An antioxidant health composition and method of making the same

Abstract

The application belongs to the technical field of health food, and provides an antioxidant health composition and a preparation method thereof.The raw materials of the antioxidant health composition include whey protein powder, fish collagen peptide, vitamin E, pyrroloquinoline quinone disodium salt, aronia melanocarpa extract, grape seed oligomeric proanthocyanidin powder, triglyceride, soybean lecithin, malt dextrin and erythritol.The preparation method comprises the following steps: (1) preparing an oil phase liquid; (2) preparing a nano lipid core suspension; (3) preparing a protein wall material liquid; (4) preparing a pre-emulsified liquid; (5) preparing microcapsule particles; and (6) obtaining the product.The health composition is prepared by scientifically compounding water-soluble and fat-soluble antioxidant components, constructing a multi-pathway synergistic antioxidant system, combining an optimized nano-embedding and low-temperature forming preparation process, and solving the technical problems of single antioxidant effect, easy inactivation of active components, poor storage stability, and low in-vivo absorption and utilization rate of existing products, so that a functional health composition with wide-spectrum antioxidant effect, excellent stability and high bioavailability is prepared.

Description

Technical Field

[0001] This invention belongs to the field of health food technology, specifically relating to an antioxidant health care composition and its preparation method. Background Technology

[0002] Oxidative stress is a common physiological phenomenon in the body's normal metabolic processes. When the body is stimulated by the external environment or affected by its own metabolic disorders, a large number of free radicals are produced, including reactive oxygen species such as superoxide anions, hydroxyl radicals, and peroxyl radicals. Excessive reactive oxygen species cannot be promptly eliminated by the body's own antioxidant system and will continuously attack cellular lipids, proteins, nucleic acids, and other biomolecules, triggering a series of problems such as lipid peroxidation, cellular oxidative damage, and metabolic disorders. This leads to a decline in the body's antioxidant capacity, reduced cell activity, and physiological metabolic imbalance, making it a significant contributing factor to various sub-health conditions. Therefore, dietary intervention to supplement with highly effective, stable, and easily absorbed antioxidant active ingredients to eliminate excess free radicals, alleviate oxidative stress damage, and maintain the body's redox balance has become a research hotspot in the field of functional nutritional foods.

[0003] Currently, the formulation systems of conventional antioxidant nutritional foods on the market are relatively simple, mostly adding only a single polyphenol, vitamin, or protein ingredient. This results in a single antioxidant pathway, making it difficult to achieve multi-dimensional free radical scavenging effects and limiting overall antioxidant activity. Furthermore, existing products generally suffer from insufficient scientific compatibility of raw materials, lacking synergistic effects between various active ingredients and failing to fully leverage the antioxidant advantages of complex ingredients. More significantly, the preparation processes of existing antioxidant foods are relatively crude, often employing conventional mixing and ordinary high-temperature spray drying processes, merely achieving simple physical mixing of raw materials.

[0004] On the one hand, heat-sensitive and fat-soluble antioxidant active ingredients such as vitamin E and plant polyphenols are extremely sensitive to temperature, oxygen, and light. They are prone to oxidative degradation and activity loss during conventional high-temperature preparation and storage, resulting in low raw material retention and poor product storage stability. On the other hand, simple physical mixing systems cannot effectively protect fat-soluble active ingredients, which are easily destroyed by stomach acid and digestive juices, exhibiting poor dispersibility and low absorption and utilization in the body, significantly reducing the in vivo efficacy of antioxidants. Furthermore, the plant extracts used in commercially available products are mostly prepared using traditional crude extraction processes, resulting in high impurity content and low purity of effective active ingredients, further limiting the overall antioxidant performance of the products.

[0005] In summary, existing antioxidant nutritional foods generally suffer from technical defects such as a single antioxidant pathway, poor stability of active ingredients, high loss of heat-sensitive components, and low bioavailability in vivo, making it difficult to meet the current consumer demand for highly efficient, stable, and highly absorbable antioxidant nutritional foods.

[0006] Given the numerous technical challenges mentioned above, developing a health-care composition based on protein powder that combines high stability, high bioavailability, and significant antioxidant effects has become an urgent technical problem to be solved in this field. Summary of the Invention

[0007] To address the aforementioned shortcomings in existing technologies, the present invention aims to provide an antioxidant health care composition and its preparation method. This invention scientifically combines water-soluble and fat-soluble antioxidant components to construct a multi-pathway synergistic antioxidant system. Combined with optimized nano-encapsulation and low-temperature molding processes, it solves the technical problems of existing products, such as limited antioxidant effects, easy inactivation of active components, poor storage stability, and low in vivo absorption and utilization. The result is a functional health care composition with broad-spectrum antioxidant properties, excellent stability, and high bioavailability.

