CN112618430A - Camellia procyanidine mask and preparation method thereof - Google Patents

Camellia procyanidine mask and preparation method thereof Download PDF

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Publication number
CN112618430A
CN112618430A CN202011481501.8A CN202011481501A CN112618430A CN 112618430 A CN112618430 A CN 112618430A CN 202011481501 A CN202011481501 A CN 202011481501A CN 112618430 A CN112618430 A CN 112618430A
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camellia
mask
procyanidin
fiber
activated carbon
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CN112618430B (en
Inventor
张喜雨
孙韫理
夏张婷
颜克鸣
刘苗
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Hunan Linzhishen Linyun Oil Tea Camellia Technology Development Co ltd
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Hunan Chunyan Daily Cosmetics Co ltd
Hunan Linzhishen Biological Science & Technology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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
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    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
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    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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    • A61K8/498Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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    • A61K8/60Sugars; Derivatives thereof
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/673Vitamin B group
    • A61K8/675Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
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    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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Abstract

The application provides a camellia procyanidin mask and a preparation method thereof, the camellia procyanidin mask comprises a mask cloth and a mask liquid, the mask liquid contains camellia procyanidin concentrated solution extracted from camellia fruit cattail, the mask cloth is active carbon mask cloth prepared by taking camellia fruit cattail residues as raw materials, the camellia procyanidin mask liquid with the effects of oxidation resistance and moisture preservation is prepared by adding natural procyanidin substances extracted from camellia fruit cattail, the natural active carbon mask cloth is prepared from the residual camellia fruit cattail residues after extraction, the camellia fruit cattail procyanidin concentrated solution and the camellia fruit cattail active carbon mask cloth are used together, the camellia procyanidin mask has a synergistic function, the effects of the mask are mainly expressed in that the activity of melanocyte tyrosinase is inhibited, DPPH free radicals are removed, the skin moisture is kept, the air permeability, the adsorbability and the experience feeling of the mask are greatly improved, and the comprehensive utilization degree of the camellia fruit can be effectively improved, the high added value of the camellia products is increased, and the method has very important economic benefit and application prospect.

Description

Camellia procyanidine mask and preparation method thereof
Technical Field
The invention belongs to the technical field of facial mask skin care products, and particularly relates to a camellia procyanidine facial mask and a preparation method thereof.
Background
People can have skin problems such as color spots, dark skin color and the like along with natural changes such as environment, age and the like, and the skin problems are mainly skin pigment deposition caused by the generation of human melanocytes. The synthesis of the skin whitening composition is controlled by inhibiting the tyrosinase activity, so that the skin pigmentation can be effectively improved, the skin whitening composition is one of the important targets of the current development of whitening products, and the skin whitening composition is paid more and more attention by researchers. Related researches show that the Theaceae plant contains rich procyanidine, procyanidine is detected in branches and leaves of camellia fruit, camellia flower and camellia sinensis, and the proanthocyanidine has physiological activities of resisting oxidation, removing oxidation free radicals, inhibiting tyrosinase activity, whitening, preventing sunburn, astringing, moisturizing and the like, so that the proanthocyanidine has very good development potential in cosmetic application.
The camellia fruit peel is used as a main byproduct in the production and processing process of camellia oil, is mostly used for producing active carbon at present, has insufficient effective utilization of active substances, and causes great resource waste.
Therefore, how to improve the comprehensive utilization degree of the camellia fruit hulls and increase the high added value of camellia products has very important economic benefit and application prospect.
Disclosure of Invention
In order to solve the technical problems, the invention provides the camellia procyanidin mask, which is developed by extracting procyanidin from camellia fruit peel and preparing mask cloth from residual residues after extraction, so that the comprehensive utilization degree of the camellia fruit peel can be effectively improved, the high added value of camellia products is increased, and the camellia procyanidin mask has very important economic benefits and application prospects.
The invention also aims to provide a preparation method of the camellia procyanidin mask.
A camellia procyanidine facial mask comprises a facial mask cloth and a facial mask liquid, wherein the facial mask liquid contains camellia procyanidine concentrated solution extracted from camellia fruit cattail, and the facial mask cloth is an activated carbon facial mask cloth prepared by taking camellia fruit cattail residues as raw materials.
