Astaxanthin oil extracted from Haematococcus pluvialis and microcapsule product thereof

Abstract

Recipe for a double microencapsulated powder, characterized in that the recipe comprises the following components in parts by weight: 5-60 parts by weight of core material of group A, 5-40 parts by weight of core material of group B, 5-16 parts by weight of protein shell material, 3-19 parts by weight of polysaccharide shell material, 0.1-2 parts by weight of immobilizing enzyme, 1-10 parts by weight of filler, 1-4 parts by weight of pH regulator and 0-2 parts by weight of antioxidant.

Description

Technical field

[0001] The description concerns the technical field of microencapsulated powders and oil extraction, in particular an astaxanthin oil extracted from Haematococcus pluvialis and a microcapsule product thereof. State of the art

[0002] Microcapsule technology is a technology for enclosing a solid, liquid, or gaseous substance in a very small capsule. The capsule typically has one or more layers of thin films to protect the enclosed substance from external influences and to control the type and rate of its release. Microcapsule technology is widely used in various sectors, such as food, pharmaceuticals, cosmetics, and agriculture.

[0003] Conventional microcapsule technologies are often designed for core materials of a specific polarity and cannot simultaneously meet the encapsulation requirements for core materials of different polarities. For example, a microcapsule process for a hydrophilic core material cannot effectively encapsulate a lipophilic core material, and vice versa. Furthermore, conventional methods for encapsulating amphiphilic or insoluble amphoteric core materials typically suffer from low encapsulation efficiency and poor stability.

[0004] To overcome the limitations of conventional microcapsule technologies, a technology for a double microencapsulated powder is required. However, prior art research on double microencapsulated powders with core materials of differing polarities is mostly dependent on technologies that remain in the laboratory phase and are not yet sufficiently established, or the manufacturing process involves the use of large quantities of organic solvents. This limits the practical application of these technologies and their scaling up to industrial production, and makes it difficult to meet the stringent safety requirements in the food and pharmaceutical sectors. To overcome this bottleneck in the prior art, future research should focus on optimizing the manufacturing process for industrial implementation.Furthermore, the amount of organic solvents used should also be strictly controlled in order to reduce the residual solvent, increase the stability and biocompatibility of the microencapsulated powder, and thus enable safe use in more sectors, such as food, pharmaceuticals and cosmetics.

[0005] Therefore, it is urgently necessary to optimize the manufacturing process for a double microencapsulated powder, increase the stability and biocompatibility of the microencapsulated powder, and expand the scope of application to meet more requirements. Disclosure of the utility model

[0006] In one or more embodiments described, a recipe for a double microencapsulated powder is provided, comprising the following components by weight: 5-60 parts by weight of core material of group A, 5-40 parts by weight of core material of group B, 5-16 parts by weight of protein shell material, 3-19 parts by weight of polysaccharide shell material, 0.1-2 parts by weight of immobilizing enzyme, 1-10 parts by weight of filler, 1-4 parts by weight of pH regulator, and 0-2 parts by weight of antioxidant.

[0007] In some embodiments, the core material of group A is selected from lipophilic core materials, and the lipophilic core materials are selected from astaxanthin oils.

[0008] In one or more embodiments described above, the astaxanthin oil is provided from the recipe described above, which is produced using an astaxanthin oil extraction device comprising a mixing vessel, a cavitation agent, a static mixer, a three-phase centrifuge, and a precision filter.The system is designed as follows: the mixing vessel is configured to mix Haematococcus pluvialis, water, and phospholipase to produce a homogeneous sludge; the cavitation agent is configured to take up the sludge and, through hydraulic cavitation, disrupt the cell walls of the sludge to produce a sludge with disrupted cell walls; the static mixer is configured to mix the sludge with disrupted cell walls and an extraction agent to produce a mixed sludge; the three-phase centrifuge is configured to take up the mixed sludge and separate it into three phases to produce an astaxanthin oil phase, an aqueous phase, and a residue; and the precision filter is configured to filter the astaxanthin oil phase to remove the remaining residue and obtain the astaxanthin oil. Brief description of the characters

[0009] The description is further explained by means of exemplary embodiments, which are illustrated in more detail in conjunction with the accompanying figures. These embodiments are not exhaustive. In the embodiments, the same numbers represent the same structures. They show: Fig. 1 a schematic view of an extraction apparatus for astaxanthin oil according to some embodiments of the description; Fig. 2 an exemplary flowchart of an extraction process for astaxanthin oil according to some embodiments of the description; Fig. 3 an optical microscopic image of a sample 1 produced according to Example 2 in accordance with some embodiments of the description; Fig. 4 an optical microscopic image of a sample 2 produced according to Example 3 in accordance with some embodiments of the description; Fig.5 an optical microscopic image of a sample 3 produced according to Example 4 according to some embodiments of the description; Fig. 6 an optical microscopic image of a sample 4 produced according to Example 5 in accordance with some embodiments of the description; Fig. 7 a scanning electron microscopy (SEM) image of a microencapsulated powder prepared according to Example 2 with a composite shell material of fish gelatin and gum arabic according to some embodiments of the description; and Fig. 8 An enlarged scanning electron microscopic (SEM) image of the microencapsulated powder produced according to Example 2 with a composite shell material of fish gelatin and gum arabic according to some embodiments of the description. Detailed descriptions

[0010] To further explain the technical solutions of the embodiments described, the drawings required for illustrating these embodiments are briefly summarized below. Naturally, the following drawings merely represent some examples or embodiments of the description, and a person skilled in the art can apply the description to other similar scenarios without inventive step. Unless otherwise stated or understood from the context, the same reference numerals in the figures represent the same structures or operations.

[0011] As shown in the description and claims, the terms "a" and / or "the" do not necessarily refer to the singular form, but can also include the plural form unless clearly indicated otherwise in the context. Generally, the terms "comprise" and "contain" only include the explicitly stated steps and elements, which do not constitute an exclusive list, so the method or device may also include an additional step or element.

[0012] To overcome the problems of the prior art, the objective of this description is to provide an astaxanthin oil extracted from Haematococcus pluvialis and a microcapsule product thereof. Through precise control of the coacervation particles and the reaction parameters during coacervation, determination of the degree of cross-linking during curing, and regulation of essential steps such as the final spray drying, effective encapsulation of a hydrophilic, lipophilic, amphiphilic, or insoluble amphoteric core material is achieved in the embodiments described. Furthermore, a protein shell material is combined with a polysaccharide shell material to not only enhance the mechanical strength of the microcapsule but also improve its resistance to external environments (such as oxygen, moisture, light, and temperature).This ensures the stability of the microcapsule and its reliability for subsequent applications. This method allows nutrients with different properties to be encapsulated simultaneously in a single capsule, achieving diversity and compatibility of the core material's properties, effectively isolating the core material from negative environmental influences, and maintaining excellent stability even in humid environments. Considering the needs of downstream production and practical application, the exemplary embodiments described here select a specific combination of starting materials and process steps to ensure production efficiency and product quality. The method can find broad application in sectors such as pharmaceuticals, food, and cosmetics, providing a stable and efficient solution.

[0013] In the exemplary embodiments described, a recipe for a double microencapsulated powder is provided, comprising the following components by weight: 5-60 parts by weight of core material of group A, 5-40 parts by weight of core material of group B, 5-16 parts by weight of protein shell material, 3-19 parts by weight of polysaccharide shell material, 0.1-2 parts by weight of immobilizing enzyme, 1-10 parts by weight of filler, 1-4 parts by weight of pH regulator, and 0-2 parts by weight of antioxidant.

[0014] In some embodiments, the core material of group A is selected from lipophilic, amphiphilic and insoluble amphoteric core materials.

[0015] In some embodiments, the lipophilic core material is selected from vegetable oils, animal oils, astaxanthin oils (oils of Haematococcus pluvialis), fat-soluble vitamins, and mixtures thereof. The vegetable oil can be selected from linseed oil, safflower oil, perilla oil, camellia oil, sunflower oil, high-oleic sunflower oil, sea buckthorn kernel oil, soybean oil, pumpkin seed oil, pine nut oil, peony oil, coconut oil, walnut oil, hickory oil, olive oil, hemp seed oil, wheat germ oil, grapeseed oil, rapeseed oil, palm oil, conjugated linoleic acid, conjugated linoleic acid glycerides, medium-chain triglycerides, or silymarin kernel oil. The animal oil can be selected from whipping cream, cream (butter), anhydrous cream (anhydrous butter), or fish oil. The fat-soluble vitamin can be selected from vitamins A, B, D, E (d-α-tocopherol, dl-α-tocopherol, mixed tocopherols) and K.In some embodiments, the amount of lipophilic core material used can be 30–55 parts by weight. In some embodiments, the amount of lipophilic core material used can be 35–53 parts by weight. In some embodiments, the amount of lipophilic core material used can be 40–50 parts by weight.

[0016] In some embodiments, the amphiphilic core material is selected from diglyceride oils, phospholipid oils, glycolipid oils, and mixtures thereof. The diglyceride oil can be selected, for example, from diglyceride oils based on linseed oil, peanut oil, corn oil, rapeseed oil, coconut oil, palm oil, rice oil, soybean oil, sunflower oil, pumpkin seed oil, tomato seed oil, safflower oil, perilla oil, camellia oil, sunflower oil with a high oleic acid content, sea buckthorn kernel oil, pumpkin seed oil, pine nut oil, sea buckthorn oil, peony oil, walnut oil, olive oil, hemp seed oil, wheat germ oil, grapeseed oil, rapeseed oil, palm oil, and silymarin kernel oil. The phospholipid oil can be selected from sunflower phospholipids, soybean phospholipids, krill oil, egg yolk oil, and phospholipid oil derived from algae. The glycolipid oil can be selected from oat oil and rice bran oil. In some embodiments, the amount of amphiphilic core material used can be 8–35 parts by weight.In some embodiments, the amount of amphiphilic core material used can be 9–30 parts by weight. In some embodiments, the amount of amphiphilic core material used can be 10–20 parts by weight.

[0017] In some embodiments, the insoluble amphoteric core material is selected from polyphenols, sparingly soluble amino acids, and mixtures thereof. The polyphenol may be selected, for example, from curcumin, quercetin, rutin, and resveratrol. The sparingly soluble amino acid exhibits low solubility in water and may be selected from leucine, cystine, tyrosine, aspartic acid, glutamic acid, tryptophan, threonine, phenylalanine, methionine, isoleucine, and histidine. In some embodiments, the amount of insoluble amphoteric core material used may be 6–30 parts by weight. In some embodiments, the amount of insoluble amphoteric core material used may be 7–25 parts by weight. In some embodiments, the amount of insoluble amphoteric core material used may be 8–15 parts by weight.

[0018] In some embodiments, the core material of group B is selected from hydrophilic, amphiphilic and insoluble amphoteric core materials.

[0019] In some embodiments, the hydrophilic core material is selected from water-soluble vitamins, highly soluble amino acids, and mixtures thereof. The water-soluble vitamin can be selected, for example, from ascorbic acid, sodium ascorbate, B vitamins (vitamins B1, B2, B3, B5, B6, B7, and B1), adenine, choline, and inositol. The highly soluble amino acid exhibits high solubility in water and can be selected from lysine, arginine, proline, hydroxyproline, glycine, alanine, β-alanine, valine, serine, threonine, cysteamine, citrulline, L-glutamine, and γ-aminobutyric acid. In some embodiments, the amount of hydrophilic core material used can be 8 to 40 parts by weight. In other embodiments, the amount of hydrophilic core material used can be 10 to 35 parts by weight. In some embodiments, the amount of hydrophilic core material used can be 12 - 30 parts by weight.

[0020] For more details on the amphiphilic core material and the insoluble amphoteric core material, please refer to the explanation above.

[0021] An important feature of the embodiments described is that the combination of a protein shell material and a polysaccharide shell material enables the effective encapsulation of a hydrophilic, lipophilic, amphiphilic, or insoluble amphoteric core material. That is, the core materials of group A and group B can have different polarities to achieve the coexistence of nutrients with different properties within a single capsule, thereby ensuring the diversity and compatibility of the core materials' properties.

[0022] In some embodiments, the protein shell material is selected from fish, pork, and beef gelatin, soy protein, pea protein, pumpkin seed protein, hemp protein, chickpea protein, barley protein, and mixtures thereof. In some embodiments, the amount of protein shell material used can be 6–14 parts by weight. In some embodiments, the amount of protein shell material used can be 8–13 parts by weight. In some embodiments, the amount of protein shell material used can be 9–11 parts by weight.

[0023] In some embodiments, the protein shell material has a molecular weight of 50–250 kDa. In some embodiments, the protein shell material has a molecular weight of 60–220 kDa. In some embodiments, the protein shell material has a molecular weight of 70–195 kDa.

[0024] In some embodiments, the polysaccharide shell material is selected from gum arabic, sodium alginate, alginates, chitosan, carrageenan, pectin, starches, modified starches, cellulose, methylcellulose, ethylcellulose, carboxymethylcellulose, and mixtures thereof. In some embodiments, the amount of polysaccharide shell material used can be 4–18 parts by weight. In some embodiments, the amount of polysaccharide shell material used can be 8–17 parts by weight. In some embodiments, the amount of polysaccharide shell material used can be 9–14 parts by weight.

[0025] In some embodiments, the filler is selected from glucose syrup, lactose, maltose, solid corn syrup, oligomeric maltose, and mixtures thereof. In some embodiments, the amount of filler used can be 3 to 9 parts by weight. In some embodiments, the amount of filler used can be 5 to 7 parts by weight.

