CN112754974A - Composition with anti-allergy repairing effect and preparation method thereof - Google Patents

Composition with anti-allergy repairing effect and preparation method thereof Download PDF

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CN112754974A
CN112754974A CN202110059271.4A CN202110059271A CN112754974A CN 112754974 A CN112754974 A CN 112754974A CN 202110059271 A CN202110059271 A CN 202110059271A CN 112754974 A CN112754974 A CN 112754974A
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extract
composition
allergy
skin
ceramide
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CN112754974B (en
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李晶
王莉
岳娟
毕天宇
徐思伟
毕永贤
蒋丽刚
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Proya Cosmetics Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/68Sphingolipids, e.g. ceramides, cerebrosides, gangliosides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/732Starch; Amylose; Amylopectin; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9706Algae
    • A61K8/9722Chlorophycota or Chlorophyta [green algae], e.g. Chlorella
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/005Preparations for sensitive skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists

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Abstract

The invention relates to a composition with anti-allergy repairing efficacy and a preparation method thereof, which is characterized by comprising the following components: 0.1-1% of Enteromorpha compressa extract, 0.1-1% of onion bulb extract, 0.1-1% of quince leaf extract, 0.1-1% of Potentilla palmifolia root extract, 7-15% of squalane, 60-80% of ceramide 3 powder, 4-8% of hydroxypropyl starch phosphate and 1-3% of polyglycerol-3 methyl glucose distearate, wherein the percentages are mass percentages. The skin care product disclosed by the invention can be used for relieving and repairing sensitive skin through multi-way comprehensive effects and synergistic synergism. The preparation method has the advantages of simple process, controllable conditions, high production efficiency, good stability and solubility of the obtained composition, mildness, no irritation, remarkable anti-allergy repair effect and the like.

Description

Composition with anti-allergy repairing effect and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetic preparation, and particularly relates to a composition with an anti-allergy repairing effect and a preparation method thereof.
Background
Recent consumer survey shows that about half of female consumers consider themselves to be sensitive skin types, the tendency is more obvious in urban females, the age of 26-30 years is the age group with the most concentrated sensitive muscles, the phenomenon mainly comprises three main causes of spicy food, season change and ultraviolet rays, and meanwhile, the skin is sensitive due to high living and working pressure, irregular work and rest time and improper use of cosmetics. Not only can frequently rub with skin after the mask is worn for a long time, but also the skin barrier is easily damaged due to poor air permeability of the mask, and then the probability of sensitive reaction of the skin is greatly improved. Therefore, the cosmetics for sensitive muscles have huge market potential, and the demand of anti-sensitive repair type functional raw materials is strong.
The main causes of sensitive muscles: 1. the skin barrier is damaged, the percutaneous water loss is increased, the water content of the stratum corneum is low, external factors are induced to break the barrier function of the skin, and external stimulation factors are easier to enter the skin to cause allergic reaction of the skin; 2. the nerve growth content is high, and when the nerve growth content is stimulated by the outside, the nerve reactivity is high, and anaphylactic reaction is easy to occur; 3. due to the characteristics of barrier function damage or nerve function abnormality of sensitive skin, the sensitive skin is harder to resist the invasion of external irritants and allergens compared with normal skin, and a series of skin inflammatory reactions caused by irritation or allergy are easy to occur, so that the skin barrier structure and nerve endings are further damaged, and vicious circle is caused.
With the increasing importance of consumers on the sources and efficacies of cosmetic components, the industry is developing in the direction of more nature, safety, effectiveness and convenience in the development stage of efficacy raw materials. In the actual application and storage processes, the natural functional raw materials often have the problems of low solubility, poor stability, single action mechanism and the like, and the development and the use of the natural functional raw materials are limited. In addition, the natural plant extract has certain requirements on transportation and storage conditions and corrosion resistance, and preservatives and polyhydric alcohols are required to be added for bacteriostasis, so that the safety, the mildness and the skin feel of the product are influenced to a certain extent. Therefore, how to mix natural active ingredients with different sources, different solubility properties and different efficacies to realize synergistic interaction and more stably and conveniently apply the natural active ingredients to products has important significance for developing functional cosmetics.
