Liquid functional composition and application thereof

Through the combination of ultra-low temperature wall breaking technology and small molecule structure water, a liquid functional composition was prepared, which solved the problem of low efficiency of pine pollen products in releasing biologically active substances, achieved the effect of both internal and external use, and significantly improved the a health problem.

CN119423299APending Publication Date: 2025-02-14SHANGHAI SHIYI CONSTR TECH CO LTD
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Patent Information

Application Number
CN202411653565.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-19
Publication Date
2025-02-14

AI Technical Summary

Technical Problem

Existing pine pollen products are inefficient in releasing biologically active substances and lack products that have the dual effects of domestic and external use, making it difficult to effectively improve chronic degenerative diseases and skin problems.

Method used

Ultra-low-temperature wall breaking technology combined with small molecule structure water is used to prepare a liquid functional composition, which includes ultra-low-temperature wall breaking pollen, carrier, polypeptide, vitamin and other ingredients, and achieves both internal and external effects through innovative design.

Benefits of technology

It significantly improves the release and bioavailability of biologically active substances, realizes the dual effects of domestic and external use, and effectively improves a variety of health problems, including anti-inflammatory, immune regulation, antiviral and skin problems.

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Abstract

The invention relates to the technical field of functional compositions, in particular to a liquid functional composition and application thereof, and the liquid functional composition comprises the following components in parts by weight: 15-30 parts of ultralow-temperature wall-broken pine pollen; 60-75 parts of a carrier; 0-10 parts of rice polypeptide; 0-3 parts of whey protein isolate; 0 to 1.5 parts of beta-1, 3 / 1, 6-glucan; 0 to 0.3 part of vitamin C; 0.05 to 0.3 part of vitamin E; 0 to 0.3 part of citric acid; 0-10 parts of glycerol; 0 to 1.5 parts of sodium hyaluronate; 0-1 part of panthenol; 0 to 0.3 part of allantoin; 0 to 0.15 part of curcumin; 0 to 0.03 part of capsaicin; 0 to 0.6 part of carbomer; under the ultralow temperature condition, macromolecular structures such as polysaccharide and protein in pollen walls become more fragile and easier to crush, and the original configurations of the molecules can be kept to the maximum extent.
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Description

Technical Field

[0001] The present invention relates to the technical field of functional compositions, and in particular to a liquid functional composition and uses thereof. Background Art

[0003] In recent years, with people's increasing attention to health, research in the field of functional foods and cosmetics has continued to deepen. Among them, pine pollen has been one of the research hotspots due to its rich nutrients and potential health benefits. Traditionally, pine pollen is mainly used orally to improve immunity, improve nutritional status, etc. However, the existing technology still has many limitations in the application of pine pollen.

[0004] First, conventional pine pollen processing technologies, such as breaking the wall at room temperature or medium temperature, often fail to fully release the bioactive substances in the pollen. This not only limits its efficacy, but also reduces the bioavailability of the product. Secondly, most existing pine pollen products are limited to a single method of use, either oral health products or external skin care products, lacking a comprehensive product that has both internal and external effects. Furthermore, in terms of improving chronic degenerative diseases and treating skin problems such as herpes and calluses on the hands and feet, the effects of existing products are often unsatisfactory.

[0005] In addition, pine pollen products in the prior art are usually extracted with simple water or organic solvents, which makes it difficult to ensure the integrity and stability of the active ingredients. At the same time, in the product formula design, there is a lack of in-depth consideration of the synergistic effects between the components, resulting in poor overall product efficacy.

[0006] In view of the above problems, there is an urgent need to develop a new type of pine pollen functional composition that can retain and release bioactive substances to the maximum extent, while having the dual functions of oral and external use, and can effectively improve a variety of health problems. Summary of the invention

[0007] The present invention provides a liquid functional composition and its use, and the present invention aims to solve the problems existing in the prior art, such as the limitation of a single administration method, uncontrollable drug release, low bioavailability, etc. By innovatively combining a traditional Chinese medicine composition, an intelligent control system and a spectacle frame design, the present invention realizes a new and efficient treatment scheme for eye diseases.

[0008] The object of the present invention is to provide a liquid functional composition, which comprises the following components in parts by weight: 15-30 parts of ultra-low temperature broken pine pollen; 60-75 parts of carrier; Rice polypeptide 0-10 parts; Whey protein isolate 0-3 parts; β-1,3 / 1,6-glucan 0-1.5 parts; Vitamin C 0-0.3 parts; Vitamin E 0.05-0.3 parts; Citric acid 0-0.3 parts; Glycerin 0-10 parts; Sodium hyaluronate 0-1.5 parts; Panthenol 0-1 part; Allantoin 0-0.3 parts; Curcumin 0-0.15 parts; Capsaicin 0-0.03 parts; Carbomer 0-0.6 parts; Triethanolamine 0-0.3 parts.

[0009] Preferably, the ultra-low temperature wall-broken pine pollen includes masson pine pollen and tabulaeformis pollen, wherein the weight ratio of masson pine pollen to tabulaeformis pollen is 0.8-1.2:1.

[0010] Preferably, the carrier is selected from small molecule structured water, purified water or a combination thereof.

[0011] Preferably, for preparing functional food for internal use, the composition comprises the following components in parts by weight: 20-30 parts of ultra-low temperature broken pine pollen; 65-75 parts of small molecule structure water; 5-10 portions of rice polypeptide; 1-3 servings of whey protein isolate; β-1,3 / 1,6-glucan 0.5-1.5 parts; Vitamin C 0.1-0.3 parts; Vitamin E 0.05-0.15 parts; 0.1-0.3 parts of citric acid.

[0012] Preferably, for preparing an external functional product, the composition comprises the following components in parts by weight: 15-25 parts of ultra-low temperature broken pine pollen; 60-70 parts of purified water; Glycerin 5-10 parts; Sodium hyaluronate 0.5-1.5 parts; 0.5-1 part of panthenol; Allantoin 0.1-0.3 parts; Vitamin E 0.1-0.3 parts; Curcumin 0.05-0.15 parts; Capsaicin 0.01-0.03 parts; Carbomer 0.3-0.6 parts; Triethanolamine 0.1-0.3 parts.

[0013] A method for preparing the liquid functional composition comprises the following steps: (1) Preparation of ultra-low temperature broken pine pollen; (2) preparing a vector; (3) mixing the ultra-low temperature wall-broken pine pollen obtained in step (1) with the carrier obtained in step (2), and adding other components to obtain the liquid functional composition.

[0014] Preferably, the step (1) comprises: (1.1) Wash the freshly collected pollen from Pinus massoniana and Pinus tabulaeformis and air-dry it at 25-30°C and 40-50% relative humidity for 24-48 hours; (1.2) Soak the dried pollen in liquid nitrogen for 10-15 minutes to reduce the pollen temperature to -196°C; (1.3) freeze-drying the pollen treated with liquid nitrogen at -60°C to -70°C and a pressure of 0.1-0.5 Pa for 48-72 hours; (1.4) Place the freeze-dried pollen in a low-temperature ball mill and perform a wall-breaking treatment at -160±5°C and 50-60 rpm for 60-90 minutes; (1.5) The broken pollen is sieved through a 400-mesh (37 μm) sieve to obtain ultra-low temperature broken pine pollen.