[0008] To achieve the above objectives, the solution adopted by the present invention is as follows: An antioxidant health care composition, comprising the following raw materials by weight: 60-90 parts whey protein powder, 15-25 parts fish collagen peptides with a molecular weight less than 2000 Da, 10-20 parts vitamin E, 0.3-1 part disodium pyrroloquinoline quinone, 4-9 parts black chokeberry extract with an anthocyanin content of ≥25%, 2-5 parts grape seed oligomeric proanthocyanidins powder with an anthocyanin purity of ≥95%, 10-15 parts triglycerides, 2-4 parts soybean lecithin, 10-15 parts maltodextrin, and 3-5 parts erythritol.

[0009] A method for preparing the above-mentioned antioxidant health care composition includes: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve, and preparing an oil phase liquid; (2) homogenizing the oil phase liquid by high pressure microfluidic jet to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, black chokeberry extract, and grape seed oligomeric proanthocyanidins to purified water, stirring and dispersing, and obtaining a protein wall material liquid; (4) adding the nano lipid core suspension to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) drying the pre-emulsified liquid by electrostatic spraying to obtain microcapsule particles; (6) freeze-drying the microcapsule particles and then mixing them with erythritol to obtain the final product.

[0010] The beneficial effects of the antioxidant health care composition and its preparation method provided by this invention are: (1) The antioxidant health care composition provided by the present invention has scientifically selected raw materials with significant synergistic effects. Among them, the combination of fast and slow absorption proteins formed by separating whey protein and fish collagen peptides can quickly provide the body with nitrogen source and amino acid substrate, promote muscle protein synthesis, and at the same time target the repair of connective tissues such as skin, blood vessels and mucous membranes. Vitamin E and disodium pyrroloquinoline quinone form a highly efficient synergistic effect at the mitochondrial level. The former directly removes mitochondrial free radicals and repairs respiratory chain damage, while the latter strongly promotes mitochondrial biosynthesis and increases membrane potential. The combination of the two significantly improves ATP production efficiency. The combination of black chokeberry extract and grape seed oligomeric proanthocyanidins can efficiently remove free radicals and inhibit oxidative stress. The present application achieves a four-in-one full-chain antioxidant effect of structural repair, energy supply, oxidation removal and cell purification through the mutual promotion and complementary effects between the above three action pathways. It provides antioxidant protection from multiple levels of the body, tissues, cells and molecules. The overall efficacy is far superior to health care compositions with single ingredients or conventional simple mixtures. (2) The method for preparing the antioxidant health care composition provided by the present invention adopts a double-layer microencapsulation process, which encapsulates the fat-soluble active ingredients with a nano lipid core and uses a protein complex as the outer wall material to form microcapsule particles with uniform particle size and stable structure. On the one hand, it can completely isolate the damage of heat-sensitive and easily oxidized ingredients to external factors such as oxygen, light, moisture, and high temperature, significantly reduce the degradation and inactivation of active ingredients during storage, transportation, and placement, and greatly extend the shelf life and effective use period of the product. On the other hand, it can protect the active ingredients to safely pass through the gastric acid environment, avoid the degradation and destruction of functional substances by strong acids and digestive enzymes, achieve precise intestinal positioning and efficient absorption, significantly reduce the first-pass metabolic loss of the liver, greatly improve the bioavailability of key functional ingredients in vivo, and at the same time improve the solubility, dispersibility and sensory quality of the product, avoid problems such as layering, precipitation, and wall adhesion, and make the health care composition more suitable for long-term oral administration and daily consumption. It solves a series of common problems in the industry such as poor stability, poor absorption, weak efficacy and poor taste in the prior art. Attached Figure Description

[0011] Figure 1 This is a process flow diagram of the preparation method of the antioxidant health care composition provided in Experimental Example 1 of the present invention. Detailed Implementation

[0012] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0013] The following is a detailed description of an antioxidant health care composition and its preparation method provided by an embodiment of the present invention.

[0014] An antioxidant health care composition, comprising the following raw materials by weight: 60-90 parts whey protein powder (GlanbiaNutritionals, Provon® 290 WPI), 15-25 parts fish collagen peptides (Weishardt, Naticol® Fish 1000) with a molecular weight less than 2000 Da, 10-20 parts vitamin E (VegeToc®, VE-1430), 0.3-1 part disodium pyrroloquinoline quinone, 4-9 parts black chokeberry extract with an anthocyanin content of ≥25%, 2-5 parts grape seed oligomeric proanthocyanidins powder with an anthocyanin purity of ≥95%, 10-15 parts triglycerides, 2-4 parts soybean lecithin, 10-15 parts maltodextrin, and 3-5 parts erythritol (Shandong Dongxiao Biotechnology Co., Ltd., food-grade erythritol). The preferred composition is as follows: 80 parts whey protein powder, 20 parts fish collagen peptide, 15 parts vitamin E, 0.5 parts disodium pyrroloquinoline quinone, 6 parts black chokeberry extract, 4 parts grape seed oligomeric proanthocyanidins, 12 parts triglycerides, 3 parts soybean lecithin, 12 parts maltodextrin, and 4 parts erythritol.

