CN114869831B - A method for preparing cosmetic composition containing natural plants - Google Patents

A method for preparing cosmetic composition containing natural plants Download PDF

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CN114869831B
CN114869831B CN202210580056.3A CN202210580056A CN114869831B CN 114869831 B CN114869831 B CN 114869831B CN 202210580056 A CN202210580056 A CN 202210580056A CN 114869831 B CN114869831 B CN 114869831B
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fermentation
powder
extract
extraction
white
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CN114869831A (en
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陈秀玉
邓峰云
卢勇
詹柱
何沪宝
朱蒙
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Guangzhou Lianying Cosmetics Co ltd
Jiangsu Badian Biotechnology Co ltd
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Guangzhou Lianying Cosmetics Co ltd
Jiangsu Badian Biotechnology 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
    • A61K8/96Cosmetics 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
    • A61K8/9728Fungi, e.g. yeasts
    • 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
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/85Products or compounds obtained by fermentation, e.g. yoghurt, beer, wine

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  • Cosmetics (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention provides a preparation method of a cosmetic compound containing natural plants, which relates to the technical fields of plant extraction and purification, fermentation and cosmetics, and comprises the following steps: step one: extracting Ginseng radix, radix Angelicae sinensis, glycyrrhrizae radix, white truffle and Poria respectively, and purifying to obtain related extracts; step two: preparing rice fermentation liquor step by step according to a set sequence, firstly adding protease, amylase and cellulase for aerobic fermentation, and then adding rumen juice for anaerobic fermentation; step three: according to the invention, a plurality of plant extracts are compounded and then are compounded, and rice fermentation liquor is added, so that the defects of poor effect and incomplete exertion of a single extract are effectively overcome, active ingredients are converted into small molecules which are better absorbed through fermentation, and then a plurality of plant extracts are compounded, so that the effects of whitening, moisturizing, antioxidation and anti-aging are achieved.

Description

A method for preparing cosmetic composition containing natural plants
Technical Field
The invention provides a preparation method of a cosmetic compound containing natural plants, and relates to the technical fields of plant extraction and purification, fermentation and cosmetics.
Background
With the development of technology, human skin gradually tends to age due to age, ultraviolet radiation, diet, environment, etc. Skin aging is currently considered to be mainly involved in both natural aging and photoaging. There are various theories regarding its cause, such as genetic theory, immunological theory, free radical theory, etc., which are increasingly accepted. The radical theory suggests that skin changes with age are caused by side effects of free radicals. Normally, the generation and disappearance of free radicals in the body are in a state of dynamic equilibrium, and when the body ages, the ability to scavenge free radicals in the body is acutely or chronically impaired. The excessive free radicals can perform destructive reaction on the chemical structure of biomacromolecules constituting the tissue chest, so that the integrity of the normal tissue morphology and functions is damaged, and therefore, the development of corresponding skin care products aiming at mechanisms such as skin aging and the like has a wide development space.
In recent years, natural cosmetics with anti-aging, whitening and other effects are becoming increasingly trusted by consumers. The active ingredients in natural cosmetics mainly originate from plants, animals and microorganisms, wherein the application of the plant active ingredients is the most widely, and the plant active ingredients have been successfully applied to the fields of skin care, whitening, anti-aging and the like. In comparison with conventional cosmetics, the plant active ingredient is a natural substance extracted from plants, has finer molecules, is more easily absorbed and digested by skin, and does not cause deposition in vivo. Meanwhile, the plant extract cosmetic also has the advantages of obvious curative effect, strong pertinence, no side effect or small side effect after long-term use. The method for extracting the plant active ingredients is researched and applied to a cosmetic formula, and a human skin experiment is carried out to obtain the traditional Chinese medicine whitening and anti-aging composition, so that a research thought is provided for developing new whitening raw materials in the cosmetic industry and developing natural plant raw materials.
Disclosure of Invention
In order to obtain a cosmetic raw material with multiple effects, multiple processes are combined, and the cosmetic raw material has the effects of whitening and tendering skin, resisting oxidation and aging and the like, a preparation method of a cosmetic compound containing natural plants is provided, and the preparation method comprises the following steps: step one: extracting Ginseng radix, radix Angelicae sinensis, glycyrrhrizae radix, white truffle and Poria respectively, and purifying to obtain related extracts; step two: preparing rice fermentation liquor step by step according to a set sequence, firstly adding protease, amylase and cellulase for aerobic fermentation, and then adding rumen juice for anaerobic fermentation; step three: mixing the related extracts according to the set mass fraction, adding a preservative, sterilizing and filtering to obtain the product.
