Anti-aging composition containing dihydromyricetin and preparation method thereof

Abstract

The invention relates to the field of health-care products, and discloses an anti-aging composition containing dihydromyricetin, which comprises the following components in percentage by weight: 0.02-0.06% of dihydromyricetin, 0.02-0.06% of dihydromyricetin, 0.02-0.06% of dihydromyricetin, 0.02-0.06% of 0.20%-0.30% of a trifoliate orange seed extract; 0.10% to 0.16% of a coast pine bark extract; 0.02% to 0.06% of haematococcus pluvialis; 0.06% to 0.10% of an aronia extract; 0.02%-0.06% of a dendrobium officinale flower extract; 0.30% to 0.40% of acerola cherry powder; 0.06%-0.10% of an emblic leafflower fruit extract; and the content of the erythritol is 10.00%-12.00%. The multiple active components in the composition act together, positive influences can be generated on multiple physiological functions, dihydromyricetin shows beneficial potential in the aspect of regulating metabolic balance, and multi-dimensional regulation of an organism is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of health care products, in particular to an anti-aging composition containing dihydromyricetin and a preparation method thereof. Background Art

[0002] Currently, changes in global demographics and the evolution of modern lifestyles are posing unprecedented challenges to human health. Environmental exposure, poor dietary habits, and psychological stress are constantly inducing oxidative stress within the body, leading to the accumulation of damage at the cellular and molecular levels, accelerating physiological decline and causing a series of chronic health issues. Against this backdrop, consumer demand is growing for dietary supplements that combine anti-aging, metabolic regulation, and multidimensional physiological support, with a particular preference for naturally derived, safe active ingredients.

[0003] Traditionally, the market has relied on single synthetic chemical ingredients or unrefined natural extracts to address these health issues. For example, early antioxidants were mostly synthetic. While they possessed direct free radical scavenging capabilities, potential long-term safety risks and compatibility issues with biological systems gradually emerged, limiting their application. Natural plant extracts, on the other hand, are considered to have mild and broad health benefits due to their complex and diverse chemical composition. However, existing technologies utilizing these natural ingredients often face challenges that hinder their full potential. While some existing natural plant extracts, such as common grape seed extract or green tea extract, have demonstrated some antioxidant activity and are used in health products, their mechanisms of action often focus on providing exogenous antioxidants to scavenge free radicals or modulate inflammatory responses through specific pathways. However, these solutions based on a single or limited number of active ingredients often limit their effectiveness to specific targets. When faced with complex, multi-factorial physiological imbalances, such as metabolic disorders, the comprehensive skin aging process (involving oxidation, inflammation, collagen loss, and other mechanisms), and the multiple discomforts experienced during a woman's specific menstrual cycle, single ingredients or simply superimposed formulas struggle to achieve comprehensive and profound regulatory effects. This limited breadth of action makes them inadequate in addressing multi-dimensional health challenges and fails to meet consumers' expectations for multi-target, synergistic health interventions. Summary of the Invention

[0004] In view of the deficiencies in the prior art, the present invention provides an anti-aging composition containing dihydromyricetin and a preparation method thereof, which solves the problems of existing natural active ingredients in single efficacy, low bioavailability, poor stability and insufficient synergistic effect of multiple components.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: an anti-aging composition containing dihydromyricetin, comprising the following components in percentage by weight: Dihydromyricetin: 0.02%-0.06%; Citrus aurantium fruit extract: 0.20%-0.30%; Maritime pine bark extract: 0.10% to 0.16%; Haematococcus pluvialis: 0.02% to 0.06%; Aronia extract: 0.06%-0.10%; Dendrobium officinale flower extract: 0.02%~0.06%; Acerola powder: 0.30% to 0.40%; Emblica officinalis extract: 0.06%-0.10%; Erythritol: 10.00%-12.00%; Citric acid: 0.20% to 0.40%; Stevia powder: 0.02% to 0.10%; Grape juice concentrate: 2.00% to 10.00%; Blackcurrant juice concentrate: 2.00% to 10.00%; and the balance of water.

[0006] A method for preparing an anti-aging composition comprises the following steps: a) preparing a base liquid, comprising mixing and dissolving a portion of water with a first group of solid and / or liquid components; b) adding the active ingredient in stages, comprising adding the second set of solid and / or liquid ingredients to the base liquid in batches under specific temperature and stirring conditions; c) processing and homogenizing of specific active ingredients, including pre-dispersion of specific active ingredients and homogenization of the mixture; d) system control and fine mixing, including adjusting the pH value of the mixed solution and adding the remaining amount of water before homogenizing the entire solution; e) Sterile filtration and packaging, which includes fine filtering of the obtained composition, and filling and sealing under a controlled environment.

[0007] Preferably, the first group of solid and / or liquid ingredients in step a) includes erythritol, citric acid and stevia powder.

[0008] Preferably, the amount of pure water used in step a) is 75% to 85% of the total water volume, and the mixed dissolution is carried out at a temperature of 20° C. to 25° C. and supplemented with stirring at 50 rpm to 100 rpm.

[0009] Preferably, the second group of solid and / or liquid ingredients in step b) includes grape juice concentrate, blackcurrant juice concentrate, acerola cherry powder, emblica bud extract, dihydromyricetin, aurantium dulcis fruit extract, maritime pine bark extract, aronia berry extract and Dendrobium officinale flower extract.

