阅读说明：本技术 一种冻干全吸收膜片及其制备、使用方法 (Freeze-dried full-absorption membrane and preparation and use methods thereof ) 是由 邹杰 李鉴墨 喻振国 严炎刘星 邓欣欣 于 2021-10-20 设计创作，主要内容包括：本发明涉及一种冻干全吸收膜片及其制备、使用方法,包括一定重量浓度的如下组分,胶原蛋白溶液、去乙酰化程度不低于75％的壳聚糖溶液、透明质酸溶液,制备时则是将前述各组分按一定比例充分混合后倒入模具中在低于-80℃的温度下预冷冻一段时间后移入冷冻干燥机中冷冻干燥成型,使用时则将该膜片贴敷在相应位置然后喷水按摩促进皮肤对膜片活性成分的吸收。该发明的膜片不含有有损皮肤的成分,不需要膜布作为有效成分的载体,膜片中不含有任何防腐剂,冻干全吸收膜片最大程度的保持活性蛋白分子的生物活性,提高其中的有效成分的利用率,形式新颖,使用方便。(The invention relates to a freeze-dried full-absorption membrane and a preparation and use method thereof, which comprises the following components with certain weight concentration, namely a collagen solution, a chitosan solution with deacetylation degree not less than 75% and a hyaluronic acid solution, wherein the components are fully mixed according to a certain proportion and then poured into a mould to be pre-frozen at the temperature of less than minus 80 ℃ for a period of time, and then the mould is moved into a freeze-drying machine to be freeze-dried and formed, and when in use, the membrane is pasted at a corresponding position and then water-jet massage is carried out to promote the absorption of active ingredients of the membrane by skin. The membrane does not contain components damaging skin, does not need membrane cloth as a carrier of active ingredients, does not contain any preservative, can keep the biological activity of active protein molecules to the maximum extent by freeze-drying and fully absorbing the membrane, improves the utilization rate of the active ingredients, and has novel form and convenient use.)

1. A freeze-dried full-absorption membrane is characterized in that: the membrane comprises the following components, by weight, 0.05-0.2% of collagen solution, 0.02-0.3% of chitosan solution with deacetylation degree not less than 75%, and 0.1-0.5% of hyaluronic acid solution, wherein the collagen solution, the chitosan solution and the hyaluronic acid solution are mixed and freeze-dried to form the membrane.

2. The freeze-dried full-absorption membrane as claimed in claim 1, wherein an active substance is further added when the collagen solution, the chitosan solution and the hyaluronic acid solution are mixed, and the concentration of the mixed active substance is 0.001-3% (W/V).

3. The lyophilized fully absorbent film of claim 1 wherein said active agent is one or more of amino acids, vitamin C, vitamin B, kojic acid, niacinamide, urea, allantoin, licorice extract, aloe vera extract, and exosomes.

4. A preparation method of a freeze-dried full-absorption membrane is characterized by comprising the following steps:

s1, preparing monomer solutions, namely preparing a collagen solution, a chitosan solution with deacetylation degree not less than 75% and a hyaluronic acid solution respectively;

s2, mixing the solutions, namely mixing the collagen solution, the chitosan solution and the hyaluronic acid solution prepared in the previous step to form a mixed solution;

s3, molding, namely pouring the mixed solution into a mold, pre-freezing the mixed solution at the temperature lower than-80 ℃ for a period of time, and then transferring the mixed solution into a freeze dryer for freeze drying and molding.

5. The method for preparing a lyophilized complete absorbent membrane according to claim 4, wherein the active substance is added to the mixed solution at a concentration of 0.001% -3% (W/V) in the mixed solution.

6. The method for preparing the lyophilized full absorption membrane according to claim 5, wherein the active substance is one or more of amino acids, vitamin C, vitamin B, kojic acid, nicotinamide, urea, allantoin, licorice extract, aloe extract, and exosome.

7. The method for preparing the freeze-dried full-absorption membrane as claimed in claim 4, wherein the weight percentage concentration of collagen is 0.05% -0.2%, the weight percentage concentration of chitosan is 0.02% -0.3%, and the weight percentage concentration of hyaluronic acid is 0.1% -0.5%.

8. The method for preparing the freeze-dried full-absorption membrane as claimed in claim 4, wherein the collagen solution is a solution with a concentration of 0.01-0.5% (W/V) formed by dissolving collagen with a molecular weight of 3 KD-300 KD in an aqueous solution of a volatile acid with a concentration of 0.05-2 mol/L; the chitosan solution is formed by dissolving chitosan with deacetylation degree not less than 75% in a volatile acid aqueous solution with concentration of 0.05-2mol/L, and the concentration of the chitosan solution is 0.01% -0.8% (W/V); the hyaluronic acid solution is formed by dissolving hyaluronic acid with molecular weight of 2.5 KD-1500 KD in water and has concentration of 0.05% -1% (W/V).