The application provides a camellia procyanidine mask, which comprises mask cloth and mask liquid, wherein the mask liquid contains camellia procyanidine concentrated solution extracted from camellia fruit cattail, the mask cloth is active carbon mask cloth which is prepared by taking camellia fruit cattail residues as raw materials and is rich in micro-pore meshes, the camellia procyanidine mask liquid with the effects of resisting oxidation, whitening and moisturizing is prepared by adding natural procyanidine substances extracted from camellia fruit cattail, and the residual camellia fruit cattail residues after extraction are prepared into the natural active carbon mask cloth, so that the camellia procyanidine mask is developed The skin precipitation problems such as age increase and the like cause the skin to be more white and transparent, meanwhile, the air permeability, the adsorbability and the experience feeling of the mask are greatly improved, the comprehensive utilization degree of camellia fruit peel can be effectively improved, the high added value of camellia products is increased, and the method has very important economic benefits and application prospects.
The camellia procyanidin mask comprises the following raw materials in percentage by mass: 0.5-1.5% of camellia procyanidin concentrated solution, 2-5% of camellia extract, 0.5-1% of squalane, 0.01-0.03% of nicotinamide, 0.2-0.5% of sodium hyaluronate, 2-6% of butanediol, 0.5-1.5% of trehalose, 0.5-1% of glycerol, 0.1-0.3% of phenoxyethanol, 0.8-1.5% of ethylhexyl glycerol, 0.1-0.5% of carbomer, 0.2-0.4% of EDTA disodium, 0.1-0.8% of citric acid and the balance of deionized water. The camellia extract adopted by the invention has the functions of natural antioxidation, moisture retention and convergence; the adopted squalane has an antioxidant effect; the adopted nicotinamide has an anti-oxidation effect; the sodium hyaluronate adopted by the invention has the functions of locking water and moisturizing; the butanediol adopted by the invention has a moisturizing effect; the trehalose adopted by the invention has the effects of maintaining stability and preserving moisture; the glycerin adopted by the invention has the functions of moistening and moisturizing; the phenoxyethanol adopted by the invention has an antiseptic effect; the adopted ethylhexyl glycerin has the function of an anticorrosion synergist; the carbomer adopted by the invention has a thickening effect; the EDTA disodium adopted by the invention is provided with a metal chelating agent; the citric acid adopted by the invention has a pH adjusting function. The camellia procyanidin mask solution with the effects of resisting oxidation, whitening and moisturizing is prepared by adding natural procyanidin substances extracted from camellia fruit cattails and matching with natural active substances such as camellia flower extracts, and the camellia procyanidin mask solution is prepared by assisting natural active carbon mask cloth. Can effectively remove DPPH free radicals, solves the problems of skin precipitation caused by environmental pollution, age increase and the like, and makes the skin more white and bright. The skin care cream is natural in raw materials, does not contain essence and preservative, can form a natural barrier on the surface of skin while mildly moistening the skin, and can continuously care the health of the skin.
The camellia procyanidin facial mask is characterized in that the camellia fruit peel is the camellia fruit shell left after fresh camellia fruit is peeled. The camellia fruit peel is used as a main byproduct in the production and processing process of camellia oil, is mostly used for producing active carbon at present, has insufficient effective utilization of active substances, and causes great resource waste. Through extracting procyanidine in camellia fruit cattails and preparing mask cloth from residual residues after extraction, the camellia procyanidine mask is developed.
The camellia procyanidine mask comprises a fiber outer surface layer, an activated carbon particle layer and a fiber inner surface layer which are sequentially arranged. The facial mask cloth has a three-layer structure, and can well lock facial mask liquid. The inner active carbon particle layer is a gap between the outer surface layer and the inner surface layer, active carbon particles are filled in the gap, and the outer surface layer and the inner surface layer are rich microporous reticular fiber membrane cloth formed by blending active carbon fibers and long-staple cotton cloth. The activated carbon mask cloth disclosed by the invention is soft and skin-friendly, has strong air permeability and liquid adsorption, and greatly improves the use experience of the mask while protecting the skin. The yarn mixing ratio of the two fibers is as follows: activated carbon fiber: 1% -80%; 20 to 99 percent of long staple cotton fiber. Two fiber blend ratios are preferred: activated carbon fiber: 30-60 percent; 40-70% of long staple cotton fiber. Or the mixing ratio of the two fibers: activated carbon fiber: 40-50%; 50-60% of long-staple cotton fiber. Or the two fiber mixed yarn ratios are as follows: activated carbon fiber: 45 percent; 55% of long staple cotton fiber.