[0010] Preferably, in the step b), the temperature is controlled at 20° C. to 25° C., and after adding each second component, the stirring speed is 100 rpm to 200 rpm, and the stirring time is 10 minutes to 20 minutes.

[0011] Preferably, the specific active ingredient in step c) is Haematococcus pluvialis; the pre-dispersion treatment includes ultrasonic treatment with a frequency of 20kHz to 40kHz and a treatment time of 5 minutes to 15 minutes; the pressure of the homogenization treatment is 50bar to 200bar, and the number of cycles is 2 to 5 times.

[0012] Preferably, the pH value in step d) is adjusted to a range of 3.0 to 5.0; the pressure of the overall homogenization treatment is 80 bar to 200 bar, and the cycle time is 10 minutes to 20 minutes.

[0013] Preferably, the fine filtration in step e) uses a 0.2 μm to 0.45 μm microporous filter membrane.

[0014] Preferably, the controlled environment in step e) is a low-oxygen environment, which includes pre-purging the container with an inert gas before filling and quickly sealing the container after filling.

[0015] The present invention provides an anti-aging composition containing dihydromyricetin and a preparation method thereof. It has the following beneficial effects: 1. The present invention, through the synergistic action of multiple active ingredients in this composition, can positively impact multiple physiological functions. Dihydromyricetin demonstrates beneficial potential in regulating metabolic balance; simultaneously, other plant extracts (such as Dendrobium officinale flower extract and Phyllanthus emblica extract) help improve the skin microenvironment and regulate specific physiological functions. Through the synergistic action of multiple ingredients, the present invention achieves multi-dimensional regulation of the body.

[0016] 2. This invention achieves a significant synergistic effect through the optimized ratio of multiple natural antioxidant ingredients. This synergistic formula enables the combination to exhibit superior activity compared to a single antioxidant. The potent antioxidant capacity helps effectively scavenge free radicals in the body and reduce oxidative stress levels. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 Schematic diagram of the process steps of the present invention. DETAILED DESCRIPTION

[0018] The following will clearly and completely describe the technical solution of the present invention in conjunction with the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0019] Please see the attached Figure 1 The embodiment of the present invention provides an anti-aging composition containing dihydromyricetin, comprising the following components by weight percentage: Dihydromyricetin: 0.02%-0.06%; Citrus aurantium fruit extract: 0.20%-0.30%; Maritime pine bark extract: 0.10% to 0.16%; Haematococcus pluvialis: 0.02% to 0.06%; Aronia extract: 0.06%-0.10%; Dendrobium officinale flower extract: 0.02%~0.06%; Acerola powder: 0.30% to 0.40%; Emblica officinalis extract: 0.06%-0.10%; Erythritol: 10.00%-12.00%; Citric acid: 0.20% to 0.40%; Stevia powder: 0.02% to 0.10%; Grape juice concentrate: 2.00% to 10.00%; Blackcurrant juice concentrate: 2.00% to 10.00%; and the balance of water.

[0020] An anti-aging composition containing dihydromyricetin comprises the following steps: a) Preparing a base liquid, comprising mixing and dissolving a portion of water with a first group of solid and / or liquid ingredients; the first group of solid and / or liquid ingredients includes erythritol, citric acid, and stevia powder, with purified water accounting for 75% to 85% of the total water volume, and the mixed dissolution is carried out at a temperature of 20° C. to 25° C. and with stirring at 50 rpm to 100 rpm.

[0021] b) adding the active ingredients in stages, comprising sequentially adding a second group of solid and / or liquid ingredients to the base liquid under specific temperature and stirring conditions; the second group of solid and / or liquid ingredients comprising grape juice concentrate, blackcurrant juice concentrate, acerola cherry powder, emblica fruit extract, dihydromyricetin, aconitum citrus fruit extract, maritime pine bark extract, aronia berry extract, and Dendrobium officinale flower extract. The temperature is controlled at 20°C to 25°C, and after each addition of the second group of ingredients, the stirring speed is 100-200 rpm for 10-20 minutes.

[0022] c) processing and homogenizing the special active ingredient, including pre-dispersion of the specific active ingredient and homogenization with the mixed solution; the specific active ingredient is Haematococcus pluvialis; the pre-dispersion treatment includes ultrasonic treatment at a frequency of 20 kHz to 40 kHz, a treatment time of 5 minutes to 15 minutes, and a homogenization pressure of 50 bar to 200 bar, with a number of cycles of 2 to 5 times.

[0023] d) System control and fine mixing, including adjusting the pH of the mixed solution and adding the remaining water before overall homogenization; the pH value is adjusted to a range of 3.0 to 5.0; the overall homogenization pressure is 80 bar to 200 bar, and the cycle time is 10 minutes to 20 minutes.

[0024] e) aseptic filtration and packaging, comprising fine filtration of the resulting composition, and filling and sealing under a controlled environment, wherein the fine filtration utilizes a 0.2 μm to 0.45 μm microporous filter membrane in a low-oxygen controlled environment, and comprises pre-purging the container with an inert gas before filling, and rapidly sealing the container after filling.

[0025] Example 1: This example aims to demonstrate a standard formula of an anti-aging oral composition containing dihydromyricetin and its preparation process.

[0026] Composition formula: Preparation steps: To prepare the aqueous base: Pour approximately 75.0% purified water into a stainless steel mixing tank. Maintain the water temperature at 22°C. Start a low-speed agitator at 80 rpm.