9. The method for preparing a freeze-dried full absorption membrane according to claim 4, wherein the thickness of the mixed solution poured into the mold in the step S3 is 1-2.5mm, and the pre-freezing time is 2-4 hours.

10. A method for using a freeze-dried full-absorption membrane is characterized by comprising the following steps of A1, cleaning the part to be coated with the membrane and wiping the part to be coated with the membrane; a2, applying the film on the corresponding part after cleaning and drying, spraying water to the film, kneading, wherein the water is one or more of purified water, citric acid water with citric acid content less than 0.1%, and active substance water solution.

Technical Field

The invention relates to the field of skin care products, in particular to a freeze-dried full-absorption membrane and preparation and use methods thereof.

Background

The facial mask (eye mask and neck mask) is an enhanced functional product in skin care products, and can soften the horny layer and promote skin metabolism by covering the skin, so that the skin can absorb the effective components of the facial mask (eye mask and neck mask) more easily, and the skin care is enhanced. The traditional facial mask (eye mask and neck mask) mainly comprises two parts of active ingredient liquid and mask cloth. The membrane cloth is a non-absorbable component and is mainly used as a carrier of active ingredient liquid, and the membrane cloth can be discarded after use. Because the membrane cloth is a carrier for separating the active ingredients, a large amount of active ingredients are still loaded in the membrane cloth and discarded after the membrane cloth is used, so that the utilization rate of the active ingredients is low. In addition, the effective component liquid contains various nutrient components and active small molecules such as: collagen, hyaluronic acid, small molecular polypeptide, amino acid, vitamin, polyphenol substances, plant extract and the like. These nutrients and active molecules are susceptible to hydrolysis in aqueous solution and to bacterial growth. In order to ensure that the active ingredients are not contaminated by bacteria, it is usual to add to them an amount of preservative such as: parabens, imidazolidinyl urea, hydantoin, and the like. The antiseptic also has certain damage to skin, is easy to cause allergic reaction of skin, and causes red swelling, stabbing pain and acne, and may cause blister, skin crack and other phenomena.

Disclosure of Invention

Aiming at the existing defects, the invention provides a freeze-dried full-absorption membrane and preparation and use methods thereof.

The technical scheme adopted by the invention for solving the technical problems is as follows: a freeze-dried full-absorption membrane comprises the following components, by weight, 0.05% -0.2% of a collagen solution, 0.02% -0.3% of a chitosan solution with deacetylation degree not less than 75%, and 0.1% -0.5% of a hyaluronic acid solution, wherein the collagen solution, the chitosan solution and the hyaluronic acid solution are mixed and freeze-dried to form the membrane.

Preferably, an active substance is further added when the collagen solution, the chitosan solution and the hyaluronic acid solution are mixed, and the concentration of the active substance after mixing is 0.001% to 3% (W/V).

Preferably, the active substance is one or more of amino acids, vitamin C, vitamin B, kojic acid, nicotinamide, urea, allantoin, licorice extract, aloe extract, and extracellular exosomes.

A preparation method of a freeze-dried full-absorption membrane comprises the following steps:

s1, preparing monomer solutions, namely preparing a collagen solution, a chitosan solution with deacetylation degree not less than 75% and a hyaluronic acid solution respectively;

s2, mixing the solutions, namely mixing the collagen solution, the chitosan solution and the hyaluronic acid solution prepared in the previous step to form a mixed solution;

s3, molding, namely pouring the mixed solution into a mold, pre-freezing the mixed solution at the temperature lower than-80 ℃ for a period of time, and then transferring the mixed solution into a freeze dryer for freeze drying and molding.

Preferably, the active material is added to the mixed solution, and the concentration of the active material in the mixed solution is 0.001% to 3% (W/V).

Preferably, the active substance is one or more of amino acids, vitamin C, vitamin B, kojic acid, nicotinamide, urea, allantoin, licorice extract, aloe extract, and extracellular exosomes.

Preferably, in the mixed solution, the weight percentage concentration of the collagen is 0.05-0.2%, the weight percentage concentration of the chitosan is 0.02-0.3%, and the weight percentage concentration of the hyaluronic acid is 0.1-0.5%.

Preferably, the collagen solution is a solution with the concentration of 0.01-0.5% (W/V) formed by dissolving collagen with the molecular weight of 3 KD-300 KD in an aqueous solution of volatile acid with the concentration of 0.05-2 mol/L; the chitosan solution is formed by dissolving chitosan with deacetylation degree not less than 75% in a volatile acid aqueous solution with concentration of 0.05-2mol/L, and the concentration of the chitosan solution is 0.01% -0.8% (W/V); the hyaluronic acid solution is formed by dissolving hyaluronic acid with molecular weight of 2.5 KD-1500 KD in water and has concentration of 0.05% -1% (W/V).

