A pet nutrition paste with a complex vitamin-mineral synergy and a method for preparing the same

Abstract

The present application relates to the field of pet nutrition food, and discloses a kind of compound vitamin mineral synergistic pet nutrition cream and preparation method thereof, and the nutrition cream includes glycerol, liquid sorbitol, purified water, octenyl succinic anhydride modified starch, sodium alginate, hydrophilic fumed silica, micronized calcium sulfate dihydrate, fat-soluble active ingredient and water-soluble nutrient salt.By dispersing sodium alginate and modified starch in glycerol in advance, direct entry of polysaccharide powder into water is avoided, and surface hydration aggregation occurs;At the same time, the slow release of calcium ions from micronized calcium sulfate dihydrate and the coordination complexation with sodium alginate are combined with the amphiphilic structure of modified starch to construct a three-dimensional gel emulsion network.The above-mentioned formula and asynchronous feeding process resist the salting-out and dehydration shrinkage tendency caused by high concentration of electrolyte, solve the problems of free water precipitation, oil-water separation and polysaccharide precipitation that easily occur in high salt load nutrition cream, and obtain a product with uniform texture and stable phase.

Description

Technical Field

[0001] This invention relates to the field of pet nutritional food, specifically to a pet nutritional paste containing compound vitamins and minerals and its preparation method. Background Technology

[0002] Pet nutritional pastes, as a high-density nutritional supplement, are widely used in pets' daily health care and nutritional recovery during special physiological periods. Current nutritional paste products are typically formulated with a mixture of polyhydroxy alcohol bases, water, oils, and various vitamins and minerals. To meet the comprehensive nutritional needs of pets, the research and production process requires the simultaneous addition of a high proportion of fat-soluble active ingredients and water-soluble nutrient salts to a limited paste matrix. Simultaneously, to maintain the stable physical form of the paste and impart suitable extrusion properties, high-molecular-weight polysaccharides are often introduced into the formulation as thickeners or emulsifiers to construct a continuous phase system.

[0003] In the large-scale preparation of nutritional pastes, the feeding and dispersion of polymer materials face objective physical limitations. When polysaccharide powders such as sodium alginate or modified starch are directly added to a continuous aqueous phase, the outer surface of the powder particles rapidly absorbs water and hydrates, forming a dense and viscous colloidal layer. This outer structure hinders the further penetration of water into the particle interior, causing the internal dry powder to be encapsulated, thus forming agglomerates in the system that are difficult to dissociate by conventional mechanical stirring. This uneven dispersion at the microscopic level directly affects the full performance of the thickening and emulsifying functions of the polymer materials, easily resulting in a rough texture in the final paste, and consequently affecting the batch stability of industrial production.

[0004] When a paste formulation is loaded with a high concentration of water-soluble nutrients, the introduction of a large number of inorganic ions and polar molecules alters the osmotic pressure and ionic strength of the continuous phase. High concentrations of electrolytes in the aqueous phase easily trigger salting-out, stripping the hydration layer around the polysaccharide molecular chains and weakening the double-layer repulsion and steric hindrance at the oil-water interface. Under this high-salt stress, the originally dispersed lipid-soluble droplets are prone to aggregation and demulsification, while the polysaccharide continuous phase also weakens its capillary retention capacity for free water due to dehydration and shrinkage tendencies. With prolonged storage time or fluctuations in ambient temperature, phase separation phenomena such as oil-water separation, free water precipitation, and polysaccharide precipitation easily occur within the paste, affecting the product's physical stability and the final user experience. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a pet nutritional paste with synergistic effects of complex vitamins and minerals and its preparation method. This solves the problems of water and oil separation and polysaccharide precipitation caused by the electrolyte salting-out effect damaging the emulsion interface and polysaccharide hydration layer when existing pet nutritional pastes are loaded with high concentrations of water-soluble nutrient salts and fat-soluble components, as well as the problem of surface hydration and formation of difficult-to-dissociate aggregates when polymer powders are directly added to water.

[0006] To achieve the above objectives, the present invention provides a pet nutritional paste with synergistic effects of compound vitamins and minerals, using the following technical solution: A pet nutritional paste containing a complex of vitamins and minerals is made from the following ingredients in parts by weight: 300-435 parts glycerin; 250-300 parts liquid sorbitol; 50-111 parts purified water; 20-50 parts octenyl succinic anhydride-modified starch; 5-20 parts sodium alginate; 5-15 parts hydrophilic fumed silica; 2-10 parts micronized calcium sulfate dihydrate; 4-12 parts fat-soluble active ingredients; and 166-245 parts water-soluble nutrients. In this pet nutritional paste, the micronized calcium sulfate dihydrate slowly releases calcium ions, which coordinate and complex with sodium alginate. This, combined with the amphiphilic properties of the octenyl succinic anhydride-modified starch, forms a three-dimensional gel emulsion network to resist phase separation stress caused by the water-soluble nutrients. Simultaneously, the sodium alginate and octenyl succinic anhydride-modified starch are pre-dispersed in the glycerin to prevent direct contact and hydration aggregation of the polymer powders in the aqueous phase.

[0007] By adopting the above technical solution, a highly stable phase state of the system is achieved due to the combination of a multi-component composite formulation and a multiphase interface assembly strategy. To achieve this stable phase state, this solution incorporates targeted designs in the compatibility and mixing mechanisms. Specifically, polysaccharide macromolecules are prone to agglomeration when directly introduced into water; therefore, this invention utilizes glycerol as a medium for initial physical isolation. After dispersing sodium alginate and octenyl succinic anhydride modified starch powder in the glycerol system, the surface of the polymer powder is wetted and coated by glycerol molecules, forming a physical isolation layer. This effectively cuts off the initial diffusion path of polysaccharide macromolecules to purified water, physically preventing the agglomeration of the powder particles due to water absorption and swelling of the outer layer, thus ensuring uniform release of the polymer during subsequent mixing.

[0008] After solving the agglomeration problem of powdered raw materials, the key is to construct and maintain a stable oil-water interface. In this process, octenyl succinic anhydride-modified starch molecules, due to their hydrophilic and hydrophobic dual-block structure, actively adsorb and anchor their hydrophobic ends to the surface of lipid-soluble active ingredient droplets under the action of a fluid shear field, while their hydrophilic ends extend outward into the continuous aqueous phase. This molecular assembly process forms a dense protective film and a three-dimensional barrier at the oil-water interface, preventing lipid droplets from agglomerating and demulsifying under Brownian motion collisions and high-salt stress.

[0009] Furthermore, to further resist continuous phase separation caused by the high-salt environment, an endogenous slow-release crosslinking mechanism is introduced to solidify the three-dimensional framework. Specifically, the dispersed micronized calcium sulfate dihydrate in the system slowly dissociates into free calcium ions in the liquid phase through solid-liquid equilibrium. With the mixing of the fluid microenvironment, the dissociated calcium ions undergo a steady-state coordination complexation reaction with the guluronic acid units on the sodium alginate molecular chain. The specific reaction formula is as follows: CaSO4·2H2O⇌Ca 2+ +SO4 2+ +2H2O; 2Alg-COO - +Ca 2+ →(Alg-COO)2Ca; The delayed dissociation kinetics constructed using slightly soluble salts effectively suppressed the localized, violent coagulation phenomenon caused by excessively high instantaneous concentrations of free calcium ions. This design allows the system to maintain cross-linking activity during hydrodynamic shearing, preventing the formation of microscopic precipitates that lose their adhesiveness. As mixing progresses, the coordination complexation reaction is gradually completed throughout the entire domain, generating a uniformly distributed and dense three-dimensional gel network. This three-dimensional gel network forms capillary retention forces on water molecules and oil droplets encapsulated by modified starch. Combined with the thixotropic space constructed by hydrophilic fumed silica, it jointly resists the tendency of continuous phase dehydration and shrinkage caused by high concentrations of water-soluble nutrients, thus maintaining a stable physical phase without water or oil separation when facing mechanical stress and thermodynamic competition.

