CN112156033A - Essence containing ultra-small molecule sodium hyaluronate and preparation method thereof - Google Patents

Essence containing ultra-small molecule sodium hyaluronate and preparation method thereof Download PDF

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CN112156033A
CN112156033A CN202011107935.1A CN202011107935A CN112156033A CN 112156033 A CN112156033 A CN 112156033A CN 202011107935 A CN202011107935 A CN 202011107935A CN 112156033 A CN112156033 A CN 112156033A
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sodium hyaluronate
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essence
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CN112156033B (en
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田悦
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Nanjing Letao Biotechnology Co ltd
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Nanjing Baiziya Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
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Abstract

The invention discloses an essence containing ultra-small molecule sodium hyaluronate and a preparation method thereof, belonging to the technical field of cosmetics. The essence comprises the following components in percentage by weight: 0.01-3 wt% of ultra-small molecular sodium hyaluronate with molecular weight of 1-3kDa, 0.01-2 wt% of hydrolyzed sodium hyaluronate with molecular weight of 10-50kDa, 0.01-1 wt% of macromolecular sodium hyaluronate with molecular weight of 1000kDa or more, 0.2-16 wt% of humectant, 0.2-7 wt% of bacteriostatic agent and the balance of water. The essence disclosed by the invention is unexpectedly found to have excellent anti-wrinkle and anti-aging effects on the basis of long-acting water replenishing and moisturizing, is not sticky and greasy in skin feel after being applied, is better absorbed, and has the effects of repairing cuticles, improving skin textures and regulating skin cell activity.

Description

Essence containing ultra-small molecule sodium hyaluronate and preparation method thereof
Technical Field
The invention relates to an essence containing ultra-small molecular sodium hyaluronate and a preparation method thereof, belonging to the technical field of cosmetics.
Background
With the increasing pursuit of beauty, the skin care requirement of people is higher and higher, and the naturalization, the safety and the curative effect become more and more important development directions. The essence is an important product in skin care products, and the components of the high-efficiency refined essence have multiple effects of moisturizing, repairing, whitening, removing freckles, resisting wrinkles and the like.
Hyaluronic acid has super-strong water absorption and water locking capacity and is widely used in cosmetic formulas, but in order to pursue short-term functional effects, hyaluronic acid essence on the prior world can be added with various complex chemical components and preservatives, and after long-term use, the hyaluronic acid essence can erode human skin and cause various adverse reactions such as allergy, redness and swelling and the like; macromolecular hyaluronic acid of single component has a large molecular weight, and skin absorption efficiency is low, so that the effective components of the macromolecular hyaluronic acid stay on the surface of skin, and the macromolecular hyaluronic acid is difficult to achieve the effects of moisturizing and wrinkle resistance.
The components disclosed in the prior art patent application CN109223618A contain 7 components in total, including 4 different forms of sodium hyaluronate, except hydrolyzed sodium hyaluronate with a molecular weight of less than 10kDa and sodium hyaluronate with a molecular weight of 60 kDa-1000 kDa, acetylated sodium hyaluronate, a sodium hyaluronate cross-linked polymer, a humectant, a soothing and repairing agent and a stabilizer, so that sodium hyaluronate with different forms needs to be prepared or purchased respectively, and there are many types of additives, which has a certain safety risk problem.
Patent application CN107432849A discloses a micromolecular hyaluronic acid muscle base fluid, the molecular weight of which is less than 3kDa, the main functions are to inhibit the generation of melanin, fade spots, enable damaged cells to be quickly filled, and have a good improvement effect on acne, the micromolecular hyaluronic acid muscle base fluid comprises 16 total components such as micromolecular sodium hyaluronate, hyaluronic acid and the like, the components are complex, certain potential safety hazards exist, and the cost is high.
Sodium hyaluronate essence adopts multi-dose packing in the market mostly, easily causes pollution waste, needs to add antiseptic in order to guarantee the validity period of essence, and the antiseptic easily causes many-sided problem of skin, and single dose packing that does not add the antiseptic becomes a form that people preferred gradually.