[0015] This application uses raw materials within the above-mentioned specific ratio range, which can produce a synergistic effect and have a significant antioxidant effect.

[0016] In this application, the preparation method of black chokeberry extract includes: taking mature black chokeberry fruit, washing and drying it until the moisture content is less than 6%, pulverizing it and passing it through a 60-mesh sieve to obtain black chokeberry fruit powder; adding 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20, adjusting the pH to 3.5-4.0, and extracting it twice with ultrasonic assistance at 45℃ for 30 min at an ultrasonic power of 250W, and combining the extracts; filtering it through a plate and frame filter, concentrating it under reduced pressure at 45℃ until there is no alcohol odor, purifying it with AB-8 macroporous resin at a flow rate of 1.5 mL / min, washing it with water to remove impurities, eluting it with 70% ethanol, collecting the eluent, concentrating it under reduced pressure, and then freeze-drying it to obtain black chokeberry extract powder.

[0017] This method is simple and controllable, and can prepare anthocyanin content greater than or equal to 25% of black chokeberry extract.

[0018] In this application, the preparation method of grape seed oligomeric proanthocyanidins includes: removing impurities from grape seeds, drying them, pulverizing them through a 60-mesh sieve, defatting them twice with petroleum ether under reflux for 30 minutes each time, evaporating the solvent to obtain defatted grape seed powder; adding 65% ethanol aqueous solution at a material-to-liquid ratio of 1:15, extracting at 50℃ for 40 minutes, extracting twice, and combining the extracts; filtering and concentrating under reduced pressure to remove ethanol, purifying by adsorption with AB-8 macroporous resin, washing with water to remove impurities, eluting with 60% ethanol, collecting the eluent, concentrating under reduced pressure, and vacuum drying to obtain grape seed oligomeric proanthocyanidin powder.

[0019] This operation method is simple and controllable, and can prepare grape seed oligomeric proanthocyanidin powder with an anthocyanin purity of ≥95%.

[0020] This application also provides a method for preparing the above-mentioned antioxidant health care composition, comprising: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve, and preparing an oil phase liquid; (2) subjecting the oil phase liquid to high-pressure microfluidic homogenization and circulation treatment at a pressure of 1600-2000 bar for 2-4 times to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, black chokeberry extract, and grape seed oligomeric proanthocyanidins to purified water, stirring and dispersing, to obtain a protein wall material liquid; (4) adding the nano lipid core suspension to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) subjecting the pre-emulsified liquid to electrostatic spray drying at a feed flow rate of 4-6 mL / min and a voltage of 12-18 kV to obtain microcapsule particles; (6) subjecting the microcapsule particles to a pre-freezing temperature of - Freeze-dry at 40 to -50°C under a vacuum of 15 Pa for 20 to 30 hours, then mix with erythritol to obtain the final product.

[0021] According to the preparation method under the specific technical conditions described above in this application, by employing a double-layer microcapsule encapsulation process, a lipid-soluble active ingredient is encapsulated with a nano-lipid core, and a protein complex is used as the outer wall material, resulting in microcapsule particles with uniform particle size and stable structure, ranging from 300 to 500 nm.

[0022] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0023] Example 1 This embodiment provides an antioxidant health care composition, the raw materials of which include, by weight: 80 parts whey protein powder, 20 parts fish collagen peptides with a molecular weight of less than 2000 Da, 15 parts vitamin E, 0.5 parts disodium pyrroloquinoline quinone, 6 parts black chokeberry extract with an anthocyanin content of greater than or equal to 25%, 4 parts grape seed oligomeric proanthocyanidins with an anthocyanin purity of greater than or equal to 95%, 12 parts triglycerides, 3 parts soybean lecithin, 12 parts maltodextrin, and 4 parts erythritol; In this embodiment, the preparation method of black chokeberry extract includes: taking mature black chokeberry fruit, washing and drying it until the moisture content is less than 6%, pulverizing it through a 60-mesh sieve to obtain black chokeberry fruit powder; adding 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20, adjusting the pH to 3.8, and extracting it twice with ultrasonic assistance at 45℃ for 30 min at an ultrasonic power of 250W, and combining the extracts; filtering the extract through a plate and frame filter, concentrating it under reduced pressure at 45℃ until there is no alcohol odor, purifying it with AB-8 macroporous resin at a loading flow rate of 1.5 mL / min, washing it with water to remove impurities, eluting it with 70% ethanol, collecting the eluent, concentrating it under reduced pressure, and then freeze-drying it to obtain black chokeberry extract powder; In this application, the preparation method of grape seed oligomeric proanthocyanidins includes: removing impurities from grape seeds, drying them, pulverizing them through a 60-mesh sieve, defatting them twice with petroleum ether under reflux for 30 minutes each time, evaporating the solvent to obtain defatted grape seed powder; adding 65% ethanol aqueous solution at a material-to-liquid ratio of 1:15, extracting at 50℃ for 40 minutes, extracting twice, and combining the extracts; filtering and concentrating under reduced pressure to remove ethanol, purifying by adsorption with AB-8 macroporous resin, washing with water to remove impurities, eluting with 60% ethanol, collecting the eluent, concentrating under reduced pressure, and vacuum drying to obtain grape seed oligomeric proanthocyanidin powder; This embodiment also provides a method for preparing the above-mentioned antioxidant health care composition, the process flow diagram of which is shown below. Figure 1 As shown, the specific steps include: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve, and preparing an oil phase liquid; (2) subjecting the oil phase liquid to high-pressure micro-jet homogenization and circulation treatment at a pressure of 1800 bar three times to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, black chokeberry extract, and grape seed oligomeric proanthocyanidins to purified water, stirring and dispersing, and obtaining a protein wall material liquid; (4) adding the nano lipid core suspension to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) subjecting the pre-emulsified liquid to electrostatic spray drying at a feed flow rate of 5 mL / min and a voltage of 16 kV to obtain microcapsule particles; (6) freezing the microcapsule particles at a pre-freezing temperature of -45℃ and a vacuum degree of less than or equal to 15 Pa for 25 h, and then mixing them with erythritol to obtain the final product.

