CN115645301A - Collagen freeze-dried powder preparation method, skin care product and dressing - Google Patents
Collagen freeze-dried powder preparation method, skin care product and dressing Download PDFInfo
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- CN115645301A CN115645301A CN202210871617.5A CN202210871617A CN115645301A CN 115645301 A CN115645301 A CN 115645301A CN 202210871617 A CN202210871617 A CN 202210871617A CN 115645301 A CN115645301 A CN 115645301A
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Abstract
The invention aims to overcome the problems of easy chain scission and unstable effect of the existing micromolecule collagen, provides a preparation method of collagen freeze-dried powder, the product of the collagen freeze-dried powder is suitable for skin absorption and use, has stable effect and anti-aging effect, and can be used in skin care products and dressings, and the preparation method of the collagen freeze-dried powder comprises the following steps: s100, carrying out decellularization on the small intestine submucosa extracellular matrix, carrying out enzymolysis and hydrolysis treatment to obtain small molecules with the molecular weight of 300-1000, grinding in a sterile environment, and filtering by using a 20, 40, 60 or 80-mesh screen to obtain decellularized small intestine mucosa extracellular matrix powder; s110, preparing a medical high polymer material into cosmetic microspheres of 30-100 microns, and uniformly mixing the decellularized small intestine mucosa extracellular matrix powder with the cosmetic microspheres according to the proportion of 300; and S120, placing the final product of the step S110 in an environment with the temperature of-40 to-80 ℃ for freeze drying for 12 to 48 hours to obtain collagen freeze-dried powder.
Description
Technical Field
The invention relates to the technical field of cell biology, in particular to a collagen freeze-dried powder preparation method, a skin care product and a dressing.
Background
Skin aging is a phenomenon of skin aging caused by natural factors or non-natural factors. The natural causes such as aging are increased, the growth period of skin tissues generally ends at about 25 years old, which is called as 'skin bend angle', since the growth and aging progress simultaneously, the elastic fibers of the skin gradually become coarse, and the aging of the skin is gradually obvious at the early stage of 40-50 years. The unnatural factors mainly refer to artificial environmental damage, air pollution and the like, and various harmful substances, dust and the like in the air are attached to the skin to influence the normal metabolism function of the skin in the Newcastle, so that skin injury, aging and the like are caused. Skin aging is caused by various reasons, the essence of the skin aging is that elastic fibers of the skin become thicker gradually, subcutaneous fat is reduced, and the elasticity and tension of the skin are gradually lost due to the change of the elastic fibers and collagen fibers, so that skin relaxation and wrinkles are further caused, and therefore, the timely supplement of collagen is very important for resisting aging.
The extracellular matrix of the small intestinal mucosa is a material with good biocompatibility and safety, and the decellularized product contains a large amount of collagen, so that the extracellular matrix can be widely applied to a plurality of fields of medical dressing, beauty and skin care, regenerative medicine and the like.
At present, collagen products related to skin rehabilitation, maintenance and regeneration generally have larger molecular weight, and micromolecular collagen is easy to chain scission and is not easy to process and use. Based on the research in the technical fields of decellularization, microsphere and freeze drying, the inventor proposes that the cell can be processed into freeze-dried powder by the decellularization and microsphere technology and the freeze drying technology, and then the freeze-dried powder is applied.
Disclosure of Invention
The invention aims to overcome the problems of easy chain scission and unstable effect of the existing micromolecule collagen, and provides a preparation method of collagen freeze-dried powder, which is suitable for skin absorption, has stable effect and anti-aging effect, and can be used in skin care products and dressings.
According to one aspect of the invention, a method for preparing collagen freeze-dried powder is provided, which is characterized by comprising the following steps:
s100, after the small intestine submucosa extracellular matrix is decellularized, carrying out enzymolysis and hydrolysis treatment on the small intestine submucosa extracellular matrix to obtain small molecules with the molecular weight of 300-1000, grinding the small molecules in a sterile environment, and filtering the small molecules by using a 20, 40, 60 or 80-mesh sieve to obtain decellularized small intestine mucosa extracellular matrix powder;
s110, preparing a medical polymer material into cosmetic microspheres with the particle size of 30-100 microns, and uniformly mixing the decellularized small intestine mucosa extracellular matrix powder and the cosmetic microspheres according to the proportion of 300;
s120, placing the final product of the step S110 in an environment with the temperature of-40 to-80 ℃ for freeze drying for 12 to 48 hours to obtain collagen freeze-dried powder.
Further, the medical polymer material comprises: polylactic acid and poly (lactide-co-glycolide).
Further, step S110 is followed by step S111: and S112, adding 5% -35% of a plasticizer into the mixture, dissolving the mixture into acidic pepsin and proteinase K to obtain a digestive juice, filtering, centrifuging and taking a supernatant.
Further, the plasticizer comprises one or more of: d-mannitol, sucrose, glucose, disodium or monosodium phosphate, BAS.
