A composition based on anti-fatigue giant salamander peptide and its preparation method and application

By combining modified β-cyclodextrin and modified chitosan complex with giant salamander peptide, the problem of giant salamander peptide being sensitive to changes in the external environment in skin care products is solved, and the long-term stay of giant salamander peptide on the surface of the skin and the improvement of skin care effect is achieved.

CN120284770BActive Publication Date: 2025-08-26HUNAN TIANJIN PHARMA
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Patent Information

Application Number
CN202510772810.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-08-26
Estimated Expiration
2045-06-11

AI Technical Summary

Technical Problem

Giant salamander peptides are sensitive to changes in the external environment in skin care products and are easy to degrade, resulting in the short stay of active ingredients on the surface of the skin, affecting the skin care effect.

Method used

Modified β-cyclodextrin and modified chitosan complex are used to combine with giant salamander peptides to form a stable inclusion compound, blocking oxygen and ultraviolet rays, providing a stable hydration environment, delaying the release of peptides, and forming a protective-sustaining release system.

Benefits of technology

Giant salamander peptide stays on the surface of the skin for a long time, exerting excellent skin care effects, enhancing skin barrier function and antioxidant effects.

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Abstract

The present application relates to the technical field of skin care products, and specifically discloses a composition based on anti-fatigue giant salamander peptide and its preparation method and application. Its raw materials include: 3-5 parts of moisturizing agent, 3-8 parts of thickener, 4-5 parts of emulsifier, 0.1-0.3 parts of antibacterial preservative, 0.03-0.06 parts of giant salamander peptide, 0.05-0.1 parts of sodium hyaluronate, 0.1-0.2 parts of carbomer, 5-8 parts of caprylic / capric triglyceride, 60-70 parts of deionized water, 1.2-1.5 parts of modified β-cyclodextrin, and 0.3-0.1 parts of modified chitosan compound. When the composition based on anti-fatigue giant salamander peptide is applied, the giant salamander peptide it contains is not easily destroyed by changes in the external environment and can stay on the surface of the skin for a long time.
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Description

Technical Field

[0001] The present application relates to the technical field of skin care products, and more specifically, to a composition based on anti-fatigue giant salamander peptide, and a preparation method and application thereof. Background Art

[0002] Giant salamander peptide is a bioactive peptide produced by enzymatically hydrolyzing the mucus, muscle, skin, and skin secretions of giant salamanders. Its main components include protein, amino acids, unsaturated fatty acids, minerals, and trace elements. It is extracted from various tissues through enzymatic hydrolysis. The molecular weight of giant salamander peptides is mostly within 1000 Daltons, making them highly bioactive and easily absorbed and utilized by cells.

[0003] The role of giant salamander peptide in medical skin care is mainly reflected in its anti-fatigue, anti-oxidation, promotion of wound healing and enhancement of skin barrier function. Among them, the anti-fatigue effect is mainly reflected in its ability to significantly reduce lactic acid accumulation after exercise, enhance liver glycogen reserves and reduce oxidative stress response after exercise, thereby effectively alleviating fatigue after exercise; the antioxidant effect is mainly reflected in its ability to scavenge free radicals in the body and reduce the damage of oxidative stress to cells; the wound healing effect is mainly reflected in its ability to stimulate cell proliferation and migration, and accelerate the healing of damaged tissues such as skin and mucous membranes; the enhancement of skin barrier function is mainly reflected in its ability to repair the skin barrier and protect the skin from external damage; in addition, giant salamander peptide also has the functions of regulating immunity and promoting collagen synthesis. These characteristics make it have potential application value in the field of skin care.

[0004] Regarding the above-mentioned related technologies, the inventors believe that in skin care products, giant salamander peptides have a small molecular weight and a compact structure. Although they are conducive to absorption, they are sensitive to changes in the external environment and are prone to degradation under high temperature or strong light conditions, resulting in partial inactivation of active ingredients. They also cause the active ingredients to stay on the skin surface for a shorter time, thereby affecting the skin care effect.