The camellia procyanidin mask is characterized in that the active carbon particle layer is nano active carbon particles prepared by taking camellia oleifera residues as raw materials. The particle size of the nano activated carbon particles is 30-50 nm. The fiber outer surface layer and the fiber inner surface layer are both woven by activated carbon fiber and long stapled cotton fiber blended yarns, and the activated carbon fiber is an activated carbon fiber layer prepared by taking residues of camellia oleifera as raw materials. The active carbon particle layer is natural nano active carbon particles prepared by utilizing the residue of camellia fruit and cattail left after preparing the procyanidine concentrated solution as an inner layer filler, the surface layer material of the mask cloth is the residue after extracting the procyanidine concentrated solution by utilizing the camellia fruit and cattail, a natural active carbon fiber layer is prepared to be a mask surface layer filler, and then the active carbon fiber and long stapled cotton fiber blended yarn are matched to prepare the mask surface layer. The thickness of the outer layer of the fiber is 0.12-0.16 mm; the thickness of the inner surface layer of the fiber is 0.10-0.14 mm; the thickness of the active carbon particle layer is 0.08-0.15 mm. The active carbon particle layer is used as the middle filler of the fiber cloth on the two surface layers to prepare the soft adhesive net-shaped pore mask cloth with good air permeability and good adsorbability.
A preparation method of a camellia procyanidin mask comprises the following steps:
s1, preparing camellia procyanidin concentrated solution by taking camellia fruit peel as a raw material;
s2, preparing the following raw materials in percentage by mass: 0.5-1.5% of camellia procyanidin concentrated solution, 2-5% of camellia extract, 0.5-1% of squalane, 0.01-0.03% of nicotinamide, 0.2-0.5% of sodium hyaluronate, 2-6% of butanediol, 0.5-1.5% of trehalose, 0.5-1% of glycerol, 0.1-0.3% of phenoxyethanol, 0.8-1.5% of ethylhexyl glycerol, 0.1-0.5% of carbomer, 0.2-0.4% of EDTA disodium, 0.1-0.8% of citric acid and the balance of deionized water, and mixing the raw materials to obtain a mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
In the preparation method of the camellia procyanidin mask, step S1 specifically includes the following steps:
s101, pre-treating camellia fruit peel: cleaning herba Camelliae Japonicae, drying in oven at 55-65 deg.C for 22-25 hr, and pulverizing to powder of below 100 mesh to obtain herba Camelliae Japonicae powder;
s102, preparing an anthocyanin extracting solution: adding 50% edible ethanol solution into herba Camelliae Japonicae powder, ultrasonic extracting at 70 deg.C, centrifuging, and filtering to obtain anthocyanin extractive solution;
s103, preparing a camellia procyanidin concentrated solution: separating and purifying the anthocyanin extracting solution by macroporous resin, performing gradient elution by edible ethanol with different concentrations to obtain an anthocyanin solution, and concentrating at low temperature to obtain the camellia procyanidin concentrated solution.
In the preparation method of the camellia procyanidin facial mask, in step S102, the ratio of the camellia fruit powder to the 50% edible ethanol solution is 1: 8. The proportion can well extract procyanidine of camellia fruit peel, so that the purification is optimized.
In the preparation method of the camellia procyanidin facial mask, in step S102, the ultrasonic extraction power is 40 kHz.
In step S3, the amount of facial mask solution is 28ml-32 ml. The gram weight of the mask cloth is 20-100g/m2
The mask cloth comprises a fiber outer surface layer, an activated carbon particle layer and a fiber inner surface layer which are sequentially arranged; the active carbon particle layer is nano active carbon particles prepared by taking residues of camellia oleifera as raw materials; the fiber outer surface layer and the fiber inner surface layer are both woven by activated carbon fiber and long stapled cotton fiber blended yarns, and the activated carbon fiber is prepared by taking residues of camellia oleifera as raw materials. The residue of herba Camelliae Japonicae is 100 mesh active carbon powder of fruit shell after procyanidin extraction.
The preparation method of the nano activated carbon particles comprises the following steps: drying the residues of the camellia oleifera fruits by using a solvent, and adding K into the dried residues according to the mass ratio of 5:12CO3And (3) adding distilled water in a ratio of 1:10, soaking for 10 hours, putting the soaked product into a vacuum tube type high-temperature furnace, activating for 1 hour at a temperature of 500-600 ℃, and carbonizing for 24 hours at a temperature of 300 ℃ to obtain the nano carbon fiber.
The preparation of the activated carbon fiber comprises the following steps: taking camellia fruit cattail residue as a raw material, and taking K2CO3Preparing plant fiber-based activated carbon as an activating agent, and activating at 800 ℃ to obtain the activated carbon fiber.