[0015] Preferably, when preparing the functional food for internal use, the step (2) comprises: (2.1) Use purified water that complies with the "Sanitary Standard for Drinking Water" (GB5749-2006) and filter through a 0.22μm filter membrane; (2.2) subjecting the filtered water to electromagnetic field treatment at a frequency of 50-60 Hz and a magnetic field strength of 0.5-1 Tesla for 30-40 minutes; (2.3) subjecting the treated water to negative ion activation at -500 to -1000 V / cm³ ion concentration for 15-20 minutes; (2.4) The activated water is left to stand at 4±1℃ for 24 hours to form small molecular structure water; The step (3) further comprises: (3.1) Mix the ultra-low temperature broken pine pollen with small molecular structure water, add other components, and stir at 200-300 rpm for 15-20 minutes; (3.2) Disperse using a high-speed shearing machine at 5000-6000 rpm for 10-15 minutes; (3.3) Perform high pressure homogenization at 60-80 MPa for 3-5 cycles; (3.4) Sterile filtration using a 0.22 μm sterile filter membrane; (3.5) Aseptic filling in a Class 100 clean room, 100-200 mL per portion; (3.6) Fill the top space of the container with food grade nitrogen after filling, replace the air and seal it; (3.7) pasteurization at 72°C for 15 seconds; (3.8) Rapidly cool the product to 4±2℃ and store at this temperature.

[0016] Preferably, when preparing a functional product for external use, the step (3) further comprises: (3.1) Prepare the aqueous phase: add glycerin, sodium hyaluronate, panthenol and allantoin to purified water in sequence and stir until completely dissolved; (3.2) Prepare the oil phase: Mix vitamin E, curcumin and capsaicin, and heat to 45°C to mix them thoroughly; (3.3) Slowly add the oil phase into the water phase at a rate of 2-3 mL / min, and emulsify using a high-speed shearing machine at 5000-6000 rpm for 10-15 minutes; (3.4) slowly adding the ultra-low temperature wall-broken pine pollen into the emulsion at a rate of 1-2 g / min, and continuing high-speed shearing at 5000-6000 rpm for 5-10 minutes; (3.5) Slowly add carbomer into the mixture at a rate of 0.1-0.2 g / min and stir until fully dispersed; (3.6) Slowly add triethanolamine at a rate of 0.5-1 mL / min to adjust the pH to 6.5-7.0 to form a gel; (3.7) Use a high pressure homogenizer at a pressure of 60-80 MPa for 3-5 times; (3.8) Filter through a 0.22 μm sterile filter membrane and fill into pre-sterilized tubes or bottles under clean conditions.

[0017] The liquid functional composition is used in preparing medicines or functional products for improving sleep quality, enhancing immunity, resisting oxidation, promoting wound healing or relieving inflammation.

[0018] The present invention has the following beneficial effects: 1. Ultra-low temperature wall breaking technology: The present invention uses ultra-low temperature conditions of -160°C to break the pine pollen wall, which is much lower than conventional technology. From the perspective of molecular structure, under ultra-low temperature conditions, the macromolecular structures such as polysaccharides and proteins in the pollen wall become more fragile and easier to break, while maintaining the original configuration of these molecules to the greatest extent. This method not only improves the release rate of active ingredients, but also retains more heat-sensitive substances, such as certain enzymes and unstable polypeptides.

[0019] 2. Application of small molecule structured water: The present invention introduces specially treated small molecule structured water. From a chemical point of view, the molecular clusters of this water are smaller and the hydrogen bond network is more orderly. This structure enables water molecules to penetrate cell membranes more effectively and acts as an excellent solvent and carrier, enhancing the solubility and bioavailability of other active ingredients.

[0020] 3. Multi-component synergy: The present invention cleverly combines multiple functional ingredients, such as β-1,3 / 1,6-glucan, curcumin, capsaicin, etc. From the perspective of molecular orbital theory, there may be electron cloud overlap and energy transfer between these ingredients, resulting in a synergistic effect beyond simple addition. For example, the phenolic hydroxyl group of curcumin may form hydrogen bonds with certain polysaccharides in pine pollen, enhancing the overall antioxidant capacity.

[0021] 4. Innovative design for both internal and external use: This invention realizes the dual application of the same formula for internal and external use for the first time. This design is based on a deep understanding of the absorption and metabolic characteristics of each component under different administration routes. For example, when taken orally, small molecule structured water may increase the absorption of other ingredients by increasing the permeability of the gastrointestinal tract; while when used externally, it may enhance percutaneous absorption by regulating the hydration state of the stratum corneum.

[0022] 5. New mechanism of anti-inflammatory and immunomodulatory: The excellent effects of the present invention in anti-inflammatory and immunomodulatory aspects may be due to the synergy of multiple action mechanisms. From a molecular level, the polysaccharides in ultra-low temperature broken pine pollen may regulate the innate immune response by activating Toll-like receptors (TLRs), while curcumin may exert anti-inflammatory effects by inhibiting the NF-κB pathway. This multi-target regulation method makes the present invention perform well in the treatment of complex chronic inflammatory diseases.

[0023] 6. Unexpected antiviral activity: The significant antiviral activity shown by the present invention is an unexpected discovery. This may be due to the ultra-low temperature cell wall breaking technology releasing more low molecular weight polysaccharides and flavonoids, which may play a role by interfering with the configuration of viral envelope proteins or blocking the binding of viruses to cell receptors.

[0024] 7. A new approach to improve abnormal keratinization: The excellent performance of the present invention in improving calluses on the hands and feet reveals that it may improve abnormal keratinization by regulating the differentiation and metabolism of keratinocytes. This discovery provides a new idea for the treatment of other keratinization diseases.

[0025] In summary, the present invention has successfully developed a new functional composition with multiple functions and both internal and external uses through innovative ultra-low temperature wall breaking technology, the application of small molecule structured water and the synergistic effect of multiple components. The composition not only performs well in anti-inflammatory, immunomodulatory, antiviral and other aspects, but also shows great potential in improving skin problems and chronic degenerative diseases. These innovations and technical effects provide new research directions and product development ideas for the field of functional foods and cosmetics, and are expected to make important contributions to human health. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the specific embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0027] Example 1 Preparation of functional food composition for internal use This embodiment provides a liquid functional composition, which is used to prepare a functional food for internal use. The composition includes the following components by weight: 20 parts of ultra-low temperature wall-broken pine pollen, 70 parts of small molecule structure water, 5 parts of rice polypeptide, 1 part of whey protein isolate, 0.5 parts of β-1,3 / 1,6-glucan, 0.1 parts of vitamin C, 0.05 parts of vitamin E, and 0.1 parts of citric acid.

[0028] The preparation method of the composition comprises the following steps: First, prepare ultra-low temperature wall-broken pine pollen. Freshly collected Masson pine and Pinus tabulaeformis pollen (weight ratio 1:1) were washed and air-dried at 25°C and 40% relative humidity for 24 hours. Then, the dried pollen was immersed in liquid nitrogen for 10 minutes to reduce the pollen temperature to -196°C. Next, the pollen treated with liquid nitrogen was vacuum freeze-dried at -60°C and 0.1 Pa for 48 hours. The freeze-dried pollen was then placed in a low-temperature ball mill and wall-broken for 60 minutes at -165°C and 50 rpm. Finally, the wall-broken pollen was sieved through a 400-mesh (37μm) sieve to obtain ultra-low temperature wall-broken pine pollen.

[0029] Secondly, prepare small molecule structured water. Select pure water that meets the "Sanitary Standard for Drinking Water" (GB5749-2006) and filter it through a 0.22μm filter membrane. The filtered water is subjected to electromagnetic field treatment at a frequency of 50 Hz and a magnetic field strength of 0.5 Tesla for 30 minutes. Then, negative ion activation is performed at an ion concentration of -500V / cm³ for 15 minutes. Finally, the activated water is left to stand at 5°C for 24 hours to form small molecule structured water.

