CN115670942B - Freeze-dried eye mask and preparation method thereof - Google Patents
Freeze-dried eye mask and preparation method thereof Download PDFInfo
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- CN115670942B CN115670942B CN202211200133.4A CN202211200133A CN115670942B CN 115670942 B CN115670942 B CN 115670942B CN 202211200133 A CN202211200133 A CN 202211200133A CN 115670942 B CN115670942 B CN 115670942B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000004475 Arginine Substances 0.000 claims abstract description 42
- 239000004472 Lysine Substances 0.000 claims abstract description 42
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- 229920001184 polypeptide Polymers 0.000 claims abstract description 42
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- 102000004196 processed proteins & peptides Human genes 0.000 claims abstract description 42
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- 108010035532 Collagen Proteins 0.000 claims abstract description 41
- 229920002385 Sodium hyaluronate Polymers 0.000 claims abstract description 41
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- 229940010747 sodium hyaluronate Drugs 0.000 claims abstract description 41
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- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 description 1
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- SSISHJJTAXXQAX-ZETCQYMHSA-N L-ergothioneine Chemical compound C[N+](C)(C)[C@H](C([O-])=O)CC1=CNC(=S)N1 SSISHJJTAXXQAX-ZETCQYMHSA-N 0.000 description 1
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Landscapes
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
- Medicinal Preparation (AREA)
Abstract
The application is applicable to the technical field of skin care products, and provides a freeze-dried eye mask and a preparation method thereof, wherein the freeze-dried eye mask comprises the following main components: sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, and arginine/lysine polypeptides; wherein, the mass ratio of the sodium hyaluronate, the carnosine, the centella asiatica extract, the cyclodextrin, the collagen, the acetyl hexapeptide-8 and the arginine/lysine polypeptide is (0.05-0.5): (0.0001-0.2): (0.05-0.4): (0.2-0.6): (0.01-0.2): (0.008-0.05): (0.0001-0.1). The application has no carrier and no traditional excipient, can realize the conversion of 100% active ingredients, and has excellent instant and long-acting wrinkle-removing effects.
Description
Technical Field
The application belongs to the technical field of skin care products, and particularly relates to a freeze-dried eye mask and a preparation method thereof.
Background
In recent years, various problems of human skin, especially problems of eyes such as dry eyes, fish tail lines, eye bags, black eyes and the like, are caused by comprehensive factors such as excessive environmental and living pressure, improper use of skin care products, electronic products, age and the like, so that people pay more attention to the efficacy and safety of the eye skin care products.
At present, the form of the eye mask is also in a form that the eye mask cloth is taken as a carrier, essence is soaked on the eye mask cloth, firstly, the wet mask generally contains components which do not greatly help to the efficacy, such as a thickening agent, a preservative, a bacteriostat and the like, and the components are numerous, so that unpredictable potential risks, such as stinging, itching, swelling and the like, can be brought to the skin; secondly, the eye mask cloth of the wet mask has little help to the efficacy, most of the eye mask cloth can be thrown away after being applied, so that the resource waste is caused, the environment-friendly concept is not met, and in addition, most of freeze-dried products adopt the mask cloth as a carrier.
Disclosure of Invention
The embodiment of the application aims to provide a freeze-dried eye mask, which aims to solve the problems that the existing eye mask has poor skin care effect and the environment protection is not facilitated by taking a film cloth as a carrier.
The embodiment of the application is realized in such a way that the freeze-dried eye mask comprises the following main components:
sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, and arginine/lysine polypeptides;
wherein, the mass ratio of the sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8 and arginine/lysine polypeptide is (0.05-0.5): (0.0001-0.2): (0.05-0.4): (0.2-0.6): (0.01-0.2): (0.008-0.05): (0.0001-0.1).
Another object of an embodiment of the present application is a method for preparing a frozen dry eye film, comprising:
weighing all the raw materials according to the formula of the frozen dry eye film for standby;
uniformly mixing water and sodium hyaluronate, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide are completely dissolved to obtain a first mixed solution;
adding collagen into the first mixed solution, stirring to obtain uniform liquid, and freeze-drying in a freeze dryer according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 to-45 ℃ and keeping the temperature for 2 to 4 hours;
(2) Once sublimating, setting the temperature to-10 to-15 ℃, heating for 0.5-2 h, keeping for 5-8 h, and vacuum degree 0.1-0.18;
(3) Setting the temperature to-3-2 ℃, heating for 0.5-1.5 h, keeping for 3-5 h, and vacuum degree 0.1-0.18;
(4) And (3) analyzing and drying, wherein the temperature is set to be 20-30 ℃, the temperature rising time is 0.5-1 h, the holding time is 2-4 h, and the vacuum degree is 0.02-0.08.