[0026] In some embodiments, the filler may have a dextrose equivalent (DE) of 40–70. The dextrose equivalent (DE) is a measure of the reductive saccharide content in a starch hydrolysate and indicates the mass percentage of reductive saccharides (calculated as dextrose) in the starch hydrolysate relative to the total dry matter. In some embodiments, the DE value of the filler may be 55–65 parts by weight. In some embodiments, the DE value of the filler may be 50–60 parts by weight.

[0027] In some embodiments, the immobilizing enzyme is primarily glutamine transaminase. In some embodiments, the amount of immobilizing enzyme used can be 0.2–1.5 parts by weight. In some embodiments, the amount of immobilizing enzyme used can be 0.3–1.2 parts by weight. In some embodiments, the amount of immobilizing enzyme used can be 0.5–1.0 parts by weight.

[0028] In some embodiments, the antioxidant is selected from d-α-tocopherol, dl-α-tocopherol, mixed tocopherols, rosemary extract, phospholipids, butylhydroxyanisole, antioxidant 264, t-butylhydroquinone, and mixtures thereof. In some embodiments, the antioxidant is selected from mixed tocopherols, antioxidant 264, rosemary extract, phospholipids, butylhydroxyanisole, and mixtures thereof. In some embodiments, the amount of antioxidant used can be 0–2 parts by weight. In some embodiments, the amount of antioxidant used can be 0.02–1.0 parts by weight. In some embodiments, the amount of antioxidant used can be 0.1–0.2 parts by weight.

[0029] In some embodiments, the rosemary extract is produced according to GB 1886.172-2016 "State Standard for Solvent Safety - Food Additive - Rosemary Extract" by extracting and refining the stem and leaf of rosemary as starting materials using a solvent or supercritical carbon dioxide to produce the rosemary extract as a food additive. The extraction solvent is water, methanol, ethanol, acetone, or n-hexane. The total proportion of antioxidant components (calculated as carnosic acid and carnosol) is ≥ 10%.

[0030] In some embodiments, the pH regulator comprises acidic and basic regulators. In some embodiments, the acidic regulator is selected from citric acid, sulfuric acid, hydrochloric acid, phosphoric acid, malic acid, and mixtures thereof. In one embodiment, the acidic regulator is selected from citric acid and phosphoric acid. In some embodiments, the basic regulator is selected from sodium hydroxide, sodium carbonate, potassium hydroxide, and mixtures thereof. In some embodiments, the basic regulator is sodium hydroxide.

[0031] The process for producing a microencapsulated powder with the recipe described above in this exemplary embodiment of the description comprises the following steps:

[0032] In step (1) the protein shell material is completely dissolved in 50 - 150 parts by weight of water.

[0033] In step (2) the polysaccharide shell material is completely dissolved in 30 - 190 parts by weight of water.

[0034] In step (3) the liquids produced in step (1) and step (2) are mixed sufficiently.

[0035] In step (4) 0 - 1 parts by weight of antioxidant is added to the core material of group A and mixed sufficiently.

[0036] In step (5) 30 - 70 wt% of the liquid produced in step (3) and the liquid produced in step (4) are mixed and emulsified by shearing at a speed of 5000 - 9000 rpm to obtain a concentrated emulsion with a mass concentration of 55 - 65 wt%.

[0037] In step (6) 0 - 1 parts by weight of antioxidant are added to the core material of group B.

[0038] In step (7) the remaining amount of liquid produced in step (3) and the liquid produced in step (6) are mixed and emulsified by shearing at a speed of 5000 - 9000 rpm to obtain a concentrated emulsion.

[0039] In step (8), the concentrated emulsion prepared in step (5) is diluted to a solids content of 4–7 wt%. The pH of the diluted emulsion is then adjusted to 5.0–5.2 and the particle size D90 of the system to 2–20 µm. The emulsion is cooled and hardened by adding an immobilizing enzyme to form a first layer of multinucleated microcapsules. The immobilizing enzyme is then deactivated. In some embodiments, the pH of the diluted emulsion can be adjusted to 5.10–5.15 and the particle size D90 of the system to 3–18 µm, but also to 4–15 µm.

[0040] In step (9), the concentrated emulsion prepared in step (7) is mixed with the emulsion from step (8). The pH is then adjusted to 4.4–4.5 and the particle size D90 of the system to 20–50 µm. The mixture is cooled and hardened by adding an immobilizing enzyme to form a second layer of multinucleated microcapsules. The immobilizing enzyme is then deactivated. In some embodiments, the pH can be adjusted to 4.43–4.48 and the particle size D90 of the system to 30–40 µm, but also to 35–40 µm.

[0041] In some embodiments, the total amount of immobilizing enzyme in steps (8) and (9) is 0.1 - 2 parts by weight, and the amount of immobilizing enzyme used in step (8) is 50 - 60% by weight of this, while the remaining amount of immobilizing enzyme is used in step (9).

[0042] In step (10), a filler is added to step (9), mixed until completely dissolved, and dried by spraying to obtain the doubly microencapsulated powder. In some embodiments, the DE value of the filler is 40–70 parts by weight. In some embodiments, the DE value of the filler can be 45–65 parts by weight. In some embodiments, the DE value of the filler can also be 50–60 parts by weight.

[0043] In steps (8) and (9), a commercially available immobilizing enzyme is used. Immobilization is achieved by heating the emulsion containing this enzyme to 50–55°C and maintaining this temperature for 2–3 hours. The temperature is then increased to 90–95°C and held for 20–30 minutes. If no obvious cracking occurs, the curing process is considered complete.

[0044] In the exemplary embodiments described, a double-microencapsulated powder for core materials with different polarities, produced according to the above-described recipe, is also provided. This powder is multilayered and multinucleated with polyunsaturated fats and exhibits high insulating properties and resistance to comminution. The powder comprises the core materials of Group A and Group B with different polarities. In some exemplary embodiments, the particle size D90 of the multinucleated microcapsule of the first layer is in the range of 2–20 µm. In some exemplary embodiments, the particle size D90 of the multinucleated microcapsule of the first layer can be in the range of 3–18 µm. In some exemplary embodiments, the particle size D90 of the multinucleated microcapsule of the first layer can also be in the range of 4–15 µm.In some embodiments, the particle size D90 of the multinucleated microcapsule of the second layer is in the range of 20–50 µm. In some embodiments, the particle size D90 of the multinucleated microcapsule of the second layer can be in the range of 30–40 µm. In some embodiments, the particle size D90 of the multinucleated microcapsule of the second layer can also be in the range of 35–40 µm.

[0045] The exemplary embodiments described above demonstrate the use of the microencapsulated powder in food or health products.

[0046] In some embodiments, it is used in tablets, powdered medicines, confectionery, gums, soft capsules, baked goods, milk powder, yogurt, liquid and solid drinks, energy bars, cheeses, nutritional supplements, various sauces and ice creams.

[0047] In some embodiments of the description, the recipe for the double microencapsulated powder has the following advantages: (1) Versatility and compatibility: By the specific combination of starting materials and process steps, a double microencapsulated powder can be produced with core materials of different polarities (such as hydrophilic, lipophilic, amphiphilic and insoluble amphoteric) so that nutrients of different properties can be encapsulated simultaneously in a single capsule and the versatility and compatibility of the product are greatly improved.(2) Improved stability: The microencapsulated powder effectively isolates the core material from the negative effects of environmental factors (such as oxygen, humidity, light, and temperature changes) and maintains excellent stability even in humid environments. This not only extends the product's shelf life but also ensures the efficacy and safety of the active ingredients. (3) Optimization of the production process: The key steps described include the preparation of the coacervation phases of core materials with different polarities, the fine-tuning of the coacervation particles, the reaction parameters during coacervation, and the degree of cross-linking during curing, as well as the final spray drying. These steps ensure consistent and controllable product quality and are suitable for industrial mass production.(4) Environmental friendliness: The design of the process avoids pollution from organic solvents, reduces the use of chemical additives, and meets the requirements of green production and environmental protection. Furthermore, it simplifies production processes, reduces production costs, and achieves economic benefits. (5) High encapsulation and low surface area: The results of the experiments show that the microencapsulated powder produced according to the embodiments described exhibits excellent encapsulation and a low surface area (≤ 2%) to ensure effective protection and release of the core materials, thereby increasing the overall quality of the product.(6) Good properties for tablet pressing: The microencapsulated powder produced in this way exhibits good hardness and friability during tablet pressing, ensuring that tablet quality standards regarding completeness and degree of disintegration are met. This guarantees the effective dissolution of the pharmaceutical components and prevents tablet breakage, which facilitates subsequent coating, packaging, and transfer. (7) Wide application: The microencapsulated powder finds application in many sectors, including but not limited to tablets, powdered medications, confectionery, gums, softgels, baked goods, milk powder, yogurt, liquid and solid beverages, energy bars, cheese, nutritional supplements, various sauces, and ice cream. Such a wide application provides more opportunities for product development.

[0048] In some embodiments, the core material of group A is selected from lipophilic core materials, and the lipophilic core materials are selected from astaxanthin oils. In some embodiments, the astaxanthin oil is produced using an astaxanthin oil extraction device.

[0049] Fig. Figure 1 is a schematic view of an extraction apparatus for astaxanthin oil according to some embodiments described in the description. As in Fig.Figure 1 shows an extraction apparatus for astaxanthin oil 100 comprising a mixing vessel 110, a cooler 120, a cavitation agent 130, a feed pump for mixed materials 140, a three-phase centrifuge 150, a storage vessel for oleoresin 160, a waste storage vessel 170, a waste storage vessel 180, a tank for extraction agent 190, a feed pump for extraction agent 1100, a storage vessel for sludge with destroyed cell walls 1110, a feed pump for sludge with destroyed cell walls 1120, a static mixer 1130 and a precision filter 1140.

[0050] The mixing vessel 110 is a container in which the starting materials are premixed. For example, the starting materials include Haematococcus pluvialis, water, phospholipase, etc.

[0051] In some embodiments, the mixing vessel 110 is configured to mix Haematococcus pluvialis, water and phospholipase to produce a uniform sludge.

[0052] The cavitation agent 130 is a device for hydraulic cavitation of the sludge to destroy the cell walls of the sludge. In some embodiments, the cavitation agent 130 is configured to take up the sludge and destroy the cell walls of the sludge by hydraulic cavitation to produce sludge with destroyed cell walls. For more details on hydraulic cavitation, see [reference to be inserted here]. Fig. 2 and the description for it are referenced.

[0053] The static mixer 1130 is a device that mixes sludge with damaged cell walls and an extraction solvent. The static mixer 1130 achieves this mixing of the sludge with damaged cell walls and the extraction solvent simply through the flow of the two, without any mechanical drive.

[0054] In some embodiments, the static mixer 1130 is configured to mix the sludge with destroyed cell walls and the extraction agent to produce a mixed sludge.

[0055] The three-phase centrifuge 150 is a device that separates the components of mixed sludge into three phases. These components are the oily components, the aqueous components, and the solid residue from the mixed sludge, corresponding to an astaxanthin oil phase, an aqueous phase, and a residue from the mixed sludge, respectively. The three-phase centrifuge 150 also includes an outlet for the oily phase, an outlet for the aqueous phase, and an outlet for the solid phase, which are connected to the precision filter 1140, the wastewater storage tank 170, and the waste storage tank 180, respectively.

[0056] In some embodiments, the three-phase centrifuge 150 is configured to receive the mixed sludge and separate it into three phases to produce an astaxanthin oil phase, an aqueous phase and a residue.

[0057] The Precision Filter 1140 is a device for deep filtration of the astaxanthin oil phase. In some embodiments, the Precision Filter 1140 is configured to filter the astaxanthin oil phase to remove the remaining residue and obtain the astaxanthin oil. For more details on the Precision Filter 1140, see [link / reference]. Fig. 2 and the relevant description for it are referenced.

[0058] In some embodiments, the extraction device for astaxanthin oil 100 further comprises the cooler 120. The cooler 120 is configured to receive the sludge with destroyed cell walls from the cavitation agent 130, cool it, and transfer it to the static mixer 1130.

[0059] In some embodiments, the astaxanthin oil extraction apparatus 100 further comprises several power pumps. A power pump is a pump that provides the force for the flow of materials. The several power pumps include the feed pump for mixed materials 140, the feed pump for sludge with disrupted cell walls 1120, and the feed pump for extraction solvent 1100.

[0060] In some embodiments, the feed pump for mixed materials 140 is configured to provide power for the transfer of the sludge in order to transfer the sludge from the mixing vessel 110 to the cavitation medium 130.

[0061] In some embodiments, the feed pump for sludge with destroyed cell walls 1120 is configured to provide power for the transfer of the sludge with destroyed cell walls in order to transfer the sludge with destroyed cell walls in the storage tank for sludge with destroyed cell walls 1110 from the cavitation medium 130 to the cooler 120.

[0062] In some embodiments, the feed pump for extraction solvent 1100 is configured to provide power for the transfer of the extraction solvent in order to introduce the extraction solvent in the container for extraction solvent 190 into the static mixer 1130.

[0063] In some embodiments, the astaxanthin oil extraction apparatus 100 further comprises several storage containers for storing the materials during or after the extraction of the astaxanthin oil. For example, the several storage containers include the storage container for sludge with destroyed cell walls 1110, the storage container for oleoresin 160, the wastewater storage container 170, the waste storage container 180, and the container for extraction solvent 190.

[0064] In some embodiments, the storage tank for sludge with destroyed cell walls 1110 is configured to store the sludge with destroyed cell walls.

[0065] In some embodiments, the storage container for oleoresin 160 is configured to store the astaxanthin oleoresin separated during the three-phase separation.

[0066] In some embodiments, the wastewater storage tank 170 is configured to store the aqueous phase separated during the three-phase separation.

[0067] In some embodiments, the waste storage container 180 is configured to store the residue separated during the three-phase separation process.