[0005] Therefore, it is urgent to propose a solution to solve the above technical problems. Summary of the Invention

[0006] In order to improve the sensitivity of giant salamander peptides in skin care products to changes in the external environment, increase the retention of giant salamander peptides in skin care products on the skin surface, and thus improve the skin care effect, the present application provides a composition based on anti-fatigue giant salamander peptides and its preparation method and application.

[0007] In a first aspect, the present application provides an anti-fatigue composition based on giant salamander peptide, which adopts the following technical solution:

[0008] A composition based on anti-fatigue giant salamander peptide comprises the following components in parts by weight:

[0009] 3-5 parts of moisturizer;

[0010] 3-8 parts thickener;

[0011] 4-5 parts of emulsifier;

[0012] 0.1-0.3 parts of antibacterial preservatives;

[0013] Giant salamander peptide 0.03-0.06 parts;

[0014] Sodium hyaluronate 0.05-0.1 part;

[0015] Carbomer 0.1-0.2 parts;

[0016] Caprylic / capric triglyceride 5-8 parts;

[0017] 60-70 parts of deionized water;

[0018] 1.2-1.5 parts of modified β-cyclodextrin;

[0019] 0.3-1 part of modified chitosan compound;

[0020] The modified β-cyclodextrin is prepared by the following method:

[0021] Take sodium hydroxide solution, add β-cyclodextrin raw material and stir to dissolve, then add dimethyl sulfate, stir and react at 55-65°C for 7-9 hours, cool and neutralize, remove ions and concentrate by vacuum distillation, then add dropwise to acetone, and finally filter and dry to obtain modified β-cyclodextrin;

[0022] The modified chitosan compound is prepared by the following method:

[0023] Take acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomaceous earth raw material to soak, react at 55-65°C for 1.5-2.5 hours, and dry to obtain an intermediate product; then disperse the intermediate product in deionized water, add carboxymethyl cellulose and stir to dissolve, then add a cross-linking agent to react, wash and dry the obtained reaction product to obtain a modified chitosan compound.

[0024] By adopting the above technical solution, after the β-cyclodextrin raw material is modified, its own solubility and surface activity are significantly improved, and it can effectively wrap peptide molecules to form a stable inclusion complex, blocking the oxidation or photodegradation damage of peptides by external environments such as oxygen and ultraviolet rays. The modified β-cyclodextrin can also chelate heavy metal ions (such as iron and copper) and scavenge free radicals, inhibiting the damage of the oxidative chain reaction to the peptide structure, thereby effectively protecting the giant salamander peptide. In the preparation of the modified chitosan compound, among the raw materials used, chitosan and bentonite are natural environmentally friendly substances with small particle size and easy dispersion; carboxymethyl cellulose is a gel polymer material with a large number of functional groups in its network structure; the modified chitosan compound obtained by the above preparation method can rely on the intermolecular hydrogen bonds or ionic bonds of chitosan, combined with the porous structure and large specific surface area of ​​bentonite and the gel film-forming properties of carboxymethyl cellulose, to form a special three-dimensional network structure when used, which can wrap the giant salamander peptide while providing a stable hydration environment and a strong carrier effect, thereby maintaining the stability of the giant salamander peptide molecular conformation and ensuring its excellent effect. At the same time, in the product system of the composition based on the anti-fatigue giant salamander peptide, the combination of modified β-cyclodextrin and modified chitosan can bring about a compound synergistic effect, which can not only stably adsorb, immobilize and include giant salamander peptide, but also delay the rapid release of giant salamander peptide, forming a "protection-sustained release" system, and the synergy between the two has excellent resistance to changes in the external environment, and promotes the stable performance of giant salamander peptide activity; in this way, when the composition based on the anti-fatigue giant salamander peptide is used, the giant salamander peptide it contains is not easily destroyed by changes in the external environment, and can stay on the surface of the skin for a long time, thereby exerting an excellent skin care effect.

[0025] Preferably, the weight ratio of the modified β-cyclodextrin and modified chitosan compound is 2:1.

