Natural essence capsule containing caviar and preparation method thereof

Abstract

The invention relates to the technical field of culture medium preparation, in particular to a caviar-containing natural essence capsule and a preparation method thereof.The capsule is composed of a capsule shell and a core material, and the core material is prepared from, by weight, 10-20% of caviar extract, 5-12% of cod skin collagen peptide, 3-8% of sodium hyaluronate and other natural active ingredients and further contains fullerene and phytosphingosine; and the balance of deionized water. The caviar extract is subjected to enzymolysis, ceramide NP and sodium hyaluronate are combined through hydrogen bonds, a capsule shell is composed of gelatin, glycerin and the like, the particle size is 0.5-2 mm, the loading rate of a core material is larger than or equal to 90%, and the pH value is 5.5-7.0. According to the invention, the enzymolysis caviar extract is taken as a core, multiple components have synergistic interaction, multiple effects of resisting aging, moisturizing and repairing are achieved, and the capsule type can isolate oxygen and light, protect stable active components, is free of extra preservatives, mild and non-irritant, convenient and sanitary to use, accurate in dosage and suitable for various skin types.

Description

Technical Field

[0001] This invention relates to the field of precision processing technology for natural extracts, specifically to a natural essence capsule containing caviar and its preparation method. Background Technology

[0002] As the beauty and skincare industry upgrades towards natural, efficient, and precise products, consumers are placing higher demands on the safety of skincare ingredients, the targeted nature of efficacy, and ease of use. Serums, as carriers of high-concentration active ingredients, have become core products in the skincare field due to their ability to quickly penetrate the skin and address specific skincare problems. Among them, caviar extract, rich in amino acids, vitamins, minerals, and bioactive peptides, possesses excellent anti-aging, repairing, and moisturizing effects, and is gradually becoming a popular core ingredient in high-end serums.

[0003] However, existing caviar-containing serums face several technological bottlenecks. First, the large protein molecules in caviar extracts are difficult for the skin to absorb directly. Without precise enzymatic hydrolysis, the utilization rate of active ingredients is low, failing to fully realize their skincare benefits. Furthermore, natural active ingredients are easily affected by factors such as light, oxygen, and temperature, leading to oxidative decomposition or inactivation, resulting in reduced product efficacy and a shortened shelf life. Second, traditional serums are mostly liquid formulations, resulting in uneven dispersion of active ingredients. They are also prone to evaporation and loss during use, making it difficult to form a stable nutrient supply system on the skin's surface, and the moisturizing effect has a short duration. Simultaneously, liquid products have higher requirements for packaging and transportation, and improper sealing can easily lead to contamination or ingredient deterioration, affecting safety.

[0004] To address these issues, some products extend their shelf life by adding preservatives and antioxidants. However, excessive preservatives can irritate the skin, especially for those with sensitive skin. Some products attempt to be formulated into capsules to protect active ingredients from oxygen and light, but existing capsules suffer from low core material loading, easy shell breakage, and difficulty in controlling the release rate of active ingredients. Furthermore, the ingredient combinations in existing products lack synergistic design, often relying solely on the single effect of caviar extract without combining it with other natural active ingredients to form a synergistic system. This results in limited skincare efficacy, failing to simultaneously meet multiple needs such as anti-aging, moisturizing, repair, and anti-oxidation.

[0005] In terms of capsule manufacturing processes, existing technologies mostly employ single emulsification or molding processes, resulting in insufficient uniformity and stability of the core material dispersion, easily leading to stratification and sedimentation. Furthermore, unreasonable capsule shell formulations result in poor flexibility, brittleness, or excessively rapid dissolution, negatively impacting the user experience. Simultaneously, some capsule products use chemically synthesized additives during preparation, contradicting consumer demands for "natural and gentle" products. Therefore, developing a natural essence capsule with caviar extract as its core, combined with multiple natural active ingredients to form a synergistic system, employing an innovative capsule formulation to protect the stability of active ingredients, and utilizing a gentle and safe manufacturing process, has become a crucial breakthrough in the beauty and skincare industry. This approach aligns with market trends and can drive technological upgrades in high-end natural skincare products. Summary of the Invention

[0006] (a) Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a natural essence capsule containing caviar and its preparation method.

[0007] (II) Technical Solution A natural essence capsule containing caviar, comprising a capsule shell and a core material, wherein the core material comprises, by weight percentage: 10-20% caviar extract, 5-12% deep-sea cod skin collagen peptide, 3-8% sodium hyaluronate, 2-5% ceramide NP, 1-4% β-glucan, 2-6% niacinamide, 1-3% tocopheryl acetate, 1-4% phytosterols, 0.5-2% polyglutamic acid, 3-7% hydrolyzed elastin, 2-5% centella asiatica extract, 1-4% calendula extract, 0.3-1% vitamin C palmitate, 0.01-0.05% nano silver, with the balance being deionized water; Caviar extract was prepared by enzymatic hydrolysis at 45-55℃ for 3-5 hours, with a molecular weight ≤5kDa; cod skin collagen peptides had a molecular weight of 1-3kDa and a purity ≥95%; sodium hyaluronate had a molecular weight of 80-120kDa; ceramide NP had a purity ≥98%; and β-glucan was derived from oats with a molecular weight of 20-50kDa. In the core material, nicotinamide and tocopheryl acetate undergo a synergistic antioxidant reaction, and ceramide NP and sodium hyaluronate are bonded through hydrogen bonds, with the reaction formula being ceramide NP-COOH + sodium hyaluronate-OH → ceramide NP-O-sodium hyaluronate + H2O, thus enhancing moisturizing stability. The capsule shell is composed of 30-40% gelatin, 10-15% glycerin, 5-10% carrageenan, 5-8% sorbitol, 0.1-0.3% disodium EDTA, and 27-49.9% deionized water. The capsule particle size is 0.5-2mm, the core material loading rate is ≥90%, the pH value is 5.5-7.0, and the viscosity is 100-300mPa・s.

