Astaxanthin chitin nanofiber oleogel and preparation method thereof

Abstract

The invention relates to the field of biological medicine, and discloses astaxanthin chitin nanofiber oil gel and a preparation method thereof.The astaxanthin chitin nanofiber oil gel is prepared from, by mass, 0.01%-0.2% of astaxanthin, 95.0%-99.5% of tea seed oil and 0.3%-4.8% of chitin nanofiber. The astaxanthin chitin nanofiber oleogel is free of chemical additives, high in component adaptability and simple in preparation process, stable loading of astaxanthin can be achieved, the stability of astaxanthin is greatly improved, oxidative degradation of astaxanthin is effectively delayed, and the product validity period is prolonged.

Description

Technical Field

[0001] This application relates to the field of biomedicine, and mainly to an astaxanthin-chitoxin nanofiber oleogel and its preparation method. Background Technology

[0002] Skin damage repair is an important research direction in the fields of biomedicine and skin care. Currently, there are various skin damage repair products on the market, such as ointments, gels, and dressings. These products mainly work through three mechanisms: first, they form a physical protective layer to act as a barrier, blocking external bacterial infection while maintaining a moist environment on the wound; second, they gradually act on the wound to promote healing by releasing drug components; and third, they rely on bioactive ingredients to regulate cell proliferation and differentiation, achieving repair effects at the cellular level.

[0003] Astaxanthin, a ketocarotenoid, possesses the antioxidant properties of carotenoids. Its ability to quench singlet oxygen and scavenge free radicals is far superior to β-carotene and vitamin E, exceeding β-carotene by more than 10 times and vitamin E by more than 100 times, thus earning it the title of "super vitamin E." Its antioxidant properties, coloring properties, and ability to enhance the body's immunity are widely recognized. Natural astaxanthin is an extremely potent antioxidant carotenoid, possessing antioxidant, anti-aging, anti-tumor, and cardiovascular disease prevention effects. It is currently used internationally in health foods, high-end cosmetics, and pharmaceuticals. However, its poor stability and susceptibility to oxidation significantly limit its practical application in skin damage repair products.

[0004] Tea seed oil is a woody edible oil extracted from the fruit of the tea tree (Camellia sinensis). Due to its scarcity and rich nutrition, it is known as "oil gold." Its unsaturated fatty acid content exceeds 82%, and its linoleic acid and vitamin E content are approximately 3-6 times and 5-10 times that of olive oil, respectively. It also contains active ingredients such as tea polyphenols, phytosterols, and squalene. The fatty acid ratio meets the WHO's recommended ω6 / ω3 standard, and it has antioxidant and lipid-lowering effects. It is a high-quality natural matrix in the field of skin damage repair that combines moisturizing and active auxiliary functions.

[0005] Chitin is mostly extracted from shrimp and crab shells. After being nanoscaled through processes such as ultrasonication, mechanical grinding, and high-pressure homogenization, chitin nanofibers can be obtained. This product not only retains the excellent properties of chitin itself, but also has the characteristics of high aspect ratio, high specific surface area, and low density. In addition, it contains nitrogen-containing functional groups that are beneficial to surface functionalization. It can play a role in promoting cell proliferation and film formation protection in skin wound repair. At present, it has been widely used in many fields such as food and medicine, and is also an important biomaterial in the field of skin care.

[0006] However, current skin damage repair technologies and products still face many unresolved issues. On one hand, the instability of astaxanthin is a core pain point in its application; its inherent oxidative properties significantly reduce product efficacy, making it difficult to fully realize its antioxidant and repairing effects. On the other hand, the overall repair efficiency of these products is generally low. Traditional repair products have long healing cycles for superficial injuries such as acne and sunburn, and their repair effects on deep wounds are also very limited, failing to meet the demand for efficient wound healing. Furthermore, some products have poor biocompatibility, and added ingredients can easily trigger skin allergic reactions, negatively impacting product safety. In addition, existing products suffer from insufficient synergistic effects, relying mostly on single ingredients for repair without achieving a scientific combination and synergistic effect of multiple active ingredients, making it difficult to achieve a synergistic repair effect greater than the sum of its parts (1+1>2). They also fail to fully exploit the composite repair value of high-quality raw materials such as astaxanthin, tea seed oil, and chitosan nanofibers.

