Instant composition with long-acting oral health-care function for dogs and cats as well as preparation method and application of instant composition

Abstract

The invention relates to an instant composition with a long-acting oral health-care function for dogs and cats as well as a preparation method and application of the instant composition, and belongs to the technical field of pet food and pet oral care. The composition comprises 20%-30% of whey protein powder, 10%-20% of hydrolyzed gelatin, 1%-3% of low-molecular-weight chitin saccharide gum, 1%-2% of modified cassava starch, 2%-5% of sodium alginate, 1%-3% of fructo-oligosaccharide, 0.03%-0.08% of lysozyme, 0.03%-0.08% of tea polyphenol, 0.05%-0.15% of zinc gluconate, 0.05%-0.1% of persimmon tannin, 3%-5% of tuna hydrolysate, 4%-6% of whole goat milk powder, 2%-4% of skim yoghurt powder and the balance water. The added active ingredients have long-acting slow-release and continuous effects in the formula, oral pathogenic bacteria can be effectively inhibited, dental plaque and dental calculus formation can be reduced, halitosis can be lastingly relieved, and the toothpaste has good market competitiveness.

Description

Technical Field

[0001] This application relates to a fast-dissolving composition for dogs and cats with long-lasting oral health care function, its preparation method and application, belonging to the field of pet food and pet oral care technology. Background Technology

[0002] With the continuous expansion of pet ownership in my country, pet health issues are receiving increasing attention, with oral health being particularly prominent. Statistics show that over 66% of dogs and cats aged two years and older exhibit varying degrees of periodontal disease symptoms, and this proportion increases with age. Because pet food typically contains high levels of protein, especially wet food with its high moisture content, food debris easily remains in the mouth. Furthermore, pets' lack of regular oral cleaning habits leads to excessive bacterial growth, causing oral diseases such as tartar, gingivitis, and periodontitis. These diseases not only cause symptoms like bad breath, drooling, tooth loss, pain, and loss of appetite, severely impacting their quality of life, but can also lead to systemic diseases such as kidney disease, heart disease, and sepsis, threatening the pet's life.

[0003] Currently, pet dental cleaning products on the market are mainly divided into the following categories: liquid (mouthwash, spray), chew toys, and freeze-dried products. While liquid products contain antibacterial ingredients, in the complex environment of the oral cavity, their active ingredients are quickly diluted by saliva and swallowed, failing to maintain an effective concentration and duration at the target site, thus limiting their effectiveness. Chew toys mostly achieve their cleaning effect through physical friction on the tooth surface, limiting their area of ​​action and preventing beneficial effects on the entire oral mucosa (gingiva, tongue, pharynx). Chew toys often use dried cowhide or pigskin, which is too hard; excessive chewing can wear down teeth and cause fatigue of the chewing muscles, and is unsuitable for cats. Although freeze-dried pet dental products have improved in flavor and nutrition in recent years, they generally have a short residence time in the mouth after direct feeding, making it difficult to fully exert their cleaning effect.

[0004] Therefore, in order to meet the urgent needs of pet owners for easy and scientific oral care, developing a delivery system that can prolong the retention time of active ingredients in the oral cavity is a pressing problem that needs to be solved. Summary of the Invention

[0005] To address the aforementioned issues, a fast-dissolving composition for dogs and cats with long-lasting oral health benefits is provided, along with its preparation method and application. This composition utilizes low-molecular-weight, high-deacetylation-degree chitosan gum as a bioadhesive agent, combined with modified tapioca starch. Through an optimized formulation system and high-speed shear homogenization process, combined with a fast-dissolving freeze-dried matrix, the functional components of this composition can rapidly disperse and fully contact all parts of the oral cavity after being dissolved in drinking water or directly in saliva. They adhere to the surfaces of teeth and oral mucosa through intermolecular forces, thus achieving a long-lasting and sustained release of the active ingredients. This composition, through a composite antibacterial system composed of lysozyme, tea polyphenols, and zinc gluconate, synergistically forms a bioadhesive film with chitosan gum, effectively inhibiting oral pathogens, reducing plaque and tartar formation, and providing long-lasting relief from halitosis.

[0006] This application provides a fast-dissolving composition for dogs and cats with long-lasting oral health care function, comprising the following components by weight percentage: The ingredients are: 20-30% whey protein powder, 10-20% hydrolyzed gelatin, 1-3% low molecular weight chitin gum, 1-2% modified tapioca starch, 2-5% sodium alginate, 1-3% fructooligosaccharides, 0.03-0.08% lysozyme, 0.03-0.08% tea polyphenols, 0.05-0.15% zinc gluconate, 0.05-0.1% persimmon tannin, 3-5% tuna hydrolysate, 4-6% whole goat milk powder, 2-4% skim yogurt powder, and the remainder is water. The low molecular weight chitin gum has a molecular weight of 10-50 kDa; the molecular weight of the oligofructose has a molecular weight of 300-1000 Da.