The product obtained by adopting the technical scheme is natural, has no stimulation, rich nutrition, strong efficacy and easy absorption, is a safe raw material which can be used with confidence, and can be applied to the fields of skin care, beauty and the like.
Further, crushing white ginseng by a crusher to obtain white ginseng powder, adding white rot fungi laccase, cellulase and mannanase into the white ginseng powder, adding water into the white ginseng powder, carrying out constant-temperature water bath for 2 hours at the temperature of 40 ℃, extracting the white ginseng powder, the white rot fungi laccase, the cellulase and the mannanase by 60-75% ethanol solution at the mass ratio of 1:0.05:0.05:0.01, extracting the white ginseng powder and the ethanol solution by 1:15-1:25 at the ultrasonic temperature of 45-55 ℃ at the ultrasonic frequency of 40-50kHz for 0.5-1.5 hours, heating the white ginseng powder to the temperature of 65-75 ℃, carrying out reflux extraction for 3-6 hours, and filtering and collecting filtrate; extracting the filter residue for the second time, wherein the mass ratio of the filter residue to the ethanol solution is 1:10-1:20, heating and reflux extracting the filter residue for 3-6 hours, and filtering and collecting filtrate; combining the two filtrates, adsorbing the combined filtrate with macroporous resin, and heating and concentrating the filtrate at 75-85 ℃ until no alcohol exists, thus obtaining the ginseng extract.
By adopting the technical scheme, as the ginseng contains the effective components such as ginsenoside, ginseng polysaccharide, ginseng polypeptide, vitamin, trace elements and the like, the ginsenoside is mainly extracted and purified, so according to the similar principle of compatibility, 5-year-old white ginseng is selected first, and then the white ginseng is extracted by using a plurality of processes for compounding, the extraction yield is effectively improved, and the active substances can be effectively enriched compared with the single process extraction.
Further, pulverizing radix Angelicae sinensis, sieving with 24 mesh sieve and containing powder not more than 40% of 60 mesh sieve, soaking and mixing with 65-75% methanol 15-25 times of radix Angelicae sinensis powder, extracting with ultrasound for three times at 35-55deg.C for 0.5-1.0 hr, mixing filtrates of three times, heating and concentrating under reduced pressure to half volume of filtrate, cooling the concentrate, precipitating with 95% ethanol 3 times of the concentrate, centrifuging to extract supernatant, collecting centrifuging precipitate, collecting supernatant with microporous membrane 0.45 μm, filtering precipitate, centrifuging to precipitate, mixing with filtering precipitate, and drying to obtain radix Angelicae sinensis extract.
By adopting the technical scheme, the Chinese angelica is crushed into Chinese angelica coarse powder or medium powder, so that the extraction is convenient, and the influence of excessive fineness of the Chinese angelica powder on the filtering effect is avoided; the purity of the extract is improved, the extraction pollution is reduced, and the economic benefit and the environmental benefit are high.
Further, the poria cocos is crushed to obtain poria cocos powder, the poria cocos powder is sieved by a 60-mesh sieve, distilled water with the mass of 20-30 times of that of the poria cocos powder is added for microwave extraction, the microwave power is 450-550W, the radiation time is 5-9min, suction filtration is carried out, the filter residues are extracted repeatedly once again, the extracting solutions of the two times are combined and then concentrated into paste in vacuum by a rotary evaporator, and the paste is dried for 18-24 hours at 65-75 ℃ in a drying box to obtain the poria cocos extract.
Further, washing fresh white truffle, vacuum freeze-drying, crushing the white truffle in a crusher to obtain white truffle powder, soaking and mixing the white truffle powder with 40-60% ethanol 15-20 times of the white truffle powder, performing ultrasonic auxiliary extraction for 1-2 h, performing ultrasonic auxiliary extraction for 3-6kHz, performing filtration to obtain a crude extract, purifying the crude extract by nonpolar macroporous resin (styrene-divinylbenzene polymer), pre-treating the macroporous resin, fully swelling the macroporous resin by absolute ethanol, placing the macroporous resin in a chromatographic column, performing flow cleaning by absolute ethanol until the liquid after cleaning is mixed with distilled water with equal amount, stopping washing the macroporous resin until no ethanol smell exists, controlling the flow rate of the crude extract to be 3ml/min, performing loading by using 40-60% ethanol solution after the crude extract is adsorbed by the macroporous resin, performing elution by using the 40-60% ethanol solution, heating the eluent to 65-75 ℃ and concentrating the filtrate under reduced pressure to obtain the white truffle extract.