[0010] Preferably, the fat-soluble active ingredient is composed of a mixture of coenzyme Q10, vitamin A acetate, cholecalciferol, and dl-α-tocopherol acetate.

[0011] More preferably, the mass ratio of the coenzyme Q10, vitamin A acetate, cholecalciferol and dl-α-tocopherol acetate is 1:1:1:1.

[0012] By adopting the above technical solution, fat-soluble vitamins and coenzyme components form a stable composite microemulsion core system in equal mass ratios, ensuring the uniform distribution of active substances within the modified starch emulsion network, avoiding interfacial tension imbalance caused by excessive concentration of a single component, and maintaining the uniformity of emulsion droplet size distribution.

[0013] Preferably, the water-soluble nutrient salt is composed of a mixture of pig heart hydrolysate, taurine, L-carnitine, magnesium aspartate, and ferrous glycine.

[0014] More preferably, the mass ratio of the hydrolyzed pig heart powder, taurine, L-carnitine, magnesium L-aspartate, and ferrous glycine is 1:1:1:1:1.

[0015] By adopting the above technical solution, amino acids, peptides and inorganic metal salts are compounded in equal proportions to construct a continuous aqueous environment with stable ionic strength and uniform osmotic pressure distribution. This promotes a relatively stable dynamic equilibrium of electrolyte concentration in the aqueous phase and reduces the selective damage to local areas of the three-dimensional gel skeleton caused by a single high-salt component.

[0016] Preferably, the degree of substitution parameter of the octenyl succinic anhydride modified starch is in the range of 0.015 to 0.020.

[0017] By employing the above technical solution, the degree of substitution of modified starch was controlled within this specific parameter range, establishing a balance between the number of hydrophobic octenyl long chains and hydrophilic hydroxyl groups on the molecular chain. This structural ratio ensures that the polymer has sufficient lipophilic anchoring ability while retaining a hydrophilic extended conformation to penetrate into the calcium alginate gel network, establishing physical entanglement between the emulsion interface and the continuous phase backbone, and preventing oil phase aggregation due to excessive hydrophobicity or interfacial desorption due to excessive hydrophilicity.

[0018] Preferably, the octenyl succinic anhydride modified starch is prepared by a specific method comprising the following steps: uniformly dispersing waxy corn starch in purified water to prepare a starch milk suspension with a mass fraction of 35%–40%; raising the system temperature to 35–40°C, adding a 3% sodium hydroxide aqueous solution dropwise to maintain the pH value of the system at 8.0–8.5; adding 2.5%–3.5% of the dry starch stock solution dropwise at a constant rate over 1–2 hours under mechanical stirring, while continuously adding the sodium hydroxide aqueous solution to maintain the pH value; continuing the reaction for 2–4 hours after the addition is complete, adding a 1 mol / L hydrochloric acid solution to adjust the pH to 6.0–6.5 to terminate the reaction; centrifuging and washing, vacuum drying at 40–45°C until the moisture content is below 10%, and pulverizing through a 100-mesh sieve to obtain the final product.

[0019] By employing the above technical solution, the pH of the esterification microenvironment is dynamically controlled by a low-concentration alkaline solution. Combined with the constant-rate dropwise addition of octenyl succinic anhydride stock solution and synergistic temperature regulation, uniform surface and internal esterification of starch granules is achieved in a non-gelatinized state. Subsequent washing and vacuum drying processes remove free reagents and reaction byproducts, ensuring the physicochemical stability of the modified starch as an emulsifier.

[0020] Secondly, the present invention provides a method for preparing a pet nutritional paste with synergistic effects of compound vitamins and minerals, using the following technical solution: A method for preparing a pet nutritional paste with synergistic effects of complex vitamins and minerals includes the following steps: S1. Weigh out each component raw material according to the formula weight of the pet nutritional paste and set aside. S2, micronized calcium sulfate dihydrate, fat-soluble active ingredients, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred to disperse to obtain the first mixture; S3, add water-soluble nutrients to a mixture of purified water and liquid sorbitol, heat and stir until the solid disintegrates to obtain a supersaturated nutrient suspension syrup, i.e., the second mixture; S4, the first mixture is put into a high-shear homogenizing reactor, and the second mixture is slowly pumped into the reactor under continuous high-speed shear, maintaining the high-shear state until the material emulsifies and cross-links. S5. Cool the reactor and start the vacuum pump to draw it to negative pressure. Under the set absolute vacuum and high shear rate, continue to homogenize and degas. Release the vacuum and discharge the material to obtain the target product.

[0021] By adopting the above technical solution, this invention designs an asynchronous feeding process from the perspective of phase separation in the preparation method. Specifically, glycerol is first used as a medium to prevent the agglomeration and dispersion of the dry powder components, while sorbitol and aqueous solution are used to carry high-concentration nutrients. When these two mixed systems converge in the high-intensity mechanical field of the homogenizing equipment, it promotes the assembly of hydrophobic groups to form a coating interface, and the hydration and unfolding of the polymer. Accompanied by the continuous release of calcium ions and the driving of coordination reactions, this ensures the synchronous construction and uniform distribution of the micro-gel crosslinking network and microemulsion droplets in the hydrodynamic field. The vacuum cooling and degassing operation at the end removes the gas-phase microbubbles encapsulated inside the material, eliminating structural defects and oxidation risks caused by cavitation effects.

[0022] Preferably, in step S2, the processing parameters are controlled as follows: at room temperature, mechanically stir and disperse at a speed of 400-600 r / min for 15-25 minutes.

[0023] By adopting the above technical solution, the set stirring speed and time conditions are sufficient to break the physical agglomeration between powder particles, so that glycerol molecules can be fully infiltrated into the gaps between powder particles to form a fully isolated suspension system. At the same time, it avoids the system heating caused by long-term high-intensity shear, which would lead to the degradation of polysaccharide molecules.

[0024] Preferably, in step S3, the controlled processing parameters are: heating temperature of 40-50℃ and mechanical stirring speed of 200-400 r / min.

[0025] By adopting the above technical solution, the ability of purified water and sorbitol to dissolve multi-component mixed salt systems is improved by moderately increasing the temperature. Combined with stirring, the rapid dissociation and suspension of solid crystals are ensured, thus creating a high-concentration nutrient continuous phase environment without the residue of coarse particles.

[0026] Preferably, the specific implementation method and process parameters of step S4 are as follows: the rotor speed is set to 3000-3800 r / min, the second mixture is pumped in at a constant speed within 10-20 minutes, and the system temperature is controlled between 38-48℃ during the injection period.

[0027] By employing the above technical solution, the high-intensity shear force of the stator and rotor rapidly breaks down and recombines the incoming aqueous phase and nutrients with the non-solvent system containing oil and polysaccharides. During this process, the controlled pumping rate ensures that the expansion of the phase interface matches the rate of the calcium ion-driven cross-linking reaction. Furthermore, the reaction temperature range of 38–48°C not only guarantees the chain mobility of the modified starch molecules and accelerates emulsification, but also avoids the problem of heat-sensitive vitamin oxidation and inactivation caused by high temperatures.