Preferably, the thickness of the mixed solution poured into the mold in the step S3 is 1-2.5mm, and the pre-freezing time is 2-4 hours.

A method for using a freeze-dried full-absorption membrane comprises the following steps of A1, cleaning a part to be applied with the membrane and wiping the part to be applied with the membrane; a2, applying the film on the corresponding part after cleaning and drying, spraying water to the film, kneading, wherein the water is one or more of purified water, citric acid water with citric acid content less than 0.1%, and active substance water solution.

The invention has the beneficial effects that: the membrane does not contain components damaging the skin, any preservative is not added, an ultralow temperature freeze drying process is adopted, the prepared membrane can be stored at normal temperature for a long time, the components can be completely absorbed by the skin, membrane cloth is not needed for freeze drying forming to be used as a carrier of active ingredients, main active ingredients are directly prepared into the membrane, the active ingredients are absorbed and utilized to the maximum extent, the utilization rate of the active ingredients of the membrane is improved, meanwhile, the membrane does not contain any preservative, the skin cannot be damaged, the biological activity of the active ingredients is kept by freeze drying forming, the use is convenient, the sprayed water is convenient to obtain during use, the active ingredients in the membrane are quickly hydrated after meeting water and are absorbed by the skin to form a complete invisible effect, further cleaning treatment is not needed, and the absorption rate of the skin to the active ingredients is high.

Detailed Description

To more clearly illustrate the objects, technical solutions and advantages of the embodiments of the present invention, the present invention will be further described with reference to the following embodiments, which are clearly and completely described, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without inventive step, are within the scope of the present invention.

The steps and the using mode of the freeze-dried full-absorption membrane prepared by the method are as follows:

s1, dissolving collagen (Mw 3 KD-300 KD) and chitosan with deacetylation degree not less than 75% with 0.05-2mol/L volatile acid water solution to obtain two solutions, wherein the concentration of collagen in the prepared solution is 0.01-0.5% (W/V), the concentration of chitosan is 0.01-0.8% (W/V), and hyaluronic acid (Mw 2.5 KD-1500 KD) is dissolved in pure water to obtain 0.05-1% (W/V);

s2, mixing the prepared collagen solution, the chitosan solution and the hyaluronic acid solution to prepare a mixed solution, wherein the weight percentage concentration of the collagen in the mixed solution is 0.05-0.2%, the weight percentage concentration of the chitosan is 0.02-0.3%, and the weight percentage concentration of the hyaluronic acid is 0.1-0.5%; at this time, other active substances can be added into the prepared mixed solution according to different requirements, the concentration of the added active substances in the mixed solution is 0.001-3% (W/V), the active substances are one or more of amino acid, vitamin C, vitamin B, kojic acid, nicotinamide, urea, allantoin, licorice extract, aloe extract, extracellular secretion and the like, and the like can also be other similar active substances.

S3, pouring the mixed solution prepared in the step S2 into a pre-designed mold, wherein the thickness of the mixed solution in the mold is 1-2 mm, pre-freezing the mold and the mixed solution in the mold in an ultra-low temperature refrigerator or freezer at the temperature of lower than-80 ℃ for 2-4 hours, then putting the frozen mold and the frozen solution into a freeze dryer for freeze drying treatment, and after water and volatile acid are completely volatilized, obtaining the solid membrane in the mold, namely the frozen full-absorption skin repair membrane.

Before the skin repairing film is completely absorbed by freezing, the used part is cleaned, the prepared film is applied to the required repairing part (including but not limited to face, neck, eye pouch, canthus and the like) after water is wiped, then one or more of purified water, citric water with the citric acid content of less than 0.1% and active substance aqueous solution are sprayed on the film by using a spray can, the active substance is one or more of amino acid, vitamin C, vitamin B, kojic acid, nicotinamide, urea, allantoin, licorice extract, aloe extract, cell exosome and the like, the active substance aqueous solution is formed by dissolving the active substance aqueous solution in water, the spraying is convenient, or other active small molecule aqueous solution is adopted, and then the skin of the repairing part is massaged, so that the effective components are absorbed by the skin.