[0068] In some embodiments, the container for extraction solvent 190 is configured to store the extraction solvent.

[0069] In some embodiments, the extraction device for astaxanthin oil 100 further comprises a pipe valve 1150, as shown in Fig.Figure 1 shows the pipe valve 1150, which controls the direction of sludge transfer to change it during the cyclic cell wall destruction process. For example, the pipe valve 1150 could be a gate valve. After the cyclic cell wall destruction process is complete, switching the pipe valve 1150 controls the sludge flow, transferring it to the storage tank for sludge with destroyed cell walls 1110 to complete the cycles. For more details on the cyclic cell wall destruction process, see Figure 1. Fig. 2 and the description for it are referenced.

[0070] In some embodiments, the astaxanthin oil extraction device 100 further comprises a processing device 1160. The processing device 1160 can process the data and / or information from the components in the astaxanthin oil extraction device 100 and / or from an external data source. In some embodiments, the processing device 1160 can execute program instructions based on this data, information, and / or processing results to perform one or more functions mentioned in the description. For example, the processing device 1160 can execute one or more steps in the sequence 200.

[0071] In some embodiments, the processing device 1160 can be a single server or a group of servers. The group of servers can be centrally or decentrally located. In some embodiments, the processing device 1160 can be located locally or remotely. In some embodiments, the processing device 1160 can be implemented on a cloud platform. For example, the cloud platform can include a private cloud, a public cloud, a mixed cloud, a community cloud, a distributed cloud, an internal cloud, a multi-tiered cloud, and any combination thereof. In some embodiments, the processing device 1160 can be a field-programmable gate array (FPGA) or a digital signal processor (DSP). In some embodiments, the processing device 1160 can be integrated into or incorporated into the astaxanthin oil extraction device 100.

[0072] In some embodiments described above, the integration and combination of modular components, such as the mixing vessel, cavitation agent, static mixer, three-phase centrifuge, precision filter, etc., allows for a streamlined astaxanthin oil extraction process, significantly increasing extraction efficiency and product quality of the astaxanthin oil eoresin. Furthermore, the modular components are conventional and well-established, resulting in low maintenance costs and facilitating system integration and application in industrial mass production. Hydraulic cavitation is used instead of traditional cell wall disruption techniques, thus significantly reducing the energy consumption of the astaxanthin oil extraction system.The inclusion of a cooler effectively prevents the thermal degradation of the active components of astaxanthin during cell wall disruption and extraction, thus improving the extraction rate of astaxanthin oil and the stability of the product. The high-precision purification of the astaxanthin oil phase using the precision filter results in astaxanthin oil with high purity and low residue content.

[0073] Fig. Figure 2 is an exemplary flowchart of an extraction process for astaxanthin oil according to some embodiments described. In some embodiments, step 200 can be carried out with a processing unit in the astaxanthin oil extraction unit. As shown in Fig. As shown in Figure 2, the process 200 comprises the following steps.

[0074] In step 210, Haematococcus pluvialis, water and phospholipase are dosed into a mixing container and mixed to produce a uniform sludge.

[0075] Phospholipase is an enzyme that is added to the mixing container to break down the emulsion components of the phospholipid and glycolipid types in the cells of Haematococcus pluvialis.

[0076] Haematococcus Pluvialis is a single-celled alga in freshwater, belonging to Haematococceae, Chlorophyceae, Chlorophyta.

[0077] The sludge refers to a fluid mixture of Haematococcus pluvialis, water and phospholipase.

[0078] In some embodiments, Haematococcus pluvialis, water, and phospholipase can be dosed and mixed in a mass ratio into the mixing vessel to produce a uniform sludge. This mixing can be achieved by circulating the fluid, by stirring, or by another method to ensure the uniform distribution of Haematococcus pluvialis, water, and phospholipase.

[0079] The aim here is to ensure good flowability and stability of the sludge during mixing and cell wall disruption, to promote the subsequent disruption of the sludge cell walls, and to avoid both difficulties in transferring the sludge due to excessive concentration and a reduction in astaxanthin concentration due to excessive dilution. Therefore, in some embodiments, the mass ratio of Haematococcus pluvialis to water is 1:4 to 1:11. In some embodiments, the mass ratio of Haematococcus pluvialis to water can be 1:3 to 1:10. In some embodiments, the mass ratio of Haematococcus pluvialis to water can also be 1:5 to 1:10.

[0080] The aim is also to effectively separate the emulsion components, such as phospholipids and glycolipids, within the cells of Haematococcus pluvialis, thereby significantly facilitating oil-water separation and increasing the purity and extraction efficiency of the astaxanthin oil. Therefore, in some embodiments, the amount of phospholipase used is 0.5% to 5.5% of the mass of Haematococcus pluvialis. In some embodiments, the amount of phospholipase used can be 1% to 5% of the mass of Haematococcus pluvialis. In some embodiments, the amount of phospholipase used can even be 2% to 5% of the mass of Haematococcus pluvialis.

[0081] In some embodiments of the description, adjusting the mass ratio of Haematococcus pluvialis to water within the aforementioned range (e.g., 1:3 to 1:10) ensures good flowability and stability of the sludge during mixing and cell wall disruption, promotes subsequent cell wall disruption of the sludge, and avoids both difficulties in transferring the sludge due to excessive concentration and a reduction in astaxanthin concentration due to excessive dilution. Adjusting the amount of phospholipase used within the aforementioned range (e.g., 1%–5% of the mass of Haematococcus pluvialis) effectively separates the emulsion components, such as phospholipids and glycolipids, within the cells of Haematococcus pluvialis, significantly facilitating oil-water separation and increasing the purity and extraction efficiency of the astaxanthin oil.

[0082] In some embodiments, the phospholipase is selected from phospholipase A1, phospholipase A2, phospholipase B, and mixtures thereof. Depending on the type of phospholipase, a person skilled in the art can adjust the ratio of Haematococcus pluvialis to water and the amount of phospholipase used to achieve better emulsion breakdown. For example, when phospholipase B is used, a mass ratio of Haematococcus pluvialis to water of 1:5 and an amount of phospholipase of 2% to 4% of the mass of Haematococcus pluvialis can be chosen. When, for example, a combination of phospholipases A1 and A2 is used, a mass ratio of Haematococcus pluvialis to water of 1:10 and an amount of phospholipase of approximately 2% of the mass of Haematococcus pluvialis can be chosen.By using different phospholipases, the efficiency of phospholipase degradation of components within the algal cells can be optimized by appropriately adjusting the mass ratio of Haematococcus pluvialis to water. Furthermore, adjusting the amount of phospholipase used can synergistically increase both the cell wall destruction effect of the sludge and the extraction rate of astaxanthin oil.

[0083] In some embodiments, the use of phospholipase A1, phospholipase A2, phospholipase B or a combination thereof can achieve better suitability and stability compared to phospholipases of other types in the degradation of the emulsion structure in the cells of Haematococcus pluvialis, efficient degradation of the emulsion components of the phospholipid and glycolipid types at a low dosage, and thus promote the release of astaxanthin and the effective stratification of the oily and aqueous phases.

[0084] In step 220, the sludge is fed to the cavitation agent via the mixed materials feed pump, where the cell walls of the sludge are cyclically destroyed.

[0085] In some embodiments, the feed pump for mixed materials can be connected via lines to both the outlet of the mixing vessel and the inlet of the cavitation agent. After the sludge has been generated in the mixing vessel, it can be transferred to the cavitation agent by the force provided by the feed pump for mixed materials.

[0086] Hydraulic cavitation is the cavitation of the liquid due to a high local flow velocity and a low local pressure when the sludge flows through the cavitating agent.

[0087] In some embodiments, the destruction of the sludge cell walls involves the destruction of the cell walls of Haematococcus pluvialis in the sludge by means of the mechanical shear force and energy pulse generated by hydraulic cavitation. Specifically, the sludge is introduced into the cavitation medium by the feed pump for mixed materials, and as it flows through a section of the cavitation medium with a sudden structural change (e.g., a constriction or nozzle), a large number of cavitated bubbles are formed due to a local, significant increase in flow velocity and a rapid decrease in pressure. Upon pressure return, the bubbles rapidly rupture, generating strong mechanical shear forces and energy pulses that act on Haematococcus pluvialis in the sludge to destroy its cell walls and thereby release fat-soluble active substances such as astaxanthin.

[0088] In some embodiments, the processing equipment can perform the cyclical disruption of the sludge cell walls. This cyclical disruption involves hydraulic cavitation of the sludge using the cavitation medium and subsequent cooling by the chiller. In each cycle, the sludge is introduced into the cavitation medium by the feed pump for mixed materials, where cavitated bubbles are formed to disrupt the cell walls of Haematococcus pluvialis in the sludge. It is then cooled by the chiller to prevent the thermal degradation of the astaxanthin. The cooled sludge is returned to the mixing tank and prepared for the next cycle.

[0089] In step 230, the cyclic destruction of the cell walls is stopped in response to the fact that the duration of the cyclic destruction of the cell walls and the destruction rate of the cell walls reach predetermined thresholds in order to produce a sludge with destroyed cell walls.

[0090] In some embodiments, the processing device can stop the cyclic destruction of the cell walls by switching the pipe valve after the cyclic destruction of the cell walls has ended, and transfer the sludge with destroyed cell walls to the storage tank for sludge with destroyed cell walls, in order to later transfer it together with the extraction agent for mixing into the static mixer.

[0091] The predetermined thresholds include a duration of cyclic cell wall destruction of 0.5 hours to 3 hours and a cell wall destruction rate in the sludge sample of more than 90%.

[0092] In some embodiments, the duration of cyclic cell wall destruction is less than 4 hours. To achieve sufficient cell wall destruction of the algae and to ensure extraction efficiency and product stability, the duration of cyclic cell wall destruction can preferably be between 0.5 and 3 hours. In some embodiments, the duration of cyclic cell wall destruction can also be between 2 and 3 hours.

[0093] The circulating water is the water used as a coolant in the radiator. For example, the circulating water could be condensed water, as in Fig.Figure 1 shows that the circulating water can indirectly exchange heat with the sludge to reduce the temperature increase of the sludge during the cyclical disruption of the cell walls. In some embodiments, the temperature of the circulating water in the cooler (i.e., the temperature of the condensed water) is not higher than 20°C. To suppress the degradation of astaxanthin during the release of fat-soluble active substances such as astaxanthin, which is caused by the temperature increase, and thus to ensure the extraction efficiency and stability of the product, the temperature of the circulating water in the cooler can preferably be in the range of 5–15°C. In some embodiments, the temperature of the circulating water in the cooler can be in the range of 8–10°C.

[0094] In some embodiments of the description, the duration for the destruction of the cell walls is kept within a certain range (such as between 0.5 hours and 3 hours) and the temperature of the circulating water in the cooler is kept within a certain range (such as not exceeding 20°C) in order to suppress the degradation of astaxanthin caused by an increase in temperature while ensuring sufficient destruction of the algal cell walls and release of the fat-soluble active substances, such as astaxanthin, and thus guaranteeing the extraction efficiency and stability of the product.

[0095] In step 240, the sludge with destroyed cell walls, along with the extraction agent, is fed to the static mixer for mixing to produce a mixed sludge.

[0096] The extraction solvent is an oily material used to extract a fat-soluble active substance, such as astaxanthin, from sludge with damaged cell walls. The extraction solvent can be pre-filled into the extraction solvent container.

[0097] In some embodiments, the extraction agent is a medium-chain fatty acid glyceride (MCT) or an ethylated vegetable oil.

[0098] In some embodiments of the description, the use of a medium-chain fatty acid glyceride (MCT) or an ethylated vegetable oil as the extraction solvent can significantly increase the efficiency of the subsequent astaxanthin extraction and the astaxanthin content in the oily phase. Compared to natural vegetable oils (such as coconut oil), a modified oil or fat with a low viscosity (such as a medium-chain fatty acid glyceride, ethylated safflower oil, ethylated sunflower oil, and the like) as an extraction solvent exhibits lower viscosity and better flowability and is difficult to emulsify, thus facilitating subsequent oil-water separation and significantly increasing the separation efficiency and purity of the product during astaxanthin extraction.Furthermore, no solvent needs to be removed, thus avoiding the problem of residual solvent and making the process simpler and more reliable. In addition, MCT and ethylated vegetable oils are food-grade oils and fats, suitable for use in sectors such as solvents and health products due to their good stability and safety, and effectively avoid the problem with traditional organic solvents of incomplete emulsion formation or insufficient dissolution capacity.

[0099] The mixed sludge refers to a liquid mixture of the sludge with disrupted cell walls and the extraction solvent mixed with it. In some embodiments, the mixed sludge is a three-phase system consisting of an oily phase, an aqueous phase, and a solid phase. The oily phase consists predominantly of a medium-chain fatty acid glyceride or ethylated vegetable oil, which serves as the extraction solvent, and is used to dissolve the fat-soluble active substances, such as astaxanthin, from the sludge with disrupted cell walls. The aqueous phase originates from the water in the sludge with disrupted cell walls and includes some of the insoluble impurities. The solid phase comprises the remaining fragments of the algal cells after the cell walls have been disrupted.