Based on the reasons, the development of the sodium hyaluronate essence which is safe, natural, simple and effective and has excellent moisturizing, anti-wrinkle and anti-aging effects is urgently needed.
Disclosure of Invention
In order to overcome the problems of complex components, poor safety, low skin absorption efficiency and non-ideal anti-aging effect of the existing essence products on the market, the invention aims to provide the essence which is safe, natural, simple and effective and has excellent water replenishing, moisturizing, anti-wrinkle and anti-aging effects and the preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
an essence containing ultra-small molecule sodium hyaluronate, comprising: the weight percentage of the ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa-3kDa is 0.01-3 percent, the weight percentage of the hydrolyzed sodium hyaluronate with the molecular weight of 10kDa-50kDa is 0.01-2 percent, the weight percentage of the macromolecular sodium hyaluronate with the molecular weight of more than or equal to 1000kDa is 0.01-1 percent, the weight percentage of the humectant is 0.2-16 percent, the weight percentage of the bacteriostatic agent is 0.2-7 percent, and the balance is water.
As a further improvement of the invention, the weight percentage of the ultra-small molecule sodium hyaluronate is 0.1-1.0%; the weight percentage of the hydrolyzed sodium hyaluronate is 0.1-1.0%; the weight percentage of the macromolecular sodium hyaluronate is 0.1-0.5%; the humectant accounts for 3 to 13 percent by weight; the weight percentage of the bacteriostatic agent is 0.5-5%; the balance being water.
As a further improvement of the invention, the water is purified water.
As a further improvement of the invention, the humectant is methyl glucitol polyether and 1, 3-butanediol, and the bacteriostatic agent is 1, 2-pentanediol and 1, 2-hexanediol.
As a further improvement of the invention, the weight percentage of the methyl glucitol polyether is 0.1% -6%, and the weight percentage of the 1, 3-butanediol is 0.1% -10%; the weight percentage of the 1, 2-pentanediol is 0.1-5%, and the weight percentage of the 1, 2-hexanediol is 0.1-2%.
As a further improvement of the invention, the weight percentage of the methyl glucitol polyether is 1% -5%, and the weight percentage of the 1, 3-butanediol is 2% -8%; the weight percentage of the 1, 2-pentanediol is 0.4% -4%, and the weight percentage of the 1, 2-hexanediol is 0.5% -1%.
As a further improvement of the invention, the essence comprises 1 weight percent of ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa, 0.5 weight percent of hydrolyzed sodium hyaluronate with the molecular weight of 50kDa, 0.5 weight percent of macromolecular sodium hyaluronate with the molecular weight of 1000kDa, 3 weight percent of methyl glucitol polyether, 6 weight percent of 1, 3-butanediol, 2 weight percent of 1, 2-pentanediol, 0.5 weight percent of 1, 2-hexanediol and the balance of purified water.
The second purpose of the invention is to provide a preparation method of the essence containing the ultra-small molecule sodium hyaluronate, which comprises the following steps:
1) heating water to 50-80 deg.C, and maintaining the temperature;
2) uniformly mixing a humectant, a bacteriostatic agent, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate to obtain a mixed solution;
3) mixing the mixed solution obtained in the step 2) with the water obtained in the step 1), and stirring and dissolving to obtain the essence.
As a further improvement of the present invention, the preparation method comprises the following steps:
1) heating water to 50-80 deg.C, and maintaining the temperature;
2) uniformly mixing methyl glucitol polyether, 1, 3-butanediol, 1, 2-pentanediol and 1, 2-hexanediol with macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate to obtain a mixed solution;
3) mixing the mixed liquid obtained in the step 2) with the purified water obtained in the step 1), and stirring for dissolving to obtain the essence.
The third purpose of the invention is to provide the application of the essence containing the ultra-small molecular sodium hyaluronate in the technical field of cosmetics, and the essence has the effects of long acting, deep moisturizing, skin texture improvement and wrinkle resistance.
