CN109157454A - A kind of Camellia combined extracts and its preparation and the application in cosmetics - Google Patents

A kind of Camellia combined extracts and its preparation and the application in cosmetics Download PDF

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Publication number
CN109157454A
CN109157454A CN201811251030.4A CN201811251030A CN109157454A CN 109157454 A CN109157454 A CN 109157454A CN 201811251030 A CN201811251030 A CN 201811251030A CN 109157454 A CN109157454 A CN 109157454A
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camellia
extract
floral leaf
combined extracts
red hill
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CN109157454B (en
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奕志英
黄静
桑建梅
张春雷
章秀芳
高宏旗
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Shanghai linqingxuan Biotechnology Co., Ltd
SHANGHAI QITAN BIOTECHNOLOGY Co.,Ltd.
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Shanghai Qi Tan Biotechnology Co Ltd
SHANGHAI QINGXUAN 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]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of 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
    • A61K2800/80Process 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Dermatology (AREA)
  • Engineering & Computer Science (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Cosmetics (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The present invention provides a kind of Camellia combined extracts and its preparations and the application in cosmetics, the combined extracts include each component of following weight percentage: Red Hill tea seed supercritical extract 50-80%, Camellia floral leaf supercritical extract 10-30%, Camellia floral leaf residue extract 10-30%.The present invention is by carrying out means of supercritical extraction and the enzymatic hydrolysis alcohol extracting of Camellia floral leaf residue further progress after Red Hill tea seed is carried out means of supercritical extraction, the mixing of Camellia floral leaf, gained combined extracts contain sitosterol, squalene, the oleic acid of a variety of active ingredients such as α-VE and high level, antioxygenic property are more excellent.The cosmetics prepared have the effect of better moisturizing water lock, anti-oxidant, raising skin elasticity etc. repairs skin barrier.

Description

A kind of Camellia combined extracts and its preparation and the application in cosmetics
Technical field
The present invention relates to the deep process technology fields of camellia raw material, and in particular to a kind of raising camellia comprehensive plant benefit Camellia combined extracts and its preparation and the application in cosmetics.Camellia combined extracts of the present invention have Enhance skin oxidation resistance, improve skin elasticity, improves the effect of skin water lock ability etc. repairs skin barrier, can be used as height End cosmetic industry raw material, which is added in cosmetics, to be used.
Background technique
Camellia (Camellia japonica L.) is Theaceae Camellia Plants, belongs to evergreen broadleaf forest xylophyta, Also known as camellia, camellia, resistance to winter, it is one of the 10 famous flowers of China;Camellia is widely distributed, and main product is in China Zhejiang, Yunnan, river The ground such as west, Sichuan.As the camellia of natural resources, flavones, polyphenol, VE, oleic acid, spiny dogfish are rich in the positions such as flower, leaf, seed The nutrients such as the various bioactive components such as alkene, phytosterol and calcium, potassium, magnesium, manganese;Numerous studies have shown with camellia Extract prepared by flower, leaf, seed has effects that good reparation skin barrier, but its effective component is underutilized, Lack scientific and technological content and the high product of added value.
CO_2 supercritical technology has simple process, and organic solvent-free residual, operating condition is mild, and active constituent is protected It stays, collection is extracted, is concentrated, being located away from the incomparable advantage of traditional handicrafts such as integrated, the extraction suitable for natural products.But it is same When be suitable for the extraction of low molecule, low polarity, lipophilicity, low boiling point component in view of supercritical extraction technique, to water-soluble strong, The strong active constituent extraction yield of polarity is not high;And the effective component property contained in camellia, leaf, seed is different, it is single super to face Boundary's abstraction technique is difficult to meet the comprehensive utilization of plant.The synthesis extractive technique of exploitation each active constituent of camellia is conducive to improve The utilization rate of raw material reduces production cost, extracts active constituent to greatest extent, make playing a role for plant maximum efficiency.
Currently, being concentrated mainly on camellia seed oil and its conventional press technique side to the research of Camellia Plants functional component Face, and the research in relation to camellia floral leaf is also relatively fewer, the natural extract especially developed using camellia floral leaf as raw material is in skin care Application study and efficacy test research on product is very few;The product of camellia seed oil is at present on the market mainly with consumable products simultaneously Based on, as the high-end raw material of cosmetics using less;Existing camellia seed oil refining techniques is difficult to be refined into the dedicated height of cosmetics again Grade camellia oil;And phenomena such as tea seed harvest season property is strong, storage condition is more stringent, it is mildew and rot easily to occur during storage, oxidation. With the further investigation in terms of active constituent effect in camellia, camellia leaf, camellia seed, the Camellia of development and production high added value Combined extracts have great potential.
Summary of the invention
It is not high to solve existing resource of Camellia overall availability, fill up sky of the camellia raw material in high-end raw material of skin care articles White, the present invention provides a kind of Camellia combined extracts and its preparations and the application in cosmetics, by oil-soluble obtained Camellia combined extracts are applied to improve the cosmetics moisturizing that skin elasticity, moisturizing water lock, anti-oxidant etc. have effects that reparation In the products such as oil, cream, lotion.
The purpose of the present invention is what is be achieved through the following technical solutions:
The present invention provides a kind of Camellia combined extracts, each component including following weight percentage:
Red Hill tea seed supercritical extract 50-80%,
Camellia floral leaf supercritical extract 10-30%,
Camellia floral leaf residue extract 10-30%.
Preferably, the Camellia combined extracts include each component of following weight percentage:
Red Hill tea seed supercritical extract 65-75%,
Camellia floral leaf supercritical extract 15-25%,
Camellia floral leaf residue extract 10-15%.