The preparation method of the fiber outer surface layer and the fiber inner surface layer comprises the following steps:
(1) mixing, opening and carding 1-80% of activated carbon fiber and 20-99% of long stapled cotton fiber by using an opener to form a fiber web;
(2) the fiber net is folded in a crossed manner, and is subjected to pre-spunlace treatment to obtain a reinforced spunlace non-woven fabric fiber net;
(3) and carrying out positive and negative spunlace on the fiber web to enable the fibers to be intertwined with each other to form a spunlace natural activated carbon fiber layer with higher strength, thereby obtaining the fiber web.
When in use, the activated carbon mask cloth full of essence is applied on the face, and the face is stood for 15-20min to ensure that the mask liquid is fully absorbed by the face, then the mask cloth is taken off, and the finger abdomen is gently massaged until the face is absorbed. The main functional raw materials of the product are a large amount of camellia fruit shells remained in the production and processing process of camellia oil, and a large amount of underutilized raw materials, so that the product is suitable for industrial production and has wide production and application values and prospects in the field of cosmetics.
Compared with the prior art, the invention has the following advantages:
1. the application provides a camellia procyanidin mask which comprises mask cloth and mask liquid, wherein the mask liquid contains camellia procyanidin concentrated solution extracted from camellia fruit cattail, the mask cloth is active carbon mask cloth with rich micropores and a net shape and prepared by taking camellia fruit cattail residues as raw materials, the camellia procyanidin mask liquid with the effects of resisting oxidation, whitening and moisturizing is prepared by adding natural procyanidin substances extracted from camellia fruit cattail, and the residual camellia fruit cattail residues after extraction are prepared into natural active carbon mask cloth, so that camellia procyanidin is developed, the camellia fruit cattail procyanidin concentrated solution and the camellia fruit active carbon mask cloth are used together, the camellia procyanidin mask has a synergistic function, the effects of the mask are mainly expressed in that melanocyte tyrosinase activity is inhibited, DPPH free radicals are removed, skin moisture is kept, and the effects of preventing skin from being polluted by environment are effectively achieved, The skin precipitation problems such as age increase and the like cause the skin to be more white and transparent, meanwhile, the air permeability, the adsorbability and the experience feeling of the mask are greatly improved, the comprehensive utilization degree of camellia fruit peel can be effectively improved, the high added value of camellia products is increased, and the method has very important economic benefits and application prospects.
2. The application provides a preparation method of a camellia procyanidin mask, natural procyanidin substances extracted from camellia fruit peel are added, natural active substances such as camellia flower extracts are matched, camellia procyanidin mask liquid with the effects of oxidation resistance, whitening and moisture preservation is prepared, the camellia procyanidin mask liquid is prepared by assisting natural active carbon mask cloth, the raw materials are natural, essence and preservatives are not added, a natural barrier can be formed on the surface of skin while skin is nourished mildly, skin health is continuously cared, the comprehensive utilization degree of the camellia fruit peel can be effectively improved, the high added value of a camellia product is increased, and very important economic benefits and application prospects are realized.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly introduced below.
FIG. 1 is a schematic structural diagram of a camellia procyanidin mask of the invention.
Detailed Description
As shown in fig. 1, the camellia procyanidin facial mask disclosed by the application comprises a facial mask cloth 1 and a facial mask liquid 2 arranged on the surface of the facial mask cloth 1, wherein the facial mask cloth 1 comprises a fiber outer surface layer 11, an activated carbon particle layer 12 and a fiber inner surface layer 13 which are sequentially arranged. The active carbon mask cloth has a three-layer structure, the inner surface layer and the outer surface layer of the fiber are soft and skin-friendly, the active carbon particle layer 12 has strong air permeability and liquid adsorption, and the mask liquid 2 is matched, so that the active carbon mask cloth has a synergistic effect function while protecting skin, and the effects of the mask are mainly represented by inhibiting the activity of melanocyte tyrosinase, removing DPPH free radicals and keeping skin moisture, so that the problems of skin precipitation caused by environmental pollution, age increase and the like are effectively solved, the skin is white and bright, and the air permeability, the adsorption and the experience of the mask are greatly improved.
The following describes a specific embodiment of the present invention with reference to specific examples 1 to 4 and comparative examples 1 to 3:
example 1:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 60 ℃ for 24 hours, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1 hour, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 1.0% of camellia fruit and cattail anthocyanin concentrated solution, 2% of camellia flower extract, 0.5% of squalane, 0.01% of nicotinamide, 0.2% of sodium hyaluronate, 2% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.1% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.1% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
The activated carbon mask cloth is prepared from natural nano activated carbon particles and activated carbon fibers, wherein the natural nano activated carbon particles and the activated carbon fibers are prepared from residues left after procyanidine solution extraction.
