CN113350234A - Preparation method and application of allergy-relieving repair compound - Google Patents

Preparation method and application of allergy-relieving repair compound Download PDF

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CN113350234A
CN113350234A CN202110648429.1A CN202110648429A CN113350234A CN 113350234 A CN113350234 A CN 113350234A CN 202110648429 A CN202110648429 A CN 202110648429A CN 113350234 A CN113350234 A CN 113350234A
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extract
ethanol
leaf
allergy
extraction
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陈秀玉
王绍梅
秦涛
郭星星
詹柱
刘晓磊
丁冲冲
郑海兵
何沪宝
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Youyi Biotechnology Jiangsu Co ltd
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Abstract

The invention provides a preparation method and application of a allergy-relieving repair compound, and belongs to the technical field of cosmetics, wherein golden chamomile extract, gentian extract, grape skin extract, olive leaf extract, asiatic centella flower/leaf/stem extract, purslane flower/leaf/stem extract, poncirus trifoliata fruit extract and glucan are heated to 70-80 ℃ and stirred to be dissolved; the allergy-relieving repair compound is compounded by the following components in parts by weight: the feed additive comprises 15-25% of a chamomile extract, 10-15% of a gentian extract, 5-10% of a grape skin extract, 5-10% of an olive leaf extract, 5-10% of a centella asiatica flower/leaf/stem extract, 5-8% of a purslane flower/leaf/stem extract, 3-5% of a poncirus trifoliata fruit extract and 1-5% of glucan. The invention can effectively solve the problems that the effect of a single extract is poor and the effect cannot be fully exerted, and has better allergy-relieving repair effect on skin.

Description

Preparation method and application of allergy-relieving repair compound
Technical Field
The invention relates to the technical field of cosmetics, in particular to a allergy-relieving repair compound, and a preparation method and application thereof.
Background
In recent years, allergic patients have been increased sharply with changes in dietary structure, air pollution, and increase in life and work pressure. Statistics data of 2017 and 2018 of five skin disease diagnosis mechanisms determined by Ministry of health in China show that contact dermatitis is most common in six major cosmetic skin diseases, and the incidence rates of two years respectively account for 82.6 percent and 93.3 percent of the total incidence rate of the cosmetic skin diseases. Most cosmetics in the market contain a large amount of chemical additives, which easily cause skin sensitivity and even inflammation, and sensitive skin is very easy to have allergy when common cosmetics are used for sensitive skin. Increasingly, cosmetics with allergy-relieving, repairing and anti-irritation effects are being valued, and substances with allergy-relieving, repairing and anti-irritation activities, particularly plant-derived substances, are favored by scholars and markets.
Chinese patent CN110179709A, a compound liquid for moisturizing and soothing allergy, a preparation method and an application thereof, the method comprises the following steps: s1, preparing a tremella extract; s2, preparing a poncirus trifoliata fruit extract; s3, selecting a golden chamomile raw material, adding 5-10 times of 50% ethanol, adding a proper amount of sodium citrate to adjust the pH of an extracting solution to be about 8, extracting at normal temperature for 48 hours, and filtering by 1um filter paper to obtain a golden chamomile extract; s4, selecting a purslane raw material, adding 5-10 times of water, performing microwave extraction for 30-60 minutes, and filtering with 1um filter paper to obtain a purslane extracting solution; s5, and 4 plant extracts obtained from S1-S4, according to the raw material formula in claim 1, the plant extracts are compounded in proportion to obtain the moisturizing and allergy-relieving compound liquid. In the technical field of cosmetics, people are increasingly disliked to synthetic chemical reagents and are increasingly interested in natural raw materials, and the scheme provides a moisturizing and allergy-relieving compound liquid formed by mixing 4 plant extracts.
In the prior art, the problem of insufficient mixing among various liquids possibly occurs in the compounding process of a plurality of extracting solutions, and related mixing media are not used in the compounding process, so that the compounding solution cannot well combine the effects of the components, and the effects of the components cannot be fully exerted.
Disclosure of Invention
In order to overcome the problems of poor combination effect and incomplete exertion of effect of composite liquid in the prior art, the preparation method of the allergy-relieving repair composite is provided, and is characterized in that: heating a golden chamomile extract, a gentian extract, a grape skin extract, an olive leaf extract, a centella asiatica flower/leaf/stem extract, a purslane flower/leaf/stem extract, a poncirus trifoliata fruit extract and glucan to 70-80 ℃, and stirring for dissolving; the allergy-relieving repair compound is compounded by the following components in parts by weight: the feed additive comprises 15-25% of a chamomile extract, 10-15% of a gentian extract, 5-10% of a grape skin extract, 5-10% of an olive leaf extract, 5-10% of a centella asiatica flower/leaf/stem extract, 5-8% of a purslane flower/leaf/stem extract, 3-5% of a poncirus trifoliata fruit extract and 1-5% of glucan.
Application of a soothing and repairing compound in water, milk and cream is provided.
By adopting the technical scheme, the allergy-relieving effect of a single extract is enhanced through the common action of multiple plant extracts, and the plant extracts have the functions of clearing away heat and toxic materials, relieving pain, resisting inflammation, inhibiting bacteria and the like, and all the components are effectively combined by heating, stirring and dissolving the plant extracts.
Preferably, the golden chamomile extract is prepared by mixing golden chamomile and water at 50-65 ℃, carrying out ultrasonic-assisted extraction for 70-90 min at a feed liquid weight ratio of 1:15-25, then heating and boiling, and concentrating to a density of 1.01-1.20 g/mL.
By adopting the technical scheme, the golden chamomile is mixed with warm water, and the golden chamomile is fully dissolved in water by heating and boiling, and is concentrated to a certain density to obtain a refined extract.
Preferably, the gentiana scabra bunge extract is prepared by extracting gentiana scabra bunge and 50% -75% of ethanol as a solvent for 3 times, wherein the weight ratio of first feed liquid is 1: 8-10, the weight ratio of second feed liquid is 1: 5-8, the weight ratio of third feed liquid is 1: 5-8, the extraction temperature is 70-80 ℃, the extraction time is 4-6 hours, filtering is carried out, the aperture of a filter membrane or filter paper for three-time filtering is 3 microns, 1 micron and 0.45 micron in sequence, then the three-time filtrate is combined, ethanol is concentrated at 75-85 ℃, and vacuum drying is carried out to obtain the gentiana scabra bunge extract.