[0027] Dissolve the excipients: Slowly add 11.00% erythritol, 0.30% citric acid, and 0.05% stevia powder. Stir continuously for approximately 25 minutes to ensure complete dissolution and form a clear base solution.

[0028] Concentrate blending: Under the same temperature and stirring conditions, add 6.00% grape juice concentrate and 6.00% blackcurrant juice concentrate in sequence. Mix for about 18 minutes to ensure uniform flavor.

[0029] Add and disperse the active ingredients in batches: Maintain the temperature at 22°C. First, add 0.35% acerola cherry powder and 0.08% emblica extract. Stir at 120 rpm for 15 minutes.

[0030] Then, slowly add 0.04% dihydromyricetin, 0.25% aurantium dulcis fruit extract, 0.13% maritime pine bark extract, 0.08% aronia berry extract, and 0.04% dendrobium officinale flower extract one by one. Stir each ingredient for approximately 15 minutes at 150 rpm to ensure thorough dispersion.

[0031] Pretreatment and homogenization of Haematococcus pluvialis: 0.04% of Haematococcus pluvialis was pre-dispersed in a small amount of pure water (about 1% of the total water volume) using an ultrasonic processor at a frequency of 30 kHz for 8 minutes.

[0032] The pre-dispersed liquid was added to the main mixing tank. Then, it was circulated and homogenized by a homogenizer with a homogenization pressure of 100 bar and circulated 3 times to ensure that the astaxanthin particles were uniform and stable.

[0033] pH Adjustment and Water Addition: Measure the pH of the mixture and carefully add 5% citric acid solution dropwise to adjust the pH to 3.8. Once adjusted, add the remaining purified water to the total weight. Continue stirring at a moderate speed (80 rpm) for approximately 15 minutes to ensure uniformity.

[0034] Fine Filtration and Hypoxic Filling: The composition is finely filtered through a 0.45μm microporous membrane. The filtered product is immediately transferred to the hypoxic filling system. Prior to filling, the interior of the oral solution bottle is pre-purged with food-grade nitrogen and quickly sealed after filling.

[0035] Example 2: This example aims to demonstrate a composition formulation with a higher active ingredient content and adopts more stringent process parameters to further ensure the stability and bioavailability of the active ingredient.

[0036] Composition formula: Ingredient name Weight percentage (%) Dihydromyricetin 0.06 Citrus aurantium extract 0.30 Maritime pine bark extract 0.16 Haematococcus pluvialis 0.06 Aronia Extract 0.10 Dendrobium officinale flower extract 0.06 Acerola powder 0.40 Emblica officinalis extract 0.10 erythritol 12.00 Citric acid 0.40 Stevia powder 0.10 Grape juice concentrate 10.00 Blackcurrant juice concentrate 10.00 purified water Remaining capacity (approximately 65.26) Preparation steps: Aqueous base preparation: 80.0% pure water, temperature strictly controlled at 20°C. Stir at low speed, 50 rpm.

[0037] Dissolve the following excipients: 12.00% erythritol, 0.40% citric acid, and 0.10% stevia powder. Stir and dissolve for 35 minutes.

[0038] Mix in the following juice concentrates: 10.00% grape juice concentrate, 10.00% blackcurrant juice concentrate. Mix for 22 minutes.

[0039] Batch addition and dispersion of active ingredients: Maintain the temperature at 20°C. First, add 0.40% acerola powder and 0.10% emblica extract. Stir at 180 rpm for 20 minutes.

[0040] Then, slowly add 0.06% dihydromyricetin, 0.30% Citrus aurantium fruit extract, 0.16% maritime pine bark extract, 0.10% aronia berry extract, and 0.06% Dendrobium officinale flower extract one by one, stirring at 200 rpm for 18 minutes after each addition.

[0041] Pretreatment and homogenization of Haematococcus pluvialis: 0.06% Haematococcus pluvialis is pre-dispersed in a small amount of pure water (about 0.8% of the total water volume) using a high shear emulsifier.

[0042] Add the pre-dispersed liquid into the main tank and homogenize in a circulating homogenizer at a pressure of 180 bar for 5 cycles.

[0043] pH Adjustment and Water Addition: Measure the pH and fine-tune to 4.2 with 1% sodium hydroxide solution. Add the remaining purified water. Homogenize at high speed, at 150 bar, for 18 minutes.

[0044] Fine filtration and hypoxic filling: The composition is sterile filtered through a 0.2μm microporous filter membrane. Hypoxic filling is performed under nitrogen protection, and the container is pre-purged with nitrogen before filling.

[0045] Example 3: This example explores how to achieve product performance at a lower active ingredient content through an optimized preparation process. Ingredient name Weight percentage (%) Dihydromyricetin 0.02 Citrus aurantium extract 0.20 Maritime pine bark extract 0.10 Haematococcus pluvialis 0.02 Aronia Extract 0.06 Dendrobium officinale flower extract 0.02 Acerola powder 0.30 Emblica officinalis extract 0.06 erythritol 10.00 Citric acid 0.20 Stevia powder 0.02 Grape juice concentrate 2.00 Blackcurrant juice concentrate 2.00 purified water Remaining amount (about 84.96)

[0046] Preparation steps: Aqueous base preparation: approximately 85.0% purified water, temperature 25° C. Stirring speed 100 rpm.