[0028] Preferably, in step S5, the reaction performance parameters and processing method are controlled as follows: the reaction system is cooled to 30-40°C, the absolute vacuum in the reactor is evacuated to -0.08 to -0.095 MPa, and homogenization and degassing are carried out continuously for 20-40 minutes at this vacuum and a high shear rate of 3000-3800 r / min.

[0029] By employing the above technical solution, material cooling promotes the shrinkage, fixation, and strength enhancement of the calcium alginate coordination gel network. Furthermore, the combination of negative pressure and mechanical shearing causes the tiny air bubbles encapsulated within the material to expand, rupture, and overflow to the surface, ultimately yielding a dense, microstructured, and continuous fluid matrix as the final product.

[0030] This invention provides a pet nutritional paste containing compound vitamins and minerals in synergistic effects and its preparation method. It has the following beneficial effects: 1. This invention pre-disperses sodium alginate and octenyl succinic anhydride-modified starch in glycerol, utilizing the glycerol medium to initially wet and physically isolate the surface of the polymer powder. This feeding strategy cuts off the path of direct contact between polysaccharide macromolecules and large amounts of purified water, avoiding the formation of agglomerates by the polymer powder rapidly absorbing water and swelling in the aqueous phase, thus ensuring uniform dispersion of the polymer material in the system and reducing macroscopic phase defects in the industrial preparation process; 2. This invention utilizes micronized calcium sulfate dihydrate to slowly release calcium ions, which coordinate with sodium alginate to form a complex. Simultaneously, it leverages the amphiphilic properties of octenyl succinic anhydride-modified starch to construct a three-dimensional gel emulsion network. The modified starch anchors lipid-soluble droplets, forming a spatial barrier, while the calcium alginate gel network generates capillary retention force on the continuous aqueous phase. Together, they resist the salting-out and dehydration shrinkage tendencies caused by high concentrations of water-soluble nutrients, thus solving the problems of free water precipitation and oil-water separation that are prone to occur in high-salt-load formulations. 3. This invention achieves the simultaneous construction of the microemulsion interface and cross-linked network through an asynchronous feeding mixing process combined with end-of-pipe vacuum cooling. In the preparation process, the oil-containing phase and polysaccharide non-solvent system are combined with a high-salt aqueous solution under a high shear field, matching the phase interface reorganization rate with the calcium ion cross-linking reaction rate. Subsequently, continuous homogenization under negative pressure cooling not only promotes the shrinkage and fixation of the gel skeleton but also eliminates air bubbles trapped within the material, thereby eliminating cavitation defects within the structure and mitigating the risk of oxidative inactivation of heat-sensitive vitamins. Attached Figure Description

[0031] Figure 1 This is a diagram showing the correlation between the rheological characteristics and particle sedimentation dynamics of the composite pet nutritional paste of the present invention. Figure 2 The graph shows the trend of the retention rate of fat-soluble active ingredients in the nutritional paste of the present invention during accelerated aging, wherein (a) is a graph showing the change in the retention rate of coenzyme Q10 in the system during a 90-day storage period; and (b) is a graph showing the change in the retention rate of vitamin A acetate in the system during a 90-day storage period. Figure 3 This is a graph showing the relationship between the time required for dispersing the solution and the particle size of the finished nutritional paste according to the present invention. Figure 4 This is a correlation diagram showing the results of accelerated centrifugation forced destruction test of the high-salt-loaded system of the present invention. Detailed Implementation

[0032] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0033] The main raw materials and reagents used in the following examples and comparative examples have the following sources and specifications. Reagents not specifically mentioned are all commercially available analytical grade or higher grade products.

[0034] Glycerin, pharmaceutical grade, purity greater than or equal to 99.5%, CAS No.: 56-81-5.

[0035] Liquid sorbitol, food grade, 70% solids content, CAS No.: 50-70-4.

[0036] Waxy corn starch, with amylopectin content greater than or equal to 95%, CAS No.: 9005-25-8.

[0037] Octenyl succinic anhydride, purity greater than or equal to 97%, CAS No.: 42482-06-4.

[0038] Sodium alginate, with a weight-average molecular weight of 200,000 to 300,000, contains guluronic acid and mannouronic acid in its molecular chain, and the molar ratio of guluronic acid to mannouronic acid is 1.5. CAS No.: 9005-38-3.

[0039] Hydrophilic fumed silica with a specific surface area of ​​200 square meters per gram, CAS No.: 112945-52-5.

[0040] Micronized calcium sulfate dihydrate, with a median particle size (D50) of 5 to 10 micrometers and a purity greater than or equal to 98%, CAS No.: 10101-41-4.

[0041] Pig heart hydrolyzed powder is a commercially available powder extract obtained by enzymatic hydrolysis of pig heart with protease, followed by concentration and drying. The crude protein content is greater than or equal to 70%.

[0042] Taurine, purity greater than or equal to 99%, CAS No.: 107-35-7.

[0043] L-carnitine, purity greater than or equal to 99%, CAS No.: 541-15-1.

[0044] L-aspartic acid magnesium salt, purity greater than or equal to 98%, CAS No.: 2068-80-6.

[0045] Ferrous glycine, with an iron mass fraction greater than or equal to 20% and a purity greater than or equal to 98%, CAS No.: 20150-34-9.

[0046] Coenzyme Q10, purity greater than or equal to 98%, CAS number: 303-98-0.

[0047] Vitamin A acetate, with a potency of 500,000 IU per gram, CAS No.: 127-47-9.

[0048] Cholecalciferol, with a potency of 100,000 IU per gram, CAS No.: 67-97-0.

[0049] dl-α-tocopherol acetate, purity greater than or equal to 98%, CAS No.: 7695-91-2.

[0050] Preparation Example 1: This preparation example provides a method for preparing a centrally preferred octenyl succinic anhydride modified starch with a degree of substitution of 0.018, comprising the following steps: Step 1: Weigh a certain amount of waxy corn starch and disperse it evenly in purified water to prepare a starch milk suspension with a mass fraction of 38%. Step 2: Place the reaction vessel containing the suspension in a constant temperature water bath, slowly raise the system temperature to 38°C, and add a 3% sodium hydroxide aqueous solution to adjust and stabilize the pH of the system at 8.2. Step 3: Accurately weigh 3.0% of the dry starch mass of octenyl succinic anhydride, and slowly add the octenyl succinic anhydride stock solution to the starch milk at a constant rate over 1.5 hours under a mechanical stirring speed of 350 r / min. During the addition, continuously add a 3% sodium hydroxide aqueous solution to strictly maintain the dynamic equilibrium of the system pH value at 8.2. Step 4: After the addition is complete, maintain the system temperature at 38℃ and continue stirring for 3 hours. Add 1 mol / L hydrochloric acid solution to adjust the pH value of the system back to 6.2 to terminate the esterification reaction. Transfer the resulting reaction solution to a centrifuge and centrifuge at 3500 r / min for 12 minutes. Discard the supernatant and wash the bottom precipitate three times alternately with purified water and anhydrous ethanol. Step 5: Place the washed filter cake in a vacuum drying oven at 42°C and dry it until the moisture content of the product is less than 10%. After cooling, crush it and pass it through a 100-mesh sieve to obtain the target product. Seal and store it in the dark for later use.