Wherein, the water is a common additive solvent in the vacuum freeze-drying freezing technology, and the mass ratio of the water is generally 80.00-98.99%.
The frozen dry eye film provided by the embodiment of the application has no carrier and no traditional excipient, and can realize the conversion of 100% of active ingredients; according to the application, sodium hyaluronate and collagen are used as main components of a skeleton to facilitate large-area lamellar forming of freeze-dried eye films, powdery non-hygroscopic small molecular compounds such as carnosine and centella asiatica extract are used as fillers, acetyl hexapeptide-8, arginine/lysine polypeptide and the like are used as active substances, and a specific freeze-drying curve program is adopted to obtain the frozen dry eye film product, wherein the appearance of the frozen dry eye film product is a loose porous lamellar structure with larger area, so that the frozen dry eye film product can cover and fit the skin at the lower part of the periphery of eyes, is light, thin, not easy to break, has toughness, has high dissolution rate in water addition, is not sticky in skin feel and good stability; on the other hand, the application has excellent instant and long-acting wrinkle-removing effect, the number of wrinkles around eyes is reduced by 13.97% after the product is used for 14 days, the score of skin wrinkles around eyes is reduced by about 35.73%, the skin elasticity is improved by 3.9%, and the skin glossiness is improved by 12.54%. In addition, the frozen dry eye film is a dehydrated dry object, and is vacuum-packed, so that the frozen dry eye film can be stored for a long time without adding a preservative, and the problem of skin allergy caused by adding the preservative in the conventional cosmetics is avoided.
Drawings
Fig. 1 shows the effect of the frozen dry eye film provided in the embodiment of the application within 14 days.
Detailed Description
The present application will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides the freeze-dried eye mask, which is free of a carrier and a traditional excipient and can realize the conversion of 100% of active ingredients in order to solve the problems that the existing eye mask has poor skin care effect and the film cloth is not beneficial to environmental protection because of being used as the carrier; specifically, the application uses sodium hyaluronate and collagen as main components of a framework to facilitate sheet-shaped formation of freeze-dried eye mask, uses powdery non-hygroscopic small molecular compounds such as carnosine, centella asiatica extract and the like as filling agents, and simultaneously uses acetyl hexapeptide-8, arginine/lysine polypeptide and the like as active substances, and the appearance of the freeze-dried eye mask product can be a loose porous sheet-shaped structure through a specific freeze-drying curve procedure, thus the freeze-dried eye mask is not easy to break, has toughness, has high dissolution speed in water addition, is not sticky in skin feel and has good stability; on the other hand, the application has excellent instant and long-acting wrinkle-removing effect, the number of wrinkles around eyes is reduced by 13.97% after the product is used for 14 days, the score of skin wrinkles around eyes is reduced by about 35.73%, the skin elasticity is improved by 3.9%, and the skin glossiness is improved by 12.54%.
The application provides a freeze-dried eye mask, which comprises the following main components:
sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, and arginine/lysine polypeptides;
wherein, the mass ratio of the sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8 and arginine/lysine polypeptide is (0.05-0.5): (0.0001-0.2): (0.05-0.4): (0.2-0.6): (0.01-0.2): (0.008-0.05): (0.0001-0.1).
Sodium hyaluronate is an excellent humectant and moisture absorber, and can form a breathable water film on the surface of skin to realize surface water locking and soften the stratum corneum; the acetyl hexapeptide-8 multiplied by arginine/lysine polypeptide aims at muscle layers, and various expression lines are reduced by inhibiting excessive contraction of muscles; carnosine has the effects of resisting oxidation, preventing free radical damage, maintaining normal metabolism of skin, accelerating the excretion of metabolites from skin, homogenizing skin complexion and improving skin self-resistance; centella Asiatica (CENTELLAASIATICA) extracts can remarkably promote synthesis of fibroblast and skin collagen, and stimulate granulation growth, so that wound healing is facilitated; through scientific and reasonable proportion of the components, the effects of supplementing water and preserving moisture, promoting collagen production, resisting saccharification, inhibiting excessive muscle contraction and the like can be cooperatively exerted, and the complete absorption effect is realized.