Preferably, the raw material variety that the Camellia combined extracts use is 500 meters of height above sea level or more of C.chekiangoleosa Kind, compared with the camellia of other places of production and other kinds, extract obtained active component content is higher, especially camellia Oleic acid and linoleic acid content in seed.
Preferably, the Red Hill tea seed supercritical extract preparation method the following steps are included:
A1, after Red Hill tea seed pulverizes and sieves, after admixing anti-agglomerating agent, atlapulgite is added, carries out supercritical extract, Then two-stage separation is carried out;
A2, the primary extract obtained through step A1 is subjected to refinement treatment to get Red Hill tea seed supercritical extract.
Preferably, in step A1, the parameter of the extraction of boundary over zero are as follows: CO2The flow velocity of fluid is 15-30ml/min;Extraction Pressure power is 15-30Mpa;Extraction temperature is 30-40 DEG C;Extraction time is 0.5-1.5h;
The parameter of the two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure For 5-6Mpa, temperature is 25-40 DEG C;More preferable II grade of separation temperature is 25-30 DEG C.
The additive amount of the anti-agglomerating agent is the 5-10% of Red Hill tea seed weight, and the additive amount of atlapulgite is Red Hill tea seed The 2-10% of weight.
Preferably, in the active constituent of the Red Hill tea seed supercritical extract, squalene content is 250-350ppm, dimension Raw element E content is 150-250ppm, and cupreol content is 80-120ppm.
Preferably, it is 80 mesh, pellet through sieves rate >=98% that the Red Hill tea seed, which crushes mesh number,.
Preferably, the anti-agglomerating agent is silica.
In the preparation method of the Red Hill tea seed supercritical extract, the addition of atlapulgite can be to the camellia seed oil of extraction It decolourizes;The two-stage separation can separate phospholipid substance, wax material with camellia seed oil, instead of the degumming of camellia seed oil With winterization processing;The step of refinement treatment is depickling, dehydration and deodorization processing.
Preferably, the Camellia floral leaf supercritical extract preparation method the following steps are included:
B1, Red Hill camellia, Red Hill tealeaves are mixed, after pulverizing and sieving, carries out supercritical extract, then carry out two fractions From;
B2, the primary extract obtained through step B1 is subjected to refining filtering to get Red Hill tea seed supercritical extract and Red Hill Camellia leaf residue.
Preferably, in step B1, the Camellia floral leaf includes the Red Hill camellia and Red Hill tealeaves that mass ratio is 1:1-4, More preferable ratio is 1:2;
The parameter of the supercritical extract are as follows: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa; Extraction temperature is 30-50 DEG C;Extraction time is 1-2h;
The parameter of the two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure For 7-8Mpa, temperature is 25-40 DEG C;
In step B2, the filtering uses the filter membrane of 0.1-0.22um.
Preferably, the Red Hill camellia, Red Hill tealeaves crushing mesh number be 80 mesh, pellet through sieves rate >=98%.
Preferably, the preparation method of the Camellia floral leaf residue extract includes the following steps:
C1, it addition enzyme preparation, alcoholic solvent will be stirred in the Camellia floral leaf residue obtained through claim 6 the method Reaction is mixed, Camellia floral leaf residue enzymatic hydrolysis alcohol extract is obtained;
C2, by Camellia floral leaf residue digest alcohol extract coarse filtration after, gained filtrate carries out being concentrated in vacuo to obtain medicinal extract;
C2, medicinal extract is redissolved, then refinement treatment is to get the Camellia floral leaf residue extract.
Preferably, in step C1, the enzyme preparation include: the pectase for accounting for Camellia floral leaf residue weight 0.1-0.5 ‰, It accounts for the cellulase of Camellia floral leaf residue weight 1-5 ‰ and accounts for the amylase of Camellia floral leaf residue weight 1-5 ‰;It is described molten The additional amount of agent is 15-20 times of Camellia floral leaf residue weight;The condition being stirred to react are as follows: 40-50 DEG C of reaction temperature, anti- 30-60min, mixing speed 100-200rpm/min between seasonable;
In step C2, the temperature of the vacuum concentration is 50-55 DEG C, is concentrated into the 1/12 to 1/16 of filtrate volume, is passed through Pre-stage test proves that the selection of the cycles of concentration is more advantageous to and improves the extract in Camellia combined extracts used for cosmetic Stability in system;
In step C3, the group used of redissolving is divided into dehydrated alcohol and rilanit special, and rilanit special is easily soluble in Ethyl alcohol, ethyl alcohol can retain the hydrophilic active agents such as flavones, the polyphenol in camellia to greatest extent;The redissolution is resulting molten In liquid, the mass percentage of each component is as follows: medicinal extract 1-5%, dehydrated alcohol 40-50%, rilanit special 40-50%;Institute Stating refinement treatment includes ceramic membrane filter and ultrafiltration membrance filter.
It is highly preferred that in step C1, the alcoholic solvent is the ethanol solution that mass fraction is 60-80%, more preferable 70% Ethanol solution;
It is described to be concentrated into the 1/12 of filtrate volume in step C2;
In step C3, the ceramics membrane aperture is 30-200nm, the molecular cut off of ultrafiltration membrane is 2000Da-5000Da.
The present invention by will Red Hill tea seed carry out means of supercritical extraction, Camellia floral leaf mix after carry out means of supercritical extraction, with And Camellia floral leaf residue further progress digests alcohol extracting, gained combined extracts contain sitosterol, squalene, and α-VE etc. is a variety of The oleic acid of active constituent and high level, antioxygenic property are more excellent.
The present invention also provides a kind of preparation methods of Camellia combined extracts, including each component is mixed in proportion, ?.