[0100] In some embodiments, the damaged cell wall sludge or the extraction solvent can be fed to the static mixer by the damaged cell wall sludge feed pump or the extraction solvent feed pump, respectively, to produce a mixed sludge. Specifically, the damaged cell wall sludge can be drawn from the damaged cell wall storage tank by the damaged cell wall sludge feed pump, and the extraction solvent can be drawn from the extraction solvent storage tank by the extraction solvent feed pump via a tube and fed to the static mixer at a specific feed rate ratio. The static mixer can achieve the mixing of the damaged cell wall sludge and the extraction solvent through the flow of the fluids without mechanical drive to produce a mixed sludge.By adjusting the feed rate ratio, sufficient contact and mixing of the sludge with damaged cell walls and the oily extraction solvent can be ensured to promote efficient astaxanthin transfer and optimize the effectiveness of the subsequent separation by the three-phase centrifuge. The feed rate ratio can be preset by a person skilled in the art, depending on the materials. For example, the feed rate ratio of the sludge with damaged cell walls to the extraction solvent can be 2:1. For more details on the feed rate ratio, please refer to Tables 1 and 2 and the accompanying descriptions.

[0101] In some embodiments, the amount of extraction solvent used is 0.2 to 6 times the dry weight of Haematococcus pluvialis. To reduce the amount of extraction solvent used while achieving sufficient astaxanthin extraction, to ease the burden during subsequent concentration and separation of the oily phase, and to improve overall extraction efficiency and cost control, the amount of extraction solvent used is preferably 0.3 to 5 times the dry weight of Haematococcus pluvialis.

[0102] In some embodiments, the sludge with disrupted cell walls and the extraction solvent can be continuously fed to the static mixer. The amount of extraction solvent used can be adjusted by the feed rate ratio of the sludge with disrupted cell walls to the extraction solvent. For example, with a feed rate ratio of 2:1, the amount of extraction solvent used is twice the dry weight of Haematococcus pluvialis. Similarly, with a feed rate ratio of 11:5, the amount of extraction solvent used is five times the dry weight of Haematococcus pluvialis.

[0103] In some embodiments of the description, by adjusting the amount of extraction agent used within a range (e.g., between 0.3 and 5 times the dry amount of Haematococcus pluvialis) while ensuring sufficient extraction of astaxanthin, the amount of extraction agent used can be reduced, the burden on the subsequent concentration and separation of the oily phase eased, and the overall efficiency of the extraction and cost control improved.

[0104] In step 250, the mixed sludge is fed to the three-phase centrifuge for separation to produce an astaxanthin oil phase, an aqueous phase and a residue.

[0105] In some embodiments, the processing equipment can feed the mixed sludge to the three-phase centrifuge for separation to produce an astaxanthin oil phase, an aqueous phase, and a residue. Specifically, a strong centrifugal force field can be generated in the three-phase centrifuge at high speed, and the mixed sludge is separated into the astaxanthin oil phase, the aqueous phase, and the residue based on the differences in density between the oily phase, the aqueous phase, and the solid phase. The outlets for the oily phase, the aqueous phase, and the solid phase are connected to the precision filter, the wastewater storage tank, and the waste storage tank, respectively. The aqueous phase and the residue can then be fed into the wastewater storage tank and the waste storage tank, respectively.After filtering through the precision filter, the astaxanthin oil phase can be introduced into the storage container for oleoresin. This allows for the independent collection and storage of the astaxanthin oil phase, the aqueous phase, and the residue.

[0106] In some embodiments, the rotational speed of the three-phase centrifuge is in the range of 2000 rpm to 7000 rpm. To ensure efficient separation while avoiding excessive energy consumption and wear on the astaxanthin oil extraction unit, thereby reducing operating costs, effectively preventing astaxanthin degradation due to elevated temperatures during separation, and thus increasing the astaxanthin extraction rate and the purity of the oily phase, as well as extending the service life of the astaxanthin oil extraction unit, the rotational speed of the three-phase centrifuge is preferably in the range of 3000 rpm to 6000 rpm.

[0107] In some embodiments of the description, adjusting the rotational speed of the three-phase centrifuge in the range of 3000 rpm to 6000 rpm can ensure the efficiency of the separation, avoid excessive energy consumption and wear on the astaxanthin oil extraction unit, reduce operating costs, effectively prevent the degradation of astaxanthin due to increased temperature during separation, and thereby increase the astaxanthin extraction rate and the purity of the oily phase, as well as extend the service life of the astaxanthin oil extraction unit.

[0108] In step 260, the astaxanthin oil phase is filtered through a precision filter to remove the remaining residue and obtain the astaxanthin oil eoresin.

[0109] In some embodiments, the astaxanthin oil phase obtained by separation using the three-phase centrifuge can be filtered through the precision filter to remove the remaining residue and obtain the astaxanthin oil eoresin. In particular, a micrometer filter can be used in the precision filter, which separates the remaining residue in the oily phase by physical sieving and trapping. The filtered astaxanthin oil phase can be introduced into the oil eoresin storage container to obtain astaxanthin oil eoresin of high purity, suitable for further processing or immediate application.

[0110] In some embodiments, the filter precision of the precision filter is 3000 mesh. To effectively remove the residue of small particle sludge in the astaxanthin oil phase, to avoid settling, oxidation and deterioration of product quality due to the remaining impurities, and thus to increase the purity and quality of the filtered astaxanthin oil eoresin, the filter precision of the precision filter is preferably at least 2000 mesh.

[0111] In some embodiments of the description, by adjusting the filter precision of the precision filter to a certain range (e.g. 2000 mesh or more), the residue of small particle size sludge in the astaxanthin oil phase can be effectively removed, settling, oxidation and deterioration of product quality due to the remaining impurities can be avoided, and thus the purity and quality of the filtered astaxanthin oil eoresin can be increased.

[0112] In some embodiments of the process, the sludge is fed to the cavitating agent, and the cell walls of the sludge are cyclically disrupted by hydraulic cavitation. During this cyclic disruption, the sludge is cooled by a chiller. Under the influence of hydraulic cavitation, the generated mechanical energy effectively disrupts the cell wall structures of the algae, facilitating the release of fat-soluble active components such as astaxanthin. The chiller suppresses thermal degradation caused by local heating during processing, thereby increasing the activity and stability of the product. Compared to traditional cell wall disruption methods, this process offers advantages such as a significant reduction in consumption, continuous operation, high production efficiency, and an increased astaxanthin extraction rate.Furthermore, the equipment used, such as the three-phase centrifuge, the static mixer, etc., are standard industrial devices that are inexpensive to manufacture and suitable for mass production. The separation process using the three-phase centrifuge also allows the astaxanthin oil phase to be obtained, and the precision filter removes fine impurities to yield pure and stable astaxanthin oil eoresin, which is suitable for further processing or direct application.

[0113] It should be noted that the above description of process 200 serves only as an example and does not limit the scope of the description. It should be clear to those skilled in the art that various modifications and changes to the process are possible under the teachings of the description. However, these modifications and changes remain within the scope of the description. Example

[0114] The non-restrictive embodiments serve to further explain the technical solutions and effects of the description and should in no way be understood as limiting the content of the invention. Example 1: Extraction of highly purified astaxanthin oil

[0115] Experimental groups 1 to 8 were adjusted with respect to the ratio of starting materials, the type and amount of phospholipase used, the cooling water temperature, the time required for cell wall disruption, the feed rate ratio of the sludge with disrupted cell walls to the extraction solvent, and the centrifuge speed. The specific process parameters and the effect of astaxanthin extraction are shown in Tables 1 and 2. For example, as shown in experimental group 1 from Tables 1 and 2, in the processing setup, Haematococcus pluvialis and water could be fed into the mixing vessel in a mass ratio of 1:3, phospholipase B could be added at a rate of 2% of the dry weight of Haematococcus pluvialis, and they could be mixed to form a homogeneous sludge. The sludge was then fed to the cavitation solvent by the feed pump.At a cooling water temperature of 8°C, the cell walls were cyclically destroyed by hydraulic cavitation for 3 hours. Once the cell wall destruction rate exceeded 90%, the cyclic cell wall destruction was stopped to obtain a sludge containing destroyed cell walls. This sludge and a medium-chain triglyceride (MCT) were then fed to a static mixer at a rate of 2:1 to obtain a mixed sludge. The mixed sludge was then fed into a three-phase centrifuge for separation at a centrifuge speed of 3000 rpm. After filtration through a precision filter, an astaxanthin oil with an extraction rate of 85% and an astaxanthin content of 4.4% was obtained. Experimental groups 2 to 8 are as shown in Tables 1 and 2, which are not discussed further here. Table 1 Experimental group 1 Experimental group 2 Experiment group 3 Experimental group 4 Experimental group 5 ratio of Haematococcus pluvialis to water 1 : 3 1 : 5 1 : 10 1 : 5 1 : 5 Type of phospholipase Phospholipase B Phospholipase B Phospholipase A1+Phospholipase A2 Phospholipase B Phospholipase A1 Amount of phospholipase used 2% 2% 2% 4% 5% Cooling water temperature 8°C 10°C 10°C 10°C 10°C Time required for the destruction of cell walls 3h 3h 2h 3h 3h Destruction rate of cell walls 90% 97% 99,5% 97% 97% Extraction solvent MCT MCT MCT Ethylated sunflower oil ethylated safflower oil feed rate ratio of the sludge with destroyed 2 : 1 6 : 1 11 : 5 3 : 1 6 : 0, 3 cell walls to the extraction agent Ratio of dry substances from extraction solvent to Haematococcus pluvialis 2 : 1 1 : 1 5 : 1 2 : 1 0,3 : 1 Centrifuge speed 3000 RPM 6000 RPM 6000 RPM 6000 RPM 6000 RPM Extraction rate of astaxanthin oil 85% 93% 98% 96% 86% Astaxanthin content 4,4% 7,3% 2,2% 4,7% 12,1% Table 2 Experimental group 6 Experimental group 7 Experimental group 8 ratio of Haematococcus pluvialis to water 1 : 10 1 : 7 1 : 5 Type of phospholipase Phospholipase B Phospholipase B Phospholipase A2 Amount of phospholipase used 1% 3% 5% Cooling water temperature 15°C 5°C 20°C Time required for the destruction of cell walls 3h 0, 5h 2h Destruction rate of cell walls 99,5% 91,5% 96% Extraction solvent MCT MCT MCT Feed rate ratio of the sludge with destroyed cell walls to the extraction solvent 11 : 5 2 : 1 2 : 1 Ratio of dry substances from extraction solvent to Haematococcus pluvialis 5 : 1 4 : 1 3 : 1 Centrifuge speed 6000 RPM 6000 RPM 6000 RPM Extraction rate of astaxanthin oil 95% 87% 92% Astaxanthin content 2,1% 2,8% 3,6%

[0116] To further demonstrate the advantages of the astaxanthin oil extraction equipment and the astaxanthin oil extraction process as described, a control group was included. The process parameters and the effect of the astaxanthin extraction in this group are shown in Table 3. The procedure for the control group was the same as for the experimental groups. However, there were differences between the control group and the experimental groups with regard to some of the process parameters or processing conditions. For example, in comparison to experimental group 1, no phospholipase was used in control group 1, Haematococcus pluvialis and water were dosed into the mixing vessel in a mass ratio of 1:5, the cooling water temperature was set to 10°C, and the time required to destroy cell walls was set to 3 hours to obtain the sludge with destroyed cell walls, as shown in Table 3.Sludge with damaged cell walls and a medium-chain triglyceride (MCT) were fed into a static mixer at a rate of 6:1 to obtain a blended sludge. The blended sludge was then transferred to a three-phase centrifuge for separation. The centrifuge speed was 6000 rpm. After filtration through a precision filter, an astaxanthin oil was obtained with an extraction rate of 61% and an astaxanthin content of 5.4%. Table 3 Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 ratio of Haematococcus pluvialis to water 1 : 5 1 : 5 1 : 5 1 : 5 Type of phospholipase / alkaline proteinase Phospholipase B Phospholipase B Amount of phospholipase used / 2% 2% 2% Cooling water temperature 10°C 10°C 10°C 10°C Time required for the destruction of cell walls 3h 3h 3h 3h Destruction rate of cell walls 97% 97,5% 97% 97% Extraction solvent MCT MCT Coconut oil Safflower oil Feed rate ratio of the sludge with destroyed cell walls to the extraction solvent 6 : 1 6 : 1 6 : 1 6 : 1 Centrifuge speed 6000 RPM 6000 RPM 6000 RPM 6000 RPM Astaxanthin extraction rate 61% 62% 87% 86% Astaxanthin content 5,4% 5,7% 7,2% 7,1%

[0117] By comparing experimental group 2 with control group 2, it is evident that only the type of phospholipase differs, while the ratio of Haematococcus pluvialis to water, the amount of phospholipase used, the temperature of the cooling water, the time required for cell wall disruption, the type of extraction solvent, the feed rate ratio, and the centrifuge speed remain the same. Phospholipase B was used in experimental group 2, and an alkaline proteinase was used in control group 2. The results showed that in experimental group 2, the extraction rate of astaxanthin oil was 93% and the astaxanthin content was 7.3%. In contrast, in control group 2, the extraction rate of astaxanthin oil was only 62% and the astaxanthin content was 5.7%.This indicates that phospholipase B could more effectively degrade the emulsion components of phospholipids and glycolipids in the cells of Haematococcus pluvialis, thus significantly increasing the amount of astaxanthin released. In contrast, the extraction of astaxanthin oil was only marginally improved by a non-specific proteinase (e.g., alkaline proteinase). This demonstrates the aforementioned technological advantages of using a specific phospholipase selected from phospholipase A1, phospholipase A2, phospholipase B, and mixtures thereof, according to one or more embodiments described above, in the efficient extraction of astaxanthin oil.