Further, the freeze-drying method in step S120 includes:
s121, adding 0.5-2ml of the supernatant into a freezing bottle, wherein the pre-freezing temperature is-10 to-25 ℃, the time lasts for 1-10 hours, the temperature is reduced to-40 to-80 ℃ after pre-freezing, and an intermediate product is obtained after 24-72 hours;
and S122, drying one or more of fat-soluble vitamins A, D, E, K, mixing the dried fat-soluble vitamins 5363 with the intermediate product according to the proportion of 1.
According to a second aspect of the present invention, a collagen skin care product is provided, which is characterized by comprising the collagen lyophilized powder prepared by the above preparation method.
Further, the skin care product comprises: facial mask, essence, cream, and hand cream.
According to a third aspect of the invention, a collagen dressing is provided, which is characterized by comprising the collagen freeze-dried powder prepared by the preparation method.
The preparation method of the collagen powder, the skin care product and the dressing provided by the invention have the beneficial effects that:
(1) After the small intestinal submucosa is treated by a decellularization technology and a high polymer material microsphere technology, collagen with a large molecular weight and suitable for skin absorption can be obtained, and meanwhile, the microspheres have a slow release effect and wrap the collagen, so that the collagen can be maintained at a sufficient concentration for a period of time, and the effects of continuously providing nutrition and repairing are achieved;
(2) The collagen can be prepared into freeze-dried powder, so that the biological activity of the collagen can be preserved, the collagen is convenient to preserve, the collagen can be directly used after being added with a solvent, the collagen is very convenient to use, the collagen can be directly used as an additive to be added into a skin care product or a dressing, and the effect is not influenced completely;
(3) The extracellular matrix with small molecular weight is processed by enzymolysis and hydrolysis, and is processed into lyophilized powder, which is convenient for subsequent use and more important for ensuring the stability and activity of the collagen with small molecular weight.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of the present invention.
The embodiment of the invention provides a preparation method of collagen freeze-dried powder, which comprises the following steps:
s100, after the small intestine submucosa extracellular matrix is decellularized, carrying out enzymolysis and hydrolysis treatment on the small intestine submucosa extracellular matrix to obtain small molecules with the molecular weight of 300-1000, grinding the small molecules in a sterile environment, and filtering the small molecules by using a 20, 40, 60 or 80-mesh sieve to obtain decellularized small intestine mucosa extracellular matrix powder;
s110, preparing a medical polymer material into cosmetic microspheres of 30-100 micrometers, and uniformly mixing the acellular small intestinal mucosa extracellular matrix powder with the cosmetic microspheres according to the ratio of 300-300;
and S120, placing the final product of the step S110 in an environment with the temperature of-40 to-80 ℃ for freeze drying for 12 to 48 hours to obtain collagen freeze-dried powder.
In the embodiment, firstly, the acellular matrix of the small intestinal submucosa is processed into a product with small molecular weight which can penetrate through the stratum corneum of the skin, and then the product is ground into powder; the microspheres prepared by mixing the medical high polymer materials can be slowly and continuously released while keeping the stability of small molecules, and finally freeze-dried powder is obtained by freeze-drying, so that the microspheres can be conveniently stored and transported and can be directly used as additives to be applied to related products.
The inventor confirms the experimental conditions, the dosage and the properties of the finished product through a plurality of experiments, and the collagen freeze-dried powder obtained by processing according to the method can achieve the stable and effective target.
The specific molecular weight, amount and time parameters are selected according to the following examples:
the embodiment of the invention can also add the operations of shaping, secondary digestion and freeze-drying, so that the formed freeze-dried powder is more stable, and the specific steps are as follows:
s210, after the small intestine submucosa extracellular matrix is decellularized, carrying out enzymolysis and hydrolysis treatment on the small intestine submucosa extracellular matrix to obtain small molecules with the molecular weight within 500, grinding the small molecules in a sterile environment, and filtering the small molecules by using a 60-mesh screen to obtain decellularized small intestine mucosa extracellular matrix powder;
s220, preparing a polylactic acid material into a 60-micron cosmetic microsphere, and uniformly mixing the decellularized small intestine mucosa extracellular matrix powder and the cosmetic microsphere according to the proportion of 300;
s230, adding 5-35% of a shaping agent into the mixture;
s240, dissolving the mixture added with the shaping agent into acidic pepsin and proteinase K to obtain a digestive juice, filtering and centrifuging to obtain a supernatant, wherein the shaping agent can be selected from the following components: d-mannitol, sucrose, glucose, disodium or monosodium phosphate, BAS;
s250, adding 0.5-2ml of supernatant into a freezing bottle, pre-freezing at the temperature of-10 to-25 ℃ for 1-10 h, cooling to-40 to-80 ℃ after pre-freezing, and obtaining an intermediate product after 24-72 h;
s260, drying one or more of fat-soluble vitamins A, D, E, K, mixing the dried fat-soluble vitamins with an intermediate product according to the proportion of 1.