The present invention also provides a kind of application of Camellia combined extracts above-mentioned in cosmetics, are applied especially to mention High skin elasticity, moisturizing water lock, anti-oxidant etc. have effects that repairing the cosmetics such as soothing oil, lotion, the cream of skin barrier produces In product.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, camellia combined extracts contain 3 positions of flower, leaf, seed of camellia, and raw material is using comprehensively;Screening simultaneously The C.chekiangoleosa kind that raw material variety is 500 meters of height above sea level or more, compared with the camellia of other places of production and other kinds, activity Component content is higher, the oleic acid and linoleic acid content especially in camellia seed.
2, camellia seed avoids solvent from using the pollution to environment through means of supercritical extraction in addition to being effectively retained active constituent;More Prominent feature is to avoid the decoloration and Degumming Procedures of camellia seed by process modification in means of supercritical extraction, reduce post-processing Link is refined, more environmentally friendly, energy conservation.
3, after the effective component of camellia, leaf is by supercritical extract and enzymatic hydrolysis alcohol extracting extraction, fat-soluble low pole activity Object and the highly polar active matter of alcohol-soluble have obtained maximum extraction;Chemically by dehydrated alcohol and castor oil itself Matter compounds fat-soluble low pole active matter and the highly polar active matter science of alcohol-soluble, and compatibility coexists, system balance.
4, camellia floral leaf (15-30Mpa) after supercritical, high pressure is handled, cell breakage is higher, and collaboration promotes active matter Dissolution so that active constituent in camellia floral leaf residue extract it is more abundant.
5, by enzymolysis processing, slightly solubility component can be promoted effectively to convert in camellia floral leaf and turn to soluble component, with The further destruction for deeply promoting institutional framework of enzyme reaction, increase cell wall, permeability of cell membranes, be conducive to endogenous object Release is leached, and the depth for being conducive to reaction carries out;The effect of enzyme addition makes camellia leaf tissue structure become loosely, to be conducive to The separation for realizing camellia leaf slag and liquid in slurries is conducive to improve subsequent process, such as shortens separation, filtering behaviour Make process time, realizability is strong in technique.
6, the present invention by will Red Hill tea seed carry out means of supercritical extraction, Camellia floral leaf mix after carry out means of supercritical extraction, And Camellia floral leaf residue further progress digests alcohol extracting, gained combined extracts are rich in sitosterol, and squalene, α-VE etc. is more The oleic acid of kind active constituent and high level, antioxygenic property is more excellent, and the effect for improving skin elasticity is preferable, and has significant Reduce the effect of percutaneous water loss, test result shows: the clearance rate of DPPH may be up to 89%;The variation of skin elasticity R2 value Rate is up to 8.32%;Percutaneous soil and water loss rate after 4 weeks can be down to 21.14g/ (hm2)。
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention Protection scope.
Embodiment 1
Present embodiments provide a kind of preparation method of Camellia combined extracts, comprising the following steps:
1, the safflower oil tea for selecting the big Yang mountain of Lishui of Zhejiang is raw material, picks camellia seed, camellia and camellia leaf.
2, the preparation of Red Hill tea seed supercritical extract:
2.1 pulverize and sieve Red Hill tea seed, and crushing mesh number is 80 mesh, pellet through sieves rate >=98%;
2.2 admix the camellia seed after sieving 5% anti-agglomerating agent silica of Red Hill tea seed weight, mix loading extraction thoroughly Kettle is taken, then atlapulgite is fitted into extraction kettle, the additive amount of atlapulgite is the 5% of camellia seed weight, wherein atlapulgite On the top of extraction kettle, supercritical CO2Entered by high-pressure pump from extraction kettle bottom.Atlapulgite is layered on upper layer, is conducive to The decoloration of camellia seed oil in camellia seed extraction process.
The parameter of 2.3 setting supercritical extracts: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15- 30Mpa;Extraction temperature is 30-40 DEG C;Extraction time is 0.5-1.5h;Supercritical extract is carried out, and carries out two-stage separation, I grade Separating pressure is 8-12Mpa, and temperature is 25 DEG C;II grade of separating pressure is 5-6Mpa, and temperature is 30 DEG C.
2.4 after step 2.3 processing resulting primary extract carry out refinement treatment, specially depickling, dehydration and deodorization processing, Up to Red Hill tea seed supercritical extract, active component content are as follows: squalene content is 350ppm, and content of vitamin E is 250ppm, cupreol content are 120ppm.
3, the preparation of Camellia floral leaf supercritical extract
3.1 are mixed Red Hill camellia, Red Hill tealeaves in the ratio of 1:2, are pulverized and sieved, crushing mesh number is 80 mesh, sample mistake Sieve rate >=98%.
Camellia seed after sieving is carried out supercritical extract by 3.2, then carries out two-stage separation;The parameter of supercritical extract: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa;Extraction temperature is 30-50 DEG C;Extraction time is 1- 2h;The parameter of two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure is 7-8Mpa, Temperature is 25-40 DEG C.
3.3 primary extracts for obtaining step 3.2 carry out refining filtering, cross the filter membrane of 0.1-0.22um, it is super to obtain Red Hill tea seed Critical extract and Camellia floral leaf residue.
4, the preparation of Camellia floral leaf residue extract
4.1, by Camellia floral leaf residue made from step 3.3, are added the pectin for accounting for camellia floral leaf residue weight 0.1 ‰ Enzyme, the cellulase for accounting for camellia floral leaf residue weight 5 ‰ account for the amylase of camellia floral leaf residue weight 2.5 ‰ as enzyme preparation, The ethanol solution (mass fraction 70%) of 20 times of camellia floral leaf residue weights is added, and is stirred to react 30- at 40-50 DEG C 60min, mixing speed 100rpm/min obtain Camellia floral leaf residue enzymatic hydrolysis alcohol extract.