[0024] Example 2 This embodiment provides an antioxidant health care composition and its preparation method. The difference from Embodiment 1 is that the raw materials, by weight, include: 60 parts whey protein powder, 25 parts fish collagen peptide with a molecular weight of less than 2000 Da, 10 parts vitamin E, 1 part disodium pyrroloquinoline quinone, 4 parts black chokeberry extract with an anthocyanin content of greater than or equal to 25%, 5 parts grape seed oligomeric proanthocyanidin powder with an anthocyanin purity of greater than or equal to 95%, 10 parts triglycerides, 4 parts soybean lecithin, 10 parts maltodextrin, and 5 parts erythritol.

[0025] Example 3 This embodiment provides an antioxidant health care composition and its preparation method. The difference from Embodiment 1 is that the raw materials, by weight, include: 90 parts whey protein powder, 15 parts fish collagen peptide with a molecular weight of less than 2000 Da, 20 parts vitamin E, 0.3 parts disodium pyrroloquinoline quinone, 9 parts black chokeberry extract with an anthocyanin content of greater than or equal to 25%, 2 parts grape seed oligomeric proanthocyanidin powder with an anthocyanin purity of greater than or equal to 95%, 15 parts triglycerides, 2 parts soybean lecithin, 15 parts maltodextrin, and 3 parts erythritol.

[0026] Example 4 This embodiment provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method includes: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve, and preparing an oil phase liquid; (2) subjecting the oil phase liquid to high-pressure microfluidic homogenization and circulation treatment at a pressure of 1600 bar for 4 times to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, black chokeberry extract, and grape seed oligomeric proanthocyanidins to purified water, stirring and dispersing, to obtain a protein wall material liquid; (4) adding the nano lipid core suspension to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) subjecting the pre-emulsified liquid to electrostatic spray drying at a feed flow rate of 4 mL / min and a voltage of 18 kV to obtain microcapsule particles; (6) freeze-drying the microcapsule particles at a pre-freezing temperature of -40°C and a vacuum degree of less than or equal to 15 Pa for 30 h, and then mixing with erythritol to obtain the final product.

[0027] Example 5 This embodiment provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method includes: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve, and preparing an oil phase liquid; (2) subjecting the oil phase liquid to high-pressure microfluidic homogenization and circulation treatment at a pressure of 2000 bar twice to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, black chokeberry extract, and grape seed oligomeric proanthocyanidins to purified water, stirring and dispersing, and obtaining a protein wall material liquid; (4) adding the nano lipid core suspension to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) subjecting the pre-emulsified liquid to electrostatic spray drying at a feed flow rate of 6 mL / min and a voltage of 12 kV to obtain microcapsule particles; (6) freeze-drying the microcapsule particles at a pre-freezing temperature of -50°C and a vacuum degree of less than or equal to 15 Pa for 20 h, and then mixing with erythritol to obtain the final product.

[0028] Comparative Example 1 This comparative example provides an antioxidant health care composition, the raw materials of which, by weight, include: 60 parts whey protein powder, 20 parts fish collagen peptides (Shanxi Baichuan Biotechnology, ordinary hydrolyzed fish collagen peptides) with a molecular weight of 2000-5000 Da, 1.5 parts vitamin C, 0.5 parts vitamin E, 0.3 parts zinc gluconate, 3 parts grape seed extract, 12 parts maltodextrin, 0.2 parts edible flavor, and 0.5 parts magnesium stearate; The preparation of grape seed extract includes: taking grape seed raw material, removing impurities, washing and drying at 60℃, pulverizing and passing through a 40-mesh sieve; adding 40% ethanol aqueous solution at a material-to-liquid ratio of 1:10, and refluxing and extracting twice at 60℃ for 60 minutes each time, combining the extracts; filtering and concentrating under reduced pressure to remove ethanol, and directly spray drying the concentrate to obtain grape seed extract powder. This comparative example also provides a method for preparing the above-mentioned antioxidant health care composition, including: (1) passing whey protein powder, collagen peptide and maltodextrin through an 80-mesh sieve respectively; (2) weighing each raw material according to the formula and placing them in a mixing tank; (3) putting them into a three-dimensional motion mixer and mixing for 20 minutes at a speed of 15 r / min to simply mix them; (4) drying them with hot air at 55℃ for 30 minutes, with the moisture content controlled at ≤5%; (5) passing them through a 60-mesh sieve to remove lumps, and thus obtaining the product.

