CN107648168B - Puffer fish collagen mask liquid and preparation method thereof - Google Patents
Puffer fish collagen mask liquid and preparation method thereof Download PDFInfo
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- CN107648168B CN107648168B CN201711047930.2A CN201711047930A CN107648168B CN 107648168 B CN107648168 B CN 107648168B CN 201711047930 A CN201711047930 A CN 201711047930A CN 107648168 B CN107648168 B CN 107648168B
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Classifications
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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
- A61K8/99—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from microorganisms other than algae or fungi, e.g. protozoa or bacteria
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- A—HUMAN NECESSITIES
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- 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
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- 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
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- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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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
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61Q19/08—Anti-ageing preparations
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Abstract
The invention relates to a puffer fish collagen mask liquid and a preparation method thereof, wherein the mask liquid is prepared from the following raw materials in parts by weight: 5-10 parts of black tea fungus fermentation liquor, 1-5 parts of puffer fish skin collagen oligopeptide, 3-10 parts of glycerol, 0.3-1.2 parts of hyaluronic acid, 1-2 parts of water-soluble camellia seed oil, 3-8 parts of rose hydrosol, 0.5-1 part of hydroxyethyl urea, 0.5-1 part of black tea fungus fermentation membrane modifier and 60-75 parts of deionized water. The black tea fungus fermentation facial mask liquid is prepared from natural substances, can effectively clean and preserve moisture, can deeply nourish skin, repair damaged cells, improve dull complexion and whiten skin, and is a facial mask liquid product which can be used for a long time.
Description
Technical Field
The invention relates to a puffer fish collagen mask liquid and a preparation method thereof, belonging to the technical field of skin care products.
Background
With the improvement of living standard, people pay more and more attention to skin care, but a series of problems of dry skin, dark skin color and the like are caused by outdoor ultraviolet rays and dust, computer radiation in a workshop, mobile phone radiation and the like, and meanwhile, skin care products are layered endlessly. Most of facial mask products in the prior art are made of chemical medicines, so that after being used by consumers, the facial mask not only can not achieve the skin care effect, but also promotes the aging of the skin, enables the skin to be loose and generates a large amount of wrinkles; even some facial masks can cause skin diseases, and cause consumer itching. Therefore, the pursuit of people for green and healthy masks is higher and higher, so that a large number of researchers add Chinese herbal medicine components into the mask production, the use of chemical medicines is avoided, and the quality of the mask is improved; however, with the continuous improvement of the quality of life and the urgent desire of people for healthy life, the quality of products in the field of skin care is continuously improved, and meanwhile, the direction of providing higher-quality products in the field of skin care is also continuously pursued by the technicians in the field. The first step of skin care is from the face, and the fastest to take effect is the mask, which can inject the nutrients needed by the skin in a short time. Natural facial mask solutions are the choice of people today.
The globefish skin collagen oligopeptide consists of 2-12 amino acids, is rich in amino hydroxyl, has the moisture-keeping effect, and has good oxidation resistance and the effect of scavenging free radicals. Research shows that the puffer fish skin collagen oligopeptide can promote the metabolism of skin collagen, inhibit the expression of melanin, delay senility and whiten skin. The puffer fish skin collagen oligopeptide mask liquid prepared by the invention adopts natural plant extraction components, is safe and effective, and is convenient to carry.
In the prior art, researchers have studied the application of natural component extract and the like as raw materials in the field of facial masks, but the preparation cost is high due to the complex formula, more components and complex preparation process.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the puffer fish collagen facial mask liquid and the preparation method thereof, the facial mask liquid can effectively clean and moisturize skin, can also deeply nourish the skin, repair damaged cells, improve dull skin color and whiten the skin, is a natural facial mask liquid product which can be used for a long time, and has the advantages of easily obtained raw materials, easy operation, mild reaction conditions, obvious effect, low cost and the like.