After Camellia floral leaf residue is digested alcohol extract coarse filtration by 4.2, gained filtrate is concentrated in vacuo;Vacuum concentration condition It is 50-55 DEG C for revolving instrument heating temperature;It is concentrated to the 1/12 of filtrate, obtains medicinal extract.
4.3 dissolve medicinal extract dehydrated alcohol and rilanit special, obtain redissolution object, wherein medicinal extract accounting 1-5%;Anhydrous second Alcohol accounting 40-50%, rilanit special accounting are 40-50%.
4.4, which will redissolve object, carries out refinement treatment using integrated membrane separation technique, specifically includes the ceramics for being 30nm with aperture Film filtering and molecular cut off are the ultrafiltration membrance filter of 2000Da to get Camellia floral leaf residue extract.
5, by the Red Hill tea seed supercritical extract of preparation, Camellia floral leaf supercritical extract, Camellia floral leaf residue Extract is 70%, 20%, 10% to be mixed to prepare Camellia combined extracts in mass ratio.
Embodiment 2
This implementation column provides a kind of preparation method of Camellia combined extracts, comprising the following steps:
1, the safflower oil tea for selecting the big Yang mountain of Lishui of Zhejiang is raw material, picks camellia seed, camellia and camellia leaf.
2, the preparation of Red Hill tea seed supercritical extract:
2.1 pulverize and sieve Red Hill tea seed, and crushing mesh number is 80 mesh, pellet through sieves rate >=98%;
2.2 admix the camellia seed after sieving 10% anti-agglomerating agent silica of Red Hill tea seed weight, mix loading thoroughly Extraction kettle, then atlapulgite is fitted into extraction kettle, the additive amount of atlapulgite is the 10% of camellia seed weight, wherein active white Soil is in the top of extraction kettle, supercritical CO2Entered by high-pressure pump from extraction kettle bottom.Atlapulgite is layered on upper layer, favorably The decoloration of camellia seed oil in camellia seed extraction process.
The parameter of 2.3 setting supercritical extracts: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15- 30Mpa;Extraction temperature is 30-40 DEG C;Extraction time is 0.5-1.5h;Supercritical extract is carried out, and carries out two-stage separation, I grade Separating pressure is 8-12Mpa, and temperature is 40 DEG C;II grade of separating pressure is 5-6Mpa, and temperature is 40 DEG C.
2.4 after step 2.3 processing resulting primary extract carry out refinement treatment, specially depickling, dehydration and deodorization processing, Up to Red Hill tea seed supercritical extract, active component content are as follows: squalene content is 300ppm, and content of vitamin E is 150ppm, cupreol content are 100ppm.
3, the preparation of Camellia floral leaf supercritical extract
3.1 are mixed Red Hill camellia, Red Hill tealeaves in the ratio of 1:1, are pulverized and sieved, crushing mesh number is 80 mesh, sample mistake Sieve rate >=98%.
Camellia seed after sieving is carried out supercritical extract by 3.2, then carries out two-stage separation;The parameter of supercritical extract: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa;Extraction temperature is 30-50 DEG C;Extraction time is 1- 2h;The parameter of two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure is 7-8Mpa, Temperature is 25-40 DEG C.
3.3 primary extracts for obtaining step 3.2 carry out refining filtering, cross the filter membrane of 0.1-0.22um, it is super to obtain Red Hill tea seed Critical extract and Camellia floral leaf residue.
4, the preparation of Camellia floral leaf residue extract
4.1, by Camellia floral leaf residue made from step 3.3, are added the pectin for accounting for camellia floral leaf residue weight 0.5 ‰ Enzyme, the cellulase for accounting for camellia floral leaf residue weight 1 ‰, the amylase for accounting for camellia floral leaf residue weight 5 ‰ add as enzyme preparation Enter the ethanol solution (mass fraction 60%) of 15 times of camellia floral leaf residue weights, and is stirred to react 30- at 40-50 DEG C 60min, mixing speed 100-200rpm/min obtain Camellia floral leaf residue enzymatic hydrolysis alcohol extract.
After Camellia floral leaf residue is digested alcohol extract coarse filtration by 4.2, gained filtrate is concentrated in vacuo;Vacuum concentration condition It is 50-55 DEG C for revolving instrument heating temperature;It is concentrated to the 1/16 of filtrate, obtains medicinal extract.
4.3 dissolve medicinal extract dehydrated alcohol and castor oil, wherein medicinal extract accounting 1-5%;Dehydrated alcohol accounting 40- 50%, rilanit special accounting is 40-50%, obtains redissolution object.
4.4, which will redissolve object, carries out refinement treatment using integrated membrane separation technique, specifically includes the ceramics for being 100nm with aperture Film filtering and molecular cut off are the ultrafiltration membrance filter of 5000Da to get Camellia floral leaf residue extract.
5, by the Red Hill tea seed supercritical extract of preparation, Camellia floral leaf supercritical extract, Camellia floral leaf residue Extract is 60%, 30%, 10% to be mixed to prepare the Camellia combined extracts in mass ratio.
Embodiment 3
This implementation column provides a kind of preparation method of Camellia combined extracts, comprising the following steps:
1, the safflower oil tea for selecting the big Yang mountain of Lishui of Zhejiang is raw material, picks camellia seed, camellia and camellia leaf.
