Efficient antibacterial pet oral cleaning water and preparation method thereof

Abstract

The invention relates to the technical field of pet oral cavity cleaning water, in particular to efficient antibacterial pet oral cavity cleaning water and a preparation method thereof, the pet oral cavity cleaning water comprises an extract, an inactive component, a synergist, an auxiliary agent and water; the extracts comprise a green tea extract, a herba violae extract, a pomegranate extract, a vanilla extract, erythritol and fructo-oligosaccharide; the inactive components comprise glycerol, citric acid and food-grade sodium bicarbonate; the auxiliaries comprise a flavoring agent, a thickening agent and a clarifying agent. The pet oral cavity cleaning water designed by the invention has the effects of inhibiting bacteria, preventing decayed teeth, preventing dental plaque formation, preventing gingivitis and gingivitis, removing ozostomia and coordinating intestines and stomach, and also has the advantages of no artificial perfume, pigment, filler or preservative and reduction of risks caused by pet swallowing.

Description

Technical Field

[0001] The invention relates to the technical field of pet oral cleaning water, in particular to a highly efficient antibacterial pet oral cleaning water and a preparation method thereof. Background Art

[0002] The pet oral cleaning water currently on the market has the following problems: (1) The addition of chemical antibacterial agents, although the antibacterial effect is obvious, there are safety issues in long-term use, and it is easy to produce resistance and drug resistance. For example, cetylpyridinium chloride (CPC). If oral care products containing CPC are used frequently, the teeth will have a slight brown stain, the gums will also have a slight burning sensation, and it may also promote the formation of dental calculus. According to the Hazardous Substances Database (HSDB) of the National Center for Biotechnology Information, CPC is orally toxic to rats, mice and rabbits, can cause severe eye irritation, and is also irritating to the skin. Zinc chloride itself is corrosive and highly toxic, and can severely irritate and burn the skin and mucous membranes. (2) Most pet oral cleaning products on the market use the same formula as human toothpaste and mouthwash, such as calcium carbonate and calcium phosphate abrasives, which can easily form stones after swallowing and are harmful to the pet's body. Commonly used xylitol and sorbitol moisturizers can easily cause intestinal discomfort in pets. Xylitol can trigger a large amount of insulin release, which will then reduce blood sugar, causing the pet to become weak and drowsy, and even go into coma and acute liver necrosis. The preservative sodium benzoate, although sodium benzoate itself has low acute toxicity, cats are sensitive to benzoic acid and are prone to symptoms such as excitement, nervousness, loss of hearing and balance.

[0003] For example, the invention patent with the announcement number CN112294872A discloses a pharmaceutical composition that helps to clean the oral cavity of a pet and a preparation method. The pharmaceutical composition that helps to clean the oral cavity of a pet, measured by its working concentration, includes an M component, an R component, a clarifier and water per 100L of the pharmaceutical composition, wherein the M component includes the following components by weight: 1kg to 2kg of honeysuckle, 1kg to 2kg of forsythia, 0.5kg to 1kg of mint and 0.5kg to 1kg of wild chrysanthemum; the R component includes the following components by weight: 0.8kg to 1.2kg of borax, a flavoring agent and a thickener; the pharmaceutical composition that helps to clean the oral cavity of a pet can have a good antibacterial and cleaning effect on the oral cavity of a pet, and can also assist in the treatment of oral diseases of a pet, but due to the limited residence time in the oral cavity, the efficacy of the drug cannot be fully exerted, thereby affecting the cleaning effect of the oral cavity. Summary of the invention

[0004] In view of the problems existing in the prior art, the object of the present invention is to provide a highly efficient antibacterial pet oral cleaning water and a preparation method thereof.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A highly effective antibacterial pet oral cleaning water, comprising an extract, an inactive ingredient, a synergist, an adjuvant and water;

[0007] The extract comprises green tea extract, Viola yedoensis extract, pomegranate extract, vanilla extract, erythritol, and oligofructose;

[0008] The inactive ingredients include glycerin, citric acid, and food-grade sodium bicarbonate;

[0009] The auxiliary agents include flavoring agents, thickeners and clarifying agents.