The technical scheme of the invention is as follows:
a puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 5-15 parts of black tea fungus fermentation liquor, 1-5 parts of globefish skin collagen oligopeptide, 3-10 parts of glycerol, 0.3-1.2 parts of hyaluronic acid, 1-2 parts of water-soluble camellia seed oil, 3-8 parts of rose hydrosol, 0.5-1 part of hydroxyethyl urea, 0.5-1 part of black tea fungus fermentation membrane modifier and 60-80 parts of deionized water.
Further, 6-12 parts of black tea fungus fermentation liquor, 1.5-4 parts of puffer fish skin collagen oligopeptide, 5-8 parts of glycerol, 0.5-1 part of hyaluronic acid, 1.5-2 parts of water-soluble oil tea seed oil, 4-7 parts of rose hydrosol, 0.5-0.8 part of hydroxyethyl urea, 0.5-0.7 part of black tea fungus fermentation membrane modifier and 65-80 parts of deionized water.
Further, the black tea fungus fermentation liquor is prepared from the following raw materials in parts by weight: 2-8 parts of black tea, 8-12 parts of medlar, 2-6 parts of lily, 45-55 parts of white granulated sugar, 900 parts of deionized water, 1200 parts of red tea fungus mother liquor and 45-60 parts of red tea fungus mother liquor.
Further, the black tea fungus fermentation membrane modifier is prepared from the following raw materials in parts by weight: 100 parts of black tea fungus fermentation membrane solution with the mass concentration of 1.5-3%, 20-35 parts of chloroethanol and 2-10 parts of acetic acid; the black tea fungus fermentation membrane solution is prepared from the following raw materials in parts by weight: 90-110 parts of mixed aqueous solution of NaOH with the mass concentration of 5% and hydroxyethyl urea with the mass concentration of 6% and 1-3 parts of black tea fungus fermentation membrane.
Further, the water-soluble camellia oleosa seed oil is prepared from the following raw materials in parts by weight:
further, the globefish skin collagen oligopeptide is prepared from the following raw materials in parts by weight: oven-dried Fugu ocellatus skin 100 parts, NaOH with mass concentration of 0.4% and H with mass concentration of 0.6%2SO4300 parts of mixed aqueous solution, 100 parts of distilled water, 1-8 parts of trypsin with the concentration of 40U/mL and 3-7 parts of acid protease with the mass concentration of 2%.
The invention also comprises a preparation method of the puffer fish collagen mask liquid, which comprises the following steps: (1) dissolving 0.5-1 part by weight of black tea fungus fermentation membrane modifier with 60-80 parts by weight of deionized water at normal temperature; (2) adding 1.5-4 parts by weight of globefish skin collagen oligopeptide and 0.3-1.2 parts by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 5-8 parts by weight of glycerol and 0.5-1 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 1-2 parts by weight of water-soluble camellia oleosa seed oil and 5-15 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 3-8 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing black tea in 2-8 parts by weight, medlar in 8-12 parts by weight, lily in 2-6 parts by weight, white granulated sugar in 45-55 parts by weight and deionized water in 900-1200 parts by weight, boiling for 120min, standing, cooling, filtering, adding deionized water into the filtrate to keep the filtrate in 900-1200 parts by weight, uniformly mixing, adding into a container, placing into a high-temperature sterilization and re-sterilization for 20min, cooling to room temperature after the sterilization is finished, adding black tea fungus mother liquor in 45-60 parts by weight, sealing with gauze, fermenting at normal temperature and normal pressure for 6-9 days, and filtering with a screen to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) pre-cooling 90-110 parts by weight of mixed aqueous solution of 5 mass percent NaOH and 6 mass percent hydroxyethyl urea to-7 ℃; (2) rapidly adding 1-3 weight parts of black tea fungus fermentation membrane before the solution is not frozen, rapidly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain 1.5-3% black tea fungus fermentation membrane solution; (3) adding 20-35 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 1.5-3%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) adding 100 parts by weight of polyglycerol-10 and 1-2 parts by weight of saturated disodium hydrogen phosphate solution into a three-neck flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then, dropwise adding 12-20 parts by weight of camellia oleosa seed oil, adding 2 parts by weight of p-toluenesulfonic acid, and continuing to react for 1h at 60 ℃; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 1-8 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 3-7 parts by weight of acid protease with the mass concentration of 2%, adjusting the pH to 4.5, and performing enzymolysis at 50 ℃ for 8 h; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
The invention has the following beneficial effects:
the facial mask liquid is added with globefish skin collagen oligopeptide, wherein the globefish skin collagen oligopeptide consists of 2-12 amino acids, is rich in amino hydroxyl, has moisturizing effect, and has good oxidation resistance and free radical scavenging effect. Meanwhile, the puffer fish skin collagen oligopeptide can promote the metabolism of skin collagen, inhibit the expression of melanin, and has the effects of delaying aging and whitening.