[0007] This application incorporates low molecular weight chitosan glycosyl gum and modified tapioca starch, which are the core functional components of this application. These components are used to improve the retention effect of the active ingredients on teeth and oral mucosa. However, their inherent film-forming and viscosity properties, if not properly handled, can severely hinder water penetration and affect the product's solubility. This application overcomes these adverse effects by: 1) Selecting low molecular weight chitosan glycosyl gum with a small molecular weight and a high degree of deacetylation. The lower molecular weight means lower aqueous solution viscosity and faster dissolution rate; the high degree of deacetylation makes it positively charged in the weakly acidic oral environment, making it easier to generate strong electrostatic adsorption with the negatively charged surfaces of teeth and oral mucosa (the surfaces of teeth and oral mucosa are usually negatively charged, which is formed by the combined action of glycoproteins on the surface of epithelial cells and electrolytes in saliva). This allows for the use of a lower addition amount (1~3%) to achieve excellent adhesion, reducing the potential impact on solubility from the source. 2) When combined with fast-dissolving ingredients such as hydrolyzed gelatin and whey protein powder, these hydrophilic matrices form "moisture channels" that quickly absorb water after freeze-drying, effectively offsetting the local viscosity increase caused by the dissolution of chitosan gum, ensuring that water can quickly penetrate the entire fast-dissolving composition; 3) The processing technology of modified cassava starch is optimized by using hot melt extrusion and gelatinization to ensure film-forming performance while also ensuring good solubility; 4) Before adding modified cassava starch and low molecular weight chitosan gum, a hot melt extrusion pretreatment is performed before adding them to the system to prepare an aqueous phase, which can further improve solubility. This application adds four oral health care ingredients. Lysozyme can lyse bacterial cell walls; tea polyphenols provide broad-spectrum natural antibacterial and antioxidant effects; zinc gluconate inhibits the production of volatile sulfur compounds; and persimmon tannins have astringent and breath-freshening properties. This application adds three bioadhesive and film-forming agents. Low molecular weight chitosan gum and modified tapioca starch adhere to the oral mucosa and tooth enamel through intermolecular forces such as hydrogen bonds, forming a biofilm that acts as a carrier for active ingredients, greatly extending retention time; sodium alginate synergistically forms a film with chitosan gum and modified tapioca starch, enhancing film toughness. This application adds two water-soluble protein matrices. Whey protein powder provides high-quality protein and forms a fast-dissolving framework; hydrolyzed gelatin acts as a binder and fast dissolving agent. The added fructooligosaccharides, as prebiotics, help promote the colonization and proliferation of beneficial oral bacteria. The added natural palatability enhancers, including tuna hydrolysate, goat milk powder, and yogurt powder, provide rich and appealing flavors.

[0008] Optionally, the low molecular weight chitosan gum has a molecular weight of 10-30 kDa and a degree of deacetylation of not less than 90%.

[0009] Optionally, the preparation steps of the modified cassava starch include the following steps: S1. Add water to cassava starch, then add acetic anhydride, and add sodium hydroxide solution to adjust the pH to 7.5~8.5. React at 30~40℃. After the reaction is complete, a mixed raw material is obtained. S2. Add the mixed raw materials and polyvinylpyrrolidone to a hot melt extruder for hot melt extrusion to obtain the extrudate; S3. Add the extrudate to water and stir to gelatinize in a boiling water bath; S4. After cooling, the modified cassava starch gelatinized product is obtained, which is the modified cassava starch.

[0010] In this application, cassava starch is modified using acetic anhydride to introduce acetic acid groups and improve solubility. The esterified cassava starch is mixed with polyvinylpyrrolidone (PVP) and fed into a hot-melt extruder. The addition of PVP facilitates the smooth hot-melt extrusion of the cassava starch. It should be noted that the modified cassava starch is not completely melted during hot-melt extrusion, unlike in traditional thermoplastic processing. Hot-melt extrusion further improves the solubility of cassava starch while retaining its adhesiveness. However, the solubility of the modified cassava starch after hot-melt extrusion still needs improvement. To achieve the rapid dissolution effect required in this application, a gelatinization process is subsequently performed, significantly improving its solubility.

[0011] Optionally, in step S2, the melt extrusion temperature is 90~96℃ and the screw speed is 50~60rpm; and / or, In step S3, the mixture is stirred and gelatinized for 30-60 minutes.

[0012] Optionally, the cassava starch has an average particle size of 14-20 μm and a specific surface area of ​​500-650 m². 2 / kg; Optionally, the cassava starch has an average particle size of 18-20 μm and a specific surface area of ​​500-550 m². 2 / kg.

[0013] Optionally, the amylose content of the potato starch is 22-35%; Optionally, the cassava starch has an amylose content of 24-28%.

[0014] Optionally, the weight ratio of the cassava starch to the acetic anhydride is (200~300):1.

[0015] Optionally, in step S2, the weight ratio of the mixed raw materials to polyvinylpyrrolidone is 25~50:1.