[0008] Furthermore, the fullerene is a water-soluble modified fullerene with a particle size of 10-30 nm, modified with polyethylene glycol. The fullerene and vitamin C palmitate synergistically provide antioxidant protection, reducing skin oxidative damage by scavenging free radicals. It also forms hydrogen bonds with amino acids in caviar extract, as shown in the following reaction formula: It enhances the retention of active ingredients on the skin surface and improves anti-aging effects.

[0009] Furthermore, it also includes 1-3% phytosphingosine, wherein the phytosphingosine has a purity ≥97% and a melting point of 50-55℃. It forms a lipid bilayer structure with ceramide NP and phytosterols, repairing the skin barrier. The synergistic effect of phytosphingosine and ceramide NP can increase the moisture content of the stratum corneum. Its hydroxyl groups undergo esterification with the carboxyl groups of sodium hyaluronate, as shown in the following reaction formula: This further enhances the moisture retention and water-locking ability of the core material.

[0010] Furthermore, the preparation process of the caviar extract is as follows: Select fresh caviar, remove impurities, wash 2-3 times with physiological saline, add 5-8 times the volume of deionized water, stir well, add compound protease, the amount of enzyme added is 0.5-1% of the weight of caviar, and enzymatically hydrolyze for 3-5 hours at 45-55℃ and pH 6.0-7.0. After enzymatic hydrolysis, the temperature is raised to 85-90℃ for 15-20 min to inactivate the enzyme. After cooling to room temperature, the mixture is centrifuged at 8000-10000 r / min for 15-20 min. The supernatant is then filtered through an ultrafiltration membrane with a molecular weight cutoff of 5 kDa and concentrated to a solid content of 20-30% to obtain caviar extract.

[0011] Furthermore, the preparation process of the capsule shell is as follows: weigh gelatin, glycerin, carrageenan, sorbitol, and disodium EDTA according to the proportion, add deionized water, stir and dissolve at 60-70℃ for 30-40 minutes, continuously stirring to prevent clumping, filter through a 100-200 mesh sieve to remove impurities, degas under vacuum for 20-30 minutes, vacuum degree -0.08~-0.09MPa, to obtain the capsule shell solution, with the viscosity controlled at 500-800mPa・s.

[0012] Furthermore, the complex protease is composed of trypsin, papain, and bromelain in a mass ratio of 2:1:1, with an enzyme activity ≥5000U / g; the Centella asiatica extract is prepared by ethanol reflux extraction at a temperature of 70-80℃ for 2-3 hours, with an ethanol volume fraction of 60-70%, and the purity of the extract after concentration and drying is ≥90%; the Calendula officinalis extract is prepared by water extraction at a temperature of 80-90℃ for 1.5-2.5 hours, and the solid content after concentration is ≥25%.

[0013] Furthermore, the pH value of the core material is adjusted to 5.5-7.0 by citric acid or triethanolamine, and the viscosity is adjusted by adding polyglutamic acid. The stability of each active ingredient in the core material is ensured by the following methods: tocopheryl acetate and vitamin C palmitate are compounded at a mass ratio of 2:1, and the mass ratio of nano silver to plant extracts is ≤1:200, to avoid the interaction and failure of active ingredients.

[0014] Furthermore, the preparation method of caviar-containing natural essence capsules includes the following steps: S1. Core material preparation: Weigh each core material component according to weight percentage, heat deionized water to 30-40℃, add sodium hyaluronate, ceramide NP, and β-glucan water-soluble components in sequence, stir to dissolve, then add caviar extract and collagen peptides, continue stirring for 30-40 min, then add oil-soluble components, emulsify at high speed for 15-20 min at a speed of 10000-12000 r / min, adjust pH value and viscosity to obtain core material; S2. Preparation of capsule shell solution: The prepared capsule shell solution is kept at 50-60℃ for later use; S3. Capsule Formation: Using the dripping method, the core material and capsule shell solution are injected into the inner and outer tubes of the dripping pellet machine, respectively. The flow rate of the core material is 0.5-1 mL / min, and the flow rate of the capsule shell solution is 1-2 mL / min. The capsules are dripped into the coolant liquid paraffin and cooled at 5-10℃. After formation, the capsules are collected. S4. Post-processing: Wash the molded capsules 2-3 times with anhydrous ethanol to remove residual coolant on the surface, and air dry them at 25-30℃ for 12-24 hours. Control the moisture content of the capsules to 5-8%, and screen the products with qualified particle size to obtain natural essence capsules containing caviar.