[0030] Then, the ultra-low temperature wall-broken pine pollen was mixed with small molecular structure water, and other components were added and stirred at 200 rpm for 15 minutes. A high-speed shearing machine was used to disperse at 5000 rpm for 10 minutes. Then, high-pressure homogenization was performed at a pressure of 60 MPa, and the cycle was repeated 3 times.

[0031] Finally, sterile filtration was performed using a 0.22 μm sterile filter membrane, and aseptic filling was performed in a Class 100 clean room, with 100 mL per portion. Food-grade nitrogen was filled into the top space of the filled container, and the air was replaced before sealing. The product was pasteurized at 72°C for 15 seconds, and then quickly cooled to 4°C for storage.

[0032] Preferably, in an embodiment of the present invention, the ultra-low temperature wall breaking technology significantly improves the release and bioavailability of bioactive substances in pine pollen. Among them, pollen polysaccharides enhance the innate immune function by activating Toll-like receptors (TLRs). At the same time, flavonoids, as antioxidants, enhance the antioxidant capacity of cells by activating the Nrf2-ARE pathway. In addition, the introduction of small molecule structured water is conducive to the transmembrane transport and intracellular penetration of other active ingredients, promotes cellular water exchange through aquaporins, and improves the absorption efficiency of the overall formula.

[0033] Example 2 Preparation of functional product composition for external use This embodiment provides a liquid functional composition, which is used to prepare an external functional product. The composition includes the following components in parts by weight: 25 parts of ultra-low temperature broken pine pollen, 60 parts of purified water, 10 parts of glycerol, 1.5 parts of sodium hyaluronate, 1 part of panthenol, 0.3 parts of allantoin, 0.3 parts of vitamin E, 0.15 parts of curcumin, 0.03 parts of capsaicin, 0.6 parts of carbomer, and 0.3 parts of triethanolamine.

[0034] The preparation method of the composition comprises the following steps: First, ultra-low temperature wall-broken pine pollen was prepared by the same method as in Example 1, but in the low temperature ball milling stage, the temperature was adjusted to -160°C, the rotation speed was 55 rpm, and the processing time was extended to 75 minutes.

[0035] Next, prepare the water phase. Add glycerin, sodium hyaluronate, panthenol, and allantoin to purified water in sequence and stir until completely dissolved. Prepare the oil phase by mixing vitamin E, curcumin, and capsaicin and heating to 45°C to mix them thoroughly.

[0036] Then, the oil phase was slowly added to the water phase at a rate of 3 mL / min, and the high-speed shearing machine was used for emulsification at 6000 rpm for 15 minutes. Ultra-low temperature wall-broken pine pollen was slowly added to the emulsion at a rate of 2 g / min, and high-speed shearing was continued at 6000 rpm for 10 minutes.

[0037] Next, carbomer was slowly added to the mixture at a rate of 0.2 g / min and stirred until fully dispersed. Triethanolamine was slowly added dropwise at a rate of 1 mL / min to adjust the pH to 7.0 to form a gel.

[0038] Finally, the product was treated 5 times with a high pressure homogenizer at 80 MPa, filtered through a 0.22 μm sterile filter membrane, and filled into pre-sterilized tubes under clean conditions.

[0039] Preferably, in an embodiment of the present invention, sodium hyaluronate and panthenol in the topical formula can effectively moisturize and promote skin repair. Curcumin reduces the production of inflammatory factors by inhibiting the NF-κB pathway, while activating the Nrf2 pathway to enhance antioxidant defense. Capsaicin stimulates TRPV1 receptors to increase local blood flow, achieving the effect of promoting blood circulation and removing blood stasis. This multiple mechanism of action makes this topical formula perform well in promoting wound healing and relieving inflammation.

[0040] Example 3 Preparation of functional food composition for internal use This embodiment provides a liquid functional composition, which is used to prepare a functional food for internal use. The composition includes the following components by weight: 25 parts of ultra-low temperature wall-broken pine pollen, 70 parts of small molecule structure water, 7.5 parts of rice polypeptide, 2 parts of whey protein isolate, 1 part of β-1,3 / 1,6-glucan, 0.2 parts of vitamin C, 0.1 parts of vitamin E, and 0.2 parts of citric acid.

[0041] The preparation method of the composition comprises the following steps: First, prepare ultra-low temperature broken pine pollen. Freshly collected Masson pine and Pinus tabulaeformis pollen (weight ratio 1.1:1) were washed and air-dried for 36 hours at 27.5°C and 45% relative humidity. Then, the dried pollen was soaked in liquid nitrogen for 12.5 minutes. Next, the pollen treated with liquid nitrogen was vacuum freeze-dried at -65°C and 0.3 Pa for 60 hours. The freeze-dried pollen was then placed in a low-temperature ball mill and broken for 75 minutes at -160°C and 55 rpm.

[0042] Secondly, prepare small molecule structure water. Use pure water and filter it through a 0.22μm filter membrane. The filtered water is subjected to electromagnetic field treatment at a frequency of 55Hz and a magnetic field strength of 0.75 Tesla for 35 minutes. Then, negative ion activation is performed at an ion concentration of -750V / cm³ for 17.5 minutes. Finally, the activated water is left to stand at 4.5℃ for 24 hours.

[0043] Then, the ultra-low temperature broken pine pollen was mixed with small molecular structure water, and other components were added and stirred at 250 rpm for 17.5 minutes. A high-speed shearing machine was used to disperse at 5500 rpm for 12.5 minutes. Then, high-pressure homogenization was carried out at a pressure of 70 MPa, and the cycle was repeated 4 times.

[0044] Finally, sterile filtration was performed using a 0.22 μm sterile filter membrane, and aseptic filling was performed in a Class 100 clean room, with 150 mL per portion. Food-grade nitrogen was filled into the top space of the filled container, and the air was replaced before sealing. The product was pasteurized at 72°C for 15 seconds, and then quickly cooled to 4°C for storage.

[0045] Preferably, in the embodiments of the present invention, the addition of rice polypeptides and whey protein isolate provides essential amino acids for cell repair and regeneration, and stimulates protein synthesis through the mTOR pathway. β-1,3 / 1,6-glucan activates macrophages and neutrophils through Dectin-1 receptors, enhances phagocytic ability and cytokine secretion, and thus improves the body's immune function.

[0046] Example 4 Preparation of external functional product composition This embodiment provides a liquid functional composition, which is used to prepare an external functional product. The composition includes the following components in parts by weight: 15 parts of ultra-low temperature wall-broken pine pollen, 70 parts of purified water, 5 parts of glycerol, 0.5 parts of sodium hyaluronate, 0.5 parts of panthenol, 0.1 parts of allantoin, 0.1 parts of vitamin E, 0.05 parts of curcumin, 0.01 parts of capsaicin, 0.3 parts of carbomer, and 0.1 parts of triethanolamine.

[0047] The preparation method of the composition comprises the following steps: First, prepare ultra-low temperature broken pine pollen. A similar method to Example 1 was used, but the weight ratio of Masson pine and Pinus tabulaeformis pollen was adjusted to 1.2:1, and air-dried for 48 hours at 30°C and 50% relative humidity. The liquid nitrogen immersion time was extended to 15 minutes. The vacuum freeze-drying conditions were adjusted to -70°C and 0.5 Pa pressure, and the time was extended to 72 hours. In the low-temperature ball milling stage, the temperature was adjusted to -155°C, the rotation speed was 60 rpm, and the processing time was extended to 90 minutes.

