CN110403850B - Polysaccharide whitening solid mask and preparation method and application thereof - Google Patents
Polysaccharide whitening solid mask and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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Abstract
The invention discloses a polysaccharide whitening solid mask and a preparation method and application thereof. The method comprises the following steps: (1) preparing facial mask liquid: mixing and stirring the raw materials of the mask liquid uniformly, and then homogenizing to obtain the mask liquid; the mask liquid comprises the following components in parts by mass: 5-50 parts of polysaccharide composition, 0-20 parts of sodium hyaluronate, 0-5 parts of pearl powder and 20-95 parts of water; the polysaccharide composition comprises bletilla striata polysaccharide, pachyman and white peony root polysaccharide; (2) preparing a polysaccharide whitening solid mask: and soaking the cellulose facial mask paper into the facial mask liquid, then carrying out vacuum drying until the facial mask liquid is transparent, and then carrying out sterilization to obtain the polysaccharide whitening solid facial mask. The solid facial mask prepared by the invention has good moisturizing effect, can promote wound healing, has good tyrosinase inhibition and oxidation resistance, and has an active regulation effect on skin microbial state.
Description
Technical Field
The invention relates to the technical field of skin care products, in particular to a polysaccharide whitening solid mask and a preparation method and application thereof.
Background
With the improvement of life quality of people and the pursuit of improving the overall appearance, beauty and skin care products are more and more favored. The mask is one of the most important parts of skin care products because of high nutrient content, remarkable skin care effect and convenient use. The facial mask covers the face for a short time by using the essence, temporarily isolates the outside air and pollution, improves the temperature of the skin, expands pores of the skin, promotes secretion and metabolism of sweat glands, increases the oxygen content of the skin, is beneficial to the skin to remove products of metabolism of epidermal cells and accumulated grease substances, and nutrient substances in the facial mask permeate into the horny layer of the epidermis to soften the skin, so that the skin is naturally bright and elastic.
The common facial mask is usually manufactured in a wet mode, non-woven fabric or elastic facial mask paper is soaked in essence with beauty components, when the facial mask is used, a sealed package of the facial mask is torn, and the facial mask which is full of the essence can be directly taken out and applied to the face. However, in the wet mask, since the mask essence is rich in nutrients, in order to store and retain physiological activity for a long time, a large amount of preservatives, preservatives and surfactants are added to the essence, which threatens skin health. Meanwhile, the residual microorganisms in the production process of the product can also influence the health of the skin, and meanwhile, some unstable raw materials with high biological activity can be attenuated in the mask, so that the mask is not beneficial to storage and exerting the biological effect of the mask.
The solid mask is a novel product in a skin-care mask paste, has few preservative agents, is convenient to use and is widely accepted by consumers, and can enable active substances to be uniformly distributed on the surface of a mask cloth.
Polysaccharides are polysaccharides formed by connecting more than 10 monosaccharides by glycosidic bonds, are widely distributed in nature, and are natural macromolecular substances forming cell membranes of higher plants and animals and cell walls of microorganisms. Researches show that various polysaccharides have excellent tyrosinase inhibitory activity and antioxidant activity, are beneficial to inhibiting the generation of skin melanin, and have remarkable whitening effect. The polysaccharide also has obvious effect on understanding the skin microbial homeostasis, and has good effect on inhibiting the growth of harmful bacteria and promoting the growth of beneficial bacteria. Due to the rheological property of the polysaccharide component, the polysaccharide component plays a good role of a thickening agent in the mask essence, and reduces the irritation of the essence to the skin.
Based on the technical background, the mask which is good in skin health, beneficial to regulating the skin micro-ecology and good in active ingredient performance preservation is developed, and has great market demand.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a polysaccharide whitening solid mask.
The invention also aims to provide the polysaccharide whitening solid facial mask prepared by the method.
The invention further aims to provide application of the polysaccharide whitening solid mask.
The purpose of the invention is realized by the following technical scheme: a preparation method of a polysaccharide whitening solid mask comprises the following steps:
(1) preparation of facial mask liquid
Mixing and stirring the raw materials of the mask liquid uniformly, and then homogenizing to obtain the mask liquid; the mask liquid comprises the following components in parts by mass: 5-50 parts of polysaccharide composition, 0-20 parts of sodium hyaluronate, 0-5 parts of pearl powder and 20-95 parts of water; the polysaccharide composition comprises bletilla striata polysaccharide, pachyman and white peony root polysaccharide;
(2) preparation of polysaccharide whitening solid mask
And (2) soaking cellulose facial mask paper into the facial mask liquid obtained in the step (1), then carrying out vacuum drying until the facial mask liquid is transparent, and then carrying out sterilization to obtain the polysaccharide whitening solid facial mask.