The high-shear wet granulation is a high-efficiency method for preparing powder and liquid into compact granules, and has controllable conditions and convenient amplification and mass production. The production process includes processing the material and supplementary material into powder, adding proper amount of adhesive to moisten the surface of the material powder, making the material powder to be combined together through the bridge frame of the adhesive and the adhesion, and shearing mechanical force with high speed shearing knife in the pot and the action of the liquid bridge frame to form grains in certain shape, size and density. Compared with the dry granulation, the wet granulation has the advantages of low equipment cost, simple operation, short granulation time, low energy consumption, high material yield, uniform particle size distribution of the prepared particles, good fluidity and the like. Meanwhile, because liquid is involved in the granulating process, dust and air pollution cannot be generated. The high-shear wet granulation technology can improve the solubility by adjusting the bulk density of materials, improve the application convenience, realize the mixing of various raw materials with different solubility properties, add the efficacy, and have the advantages of transportation, storage, corrosion prevention, stability and the like far exceeding those of liquid raw materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composition with anti-allergy repairing efficacy and a preparation method thereof. The preparation method has the advantages of simple process, controllable conditions and high production efficiency, and the prepared composition has long-term stability, good solubility, mildness, no irritation and remarkable anti-allergy repair effect.
In order to solve the technical problems, the invention adopts the following technical scheme: an anti-allergy repairing composition is characterized by comprising the following components: 0.1-1% of Enteromorpha compressa extract, 0.1-1% of onion bulb extract, 0.1-1% of quince leaf extract, 0.1-1% of Potentilla palmifolia root extract, 7-15% of squalane, 60-80% of ceramide 3 powder, 4-8% of hydroxypropyl starch phosphate and 1-3% of polyglycerol-3 methyl glucose distearate, wherein the percentages are mass percentages.
The invention also provides a preparation method of the anti-allergy restoration efficacy composition, which is characterized by comprising the following steps:
a: weighing 0.1-1% of Enteromorpha compressa extract, 0.1-1% of onion bulb extract, 0.1-1% of quince leaf extract, 0.1-1% of Potentilla palmifolia root extract, 7-15% of squalane, 60-80% of ceramide 3 powder, 4-8% of hydroxypropyl starch phosphate, 1-3% of polyglycerol-3 methyl glucose distearate and 10-20% of deionized water according to the following mass percentages;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 75-85 ℃ to be used as a water phase;
c: uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3-methylglucose distearate weighed in the step A in a water bath environment at the temperature of 75-85 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 75-80 ℃, wherein the rotation speed of the homogenizer is 3000-8000RPM, and the homogenization time is 10-30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, controlling the stirring speed of the high-shear wet granulator to be 300-4000 RPM (plus material plus; then transferring into a vibrating fluidized bed for vacuum drying, and drying at 50-70 deg.C for 5-15min to obtain the composition with anti-allergy repairing effect.
The obtained composition with anti-allergy repairing effect has particle size of 1.2-1.6 mm.
The composition with the anti-allergy restoration effect can be directly used after being dissolved in water, and can also be used as an active substance to be added into cosmetics with the anti-allergy restoration effect, and the addition amount is preferably 0.1-3% by mass percent.
The high-shear wet granulator is purchased from Beijing Bainaite technology Limited and has the model of GRANUMEIST; the vibrated fluidized bed was a dryer, available from Changzhou Yimin drying Equipment, Inc., model number ZLG.
The Enteromorpha compressa extract was named 01354 in catalog of names of used cosmetic raw materials (2015 edition) in China, and was purchased from Mufang Biotech Co. The content of polysaccharide in the Enteromorpha compressa extract is more than or equal to 80 percent, and the Enteromorpha compressa extract also contains active ingredients such as protein, amino acid, fatty acid, mineral substances and the like, and can improve the permeability of capillary vessels and the thickness of skin, thereby relieving sensitive skin, reducing sensitive symptoms such as irritation, redness, erythema and the like, and having good relieving and anti-allergic effects.