In some embodiments, the mass ratio of sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, arginine/lysine polypeptide is (0.12-0.4): (0.0001-0.15): (0.1-0.3): (0.4-0.6): (0.04-0.18): (0.008-0.05): (0.0001-0.1).
In some embodiments, the mass ratio of sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, arginine/lysine polypeptide is (0.12-0.2): (0.0001-0.101): (0.1-0.24): (0.56-0.6): (0.12-0.18): (0.008-0.05): (0.0001-0.1).
In some embodiments, the mass ratio of sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, arginine/lysine polypeptide is 0.2:0.101:0.24:0.56:0.12:0.05:0.1.
the basic component for forming the frozen dry eye film provided by the application can be added with other functional components with skin care assistance in reasonable content by a person skilled in the art. Specifically, in the cosmetic field, the functional components may have a moisturizing and moisturizing function, a whitening and brightening function, a tightening and anti-wrinkle function, and the like, for example, the moisturizing and moisturizing components may be trehalose, dendrobium candidum (Dendrobium Candidum) stem extract, tremella (tremella fucifolia) fruiting body extract, yeast/mother-of-pearl fermentation lysate filtrate, inositol, and the like; the whitening and brightening component can be arbutin, 3-o-ethyl ascorbic acid, nonapeptide-1, glutathione, glycyrrhiza glabra (GLYCYRRHIZA GLABRA) root extract and the like; the anti-wrinkle tightening component can be pentapeptide-3, palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, hydrolyzed flax extract, ergothioneine, DNA sodium, lysate of fermentation product of the two-split yeast and the like, and the type of the functional component is not particularly limited in the application.
The embodiment of the application provides a preparation method of a freeze-dried eye mask, which comprises the following steps:
weighing all the raw materials according to the formula of the frozen dry eye film for standby;
uniformly mixing water and sodium hyaluronate, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide are completely dissolved to obtain a first mixed solution;
adding collagen into the first mixed solution, stirring to obtain uniform liquid, and freeze-drying in a freeze dryer according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 to-45 ℃ and keeping the temperature for 2 to 4 hours;
(2) Once sublimating, setting the temperature to-10 to-15 ℃, heating for 0.5-2 h, keeping for 5-8 h, and vacuum degree 0.1-0.18;
(3) Setting the temperature to-3-2 ℃, heating for 0.5-1.5 h, keeping for 3-5 h, and vacuum degree 0.1-0.18;
(4) And (3) analyzing and drying, wherein the temperature is set to be 20-30 ℃, the temperature rising time is 0.5-1 h, the holding time is 2-4 h, and the vacuum degree is 0.02-0.08.
The carrier-free anti-wrinkle frozen dry eye film capable of being completely absorbed can be prepared, has a loose and porous shape like a flaky structure of eyes, can be matched for use according to different living scenes, can be completely absorbed by adding water or matching with an eye mask and a face mask, and realizes that the complete absorption of a product requires a plurality of screening of raw materials and proportions of the product; when the product is packaged, the product can be realized by only matching with a simple plastic suction and aluminum foil bag; the freeze-dried products in the market are mostly freeze-dried powder and freeze-dried ampoules, but the eye tablet structure is few, no carrier exists, no traditional excipient exists, and 100% of active ingredients are converted.
In some embodiments, after the water and the sodium hyaluronate are mixed uniformly, carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8, arginine/lysine polypeptide are added, and stirred until the mixture is completely dissolved, so as to obtain a first mixed solution, which comprises the following steps:
mixing water and sodium hyaluronate, heating to 80-85deg.C, maintaining the temperature for 30min, cooling to 30-60deg.C, adding carnosine, herba Centellae extract, cyclodextrin, acetyl hexapeptide-8, and arginine/lysine polypeptide, and stirring to dissolve completely to obtain first mixed solution.
In some embodiments, the step of adding collagen to the first mixed solution, stirring to a uniform liquid, and freeze-drying in a freeze dryer according to a preset freeze-drying curve procedure to obtain a freeze-dried eye mask includes:
and continuously cooling the first mixed solution to 10-25 ℃, adding collagen, stirring to be uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying according to a preset freeze-drying curve program to obtain the freeze-dried eye mask.
In some embodiments, the preset lyophilization curve program is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 to-45 ℃ and keeping the temperature for 2 to 3 hours;
(2) Once sublimating, setting the temperature to-10 to-15 ℃, heating for 1-2 h, keeping for 6-8 h, and vacuum degree of 0.15-0.16;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and controlling the vacuum degree to 0.15-0.16;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
In some embodiments, the preset lyophilization curve program is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.15;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.15;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
Examples of certain embodiments of the application are given below and are not intended to limit the scope of the application.
