Composition based on anti-fatigue giant salamander peptide as well as preparation method and application of composition

By combining modified β-cyclodextrin and modified chitosan complex with giant salamander peptides, a stable inclusion compound is formed, which solves the problem of easy degradation of giant salamander peptides in skin care products, and improves the residence time and skin care effect of giant salamander peptides on the skin surface.

CN120284770AActive Publication Date: 2025-07-11HUNAN TIANJIN PHARMA

Patent Information

Application Number
CN202510772810.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-07-11
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 inactivation of active ingredients and short residence time, 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 and a three-dimensional network structure, delaying release, and forming a protection-sustaining release system.

Benefits of technology

Improve the residence time of giant salamander peptides on the surface of the skin, enhance their resistance to changes in the external environment, maintain their activity, and improve skin care effects.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention relates to the technical field of skin care products, and particularly discloses a composition based on anti-fatigue giant salamander peptide and a preparation method and application thereof. The andrias davidianus peptide mask is prepared from the following raw materials: 3 to 5 parts of a humectant, 3 to 8 parts of a thickening agent, 4 to 5 parts of an emulsifier, 0.1 to 0.3 part of an antibacterial preservative, 0.03 to 0.06 part of andrias davidianus peptide, 0.05 to 0.1 part of sodium hyaluronate, 0.1 to 0.2 part of carbomer, 5 to 8 parts of caprylic / capric triglyceride, 60 to 70 parts of deionized water, 1.2 to 1.5 parts of modified beta-cyclodextrin and 0.3 to 0.1 part of a modified chitosan compound. When the anti-fatigue giant salamander peptide-based composition is applied, the giant salamander peptide contained in the anti-fatigue giant salamander peptide-based composition is not easily damaged due to external environment change, and can stay on the skin surface layer for a long time.
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Description

Technical Field

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

[0002] Giant salamander peptide is a bioactive peptide prepared by enzymatically hydrolyzing basic raw materials such as the mucus, muscle, skin and skin secretions of giant salamanders. The main components of giant salamander peptide include proteins, amino acids, unsaturated fatty acids, minerals and trace elements, etc. Its preparation method is extracted by enzymatically hydrolyzing various tissues of giant salamanders. The molecular weight of giant salamander peptide is mostly distributed within 1000 daltons, with extremely high biological activity and being easily absorbed and utilized by cells.

[0003] The functions of giant salamander peptide in medical skin care are mainly reflected in its anti-fatigue, antioxidant, promoting wound healing and enhancing skin barrier function, etc.; among them, the anti-fatigue effect is mainly reflected in its ability to significantly reduce the accumulation of lactic acid after exercise, enhance the liver glycogen reserve and reduce the oxidative stress response after exercise, thereby effectively relieving the fatigue feeling 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 promoting 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 enhancing 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 functions such as regulating immunity and promoting collagen synthesis, and these characteristics make it have potential application value in the skin care field.

[0004] Regarding the above related technologies, the inventor believes that in skin care products, the molecular weight of giant salamander peptide is small and the structure is compact. Although it is beneficial for absorption, it is sensitive to changes in the external environment and is prone to degradation under high temperature or strong light conditions, resulting in partial inactivation of the active ingredients, and it will also make the active ingredients stay on the skin surface for a relatively short time, thereby affecting the skin care effect.

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

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

[0007] In the first aspect, the present application provides a composition based on anti-fatigue giant salamander peptide, adopting the following technical solution: A composition based on anti-fatigue giant salamander peptide, comprising the following components in parts by weight: Humectant 3 - 5 parts; Thickener: 3 - 8 parts; Emulsifier: 4 - 5 parts; Antibacterial preservative: 0.1 - 0.3 parts; Andrias davidianus peptide: 0.03 - 0.06 parts; Sodium hyaluronate: 0.05 - 0.1 parts; Carbomer: 0.1 - 0.2 parts; Caprylic / capric triglyceride: 5 - 8 parts; Deionized water: 60 - 70 parts; Modified β - cyclodextrin: 1.2 - 1.5 parts; Modified chitosan complex: 0.3 - 1 part; The modified β - cyclodextrin is obtained 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 h, cool and neutralize, remove ions and then concentrate by vacuum distillation, then drop into acetone, and finally filter and dry to obtain modified β - cyclodextrin; The modified chitosan complex is obtained by the following method: Take acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomite raw material to infiltrate, react at 55 - 65 °C for 1.5 - 2.5 h, 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 - linker to react, and after washing and drying the obtained reaction product, obtain the modified chitosan complex.