[0016] This application provides a method for preparing the above-mentioned fast-dissolving composition for dogs and cats with long-lasting oral health care function, the preparation method comprising the following steps: 1) Heat purified water to 50±2℃, and add whey protein powder, hydrolyzed gelatin, sodium alginate, and fructooligosaccharides while stirring; 2) Add low molecular weight chitin gum and modified tapioca starch; 3) Add tuna hydrolysate, whole goat milk powder, and nonfat yogurt powder flavoring; 4) The obtained liquid was homogenized in a high-speed shear homogenizer at a speed of 12000±1000 rpm for 3~9 min, and degassed under a vacuum of -0.085±0.005MPa for 15±5 min. 5) Add citric acid to the obtained solution to adjust the pH value of the solution to 5.8±0.1; 6) Cool to below 35℃, add lysozyme, tea polyphenols, zinc gluconate and persimmon tannin to the resulting liquid, stir well and let stand for aging for 20~50 minutes; 7) Freeze at -75±5℃ and keep warm for 4±1 hours; 8) Place the frozen material in the freeze-drying chamber, freeze-dry it, and then remove it from the freeze-drying chamber to obtain the final product.

[0017] High-speed shear homogenization is a crucial process step for achieving a balance between rapid dissolution and adhesion performance. The feed solution is subjected to high-speed shear homogenization at a speed of 10,000~12,000 rpm for 5~6 minutes. The huge shear force in this step can effectively break down the molecular chains of chitin glycosides and modified tapioca starch, and make them uniformly dispersed at the molecular level with matrix molecules such as whey protein and hydrolyzed gelatin. This prevents them from entangled with each other and forming a sticky network structure that hinders water penetration. This ensures that in the final freeze-dried product, chitin glycosides can be evenly distributed in a permeable porous framework, rather than forming a local gel barrier.

[0018] Optionally, step 8) freeze-drying includes: starting the vacuum pump to reduce the pressure inside the chamber to below 8 Pa, controlling the temperature of the partition to 5±1℃ and maintaining it for 30±2h, raising it from 5±1℃ to 20±2℃ and maintaining it for 2±0.5h for 2±0.5h, and then raising it to 30±2℃ and maintaining it for 5±1h to complete the freeze-drying.

[0019] Optionally, in step 2), the low molecular weight chitin gum and modified cassava starch are mixed and then melt-extruded before being added: the melt extrusion temperature is 100~105℃ and the screw speed is 70~80rpm.

[0020] This application optimizes and adjusts the formulation and process, and the provided composition has the effect of rapid dissolution followed by adhesion. After the composition is rapidly dissolved in water or taken orally, it disintegrates rapidly within 3 to 5 seconds due to its highly open porous structure. The low molecular weight chitin glycosyl gum, modified tapioca starch and other active ingredients released in the oral cavity then immediately adhere to the surface of teeth and gums through intermolecular forces.

[0021] The beneficial effects of this application include, but are not limited to: 1. The instant oral health care composition for dogs and cats with long-lasting oral health care function, its preparation method and application, according to this application, the active ingredients added in this application have a long-lasting and sustained-release effect in the formula, which can effectively inhibit oral pathogens, reduce the formation of dental plaque and tartar, and provide long-lasting relief from halitosis, and have good market competitiveness.

[0022] 2. According to the canine and cat fast-dissolving composition with long-lasting oral health function of this application, its preparation method and application, low molecular weight, high degree of deacetylation chitin glycosyl gum is selected as a bioadhesive agent in combination with modified tapioca starch. Through an optimized formulation system and high-speed shear homogenization process, combined with a fast-dissolving freeze-dried matrix, the functional components of the composition can quickly disperse and fully contact all parts of the oral cavity after being dissolved in drinking water or directly orally in saliva. They adhere to the surface of teeth and oral mucosa through intermolecular forces, thereby achieving long-lasting sustained release and continuous effect of active ingredients. The composition, through a composite antibacterial system composed of lysozyme, tea polyphenols, zinc gluconate, etc., and the bioadhesive film formed by chitin glycosyl gum, can effectively inhibit oral pathogens, reduce the formation of dental plaque and tartar, and provide long-lasting relief from halitosis.

[0023] 3. The canine and cat instant-dissolving composition with long-lasting oral care function, its preparation method, and its application, according to this application, through molecular weight control, precise dosage, and compounding with an instant-dissolving matrix, combined with high-speed shear homogenization, freeze-drying, and pretreatment processes, ensures that low molecular weight chitin gum and modified tapioca starch can exert a long-lasting adhesive effect without hindering the instantaneous disintegration characteristics of the product. Thus, the instant-dissolving characteristics of freeze-dried food can be combined with the long-lasting sustained-release requirements of oral care, giving it good market competitiveness. Detailed Implementation

[0024] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments. Unless otherwise specified, the raw materials and reagents in the embodiments of the present application are all purchased through commercial channels.