[0047] Dissolve the following excipients: 10.00% erythritol, 0.20% citric acid, and 0.02% stevia powder. Stir and dissolve for 20 minutes.

[0048] Mix in the following juice concentrates: 2.00% grape juice concentrate, 2.00% blackcurrant juice concentrate. Mix for 15 minutes.

[0049] Batch addition and dispersion of active ingredients: Maintain the temperature at 25°C. First add 0.30% acerola powder and 0.06% emblica extract. Stir at 100 rpm for 10 minutes.

[0050] Then, slowly add 0.02% dihydromyricetin, 0.20% Citrus aurantium fruit extract, 0.10% maritime pine bark extract, 0.06% aronia berry extract, and 0.02% Dendrobium officinale flower extract one by one, stirring at 120 rpm for 10 minutes each time.

[0051] Pretreatment and homogenization of Haematococcus pluvialis: 0.02% Haematococcus pluvialis was pre-dispersed in a small amount of pure water (about 1.5% of the total water volume) using an ultrasonic processor at a frequency of 25 kHz for 5 minutes.

[0052] Add the pre-dispersed liquid into the main tank and homogenize in a circulating homogenizer at a pressure of 60 bar for 2 cycles.

[0053] pH fine-tuning and water addition: Measure the pH and fine-adjust to 3.5 with 10% citric acid solution. Add the remaining purified water. Homogenize at medium speed, 100 bar, and circulate for 10 minutes.

[0054] Fine filtration and low-oxygen filling: The composition is filtered through a 0.45μm microporous membrane and filled in a low-oxygen environment.

[0055] Comparative Example 1: This comparative example is intended to demonstrate the importance of the synergistic effect of the specific active ingredients of the present invention. The preparation process is consistent with Example 1, but the core anti-aging active ingredient is missing.

[0056] Composition formula: Preparation steps: The preparation steps are basically the same as the "Preparation Steps" of Example 1, with the only difference being that in step 4, "dihydromyricetin, Citrus aurantium extract, maritime pine bark extract, Haematococcus pluvialis, Aronia berry extract, and Dendrobium officinale flower extract" are not added, and only acerola cherry powder and emblica fruit extract are added. All other process parameters and operating procedures remain the same as in Example 1.

[0057] Comparative Example 2: This comparative example is intended to compare the necessity of "adding the active ingredient in stages" in the present invention, using a traditional one-time simple mixing method. Its formulation is the same as that of Example 1.

[0058] Composition formula: exactly the same as "3.1.1 Composition formula" in Example 1.

[0059] Preparation steps: To prepare the aqueous base and dissolve the excipients: Take approximately 75.0% purified water at 22°C. Stir at a low speed of 80 rpm. Add erythritol, citric acid, and stevia powder all at once and stir for approximately 25 minutes until dissolved.

[0060] Combine all ingredients at once: Add all remaining ingredients to the base solution: grape juice concentrate, blackcurrant juice concentrate, dihydromyricetin, aurantium dulcis fruit extract, maritime pine bark extract, Haematococcus pluvialis (untreated), aronia berry extract, Dendrobium officinale flower extract, acerola cherry powder, and emblica bud extract. Increase the stirring speed to 200 rpm and continue stirring for 60 minutes, ensuring that the mixture is thoroughly mixed.

[0061] pH adjustment and water addition: Measure the pH of the mixture and adjust it to 3.8 with 5% citric acid solution. Add the remaining purified water to the total weight. Stir at 80 rpm for approximately 15 minutes.

[0062] Simple filtration and conventional filling: The composition is filtered through a 0.45 μm microporous membrane. The filtered product is filled and sealed under normal air environment without hypoxia protection.

[0063] Comparative Example 3: This comparative example is intended to highlight the importance of pre-dispersion and homogenization of the fat-soluble active ingredient (such as Haematococcus pluvialis) in the present invention. Its formulation is the same as that of Example 1.

[0064] Composition formula: exactly the same as the “composition formula” of Example 1.

[0065] Preparation steps: The preparation steps are basically the same as those in Example 1, but the key points are: Step 5 (Haematococcus pluvialis treatment): Omit the ultrasonic pre-dispersion and subsequent homogenization of the Haematococcus pluvialis. Add 0.04% Haematococcus pluvialis powder directly to the mixture from Step 4 and continue mixing with conventional stirring (150 rpm) for approximately 20 minutes without any homogenization.

[0066] All other process parameters and operation procedures are the same as those in Example 1.

[0067] Comparative Example 4: This comparative example aims to demonstrate the importance of low-oxygen environment filling for product stability, especially for the protection of oxidizable active ingredients. The formula is the same as that of Example 1.

[0068] Composition formula: exactly the same as the “composition formula” of Example 1.

[0069] Preparation steps: The preparation steps are basically the same as those in Example 1, except that the hypoxic filling environment is eliminated. The filtered product is filled and sealed in a normal air environment (without nitrogen pre-purge).

[0070] All other process parameters and operation procedures are the same as those in Example 1.

[0071] Comparative Example 5: pH Not Adjusted (Control Process Invention Point: System Control and pH Adjustment During Fine Mixing) This comparative example is intended to illustrate the importance of precise pH adjustment for product stability and preservation of active ingredients. The formulation is the same as in Example 1.

[0072] Composition formula: exactly the same as the “composition formula” of Example 1.