By adopting the technical scheme, the physical, chemical and biological states of the white truffle by using a vacuum freeze-drying technology are basically unchanged, so that the nutrition and active ingredients of the white truffle are reserved to the maximum extent, the damage to volatile ingredients and thermosensitive substances in Bai Songlou in the drying process is reduced, and the reduction of polysaccharide content during the extraction of the white truffle is avoided.
Further, the glycyrrhiza glabra is extracted for 3 times by adding 60% -75% ethanol solvent, the first feed liquid ratio is 1:8-1:10, the second feed liquid ratio is 1:5-1:8, the third feed liquid ratio is 1:5-1:8, the extraction temperature is 70-80 ℃, the extraction time is 4-6 h, the extraction is carried out, the filtration is carried out after the extraction, the three filtrates are combined to obtain a crude extract, the crude extract is concentrated to a state without basically ethanol under reduced pressure at 60-75 ℃ to obtain a residual liquid, dichloromethane with the mass 2-3 times of the residual liquid is added into the residual liquid for extraction and a dichloromethane layer is collected, the extraction operation is repeated for 2-3 times, the dichloromethane filtrate of each time is combined, the dichloromethane filtrate is concentrated to 30% -50% of the total content under reduced pressure at 50-60 ℃, the concentrated solution is purified by a silica gel column, methanol is added into the concentrated solution for elution, the dichloromethane and the methanol has the mass ratio of 90:1, the elution flow rate is 1-3 drops/s, the eluent is collected, the eluent is concentrated to a state without liquid outflow under reduced pressure at 50-60 ℃, and the solid after concentration is frozen and dried to obtain the glycyrrhiza glabra extract.
Further, crushing dried rice to obtain rice powder, sieving the rice powder with a 80-mesh sieve, adding water, steaming to obtain rice slurry, sequentially adding 0.1-0.8% protease, 0.1-1.2% amylase and 0.1-0.65% cellulase into the rice slurry according to the mass ratio of the rice powder to the water of 1:10-1:30, continuously stirring and dissolving, heating to 55-60 ℃, fermenting to pH of 7.0-7.3, fermenting for 6-10h, continuously introducing filtered sterile air oxygen in the fermentation process, and obtaining a rice fermentation liquid primary product according to the air flow rate of 2-4L/min.
By adopting the technical scheme, digestive enzymes such as protease, amylase, cellulase and the like are added, so that the anti-nutritional factors of the rice can be eliminated, macromolecular proteins are degraded, and the aerobic fermentation of the rice is realized.
Further, taking rumen fluid, placing the rumen fluid in a separating funnel, incubating for 1-3 hours at the temperature of 35-45 ℃, reserving upper rumen fluid, adding 0.5-1.5% rumen fluid into a primary product of rice fermentation fluid, stirring for 2-3 minutes, fermenting, setting the fermentation temperature to 36-42 ℃, fermenting pH value to 6.6-6.8, continuously introducing carbon dioxide in the fermentation process, mixing and stirring gas and liquid for 1 minute, resting for 9 minutes, fermenting for 8-12 hours, sterilizing the fermentation fluid after fermentation, filtering and collecting filtrate, and obtaining the rice fermentation fluid.
By adopting the technical scheme, after the rice is subjected to aerobic fermentation, rumen microorganisms are utilized for anaerobic fermentation, so that fibers and proteins can be effectively degraded, the rice is degraded into small molecular substances which are harmless and are more suitable for human body absorption, active substances are enriched, the mildness of the product is improved, toxic and side effects are reduced, and a plurality of novel active substances can be generated with plant extracts. By simulating biological stomach digestion food in an in-vitro environment, a bionic multiple fermentation process is adopted, so that rice is fermented into active ingredients which are better absorbed and safer to obtain.
