CN110613628B - Anti-aging composition, freeze-dried powder containing anti-aging composition and preparation method of freeze-dried powder - Google Patents
Anti-aging composition, freeze-dried powder containing anti-aging composition and preparation method of freeze-dried powder Download PDFInfo
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- CN110613628B CN110613628B CN201910837576.6A CN201910837576A CN110613628B CN 110613628 B CN110613628 B CN 110613628B CN 201910837576 A CN201910837576 A CN 201910837576A CN 110613628 B CN110613628 B CN 110613628B
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
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- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
The invention relates to the technical field of cosmetics, and particularly relates to an anti-aging composition, freeze-dried powder containing the anti-aging composition and a preparation method of the freeze-dried powder. The anti-aging composition consists of 0.2 to 2 parts by weight of serum albumin and 0.05 to 40 parts by weight of oligopeptides. The serum albumin and the specific oligopeptide are compounded, and test results show that the compounded composition has remarkable moisturizing and anti-aging effects. The freeze-dried powder prepared by the composition has obvious anti-aging effect, the frozen appearance is beautiful and smooth, no crack, no atrophy, no wall separation, no roughness, no delamination and long storage life; meanwhile, no preservative is added, so that the safety is higher.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to an anti-aging composition, freeze-dried powder containing the anti-aging composition and a preparation method of the freeze-dried powder.
Background
"anti-aging" is never a stale topic. The largest organ on the surface of the human body is, by no means, the skin, which is in direct contact with the external environment, and is subjected to conditions such as: air pollution, oxidation, ultraviolet irradiation, and other harmful factors. People who love beauty will not feel worry all the time. Furthermore, with age, the skin is more or less characterised by facial ageing, such as wrinkles, decreased elasticity, pigmentation and the like. This phenomenon is contrary to the current pursuit of beauty.
Although the eight five-flower efficacy declaration appears in the market in the past rapid development stage, the anti-aging effect is still high, and the development quantity of the anti-aging effect product in the markets in China and Japan is rapidly increased according to the development trend of new products in the world, which is in line with the demand of consumers.
However, most of the anti-aging products on the market are added with concepts, and the number of products really effective is very small. At the same time, consumers are still at the level of the loss of cognition, only knowing the "alleged ingredient" and not knowing the exertion of a specific role. This has led to a very popular "fry concept" for some time, ignoring the real value of the product itself.
The majority of the products currently on the market are traditional cosmetic formulations such as: the water emulsion cream, and the products of the preparation formulation can not protect the activity of the functional raw materials in the formula, thereby greatly reducing the efficacy of the product. In particular, the development of a composition with remarkable anti-aging effect and a freeze-dried powder preparation capable of protecting the activity of functional raw materials of the product for a long time have important practical significance.
Disclosure of Invention
In view of the above, the present invention aims to provide an anti-aging composition, a lyophilized powder containing the anti-aging composition, and a preparation method thereof. The composition provided by the invention has a remarkable anti-aging effect, and the freeze-dried powder prepared from the composition has a good anti-aging effect, is beautiful and smooth in frozen appearance, is free from crack, atrophy, wall separation, roughness and delamination, and is long in storage life; meanwhile, no preservative is added, so that the safety is higher.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
the invention provides an anti-aging composition, which consists of 0.2 to 2 parts of serum albumin and 0.05 to 40 parts of oligopeptides in parts by weight.
In some embodiments, the anti-aging composition consists of 0.2 to 1 part serum albumin and 0.4 to 1.5 parts oligopeptides.
In some embodiments, the oligopeptide is at least one of oligopeptide-1, oligopeptide-3, oligopeptide-5.
The invention also provides application of the composition in preparing health care products and/or cosmetics with anti-aging effect.
The invention also provides anti-aging freeze-dried powder which consists of the anti-aging composition, a stabilizer and deionized water.
In some embodiments, the lyophilized powder is made from the following components in parts by weight:
0.2 to 1 portion of serum albumin, 0.4 to 1.5 portions of oligopeptide, 207 to 257.23 portions of stabilizer and 771.37 to 821 portions of deionized water.
In some embodiments, the stabilizing agent is one or more of a lyoprotectant, an acid-base modifier, an emulsifier.