[0073] Preparation steps: The preparation steps are basically the same as those in "3.1.2 Preparation Steps" of Example 1, but the key points are: No pH adjustment is performed. After all ingredients are mixed, add the remaining purified water to the total weight and stir the entire mixture for uniformity (80 rpm for approximately 15 minutes). The final pH of the composition will be determined by the natural pH of the ingredients.

[0074] All other process parameters and operation procedures are the same as those in Example 1.

[0075] Experiment 1: Evaluation of the antioxidant capacity of the composition: Experimental Purpose: To evaluate the in vitro scavenging abilities of the oral anti-aging compositions prepared in Examples 1, 2, and 3, compared to Comparative Example 1 (a formulation without a specific active ingredient) and Comparative Example 2 (a simple, random mixing process). This experiment aimed to demonstrate the synergistic effects of the compositions and the contribution of the optimized process to maintaining activity.

[0076] Sample preparation: Samples of Example 1, Example 2, and Example 3.

[0077] Comparative Example 1 (no special active ingredient formula) sample.

[0078] Comparative Example 2 (disordered simple mixing process) sample.

[0079] Positive control: freshly prepared 100 μg / mL vitamin C (ascorbic acid) aqueous solution, 50 μg / mL resveratrol ethanol solution.

[0080] Negative control: purified water.

[0081] All samples were appropriately diluted before use to ensure that the absorbance was within the detection range and could be effectively compared.

[0082] Reagent preparation: DPPH solution: Accurately weigh DPPH and prepare a 0.2 mmol / L stock solution with anhydrous ethanol. Dilute to the working concentration (about 0.1 mmol / L) before use and store in the dark.

[0083] ABTS solution: Accurately weigh ABTS and potassium persulfate, prepare with purified water, mix thoroughly, and activate in a dark place at room temperature for 12-16 hours. Before use, dilute with purified water to an absorbance of 0.70 ± 0.02 at 734 nm.

[0084] Experimental steps: DPPH free radical scavenging ability determination: In a 96-well plate, add 100 μL of sample dilution (or control solution) to each well.

[0085] Immediately add 100 µL of DPPH working solution.

[0086] Mix quickly (shake for 30 seconds) and place in a 25°C dark incubator for 30 minutes.

[0087] The absorbance of each well was measured at a wavelength of 517 nm using a multifunctional microplate reader.

[0088] Set up a blank control (100 μL sample diluent + 100 μL anhydrous ethanol) and a DPPH control (100 μL pure water + 100 μL DPPH working solution).

[0089] Three parallel wells were set up for each group of samples and controls.

[0090] ABTS free radical scavenging ability assay: In a 96-well plate, add 20 μL of sample dilution (or control solution) to each well.

[0091] Immediately add 180 µL of ABTS working solution.

[0092] Mix quickly (shake for 30 seconds) and place in a 25°C dark incubator for 6 minutes.

[0093] The absorbance of each well was measured at a wavelength of 734 nm using a multifunctional microplate reader.

[0094] Set up a blank control (20 μL sample diluent + 180 μL purified water) and an ABTS control (20 μL purified water + 180 μL ABTS working solution).

[0095] Three parallel wells were set up for each group of samples and controls.

[0096] Data processing: Calculation of DPPH clearance rate: Clearance rate (%) = [1-(A 样品 -A 空白样品 ) / (A DPPH对照 -A 空白DPPH )]×100%; Among them, A 样品 is the absorbance after the sample is mixed with DPPH; A 空白样品 is the absorbance of the sample after mixing with anhydrous ethanol; A DPPH对照 is the absorbance of pure water mixed with DPPH; A 空白DPPH It is the absorbance of the mixture of pure water and anhydrous ethanol.

[0097] Calculation of ABTS clearance rate: Clearance rate (%) = [1-(A 样品 -A 空白样品 ) / (A ABTS对照 -A 空白ABTS )]×100%; Among them, A 样品 is the absorbance of the sample after mixing with ABTS; A 空白样品 A is the absorbance of the sample after mixing with pure water; ABTS对照 A is the absorbance of pure water mixed with ABTS; 空白ABTS It is the absorbance of pure water mixed with pure water.

[0098] The free radical scavenging rates of samples in each group were compared to evaluate their antioxidant capacity and compared with the positive control.

[0099] Table 1: DPPH and ABTS free radical scavenging rates of the compositions: Sample number DPPH clearance rate (%) ± SD ABTS clearance rate (%) ± SD Example 1 78.6±1.2 85.1±1.8 Example 2 86.3±0.9 91.7±1.3 Example 3 70.1±1.5 76.5±2.1 Comparative Example 1 22.5±2.8 28.9±3.1 Comparative Example 2 55.7±2.3 61.4±2.6 Vitamin C 92.8±0.7 95.5±0.6 Resveratrol 88.1±1.1 90.2±1.0 It can be seen from the above data that the oral anti-aging composition of the present invention exhibits significant antioxidant activity, which is not accidental, but the inevitable result of its unique formula and preparation process. The carefully selected dihydromyricetin, coastal pine bark extract, Haematococcus pluvialis and other natural antioxidant ingredients in the formula of the present invention can effectively capture and neutralize excess free radicals at the body level, slowing down their oxidative damage to cells. This multi-component, multi-pathway free radical scavenging mechanism surpasses the limitations of a single antioxidant, so that the overall scavenging ability presents a significant synergistic effect. For example, the unique conjugated double bond structure of astaxanthin gives it a powerful ability to quench singlet oxygen, while dihydromyricetin regulates oxidative stress through multiple pathways, which is contrasted by the low clearance rate of Comparative Example 1, clearly demonstrating the indispensability of specific active components.