[0007] Therefore, existing technologies still need to be improved and developed. Summary of the Invention

[0008] In view of the shortcomings of the prior art, the purpose of this application is to provide an astaxanthin-chitoxin nanofiber oleogel and its preparation method. The astaxanthin-chitoxin nanofiber oleogel has skin damage repair function, aiming to solve the problem that the instability of astaxanthin in existing skin damage repair products makes it difficult to fully exert its antioxidant repair effect.

[0009] The technical solution of this application is as follows: An astaxanthin-chitoxin nanofiber oleogel, comprising, by weight percentage, the following raw materials: Astaxanthin 0.01%-0.2%, tea seed oil 95.0%-99.5%, chitin nanofibers 0.3%-4.8%.

[0010] The astaxanthin-chitosan nanofiber oleogel, wherein the astaxanthin is natural astaxanthin.

[0011] The astaxanthin-chitosan nanofiber oleogel is wherein the tea seed oil is prepared using a low-temperature cold pressing process.

[0012] The astaxanthin-chitosan nanofiber oleogel, wherein the chitosan nanofiber has a fiber diameter of 50-200 nm.

[0013] The astaxanthin-chitosan nanofiber oleogel mentioned above, wherein the natural astaxanthin is derived from natural algae.

[0014] A method for preparing the astaxanthin-chitoxin nanofiber oleogel as described above, comprising the following steps: Astaxanthin was mixed with tea seed oil to obtain an astaxanthin-tea seed oil solution. Chitosan nanofibers were added to obtain a mixed solution; The mixed solution is subjected to high-pressure homogenization.

[0015] The preparation method of the astaxanthin-chitoxin nanofiber oleogel, wherein the high-pressure homogenization process is controlled at 100-200 MPa.

[0016] The method for preparing the astaxanthin-chitoxin nanofiber oleogel includes a high-pressure homogenization process involving 3-5 cycles.

[0017] The method for preparing the astaxanthin-chitosan nanofiber oleogel, wherein the astaxanthin is completely dissolved during the mixing process of astaxanthin and tea seed oil.

[0018] The method for preparing the astaxanthin-chitosan nanofiber oleogel includes, after the step of adding chitosan nanofibers, continuously stirring until the chitosan nanofibers are evenly dispersed in the astaxanthin-tea seed oil solution.

[0019] Beneficial Effects: The astaxanthin-chitosan nanofiber oleogel of this application is free of chemical additives, has high component compatibility, and a simple preparation process. It can achieve stable loading of astaxanthin, significantly improving its stability, effectively delaying its oxidative degradation, and extending the product's shelf life. Simultaneously, it can achieve synergistic and enhanced effects from multiple components, breaking through the limitations of single-component repair. This allows the antioxidant effect of astaxanthin, the healing-promoting and barrier-protecting effects of chitosan nanofibers, and the moisturizing and anti-inflammatory effects of tea seed oil to complement and reinforce each other. Attached Figure Description

[0020] Figure 1 This is a schematic flowchart illustrating the preparation method of the astaxanthin-chitoxin nanofiber oleogel of this application.

[0021] Figure 2 This is a schematic diagram of the microstructure of the astaxanthin-chitoxin nanofiber oleogel of this application.

[0022] Figure 3 This is a comparative study of the repair effect of full-thickness skin wounds in rats over 7 days, as shown in Example 1 of this application.

[0023] Labeling Explanation: 10, Astaxanthin; 20, Chitosan Nanofibers; 30, Tea Seed Oil. Detailed Implementation

[0024] This application provides an astaxanthin-chitoxin nanofiber oleogel and its preparation method. To make the objectives, technical solutions, and effects of this application clearer and more explicit, the following provides a more detailed description. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.

[0025] This application provides an astaxanthin-chitosan nanofiber oleogel, which has skin damage repair function and comprises the following raw materials by weight percentage: Astaxanthin 0.01%-0.2%, tea seed oil 95.0%-99.5%, chitin nanofibers 0.3%-4.8%.