[0015] Furthermore, after high-speed shear emulsification in step S1, high-pressure homogenization is required, with a homogenization pressure of 20-30 MPa and 2-3 homogenization cycles to ensure that the core material particle size is ≤5 μm and there is no stratification. In step S3, the viscosity of the coolant liquid paraffin is 100-200 mPa·s, and the dropper diameter is 0.3-0.5 mm. After the capsule is formed, it is immersed in the coolant for 30-60 minutes to ensure that the capsule shell is completely solidified.

[0016] Furthermore, after drying in step S4, sterilization is required using irradiation sterilization with an irradiation dose of 5-10 kGy and a sterilization time of 15-20 min. This ensures that the microbiological indicators of the capsules meet the requirements: total bacterial count ≤100 CFU / g, total mold and yeast count ≤10 CFU / g, and no pathogenic bacteria detected. The final finished capsules must undergo a sealing test using a negative pressure method with a negative pressure of -0.05 MPa for 30 seconds. No leakage is considered acceptable.

[0017] (iii) Beneficial technical effects Compared with existing technologies, the beneficial effects of this invention are: First, the core material formula of this invention achieves synergistic effects from multiple natural active ingredients, resulting in comprehensive and powerful skincare benefits. Using precisely enzymatically hydrolyzed caviar extract as the core, combined with deep-sea cod skin collagen peptides and hydrolyzed elastin, it replenishes the skin with abundant amino acids and active peptides, synergistically promoting collagen synthesis, enhancing skin elasticity, and delaying the formation of wrinkles. Sodium hyaluronate, ceramide NP, phytosterols, and other ingredients form a moisturizing and repairing system that quickly replenishes skin moisture, repairs damaged skin barriers, enhances the skin's water-locking ability, and improves dryness and roughness.

[0018] Ingredients such as niacinamide, tocopheryl acetate, and vitamin C palmitate work synergistically to combat oxidation, effectively eliminate free radicals in the skin, reduce oxidative damage, brighten skin tone, and improve dullness. The combination of these ingredients achieves a unified range of skincare benefits, including anti-aging, moisturizing, repairing, and antioxidant effects, meeting diverse consumer skincare needs.

[0019] Secondly, the capsule formulation effectively solves many drawbacks of traditional liquid serums, significantly improving product stability and safety. The capsule shell isolates the product from oxygen, light, and external pollution, providing a strong protective barrier for the natural active ingredients in the core material. This prevents the active ingredients from oxidizing, decomposing, or becoming inactive, extending the product's shelf life and ensuring it maintains its superior efficacy throughout use. Simultaneously, the capsule formulation allows for precise, quantitative packaging of the core material. One capsule is used per application, ensuring controllable dosage and avoiding waste caused by excessive pouring of liquid products. Furthermore, the absence of air contact during use reduces the risk of contamination, making it more hygienic and convenient.

[0020] Furthermore, the preparation process of this invention is scientifically sound and ensures the quality and performance of the product. The core material preparation process employs a combination of high-speed shear emulsification and high-pressure homogenization, ensuring uniform dispersion of all active ingredients without stratification or sedimentation, thus enhancing the stability of the core material. The capsule shell is prepared from natural raw materials such as gelatin, glycerin, and carrageenan, exhibiting good flexibility, resistance to breakage, and a moderate dissolution rate, allowing it to slowly dissolve on the skin surface, releasing the core material components and extending the nutrient supply time. The entire preparation process does not involve excessive chemically synthesized additives, making the product gentle and non-irritating, suitable for all skin types, and especially friendly to those with sensitive skin.

[0021] Finally, the product of this invention combines naturalness, high efficacy, and convenience, making it highly competitive in the market. The product is primarily composed of natural active ingredients; its novel capsule formulation is convenient to use, easy to carry and store, enhancing the user experience; the synergistic effect of multiple ingredients provides comprehensive and significant skincare benefits, effectively addressing various skin problems and meeting the needs of different consumer groups. Furthermore, the product's manufacturing process is mature, with controllable costs, suitable for large-scale production, and possesses broad market application prospects and commercial value. It can provide the beauty and skincare industry with a new, highly effective natural essence product, driving the industry towards a more natural, precise, and safer direction. Attached Figure Description

[0022] Figure 1 This is a flowchart of a method for preparing a natural essence capsule containing caviar, as disclosed in this invention. Figure 2 This is a bar chart showing the retention rates of active ingredients in the examples and comparative examples; Figure 3 It is a line graph showing changes in skin moisture content during volunteer trials; Figure 4 These are histograms of core material particle size distribution under different processes; Figure 5 This is a bar chart showing the changes in the number of microorganisms in the examples and comparative examples; Figure 6 This is a radar chart showing the synergistic antioxidant capacity of different components. Detailed Implementation