Further, 10 to 20 percent of ginseng root extract, 8 to 16 percent of angelica extract, 8 to 16 percent of tuckahoe extract, 8 to 16 percent of licorice root extract, 8 to 16 percent of white truffle extract, 0.5 to 2 percent of 1, 2-hexanediol and 0.2 to 1 percent of p-hydroxyacetophenone are taken, and the balance is supplemented to 100 percent by rice fermentation liquor, and the product is obtained after uniform stirring, sterilization and filtration.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a cosmetic composition comprising natural plants;
FIG. 2 is a DPPH inhibition chart of a cosmetic composition comprising natural plants;
FIG. 3 is a concentration graph of tyrosinase activity assay for cosmetic compositions containing natural plants.
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A preparation method of a cosmetic compound containing natural plants, as shown in figure 1, specifically comprises the following steps:
1. the invention selects 5-year-old white ginseng, pulverizes the selected white ginseng by a pulverizer, extracts with 70% ethanol as solvent after enzyme water bath, and carries out ultrasonic auxiliary extraction for 1h at the solid-liquid ratio of 1:20 and 45 ℃ at the temperature of 70 ℃, carries out heating reflux extraction for 5 hours, and filters and collects filtrate; extracting the filter residue for two times at a solid-to-liquid ratio of 1:12, heating and refluxing for 4.5 hours, and filtering to collect filtrate. Mixing the filtrates, concentrating at 80deg.C until no alcohol is present, and finally obtaining radix Ginseng extract.
2. Radix Angelicae sinensis extract is prepared by pulverizing radix Angelicae sinensis, sieving, extracting radix Angelicae sinensis powder with 1:20 times of 70% methanol under ultrasonic wave for 0.6 hr, extracting with ultrasonic wave for three times at 40deg.C, mixing filtrates, concentrating under reduced pressure to half, cooling the concentrate, precipitating with 3 times of 95% ethanol, centrifuging to obtain supernatant, collecting the supernatant, filtering, collecting the filtrate, centrifuging, mixing the precipitate with the filtrate, and drying to obtain radix Angelicae sinensis extract.
3. Poria extract is prepared by pulverizing Poria to obtain Poria powder, adding distilled water, extracting Poria with microwave-assisted extraction (solid-to-liquid ratio of 1:20) under microwave power of 520W for 7min, vacuum filtering, extracting the residue for 1 time under the same conditions, mixing the extractive solutions, vacuum concentrating into paste with rotary evaporator, and drying to obtain Poria extract.
4. Vacuum freeze drying fresh white truffle extract, pulverizing white truffle, ultrasonic-extracting with 50% ethanol 15 times of white truffle powder for 1 hr under assistance of ultrasonic wave with ultrasonic frequency of 5kHz to obtain crude extract, adsorbing and eluting the crude extract with macroporous resin to obtain eluent, concentrating the eluent at 70deg.C under reduced pressure until no alcohol is present to obtain white truffle extract.
5. Crushing licorice into powder, extracting with 70% ethanol for 3 times, wherein the first feed-liquid ratio is 1:8, the second feed-liquid ratio is 1:6, the third feed-liquid ratio is 1:6, the extraction temperature is 70 ℃, the extraction time is 4 hours, filtering after extraction, combining the three filtrates to obtain a crude extract, concentrating the crude extract at 70 ℃ to obtain a residual liquid, adding twice of dichloromethane into the residual liquid, mixing uniformly, standing for layering, collecting a dichloromethane layer, removing an extraction reagent, and repeating extraction for 3 times to ensure the completeness of the extraction effect. And (3) adsorbing, eluting and collecting the eluent by a silica gel column, concentrating the eluent at 60 ℃ under reduced pressure, concentrating the solid, and freeze-drying to obtain the glycyrrhiza glabra extract.
6. Adding 0.5% protease and 0.7% amylase into rice fermentation filtrate, and performing aerobic fermentation on 0.35% cellulase at 58 ℃ and pH7.1 for 8 hours to obtain a rice fermentation liquor primary product; adding 1% rumen juice into the primary rice fermentation liquid, performing anaerobic fermentation at 37deg.C and pH of 6.7 for 10 hr, sterilizing the fermentation liquid after fermentation, filtering, and collecting filtrate to obtain rice fermentation liquid.
7. After the plant extracts are obtained, the ginseng root extract 15%, the angelica extract 10%, the poria cocos extract 10%, the licorice root extract 10%, the white truffle extract 10%, the saccharomycete/rice fermentation product filtrate 43.8%, the 1, 2-hexanediol 1% and the p-hydroxyacetophenone 0.2% are mixed, sterilized and filtered to obtain the product.