The stirring conditions in the step (1) are as follows: stirring for 20-60 min at a speed of 100-2500 r/min; preferably: stirring at the temperature of 4 ℃ and the speed of 600r/min to 1000r/min for 20 to 60 min.
The homogenization in the step (1) is preferably carried out by adopting a micro-jet homogenizer under the following conditions: homogenizing for 2-20 times under 100-300 Mpa; preferably: homogenizing for 10-20 times under 200-300 Mpa.
The facial mask liquid in the step (1) preferably comprises the following components in parts by mass: 20-50 parts of polysaccharide component, 10-15 parts of sodium hyaluronate, 2-5 parts of pearl powder and 30-68 parts of water; more preferably comprises the following components in mass fraction: 20-50 parts of polysaccharide component, 10-15 parts of sodium hyaluronate, 2 parts of pearl powder and 38-68 parts of water.
The molecular weight of the sodium hyaluronate is 80-200 ten thousand daltons, and the purity of the sodium hyaluronate is more than or equal to 90%.
The pearl powder is preferably fresh water pearl powder.
The polysaccharide composition in the step (1) is a polysaccharide composition with the concentration of 1-500 mg/ml; preferably, the polysaccharide composition has a concentration of 10-15 mg/ml.
The mass ratio of the bletilla striata polysaccharide to the pachyman to the white paeony root polysaccharide in the step (1) is 1: 0.01-0.8: 0.01 to 0.8; preferably 1: 0.1-0.5: 0.1 to 0.5.
The polysaccharide composition described in step (1) is preferably prepared by the following method:
stirring bletilla striata polysaccharide, pachyman and white peony root polysaccharide at 4 ℃ and 1000r/min for 20 minutes; then homogenizing and stirring for 10 times under 200Mpa to obtain polysaccharide composition of uniform system.
The homogenization is preferably carried out by a microfluidizer.
The polysaccharide content of the bletilla striata polysaccharide, the pachyman and the white peony root polysaccharide in the step (1) is more than or equal to 97 percent, and the bletilla striata polysaccharide, the pachyman and the white peony root polysaccharide can be extracted from bletilla striata, poria cocos and white peony root serving as raw materials.
The bletilla striata polysaccharide, pachyman and white peony root polysaccharide in the step (1) are preferably prepared by the following method:
(I) sun drying rhizoma Bletillae or Poria or radix Paeoniae alba, pulverizing into powder, sieving, extracting with anhydrous ethanol for defatting, vacuum filtering, repeating for more than 2 times, filtering, and vacuum drying the filter cake to obtain defatted rhizoma Bletillae or Poria or radix Paeoniae alba;
(II) adding distilled water into the degreased bletilla striata, poria cocos or white paeony root, extracting in a water bath at 70-80 ℃ at a material-liquid ratio of 1:30(g/mL), filtering, repeating for more than 2 times, then combining the filtrates, concentrating to 1/4 volume, adding absolute ethyl alcohol until the volume fraction of the system ethyl alcohol reaches 80%, standing overnight, finally carrying out suction filtration, taking out a precipitate, washing, and freeze-drying to obtain crude polysaccharide;
(III) decolorizing the crude polysaccharide, purifying, concentrating, and freeze drying to obtain purified rhizoma bletilla polysaccharide, pachyman or radix Paeoniae alba polysaccharide.
The sieving described in step (I) is preferably a 100 mesh sieve.
The time for degreasing in step (I) is preferably 4 h.
The vacuum drying in the step (I) is vacuum drying at 50 ℃.
The extraction conditions in step (II) are preferably: extracting with 400W ultrasound assisted water bath at 50 deg.C for 30 min, and extracting with 70 deg.C water bath for 3 hr.
The filtration in step (II) is preferably carried out using 4 layers of 200 mesh filter cloth.
The concentration in the step (II) is vacuum rotary evaporation for concentration; concentration is preferably carried out by rotary evaporation under vacuum at 65 ℃.
The washing described in step (II) is preferably carried out with acetone and diethyl ether.
The decolorization in the step (III) is preferably performed by adopting activated carbon; preferably by the following steps: adding water to the crude polysaccharide for redissolving to obtain polysaccharide liquid; and then adding activated carbon, treating for 30-60 minutes in a water bath at 50 ℃, and filtering to obtain decolorized polysaccharide.
The concentration of the polysaccharide solution is preferably 10 mg/mL.