The black tea fungus fermentation liquor is added into the product, the black tea fungus fermentation liquor contains rich tea polyphenol, small molecular peptide, acetic acid, heat-resistant protein, polysaccharide and other antibacterial substances, has a good inhibition effect on common pathogenic bacteria such as escherichia coli, salmonella enteritidis, shigella dysenteriae, listeria monocytogenes, pseudomonas fluorescens, staphylococcus aureus and the like, has no drug resistance on the bacteria, is not added with artificial preservatives, has a good anticorrosion effect, has good biocompatibility of components and human skin, and has no uncomfortable effects such as allergy, stimulation and the like. Meanwhile, the black tea fungus fermentation liquor contains rich tea polyphenol, amino acid and other components, and has strong oxidation resistance. The product has the effects of repairing cells and protecting mucosa.
The product is added with a black tea fungus fermentation membrane modifier, the black tea fungus fermentation membrane is natural cellulose generated by black tea fungus fermentation, has the same chemical composition with plant cellulose, belongs to typical biological nano-cellulose, and has the characteristics of high water retention, high tensile strength and the like. The black tea fungus fermentation membrane modifier is modified on the basis of the black tea fungus fermentation membrane, cellulose polysaccharide and protein in the black tea fungus fermentation membrane are modified into active substances such as small molecular peptides, oligosaccharides and the like, so that the water retention property of the black tea fungus fermentation membrane modifier is maintained, the modified small molecular bioactive substances can be well combined with skin, and the black tea fungus fermentation membrane modifier has good effects of resisting bacteria, resisting wrinkles, whitening and the like.
The water-soluble oil tea seed oil is modified on the basis of the oil tea seed oil, and the water-insoluble oil tea seed oil is modified to be soluble in water, so that the oil tea seed oil can be matched with other components in the facial mask liquid, and the anti-aging and anti-oxidation effects of the facial mask liquid are improved.
The puffer fish collagen mask liquid disclosed by the invention can be effectively cleaned and moisturized, can deeply nourish skin, repair damaged cells, improve dull skin color and whiten skin, and is a mask liquid product which can be used for a long time.
In addition, the invention has the advantages of easily obtained raw materials, easy operation, mild reaction conditions, obvious effect, low cost and the like.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
A puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 7 parts of black tea fungus fermentation liquor, 2 parts of globefish skin collagen oligopeptide, 7 parts of glycerol, 0.8 part of hyaluronic acid, 1.5 parts of water-soluble camellia seed oil, 4.5 parts of rose hydrosol, 0.6 part of hydroxyethyl urea, 0.5 part of black tea fungus fermentation membrane modifier and 76.1 parts of deionized water.