Example 2
A preparation method of a cosmetic compound containing natural plants, as shown in figure 1, specifically comprises the following steps:
1. The ginseng root extract is prepared by selecting 5-year-old white ginseng, crushing the selected white ginseng by a crusher, adding enzyme water bath, extracting by using 70% ethanol as a solvent, carrying out ultrasonic-assisted extraction for 1.5 hours at the solid-liquid ratio of 1:18 and the temperature of 65 ℃, carrying out heating reflux extraction for 5.5 hours, and filtering and collecting filtrate; extracting the filter residue for 5 hours under reflux with a solid-to-liquid ratio of 1:15, filtering and collecting the filtrate. Mixing the filtrates, concentrating at 75deg.C until no alcohol is present, and finally obtaining radix Ginseng extract.
2. Pulverizing radix Angelicae sinensis, sieving, extracting radix Angelicae sinensis powder with 1:18 times of 70% methanol under ultrasonic wave for 0.8 hr, extracting with ultrasonic wave for three times at 45deg.C, mixing filtrates, concentrating under reduced pressure to half, cooling the concentrate, precipitating with 3 times of 95% ethanol, centrifuging to obtain supernatant, collecting the supernatant, filtering, collecting the filtrate, mixing the filtrate with the precipitate, and drying to obtain radix Angelicae sinensis extract.
3. Poria extract is prepared by pulverizing Poria, adding distilled water, extracting Poria with microwave-assisted extraction (solid-to-liquid ratio of 1:25) under microwave power of 520W for 10min, vacuum filtering, extracting the residue under the same conditions for 1 time, mixing the extractive solutions, vacuum concentrating into paste with rotary evaporator, and drying to obtain Poria extract.
4. Vacuum freeze drying fresh white truffle extract, pulverizing white truffle, ultrasonic-extracting with 45% ethanol 15 times of white truffle powder for 1.5 hr under the assistance of ultrasonic wave with ultrasonic frequency of 6kHz to obtain crude extract, adsorbing and eluting the crude extract with macroporous resin to obtain eluent, and concentrating the eluent at 70deg.C until no alcohol is present to obtain white truffle extract.
5. The licorice root extract is prepared by crushing licorice into powder, extracting with 75% concentration ethanol for 3 times, wherein the first material-liquid ratio is 1:9, the second material-liquid ratio is 1:8, the third material-liquid ratio is 1:8, the extraction temperature is 70 ℃, the extraction time is 5.5h, filtering after extraction, combining the three filtrates to obtain a crude extract, concentrating the crude extract at 70 ℃ to remove ethanol to obtain a residual liquid, adding twice of dichloromethane into the residual liquid, mixing uniformly, standing for layering, collecting a dichloromethane layer, removing an extraction reagent, and repeating extraction for 3 times to ensure the integrity of the extraction effect. And (3) adsorbing, eluting and collecting the eluent by a silica gel column, concentrating the eluent at 60 ℃ under reduced pressure, concentrating the solid, and freeze-drying to obtain the glycyrrhiza glabra extract.
6. Adding 0.5% protease and 0.7% amylase into rice fermentation filtrate, and performing aerobic fermentation on 0.35% cellulase at 58 ℃ and pH7.1 for 8 hours to obtain a rice fermentation liquor primary product; adding 1% rumen juice into the primary rice fermentation liquid, performing anaerobic fermentation at 37deg.C and pH of 6.7 for 10 hr, sterilizing the fermentation liquid after fermentation, filtering, and collecting filtrate to obtain rice fermentation liquid.
7. After the plant extracts are obtained, the ginseng root extract 15%, the angelica extract 15%, the poria cocos extract 15%, the licorice root extract 15%, the white truffle extract 15%, the saccharomycete/rice fermentation product filtrate 23.5%, the 1, 2-hexanediol 1% and the p-hydroxyacetophenone 0.5% are mixed, sterilized and filtered to obtain the product.
Effect example 1:
DPPH radical scavenging test
1. Reagent preparation
(1) 3.913MgDPPH constant volume to 50mL with 95% ethanol
(2) 8MgTrolox to 100mL with 95% ethanol
(3) Random example 1 composition (hereinafter abbreviated example 1)
2. Experimental procedure
(1) UV zeroing, 95% ethanol as blank
(2) Pre-experiment (DPPH concentration selection)
500 Mu L DPPH+1000 mu L95% ethanol, shaking for 10s, standing for 10min, and measuring absorbance (absorbance at 520nm 0.45-0.55, which can be used as DPPH solution in the following experiment)
(3) Determination of Trolox
Sample Trolox(μL) 95% Ethanol (mu 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, oscillating for 10s, standing for 10min, and measuring absorbance value
(4) Experimental procedure
Adding DPPH or 95% ethanol, oscillating for 10s, standing for 10min
(5) Absorbance values were measured at 520nm, respectively, and a table was prepared and plotted to obtain IC50 values.