The dosage of the active carbon is 1-3% of the mass of the polysaccharide liquid.
The purification in the step (III) is carried out by adopting a dialysis bag with the molecular weight cutoff of 5000 Da; preferably, the purification is carried out for 12h by using a dialysis bag with the molecular weight cutoff of 5000 Da.
The concentration described in step (III) was to 1/4 volumes.
The polysaccharide content of the purified bletilla striata polysaccharide, pachyman and white peony root polysaccharide in the step (III) is more than or equal to 97 percent.
The cellulose facial mask paper in the step (2) is obtained by doping cellulose nano-fibrils with plant fibers as raw materials, and specifically refers to Chinese patent applications: the mask paper is prepared by the method in the application number of 201810266299.3, namely 'high-water-retention high-flexibility ultrathin mask paper and the preparation method and application thereof' (preferably, the method in the embodiment 6), and the quantitative amount of the mask paper is 10-100 g/m2Preferably 60 to 80g/m2。
The impregnation conditions in the step (2) are as follows: dipping for 8-24 hours at 4 ℃ in a sterile environment; preferably: and soaking for 18-24 hours at 4 ℃ in a sterile environment.
The vacuum drying conditions in the step (2) are as follows: drying for 3-24 hours at 40-60 ℃; preferably: drying at 50 deg.C for 24 hr.
The preparation method of the polysaccharide whitening solid mask further comprises the steps of sealing and sterilizing the polysaccharide whitening solid mask after the step (2).
The sealing is performed in a vacuum state.
The sterilization is performed by adopting a pasteur method.
The sterilization conditions of the pasteur method are as follows: sterilizing at 70 deg.C for 24 hr.
A polysaccharide whitening solid mask is prepared by any one of the methods.
The polysaccharide whitening solid mask is applied to the field of cosmetics.
Compared with the prior art, the invention has the following advantages and effects:
1. the cellulose facial mask paper used by the invention is prepared from the micro-nano fibrils serving as raw materials, the micro-nano fibrils have the characteristics of high specific surface area, large modulus and strong adsorption capacity, have a micro-stripping effect on skin aging keratinocytes, and can quickly adsorb and permeate nutrients of essence into the skin by combining the facial mask with the essence.
2. The facial mask liquid is prepared from bletilla striata polysaccharide, pachyman, white peony root polysaccharide, sodium hyaluronate, pearl powder and water, the main functional components of the facial mask liquid are plant sources, the polysaccharide component has viscosity, low irritation to skin and regulation of skin microbial state, the active ingredients can keep the best effect, and the facial mask liquid has the effects of moisturizing, moistening, whitening, pore astringing, skin brightening and the like after being used.
3. The facial mask liquid full of polysaccharide components is retained on the facial mask paper, and the physiological activity of the polysaccharide components is retained by using a low-temperature drying technology, so that the facial mask liquid is easy to store, the probability of bacterial breeding is reduced, no preservative is required to be added, and the skin health of a user is guaranteed; when in use, the matched sterile water is poured into the container, the mask paper is taken out after being soaked in the water and is applied to the face, so that a user can simply use the mask and keep the mask clean.
4. The solid facial mask is prepared by utilizing a vacuum drying technology, has a good moisturizing effect, can promote wound healing, has good tyrosinase inhibition and oxidation resistance, has an active regulation effect on skin microbial state, maintains skin stability, and improves skin color; the invention does not add preservative, essence and surfactant, has good safety and no stimulation to skin, protects bioactive factors to maintain the optimal state by utilizing low-temperature drying technology, effectively prevents microorganism from breeding and has wide safety and economic benefit.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. The test methods in the following examples, in which specific experimental conditions are not specified, are generally performed according to conventional experimental conditions or according to the experimental conditions recommended by the manufacturer. Unless otherwise specified, reagents and starting materials for use in the present invention are commercially available.