The onion bulb extract has the serial number of 07442 in Chinese catalogue of names of used cosmetic raw materials (2015 edition), and the commercially available product is Quercea 20 of Xianglin corporation Limited. The content of active ingredients in the onion bulb extract is more than or equal to 20 percent, the onion bulb extract mainly comprises quercetin, quercetin glycoside, protocatechuic acid and the like, can prevent ultraviolet rays and bacteria from damaging skin, and has the effects of sun protection, oxidation resistance and bacteriostasis, so that the capacity of the skin for resisting external stimulation is improved, the barrier function of the skin is enhanced, and a better anti-allergy effect is realized.
The quince leaf extract has serial number of 06800 in catalog of used cosmetic materials (2015) in China, and the commercially available product is Ko' zen from BERKEM®Quince leaf extract. The content of total polyphenols in the main active components of the quince leaf extract is more than or equal to 12%, the content of glycosylated flavonoid is more than or equal to 3%, the quince leaf extract can play a significant anti-inflammatory role by inhibiting the generation of inflammatory factors, and the quince leaf extract can play a role in resisting inflammationSo as to relieve the sensitive symptoms of skin after external stimulation, and has the effects of resisting inflammation and relieving.
The extract of the root of Potentilla palmitata has CAS number of 1134080-01-5, and the commercial product is Berkemyol Potentilla manufactured by Berkelem company. The palmitoyl Potentilla chinensis root extract is prepared from Potentilla chinensis root extract by esterification, wherein the esterified Potentilla chinensis root has polyphenol content of more than 95%, also contains partial oligomeric procyanidin, can exert strong antioxidant effect by scavenging free radicals and inhibiting lipid peroxidation, and also has effects of resisting wrinkle, inflammation and saccharification.
The SQUALANE was numbered 03432 in the catalogue of names of used cosmetic raw materials (2015 edition) in China, and the commercially available product was NIKKOL OLIVE SQUALANE available from Japan Sun-light company. Squalane is a natural oil of animal and plant sources commonly used in cosmetics, is a natural component of skin, can be rapidly dissolved with moisture and grease in the skin, forms a natural protective barrier on the skin surface, and protects the skin from being damaged by external substances. The squalane has excellent stability, can not generate oxidation with ultraviolet rays and the like, has excellent permeability and high-efficiency oxygen carrying performance, can adjust the water-oil balance of the skin, avoids the rough and dark skin, and enables the skin to recover the original tender touch.
The ceramide 3 was designated as 06016 in the catalogue of names of used cosmetic raw materials (2015 edition) in China, and is commercially available as DS-CERAMIDE Y30 from Korea bucket mountain company. Ceramide 3 is a lipid substance, has a structure similar to that of the substances constituting the stratum corneum of the skin, can quickly permeate into the skin, helps the renewal of the natural protective layer of the skin, can promote the balance of natural hydration, and can combine with water in the stratum corneum to form a network structure to promote the retention of water. It also has good effect on skin moisture retention and repair, is an important skin-activating component in the horny layer, and can enhance the skin barrier and form an effective barrier to prevent water loss and reduce the influence of external environment such as water loss and the like. The stimulated skin in particular requires more ceramide, and studies have shown that products containing ceramide components can reduce redness and skin moisture loss, act to enhance the skin barrier and help the damaged skin to relieve a dry state.
The polyglycerol-3-methylglucdistearate has a number of 03830 in catalog of names of used cosmetic raw materials (2015 edition) in China, and is commercially available as TEGO CARE 450 of Germany winning and creating company. Polyglycerol-3-methylglucidistearate is a universal emulsifier of vegetable origin free of polyethylene glycol, suitable for the preparation of oil-in-water creams and emulsions, stable at high temperatures and having good freeze-thaw stability, compatible with all cosmetic oils, highly compatible with active additives, very mild to the skin, moisturizing and helping to improve water resistance.