The fourth purpose of the invention is to provide a cosmetic product containing the essence containing the ultra-small molecular sodium hyaluronate.
Compared with the prior art, the invention has the following advantages:
1. the essence containing the ultra-small molecular sodium hyaluronate adopts a unique combination mode of the ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa-3kDa, hydrolyzed sodium hyaluronate with the molecular weight of 10kDa-50kDa, macromolecular sodium hyaluronate with the molecular weight of more than or equal to 1000kDa, a humectant, a bacteriostatic agent and the balance of purified water, wherein the sodium hyaluronate is divided into three different average molecular weights, different functions are respectively realized, and the essence has the advantages of few types of additives, relatively simpler components, lower cost and better safety performance.
2. The essence containing the ultra-small molecular sodium hyaluronate disclosed by the invention is unexpectedly found to have excellent anti-wrinkle and anti-aging effects on the basis of moisturizing, and the essence is not sticky in skin after being applied and is better absorbed.
3. The invention adopts single-dose package without adding preservative, avoids skin problems caused by using the preservative, and has safer prescription proportion.
4. According to the invention, 1, 2-pentanediol and 1, 2-hexanediol are added to form a unique antibacterial system, no additional preservative is required to be added, and the cost is greatly saved.
5. The sodium hyaluronate contained in the invention has a non-single molecular weight, generates a complementary effect by the sodium hyaluronate with large and small molecules, and has no sticky feeling and better absorption when being used.
Drawings
Fig. 1 shows the results of the test of the water content of the stratum corneum of the skin before and after 4 weeks of continuous use of the ultra-small molecule sodium hyaluronate essence in examples and comparative examples.
Fig. 2 shows wrinkle improvement before and after 4 weeks of continuous use of the ultra-small molecule sodium hyaluronate essence in examples and comparative examples.
Detailed Description
The present invention is further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Prescription:
table 1 formula of essence of example 1
Figure BDA0002727575100000031
Figure BDA0002727575100000041
The preparation process of the ultra-small molecule sodium hyaluronate essence comprises the following steps: heating the deionized purified water to 60 ℃, and preserving heat; adding 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, methyl glucitol polyether, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate according to the formula amount, and stirring and mixing to uniformly disperse the materials to obtain a mixed solution; and stirring and dissolving the mixed solution and deionized purified water, cooling to room temperature, inspecting, and discharging after the mixed solution is qualified to obtain the colorless transparent essence.
Example 2
Prescription:
table 2 formula of essence of example 2
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1kDa) 1g 1%
2 Hydrolyzed sodium hyaluronate (50kDa) 0.5g 0.5%
3 Macromolecule sodium hyaluronate (1000kDa) 0.5g 0.5%
4 Humectant: methyl glucitol polyether 3g 3%
5 Humectant: 1, 3-butanediol 6g 6%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100ml Adding to 100 percent
The preparation process of the ultra-small molecule sodium hyaluronate essence comprises the following steps: heating the deionized purified water to 80 ℃, and preserving heat; adding 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, methyl glucitol polyether, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate according to the formula amount, and stirring and mixing to uniformly disperse the materials to obtain a mixed solution; and stirring and dissolving the mixed solution and deionized purified water, cooling to room temperature, inspecting, and discharging after the mixed solution is qualified to obtain the colorless transparent essence.
Example 3
Prescription:
table 3 formula of serum of example 3
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (2kDa) 0.5g 0.5%
2 Hydrolyzed sodium hyaluronate (30kDa) 0.5g 0.5%
3 Macromolecular hyaluronic acidSodium (3000kDa) 0.3g 0.3%
4 Humectant: methyl glucitol polyether 3g 3%
5 Humectant: 1, 3-butanediol 5g 5%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.8g 0.8%
8 Purified water Adding to 100mL Adding to 100 percent
The preparation process of the ultra-small molecule sodium hyaluronate essence comprises the following steps: heating the deionized purified water to 50 ℃, and preserving heat; adding 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, methyl glucitol polyether, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate according to the formula amount, and stirring and mixing to uniformly disperse the materials to obtain a mixed solution; and stirring and dissolving the mixed solution and deionized purified water, cooling to room temperature, inspecting, and discharging after the mixed solution is qualified to obtain the essence.