[0026] By adopting the above technical solution, when the modified β-cyclodextrin and modified chitosan compound in the above weight ratio are used in combination, the composite system formed by the two synergistically has a relatively excellent effect on the corresponding effect of giant salamander peptide, thereby obtaining a composition based on anti-fatigue giant salamander peptide with better application quality.

[0027] Preferably, in the preparation of the modified β-cyclodextrin, the ratio of the β-cyclodextrin raw material to dimethyl sulfate is (1.5-2.5) g:1 mL.

[0028] By adopting the above technical solution, when the ratio of β-cyclodextrin raw material and dimethyl sulfate is lower than the above range, the cavity structure of the β-cyclodextrin raw material will be destroyed, thereby reducing the ability of the modified β-cyclodextrin to encapsulate the giant salamander peptide; when the ratio of β-cyclodextrin raw material and dimethyl sulfate is lower than the above range, the β-cyclodextrin raw material cannot be effectively modified; the above situations will greatly reduce the corresponding application effect of the modified β-cyclodextrin. However, the β-cyclodextrin raw material and dimethyl sulfate in the above ratio range can ensure that the prepared modified β-cyclodextrin exerts an excellent coordination effect with the modified chitosan compound after application, thereby ultimately obtaining a composition based on anti-fatigue giant salamander peptide with stable and excellent application quality.

[0029] Preferably, the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2g:1mL.

[0030] By adopting the above technical solution, after applying the above ratio of β-cyclodextrin raw material and dimethyl sulfate, the corresponding effect brought by the application of modified β-cyclodextrin is better, and the overall application quality of the anti-fatigue giant salamander peptide-based composition is also better.

[0031] Preferably, in the preparation of the modified chitosan compound, the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1: (2-3): (4-5).

[0032] By adopting the above technical solution, when the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is lower than the above range, it is easy to form a uniform and stable combination during the combination of the three due to the high viscosity of the system; when the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is higher than the above range, excessive cross-linking is easy to occur during the preparation, so that the obtained modified chitosan compound is easy to agglomerate and adhere after application, and cannot form a relatively uniform and dense special three-dimensional network structure; the above situations will greatly reduce the corresponding application effect of the modified chitosan compound. However, the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose in the above ratio range can ensure that the prepared modified chitosan compound has an excellent coordination effect with the modified β-cyclodextrin after application, and finally obtain a composition based on anti-fatigue giant salamander peptide with stable and excellent application quality.

[0033] Preferably, the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:2.5:4.5.

[0034] By adopting the above technical solution, after applying the above proportions of chitosan raw material, diatomaceous earth raw material and carboxymethyl cellulose, the corresponding effect brought by the application of the modified chitosan compound is better, and the overall application quality of the anti-fatigue giant salamander peptide-based composition is also better.

[0035] Preferably, the moisturizing agent is one or a combination of glycerin, vitamin E, allantoin, polyethylene glycol, ceramide and urea.

[0036] By adopting the above technical solution, the moisturizer absorbs moisture from the environment or deep layers of the skin through the hydrophilic group to form a hydration layer, and can reduce the water holding capacity caused by barrier damage, thereby maintaining a healthy hydration environment for the skin, and to a certain extent, can also ensure the excellent effects of the giant salamander peptide. The above types of moisturizers are all suitable for the preparation of the anti-fatigue giant salamander peptide-based composition, and can exert an excellent and stable moisturizing effect, thereby obtaining an anti-fatigue giant salamander peptide-based composition with excellent quality and stability.

[0037] Preferably, the thickener is one or a combination of xanthan gum, carrageenan, stearic acid, polyvinyl alcohol and cellulose derivatives.

[0038] By adopting the above technical solution, the thickener can evenly disperse the various component raw materials through physical support, prevent stratification or precipitation, and thus ensure the excellent coordination between the raw materials. At the same time, it can also enhance the adhesion of the product on the skin surface, ensuring the stable performance of the excellent efficacy of the anti-fatigue giant salamander peptide-based composition during the application process; and the above-mentioned types of thickeners are all suitable for the application requirements of the anti-fatigue giant salamander peptide-based composition, and can exert excellent and stable corresponding effects.