[0023] according to Figures 1 to 4 The specific embodiments of the present invention are as follows: The technical solution of the present invention will be described in detail below with reference to specific embodiments and comparative examples. All operations are carried out in a clean room that meets the safety standards for cosmetic production. All raw materials used are qualified cosmetic-grade products. All parameters are strictly selected in accordance with the scope of the claims, covering both ends and the middle values, to ensure the repeatability and practicality of the technical solution. Example

[0024] Raw material preparation: Accurately weigh each component of the core material according to weight percentage: caviar extract 15%, deep-sea cod skin collagen peptide 8%, sodium hyaluronate 5%, ceramide NP 3%, β-glucan 2%, nicotinamide 4%, tocopheryl acetate 2%, phytosterol 2%, polyglutamic acid 1%, hydrolyzed elastin 5%, centella asiatica extract 3%, calendula extract 2%, vitamin C palmitate 0.6%, nano silver 0.03%, fullerene 1%, phytosphingosine 2%, and the remainder is deionized water.

[0025] Preparation of caviar extract: Select fresh caviar, remove impurities such as fascia, rinse 3 times with physiological saline, add 6 times the volume of deionized water, stir evenly and then add complex protease.

[0026] The complex protease is a mixture of trypsin, papain, and bromelain in a mass ratio of 2:1:1, with an enzyme activity of 6000 U / g, and the amount added is 0.8% of the caviar mass.

[0027] Enzymatic hydrolysis was performed at 50℃ and pH 6.5 for 4 hours. After hydrolysis, the temperature was raised to 88℃ for 18 minutes to inactivate the enzyme. After cooling to room temperature, the mixture was centrifuged at 9000 r / min for 18 minutes. The supernatant was collected and filtered through an ultrafiltration membrane with a molecular weight cutoff of 5 kDa. The mixture was then concentrated to a solid content of 25% to obtain caviar extract with a molecular weight ≤ 5 kDa.

[0028] Deep-sea cod skin collagen peptides have a molecular weight of 2 kDa and a purity of 96%; sodium hyaluronate has a molecular weight of 100 kDa; ceramide NP has a purity of 99%; β-glucan is derived from oats and has a molecular weight of 35 kDa; nicotinamide has a purity of 99.5%; tocopheryl acetate has a purity of 98%; phytosterols have a purity of 97%; polyglutamic acid has a molecular weight of 80 kDa and a purity of 95%; hydrolyzed elastin has a purity of 94%; Centella asiatica extract was extracted by reflux with ethanol at 75℃ for 2.5 h, with an ethanol volume fraction of 65%, and after concentration and drying, the purity was 92%. Calendula extract was obtained through water extraction at 85℃ for 2 hours, resulting in a solid content of 28% after concentration. Vitamin C palmitate had a purity of 98%. Nano-silver particles had a diameter of 20nm and a purity of 99.6%. Fullerene was a water-soluble modified product with a particle size of 20nm and a purity of 99.2%, modified with polyethylene glycol to a degree of 85%. Phytosphingosine had a purity of 97.5% and a melting point of 52℃.

[0029] The capsule shell components were weighed as follows by weight percentage: gelatin 35%, glycerin 12%, carrageenan 8%, sorbitol 6%, disodium EDTA 0.2%, and deionized water 38.8%. The gelatin viscosity was 15 mPa·s; the glycerin purity was 99.5%; the carrageenan viscosity was 800 mPa·s; the sorbitol purity was 99%; and the disodium EDTA purity was 99%.

[0030] For core material preparation, deionized water was heated to 35°C, and sodium hyaluronate, ceramide NP, β-glucan, polyglutamic acid, and nicotinamide were added sequentially. The stirrer was turned on and stirred at 500 r / min for 20 min until completely dissolved.

[0031] Add caviar extract, deep-sea cod skin collagen peptides, hydrolyzed elastin, centella asiatica extract, and calendula extract, and continue stirring for 25 minutes until well mixed. Add tocopheryl acetate, phytosterols, vitamin C palmitate, fullerene, and phytosphingosine. Turn on a high-speed shear emulsifier at 11,000 rpm for 18 minutes, followed by high-pressure homogenization at 25 MPa, twice to ensure the core material particle size is ≤5 μm.

[0032] The pH of the core material was adjusted to 6.2 with citric acid, and the viscosity was measured to be 200 mPa·s, resulting in a uniform and stable core material.

[0033] To prepare the capsule shell solution, gelatin, glycerin, carrageenan, sorbitol, and disodium EDTA were added to deionized water and placed in a 65°C constant temperature water bath. The stirrer was turned on and stirred at 300 rpm for 35 minutes until completely dissolved, with continuous stirring to prevent clumping.

[0034] After dissolution, the solution is filtered through a 150-mesh sieve to remove impurities and then transferred to a vacuum degassing tank. The vacuum level is -0.085 MPa, and the solution is degassed for 25 minutes to obtain a capsule shell solution with a viscosity of 650 mPa·s. The solution is then kept at 55°C for later use.