Example 2:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 60 ℃ for 23h, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1h, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 1.0% of camellia fruit and cattail anthocyanin concentrated solution, 5% of camellia flower extract, 0.5% of squalane, 0.02% of nicotinamide, 0.4% of sodium hyaluronate, 2.5% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.15% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.12% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain facial mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
The active carbon mask cloth is prepared from natural nano active carbon particles and active carbon fibers, wherein the natural nano active carbon particles are prepared from the residue of camellia fruit and cattail after procyanidine solution is extracted.
Example 3:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 55 ℃ for 25h, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1h, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 0.5% of camellia fruit and cattail anthocyanin concentrated solution, 2% of camellia flower extract, 0.7% of squalane, 0.02% of nicotinamide, 0.5% of sodium hyaluronate, 2.5% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.15% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.12% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain facial mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
The active carbon mask cloth is prepared from natural nano active carbon particles and active carbon fibers, wherein the natural nano active carbon particles are prepared from the residue of camellia fruit and cattail after procyanidine solution is extracted.
Example 4:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 65 ℃ for 22h, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1h, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 1.5% of camellia fruit and cattail anthocyanin concentrated solution, 2% of camellia flower extract, 0.7% of squalane, 0.02% of nicotinamide, 0.5% of sodium hyaluronate, 2.5% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.15% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.12% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain facial mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
The active carbon mask cloth is prepared from natural nano active carbon particles and active carbon fibers, wherein the natural nano active carbon particles are prepared from the residue of camellia fruit and cattail after procyanidine solution is extracted.
Comparative example 1:
s1: preparing the following raw materials in percentage by mass: 2% of camellia extract, 0.5% of squalane, 0.01% of nicotinamide, 0.2% of sodium hyaluronate, 2% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.1% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.1% of citric acid and 100% of deionized water, and mixing the raw materials to obtain a mask liquid;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
The activated carbon mask cloth is prepared from natural nano activated carbon particles and activated carbon fibers, wherein the natural nano activated carbon particles are prepared from residues of camellia oleifera and cattail after procyanidine solution is extracted.
Comparative example 2:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 60 ℃ for 23h, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1h, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 1.0% of camellia fruit and cattail anthocyanin concentrated solution, 5% of camellia flower extract, 0.5% of squalane, 0.02% of nicotinamide, 0.4% of sodium hyaluronate, 2.5% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.15% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.12% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain facial mask solution;
s3, placing the facial mask cloth prepared by taking walnut shells as raw materials into an aluminum film bag, performing irradiation sterilization, filling the facial mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the facial mask cloth.
The activated carbon mask cloth is prepared from natural nano activated carbon particles prepared from walnut shells and activated carbon fibers.
Comparative example 3:
s1: selecting intact, mildew-free and pest-free plump camellia fruits to prepare camellia fruit cattails, cleaning the camellia fruit cattails, drying in an oven at 60 ℃ for 24 hours, crushing to below 100 meshes to obtain camellia fruit cattail powder, adding 50% edible ethanol solution, performing ultrasonic extraction at 70 ℃ for 1 hour, and repeating the extraction for three times. Centrifuging the extractive solution at 4000r/min for 10min, filtering to obtain anthocyanin extractive solution, separating and purifying with macroporous resin, performing gradient elution with edible ethanol of different concentrations to obtain anthocyanin solution, and concentrating at low temperature to obtain concentrated solution;
s2, preparing the following raw materials in percentage by mass: 0.5% of camellia fruit and cattail anthocyanin concentrated solution, 2% of camellia flower extract, 0.7% of squalane, 0.02% of nicotinamide, 0.5% of sodium hyaluronate, 2.5% of butanediol, 0.5% of trehalose, 0.5% of glycerol, 0.15% of phenoxyethanol, 0.8% of ethylhexyl glycerol, 0.1% of carbomer, 0.2% of EDTA disodium, 0.12% of citric acid and deionized water are added to 100%, and all the raw materials are mixed to obtain facial mask solution;
s3, placing the facial mask cloth prepared by taking masson pine as a raw material into an aluminum film bag, performing irradiation sterilization, filling facial mask liquid in a sterile environment, and sealing the aluminum film bag in vacuum to obtain the facial mask cloth.
The active carbon mask cloth is prepared from natural nano active carbon particles and active carbon fibers prepared from masson pine.