[0100] In addition, the preparation process is crucial to maintaining and optimizing the biological effects of these active ingredients. Comparing Example 2 with Comparative Example 2, the antioxidant effect of the latter is significantly weakened due to the use of a simple disordered mixing method. This confirms the strategy of "adding active ingredients in stages" in the process of the present invention, which ensures that each component is gradually dissolved and dispersed under suitable temperature and stirring conditions, avoiding the destruction of some active ingredients by high temperature or strong shear force. In particular, the pre-dispersion and homogenization treatment of fat-soluble Haematococcus pluvialis improves the uniform dispersion of astaxanthin in the aqueous phase system, enabling it to more effectively exert its antioxidant effect. This fine process control significantly guarantees the stable presence and active conformation of the active ingredient in the final product, so that it can maximize its potential to scavenge free radicals after entering the body.

[0101] Experiment 2: Key active ingredient content stability evaluation experiment: This experiment aims to quantify the protective effect of the innovative preparation process of the present invention on the stability of key active ingredients in the composition (such as dihydromyricetin, astaxanthin, and vitamin C) during storage, which is directly related to the beneficial effect of "optimization of active ingredient stability and bioavailability".

[0102] Experimental purpose: By monitoring the content changes of key active ingredients under accelerated and long-term stability conditions, the protective effect of the preparation process of the present invention (staged mixing, special homogenization treatment, and low-oxygen filling) on ​​easily degradable ingredients such as dihydromyricetin, astaxanthin, and vitamin C was evaluated.

[0103] Sample preparation: Oral anti-aging composition samples prepared in Example 1, Example 2, and Example 3.

[0104] Comparative Example 2 (disordered simple mixing process) sample.

[0105] Comparative Example 3 (Haematococcus pluvialis without special treatment) sample.

[0106] Comparative Example 4 (conventional air filling) sample.

[0107] All samples were completed and packaged according to their respective preparation methods, and sufficient quantity of each sample was prepared to meet the testing requirements of all sampling points.

[0108] Stability test conditions: Accelerated stability testing: Place samples in a constant temperature and humidity chamber that complies with ICH (International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use) guidelines or industry-standard food stability testing requirements. Set the temperature to 40°C ± 2°C and the relative humidity to 75% ± 5%. Sampling is performed at 0 days, 1 month, 2 months, and 3 months.

[0109] Long-term stability test: Place the samples in a constant temperature and humidity chamber. Set the conditions to 25°C ± 2°C and 60% ± 5%. Sampling time points: 0 day, 3 months, and 6 months.

[0110] Active ingredient content determination steps: At each preset sampling time point, three sample bottles were randomly taken from each group.

[0111] Sample pretreatment: Based on the specific characteristics of the components, the sample is subjected to necessary pretreatment steps such as extraction, dilution, and filtration to obtain a clear solution suitable for chromatographic analysis.

[0112] Determination of dihydromyricetin content (HPLC method): Standard basis: Refer to the general principles for the determination of flavonoids in the "Chinese Pharmacopoeia" and conduct methodological verification in combination with the physical and chemical properties of dihydromyricetin.

[0113] Chromatographic conditions: Use a C18 reverse phase column (for example: Agilent ZorbaxSB-C18, 4.6×250 mm, 5 μm).

[0114] Mobile phase A: 0.1% phosphoric acid in water, mobile phase B: acetonitrile. Gradient elution program: 0-10 min, 10-25% B; 10-20 min, 25-40% B; 20-25 min, 40% B; 25-30 min, 40-10% B. Flow rate: 1.0 mL / min. Column temperature: 30°C. Detection wavelength: 290 nm. Injection volume: 10 μL.

[0115] Quantification: External standard method, the content of dihydromyricetin in the sample was calculated by standard curve.

[0116] Astaxanthin content determination (HPLC method): Standard basis: Based on the method in Appendix A of GB / T23793-2009 "Determination of astaxanthin content in aquatic feeds - High performance liquid chromatography" or GB / T23745-2009 "Feed additive 10% astaxanthin".

[0117] Chromatographic conditions: Use a C30 column (e.g., YMC Carotenoid S-5, 4.6 × 250 mm, 5 μm). Mobile phase: methanol-methyl tert-butyl ether (usually 85:15 or optimized ratio). Flow rate: 1.0 mL / min. Column temperature: 25°C. Detection wavelength: 470 nm. Injection volume: 10 μL.

[0118] Quantification: External standard method, calculate the astaxanthin content in the sample through the standard curve.

[0119] Determination of Vitamin C (Ascorbic Acid) Content (HPLC Method): Standard basis: Refer to the determination method of vitamin C content in the Chinese Pharmacopoeia (HPLC method).

[0120] Chromatographic conditions: Use a C18 column (e.g., Waters Symmetry C18, 4.6 × 250 mm, 5 μm). Mobile phase: 0.05 mol / L potassium dihydrogen phosphate solution (pH adjusted to 2.5 with phosphoric acid). Flow rate: 1.0 mL / min. Column temperature: 30°C. Detection wavelength: 245 nm. Injection volume: 10 μL.

[0121] Quantification: External standard method, calculate the content of vitamin C in the sample through the standard curve.