2, the preparation of Red Hill tea seed supercritical extract:
2.1 pulverize and sieve Red Hill tea seed, and crushing mesh number is 80 mesh, pellet through sieves rate >=98%;
2.2 admix the camellia seed after sieving 8% anti-agglomerating agent silica of Red Hill tea seed weight, mix loading extraction thoroughly Kettle is taken, then atlapulgite is fitted into extraction kettle, the additive amount of atlapulgite is the 2% of camellia seed weight, wherein atlapulgite On the top of extraction kettle, supercritical CO2Entered by high-pressure pump from extraction kettle bottom.Atlapulgite is layered on upper layer, is conducive to The decoloration of camellia seed oil in camellia seed extraction process.
The parameter of 2.3 setting supercritical extracts: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15- 30Mpa;Extraction temperature is 30-40 DEG C;Extraction time is 0.5-1.5h;Supercritical extract is carried out, and carries out two-stage separation, I grade Separating pressure is 8-12Mpa, and temperature is 25 DEG C;II grade of separating pressure is 5-6Mpa, and temperature is 25 DEG C.
2.4 after step 2.3 processing resulting primary extract carry out refinement treatment, specially depickling, dehydration and deodorization processing, Up to Red Hill tea seed supercritical extract, active component content are as follows: squalene content is 250ppm, and content of vitamin E is 200ppm, cupreol content are 80ppm.
3, the preparation of Camellia floral leaf supercritical extract
3.1 are mixed Red Hill camellia, Red Hill tealeaves in the ratio of 1:4, are pulverized and sieved, crushing mesh number is 80 mesh, sample mistake Sieve rate >=98%.
Camellia seed after sieving is carried out supercritical extract by 3.2, then carries out two-stage separation;The parameter of supercritical extract: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa;Extraction temperature is 30-50 DEG C;Extraction time is 1- 2h;The parameter of two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure is 7-8Mpa, Temperature is 25-40 DEG C.
3.3 primary extracts for obtaining step 3.2 carry out refining filtering, cross the filter membrane of 0.1-0.22um, it is super to obtain Red Hill tea seed Critical extract and Camellia floral leaf residue.
4, the preparation of Camellia floral leaf residue extract
4.1, by Camellia floral leaf residue made from step 3.3, are added the pectin for accounting for camellia floral leaf residue weight 0.3 ‰ Enzyme, the cellulase for accounting for camellia floral leaf residue weight 2 ‰, the amylase for accounting for camellia floral leaf residue weight 1 ‰ add as enzyme preparation Enter the ethanol solution (mass fraction 80%) of 20 times of camellia floral leaf residue weights, and is stirred to react 30- at 40-50 DEG C 60min, mixing speed 100-200rpm/min obtain Camellia floral leaf residue enzymatic hydrolysis alcohol extract.
After Camellia floral leaf residue is digested alcohol extract coarse filtration by 4.2, gained filtrate is concentrated in vacuo;Vacuum concentration condition It is 50-55 DEG C for revolving instrument heating temperature;It is concentrated to the 1/15 of filtrate, obtains medicinal extract.
4.3 dissolve medicinal extract dehydrated alcohol and castor oil, wherein medicinal extract accounting 1-5%;Dehydrated alcohol accounting 40- 50%, rilanit special accounting is 40-50%, obtains redissolution object.
4.4, which will redissolve object, carries out refinement treatment using integrated membrane separation technique, specifically includes the ceramics for being 200nm with aperture Film filtering and molecular cut off are the ultrafiltration membrance filter of 3000Da to get Camellia floral leaf residue extract.
5, by the Red Hill tea seed supercritical extract of preparation, Camellia floral leaf supercritical extract, Camellia floral leaf residue Extract is 80%, 10%, 10% to be mixed to prepare the Camellia combined extracts in mass ratio.
Embodiment 4
A kind of preparation method of Camellia combined extracts is present embodiments provided, it is essentially identical with the method for embodiment 3, The difference is that only: Red Hill tea seed supercritical extract, Camellia floral leaf supercritical extract, Camellia floral leaf residue extract Object is 50%, 20%, 30% to be mixed to prepare the Camellia combined extracts in mass ratio.
Embodiment 5
A kind of preparation method of Camellia combined extracts is present embodiments provided, it is essentially identical with the method for embodiment 1, The difference is that only: Red Hill tea seed supercritical extract, Camellia floral leaf supercritical extract, Camellia floral leaf residue extract Object is 65%, 25%, 10% to be mixed to prepare the Camellia combined extracts in mass ratio.
Embodiment 6
A kind of preparation method of Camellia combined extracts is present embodiments provided, it is essentially identical with the method for embodiment 1, The difference is that only: Red Hill tea seed supercritical extract, Camellia floral leaf supercritical extract, Camellia floral leaf residue extract Object is 75%, 15%, 10% to be mixed to prepare the Camellia combined extracts in mass ratio.
Embodiment 7
A kind of preparation method of Camellia combined extracts is present embodiments provided, it is essentially identical with the method for embodiment 1, The difference is that only: Red Hill tea seed supercritical extract, Camellia floral leaf supercritical extract, Camellia floral leaf residue extract Object is 70%, 15%, 15% to be mixed to prepare the Camellia combined extracts in mass ratio.
The comparative example of embodiment 1:
Comparative example 1-1
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no It is only that with place: being added without anti-agglomerating agent in the step 2.2 of this comparative example.The agglomeration of camellia seed material is serious when extraction, extracts It is insufficient, the active component content of gained Red Hill tea seed supercritical extract are as follows: squalene content is 150ppm, and vitamin E contains Amount is 100ppm, and cupreol content is 80ppm.
Comparative example 1-2
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no It is only that with place: being added without atlapulgite in the step 2.2 of this comparative example.The supercritical extract object of camellia seed oil after extraction Expect that color is deeper, refinement treatment process increases, and leads to the active component content of gained Red Hill tea seed supercritical extract are as follows: spiny dogfish Alkene content is 100ppm, and content of vitamin E 150ppm, cupreol content is 100ppm.