By adopting the technical scheme, the gentian is crushed and fully contacted with an ethanol solvent, extracted at high temperature for a plurality of times, soaked to enable the gentian to contain compounds such as picrorhizin, flavonoid, ketone, triterpenes, amino acids, gentianose, coumarins, lactone and the like, leached, and then concentrated at high temperature and dried in vacuum to obtain the high-purity extract.
Preferably, the grape skin extract is obtained by crushing grape skin, soaking and extracting with ethyl acetate as a solvent at a feed liquid weight ratio of 1: 10-25 at 20-35 ℃ for 2-3 d at a centrifugal rotation speed of 10000-12000 r/min for 10-12 min.
By adopting the technical scheme, the main components of the grape skin are grape skin anthocyanin and phenols, the physiological activity of the anthocyanin is good in removing hydroxyl free radical and superoxide free radical due to the grape skin anthocyanin, and the allergy-relieving and oxidation-resisting effects of the anthocyanin can be improved by extracting and adding the grape skin anthocyanin into the compound.
Preferably, the olive leaf extract is prepared by taking 75-85% ethanol as a solvent for olive leaves, wherein the weight ratio of feed liquid is 1:15-25, the extraction temperature is 70-85 ℃, the extraction time is 3-5 h, the olive leaves are extracted for 2 times in a water bath hot reflux extraction mode, the filtration is carried out, the ethanol is concentrated at 75-85 ℃, and AB-8 resin is separated and purified to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are 0.5-2 ml/min, 60-80% ethanol and 2-4 ml/min respectively.
By adopting the technical scheme, the olive leaves are added with ethanol in a large proportion, so that the olive leaves can be effectively sterilized and fully contacted, heating extraction is carried out, components in the olive leaves can be fully extracted, then the ethanol is concentrated, finally, the impurities are absorbed by macroporous resin, and the impurities are separated and purified by the macroporous resin to obtain the purified extract.
Preferably, the centella asiatica flower/leaf/stem extract is prepared by crushing centella asiatica, adding 60-75% of ethanol as a solvent, carrying out ultrasonic-assisted extraction at 45-55 ℃ for 1-2 hours with the feed liquid weight ratio of 1:15-25, concentrating the ethanol at 60-75 ℃, removing impurities by a chitosan flocculation method, wherein the addition amount of a flocculation solution is 0.3-0.8%, the flocculation temperature is 35-45 ℃, the flocculation time is 2-3 hours, separating and purifying D-4020 resin, and carrying out purification at a sample injection speed, an eluent concentration and an elution speed of 0.4-1 ml/min, 60-75% of ethanol and 4-8 ml/min respectively, and then purifying by macroporous resin to obtain the extract.
By adopting the technical scheme, the centella asiatica flower/leaf/stem extract is prepared by crushing, adding an ethanol solvent for dissolving, performing ultrasonic extraction and concentration, and finally adopting a chitosan flocculant to replace repeated extraction and chromatography, so that the purification steps are simplified, and finally, the finally purified extract is obtained by macroporous resin extraction.
Preferably, the purslane flower/leaf/stem extract is prepared by crushing purslane, adding 60-75% of ethanol as a solvent, wherein the weight ratio of feed liquid is 1:15-25, carrying out ultrasonic-assisted extraction for 30-60 min, heating and extracting for 2-4 h at the extraction temperature of 70-85 ℃, then concentrating off ethanol at the temperature of 60-75 ℃, and carrying out macroporous resin separation and purification to obtain the extract, wherein the sample injection speed, the eluent concentration and the elution speed are respectively 0.5-2 ml/min, 60-80% of ethanol and 1-4 ml/min.
By adopting the technical scheme, a large proportion of ethanol is added into the purslane, so that the purslane can be effectively sterilized and fully contacted with the purslane, damage to the purslane during extraction can be reduced by utilizing ultrasonic-assisted extraction, loss of components is prevented, the components in the purslane can be fully extracted during heating extraction, then the ethanol is concentrated, finally, impurities are adsorbed by adopting macroporous resin, and the impurities are separated and purified by adopting the macroporous resin, so that the purified extract is obtained.
Preferably, the poncirus trifoliata fruit extract is prepared by crushing poncirus trifoliata fruits, taking 75-85% ethanol as a solvent, heating and soaking the materials at the weight ratio of 1: 10-15 at the extraction temperature of 75-85 ℃ for 4-6 h, filtering, and concentrating at the temperature of 75-85 ℃ to the density of 1.01-1.20 g/mL to obtain the poncirus trifoliata fruit extract.
By adopting the technical scheme, the high-purity extract is obtained by crushing, fully contacting with an ethanol solvent, extracting at a high temperature for a plurality of times, soaking to fully separate out the components in the poncirus trifoliata fruits and concentrating at a high temperature.
In summary, compared with the prior art, the invention has the following advantages and effects: the chemical components of the golden yellow chamomile comprise coumarins, flavonoids, volatile oil, polysaccharides, terpenoids, guaianolides, sterols, organic acids and other components, and have biological activities of resisting inflammation, inhibiting bacteria, relieving spasm, tranquilizing, resisting oxidation, resisting cancer and the like on the skin. Radix Gentianae has effects of clearing heat, eliminating dampness, and purging liver and gallbladder fire. The effective components of radix Gentianae mainly comprise secoiridoid glycosides, such as gentiopicroside, swertiamarin, gentiopicroside, swertiamarin, and tetraacetylgentiamarin. Has obvious effects of resisting inflammation, resisting bacteria, calming and the like on the skin. The grape skin mainly contains anthocyan, resveratrol and flavonoid, and has effects of resisting oxidation, resisting bacteria, relieving inflammation, tranquilizing, improving blood vessel function, prolonging life and delaying aging. The olive leaf has pharmacological activities of resisting bacteria and inflammation, improving immunity, resisting oxidation, repairing articular cartilage, etc. The olive leaves are rich in functional components, such as essential oil, flavonoid, polysaccharide, polyphenol, mineral elements, terpenoids, amino acid and the like, wherein the polyphenol is the most important and highest-content functional component of the olive leaves. The active ingredients in centella asiatica mainly comprise saponins and sapogenins, including asiaticoside, madecassoside, asiatic acid, madecassic acid and the like, and modern medical researches show that the centella asiatica has physiological effects of resisting depression, promoting wound healing, treating scars, resisting tumors, gastric ulcer, bacteria, oxidation and the like. Herba Portulacae has effects of clearing away heat and toxic materials, cooling blood, stopping bleeding, and relieving dysentery. Modern medical research also shows that the purslane mainly contains chemical components such as alkaloids, terpenes, coumarins, flavonoids, organic acids, volatile oil, polysaccharide and the like, and has obvious effects of resisting inflammation and relieving pain of the skin. The main components of fructus Ponciri Trifoliatae include flavone, volatile oil and small amount of alkaloid compounds, and have antioxidant, antiinflammatory and tranquilizing effects on skin. Beta-glucan is a new product developed by a unique process and is derived from strain fermentation. It is a polysaccharide, and has good effects of resisting oxidation and aging, assisting the accelerated recovery of damaged tissues and the like. The invention combines different plant extraction technologies, and enhances the efficacy of the product in the aspect of allergy relief and repair by compounding various plant extracts on the basis of the efficacy of a single extract. Compared with the product obtained by chemical synthesis, the plant extract is safer and has no irritation.