The efficacy test is carried out on the camellia procyanidin mask solution obtained according to the examples 1-4 and the comparative examples 1-3 according to the performance indexes of antioxidation, whitening and moisturizing effects and the like:
test 1: DPPH radical scavenging ability test
The test evaluates the antioxidant capacity of the embodiments of the present invention by measuring the ability of the facial mask fluid to scavenge DPPH free radicals.
(1) Test samples: the stock solutions prepared in examples 1 to 4 and comparative example 1 were diluted with deionized water to give a test solution having a mass fraction of 1%.
(2) The test method comprises the following steps: preparing an antioxidant activity system for DPPH (DPPH) evaluation: 0.0197g of DPPH is weighed, dissolved by absolute ethyl alcohol and metered to 250mL to obtain DPPH solution with the concentration of 0.2 mmol/L. Respectively sucking 2mL of sample to be detected and 2mL of DPPH solution in the A1 group of solutions; a2 group solution, 2ml of sample and 2ml of absolute ethyl alcohol are sucked; group A3 solution 2ml of DPPH solution and 2ml of absolute ethanol. Shaking up each component, standing in dark for 30min, adjusting to zero with anhydrous ethanol at wavelength of 517nm, and measuring absorbance of A1, A2, and A3 groups respectively. DPPH radical clearance was calculated as follows: DPPH radical clearance (%) [1- (a1-a2)/A3] × 100%, average of three measurements. The test results are shown in table 1:
TABLE 1 DPPH radical scavenging Capacity
Serial number Testing mask sources DPPH radical scavenging ability/%)
1 Example 1 81.3
2 Example 2 82.7
3 Example 3 77.2
4 Example 4 88.2
5 Comparative example 1 70.6
As can be seen from the test results in Table 1, the mask solution of the present invention has a strong DPPH radical scavenging ability. From examples 1-4, it can be seen that the effect of example 4 is the best, as the DPPH of the facial mask fluid is more radical scavenging capacity, the greater the concentration of camellia anthocyanin facial mask fluid added in a certain concentration range. As can be seen from comparative example 1, the DPPH radical scavenging effect of the example is significantly higher than that of the comparative example. The facial mask liquid composition has a certain synergistic effect, can improve the DPPH free radical scavenging capacity and enhance the antioxidant effect.
And (3) testing 2: tyrosinase inhibition rate
The test evaluates the whitening efficacy of the embodiments of the present invention by measuring the tyrosinase inhibition rate by the facial mask fluid.
Test samples: examples 1-4 and comparative example 1;
the test method comprises the following steps:
(1) and 0.05mol/L PBS buffer solution preparation: 53mL of 0.5mol/L KH2PO4 solution and 47mL of 0.5mol/L K2HPO4 solution are measured, mixed uniformly, added with 9g of NaCl, subjected to constant volume of 1000mL, and adjusted to pH 6.8 to obtain 05mol/L PBS buffer solution.
(2) And 5mmol/L of tyrosine solution preparation: weighing 18.1mg of tyrosine, dissolving in 20mL of PBS buffer solution, heating and stirring until the solution is transparent to obtain 5mmol/L of tyrosine solution.
(3) And preparing a tyrosinase solution: weighing 1.9g (10000U) of tyrosinase, adding 10mL of PBS solution, keeping out of the sun, and carrying out ultrasonic oscillation on ice bath until the solution is transparent, thus obtaining 1000U/mL of tyrosinase solution.
(4) Tyrosinase inhibition assay
50uL of the tyrosinase solution and 100uL of the test sample are mixed uniformly and placed in a 96-well plate, 20uL of the tyrosinase solution is added under the condition of keeping out of the light, and the reaction is carried out for 10min at the temperature of 25 ℃. The absorbance of the sample was measured at 475nm and purified water was used as a blank. The tyrosinase inhibition rates for each sample are shown in table 2 below:
TABLE 2 tyrosinase inhibition
Figure BDA0002838249560000161
Figure BDA0002838249560000171
And (3) testing: test for efficacy of use
The test evaluates the moisturizing efficacy of the volunteers by measuring the change of the moisture value in 12h of the skin of the volunteers after using the mask.