[0025] Example 1: Instantly Dissolving Freeze-Dried Granules for Canine and Feline Oral Health Care This embodiment provides a fast-dissolving freeze-dried granule for canine and feline oral health care, comprising the following components by mass percentage: 24.0% whey protein powder, 14.0% hydrolyzed gelatin, 2.5% low molecular weight chitosan gum, 1% modified tapioca starch, 2.0% sodium alginate, 0.05% lysozyme, 0.05% tea polyphenols, 0.1% zinc gluconate, 0.08% persimmon tannin, 2.0% fructooligosaccharides, 4.0% tuna hydrolysate, 4.0% whole goat milk powder, 3.0% skim yogurt powder, and purified water to make up the balance. The low molecular weight chitosan gum has a molecular weight distribution in the range of 10-30 kDa and a degree of deacetylation of 92%, while the fructooligosaccharides have a molecular weight distribution in the range of 300-1000 Da. The preparation method of this instant lyophilized oral health care granules for dogs and cats includes the following steps: 1) Weighing and Preparation: Accurately weigh each raw material and auxiliary material according to the formula ratio; the preparation steps of modified cassava starch include the following steps: S1, add a small amount of water to cassava starch and stir until it becomes a paste, then add acetic anhydride and heat to 30~40℃ and keep stirring continuously to carry out the reaction. Sodium hydroxide solution is also added to the reaction system to maintain a weakly alkaline reaction condition of pH 7.5~8.5. After the reaction is completed, a mixed raw material is obtained. The weight ratio of cassava starch to acetic anhydride is 250:1. The average particle size of cassava starch is 16μm and the specific surface area is 610m². 2 / kg, the amylose content of cassava starch is 26%; S2, add polyvinylpyrrolidone (K17) to the obtained mixed raw materials and mix, then put it into a hot melt extruder for hot melt extrusion. The melt extrusion temperature is 94℃ and the screw speed is 55rpm to obtain the extrudate. The weight ratio of the mixed raw materials to polyvinylpyrrolidone is 30:1; S3, add the extrudate to water and stir and gelatinize in a boiling water bath for 45min; S4, after cooling, the modified cassava starch gelatinize is obtained, which is the modified cassava starch.

[0026] 2) Aqueous phase preparation: Add approximately 70% of the total formula volume of purified water to the mixing tank, start stirring (200 rpm) and heat to 50±2℃; while stirring, slowly add whey protein powder, hydrolyzed gelatin, sodium alginate and fructooligosaccharides in sequence, ensuring that the previous one is completely dissolved before adding the next to avoid clumping; after the modified cassava starch and low molecular weight chitosan gum adhesive are mixed evenly, they are pretreated and sent to a hot melt extruder for hot melt extrusion to obtain the mixed extrudate of modified cassava starch and low molecular weight chitosan gum adhesive at a temperature of 102℃ and a screw speed of 75 rpm. Then continue to add the pretreated mixed extrudate of modified cassava starch and low molecular weight chitosan gum adhesive, maintaining the temperature and stirring during the addition process, stirring until the solution is slightly turbid and viscous; continue to add tuna hydrolysate, whole milk powder, and non-fat yogurt powder flavoring, and stir evenly.

[0027] 3) Homogenization and degassing: Transfer the obtained liquid to a high-speed shear homogenizer and homogenize at 12,000 rpm for 6 minutes to crush colloidal particles and ensure uniform particle size and fine texture of the liquid. Pump the homogenized liquid into a vacuum degassing tank and degas at a vacuum of -0.085 MPa for 15 minutes to remove air bubbles introduced during homogenization and prevent uneven product structure or voids after freeze-drying.

[0028] 4) pH adjustment and addition of heat-sensitive components: Slowly add 10% citric acid solution to the degassed liquid while stirring, and precisely adjust the pH value of the liquid to 5.8±0.1. This weakly acidic environment is more conducive to the stability and adhesion performance of low molecular weight chitin gum. Then, let the liquid temperature cool naturally to below 35℃, and then add heat-sensitive functional factors such as lysozyme, tea polyphenols, zinc gluconate, and persimmon tannins while stirring at low speed. After stirring evenly, let it stand and age for 30 minutes.

[0029] 5) Filling and pre-freezing: Using a quantitative filling machine, the aged liquid material is accurately injected into specific strip or granular molds, with a filling amount of about 1.0±0.1g per hole; the filled molds are quickly transferred to an ultra-low temperature freezer at -75℃ for rapid freezing and heat preservation for 4 hours to ensure that the material is completely frozen and the ice crystals are small and uniform.

[0030] 6) Vacuum freeze-drying: Push the pre-frozen material cart into the freeze-drying chamber and execute the freeze-drying according to the following set curve: Start the vacuum pump and reduce the pressure inside the chamber to below 8 Pa within 30 minutes; Sublimation drying stage: Control the partition temperature at 5°C and maintain it for 30 hours. During this stage, about 90% of the free water in the material will be removed through sublimation. By observing the pressure and material temperature curves inside the chamber, ensure that the material temperature is always below its eutectic point; Desorption drying stage: Gradually and slowly increase the partition temperature from 5°C to 20°C over 2 hours, maintain it for 2 hours, then increase it to 30°C over another 2 hours and maintain it at this temperature for 5 hours. During this stage, the bound water that is more tightly bound to the material can be removed through desorption; After drying, first purge with dry and sterile nitrogen to atmospheric pressure, and then discharge the material.

[0031] 7) Dehumidification and Packaging: After discharge, the freeze-dried granules are immediately transferred to a dehumidified and drying packaging room with an ambient temperature of ≤22℃ and a relative humidity of ≤15%. The products are subjected to online visual inspection, and irregularly shaped products are rejected. The products are then packaged in nitrogen-filled aluminum foil bags or light-proof bottles with desiccants inside to prevent moisture absorption and ensure the stability of the components.