The calculation formula is as follows: inhibition (%) = [1- (S-SB)/(C-CB) ]. 100
3. Experimental results
Inner(μL) Con(μL/mL) DPPH(%)
150 100 65.301
50 33.3 51.875
20 13.33 40.381
Experimental results: example 1 has the effect of scavenging DPPH free radicals, and the higher the concentration of the product, the higher the scavenging efficiency of DPPH free radicals, and as can be seen from FIG. 2, the IC50 value is about 27. Mu.L/mL.
Effect example 2:
and (3) detection of moisturizing effect:
1. Experimental procedure
Instrument: cornemeter CMB25 (Germany CK company)
Sample to be tested: no. 1 (pure water), no. 2 (sample of random example)
2. Experimental conditions
① Indoor environment
② No strong sunlight or light direct irradiation
③ Ambient temperature 20+/-2 ℃ and ambient humidity 40-60%
3. Subject conditions
① Normal subjects 18-60 years old, both men and women, women give priority to
② Patients with severe systemic disease, immunodeficiency or autoimmune disease
③ Patients with inactive allergic diseases
④ Has no allergic history to skin care cosmetics
⑤ Hormone drugs and immunosuppressants have not been used for one month in the recent past
⑥ Not taking part in other clinical experiments
⑦ Volunteer participated and can complete specified content according to experimental requirement
4. Skin moisture content detection working principle
The principle of the world-recognized Cornemeter method, namely the capacitance method, is based on that the dielectric constants (< 7) of water (81) and other substances are quite variable, and according to the water content, a properly-shaped measuring capacitor can be changed along with the change of the capacitance of the skin, and the capacitance of the skin is in the measuring range, so that the moisture content of the skin can be measured. The capacitance measuring method is superior to other methods in that the skin to be tested and the test probe have no unnatural contact and almost no current passes through the skin to be tested, so that the test result is practically not affected by polarization effect and ionic conductivity. The instrument probe and the moisture in the skin have no inertia in the process of establishing balance, and the quick measurement can be realized, so that the influence of the active skin on the measurement result is eliminated.
5. Test procedure
① Test area: inner side of forearm
② Preparation before testing
The skin whitening effect product (cosmetics, external medicines or oral health care products) cannot be used 2-3 days before the tested part, the inner side of the forearm of the tested person needs to be cleaned uniformly before the test, the cleaned person is wiped with dry facial tissues, region marks are made on the inner side of the forearm of the tested person after the cleaning, the tested person should sit still for at least 30 minutes in a room meeting the standard before formal test, and the forearm is exposed and placed in a test state, so that the test is easy.
③ Test procedure
In the experiment, 3 x 4cm 2 experimental areas are marked on the inner side of the forearm, a plurality of areas can be marked on the same arm at the same time, and the areas are separated by 2cm. The test products and the blank control are randomly distributed on the forearm, blank values of 30min after cleaning of each test area are measured firstly, then the test sample is uniformly coated in an experimental area by using a latex fingerstall according to the dosage of 2.0+/-0.1 mg sample/cm 2, and the skin moisture contents of the test area and the control area are measured in a distribution manner of 0h, 1h, 2h and 4h after coating. Measurements of the same volunteer were performed by the same measurer.
6. Measurement index
Skin moisture content measurement, measurement of two times, and average value
7. Control form
Control of the different treatments by themselves
8. Results and analysis
Participation in test person measurements
Results: as can be seen from the table, the skin moisture content was essentially unchanged for the blank, and for the different test persons within 4 hours.
In the water group, after the skin test part is coated with pure water, the skin moisture content is slightly increased within 1 hour, but the water returns to the previous level immediately after the skin test part is coated with pure water, which indicates that the skin moisture content cannot be increased by coating pure water.
After the sample is smeared on the skin test part, the moisture content of the skin is obviously increased, and the water content is stable within 2 hours, so that the composition provided by the invention has the moisturizing effect.