The hydroxypropyl starch phosphate was numbered 05225 in the catalog of names of used cosmetic raw materials (2015 edition) in China, and commercially available was Structure XL from Ack Sunobel corporation. Hydroxypropyl starch phosphate is derived from corn crops and is a starch that has been specially pregelatinized and can be dispersed very rapidly in cold water without the need for slow dusting and premixing. The heating energy causes Structure XL to swell more fully and to give the emulsion a more refined appearance and skin feel.
The invention has the beneficial effects that: (1) the invention adopts high-shear wet granulation and fluidized bed vacuum drying to prepare the composition particles, has simple preparation process, controllable conditions and high production efficiency, can simultaneously wrap oil-soluble and water-soluble functional components, and obviously improves the solubility, the dispersibility and the stability of the functional components; (2) aiming at the cause of sensitive skin and the mechanism of stratum corneum anti-allergy repair, six functional raw materials and two auxiliary raw materials are preferably selected, and through the synergistic effect of the raw materials, the skin-stimulated reaction is improved, the skin inflammation is resisted, the barrier function of the skin is enhanced, and meanwhile, the moisturizing capability is realized, the skin-stimulated reaction is relieved and anti-allergy is resisted, the damaged skin barrier is protected and repaired, the generation of inflammation media induced by external stimulation is reduced, and the generation of skin-sensitive reaction is reduced; (3) the anti-allergy restoration effect composition prepared by the invention can be simply and conveniently directly applied to anti-allergy restoration effect cosmetics in various dosage forms such as water, essence, emulsion, cream, mask and the like.
To demonstrate the beneficial effects of the present invention, the present invention further performed the following tests.
The following in vitro hyaluronidase inhibition experiments were performed with the compositions of the present invention:
preparing an acetic acid buffer solution with the pH value of 5.0 by using a glacial acetic acid diluted solution and a sodium acetate crystal water solution; then, preparing a hyaluronidase solution (with the final working concentration of 1250U/mL) and a sodium hyaluronate solution (with the concentration of 0.5 g/L) by using the prepared acetic acid buffer solution; preparing calcium chloride into an aqueous solution with the concentration of 0.25 mmol/L; preparing aqueous solution with the concentration of 0.4mol/L by using sodium hydroxide; after sodium carbonate is prepared into an aqueous solution with the concentration of 1mol/L, 50ml of the aqueous solution of the sodium carbonate is taken to be evenly mixed with 3.5ml of acetylacetone to prepare an acetylacetone solution for later use; weighing 1.6g of p-dimethylaminobenzaldehyde, and dissolving the p-dimethylaminobenzaldehyde in 30mL of concentrated hydrochloric acid and 30mL of absolute ethyl alcohol to prepare an Ellisib reagent; the composition prepared in example 1 was formulated into an aqueous solution having a mass concentration of 1% for use.
Taking 0.5mL of hyaluronidase solution and 0.1mL of 0.25mmol/L calcium chloride solution, and carrying out heat preservation culture at 37 ℃ for 20 min; adding 0.5mL of the composition water solution, and continuing to culture at 37 ℃ for 20 min; adding 0.5mL sodium hyaluronate solution, keeping the temperature at 37 ℃ for 30min, and standing at normal temperature for 5 min; adding 0.1mL of 0.4mol/L sodium hydroxide solution and 0.5mL of acetylacetone solution, heating in a boiling water bath for 15min, and immediately cooling with ice water for 5 min; 1.0mL of Ellisib reagent was added, and the mixture was diluted with 3.0mL of absolute ethanol, allowed to stand for 20min for color development, and the absorbance (A) was measured with a spectrophotometer. In the experiment, the A group of samples are scanned at the wavelength of 450-700nm to determine the maximum absorption wavelength, and then the deionized water is used as a reference to respectively measure the absorbance at the maximum absorption wavelength.