Wherein the freeze-drying protective agent is one or more of trehalose, glycine, mannitol, dextran and lactose;
the acid-base regulator is one or more of disodium hydrogen phosphate, sodium dihydrogen phosphate, amino acid and potassium citrate.
The emulsifier is one or more of polysorbate-20, polysorbate-60 and polysorbate-80.
In some embodiments, the lyophilized powder is made from the following components:
1 part of serum albumin, 1 part of oligopeptide-5, 2 parts of trehalose, 205 parts of mannitol and 821 parts of deionized water.
In some embodiments, the lyophilized powder is made from the following components:
1 part of serum albumin, 1.5 parts of oligopeptides, 250 parts of stabilizing agent and 8978 parts of deionized water zxft 8978;
wherein, the oligopeptides are: oligopeptide-1.5 parts, oligopeptide-3.5 parts and oligopeptide-5.5 parts;
the stabilizer is: 10 parts of trehalose and 240 parts of mannitol.
In some embodiments, the lyophilized powder is made from the following components:
1 part of serum albumin, 0.4 part of oligopeptides, 257.23 parts of stabilizer and 771.37 parts of deionized water;
wherein, the oligopeptides comprise oligopeptide-1.2 parts and oligopeptide-5.2 parts;
the stabilizer is: trehalose 0.7 parts, glycine 1 part, sodium dihydrogen phosphate 0.06 parts, disodium hydrogen phosphate 0.4 parts, polysorbate-20.07 parts and mannitol 255 parts.
The invention also provides a preparation method of the anti-aging freeze-dried powder, which comprises the steps of mixing the serum albumin, the oligopeptides, the stabilizer and the deionized water, filtering for sterilization, and carrying out vacuum freeze-drying to obtain the anti-aging freeze-dried powder.
In some embodiments, the filter sterilization is performed by sequentially passing through 0.45 μm and 0.22 μm filter elements.
In some embodiments, the vacuum freeze-drying is performed by pre-freezing at-40 ℃ for 1-4 h, vacuumizing to 0.19mbar, and heating for sublimation drying for 20-28 h until the water is completely sublimated.
In some embodiments, the preparation method of the anti-aging freeze-dried powder comprises the following steps:
dissolving and mixing raw materials of the freeze-dried powder in sequence, filtering through filter elements with the particle size of 0.45 mu m and 0.22 mu m respectively, adding the mixture into a container in a hundred-grade area, placing the container in a vacuum freeze-drying machine after plugging, pre-freezing for 1 to 4 hours at the temperature of minus 40 ℃, vacuumizing to 0.19mbar, heating for sublimation and drying for 20 to 28 hours until the water is completely sublimated, and sealing by pressing a plug under the vacuum condition and then bundling and packaging.
The serum albumin and the specific oligopeptide are compounded, and test results show that the compounded composition has remarkable moisturizing and anti-aging effects. The freeze-dried powder prepared by the composition has obvious anti-aging effect and long storage life; meanwhile, no preservative is added, so that the safety is higher.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 shows the recovery effect of three oligopeptides on cell scratch;
FIG. 2 is a graph of the mean values of examples 1-3 after testing and comparative examples 1-8 after testing, respectively, showing the effect of lyophilized powder on skin moisture content;
FIG. 3 is a graph of skin wrinkles, wherein 3-a is a result of the fourth week after using the lyophilized powder of comparative example 5, the overrun inclusion ratio in the whole data system is 53%;3-b is the result of the fourth week after using the lyophilized powder of example 3, the overrun occupancy ratio in the whole data system is 89%;
FIG. 4 is a skin texture condition, where 4-a is the result of the fourth week after use of the lyophilized powder of comparative example 5, with an over-inclusion ratio of 16% in the entire data system; 4-b is the results of the fourth week after using the lyophilized powder of example 3, with an over-range of 93% in the overall data system (the test instrument is VISIA, with a certain amount of its own database inside, 16% indicating that the degree of good texture state is only over 16% of the skin texture state of the person in the database, and 93% indicating that the degree of good texture state is over 93% of the skin texture state of the person in the database).
Detailed Description
The invention discloses an anti-aging composition, freeze-dried powder containing the anti-aging composition and a preparation method thereof, and a person skilled in the art can realize the anti-aging composition by appropriately improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
Interpretation of terms:
freeze-drying powder: freezing the water in the components in advance by adopting a vacuum freeze-drying method of a freeze dryer, and then sublimating the frozen water in the components in a vacuum sterile environment to obtain a freeze-dried product.