[0051] Preparation Example 2: This preparation example provides a method for preparing low-substitution-degree boundary octenyl succinic anhydride modified starch with a substitution degree of 0.015, including the following steps: Step 1: Weigh a certain amount of waxy corn starch and disperse it evenly in purified water to prepare a starch milk suspension with a mass fraction of 35%. Step 2: Place the reaction vessel containing the suspension in a constant temperature water bath, slowly raise the system temperature to 35°C, add 3% sodium hydroxide aqueous solution, adjust the pH value of the system and stabilize it at 8.0. Step 3: Accurately weigh 2.5% of the dry starch mass of octenyl succinic anhydride, and slowly add the octenyl succinic anhydride stock solution to the starch milk at a constant rate over 1 hour under a mechanical stirring speed of 300 r / min. During the addition, continuously add a 3% sodium hydroxide aqueous solution to strictly maintain the dynamic equilibrium of the system pH value at 8.0. Step 4: After the addition is complete, keep the system temperature at 35℃ and continue stirring for 2 hours. Add 1 mol / L hydrochloric acid solution to adjust the pH value of the system back to 6.0 to terminate the esterification reaction. Transfer the resulting reaction solution to a centrifuge and centrifuge at 3000 r / min for 10 minutes. Discard the supernatant and wash the bottom precipitate three times alternately with purified water and anhydrous ethanol. Step 5: Place the washed filter cake in a vacuum drying oven at 40°C and dry it until the moisture content of the product is less than 10%. After cooling, crush it and pass it through a 100-mesh sieve to obtain the target product. Seal and store it in the dark for later use.

[0052] Preparation Example 3: This preparation example provides a method for preparing a high-substitution-degree boundary octenyl succinic anhydride modified starch with a substitution degree of 0.020, comprising the following steps: Step 1: Weigh a certain amount of waxy corn starch and disperse it evenly in purified water to prepare a starch milk suspension with a mass fraction of 40%. Step 2: Place the reaction vessel containing the suspension in a constant temperature water bath, slowly raise the system temperature to 40°C, and add a 3% sodium hydroxide aqueous solution to adjust and stabilize the pH of the system at 8.5. Step 3: Accurately weigh 3.5% of the dry starch mass of octenyl succinic anhydride, and slowly add the octenyl succinic anhydride stock solution to the starch milk at a constant rate over 2 hours under a mechanical stirring speed of 400 r / min. During the addition, continuously add a 3% sodium hydroxide aqueous solution to strictly maintain the dynamic equilibrium of the system pH value at 8.5. Step 4: After the addition is complete, keep the system temperature at 40℃ and continue stirring for 4 hours. Add 1 mol / L hydrochloric acid solution to adjust the pH value of the system back to 6.5 to terminate the esterification reaction. Transfer the resulting reaction solution to a centrifuge and centrifuge at 4000 r / min for 15 minutes. Discard the supernatant and wash the bottom precipitate three times alternately with purified water and anhydrous ethanol. Step 5: Place the washed filter cake in a vacuum drying oven at 45°C and dry it until the moisture content of the product is less than 10%. After cooling, crush it and pass it through a 100-mesh sieve to obtain the target product. Seal and store it in the dark for later use.

[0053] Example 1: This example provides a method for preparing a pet nutritional paste with synergistic effects of compound vitamins and minerals, including the following steps: S1, accurately weigh 380 g glycerol, 280 g liquid sorbitol, 100 g purified water, 35 g octenyl succinic anhydride modified starch obtained in Preparation Example 1, 12 g sodium alginate, 10 g hydrophilic fumed silica, 5 g micronized calcium sulfate dihydrate, 2 g coenzyme Q10, 2 g vitamin A acetate, 2 g cholecalciferol, 2 g dl-α-tocopherol acetate, 34 g hydrolyzed pig heart powder, 34 g taurine, 34 g L-carnitine, 34 g magnesium aspartate, and 34 g ferrous glycinate; S2, micronized calcium sulfate dihydrate, coenzyme Q10, vitamin A acetate, cholecalciferol, dl-α-tocopherol acetate, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred and dispersed at 500 r / min for 20 minutes at room temperature to obtain the first mixture. S3, add the hydrolyzed pig heart powder, taurine, L-carnitine, magnesium aspartate and ferrous glycine to a mixture of purified water and liquid sorbitol, heat to 45°C and stir at 300 r / min until the large solid particles disintegrate, to obtain a uniform supersaturated nutrient suspension syrup, i.e. the second mixture. S4. The first mixture is put into the high-shear homogenizing reactor. The stator and rotor are turned on and the speed is set to 3400 r / min. Under continuous high-speed shear, the second mixture is slowly pumped into the reactor within 15 minutes. During the feeding process, the system temperature is controlled at 43°C and the high-shear state is maintained until the material is completely emulsified and cross-linked. S5. Cooling water is introduced into the jacket of the reactor to cool the system to 35°C. The vacuum pump is started to draw the absolute vacuum inside the reactor to -0.09MPa. Homogenization and degassing are carried out for 30 minutes at this vacuum and a high shear rate of 3400r / min. The vacuum is then released and the product is discharged to obtain the target product.

[0054] Example 2: This example provides a method for preparing a pet nutritional paste with synergistic effects of compound vitamins and minerals, including the following steps: S1, accurately weigh 435 g glycerol, 250 g liquid sorbitol, 50 g purified water, 50 g octenyl succinic anhydride modified starch obtained in Preparation Example 2, 20 g sodium alginate, 15 g hydrophilic fumed silica, 10 g micronized calcium sulfate dihydrate, 1 g coenzyme Q10, 1 g vitamin A acetate, 1 g cholecalciferol, 1 g dl-α-tocopherol acetate, 33.2 g hydrolyzed pig heart powder, 33.2 g taurine, 33.2 g L-carnitine, 33.2 g magnesium L-aspartate, and 33.2 g ferrous glycine; S2, micronized calcium sulfate dihydrate, coenzyme Q10, vitamin A acetate, cholecalciferol, dl-α-tocopherol acetate, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred and dispersed at 400 r / min for 25 minutes at room temperature to obtain the first mixture; S3, add pig heart hydrolysate, taurine, L-carnitine, magnesium aspartate and ferrous glycine to a mixture of purified water and liquid sorbitol, heat to 40°C and stir at 200 r / min until large solid particles disintegrate, to obtain a uniform supersaturated nutrient suspension syrup, i.e. the second mixture. S4. The first mixture is put into the high-shear homogenizing reactor. The stator and rotor are turned on and the speed is set to 3000 r / min. Under the continuous high-speed shear state, the second mixture is slowly pumped into the reactor within 20 minutes. During the feeding process, the system temperature is controlled at 38°C and the high-shear state is maintained until the material is completely emulsified and cross-linked. S5. Cooling water is introduced into the jacket of the reactor to cool the system to 30°C. The vacuum pump is started to draw the absolute vacuum inside the reactor to -0.08MPa. Homogenization and degassing are carried out for 40 minutes at this vacuum and a high shear rate of 3000r / min. The vacuum is then released and the product is discharged to obtain the target product.