Effect example 3
1. The purpose is as follows: semi-inhibition of tyrosinase by cosmetic compositions containing natural plants
2. Materials: sample: cosmetic composition containing natural plant (composition of example 1)
Buffer solution: k2HPO4 (8.71 g/500 ml) +kh2po4 (6.805 g/500 ml) →ph=6.80 (±0.02) spectrophotometer: uv,480nm
3. The steps are as follows:
(1) Enzyme concentration selection:
Dissolving a small amount of enzyme in buffer solution, and coloring brown; a1.5 ml centrifuge tube was added (L-tyrosine (0.3 mg/ml) 500. Mu.L+buffer 500. Mu.L+water 450. Mu.L+enzyme 50. Mu.L); before enzyme addition, the temperature is 37 ℃ for 20min; after the enzyme addition, absorbance was measured at 480nm of the spectrophotometer wavelength at 37℃for 10min (enzyme addition-test). The enzyme concentration was adjusted to give an Absorbance (ABS) of 0.45-0.55. The enzyme at this concentration was used as an experimental enzyme solution.
(2) Experimental addition
(3) Absorbance was measured at 480nm, respectively, to prepare a table. Mapping to obtain the IC 50.
The calculation formula is as follows: inhibition (%) = [1- (S-SB)/(C-CB) ]. 100
Note that: before enzyme addition, the temperature is 37 ℃ for 20min; after the enzyme addition, absorbance was measured at 480nm of the spectrophotometer wavelength at 37℃for 10min (enzyme addition-test). Enzyme was not added at 37℃for 20min.
S:Sample SB:Sample Blank C:Control CB:Control Blank
4. Results
The results of inhibition of tyrosinase activity by natural plant-containing cosmetic complexes are shown in the table:
usage amount (mu L) Concentration (μL/mL) Inhibition ratio (%)
30 20 88.36
10 6.67 70.61
5 3.33 43.36
5. Conclusion: the cosmetic composition containing natural plant has effect in inhibiting tyrosinase activity, and the higher the concentration of the composition, the stronger the effect in inhibiting tyrosinase activity, and as can be seen from FIG. 3, the IC50 value of the composition is about 4. Mu.L/mL.

Claims (1)

1. A preparation method of a cosmetic compound containing natural plants is characterized in that: comprising the following steps:
Step one: extracting Ginseng radix, radix Angelicae sinensis, glycyrrhrizae radix, white truffle and Poria respectively, and purifying to obtain related extracts; crushing white ginseng by using a crusher to obtain white ginseng powder, adding white rot fungi laccase, cellulase and mannanase into the white ginseng powder, adding water into the white ginseng powder for 2 hours at a constant temperature of 40 ℃, extracting the white ginseng powder, the white rot fungi laccase, the cellulase and the mannanase by a mass ratio of 1:0.05:0.05:0.01, extracting the white ginseng powder and the ethanol by using 60% -75% ethanol solution by a mass ratio of 1:15-1:25, carrying out reflux extraction at an ultrasonic temperature of 45-55 ℃ for 40-50kHz for 0.5-1.5 hours, then carrying out reflux extraction at a temperature of 65-75 ℃ for 3-6 hours, filtering and collecting filtrate, carrying out secondary extraction on filter residues, extracting the filter residues and the ethanol solution by heating and reflux for 3-6 hours, filtering and collecting filtrate, combining the two filtrates, and carrying out heat concentration on the filtrate at a temperature of 75-85 ℃ until the filtrate is free of alcohol, thereby obtaining the ginseng root extract; pulverizing radix Angelicae sinensis, sieving with 24 mesh sieve and containing powder not more than 40% of 60 mesh sieve, soaking and mixing with 15-25 times of 65-75% methanol of radix Angelicae sinensis powder, extracting with ultrasound for three times at 35-55deg.C for 0.5-1.0 hr, mixing filtrates, heating and concentrating under reduced pressure to half volume of filtrate, cooling the concentrate, precipitating with 95% ethanol 3 times of the concentrate, centrifuging to obtain supernatant, collecting the supernatant, filtering with microporous membrane of 0.45 μm, centrifuging to obtain precipitate, mixing with the filtrate, and drying to obtain radix Angelicae sinensis extract; pulverizing Poria to obtain Poria powder, sieving with 60 mesh sieve, adding distilled water 20-30 times of Poria powder, performing microwave extraction with microwave power of 450-550W for 5-9min, performing suction filtration, extracting residue again, mixing the two extractive solutions, vacuum concentrating into paste with rotary evaporator, and drying