[0008] 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 encapsulate peptide molecules to form a stable inclusion complex, blocking the oxidation or photo-degradation damage of the peptide by external environments such as oxygen and ultraviolet rays. Moreover, the modified β-cyclodextrin can also chelate heavy metal ions (such as iron and copper) and scavenge free radicals, inhibiting the damage of the peptide structure by the oxidation chain reaction, and thus can effectively protect the giant salamander peptide. In the preparation of the modified chitosan complex, 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. When the modified chitosan complex obtained by the above preparation method is applied, relying 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 property of carboxymethyl cellulose, a special three-dimensional network structure can be formed. While encapsulating the giant salamander peptide, it can provide a stable hydration environment and a firm carrier effect, thereby maintaining the stability of the giant salamander peptide molecular conformation and ensuring the exertion of its excellent effects. At the same time, in the product system of the composition based on the anti-fatigue giant salamander peptide, by using the combination of the modified β-cyclodextrin and the modified chitosan complex, a compound synergistic effect can be brought. It can not only stably adsorb, immobilize and encapsulate the giant salamander peptide, but also delay the rapid release of the giant salamander peptide, forming a "protection-sustained release" system. Moreover, 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. Thus, when the composition based on the anti-fatigue giant salamander peptide is applied, the giant salamander peptide contained therein is not easily damaged due to changes in the external environment and can stay on the skin surface for a long time, thereby exerting excellent skin care effects.

[0009] Preferably, the weight ratio of the modified β-cyclodextrin to the modified chitosan complex is 2:1.

[0010] By adopting the above technical solution, when the modified β-cyclodextrin and the modified chitosan complex in the above weight ratio are used in combination, the compound system formed by their synergy has relatively excellent corresponding effects on the giant salamander peptide, and thus a composition based on the anti-fatigue giant salamander peptide with better application quality can be obtained.

[0011] Preferably, in the preparation of the modified β-cyclodextrin, the ratio of the β-cyclodextrin raw material used to dimethyl sulfate is (1.5 - 2.5) g:1 mL.

[0012] By adopting the above technical solution, when the ratio of β-cyclodextrin raw material to dimethyl sulfate is lower than the above range, the cavity structure of the β-cyclodextrin raw material will be damaged, which will lead to a decrease in the encapsulation ability of the modified β-cyclodextrin for giant salamander peptides; when the ratio of β-cyclodextrin raw material to dimethyl sulfate is higher than the above range, the β-cyclodextrin raw material cannot be effectively modified; both of the above situations will lead to a great reduction in the corresponding application effect of the modified β-cyclodextrin. The β-cyclodextrin raw material and dimethyl sulfate within the above ratio range can ensure that the prepared modified β-cyclodextrin can exert excellent cooperation effects with the modified chitosan complex after application, and ultimately obtain a composition based on anti-fatigue giant salamander peptides with stable and excellent application quality.

[0013] Preferably, the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2 g:1 mL.

[0014] By adopting the above technical solution, after the β-cyclodextrin raw material and dimethyl sulfate in the above ratio are applied, the corresponding effects brought by the application of the modified β-cyclodextrin are better, and the overall application quality of the composition based on anti-fatigue giant salamander peptides is also better.

[0015] Preferably, in the preparation of the modified chitosan complex, the weight ratio of the chitosan raw material, diatomite raw material and carboxymethyl cellulose is 1:(2 - 3):(4 - 5).

[0016] By adopting the above technical solution, when the weight ratio of the chitosan raw material, diatomite raw material and carboxymethyl cellulose is lower than the above range, it is easy to fail to form a uniform and stable combination due to the too high viscosity of the system during the combination of the three; when the weight ratio of the chitosan raw material, diatomite raw material and carboxymethyl cellulose is higher than the above range, excessive cross-linking is likely to occur during the preparation, making the obtained modified chitosan complex prone to agglomeration and adhesion after application, and unable to form a relatively uniform and dense special three-dimensional network structure; both of the above situations will lead to a great reduction in the corresponding application effect of the modified chitosan complex. The chitosan raw material, diatomite raw material and carboxymethyl cellulose within the above ratio range can ensure that the prepared modified chitosan complex can exert excellent cooperation effects with the modified β-cyclodextrin after application, and ultimately obtain a composition based on anti-fatigue giant salamander peptides with stable and excellent application quality.

