CN110960443A - Composition containing recombinant human collagen, freeze-dried material, preparation method of freeze-dried material and cosmetic - Google Patents
Composition containing recombinant human collagen, freeze-dried material, preparation method of freeze-dried material and cosmetic Download PDFInfo
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- CN110960443A CN110960443A CN201911367084.1A CN201911367084A CN110960443A CN 110960443 A CN110960443 A CN 110960443A CN 201911367084 A CN201911367084 A CN 201911367084A CN 110960443 A CN110960443 A CN 110960443A
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Abstract
The invention provides a composition containing recombinant human collagen, a freeze-dried material, a preparation method of the freeze-dried material and cosmetics. The composition containing the recombinant human collagen comprises the following raw materials in percentage by mass: 0.1 to 10 percent of mannitol, 0.01 to 3 percent of pullulanase polysaccharide, 0.01 to 1.2 percent of recombinant human collagen, 0.01 to 0.1 percent of mevalonolactone and the balance of water. Lyophilized material, prepared by using the composition containing recombinant human collagen. The preparation method of the freeze-dried material comprises the following steps: and dissolving the active ingredients in the raw materials in water, and freeze-drying to obtain the freeze-dried material. Cosmetic comprising said composition containing recombinant human collagen. The composition, the freeze-dried material and the cosmetics containing the recombinant human collagen have the effects of moisturizing, brightening skin, resisting aging, removing wrinkles, protecting, repairing and the like.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a composition containing recombinant human collagen, a freeze-dried material, a preparation method of the freeze-dried material and cosmetics.
Background
With the improvement of living standard of people, the demand of cosmetics is more and more, and the demand is gradually improved. Particularly, there is a strong demand for cosmetics for improving and restoring skin conditions. People particularly have obvious requirements on products with the functions of moisturizing, brightening skin, removing wrinkles, repairing skin, removing acne marks and the like.
In many cosmetics currently on the market, the principal component that provides the core efficacy is growth factor. However, with the discovery of a series of problems caused by the use of growth factors, our country prohibits the addition of growth factors to cosmetics.
Therefore, it is a problem to be solved to provide a product that can achieve or exceed the efficacy of growth factors.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a composition with recombinant human collagen, a freeze-dried material, a preparation method thereof and a cosmetic, so as to solve the problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a composition containing recombinant human collagen comprises the following raw materials in percentage by mass:
0.1 to 10 percent of mannitol, 0.01 to 3 percent of pullulanase polysaccharide, 0.01 to 1.2 percent of recombinant human collagen, 0.01 to 0.1 percent of mevalonolactone and the balance of water.
Mannitol and pullulanase are mainly used as a filler and an excipient to ensure the forming of the composition; the Recombinant Human Collagen (RHC) is applied to a facial mask on the surface of the skin, so that the skin is protected from external damage (ultraviolet rays, PM2.5 and the like), and meanwhile, the water loss of the stratum corneum is reduced; regulating sebum metabolism of skin, recovering microenvironment balance of skin, and moisturizing skin, nourishing skin, and improving skin color; the epidermal cell recognizes that the RHC is a substance per se, and the RHC is actively absorbed through a protein network structure formed by densely crosslinking stratum corneum cells and a regular arrangement structure of a large amount of microfilament keratin and fibroin; the RHC has excellent tissue intermiscibility and affinity, and can efficiently pass through the transparent layer, the granular layer, the spinous layer and the basal layer to reach the dermis layer; the collagen is directly filled, and on the other hand, the collagen can be absorbed by fibroblasts as raw materials for synthesizing the collagen, the collagen power is simultaneously excited, the collagen synthesizing capability of cells is promoted, the expression of elastin genes is promoted, the synthesis of endogenous collagen of the cells is simultaneously excited while exogenous collagen is supplemented, the double effects are achieved, and the skin is in a young state; the RHC has strong repairing effect, improves the living environment of skin cells, promotes the metabolism of skin tissues and repairs damaged skin. The mevalonic lactone can promote the activation of skin cholesterol synthesis ability due to age and other factors; has the effect of restoring the skin protective function due to the low synthesis ability such as aging.
Optionally, the raw materials of the composition containing the recombinant human collagen comprise, by mass: mannitol can be any value between 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, and 0.1% -10%; the pullulanase may be any value between 0.01%, 0.05%, 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3% and 0.01-3%; the recombinant human collagen may be any value between 0.01%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, and 0.01% -1.2%; the mevalonolactone may be any value between 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.10%, and 0.01% -0.1%.