at 65-75deg.C for 18-24 hr to obtain Poria extract; washing fresh white truffle, vacuum freeze-drying, crushing the white truffle in a crusher to obtain white truffle powder, soaking and mixing the white truffle powder with 40-60% ethanol 15-20 times of the white truffle powder, carrying out ultrasonic-assisted extraction for 1-2 h and ultrasonic frequency for 3-6kHz, carrying out ultrasonic-assisted extraction and filtering to obtain crude extract, purifying the crude extract by nonpolar macroporous resin-styrene and divinylbenzene polymers, pretreating the macroporous resin, fully swelling the macroporous resin by absolute ethanol, placing the macroporous resin in a chromatographic column, carrying out flow cleaning by absolute ethanol until the liquid after cleaning is added with equal amount of distilled water and stops mixing, then washing the macroporous resin by using a large amount of distilled water until no ethanol smell exists, carrying out loading by controlling the flow rate of the crude extract, eluting by 40-60% ethanol solution after the crude extract is adsorbed by the macroporous resin, carrying out elution by controlling the flow rate of the macroporous resin to be 2ml/min, and heating the eluent to 65-75 ℃ and concentrating the filtrate under reduced pressure to obtain white truffle extract; extracting Glycyrrhiza glabra with 60-75% ethanol solvent for 3 times, wherein the first feed liquid ratio is 1:8-1:10, the second feed liquid ratio is 1:5-1:8, the third feed liquid ratio is 1:5-1:8, the extraction temperature is 70-80 ℃, the extraction time is 4-6 h, filtering after extraction, combining the three filtrates to obtain a crude extract, concentrating the crude extract under reduced pressure at 60-75 ℃ until no ethanol exists to obtain a residual liquid, adding 2-3 times of dichloromethane into the residual liquid for extraction, collecting a dichloromethane layer, repeating the extraction operation for 2-3 times, combining the dichloromethane filtrate of each time, concentrating the dichloromethane filtrate under reduced pressure at 50-60 ℃ until the total content is 30-50%, purifying the concentrated solution by a silica gel column, adding methanol for elution after adsorbing the concentrated solution, eluting dichloromethane and methanol at a mass ratio of 90:1, eluting the flow rate of 1-3 drops/s, collecting the eluent, concentrating the eluent under reduced pressure at 50-60 ℃ until no liquid flows out, and freeze-drying the concentrated solid to obtain Glycyrrhiza glabra root extract;
Step two: preparing rice fermentation liquor step by step according to a set sequence, firstly adding protease, amylase and cellulase for aerobic fermentation, and then adding rumen juice for anaerobic fermentation; crushing dried rice to obtain rice powder, sieving the rice powder with a 80-mesh sieve, adding water, steaming to obtain rice slurry, sequentially adding 0.1-0.8% protease, 0.1-1.2% amylase and 0.1-0.65% cellulase into the rice slurry according to the mass ratio of the rice powder to the water of 1:10-1:30, continuously stirring and dissolving, heating to 55-60 ℃, fermenting to pH of 7.0-7.3, fermenting for 6-10h, continuously introducing filtered sterile air oxygen in the fermentation process, and obtaining a rice fermentation liquid primary product according to the air flow rate of 2-4L/min; placing rumen fluid in a separating funnel, incubating at 35-45deg.C for 1-3h, collecting upper rumen fluid, adding 0.5-1.5% rumen fluid into the primary rice fermentation broth, stirring for 2-3min, fermenting, setting fermentation temperature at 36-42deg.C and fermentation pH at 6.6-6.8, continuously introducing carbon dioxide during fermentation, mixing gas and liquid, stirring for 1min, resting for 8-12h, sterilizing the fermentation broth after fermentation, filtering, and collecting filtrate to obtain rice fermentation broth;
Step three: mixing related extracts according to a set mass fraction, adding a preservative, sterilizing and filtering to obtain a product, taking 10-20% of ginseng root extract, 8-16% of Chinese angelica extract, 8-16% of poria cocos extract, 8-16% of licorice root extract, 8-16% of truffle extract, 0.5-2% of 1, 2-hexanediol, 0.2-1% of p-hydroxyacetophenone, and the balance of rice fermentation liquor to 100%, uniformly stirring, sterilizing and filtering to obtain the product.
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