Drawings
FIG. 1 shows the inhibition of hyaluronidase activity by each of the extracts and examples;
FIG. 2 repair of skin in example 1;
FIG. 3 repair of skin by example 2;
FIG. 4 repair of skin in example 3;
FIG. 5 example 4 repair of skin;
FIG. 6 patch test results for example 1 against a common allergen;
FIG. 7 results of patch test on common sensitizers in example 2;
FIG. 8 results of patch test on common sensitizers in example 3;
FIG. 9 results of patch test on common sensitizers in example 4.
Detailed Description
The present invention will be described in further detail with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1. The extraction temperature of golden yellow chamomile is 65 ℃, the feed liquid weight ratio is 1:22, the ultrasonic-assisted extraction time is 75min, then the golden yellow chamomile is heated and boiled, the golden yellow chamomile is concentrated to the density of 1.10g/mL (60 ℃), double-layer gauze is used for filtering to obtain filtrate, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
2. Extracting radix Gentianae with 50% ethanol as solvent for 3 times, the weight ratio of the first material liquid to the second material liquid is 1:10, the weight ratio of the third material liquid to the second material liquid is 1:8, the extraction temperature is 70 deg.C, the extraction time is 4 hr, filtering, mixing the three filtrates, concentrating at 80 deg.C to remove ethanol, and vacuum drying to obtain radix Gentianae extract.
3. The grape skin extraction adopts ethyl acetate as solvent, the weight ratio of the material liquid is 1:20, the extraction temperature is 30 ℃, the extraction time is 2d, the centrifugal rotation speed is 10000r/min, the centrifugal time is 10min, the supernatant is taken and filtered by a 0.22 mu m microporous membrane, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
4. The olive leaf extract is prepared by using 80% ethanol as a solvent, wherein the weight ratio of the material liquid is 1:20, the extraction temperature is 70 ℃, the extraction time is 3h, extracting for 2 times in a water bath hot reflux extraction mode, filtering, concentrating to remove ethanol at 75 ℃, and separating and purifying AB-8 resin to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are respectively 0.5ml/min, 60% ethanol and 2 ml/min.
5. The solvent used for extracting the centella asiatica is 70% ethanol, the weight ratio of the feed liquid is 1:20, the ultrasonic-assisted extraction temperature is 50 ℃, the ultrasonic time is 1h, ethanol is concentrated at 70 ℃, the ethanol is filtered by a 1um filter paper plate, and the impurity removal conditions of the chitosan flocculation method are as follows: the addition amount of the flocculation liquid is 0.8 percent, the flocculation temperature is 40 ℃, and the flocculation time is 2 hours. Separating and purifying with D-4020 resin at a sample injection rate of 0.8ml/min, an eluent concentration of 6ml/min, and adding butanediol to obtain solution with a ratio of 1: 1.
6. The solvent used for extracting purslane is 65% ethanol, the weight ratio of feed liquid is 1:20, the ultrasonic auxiliary extraction time is 40min, then the heating extraction is carried out for 2h, the extraction temperature is 75 ℃, the ethanol is concentrated at 70 ℃, the filtration is carried out by a 1um filter paper plate, the separation and purification are carried out by macroporous resin, and the sample injection speed, the eluent concentration and the elution speed are respectively 1ml/min, 60% ethanol and 1.8 ml/min. Adding butanediol to prepare a solution with the ratio of liquid to butanediol being 1: 1.
7. The method comprises extracting fructus Ponciri Trifoliatae with ethanol at 80% concentration and 1:15 weight ratio at 85 deg.C for 4 hr, concentrating at 75 deg.C to density of 1.10g/mL, filtering with 1um filter paper plate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
8. Adding 15% of the golden chamomile extract in the step 1, 10% of the gentian extract in the step 2, 5% of the grape skin extract in the step 3, 5% of the olive leaf extract in the step 4, 5% of the centella asiatica extract in the step 5, 5% of the purslane extract in the step 6, 3% of the poncirus trifoliata extract in the step 7 and 1% of glucan according to the following proportion, preparing a solution with the liquid-butanediol ratio of 1:1, heating and stirring at 75 ℃ to dissolve, and finally obtaining the needed anti-allergic repair compound.
Example 2
1. The method comprises extracting flos Chrysanthemi with ultrasonic at 50 deg.C for 70min at a feed liquid weight ratio of 1:15, boiling, concentrating to density of 1.08g/mL (60 deg.C), filtering with double-layer gauze to obtain filtrate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
2. Extracting radix Gentianae with 70% ethanol as solvent for 3 times, the weight ratio of the first material liquid to the second material liquid is 1:8, the weight ratio of the third material liquid to the second material liquid is 1:5, the extraction temperature is 80 deg.C, the extraction time is 5 hr, filtering, mixing the three filtrates, concentrating at 80 deg.C to remove ethanol, and vacuum drying to obtain radix Gentianae extract.
3. The grape skin extraction adopts ethyl acetate as solvent, the weight ratio of the material liquid is 1:10, the extraction temperature is 20 ℃, the extraction time is 2d, the centrifugal rotation speed is 10000r/min, the centrifugal time is 10min, the supernatant is taken and filtered by a 0.22 mu m microporous membrane, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
4. The olive leaf extract is prepared by using 80% ethanol as a solvent, wherein the weight ratio of the material liquid is 1:15, the extraction temperature is 70 ℃, the extraction time is 4h, extracting for 2 times in a water bath hot reflux extraction mode, filtering, concentrating to remove ethanol at 75 ℃, and separating and purifying AB-8 resin to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are respectively 1ml/min, 70% ethanol and 3 ml/min.