[0039] Preferably, the emulsifier is one or a combination of steareth-6, glyceryl stearate, ceteareth-20 and sodium lauryl sulfate.

[0040] By adopting the above technical solution, the emulsifier can improve the application uniformity of the anti-fatigue giant salamander peptide-based composition, increase the contact area between the active ingredient and the skin, and at the same time reduce the impact on the skin microecology while ensuring stability; and the above types of emulsifiers are all suitable for the application requirements of the anti-fatigue giant salamander peptide-based composition and can exert excellent and stable corresponding effects.

[0041] In a second aspect, the present application provides a method for preparing a composition based on anti-fatigue giant salamander peptide, using the following technical solution:

[0042] A method for preparing an anti-fatigue composition based on giant salamander peptide comprises the following steps:

[0043] (1) Prepare raw materials including moisturizer, thickener, emulsifier, antimicrobial preservative, giant salamander peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, modified β-cyclodextrin and modified chitosan according to the ratio;

[0044] (2) mixing and heating the moisturizer, sodium hyaluronate, carbomer and deionized water in step (1) to obtain a phase A mixture; heating and stirring the thickener, emulsifier and caprylic / capric triglyceride in step (1) to obtain a phase B mixture;

[0045] (3) After mixing the phase A mixture and the phase B mixture, add the giant salamander peptide, modified β-cyclodextrin and modified chitosan compound and stir and mix them, and finally add the antibacterial preservative and mix to obtain an anti-fatigue giant salamander peptide-based composition.

[0046] By adopting the above technical solution, the above preparation method is simple to operate, and the raw materials are added and mixed in steps, which is not only conducive to quality control during the process, but also enables the raw materials to be fully combined with each other, thereby obtaining a high-quality composition based on anti-fatigue giant salamander peptides. The composition is also suitable for large-scale industrial production as a whole and has strong overall applicability.

[0047] In a third aspect, the present application provides an application of a composition based on anti-fatigue giant salamander peptide in skin care products.

[0048] In summary, this application has the following beneficial effects:

[0049] The present application uses a modified β-cyclodextrin and a modified chitosan compound to form a "protection-sustained release" system. The modified β-cyclodextrin and the modified chitosan compound are used in combination, which can not only stably adsorb, immobilize and include the giant salamander peptide, but also delay the rapid release of the giant salamander peptide, forming a "protection-sustained release" system. The synergy between the two has excellent resistance to changes in the external environment and promotes the stable performance of the giant salamander peptide activity. In this way, when the composition based on the anti-fatigue giant salamander peptide is used, the giant salamander peptide contained therein is not easily destroyed by changes in the external environment, and can stay on the skin surface for a long time, thereby exerting an excellent skin care effect. DETAILED DESCRIPTION

[0050] The present application is further described in detail below with reference to preparation examples, embodiments and comparative examples.

[0051] Unless otherwise specified, the raw materials used in the preparation examples, embodiments and comparative examples of the present application are all commercially available.

[0052] β-cyclodextrin raw material was purchased from Guangdong Mingtong Biotechnology Co., Ltd., particle size 120 mesh, CAS number 68168-23-0;

[0053] Chitosan raw materials were purchased from Shaanxi Tangyao Biotechnology Co., Ltd. Pharmaceutical grade chitosan Pharmacopoeia version 500g acid soluble CDE registration 9012-76-4;

[0054] Diatomite raw materials were purchased from Shijiazhuang Xunhua Mineral Products Co., Ltd. with a specification of 325 mesh;

[0055] Carboxymethyl cellulose was purchased from Guangzhou Yiming Chemical Co., Ltd. with a viscosity specification of 800.