[0026] The astaxanthin-chitosan nanofiber oleogel of this application uses natural active ingredients as its core and natural oils as its carrier. Through scientific formulation and a specific preparation process, a stable gel system is constructed, possessing multiple effects including antioxidant, anti-inflammatory, healing-promoting, moisturizing, and repairing properties. It has a highly effective repairing effect on skin damage. Furthermore, the ingredients are natural and free of chemical additives, exhibiting excellent biocompatibility and being gentle and non-irritating to use. Based on this astaxanthin-chitosan nanofiber oleogel formula, it has skin damage repair functions and is suitable for repairing acne, sunburn, skin redness and swelling, abrasions, and other superficial wounds.

[0027] In this application, astaxanthin is the core active ingredient. Preferably, high-purity natural astaxanthin is obtained through extraction and purification techniques (high purity refers to an astaxanthin mass fraction of ≥95%, preferably 98%–99%), without the use of chemically synthesized astaxanthin. Natural astaxanthin can be derived from natural algae such as Haematococcus pluvialis. The function of astaxanthin is to precisely eliminate free radicals in skin wounds and surrounding tissues, block oxidative stress reactions, reduce oxidative damage to skin cells, and simultaneously provide an antioxidant microenvironment for wound repair, assisting in promoting normal cell proliferation.

[0028] Natural astaxanthin can be purchased as a commercially available product or prepared using known extraction and purification methods. Methods for obtaining natural astaxanthin through extraction and purification of natural algae are existing technologies and will not be elaborated upon here. In the embodiments of this application, the natural astaxanthin used was purchased from Shaanxi Jinkangtai Biotechnology Co., Ltd., with a purity of 96%.

[0029] Tea seed oil serves as a natural carrier matrix, preferably extracted from the fruit of the tea tree (Camellia sinensis) using a low-temperature cold-pressing process. This process avoids high-temperature processing throughout, maximizing the retention of inherent active ingredients such as tea polyphenols, phytosterols, squalene, and natural vitamin E. Tea seed oil acts as a natural carrier, dissolving astaxanthin and dispersing chitosan nanofibers, while also providing moisturizing, water-locking, anti-inflammatory, and soothing effects. It replenishes the lipid components needed by skin wounds, improves skin barrier function, and alleviates inflammatory responses such as redness, swelling, and pain.

[0030] Chitosan nanofibers are oleogels with fiber diameters ranging from 50 to 200 nm. They are prepared by extracting chitosan from shrimp and crab shells, and then nano-sizing it using methods such as ultrasonication, mechanical grinding, or high-pressure homogenization. This process yields chitosan nanofibers with high specific surface area and high activity. These nanofibers exhibit natural biological activity, promoting the adhesion and proliferation of skin fibroblasts and epithelial cells, regulating local immune responses at the wound site, and reducing the excessive release of inflammatory factors. Simultaneously, the nanofiber properties enable the formation of a physical support structure, creating a protective barrier for the wound and reducing external irritation.

[0031] Chitosan nanofibers can be purchased as commercially available products or prepared using known methods. The preparation of chitosan nanofibers using chitosan is existing technology and will not be elaborated upon here. In the embodiments of this application, the preparation process of chitosan nanofibers is as follows: chitosan with a degree of deacetylation of 15%-50% is added to a 33% NaOH solution (1400 mL of NaOH solution is added for every 100 g of chitosan), reacted at 60°C for 5 hours, washed with water until neutral after the reaction, coarsely pulverized using an emulsifier, and then processed using a high-pressure homogenizer at a pressure of 100 MPa for 3 cycles to obtain a chitosan nanofiber paste. An equal volume of tert-butanol is added to the paste, mixed thoroughly, and then freeze-dried to obtain chitosan nanofibers with a degree of deacetylation of 28%-30%.

[0032] The astaxanthin-chitosan nanofiber oleogel of this application is prepared by a specific process of "stepwise dissolution-composite dispersion-homogenization gelation", with astaxanthin as the core active ingredient, tea seed oil as the natural carrier matrix, and chitosan nanofiber as the oleogel agent.