A preparation method of puffer fish collagen mask liquid comprises the following steps: (1) dissolving 0.5 weight part of black tea fungus fermentation membrane modifier with 76.1 weight parts of deionized water at normal temperature; (2) adding 2 parts by weight of globefish skin collagen oligopeptide and 0.8 part by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 7 parts by weight of glycerol and 0.6 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 1.5 parts by weight of water-soluble camellia oleosa seed oil and 7 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 4.5 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing and boiling 2 parts by weight of black tea, 8 parts by weight of medlar, 2 parts by weight of lily, 45 parts by weight of white granulated sugar and 900 parts by weight of deionized water for 100min, standing, cooling, filtering, adding the deionized water into the filtrate to keep the filtrate at 900 parts by weight, uniformly mixing, adding the filtrate into a container, placing the container into a high-temperature sterilization and over-sterilization container for 20min, cooling to room temperature after sterilization, adding 45 parts by weight of black tea fungus mother liquor, sealing the container with gauze, fermenting for 7 days at normal temperature and normal pressure, and filtering with a screen to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) pre-cooling 95 parts by weight of mixed aqueous solution of 5 mass percent NaOH and 6 mass percent hydroxyethyl urea to-7 ℃; (2) rapidly adding 2 parts by weight of black tea fungus fermentation membrane before the solution is not frozen, rapidly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain black tea fungus fermentation membrane solution with mass concentration of 2%; (3) adding 25 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 2%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) 100 parts by weight of polyglycerol-10 and 2 parts by weight of saturated disodium hydrogen phosphate solution are added into a three-neck flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then 14 parts by weight of camellia seed oil is dripped, 2 parts by weight of p-toluenesulfonic acid is added, and the reaction is continued at 60 ℃ for 1 hour; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 6 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 4 parts by weight of acid protease with the mass concentration of 2%, adjusting the pH value to 4.5,performing enzymolysis at 50 deg.C for 8 hr; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
Example 2
A puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 7 parts of black tea fungus fermentation liquor, 2 parts of globefish skin collagen oligopeptide, 5 parts of glycerol, 0.6 part of hyaluronic acid, 2 parts of water-soluble camellia seed oil, 4.5 parts of rose hydrosol, 0.8 part of hydroxyethyl urea, 0.5 part of black tea fungus fermentation membrane modifier and 77.6 parts of deionized water.
A preparation method of puffer fish collagen mask liquid comprises the following steps: (1) dissolving 0.5 weight part of black tea fungus fermentation membrane modifier with 77.6 weight parts of deionized water at normal temperature; (2) adding 2 parts by weight of globefish skin collagen oligopeptide and 0.6 part by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 5 parts by weight of glycerol and 0.8 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 2 parts by weight of water-soluble camellia oleosa seed oil and 7 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 4.5 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing 3 parts by weight of black tea, 10 parts by weight of medlar, 4 parts by weight of lily, 50 parts by weight of white granulated sugar and 1000 parts by weight of deionized water, boiling for 110min, standing, cooling, filtering, adding deionized water into the filtrate to keep the filtrate at 1000 parts by weight, uniformly mixing, adding into a container, placing into a high-temperature sterilization and over-sterilization container for 20min, cooling to room temperature after sterilization, adding 50 parts by weight of black tea fungus mother liquor, sealing with gauze, fermenting for 8 days at normal temperature and normal pressure, and filtering with a screen mesh to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) pre-cooling 95 parts by weight of mixed aqueous solution of 5 mass percent NaOH and 6 mass percent hydroxyethyl urea to-7 ℃; (2) quickly adding 1.5 weight parts of black tea fungus fermentation membrane before the solution is not frozen, quickly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain 1.5-3% black tea fungus fermentation membrane solution; (3) adding 20 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 1.5%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) 100 parts by weight of polyglycerol-10 and 1.5 parts by weight of saturated disodium hydrogen phosphate solution are added into a three-necked flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then dropwise adding 15 parts by weight of camellia oleosa seed oil, adding 2 parts by weight of p-toluenesulfonic acid, and continuing to react for 1h at 60 ℃; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 3 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 4 parts by weight of 2% acid protease, adjusting pH to 4.5, and performing enzymolysis at 50 deg.C for 8 h; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
Example 3
A puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 8 parts of black tea fungus fermentation liquor, 2.5 parts of globefish skin collagen oligopeptide, 6 parts of glycerol, 0.7 part of hyaluronic acid, 1.8 parts of water-soluble camellia seed oil, 4 parts of rose hydrosol, 0.6 part of hydroxyethyl urea, 0.7 part of black tea fungus fermentation membrane modifier and 75.7 parts of deionized water.