5. The solvent used for extracting the centella asiatica is 75% ethanol, the weight ratio of the feed liquid is 1:25, the ultrasonic-assisted extraction temperature is 55 ℃, the ultrasonic time is 2 hours, the ethanol is concentrated at 75 ℃, the ethanol is filtered by a 1um filter paper plate, and the impurity removal conditions by a chitosan flocculation method are as follows: the addition amount of the flocculation liquid is 0.6 percent, the flocculation temperature is 45 ℃, and the flocculation time is 3 hours. Separating and purifying with D-4020 resin at a sample injection rate, eluent concentration and elution rate of 1ml/min, 65% ethanol at 7ml/min, and adding butanediol to obtain solution with liquid-butanediol ratio of 1: 1.
6. The solvent used for extracting purslane is 75% ethanol, the weight ratio of feed liquid is 1:20, the ultrasonic auxiliary extraction time is 50min, then the heating extraction is carried out for 2.5h, the extraction temperature is 80 ℃, the ethanol is concentrated at 70 ℃, the filtration is carried out by a 1um filter paper plate, the separation and purification are carried out by macroporous resin, and the sample injection speed, the eluent concentration and the elution speed are respectively 2ml/min, 65% ethanol and 2 ml/min. Adding butanediol to prepare a solution with the ratio of liquid to butanediol being 1: 1.
7. The method comprises extracting fructus Ponciri Trifoliatae with ethanol at 75% concentration, material liquid weight ratio of 1:10, extraction temperature of 75 deg.C, extraction time of 4h, concentrating at 75 deg.C to density of 1.10g/mL, filtering with 1um filter paper plate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
8. Adding 25% of the golden chamomile extract in the step 1, 10% of the gentian extract in the step 2, 10% of the grape skin extract in the step 3, 5% of the olive leaf extract in the step 4, 10% of the centella asiatica extract in the step 5, 5% of the purslane extract in the step 6, 5% of the trifoliate orange extract in the step 7 and 3% of glucan according to the following proportion to prepare a solution with the liquid-butanediol ratio of 1:1, and heating and stirring the solution at 75 ℃ to dissolve the solution to obtain the needed allergy-relieving compound.
Example 3
1. The extraction temperature of golden yellow chamomile is 65 ℃, the feed liquid weight ratio is 1:25, the ultrasonic-assisted extraction time is 90min, then the golden yellow chamomile is heated and boiled, the golden yellow chamomile is concentrated to the density of 1.10g/mL (60 ℃), double-layer gauze is used for filtering to obtain filtrate, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
2. Extracting radix Gentianae with 75% ethanol as solvent for 3 times, the weight ratio of the first material liquid to the second material liquid is 1:10, the weight ratio of the second material liquid to the third material liquid is 1:8, the extraction temperature is 80 deg.C, the extraction time is 4 hr, filtering, mixing the three filtrates, concentrating at 80 deg.C to remove ethanol, and vacuum drying to obtain radix Gentianae extract.
3. The grape skin extraction adopts ethyl acetate as solvent, the weight ratio of the material liquid is 1:18, the extraction temperature is 35 ℃, the extraction time is 3d, the centrifugal rotation speed is 10000r/min, the centrifugal time is 10min, the supernatant is taken and filtered by a 0.22 mu m microporous membrane, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
4. The olive leaf extract is prepared by using 80% ethanol as a solvent, wherein the weight ratio of the material liquid is 1:20, the extraction temperature is 85 ℃, the extraction time is 3h, extracting for 2 times in a water bath hot reflux extraction mode, filtering, concentrating to remove ethanol at 80 ℃, and separating and purifying AB-8 resin to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are respectively 2ml/min, 70% ethanol and 2 ml/min.
5. The solvent used for extracting the centella asiatica is 70% ethanol, the weight ratio of the feed liquid is 1:20, the ultrasonic-assisted extraction temperature is 50 ℃, the ultrasonic time is 1h, the ethanol is concentrated at 75 ℃, the ethanol is filtered by a 1um filter paper plate, and the impurity removal conditions of the chitosan flocculation method are as follows: the addition amount of the flocculation liquid is 0.4 percent, the flocculation temperature is 38 ℃, and the flocculation time is 2 hours. Separating and purifying with D-4020 resin at a sample injection rate of 0.8ml/min, eluent concentration and elution rate of 6ml/min with 60% ethanol, and adding butanediol to obtain solution with liquid-butanediol ratio of 1: 1.
6. The solvent used for extracting purslane is 60% ethanol, the weight ratio of feed liquid is 1:15, the ultrasonic assisted extraction time at room temperature is 30min, then the heating extraction is carried out for 2h, the extraction temperature is 70 ℃, the ethanol is concentrated at 65 ℃, the filtration is carried out by a 1um filter paper plate, the separation and purification are carried out by macroporous resin, and the sample injection speed, the eluent concentration and the elution speed are respectively 0.5ml/min, 60% ethanol and 1 ml/min. Adding butanediol to prepare a solution with the ratio of liquid to butanediol being 1: 1.
7. The method comprises extracting fructus Ponciri Trifoliatae with ethanol at 80% concentration and 1:15 weight ratio at 75 deg.C for 4 hr, concentrating at 75 deg.C to density of 1.10g/mL, filtering with 1um filter paper plate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
8. Adding 20% of the golden chamomile extract in the step 1, 15% of the gentian extract in the step 2, 5% of the grape skin extract in the step 3, 8% of the olive leaf extract in the step 4, 6% of the centella asiatica extract in the step 5, 8% of the purslane extract in the step 6, 3% of the poncirus trifoliata extract in the step 7 and 5% of glucan according to the following proportion, preparing a solution with the liquid-butanediol ratio of 1:1, heating and stirring at 75 ℃ to dissolve the solution, and finally obtaining the needed anti-allergic repair compound.
Example 4
1. The method comprises extracting flos Chrysanthemi with ultrasonic at 60 deg.C for 80min at a feed liquid weight ratio of 1:18, boiling, concentrating to density of 1.10g/mL (60 deg.C), filtering with double-layer gauze to obtain filtrate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
2. Extracting radix Gentianae with 60% ethanol as solvent for 3 times, the weight ratio of the first material liquid to the second material liquid is 1:8, the weight ratio of the third material liquid to the second material liquid is 1:5, the extraction temperature is 85 deg.C, the extraction time is 6 hr, filtering, mixing the three filtrates, concentrating at 80 deg.C to remove ethanol, and vacuum drying to obtain radix Gentianae extract.
3. The grape skin extraction adopts ethyl acetate as solvent, the weight ratio of the material liquid is 1:15, the extraction temperature is 30 ℃, the extraction time is 2d, the centrifugal rotation speed is 10000r/min, the centrifugal time is 10min, the supernatant is taken and filtered by a 0.22 mu m microporous membrane, and butanediol is added to prepare a solution with the liquid to butanediol ratio of 1: 1.