[0035] Capsule forming is performed using a dripping method, where the core material and capsule shell solution are injected separately into the inner and outer tubes of the dripping pellet machine. The core material flow rate is 0.8 mL / min, the capsule shell solution flow rate is 1.5 mL / min, and the dropper diameter is 0.4 mm. The solution is dripped into the coolant liquid paraffin. The coolant liquid paraffin has a viscosity of 150 mPa·s and a cooling temperature of 8°C. After forming, the capsules are immersed in the coolant for 45 minutes to ensure complete solidification of the capsule shell, after which the formed capsules are collected.

[0036] Post-processing involved immersing the molded capsules in anhydrous ethanol for 1 minute, washing twice to remove residual coolant, and then drying them in a 28°C ventilated drying oven for 18 hours, controlling the capsule moisture content to 6.5%. Capsules with a particle size of 0.5-2 mm were screened using a sieving device, and unqualified products were discarded. The screened capsules were then sterilized by irradiation at a dose of 8 kGy for 18 minutes. A negative pressure method was used for sealing testing: a negative pressure of -0.05 MPa was maintained for 30 seconds; no leakage was considered acceptable, ultimately yielding natural essence capsules containing caviar. Example

[0037] Raw material preparation: Weigh the core material components by weight percentage as follows: caviar extract 12%, deep-sea cod skin collagen peptide 6%, sodium hyaluronate 4%, ceramide NP 2.5%, β-glucan 1.5%, nicotinamide 3%, tocopheryl acetate 1.5%, phytosterol 1.5%, polyglutamic acid 0.8%, hydrolyzed elastin 4%, centella asiatica extract 2.5%, calendula extract 1.5%, vitamin C palmitate 0.4%, nano silver 0.02%, fullerene 0.8%, phytosphingosine 1.5%, with the remainder being deionized water.

[0038] Preparation of caviar extract: The amount of compound protease added was 0.6% of the mass of caviar, the enzymatic hydrolysis temperature was 48℃, the time was 3.5h, the inactivation temperature was 86℃, the time was 16min, the centrifugation speed was 8500r / min, the time was 16min, and the solid content after concentration was 22%.

[0039] The deep-sea cod skin collagen peptides have a molecular weight of 1.5 kDa and a purity of 95%; sodium hyaluronate has a molecular weight of 90 kDa; ceramide NP has a purity of 98.5%; β-glucan has a molecular weight of 25 kDa; fullerene has a particle size of 15 nm and a modification degree of 82%; phytosphingosine has a purity of 97% and a melting point of 51℃; other core material raw material parameters are the same as in Example 1. The capsule shell components were weighed by weight percentage as follows: gelatin 32%, glycerin 11%, carrageenan 7%, sorbitol 5.5%, disodium EDTA 0.15%, and deionized water 44.35%, with raw material parameters the same as in Example 1.

[0040] For core material preparation, deionized water was heated to 32°C, and water-soluble components were added sequentially, stirring for 18 minutes until dissolved. Extract components were then added and stirring continued for 22 minutes. Oil-soluble components were then added, and high-speed shear emulsification was performed at 10500 r / min for 16 minutes. High-pressure homogenization was carried out at 22 MPa, and homogenization was performed twice. The pH was adjusted to 6.0 with citric acid, and the viscosity was measured to be 180 mPa·s, yielding the core material.

[0041] After preparing the capsule shell solution by mixing the raw materials, the mixture was stirred in a water bath at 62°C for 32 min, filtered through a 120-mesh sieve, and degassed under vacuum for 22 min at a vacuum degree of -0.082 MPa to obtain a capsule shell solution with a viscosity of 600 mPa·s. The solution was then kept at 52°C for later use.

[0042] The flow rate of the capsule core material was 0.6 mL / min, the flow rate of the capsule shell solution was 1.2 mL / min, the dropper diameter was 0.35 mm, the coolant temperature was 7 °C, the soaking time was 40 min, and other operations were the same as in Example 1.

[0043] The post-processed capsules were washed twice with anhydrous ethanol, dried at 26°C for 16 hours with a moisture content controlled at 6%, sterilized by irradiation at a dose of 7 kGy for 16 minutes, and the finished product was obtained after passing the sealing test. Example

[0044] Raw material preparation: Weigh the core material components by weight percentage as follows: caviar extract 18%, deep-sea cod skin collagen peptide 10%, sodium hyaluronate 7%, ceramide NP 4%, β-glucan 3%, nicotinamide 5%, tocopheryl acetate 2.5%, phytosterol 3%, polyglutamic acid 1.5%, hydrolyzed elastin 6%, centella asiatica extract 4%, calendula extract 3%, vitamin C palmitate 0.8%, nano silver 0.04%, fullerene 1.5%, phytosphingosine 2.5%, with the remainder being deionized water.

[0045] Preparation of caviar extract: The amount of compound protease added was 0.9% of the caviar mass; enzymatic hydrolysis temperature was 52℃, time was 4.5 h; inactivation temperature was 89℃, time was 19 min; centrifugation speed was 9500 r / min, time was 19 min; and the solid content after concentration was 28%. Deep-sea cod skin collagen peptides had a molecular weight of 2.5 kDa and a purity of 97%; sodium hyaluronate had a molecular weight of 110 kDa; ceramide NP had a purity of 99.2%; β-glucan had a molecular weight of 45 kDa; fullerene had a particle size of 25 nm and a modification degree of 88%; phytosphingosine had a purity of 98% and a melting point of 54℃; other core material raw material parameters were the same as in Example 1.