Preferably, the composition further comprises the following raw materials in percentage by mass: 0.01 to 0.5 percent of sodium hyaluronate;
preferably, the composition further comprises the following raw materials in percentage by mass: centella asiatica extract 0.01-1.5%;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01 to 0.5 percent of lycopene;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.001-0.1% of water-soluble peptide powder;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01% -1% of blue copper peptide;
preferably, the water-soluble peptide powder comprises one or more of oligopeptide-5, tripeptide-1, acetyl hexapeptide-8 and pentapeptide-3.
The sodium hyaluronate for cosmetics is white fibrous or powdery solid, has strong hygroscopicity, negative charge of aqueous solution, and high viscoelasticity and osmotic pressure at high concentration. Sodium hyaluronate is an inherent component in the human body, is a glucuronic acid, has an excellent moisturizing effect, and is internationally called an ideal Natural Moisturizing Factor (NMF). The sodium hyaluronate with different molecular weights acts on the surface of the skin, and the macromolecular hyaluronic acid can form a layer of breathable film on the surface of the skin, so that the skin is smooth and moist, the invasion of external bacteria, dust and ultraviolet rays can be blocked, and the skin is protected from being damaged; the small molecular hyaluronic acid can permeate into dermis, has the effects of slightly expanding capillary vessels, increasing blood circulation, improving intermediate metabolism, promoting skin nutrition absorption, has a strong wrinkle removing function, can increase skin elasticity, and can delay skin aging. The hyaluronic acid can promote proliferation and differentiation of epidermal cells, remove oxygen free radicals, and prevent and repair skin injury.
The centella asiatica extract contains asiaticoside, madecassoside, asiatic acid, and madecassic acid. Has the effects of remarkably promoting the synthesis of collagen, elastin and hyaluronic acid, reducing wrinkles from the inside of the skin and resisting aging; accelerate the healing of the skin, thereby reconstructing the damaged skin.
The lycopene contains polyhydrolycopene (phytoene and phytofluene), and has an anti-pollution function: lycopene removes the photo-toxic effect of polycyclic aromatic hydrocarbon by scavenging free radicals, and can also directly eliminate toxic substances in cigarette and automobile exhaust; anti-aging: free radicals attack the active macromolecules of cells, causing the destruction of cellular structure and function, thus causing and accelerating skin aging; sun protection: the lycopene can remove excessive free radicals caused by ultraviolet rays, has direct antagonism on the ultraviolet rays, and increases the tolerance of the skin to the ultraviolet rays; whitening and brightening the skin: the lycopene contains antioxidant substances, and has effects in decomposing and removing pigment in skin tissue, preventing pigmentation, and homogenizing skin color.
The water-soluble peptide powder comprises oligopeptide-5 (EDP3), tripeptide-1, acetyl hexapeptide-8 and pentapeptide-3. Oligopeptide-5 (EDP3) is a biomimetic peptide, a bilayer encapsulation technique, and is effectively a liposome capsule of a transdermal absorption system, delivering active ingredients to the dermis layer through the stratum corneum. Promoting new skin cell generation, and reducing and preventing fine lines and wrinkles; the vitality and energy of the skin are increased, and the skin color is lightened; improving cell survival, slowing down apoptosis, increasing extracellular matrix (collagen, elastin, hyaluronic acid, etc.), improving skin quality (tightening and loosening skin, improving skin elasticity, density and tightness); promoting cell regeneration, cell migration and cell adhesion, regulating gene expression of aquaporin 3, promoting skin hydration, and promoting wound healing and scar repair. The product is white powder, amino acid: a, molecular weight: 1271.4 Da. Tripeptide-1 is a signal peptide that acts on the dermis to promote the synthesis of extracellular matrix type I and type II collagen, elastin, structural glycoproteins such as laminin and fibronectin, promote wound healing and tissue remodeling, strengthen the dermis, make the skin thicker and firmer, smooth wrinkles, and provide greater resistance to uv radiation. Acetyl hexapeptide-8 and pentapeptide-3 are safe and effective substitutes for botulinum toxin. Acetyl hexapeptide-8 is a peptide consisting of six amino acids that mimics the N-terminus of the SNAP-25 protein, and prevents the generation of wrinkles by reducing the release of the neurotransmitter acetylcholine, resulting in a reduction in muscle contraction; pentapeptide-3 is a sensitizer of acetyl hexapeptide-8, and the two are used together to have synergistic effect and increase wrinkle-removing effect.