(1) Test samples: examples 1 to 4 and comparative examples 1 to 3;
(2) the test method comprises the following steps: 49 female skin health volunteers with the average age of 20-45 years were selected and randomly divided into 7 groups (7 subjects of examples 1-4 and comparative examples 1-3), the subjects did not use any cosmetics 2 days before the test, and the moisture content and the skin color brightness of the skin of the subjects under the natural condition were recorded in detail before the test started. The test masks were used by the testers for 4 consecutive days. After the use is finished, the moisture and the brightness of the skin are tested. Each test is carried out in the environment with the temperature of 20-22 ℃ and the humidity of 45-55 percent, and the skin test probe has the test effect. The water replenishing rate calculation formula is as follows: water supplement rate/% (skin moisture content after test-skin moisture content before test)/skin moisture content before test × 100%; the formula for calculating the skin lightening color ratio is as follows: skin lightening ratio/%, skin brightness after test-skin brightness before test)/skin brightness before test × 100%. The results of the measurements are shown in Table 3 below.
Table 3 evaluation table of use efficacy
Figure BDA0002838249560000172
Figure BDA0002838249560000181
As can be seen from the test results in Table 3, the formula of this example has the effects of moisturizing and lightening skin color. It can be seen from comparative examples 1-3 that the influence of the camellia chrysantha anthocyanin mask solution and the camellia fruit and cattail activated carbon mask cloth on the mask effect is improved compared with that of a control group, wherein the camellia procyanidin mask solution has a promoting effect on the mask effect within the range of the formula addition; the camellia fruit and cattail active carbon mask cloth and the mask liquid are used together, so that the synergistic effect is achieved. The camellia procyanidin mask disclosed by the invention has a moisturizing effect, and can effectively nourish the skin while resisting the problem of skin darkness.
A camellia procyanidin facial mask was prepared as described in examples 1-4 and comparative examples 1-3 above.
The air permeability and the adsorbability to the material body of the mask cloth are verified according to the specific surface area and the mesoporous rate of the activated carbon.
The specific surface area and the mesoporous rate of the activated carbon particles prepared by using the camellia oleifera fruit hulls, the walnut shells and the masson pine as raw materials are respectively measured, and the results are shown in the following table 4
Table 4 activated carbon particle porosity test
Figure BDA0002838249560000182
The results show that the specific surface area and the mesoporous rate of the camellia fruit and the camellia husk are superior to those of the activated carbon particles prepared from walnut shells and masson pine. The adsorption capacity and the adsorption kinetic performance are faster due to larger specific surface area and mesoporous rate. Therefore, compared with the porosity test results of the activated carbon prepared from the camellia oleifera fruit shell, the walnut shell and the masson pine, the adsorbability of the camellia oleifera fruit shell activated carbon is obviously superior to that of the activated carbon particles prepared from the walnut shell and the masson pine shell.
In conclusion, the camellia procyanidine mask and the preparation method thereof have the advantages that the camellia fruit procyanidine concentrated solution and the camellia extract have certain effects of resisting oxidation, whitening and moisturizing, especially the camellia fruit procyanidine concentrated solution is added to have a certain synergistic effect on the effect of the mask, and the camellia fruit procyanidine concentrated solution is matched with the camellia fruit procyanidine with high porosity to prepare the active carbon mask cloth, so that the camellia procyanidine mask with good effects of resisting oxidation, whitening and moisturizing is obtained. Can effectively remove DPPH free radicals, solves the problems of skin precipitation caused by environmental pollution, age increase and the like, and makes the skin more white and bright.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. The camellia procyanidin mask is characterized by comprising mask cloth and mask liquid, wherein the mask liquid contains camellia procyanidin concentrated solution extracted from camellia fruit cattail, and the mask cloth is active carbon mask cloth prepared by taking camellia fruit cattail residues as raw materials.
2. A camellia procyanidin mask as claimed in claim 1, wherein: the mask liquid consists of the following raw materials in percentage by mass: 0.5-1.5% of camellia procyanidin concentrated solution, 2-5% of camellia extract, 0.5-1% of squalane, 0.01-0.03% of nicotinamide, 0.2-0.5% of sodium hyaluronate, 2-6% of butanediol, 0.5-1.5% of trehalose, 0.5-1% of glycerol, 0.1-0.3% of phenoxyethanol, 0.8-1.5% of ethylhexyl glycerol, 0.1-0.5% of carbomer, 0.2-0.4% of EDTA disodium, 0.1-0.8% of citric acid and the balance of deionized water.
3. A camellia procyanidin mask as claimed in claim 1, wherein: the camellia fruit peel is the residual camellia fruit shell after fresh camellia fruit is peeled.