[0033] This application also provides a method for preparing astaxanthin-chitosan nanofiber oleogels with skin damage repair functions, such as... Figure 1 As shown, it includes the following steps: First, mix astaxanthin with tea seed oil thoroughly until the astaxanthin is completely dissolved, forming a homogeneous and stable astaxanthin-tea seed oil solution. Next, chitin nanofibers were added to the astaxanthin tea seed oil solution, and the mixture was stirred until the chitin nanofibers were evenly dispersed in the astaxanthin tea seed oil solution to obtain a mixed solution. The mixed solution is subjected to high-pressure homogenization.

[0034] After high-pressure homogenization, the three components are fully integrated and interact with each other, ultimately forming a stable astaxanthin-chitoxin nanofiber oleogel with well-preserved activity.

[0035] In the preparation method provided in this application, the composite system needs to be treated with a high-pressure homogenizer, with the treatment pressure controlled at 100-200 MPa, and cyclically treated 3-5 times to ensure that astaxanthin, chitosan nanofibers, and tea seed oil are fully mixed and uniformly dispersed. This allows astaxanthin to be adsorbed onto the surface of the chitosan nanofibers and uniformly dispersed in the tea seed oil matrix, achieving a close combination and interaction of the components. Figure 2 As shown, chitin nanofibers 20 interweave to form a three-dimensional network structure, astaxanthin 10 is uniformly distributed in the three-dimensional network structure, and tea seed oil 30 fills the gaps in the three-dimensional network structure.

[0036] The astaxanthin-chitosan nanofiber oleogel of this application can achieve synergistic and enhanced effects of multiple components, breaking through the limitations of single-component repair. It allows the antioxidant effect of astaxanthin, the healing-promoting and barrier-protecting effects of chitosan nanofibers, and the moisturizing and anti-inflammatory effects of tea seed oil to complement and strengthen each other, forming a comprehensive wound repair system. Its repair effect is far superior to that of a single component or any combination of two components, and it can quickly improve skin damage symptoms such as acne, sunburn, and abrasions, improving the overall repair efficiency and effect.

[0037] The astaxanthin-chitosan nanofiber oleogel of this application is free of chemical additives, has high component compatibility, and a simple preparation process. It can achieve stable loading of astaxanthin, greatly improve the stability of astaxanthin, effectively delay its oxidative degradation, and extend the product's shelf life. At the same time, the thin barrier formed by the chitosan nanofibers can block the invasion of external bacteria without affecting the breathability of the wound, reduce the risk of infection, and reduce the formation of scar tissue, thereby improving the quality of wound repair.

[0038] Compared with existing technologies, the astaxanthin-chitoxin nanofiber oleogel of this application has the following advantages: (1) Raw materials are readily available and environmentally friendly: The core raw materials, astaxanthin, tea seed oil and chitin, are all natural sources. Chitin can also be extracted from shrimp and crab shells and aquatic waste, realizing resource reuse, which is in line with the development trend of green and environmental protection.

[0039] (2) The preparation process is simple and easy to industrialize: the entire preparation process does not involve harsh conditions such as high temperature and high pressure. The core steps are only dissolution, dispersion and high pressure homogenization. The equipment requirements are conventional and it is easy to scale up production.

[0040] (3) Astaxanthin stability is greatly improved: the fat-soluble protection of tea seed oil and the physical encapsulation of chitin nanofiber three-dimensional network effectively reduce the oxidative degradation of astaxanthin, significantly extend the product shelf life, and improve the effective utilization rate of astaxanthin.

[0041] (4) Good biocompatibility and high safety: All raw materials are natural ingredients or high-purity natural extracts, with no chemical additives. Verified by cytotoxicity test and skin irritation test, there is no obvious skin allergic reaction.

[0042] (5) Significant synergistic effect: Breaking through the limitations of the single component effect of traditional products, it achieves the superposition of three major functions: anti-oxidation, anti-inflammation and healing promotion.

[0043] The present application will be further described below through specific embodiments.

[0044] Example 1 The astaxanthin-chitosan nanofiber oleogel with skin damage repair function in this application embodiment includes the following raw materials by mass percentage: Astaxanthin 0.1%, tea seed oil 98.1%, chitin nanofibers 1.8%.