Comparative example 1-3
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no It is only that with place: processing of this comparative example without step 4, the method for step 5 are as follows: mention the Red Hill tea seed of preparation is overcritical Take object, Camellia floral leaf supercritical extract is 70%, 30% to be mixed to prepare Camellia combined extracts in mass ratio.
Comparative example 1-4
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no It is only that with place: the method for step 5 in this comparative example are as follows: by the Red Hill tea seed supercritical extract of preparation, Camellia floral leaf Supercritical extract, Camellia floral leaf residue extract be in mass ratio 50%, 30%, 20% be mixed to prepare Camellia combination mention Take object.
Comparative example 1-5
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no Be only that with place: the step 2 of this comparative example is that camellia seed extract is made using conventional crushing, filtering, decolorization.
Comparative example 1-6
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 1, no Be only that with place: the step 3 of this comparative example is residual using the obtained camellia leaf extract of room temperature seepage pressure effects and camellia floral leaf Slag.
The comparative example of embodiment 2:
Comparative example 2-1
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 2, no It is only that with place: in the step 2.3 of this comparative example, only carrying out I grades of separation, separated without II grades.It separates after extraction and does not fill Point, cause the impurity composition content of gained camellia seed supercritical extract high, the activity of gained Red Hill tea seed supercritical extract Component content are as follows: squalene content is 150ppm, and content of vitamin E 100ppm, cupreol content is 80ppm.
Comparative example 2-2
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 2, no Be only that with place: in the step 2.3 of this comparative example, the extracting pressure used is 10MPa.Gained Red Hill tea seed means of supercritical extraction The active component content of object are as follows: squalene content is 180ppm, content of vitamin E 120ppm, and cupreol content is 90ppm。
Comparative example 2-3
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 2, no Be only that with place: in the step 3.1 of this comparative example, the mixed proportion of the Red Hill camellia, Red Hill tealeaves that use is 2:1.
Comparative example 2-4
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 2, no It is only that with place: in the step 3 of this comparative example, being free of Red Hill tealeaves, products therefrom is Red Hill camellia supercritical extract;Step Rapid 4 products therefrom is Red Hill camellia residue extract.
The comparative example of embodiment 3:
Comparative example 3-1
This comparison provides a kind of preparation method of Camellia combined extracts, essentially identical with the method for embodiment 3, no Be only that with place: the step of this comparative example is without Camellia floral leaf means of supercritical extraction, 4.1 steps do not use camellia floral leaf residual Slag extracts preparation, but the raw material for directlying adopt step 3.1 carries out the enzymatic hydrolysis alcohol extracting of step 4, obtains camellia floral leaf enzymatic hydrolysis alcohol Mention product.
Comparative example 3-2
This comparative example provides a kind of preparation method of Camellia combined extracts, comprising the following steps:
1, identical as the step 1 of embodiment 3.
2, the preparation of Red Hill tea seed supercritical extract: identical as the step 2 of embodiment 3.
3, the preparation of Red Hill camellia supercritical extract: using in embodiment 3 step 3 and 4 method prepare.
4, the preparation of Red Hill tealeaves supercritical extract: using in embodiment 3 step 3 and 4 method prepare.
5, Red Hill tea seed supercritical extract, Red Hill camellia supercritical extract, Red Hill tealeaves supercritical extract are pressed Mass ratio is mixed to prepare the Camellia combined extracts for 80%, 10%, 10%.
Compliance test result experiment 1:
The Camellia combined extracts of above-mentioned all embodiment and comparative example preparations are subjected to DPPH free radical scavenging activity Anti-oxidant test select common antioxygen while in order to more intuitively observe the oxidation resistance of Camellia combined extracts Agent Vc is as control.The specific method is as follows:
Experimental procedure: 2mL DPPH ethanol solution and 2mL sample to be tested (Camellia combined extracts, Vc) are added in test tube Solution, concussion mix after be protected from light 30min, in 517nm at survey light absorption value A, while survey 2mL DPPH ethanol solution and 2mL without The light absorption value A of water-ethanol mixed liquor0And the light absorption value A of 2mL dehydrated alcohol and 2mL sample to be tested mixed liquorb, calculate DPPH Free radical scavenging activity:
Clearance rate (%)=(A of DPPH free radical0-(A-Ab))/A0×100
Test result is as shown in table 1, and the DPPH clearance rate of extract is higher, and the antioxygenic property of extract is stronger.As a result Showing comparative example, there are significant differences with embodiment 1, while the oxidation resistance of Camellia combined extracts of the invention is better than VC solution.
Table 1
Number The clearance rate (%) of DPPH Number The clearance rate (%) of DPPH
Vc solution (control group) 70 Comparative example 1-3 81
Embodiment 1 89 Comparative example 1-4 74
Embodiment 2 85 Comparative example 1-5 72
Embodiment 3 83 Comparative example 1-6 79
Embodiment 4 83 Comparative example 2-1 83
Embodiment 5 87 Comparative example 2-2 82
Embodiment 6 86 Comparative example 2-3 76
Embodiment 7 87 Comparative example 2-4 73
Comparative example 1-1 80 Comparative example 3-1 78
Comparative example 1-2 78 Comparative example 3-2 75
Compliance test result experiment 2:
The Camellia combined extracts of above-mentioned all embodiment and comparative example preparations are subjected to the survey of human safety patch Examination, test method is referring to the human skin patch in " 2015 cosmetics safety technical specification ".The examination of skin closure type patch The method tested are as follows: selecting the age is personnel 30 of 18-60 one full year of life, and area is selected to be no more than 50mm2, depth about 1mm qualification Spot tester material, the Camellia combined extracts for taking 0.020mL above-described embodiment and comparative example preparation are put into the small interior of spot tester, Control wells are blank control (not setting any substance), will be sticked added with the spot tester of Camellia combined extracts with low sensitization adhesive tape In the forearm song side of subject, is gently pressed with palm and be allowed to equably be pasted on skin, continued for 24 hours.Contain Red Hill respectively at removal 30min after tea combined extracts spot tester (after impression disappearance), with 48h 2 standard sight dermoreaction of table is pressed for 24 hours, and recorded Observe result.The patch test of Camellia combined extracts the results are shown in Table 3.