[0010] As a further preferred embodiment of the present invention, the flavoring agent is at least one of glycerol, mannitol and saccharin sodium;

[0011] The thickener is at least one of sodium alginate, sodium carboxymethyl cellulose and sodium carboxymethyl starch;

[0012] The clarifier is ZTC1+1-III clarifier.

[0013] As a further preferred embodiment of the present invention, in the pet oral cleaning water, the mass ratio of the extract, the inactive ingredient, the synergist, the adjuvant and the water is (50-70): (10-20): (3-8): (5-10): (500-800);

[0014] The weight proportions of the components in the extract are: 0.1-0.5 parts of green tea extract, 0.5-1 parts of Viola yedoensis extract, 1-2 parts of pomegranate extract, 0.1-0.5 parts of vanilla extract, 1-3 parts of erythritol, and 1-3 parts of oligofructose;

[0015] The weight parts of the inactive ingredients are: 1 to 3 parts of glycerin, 0.5 to 1.2 parts of citric acid, and 0.2 to 0.6 parts of food-grade sodium bicarbonate;

[0016] The weight proportions of the components in the auxiliary agent are: 1 to 2 parts of flavor corrector, 1 to 2 parts of thickener, and 1 to 2 parts of clarifier.

[0017] As a further preferred embodiment of the present invention, the preparation method of the synergist is as follows:

[0018] 1) Weigh maleic anhydride, mix it with chitosan, seal it in a container, place it in a thermostat at 120-125° C. for reaction for 3-5 hours, after the reaction is completed, wash the product with anhydrous ethanol to remove the color, continue to wash with pure water until the pH value is 7, then drip sodium hydroxide solution into the system until the pH value is 11.0-11.5, wash it by centrifugation until the pH value is 7.5-7.8, and dilute it with pure water to a concentration of 1-2wt% to obtain an acylated chitosan dispersion;

[0019] 2) The acylated chitosan dispersion is placed in a container, and treated with a 22-25KHz ultrasonic generator at a power of 500-600W and a 1s on / 1s off pulse for 30-50min to obtain a chitosan nanofiber dispersion. A porous carrier is then added to the chitosan nanofiber dispersion at a solid-liquid ratio of 1g: (10-20)mL, and ultrasonically dispersed for 1-2h, and then mechanically stirred for 1-2h. After the treatment is completed, the dispersion is centrifuged, repeatedly washed with deionized water, and dried to obtain a synergist.

[0020] As a further preferred embodiment of the present invention, in step 1), the mass of the maleic anhydride is 12-20% of the mass of the chitin;

[0021] The concentration of the sodium hydroxide solution is 1.0-1.5 mol / L.

[0022] As a further preferred embodiment of the present invention, in step 2), the power of the ultrasonic dispersion is 300 to 500 W;

[0023] The rotation speed of the mechanical stirring is 1500-2000r / min.

[0024] As a further preferred embodiment of the present invention, the preparation method of the porous carrier is as follows:

[0025] 1) Cut the silk cocoons into pieces and add them to a boiling sodium carbonate solution, boil for 60 to 80 minutes, then soak and wash them with distilled water for 10 to 30 minutes, repeat 2 to 5 times and then dry them to obtain degummed silk, then dissolve the degummed silk in a lithium bromide solution at 60 to 65° C. in a mass ratio of 1:(6 to 8), cool to room temperature and filter, transfer to a dialysis bag after centrifugation, dialyze with ultrapure water for 3 to 5 days, and then put them into a polyethylene glycol solution for concentration for 12 to 15 hours to obtain a silk fibroin solution;