[0029] Comparative Example 2 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the raw materials, by weight, include: 50 parts whey protein powder, 30 parts fish collagen peptide with a molecular weight of less than 2000 Da, 5 parts vitamin E, 1.5 parts disodium pyrroloquinoline quinone, 3 parts black chokeberry extract with an anthocyanin content of greater than or equal to 25%, 6 parts grape seed oligomeric proanthocyanidin powder with an anthocyanin purity of greater than or equal to 95%, 8 parts triglycerides, 5 parts soybean lecithin, 8 parts maltodextrin, and 6 parts erythritol.

[0030] Comparative Example 3 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method of the black chokeberry extract includes: taking mature black chokeberry fruits, washing and drying them until the moisture content is below 6%, pulverizing them through a 60-mesh sieve to obtain black chokeberry fruit powder; adding 50% ethanol aqueous solution at a material-to-liquid ratio of 1:15, adjusting the pH to 3, and extracting twice at 50℃ with ultrasonic assistance for 25 min at an ultrasonic power of 280W, combining the extracts; filtering by plate and frame filter, concentrating under reduced pressure at 50℃ until no alcohol odor remains, purifying with AB-8 macroporous resin at a loading flow rate of 1 mL / min, washing with water to remove impurities, eluting with 80% ethanol, collecting the eluent, concentrating under reduced pressure, and then freeze-drying to obtain black chokeberry extract powder.

[0031] Comparative Example 4 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method of grape seed oligomeric proanthocyanidins includes: removing impurities from grape seeds, drying them, pulverizing them through a 60-mesh sieve, defatting them twice with petroleum ether for 30 minutes each time, evaporating the solvent to obtain defatted grape seed powder; adding 70% ethanol aqueous solution at a material-to-liquid ratio of 1:20, extracting at 45℃ for 60 minutes, extracting twice, and combining the extracts; filtering and concentrating under reduced pressure to remove ethanol, purifying by adsorption with AB-8 macroporous resin, washing with water to remove impurities, eluting with 55% ethanol, collecting the eluent, concentrating under reduced pressure, and vacuum drying to obtain grape seed oligomeric proanthocyanidin powder.

[0032] Comparative Example 5 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method includes: (1) weighing each raw material according to the formula and placing it in a mixing tank; (3) putting it into a three-dimensional motion mixer and mixing for 20 minutes at a speed of 15 r / min to simply mix it; (4) drying it with hot air at 55℃ for 30 minutes and controlling the moisture content to ≤5%; (5) passing it through a 60-mesh sieve to remove lumps, and the product is obtained.

[0033] Comparative Example 6 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method includes: (1) adding vitamin E, disodium pyrroloquinoline quinone, and soybean lecithin to triglycerides, heating and stirring to dissolve them, and preparing an oil phase liquid; (2) subjecting the oil phase liquid to high-pressure microfluidic homogenization and circulation treatment at a pressure of 1500 bar 5 times to obtain a nano lipid core suspension; (3) adding whey protein powder, fish collagen peptide, maltodextrin, and black fruit gland Chokeberry extract and grape seed oligomeric proanthocyanidins were added to purified water and stirred to disperse, thus obtaining a protein wall material liquid; (4) the nano lipid core suspension was added dropwise to the protein wall material liquid for pre-emulsification, thus obtaining a pre-emulsified liquid; (5) the pre-emulsified liquid was electrostatically spray-dried at a feed flow rate of 3 mL / min and a voltage of 20 kV to obtain microcapsule particles; (6) the microcapsule particles were freeze-dried at a pre-freezing temperature of -55℃ and a vacuum degree of 20 Pa for 10 h, and then mixed with erythritol to obtain the final product.

[0034] Comparative Example 7 This comparative example provides an antioxidant health care composition and its preparation method. The difference from Example 1 is that the preparation method includes: mixing all raw materials and adding them to purified water, stirring continuously at room temperature (25°C) and stirring speed (300 r / min) for 60 min; using a high-pressure homogenizer to process once at a pressure of 40 bar; setting the inlet air temperature to 185°C, the outlet air temperature to 90°C, and the feed flow rate to 20 mL / min, and directly spray drying to obtain powder; mixing the dried powder with erythritol and passing it through an 80-mesh sieve to obtain the final product.