The blue copper peptide (GHK-Cu) is a compound which is found in serum and consists of three amino acids and a divalent copper ion, and has the functions of restoring the skin repair capacity, increasing the generation of intercellular adhesions of the skin and reducing the skin damage; stimulating the formation of glucose polyamine, increasing the thickness of the skin, and reducing the looseness and tightness of the skin; stimulating the formation of collagen and elastin, firming skin and reducing fine lines; the auxiliary antioxidant enzyme SOD has strong and favorable free radical resisting function; promoting blood vessel proliferation, and increasing oxygen supply to skin.
Optionally, the composition may comprise, by mass, sodium hyaluronate in an amount of any one of 0.01%, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, and 0.01% to 0.5%; the content of centella asiatica extract may be any value between 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5% and 0.01% -1.5%; the lycopene content may be any value between 0.01%, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5% and 0.01% -0.5%; the content of the water-soluble peptide powder may be any value between 0.001%, 0.005%, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.10%, and 0.001-0.1%; the content of the copper-coated peptides may be any value between 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, and 0.01% -1%.
Preferably, the composition further comprises the following raw materials in percentage by mass: 0.01% -10% of astaxanthin;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01% -1% of superoxide dismutase.
Astaxanthin is Haematococcus pluvialis extract, has 100% L-turn (3S-3' S) structure, and has strongest biological activity. One of the strongest natural antioxidants of natural astaxanthin in the world effectively eliminates oxygen free radicals in cells, enhances the regeneration capability of the cells, maintains the balance of the organism and reduces the accumulation of aging cells, protects the health of the cells and DNA from inside to outside, thereby protecting the health of skin, promoting the growth of hair, resisting aging, relieving sports fatigue and enhancing the vitality.
Superoxide dismutase (SOD, a biological fermentation source) is an antioxidant metalloenzyme existing in organisms, and the SOD has the effect of clearing superoxide radicals and improving the capabilities of inflammation resistance, infection resistance, self protection and self repair. Has obvious effects of resisting aging, fading or fading color spots, resisting radiation and diminishing inflammation.
Alternatively, the composition may comprise astaxanthin at any one of 0.01%, 0.05%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10% and 0.01% to 10% in terms of mass% of the raw materials, and superoxide dismutase at any one of 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1% and 0.01% to 1% in terms of mass% of the raw materials.
A freeze-dried material is prepared by freeze-drying the composition containing the recombinant human collagen.
Preferably, the freeze-dried material comprises one or more of freeze-dried powder, freeze-dried balls and freeze-dried tablets.
The composition can be lyophilized to obtain lyophilized powder, lyophilized tablet or lyophilized pellet as required.
The preparation method of the freeze-dried material comprises the following steps:
dissolving the components in the raw materials in water, and freeze-drying to obtain the freeze-dried material.
Preferably, the mass content of water in the freeze-dried material is less than or equal to 5%.
Alternatively, the mass content of water in the freeze-dried material may be any of 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, and 5% or less.
Preferably, the specific process of dissolving the components of the raw materials in water comprises the following steps:
dissolving mannitol and pullulanase in water, and then carrying out first filtration and sterilization to obtain a solution A;
dissolving the recombinant human collagen and the mevalonolactone in water, and then carrying out second filtration to obtain a solution B;
mixing the solution A and the solution B, and uniformly stirring;
preferably, the first filtration and the second filtration independently use 400 mesh or 500 mesh filter cloth.
Through the optimization of the mixing and dissolving sequence of the raw materials, the processing process can be smoother, the effective components can be dissolved more sufficiently, and the obtained liquid is more uniform and more stable.
Preferably, the process of lyophilization comprises a freezing phase, a sublimation phase and a desorption drying phase;
preferably, the temperature of the material in the freezing stage is-33 ℃ to-35 ℃, and the freezing time is 100-;
preferably, the vacuum degree of the sublimation stage is 28-33 pa;
preferably, the sublimation stage adopts temperature programming;
preferably, the mass temperature of the desorption drying stage is 32-34 ℃.
By controlling the change of temperature and pressure, the shape of the freeze-dried material can be ensured in the process of preparing the freeze-dried balls and the freeze-dried tablets.