Hyaluronidase inhibition rate
Figure RE-DEST_PATH_IMAGE001
In the formula: a is the absorbance of the control solution (acetic acid buffer solution is used instead of the composition solution)
B is the absorbance of the control blank solution (acetic acid buffer solution is used to replace the composition solution and the enzyme solution)
C is the absorbance value of the composition solution
D is the absorbance of the composition blank solution (acetic acid buffer solution is used for replacing enzyme solution)
The experimental result shows that the inhibition rate of the composition water solution with the mass concentration of 1% on the hyaluronidase is 82.6%, and the experimental result shows that the anti-allergy repair composition prepared by the invention has better anti-allergy effect.
The following is an in vitro Red Blood Cell (RBC) hemolysis experiment performed by the present invention:
preparation of red blood cell suspension: phosphate Buffer (PBS) at pH 7.4 (1.8 g/L glucose was added) and citric acid (C) as anticoagulant were prepared in advance6H5Na3O7·2H2O0.02 g/ml, citric acid C6H8O70.008 g/ml) to treat fresh blood; subpackaging the collected blood sample by a centrifuge tube, centrifuging for 15min at 5000r/min, discarding the supernatant, adding PBS, gently shaking, mixing, centrifuging again, repeatedly washing until the supernatant is colorless and transparent, diluting the precipitate with PBS to 2% of red blood cell suspension, and storing in a refrigerator at 4 deg.C for later use.
Determination of appropriate experimental concentrations of Sodium Dodecyl Sulfate (SDS): 0.5ml of a solution of samples to be detected (SDS) with different concentrations, which is diluted by PBS in advance, and 0.5ml of a suspension of red blood cells with the mass concentration of 2 percent are respectively added into a centrifugal tube and fully and uniformly mixed. PBS was used as a negative control, and 100mg/L SDS solution was used as a positive control. After being placed in an incubator at 37 ℃ for incubation for 3h, the mixture is centrifuged at 2000r/min for 3min, and the supernatant is absorbed to measure the light absorption value at the wavelength of 530 nm. The hemolysis rate, hemolysis rate (%) = (test sample A) was calculated according to the formula530The sample to be tested A530Negative control A530) /(Positive control A)530Negative control A530) X 100%, the mass concentration of SDS at 70% hemolysis rate was selected as the experimental concentration.
The samples prepared in example 1 were tested for their hemolytic rate in erythrocytes after interaction with SDS at different mass concentrations: the composition prepared in example 1 was diluted with PBS to 1%, 3%, 5% solutions by mass concentration for use, 0.5ml of the composition sample to be tested with different mass concentrations was pre-mixed with 0.5ml of the red blood cell suspension with 2% mass concentration, 0.5ml of SDS solution with experimental concentration was added, after mixing well, the subsequent incubation and centrifugation were performed to calculate the hemolysis rate, table 1 is the hemolysis rate of red blood cells after the sample prepared in example 1 with different mass concentrations and SDS combined.
TABLE 1 haemolysis rates of erythrocytes for samples of different mass concentrations
Figure 66259DEST_PATH_IMAGE003
As can be seen from table 1, samples 2, 3 and 4 have certain inhibitory effects on SDS-induced RBC hemolysis, and as the sample concentration increases, the corresponding RBC hemolysis rate decreases, indicating that the anti-allergy restoration efficacy composition prepared by the present invention has irritation-reducing, anti-allergy-relieving effects.
The following are experiments on the skin barrier repair efficacy of human body carried out by the present invention:
60 female volunteers aged 20-40 years are selected according to the voluntary principle, and are all light and moderate sensitive skin, and no medicine or cosmetics which are irrelevant to the experiment are applied during the test period. Using randomized, single-blind, control testing, the subject's cheeks were randomized using a 1% strength by mass aqueous solution of the composition prepared according to example 1 of the present invention and a blank control, 1 time each in the morning and evening, for 28 days. The test is carried out before, 14 th and 28 th days, and before the test, the test part is cleaned by clean water and wiped dry to expose the test part, and the test part is required to sit still for 20min under the environment of constant temperature and humidity (room temperature 22 +/-2 ℃ and relative humidity 45% +/-5%).
TEWL values for the skin trans-epidermal water loss were measured on both cheeks of the subjects using a Tewameter TM300 trans-epidermal water loss tester before application of the spreading solution for 14 days and 28 days, and the test data are shown in table 2.