4. The olive leaf extract is prepared by using 85% ethanol as a solvent, wherein the weight ratio of the material liquid is 1:15, the extraction temperature is 75 ℃, the extraction time is 5h, extracting for 2 times in a water bath hot reflux extraction mode, filtering, concentrating to remove ethanol at 80 ℃, and separating and purifying AB-8 resin to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are respectively 1ml/min, 70% ethanol and 3 ml/min.
5. The solvent used for extracting the centella asiatica is 65% ethanol, the weight ratio of the feed liquid is 1:15, the ultrasonic-assisted extraction temperature is 45 ℃, the ultrasonic time is 1h, the ethanol is concentrated at 60 ℃, the ethanol is filtered by a 1um filter paper plate, and the impurity removal conditions of the chitosan flocculation method are as follows: the addition amount of the flocculation liquid is 0.3 percent, the flocculation temperature is 35 ℃, and the flocculation time is 2 hours. Separating and purifying with D-4020 resin at a sample injection rate, eluent concentration and elution rate of 0.4ml/min and 60% ethanol at a sample injection rate of 4ml/min, and adding butanediol to obtain solution with a ratio of 1: 1.
6. The solvent used for extracting purslane is 70% ethanol, the weight ratio of feed liquid is 1:25, the ultrasonic auxiliary extraction time is 60min, then the heating extraction is carried out for 4h, the extraction temperature is 85 ℃, the ethanol is concentrated at 75 ℃, the filtration is carried out by a 1um filter paper plate, the separation and purification are carried out by macroporous resin, and the sample injection speed, the eluent concentration and the elution speed are respectively 1.8ml/min, 70% ethanol and 3.5 ml/min. Adding butanediol to prepare a solution with the ratio of liquid to butanediol being 1: 1.
7. The method comprises extracting fructus Ponciri Trifoliatae with ethanol at 80% concentration and 1:10 weight ratio at 80 deg.C for 6 hr, concentrating at 75 deg.C to density of 1.10g/mL, filtering with 1um filter paper plate, and adding butanediol to obtain solution with liquid to butanediol ratio of 1: 1.
8. Adding 25% of the golden chamomile extract in the step 1, 10% of the gentian extract in the step 2, 8% of the grape skin extract in the step 3, 10% of the olive leaf extract in the step 4, 10% of the centella asiatica extract in the step 5, 5% of the purslane extract in the step 6, 5% of the trifoliate orange extract in the step 7 and 3% of glucan according to the following proportion to prepare a solution with the liquid-butanediol ratio of 1:1, and heating and stirring the solution at 75 ℃ to dissolve the solution to obtain the needed allergy-relieving compound.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Effect embodiment:
firstly, detecting the allergy-relieving repair effect:
hyaluronidase Activity inhibition assay
The test principle is as follows: when the allergen invades the organism for the first time, the organism generates antibody IgE, and when the allergen invades the organism again, the antibody is combined with IgE on the surface of a sensitized cell to generate FceRI cross-linking, so that an activation signal is started to trigger signal conduction, and a plurality of enzymes including intracellular hyaluronidase are activated, and the process is called as anaphylactic reaction. Hyaluronic acid is a component in the tissue matrix that limits the diffusion of water and other extracellular substances, and after being hydrolyzed by hyaluronidase, cells become non-viscous, causing degranulation of cells and the exudation of new synthesized mediators, exerting a biological effect, resulting in the occurrence of immediate type hypersensitivity. The hyaluronidase is a participant of anaphylactic reaction, and researches show that the hyaluronidase is closely related to inflammation and allergy, and the inhibition of the activity of the hyaluronidase can prevent the hyaluronic acid from being decomposed and maintain normal physiological functions, thereby achieving the effect of allergy relieving and repairing.
1) Solution preparation
Hyaluronidase solution: 0.01g hyaluronidase was accurately weighed and added to 4mL acetic acid buffer to a final concentration of 1250. mu.g/mL.
0.5mg/mL sodium hyaluronate solution: accurately weighing 0.005g of sodium hyaluronate, adding the sodium hyaluronate into 10mL of acetic acid buffer solution, and fully dissolving for later use.
Acetic acid buffer solution (pH 5.6): diluting 1155 mu L of glacial acetic acid in a volumetric flask to 100mL, and uniformly mixing to obtain 4.8mL of solution A; taking 2.72g of sodium acetate crystal, dissolving and fixing the volume to 100mL, uniformly mixing, and measuring 45.2mL to obtain a solution B; a, B solution is mixed, deionized water is added to 100mL volume and mixed. The pH was measured precisely and adjusted to 5.6 with solution A or B.
An ellichi reagent: accurately weighing 0.8g of p-dimethylaminobenzaldehyde, and dissolving the p-dimethylaminobenzaldehyde in 15mL of concentrated hydrochloric acid and 15mL of absolute ethyl alcohol for later use.
Acetylacetone solution: exactly 3.5mL of acetylacetone was dissolved in 50mL of a 1.0mol/L sodium carbonate solution. The acetylacetone solution needs to be prepared as before.
Test sample solution: respectively taking 10mL of the compound extracted from each plant in the product for later use, and taking 10mL of the final product for later use.
2) Procedure of experiment
Adding 0.1mL of 0.25mmol/L CaCl2 solution and 0.5mL of hyaluronidase solution into a test tube, and performing heat preservation culture at 37 ℃ for 20 min; adding 0.5mL of sample solution, and carrying out heat preservation culture at 37 ℃ for 20 min; adding 0.5mL of sodium hyaluronate solution, and keeping the temperature at 37 ℃ for 30 min; then standing for 5min at normal temperature, adding 0.1mL of 0.4mol/L NaOH solution and 0.5mL of acetylacetone solution, heating in a boiling water bath for reaction for 15min, and immediately carrying out ice bath for 5 min; then adding 1.0mL of Ellisib reagent, diluting with 3.0mL of absolute ethyl alcohol, standing for 20min, developing, measuring the absorbance value, and substituting into the following formula to calculate the inhibition rate.
Figure BDA0003110802870000111
In the formula: a is the absorbance value of the control solution (the sample solution is replaced by acetic acid buffer solution);
b is the absorbance value of the blank control solution (acetic acid buffer solution is used for replacing the sample solution and the enzyme solution);
c is the absorbance value of the tested sample solution;
d is the absorbance value of the sample blank solution (the enzyme solution is replaced by acetic acid buffer solution).