The cellulose facial mask paper related in the embodiment of the invention is high-water-retention high-flexibility ultrathin facial mask paper, is obtained by doping cellulose nanofibrils with plant fibers as raw materials, and specifically refers to Chinese patent applications: the name of application No. 201810266299.3 is 'a high water retention high softness ultrathin facial mask paper and a preparation method and application thereof' prepared by the method in example 6; wherein the quantitative amount of the facial mask paper is 10-100 g/m2(preferably 60 to 80 g/m)2)。
The bletilla striata polysaccharide, the pachyman and the white peony root polysaccharide in the whitening plant polysaccharide composition related to the embodiment of the invention can be obtained by conventional commercial methods (the polysaccharide content is more than or equal to 90 percent, preferably more than or equal to 95 percent) or can be prepared by self-extraction. The plant polysaccharide in the embodiment of the invention is prepared by self-extraction, and the specific preparation method comprises the following steps:
1. the preparation method of the bletilla striata polysaccharide comprises the following steps:
(1) rhizoma Bletillae (produced rehmannia, Zhejiang) is dried in the sun, crushed into powder and sieved with a 100-mesh sieve. Adding anhydrous ethanol, leaching and degreasing for 4h, performing suction filtration, repeating for 2 times, vacuum drying and drying filter cakes at 50 ℃, accurately weighing degreased bletilla striata, putting into a large conical flask, adding distilled water, performing water bath extraction at 70 ℃ for 3h, filtering with 4 layers of 200-mesh filter cloth to obtain filtrate, and repeating for 2 times; mixing filtrates, vacuum rotary evaporating at 65 deg.C, concentrating to 1/4 volume, adding anhydrous ethanol until the volume fraction of ethanol reaches 80%, and standing overnight; and (4) carrying out suction filtration to obtain a precipitate, washing the precipitate with acetone and diethyl ether, and carrying out freeze drying to obtain the crude bletilla polysaccharide.
(2) Redissolving the bletilla striata crude polysaccharide by water until the concentration is 10mg/mL, decoloring by using activated carbon, wherein the adding amount of the activated carbon is 1-3% of the mass of the polysaccharide liquid, and treating for 30-60 minutes in water bath at 50 ℃; filtering, loading the polysaccharide filtrate into a 5000Da dialysis bag at room temperature, and performing flow dialysis with distilled water for 12h for purification. Concentrating the dialysate to 1/4 volume, adding anhydrous ethanol until the volume fraction of ethanol reaches 80%, and standing overnight; and (3) carrying out suction filtration to obtain a precipitate, carrying out freeze drying on the precipitate to obtain purified bletilla polysaccharide, wherein the polysaccharide content is 97% by measuring with a phenol-sulfuric acid method.
2. The preparation method of pachyman comprises the following steps:
(1) poria (produced rehmannia, Zhejiang) is dried in the sun, crushed into powder and sieved by a 100-mesh sieve. Adding absolute ethyl alcohol, extracting and degreasing for 4 hours, carrying out suction filtration, repeating for 2 times, carrying out vacuum drying and drying on a filter cake at 50 ℃, accurately weighing degreased poria cocos, putting the degreased poria cocos into a large conical flask, adding distilled water, wherein the material-liquid ratio is 1:30(g/mL), extracting for 30 minutes in a water bath at 50 ℃ under the assistance of 400W ultrasound, extracting for 3 hours in a water bath at 70 ℃, filtering by using 4 layers of 200-mesh filter cloth to obtain a filtrate, and repeating for 2 times; mixing filtrates, vacuum rotary evaporating at 65 deg.C, concentrating to 1/4 volume, adding anhydrous ethanol until the volume fraction of ethanol reaches 80%, and standing overnight; and (4) carrying out suction filtration to obtain a precipitate, washing the precipitate with acetone and diethyl ether, and carrying out freeze drying to obtain the pachyman crude polysaccharide.
(2) Re-dissolving the crude tuckahoe polysaccharide in water to a concentration of 10mg/mL, decoloring the solution by using activated carbon, wherein the addition amount of the activated carbon is 1-3% of the mass of the polysaccharide solution, and treating the solution in water bath at 50 ℃ for 30-60 minutes; filtering, loading the polysaccharide filtrate into a 5000Da dialysis bag at room temperature, and performing flow dialysis with distilled water for 12h for purification. And (3) carrying out suction filtration to obtain a precipitate, carrying out freeze drying on the precipitate to obtain the poria cocos purified polysaccharide, wherein the polysaccharide content is 97% by measuring through a phenol-sulfuric acid method.
3. The preparation method of the white paeony root polysaccharide comprises the following steps:
(1) radix Paeoniae alba (produced rehmannia, Zhejiang) is dried in the sun, crushed into powder and sieved with a 100-mesh sieve. Adding absolute ethyl alcohol, extracting and degreasing for 4h, carrying out suction filtration, repeating for 2 times, drying a filter cake at 50 ℃ in vacuum, accurately weighing degreased white paeony root, putting the degreased white paeony root into a large conical flask, adding distilled water, carrying out water bath extraction at 80 ℃ for 3 hours, filtering by using 4 layers of 200-mesh filter cloth to obtain a filtrate, and repeating for 2 times; mixing filtrates, vacuum rotary evaporating at 65 deg.C, concentrating to 1/4 volume, adding ethanol until the volume fraction of ethanol reaches 80%, standing overnight; and (4) carrying out suction filtration to obtain a precipitate, washing the precipitate with acetone and diethyl ether, and carrying out freeze drying to obtain the crude white paeony root polysaccharide.