Example 4
Prescription:
table 4 formula of serum of example 4
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1.5kDa) 0.1g 0.1%
2 Hydrolyzed sodium hyaluronate (10kDa) 1.0g 1.0%
3 Macromolecule sodium hyaluronate (8000kDa) 0.5g 0.5%
4 Humectant: methyl glucitol polyether 1g 1%
5 Humectant: 1, 3-butanediol 8g 8%
6 Bacteriostatic agent: 1, 2-pentanediol 4g 4%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100mL Adding to 100 percent
The preparation process of the ultra-small molecule sodium hyaluronate essence comprises the following steps: heating the deionized purified water to 70 ℃, and preserving heat; adding 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, methyl glucitol polyether, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate according to the formula amount, and stirring and mixing to uniformly disperse the materials to obtain a mixed solution; and stirring and dissolving the mixed solution and deionized purified water, cooling to room temperature, inspecting, and discharging after the mixed solution is qualified to obtain the essence.
Example 5
Prescription:
table 5 formula for serum of example 5
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (2.5kDa) 1.0g 1.0%
2 Hydrolyzed sodium hyaluronate (40kDa) 0.1g 0.1%
3 Macromolecule sodium hyaluronate (4000kDa) 0.1g 0.1%
4 Humectant: methyl glucitol polyether 5g 5%
5 Humectant: 1, 3-butanediol 2g 2%
6 Bacteriostatic agent: 1, 2-pentanediol 0.4g 0.4%
7 Bacteriostatic agent: 1, 2-hexanediol 1g 1%
8 Purified water Adding to 100mL Adding to 100 percent
The preparation process of the ultra-small molecule sodium hyaluronate essence comprises the following steps:
heating the deionized purified water to 65 ℃, and preserving heat; adding 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, methyl glucitol polyether, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate according to the formula amount, and stirring and mixing to uniformly disperse the materials to obtain a mixed solution; and stirring and dissolving the mixed solution and deionized purified water, cooling to room temperature, inspecting, and discharging after the mixed solution is qualified to obtain the essence.
Comparative example 1
The serum was prepared according to the recipe of table 6, and the preparation process was the same as in example 2.
Table 6 formula of essence of comparative example 1
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1kDa) 1g 1%
3 Macromolecule sodium hyaluronate (1000kDa) 0.5g 0.5%
4 Humectant: methyl glucitol polyether 3g 3%
5 Humectant: 1, 3-butanediol 6g 6%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100ml Adding to 100 percent
Comparative example 2
The serum was prepared according to the recipe of table 7, and the preparation process was the same as in example 2.
Table 7 formula of essence of comparative example 2
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1kDa) 1g 1%
2 Hydrolyzed sodium hyaluronate (50kDa) 0.5g 0.5%
4 Humectant: methyl glucitol polyether 3g 3%
5 Humectant: 1, 3-butanediol 6g 6%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100ml Adding to 100 percent
Comparative example 3
The serum was prepared according to the recipe of table 8, and the preparation process was the same as in example 2.
Table 8 formula of essence of comparative example 3
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1kDa) 1g 1%
2 Hydrolyzed sodium hyaluronate (50kDa) 0.5g 0.5%
3 Macromolecule sodium hyaluronate (1000kDa) 0.5g 0.5%
4 Humectant: polyglutamic acid 3g 3%
5 Humectant: luba gum oil 6g 6%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100ml Adding to 100 percent
Comparative example 4
The serum was prepared according to the recipe of table 9, and the preparation process was the same as in example 2.
Table 9 formula of essence of comparative example 4
Figure BDA0002727575100000061
Figure BDA0002727575100000071
Comparative example 5
The serum was prepared according to the recipe in table 10, and the preparation process was the same as in example 2.