During the experiment, the group A samples are subjected to wavelength scanning within the wavelength range of 450-700nm to determine the maximum absorption wavelength, deionized water is used as a reference, and ABS values of other samples are respectively measured under the maximum absorption wavelength.
The inhibition rate of each extract and example of the present invention on hyaluronidase activity is shown in fig. 1.
In table 1, 1% dipotassium glycyrrhizinate is used as a control, the inhibition rate of dipotassium glycyrrhizinate on hyaluronidase reaches 94.8%,
the hyaluronidase inhibition rates of examples 1, 2, 3 and 4 reach 95.6%, 95.1%, 97.1% and 96.8%, respectively. Compared with dipotassium glycyrrhizinate, the product has good allergy-relieving and repairing effects and higher safety.
Skin irritation repair test
The test principle is as follows: when skin is stimulated, the TEWL can be increased and the water content of the skin can be reduced due to the increase of local blood flow, the increase of local temperature, the increase of sweat gland secretion and the acceleration of metabolism, so that the characteristic changes of physiological function parameters of the TEWL, the moisture of epidermis, the erythema quantity on the surface of the skin and the like of sensitive skin can be generated. The test is aimed at comparing the rate of skin self-healing with the rate of skin healing after addition of the product.
Generally, the left and right internal arm tests of a subject are selected as tested parts, and a square area with the specification of 2cm multiplied by 2cm is circularly marked; washing a tested area (the same area) with clear water, standing the tested area for 10min, measuring a blank value of a skin red value, and then entering a smearing experiment stage; stimulating the tested area with 50% capsaicin water solution (about 0.01 mL); continuously stimulating for 15min and 30min, and collecting numerical values; smearing a test sample on a tested area, and performing data acquisition after about 0.1mL, 15min, 30min and 45 min; smearing 0.05mL of pure water on the blank control; counting the value measured at each time of the experimental part of the subject, and analyzing the change of the red value. The change of the skin red value is reflected in the change rule of the skin redness of the experimental area along with the time in the testing period. The greater the value, the greater the degree of redness of the skin. Skin red change rate (%) - (T-T blank)/T blank × 100%.
Example 1 the skin repair effect is shown in figure 2.
Example 2 the skin repair effect is shown in figure 3.
Example 3 the skin repair effect is shown in figure 4.
Example 4 the skin repair effect is shown in figure 5.
In FIGS. 2 to 5, the rate of change of red color after application of purified water from the blank control showed a decrease, indicating that the skin had self-healing ability.
Examples 1-4 compare with the blank, and respond that the product has obvious repairing effect on the skin after being stimulated.
Skin irritation test
The test principle is as follows: when skin is stimulated by certain specific antigens, abnormal and specific immune responses, mainly physiological disorders or tissue cell damage, also called allergies, occur. The main pathological changes of skin allergy are increased permeability, skin capillary vessel dilatation, tissue degeneration and necrosis and the like, and the skin can have symptoms of pruritus, redness, swelling, desquamation and the like.
The test subjects performed a skin patch test (patch test) on the forearm using Finn Chamber. However, patients with psoriasis (psoriasis), eczema (rash) or other skin lesions who are pregnant, lactating or taking contraceptives, antihistamines etc. cannot participate in this study. After wiping the test site with 70% ethanol and drying, 25-30. mu.L of the sample was added to the Finnish chamber, which was fixed to the arm area without water. Removing the patch after 24 h; marking the test part by using a marking pen, observing the test part again after 24 hours after 30min, and recording the information of the tester in detail. The degree of irritation is classified according to the standard of ((International Contact Dermatitis Research Group: ICDRG)), and is determined after 30min after the patch is removed, and is determined again after 24h, and after the judgment according to the judgment standard of the International Contact Dermatitis Research institute of skin reaction (Table 1), the average score is estimated according to the skin reaction average score formula [ Table 2], and whether the skin patch test (patch test) stimulates is determined according to the score result.
TABLE 1 International Research Group of Contact Dermatitis ((ICDRG)
And (3) judging standard:
Figure BDA0003110802870000131
Figure DA00031108028753026169
the standard for judging skin reaction
1) Negative (-): has no irritation
2) Double or slice interaction and erythrema (+ -); micro-stimulation
Faint barely visible mild erythema
3) Erythema + Industration (+); mild stimulation
Has obvious erythema and skin sclerosis
4) Erythema + Industration + Vesicle (++); middle stimulation
Erythema, sclerosis, blisters
5) Erythema + Industration + Bullae (++); strong stimulation
Erythema, sclerosis, and blisters
Equation for calculating average skin reaction score Mean score
Figure BDA0003110802870000141
i-results of respective scores obtained by removing the patch and measuring the sites 24 hours after 30min according to the ICDRG standard. The two reactions labeled erythena and edema, all apply.
j is the number of skin reaction testers after 30min and 24h after removing the patch, and marks both the erythema and edema reactions, and all the applications are applicable.
TABLE 2 skin Patch test results
Determination (Grade) MeanScore
Without irritation (1) 0.00~0.75
Micro-stimulation (2) 0.76~1.50
Light stimulus (3) 1.51~2.50
Middle stimulus (4) 2.51~4.00
Strong stimulation (5) 4.01
TABLE 1 skin condition 30min after patch removal
Figure BDA0003110802870000142
Figure BDA0003110802870000151
TABLE 2 skin condition 24h after patch removal
Figure BDA0003110802870000152
The patch tests in tables 1 and 2 reflect that the product has no irritation to skin and shows the safety of plant extracts.
Patch test for irritants
After the product is applied, the patch test of the stimulant is carried out according to the test (3).
Example 1 the patch test results for a common sensitiser are shown in figure 6.
Example 2 the patch test results for a common sensitiser are shown in figure 7.
Example 3 the patch test results for a common sensitiser are shown in figure 8.
Example 4 the patch test results for a common sensitiser are shown in figure 9.
After the product is smeared, a patch test of an irritant is carried out, and the damage of the irritant to the skin can be greatly relieved in a smearing area, which is far less than the sensitization rate of a blank control, so that the product can protect the structural integrity and the barrier function of an epidermal cell membrane to a certain extent, improve the tolerance of the skin, repair the damaged skin and relieve the allergic symptoms.