[0055] Example 3: This example provides a method for preparing a pet nutritional paste with synergistic effects of complex vitamins and minerals, including the following steps: S1, accurately weigh 300g glycerol, 300g liquid sorbitol, 111g purified water, 20g octenyl succinic anhydride modified starch obtained in Preparation Example 3, 5g sodium alginate, 5g hydrophilic fumed silica, 2g micronized calcium sulfate dihydrate, 3g coenzyme Q10, 3g vitamin A acetate, 3g cholecalciferol, 3g dl-α-tocopherol acetate, 49g hydrolyzed pig heart powder, 49g taurine, 49g L-carnitine, 49g magnesium aspartate, and 49g ferrous glycinate; S2, micronized calcium sulfate dihydrate, coenzyme Q10, vitamin A acetate, cholecalciferol, dl-α-tocopherol acetate, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred and dispersed at 600 r / min for 15 minutes at room temperature to obtain the first mixture. S3, add pig heart hydrolysate, taurine, L-carnitine, L-aspartate magnesium salt and glycine ferrous salt to a mixture of purified water and liquid sorbitol, heat to 50°C and stir at 400 r / min until large solid particles disintegrate, to obtain a uniform supersaturated nutrient suspension syrup, i.e. the second mixture. S4. The first mixture is put into the high-shear homogenizing reactor. The stator and rotor are turned on and the speed is set to 3800 r / min. Under continuous high-speed shear, the second mixture is slowly pumped into the reactor within 10 minutes. During the feeding process, the system temperature is controlled at 48℃ and the high-shear state is maintained until the material is completely emulsified and cross-linked. S5. Cooling water is introduced into the jacket of the reactor to cool the system to 40°C. The vacuum pump is started to draw the absolute vacuum inside the reactor to -0.095MPa. Homogenization and degassing are carried out for 20 minutes at this vacuum and a high shear rate of 3800r / min. The vacuum is then released and the product is discharged to obtain the target product.

[0056] Example 4: This example provides a method for preparing a pet nutritional paste with synergistic effects of complex vitamins and minerals, including the following steps: S1, accurately weigh 380 g glycerol, 280 g liquid sorbitol, 100 g purified water, 35 g octenyl succinic anhydride modified starch obtained in Preparation Example 1, 12 g sodium alginate, 10 g hydrophilic fumed silica, 5 g micronized calcium sulfate dihydrate, 2 g coenzyme Q10, 2 g vitamin A acetate, 2 g cholecalciferol, 2 g dl-α-tocopherol acetate, 34 g hydrolyzed pig heart powder, 34 g taurine, 34 g L-carnitine, 34 g magnesium aspartate, and 34 g ferrous glycinate; S2, micronized calcium sulfate dihydrate, coenzyme Q10, vitamin A acetate, cholecalciferol, dl-α-tocopherol acetate, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred and dispersed at 600 r / min for 15 minutes at room temperature to obtain the first mixture. S3, add pig heart hydrolysate, taurine, L-carnitine, L-aspartate magnesium salt and glycine ferrous salt to a mixture of purified water and liquid sorbitol, heat to 50°C and stir at 400 r / min until large solid particles disintegrate, to obtain a uniform supersaturated nutrient suspension syrup, i.e. the second mixture. S4. The first mixture is put into the high-shear homogenizing reactor. The stator and rotor are turned on and the speed is set to 3800 r / min. Under continuous high-speed shear, the second mixture is slowly pumped into the reactor within 10 minutes. During the feeding process, the system temperature is controlled at 48℃ and the high-shear state is maintained until the material is completely emulsified and cross-linked. S5. Cooling water is introduced into the jacket of the reactor to cool the system to 40°C. The vacuum pump is started to draw the absolute vacuum inside the reactor to -0.095MPa. Homogenization and degassing are carried out for 40 minutes at this vacuum and a high shear rate of 3800r / min. The vacuum is then released and the product is discharged to obtain the target product.

[0057] Comparative Example 1: Compared with Example 1, the difference is that the order of feeding was changed, the non-solvent pre-dispersion step was skipped, and sodium alginate and octenyl succinic anhydride modified starch were directly added to the mixture of purified water and liquid sorbitol without glycerol pre-dispersion and heated and stirred. The micronized calcium sulfate dihydrate, fumed silica and each fat-soluble vitamin component in step S2 were still added to glycerol and mixed according to the original steps, and the rest were the same.

[0058] Comparative Example 2: Compared with Example 1, the difference is that the endogenous sustained-release cross-linking mechanism is disrupted, the 5 grams of micronized calcium sulfate dihydrate in step S2 are replaced with 3.2 grams of anhydrous calcium chloride to provide equimolar calcium ions, and 1.8 grams of purified water is added to the mixed aqueous phase system in step S3 to make up the total weight. All other aspects are the same.

[0059] Comparative Example 3: Compared with Example 1, the difference is that the modified component with high molecular steric hindrance and emulsification network mechanism was removed, and 35 grams of octenyl succinic anhydride modified starch obtained in Preparation Example 1 were replaced with an equal amount of unmodified conventional waxy corn starch, while the rest were the same.

[0060] Comparative Example 4: Compared with Example 1, the difference is that the synergistic components of the hydrogen bond network and thixotropic structure were removed, hydrophilic fumed silica was not added, and it was replaced with glycerol in equal mass; otherwise, they are the same.

[0061] Test Example 1: Test Description: This test case mainly verifies the anti-settling and shear-thinning behavior of the three-dimensional thixotropic fluid mechanism synergistically constructed by fumed silica and polysaccharide network in a macroscopic system.

[0062] Test steps: 1. The compound pet nutritional pastes prepared in Examples 1 to 4, and Comparative Examples 2 and 4, were used as experimental subjects. Each group of ointment samples was squeezed into sterile wide-mouth test bottles, sealed, and placed in a constant temperature incubator at 25°C for 24 hours to completely eliminate the residual shear stress accumulated during high-speed homogenization and filling, and to promote the complete relaxation and recovery of the internal gel network structure.

[0063] 2. The apparent viscosity of the equilibrated sample was determined using a rotational viscometer equipped with a coaxial cylindrical measuring system at low shear rate. The rotor speed was set to 2 r / min, and the sample was continuously run for 5 minutes under this constant low shear. The apparent viscosity value after the internal shear stress of the fluid reached dynamic equilibrium was recorded as the low shear viscosity of the system.

[0064] 3. Without changing the measuring cylinder and rotor, immediately increase the test speed of the same sample to 20 r / min. Continue running at this high shear rate for 5 minutes, and record the apparent viscosity value after the system structure is disrupted and reaches a stable state again, as the high shear viscosity of the system. Calculate the corresponding thixotropic index by dividing the low shear viscosity by the high shear viscosity.

[0065] 4. Weigh 50 grams of the nutrient paste sample obtained from each group of experiments and pour it into a transparent glass settling tube with a millimeter-scale ruler, ensuring no air bubbles are present. Seal the tube opening with a silicone stopper and place it vertically on a vibration-free workbench at room temperature for 30 days. After the 30-day period, use a high-precision vernier caliper to measure the absolute thickness of the inorganic mineral enrichment layer that appears at the bottom of the settling tube and record it as the settling height.

[0066] The test data is shown in Table 1: Table 1: Rheological characteristic parameters of nutritional paste and dynamic monitoring data of particle sedimentation

[0067] according to Figure 1 As shown in Table 1, Examples 1 to 4 all exhibited apparent viscosities exceeding 140,000 mPa·s at low shear rates, and the mineral sedimentation height after 30 days of standing was 0.00 mm. In the industrial scale-up process of conventional nutrient paste matrices, high-density inorganic salts often migrate downwards under gravity, leading to component enrichment in the lower layer of the system. This solution introduces micronized calcium sulfate dihydrate and sodium alginate to construct a slow-release cross-linking network, while utilizing the silanol groups on the surface of hydrophilic fumed silica to form a spatially interlocked structure. This three-dimensional physical gel framework generates yield stress sufficient to offset gravitational sedimentation in a low shear environment of 2 r / min, stably suspending inorganic phases such as ferrous glycine in a continuous aqueous phase, maintaining the macroscopic homogeneity of the material during long-term storage.