[0026] 2) A silk fibroin solution, a chitosan solution and a gelatin solution with a mass fraction of 3 to 5% were mixed in equal volume ratios to obtain a mixed solution, and then hydroxyapatite was added to the mixed solution according to 2 to 5% of the total mass of the mixed solution, and magnetic stirring was performed for 60 to 80 minutes, and then 1 mL per well was transferred to a 48-well plate, and pre-frozen overnight at -20 to -30°C, and then continued to be frozen at -80 to -90°C for 24 to 30 hours, and then vacuum freeze-dried for 48 to 60 hours to obtain a cylindrical freeze-dried scaffold, and each well after freeze-drying Add 2-3 mL of a cross-linking agent, cross-link overnight at 4-6° C., then wash repeatedly with ethanol and deionized water, then soak in a 75-78 wt% ethanol solution for 24-30 hours, and soak in a 1-2 mol / L sodium hydroxide solution for neutralization for 6-10 hours, after repeated washing with deionized water, freeze again at -20--30° C. overnight, then continue freezing at -80--90° C. for 24-30 hours, and then freeze-dry in vacuum for 48-60 hours, and grind the dried product to obtain a granular porous carrier.

[0027] As a further preferred embodiment of the present invention, in step 1), the concentration of the sodium carbonate solution is 0.5-0.8 wt %;

[0028] The concentration of the lithium bromide solution is 9.2-9.8 mol / L;

[0029] The concentration of the polyethylene glycol solution is 10-13 wt %.

[0030] As a further preferred embodiment of the present invention, in step 2), the cross-linking agent is composed of equal volumes of 50-60 mmol / L carbodiimide solution and 25-28 mmol / L N-hydroxysuccinimide solution.

[0031] A method for preparing highly effective antibacterial pet oral cleaning water comprises the following steps:

[0032] 1) Weigh the extract according to the formula into a beaker, add half the amount of water and stir to dissolve;

[0033] 2) Weigh the inactive ingredients according to the formula and add the remaining half of the water to dissolve;

[0034] 3) After mixing the solution obtained in step 1) and the solution obtained in step 2), a synergist is added, and the vacuum is evacuated to 50-80 Pa and maintained for 10-20 min, and then the pressure is slowly released to normal pressure, and then an auxiliary agent is added, and the mixture is stirred and mixed evenly, and then the pH is adjusted to 7.0.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] In the present invention, silk fibroin, gelatin, chitosan and hydroxyapatite are used as basic materials, vacuum freeze drying and chemical crosslinking are performed to obtain a porous carrier with a porous structure, and then chitosan is acylated with maleic anhydride, and the hydrogen bonds and van der Waals forces between chitosan fibers are destroyed by ultrasonic crushing, thereby obtaining nanoscale chitosan fiber bundles, and then an enhancer is obtained by ultrasonic and mechanical stirring. The chitosan fiber bundles are embedded in the pores of the porous carrier by the effects of ultrasonic and mechanical stirring, and the nanoscale chitosan fiber bundles are partially embedded in the pores of the porous carrier, and a network structure is formed by mutual crosslinking. The formed network structure can limit the substances that penetrate into the pores later, delay the time of their outflow, and achieve a sustained release effect. At the same time, part of the nanoscale chitosan fiber bundles will be exposed outside the porous carrier to form protruding nano whiskers, thereby increasing the contact area with the matrix, so that it can better adhere to the surface, and slowly release the loaded substances by slow release, thereby achieving a long-term effect.

[0037] In the present invention, the extract and the inactive ingredient are mixed, and then the prepared enhancer is added, and the extract and the inactive ingredient are infiltrated into the pores of the enhancer by vacuum evacuation and vacuum impregnation. Due to the limiting effect of the internal network structure, the outflow rate of the extract and the inactive ingredient is relatively slow. When in use, after entering the oral cavity, a large number of nano whiskers on the surface can easily form a firm structure with the teeth, so that they are stably attached to the teeth, and the loaded extract and the inactive ingredient are slowly released in a slow release manner, so that the efficacy of the extract can be fully exerted, thereby achieving long-term antibacterial and anti-halitosis effects, better antibacterial and anti-caries, preventing the formation of dental plaque, and preventing the occurrence of gingivitis and gingivitis.