[0035] Experiment Example 1: Stability Testing Vitamin E retention (%) of the antioxidant health care compositions provided in Examples 1-5 and Comparative Examples 1-7: According to GB 5009.82-2016 "National Food Safety Standard - Determination of Vitamins A, D and E in Food": the samples were stored at 25℃±2℃ under light-proof and sealed conditions for 6 months. Samples were taken at the beginning and end of the storage period, extracted with anhydrous ethanol by ultrasonication, and then detected by HPLC after centrifugation and filtration.

[0036] Chromatographic conditions: C18 column (4.6 mm × 250 mm, 5 μm), mobile phase methanol:water = 95:5 (V / V), flow rate 1.0 mL / min, detection wavelength 292 nm, column temperature 30 ℃, external standard method for quantification, vitamin E retention rate was calculated as follows: vitamin E retention rate (%) = (vitamin E content after 6 months of storage ÷ initial vitamin E content) × 100%, results are shown in Table 1.

[0037] Table 1 As shown in Table 1, the vitamin E retention rates of Examples 1-5 are high, indicating that the formulation and preparation process of this application provide the best protection for the active ingredients. Comparative Example 7, using conventional stirring and ordinary high-temperature spray drying, caused the most severe damage to vitamin E, resulting in the lowest retention rate. Comparative Example 1, using a common formulation and process, also showed a significantly low retention rate. Comparative Example 2 used a formulation outside the protection scope of this embodiment, and Comparative Example 6 used process parameters outside the scope of this embodiment, resulting in a significant decrease in stability. Comparative Examples 3-4 used extraction processes outside the scope, and Comparative Example 5 only used simple physical mixing, also leading to a significant decrease in stability. These results indicate that the formulation composition, extract preparation process, double-layer microencapsulation, and low-temperature drying process of this application form a synergistic protective effect, significantly improving the storage stability of the antioxidant active components.

[0038] Example 2 Antioxidant Performance Test Test the DPPH free radical scavenging rate (%) of the antioxidant health care compositions provided in Examples 1-5 and Comparative Examples 1-7: Referring to GB / T 39100-2020 "Determination of Antioxidant Activity of Peptides - DPPH and ABTS Methods": Prepare a 0.2 mmol / L DPPH anhydrous ethanol solution and store it in the dark for later use; take 2.0 mL of the sample solution to be tested in a test tube, add 2.0 mL of freshly prepared DPPH solution, and vortex thoroughly to mix; react at room temperature in the dark for 30 min; use a UV-Vis spectrophotometer to measure the absorbance value at a wavelength of 517 nm, and record it as A1; simultaneously prepare a blank group: 2.0 mL sample solution + 2.0 mL anhydrous ethanol, measure the absorbance, and record it as A0; control group: 0.0 mL distilled water + 2.0 mL DPPH solution, measure the absorbance, and record it as A2; calculate the DPPH free radical scavenging rate according to the following formula: DPPH free radical scavenging rate (%) = [1-(A1-A0) / A2] × 100%, the results are shown in Table 2; Intracellular ROS scavenging rate (%) of the antioxidant health care compositions provided in Examples 1-5 and Comparative Examples 1-7 was tested using the DCFH-DA fluorescent probe method: Logarithmic growth phase human embryonic lung fibroblasts (WI-38) were seeded at an appropriate density in 96-well culture plates and cultured at 37 ℃ in a 5% CO2 incubator for 24 h until cell adhesion. The original culture medium was discarded, and complete culture medium containing different concentrations of the test sample was added, and the cells were cultured for another 24 h. Except for the normal control group, H2O2 working solution was added to the other groups to induce oxidative damage, and incubation was continued. The culture medium was aspirated, and the cells were washed twice with PBS buffer. 10 μmol / L DCFH-DA fluorescent probe was added, and the cells were incubated at 37 ℃ in the dark for 20–30 min. The probe solution was discarded, and the cells were washed twice with PBS. The fluorescence intensity was measured using a microplate reader: excitation wavelength 488 nm, emission wavelength 525 nm. The intracellular ROS scavenging rate was calculated using the following formula: Intracellular ROS scavenging rate (%) = [1-(F1-F0) / (F2-F0)] ×100%, where: F1 - fluorescence intensity of the sample group; F0 - fluorescence intensity of the normal control group; F2 - fluorescence intensity of the model group. The results are shown in Table 2. Table 2 As shown in Table 2, the DPPH free radical scavenging rate and intracellular ROS scavenging rate of Examples 1-5 were relatively high, indicating that the formulation and process within the scope of protection of this application can achieve good antioxidant effects. In this application, there is a significant synergistic antioxidant effect among the dual-protein component, mitochondrial activating component, black chokeberry extract, and grape seed oligomeric proanthocyanidins, with the overall effect far exceeding the sum of the effects of each individual component. Comparative Example 1 used a common formulation, Comparative Example 7 used a conventional high-temperature process, Comparative Example 2's formulation was outside the scope, Comparative Examples 3-4's extract preparation processes were outside the scope, Comparative Example 5 used only physical mixing, and Comparative Example 6's process parameters were outside the scope. Their antioxidant capacity all showed varying degrees of reduction, further demonstrating that the raw material components, extract quality, and preparation process parameters of this application produced a synergistic effect, enabling the product to achieve high-efficiency antioxidant effects.