[0118] By comparing experimental group 2 with control group 3, it is evident that only the type of extraction solvent differed, while the ratio of Haematococcus pluvialis to water, the type and amount of phospholipase used, the temperature of the cooling water, the time required for cell wall disruption, the feed rate ratio, and the centrifuge speed remained the same. In experimental group 2, a medium-chain triglyceride (MCT) was used as the extraction solvent, and in control group 3, coconut oil was used. The results showed that in experimental group 2, the extraction rate of astaxanthin oil was 93% and the astaxanthin content was 7.3%. In control group 3, the extraction rate of astaxanthin oil was 87%, and the astaxanthin content was only 2.7%.The results of this comparison show that MCT, due to its low viscosity, higher fat solubility, and better polarity matching with astaxanthin, could more efficiently promote the transfer of astaxanthin from the aqueous phase to the oily phase in the mixed sludge, thereby achieving a higher astaxanthin content in the oily phase. In contrast, coconut oil, due to its higher viscosity and stronger tendency to emulsify, exhibits a lack of ability to concentrate the astaxanthin. Therefore, in one or more embodiments of the description, MCT or an ethylated vegetable oil is used as the extraction solvent to significantly increase the extraction efficiency and the purity of the astaxanthin oil.

[0119] By comparing experimental groups 1 to 8 in Tables 1 and 2 with control groups 1 to 4 in Table 3, it is evident that the setup and procedure for extracting astaxanthin oil as described uses a medium-chain fatty acid glyceride (MCT) or an ethylated vegetable oil as a diluent and extraction solvent to enable efficient astaxanthin extraction at low energy consumption and temperature. Compared to control groups 1 to 4, which do not use phospholipase, another enzyme, or a different ratio of sludge with damaged cell walls to the extraction solvent, the extraction rate and content of astaxanthin oil increase significantly in the described process, resulting in improved extraction efficiency and process stability.

[0120] In the following examples, samples of microencapsulated powder are evaluated with regard to product properties. First, each sample is taken and divided into several parallel subsamples. To ensure the scientific rigor and reliability of the product property evaluation, an equal number of subsamples are randomly selected for each product. These subsamples are then evaluated under identical measurement conditions using the same measurement technique. Statistical analysis (averaging) of the resulting data is then used to quantify and compare the properties.

[0121] Example 2: Preparation of sample 1 of the microencapsulated powder with a combination of a lipophilic core material and a hydrophilic core material

[0122] Step (1): 90 g of water was weighed and placed in a 500 mL container. At a water temperature of 60°C, 11 g of fish gelatin with an average molecular weight of 130 kDa was added and stirred at 150 rpm until completely dissolved.

[0123] Step (2): 14 g of gum arabic was weighed and placed in a 500 mL container. 120 g of water at a temperature of 60°C was added and stirred at 150 rpm until completely dissolved.

[0124] Step (3): The fish gelatin solution was introduced into the aqueous solution of gum arabic and stirred at 150 rpm for 20 min to obtain a mixed solution of the shell materials.

[0125] Step (4): 50 g of algal oil DHA was weighed and placed in a 200 mL container together with 0.2 g of mixed tocopherols. They were stirred in a water bath at 60°C to form a homogeneous mixture, which was designated as the core material of group A.

[0126] Step (5): 60 wt% of the mixed solution of shell materials was mixed with the core material of Group A and emulsified by shearing at a rotational speed of 9000 rpm to obtain the emulsion of the core material of Group A. The emulsion was introduced into a stirred tank, diluted to a solids content of 6 wt%, and then adjusted to a pH of 5.1 using 0.1% hydrochloric acid as a diluent. The particle size D90 of the system was adjusted to 6.0 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to obtain a multinucleate microcapsule of a first layer.

[0127] Step (6): 12 g of ascorbic acid was weighed and placed in a 200 mL Becker, which was designated as core material of group B.

[0128] Step (7): The core material of group B was mixed with the remaining 40 wt% of the shell material mixture and emulsified by shearing at 5000 rpm to obtain the core material solution of group B. The solution was introduced into a stirred tank for the above procedure and then adjusted to a pH of 4.5 using 0.1% hydrochloric acid as a diluent. This resulted in a D90 particle size of 36 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to generate a multinucleate second-layer microcapsule.

[0129] Step (8): Finally, 12 g of filler of a solid corn syrup with a DE value of 60 was dosed into the emulsion prepared in step (7), stirred until completely dissolved, and dried by spraying at an air inlet temperature of 180°C and an air outlet temperature of 85°C to obtain a suitable, double-microencapsulated powder. The dried powder was sieved and packaged, and designated as Sample 1.

[0130] In this example, fish gelatin and gum arabic were used as shell materials, mixed tocopherols as antioxidants, algal oil DHA as lipophilic core material A, and ascorbic acid as hydrophilic core material B. Double coacervation by acidification after separate emulsification resulted in a multinucleated microcapsule with two layers of different polarities, the D90 of the primary shell layer being 6.0 µm and the D90 of the secondary shell layer being 36.0 µm, as shown in Fig. 3 shown.

[0131] Example 3: Preparation of sample 2 of the microencapsulated powder with a combination of a lipophilic core material and an amphiphilic core material

[0132] Step (1): 140g of water at a water temperature of 65°C was weighed and placed in a 500mL container. 13g of bovine gelatin with an average molecular weight of 195 kDa was added and stirred at 150 rpm until completely dissolved.

[0133] Step (2): 17 g of sodium carboxymethylcellulose was weighed and placed in a 500 mL Becker container. 80 g of water at a temperature of 65°C was added and stirred at 150 rpm until completely dissolved.

[0134] Step (3): The bovine gelatin solution was introduced into the aqueous solution of sodium carboxymethylcellulose and stirred at 150 rpm for 20 min to obtain a mixed solution of the shell materials.

[0135] Step (4): 30g of linseed oil was weighed and placed in a 200mL container together with 0.02g of antioxidant 264. They were stirred in a water bath at 55°C to form a homogeneous mixture, which was designated as the core material of Group A.

[0136] Step (5): 50 wt% of the mixed solution of shell materials was mixed with the core material of Group A and emulsified by shearing at a rotational speed of 8000 rpm to obtain the emulsion of the core material of Group A. The emulsion was introduced into a stirred tank reactor, diluted to a solids content of 6 wt%, and then adjusted to a pH of 5.2 using 0.1% sulfuric acid as a diluent. The particle size D90 of the system was adjusted to 4.0 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to obtain a multinucleate microcapsule of a first layer.

[0137] Step (6): 20 g of krill oil was weighed and placed in a 200 mL container together with 0.02 g of antioxidant 264. They were stirred in a water bath at 40°C to form a homogeneous mixture, which was designated as core material of group B.

[0138] Step (7): The core material of group B was mixed with the remaining 50 wt% of the shell material mixture and emulsified by shearing at a rotational speed of 6000 rpm to obtain the solution of the core material of group B. The solution was introduced into a stirred tank reactor for the above procedure and then adjusted to a pH of 4.5 using 0.1% sulfuric acid as a diluent. This resulted in a D90 particle size of 31 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was then added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to generate a multinucleate second-layer microcapsule.

[0139] Step (8): Finally, 19 g of filler glucose syrup with a DE value of 55 was dosed into the emulsion prepared in step (7), stirred until completely dissolved, and dried by spraying at an air inlet temperature of 170°C and an air outlet temperature of 75°C to obtain a suitable, double-microencapsulated powder. The dried powder was sieved and packaged, and designated as Sample 2.

[0140] In this example, bovine gelatin and sodium carboxymethylcellulose were used as shell materials, antioxidant 264 as the antioxidant, linseed oil as lipophilic core material A, and krill oil as amphiphilic core material B. Double coacervation by acidification after separate emulsification resulted in a multinucleated microcapsule with two layers of different polarities, the D90 of the primary shell layer being 4.0 µm and the D90 of the secondary shell layer being 31.0 µm, as shown in Fig.4 shown.

[0141] Example 4: Preparation of sample 3 of the microencapsulated powder with a combination of an insoluble amphoteric core material with an amphiphilic core material

[0142] Step (1): 140 g of water at a water temperature of 55°C was weighed and placed in a 500 mL container. 14 g of soy protein with an average molecular weight of 78 kDa was added and stirred at 150 rpm until completely dissolved.

[0143] Step (2): 18 g of sodium alginate was weighed and placed in a 500 mL container. 170 g of water was added and stirred at a water temperature of 55°C at 150 rpm until completely dissolved.

[0144] Step (3): The soy protein solution was introduced into the sodium alginate solution and stirred at 150 rpm for 20 min to obtain a mixed solution of the shell materials.

[0145] Step (4): 10 g of resveratrol was weighed and placed together with 0.07 g of rosemary extract in a 200 mL container. They were stirred to form a homogeneous mixture, which was designated as core material of group A.

[0146] Step (5): 40 wt% of the mixed solution of shell materials was mixed with the core material of Group A and emulsified by shearing at a rotational speed of 9000 rpm to obtain the emulsion of the core material of Group A. The emulsion was introduced into a stirred tank, diluted to a solids content of 6 wt%, and then adjusted to a pH of 5.0 using 0.1% phosphoric acid as a diluent. The particle size D90 of the system was adjusted to 15.0 µm. The system was then cooled to 15°C. 1.0 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to obtain a multinucleate microcapsule of a first layer.

[0147] Step (6): 40 g of rapeseed diglyceride oil was weighed and placed in a 200 mL container together with 0.07 g of rosemary extract. They were stirred in a water bath at 55°C to form a homogeneous mixture, which was designated as core material of group B.

[0148] Step (7): The core material of group B was mixed with the remaining 60 wt% of the shell material mixture and emulsified by shearing at a rotational speed of 5000 rpm to obtain the core material solution of group B. The solution was introduced into a stirred tank reactor for the above procedure and then adjusted to a pH of 4.4 using 0.1% phosphoric acid as a diluent. This resulted in a D90 particle size of 39 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to generate a multinucleate second-layer microcapsule.

[0149] Step (8): Finally, 16 g of filler maltose with a DE value of 50 was dosed into the emulsion prepared in step (7), stirred until completely dissolved, and dried by spraying at an air inlet temperature of 200°C and an air outlet temperature of 90°C to obtain a suitable, double-microencapsulated powder. The dried powder was sieved and packaged, and designated as Sample 3.

[0150] In this example, soy protein and sodium alginate were used as shell materials, rosemary extract as an antioxidant, resveratrol as the insoluble amphoteric core material A, and rapeseed diglyceride oil as the amphiphilic core material B. Double coacervation by acidification after separate emulsification resulted in a multinucleated microcapsule with two layers of different polarities, the D90 of which was 15.0 µm for the primary shell layer and 39.0 µm for the secondary shell layer, as shown in Fig.5 shown.

[0151] Example 5: Preparation of sample 4 of the microencapsulated powder with a combination of a lipophilic core material and a hydrophilic core material

[0152] Step (1): 130 g of water at a water temperature of 55°C was weighed and placed in a 500 mL container. 14 g of casein with an average molecular weight of 20 kDa was added and stirred at 150 rpm until completely dissolved.

[0153] Step (2): 18 g of pectin was weighed and placed in a 500 mL container. 170 g of water at a temperature of 55°C was added and stirred at 150 rpm until completely dissolved.

[0154] Step (3): The casein solution was introduced into the pectin solution and stirred at 150 rpm for 20 min to obtain a mixed solution of the shell materials.

[0155] Step (4): 30 g of astaxanthin oil produced in Experiment 1, group 3, was weighed and placed in a 200 mL Becker container together with 0.1 g of sunflower phospholipid. They were stirred in a water bath at 45°C to form a homogeneous mixture, which was designated as the core material of group A.

[0156] Step (5): 40 wt% of the mixed solution of shell materials was mixed with the core material of Group A and emulsified by shearing at a rotational speed of 9000 rpm to obtain the emulsion of the core material of Group A. The emulsion was introduced into a stirred tank, diluted to a solids content of 6 wt%, and then adjusted to a pH of 5.0 using 0.1% phosphoric acid as a diluent. The particle size D90 of the system was adjusted to 15.0 µm. The system was then cooled to 15°C. 1.0 g of an immobilizing enzyme was subsequently added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to obtain a multinucleate microcapsule of a first layer.

[0157] Step (6): 20 g of γ-aminobutyric acid was weighed and placed together with 0.1 g of phospholipid in a 200 mL Becker. They were stirred in a water bath at 55°C to form a homogeneous mixture, which was designated as the core material of group B.

[0158] Step (7): The core material of group B was mixed with the remaining 60 wt% of the shell material mixture and emulsified by shearing at a rotational speed of 5000 rpm to obtain the solution of the core material of group B. The solution was introduced into a stirred tank reactor for the above procedure and then adjusted to a pH of 4.4 using 0.1% phosphoric acid as a diluent. This resulted in a D90 particle size of 38 µm. The system was then cooled to 15°C. 0.5 g of an immobilizing enzyme was then added. The mixture was heated to 80°C, held at this temperature for 30 min to deactivate the immobilizing enzyme, and then cooled to 60°C to generate a multinucleate second-layer microcapsule.

[0159] Step (8): Finally, 17 g of filler glucose syrup with a DE value of 55 was dosed into the emulsion prepared in step (7), stirred until completely dissolved, and dried by spraying at an air inlet temperature of 200°C and an air outlet temperature of 90°C to obtain a suitable, double-microencapsulated powder. The dried powder was sieved and packaged, and designated as Sample 4.

[0160] In this example, casein and pectin were used as shell materials, phospholipid as an antioxidant, astaxanthin oil (oil from Haematococcus pluvialis) as lipophilic core material A, and γ-aminobutyric acid as hydrophilic core material B. Double coacervation by acidification after separate emulsification resulted in a multinucleated microcapsule with two layers of different polarities, the D90 of which is 5.0 µm of the primary shell layer (where the primary shell layer is very thin, as shown by the dense, dark part in the image). Fig. 6 shows) and D90 of the secondary shell layer was 38.0 µm. As in Fig. As shown in Figure 6, the black part represents the fine and dense multinucleate microcapsule of the first layer made of astaxanthin oil, and the transparent particles represent the multinucleate microcapsule of the second layer made of γ-aminobutyric acid.