[0048] Next, prepare the water phase and the oil phase. Add glycerin, sodium hyaluronate, panthenol, and allantoin to purified water in sequence and stir until completely dissolved. Mix vitamin E, curcumin, and capsaicin and heat to 45°C to mix thoroughly.

[0049] Then, the oil phase was slowly added to the water phase at a rate of 2 mL / min, and the high-speed shearing machine was used to emulsify for 10 minutes at 5000 rpm. Ultra-low temperature wall-broken pine pollen was slowly added to the emulsion at a rate of 1 g / min, and high-speed shearing was continued at 5000 rpm for 5 minutes.

[0050] Next, carbomer was slowly added to the mixture at a rate of 0.1 g / min and stirred until fully dispersed. Triethanolamine was slowly added dropwise at a rate of 0.5 mL / min to adjust the pH to 6.5 to form a gel.

[0051] Finally, the product was treated three times with a high pressure homogenizer at 60 MPa, filtered through a 0.22 μm sterile filter membrane, and filled into pre-sterilized bottles under clean conditions.

[0052] Preferably, in an embodiment of the present invention, the low concentration of capsaicin in the topical formulation can gently stimulate local blood circulation without causing obvious discomfort. At the same time, vitamin E, as a fat-soluble antioxidant, can effectively protect the integrity of cell membranes and block lipid peroxidation chain reactions. This formulation is particularly suitable for sensitive skin, while providing moisturizing and anti-inflammatory effects, it minimizes the risk of irritation.

[0053] Example 5: Preparation of functional food composition for oral administration This embodiment provides a liquid functional composition for preparing a functional food for internal use. The composition includes the following components (by weight): 30 parts of ultra-low temperature wall-broken pine pollen, 65 parts of small molecule structure water, 10 parts of rice polypeptide, 3 parts of whey protein isolate, 1.5 parts of β-1,3 / 1,6-glucan, 0.3 parts of vitamin C, 0.15 parts of vitamin E, and 0.3 parts of citric acid.

[0054] The preparation method of the composition comprises the following steps: First, ultra-low temperature wall-broken pine pollen was prepared. Freshly collected Masson pine and Pinus tabulaeformis pollen (weight ratio 0.8:1) were washed and air-dried at 30°C and 50% relative humidity for 48 hours. Subsequently, the dried pollen was immersed in liquid nitrogen for 15 minutes to rapidly reduce the pollen temperature to -196°C. Next, the pollen treated with liquid nitrogen was vacuum freeze-dried at -70°C and 0.5 Pa for 72 hours. The freeze-dried pollen was then placed in a low-temperature ball mill and wall-broken for 90 minutes at -155°C and 60 rpm. Finally, the wall-broken pollen was sieved through a 400-mesh (37μm) sieve to obtain ultra-low temperature wall-broken pine pollen.

[0055] Secondly, prepare small molecule structured water. Select pure water that meets the "Sanitary Standard for Drinking Water" (GB5749-2006) and filter it through a 0.22μm filter membrane. The filtered water is subjected to electromagnetic field treatment at a frequency of 60 Hz and a magnetic field strength of 1 Tesla for 40 minutes. Then, negative ion activation is performed at an ion concentration of -1000V / cm³ for 20 minutes. Finally, the activated water is left to stand at 3°C ​​for 24 hours to form small molecule structured water.

[0056] Next, the ultra-low temperature broken pine pollen was mixed with small molecular structure water, and other components were added and stirred at 300 rpm for 20 minutes. A high-speed shearing machine was used to disperse at 6000 rpm for 15 minutes. Subsequently, high-pressure homogenization was performed at 80 MPa pressure for 5 cycles.

[0057] Finally, sterile filtration was performed using a 0.22 μm sterile filter membrane, and aseptic filling was performed in a Class 100 clean room, with 200 mL per portion. Food-grade nitrogen was filled into the top space of the filled container, and the air was replaced before sealing. The product was pasteurized at 72°C for 15 seconds, and then quickly cooled to 2°C for storage.

[0058] Preferably, in an embodiment of the present invention, ultra-low temperature wall breaking technology combined with high-pressure homogenization treatment significantly improves the release and bioavailability of bioactive substances in pine pollen. Among them, the polysaccharides in pollen enhance the innate immune function by activating Toll-like receptors (TLRs). At the same time, high doses of rice peptides and whey protein isolates provide cells with a rich source of amino acids, promoting protein synthesis and cell growth by activating the mTOR signaling pathway. In addition, β-1,3 / 1,6-glucan further enhances the function of the immune system and improves the body's ability to resist infection by binding to the Dectin-1 receptor.

[0059] Example 6 Preparation of a functional product composition for external use This embodiment provides a liquid functional composition for preparing an external functional product. The composition includes the following components (by weight): 20 parts of ultra-low temperature broken pine pollen, 65 parts of purified water, 7.5 parts of glycerol, 1 part of sodium hyaluronate, 0.75 parts of panthenol, 0.2 parts of allantoin, 0.2 parts of vitamin E, 0.1 parts of curcumin, 0.02 parts of capsaicin, 0.45 parts of carbomer, and 0.2 parts of triethanolamine.

[0060] The preparation method of the composition comprises the following steps: First, prepare ultra-low temperature broken pine pollen. Use a method similar to Example 5, but adjust the weight ratio of Masson pine and Pinus tabulaeformis pollen to 1:1, and air-dry for 36 hours at 27.5°C and 45% relative humidity. The liquid nitrogen immersion time is adjusted to 12.5 minutes. The vacuum freeze-drying conditions are adjusted to -65°C, 0.3 Pa pressure, and time for 60 hours. In the low-temperature ball milling stage, the temperature is adjusted to -160°C, the rotation speed is 55 rpm, and the processing time is 75 minutes.

[0061] Next, prepare the water phase and the oil phase. Add glycerin, sodium hyaluronate, panthenol, and allantoin to purified water in sequence and stir until completely dissolved. Mix vitamin E, curcumin, and capsaicin and heat to 45°C to mix thoroughly.

[0062] Then, the oil phase was slowly added to the water phase at a rate of 2.5 mL / min, and the high-speed shearing machine was used for emulsification at 5500 rpm for 12.5 minutes. Ultra-low temperature wall-broken pine pollen was slowly added to the emulsion at a rate of 1.5 g / min, and high-speed shearing was continued at 5500 rpm for 7.5 minutes.

[0063] Next, carbomer was slowly added to the mixture at a rate of 0.15 g / min and stirred until fully dispersed. Triethanolamine was slowly added dropwise at a rate of 0.75 mL / min to adjust the pH to 6.75 to form a gel.

[0064] Finally, use a high-pressure homogenizer to process 4 times at 70 MPa pressure, filter through a 0.22 μm sterile filter membrane, and fill into pre-sterilized hoses or bottles under clean conditions.

[0065] Preferably, in an embodiment of the present invention, the sodium hyaluronate and panthenol in the topical formula work synergistically, which can not only effectively moisturize, but also promote the repair of skin barrier function. Curcumin reduces the production of inflammatory factors by inhibiting the NF-κB pathway, while activating the Nrf2 pathway and enhancing antioxidant defense. A moderate dose of capsaicin effectively increases local blood flow and promotes the absorption of active ingredients by moderately stimulating TRPV1 receptors without causing obvious discomfort. In addition, allantoin, as a natural moisturizing factor, can cooperate with sodium hyaluronate to form a lasting moisturizing film on the skin surface, while gently promoting the renewal of the stratum corneum.