(2) Redissolving the crude white paeony root polysaccharide by water until the concentration is 10mg/mL, decoloring by using activated carbon, wherein the adding amount of the activated carbon is 1-3 percent of the mass of the polysaccharide liquid, and treating for 30-60 minutes in a water bath at 50 ℃; filtering, loading the polysaccharide filtrate into a 5000Da dialysis bag at room temperature, and performing flow dialysis with distilled water for 12h for purification. And (3) carrying out suction filtration to obtain a precipitate, carrying out freeze drying on the precipitate to obtain the purified white paeony root polysaccharide, wherein the polysaccharide content is 97% by measuring through a phenol-sulfuric acid method.
The molecular weight of the sodium hyaluronate is 80-200 ten thousand daltons, and the purity of the sodium hyaluronate is more than or equal to 90%.
The polysaccharide component involved in the embodiment of the invention is prepared by the following method: stirring bletilla striata polysaccharide, pachyman and white peony root polysaccharide at 4 ℃ and 1000r/min for 20 minutes; then homogenizing and stirring for 10 times under 200Mpa to obtain polysaccharide component of uniform system; wherein the mass ratio of the bletilla striata polysaccharide to the pachyman to the white peony root polysaccharide is 1: 0.01-0.8: 0.01 to 0.8.
Example 1
A polysaccharide whitening solid mask is prepared by the following steps:
(1) the cellulose facial mask paper has a mass of 60g per square meter (i.e., a basis weight of 60 g/m)2)；
(2) Mixing 50 parts by mass of polysaccharide component, 10 parts by mass of sodium hyaluronate, 2 parts by mass of fresh water pearl powder (purchased from Zhejiang Changsheng bird health science and technology Co., Ltd.) and 38 parts by mass of sterile water; wherein the initial concentration of the polysaccharide component is 10mg/ml, and the mass ratio of the bletilla striata polysaccharide, the pachyman and the white peony root polysaccharide in the polysaccharide is 1:0.1: 0.1. Mixing for 30 minutes by a stirrer at the temperature of 4 ℃ and the speed of 600 r/min; homogenizing and stirring the mixture for 10 times under 300Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking cellulose facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) and (3) sterilizing the sealed solid facial mask by a pasteur method, and sterilizing at 70 ℃ for 24 hours to obtain the polysaccharide whitening solid facial mask.
Example 2
A polysaccharide whitening solid mask is prepared by the following steps:
(1) the mass of the cellulose facial mask paper per square meter is 80 g;
(2) mixing 45 parts by mass of polysaccharide component, 15 parts by mass of sodium hyaluronate, 2 parts by mass of fresh water pearl powder (purchased from Zhejiang Changsheng bird health science and technology Co., Ltd.) and 38 parts by mass of sterile water; wherein the initial adding concentration of the polysaccharide component is 15mg/ml, and the mass ratio of the bletilla striata polysaccharide to the pachyman to the white peony root polysaccharide is 1:0.3: 0.3. Mixing for 20 minutes at the speed of 1000r/min at 4 ℃ by a stirrer; homogenizing and stirring the mixture for 10 times under 200Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking cellulose facial mask paper in the obtained facial mask liquid for 24 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) and (3) sterilizing the sealed solid facial mask by a pasteur method, and sterilizing at 70 ℃ for 24 hours to obtain the polysaccharide whitening solid facial mask.
Example 3
A polysaccharide whitening solid mask is prepared by the following steps:
(1) the mass of the cellulose facial mask paper per square meter is 80 g;
(2) mixing 20 parts by mass of polysaccharide component, 10 parts by mass of sodium hyaluronate, 2 parts by mass of fresh water pearl powder (purchased from Zhejiang Changsheng bird health science and technology Co., Ltd.) and 68 parts by mass of sterile water, wherein the initial adding concentration of the polysaccharide component is 10mg/ml, and the mass ratio of bletilla striata polysaccharide, pachyman and white peony root polysaccharide in the polysaccharide is 1:0.5: 0.5. Mixing the mixture for 60 minutes by a stirrer at the temperature of 4 ℃ and the speed of 1000 r/min; homogenizing and stirring the mixture for 20 times under 200Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking cellulose facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) and (3) sterilizing the sealed solid facial mask by a pasteur method, and sterilizing at 70 ℃ for 24 hours to obtain the polysaccharide whitening solid facial mask.