[0056] Preparation examples of raw materials and / or intermediates

[0057] Preparation Example 1

[0058] A modified β-cyclodextrin is prepared by the following method:

[0059] Take sodium hydroxide solution, add β-cyclodextrin raw material and stir to dissolve, then add dimethyl sulfate, stir and react at 55-65°C for 7-9 hours (this preparation example uses 60°C for 8 hours), cool to 25°C and neutralize with hydrochloric acid, remove ions with ion exchange resin, and concentrate by vacuum distillation, then add dropwise into acetone, and finally filter and dry to obtain modified β-cyclodextrin.

[0060] Note: In the above operation, the sodium hydroxide solution is obtained by mixing 2g of sodium hydroxide and 30mL of water; the ratio of β-cyclodextrin raw material and dimethyl sulfate used is 2g:1mL.

[0061] Preparation Example 2

[0062] A modified β-cyclodextrin is different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 1.5 g:1 mL.

[0063] Preparation Example 3

[0064] A modified β-cyclodextrin is different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2.5 g:1 mL.

[0065] Preparation Example 4

[0066] A modified β-cyclodextrin is different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 1.4 g:1 mL.

[0067] Preparation Example 5

[0068] A modified β-cyclodextrin is different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2.6 g:1 mL.

[0069] Preparation Example 6

[0070] A modified chitosan compound is prepared by the following method:

[0071] Take acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomaceous earth raw material for infiltration, react at 55-65°C for 1.5-2.5 hours (this preparation example uses 60°C for 2 hours), and dry to obtain an intermediate product; then disperse the intermediate product in deionized water at a ratio of 25g:1L, add carboxymethyl cellulose and stir to dissolve, then add a cross-linking agent to react, and wash and dry the obtained reaction product to obtain a modified chitosan compound.

[0072] Note: In the above operation, the mass fraction of acetic acid solution is 3%; the cross-linking agent is ferric chloride, and the amount of cross-linking agent used is 1.2% of the total mass of the intermediate product and carboxymethyl cellulose; the weight ratio of chitosan raw material, diatomaceous earth raw material and carboxymethyl cellulose used is 1:2.5:4.5.

[0073] Preparation Example 7

[0074] A modified chitosan compound is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:2:4.

[0075] Preparation Example 8

[0076] A modified chitosan compound is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:3:5.

[0077] Preparation Example 9

[0078] A modified chitosan compound is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:1.8:3.8.

[0079] Preparation Example 10

[0080] A modified chitosan compound is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:3.2:5.2.

[0081] Example

[0082] Example 1

[0083] A composition based on anti-fatigue giant salamander peptide, the raw materials used in its preparation and their corresponding weight parts are shown in Table 1, and it is prepared by the following steps:

[0084] (1) Prepare raw materials including moisturizer, thickener, emulsifier, antimicrobial preservative, giant salamander peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, modified β-cyclodextrin and modified chitosan according to the ratio;

[0085] (2) The moisturizer, sodium hyaluronate, carbomer and deionized water in step (1) are mixed and heated to 80° C. to obtain a phase A mixture; the thickener, emulsifier and caprylic / capric triglyceride in step (1) are heated to 75° C. and stirred to obtain a phase B mixture;

[0086] (3) The phase A mixture and the phase B mixture were mixed, homogenized at 1500 rpm for 20 min, and then cooled to 45°C. Then, a compound of giant salamander peptide, modified β-cyclodextrin and modified chitosan was added and stirred, and the mixture was cooled to 25°C. Finally, an antibacterial preservative was added and mixed to obtain a composition based on anti-fatigue giant salamander peptide.

[0087] Note: In the above operation, the moisturizer is glycerin, the thickener is xanthan gum, the emulsifier is steareth-6, and the antibacterial preservative is p-hydroxyacetophenone; the molecular weight of sodium hyaluronate is 3500 Daltons; the carbomer selected is carbomer 940; the giant salamander peptide is giant salamander oligopeptide 350 Daltons; the modified β-cyclodextrin is obtained from Preparation Example 1, and the modified chitosan compound is obtained from Preparation Example 6.

[0088] Example 2-3

[0089] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the raw materials used in its preparation and their corresponding weight parts are shown in Table 1.