Optionally, the temperature of the material in the freezing stage can be any value between-33, -34, -35 and-33 ℃ to-35 ℃, and the freezing time can be any value between 100min, 110min, 120min, 130min, 140min and 100-140 min; the degree of vacuum of the sublimation stage may be any value between 28pa, 29pa, 30pa, 31pa, 32pa, 33pa and 28-33 pa.
A cosmetic comprising the recombinant human collagen-containing composition or the lyophilizate of claim 4 or 5.
Compared with the prior art, the invention has the beneficial effects that:
the application provides a composition, a freeze-dried material and cosmetics containing recombinant human collagen, through the cooperation of recombinant human collagen and mevalonolactone to add mannitol and pullulanase polysaccharide, can obtain the cosmetic active ingredient with equivalent effect and better stability than growth factor, can effectively solve all kinds of skin problems.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, and it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope of the present invention.
FIG. 1 is a control chart of facial red blood streak repair using the lyophilized pellet prepared in example 4.
Detailed Description
The terms as used herein:
"prepared from … …" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of … …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 ~ 5" is disclosed, the ranges described should be construed to include the ranges "1 ~ 4", "1 ~ 3", "1 ~ 2 and 4 ~ 5", "1 ~ 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In these examples, the parts and percentages are by mass unless otherwise indicated.
"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent any unit mass, for example, 1g or 2.689 g. If we say that the part by mass of the component A is a part by mass and the part by mass of the component B is B part by mass, the ratio of the part by mass of the component A to the part by mass of the component B is a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
First, the sources of various substances used in the examples of the present application are described, as shown in table 1:
TABLE 1 raw materials manufacturer
Example 1
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 1% of mannitol, 1.5% of pullulanase polysaccharide, 0.7% of recombinant human collagen, 0.05% of mevalonolactone and 96.75% of water.
Mixing the above materials, sterilizing, sieving with 400 mesh filter cloth, packaging, and lyophilizing to obtain lyophilized powder.
Example 2
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 1% of mannitol, 1.5% of pullulanase polysaccharide, 0.1% of sodium hyaluronate, 0.7% of recombinant human collagen, 0.5% of centella asiatica extract, 0.05% of mevalonolactone and 96.15% of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 400 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen and herba Centellae extract with sterile warm water (31 deg.C) until completely dissolved, adding mevalonolactone, stirring, and filtering with 500 mesh filter cloth to obtain solution B;
cooling the solution A to 25 ℃, filtering the solution A by a 400-mesh filter cloth, adding the solution B, stirring uniformly, and immediately subpackaging the mixture into a mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-34 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried balls.
Example 3
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 5% of mannitol, 1.5% of pullulanase polysaccharide, 0.01% of sodium hyaluronate, 0.7% of recombinant human collagen, 0.5% of centella asiatica extract, 0.05% of mevalonolactone and 92.24% of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 500 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen and herba Centellae extract with sterile warm water (35 deg.C) until completely dissolved, adding mevalonolactone, stirring, and filtering with 500 mesh filter cloth to obtain solution B;
cooling the solution A to normal temperature, filtering with 500 mesh filter cloth, adding the solution B, stirring, and packaging into mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-34 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried tablet.
Example 4
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 1% of mannitol, 1.5% of pullulanase polysaccharide, 0.1% of sodium hyaluronate, 0.5% of recombinant human collagen, 0.3% of centella asiatica extract, 0.05% of lycopene, 0.03% of tripeptide-1, 0.03% of mevalonic lactone, 1% of astaxanthin, 0.05% of superoxide dismutase (10000IU/ml) and 95.44% of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 400 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen, herba Centellae extract, lycopene and tripeptide-1 with sterile warm water (30 deg.C) until completely dissolved, adding mevalonic lactone, astaxanthin and superoxide dismutase, stirring, and filtering with 500 mesh filter cloth to obtain solution B;
cooling the solution A to 25 ℃, filtering the solution A by a 400-mesh filter cloth, adding the solution B, stirring uniformly, and immediately subpackaging the mixture into a mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-34 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried balls.