The experimental results showed that the Camellia combined extracts of all embodiment and comparative example preparations pass through human body patch safety Property test.
2 skin closure type patch test dermoreaction grade scale of table
3 human safety test result of table
Compliance test result experiment 3:
It is carried out after the Camellia combined extracts of above-mentioned all embodiment and comparative example preparations are diluted with certain solvent Human skin flexibility test, test equipment are skin elasticity tester (Cutometer dual MPA580), test method are as follows: Every group of Camellia combined extracts dilute sample selects 30 healthy womens, and the age smears sample at 30 ± 2 one full year of life, cheek, Sample smears preceding and sample and carries out skin elasticity test with instrument using after four weeks, parallel testing 3 times, is averaged, records R2 Value.
Wherein every group of Camellia combined extracts sample is diluted with olive oil, and configuration proportion is that Camellia combination is extracted Object: olive oil=1:9.
Wherein the change rate before change rate, that is, relative usage, calculation formula are as follows:
Δ (difference)=T after four weeks4-T0
In formula, T0--- tested area uses the R2 value before cosmetics.
T4--- tested area uses the R2 value after cosmetics four weeks.
N --- number of subjects.
Simultaneously in order to more intuitively observe the effect of Camellia combined extracts are for improving skin elasticity, olive oil is deducted Influence to skin elasticity, using olive oil as blank control.
Test result such as table 4, for skin elasticity R2 value closer to 1, skin elasticity is better.The change rate of R2 value is higher, sample The effect for improving skin elasticity is better.There are significant differences for comparative example and embodiment 1, while Camellia of the invention is combined and extracted It is preferable that object improves skin elasticity effect.
Table 4
Compliance test result experiment 4:
It is carried out after the Camellia combined extracts of above-mentioned all embodiment and comparative example preparations are diluted with certain solvent The percutaneous water loss test of human body, test equipment is 300 (German CK of skin surface water loss tester Tewameter TM Company), test method are as follows: every group of Camellia combined extracts dilute sample selects 30 healthy womens, and the age was at 30 ± 2 weeks Year sample is smeared at cheek, before sample is smeared and sample is using carrying out percutaneous water flow with instrument after four weeks and lose to measure, parallel testing It 3 times, is averaged, records percutaneous soil and water loss rate value.
Wherein every group of Camellia combined extracts sample is diluted with olive oil, and configuration proportion is that Camellia combination is extracted Object: olive oil=1:9.
Wherein the change rate before change rate, that is, relative usage, calculation formula are as follows:
Δ (difference)=A after four weeks4-A0
In formula, A0--- tested area uses the percutaneous soil and water loss rate value before cosmetics.
A4--- tested area uses the percutaneous soil and water loss rate value after cosmetics four weeks.
N --- number of subjects.
Simultaneously in order to more intuitively observe the effect of Camellia combined extracts are for improving skin water lock, olive oil is deducted Influence to skin water lock ability, using olive oil as blank control.
Percutaneous water loss rate value is smaller, and moisture loss is fewer, and water lock ability is stronger, and the barrier of skin is better.
Percutaneous water loss rate statistical result, is shown in Table 5.The result shows that: all embodiment and comparative examples are after smearing, warp Skin water loss rate value significantly reduces, especially embodiment 1, has the effect for significantly reducing percutaneous water loss, that is, has and significantly repair The effect of multiple skin barrier.
Table 5
Application Example 1
A kind of soothing oil is present embodiments provided, each component including formula as below: Camellia combined extracts 10% are small Wheat germ oil 20%, Sweet Almond Oil 20%, pond caul-fat 20%, Queensland nut seed oil 10%, jojoba seed oil 5%, cloth Ritchie fruit Oil 5%, aloe 5%, rose hip oil 5%, plant alkane 0.5%, tocopherol acetate 0.2%, phytosterol 0.2%, mouse Tail oxalic acid 0.02%, plant saualane 0.2%.
The soothing oil the preparation method comprises the following steps:
1) above-mentioned composition is kept the temperature into 60min, until clear in 85 ± 5 DEG C of addition emulsion pots;
2) 50 DEG C are cooled to hereinafter, essence selected by addition, is uniformly mixed (rate 50r/min);
3) it is filtered with 10um terminal filter, obtains the soothing oil of the combined extracts containing Camellia.
To the study on the stability of gained soothing oil, safety investigation, packaging material compatibility test, human efficiency's test, as a result Show the camellia soothing oil using this research, without any chemical preservative, skin zero is born;Simultaneously because the mountain of addition Tea combined extracts contain sitosterol, squalene, the oleic acid of a variety of active ingredients such as α-VE and high level, to skin have compared with Good skin-friendly, anti-oxidant, anti-aging, anti-inflammatory, antibacterial, protection skin barrier and other effects;In conjunction with other in camellia soothing oil Component, so that this camellia soothing oil has better moisturizing, water lock increases skin elasticity, greasy skin and oxidation resistant Repair effect.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase Mutually combination.

Claims (10)

1. a kind of Camellia combined extracts, which is characterized in that each component including following weight percentage:
Red Hill tea seed supercritical extract 50-80%,
Camellia floral leaf supercritical extract 10-30%,
Camellia floral leaf residue extract 10-30%.