The type and usage amount of the plasticizer and the type and proportion of the vitamin in the embodiment refer to the prior art, and the addition of the plasticizer still has a positive effect on the preparation of the freeze-dried powder in the embodiment.
The specific molecular weight, the amount and the time parameters are selected according to the following examples:
example 27:
the collagen mask comprises 5% of the lyophilized powder prepared in example 2 by weight.
Example 28:
collagen hand cream, comprising 3.8% by weight of the lyophilized powder prepared in example 17.
Example 29:
a collagen dressing comprising 15% by weight of the lyophilized powder prepared in example 17.
The molecular weight and the collagen content and the anti-aging effect of the embodiment are respectively detected, and the experimental method and the result are as follows:
(1) The collagen detection method comprises the following steps:
using normal saline as a solvent, preparing the freeze-dried powder into a solution of 1mg/mL, and detecting the content of collagen in the solution by an ELISA method; examples 27-29 were formulated as 5mg/mL solutions.
(2) The anti-aging detection method comprises the following steps: according to the background information, the skin aging is mainly related to the elastic fiber, and the elastic fiber is composed of elastin and microfibril, wherein the elastic fiber can be decomposed by elastase to cause loss of collagen and cause skin aging, therefore, the purpose of anti-sunburn effect detection can be achieved by measuring the inhibition rate of the freeze-dried powder on the elastase. Specifically, 100 microliters of 0.2mol/L tris-HCL buffer solution, 25 microliters of 10mmol/L N-methoxysuccinyl-alanine-proline-valine-4-nitroaniline and 30mg of freeze-dried powder are mixed, the mixture is kept stand at 25 ℃ for 15min, 25 microliters of 0.3U/ml elastase is added to continue to be kept stand for 15min, finally, the OD value is detected under the condition of 410nm, and the elastase inhibition rate is calculated by the following formula:
inhibition (%) = (control OD value-experimental OD value)/control OD value 100
The amount of product used in examples 27-29 was 50mg.
(3) The experimental results are as follows:
TABLE 1 collagen content and anti-aging Effect table
From the experimental results in table 1, it can be seen that the collagen content in the claims is stable, the performance is stable, and in addition, the most exciting is that the inhibition rate of elastase reaches the level of more than 60%, and it can be seen that the collagen lyophilized powder and related products prepared by the example method really have the anti-aging effect.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for preparing collagen freeze-dried powder is characterized by comprising the following steps:
s100, carrying out decellularization on the small intestine submucosa extracellular matrix, carrying out enzymolysis and hydrolysis treatment to obtain small molecules with the molecular weight of 300-1000, grinding in a sterile environment, and filtering by using a 20, 40, 60 or 80-mesh screen to obtain decellularized small intestine mucosa extracellular matrix powder;
s110, preparing a medical high polymer material into cosmetic microspheres of 30-100 microns, and uniformly mixing the decellularized small intestine mucosa extracellular matrix powder with the cosmetic microspheres according to the proportion of 300;
s120, placing the final product of the step S110 in an environment with the temperature of-40 to-80 ℃ for freeze drying for 12 to 48 hours to obtain collagen freeze-dried powder.
2. The method for preparing collagen freeze-dried powder according to claim 1, wherein the medical polymer material comprises: polylactic acid and poly (lactide-co-glycolide).
3. The method for preparing collagen lyophilized powder according to claim 1, wherein step S110 is followed by step S111: and S112, adding 5% -35% of a shaping agent into the mixture, dissolving the mixture into acidic pepsin and proteinase K to obtain a digestive juice, filtering, centrifuging and taking a supernatant.
4. The method for preparing collagen lyophilized powder according to claim 3, wherein the shaping agent comprises one or more of the following: d-mannitol, sucrose, glucose, disodium or monosodium phosphate, BAS.
5. The method for preparing collagen freeze-dried powder according to claim 3, wherein the freeze-drying method in the step S120 is as follows:
s121, adding 0.5-2ml of the supernatant into a freezing bottle, wherein the pre-freezing temperature is-10 to-25 ℃, the time lasts for 1-10 hours, the temperature is reduced to-40 to-80 ℃ after pre-freezing, and an intermediate product is obtained after 24-72 hours;
and S122, drying one or more of fat-soluble vitamins A, D, E, K, mixing the dried fat-soluble vitamins 5363 with the intermediate product according to the proportion of 1.
6. A collagen skin care product, which is characterized by comprising the collagen freeze-dried powder prepared by the preparation method of any one of claims 1 to 5.
7. The collagen skin care product according to claim 6, wherein said skin care product comprises: facial mask, essence, cream, and hand cream.
8. A collagen dressing comprising the collagen lyophilized powder prepared by the method of any one of claims 1 to 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116196259A (en) * | 2023-02-23 | 2023-06-02 | 西安博和医疗科技有限公司 | Preparation method of high-activity freeze-dried mask |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116196259A (en) * | 2023-02-23 | 2023-06-02 | 西安博和医疗科技有限公司 | Preparation method of high-activity freeze-dried mask |
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