TABLE 10 formula of essence of comparative example 5
# Composition (I) Prescription amount (g or ml) Weight percent of
1 Ultra-small molecule sodium hyaluronate (1kDa) 1g 1%
2 Hydrolyzed sodium hyaluronate (500kDa) 0.5g 0.5%
3 Macromolecule sodium hyaluronate (1000kDa) 0.5g 0.5%
4 Humectant: methyl glucitol polyether 3g 3%
5 Humectant: 1, 3-butanediol 6g 6%
6 Bacteriostatic agent: 1, 2-pentanediol 2g 2%
7 Bacteriostatic agent: 1, 2-hexanediol 0.5g 0.5%
8 Purified water Adding to 100ml Adding to 100 percent
In order to prove that the skin-moistening cream has the effect of lasting skin moistening, can repair cuticle to a certain degree, achieves the effects of deep moisturizing and skin bottom repairing, and also has a certain anti-wrinkle effect, the skin-moistening cream is subjected to the following skin moisture test, anti-wrinkle effect test and skin irritation test.
Example 6 skin moisture test
Testing an instrument: skin moisture tester corneometer cm 825.
The test method comprises the following steps: 80 subjects were selected, aged 35-55 years, and divided into 10 groups of 8 persons each. The Corneometer value test of the water content of the horny layer of the face skin is respectively carried out on each group of subjects before the face uses the test product, 14 days after the essence liquid is used together with the essence liquid of the examples 1-5 and the comparative examples 1-4, the higher the Corneometer value is, the higher the moisture content of the horny layer of the face skin is, the test of the same subject is finished by the same expert evaluator, and the measured parts and indoor temperature and humidity are kept consistent. The tested environment temperature is 20.3-21.8 ℃, and the relative humidity is 48.0-54.0%.
The results of the Corneometer value measurements of the water content of the stratum corneum are shown in tables 11 and 12 below:
TABLE 11 measurement results of moisture content of stratum corneum of examples 1 to 5 and comparative examples 1 to 5
Figure BDA0002727575100000072
Figure BDA0002727575100000081
The test results are shown in figure 1. The test result shows that the Corneometer value of the stratum corneum of the skin is remarkably increased (p is less than 0.01) after the test products of the examples 1 to 5 are continuously used for 14 days and 28 days, and the water content reaches more than 60 on the 14 th day of the product use; the ultra-small molecular sodium hyaluronate essence can lock water on the surface of skin, replenish water and soften the skin, can be quickly absorbed through skin to reach an epidermal layer and a corium layer, restores the horny layer through nutrition, increases the water content of the horny layer, and plays a role in deeply replenishing water and moisturizing. Especially, the formula of the example 2 has the best moisturizing effect.
In addition, in example 2, compared with comparative examples 1-2, when hydrolyzed sodium hyaluronate or macromolecular sodium hyaluronate is not contained, the moisturizing performance of the essence is obviously reduced, and the possible reason is that a good moisturizing structure or state cannot be formed after the sodium hyaluronate is lost and enters the inside of the skin, and finally the moisturizing effect is reduced; as compared with comparative example 3, it is clear that the choice of the moisturizer of the present invention is very important; compared with comparative example 4, the change of the bacteriostatic agent may affect the exertion of the effect of the whole essence.
TABLE 12 significance analysis of skin horny layer water content detection results of examples 1 to 5 and comparative examples 1 to 5
Figure BDA0002727575100000082
Figure BDA0002727575100000091
Statistical method: the analysis was carried out by the t-test method, and the test level α was 0.05. The significance labeling method comprises the following steps that n.s. indicates that no statistical difference exists, and p is more than or equal to 0.05; "+" indicates significant difference, p is more than or equal to 0.01 and less than 0.05; "x" indicates a very significant difference, p < 0.01; "x" indicates there was a very significant difference, p < 0.001. The number of the N used products is 80.
Example 7: anti-wrinkle efficacy test
Testing an instrument: VISIA-CR (CANFIELD, USA).