[0017] Preferably, the weight ratio of the chitosan raw material, diatomite raw material and carboxymethyl cellulose is 1:2.5:4.5.

[0018] By adopting the above technical solution, after the chitosan raw material, diatomite raw material and carboxymethyl cellulose in the above ratio are applied, the corresponding effects brought by the application of the modified chitosan complex are better, and the overall application quality of the composition based on anti-fatigue giant salamander peptides is also better.

[0019] Preferably, the humectant is a composition of one or more of glycerin, vitamin E, allantoin, polyethylene glycol, ceramide, and urea.

[0020] By adopting the above technical solution, the humectant adsorbs moisture in the environment or deep in the skin through hydrophilic groups to form a hydration layer, and can reduce the water-holding capacity caused by barrier damage, maintain a healthy skin hydration environment, and to a certain extent, can also ensure the excellent effect of the giant salamander peptide; and the above types of humectants are all applicable to the preparation of the composition based on the anti-fatigue giant salamander peptide and can exert excellent and stable moisturizing effects, and thus a composition based on the anti-fatigue giant salamander peptide with excellent and stable quality can be obtained.

[0021] Preferably, the thickener is a composition of one or more of xanthan gum, carrageenan, stearic acid, polyvinyl alcohol, and cellulose derivatives.

[0022] By adopting the above technical solution, the thickener can evenly disperse each component raw material through physical support, prevent stratification or precipitation, and thus ensure the excellent exertion of the cooperation effect between the raw materials. At the same time, it can also enhance the adhesion of the product on the skin surface and ensure the stable exertion of the excellent efficacy during the application of the composition based on the anti-fatigue giant salamander peptide; and the above types of thickeners are all applicable to the application of the composition based on the anti-fatigue giant salamander peptide and can exert excellent and stable corresponding effects.

[0023] Preferably, the emulsifier is a composition of one or more of steareth-6, glyceryl stearate, ceteth-20, and sodium lauryl sulfate.

[0024] By adopting the above technical solution, the emulsifier can improve the application uniformity of the composition based on the anti-fatigue giant salamander peptide, 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 applicable to the application of the composition based on the anti-fatigue giant salamander peptide and can exert excellent and stable corresponding effects.

[0025] In a second aspect, the present application provides a preparation method of a composition based on an anti-fatigue giant salamander peptide, adopting the following technical solution: A preparation method of a composition based on an anti-fatigue giant salamander peptide, comprising the following steps: (1) Prepare raw materials including a humectant, a thickener, an emulsifier, an antibacterial preservative, a giant salamander peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, a modified β-cyclodextrin, and a modified chitosan complex according to the ratio. (2) Mix and heat the humectant, sodium hyaluronate, carbomer and deionized water in step (1) to obtain a phase A mixture; heat and stir the thickener, emulsifier and triglyceride caprylate / caprate 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 complex and stir to mix, and finally add the antibacterial preservative and mix to obtain a composition based on anti-fatigue giant salamander peptide.

[0026] By adopting the above technical solution, the above preparation method is simple in operation, and the raw materials are added and mixed in steps, which is not only beneficial to quality control during the process, but also enables the raw materials to be fully combined with each other, and then a composition based on anti-fatigue giant salamander peptide with better quality is obtained. Moreover, the whole is also applicable to large-scale industrial production, and the overall applicability is relatively strong.

[0027] In the third aspect, the present application provides an application of a composition based on anti-fatigue giant salamander peptide in skin care products.

[0028] To sum up, the present application has the following beneficial effects: By using the modified β-cyclodextrin and modified chitosan complex in combination, the present application can not only stably adsorb, immobilize and include the giant salamander peptide, but also delay the rapid release of the giant salamander peptide to form a "protection-sustained release" system. Moreover, the synergy between the two has excellent resistance to changes in the external environment and promotes the stable performance of the activity of the giant salamander peptide. In this way, when the composition based on anti-fatigue giant salamander peptide is applied, the giant salamander peptide contained therein is not easily damaged due to changes in the external environment and can stay on the skin surface for a long time, thereby exerting excellent skin care effects. Specific Embodiments

[0029] The present application will be further described in detail below with reference to preparation examples, examples and comparative examples.