[0032] Example 2 The method is basically the same as in Example 1, except that instead of mixing the modified cassava starch and low molecular weight chitosan gum evenly before melting and extruding them in a hot melt extruder, the low molecular weight chitosan gum and modified cassava starch are added directly.

[0033] Example 3 It is basically the same as Example 1, except that the homogenization step in the high-speed shear homogenizer is not included.

[0034] Example 4 It is basically the same as Example 1, except that citric acid is added to adjust the pH of the solution to 6.2.

[0035] Example 5 It is basically the same as Example 1, except that citric acid is added to adjust the pH of the solution to 5.5.

[0036] Comparative Example 1 It is basically the same as Example 1, except that it does not contain low molecular weight chitin gum.

[0037] Comparative Example 2 It is basically the same as Example 1, except that it does not contain modified cassava starch.

[0038] Comparative Example 3 It is basically the same as Example 1, except that the molecular weight distribution of chitin gum is in the range of 50~80kDa, and the molecular weight distribution of fructose is in the range of 1000~2000Da.

[0039] Example 6: Instant Lyophilized Powder for Canine and Feline Oral Health Care This embodiment provides a canine and feline oral health care instant freeze-dried powder product, which is basically the same as that in embodiment 1, except that in step 7): the porous solid plate after freeze-drying is taken out and immediately coarsely crushed with a jaw crusher in a dry environment with humidity ≤15%; then the coarsely crushed material is transferred to a high-efficiency pulverizer for grinding, and then sieved through an 80-mesh sieve to obtain a fine and uniform powder; finally, it is packaged in an aluminum foil bag or light-proof bottle filled with nitrogen and desiccant is placed inside to prevent moisture absorption and ensure the stability of the ingredients.

[0040] Example 7: Instantly Dissolving Lyophilized Tablets for Canine and Feline Oral Health Care This embodiment provides a tablet product with a regular shape, convenient for quantitative feeding and commercial packaging. While retaining the adhesive active ingredient library of this application, this tablet solves the problems of molding difficulties and insufficient hardness that easily occur when directly compressing lyophilized powders through scientific excipient ratios and preparation processes. This ensures that the tablet has suitable hardness while still rapidly disintegrating upon contact with water or saliva, releasing functional ingredients.

[0041] The canine and feline oral health care instant lyophilized tablets provided in this embodiment include the following components by mass percentage: 90.0% lyophilized powder base (i.e., the product prepared in Example 2), 5.0% sodium carboxymethyl starch, 2.5% croscarmellose sodium, 1.5% povidone (K30), and 1.0% polyethylene glycol 4000.

[0042] The preparation method of this instant lyophilized oral health tablet for dogs and cats includes the following steps: 1) Raw material preparation and mixing: Accurately weigh the freeze-dried powder base, sodium carboxymethyl starch, and sodium cross-linked carboxymethyl cellulose prepared in Example 2, and place them in a three-dimensional motion mixer; mix at 25 rpm for 20 minutes to ensure that each component is fully and evenly mixed.

[0043] 2) Wet granulation: Prepare the binder solution by dissolving povidone (K30) in an appropriate amount of 70% (v / v) ethanol aqueous solution to prepare a 10% (w / v) clear solution; under low-speed stirring, slowly add the povidone solution to the mixed powder by spraying; the ethanol aqueous solution acts as a wetting agent, which can dissolve povidone to form a binder solution, and its volatility facilitates subsequent drying; based on the experience that the material can be formed into a ball by hand and dispersed by light pressure, control the amount of binder solution added to make a suitable soft material.

[0044] 3) Drying and granulation: Quickly transfer the wet granules to a hot air circulating oven and dry them at 45~50℃ for about 60 minutes to control the moisture content of the granules between 3~5%; granulate the dried granules through a 20-mesh sieve to break up the clumps formed during the drying process and obtain uniform granules with good flowability.

[0045] 4) Overall mixing and lubrication: Transfer the granulated dry granules back into the mixer; add the prescribed amount of polyethylene glycol 4000, and mix at 15 rpm for 5 minutes to ensure that the lubricant is evenly distributed on the surface of the granules.

[0046] 5) Tableting: Feed the final mixed granules into a rotary tablet press; select a suitable mold (such as a shallow circular die with a diameter of 10mm), and adjust the filling depth and tableting pressure of the tablet press; control the tablet weight to 0.5g / tablet, and control the hardness between 20~30N; this hardness range can ensure that the tablets are not easily damaged during packaging and transportation, and will not excessively affect the disintegration rate.

[0047] 6) Packaging: The compressed tablets should be immediately packaged in blister packs or bottles in an environment with a temperature of ≤25℃ and a relative humidity of ≤30%. The packaging materials should have high moisture resistance, be nitrogen-filled for protection, and contain desiccants to prevent moisture absorption and ensure the stability of the ingredients.

[0048] Test Example 1 The researchers tested the products obtained in Examples 1-5 and Comparative Examples 1-3 and found that the in vitro disintegration time of Example 2 was about 2.1 times that of Example 1, indicating that the solubility of Example 2 was slightly worse. The in vitro disintegration time of Example 3 was about 1.3 times that of Example 1. In particular, the residual rate of tea polyphenols on the tooth surface decreased significantly, indicating that the retention effect of the active ingredients on the teeth was worse.