[0161] The shell material selected for Examples 2 and 3 was gelatin, for Example 5 casein (both derived from animal sources), and for Example 4 soy protein (derived from a plant source). The core materials selected for Examples 2 and 5 were a combination of a lipophilic and a hydrophilic core material, for Example 3 a combination of a lipophilic and an amphiphilic core material, and for Example 4 a combination of an insoluble amphoteric and an amphiphilic core material, where significant differences existed between the various core materials. The antioxidants selected for Examples 2, 3, and 5, respectively, were a mixture of tocopherol, antioxidant 264, and phospholipid, which are common antioxidants in quality of life. In contrast, rosemary extract, a natural antioxidant, was used in Example 4. Example 6: Assessment of product characteristics

[0162] Samples 1 to 4 from Examples 2 to 5 were evaluated with regard to product properties. Measuring the surface area can directly reflect the encapsulation of the two core materials. The lower the surface area, the better the encapsulation. The surface area is calculated using the following equation: Surface area % = Content of a component extracted from the surface % / Content of the component in the starting material for the core material % * 100%. Using DHA as an example, the surface area of ​​DHA = Content of docosahexaenoic acid extracted from the surface % / Content of docosahexaenoic acid in the starting material of DHA oil % * 100%. It is generally assumed that good encapsulation can be achieved with a surface area ≤ 2%. The tablet press trials were conducted with a surface area of ​​5%.After tablet pressing, tablet hardness was evaluated as a criterion that significantly influences tablet integrity and disintegration. If the hardness is too high, the medication and excipients adhere tightly, making the tablets difficult to disintegrate and preventing effective dissolution of the pharmaceutical components, thus impairing any potential therapeutic effect. Conversely, if the hardness is too low, tablet integrity is difficult to maintain, potentially leading to tablet breakage and significantly compromising subsequent coating, packaging, and transfer. The optimal tablet hardness is generally considered to be in the range of 160–210 N. Tablet friability reflects the tablets' resistance to abrasion and vibration and is also an important criterion in tablet quality control.Generally, the product will be considered qualified if the weight loss is no more than 1% and no broken, cracked, or crushed tablets are observed. The final results of all measurements are summarized in Table 4. Table 4 Name Appearance, smell and taste Particle size surface content of the surface area content Hardness of the pre Friability of the D50 / D90 / D99 µm Group A core material, % Group B core material, % sstenTablettenN pressed tablets % Sample 1 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor 21,5 / 35,8 / 69,8 DHA (calculated as docosahexaenoic acid): 0.16% VC (calculated as L-ascorbic acid): 0.53% 179 0.2% no cracking or fragmentation Sample 2 Light yellow to yellow-orange powder with the inherent smell and taste of the product, without any unusual odor. 21, 3 / 31,2 / 64, 0 Linseed oil (calculated as α-linolenic acid): 0.14% Krill oil (calculated as Ω-3 fatty acid): 0.31% 183 0.1% no cracking or fragmentation Sample 3 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor 27,6 / 39,0 / 94,2 Resveratrol: 0.23% Rapeseed diglyceride oil: 0.12% 198 0.2% no cracking or fragmentation Sample 4 red powder with the inherent smell and taste of the product, without any unusual odor 25,0 / 38,0 / 91,0 Astaxanthin oil 0.35% γ - Aminobutyric acid 0.30% 188 0.2% no cracking or fragmentation

[0163] The results show that the doubly microencapsulated powders with core materials of different polarities provided in the exemplary embodiments of the description exhibit a good appearance, odor, and taste, and occupy a surface area of ​​the individual components ≤ 2%. This proves that, through the specific combination of starting materials and process steps of the invention, a doubly microencapsulated powder with two of the, for example, hydrophilic, lipophilic, amphiphilic, or insoluble amphoteric core materials of different polarities is produced, so that nutrients with different original properties can be simultaneously encapsulated in a single capsule, thus enabling the versatility and compatibility of the product.Furthermore, the hardness of the pressed tablets is within the optimal range of 160–210 N, and the friability is ≤ 1%, ensuring a state free from cracking or fragmentation. This guarantees the tablets meet quality standards regarding completeness and degree of disintegration. This ensures effective dissolution of the pharmaceutical components and prevents tablet breakage, thus ensuring the smooth subsequent coating and packaging, as well as the storage and transfer of the products. Example 7: Assessment of product stability

[0164] Samples 1, 2, 3, and 4 were each divided into several parallel subsamples. The subsamples were each subjected to an accelerating oven at 40°C and 75% humidity for three months to assess their stability, with degradation calculated using the following equation: Degradation % = (original content of a component in the sample - content in the sample after storage) / original content in the sample * 100%. Using DHA as an example, the degradation of DHA % = (original content of docosahexaenoic acid % - content of docosahexaenoic acid in the sample after storage %) / original content of docosahexaenoic acid in the sample * 100%. The other measurements were performed according to government or industry standards. The results are summarized in Table 5. Table 5 name 0 month Appearance, smell and taste Reduction in the salary of group A, % (initially considered as 0%) Reduction in the content of group B, % (initially considered as 0%) Hydrogen peroxide content, meq / kg Acidity 1 mg KOH / g Sample 1 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor DHA (calculated as docosahexaenoic acid): 0% VC (recalculated as L-ascorbic acid): 0% 0,1 0,2 Sample 2 Light yellow to yellow-orange powder with the inherent smell and taste of the product, without any unusual odor. Linseed oil (calculated as α-linolenic acid): 0% Krill oil (calculated as docosahexaenoic acid): 0% 0,4 0,6 Sample 3 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor Resveratrol (calculated as Resveratrol+ Polydatin): 0% Rapeseed diglyceride oil (calculated as oleic acid): 0% 0,2 0,7 Sample 4 red powder with the inherent smell and taste of the product, without any unusual odor Astaxanthin oil: 0% G-Aminobutyric acid: 0% 0,2 0,5 name 1 month Appearance, smell and taste Reduction in the salary of Group A % Reduction in the salary of Group B % Hydrogen peroxide content, meq / kg Acidity 1 mg KOH / g Sample 1 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor DHA (calculated as docosahexaenoic acid): 0.2% VC (calculated as L-ascorbic acid): 0.9% 0, 8 0,3 Sample 2 Light yellow to yellow-orange powder with the inherent smell and taste of the product, without any unusual odor. Linseed oil (calculated as α-linolenic acid): 0.2% Krill oil (calculated as docosahexaenoic acid): 0.6% 2,5 0,5 Sample 3 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor Resveratrol (calculated as Resveratrol+ Polydatin): 2.1% Rapeseed diglyceride oil (calculated as oleic acid): 0.2% 1,3 0,7 Sample 4 red powder with the inherent smell and taste of the product, without any unusual odor Astaxanthin oil: 2.4% G-Aminobutyric acid: 0.3% 0, 8 0,5 name 2 months Appearance, smell and taste Reduction in the salary of Group A % Reduction in the salary of Group B % Hydrogen peroxide content, meq / kg Acidity 1 mg KOH / g Sample 1 white to light yellow powder with the inherent smell and taste of the product, with a slightly smelly DHA (calculated as docosahexaenoic acid): 0.3% VC (calculated as L-ascorbic acid): 1.2% 1,2 0,5 smell of algae Sample 2 Light yellow to yellow-orange powder with the inherent smell and taste of the product, without any unusual odor. Linseed oil (calculated as α-linolenic acid): 0.3% Krill oil (calculated as DHA): 0.5% 4,5 0,6 Sample 3 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor Resveratrol (calculated as Resveratrol+ Polydatin): 3.8% Rapeseed diglyceride oil (calculated as oleic acid): 0.5% 3,2 0,7 Sample 4 red powder with the inherent smell and taste of the product, with a slightly foul odor Astaxanthin oil: 2.9% G-Aminobutyric acid: 0.6% 1,5 0,6 name 3 months Appearance, smell and taste Reduction in the salary of Group A % Reduction in the salary of Group B % Hydrogen peroxide content, meq / kg Acidity 1 mg KOH / g Sample 1 white to light yellow powder with the inherent smell and taste of the product, with a slightly pungent smell of algae. DHA (calculated as docosahexaenoic acid): 0.4% VC (calculated as L-ascorbic acid): 4.0% 2,4 0,4 Sample 2 light yellow to yellow-orange powder with inherent Linseed oil (as α-linolenic acid e Krill oil (calculated as DHA): 1.1% 6,7 0,6 The product's smell and taste have a slight scent of linseed oil. (calculated): 0.6% Sample 3 white to light yellow powder with the inherent smell and taste of the product, without any unusual odor Resveratrol (calculated as Resveratrol+ Polydatin): 4.9% Rapeseed diglyceride oil (calculated as oleic acid): 0.7% 4, 4 0, 8 Sample 4 red powder with the inherent smell and taste of the product, with an enhanced, but still acceptable, odor Astaxanthin oil: 3.7% G-Aminobutyric acid: 1.0% 2,2 0,5

[0165] The accelerated stability test in a thermostatic and hygrostatic chamber showed that the appearance, odor, and taste of the four samples did not change significantly after three months of acceleration, with only a slightly oily odor developing. Although the hydrogen peroxide content and acid number increased slightly, a product is generally considered to have good stability if, after three months of acceleration, it exhibits a hydrogen peroxide content of ≤ 10.0 meq / kg and an acid number of ≤ 1.0 mg KOH / g. Acceleration for three months can ensure that the degradation of the components is ≤ 5.0 meq / kg.It is evident that the double microencapsulated powder produced according to the recipe of the exemplary embodiments described is tightly encapsulated and well insulated, exhibiting excellent resistance to heat and oxidation as well as high storage stability. Furthermore, the degradation of different core materials also reflects the consistency and reliability in processing core materials of varying polarities according to the recipe of the exemplary embodiments described, which provides a solid basis for the application of the product in sectors such as pharmaceuticals, food, cosmetics, etc.

[0166] Example 8: Influence of the particle size D90 of the primary shell layer on the properties of the product

[0167] Based on the process of Example 2, only the amount of acid used was changed, without altering the materials and their proportions in the recipe. The primary focus was on observing the influence of particle size on the surface areas of the individual components during the formation of the primary shell layer, i.e., on the effect of microencapsulation. The product states are summarized in Table 6. Table 6 name Particle size of the primary shell layer: D90 µm Surface area of ​​the core material of Group A % Surface area of ​​the core material of group B % Hardened pressed tablets N Friability of the compressed tablets% Sample 1 6,0 DHA (calculated as docosahexaenoic acid): 0.16% VC (calculated as L-ascorbic acid): 0.53% 179 0.2% no cracking or fragmentation Sample 2 4,0 Linseed oil (calculated as α-linolenic acid): 0.14% Krill oil (calculated as Ω-3 fatty acid): 0.31% 183 0.1% no cracking or fragmentation Sample 3 15,0 Resveratrol: 0.23% Rapeseed diglyceride oil: 0.12% 198 0.2% no cracking or fragmentation Sample 4 8, 0 Astaxanthin oil: 0.29% γ-Aminobutyric acid: 0.13% 190 0.1% no cracking or fragmentation Comparative example 1 1,0 The particle size of the primary shell layer was too small, so that no subsequent coacervation layer could be created by adhesion and the microencapsulated powder could not be produced. Comparative example 2 2,0 DHA (calculated as docosahexaenoic acid): 0.66% VC (calculated as L-ascorbic acid): 3.12% 172 0.4% no cracking or fragmentation Comparative example 3 18, 0 DHA (calculated as docosahexaenoic acid): 1.53% VC (calculated as L-ascorbic acid): 2.05% 112 3.5% comprising tablets that clearly show no cracking or breakage. Comparative example 4 20,0 DHA (calculated as docosahexaenoic acid): 1.98% VC (calculated as L-ascorbic acid): 3.02% 98 6.2% comprising tablets that are clearly without Cracking or breakage patterns Comparative example 5 30,0 The particle size was subsequently increased too much, so that the particles adhered strongly to the tower during both spray drying processes, and thus no dried microencapsulated powder was obtained.