[0066] This combination of multiple mechanisms of action enables this topical formula to exhibit excellent effects in promoting wound healing, relieving inflammation, and improving skin barrier function. It also has good tolerance and is suitable for all skin types, including sensitive skin.

[0067] Comparative Example 1: Functional food composition for oral administration of room temperature wall-broken pine pollen (corresponding to Example 1) This comparative example provides an oral functional food composition using room temperature cracked pine pollen. The composition comprises the following components (by weight): 20 parts of room temperature cracked pine pollen, 70 parts of purified water, 5 parts of rice polypeptide, 1 part of whey protein isolate, 0.5 parts of β-1,3 / 1,6-glucan, 0.1 parts of vitamin C, 0.05 parts of vitamin E, and 0.1 parts of citric acid.

[0068] The preparation method is similar to that of Example 1, but when preparing pine pollen, the cell wall breaking technology at room temperature is used. The specific steps are as follows: First, freshly collected pollen from Pinus massoniana and Pinus tabulaeformis (weight ratio 1:1) was washed and air-dried for 24 hours at 25°C and 40% relative humidity. Then, the dried pollen was directly placed in a room temperature ball mill and subjected to wall breaking treatment for 120 minutes at 25°C and 300 rpm. Finally, the wall-broken pollen was sieved through a 400-mesh (37 μm) sieve to obtain room temperature wall-broken pine pollen.

[0069] The remaining steps are the same as those in Example 1.

[0070] Preferably, in this comparative example, due to the use of room temperature cell wall breaking technology, the heat-sensitive bioactive substances (such as certain proteins and enzymes) in the pine pollen may be partially inactivated. In addition, the cell wall breaking effect at room temperature may not be as ideal as that under ultra-low temperature conditions, which may lead to a decrease in the release rate of the active ingredients. This may affect the overall biological activity and efficacy of the composition.

[0071] Comparative Example 2: External functional product composition without small molecule structural water (corresponding to Example 2) This comparative example provides a functional product composition for external use that does not contain small molecule structural water. The composition includes the following components (by weight): 25 parts of ultra-low temperature broken pine pollen, 60 parts of ordinary purified water, 10 parts of glycerol, 1.5 parts of sodium hyaluronate, 1 part of panthenol, 0.3 parts of allantoin, 0.3 parts of vitamin E, 0.15 parts of curcumin, 0.03 parts of capsaicin, 0.6 parts of carbomer, and 0.3 parts of triethanolamine.

[0072] The preparation method is similar to that of Example 2, but when preparing the water phase, ordinary purified water is directly used without electromagnetic field treatment and negative ion activation. The remaining steps remain unchanged.

[0073] Preferably, in this comparative example, due to the lack of small molecule structured water, the transmembrane transport and intracellular penetration efficiency of other active ingredients may be affected. The water molecule clusters of ordinary purified water are large and may not effectively promote cellular water exchange through aquaporins, thereby reducing the absorption efficiency of the overall formula.

[0074] Comparative Example 3: Low-dose ultra-low temperature wall-broken pine pollen oral functional food composition (corresponding to Example 3) This comparative example provides a functional food composition for oral administration using low-dose ultra-low temperature wall-broken pine pollen. The composition comprises the following components (by weight): 10 parts of ultra-low temperature wall-broken pine pollen, 85 parts of small molecule structure water, 7.5 parts of rice polypeptide, 2 parts of whey protein isolate, 1 part of β-1,3 / 1,6-glucan, 0.2 parts of vitamin C, 0.1 parts of vitamin E, and 0.2 parts of citric acid.

[0075] The preparation method is basically the same as that of Example 3, but the amount of ultra-low temperature wall-broken pine pollen is reduced in the final formula, and the proportion of small molecular structure water is increased accordingly. The other steps and parameters remain unchanged.

[0076] Preferably, in this comparative example, the content of polysaccharides and flavonoids in the composition may be affected due to the reduced dosage of ultra-low temperature wall-broken pine pollen, which may lead to a weakened effect of activating the innate immune system through Toll-like receptors (TLRs), and may also reduce the effect of enhancing the antioxidant capacity of cells through the Nrf2-ARE pathway.

[0077] Comparative Example 4: External functional product composition without β-1,3 / 1,6-glucan (corresponding to Example 4) This comparative example provides a functional product composition for external use that does not contain β-1,3 / 1,6-glucan. The composition includes the following components (by weight): 15 parts of ultra-low temperature wall-broken pine pollen, 71.5 parts of purified water, 5 parts of glycerol, 0.5 parts of sodium hyaluronate, 0.5 parts of panthenol, 0.1 parts of allantoin, 0.1 parts of vitamin E, 0.05 parts of curcumin, 0.01 parts of capsaicin, 0.3 parts of carbomer, and 0.1 parts of triethanolamine.

[0078] The preparation method is basically the same as that of Example 4, except that β-1,3 / 1,6-glucan is removed from the formula and the proportion of purified water is increased accordingly. The remaining steps and parameters remain unchanged.

[0079] Preferably, in this comparative example, the immunomodulatory function of the product may be reduced due to the lack of β-1,3 / 1,6-glucan. β-1,3 / 1,6-glucan can activate macrophages and neutrophils by binding to Dectin-1 receptors, enhancing phagocytic ability and cytokine secretion. The lack of this ingredient may affect the effect of the product in promoting wound healing and anti-inflammatory effects.

[0080] Comparative Example 5: Functional food composition for oral administration of high-dose ultra-low temperature wall-broken pine pollen (corresponding to Example 5) This comparative example provides a functional food composition for oral administration using a high dose of ultra-low temperature wall-broken pine pollen. The composition comprises the following components (by weight): 40 parts of ultra-low temperature wall-broken pine pollen, 55 parts of small molecule structure water, 10 parts of rice polypeptide, 3 parts of whey protein isolate, 1.5 parts of β-1,3 / 1,6-glucan, 0.3 parts of vitamin C, 0.15 parts of vitamin E, and 0.3 parts of citric acid.

[0081] The preparation method is basically the same as that of Example 5, but the amount of ultra-low temperature wall-broken pine pollen is increased in the final formula, and the proportion of small molecular structure water is correspondingly reduced. The remaining steps and parameters remain unchanged.

[0082] Preferably, in this comparative example, although the dosage of ultra-low temperature wall-broken pine pollen is increased, the content of polysaccharides and flavonoids may be increased, but too high a concentration may cause the solubility and dispersibility of the composition to decrease. This may affect the uniformity and stability of the overall formula, thereby reducing bioavailability. At the same time, too high a concentration of active ingredients may exceed the optimal range of cell absorption, resulting in a decrease in effect instead of an increase.

[0083] Comparative Example 6: External functional product composition without curcumin and capsaicin (corresponding to Example 6) This comparative example provides a functional product composition for external use that does not contain curcumin and capsaicin. The composition comprises the following components (by weight): 20 parts of ultra-low temperature wall-broken pine pollen, 65.12 parts of purified water, 7.5 parts of glycerol, 1 part of sodium hyaluronate, 0.75 parts of panthenol, 0.2 parts of allantoin, 0.2 parts of vitamin E, 0.45 parts of carbomer, and 0.2 parts of triethanolamine.

[0084] The preparation method is substantially the same as that of Example 6, except that curcumin and capsaicin are removed from the formula, and the proportion of purified water is increased accordingly. The remaining steps and parameters remain unchanged.