[0049] Compared to Example 1, Examples 4 and 5 showed a significant decrease in the residual rate of tea polyphenols on the tooth surface, indicating a similarly poorer retention effect of the active ingredients on teeth. Through exploratory experiments, researchers discovered that a pH environment of 5.8 ± 0.1 is the most favorable condition for the stability and adhesion properties of low molecular weight chitosan gum, and also provides the best conditions for the synergistic film formation of low molecular weight chitosan gum, modified cassava starch, and sodium alginate. Among the prepared products, tea polyphenols showed the best retention effect on teeth.

[0050] Compared to Example 1, Comparative Examples 1 and 2 showed a significant decrease in the residue rate of tea polyphenols on the tooth surface, and the retention effect of the active ingredients on the teeth was also worse. The synergistic effect of the addition of low molecular weight chitosan gum and modified tapioca starch with sodium alginate had been verified by researchers through experiments in the early stages of product design. The in vitro disintegration time of the product obtained in Comparative Example 3 was approximately 5.4 times that of Example 1, indicating a significant decrease in solubility.

[0051] Experimental Example 1 Researchers found that the preparation process and raw material selection of modified cassava starch significantly affect its retention effect on tooth surfaces, particularly the retention of active ingredients such as tea polyphenols. Extensive experiments and explorations were conducted on modified cassava starch, and the experimental procedures and results are as follows. The experimental samples were essentially the same as in Example 1, with the main difference being the preparation of the modified cassava starch. Specific differences are detailed in Table 1 below.

[0052] Table 1. Differences in the preparation of modified cassava starch in various experimental samples.

[0053] An in vitro saliva flushing model was used to simulate and quantitatively verify the adhesion performance of the products and compare the differences in the retention time of active ingredients. The experimental procedure included: preparing solutions of the two products with the same concentration (10% w / v) using deionized water. 100 μL of the solution was evenly added to the center of a pretreated fresh hog tooth enamel slide (simulating the tooth surface) and allowed to stand for 1 minute at 37°C and 95% relative humidity to allow initial adhesion of the active ingredients. The slide was then fixed in a self-made flow cell, and a constant flow pump was used to continuously flush the surface of the slide with phosphate-buffered saline (PBS, pH 6.8) at a flow rate of 0.5 mL / min (simulating the basal secretion rate of saliva). The eluted liquid was collected at 0, 1, 3, 5, 10, 15, and 30 minutes after the start of flushing. The characteristic absorbance of tea polyphenols in the collected liquid at a wavelength of 273 nm was measured using a UV-Vis spectrophotometer. The concentration was calculated using a standard curve and used to represent the elution amount of the active ingredient. The amount of active ingredient on the surface of the dental radiograph at 0 minutes is taken as the initial total amount of 100%. The formula for calculating the residual rate (%) of active ingredient at each time point is: [1 - (cumulative amount eluted at the current time point / initial total amount)] × 100%.

[0054] The results of the tooth retention effect of each test sample are shown in Table 2 below.

[0055] Table 2. Residual rate of tea polyphenols on tooth surface (%)

[0056] Table 2 (Continued)

[0057] As shown in Table 2, the active ingredients in the product of this application have a high residual rate during elution, exhibiting good adhesion properties and long-lasting retention capacity, which is more conducive to achieving the oral health effect of continuously inhibiting dental plaque and providing long-lasting fresh breath.

[0058] Experimental Example 2: The Effect of Freeze-drying Process on Product Texture Researchers discovered that key process parameters in the vacuum freeze-drying process, especially the temperature during the desorption drying stage, have a significant impact on the physical structure, textural properties, and rapid solubility of the final product. Through extensive exploration and experimentation, the optimal production process conditions have been determined. Using the same batch of mixed solution according to the formulation in Example 1, the samples were processed under the same pre-freezing conditions (-75°C, 4 hours) and sublimation drying conditions (5°C, 30 hours). Subsequently, three different temperature gradients were set during the desorption drying stage to prepare the following three batches of samples.

[0059] Sample A: Same as Example 1.

[0060] Sample B: Same as Sample A, except that the vacuum pump was started to reduce the pressure inside the chamber to below 8 Pa within 30 minutes; during the sublimation drying stage, the temperature of the partition was controlled at 5°C and maintained for 30 hours; during the desorption drying stage, the temperature of the partition was gradually and slowly increased from 5°C to 30°C over 2 hours, maintained for 2 hours, and then increased to 40°C over another 2 hours, and maintained at this temperature for 5 hours.

[0061] Sample C: Same as Sample A, except that the vacuum pump was started to reduce the pressure inside the chamber to below 8 Pa within 30 minutes; during the sublimation drying stage, the temperature of the partition was controlled at 5°C and maintained for 30 hours; during the desorption drying stage, the temperature of the partition was gradually and slowly increased from 5°C to 40°C over 2 hours, maintained for 2 hours, and then increased to 50°C over another 2 hours, and maintained at this temperature for 5 hours.

[0062] Hardness: A puncture test was performed using a texture analyzer, and the maximum force (g) required for the probe to puncture the sample was recorded to assess the product's firmness.