The invention is further illustrated by the following examples:
example 1 preparation of anti-aging lyophilized powder of the invention
Weighing 1 part of serum albumin, 1 part of oligopeptide (oligopeptide-5), 207 parts of stabilizer (trehalose 2 and mannitol 205) and 821 parts of deionized water, uniformly mixing, filtering and sterilizing, placing in a penicillin bottle of 3ml/5ml, plugging, placing in a vacuum freeze dryer, pre-freezing for 1-4 h at-40 ℃, vacuumizing to 0.19mbar, heating for sublimation drying for 20-28 h until water is completely sublimated, capping and packaging after plugging and sealing, thus obtaining the anti-aging freeze-dried powder.
Example 2 preparation of anti-aging lyophilized powder of the present invention
Weighing 1 part of serum albumin, 1.5 parts of oligopeptides, 250 parts of stabilizer and 8978 parts of deionized water of 777.5, mixing uniformly, filtering and sterilizing, putting the mixture into a penicillin bottle of 3ml/5ml, placing the penicillin bottle into a vacuum freeze dryer after plugging, pre-freezing for 1-4 h at minus 40 ℃, vacuumizing to 0.19mbar, heating for sublimation and drying for 20-28 h until water is completely sublimated, and capping and packaging after plugging and sealing to obtain the anti-aging freeze-dried powder.
Wherein, the oligopeptides are: oligopeptide-1.5 parts, oligopeptide-3.5 parts and oligopeptide-5.5 parts.
Wherein, the stabilizer is: 10 parts of trehalose and 240 parts of mannitol.
Example 3 preparation of anti-aging lyophilized powder of the invention
Weighing 1 part of serum albumin, 0.4 part of oligopeptides, 257.23 parts of stabilizer and 771.37 parts of deionized water, uniformly mixing, filtering and sterilizing, putting into a penicillin bottle of 3ml/5ml, adding a stopper, putting into a vacuum freeze dryer, adding the stopper, putting into the vacuum freeze dryer, pre-freezing for 1-4 h at-40 ℃, vacuumizing to 0.19mbar, heating for sublimation and drying for 20-28 h until water is completely sublimated, pressing the stopper, sealing, and then bundling and packaging to obtain the anti-aging freeze-dried powder.
Wherein, the oligopeptides comprise oligopeptide-1.2 parts and oligopeptide-5.2 parts;
the stabilizer is: trehalose 0.7 parts, glycine 1 part, sodium dihydrogen phosphate 0.06 parts, disodium hydrogen phosphate 0.4 parts, polysorbate-20.07 parts and mannitol 255 parts.
Comparative example 1
Comparative example 1 is different from example 1 in that serum albumin was not added while 45 parts of mannitol was reduced, and the remaining components and amounts were the same as in example 1.
Comprises the following components: oligopeptide-5 parts, stabilizer 162 parts (trehalose 2 parts, mannitol 160 parts), deionized water 867 parts
The lyophilized powder was prepared in the same manner as in example 1.
Comparative example 2 preparation of lyophilized powder
Comparative example 2 differs from example 1 in that no oligopeptides were added and the stabilizer consisted of 10 parts trehalose and 195 parts mannitol.
Comprises the following components: 1 part of serum albumin, 205 parts of stabilizer (10 parts of trehalose and 195 parts of mannitol) and 824 parts of deionized water.
The process for preparing the lyophilized powder is the same as in example 1.
Comparative example 3 preparation of lyophilized powder
Comparative example 3 is different from example 2 in that trehalose was reduced by 5 parts and mannitol was reduced by 80 parts without adding serum albumin, and the remaining components and amounts were the same as in example 2.
Comprises the following components: 1.5 parts of oligopeptides, 165 parts of stabilizer and 8978 parts of deionized water of 863.5 parts;
wherein, the oligopeptides are: oligopeptide-10.5 parts, oligopeptide-30.5 parts and oligopeptide-50.5 parts; the stabilizer is: 5 parts of trehalose and 160 parts of mannitol.
The process for preparing the lyophilized powder is the same as in example 2.
Comparative example 4 preparation of lyophilized powder
Comparative example 4 differs from example 2 in that, without addition of oligopeptides, trehalose was reduced by 5 parts while mannitol was reduced by 80 parts, and the remaining components and relative contents were the same as in example 2.