TABLE 2 TEWL values for the transepidermal water loss of skin using samples at various times
Figure 851681DEST_PATH_IMAGE004
As can be seen from the results in table 2, the moisture loss value of the cheek coated with the solution of the composition of the present invention through the epidermis was significantly reduced, while the other half of the cheek coated with the blank sample did not show significant changes, indicating that the composition of the present invention has good skin barrier repair efficacy.
The following is an experiment of synergistic effect of the composition of the present invention on soothing repair of human body:
the experiment uses the inner side of the arm to carry out a test, generates pruritus through lactic acid stimulation, then treats the pruritus part by using the anti-allergy repairing efficacy composition prepared by the invention, and verifies the itching relieving efficacy of the anti-allergy repairing efficacy composition prepared by the invention. 60 lactic acid stabbing pain patients of 20-40 years old were selected as volunteers, the groups were equally divided into 10 groups, samples 1-10 were prepared by the method of example 1, three pieces of skin were selected on the inner side of the arm of the volunteer for blind test, and the test was performed under constant temperature and humidity (room temperature 20 ℃, relative humidity 45%). Respectively applying 2 × 2cm nonwoven fabrics soaked with 5% lactic acid water solution for 5 min. After the non-woven fabric is removed, 2g of test samples are respectively smeared on the three skins, the skins are massaged until the skin is absorbed, the pain conditions of the patch positions are inquired (100 grades, 75-100 grades are severe pruritus, 50-75 grades are obvious pruritus, 25-50 grades are slight pruritus and 0-25 grades are no pruritus) when the skin is removed, smeared for 10min, 30min and 60min respectively, and the TEWL value test is carried out on the experimental positions (the average value is obtained by three tests).
TABLE 3 Patch test scratchiness data
Figure 728370DEST_PATH_IMAGE005
Sample 1: 1% aqueous solution of only 73% by mass of ceramide 3, one active composition;
sample 2: 1% aqueous solution of a composition containing 1% of Enteromorpha compressa extract and 73% of ceramide 3 in mass percentage;
sample 3: a 1% aqueous solution containing a composition of 1% onion bulb extract and 73% ceramide 3 by mass;
sample 4: 1% aqueous solution of a composition containing 1% by mass of a combination of two active ingredients, namely, a palmitoyl Potentilla chinensis root extract and 73% by mass of ceramide 3;
sample 5: a 1% aqueous solution containing a composition of 1% quince leaf extract and 73% ceramide 3 active ingredients by mass;
sample 6: a 1% aqueous solution of a composition containing 7% by mass of squalane and 73% by mass of ceramide 3;
sample 7: a 1% aqueous solution of a composition containing 0.5% by mass of an Enteromorpha compressa extract, 0.5% by mass of an onion bulb extract and 73% by mass of ceramide 3;
sample 8: a 1% aqueous solution containing a composition of four active substances, namely 0.3% of Enteromorpha compressa extract, 0.3% of onion bulb extract, 0.4% of quince leaf extract and 73% of ceramide 3 in percentage by mass;
sample 9: a 1% aqueous solution containing a composition of five active substances, namely 0.25% of an Enteromorpha compressa extract, 0.25% of an onion bulb extract, 0.25% of a quince leaf extract, 0.25% of a palmitoyl Potentilla chinensis root extract and 73% of ceramide 3 by mass fraction;
sample 10: 1% aqueous solution of six anti-allergy restoration efficacy compositions prepared in example 1;
a decrease in TEWL values objectively indicates that the skin barrier is repaired, which has an effect on the relief of skin itch. As can be seen from the data in Table 3, the anti-allergy restoration effect of the combination of 6 active substances is better than that of the combination of single active substances or parts of the combination of the active substances, which indicates that the Enteromorpha compressa extract, the onion bulb extract, the quince leaf extract, the palmitoyl Potentilla chinensis root extract, the squalane and the ceramide 3 adopted by the invention have synergistic effect in the anti-allergy restoration aspect.