[0068] The effectiveness of the spatial interlocking mechanism was verified by the test results of Comparative Example 4. After stripping the fumed silica component, the polysaccharide framework alone failed to provide an equivalent amount of support. The low-shear viscosity of Comparative Example 4 decreased to 82340 mPa·s, and a particle-rich layer of 11.20 mm appeared at the bottom of the tube at the end of the test period. The lack of a synergistic hydrogen bond network of silanol groups meant that the static structural strength inside the fluid was insufficient to counteract the density difference between the solid and liquid phases, thus inducing phase separation. The dual network structure formed by polysaccharide cross-linking and inorganic particles is a necessary condition for overcoming particle sedimentation defects.

[0069] While possessing high static yield stress, the system needs to flow during mechanical filling and routine extrusion. The dynamic response data of apparent viscosity explains the fluid's evolution behavior. When the test shear rate jumps to 20 r / min, the apparent viscosity of each embodiment decreases rapidly, and the calculated thixotropic index ranges from 4.180 to 4.673. The applied external force causes the physical entanglement points and some hydrogen bonds between polymer chain segments to unwind, and the trapped sorbitol and free water are released to act as lubricating media, resulting in shear thinning of the system. Comparative Example 2 uses anhydrous calcium chloride with high solubility. The large amount of free calcium ions released in a short time triggers the local instantaneous solidification of sodium alginate. The resulting rigid gel block breaks into non-crosslinking active particles under the high-speed shear of the homogenizing device. The thixotropic index of this comparative example drops to 1.622, and the fluid loses its dynamic unentanglement and network recombination function, confirming that the slow-release calcium source plays a decisive role in constructing the thixotropic fluid network.

[0070] After the external shear stress is removed, the broken non-covalent bonds between molecules recombine under thermodynamic drive, and the rheological state of the system is restored. These shear thinning and viscosity recovery characteristics manifest in the production end as the paste being able to adapt to high-speed pumping by automated equipment, with smooth material flow from the nozzle when the consumer squeezes the tube, and the fluid's internal structure closing and cutting off the flow the instant the pressure is released. The correspondence between macroscopic test data and microscopic mechanisms indicates that this technical solution achieves a balance between processing fluidity and static stability by combining raw materials with specific physicochemical properties.

[0071] Test Example 2: Test Description: This test case mainly verifies the interfacial isolation and protection efficacy of the oil-in-water microemulsion system constructed by octenyl succinic anhydride modified starch for lipid-soluble core active ingredients under continuous thermodynamic stress.

[0072] Test steps: 1. The compound pet nutritional pastes prepared in Examples 1 to 4 and Comparative Example 3 were used as experimental subjects. Each group of ointment samples was filled into a standard aluminum-plastic composite light-proof tube and the tail was sealed. The tubes were then placed in an accelerated aging constant temperature and humidity test chamber with a set temperature of 40°C and a relative humidity of 75% and stored continuously in the dark for 90 days.

[0073] 2. Sampling was performed on day 0 before the start of the testing period, and on days 30, 60, and 90 during storage. Each time, three individually packaged tubes were removed parallel to each other from the container, the initial material was squeezed out and discarded, and 2 grams of the middle sample was taken from each tube and placed in a stoppered centrifuge tube.

[0074] 3. Add an appropriate amount of a mixture of isopropanol and methanol as extraction solvent to the centrifuge tube, and place it in an ice-bath ultrasonic cleaner for 20 minutes. This utilizes the ultrasonic cavitation effect to disrupt the polymer gel network and fully extract the lipid-soluble components encapsulated within the microemulsion. After extraction, centrifuge at 10000 r / min to collect the supernatant. Filter the supernatant through a 0.22 μm organic phase microporous membrane and collect the filtrate as the sample to be tested.

[0075] 4. The samples were analyzed using a high-performance liquid chromatograph equipped with a UV-Vis detector. A C18 reversed-phase column was used with gradient elution of methanol and water as the mobile phase. The peak areas of coenzyme Q10 and vitamin A acetate were recorded at wavelengths of 275 nm and 326 nm, respectively. The absolute contents at each time point were calculated using the external standard method, and the retention rates for different storage periods were calculated based on the initial contents on day 0.

[0076] The test data is shown in Table 2: Table 2: Results of Coenzyme Q10 and Vitamin A Acetate Retention Rate Tests During Accelerated Aging Processes in Nutritional Pastes

[0077] according to Figure 2 According to the data in Table 2, after 90 days of accelerated aging tests under high temperature and humidity, the retention rates of coenzyme Q10 in Examples 1 to 4 ranged from 89.4% to 92.6%, and the retention rates of vitamin A acetate remained between 87.1% and 90.3%. In the formulation and processing research of animal nutrition products, fat-soluble active substances containing unsaturated double bonds often face a definite risk of chemical degradation, especially in complex fluids containing a large amount of free water and transition metal ions such as ferrous glycine, where free iron ions easily act as catalysts to initiate oxidation chain reactions. The above retention rate indicators reflect that the phase interface isolation mechanism constructed in this technical solution has a substantial blocking effect. The molecular structure of octenyl succinic anhydride modified starch includes a hydrophilic main chain and lipophilic side chains. During homogenization, its long octenyl chain extends into the interior of tiny oil droplets and completes anchoring, while the main chain unfolds in the external continuous aqueous phase. This amphiphilic polymer assembles a robust protective film with steric hindrance at the oil-water interface, confining easily oxidized coenzymes and vitamins within micron-sized oil-in-water droplets, thus physically severing the contact diffusion path between pro-oxidants and core components in the continuous phase.

[0078] Systems lacking the protective amphiphilic interface exhibit drastically different evolutionary trajectories, as illustrated by the decay data in Comparative Example 3. This example used conventional waxy corn starch instead of modified starch; by day 90, the coenzyme Q10 retention rate had decreased to 41.3%, and vitamin A acetate had plummeted to 28.7%. Conventional polysaccharide molecules, rich only in hydrophilic hydroxyl groups, struggle to establish effective adsorption on oil droplet surfaces and reduce interfacial tension. Driven by the continuous heat energy provided by the accelerated aging environment, the unprotected micro-oil droplets, affected by thermodynamic instability, gradually undergo Brownian motion collisions and flocculation. Complete demulsification of the microemulsion system exposes a large amount of internal lipid-soluble substances to the free phase, where their conjugated structure is rapidly destroyed by dissolved oxygen and metal ions diffusing from the aqueous phase. Conventional thickeners cannot replace the phase-maintaining function of the amphiphilic components.

[0079] The long-term stability of the micro-emulsion network against thermal stress is crucial to the product's pharmacodynamic performance throughout its entire lifecycle. The 40°C environment used in the test accelerated molecular thermal motion; in the example, only a single-digit percentage of the active substance was slowly lost, indicating that the dense macro-gel framework formed by the crosslinking of modified starch with sodium alginate and fumed silica further restricts the relative displacement between oil droplets. The polymer network increases the viscosity of the liquid phase while reducing the diffusion mass transfer coefficient of oxygen molecules. This synergistic dual physical barrier mechanism enables this solution to address the technical challenge of inactivating sensitive target substances in high-salt-phase environments without relying on excessive addition of chemical antioxidants.

[0080] Test Example 3: Test Description: This test case mainly verifies the actual effectiveness of non-solvent pre-dispersion mechanism in solving the pain point of hydration and agglomeration of polymeric polysaccharide powders, and evaluates its impact on solution preparation efficiency and material micro-uniformity.