The prepared membrane can be preserved for a long time at normal temperature by adopting an ultralow temperature freeze drying process, wherein the components can be completely absorbed by the skin, Collagen (Collagen) is the most important component of extracellular matrix, is a skeleton structure in the extracellular matrix, is a polymer for forming various extracellular matrixes, plays a role of combining tissues in animal cells, is the most main structural protein of the animal structural tissues, mainly exists in the form of insoluble fibrin, and Collagen of Collagen fibers in the dermis of the skin forms a scaffold of the skin; the chitosan has biodegradability, is characterized by a double-helix structure, has film forming property, spinnability and anticoagulation property, can be used as a film forming material to be used as a carrier of collagen and hyaluronic acid, can be degraded and absorbed and can also be used as a carrier, so that the utilization rate is improved; hyaluronic acid is a main component constituting connective tissues such as human intercellular substance, ocular vitreous body, joint synovial fluid, etc., and plays important physiological functions of retaining water, maintaining extracellular space, regulating osmotic pressure, lubricating, and promoting cell repair in vivo. Hyaluronic acid molecules contain a large amount of carboxyl and hydroxyl, intramolecular and intermolecular hydrogen bonds are formed in an aqueous solution, a complex three-stage network structure can be formed by intermolecular action, and the aqueous solution has obvious viscoelasticity; the freeze-drying shaping does not need the carrier of membrane cloth as active ingredient, but directly prepare into the diaphragm with main active ingredient, active ingredient is utilized by the absorption of maximize, the utilization ratio of diaphragm active ingredient has been improved, do not contain any antiseptic in the diaphragm simultaneously, can not cause the damage to skin, the freeze-drying shaping has still kept active ingredient's biological activity, high durability and convenient use, spray water during the use can convenient for obtaining materials, active ingredient in the diaphragm meets quick hydration in water back and is absorbed by skin, form complete stealthy effect, need not further cleaning process, the absorption rate of skin to active ingredient is high.

Example 1:

1, dissolving collagen with 0.1mol of hydrochloric acid to prepare a collagen solution with the concentration of 0.5% (W/V); dissolving chitosan with the hydrochloric acid to obtain a solution with a concentration of 0.3% (W/V); hyaluronic acid with molecular weight of 3KD and 1500KD is dissolved with pure water to obtain concentration of 1% (W/V) and 0.5% (W/V).

Mixing the four prepared solutions of collagen, chitosan, hyaluronic acid (3KD) and hyaluronic acid (1500KD) according to a certain proportion to prepare a mixed solution, wherein the weight contents of the four substances in the mixed solution are respectively 0.1%, 0.05%, 0.1% and 0.3%, and the mixing proportion can be realized by adding a certain amount of pure water.

3, adding the prepared mixed solution into a pre-prepared mould, freezing the mixed solution for 2 hours at the temperature of-85 ℃ after the solution is 1.5mm thick, then putting the frozen mixed solution into a freeze dryer, freezing the frozen mixed solution for 24 hours at the temperature of-80 ℃ of a cold trap and the vacuum degree of less than 5Pa, and preparing the frozen full-absorption skin repair membrane.

And 4, when the prepared membrane is used for repairing the face, cleaning the face, wiping water, then pasting the prepared membrane on the face, uniformly spraying pure water on the membrane by using a small spray can, and then kneading the repaired face.

Example 2:

1, dissolving collagen with 0.2M acetic acid to prepare a collagen solution with the concentration of 0.3% (W/V); dissolving chitosan in 0.1M hydrochloric acid to obtain a solution with a concentration of 0.6% (W/V); hyaluronic acid with molecular weight of 3KD and 1500KD is dissolved with pure water to obtain concentration of 0.3% (W/V) and 0.3% (W/V), respectively.

2, mixing the four prepared solutions of collagen, chitosan, hyaluronic acid (3KD) and hyaluronic acid (1500KD) according to a certain proportion to prepare a mixed solution, wherein the content of the four substances in the mixed solution is respectively 0.05%, 0.25%, 0.15% and 0.1%, the mixing proportion can be realized by adding a certain amount of pure water, simultaneously adding vitamin C, kojic acid and aloe extract into the prepared mixed solution, and the weight percentage concentration of the three substances after stirring and dissolving is respectively 0.005%, 2% and 0.1%.

3, adding the prepared mixed solution into a pre-prepared mold, wherein the depth of the solution is 1 mm. Then placing the mixture into a freezing cabinet with a liquid nitrogen as a bottom layer for freezing for 3 hours, then placing the mixture into a freeze drier, freezing and drying the mixture for 24 hours at the temperature of minus 80 ℃ and the vacuum degree of less than 5 Pa. The frozen full-absorption skin repairing film is prepared.

And 4, when the prepared membrane is used for repairing the neck, cleaning the neck, wiping water, then pasting the prepared membrane on the neck, uniformly spraying water soaked with lemon slices on the membrane by using a small spray can, and then kneading the repaired part of the neck.

It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.