In conclusion, the traditional Chinese medicine composition disclosed by the invention can be used for soothing and repairing sensitive skin through multi-way omnibearing action and synergistic interaction. The preparation method has the advantages of simple process, controllable conditions, high production efficiency, good stability and solubility of the obtained composition, mildness, no irritation, remarkable anti-allergy repair effect and the like.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples, but the scope of the present invention is not limited thereto.
Example 1: the anti-allergy repairing efficacy composition and the preparation method thereof adopt the following steps:
a: weighing 1% of Enteromorpha compressa extract, 1% of onion bulb extract, 1% of quince leaf extract, 1% of Potentilla palmifolia root extract, 10% of squalane, 70% of ceramide 3 powder, 4% of hydroxypropyl starch phosphate, 1.5% of polyglycerol-3 methyl glucose distearate and 10.5% of deionized water according to the following mass percentage;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 85 ℃ to obtain a water phase;
c: b, uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3 methyl glucose distearate weighed in the step A in a water bath environment at the temperature of 80 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 80 ℃, wherein the rotation speed of the homogenizer is 8000RPM, and the homogenization time is 30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, and controlling the stirring speed of the high-shear wet granulator to be 1000RPM, the speed of a cutting knife to be 4000RPM and the granulation time to be 30 min; then transferring the mixture into a vibrating fluidized bed for vacuum drying, and drying at 70 ℃ for 15min to prepare the composition with the particle size of 1.2mm and the anti-allergy repairing effect.
Example 2: the anti-allergy repairing efficacy composition and the preparation method thereof adopt the following steps:
a: respectively weighing 0.5% of Enteromorpha compressa extract, 0.5% of onion bulb extract, 0.5% of quince leaf extract, 0.5% of Potentilla palmifolia root extract, 8% of squalane, 65% of ceramide 3 powder, 4% of hydroxypropyl starch phosphate, 1% of polyglycerol-3 methyl glucose distearate and 20% of deionized water according to the following mass percentage;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 80 ℃ to obtain a water phase;
c: b, uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3 methyl glucose distearate weighed in the step A in a water bath environment at the temperature of 80 ℃ to obtain an oil phase; (ii) a
D: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 80 ℃, wherein the rotation speed of the homogenizer is 6000RPM, and the homogenization time is 30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, and controlling the stirring speed of the high-shear wet granulator to be 800RPM, the speed of a cutting knife to be 3000RPM and the granulation time to be 20 min; then transferring the mixture into a vibrating fluidized bed for vacuum drying, and drying for 15min at the temperature of 60 ℃ to prepare the composition with the particle size of 1.4mm and the anti-allergy repairing effect.
Example 3: the anti-allergy repairing efficacy composition and the preparation method thereof adopt the following steps:
a: respectively weighing 0.1% of Enteromorpha compressa extract, 0.2% of onion bulb extract, 0.4% of quince leaf extract, 0.3% of Potentilla palmifolia root extract, 10% of squalane, 70% of ceramide 3 powder, 4% of hydroxypropyl starch phosphate, 1% of polyglycerol-3 methyl glucose distearate and 14% of deionized water according to the following mass percentage;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 85 ℃ to obtain a water phase;
c: b, uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3 methyl glucose distearate weighed in the step A in a water bath environment at the temperature of 80 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 80 ℃, wherein the rotation speed of the homogenizer is 5000RPM, and the homogenization time is 30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, and controlling the stirring speed of the high-shear wet granulator to be 700RPM, the speed of a cutting knife to be 3000RPM and the granulation time to be 30 min; then transferring the mixture into a vibrating fluidized bed for vacuum drying, and drying for 15min at 65 ℃ to prepare the composition with the particle size of 1.5mm and the anti-allergy repairing effect.