In addition, it should be noted that the numerical values set forth in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be construed as a divisor rather than an absolute precise numerical value due to measurement errors and experimental operation problems that cannot be avoided. For example, it should be understood that the weight value of each raw material in each coating layer of each embodiment may have an error of ±2% or ±1%, due to an error of the weighing instrument.
Example 1
In the embodiment, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.2%, carnosine 0.101%, centella asiatica extract 0.24%, cyclodextrin 0.56%, collagen 0.12%, acetyl hexapeptide-80.05%, arginine/lysine polypeptide 0.1%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.15;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.15;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
Example 2
In the embodiment, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.12%, carnosine 0.0001%, centella asiatica extract 0.1%, cyclodextrin 0.6%, collagen 0.18%, acetyl hexapeptide-80.008%, arginine/lysine polypeptide 0.0001%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-45 ℃ and keeping the temperature for 3 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.15;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.15;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
Example 3
In the embodiment, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.4%, carnosine 0.15%, centella asiatica extract 0.3%, cyclodextrin 0.4%, collagen 0.04%, acetyl hexapeptide-80.02%, arginine/lysine polypeptide 0.05%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One sublimation, setting the temperature to-15 ℃, heating for 2 hours, keeping for 8 hours, and carrying out vacuum degree of 0.16;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.16;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
Example 4
In the embodiment, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.3%, carnosine 0.2%, centella asiatica extract 0.4%, cyclodextrin 0.2%, collagen 0.08%, acetyl hexapeptide-80.01%, arginine/lysine polypeptide 0.02%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.18;
(3) Setting the temperature to-3 ℃, heating for 1.5h, keeping for 5h, and carrying out vacuum degree of 0.18;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
Example 5
In the embodiment, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.5%, carnosine 0.0001%, centella asiatica extract 0.4%, cyclodextrin 0.2%, collagen 0.01%, acetyl hexapeptide-80.05%, arginine/lysine polypeptide 0.0001%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-45 ℃ and keeping the temperature for 4 hours;
(2) One sublimation, setting the temperature to-15 ℃, heating for 1.5h, keeping for 8h, and vacuum degree being 0.1;
(3) Setting the temperature to 2 ℃, heating for 1.5h, keeping for 5h, and carrying out vacuum degree to 0.1;
(4) And (3) performing analytical drying, wherein the temperature is set to be 30 ℃, the heating time is 1h, the holding time is 4h, and the vacuum degree is 0.08.
The frozen dry eye films prepared in examples 1 to 5 were subjected to the appearance, solubility, stability and skin care effect test according to the test methods of table 1 below, and the test results are shown in table 2.
TABLE 1
TABLE 2
From table 2, it is clear that the macromolecular structure of sodium hyaluronate and collagen forms a space network skeleton of the freeze-dried eye mask, and the proportion of sodium hyaluronate and collagen determines the toughness and solubility of the freeze-dried eye mask skeleton, and small molecular substances such as carnosine, centella asiatica, cyclodextrin, acetyl hexapeptide-8, arginine/lysine polypeptide and the like are filled in the network structure of the freeze-dried eye mask to form a very saturated and non-atrophy appearance form. In addition, it can be derived from the above embodiments: the ratio of each substance in example 1 was the optimum ratio.
Fig. 1 shows skin changes in the subject 14 days after using the frozen dry eye film prepared in example 1, and it can be seen from fig. 1 that the subject has 13.97% reduced number of wrinkles around eyes, 35.73% reduced score of wrinkles around eyes, 3.9% improved skin elasticity, and 12.54% improved skin gloss after using the product 14 d.
In the early development process of the application, related researches on the composition, the proportion and the freeze-drying process condition of the freeze-dried eye mask are also carried out, and the specific examples are shown in comparative examples 1-7.
Comparative example 1
On the basis of example 1, only sodium hyaluronate was replaced with xanthan gum, the remaining components and the process conditions were unchanged.
Comparative example 2
Based on example 1, only the collagen was replaced with hydroxyethylcellulose, and the rest of the components and the process conditions were unchanged.
Comparative example 3
Based on the embodiment 1, the mass percentage content of the arginine/lysine polypeptide is only increased from 0.1% to 1%, and the rest components and the process conditions are unchanged.