[0122] Data Analysis: Calculate the residual percentage of each active ingredient at different time points and plot the content-time curve. Evaluate the stability of each sample group by comparing the slope of the curve and the final residual amount.

[0123] Table 2: Changes in the content of key active ingredients in the composition during the accelerated stability test (40°C / 75%RH) (as a percentage of the initial content) The results of this stability test clearly reveal the significant improvement effect of the innovative preparation process of the present invention on the stability of the key active ingredients in the composition. The accelerated degradation of the active ingredients in Comparative Example 2 (disordered simple mixing) directly verifies the necessity and superiority of the staged mixing process of the present invention. This process effectively avoids the adverse intermolecular interactions or local overheating effects that may occur in the early stage by precisely controlling the timing of addition and mixing conditions of each component, thereby maintaining the initial structural integrity and bioactive conformation of easily degradable components such as dihydromyricetin and vitamin C to the greatest extent, which is the key to achieving precise controlled release and stable existence of active substances.

[0124] The rapid oxidative degradation of astaxanthin in Comparative Example 3 (Haematococcus pluvialis without special treatment) strongly demonstrates the decisive role of the pretreatment and homogenization steps of the special active ingredients of the present invention. As a highly active fat-soluble molecule, the dispersion state of astaxanthin in the aqueous phase system directly affects its stability and bioavailability. The present invention successfully refines astaxanthin particles to the nano / micrometer level through ultrasonic-assisted pre-dispersion and high-pressure homogenization treatment, and evenly embeds them in the system, significantly reducing the contact interface with the oxidant, thereby fundamentally inhibiting its oxidative degradation pathway. This stability enhancement strategy based on the regulation of microscopic dispersed phase morphology is the fundamental guarantee to ensure the long-term effect of such special active ingredients.

[0125] Furthermore, the sustained degradation of the active ingredient in Comparative Example 4 (conventional air filling) highlights the profound impact of the present invention's low-oxygen environment filling on product stability. Oxygen is the dominant factor in the oxidative inactivation of many natural active ingredients, particularly antioxidants. By introducing inert gas protection and strict sealing during the filling process, the present invention successfully creates a low-oxygen microenvironment within the product, effectively blocking direct contact between oxygen and sensitive active ingredients, thereby slowing the kinetics of the oxidation reaction.

[0126] Experiment 3: Physical stability evaluation experiment of the composition: Experimental purpose: To evaluate the effect of the optimized process (staged mixing, special homogenization, precise pH adjustment, and low-oxygen filling) of the present invention on the physical stability of the composition by monitoring the appearance, pH value, turbidity, and particle size distribution of key particles of the sample under accelerated storage conditions.

[0127] Sample preparation: The oral anti-aging composition sample prepared in Example 1.

[0128] Comparative Example 2 (disordered simple mixing process) sample.

[0129] Comparative Example 3 (Haematococcus pluvialis without special treatment) sample.

[0130] Comparative Example 4 (conventional air filling) sample.

[0131] Comparative Example 5 (pH not adjusted) sample.

[0132] Each group of samples was prepared and packaged according to their own method.

[0133] Stability test setup: After all samples are divided and packed, they are placed in a constant temperature and humidity chamber with the set conditions of temperature: 40℃±2℃, relative humidity: 75%±5%.

[0134] Sampling time points: 0 day, 1 month, 2 months, and 3 months.

[0135] Physical stability index determination steps: At each preset sampling time point, three sample bottles were randomly taken from each group.

[0136] Appearance inspection: Visually inspect the contents of the sample bottle. Record color changes, clarity (transparent, translucent, turbid), and any visible precipitation, stratification, or flocculent formation, and take photos.

[0137] pH value determination: Use a precision pH meter (compliant with the requirements of JJG119-2005 "pH meter" verification regulations), insert it directly into the sample, and record the pH value after the reading stabilizes.

[0138] Turbidity measurement: Use a turbidimeter (such as a scattered light turbidimeter that complies with ISO 7027) to thoroughly mix the sample, pour it into a cuvette, and measure its turbidity value (NTU). Refer to the basic principles of GB / T 13200-91 "Water Quality Turbidity Determination Method" for operation, ensuring consistency in the light source and detector angles.

[0139] Particle size distribution determination (for insoluble particles such as Haematococcus pluvialis): For the samples of Example 1, Comparative Example 2, and Comparative Example 3, the samples were appropriately diluted (if necessary) at 0 days and 3 months, and the particle size distribution (such as D10, D50, and D90 values) was determined using a laser particle size analyzer (in compliance with GB / T19077.1-2016 "Particle Size Analysis by Laser Diffraction Method"), and the trend of particle size change over time was analyzed.

[0140] Data analysis: Comprehensively analyze the changes in appearance, pH fluctuations, turbidity increments, and particle size distribution of each sample at different time points.

[0141] Table 3: Changes in physical stability indicators of the composition during the accelerated stability test (40°C / 75%RH): The data from this physical stability assessment clearly demonstrates the significant advantages of the present preparation process in improving the macroscopic and microscopic physical stability of the composition. Comparative Example 5, due to the lack of precise pH control, exhibited significant pH drift over time, accompanied by severe precipitation and flocculation, highlighting the critical role of pH regulation in complex biological systems. Maintaining the product within a specific pH window not only effectively inhibits hydrolysis or polymerization reactions but also ensures the solubility and colloidal stability of the amphoteric or ionic components in the system, thereby fundamentally preventing the precipitation and aggregation of substances caused by pH fluctuations at the level of charge balance and solvation.