[0046] The capsule shell components were weighed according to the following percentages by weight: gelatin 38%, glycerin 14%, carrageenan 9%, sorbitol 7%, disodium EDTA 0.25%, and deionized water 31.75%. The raw material parameters were the same as in Example 1.

[0047] For core material preparation, deionized water was heated to 38°C, and water-soluble components were added sequentially with stirring for 22 min. Extract components were then added and stirred for 28 min. Oil-soluble components were subjected to high-speed shear emulsification at 11500 r / min for 20 min. High-pressure homogenization was performed at 28 MPa, and the homogenization was repeated three times. The pH was adjusted to 6.5 with triethanolamine, and the viscosity was measured to be 250 mPa·s, yielding the core material.

[0048] After preparing the capsule shell solution by mixing the raw materials, the mixture was stirred in a water bath at 68°C for 38 min, filtered through a 180-mesh sieve, and degassed under vacuum for 28 min at a vacuum degree of -0.088 MPa to obtain a capsule shell solution with a viscosity of 750 mPa·s. The solution was then kept at 58°C for later use.

[0049] The flow rate of the capsule core material was 0.9 mL / min, the flow rate of the capsule shell solution was 1.8 mL / min, the dropper diameter was 0.45 mm, the coolant temperature was 9 °C, the soaking time was 50 min, and other operations were the same as in Example 1.

[0050] The post-processed capsules were washed three times with anhydrous ethanol, dried at 30°C for 20 hours with a moisture content controlled at 7%, sterilized by irradiation at a dose of 9 kGy for 19 minutes, and the finished product was obtained after passing the sealing test.

[0051] Comparative Example Raw material preparation: The components were weighed according to the following percentages by weight: caviar extract 15%, sodium hyaluronate 5%, nicotinamide 4%, tocopheryl acetate 2%, centella asiatica extract 3%, preservative 0.3% (phenoxyethanol), fragrance 0.1%, and the remainder was deionized water. The caviar extract was not enzymatically hydrolyzed and had a molecular weight ≥10kDa; other raw material parameters were the same as in Example 1, but without functional components such as deep-sea cod skin collagen peptides and ceramide NP, and without innovative added ingredients such as fullerene and phytosphingosine.

[0052] The preparation process involves heating deionized water to 35°C, adding sodium hyaluronate and nicotinamide, stirring until dissolved, then adding caviar extract and centella asiatica extract, continuing stirring for 30 minutes, adding tocopheryl acetate, and performing high-speed shear emulsification for 15 minutes at 8000 rpm, without the need for high-pressure homogenization. Preservatives and fragrances are added, stirred until homogeneous, and the pH is adjusted to 6.2. After filtration, the liquid essence is obtained and sealed in ordinary glass bottles.

[0053] Performance testing and comparison Table 1: Details of Raw Material Proportions for Examples and Comparative Examples

[0054] This table presents the differences in raw material composition between the examples and the comparative examples. The core difference lies in the fact that the examples construct a synergistic system of "caviar extract + multiple natural active ingredients + innovative functional components," encompassing moisturizing and anti-aging ingredients such as collagen peptides and ceramide NP, as well as innovative additives like fullerene and phytosphingosine, without preservatives or fragrances. The comparative examples, on the other hand, retain only basic ingredients such as caviar extract and sodium hyaluronate, relying on preservatives and adding fragrances, resulting in a single composition lacking synergy. The examples, through precise control of the weight ratio of each component, achieve a multi-faceted fusion of anti-aging, moisturizing, repairing, and antioxidant effects. The comparative examples, lacking functional and innovative components, struggle to meet multiple skincare needs, clearly demonstrating the innovation and comprehensiveness of the formulation design of this invention.

[0055]

[0056] This table highlights the performance advantages of the capsule product of this invention through key indicators such as dosage form, particle size, and stability. The examples all feature uniform, round capsules of 0.5-2 mm in size, with a core material loading rate of 92%-94%. Viscosity and pH values ​​meet the requirements for skincare products, water content is reasonably controlled, there is no leakage during sealing, and microbial indicators are more stringent. The comparative example is a liquid dosage form, exhibiting slight stratification, lacking core performance parameters such as core material loading rate, and having lower microbial control standards than the examples. The capsule dosage form design not only solves the problem of easy stratification in liquid products but also ensures product stability and safety through excellent sealing and precise process control, verifying the scientific validity and reliability of the preparation process of this invention.

[0057]

[0058] The table presents test data obtained through accelerated storage at 45°C for 3 months, confirming the excellent stability of the product of this invention. In the examples, the retention rates of active ingredients such as caviar extract, sodium hyaluronate, and niacinamide reached 90%-96%, while fullerene and vitamin C palmitate also maintained good stability, with no discoloration, off-odor, or stratification. In the comparative example, the retention rate of the core active ingredients was only 65%-78%, and yellowing, a slight off-odor, and obvious stratification occurred after storage. The difference stems from the fact that the capsule shell of the examples isolates oxygen and light, and multiple components enhance stability through synergistic effects, while the liquid dosage form of the comparative example lacks effective protection, making the active ingredients prone to oxidation and decomposition. The data fully demonstrates that the capsule dosage form and formulation design of this invention can significantly extend the product's shelf life and ensure long-lasting efficacy.