2. Camellia combined extracts according to claim 1, which is characterized in that including each of following weight percentage Component:
Red Hill tea seed supercritical extract 65-75%,
Camellia floral leaf supercritical extract 15-25%,
Camellia floral leaf residue extract 10-15%.
3. Camellia combined extracts according to claim 1, which is characterized in that the Red Hill tea seed supercritical extract Preparation method the following steps are included:
A1, after Red Hill tea seed pulverizes and sieves, after admixing anti-agglomerating agent, atlapulgite is added, carries out supercritical extract, then Carry out two-stage separation;
A2, the primary extract obtained through step A1 is subjected to refinement treatment to get Red Hill tea seed supercritical extract.
4. Camellia combined extracts according to claim 3, which is characterized in that in step A1, the extraction of boundary over zero Parameter are as follows: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa;Extraction temperature is 30-40 DEG C;Extraction Time is 0.5-1.5h;
The parameter of the two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure is 5- 6Mpa, temperature are 25-40 DEG C;
The additive amount of the anti-agglomerating agent is the 5-10% of Red Hill tea seed weight, and the additive amount of atlapulgite is Red Hill tea seed weight 2-10%.
5. Camellia combined extracts according to claim 1 or 2 or 3, which is characterized in that the Red Hill tea seed is overcritical In the active constituent of extract, squalene content is 250-350ppm, content of vitamin E 150-250ppm, and cupreol contains Amount is 80-120ppm.
6. Camellia combined extracts according to claim 1, which is characterized in that the Camellia floral leaf means of supercritical extraction The preparation method of object the following steps are included:
B1, Red Hill camellia, Red Hill tealeaves are mixed, after pulverizing and sieving, carries out supercritical extract, then carries out two-stage separation;
B2, the primary extract obtained through step A1 is subjected to refining filtering to get Red Hill tea seed supercritical extract and Red Hill camellia Leaf residue.
7. Camellia combined extracts according to claim 6, which is characterized in that in step B1, the Camellia floral leaf The Red Hill camellia and Red Hill tealeaves for being 1:1-4 including mass ratio;
The parameter of the supercritical extract are as follows: CO2The flow velocity of fluid is 15-30ml/min;Extracting pressure is 15-30Mpa;Extraction Temperature is 30-50 DEG C;Extraction time is 1-2h;
The parameter of the two-stage separation are as follows: I grade of separating pressure is 8-12Mpa, and temperature is 25-40 DEG C;II grade of separating pressure is 7- 8Mpa, temperature are 25-40 DEG C;
In step B2, the filtering uses the filter membrane of 0.1-0.22um.
8. Camellia combined extracts according to claim 1, which is characterized in that the Camellia floral leaf residue extract Preparation method include the following steps:
C1, it addition enzyme preparation, alcoholic solvent will be stirred instead in the Camellia floral leaf residue obtained through claim 6 the method It answers, obtains Camellia floral leaf residue enzymatic hydrolysis alcohol extract;
C2, by Camellia floral leaf residue digest alcohol extract coarse filtration after, gained filtrate carries out being concentrated in vacuo to obtain medicinal extract;
C2, medicinal extract is redissolved, then refinement treatment is to get the Camellia floral leaf residue extract.
9. Camellia combined extracts according to claim 8, which is characterized in that in step C1, the enzyme preparation includes: The pectase of Camellia floral leaf residue weight 0.1-0.5 ‰ is accounted for, the cellulase of Camellia floral leaf residue weight 1-5 ‰ is accounted for and accounts for The amylase of Camellia floral leaf residue weight 1-5 ‰;The additional amount of the solvent is 15-20 times of Camellia floral leaf residue weight; The condition being stirred to react are as follows: 40-50 DEG C of reaction temperature, reaction time 30-60min, mixing speed 100-200rpm/min;
In step C2, the temperature of the vacuum concentration is 50-55 DEG C, is concentrated into the 1/12 to 1/16 of filtrate volume;
In step C3, the group used of redissolving is divided into dehydrated alcohol and rilanit special;It is described to redissolve in resulting solution, respectively The mass percentage of component is as follows: medicinal extract 1-5%, dehydrated alcohol 50-70%, rilanit special 50-70%;At the purification Reason includes ceramic membrane filter and ultrafiltration membrance filter.
10. a kind of application of Camellia combined extracts according to claim 1 in cosmetics.
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CN115197777A (en) * 2022-08-03 2022-10-18 广西大学 Method for preparing camellia oil for cosmetics based on rotary dynamic ceramic membrane filtration technology
CN115252489A (en) * 2022-07-13 2022-11-01 上海林清轩生物科技有限公司 Preparation method and application of camellia japonica flower and leaf extract
CN115300424A (en) * 2022-07-25 2022-11-08 上海林清轩生物科技有限公司 Multiple anti-wrinkle composition containing camellia japonica extract, preparation method and application
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CN110522690A (en) * 2019-09-05 2019-12-03 上海清轩生物科技有限公司 Antioxidant composition containing camellia and the soothing oil containing the antioxidant composition
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CN115252489A (en) * 2022-07-13 2022-11-01 上海林清轩生物科技有限公司 Preparation method and application of camellia japonica flower and leaf extract
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CN115197777A (en) * 2022-08-03 2022-10-18 广西大学 Method for preparing camellia oil for cosmetics based on rotary dynamic ceramic membrane filtration technology
CN116515553A (en) * 2022-11-28 2023-08-01 九江学院 Preparation method and application of externally-applied active tea oil
CN117778095A (en) * 2023-08-07 2024-03-29 湖南金昌生物技术有限公司 Preparation method of camellia seed extract

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