Example 5
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 3.5 percent of mannitol, 1.5 percent of pullulanase polysaccharide, 0.5 percent of recombinant human collagen, 0.4 percent of centella asiatica extract, 0.05 percent of lycopene, 0.03 percent of tripeptide-1, 0.03 percent of mevalonic lactone, 1 percent of astaxanthin, 0.05 percent of superoxide dismutase (10000IU/ml) and 92.94 percent of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 400 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen, lycopene, herba Centellae extract and tripeptide-1 with sterile warm water (32 deg.C) until completely dissolved, adding mevalonic lactone, astaxanthin and superoxide dismutase, stirring, and filtering with 400 mesh filter cloth to obtain solution B;
cooling the solution A to 25 ℃, filtering the solution A by a 400-mesh filter cloth, adding the solution B, stirring uniformly, and immediately subpackaging the mixture into a mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-33 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried tablet.
Example 6
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 1.5% of mannitol, 1.5% of pullulanase polysaccharide, 0.12% of sodium hyaluronate, 0.4% of recombinant human collagen, 0.4% of centella asiatica extract, 0.001% of oligopeptide-5, 0.3% of bluecopper peptide, 0.03% of mevalonolactone, 0.08% of superoxide dismutase (10000IU/ml) and 95.669% of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 500 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen, herba Centellae extract, oligopeptide-5 and bluecopper peptide with sterile warm water (33 deg.C) until completely dissolved, adding mevalonic lactone and superoxide dismutase, stirring, and filtering with 500 mesh filter cloth to obtain solution B;
cooling the solution A to normal temperature, filtering with 500 mesh filter cloth, adding the solution B, stirring, and packaging into mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-35 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried balls.
Example 7
A composition containing recombinant human collagen comprises the following raw materials in percentage by mass: 4% of mannitol, 1.5% of pullulanase polysaccharide, 0.02% of sodium hyaluronate, 0.4% of recombinant human collagen, 0.4% of centella asiatica extract, 0.001% of oligopeptide-5, 0.3% of copper-peptide, 0.03% of mevalonic lactone, 0.08% of superoxide dismutase (10000IU/ml) and 93.269% of water.
Mixing mannitol, pullulanase and ultrapure water, stirring until the solution is clear and transparent, filtering with 400 mesh filter cloth, subpackaging, and sterilizing at high temperature (121 deg.C, 0.1Mpa, 30 min) in high pressure steam sterilizing pot to obtain solution A;
stirring sodium hyaluronate, recombinant human collagen, herba Centellae extract, oligopeptide-5 and bluecopper peptide with sterile warm water (34 deg.C) until completely dissolved, adding mevalonic lactone and superoxide dismutase, stirring, and filtering with 400 mesh filter cloth to obtain solution B;
cooling the solution A to normal temperature, filtering with 500 mesh filter cloth, adding the solution B, stirring, and packaging into mold.
Placing the mold filled with the solution into a freeze-drying device, setting the temperature of a plate layer to be-41 ℃, controlling the temperature of a product to be-34 ℃, keeping the temperature for 90min, and then demolding; returning the demolded freeze-dried substance to continue freeze-drying for about 20 min;
starting a vacuum device for vacuumizing, and keeping the environmental pressure at 28-33 pa; then, starting temperature rise, and entering a sublimation stage:
firstly, heating to-5 ℃, keeping the temperature for 60min, and keeping the temperature for 90 min; then heating to 5 deg.C, using for 10min, and keeping the temperature for 80 min; heating to 13 deg.C, keeping the temperature for 10min, and keeping the temperature for 60 min;
finally, carrying out analysis and drying:
heating the shelf to 41 deg.C, heating the product to 33 deg.C, maintaining the temperature for 60min, and maintaining the temperature for 300 min; controlling the water content in the product to be lower than 5 wt% to obtain the freeze-dried tablet.
In order to demonstrate the effects of the recombinant human collagen-containing composition, the lyophilized product and the cosmetic provided in the present application, the following experiments were performed:
1. skin hydration
Selecting 50 women of 35-55 years old as testers, dissolving the freeze-dried balls provided in the embodiment 2 in water in the morning and evening every day, and smearing the mixture on the face once in the morning and at night to serve as an experimental group 1;
control group 1
50 women in the same area and age were selected as a control group without any cosmetics.
After 7 days of the experiment, the moisturizing effect was evaluated by measuring with a skin cutin tester, and the hydration of the facial skin of the experimental group was increased by 40.37% on average as compared with the control group. It is shown that the skin can be made healthier and more moist by using the lyophilized pellet provided in example 2.