[0168] The results show that, based on the process of Example 2, the properties of the microencapsulated powder product are influenced by adjusting the particle size of the primary shell layer. An appropriate primary shell layer particle size can improve the product's suitability for encapsulated tablet pressing. Conversely, a primary shell layer particle size that is too small or too large leads to the failure of microencapsulated powder production or a deterioration in product quality. For the production of a multinucleated, multilayer microcapsule, the primary shell layer particle size D90 must be in the range of 2–20 µm. The first layer of the multinucleated microcapsule is then produced by cooling and immobilization using an immobilizing enzyme. The D90 particle size can be 3–18 µm or 4–15 µm.If the particle size exceeds this range, it becomes too large and thus differs too greatly from the particle size of the base material powder. This leads to poor hardness and abrasion resistance of the pressed tablets, increased susceptibility to leakage after shearing, and an increase in surface area. With an even larger particle size, the particles can adhere to the stack during spray drying, preventing the formation of a suitable microencapsulated powder. Conversely, if the particle size is too small, coacervation of the particles cannot be achieved, or the subsequent layer cannot adhere and grow through coacervation, potentially resulting in the formation of no coacervated particles at all.Furthermore, a particle size that is too small leads to an excessively large surface area, resulting in a thin encapsulated shell layer. This also impairs the final effectiveness of the microencapsulation and significantly increases the surface area. In the sample exhibiting a primary shell layer particle size D90 in the range of 4–10 µm, a low initial amount of oils formed on the surface, qualified tablet hardness and friability, and measured surface areas of ≤ 2%. This product was considered satisfactory. Therefore, the particle size of the primary shell layer D90 must be in the range of 3–18 µm, but also in the range of 4–15 µm, to achieve the desired encapsulation effect and tablet properties. Example 9: Influence of the molecular weight of the protein shell material on the state of the product

[0169] Based on the process of Example 2, only the molecular weight of the protein shell material was changed, without altering the materials and their proportions in the recipe. The primary focus was on the influence of the molecular weight of the protein shell material on the state of the sample. The measurement results are summarized in Table 7. Table 7 name average molecular weight of protein shell material 1s Appearance, smell and taste Surface area of ​​the core material of Group A % Surface area of ​​the core material of group B % Hardened pressed tablets N Friability of the compressed tablets % Sample 1 130 kDa white to pale yellow DHA (as Docosahex) VC (as L-ascorbic acid) 179 0,2% Powder with the inherent smell and taste of the product, without any unusual odor. (calculated acetic acid): 0.16% (calculated): 0.53% no cracking or fragmentation Sample 2 195 kDa Light yellow to yellow-orange powder with the inherent smell and taste of the product, without any unusual odor. Linseed oil (calculated as α-linolenic acid): 0.14% Krill oil (calculated as Ω-3 fatty acid): 0.31% 183 0.1% no cracking or fragmentation Sample 3 78 kDa white to light yellow powder with the inherent smell and taste of the product, without any unusual odor Resveratrol: 0.23% Rapeseed diglyceride oil: 0.12% 198 0.2% no cracking or fragmentation Sample 4 149 kDa red powder with the inherent smell and taste of the product, without any unusual odor Astaxanthin oil: 0.29% γ-Aminobutyric acid: 0.13% 190 0.1% no cracking or fragmentation Comparative example 6 10 kDa white to pale yellow powder with a foul odor of algae DHA (calculated as docosahexaenoic acid): 8.03% VC (calculated as L-ascorbic acid): 5.02% 122 3.9% no cracking or fragmentation Comparative example 7 20 kDa white to pale yellow powder with a slight DHA (calculated as docosahexaenoic acid): 3.52% VC (calculated as L-ascorbic acid): 2.05% 131 2.3% comprising tablets that smell of algae clearly without cracking or breaking templates Comparative example 8 40 kDa white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 1.38% VC (calculated as L-ascorbic acid): 2.53% 143 1.8% comprising tablets that clearly show no cracking or breakage. Comparative example 9 200 kDa white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 0.98% VC (calculated as L-ascorbic acid): 1.02% 170 0.6% no cracking or fragmentation Comparative example 10 220 kDa white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 1.32% VC (calculated as L-ascorbic acid): 1.21% 168 0.7% no cracking or fragmentation Comparative example 11 250 kDa white to light yellow powder with a slightly foul-smelling odor of algae DHA (calculated as docosahexaenoic acid): 1.98% VC (calculated as L-ascorbic acid), 1.53% 162 0.9% no cracking or fragmentation Comparative example 12 300 kDa white to light yellow, viscous powder with distinct DHA (calculated as docosahexaenoic acid): 4.80% VC (calculated as L-ascorbic acid): 6.03% 143 4.0% comprising tablets that clearly foul odor h without cracking or breaking templates Comparative example 13 400 kDa white to light yellow, viscous powder with a distinctly foul odor DHA (calculated as docosahexaenoic acid): 5.11% VC (calculated as L-ascorbic acid): 5.63% 89 6.9% comprising tablets that clearly show no cracking or breakage.

[0170] The results show that samples 1, 2, 3, and 4 are rated as good in terms of appearance, odor, and taste, and do not emit any unusual smell. Reducing the average molecular weight of the protein shell material gradually intensifies the foul odor of the algae in the samples, and correspondingly increases the surface oil content. Furthermore, the viscosity of the powder increases, resulting in a distinctly foul odor, if the average molecular weight of the protein shell material is too high. In some embodiments, the protein shell material has a molecular weight of 50–250 kDa. In some embodiments, the protein shell material can have a molecular weight of 60–220 kDa. In some embodiments, the protein shell material can also have a molecular weight of 70–195 kDa.If the molecular weight is less than 50 kDa, the emulsion in the protein phase is thin, and the layering during the emulsification process of the oily phase is pronounced, resulting in a tendency for floating oil to occur during final encapsulation and thus a high surface area of ​​the product. If the molecular weight is greater than 250 kDa, the formation of the multinucleated microcapsule becomes more difficult, and the shape of the microcapsule becomes more irregular, impairing the final encapsulation effect. For example, the tablets in Examples 9 to 11 and 14 to 16 were evaluated because they exhibited insufficient hardness and a high friability of ≥ 1%, and were therefore considered unqualified.Therefore, the average molecular weight of the protein shell material must be in the range of 50 - 250 kDa, preferably 70 - 195 kDa, to ensure a good appearance and taste of the product while achieving a low surface area and the corresponding effect of tablet pressing. Example 10: Influence of the filler's DE value on the product's condition

[0171] Based on the process described in Example 2, only the DE value of the filler was changed, without altering the materials and their proportions in the recipe. The primary focus was on the influence of the DE value on the state of the sample. The measurement results are summarized in Table 8. Table 8 name DE value of the fountain pen Appearance, smell and taste Surface area of ​​the core material of Group A % Surface area of ​​the core material of group B % Sample 1 60 white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 0.16% VC (calculated as L-ascorbic acid): 0.53% Sample 2 55 light yellow-yellow-orange Linseed oil (as α-linolenic acid) Krill oil (as Ω-3 fatty acid) Powder without unusual odor (calculated): 0.14% (calculated): 0.31% Sample 3 50 white to light yellow powder without unusual odor Resveratrol: 0.23% Rapeseed diglyceride oil: 0.12% Sample 4 57 red powder with the inherent smell and taste of the product, without any unusual odor Astaxanthin oil: 0.29% γ-Aminobutyric acid: 0.13% Comparison example 14 40 white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 1.02% VC (calculated as L-ascorbic acid): 1.33% Comparison example 15 30 white to light yellow powder with a slightly foul-smelling odor of algae DHA (calculated as docosahexaenoic acid): 2.56% VC (calculated as L-ascorbic acid): 2.89% Comparison example 16 20 white to pale yellow powder with a foul odor of algae DHA (calculated as docosahexaenoic acid): 3.40% VC (calculated as L-ascorbic acid): 4.02% Comparative example 17 10 white to light yellow powder with DHA (as docosahexaenoic acid) VC (as L-ascorbic acid e distinctly foul-smelling (calculated): 8.53% (calculated): 6.02% Comparative example 18 70 white to light yellow powder without unusual odor DHA (calculated as docosahexaenoic acid): 1.02% VC (calculated as L-ascorbic acid): 2.33% Comparative example 19 80 white to light yellow, viscous powder with a foul odor of algae DHA (calculated as docosahexaenoic acid): 0.89% VC (calculated as L-ascorbic acid): 2.51% Comparison example 20 90 white to light yellow, viscous powder with a foul odor of algae DHA (calculated as docosahexaenoic acid): 0.66% VC (calculated as L-ascorbic acid): 1.02%

[0172] The results show that the DE value has a certain influence on the condition of the sample. Increasing the DE value of the filler does not result in any significant change in the appearance, odor, and taste of samples 1, 2, 3, and 4, but it does result in a slight change in the surface area of ​​the core material. In some embodiments, the DE value of the filler is 40–70 parts by weight. In some embodiments, the DE value of the filler can be 45–65 parts by weight. In some embodiments, the DE value of the filler can also be 50–60 parts by weight. Table 8 shows that if the DE value is too low (< 20, as in comparative examples 17 to 19), the viscosity after dissolution of saccharides is too high, leading to poor filling, the formation of pores, and an increase in surface area.If the DE value is too high (> 70), the filler tends to agglomerate after spray drying, absorbing moisture and forming a viscous powder. While this exhibits a low surface area, it is in poor condition and emits an unpleasant odor, as seen in comparative examples 21 and 22. Samples with a filler DE value in the range of 40–70 exhibit good condition, a favorable odor and taste, and surface areas of individual components of ≤ 2.0%. Therefore, the product is considered qualified. Example 11: Influence of the shell material on the state of the product

[0173] Based on the process of Example 2, only the amount of shell material used was changed, without altering the recipe quantity or the process parameters. The primary focus was on the influence of the shell material on the sample's condition. The measurement results are summarized in Table 9. Table 9 name Protein shell material (parts by weight) Polysaccharide shell material (parts by weight) Appearance, smell and taste Surface area of ​​the core material of Group A % Surface area of ​​the core material of Group B % Hardened pressed tablets N Friability of the compressed tablets% Sample 1 11 14 white to light yellow powder with inherent odor and taste of DHA (calculated as docosahexaenoic acid): 0.16% VC (calculated as L-ascorbic acid): 0.53% 179 0.2% no cracking or fragmentation Product, without unusual odor Comparative example 21 20 1 yellow, stringy powder with a distinctly foul odor DHA (calculated as docosahexaenoic acid): 8.53% VC (calculated as L-ascorbic acid): 12.6% comprehensive, many strip-shaped particles and not suitable for tablet presses Comparative example 22 19 2 yellow, stringy powder with a distinctly foul odor DHA (calculated as docosahexaenoic acid): 7.52% VC (calculated as L-ascorbic acid): 12.1% comprehensive, many strip-shaped particles and not suitable for tablet presses Comparative example 23 18 3 yellow, stringy powder with a distinctly foul odor DHA (calculated as docosahexaenoic acid): 4.55% VC (calculated as L-ascorbic acid): 3.15% 83 8.5% showing significant cracking and fragmentation Comparative example 24 17 4 yellow powder with a slightly smelly odor DHA (calculated as docosahexaenoic acid): 2.01% VC (calculated as L-ascorbic acid): 1.89% 158 0.8%, with cracking, without cerclage a Comparative example 25 16 5 light yellow powder with no unusual odor DHA (calculated as docosahexaenoic acid): 1.56% VC (calculated as L-ascorbic acid): 1.45% 161 0.6%, with cracking, without crushing Comparative example 26 15 6 light yellow powder with no unusual odor DHA (calculated as docosahexaenoic acid): 1.73% VC (calculated as L-ascorbic acid): 0.92% 167 0.4% no cracking or fragmentation Comparative example 28 6 15 light yellow powder with a slightly foul-smelling odor DHA (calculated as docosahexaenoic acid): 1.98% VC (calculated as L-ascorbic acid): 0.82% 161 0.3% no cracking or fragmentation Comparative example 29 4 17 white powder with a distinctly foul odor DHA (calculated as docosahexaenoic acid): 3.02% VC (calculated as L-ascorbic acid): 1.52% 133 %1.8%, with cracking and less crushing Comparative example 30 2 19 white, slightly viscous powder with DHA (as docosahexaenoic acid) VC (calculated as L-ascorbic acid) 118 3.0%, with cracking and distinctly foul-smelling odor (calculated): 6.33% et): 2.05% significant reduction in size Comparative example 31 1 20 white, distinctly viscous powder with a distinctly foul-smelling odor DHA (calculated as docosahexaenoic acid): 11.20% VC (calculated as L-ascorbic acid): 8.3% The particle condition is not good enough for tablet presses.

[0174] The results show that an excessively high proportion of protein shell material leads to significant stringing after spray drying and poor product condition, while an excessively low proportion of protein shell material results in poor encapsulation and an excessively high surface area. Furthermore, an excessively high proportion of polysaccharide shell material leads to high powder viscosity, while an excessively low proportion results in poor encapsulation, an excessively high surface area, and the emission of the foul odor shown in Examples 21 to 23 and 29 to 31. Good encapsulation is achieved with a protein shell material content of 5–16 parts by weight and a polysaccharide shell material content of 3–19 parts by weight.Furthermore, the hardness of the pressed tablets is within the optimal range of 160–210 N, and the friability is ≤ 1%, ensuring a state free from cracking or fragmentation. This guarantees the tablets meet quality standards regarding completeness and degree of disintegration. This ensures effective dissolution of the pharmaceutical components and prevents tablet breakage, thus ensuring the safe subsequent coating and packaging, as well as the storage and transfer of the products. Example 12: Characterization of the structure and verification of the mechanism

[0175] Samples 1 to 4 were systematically characterized to investigate the microscopic properties and encapsulation mechanism of the microencapsulated powder. 1. Determination of structural characteristics

[0176] Samples 1 to 4 were observed using an optical microscope. As in Fig. As shown in Figures 3 to 6, the microencapsulated powder was in an ellipsoidal or spindle-like shape, exhibiting uniform shrinkage on the surface and a D90 value of the primary shell layer of 6.0 µm (sample 1), 4.0 µm (sample 2), 15.0 µm (sample 3), and 5.0 µm (sample 4), and a D90 value of the secondary shell layer of 36.0 µm (sample 1), 31.0 µm (sample 2), 39.0 µm (sample 3), and 38.0 µm (sample 4), thus forming a multinucleated encapsulated structure. These data correspond to the D50 / D90 / D99 data in Table 4. 2. Structure of the shell layer

[0177] The shell material of the primary shell layer was prepared by complex coacervation of fish gelatin and gum arabic (sample 1), bovine gelatin and sodium carboxymethylcellulose (sample 2), soy protein and sodium alginate (sample 3), and casein and pectin (sample 4). The secondary shell layer consisted of the same combination of shell materials. In Example 9, the molecular weight was in the preferred range of 50–250 kDa to ensure completeness of the film at the interface. 3. Internal structure and distribution of components

[0178] Coacervation by stepwise acidification (in Examples 2 to 5) resulted in the preferential removal of a lipophilic core material (DHA, linseed oil, and astaxanthin oil), an insoluble amphoteric core material (resveratrol), and an amphiphilic core material (krill oil and rapeseed diglyceride oil) from the primary shell layer (the dark areas in Fig.3 to 6). The hydrophilic core material (ascorbic acid and γ-aminobutyric acid) and other shell materials were enclosed via the secondary shell layer (the light ring-shaped areas in Fig. 3 to 6) enriched to form a multinucleate multilayer microcapsule that enables spatial isolation of the core materials of different polarities. 4th position for additives

[0179] Mixed tocopherols (sample 1), antioxidant 264 (sample 2), rosemary extract (sample 3), or sunflower phospholipid (sample 4) were premixed with the core material. The antioxidant effect of these mixtures was investigated using the acceleration test shown in Table 5, in which the hydrogen peroxide content showed an increase of ≤ 6.9 meq / kg, demonstrating the effective distribution of the antioxidant to the active sites. 5. Pore structure

[0180] The SEM images in Fig. 7 and Fig. 8 showed that after the complex coacervation of the outer shell material, a dense structure was observed and, in combination with the low degradation of ≤ 4.9% in example 7, the insulating capacity proved its worth. 6. Properties of the interface

[0181] With a D90 value of the primary shell layer of 4 to 15 µm in Example 8, the surface oil content was ≤ 2% (in Table 6), which, in combination with the pH regulation step in Examples 2 to 5, demonstrates the stability of the film at the interface predominantly through electrostatic interaction.