Comparative example 4
Based on the embodiment 1, the mass percentage content of the sodium hyaluronate is only increased from 0.2% to 0.6%, and the rest components and the process conditions are unchanged.
Comparative example 5
Based on the embodiment 1, the mass percentage content of the collagen is only increased from 0.12% to 0.5%, and the rest components and the process conditions are unchanged.
Comparative example 6
On the basis of example 1, only the lyophilization process conditions were adjusted as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-30 ℃ and keeping the temperature for 1h;
(2) Once sublimating, setting the temperature to-10 ℃, heating for 1h, keeping for 4h, and keeping the vacuum degree to be 0.2;
(3) Setting the temperature to-5 ℃, heating for 0.5h, keeping for 5h, and keeping the vacuum degree to be 0.2;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.2.
Comparative example 7
In the comparative example, the following raw materials are weighed according to the mass percentage:
sodium hyaluronate 0.04%, carnosine 0.0001%, centella asiatica extract 0.5%, cyclodextrin 0.65%, collagen 0.25%, acetyl hexapeptide-80.001%, arginine/lysine polypeptide 0.11%, the balance being water.
Uniformly mixing water and sodium hyaluronate, heating to 80-85 ℃, preserving heat for 30min, cooling to 40 ℃, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the mixture is completely dissolved to obtain a first mixed solution;
continuously cooling the first mixed solution to 20 ℃, adding collagen, stirring to uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying treatment according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.15;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.15;
(4) And (3) performing analytical drying, wherein the temperature is set to be 30 ℃, the heating time is 1h, the holding time is 2h, and the vacuum degree is 0.02.
The frozen dry eye films prepared in comparative examples 1 to 7 were tested for appearance, solubility, stability, and skin care effect, and the test results are shown in table 3.
TABLE 3 Table 3
From Table 3, comparative examples 1 to 2 show irreplaceability of sodium hyaluronate and collagen forming a skeleton of frozen dry eye film; comparative example 3 demonstrates that too high an arginine/lysine polypeptide ratio will disrupt the freeze-dried eye membrane backbone and result in poor appearance; comparative examples 4-5 show that sodium hyaluronate with too high a collagen ratio can give a certain anti-wrinkle effect to the finished product, but has the problems of poor solubility and sticky feel; comparative example 6 demonstrates that the lyophilization process has a significant impact on the final appearance morphology of the frozen dry eye film; comparative example 7 illustrates the mass ratio of the ingredients, which has a certain effect on the properties or efficacy of the product.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (7)
1. A freeze-dried eye mask, characterized by comprising the following main components:
sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, and arginine/lysine polypeptides;
wherein, the mass ratio of the sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8 and arginine/lysine polypeptide is (0.12-0.2): (0.0001-0.101): (0.1-0.24): (0.56-0.6): (0.12-0.18): (0.008-0.05): (0.0001-0.1);
the preparation method of the freeze-dried eye mask comprises the following steps:
weighing all raw materials according to the formula of the frozen dry eye film for standby;
uniformly mixing water and sodium hyaluronate, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide are completely dissolved to obtain a first mixed solution;
adding collagen into the first mixed solution, stirring to obtain uniform liquid, and freeze-drying in a freeze dryer according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 to-45 ℃ and keeping the temperature for 2-4 hours;
(2) One-time sublimation is carried out, the temperature is set to minus 10 to minus 15 ℃, the heating time is 0.5 to 2 hours, the holding time is 5 to 8 hours, and the vacuum degree is 0.1 to 0.18;
(3) Setting the temperature to-3-2 ℃, heating for 0.5-1.5 h, keeping for 3-5 h, and performing vacuum degree of 0.1-0.18;
(4) And (3) performing analysis drying, wherein the temperature is set to be 20-30 ℃, the temperature rising time is 0.5-1 h, the holding time is 2-4 h, and the vacuum degree is 0.02-0.08.
2. The lyophilized ophthalmic film according to claim 1, wherein the mass ratio of sodium hyaluronate, carnosine, centella asiatica extract, cyclodextrin, collagen, acetyl hexapeptide-8, arginine/lysine polypeptide is 0.2:0.101:0.24:0.56:0.12:0.05:0.1.
