the Terminalia catappa leaf extract comprises the following steps:
s1: pulverizing Terminalia catappa leaf raw material;
s2: adding the crushed Terminalia catappa leaf raw materials into an extraction tank, and extracting by using water and alcohol, wherein the mass ratio of the Terminalia catappa leaf raw materials to the water to the alcohol is 1:0.05 to 5: extracting 1~5 times at 50-80 deg.C for 1~5 hr for 0.05-5 to obtain coarse extract of Terminalia catappa leaves;
s3: filtering the obtained crude extract of Terminalia catappa leaves, concentrating in an external circulation tank and a settling tank, freeze drying, and dissolving in 50% butanediol aqueous solution to obtain Terminalia catappa leaf extract.
8. The soothing emulsion of claim 7, wherein the soothing emulsion is prepared by a method comprising the steps of:
1) Adding the phase A raw material into an oil phase pot, stirring and heating to 75 to 85 ℃, and completely dissolving; adding the raw material of the phase B into an oil phase pot before emulsification, and keeping the temperature at 75 to 85 ℃ for 5 to 20min;
2) Adding the C-phase raw material into a water phase pot, stirring and dissolving completely, heating to 75 to 85 ℃, and keeping the temperature for 5 to 20min;
3) Vacuumizing, preheating and drying an emulsifying pot, pumping the phase C, pumping the phase A/B mixed phase in vacuum, homogenizing for 1 to 10 minutes at a stirring speed of 1000 to 1500 rpm, and stirring for 20 to 40 minutes at a temperature of 75 to 85 ℃;
4) Cooling to 55 to 65 ℃, adding the phase D, stirring at the speed of 500 to 1000 r/min, and stirring uniformly;
5) Cooling to 40-50 ℃, adding the phase E, and uniformly stirring;
6) Cooling to 30-40 ℃, discharging after the test is qualified, and standing for 12-48 hours to obtain the allergy-relieving emulsion.
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