[0039] Example 3 The maximum blood concentration of vitamin E in the antioxidant health care compositions provided in Examples 1-5 and Comparative Examples 1-7 was determined as follows: (1)Experimental animals and grouping: SPF - level healthy SD rats, male, weighing 180 - 220 g, animal license number: SYXK(Beijing)2022 - 0018; Rearing environment: temperature 22±2°C, relative humidity 50%±10%, 12h / 12h light - dark cycle, free access to water. After 7 days of adaptive feeding, the experiment was started; The rats were randomly divided into 12 groups, namely Example 1 - 5 groups and Comparative Example 1 - 7 groups, with 6 rats in each group. Before the experiment, the rats were fasted for 12 h and had free access to water.

[0040] (2)Administration method and dosage: Each group was given the corresponding sample by gavage at a dose of 100 mg / kg·bw, and the gavage volume was 1.0 mL / 100 g body weight. During the administration period, the rats were normally fasted and were allowed to eat uniformly 4 h after administration.

[0041] (3)Blood sampling time points: Before administration (0 h) and at 0.5, 1, 2, 4, 6, 8, 12, 24 h after administration, 0.5 mL of blood was taken from the retinal venous plexus and placed in a heparin - sodium anticoagulant centrifuge tube. After centrifugation at 3000 r / min for 10 min, the upper - layer plasma was separated and stored at - 20 °C in the dark for further measurement.

[0042] (4)Plasma sample pretreatment method: Take 200 μL of plasma sample and place it in a 1.5 mL centrifuge tube. Add 400 μL of absolute ethanol, vortex for 3 min to fully precipitate proteins; Then add 600 μL of n - hexane, vortex for 5 min to extract vitamin E in the plasma; Centrifuge at 10000 r / min for 10 min, aspirate the upper - layer n - hexane phase and place it in a centrifuge tube, and dry it under nitrogen at 40 °C; The residue was re - dissolved with 100 μL of mobile phase, vortexed for 2 min, centrifuged at 12000 r / min for 15 min, and the supernatant was taken for HPLC detection.

[0043] (5)HPLC detection conditions: C18 chromatographic column (4.6 mm×250 mm, 5 μm), mobile phase methanol: water = 95:5 (V / V), flow rate 1.0 mL / min, detection wavelength 292 nm, column temperature 30 °C; Injection volume: 20 μL; Detection method: external standard method.

[0044] (6)Standard curve preparation: Accurately weigh the vitamin E reference substance, and prepare standard working solutions with concentrations of 0.1, 0.5, 1, 5, 10, 20 μg / mL using the mobile phase. Inject and detect according to the above HPLC conditions. Taking the reference substance concentration as the abscissa and the peak area as the ordinate, draw the standard curve, calculate the regression equation and the correlation coefficient, and require R 2 ≥0.999.

[0045] (7) Data processing: Calculate the plasma vitamin E concentration at each time point according to the standard curve. Plot a plasma concentration-time curve with time as the x-axis and plasma drug concentration as the y-axis. Read the maximum plasma drug concentration Cmax for each group. Using Comparative Example 1 as the reference group (100%), calculate the relative bioavailability (F) according to the following formula: Relative bioavailability F (%) = (AUC of test drug) / (AUC of test drug) / (AUC of test drug) / AUC of test drug ... 0-24 / Reference drug AUC 0-24 The result is shown in Table 3: (1) × 100%. Table 3 As shown in Table 3, the maximum plasma concentration (Cmax) of vitamin E in Examples 1-5 reached 186.4 ng / mL, with a relative bioavailability of 196.0%, indicating excellent in vivo absorption and utilization. This demonstrates that the nano-encapsulation and low-temperature molding process of this invention can maximize the protection of fat-soluble vitamin E from gastric acid degradation, significantly improving the in vivo dissolution and absorption efficiency of the active ingredient.

[0046] Comparative Example 1 used a standard formulation, and Comparative Example 7 used conventional high-temperature spray drying. The formulation of Comparative Example 2 was out of range, the extract processing of Comparative Examples 3-4 was out of range, Comparative Example 5 used only physical mixing, and the process parameters of Comparative Example 6 were out of range. The absorption efficiency of Comparative Examples 1-7 was reduced to varying degrees. The results indicate that the formulation composition, extract quality, double-layer microencapsulation, and low-temperature drying process of this application can synergistically improve the in vivo bioavailability of antioxidant active ingredients, ensuring that the composition exerts a stable and efficient antioxidant effect in vivo.