Comparative example 1
A solid facial mask is prepared by the following steps:
(1) commercially available facial mask paper (purchased from hydroentangled nonwoven products limited, Guangzhou) is made from cotton, and has a mass of 60g per square meter.
(2) Mixing 50 parts by mass of polysaccharide component, 10 parts by mass of sodium hyaluronate, 2 parts by mass of pearl powder and 38 parts by mass of sterile water, wherein the initial concentration of the polysaccharide component is 10mg/ml, and the mass ratio of bletilla striata polysaccharide, pachyman and white paeony root polysaccharide in the polysaccharide is 1:0.1: 0.1. Mixing for 30 minutes by a stirrer at the temperature of 4 ℃ and the speed of 600 r/min; homogenizing and stirring the mixture for 10 times under 300Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) sterilizing the sealed solid facial mask by Pasteur method, and sterilizing at 70 deg.C for 24 hr to obtain solid facial mask.
Comparative example 2
A solid facial mask is prepared by the following steps:
(1) commercially available facial mask paper (purchased from hydroentangled nonwoven products limited, Guangzhou) is made from cotton, and has a mass of 60g per square meter.
(2) Mixing 20 parts by mass of sodium hyaluronate with 80 parts by mass of sterile water, and mixing for 30 minutes at the speed of 600r/min by a stirrer at the temperature of 4 ℃; homogenizing and stirring the mixture for 10 times under 300Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) sterilizing the sealed solid facial mask by Pasteur method, and sterilizing at 70 deg.C for 24 hr to obtain solid facial mask.
Comparative example 3
A polysaccharide whitening solid mask is prepared by the following steps:
(1) the mass of the cellulose facial mask paper per square meter is 80 g;
(2) mixing 10 parts by mass of bletilla striata polysaccharide, 10 parts by mass of sodium hyaluronate and 80 parts by mass of sterile water, wherein the initial adding concentration of the bletilla striata polysaccharide is 15 mg/ml. Mixing the mixture for 60 minutes by a stirrer at the temperature of 4 ℃ and the speed of 1000 r/min; homogenizing and stirring the mixture for 20 times under 200Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking cellulose facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) and (3) sterilizing the sealed solid facial mask by a pasteur method, and sterilizing at 70 ℃ for 24 hours to obtain the polysaccharide whitening solid facial mask.
Comparative example 4
A polysaccharide whitening solid mask is prepared by the following steps:
(1) the mass of the cellulose facial mask paper per square meter is 80 g;
(2) mixing 10 parts by mass of polysaccharide component (wherein the polysaccharide is composed of bletilla striata polysaccharide and white paeony root polysaccharide), 10 parts by mass of sodium hyaluronate and 80 parts by mass of sterile water, wherein the initial adding concentration of the polysaccharide component is 15mg/ml, and the mass ratio of the bletilla striata polysaccharide to the white paeony root polysaccharide in the polysaccharide is 1: 0.3. Mixing the mixture for 60 minutes by a stirrer at the temperature of 4 ℃ and the speed of 1000 r/min; homogenizing and stirring the mixture for 20 times under 200Mpa by using a micro-jet homogenizer to obtain a uniform system as mask liquid;
(3) soaking cellulose facial mask paper in the obtained facial mask liquid for 18 hours at the temperature of 4 ℃ in an aseptic environment;
(4) vacuum drying the soaked facial mask at 50 deg.C for 24 hr until the facial mask liquid is transparent, and sealing under vacuum;
(5) and (3) sterilizing the sealed solid facial mask by a pasteur method, and sterilizing at 70 ℃ for 24 hours to obtain the polysaccharide whitening solid facial mask.
Effect example 1 determination of moisture absorption and retention properties of solid mask
Experimental methods
(1) Moisture absorption test: the solid masks prepared in examples 1 to 3 and comparative examples 1 to 4 were placed in incubators respectively at constant relative humidity of RH 43% and RH 81%, and at a temperature of 20 ℃, and the mass of each sample was weighed at regular intervals, and the moisture absorption rate was calculated as (Wn-Wo)/Wo, where: wo is the mass of the sample after it has been removed from the package, and Wn is the mass of the sample after it has been allowed to absorb moisture for a certain period of time. The time required for moisture absorption to reach saturation was calculated by model analysis.
(2) Moisture retention test: and (3) continuously placing the solid mask sample with saturated moisture absorption in a constant-temperature constant-humidity drying oven (the temperature is 20 ℃, the relative humidity is RH (43%) and RH (81%) for 24h, weighing the mass of each sample after 24h, and calculating the moisture retention rate Hn/Ho. In the formula: ho is the mass of the sample when the sample reaches saturation after moisture absorption, and Hn is the mass of the sample after the sample is placed for 24 hours.