4. A camellia procyanidin mask as claimed in claim 1, wherein: the mask cloth comprises a fiber outer surface layer, an activated carbon particle layer and a fiber inner surface layer which are sequentially arranged;
the active carbon particle layer is nano active carbon particles prepared by taking residues of camellia oleifera as raw materials;
the fiber outer surface layer and the fiber inner surface layer are both woven by activated carbon fiber and long stapled cotton fiber blended yarns, and the activated carbon fiber is prepared by taking residues of camellia oleifera as raw materials.
5. A camellia procyanidin mask as claimed in claim 4, wherein: the particle size of the nano activated carbon particles is 30-50 nm;
the thickness of the outer layer of the fiber is 0.12-0.16 mm;
the thickness of the inner surface layer of the fiber is 0.10-0.14 mm;
the thickness of the active carbon particle layer is 0.08-0.15 mm.
6. The preparation method of the camellia procyanidin mask is characterized by comprising the following steps:
s1, preparing camellia procyanidin concentrated solution by taking camellia fruit peel as a raw material;
s2, preparing the following raw materials in percentage by mass: 0.5-1.5% of camellia procyanidin concentrated solution, 2-5% of camellia extract, 0.5-1% of squalane, 0.01-0.03% of nicotinamide, 0.2-0.5% of sodium hyaluronate, 2-6% of butanediol, 0.5-1.5% of trehalose, 0.5-1% of glycerol, 0.1-0.3% of phenoxyethanol, 0.8-1.5% of ethylhexyl glycerol, 0.1-0.5% of carbomer, 0.2-0.4% of EDTA disodium, 0.1-0.8% of citric acid and the balance of deionized water, and mixing the raw materials to obtain a mask solution;
s3, placing a mask cloth prepared by taking residues of the camellia oleifera as raw materials into an aluminum film bag, performing irradiation sterilization, filling the mask liquid into a sterile environment, and sealing the aluminum film bag in vacuum to obtain the mask cloth.
7. The method for preparing a camellia procyanidin mask as claimed in claim 6, wherein the step S1 specifically comprises the following steps:
s101, pre-treating camellia fruit peel: cleaning herba Camelliae Japonicae, drying in oven at 55-65 deg.C for 22-25 hr, and pulverizing to powder of below 100 mesh to obtain herba Camelliae Japonicae powder;
s102, preparing an anthocyanin extracting solution: adding 50% edible ethanol solution into herba Camelliae Japonicae powder, ultrasonic extracting at 70 deg.C, centrifuging, and filtering to obtain anthocyanin extractive solution;
s103, preparing a camellia procyanidin concentrated solution: separating and purifying the anthocyanin extracting solution by macroporous resin, performing gradient elution by edible ethanol with different concentrations to obtain an anthocyanin solution, and concentrating at low temperature to obtain the camellia procyanidin concentrated solution.
8. The preparation method of a camellia procyanidin mask as claimed in claim 7, wherein the mask cloth comprises a fiber outer surface layer, an activated carbon particle layer and a fiber inner surface layer which are sequentially arranged;
the active carbon particle layer is nano active carbon particles prepared by taking residues of camellia oleifera as raw materials;
the fiber outer surface layer and the fiber inner surface layer are both woven by activated carbon fiber and long stapled cotton fiber blended yarns, and the activated carbon fiber is prepared by taking residues of camellia oleifera as raw materials.
9. The method of claim 8The preparation method of the camellia procyanidine mask is characterized by comprising the following steps: drying the residues of the camellia oleifera fruits by using a solvent, and adding K into the dried residues according to the mass ratio of 5:12CO31:10, adding distilled water, soaking for 10 hours, putting the soaked product into a vacuum tube type high-temperature furnace, activating for 1 hour at the temperature of 500-;
the preparation of the activated carbon fiber comprises the following steps: taking camellia fruit cattail residue as a raw material, and taking K2CO3Preparing plant fiber-based activated carbon as an activating agent, and activating at 800 ℃ to obtain the activated carbon fiber.
10. The method for preparing a camellia procyanidin mask as claimed in claim 8 or 9, wherein the method for preparing the outer fiber surface layer and the inner fiber surface layer comprises the following steps:
(1) mixing, opening and carding 1-80% of activated carbon fiber and 20-99% of long stapled cotton fiber by using an opener to form a fiber web;
(2) the fiber net is folded in a crossed manner, and is subjected to pre-spunlace treatment to obtain a reinforced spunlace non-woven fabric fiber net;
(3) and carrying out positive and negative spunlace on the fiber web to enable the fibers to be intertwined with each other to form a spunlace natural activated carbon fiber layer with higher strength, thereby obtaining the fiber web.
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