[0081] Test steps: 1. The preparation process of Examples 1 to 4 and Comparative Example 1, including the liquid preparation stage and the final product, were used as experimental subjects. When the process entered the polymer powder feeding stage, an industrial stopwatch was started for synchronous timing.

[0082] 2. During the mixing process, every minute, use a stainless steel sampler to extract a small amount of fluid from the lower part of the homogenizer and spread it onto a black, high-gloss, flat glass plate. Observe the material layer under strong light to see if there are any undissolved translucent lumps or dry powder agglomerates. When no visible agglomerates are found in the field of view after three consecutive samplings, stop timing and record the corresponding powder dispersion time.

[0083] 3. Collect samples of the finished nutritional paste from each group that have completed all process steps and undergone vacuum degassing, and place them in an indoor environment at 25°C for 12 hours to maintain a constant temperature and eliminate structural stress.

[0084] 4. The fineness of the paste particles was determined using a dual-groove scraper fineness meter with a range of 0 to 100 micrometers. A suitable amount of the constant-temperature sample was placed in the deepest groove of the fineness meter. Holding the scraper with both hands, the material was smoothly scraped across the entire scale range within 3 seconds at a constant angle perpendicular to the scale surface and with uniform force. The corresponding scale value where dense particle scratches begin to appear in the groove was immediately observed. Each group of samples was measured three times in parallel, and the arithmetic mean was recorded as the maximum particle diameter.

[0085] The test data is shown in Table 3: Table 3: Results of Liquid Preparation and Dispersion Time and Fineness Test of Finished Nutritional Paste

[0086] according to Figure 3 According to the data in Table 3, the powder dispersion time in Examples 1 to 4 ranged from 4.3 to 5.8 minutes during the preparation process, and the maximum particle diameter of the final product paste was controlled within the range of 15.8 to 22.3 micrometers. In our actual engineering operations for mass production of polysaccharide hydrogel products, we observed that high-molecular-weight powders such as sodium alginate and modified starch contain a large number of hydrophilic hydroxyl and carboxyl groups, which have extremely high thermodynamic affinity for water molecules. When these powders are directly poured into the aqueous phase using conventional feeding processes, the outer layer of the particles at the gas-liquid-solid three-phase interface undergoes intense hydration instantly, causing the molecular chains to expand rapidly and intertwine to form a dense, high-viscosity colloidal outer film. This gel outer film blocks the diffusion path of free water molecules into the particle core, resulting in the internal dry powder being encapsulated and macroscopically manifested as insoluble, fish-eye-like agglomerates. These agglomerates possess strong internal stress and extremely high structural toughness, making them difficult to completely pulverize and peel off using conventional mechanical stirring, shearing, or even high-speed homogenization.

[0087] The non-solvent pre-dispersion mechanism introduced in this scheme effectively avoids the aforementioned interfacial hydration conflicts. The polymer powder is pre-dispersed in a glycerol matrix. Since the polymer backbone cannot swell or depolymerize in glycerol, which is a poor solvent, the powder particles remain uniformly suspended in their solid state and are physically isolated at the microscale by the glycerol molecular layer. When a water-phase matrix composed of purified water and liquid sorbitol is subsequently introduced, the pre-existing solvent isolation layer allows water molecules to simultaneously and uniformly contact the surface of each individual polymer particle. The uneven distribution of water molecules due to localized competition among particles within the system is eliminated, allowing the powder monomers to achieve complete swelling and molecular chain extension in a short time. This change in the micro-interface is reflected in the process parameters, with the solution preparation time significantly reduced to less than 6 minutes. This improves batch turnover and avoids the mechanical and thermal damage to heat-sensitive substances such as coenzyme Q10 caused by prolonged high-frequency shearing.

[0088] Skipping the non-solvent pre-dispersion step significantly deteriorates the fluid state, as confirmed by the test records of Comparative Example 1. This comparative example altered the feeding sequence, directly adding polysaccharide powder to the aqueous mixture, resulting in a dramatic increase in dispersion time to 58.4 minutes. Even after nearly an hour of continuous stirring and homogenization, a significant number of incompletely disintegrated colloids remained within the material, with the largest particle diameter of the final paste reaching 89.2 micrometers. This coarse fluid microstructure severely reduces the spreadability and palatability of the nutritional paste. Furthermore, clumps suspended in the matrix interfere with the uniform dispersion of fat-soluble vitamins and inorganic mineral particles, leading to localized concentration variations during the product's shelf life. By incorporating a pre-treatment with a poor solvent suspension step, this technique establishes a steady-state dispensing method compatible with high-concentration polysaccharide thickening systems, resolving the common defect of localized colloid residue in traditional mixing processes.

[0089] Test Example 4: Test Description: This test case mainly verifies the endogenous slow-release crosslinking mechanism and the core role of the modified starch emulsion network in maintaining the phase stability of the material under the dual stress of high concentration of nutrients and extreme mechanical forces.

[0090] Test steps: 1. The finished nutritional pastes from Examples 1 to 4, and Comparative Examples 2 and 3, after preparation and equilibration at room temperature for 24 hours, were used as experimental subjects. Clean, dry 50 mL polycarbonate centrifuge tubes were taken, and the mass of the empty tubes was accurately weighed on an analytical balance.

[0091] 2. Carefully insert each group of ointment samples into the bottom of the centrifuge tube using a sterile syringe, avoiding the formation of internal air bubbles. Accurately weigh the sample to ensure the net weight of each tube is approximately 30.00 grams, and then seal the tube cap.

[0092] 3. Place the centrifuge tubes containing the samples symmetrically inside the rotor of the high-speed refrigerated centrifuge. Set the centrifuge chamber temperature to 20°C and the centrifugation speed to 15,000 rpm, and run continuously for 30 minutes under this extreme centrifugal force.

[0093] 4. After the centrifugation program is complete, remove the centrifuge tubes and let them stand on the operating table for 5 minutes. Carefully aspirate the clear or translucent oil phase floating on top of the material using a high-precision micropipette, and transfer it to a pre-weighed receiving bottle to calculate the mass of the oil phase precipitation.

[0094] 5. Tilt the centrifuge tube to pour out the free water precipitated from the surface and side walls. Use absorbent paper to dry any remaining water droplets adhering to the tube wall. Weigh the total mass of the remaining solid-liquid mixture and calculate the mass of water precipitated. Divide the precipitated mass by the initial net weight of the material to calculate the percentage of free precipitated water and the percentage of oil phase precipitated from the top layer.

[0095] The test data is shown in Table 4: Table 4: Results of Accelerated Centrifugation Forced Destruction Test on High-Salt Loading Systems

[0096] according to Figure 4 As shown in Table 4, after undergoing extreme centrifugation with accelerations thousands of times greater than gravity, Examples 1 to 4 maintained a stable physical phase with zero water and oil separation. In the formulation development of pet nutritional supplements, high contents of hydrolyzed pig heart peptides, taurine, and inorganic mineral salts can trigger a strong salting-out effect in the aqueous phase. A high-salt environment can thermodynamically compete for the hydration layer around the polysaccharide chains, disrupting the electric double layer and steric hindrance on the emulsifier surface, leading to polysaccharide precipitation, water release, and oil-water separation in conventional fluid matrices. Test data show that the examples maintained structural integrity even under extreme external forces. The system utilizes the extremely slow release of calcium ions from micronized dihydrate calcium sulfate, which steadily coordinates with the guluronic acid units on the sodium alginate molecular chain to construct a dense and uniform three-dimensional gel framework. With the hydrophobic ends of octenyl succinic anhydride-modified starch anchoring lipid droplets and the hydrophilic ends interspersed in the continuous phase, the entire three-dimensional physical network generates extremely strong capillary binding forces on water molecules and dispersed oil droplets. This internal framework, constructed by the synergy of slow-release crosslinking and amphiphilic polymers, successfully resists the tendency for dehydration and deoiling caused by high concentrations of electrolytes.