The test method comprises the following steps: 80 subjects with age ranging from 35 to 55 years old, facial skin wrinkles, and canthus wrinkle score of 3 points or more (D0) were selected for this test and divided into 10 groups of 8 persons on average. The Ra value of skin wrinkles (one side canthus) on the eyes of each group of subjects is measured before the face of the subject uses the product, 14 days after the face of the subject uses the essence described in examples 1-5 and comparative examples 1-5, and 28 days after the face of the subject uses the essence, wherein the Ra value reflects the roughness degree of the skin texture, and the larger the Ra value is, the rougher the skin is, and the deeper the wrinkles are; as shown in tables 13 and 14 below. The test of the same subject should be done by the same expert evaluator. The tested environment temperature is 20.3-21.8 ℃, and the relative humidity is 48.0-54.0%.
TABLE 13 results of Ra value measurement of skin wrinkles using the essences of examples 1 to 5 and comparative examples 1 to 5
Product(s) Basic value (0 day) After using the product for 14 days The product is used 28 days later
Essence of example 1 52.39 51.37 49.86
Essence of example 2 52.44 51.38 48.88
Essence of example 3 52.23 51.30 49.56
Essence of example 4 52.46 51.10 49.30
Essence of example 5 52.38 51.43 49.89
Essence of comparative example 1 52.56 52.16 51.08
Essence of comparative example 2 52.38 52.17 51.86
Essence of comparative example 3 52.36 52.08 51.10
Essence of comparative example 4 52.35 52.13 51.06
Essence of comparative example 5 52.41 52.21 51.05
The test results are shown in FIG. 2. The test result shows that after the test products of examples 1-5 are continuously used for 14 days and 28 days, the Ra value of the skin wrinkles (one side canthus) of the ultra-small molecular sodium hyaluronate essence has no significant difference on the 14 th day of the use of the products, and is significantly reduced (p is more than or equal to 0.01 and less than 0.05) on the 28 th day, and the Ra value is less than 50, namely the product can deeply nourish the skin, improve the skin texture, solve the problems of dry fine lines, aging and the like, and achieve the anti-wrinkle effect to a certain extent by enabling the skin to be more delicate. In particular, comparing example 2 with comparative example 2, it is understood that the presence or absence of macromolecular sodium hyaluronate has a great influence on wrinkle removal effect.
TABLE 14 significance analysis of Ra value of skin wrinkles measured using the essences of examples 1 to 5 and comparative examples 1 to 5
Figure BDA0002727575100000101
Statistical method: the analysis was carried out by the t-test method, and the test level α was 0.05. The significance labeling method comprises the following steps that n.s. indicates that no statistical difference exists, and p is more than or equal to 0.05; "+" indicates significant difference, p is 0.01 ≦ p < 0.05. The number of the N used products is 80.
Example 8: skin irritation test
40 subjects were selected and evenly divided into 5 groups, and 8 subjects per group were subjected to a human trial test for 4 weeks, and the human trial test was studied to observe the safety of the essence of examples 1 to 5 on human skin, and no adverse skin reaction was observed by visual observation, as shown in table 15 below. The evaluation standard refers to the grading standard of adverse reaction of human trial test skin specified in 2015 edition of technical Specification for cosmetic safety.
TABLE 15 results of skin irritation test using the essences of examples 1 to 5
Figure BDA0002727575100000102
Figure BDA0002727575100000111
Test results show that the ultra-small molecule sodium hyaluronate essence provided by the invention has no adverse reaction to skin, is safe and has no stimulation to skin.
Example 9: experiment for inhibiting bacteria
The essences of the embodiment 2 and the comparative example 4 of the invention are respectively adopted, staphylococcus aureus and candida albicans are selected as test strains to carry out bacteriostatic performance experiments, and the results are shown in table 16.
Table 16: experimental comparison data of antibacterial performance
# Sterilizing rate for staphylococcus aureus Sterilizing rate of Candida albicans
Example 2 93.20% 94.53%
Comparative example 4 88.90% 85.61%
The test result shows that the 1, 2-pentanediol and the 1, 2-hexanediol are combined to be used as the bacteriostatic agent, and the bacteriostatic effect is better when the 1, 2-pentanediol is used as the bacteriostatic agent.