[0030] Unless otherwise specified, the raw materials used in the preparation examples, examples and comparative examples of the present application are all commercially available.

[0031] The β-cyclodextrin raw material is purchased from Guangdong Mingtong Biotechnology Co., Ltd., with a particle size of 120 mesh and a CAS number of 68168-23-0; The chitosan raw material is purchased from the medicinal-grade chitosan of Shaanxi Tangyao Biotechnology Co., Ltd., Pharmacopoeia Edition 500g acid-soluble CDE registration number 9012-76-4; The diatomite raw material is purchased from Shijiazhuang Xunhua Mineral Products Co., Ltd., with a specification of 325 mesh; The carboxymethyl cellulose is purchased from Guangzhou Yiming Chemical Industry Co., Ltd., with a viscosity specification of 800.

[0032] Preparation Examples of Raw Materials and / or Intermediates Preparation Example 1 A modified β-cyclodextrin is obtained by the following method: Take a 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 h (in this preparation example, the reaction is carried out at 60 °C for 8 h), cool to 25 °C and neutralize with hydrochloric acid. After removing ions by ion exchange resin, concentrate by vacuum distillation, then drop into acetone, and finally obtain the modified β-cyclodextrin through filtration and drying.

[0033] Note: In the above operation, the sodium hydroxide solution is obtained by mixing 2 g of sodium hydroxide and 30 mL of water; the ratio of the used β-cyclodextrin raw material to dimethyl sulfate is 2 g:1 mL.

[0034] Preparation Example 2 A modified β-cyclodextrin, different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 1.5 g:1 mL.

[0035] Preparation Example 3 A modified β-cyclodextrin, different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2.5 g:1 mL.

[0036] Preparation Example 4 A modified β-cyclodextrin, different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 1.4 g:1 mL.

[0037] Preparation Example 5 A modified β-cyclodextrin, different from Preparation Example 1 in that the ratio of the β-cyclodextrin raw material to dimethyl sulfate is 2.6 g:1 mL.

[0038] Preparation Example 6 A modified chitosan complex is obtained by the following method: Take an acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomite raw material to infiltrate, react at 55 - 65 °C for 1.5 - 2.5 h (in this preparation example, the reaction is carried out at 60 °C for 2 h), and dry to obtain an intermediate product; then disperse the intermediate product in deionized water at a ratio of 25 g:1 L, add carboxymethyl cellulose and stir to dissolve, then add a crosslinking agent for reaction. After washing and drying the obtained reaction product, a modified chitosan complex is obtained.

[0039] Note: In the above operation, the mass fraction of the acetic acid solution is 3%; the crosslinking agent is ferric chloride, and the dosage of the crosslinking agent is 1.2% of the total mass of the intermediate product and carboxymethyl cellulose; the weight ratio of the used chitosan raw material, diatomite raw material and carboxymethyl cellulose is 1:2.5:4.5.

[0040] Preparation Example 7 A modified chitosan complex, which is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomite raw material and the carboxymethyl cellulose is 1:2:4.

[0041] Preparation Example 8 A modified chitosan complex, which is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomite raw material and the carboxymethyl cellulose is 1:3:5.

[0042] Preparation Example 9 A modified chitosan complex, which is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomite raw material and the carboxymethyl cellulose is 1:1.8:3.8.

[0043] Preparation Example 10 A modified chitosan complex, which is different from Preparation Example 6 in that the weight ratio of the chitosan raw material, the diatomite raw material and the carboxymethyl cellulose is 1:3.2:5.2.

[0044] Examples Example 1 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 obtained through the following steps: (1) Prepare raw materials including a humectant, a thickener, an emulsifier, an antibacterial preservative, giant salamander peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, modified β-cyclodextrin and a modified chitosan complex according to the ratio; (2) Mix the humectant, sodium hyaluronate, carbomer and deionized water in step (1) and heat to 80 °C to obtain a phase A mixture; heat the thickener, emulsifier and caprylic / capric triglyceride in step (1) to 75 °C and stir to obtain a phase B mixture; (3) Mix the phase A mixture and the phase B mixture, homogenize at 1500 rpm for 20 min, then cool to 45 °C, add giant salamander peptide, modified β-cyclodextrin and the modified chitosan complex and stir to mix, and cool to 25 °C, and finally add the antibacterial preservative and mix to obtain the composition based on anti-fatigue giant salamander peptide.