[0097] Disruption of specific spatial network nodes triggers a rapid collapse of the matrix's load-bearing capacity. Comparative Example 2 reveals the impact of crosslinking kinetics on macroscopic stability. Using highly soluble anhydrous calcium chloride, Comparative Example 2 exhibited a water content as high as 19.34% after centrifugation. The readily dissociated calcium ions induce localized, intense rigid solidification upon contact with polysaccharide molecules. The instantaneously formed crosslinked microregions are torn into fragments lacking adhesive activity under the high-frequency shearing of the homogenizing device. It is difficult to construct long-range continuous coordination chelate networks within the fluid. The mechanical stress generated by high-frequency centrifugation rapidly destroys the remaining weak physical entanglement structures within the system. The continuous aqueous phase loses the steric hindrance and capillary retention of the polymer gel skeleton, leading to large-scale dispersion under centrifugal force. This microscopic phase collapse manifests macroscopically as irreversible dehydration and shrinkage of the matrix and significant solid-liquid phase separation. The endogenous ion release mechanism constitutes the physicochemical basis for maintaining crosslinking activity and ultimately achieving homogeneous gelation in the polysaccharide macromolecular system under strong shear flow.

[0098] The suspension stability of fat-soluble active ingredients is highly dependent on the precise control and spatial isolation of the oil-water interfacial tension. In Comparative Example 3, where the core emulsifying component was replaced with ordinary waxy corn starch, the top layer of oil phase accounted for 8.27% after centrifugation. Ordinary starch molecules lack the lipophilic octenyl chain and cannot form an effective anchor at the oil droplet interface. Under the dual physical stress of high salt load depriving the continuous phase hydration layer and high centrifugal force, the microemulsion structure underwent irreversible demulsification. Driven by surface tension, the fat-soluble vitamins and coenzyme Q10 microdroplets, no longer protected by steric hindrance, collided with Brownian motion and rapidly aggregated, eventually fusing into a macroscopic oil phase floating at the top of the system. This extreme oil-water separation verifies that simply increasing the viscosity of the aqueous phase cannot maintain the stability of complex oil-in-water emulsion structures in the long term. It is necessary to achieve thermodynamic and kinetic stability of multiphase systems in industrial high-salt formulations through interfacial assembly of amphiphilic molecules combined with the physical isolation of macroscopic gel networks.

[0099] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A pet nutritional paste with synergistic effects of complex vitamins and minerals, characterized in that, Made from the following ingredients in parts by weight: 300-435 parts of glycerin; 250-300 parts of liquid sorbitol; 50-111 parts purified water; Octenyl succinic anhydride modified starch, 20-50 parts; 5-20 parts of sodium alginate; 5-15 parts of hydrophilic fumed silica; 2-10 parts of micronized calcium sulfate dihydrate; 4–12 parts of fat-soluble active ingredient; 166–245 parts of water-soluble nutrients; In the pet nutritional paste, calcium ions are slowly released through the micronized calcium sulfate dihydrate, which coordinate and complex with sodium alginate. Combined with the amphiphilic characteristics of octenyl succinic anhydride-modified starch, a three-dimensional gel emulsion network is constructed to resist the phase separation stress caused by the water-soluble nutrients. At the same time, the sodium alginate and octenyl succinic anhydride-modified starch are pre-dispersed in the glycerol to avoid direct contact and hydration aggregation of polymer powders in the aqueous phase.

2. The pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 1, characterized in that, The fat-soluble active ingredient is composed of a mixture of coenzyme Q10, vitamin A acetate, cholecalciferol, and dl-α-tocopherol acetate.

3. The pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 1, characterized in that, The water-soluble nutrient salt is composed of a mixture of pig heart hydrolysate, taurine, L-carnitine, magnesium L-aspartate, and ferrous glycine.

4. The pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 1, characterized in that, The degree of substitution parameter of the octenyl succinic anhydride modified starch ranges from 0.015 to 0.

020.

5. The pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 1, characterized in that, The octenyl succinic anhydride modified starch is prepared by a specific preparation method comprising the following steps: Waxy corn starch was uniformly dispersed in purified water to prepare a starch emulsion suspension with a mass fraction of 35% to 40%. When the system temperature is raised to 35-40℃, add a 3% sodium hydroxide aqueous solution dropwise to maintain the pH value of the system at 8.0-8.5; Under mechanical stirring, 2.5% to 3.5% of the dry starch mass of octenyl succinic anhydride stock solution was added dropwise at a constant rate over 1 to 2 hours, while the sodium hydroxide aqueous solution was continuously added dropwise to maintain the pH value. After the addition is complete, continue the reaction for 2 to 4 hours. Add a 1 mol / L hydrochloric acid solution to adjust the pH to 6.0 to 6.5 to terminate the reaction. After centrifugation and washing, vacuum dry at 40 to 45°C until the moisture content is below 10%. Grind and pass through a 100-mesh sieve to obtain the final product.

6. A method for preparing a pet nutritional paste with synergistic effects of complex vitamins and minerals, used to prepare the pet nutritional paste with synergistic effects of complex vitamins and minerals as described in any one of claims 1-5, characterized in that, Includes the following steps: S1. Weigh out each component raw material according to the formula weight of the pet nutritional paste and set aside. S2, micronized calcium sulfate dihydrate, fat-soluble active ingredients, sodium alginate, octenyl succinic anhydride modified starch and hydrophilic fumed silica are added to glycerol in sequence and stirred to disperse to obtain the first mixture; S3, add water-soluble nutrients to a mixture of purified water and liquid sorbitol, heat and stir until the solid disintegrates to obtain a supersaturated nutrient suspension syrup, i.e., the second mixture; S4, the first mixture is put into a high-shear homogenizing reactor, and the second mixture is slowly pumped into the reactor under continuous high-speed shear, maintaining the high-shear state until the material emulsifies and cross-links. S5. Cool the reactor and start the vacuum pump to draw it to negative pressure. Under the set absolute vacuum and high shear rate, continue to homogenize and degas. Release the vacuum and discharge the material to obtain the target product.

7. The method for preparing the pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 6, characterized in that, In step S2, the control parameters are as follows: at room temperature, mechanically stir and disperse at a speed of 400-600 r / min for 15-25 minutes.

8. The method for preparing the pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 6, characterized in that, In step S3, the controlled processing parameters are: heating temperature of 40-50℃ and mechanical stirring speed of 200-400 r / min.

9. The preparation method of the pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 6, characterized in that, The specific implementation method and process parameters of step S4 are as follows: the rotor speed is set to 3000-3800 r / min, the second mixture is pumped in at a constant speed within 10-20 minutes, and the system temperature is controlled between 38-48℃ during the injection period.

10. The method for preparing the pet nutritional paste with synergistic effects of compound vitamins and minerals according to claim 6, characterized in that, In step S5, the reaction performance parameters and processing method are controlled as follows: the reaction system is cooled to 30-40℃, the absolute vacuum in the reactor is evacuated to -0.08 to -0.095 MPa, and homogenization and degassing are carried out continuously for 20-40 minutes at this vacuum and a high shear rate of 3000-3800 r / min.

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