Comprises the following components: 1 part of serum albumin, 165 parts of a stabilizer and 864 parts of deionized water;
wherein, the stabilizer is: 5 parts of trehalose and 160 parts of mannitol.
The process for preparing the lyophilized powder is the same as in example 2.
Comparative example 5 preparation of lyophilized powder
Comparative example 5 is different from example 3 in that mannitol was reduced by 100 parts without adding sodium dihydrogen phosphate and without adding disodium hydrogen phosphate, and the remaining components and amounts were the same as example 3.
Comprises the following components: 1 part of serum albumin, 0.4 part of oligopeptides, 5363 parts of stabilizer 156.77 parts, 3242 parts of deionized water 871.83 parts,
wherein, the oligopeptides are: oligopeptide-10.2 parts, oligopeptide-50.2 parts;
the stabilizer is: trehalose 0.7 parts, glycine 1 part, polysorbate-20.07 parts and mannitol 155 parts.
The process for preparing the lyophilized powder is the same as in example 3.
Comparative example 6 preparation of lyophilized powder
Comparative example 6 is different from example 3 in that mannitol was reduced by 100 parts without adding serum albumin, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the remaining components and amounts thereof were the same as in example 2.
Comprises the following components: 0.4 parts of oligopeptides, 5363 parts of stabilizer 156.77 parts and 3242 parts of deionized water 872.83 parts;
wherein, the oligopeptides are: oligopeptide-1, oligopeptide-5, oligopeptide-10.2 parts, oligopeptide-50.2 parts;
the stabilizer is: trehalose 0.7 parts, glycine 1 part, polysorbate-20.07 parts and mannitol 155 parts.
The process for preparing the lyophilized powder is the same as in example 3.
Comparative example 7 preparation of lyophilized powder
Comparative example 7 is different from example 3 in that mannitol was reduced by 100 parts without adding serum albumin, polysorbate-20, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the remaining components and relative contents were the same as those of example 2.
Comprises the following components: 0.4 part of oligopeptides, 156.7 parts of stabilizing agent and 8978 parts of deionized water 872.9 parts;
wherein, the oligopeptides are: oligopeptide-1, oligopeptide-5, oligopeptide-10.2 parts, oligopeptide-50.2 parts;
the stabilizer is: 0.7 part of trehalose, 1 part of glycine and 155 parts of mannitol.
The process for preparing the lyophilized powder is the same as in example 3.
Comparative example 8 preparation of lyophilized powder
Comparative example 8 is different from example 3 in that, without adding oligopeptides, polysorbate-20, sodium dihydrogen phosphate and disodium hydrogen phosphate, mannitol was reduced by 100 parts, and the remaining components and relative contents were the same as those of example 2.
Comprises the following components: 1 part of serum albumin, 156.7 parts of stabilizing agent and 5363 parts of deionized water 872.3;
wherein, the stabilizer is: 0.7 part of trehalose, 1 part of glycine and 155 parts of mannitol.
The process for preparing the lyophilized powder is the same as in example 3.
Example 4 testing of appearance of lyophilized powder
TABLE 1
As can be seen from table 1, the freeze-dried powders of embodiments 1 to 3 of the present invention have good appearance, which is specifically represented as: the surface is not rough, and the conditions of layering, atrophy, cracking and wall separation do not exist, while the appearance state of the freeze-dried powder prepared by adopting other formulas in comparative examples 1-8 is poorer.
Example 5 oligopeptide cell regeneration repair assay
Experimental products: oligopeptide-1, oligopeptide-3, oligopeptide-5
The effect of oligopeptide-1, oligopeptide-3 and oligopeptide-5 on repairing and proliferating the scratched cells is measured by using a cell culture technology, and the test method comprises the following steps: firstly culturing cells, then putting a mark pen at the back of a 6-hole plate, using a ruler to draw transverse lines uniformly, and traversing through holes approximately every 0.5-1 cm. Each hole passes through at least 5 lines.
Resuspending the cells in a cell passaging step at a density of about 25000 to 30000 cells/mL and in an amount slightly greater than that required for plating. When plating, the cell suspension was added to a 6-well plate using a pipette gun while shaking the cell suspension, and 2ml of the cell suspension was added to each well. And after the plate paving is finished, putting the 6-hole plate into a cell culture box, and culturing for 24 +/-2 hours.