[0059]

[0060] The 30-day volunteer trial data in this table directly reflects the actual skincare effects of the product. The examples demonstrated outstanding performance in skin hydration, elasticity, skin tone brightening, barrier repair, and wrinkle improvement, with Example 3 showing the most significant effect and exhibiting no irritation; overall volunteer satisfaction reached 90%-97%. The comparative examples only showed moderate effects in moisturizing and barrier repair, with slight improvements in skin elasticity and skin tone brightening, and minimal wrinkle improvement. They also had a 6.7% allergy rate, and overall satisfaction was only 65%. The superior efficacy of the examples stems from the synergistic effect of multiple natural active ingredients. The capsule formulation ensures the stability of the active ingredients, further enhancing the skincare effect. In contrast, the comparative examples, due to their single ingredient and the ease with which active ingredients are deactivated, struggle to achieve comprehensive and effective skincare goals, fully demonstrating the market competitiveness of this invention.

[0061] The test data above show that the caviar-containing natural essence capsules prepared in Examples 1 to 3 of this invention are significantly superior to the comparative examples in terms of product performance, stability of active ingredients, and skincare efficacy. The products in the examples are uniformly round capsules with high core material loading, good sealing, and superior microbial indicators. They maintain good stability even without added preservatives or fragrances. In contrast, the comparative examples are liquid, which is prone to separation and discoloration after storage, and has a low retention rate of active ingredients. Regarding skincare efficacy, the examples, due to the synergistic effect of multiple functional ingredients, show significant effects in moisturizing, anti-aging, brightening, and repair, and are non-irritating, resulting in high volunteer satisfaction. The comparative examples, due to their single ingredient and the easy deactivation of active ingredients, have limited skincare effects and also exhibit some irritation. This fully demonstrates that this invention, through innovative ingredient combinations, precise preparation processes, and capsule formulation design, solves the problems of unstable active ingredients, single efficacy, and insufficient safety in existing liquid essences, achieving the goal of natural, efficient, and safe skincare.

[0062] Figure 2 This demonstrates the protective advantages of capsule formulations for active ingredients. The retention rates of caviar extract, sodium hyaluronate, and nicotinamide in the embodiment were significantly higher than in the comparative example, confirming the role of the capsule shell in isolating oxygen and light. In contrast, the liquid formulation in the comparative example, lacking protection, resulted in the active ingredients being easily oxidized and decomposed, leading to a significant decrease in retention rates. This highlights the rationality of the dosage form design in this invention.

[0063] Figure 3 This reflects the product's sustained moisturizing effect. In the example, the skin moisture content steadily increased over the trial period, and the increase was significantly greater than that in the comparative example, reaching a higher level after 28 days. This indicates that the multi-component synergistic moisturizing system of the present invention can continuously replenish and lock in moisture, while the comparative example, due to its single component, had limited moisturizing effect and a slow increase.

[0064] Figure 4 This demonstrates the impact of the preparation process on the uniformity of the core material. In the example, high-speed shear emulsification and high-pressure homogenization resulted in core material particle sizes controlled within 5 μm, with a high proportion of small particles and uniform distribution. In contrast, the comparative example only underwent single emulsification, resulting in a wide particle size distribution and the presence of large particles. This illustrates that the process of this invention can ensure the uniformity of the core material, laying the foundation for optimal efficacy.

[0065] Figure 5 The product's hygienic stability was verified. In the example, after 6 months of storage, the number of microorganisms remained at a low level with no significant proliferation, thanks to the capsule's sealing properties and the antibacterial effect of nano-silver. In the comparative example, the number of microorganisms increased rapidly with storage time, and even with the addition of preservatives, it was difficult to completely control them, highlighting the safety advantages of the product of this invention.

[0066] Figure 6The study demonstrated a synergistic antioxidant effect from multiple components. The tested examples showed excellent performance in DPPH, superoxide anion, and hydroxyl radical scavenging rates, with broad radar chart coverage. In contrast, the comparative examples, lacking synergistic components such as vitamin C palmitate and fullerene, exhibited weak antioxidant capacity, illustrating that the formulation design of this invention can achieve a comprehensive improvement in antioxidant efficacy.

[0067] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A natural essence capsule containing caviar, characterized in that, The essence capsule is composed of a capsule shell and a core material, the core material comprising, by weight percentage: Caviar extract 10-20%; Deep-sea cod skin collagen peptides 5-12%; Sodium hyaluronate 3-8%; Ceramide NP2-5%; β-glucan 1-4%; Nicotinamide 2-6%; Tocopheryl acetate 1-3%; Phytosterols 1-4%; Polyglutamic acid 0.5-2%; Hydrolyzed elastin 3-7%; Centella asiatica extract 2-5%; Calendula extract 1-4%; Vitamin C palmitate 0.3-1%; Nano silver 0.01-0.05%; The remainder is deionized water.