[0045] The preparation method of the astaxanthin-chitosan nanofiber oleogel with skin damage repair function according to the embodiments of this application specifically includes the following steps: Step 1, Astaxanthin Dissolution: Add the specified amount of astaxanthin (96% pure natural astaxanthin) to the tea seed oil (tea seed oil obtained by low-temperature cold pressing process), and stir thoroughly until the astaxanthin is completely dissolved to form a homogeneous and stable astaxanthin tea seed oil solution. Step 2, Chitosan nanofiber addition: Add the chitosan nanofibers (with a fiber diameter of 50-80nm) in the above proportion to the astaxanthin tea seed oil solution, and continue stirring until the chitosan nanofibers are evenly dispersed in the solution to obtain a mixed solution. Step 3, High-pressure homogenization: The mixed solution is introduced into a high-pressure homogenizer for high-pressure homogenization. The processing pressure of the high-pressure homogenizer is set to 200MPa, and the process is repeated 5 times to fully integrate the components and form a structurally stable astaxanthin-chitosan nanofiber oleogel. Step 4, Quality Inspection: Multiple quality performance tests were performed on the obtained astaxanthin-chitoxin nanofiber oleogel. First, the overall physicochemical stability of the astaxanthin-chitoxin nanofiber oleogel was tested, with a focus on whether astaxanthin underwent oxidative degradation. Secondly, the biocompatibility and safety of the astaxanthin-chitosan nanofiber oleogel were verified through in vitro cytotoxicity tests and skin irritation tests. Finally, the actual repair effect of astaxanthin-chitosan nanofiber oleogel on skin damage was evaluated using an in vitro wound repair model.

[0046] After conducting multiple quality and performance tests on the astaxanthin-chitoxin nanofiber oleogel of this embodiment, the test results all meet the application requirements of skin damage repair products. The specific evaluation is as follows: (1) In terms of stability testing, the astaxanthin-chitosan nanofiber oleogel was stored in a sealed environment at 25°C in the dark for 6 months. There were no signs of layering, clumping, or discoloration. The texture remained uniform. Furthermore, the astaxanthin did not show obvious oxidative degradation. Its effective component retention rate was ≥85%, which further verified that the astaxanthin-chitosan nanofiber oleogel has excellent physicochemical stability and can fully meet the shelf life requirements for regular storage and use of the product.

[0047] (2) Regarding biosafety testing, the in vitro cytotoxicity test results showed that when the extract of astaxanthin-chitosan nanofiber oleogel (astaxanthin-chitosan nanofiber oleogel was taken, and serum-free culture medium for cell culture was used as the extraction medium, and the ratio of 1g sample to 10mL extraction medium was used, it was statically extracted in a 37℃, 5% CO2 incubator for 24h. After the extraction, it was filtered through a 0.22μm sterile filter membrane to remove insoluble impurities and obtain a sterile, clear extract) was applied to skin fibroblasts, the cell survival rate was ≥90% and there was no obvious cytotoxicity. The skin irritation test was conducted using the rat skin irritation test method. After continuous application of astaxanthin-chitosan nanofiber oleogel for 7 days, no irritation reactions such as redness, swelling, itching, erythema, or edema were observed on the tested skin. The skin irritation evaluation was non-irritating, which confirmed that the astaxanthin-chitosan nanofiber oleogel has excellent biocompatibility and high safety.

[0048] (3) Regarding the detection of wound repair effect, the effect of oleogel on wound repair was evaluated by establishing a rat full-thickness skin wound repair model: All rats were fed laboratory-standard water and food and were randomly divided into 4 groups (6 rats / group): saline group (blank control group), astaxanthin group, chitin nanofiber group and astaxanthin-chitin nanofiber oleogel group.