A preparation method of puffer fish collagen mask liquid comprises the following steps: (1) dissolving 0.7 part by weight of black tea fungus fermentation membrane modifier in deionized water at normal temperature; (2) adding 2.5 parts by weight of globefish skin collagen oligopeptide and 0.7 part by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 6 parts by weight of glycerol and 0.6 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 1.8 parts by weight of water-soluble camellia oleosa seed oil and 8 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 4 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing 5 parts by weight of black tea, 10 parts by weight of medlar, 5 parts by weight of lily, 48 parts by weight of white granulated sugar and 1000 parts by weight of deionized water, boiling for 110min, standing, cooling, filtering, adding deionized water into the filtrate to keep the filtrate at 1000 parts by weight, uniformly mixing, adding into a container, placing into a high-temperature sterilization and over-sterilization container for 20min, cooling to room temperature after sterilization, adding 50 parts by weight of black tea fungus mother liquor, sealing with gauze, fermenting for 8 days at normal temperature and normal pressure, and filtering with a screen mesh to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) precooling 100 parts by weight of mixed aqueous solution of NaOH with the mass concentration of 5% and hydroxyethyl urea with the mass concentration of 6% to-7 ℃; (2) rapidly adding 1-3 weight parts of black tea fungus fermentation membrane before the solution is not frozen, rapidly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain 3% black tea fungus fermentation membrane solution; (3) adding 30 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 3%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) 100 parts by weight of polyglycerol-10 and 1.5 parts by weight of saturated disodium hydrogen phosphate solution are added into a three-necked flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then, 18 parts by weight of camellia oleosa seed oil is dropwise added, 2 parts by weight of p-toluenesulfonic acid is added, and the reaction is continued at 60 ℃ for 1 h; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 5 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 6 parts by weight of 2% acid protease, adjusting pH to 4.5, and performing enzymolysis at 50 deg.C for 8 h; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
Example 4
A puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 10 parts of black tea fungus fermentation liquor, 3 parts of globefish skin collagen oligopeptide, 5 parts of glycerol, 1 part of hyaluronic acid, 1.5 parts of water-soluble camellia seed oil, 4 parts of rose hydrosol, 0.5 part of hydroxyethyl urea, 0.6 part of black tea fungus fermentation membrane modifier and 75.4 parts of deionized water.
A preparation method of puffer fish collagen mask liquid comprises the following steps: (1) dissolving 0.6 part by weight of black tea fungus fermentation membrane modifier in deionized water at normal temperature; (2) adding 3 parts by weight of globefish skin collagen oligopeptide and 1 part by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 5 parts by weight of glycerol and 0.5 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 1.5 parts by weight of water-soluble camellia oleosa seed oil and 10 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 4 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing 6 parts by weight of black tea, 11 parts by weight of medlar, 4 parts by weight of lily, 50 parts by weight of white granulated sugar and 1100 parts by weight of deionized water, boiling for 110min, standing, cooling, filtering, adding deionized water into the filtrate to keep the weight of the filtrate at 1100 parts, uniformly mixing, adding into a container, placing into a high-temperature sterilization and over-sterilization container for 20min, cooling to room temperature after sterilization, adding 55 parts by weight of black tea fungus mother liquor, sealing with gauze, fermenting for 8 days at normal temperature and normal pressure, and filtering with a screen mesh to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) precooling 100 parts by weight of mixed aqueous solution of NaOH with the mass concentration of 5% and hydroxyethyl urea with the mass concentration of 6% to-7 ℃; (2) rapidly adding 2 parts by weight of black tea fungus fermentation membrane before the solution is not frozen, rapidly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain black tea fungus fermentation membrane solution with mass concentration of 2%; (3) adding 30 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 2%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) 100 parts by weight of polyglycerol-10 and 2 parts by weight of saturated disodium hydrogen phosphate solution are added into a three-neck flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then, 19 parts by weight of camellia seed oil is dripped, 2 parts by weight of p-toluenesulfonic acid is added, and the reaction is continued at 60 ℃ for 1 hour; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 6 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 6 parts by weight of 2% acid protease, adjusting pH to 4.5, and performing enzymolysis at 50 deg.C for 8 h; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
Example 5
A puffer fish collagen mask liquid is prepared from the following raw materials in parts by weight: 15 parts of black tea fungus fermentation liquor, 4 parts of globefish skin collagen oligopeptide, 8 parts of glycerol, 1.2 parts of hyaluronic acid, 2 parts of water-soluble camellia seed oil, 8 parts of rose hydrosol, 1 part of hydroxyethyl urea, 1 part of black tea fungus fermentation membrane modifier and 80 parts of deionized water.