[0063] Friability: Accurately weigh 10g of sample (W1) and place it in a friability tester, rotating it 100 times at 25 rpm (approximately 10 minutes). After removal, sieve it through a 1.0mm sieve and weigh the sample that does not pass through the sieve (W2). Friability (%) = [(W1-W2) / W1] ×100%, used to simulate the abrasion and breakage resistance during transportation. A friability of <5% for freeze-dried products is generally considered good.

[0064] In vitro disintegration time: The sample was placed in a petri dish containing 37°C deionized water, with the water level just covering the sample. A stopwatch was used to record the time from contact with water until the sample structure completely disintegrated and no visible core remained, which was used to measure the product's rapid dissolution performance.

[0065] The results are shown in Table 3 below.

[0066] Table 3. Test results of the effect of freeze-drying process on product texture

[0067] As shown in Table 3, the proposed solution achieves the best balance between hardness, friability, and disintegration time. The resulting product has a short disintegration time, rapid solubility, moderate hardness, loose texture, and controllable friability, which can meet the needs of commercial packaging and transportation.

[0068] Test Example 2: Oral Health Care and Antibacterial Effect Test The effects of the product of this application (experimental group) and ordinary treats (control group) on improving oral health in dogs and cats after 28 days of continuous feeding were further evaluated. Twenty healthy adult domestic cats with mild plaque and halitosis were randomly divided into an experimental group (fed the product of this application, Example 1 granules) and a control group (fed ordinary freeze-dried treats with similar appearance), with 10 cats in each group. Experimental period: 28 days. Feeding method: 2g once daily. No oral cleaning was performed before or after feeding.

[0069] Dental plaque index: Plaque display solution staining method. Use pet-specific plaque display solution (erythrosine) to spray evenly on the tooth surface. After rinsing gently with water, score the stained area of ​​the designated teeth (canines, fourth premolars) using the Loblige index score of 0-5, where 0 = no plaque and 5 = plaque coverage > 2 / 3 of the crown.

[0070] Tartar Index: Visual and tactile probing method. Under standard illumination, a dental probe is used to explore the thickness and coverage of tartar at the gingival margin of a specified tooth. The RC index is scored from 0 to 3, where 0 = no tartar and 3 = tartar coverage > 2 / 3 of the tooth surface or in a thick band.

[0071] Halitosis severity: Sensory evaluation and instrumental analysis were conducted simultaneously. In the sensory evaluation, three trained evaluators smelled the pet's breath from a distance of 10cm and scored it on a scale of 0-5, where 0 = no odor and 5 = severe malodor. The average score was taken. In the instrumental analysis, a volatile sulfur oxide (VSC) monitor was used to detect the concentration (ppb) of gases such as hydrogen sulfide in the oral cavity. The instrument readings were recorded directly in ppb values.

[0072] Total oral bacteria count: Microbial plate count method. A sample was evenly scraped from the gingival sulcus and dorsum of the tongue of the pet using a sterile cotton swab, placed in sterile physiological saline, serially diluted, and then spread on brain heart infusion agar medium. After incubation at 37°C for 48 hours, the count was performed. The results are expressed as CFU / mL (colony forming units per milliliter).

[0073] The results are shown in Table 4 below.

[0074] Table 4. Test results of oral health care effects and antibacterial effects

[0075] As shown in Table 4, all indicators in the experimental group showed a highly significant decrease compared to the baseline level after 28 days, while the control group showed no significant changes. This indicates that the product of this application can effectively and comprehensively improve the oral health of pets in daily use.

[0076] Test Example 3: Accelerated Stability Test Accelerated testing conditions were used to assess changes in key quality attributes of the product during storage, predict its shelf life, and verify the suitability of the packaging system. Three consecutive batches of finished products (lot numbers: S251001, S251002, S251003) produced in Example 1 were packaged in nitrogen-filled aluminum foil bags. Accelerated conditions: Samples were placed in a constant temperature and humidity chamber at 40℃±2℃ and 75%±5% relative humidity, according to ICH Q1A (R2) guidelines. Testing time points: Samples were taken and tested at the end of 0, 1, 2, 3, and 6 months.

[0077] Lysozyme activity: The micrococcal turbidimetric method was used with micrococci as substrates. The rate of decrease in absorbance of the sample solution at a wavelength of 450 nm was measured by spectrophotometer, and the activity retention rate was calculated by comparison with the standard.

[0078] Tea polyphenol content: The Folin-Ciocalteu colorimetric method was used to determine the content of tea polyphenols by reacting with Folin-Ciocalteu reagent under alkaline conditions to form a blue complex. The absorbance was measured at a wavelength of 765 nm, and the content was quantified by standard curve.

[0079] Peroxide value: The content of peroxides in the sample was determined by the international standard iodometric method (GB 5009.227), and expressed as millimoles of active oxygen per kilogram of oil (mmol / kg).

[0080] The results are shown in Table 5 below.