[0049] First, circular, full-thickness skin wounds (15 mm in diameter) were cut on the backs of all rats. Then, the wounds of the blank control group rats were treated with 0.2 mL of physiological saline; the wounds of the astaxanthin group rats were treated with astaxanthin physiological saline dispersion, which was evenly applied to the wounds (preparation of astaxanthin physiological saline dispersion: 2 mg of astaxanthin was placed in a sterile grinding bowl, 0.1 mL of sterile physiological saline was added, and the mixture was gently ground until a fine paste was formed); the wounds of the chitosan nanofiber group were treated with chitosan nanofiber physiological saline dispersion, which was evenly applied to the wounds (preparation of chitosan nanofiber physiological saline dispersion: 2 mg of chitosan nanofiber was placed in a sterile container, 0.1 mL of sterile physiological saline was added, and the dispersion was made into a gel); the astaxanthin-chitosan nanofiber oleogel group was treated with 0.1 mL of the astaxanthin-chitosan nanofiber oleogel prepared in this example, which was evenly applied to the wounds. During the experiment, all rats were administered physiological saline or the corresponding preparation once daily. During the experiment, the area of ​​the wound was recorded daily using a digital camera. The measurement results were expressed as a percentage change relative to the original wound area, and the average value was taken.

[0050] The results are as follows Figure 3 As shown in Table 1, after 7 days, compared with the blank control group, the wound healing rate of the astaxanthin-chitoxin nanofiber oleogel of this embodiment was significantly improved, the wound inflammation resolution time was shortened, and the epithelial cell proliferation activity was significantly enhanced. This further corroborates that the astaxanthin-chitoxin nanofiber oleogel of this embodiment has a significant promoting effect on skin injury healing, and its repair effect is clear and stable. Figure 3 In the study, 1 was the blank control group, 2 was the astaxanthin group, 3 was the chitin nanofiber group, and 4 was the astaxanthin-chitin nanofiber oleogel group.

[0051] Table 1. Wound healing rate at different times for each group

[0052] The astaxanthin-chitosan nanofiber oleogel of this embodiment has a significant healing effect on skin wounds. For superficial wounds such as abrasions, it can significantly improve symptoms such as redness, swelling, damage, and inflammation within 72 hours after application, and achieve complete wound healing within 1-2 weeks. At the same time, the oleogel structure effectively protects astaxanthin, significantly improves its stability, slows down its oxidative degradation rate, and effectively extends the product's shelf life.

[0053] It should be understood that the application of this application is not limited to the examples above. Those skilled in the art can make improvements or modifications based on the above description, and all such improvements and modifications should fall within the protection scope of this application.

Claims

1. An astaxanthin-chitoxin nanofiber oleogel, characterized in that, The following raw materials are included by weight percentage: Astaxanthin 0.01%-0.2%, tea seed oil 95.0%-99.5%, chitin nanofibers 0.3%-4.8%.

2. The astaxanthin-chitoxin nanofiber oleogel according to claim 1, characterized in that, The astaxanthin mentioned is natural astaxanthin.

3. The astaxanthin-chitoxin nanofiber oleogel according to claim 1, characterized in that, The tea seed oil is prepared using a low-temperature cold pressing process.

4. The astaxanthin-chitoxin nanofiber oleogel according to claim 1, characterized in that, The chitin nanofibers have a diameter of 50-200 nm.

5. The astaxanthin-chitoxin nanofiber oleogel according to claim 2, characterized in that, The natural astaxanthin is derived from natural algae.

6. A method for preparing astaxanthin-chitoxin nanofiber oleogel as described in any one of claims 1-5, characterized in that, Includes the following steps: Astaxanthin was mixed with tea seed oil to obtain an astaxanthin-tea seed oil solution. Chitosan nanofibers were added to obtain a mixed solution; The mixed solution is subjected to high-pressure homogenization.

7. The method for preparing astaxanthin-chitoxin nanofiber oleogel according to claim 6, characterized in that, During the high-pressure homogenization process, the processing pressure is controlled at 100-200 MPa.

8. The method for preparing astaxanthin-chitoxin nanofiber oleogel according to claim 7, characterized in that, During the high-pressure homogenization process, the process is repeated 3-5 times.

9. The method for preparing astaxanthin-chitoxin nanofiber oleogel according to claim 6, characterized in that, During the process of mixing astaxanthin with tea seed oil, the astaxanthin is completely dissolved.

10. The method for preparing astaxanthin-chitoxin nanofiber oleogel according to claim 6, characterized in that, After the step of adding chitin nanofibers, continue stirring until the chitin nanofibers are evenly dispersed in the astaxanthin tea seed oil solution.

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