[0047] In summary, the antioxidant health care composition provided by this invention scientifically combines water-soluble and fat-soluble antioxidant components to construct a multi-pathway synergistic antioxidant system. Combined with optimized nano-encapsulation and low-temperature molding processes, it solves the technical problems of existing products, such as single antioxidant effects, easy inactivation of active components, poor storage stability, and low in vivo absorption and utilization. This results in a functional health care composition with broad-spectrum antioxidant properties, excellent stability, and high bioavailability. The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. An antioxidant health care composition, characterized in that: The raw materials, by weight, include: 60-90 parts whey protein powder, 15-25 parts fish collagen peptides with a molecular weight of less than 2000 Da, 10-20 parts vitamin E, 0.3-1 parts disodium pyrroloquinoline quinone, 4-9 parts black chokeberry extract with an anthocyanin content of ≥25%, 2-5 parts grape seed oligomeric proanthocyanidin powder with an anthocyanin purity of ≥95%, 10-15 parts triglycerides, 2-4 parts soybean lecithin, 10-15 parts maltodextrin, and 3-5 parts erythritol.

2. The antioxidant health care composition according to claim 1, characterized in that: By weight, the whey protein powder comprises 80 parts, the fish collagen peptide comprises 20 parts, the vitamin E comprises 15 parts, the disodium pyrroloquinoline quinone comprises 0.5 parts, the black chokeberry extract comprises 6 parts, the grape seed oligomeric proanthocyanidins comprises 4 parts, the triglycerides comprises 12 parts, the soybean lecithin comprises 3 parts, the maltodextrin comprises 12 parts, and the erythritol comprises 4 parts.

3. The antioxidant health care composition according to claim 1, characterized in that: The preparation method of the black chokeberry extract includes: taking mature black chokeberry fruits, washing and drying them until the moisture content is less than 6%, pulverizing them and passing them through a 60-mesh sieve to obtain black chokeberry fruit powder; adding 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20, adjusting the pH to 3.5-4.0, and extracting twice with ultrasonic assistance at 45℃ for 30 min at an ultrasonic power of 250W, and combining the extracts; filtering by plate and frame filter, concentrating under reduced pressure at 45℃ until no alcohol odor is detected, purifying with AB-8 macroporous resin at a flow rate of 1.5 mL / min, washing with water to remove impurities, eluting with 70% ethanol, collecting the eluent, concentrating under reduced pressure, and then freeze-drying to obtain the black chokeberry extract powder.

4. The antioxidant health care composition according to claim 1, characterized in that: The preparation method of the grape seed oligomeric proanthocyanidins includes: removing impurities from grape seeds, drying them, pulverizing them through a 60-mesh sieve, defatting them twice with petroleum ether for 30 minutes each time, evaporating the solvent to obtain defatted grape seed powder; adding 65% ethanol aqueous solution at a material-to-liquid ratio of 1:15, extracting at 50℃ for 40 minutes, extracting twice, and combining the extracts; filtering and concentrating under reduced pressure to remove ethanol, purifying by adsorption with AB-8 macroporous resin, washing with water to remove impurities, eluting with 60% ethanol, collecting the eluent, concentrating under reduced pressure, and vacuum drying to obtain the grape seed oligomeric proanthocyanidins powder.

5. The antioxidant health care composition according to claim 1, characterized in that: The health care composition has a double-layer microcapsule structure, with the inner layer using a fat-soluble nano-lipid core and the outer layer using a water-soluble protein composite wall material.

6. The antioxidant health care composition according to claim 5, characterized in that: The particle size of the health care composition is 300-500 nm.

7. A method for preparing an antioxidant health care composition according to any one of claims 1-6, characterized in that: include: (1) The vitamin E, the disodium pyrroloquinoline quinone, and the soybean lecithin were added to the triglyceride, heated and stirred to dissolve, and an oil phase liquid was prepared. (2) The oil phase liquid is homogenized by high pressure microfluidic jet to obtain a nano lipid core suspension; (3) Add the whey protein powder, the fish collagen peptide, the maltodextrin, the black chokeberry extract, and the grape seed oligomeric proanthocyanidins to purified water, stir and disperse to obtain a protein wall material solution; (4) The nano lipid core suspension is added dropwise to the protein wall material liquid for pre-emulsification to obtain a pre-emulsified liquid; (5) The pre-emulsion is electrostatically spray-dried to obtain microcapsule particles; (6) The microcapsule particles are freeze-dried and then mixed with erythritol to obtain the final product.

8. The method for preparing the antioxidant health care composition according to claim 7, characterized in that: In step (2), the high-pressure microjet pressure is 1600-2000 bar, and the process is repeated 2-4 times.

9. The method for preparing the antioxidant health care composition according to claim 7, characterized in that: In step (5), the electrostatic spray voltage is 12-18kV and the feed flow rate is 4-6mL / min.

10. The method for preparing the antioxidant health care composition according to claim 7, characterized in that: In step (6), the freeze-drying conditions are: pre-freezing temperature of -40 to -50℃, vacuum degree of less than or equal to 15Pa, and drying time of 20-30h.

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