A preparation method of puffer fish collagen mask liquid comprises the following steps: (1) dissolving 1 part by weight of black tea fungus fermentation membrane modifier in 80 parts by weight of deionized water at normal temperature; (2) adding 4 parts by weight of globefish skin collagen oligopeptide and 1.2 parts by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 8 parts by weight of glycerol and 1 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 2 parts by weight of water-soluble camellia oleosa seed oil and 15 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 8 parts by weight of rose hydrosol, and uniformly mixing to obtain the mask liquid.
Further, the black tea fungus fermentation liquor is prepared by the following steps: mixing 8 parts by weight of black tea, 12 parts by weight of medlar, 6 parts by weight of lily, 55 parts by weight of white granulated sugar and 1200 parts by weight of deionized water, boiling for 120min, standing, cooling, filtering, adding the deionized water into the filtrate to keep the filtrate at 1200 parts by weight, uniformly mixing, adding into a container, placing into a high-temperature sterilization and over-sterilization container for 20min, cooling to room temperature after sterilization, adding 60 parts by weight of black tea fungus mother liquor, sealing with gauze, fermenting at normal temperature and normal pressure for 9 days, and filtering with a screen to obtain black tea fungus fermentation liquor.
Further, the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) pre-cooling 110 parts by weight of mixed aqueous solution of 5 mass percent NaOH and 6 mass percent hydroxyethyl urea to-7 ℃; (2) quickly adding 3 parts by weight of black tea fungus fermentation membrane before the solution is not frozen, quickly stirring at room temperature for 5min, and standing at-7 ℃ for 20min to obtain a black tea fungus fermentation membrane solution with the mass concentration of 3%; (3) adding 35 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 3%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance.
Further, the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) 100 parts by weight of polyglycerol-10 and 2 parts by weight of saturated disodium hydrogen phosphate solution are added into a three-neck flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then, 20 parts by weight of camellia seed oil is dripped, 2 parts by weight of p-toluenesulfonic acid is added, and the reaction is continued at 60 ℃ for 1 hour; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
Further, the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding into a reaction bottle, adding 300 parts by weight of the mixture with the mass concentration of 0.4%NaOH and 0.6% H by mass2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 8 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 7 parts by weight of acid protease with the mass concentration of 2%, adjusting the pH to 4.5, and performing enzymolysis at the temperature of 50 ℃ for 8 hours; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
The facial mask liquid prepared in example 1 is taken as an example, 20 female volunteers are randomly selected for testing, and the moisturizing effect, the anti-wrinkle effect and the anti-allergy and soothing effect of the facial mask liquid are observed.
The facial mask liquid has an obvious moisturizing effect, 20 female volunteers are randomly selected to use the facial mask liquid for 3 weeks, a VISIA full-face analyzer is used for detecting and finding that the skin color is remarkably improved, and a common glycerin moisturizing liquid is used as a control, and the result is shown in Table 1.