[0045] Note: In the above operations, the humectant is glycerol, 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 complex is obtained from Preparation Example 6.

[0046] Examples 2-3 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the raw materials used in its preparation and their corresponding parts by weight are shown in Table 1.

[0047] Table 1 Raw materials used in the preparation of Examples 1-3 and their corresponding parts by weight (parts / kg) Example 4 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the total amount of the modified β-cyclodextrin and the modified chitosan complex is unchanged, and the ratio of their parts by weight is adjusted to 2:1.

[0048] Example 5 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 2.

[0049] Example 6 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 3.

[0050] Example 7 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 4.

[0051] Example 8 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified β-cyclodextrin is obtained from Preparation Example 5.

[0052] Example 9 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified chitosan complex is obtained from Preparation Example 7.

[0053] Example 10 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified chitosan complex is obtained from Preparation Example 8.

[0054] Example 11 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified chitosan complex is obtained from Preparation Example 9.

[0055] Example 12 A composition based on anti-fatigue giant salamander peptide, which is different from Example 1 in that the modified chitosan complex is obtained from Preparation Example 10.

[0056] Comparative Example Comparative Example 1 A composition based on anti-fatigue giant salamander peptide, which is different from that of Example 1 in that modified β-cyclodextrin is not used in the raw materials.

[0057] Comparative Example 2 A composition based on anti-fatigue giant salamander peptide, which is different from that of Example 1 in that the modified chitosan complex is not used in the raw materials.

[0058] Comparative Example 3 A composition based on anti-fatigue giant salamander peptide, which is different from that of Example 1 in that neither modified β-cyclodextrin nor the modified chitosan complex is used in the raw materials.

[0059] Comparative Example 4 A composition based on anti-fatigue giant salamander peptide, which is different from that of Example 1 in that the modified β-cyclodextrin is replaced with β-cyclodextrin raw material in equal mass.

[0060] Comparative Example 5 A composition based on anti-fatigue giant salamander peptide, which is different from that of Example 1 in that the modified chitosan complex is replaced with chitosan raw material in equal mass.

[0061] Comparative Example 6 A composition based on anti-fatigue giant salamander peptide, which is different from that of Comparative Example 4 in that the modified chitosan complex is not used in the raw materials.

[0062] Comparative Example 7 A composition based on anti-fatigue giant salamander peptide, which is different from that of Comparative Example 5 in that modified β-cyclodextrin is not used in the raw materials.

[0063] Performance Detection Test Test Samples: The compositions based on anti-fatigue giant salamander peptide obtained in Examples 1-12 are selected as Test Samples 1-12, and the compositions based on anti-fatigue giant salamander peptide obtained in Comparative Examples 1-7 are selected as Control Samples 1-7.

[0064] Test Method: The content of giant salamander peptide in the composition based on anti-fatigue giant salamander peptide is tested by high performance liquid chromatography.

[0065] High Performance Liquid Chromatography (HPLC): HPLC is a highly efficient and rapid separation and determination technique, which is suitable for the determination of various peptide substances. By selecting a suitable chromatographic column and mobile phase, peptide substances can be separated from other impurities, and the content of peptides can be determined through the response signal of the detector.

[0066] Generally, a Sino Chrom C18 reversed-phase column and an ultraviolet variable wavelength detector are used. The detection wavelength is 280 nm. The mobile phase is a mixture of acetonitrile, methanol, and 0.1% trifluoroacetic acid (in a ratio of 5:5:90), the flow rate is 1.0 mL / min, and the injection volume is 20 μL.