[0090] Table 1 Raw materials used in the preparation of Examples 1-3 and their corresponding weight parts (parts / kg)

[0091] raw material Example 1 Example 2 Example 3 moisturizer 4 3 5 thickener 5.5 3 8 emulsifiers 4.5 4 5 antimicrobial preservatives 0.2 0.1 0.3 Giant Salamander Peptide 0.045 0.03 0.06 Sodium hyaluronate 0.075 0.05 0.1 Carbomer 0.15 0.1 0.2 Caprylic / capric triglyceride 6.5 5 8 Deionized water 65 60 70 Modified β-cyclodextrin 1.35 1.2 1.5 Modified chitosan compound 0.65 0.3 1

[0092] Example 4

[0093] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the total amount of the modified β-cyclodextrin and modified chitosan compound remains unchanged, and the weight ratio of the two is adjusted to 2:1.

[0094] Example 5

[0095] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 2.

[0096] Example 6

[0097] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 3.

[0098] Example 7

[0099] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 4.

[0100] Example 8

[0101] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 5.

[0102] Example 9

[0103] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified chitosan compound is obtained from Preparation Example 7.

[0104] Example 10

[0105] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified chitosan compound is obtained from Preparation Example 8.

[0106] Example 11

[0107] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified chitosan compound is obtained from Preparation Example 9.

[0108] Example 12

[0109] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified chitosan compound is obtained from Preparation Example 10.

[0110] Comparative Example

[0111] Comparative Example 1

[0112] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that modified β-cyclodextrin is not used in the raw materials.

[0113] Comparative Example 2

[0114] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that no modified chitosan compound is used in the raw materials.

[0115] Comparative Example 3

[0116] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the raw materials do not use a composite of modified β-cyclodextrin and modified chitosan.

[0117] Comparative Example 4

[0118] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified β-cyclodextrin is replaced by β-cyclodextrin raw material.

[0119] Comparative Example 5

[0120] A composition based on anti-fatigue giant salamander peptide is different from Example 1 in that the modified chitosan compound is replaced by chitosan raw material in equal mass.

[0121] Comparative Example 6

[0122] A composition based on anti-fatigue giant salamander peptide is different from comparative example 4 in that no modified chitosan compound is used in the raw materials.

[0123] Comparative Example 7

[0124] A composition based on anti-fatigue giant salamander peptide is different from comparative example 5 in that modified β-cyclodextrin is not used in the raw materials.

[0125] Performance testing

[0126] Test samples: The anti-fatigue giant salamander peptide-based compositions obtained in Examples 1-12 were selected as test samples 1-12, and the anti-fatigue giant salamander peptide-based compositions obtained in Comparative Examples 1-7 were selected as control samples 1-7.

[0127] Test method: High performance liquid chromatography was used to test the content of giant salamander peptide in the anti-fatigue giant salamander peptide-based composition.

[0128] High Performance Liquid Chromatography (HPLC): HPLC is an efficient and rapid separation and determination technology suitable for the determination of a variety of peptide substances. By selecting appropriate chromatographic columns and mobile phases, peptide substances can be separated from other impurities, and the peptide content can be determined by the response signal of the detector.

[0129] A Sino Chrom C18 reversed-phase column and a UV variable wavelength detector are usually used, with a detection wavelength of 280 nm, a mobile phase consisting of a mixture of acetonitrile, methanol, and 0.1% trifluoroacetic acid (ratio 5:5:90), a flow rate of 1.0 mL / min, and an injection volume of 20 μL.