[0142] The poor performance of Comparative Example 3 (no special treatment of Haematococcus pluvialis) and Comparative Example 2 (disordered simple mixing) is manifested by a sharp increase in turbidity and a significant increase in particle size, ultimately leading to irreversible precipitation and stratification, which strongly confirms the indispensability of homogenization of special active ingredients for maintaining system uniformity and long-term stability. Hydrophobic active ingredients such as astaxanthin are very prone to Ostwald ripening, aggregation or flocculation without effective micronization and uniform dispersion, thereby forming a precipitate visible to the naked eye. The present invention uses a high shear homogenization process to stably disperse these ingredients in the continuous phase to form a submicron or even nanoscale emulsion or suspension, which greatly improves the kinetic stability of the system and effectively inhibits particle agglomeration and gravity sedimentation.

[0143] It is worth noting that although the initial physical appearance of Comparative Example 4 (conventional air filling) is acceptable, its color deepens over time, which indirectly indicates that oxidation has occurred inside the product, and may be accompanied by precipitation of oxidation products in the long term. This further verifies that filling in a low-oxygen environment is not only crucial to the chemical stability of the active ingredient, but also has a profound impact on its physical appearance stability. The hypoxic environment reduces the generation of oxidation by-products that may cause color change, turbidity or non-specific precipitation from the source by slowing down the oxidation chain reaction. Overall, the process innovation of the present invention lies in the synergistic construction of an oral liquid preparation with excellent long-term physical stability through the precise control of multi-dimensional physical parameters such as pH, homogeneity and oxygen exposure.

[0144] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. An anti-aging composition containing dihydromyricetin, characterized in that: Contains the following components by weight percentage: dihydromyricetin: 0.02%~0.06%; Citrus aurantium fruit extract: 0.20%~0.30%; Maritime pine bark extract: 0.10%~0.16%; Haematococcus pluvialis: 0.02%~0.06%; Aronia extract: 0.06%~0.10%; Dendrobium officinale flower extract: 0.02%~0.06%; Acerola powder: 0.30%~0.40%; Emblica officinalis extract: 0.06%~0.10%; Erythritol: 10.00%~12.00%; Citric acid: 0.20%~0.40%; Stevia powder: 0.02%~0.10%; Grape juice concentrate: 2.00%~10.00%; Blackcurrant juice concentrate: 2.00%~10.00%; and the balance of water.

2. A method for preparing an anti-aging composition, comprising the anti-aging composition containing dihydromyricetin according to claim 1, characterized in that: The following steps are involved: a) preparing a base liquid, comprising mixing and dissolving a portion of water with a first group of solid and / or liquid components; b) adding the active ingredient in stages, comprising adding the second set of solid and / or liquid ingredients to the base liquid in batches under specific temperature and stirring conditions; c) processing and homogenizing of specific active ingredients, including pre-dispersion of specific active ingredients and homogenization of the mixture; d) system control and fine mixing, including adjusting the pH value of the mixed solution and adding the remaining amount of water before homogenizing the entire solution; e) Sterile filtration and packaging, which includes fine filtering of the obtained composition, and filling and sealing under a controlled environment.

3. The method for preparing an anti-aging composition according to claim 2, wherein: The first group of solid and / or liquid ingredients in step a) includes erythritol, citric acid and stevia powder.

4. The method for preparing an anti-aging composition according to claim 2, wherein: The amount of purified water used in step a) is 75% to 85% of the total water volume, and the mixed dissolution is carried out at a temperature of 20° C. to 25° C. and supplemented with stirring at 50 rpm to 100 rpm.

5. The method for preparing an anti-aging composition according to claim 2, wherein: The second group of solid and / or liquid ingredients in step b) includes grape juice concentrate, blackcurrant juice concentrate, acerola cherry powder, emblica fruit extract, dihydromyricetin, aurantium dulcis fruit extract, maritime pine bark extract, aronia berry extract and Dendrobium officinale flower extract.

6. The method for preparing an anti-aging composition according to claim 2, characterized in that: In the step b), the temperature is controlled at 20°C to 25°C, and after adding each second component, the stirring speed is 100 rpm to 200 rpm, and the stirring time is 10 minutes to 20 minutes.

7. The method for preparing an anti-aging composition according to claim 2, characterized in that: The specific active ingredient in step c) is Haematococcus pluvialis; the pre-dispersion treatment includes ultrasonic treatment at a frequency of 20 kHz to 40 kHz, a treatment time of 5 minutes to 15 minutes, a pressure of 50 bar to 200 bar, and a number of cycles of 2 to 5 times.

8. The method for preparing an anti-aging composition according to claim 2, characterized in that: In step d), the pH value is adjusted to a range of 3.0 to 5.0; the pressure of the overall homogenization treatment is 80 bar to 200 bar, and the cycle time is 10 minutes to 20 minutes.

9. The method for preparing an anti-aging composition according to claim 2, wherein: In step e), the fine filtration is performed using a 0.2µm to 0.45µm microporous filter membrane.

10. The method for preparing an anti-aging composition according to claim 2, characterized in that: The controlled environment in step e) is a low-oxygen environment, which includes pre-purging the container with an inert gas before filling and quickly sealing the container after filling.

Images