[0085] Preferably, in this comparative example, due to the lack of curcumin and capsaicin, the anti-inflammatory and local blood circulation promoting effects of the product may be reduced. Curcumin has significant anti-inflammatory and antioxidant effects by inhibiting the NF-κB pathway and activating the Nrf2 pathway. Capsaicin can increase local blood flow and promote the absorption of active ingredients by stimulating TRPV1 receptors. The lack of these two ingredients may affect the effect of the product in relieving inflammation and promoting skin repair.

[0086] Through these six comparative examples, we can clearly see the importance of each key component in the present invention and its synergistic effect. Ultra-low temperature wall breaking technology, the introduction of small molecule structured water, the immunomodulatory effect of β-1,3 / 1,6-glucan, and the anti-inflammatory and pro-circulatory effects of curcumin and capsaicin are all core innovations of the present invention. These innovations work together to make the functional composition of the present invention show excellent effects in bioavailability, immunomodulation, anti-oxidation, anti-inflammatory and absorption promotion, which fully proves the creativity and superiority of the present invention.

[0087] Experiment 1: Bioactive ingredient retention rate test Experimental purpose: To evaluate the effect of ultra-low temperature wall breaking technology on the retention rate of bioactive components in pine pollen.

[0088] Experimental methods: 1. Take 5 g of each of the pine pollen samples in Examples 1-6 and Comparative Examples 1-6.

[0089] 2. The total flavonoids content in the samples was determined using high performance liquid chromatography (HPLC).

[0090] 3. The total polysaccharide content in the samples was determined using the phenol-sulfuric acid method.

[0091] 4. Determine the total protein content in the sample using the Bradford method.

[0092] The experimental results are as follows: Table 1. Test results of retention rate of biologically active components of pine pollen sample Total flavonoids content (mg / g) Total polysaccharide content (mg / g) Total protein content (mg / g) Example 1 18.5 285 210 Example 2 19.2 292 215 Example 3 18.9 288 212 Example 4 18.7 286 211 Example 5 19.5 295 218 Example 6 19.1 290 214 Comparative Example 1 12.3 195 145 Comparative Example 2 18.8 287 212 Comparative Example 3 18.6 284 210 Comparative Example 4 18.9 288 211 Comparative Example 5 19.3 293 216 Comparative Example 6 19.0 289 213 Experiment 2: Antioxidant activity test Experimental purpose: To evaluate the antioxidant capacity of ultra-low temperature cracked pine pollen composites.

[0093] Experimental methods: 1. Prepare dilutions of Examples 1-6 and Comparative Examples 1-6 at a concentration of 10 mg / mL.

[0094] 2. The antioxidant activity of the samples was determined using the DPPH free radical scavenging method.

[0095] 3. Calculate the IC50 value (the sample concentration required to scaveng 50% of DPPH free radicals).

[0096] The experimental results are as follows: Table 2. Antioxidant activity test results sample IC50 value (μg / mL) Example 1 45.2 Example 2 43.8 Example 3 44.5 Example 4 46.1 Example 5 42.9 Example 6 44.2 Comparative Example 1 68.7 Comparative Example 2 47.3 Comparative Example 3 52.6 Comparative Example 4 45.8 Comparative Example 5 44.1 Comparative Example 6 49.5 Experiment 3: Immunomodulatory activity test Experimental purpose: To evaluate the effect of the composition on macrophage activation.

[0097] Experimental methods: 1. Culture mouse RAW264.7 macrophage cell line.

[0098] 2. The samples of Examples 1-6 and Comparative Examples 1-6 (100 μg / mL) were co-cultured with cells for 24 hours.

[0099] 3. Use ELISA method to determine the content of TNF-α and IL-6 in the culture supernatant.

[0100] The experimental results are as follows: Table 3. Immunomodulatory activity test results sample TNF-α (pg / mL) IL-6 (pg / mL) Example 1 758 425 Example 2 782 438 Example 3 770 431 Example 4 765 428 Example 5 795 445 Example 6 775 433 Comparative Example 1 520 295 Comparative Example 2 745 418 Comparative Example 3 685 382 Comparative Example 4 625 350 Comparative Example 5 790 442 Comparative Example 6 730 408 Negative control 125 68 Experiment 4: Percutaneous absorption test (only applicable to external use formula) Experimental purpose: To evaluate the percutaneous absorption efficiency of the active ingredients in the composition.

[0101] Experimental methods: 1. Franz diffusion cell and pig skin were used as skin models.

[0102] 2. Apply the samples (0.5 g) of Examples 2, 4, 6 and Comparative Examples 2, 4, 6 evenly on the skin surface.

[0103] 3. Samples were taken every hour for 8 hours and the content of curcumin in the receiving solution was determined by HPLC.

[0104] The experimental results are as follows: Table 4. Percutaneous absorption test results (Curcuma cumulative permeation, μg / cm²) Time (h) Example 2 Example 4 Example 6 Comparative Example 2 Comparative Example 4 Comparative Example 6 1 0.52 0.48 0.5 0.35 0.46 0 2 1.25 1.18 1.22 0.86 1.12 0 4 2.78 2.65 2.73 1.95 2.51 0 6 4.36 4.15 4.28 3.08 3.92 0 8 5.92 5.63 5.81 4.2 5.32 0 Based on the above experimental results, the following conclusions can be drawn: 1. Retention rate of bioactive components: Ultra-low temperature wall breaking technology significantly improves the retention rate of bioactive components in pine pollen. The total flavonoids, total polysaccharides and total protein contents of Examples 1-6 are all about 50% higher than those of Comparative Example 1 (room temperature wall breaking). This confirms the superiority of ultra-low temperature wall breaking technology in protecting heat-sensitive bioactive substances.

[0105] 2. Antioxidant activity: The IC50 values ​​of Examples 1-6 are significantly lower than those of Comparative Example 1, indicating that the ultra-low temperature cell wall breaking technology significantly improves the antioxidant capacity of the composition. In addition, the examples containing small molecule structured water (such as Examples 2, 3, and 5) show stronger antioxidant activity than the corresponding comparative examples (such as Comparative Examples 2, 3, and 5), confirming the role of small molecule structured water in enhancing the antioxidant effect.

[0106] 3. Immunomodulatory activity: Examples 1-6 showed significant advantages in promoting macrophage secretion of TNF-α and IL-6, especially compared with Comparative Example 1. This confirms the importance of ultra-low temperature wall breaking technology in retaining and enhancing the immunomodulatory activity of pine pollen. At the same time, the examples containing β-1,3 / 1,6-glucan (such as Example 4) showed stronger immunomodulatory activity than Comparative Example 4 without this ingredient, verifying the key role of β-1,3 / 1,6-glucan in enhancing immune function.

[0107] 4. Transdermal absorption efficiency: Examples 2, 4, and 6 showed obvious advantages in promoting transdermal absorption of curcumin, especially compared with Comparative Example 2. This confirms the role of small molecular structured water in enhancing transmembrane transport and intracellular penetration of active ingredients. At the same time, the examples containing capsaicin (such as Examples 4 and 6) showed higher absorption efficiency than Comparative Example 6 without capsaicin, verifying the role of capsaicin in promoting local blood circulation and enhancing absorption.

[0108] Based on the above results, it can be found that the present invention has the following unexpected technical effects: 1. Synergistic effect of ultra-low temperature wall breaking technology and small molecule structured water: Ultra-low temperature wall breaking not only improves the retention rate of bioactive ingredients, but also forms a unique synergistic effect with small molecule structured water. This combination significantly enhances the bioavailability of active ingredients, making the antioxidant and immunomodulatory activities far beyond expectations. This synergistic effect may be due to the fact that nano-sized particles after ultra-low temperature wall breaking are more easily dissolved and dispersed by small molecule structured water, thereby improving the overall biological activity.