DPPH radical scavenging test
The experimental principle is as follows: free radicals are radicals containing an unpaired electron, and the formation of an allergic condition, as well as the onset of an allergy, are associated with an excessive accumulation of free radicals in the body. Active oxygen radicals in the body have certain functions, such as immunity and signaling processes. However, excessive reactive oxygen radicals will have destructive action, resulting in damage to normal cells and tissues of the human body and thus causing allergic symptoms in the human body. The excellent anti-allergy cosmetic not only can efficiently remove free radicals, but also can protect cell membranes from being damaged by the free radicals, and can inhibit the release of a sensitizing factor, namely histamine, and can penetrate into cells to fundamentally block the occurrence of anaphylactic reaction.
Preparation of reagents:
3.943mg DPPH is made to 50mL with 95% ethanol
② about 10mg of Trolox is fixed to 100mL by 95 percent ethanol
EXAMPLE 1, EXAMPLE 2, EXAMPLE 3, EXAMPLE 4
The test steps are as follows:
UV zeroing with 95% ethanol as blank
② preliminary experiments (DPPH concentration selection)
Shaking 500 μ L DPPH +1000 μ L95% ethanol for 10s, standing for 10min, and measuring absorbance (absorbance at 520 nm of 0.45-0.55, can be used as DPPH solution for the following experiment)
③ measurement of Trolox
Sample Trolox(μL) 95% ethanol (μ L) DPPH(μL)
S 100 900 500
SB 100 900+500 0
C 0 100+900 500
CB 0 100+900+500 0
Adding DPPH or 95% ethanol, shaking for 10s, standing for 10min, and measuring absorbance
Experiment of
S (sample + 95% ethanol) 1000. mu.L in total), DPPH 500. mu.L
SB (sample + 95% ethanol) 1000. mu.L total) + 95% ethanol 500. mu.L
C (sample solvent + 95% ethanol) 1000. mu.L total) + DPPH 500. mu.L
CB (sample solvent + 95% ethanol) 1000. mu.L) + 95% ethanol 500. mu.L
Adding DPPH or 95% ethanol, shaking for 10s, standing for 10min, and measuring absorbance
Calculating the formula: inhibition rate (%) [1- (S-SB)/(C-CB) ]. 100
Figure DA00031108028753123978
Figure BDA0003110802870000171
Figure BDA0003110802870000181
The product can eliminate certain excessive free radicals, thereby weakening the damage of the free radicals to cell membranes of mast cells and basophils, reducing the release amount of histamine, and playing the effects of relieving allergy, repairing and relieving itching.
And (3) detection of whitening effect:
tyrosinase activity inhibition assay
The experimental principle is as follows: tyrosine generates dopa through tyrosinase catalysis, dopa forms dopaquinone after dopa dehydrogenation, the maximum absorption wavelength of the dopaquinone is 475nm, and the concentration of the generated dopaquinone can be reflected by measuring the absorbance of the wavelength of 475 nm. When tyrosinase and whitening active ingredients exist simultaneously, the catalytic activity of the tyrosinase can be inhibited to a certain degree, so that the generation of dopaquinone is reduced. According to the comparison of the front and back absorbances, the inhibition degree of the whitening active ingredients on the tyrosinase activity can be judged, and then the whitening effect of the whitening ingredients in vitro can be evaluated.
Materials: buffer solution: k2HPO4(8.71g/500mL) + KH2PO4(6.805g/mL) (pH 6.80 ═ pH
± 0.02); substrate: about 0.3mg/mL L-tyrosine; a spectrophotometer: uv (475nm)
The experimental method comprises the following steps: taking a small amount of enzyme, and dissolving the enzyme by using a buffer solution; adding 500. mu.L of (L-tyrosine (0.3mg/ml), 500. mu.L of buffer solution, 450. mu.L of water and 50. mu.L of enzyme) into a 1.5ml centrifuge tube; before adding enzyme, at 37 deg.C for 20 min; after the enzyme addition, the absorbance at the wavelength of 475nm of the spectrophotometer was measured 10min at 37 ℃. The enzyme concentration was adjusted to give an Absorbance (ABS) of between 0.45 and 0.55. The enzyme solution at this concentration was used as an experimental enzyme solution.
Figure BDA0003110802870000191
Tyrosinase inhibition (%) [1- (a-B)/(C-D) ]. 100
The results of the tyrosinase inhibition assay are as follows
Examples Inhibition rate
Example 1 56.74%
Example 2 55.55%
Example 3 67.76%
Example 4 60.03%
The product has certain whitening effect besides the allergy-relieving and repairing effects.
And (3) detecting the moisturizing effect:
test of hydration rate of stratum corneum
The worldwide recognized Cornemeter method-capacitance method was used: based on the fact that the dielectric constant (< 7) of water (81) and other substances varies considerably, a measuring capacitor of an appropriate shape varies with the change in the capacitance of the skin, which is within the measurement range, according to the water content, so that the moisture content of the skin can be measured. The capacitance measuring method is superior to other methods in that the test result is practically not affected by polarization effect and ionic conductivity since the skin to be tested is not in unnatural contact with the test probe and almost no current flows through the skin to be tested. The instrument probe and the water in the skin have no inertia in the process of establishing balance, and can realize quick measurement, thereby eliminating the influence of active skin on the measurement result.
The experimental method comprises the following steps: test area: inner side of forearm
Before the test, the testee needs to clean the inner side of the forearm uniformly, the forearm is wiped clean by using dry facial tissue, a measurement area mark is made on the inner side of the forearm of the testee after cleaning, and the testee needs to sit still for at least 30min in a room meeting the standard before formal test, the forearm is exposed and placed in a test state to keep relaxed.
In the experiment, the inner forearm is marked with 2X 4cm2 experimental area, and the same arm can mark multiple areas at the same time, and the areas are spaced by 2 cm. The test products and the blank control are randomly distributed on the forearm, the blank value of 30min after cleaning of each test area is measured, then the test sample is uniformly coated in the experimental area by using a latex finger cot according to the dosage of 2.0 +/-0.1 mg sample/cm 2, and the skin moisture content of the test area and the control area is measured after 0.5h, 1h, 2h and 4h respectively after coating. The measurements of the same volunteer were performed by the same measurement staff.
Hydration ═ (test value-blank control value)/blank control value ═ 100%
The results of the moisturizing effect test were as follows:
example 1 Example 2 Example 3 Example 4 Blank space
0.5h 39.50% 43.78% 44.09% 43.87% 36.44%
1h 45.12% 46.75% 45.66% 45.54% 37.11%
2h 47.23% 49.99% 46.77% 46.78% 36.33%
4h 37.06% 36.87% 39.46% 38.76% 35.97%
The product also has a certain moisturizing effect, but the duration of the moisturizing effect is only 2 hours.