Therefore, according to the experimental data, the test results of the effects of the ultra-small molecule sodium hyaluronate essence on the moisture retention and anti-wrinkle effects show that the product has the effects of moisture retention and texture improvement, not only can moisten skin, but also can repair cuticles to a certain extent to achieve the effects of deep moisture retention and muscle base repair, and can make the skin smoother and more delicate after long-term use to achieve a certain anti-wrinkle effect.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The essence containing the ultra-small molecule sodium hyaluronate is characterized in that: the essence comprises: the weight percentage of the ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa-3kDa is 0.01-3 percent, the weight percentage of the hydrolyzed sodium hyaluronate with the molecular weight of 10kDa-50kDa is 0.01-2 percent, the weight percentage of the macromolecular sodium hyaluronate with the molecular weight of more than or equal to 1000kDa is 0.01-1 percent, the weight percentage of the humectant is 0.2-16 percent, the weight percentage of the bacteriostatic agent is 0.2-7 percent, and the balance is water.
2. The essence containing ultra-small molecule sodium hyaluronate according to claim 1, characterized in that: the weight percentage of the ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa to 3kDa is 0.1 percent to 1.0 percent; the weight percentage of the hydrolyzed sodium hyaluronate with the molecular weight of 10kDa to 50kDa is 0.1 percent to 1.0 percent; the weight percentage of the macromolecular sodium hyaluronate with the molecular weight of more than or equal to 1000kDa is 0.1-0.5%; the humectant accounts for 3 to 13 percent by weight; the weight percentage of the bacteriostatic agent is 0.5-5%; the balance being water.
3. The essence containing ultra-small molecule sodium hyaluronate according to claim 1 or 2, characterized in that: the humectant is methyl glucitol polyether and 1, 3-butanediol, and the bacteriostatic agent is 1, 2-pentanediol and 1, 2-hexanediol.
4. The essence containing the ultra-small molecule sodium hyaluronate according to claim 3, wherein: the weight percentage of the methyl glucitol polyether is 0.1% -6%, and the weight percentage of the 1, 3-butanediol is 0.1% -10%; the weight percentage of the 1, 2-pentanediol is 0.1-5%, and the weight percentage of the 1, 2-hexanediol is 0.1-2%.
5. The essence containing the ultra-small molecule sodium hyaluronate according to claim 4, wherein: the weight percentage of the methyl glucitol polyether is 1% -5%, and the weight percentage of the 1, 3-butanediol is 2% -8%; the weight percentage of the 1, 2-pentanediol is 0.4% -4%, and the weight percentage of the 1, 2-hexanediol is 0.5% -1%.
6. The essence containing ultra-small molecule sodium hyaluronate according to any one of claims 3 to 5, wherein: the essence comprises 1 weight percent of ultra-small molecular sodium hyaluronate with the molecular weight of 1kDa, 0.5 weight percent of hydrolyzed sodium hyaluronate with the molecular weight of 50kDa, 0.5 weight percent of macromolecular sodium hyaluronate with the molecular weight of 1000kDa, 3 weight percent of methyl glucitol polyether, 6 weight percent of 1, 3-butanediol, 2 weight percent of 1, 2-pentanediol, 0.5 weight percent of 1, 2-hexanediol and the balance of purified water.
7. The preparation method of the essence containing the ultra-small molecular sodium hyaluronate, which is characterized by comprising the following steps of:
1) heating purified water to 50-80 deg.C, and maintaining the temperature;
2) uniformly mixing a humectant, a bacteriostatic agent, macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate to obtain a mixed solution;
3) mixing the mixed liquid obtained in the step 2) with the purified water obtained in the step 1), and stirring for dissolving to obtain the essence.