2. The caviar-containing natural essence capsule according to claim 1, characterized in that, It also includes 0.5-2% fullerene, which is a water-soluble modified fullerene with a particle size of 10-30 nm, modified with polyethylene glycol. The fullerene and vitamin C palmitate work synergistically to resist oxidation and form hydrogen bonds with amino acids in caviar extract.

3. The caviar-containing natural essence capsule according to claim 1, characterized in that, It also includes 1-3% phytosphingosine, which has a purity of ≥97%, a melting point of 50-55℃, and forms a lipid bilayer structure with ceramide NP and phytosterol.

4. A natural essence capsule containing caviar according to claim 1, characterized in that, The preparation process of the caviar extract is as follows: Select fresh caviar, remove impurities, wash 2-3 times with physiological saline, add 5-8 times the volume of deionized water, stir well, add compound protease, the amount of enzyme added is 0.5-1% of the weight of caviar, and enzymatically hydrolyze for 3-5 hours at 45-55℃ and pH 6.0-7.

0. After enzymatic hydrolysis, the temperature is raised to 85-90℃ for 15-20 min to inactivate the enzyme. After cooling to room temperature, the mixture is centrifuged at 8000-10000 r / min for 15-20 min. The supernatant is then filtered through an ultrafiltration membrane with a molecular weight cutoff of 5 kDa and concentrated to a solid content of 20-30% to obtain caviar extract.

5. A natural essence capsule containing caviar according to claim 1, characterized in that, The preparation process of the capsule shell is as follows: weigh gelatin, glycerin, carrageenan, sorbitol, and disodium EDTA according to the proportion, add deionized water, stir and dissolve at 60-70℃ for 30-40 minutes, and continue stirring to prevent clumping. After dissolution, filter through a 100-200 mesh sieve to remove impurities, and degas under vacuum for 20-30 minutes at a vacuum degree of -0.08-0.09 MPa to obtain a capsule shell solution with a viscosity controlled at 500-800 mPa·s.

6. A natural essence capsule containing caviar according to claim 1, characterized in that, The complex protease is composed of trypsin, papain, and bromelain in a mass ratio of 2:1:1, with an enzyme activity ≥5000U / g; Centella asiatica extract is prepared by ethanol reflux extraction at a temperature of 70-80℃ for 2-3 hours, with an ethanol volume fraction of 60-70%, and the purity of the extract after concentration and drying is ≥90%; Calendula officinalis extract is prepared by water extraction at a temperature of 80-90℃ for 1.5-2.5 hours, and the solid content after concentration is ≥25%.

7. A natural essence capsule containing caviar according to claim 1, characterized in that, The pH value of the core material is adjusted to 5.5-7.0 by citric acid or triethanolamine, the viscosity is adjusted by adding polyglutamic acid, tocopheryl acetate and vitamin C palmitate are compounded at a mass ratio of 2:1, and the mass ratio of nano silver to plant extract is ≤1:

200.

8. A method for preparing a natural essence capsule containing caviar, used to prepare the natural essence capsule containing caviar as described in any one of claims 1-7, characterized in that, Includes the following steps: S1. Core material preparation: Weigh each core material component according to weight percentage, heat deionized water to 30-40℃, add sodium hyaluronate, ceramide NP, and β-glucan water-soluble components in sequence, stir to dissolve, then add caviar extract and collagen peptides, continue stirring for 30-40 min, then add oil-soluble components, emulsify at high speed for 15-20 min, adjust pH value and viscosity to obtain core material; S2. Preparation of capsule shell solution: Prepare capsule shell solution according to the process described in claim 5, and keep it at 50-60℃ for later use; S3. Capsule Formation: Using the dripping method, the core material and capsule shell solution are injected into the inner and outer tubes of the dripping pellet machine, respectively. The flow rate of the core material is 0.5-1 mL / min, and the flow rate of the capsule shell solution is 1-2 mL / min. The solution is dripped into the coolant liquid paraffin and cooled at 5-10℃. After formation, the capsules are collected. S4. Post-processing: Wash the molded capsules 2-3 times with anhydrous ethanol to remove residual coolant on the surface, and air dry them at 25-30℃ for 12-24 hours. Control the moisture content of the capsules to 5-8%, and screen the products with qualified particle size to obtain natural essence capsules containing caviar.

9. The method for preparing a natural essence capsule containing caviar according to claim 8, characterized in that, After high-speed shear emulsification in step S1, high-pressure homogenization is required, with a homogenization pressure of 20-30 MPa and 2-3 homogenization cycles. In step S3, the viscosity of the coolant liquid paraffin is 100-200 mPa·s, the dropper diameter is 0.3-0.5 mm, and after capsule formation, it is immersed in the coolant for 30-60 minutes.

10. The method for preparing a natural essence capsule containing caviar according to claim 8, characterized in that, After drying in step S4, sterilization is required. Sterilization is performed by irradiation with an irradiation dose of 5-10 kGy and a sterilization time of 15-20 min.

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