The experimental results are as follows: the moisture absorption test data of examples 1 to 3 and comparative examples 1 to 4 are shown in table 1, and the moisture retention test data are shown in table 2. The solid mask of the present invention is demonstrated to have excellent water absorption and moisturizing properties.
TABLE 1 measurement values of moisture absorption of examples 1 to 3 and comparative examples 1 to 4
TABLE 2 measured values of moisture retention of examples 1 to 3 and comparative examples 1 to 4
The facial mask paper used by the invention is prepared by taking plant fibers as raw materials and doping cellulose nanofibrils, has the characteristics of high specific surface area and high hydrophilicity, and the facial mask liquid containing polysaccharide components is in solid-state joint with the facial mask paper, so that polysaccharide molecules are swelled in the water absorption process, and meanwhile, the hydroxyl groups of the cellulose nanofibrils and the polysaccharide molecules form hydrogen bonds to combine a large amount of water, thereby playing a strong role in water retention.
Effect example 2 detection of air permeability of solid mask
The experimental method comprises the following steps: according to the test of GB/T5453-2007, the pressure is 100Pa, and the test area is 20cm2。
The experimental results are as follows: the air permeability test data of the solid masks prepared in examples 1 to 3 and comparative examples 1 to 4 are shown in table 3.
TABLE 3 measurement values of air permeability of examples 1 to 3 and comparative examples 1 to 4
As can be seen from Table 3, the mask of the present invention has good air permeability, does not affect the normal breathing of the skin of the face during the use, and has good fitness and comfort.
Effect example 3 detection of microbial content.
The experimental method comprises the following steps: the test is carried out according to the requirements of technical Specification for cosmetic safety 2015.
The experimental results are as follows: the solid masks prepared in examples 1-3 and comparative examples 1-2 all meet the detection standard of microorganism content, wherein the detection result of example 2 is shown in table 4.
Table 4 example 2 detection of microbial content
From the above results, it can be seen that the solid mask is not conducive to the growth of microorganisms due to its storage in a dry state, and the safety of the mask is greatly ensured.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The preparation method of the polysaccharide whitening solid mask is characterized by comprising the following steps:
(1) preparation of facial mask liquid
Mixing and stirring the raw materials of the mask liquid uniformly, and then homogenizing to obtain the mask liquid; the mask liquid comprises the following components in parts by mass: 20-50 parts of polysaccharide component, 10-15 parts of sodium hyaluronate, 2-5 parts of pearl powder and 30-68 parts of water; the polysaccharide component consists of bletilla striata polysaccharide, pachyman and white peony root polysaccharide;
(2) preparation of polysaccharide whitening solid mask
Soaking cellulose facial mask paper into the facial mask liquid obtained in the step (1), then carrying out vacuum drying until the facial mask liquid is transparent, and then carrying out sterilization to obtain the polysaccharide whitening solid facial mask;
the mass ratio of the bletilla striata polysaccharide to the pachyman to the white paeony root polysaccharide in the step (1) is 1: 0.1-0.5: 0.1 to 0.5.
2. The preparation method of the polysaccharide whitening solid mask as claimed in claim 1, wherein the preparation method comprises the following steps:
the polysaccharide component in the step (1) is a polysaccharide component with the concentration of 1-500 mg/ml;
the molecular weight of the sodium hyaluronate in the step (1) is 80-200 ten thousand daltons, and the purity of the sodium hyaluronate is more than or equal to 90%;
the quantitative amount of the cellulose facial mask paper in the step (2) is 10-100 g/m2。
3. The preparation method of the polysaccharide whitening solid mask as claimed in claim 2, wherein the preparation method comprises the following steps:
the polysaccharide component in the step (1) is a polysaccharide component with the concentration of 10-15 mg/ml;
the quantitative amount of the cellulose facial mask paper in the step (2) is 60-80 g/m2。
4. The preparation method of the polysaccharide whitening solid mask as claimed in claim 1, wherein the preparation method comprises the following steps:
the bletilla striata polysaccharide, the pachyman and the white paeony root polysaccharide in the step (1) are prepared by the following methods:
(I) sun drying rhizoma Bletillae or Poria or radix Paeoniae alba, pulverizing into powder, sieving, extracting with anhydrous ethanol for defatting, vacuum filtering, repeating for more than 2 times, filtering, and vacuum drying the filter cake to obtain defatted rhizoma Bletillae or Poria or radix Paeoniae alba;
(II) adding distilled water into the degreased bletilla striata, poria cocos or white paeony root, wherein the material-liquid ratio is 1:30, extracting in a water bath at 70-80 ℃, filtering, repeating for more than 2 times, then combining the filtrates, concentrating to 1/4 volume, adding absolute ethyl alcohol until the volume fraction of the system ethyl alcohol reaches 80%, standing overnight, finally performing suction filtration, taking out a precipitate, washing, and freeze-drying to obtain crude polysaccharide;
(III) decolorizing the crude polysaccharide, purifying, concentrating, and freeze drying to obtain purified rhizoma bletilla polysaccharide, pachyman or radix Paeoniae alba polysaccharide.