[0130] Test on the persistence of giant salamander peptide on the skin surface:

[0131] A corresponding amount of the anti-fatigue giant salamander peptide-based composition was applied to perform the above test, and the measured giant salamander peptide content was recorded as A2;

[0132] Ten women aged 20-40 were randomly selected as test subjects and the standard dosage was 2 mg / cm 2 The anti-fatigue giant salamander peptide-based composition was evenly applied on the back of the hand. After applying for 60 seconds, the residual anti-fatigue giant salamander peptide-based composition on the back of the hand was collected. Then, the residual anti-fatigue giant salamander peptide-based composition was subjected to the above test in the same manner. The average value of the measured giant salamander peptide content was recorded as B2;

[0133] Finally, the residual rate of giant salamander peptide in the anti-fatigue giant salamander peptide-based composition was calculated as follows: residual rate of giant salamander peptide = B2 / A2; the greater the residual rate of giant salamander peptide, the easier it is for the giant salamander peptide component to stay on the surface of the skin for a longer period of time, and the skin care effect of the anti-fatigue giant salamander peptide-based composition is also better.

[0134] After the above tests were performed on the test samples 1-12 and the control samples 1-7, the test results were recorded in Table 2.

[0135] Table 2 Test results of test samples 1-12 and control samples 1-7

[0136] sample Test on the persistence of giant salamander peptide on the skin surface - residual rate of giant salamander peptide content (%) Test sample 1 61.52 Test sample 2 60.23 Test sample 3 60.78 Test sample 4 61.89 Test sample 5 60.46 Test sample 6 60.62 Test sample 7 58.46 Test sample 8 58.61 Test sample 9 60.57 Test sample 10 60.85 Test sample 11 58.08 Test sample 12 57.93 Control sample 1 45.77 Control sample 2 46.58 Control sample 3 37.34 Control sample 4 53.06 Control sample 5 52.82 Control sample 6 44.41 Control sample 7 43.58

[0137] In combination with Example 1 and Comparative Examples 1-3 and Table 2, it can be seen that the present application uses a modified β-cyclodextrin and a modified chitosan compound in the composition based on the anti-fatigue giant salamander peptide, which can make the giant salamander peptide less likely to be destroyed by changes in the external environment during application, and can stay on the skin surface for a longer time, thereby exerting an excellent skin care effect; if only the modified β-cyclodextrin or the modified chitosan compound is used, although it can bring about an improvement in the corresponding effect, the improvement is limited, and the sum of the improvement effects brought about by the application of each of the two alone is far less than the excellent improvement effect brought about by the combination of the two. It can be seen that the combination of the modified β-cyclodextrin and the modified chitosan compound can exert a 1+1>2 compound improvement effect in the composition based on the anti-fatigue giant salamander peptide, and the overall improvement effect is significant. Combined with Comparative Examples 4-7 and Table 2, it can be seen that if the mass of modified β-cyclodextrin is replaced by β-cyclodextrin raw material, and the mass of modified chitosan compound is replaced by chitosan raw material, the above test results of the composition based on anti-fatigue giant salamander peptide will be greatly reduced, and the β-cyclodextrin raw material and the modified chitosan compound, as well as the chitosan raw material and modified β-cyclodextrin can only bring about a simple superposition of effects, but cannot bring about the excellent compound enhancement effect; it can be seen that the significant effect brought about by the use of modified β-cyclodextrin and modified chitosan compound in this application is irreplaceable.

[0138] Combining Examples 1-3 and Example 4 with Table 2, it can be seen that when the weight ratio of the modified β-cyclodextrin and modified chitosan compound is 2:1, the synergistically formed compound system has a relatively excellent effect on the corresponding action of giant salamander peptide, and the experimental results obtained by the above test are relatively good.

[0139] From Example 1 and Examples 5-8 and Table 2, it can be seen that in the preparation of modified β-cyclodextrin, the ratio of the β-cyclodextrin raw material and dimethyl sulfate used is (1.5-2.5) g:1 mL, and the prepared modified β-cyclodextrin can exert an excellent coordination effect with the modified chitosan compound after application; and regardless of whether the ratio is lower or higher than the above-mentioned ratio range, after application of the obtained modified β-cyclodextrin, the corresponding quality of the composition based on the anti-fatigue giant salamander peptide will be significantly lost after the above-mentioned test.