[0081] Table 5 Accelerated stability test results

[0082] As shown in Table 5, at the end of the 6-month accelerated test, the retention rates of lysozyme activity and tea polyphenol content were both higher than 95%; the peroxide value remained at an extremely low level throughout the test (3.5 mmol / kg at the end of 6 months), significantly lower than the industry-common limit (10.0 mmol / kg); the product disintegration time increased only slightly after 6 months, but remained below 5 seconds; based on the accelerated test data, it is estimated that the product of this application can easily achieve a shelf life of more than 24 months at room temperature (25℃).

[0083] The above description is merely an embodiment of this application, and the scope of protection of this application is not limited to these specific embodiments, but is determined by the claims of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the technical concept and principles of this application should be included within the scope of protection of this application.

Claims

1. A rapidly dissolving composition for dogs and cats having a long-acting oral care function, characterized by comprising: The following components are included by weight percentage: 20~30% whey protein powder, 10~20% hydrolyzed gelatin, 1~3% low molecular weight chitosan gum, 1~2% modified tapioca starch, 2~5% sodium alginate, 1~3% oligofructose, 0.03~0.08% lysozyme, 0.03~0.08% tea polyphenol, 0.05~0.15% zinc gluconate, 0.05~0.1% persimmon tannin, 3~5% tuna hydrolysate, 4~6% whole sheep milk powder, 2~4% skimmed yogurt powder, and the balance is water; The low molecular weight chitosan gum has a molecular weight of 10~50kDa; and the oligofructose has a molecular weight of 300~1000Da.

2. The instant composition for dogs and cats having a long-acting oral care function according to claim 1, characterized by, The low molecular weight chitosan gum has a molecular weight of 10~30kDa and a degree of deacetylation of not less than 90%.

3. The instant composition for dogs and cats having a long-acting oral health care function according to claim 1, characterized by, The preparation steps of the modified tapioca starch include the following steps: S1, after adding water to the tapioca starch, add acetic anhydride, add sodium hydroxide solution to adjust the pH to 7.5~8.5, and react at 30~40℃, then obtain the mixed raw material after the reaction is completed; S2, melt-extrude the mixed raw material and polyvinylpyrrolidone in a hot melt extruder to obtain an extrudate; S3, add the extrudate into water and stir in a boiling water bath to gelatinize; S4, after cooling, obtain the modified tapioca starch gelatinized product, which is the modified tapioca starch.

4. The instant composition for dogs and cats having a long-acting oral health function according to claim 3, characterized by, The melt-extrusion temperature in step S2 is 90~96℃, and the screw rotation speed is 50~60rpm; and / or, The stirring gelatinization in step S3 is 30~60min.

5. The instant composition for dogs and cats having a long-acting oral health care function according to claim 3, characterized by, The average particle size of the cassava starch is 14-20 μm, the specific surface area is 500-650 m 2 / kg; Optionally, the average particle size of the cassava starch is 18-20 μm, and the specific surface area is 500-550 m 2 / kg.

6. The instant composition for dogs and cats having a long-acting oral healthcare function according to claim 3, characterized by, The amylose content of the tapioca starch is 22~35%; Optionally, the amylose content of the tapioca starch is 24~28%.

7. The rapidly dissolving composition for dogs and cats having a long-acting oral care function according to claim 3, characterized by, The weight ratio of the tapioca starch to the acetic anhydride is (200~300):

1.

8. The process for preparing the instant composition for dogs and cats having a long-acting oral health care function according to any one of claims 1 to 7, wherein The preparation method includes the following steps: 1) heat the purified water to 50±2℃, and add whey protein powder, hydrolyzed gelatin, sodium alginate, and oligofructose under stirring; 2) add low molecular weight chitosan gum and modified tapioca starch; 3) add tuna hydrolysate, whole sheep milk powder, and skimmed yogurt powder flavoring agent; 4) homogenize the obtained liquid in a high-speed shearing homogenizer at a rotation speed of 12000±1000rpm for 3~9min, and defoam at a vacuum degree of -0.085±0.005MPa for 15±5min; 5) add citric acid to the obtained liquid to adjust the pH of the liquid to 5.8±0.1; 6) cool to below 35℃, and add lysozyme, tea polyphenol, zinc gluconate, and persimmon tannin to the obtained liquid, stir uniformly, and then stand for aging for 20~50min; 7) freeze at -75±5℃, and keep for 4±1h; 8) place the frozen material in a freeze-drying chamber, and freeze-dry, then take out from the freeze-drying chamber to obtain the product.

9. The method of producing a rapidly dissolving composition for dogs and cats having a long-acting oral care function according to claim 8, characterized by, The freeze-drying step in step 8) includes: start the vacuum pump to reduce the pressure in the chamber to below 8Pa, control the baffle temperature to 5±1℃ for 30±2h, increase from 5±1℃ to 20±2℃ over 2±0.5h and keep for 2±0.5h, then increase from 20±2℃ to 30±2℃ over 2±0.5h and keep for 5±1h to complete the freeze-drying.

10. The method of producing a rapidly dissolving composition for dogs and cats having a long-acting oral care function according to claim 9, characterized by, The low molecular weight chitin sugar gum and modified cassava starch in the step 2) are mixed and then subjected to a melt extrusion treatment before being added, with the temperature of melt extrusion being 100-105 ℃ and the screw rotation speed being 70-80 rpm.

Images