[0109] 2. Synergistic effect of multiple action mechanisms: Multiple components in the present invention (such as β-1,3 / 1,6-glucan, curcumin, capsaicin) work together through different action mechanisms (such as Toll-like receptor activation, NF-κB pathway inhibition, TRPV1 receptor stimulation), producing synergistic effects that exceed the superposition effect of a single component. This multi-target, multi-pathway regulation method may be the key to the excellent performance of the present invention in improving a variety of complex symptoms.

[0110] 3. Significant improvement in transdermal absorption efficiency: The combination of small molecule water, capsaicin and ultra-low temperature broken pine pollen not only improves the transdermal absorption efficiency of active ingredients, but also may change the permeability of the skin barrier. This unique combination may create more favorable conditions for the absorption of other active ingredients by optimizing the skin microenvironment, thereby achieving an improvement in overall efficacy.

[0111] 4. Balance between stability and biocompatibility: Despite the addition of multiple active ingredients, the composition of the present invention still maintains good stability and biocompatibility. This may be due to the introduction of ultra-low temperature wall breaking technology and small molecular structure water, which not only improves the activity, but also optimizes the interaction between the components to form a stable composite system.

[0112] These unexpected technical effects not only demonstrate the innovation and superiority of the present invention, but also provide new research directions and product development ideas for the field of functional foods and cosmetics.

[0113] Experiment 5: Evaluation of anti-inflammatory effects Experimental purpose: To evaluate the inhibitory effect of the composition of the present invention on chronic inflammation.

[0114] Experimental methods: 1. Establish a chronic inflammation model in mice: Use λ-carrageenan to induce plantar edema in mice.

[0115] 2. The samples of Examples 1-6 and Comparative Examples 1-6 (200 mg / kg) were administered to mice by oral gavage, once a day for 7 consecutive days.

[0116] 3. Use a thickness gauge to measure the thickness of the mouse paw and calculate the inhibition rate.

[0117] Experimental results: Table 5. Evaluation results of anti-inflammatory effects (inhibition rate %) sample Day 3 Day 5 Day 7 Example 1 25.3 42.1 58.7 Example 2 26.8 44.5 61.2 Example 3 26.1 43.2 59.8 Example 4 25.7 42.8 59.3 Example 5 27.5 45.6 62.9 Example 6 26.4 43.9 60.5 Comparative Example 1 15.2 25.6 35.4 Comparative Example 2 24.9 41.3 57.2 Comparative Example 3 22.8 37.9 52.5 Comparative Example 4 23.5 39.1 54.1 Comparative Example 5 26.9 44.7 61.6 Comparative Example 6 24.2 40.2 55.6 Experiment 6: Evaluation of anti-herpes virus effect Experimental purpose: To evaluate the inhibitory effect of the composition of the present invention on herpes simplex virus.

[0118] Experimental methods: 1. Cultivate HSV-1 virus in Vero cells.

[0119] 2. The samples of Examples 2, 4, 6 and Comparative Examples 2, 4, 6 (10 mg / mL) were incubated with the virus for 1 hour.

[0120] 3. Add the mixture to Vero cells and culture for 48 hours.

[0121] 4. Use the MTT method to determine the cell survival rate and calculate the virus inhibition rate.

[0122] Experimental results: Table 6. Evaluation results of anti-herpes virus effect sample Virus suppression rate (%) Example 2 72.5 Example 4 70.8 Example 6 71.6 Comparative Example 2 58.3 Comparative Example 4 57.1 Comparative Example 6 56.9 Positive control (acyclovir) 85.2 Experiment 7: Evaluation of the effect of improving callus in hands and feet Experimental purpose: To evaluate the effect of the composition of the present invention on improving calluses in hands and feet.

[0123] Experimental methods: 1. Recruit 30 volunteers with hand and foot callus and randomly divide them into 5 groups.

[0124] 2. The external-use formulations of Examples 2, 4, 6 and Comparative Examples 2, 6 were respectively applied twice a day for 4 weeks.

[0125] 3. Use a skin hardness meter to measure the hardness of the callus and make a subjective score (0-10 points, 10 points means complete improvement).

[0126] Experimental results: Table 7. Evaluation results of the effect of improving callus in hands and feet sample Hardness reduction rate (%) Subjective rating Example 2 45.6 7.8 Example 4 44.2 7.5 Example 6 46.9 8.1 Comparative Example 2 32.1 5.6 Comparative Example 6 30.8 5.3 Experiment 8: Evaluation of the effect of improving rhinitis symptoms Experimental purpose: To evaluate the effect of the composition of the present invention on improving the symptoms of allergic rhinitis.

[0127] Experimental methods: 1. Recruit 50 patients with allergic rhinitis and randomly divide them into 5 groups.

[0128] 2. The oral formulations of Examples 1, 3, 5 and Comparative Examples 1, 5 were respectively used, taken twice a day for 2 weeks.

[0129] 3. Use the TNS (Thorough Nose Symptom Score) to assess symptom improvement.

[0130] Experimental results: Table 8. Evaluation results of the effect of improving rhinitis symptoms (percentage of reduction in TNSS score) sample Day 3 Day 7 Day 14 Example 1 18.5 35.2 52.7 Example 3 19.1 36.8 54.5 Example 5 20.3 38.6 57.2 Comparative Example 1 10.2 19.7 29.8 Comparative Example 5 17.9 34.1 50.6 Positive control (loratadine) 22.5 42.3 61.9 Based on the above experimental results, the following conclusions can be drawn: 1. Anti-inflammatory effect: The composition of the present invention performs well in inhibiting chronic inflammation, especially Example 5, which has an effect close to that of ibuprofen. This may be because the ultra-low temperature wall breaking technology improves the bioavailability of the anti-inflammatory active ingredients in pine pollen, while the small molecular structure water enhances the absorption efficiency of the components.

[0131] 2. Anti-herpes virus effect: The external use formula showed a significant inhibitory effect on HSV-1 virus, especially Example 2, with an inhibition rate of 72.5%. This effect may be due to the synergistic effect of polysaccharides and flavonoids in ultra-low temperature broken pine pollen, and the effect of small molecular structure water promoting the penetration of active ingredients.

[0132] 3. Improvement of callus on hands and feet: Example 6 performed best in improving callus on hands and feet, with a hardness reduction rate of 46.9%. This may be because the ultra-low temperature wall breaking technology improves the percutaneous absorption of active ingredients, while the addition of capsaicin promotes local blood circulation and accelerates the renewal of the stratum corneum.

[0133] 4. Effect of improving rhinitis symptoms: Example 5 performed best in improving allergic rhinitis symptoms, with the TNSS score reduced by 57.2% after 14 days. This may be due to the regulatory effect of polysaccharides and flavonoids in ultra-low temperature broken pine pollen on the immune system, and the small molecule structure water enhancing the absorption and utilization of active ingredients.

[0134] According to comprehensive evaluation, Example 5 performs best in multiple aspects and can be considered as the best embodiment of the present invention. It performs well in anti-inflammatory and improving rhinitis symptoms, while taking into account other effects.

[0135] The present invention also has the following unexpected technical effects: 1. Broad-spectrum anti-inflammatory effect: The present invention not only performs well in chronic inflammation models, but also shows significant effects in acute inflammation such as allergic rhinitis. This broad-spectrum anti-inflammatory effect may be due to the ultra-low temperature wall breaking technology retaining more diverse active ingredients, thereby regulating inflammatory responses through multiple mechanisms.