The gun head is perpendicular to the transverse line scratch on the back as much as possible compared with the straight ruler, and the gun head is perpendicular and cannot be inclined. The cells were washed 3 times with PBS, the scraped cells were washed off, 2ml of maintenance serum medium containing drug was added at 1 concentration per well, and 2ml of complete medium containing no drug was added to the negative control group. The cells were cultured in a 37-degree-5-vol CO2 incubator. Samples were taken at 0, 24 hours and photographed. The results are shown in FIG. 1.
As can be seen from FIG. 1, the scratches of the cells recover to different degrees from 0h to 24h, which indicates that the oligopeptides oligopeptide-1, oligopeptide-3 and oligopeptide-5 have good effects of promoting cell proliferation and repair and have good anti-aging effects.
Example 6 testing of moisturizing and anti-aging efficacy of lyophilized powder
A good anti-aging product needs to be established on the basis of a good moisturizing effect, and the moisturizing effect of the freeze-dried powders in the examples 1-3 and the comparative examples 1-8 is compared by using an in-vivo test in the embodiment.
Experimental products: EXAMPLES 1-3 AND COMPARATIVE EXAMPLES 1-8 Freeze-dried powder + physiological saline
Blank control: physiological saline
The test method comprises the following steps: 35 volunteers meeting the requirements are selected, and each volunteer is used in the morning and evening, a half-face experimental article and a half-face blank control article, and skin moisture values are tested in the Ceilala Stem cell company at the 0 th week, the 1 st week, the 2 nd week, the 3 rd week and the 4 th week, and the results are shown in a graph 2 and a table 2.
Testing an instrument: skin moisture tester (Corneometer CM825 MDD).
TABLE 2 skin moisture values
As can be seen from Table 1 and FIG. 2, the compositions of the present invention have scientific mixture ratio, the moisture value (mean moisture value in the fourth week of examples 1 to 3) is increased by 32.29% compared with that before use (mean moisture value before use in examples 1 to 3) at week 4, and compared with comparative examples 1 to 8, the compositions show significant difference (p < 0.05) in improving skin moisture, which indicates that the composition of the present invention has significant synergistic effect.
Example 7 Freeze-dried powder anti-aging efficacy test
The anti-wrinkle effect of the lyophilized powders of examples 1-3 and comparative examples 1-8 on skin was evaluated using the VISIA skin imaging system. This example illustrates the study of example 3 and comparative example 5
Experimental products: 3+ physiological saline solution
Comparison products: comparative example 5 lyophilized powder + physiological saline
The test method comprises the following steps: and selecting 35 volunteers meeting the requirements, using the experimental sample for half face and the blank reference sample for half face every morning and evening, and testing the skin in the Ceilera stem cell company in 4 th week, wherein the results are shown in figures 3-4.
Testing the instrument: skin test system (VISIA).
As can be seen from FIGS. 3 to 4, the freeze-dried powder of the invention has good wrinkle-removing effect, can well smooth the texture, and has an effect obviously superior to that of the freeze-dried powder of the comparative example.
The freeze-dried powder of the embodiment 3 with the preservation time of 1 year is adopted to carry out the tests of the embodiments 6 to 7, and the results are similar to those of the embodiments 6 to 7 and have no obvious difference. The freeze-dried powder still has obvious anti-aging effect after being stored for a long time.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. An anti-aging freeze-dried powder is characterized by consisting of 1 part of serum albumin, 0.2 part of oligopeptide, 0.7 part of trehalose, 1 part of glycine, 0.06 part of sodium dihydrogen phosphate, 0.4 part of disodium hydrogen phosphate, 0.07 part of polysorbate-20 and 255 parts of mannitol.
2. The preparation method of the anti-aging freeze-dried powder of claim 1, wherein the anti-aging freeze-dried powder is obtained by mixing serum albumin, oligopeptides, a stabilizer and deionized water, filtering for sterilization, and performing vacuum freeze-drying.
3. The preparation method according to claim 2, wherein the vacuum freeze-drying is performed by pre-freezing at-40 ℃ for 1-4 h, vacuumizing to 0.19mbar, and heating for sublimation drying for 20-28 h until water is completely sublimated.
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