The application example is as follows:
(1) water (W)
Figure BDA0003110802870000201
Figure BDA0003110802870000211
The water process comprises the following steps:
heating and dissolving A phase at 80 ℃, stirring for 40 minutes, and then cooling
2. Adding phase B into phase A, stirring and mixing uniformly
3. Cooling to 60 deg.C, sequentially adding C, D, and stirring
4. Cooling to 40 deg.C under stirring, adding phase D, and stirring
(2) Milk
Figure BDA0003110802870000212
Figure BDA0003110802870000221
The milk process comprises the following steps:
dissolving phase A by heating at 80 deg.C
Dissolving B phase in 80 deg.C under heating and stirring
Dissolving C phase in 65 deg.C under heating and stirring
Adding phase B into phase A, emulsifying for 3min at 5500 rotation
4. Cooling to 50 deg.C under stirring, adding D, E phase, and stirring
(3) Cream
Figure BDA0003110802870000222
Figure BDA0003110802870000231
The frost process comprises the following steps:
dissolving phase A by heating at 70 deg.C
2, B, C phase, heating at 80 ℃, stirring and dissolving
Slowly adding the phase A into the B, C phase after being dissolved and uniformly mixed, emulsifying for 3min at 5000r/min
4. Cooling to about 50 deg.C, sequentially adding D, E, F phases, stirring, dissolving, and mixing.

Claims (10)

1.A method for preparing a soothing and repairing compound, which is characterized by comprising the following steps: heating a golden chamomile extract, a gentian extract, a grape skin extract, an olive leaf extract, a centella asiatica flower/leaf/stem extract, a purslane flower/leaf/stem extract, a poncirus trifoliata fruit extract and glucan to 70-80 ℃, and stirring for dissolving; the allergy-relieving repair compound is compounded by the following components in parts by weight: 15-25% of a chamomile extract, 10-15% of a gentian extract, 5-10% of a grape skin extract, 5-10% of an olive leaf extract, 5-10% of a centella asiatica flower/leaf/stem extract, 5-8% of a purslane flower/leaf/stem extract, 3-5% of a poncirus trifoliata fruit extract and 1-5% of glucan.
2. A method of preparing a soothing repair complex according to claim 1, wherein: the golden chamomile extract is prepared by mixing golden chamomile and water at 50-65 ℃, carrying out ultrasonic-assisted extraction for 70-90 min at a feed liquid weight ratio of 1:15-25, then heating to boil, and concentrating to a density of 1.01-1.20 g/mL.
3.A method of preparing a soothing repair complex according to claim 1, wherein: the radix gentianae extract is prepared by crushing radix gentianae, extracting for 3 times by using 50-75% ethanol as a solvent, wherein the weight ratio of a first feed liquid to a second feed liquid is 1: 8-10, the weight ratio of the second feed liquid to the third feed liquid is 1: 5-8, the extraction temperature is 70-80 ℃, the extraction time is 4-6 hours, filtering is carried out, three filtrates are combined, ethanol is concentrated at 75-85 ℃, and vacuum drying is carried out to obtain the radix gentianae extract.
4. A method of preparing a soothing repair complex according to claim 1, wherein: the grape skin extract is obtained by crushing grape skin, soaking and extracting with ethyl acetate as a solvent at a feed liquid weight ratio of 1: 10-25 at 20-35 ℃ for 2-3 d at a centrifugal rotation speed of 10000-12000 r/min for 10-12 min.
5. A method of preparing a soothing repair complex according to claim 1, wherein: the olive leaf extract is prepared by taking 75-85% ethanol as a solvent, extracting olive leaves for 3-5 hours at 70-85 ℃ for 2 times in a water bath hot reflux extraction mode, filtering, concentrating to remove ethanol at 75-85 ℃, and separating and purifying AB-8 resin to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are 0.5-2 ml/min, 60-80% ethanol and 2-4 ml/min respectively, and the olive leaf extract is obtained.
6. A method of preparing a soothing repair complex according to claim 1, wherein: the centella asiatica flower/leaf/stem extract is prepared by crushing centella asiatica, adding 60-75% of ethanol as a solvent, carrying out ultrasonic-assisted extraction at 45-55 ℃ for 1-2 hours, concentrating the ethanol at 60-75 ℃ to remove impurities, and carrying out chitosan flocculation to remove impurities, wherein the addition amount of a flocculation liquid is 0.3-0.8%, the flocculation temperature is 35-45 ℃, the flocculation time is 2-3 hours, the D-4020 resin is used for separation and purification, the sample injection speed, the eluent concentration and the elution speed are respectively 0.4-1 ml/min, 60-75% of ethanol and 4-8 ml/min, and then carrying out purification by adopting macroporous resin to obtain the extract.
7. A method of preparing a soothing repair complex according to claim 1, wherein: the purslane flower/leaf/stem extract is prepared by crushing purslane, adding 60-75% of ethanol as a solvent, wherein the weight ratio of feed liquid is 1:15-25, carrying out ultrasonic-assisted extraction for 30-60 min, heating and extracting for 2-4 h at the extraction temperature of 70-85 ℃, then concentrating to remove ethanol at the temperature of 60-75 ℃, and carrying out macroporous resin separation and purification to obtain the extract, wherein the sampling speed, the eluent concentration and the elution speed are respectively 0.5-2 ml/min, 60-80% of ethanol and 1-4 ml/min.
8. A method of preparing a soothing repair complex according to claim 1, wherein: the poncirus trifoliata fruit extract is prepared by crushing poncirus trifoliata fruits, taking 75-85% ethanol as a solvent, heating and soaking, filtering, and concentrating at 75-85 ℃ until the density is 1.01-1.20 g/mL, wherein the weight ratio of the material liquid is 1: 10-15, the extraction temperature is 75-85 ℃, and the extraction time is 4-6 h.
9. A method of preparing a soothing repair complex according to claim 3, wherein: the pore diameters of the filter membranes or filter papers for the third filtration are 3 μm, 1 μm and 0.45 μm in sequence.
10. The application of the allergy-relieving repair compound is characterized by being applied to allergy-relieving repair essence water, allergy-relieving repair emulsion and allergy-relieving repair cream.
CN202110648429.1A 2021-06-10 2021-06-10 Preparation method and application of allergy-relieving repair compound Withdrawn CN113350234A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114796050A (en) * 2022-04-27 2022-07-29 蓓悠清(广东)健康科技有限公司 Efficient moisturizing and relieving gel mask and preparation method thereof
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Application publication date: 20210907