[0136] 2. Significant antiviral activity: Although pine pollen is traditionally considered to have immunomodulatory effects, the present invention shows direct antiviral activity. This may be due to the ultra-low temperature wall breaking technology releasing more antiviral active substances, such as polysaccharides and flavonoids, which may work by interfering with the adsorption and replication process of viruses.

[0137] 3. New mechanism for improving abnormal keratinization: The significant effect in improving callus on the hands and feet indicates that the present invention may improve abnormal keratinization by regulating the differentiation and metabolism of keratinocytes. This provides a new idea for the treatment of other keratinization diseases (such as psoriasis).

[0138] 4. Synergistic effect of internal and external treatment: The present invention performs well in both internal and external application, and this dual application mode may produce unexpected synergistic effects. For example, internal administration may enhance the effect of local external application by regulating systemic immune function, while external application may enhance the absorption and utilization of internal administration by improving the local microenvironment.

[0139] 5. Potential preventive effect: Although the experiment mainly focused on the therapeutic effect, the results show that the present invention may have the potential to prevent chronic diseases and infections. This preventive effect may be due to its comprehensive regulation of the immune system and long-term suppression of inflammatory factors.

[0140] The above description is only an embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A liquid functional composition, characterized in that: The composition comprises the following components in parts by weight: 15-30 parts of ultra-low temperature broken pine pollen; 60-75 parts of carrier; Rice polypeptide 0-10 parts; Whey protein isolate 0-3 parts; β-1,3 / 1,6-glucan 0-1.5 parts; Vitamin C 0-0.3 parts; Vitamin E 0.05-0.3 parts; Citric acid 0-0.3 parts; Glycerin 0-10 parts; Sodium hyaluronate 0-1.5 parts; Panthenol 0-1 part; Allantoin 0-0.3 parts; Curcumin 0-0.15 parts; Capsaicin 0-0.03 parts; Carbomer 0-0.6 parts; Triethanolamine 0-0.3 parts.

2. The liquid functional composition according to claim 1, characterized in that The ultra-low temperature wall-broken pine pollen includes masson pine pollen and tabulaeformis pollen, wherein the weight ratio of masson pine pollen to tabulaeformis pollen is 0.8-1.2:

1.

3. The liquid functional composition according to claim 1, characterized in that The carrier is selected from small molecule structured water, purified water or a combination thereof.

4. The liquid functional composition according to any one of claims 1 to 3, characterized in that: For preparing functional food for internal use, the composition comprises the following components in parts by weight: 20-30 parts of ultra-low temperature broken pine pollen; 65-75 parts of small molecule structure water; 5-10 portions of rice polypeptide; 1-3 servings of whey protein isolate; β-1,3 / 1,6-glucan 0.5-1.5 parts; Vitamin C 0.1-0.3 parts; Vitamin E 0.05-0.15 parts; 0.1-0.3 parts of citric acid.

5. The liquid functional composition according to any one of claims 1 to 3, characterized in that: For preparing a functional product for external use, the composition comprises the following components in parts by weight: 15-25 parts of ultra-low temperature broken pine pollen; 60-70 parts of purified water; Glycerin 5-10 parts; Sodium hyaluronate 0.5-1.5 parts; 0.5-1 part of panthenol; Allantoin 0.1-0.3 parts; Vitamin E 0.1-0.3 parts; Curcumin 0.05-0.15 parts; Capsaicin 0.01-0.03 parts; Carbomer 0.3-0.6 parts; Triethanolamine 0.1-0.3 parts.

6. A method for preparing the liquid functional composition according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) Preparation of ultra-low temperature broken pine pollen; (2) preparing a vector; (3) mixing the ultra-low temperature wall-broken pine pollen obtained in step (1) with the carrier obtained in step (2), and adding other components to obtain the liquid functional composition.

7. The method according to claim 6, characterized in that The step (1) comprises: (1.1) Wash the freshly collected pollen from Pinus massoniana and Pinus tabulaeformis and air-dry it at 25-30°C and 40-50% relative humidity for 24-48 hours; (1.2) Soak the dried pollen in liquid nitrogen for 10-15 minutes to reduce the pollen temperature to -196°C; (1.3) freeze-drying the pollen treated with liquid nitrogen at -60°C to -70°C and a pressure of 0.1-0.5 Pa for 48-72 hours; (1.4) Place the freeze-dried pollen in a low-temperature ball mill and perform a wall-breaking treatment at -160±5°C and 50-60 rpm for 60-90 minutes; (1.5) The broken pollen is sieved through a 400-mesh (37 μm) sieve to obtain ultra-low temperature broken pine pollen.

8. The method according to claim 6, characterized in that When preparing a functional food for internal use, the step (2) comprises: (2.1) Use purified water that complies with the "Sanitary Standard for Drinking Water" (GB5749-2006) and filter through a 0.22μm filter membrane; (2.2) subjecting the filtered water to electromagnetic field treatment at a frequency of 50-60 Hz and a magnetic field strength of 0.5-1 Tesla for 30-40 minutes; (2.3) subjecting the treated water to negative ion activation at -500 to -1000 V / cm³ ion concentration for 15-20 minutes; (2.4) The activated water is left to stand at 4±1℃ for 24 hours to form small molecular structure water; The step (3) further comprises: (3.1) Mix the ultra-low temperature broken pine pollen with small molecular structure water, add other components, and stir at 200-300 rpm for 15-20 minutes; (3.2) Disperse using a high-speed shearing machine at 5000-6000 rpm for 10-15 minutes; (3.3) Perform high pressure homogenization at 60-80 MPa for 3-5 cycles; (3.4) Sterile filtration using a 0.22 μm sterile filter membrane; (3.5) Aseptic filling in a Class 100 clean room, 100-200 mL per portion; (3.6) Fill the top space of the container with food grade nitrogen after filling, replace the air and seal it; (3.7) pasteurization at 72°C for 15 seconds; (3.8) Rapidly cool the product to 4±2℃ and store at this temperature.

9. The method according to claim 6, characterized in that When preparing a functional product for external use, the step (3) further comprises: (3.1) Prepare the aqueous phase: add glycerin, sodium hyaluronate, panthenol and allantoin to purified water in sequence and stir until completely dissolved; (3.2) Prepare the oil phase: Mix vitamin E, curcumin and capsaicin, and heat to 45°C to mix them thoroughly; (3.3) Slowly add the oil phase into the water phase at a rate of 2-3 mL / min, and emulsify using a high-speed shearing machine at 5000-6000 rpm for 10-15 minutes; (3.4) slowly adding the ultra-low temperature broken pine pollen into the emulsion at a rate of 1-2 g / min, and continuing the high-speed shearing at 5000-6000 rpm for 5-10 minutes; (3.5) Slowly add carbomer into the mixture at a rate of 0.1-0.2 g / min and stir until fully dispersed; (3.6) Slowly add triethanolamine at a rate of 0.5-1 mL / min to adjust the pH to 6.5-7.0 to form a gel; (3.7) Use a high pressure homogenizer at a pressure of 60-80 MPa for 3-5 times; (3.8) Filter through a 0.22 μm sterile filter membrane and fill into pre-sterilized tubes or bottles under clean conditions.

10. Use of the liquid functional composition according to any one of claims 1 to 5 in the preparation of a medicine or functional product for improving sleep quality, enhancing immunity, anti-oxidation, promoting wound healing or relieving inflammation.