3. a method of preparing a lyophilized ophthalmic film comprising:
weighing the raw materials according to the formula of the frozen dry eye film according to any one of claims 1-2 for later use;
uniformly mixing water and sodium hyaluronate, adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide, and stirring until the carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8 and arginine/lysine polypeptide are completely dissolved to obtain a first mixed solution;
adding collagen into the first mixed solution, stirring to obtain uniform liquid, and freeze-drying in a freeze dryer according to a preset freeze-drying curve program to obtain a freeze-dried eye mask;
the procedure for the preset lyophilization profile is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 to-45 ℃ and keeping the temperature for 2-4 hours;
(2) One-time sublimation is carried out, the temperature is set to minus 10 to minus 15 ℃, the heating time is 0.5 to 2 hours, the holding time is 5 to 8 hours, and the vacuum degree is 0.1 to 0.18;
(3) Setting the temperature to-3-2 ℃, heating for 0.5-1.5 h, keeping for 3-5 h, and performing vacuum degree of 0.1-0.18;
(4) And (3) performing analysis drying, wherein the temperature is set to be 20-30 ℃, the temperature rising time is 0.5-1 h, the holding time is 2-4 h, and the vacuum degree is 0.02-0.08.
4. The method for preparing a frozen dry eye film according to claim 3, wherein the step of adding carnosine, centella asiatica extract, cyclodextrin, acetyl hexapeptide-8, arginine/lysine polypeptide after uniformly mixing water and sodium hyaluronate, stirring until completely dissolving, and obtaining a first mixed solution comprises the steps of:
mixing water and sodium hyaluronate, heating to 80-85deg.C, maintaining the temperature for 30min, cooling to 30-60deg.C, adding carnosine, herba Centellae extract, cyclodextrin, acetyl hexapeptide-8, and arginine/lysine polypeptide, and stirring to dissolve completely to obtain first mixed solution.
5. The method for preparing a frozen dry eye film according to claim 3, wherein the step of adding collagen into the first mixed solution, stirring the mixture to a uniform liquid, and freeze-drying the mixture in a freeze dryer according to a preset freeze-drying curve program to obtain a freeze-dried eye film comprises the following steps:
and continuously cooling the first mixed solution to 10-25 ℃, adding collagen, stirring to be uniform liquid, and placing the uniform liquid in a freeze dryer for freeze-drying according to a preset freeze-drying curve program to obtain the freeze-dried eye mask.
6. A method of preparing a frozen dry eye film according to claim 3, characterized in that the pre-set lyophilization profile procedure is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to the temperature of-40 to-45 ℃ and keeping the temperature for 2-3 hours;
(2) Setting the temperature to minus 10 to minus 15 ℃ for one time of sublimation, heating for 1-2 hours, keeping for 6-8 hours, and carrying out vacuum degree of 0.15-0.16;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and performing vacuum degree to 0.15-0.16;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
7. A method of preparing a frozen dry eye film according to claim 3, characterized in that the pre-set lyophilization profile procedure is as follows:
(1) Pre-freezing, namely pre-freezing the freeze dryer to-40 ℃ and keeping the temperature for 2 hours;
(2) One-time sublimation, setting the temperature to-10 ℃, heating for 1h, keeping for 6h, and carrying out vacuum degree of 0.15;
(3) Setting the temperature to 0 ℃, heating for 1h, keeping for 4h, and carrying out vacuum degree to 0.15;
(4) And (3) performing analytical drying, wherein the temperature is set to 25 ℃, the heating time is 0.5h, the holding time is 3h, and the vacuum degree is 0.05.
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| CN114732778A (en) * | 2020-12-23 | 2022-07-12 | 天津拂瑞雅生物科技有限公司 | Repairing mask and preparation method thereof |
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2022
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110179738A (en) * | 2019-05-30 | 2019-08-30 | 科索瑞生物科技(天津)有限公司 | Active essence and preparation method thereof |
| CN110179737A (en) * | 2019-05-30 | 2019-08-30 | 科索瑞生物科技(天津)有限公司 | Shin moisturizer and preparation method thereof |
| CN114732778A (en) * | 2020-12-23 | 2022-07-12 | 天津拂瑞雅生物科技有限公司 | Repairing mask and preparation method thereof |
| CN113133962A (en) * | 2021-04-14 | 2021-07-20 | 珠海葆雀化妆品有限公司 | Production formula and production method of revitalizing snow skin tender freeze-dried mask |
| CN113181085A (en) * | 2021-04-29 | 2021-07-30 | 广州睿森生物科技有限公司 | Composition matrix for improving skin problems after makeup and application of composition matrix in cosmetics |
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