TABLE 1 skin hydration Change
The facial mask liquid has an obvious anti-wrinkle effect, after 20 female volunteers use the facial mask liquid for 8 weeks, the VISIA full-face analyzer is used for detecting and finding that the wrinkle quantity is remarkably improved, and the results are shown in Table 2 by taking common glycerin moisturizing liquid as a control.
TABLE 2 variation in the number of skin wrinkles
The facial mask liquid has obvious anti-allergy and relieving effects, 20 female volunteers use the facial mask liquid for 8 weeks, and use common glycerin moisturizing liquid as a control to investigate the improvement of the lactic acid stimulation pain degree after using the facial mask liquid, and the results are shown in table 3.
TABLE 3 reduction of lactic acid stimulated pain levels
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. A puffer fish collagen mask liquid is characterized by being prepared from the following raw materials in parts by weight: 5-15 parts of black tea fungus fermentation liquor, 1-5 parts of globefish skin collagen oligopeptide, 3-10 parts of glycerol, 0.3-1.2 parts of hyaluronic acid, 1-2 parts of water-soluble camellia seed oil, 3-8 parts of rose hydrosol, 0.5-1 part of hydroxyethyl urea, 0.5-1 part of black tea fungus fermentation membrane modifier and 60-80 parts of deionized water; the black tea fungus fermentation membrane modifier is prepared from the following raw materials in parts by weight: 100 parts of black tea fungus fermentation membrane solution with the mass concentration of 1.5-3%, 20-35 parts of chloroethanol and 2-10 parts of acetic acid; the black tea fungus fermentation membrane solution is prepared from the following raw materials in parts by weight: 90-110 parts of mixed aqueous solution of NaOH with the mass concentration of 5% and hydroxyethyl urea with the mass concentration of 6% and 1-3 parts of black tea fungus fermentation membrane; the water-soluble camellia seed oil is prepared from the following raw materials in parts by weight: polyglycerol-10100 parts; 1-2 parts of saturated disodium hydrogen phosphate solution; 12-20 parts of camellia seed oil; 2 parts of p-toluenesulfonic acid; 1-3 parts of saturated sodium bicarbonate solution.
2. The puffer fish collagen mask solution according to claim 1, wherein the black tea fungus fermentation broth is prepared from the following raw materials in parts by weight: 2-8 parts of black tea, 8-12 parts of medlar, 2-6 parts of lily, 45-55 parts of white granulated sugar, 900 parts of deionized water and 1200 parts of black tea fungus mother liquor and 45-60 parts of black tea fungus mother liquor.
3. The puffer fish collagen mask solution of claim 1, wherein the puffer fish skin is a globefish skin mask solutionThe collagen oligopeptide is prepared from the following raw materials in parts by weight: oven-dried Fugu ocellatus skin 100 parts, NaOH with mass concentration of 0.4% and H with mass concentration of 0.6%2SO4300 parts of mixed aqueous solution, 100 parts of distilled water, 1-8 parts of trypsin with the concentration of 40U/mL and 3-7 parts of acid protease with the mass concentration of 2%.