2. Anti-aging effect
Selecting 50 women of 40-65 years old as testers, dissolving the lyophilized tablet provided in example 5 in water in the morning and evening every day, smearing the solution on the face, and testing for 28 days in the morning and evening to obtain an experimental group 2;
control group 2
50 women in the same area and age were selected as a control group without any cosmetics.
Compared with the control group 2, the skin elasticity of the experimental group 2 is increased by 20.54 percent, the skin elasticity is increased by 32.13 percent, and the wrinkle depth is reduced by 22.47 percent by using a skin elasticity tester MAP580 for testing.
3. Restoration of red blood cell
The freeze-dried ball prepared in example 4 was dissolved in purified water and directly applied to the face of the subject once in the morning and evening, and the part with red blood streaks was reused and tapped until completely absorbed. The results after 28 days are shown in FIG. 1. As can be seen from FIG. 1, before use (left side of FIG. 1), the face of the subject had visible red blood streaks; after use (right side of fig. 1), the skin is basically disappeared, and the composition provided by the application has good skin repairing effect.
The composition, the freeze-dried material and the cosmetics containing the recombinant human collagen have the effects of moisturizing, brightening skin, resisting aging, removing wrinkles, protecting, repairing and the like. The preparation method of the freeze-dried material provided by the application can well keep the stability of the composition, and is convenient to produce, transport, sell and use.
The composition and the freeze-dried material containing the recombinant human collagen provided by the application can be compounded with other components; in aspect of form, the traditional cosmetic can be prepared into water agent, ointment, dressing and other common cosmetic forms.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (10)
1. A composition containing recombinant human collagen is characterized in that the raw materials comprise, by mass:
0.1 to 10 percent of mannitol, 0.01 to 3 percent of pullulanase polysaccharide, 0.01 to 1.2 percent of recombinant human collagen, 0.01 to 0.1 percent of mevalonolactone and the balance of water.
2. The composition according to claim 1, characterized in that the raw materials further comprise, in mass percent: 0.01 to 0.5 percent of sodium hyaluronate;
preferably, the composition further comprises the following raw materials in percentage by mass: centella asiatica extract 0.01-1.5%;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01 to 0.5 percent of lycopene;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.001-0.1% of water-soluble peptide powder;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01% -1% of blue copper peptide;
preferably, the water-soluble peptide powder comprises one or more of oligopeptide-5, tripeptide-1, acetyl hexapeptide-8 and pentapeptide-3.
3. The composition according to claim 1 or 2, characterized in that the raw materials further comprise, in mass percent: 0.01% -10% of astaxanthin;
preferably, the composition further comprises the following raw materials in percentage by mass: 0.01% -1% of superoxide dismutase.
4. A lyophilized material prepared by lyophilizing the composition containing recombinant human collagen according to any one of claims 1 to 3.
5. The lyophilizate of claim 4, wherein said lyophilizate comprises one or more of a lyophilized powder, lyophilized pellet, lyophilized tablet.
6. A method of preparing a lyophilisate according to claim 4 or 5, comprising:
dissolving the components in the raw materials in water, and freeze-drying to obtain the freeze-dried material.
7. The method according to claim 6, wherein the mass content of water in the freeze-dried material is 5% or less.
8. The preparation method according to claim 6, wherein the specific process of dissolving the components of the raw materials in water comprises:
dissolving mannitol and pullulanase in water, and then carrying out first filtration and sterilization to obtain a solution A;
dissolving the recombinant human collagen and the mevalonolactone in water, and then carrying out second filtration to obtain a solution B;
mixing the solution A and the solution B, and uniformly stirring;
preferably, the first filtration and the second filtration independently use 400 mesh or 500 mesh filter cloth.
9. The preparation method according to any one of claims 6 to 8, wherein the lyophilization process comprises a freezing stage, a sublimation stage, and a desorption drying stage;
preferably, the temperature of the material in the freezing stage is-33 ℃ to-35 ℃, and the freezing time is 100-;
preferably, the vacuum degree of the sublimation stage is 28-33 pa;
preferably, the sublimation stage adopts temperature programming;
preferably, the mass temperature of the desorption drying stage is 32-34 ℃.
10. A cosmetic comprising the recombinant human collagen-containing composition according to any one of claims 1 to 3 or the lyophilized product according to claim 4 or 5.
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Application publication date: 20200407 |