5. The preparation method of the polysaccharide whitening solid mask as claimed in claim 4, wherein the preparation method comprises the following steps:
the sieving in the step (I) is 100-mesh sieving;
the degreasing time in the step (I) is 4 h;
the vacuum drying in the step (I) is vacuum drying at 50 ℃;
the extraction conditions in the step (II) are as follows: extracting in water bath at 50 deg.C for 30 min under the assistance of 400W ultrasound, and extracting in water bath at 70 deg.C for 3 hr;
the filtration in the step (II) is carried out by adopting 4 layers of 200-mesh filter cloth;
the concentration in the step (II) is performed by vacuum rotary evaporation at the temperature of 65 ℃;
the washing in the step (II) is washing by adopting acetone and diethyl ether;
the decoloring in the step (III) is realized by adopting activated carbon;
the purification in the step (III) is carried out by adopting a dialysis bag with the molecular weight cutoff of 5000 Da;
concentration as described in step (III) to 1/4 volumes;
the polysaccharide content of the purified bletilla striata polysaccharide, pachyman and white peony root polysaccharide in the step (III) is more than or equal to 97 percent.
6. The preparation method of the polysaccharide whitening solid mask as claimed in claim 1, wherein the preparation method comprises the following steps:
the stirring conditions in the step (1) are as follows: stirring for 20-60 min at a speed of 100-2500 r/min;
the homogenizing conditions in the step (1) are as follows: homogenizing for 2-20 times under 100-300 Mpa;
the impregnation conditions in the step (2) are as follows: dipping for 8-24 hours at 4 ℃ in a sterile environment;
the vacuum drying conditions in the step (2) are as follows: drying the mixture for 3 to 24 hours at the temperature of between 40 and 60 ℃.
7. The preparation method of the polysaccharide whitening solid mask as claimed in claim 1, wherein the preparation method comprises the following steps: the step (2) is followed by the steps of sealing and sterilizing the polysaccharide whitening solid mask;
the sealing is performed in a vacuum state;
the sterilization is carried out by adopting a pasteur method under the following conditions: sterilizing at 70 deg.C for 24 hr.
8. A polysaccharide whitening solid mask, which is prepared by the method of any one of claims 1 to 7.
9. Use of the polysaccharide whitening solid mask of claim 8 in the preparation of cosmetics.
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| CN104829875A (en) * | 2015-05-26 | 2015-08-12 | 安徽中医药高等专科学校 | Polysaccharide mixture with skin whitening effect and method for manufacturing polysaccharide mixture |
| CN108517719A (en) * | 2018-03-28 | 2018-09-11 | 华南理工大学 | Ultra-thin face paper of a kind of high water conservation highly-flexible and the preparation method and application thereof |
| CN109674729A (en) * | 2019-01-17 | 2019-04-26 | 罗贤义 | A kind of face mask of traditional Chinese medicine and its application method |
| CN109998947A (en) * | 2019-04-29 | 2019-07-12 | 深圳津梁生活科技有限公司 | Tremella skin care freeze-drying facial mask without preservative and preparation method thereof |
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| CN104829875A (en) * | 2015-05-26 | 2015-08-12 | 安徽中医药高等专科学校 | Polysaccharide mixture with skin whitening effect and method for manufacturing polysaccharide mixture |
| CN108517719A (en) * | 2018-03-28 | 2018-09-11 | 华南理工大学 | Ultra-thin face paper of a kind of high water conservation highly-flexible and the preparation method and application thereof |
| CN109674729A (en) * | 2019-01-17 | 2019-04-26 | 罗贤义 | A kind of face mask of traditional Chinese medicine and its application method |
| CN109998947A (en) * | 2019-04-29 | 2019-07-12 | 深圳津梁生活科技有限公司 | Tremella skin care freeze-drying facial mask without preservative and preparation method thereof |
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