Example 4: the anti-allergy repairing efficacy composition and the preparation method thereof adopt the following steps:
a: respectively weighing 0.2% of Enteromorpha compressa extract, 0.4% of onion bulb extract, 0.8% of quince leaf extract, 0.6% of Potentilla palmifolia root extract, 10% of squalane, 66% of ceramide 3 powder, 5% of hydroxypropyl starch phosphate, 1.2% of polyglycerol-3 methyl glucose distearate and 15.8% of deionized water according to the following mass percentage;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 80 ℃ to obtain a water phase;
c: b, uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3 methyl glucose distearate weighed in the step A in a water bath environment at the temperature of 80 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 80 ℃, wherein the rotation speed of the homogenizer is 8000RPM, and the homogenization time is 25min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, and controlling the stirring speed of the high-shear wet granulator to be 1000RPM, the speed of a cutting knife to be 3000RPM and the granulation time to be 25 min; then transferring the mixture into a vibrating fluidized bed for vacuum drying, and drying at 70 ℃ for 10min to prepare the composition with the particle size of 1.3mm and the anti-allergy repairing effect.
Example 5: the anti-allergy repairing efficacy composition and the preparation method thereof adopt the following steps:
a: weighing 1% of Enteromorpha compressa extract, 0.8% of onion bulb extract, 0.4% of quince leaf extract, 0.6% of Potentilla palmifolia root extract, 12% of squalane, 65% of ceramide 3 powder, 4.5% of hydroxypropyl starch phosphate, 1.5% of polyglycerol-3 methyl glucose distearate and 14.2% of deionized water according to the following mass percentage;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 85 ℃ to obtain a water phase;
c: b, uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3 methyl glucose distearate weighed in the step A in a water bath environment at the temperature of 80 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 80 ℃, wherein the rotation speed of the homogenizer is 6000RPM, and the homogenization time is 30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, and controlling the stirring speed of the high-shear wet granulator to be 600RPM, the speed of a cutting knife to be 4000RPM and the granulation time to be 30 min; then transferring the mixture into a vibrating fluidized bed for vacuum drying, and drying at 70 ℃ for 10min to prepare the composition with the particle size of 1.6mm and the anti-allergy repairing effect.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (2)

1. An anti-allergy repairing composition is characterized by comprising the following components: 0.1-1% of Enteromorpha compressa extract, 0.1-1% of onion bulb extract, 0.1-1% of quince leaf extract, 0.1-1% of Potentilla palmifolia root extract, 7-15% of squalane, 60-80% of ceramide 3 powder, 4-8% of hydroxypropyl starch phosphate and 1-3% of polyglycerol-3 methyl glucose distearate, wherein the percentages are mass percentages.
2. The method for preparing the anti-allergy restoration efficacy composition according to claim 1, characterized by comprising the following steps:
a: weighing 0.1-1% of Enteromorpha compressa extract, 0.1-1% of onion bulb extract, 0.1-1% of quince leaf extract, 0.1-1% of Potentilla palmifolia root extract, 7-15% of squalane, 60-80% of ceramide 3 powder, 4-8% of hydroxypropyl starch phosphate, 1-3% of polyglycerol-3 methyl glucose distearate and 10-20% of deionized water according to the following mass percentages;
b: uniformly mixing the Enteromorpha compressa extract, the onion bulb extract, the hydroxypropyl starch phosphate and the deionized water which are weighed in the step A under the water bath environment of 75-85 ℃ to be used as a water phase;
c: uniformly mixing the palmitoyl tormentum root extract, the quince leaf extract, squalane and polyglycerol-3-methylglucose distearate weighed in the step A in a water bath environment at the temperature of 75-85 ℃ to obtain an oil phase;
d: homogenizing the water phase obtained in the step B and the oil phase obtained in the step C by an emulsification homogenizer at the temperature of 75-80 ℃, wherein the rotation speed of the homogenizer is 3000-8000RPM, and the homogenization time is 10-30min, so as to obtain emulsion;
e: adding the emulsion obtained in the step D and the ceramide 3 powder weighed in the step A into a high-shear wet granulator to prepare compact particles, controlling the stirring speed of the high-shear wet granulator to be 300-4000 RPM (plus material plus; then transferring into a vibrating fluidized bed for vacuum drying, and drying at 50-70 deg.C for 5-15min to obtain the composition with anti-allergy repairing effect.
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