[0067] (1) Stability test under high temperature and strong light conditions: Take the composition based on anti-fatigue giant salamander peptide for the above test, and record the content of giant salamander peptide as A1; Secondly, place the same amount of the composition based on anti-fatigue giant salamander peptide in a high and low temperature alternating test chamber. The initial temperature is 25°C. First, heat it to 55°C at a rate of 2°C / min, maintain it for 10 min, then cool it to 45°C at a rate of 1.5°C / min, maintain it for 15 min, and finally cool it to 25°C at a rate of 1°C / min. During the process, irradiate it with 1000 W / m 2 Simulate sunlight irradiation to complete the high temperature and light test. Then, perform the above test on the composition based on anti-fatigue giant salamander peptide in the same way, and record the content of giant salamander peptide as B1; Finally, calculate the change rate of the content of giant salamander peptide in the composition based on anti-fatigue giant salamander peptide. The change rate of giant salamander peptide content = (A1 - B1) / A1; and the greater the change rate of giant salamander peptide content, the better the application stability of the composition based on anti-fatigue giant salamander peptide under high temperature and strong light conditions.

[0068] (2) Persistence test of giant salamander peptide staying on the skin surface: Take the corresponding application amount of the composition based on anti-fatigue giant salamander peptide for the above test, and record the content of giant salamander peptide as A2; Randomly select 10 women aged 20 - 40 as test subjects, and apply the composition based on anti-fatigue giant salamander peptide evenly on the back of the hand at a standard dosage of 2 mg / cm 2 After applying and keeping it for 60 s, collect the remaining composition based on anti-fatigue giant salamander peptide on the back of the hand, and then perform the above test on the remaining composition based on anti-fatigue giant salamander peptide in the same way. Record the average value of the content of giant salamander peptide as B2; Finally, calculate the residual rate of the content of giant salamander peptide in the composition based on anti-fatigue giant salamander peptide. The residual rate of giant salamander peptide content = B2 / A2; and the greater the residual rate of giant salamander peptide content, the easier the giant salamander peptide component can stay and act on the skin surface for a longer time, and the better the skin care effect of the composition based on anti-fatigue giant salamander peptide.

[0069] After performing the above tests on test samples 1 - 12 and control samples 1 - 7, record the test results in Table 2 correspondingly.

[0070] Table 2 Test results of test samples 1 - 12 and control samples 1 - 7 Combined with Example 1 and Comparative Examples 1-3 and Table 2, it can be seen that in the composition based on anti-fatigue giant salamander peptide, by using the complex of modified β-cyclodextrin and modified chitosan, during the application process, the giant salamander peptide is not easily damaged due to changes in the external environment. Especially under high temperature and strong light conditions, it can maintain excellent stability and can stay on the skin surface for a relatively long time, thereby exerting excellent skin care effects. If only the complex of modified β-cyclodextrin or modified chitosan is used, although it can bring corresponding improvement in effects, the improvement amplitude is limited, and the sum of the improvement effects brought by their respective single applications is far less excellent than the improvement effect brought by their combination. Thus, it can be seen that the combination between the complex of modified β-cyclodextrin and modified chitosan can exert a synergistic improvement effect of 1 + 1 > 2 in the composition based on anti-fatigue giant salamander peptide, and the overall improvement effect is significant. Combining with Comparative Examples 4-7 and Table 2 again, it can be seen that if the modified β-cyclodextrin is replaced with β-cyclodextrin raw material of equal mass, and the modified chitosan complex is replaced with chitosan raw material of equal mass, both will cause a significant reduction in the above test results of the composition based on anti-fatigue giant salamander peptide, and only a simple addition of effects can be brought between the β-cyclodextrin raw material and the modified chitosan complex, as well as between the chitosan raw material and the modified β-cyclodextrin, and the excellent synergistic improvement effect cannot be exerted. Thus, it can be seen that the significant effect brought by the combination of the modified β-cyclodextrin and the modified chitosan complex in this application is irreplaceable.

[0071] Combined with Examples 1-3 and Example 4 and Table 2, it can be seen that when the weight ratio of the modified β-cyclodextrin and the modified chitosan complex is 2:1, the complex system formed by their synergy has relatively excellent corresponding effects on the giant salamander peptide, and the experimental results obtained from the above tests are relatively good.

[0072] Combined with Example 1 and Examples 5-8 and Table 2, it can be seen that in the preparation of the modified β-cyclodextrin, the ratio of the used β-cyclodextrin raw material to dimethyl sulfate is (1.5 - 2.5) g:1 mL, and the prepared modified β-cyclodextrin can exert excellent cooperation effects with the modified chitosan complex after application; whether it is lower or higher than the above ratio range, after the modified β-cyclodextrin is applied, the corresponding quality of the composition based on anti-fatigue giant salamander peptide will show obvious losses after the above tests.