[0140] From Example 1 and Examples 9-12 and Table 2, it can be seen that in the preparation of the modified chitosan compound, the weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose used is 1: (2-3): (4-5), and the prepared modified chitosan compound can exert an excellent coordination effect with the modified β-cyclodextrin after application; and regardless of whether the ratio is lower or higher than the above-mentioned ratio range, after application of the obtained modified chitosan compound, the corresponding quality of the composition based on the anti-fatigue giant salamander peptide will be significantly lost after the above-mentioned test.

[0141] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A composition based on anti-fatigue giant salamander peptide, characterized in that: Contains the following components in parts by weight: 3-5 parts of moisturizer; 3-8 parts thickener; 4-5 parts of emulsifier; 0.1-0.3 parts of antibacterial preservatives; Giant salamander peptide 0.03-0.06 parts; Sodium hyaluronate 0.05-0.1 part; Carbomer 0.1-0.2 parts; Caprylic / capric triglyceride 5-8 parts; 60-70 parts of deionized water; 1.2-1.5 parts of modified β-cyclodextrin; 0.3-1 part of modified chitosan compound; The modified β-cyclodextrin is prepared by the following method: Take sodium hydroxide solution, add β-cyclodextrin raw material and stir to dissolve, then add dimethyl sulfate, stir and react at 55-65°C for 7-9 hours, cool and neutralize, remove ions and concentrate by vacuum distillation, then add dropwise to acetone, and finally filter and dry to obtain modified β-cyclodextrin; The modified chitosan compound is prepared by the following method: Take acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomaceous earth raw material to soak, react at 55-65°C for 1.5-2.5 hours, and dry to obtain an intermediate product; then disperse the intermediate product in deionized water, add carboxymethyl cellulose and stir to dissolve, then add a cross-linking agent to react, wash and dry the reaction product to obtain a modified chitosan compound; In the preparation of the modified β-cyclodextrin, the ratio of the β-cyclodextrin raw material and dimethyl sulfate is (1.5-2.5) g:1 mL; the weight ratio of the chitosan raw material, diatomaceous earth raw material and carboxymethyl cellulose is 1:(2-3):(4-5).

2. The anti-fatigue composition based on giant salamander peptide according to claim 1, characterized in that: The weight ratio of the modified beta-cyclodextrin and modified chitosan compound is 2:

1.

3. The anti-fatigue composition based on giant salamander peptide according to claim 1, characterized in that: The ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2 g:1 mL.

4. The anti-fatigue composition based on giant salamander peptide according to claim 1, characterized in that: The weight ratio of the chitosan raw material, the diatomaceous earth raw material and the carboxymethyl cellulose is 1:2.5:4.

5.

5. The anti-fatigue composition based on giant salamander peptide according to claim 1, characterized in that: The moisturizing agent is one or a combination of glycerin, vitamin E, allantoin, polyethylene glycol, ceramide and urea; The thickener is one or a combination of xanthan gum, carrageenan, stearic acid, polyvinyl alcohol and cellulose derivatives; The emulsifier is one or a combination of steareth-6, glyceryl stearate, ceteareth-20 and sodium lauryl sulfate.

6. The method for preparing the anti-fatigue composition based on giant salamander peptide according to claim 1, characterized in that: The following steps are involved: (1) Prepare raw materials including moisturizer, thickener, emulsifier, antimicrobial preservative, giant salamander peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, modified β-cyclodextrin and modified chitosan according to the ratio; (2) mixing and heating the moisturizer, sodium hyaluronate, carbomer and deionized water in step (1) to obtain a phase A mixture; heating and stirring the thickener, emulsifier and caprylic / capric triglyceride in step (1) to obtain a phase B mixture; (3) After mixing the phase A mixture and the phase B mixture, add the giant salamander peptide, modified β-cyclodextrin and modified chitosan compound and stir and mix them, and finally add the antibacterial preservative and mix to obtain an anti-fatigue giant salamander peptide-based composition.

7. Use of the anti-fatigue giant salamander peptide-based composition according to any one of claims 1 to 5 in the preparation of skin care products.

Citation Information

Patent Citations

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