8. The preparation method of the essence containing the ultra-small molecule sodium hyaluronate according to claim 6, characterized by comprising the following steps:
1) heating purified water to 50-80 deg.C, and maintaining the temperature;
2) uniformly mixing methyl glucitol polyether, 1, 3-butanediol, 1, 2-pentanediol and 1, 2-hexanediol with macromolecular sodium hyaluronate, hydrolyzed sodium hyaluronate and ultra-small molecular sodium hyaluronate to obtain a mixed solution;
3) mixing the mixed liquid obtained in the step 2) with the purified water obtained in the step 1), and stirring for dissolving to obtain the essence.
9. The use of the essence containing ultra-small molecule sodium hyaluronate of any one of claims 1 to 6 in the technical field of cosmetics.
10. Cosmetic product comprising a serum containing ultra-small molecule sodium hyaluronate according to any one of claims 1 to 6.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113876623A (en) * 2021-09-24 2022-01-04 华熙生物科技股份有限公司 Application of hyaluronic acid oligosaccharide composition in resisting skin aging and promoting collagen generation
CN114748375A (en) * 2022-04-27 2022-07-15 康伦智美科技产业(青岛)有限公司 Skin care essence containing high-concentration ultra-small molecule sodium hyaluronate and preparation method thereof
CN114848520A (en) * 2022-06-20 2022-08-05 上海新高姿化妆品有限公司 Whitening and repairing composition and application thereof
CN115363991A (en) * 2021-05-20 2022-11-22 上海菲柏丽生物科技有限公司 Toning lotion and preparation method thereof
CN115850722A (en) * 2023-02-22 2023-03-28 翔鹏(北京)生物科技有限公司 Preparation method and application of efficient transdermal supramolecular sodium hyaluronate

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106109296A (en) * 2016-06-30 2016-11-16 彭燕辉 A kind of moisturizing essence lotion and preparation method thereof
CN108635247A (en) * 2018-06-27 2018-10-12 广州澳希亚实业有限公司 Cosmetic composition containing sodium hyaluronate
CN108836979A (en) * 2018-05-31 2018-11-20 哈尔滨运美达生物科技有限公司 A kind of preparation method of sodium hyaluronate reparation patch and reparation patch and reparation patch Essence
CN109223618A (en) * 2018-10-31 2019-01-18 成都珂萝瑞诗化妆品有限公司 A kind of hyaluronic acid Essence and preparation method thereof
KR20200016634A (en) * 2018-08-07 2020-02-17 상하이 볼링 만 코스메틱 씨오., 엘티디 A facial mask composition and its preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106109296A (en) * 2016-06-30 2016-11-16 彭燕辉 A kind of moisturizing essence lotion and preparation method thereof
CN108836979A (en) * 2018-05-31 2018-11-20 哈尔滨运美达生物科技有限公司 A kind of preparation method of sodium hyaluronate reparation patch and reparation patch and reparation patch Essence
CN108635247A (en) * 2018-06-27 2018-10-12 广州澳希亚实业有限公司 Cosmetic composition containing sodium hyaluronate
KR20200016634A (en) * 2018-08-07 2020-02-17 상하이 볼링 만 코스메틱 씨오., 엘티디 A facial mask composition and its preparation method
CN109223618A (en) * 2018-10-31 2019-01-18 成都珂萝瑞诗化妆品有限公司 A kind of hyaluronic acid Essence and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115363991A (en) * 2021-05-20 2022-11-22 上海菲柏丽生物科技有限公司 Toning lotion and preparation method thereof
CN113876623A (en) * 2021-09-24 2022-01-04 华熙生物科技股份有限公司 Application of hyaluronic acid oligosaccharide composition in resisting skin aging and promoting collagen generation
CN114748375A (en) * 2022-04-27 2022-07-15 康伦智美科技产业(青岛)有限公司 Skin care essence containing high-concentration ultra-small molecule sodium hyaluronate and preparation method thereof
CN114848520A (en) * 2022-06-20 2022-08-05 上海新高姿化妆品有限公司 Whitening and repairing composition and application thereof
CN115850722A (en) * 2023-02-22 2023-03-28 翔鹏(北京)生物科技有限公司 Preparation method and application of efficient transdermal supramolecular sodium hyaluronate

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