[0182] Following the above description, the microscopic structures of samples 1 to 4 were systematically characterized. (1) multi-layered shell structure

[0183] As in Fig.As shown in Figures 3 to 6, the microencapsulated powder exhibited a bilayer shell produced by complex coacervation, comprising a primary shell layer and a secondary shell layer.

[0184] Primary shell layer: It was prepared by complex coacervation of protein and polysaccharide (fish gelatin and gum arabic, bovine gelatin and sodium carboxymethylcellulose, soy protein and sodium alginate, or casein and pectin) and had a thickness of 20–30% of the D90 value of the primary shell layer (corresponding to 1.2–4.5 µm) and a molecular weight in a preferred range of 50–250 kDa. This was supported by the data in Example 9.

[0185] Secondary shell layer: Coacervation through a second acidification resulted in epitaxy on the primary shell layer, and the epitaxial layer was 10-15% of the D90 value of the secondary shell layer (corresponding to 3.1-5.9 µm).

[0186] Structural parameters: primary shell layer D90: 4 - 15 µm (data from Table 4); secondary shell layer D90: 31 - 39 µm (data from Table 4); total particle size D50 / D90 / D99: 21.3 - 27.6 µm, 31.2 - 39.0 µm, 64.0 - 94.2 µm (Table 4). (2) Sealing and insulation

[0187] As in Fig. Figure 7 (shown in a SEM image of Example 2) shows that the outer shell material was formed in a pore-free, dense structure with a surface shrinkage of > 85%. In combination with a hydrogen peroxide content of ≤ 6.9 meq / kg (Table 5) and a surface oil content of ≤ 2% (Table 4) in the acceleration test, it was demonstrated that this structure effectively prevented the penetration of moisture and oxygen and fulfilled the function of a physical barrier. (3) spatial distribution of the nuclear material of multiple polarities

[0188] By stepwise encapsulation (in examples 2 to 5), the lipophilic core material (DHA, linseed oil, and astaxanthin oil), the insoluble amphoteric core material (resveratrol), and the amphiphilic core material (krill oil and rapeseed diglyceride oil) were preferably encapsulated within the primary shell layer (the dark areas in Fig. 3 to 6). The hydrophilic core material (ascorbic acid and γ-aminobutyric acid) and other shell materials were positioned over the secondary shell layer (the light ring-shaped areas in Fig. 3 to 6) enriched to enable physically isolated encapsulation of components of different polarities. This represented a significant difference from the “porous double-walled” structure in document CN 207204054 U. (4) Mechanism for stabilizing the interface

[0189] Electrostatic complex coacervation: By controlling the pH of examples 2 to 5 to 4.4 to 5.1, the positively charged protein was electrostatically bound to the negatively charged polysaccharide.

[0190] Investigation of mechanical strength: With a D90 value of the primary shell layer of 4 to 15 µm, the surface oil content was ≤ 2% (according to embodiment 10), which proves the stability of the film at the interface.

[0191] The basic concepts have been described above. Naturally, the detailed disclosure above serves only as an example for the person skilled in the art, without limiting the description. Although not explicitly stated, a person skilled in the art may make various modifications, improvements, and changes to the description. These modifications, improvements, and changes are indicated in the description so that they are still within the spirit and scope of the exemplary embodiments described.

[0192] This description also uses specific words to describe the embodiments described. The terms "an embodiment," "an embodiment," and / or "some embodiments" represent a feature, structure, or special characteristic associated with at least one embodiment in the description. Therefore, it should be emphasized and noted that "an embodiment," "an embodiment," and / or "an alternative embodiment" mentioned in different paragraphs of the description do not necessarily refer to the same embodiment or embodiment. Furthermore, some of the features, structures, or special characteristics of one or more embodiments described may be appropriately combined.

[0193] Unless explicitly stated otherwise in the claims, the use of sequence for processing elements and sequences, as well as the use of numbers, alphabets, and other names, shall not limit the process and sequence described. Although the above disclosure discusses several embodiments of the invention currently considered useful by way of various examples, it is understood that the details provided serve only for illustrative purposes. The appended claims are not to be limited to the embodiments disclosed herein. Rather, the claims are intended to cover modifications and equivalent combinations thereof that correspond to the essence and scope of the embodiments described.For example, the system components described above can be implemented either through hardware devices or exclusively through software solutions, such as a system described above that is installed on an existing server or mobile device.

[0194] It should also be noted that in the preceding description of the embodiments of the invention, various features are sometimes grouped together in one embodiment, one figure, or descriptions thereof, in order to simplify the explanation of the disclosure in the description and to facilitate the understanding of one or more embodiments of the invention. However, this disclosure does not mean that the features of the subject matter of the description are more than those mentioned in the claims. In fact, the features of the embodiments are fewer than all the features of any one of the individual embodiments disclosed above.

[0195] In some embodiments, numerical values ​​are used to describe the components and properties. It should be understood that in some cases, these numerical values ​​are modified by "approximately," "about," or "essentially." Unless otherwise specified, the expressions "approximately," "about," or "essentially" mean that these numerical values ​​may have a deviation of ±20%. Accordingly, in some embodiments, the numerical parameters used in the description and claims are approximate values ​​that may vary depending on the requirements of the individual embodiment. In some embodiments, the prescribed significant figures for the numerical parameters are to be taken into account using a general rounding procedure.Although in some exemplary embodiments of the description the value range and the parameters for determining their extent are approximate values, in a specific exemplary embodiment the values ​​can be set as precisely as possible.

[0196] The entire contents of the patents, patent applications, patent publications, and other materials cited in this description, such as articles, books, user manuals, disclosures, documents, and the like, are incorporated herein by reference. Excluded from this are both historical application documents that do not correspond to or contradict the content of this description, and documents that were or will be added to this description before or after its publication and that limit the broadest scope of the claims in this description. It should be noted that in the event of any discrepancies between the presentation, definition, and / or use of terms in the related materials of this description and the content of this description, the presentation, definition, and use of terms in this description shall prevail.

[0197] It is finally understood that the embodiments described in this document are used only to illustrate the principle underlying them. Other variants may also be included within the scope of the description. Therefore, the alternative configurations in the embodiments are exemplary but not limiting and can be considered consistent with the teaching presented in the description. Accordingly, the embodiments in the description should not be limited to those explicitly presented and explained within the document. QUOTES INCLUDED IN THE DESCRIPTION

[0000] This list of documents cited by the applicant was automatically generated and is included solely for the reader's convenience. The list is not part of the German patent or utility model application. The DPMA accepts no liability for any errors or omissions. Cited patent literature

[0000] GB 1886.172-2016

[0029] CN 207204054 U

[0188]

Claims

[1] Recipe for a double microencapsulated powder, characterized by , that the recipe includes the following ingredients in parts by weight: 5-60 parts by weight of core material of group A, 5-40 parts by weight of core material of group B, 5-16 parts by weight of protein shell material, 3-19 parts by weight of polysaccharide shell material, 0.1-2 parts by weight of immobilizing enzyme, 1-10 parts by weight of filler, 1-4 parts by weight of pH regulator and 0-2 parts by weight of antioxidant. [2] Recipe according to claim 1, characterized by , that the core material of group A is selected from lipophilic, amphiphilic and insoluble amphoteric core materials, and that the core material of group B is selected from hydrophilic, amphiphilic and insoluble amphoteric core materials. [3] Recipe according to claim 2, characterized by, that the lipophilic core material is selected from vegetable oils, animal oils, astaxanthin oils, fat-soluble vitamins and mixtures thereof, the hydrophilic core material is selected from water-soluble vitamins, highly soluble amino acids and mixtures thereof, the amphiphilic core material is selected from diglyceride oils, phospholipid oils, glycolipid oils and mixtures thereof, and the insoluble amphoteric core material is selected from polyphenols, sparingly soluble amino acids and mixtures thereof. [4] Recipe according to any one of claims 1 to 3, characterized by , that the protein shell material is selected from fish, pork and beef gelatin, soy protein, pea protein, pumpkin seed protein, hemp protein, chickpea protein, barley protein and mixtures thereof, and that the protein shell material has a molecular weight of 50 - 250 kDa. [5] Recipe according to any one of claims 1 to 4, characterized bythat the polysaccharide shell material is selected from gum arabic, sodium alginate, alginates, chitosan, carrageenan, pectin, starches, modified starches, cellulose, methylcellulose, ethylcellulose, carboxymethylcellulose and mixtures thereof. [6] Recipe according to any one of claims 1 to 5, characterized by , that the filler is selected from glucose syrup, lactose, maltose, solid corn syrup, oligomeric maltose and mixtures thereof, and that the filler has a dextrose equivalent (DE) of 40 - 70. [7] Recipe according to any one of claims 1 to 6, characterized by that the antioxidant is selected from d-α-tocopherol, dl-α-tocopherol, mixed tocopherols, rosemary extract, phospholipids, butylhydroxyanisole, antioxidant 264, t-butylhydroquinone and mixtures thereof. [8] Double microencapsulated powder with differently polar core materials, which can be produced according to the recipe of any one of claims 1 to 7, characterized by , that the powder comprises the core materials of group A and group B with different polarities, wherein the particle size D90 of the multinucleate microcapsule of the first layer is in the range of 2 - 20 µm, and wherein the particle size D90 of the multinucleate microcapsule of the second layer is in the range of 20 - 50 µm. [9] Recipe according to any one of claims 1 to 7, characterized by that the core material of group A is selected from lipophilic core materials and the lipophilic core materials are selected from astaxanthin oils. [10] Astaxanthin oil for the recipe according to claim 9, characterized by that the astaxanthin oil is produced using an astaxanthin oil extraction device comprising a mixing vessel, a cavitation agent, a static mixer, a three-phase centrifuge and a precision filter, wherein The mixing vessel is configured to mix Haematococcus pluvialis, water and phospholipase to produce a uniform sludge. The cavitation agent is configured to take up the sludge and destroy the cell walls of the sludge by hydraulic cavitation to produce sludge with destroyed cell walls. the static mixer is configured to mix the sludge with destroyed cell walls and an extraction agent to produce a mixed sludge, the three-phase centrifuge is configured to receive the mixed sludge and separate it into three phases to produce an astaxanthin oil phase, an aqueous phase, and a residue, and The precision filter is configured to filter the astaxanthin oil phase to remove the remaining residue and obtain the astaxanthin oil. [11] Astaxanthin oil according to claim 10, characterized by, that the astaxanthin oil extraction device further includes a cooler configured to receive the sludge with destroyed cell walls from the cavitation agent, cool it, and transfer it to the static mixer. [12] Astaxanthin oil according to claim 11, characterized by , that the astaxanthin oil extraction apparatus further comprises several power pumps, the several power pumps including: a feed pump for mixed materials, configured to provide power for the transfer of the sludge in order to transfer the sludge from the mixing vessel to the cavitation medium, a feed pump for damaged cell wall sludge, configured to provide power for transferring the damaged cell wall sludge from the cavitation medium to the cooler, and a feed pump for extraction solvent, configured to provide power for the transfer of the extraction solvent to introduce the extraction solvent into the static mixer. [13] Astaxanthin oil according to claim 12, characterized by , that the astaxanthin oil extraction apparatus further comprises several storage tanks, the several storage tanks including: a storage container for sludge with destroyed cell walls, configured to store sludge with destroyed cell walls, a storage container for oleoresin, configured to store astaxanthin oil, a wastewater storage tank configured to store the aqueous phase separated during three-phase separation, and a waste storage container configured to store the residue separated during three-phase separation. [14] Astaxanthin oil according to any one of claims 10-13, characterized by , that the mass ratio of Haematococcus Pluvialis to water is 1 : 3 to 1 : 10 and the amount of phospholipase used is 1% to 5% of the mass of Haematococcus Pluvialis. [15] Astaxanthin oil according to claim 10 or 11, characterized by that the destruction of the cell walls takes 0.5 hours to 3 hours and that the temperature of the circulating water in the cooler is not higher than 20°C. [16] Astaxanthin oil according to any one of claims 10-15, characterized by that the extraction solvent is selected from medium-chain fatty acid glycerides (MCTs) and ethylated vegetable oils. [17] Astaxanthin oil according to one of claims 10-16, characterized by , that the amount of extraction solvent used is 0.3 to 5 times the dry amount of Haematococcus Pluvialis. [18] Astaxanthin oil according to one of claims 10-17, characterized by that the rotational speed of the three-phase centrifuge is in the range of 3000 rpm - 6000 rpm.

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