[0073] Combined with Example 1 and Examples 9-12 and in combination with Table 2, it can be seen that in the preparation of the modified chitosan complex, the weight ratio of the chitosan raw material, diatomaceous earth raw material, and carboxymethyl cellulose used is 1:(2-3):(4-5). The prepared modified chitosan complex can exhibit excellent cooperation effects with modified β-cyclodextrin after application; while whether lower or higher than the above ratio range, after the obtained modified chitosan complex is applied, the corresponding quality of the composition based on anti-fatigue giant salamander peptide will show obvious losses after the above tests.

[0074] This specific embodiment is only an interpretation of the present application, and it is not a limitation of the present application. After reading this specification, those skilled in the art can make modifications to this embodiment without creative contributions 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, Comprising the following components in parts by weight: Humectant 3 - 5 parts; Thickener 3 - 8 parts; Emulsifier 4 - 5 parts; Antibacterial preservative 0.1 - 0.3 parts; Andrias davidianus peptide 0.03 - 0.06 parts; Sodium hyaluronate 0.05 - 0.1 parts; Carbomer 0.1 - 0.2 parts; Caprylic / capric triglyceride 5 - 8 parts; Deionized water 60 - 70 parts; Modified β - cyclodextrin 1.2 - 1.5 parts; Modified chitosan complex 0.3 - 1 part; The modified β - cyclodextrin is obtained 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 h, cool and neutralize, remove ions and then concentrate by vacuum distillation, then drop into acetone, and finally obtain modified β - cyclodextrin through filtration and drying; The modified chitosan complex is obtained by the following method: Take acetic acid solution, add chitosan raw material and stir to dissolve, then add diatomite raw material to infiltrate, react at 55 - 65 °C for 1.5 - 2.5 h, 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 - linker for reaction, and after washing and drying the obtained reaction product, obtain the modified chitosan complex.

2. The composition based on anti-fatigue giant salamander peptide according to claim 1, wherein: The weight ratio of the modified β - cyclodextrin to the modified chitosan complex is 2:

1.

3. The composition based on anti-fatigue giant salamander peptide according to claim 1, wherein: In the preparation of the modified β - cyclodextrin, the ratio of the used β - cyclodextrin raw material to dimethyl sulfate is (1.5 - 2.5) g:1 mL.

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

5. The composition based on anti-fatigue giant salamander peptide according to claim 1, characterized in that: In the preparation of the modified chitosan complex, the weight ratio of the used chitosan raw material, diatomite raw material and carboxymethyl cellulose is 1:(2 - 3):(4 - 5).

6. The composition based on anti-fatigue giant salamander peptide according to claim 5, characterized in that: The weight ratio of the chitosan raw material, diatomite raw material and carboxymethyl cellulose is 1:2.5:4.

5.

7. The composition based on anti-fatigue giant salamander peptide according to claim 1, wherein: The humectant is a composition of one or more of glycerol, vitamin E, allantoin, polyethylene glycol, ceramide and urea; The thickener is a composition of one or more of xanthan gum, carrageenan, stearic acid, polyvinyl alcohol and cellulose derivatives; The emulsifier is a composition of one or more of steareth - 6, glyceryl stearate, cetearyl alcohol polyether - 20 and sodium lauryl sulfate.

8. The preparation method of the composition based on anti-fatigue giant salamander peptide according to claim 1, wherein: Including the following steps: (1) Prepare raw materials containing humectant, thickener, emulsifier, antibacterial preservative, Andrias davidianus peptide, sodium hyaluronate, carbomer, caprylic / capric triglyceride, deionized water, modified β - cyclodextrin and modified chitosan complex according to the ratio; (2) Mix and heat the humectant, sodium hyaluronate, carbomer and deionized water in step (1) to obtain phase A mixture; heat and stir the thickener, emulsifier and caprylic / capric triglyceride in step (1) to obtain phase B mixture; (3) After mixing phase A mixture and phase B mixture, then add Andrias davidianus peptide, modified β - cyclodextrin and modified chitosan complex and stir to mix, and finally add antibacterial preservative and mix to obtain the composition based on anti - fatigue Andrias davidianus peptide.

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

Citation Information

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