4. A preparation method of puffer fish collagen mask liquid is characterized by comprising the following steps: (1) dissolving 0.5-1 part by weight of black tea fungus fermentation membrane modifier with 60-80 parts by weight of deionized water at normal temperature; (2) adding 1.5-4 parts by weight of globefish skin collagen oligopeptide and 0.3-1.2 parts by weight of hyaluronic acid, heating to 60 ℃, stirring to dissolve and uniformly mixing; (3) keeping the temperature at 60 ℃, adding 5-8 parts by weight of glycerol and 0.5-1 part by weight of hydroxyethyl urea, stirring to dissolve and uniformly mixing; (4) cooling to room temperature, sequentially adding 1-2 parts by weight of water-soluble camellia oleosa seed oil and 5-15 parts by weight of black tea fungus fermentation liquor, and uniformly mixing; (5) adding 3-8 parts by weight of rose hydrosol, and uniformly mixing to obtain a mask liquid; the black tea fungus fermentation membrane modifier is prepared by the following steps: (1) pre-cooling 90-110 parts by weight of mixed aqueous solution of 5 mass percent NaOH and 6 mass percent hydroxyethyl urea to-7 ℃; (2) rapidly adding 1-3 weight parts of black tea fungus fermentation membrane before the solution is not frozen, rapidly stirring at room temperature for 5min, and standing at-7 deg.C for 20min to obtain 1.5-3% black tea fungus fermentation membrane solution; (3) adding 20-35 parts by weight of chloroethanol into 100 parts by weight of black tea fungus fermentation membrane solution with the mass concentration of 1.5-3%, reacting for 2 hours at room temperature, heating to 50 ℃ for reaction for 2 hours, adding acetic acid for neutralization to neutrality, and stopping reaction; (4) after the solution after reaction is dialyzed, centrifuging for 10min at 400r/min for separation; (5) collecting supernatant, and vacuum drying to obtain black tea fungus fermentation membrane modified substance; the water-soluble camellia oleosa seed oil is prepared by the following steps: (1) adding 100 parts by weight of polyglycerol-10 and 1-2 parts by weight of saturated disodium hydrogen phosphate solution into a three-neck flask provided with a spherical reflux condenser pipe; (2) stirring in water bath at 60 ℃ for 1 h; (3) then, dropwise adding 12-20 parts by weight of camellia oleosa seed oil, adding 2 parts by weight of p-toluenesulfonic acid, and continuing to react for 1h at 60 ℃; (4) dropwise adding saturated sodium bicarbonate solution until the pH value of the solution is 6.5-7.5; (5) and (3) cooling the liquid, transferring the liquid into a separating funnel, and directly separating to obtain a lower-layer solution, namely the water-soluble camellia seed oil.
5. The method for preparing a puffer fish collagen mask solution according to claim 4, wherein the black tea fungus fermentation broth is prepared by the following steps: mixing black tea in 2-8 parts by weight, medlar in 8-12 parts by weight, lily in 2-6 parts by weight, white granulated sugar in 45-55 parts by weight and deionized water in 900-1200 parts by weight, boiling for 120min, standing, cooling, filtering, adding deionized water into the filtrate to keep the filtrate in 900-1200 parts by weight, uniformly mixing, adding into a container, placing into a high-temperature sterilization and re-sterilization for 20min, cooling to room temperature after the sterilization is finished, adding black tea fungus mother liquor in 45-60 parts by weight, sealing with gauze, fermenting at normal temperature and normal pressure for 6-9 days, and filtering with a screen to obtain black tea fungus fermentation liquor.
6. The method of preparing a puffer fish collagen mask solution according to claim 4, wherein the puffer fish skin collagen oligopeptide is prepared by the following steps: (1) cleaning globefish skin, and air drying surface water; (2) weighing 100 parts by weight, adding the weighed 100 parts by weight into a reaction bottle, adding 300 parts by weight of NaOH with the mass concentration of 0.4 percent and H with the mass concentration of 0.6 percent2SO4Treating with mixed water solution, and washing with water to neutrality; (3) adding 100 parts by weight of distilled water, stirring and extracting at the constant temperature of 60 ℃ for 2 hours, cooling to room temperature, and filtering to remove residues to obtain a globefish skin collagen extracting solution for later use; (4) adding 1-8 parts by weight of trypsin with the concentration of 40U/mL into the globefish skin collagen extracting solution, adjusting the pH to 8, and carrying out enzymolysis for 6h at 40 ℃; (5) adding 3-7 parts by weight of acid protease with the mass concentration of 2%, adjusting the pH to 4.5, and performing enzymolysis at 50 ℃ for 8 h; (6) then enzyme deactivation and filtration are carried out to obtain the globefish skin collagen oligopeptide extract, and then freeze drying is carried out to obtain powder.
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