[0038] The present invention designs a pet oral cleaning water with natural animal and plant extracts as main ingredients. Aiming at the causes of pet oral diseases, the design is based on four dimensions: inhibiting oral pathogens, anti-inflammatory, hemostatic and analgesic, regulating the gastrointestinal tract to promote digestion, and removing bad breath. The water mainly contains green tea extract, stevia extract, houttuynia extract, etc. These ingredients have an antibacterial effect on harmful oral bacteria and dental plaque bacteria, and also have anti-inflammatory and analgesic effects. Combined with low-molecular amines, they can regulate intestinal flora, thereby improving the problems of oral diseases and bad breath of pets as a whole. Therefore, the pet oral cleaning water designed by the present invention has the effects of inhibiting bacteria and preventing caries, preventing the formation of dental plaque, preventing the occurrence of gingivitis and gingivitis, removing bad breath, and regulating the gastrointestinal tract. At the same time, it has the advantages of no artificial flavors, pigments, fillers or preservatives, thereby reducing the risk of swallowing by pets. DETAILED DESCRIPTION

[0039] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] In the present invention, the preparation method of Viola yedoensis extract specifically comprises the following steps:

[0041] S1: Immerse Viola yedoensis in the treatment agent at a dosage ratio of 1 g: 70 mL, and pre-treat it at a closed high temperature and high pressure of 0.4 MPa and 117 ° C for 25 minutes, and then instantly release the pressure to normal pressure;

[0042] S2 uses 99.6wt% ethanol solution as solvent, with a solid-liquid mass ratio of 1:28, and is extracted at 72°C for 43min. During the extraction process, ultrasound and microwave assistance are applied alternately, with each treatment time of 12min, an ultrasonic frequency of 25kHz, and a microwave power of 600W. The alcohol extraction product is ultrafiltered and spray-dried to obtain the Viola yedoensis extract.

[0043] The preparation method of the treatment agent is as follows:

[0044] 1) the luffa was fully dried for 3h in 108 ℃ of air blowers, ground and pulverized by a grinder, immersed in a sodium hydroxide solution of 12wt%, and heated at 63 ℃ for 40min, dried after fully washing with distilled water, and then immersed in a sodium hypochlorite solution of 15wt% for 25min, and then repeatedly washed with deionized water, and dried to obtain a pre-treatment luffa powder;

[0045] 2) 1.5 g of pretreated loofah powder was added to 130 mL of deionized water, and then 0.03 g of 2,2,6,6-tetramethylpiperidin-1-oxyl free radical and 0.3 g of sodium bromide were added, and 5 mL of 15 wt% sodium hypochlorite solution was added under 120 W ultrasound, and the reaction was continued for 2 h. During the reaction, a 0.7 wt% sodium hydroxide solution was used to adjust the pH value to 10.5, and then ethanol was added to terminate the reaction. After continuous stirring for 25 min, the mixture was centrifuged, repeatedly washed with deionized water until neutral, and freeze-dried to obtain cellulose nanofibers;

[0046] 3) 2 g of alkali lignin was dissolved in 70 mL of 1.2 mol / L sodium hydroxide solution, stirred at 260 r / min for 40 min, and then 70 mL of 1.2 mol / L zinc chloride solution was added dropwise to the system, stirred at room temperature for 3 h, and the precipitate generated by the reaction was repeatedly washed with distilled water until it was neutral, and freeze-dried to obtain a nanocomposite material;

[0047] 4) The nano-composite material is frozen with liquid nitrogen and then freeze-dried, and then placed in a muffle furnace for graded calcination, calcined at 125°C for 1.5 h, calcined at 255°C for 2.5 h, and calcined at 580°C for 2.5 h, and naturally cooled to room temperature to obtain nano-flower-like composite particles, and then the nano-flower-like composite particles are mixed with cellulose nanofibers in a mass ratio of 1:15 and added to a sufficient amount of 75wt% ethanol solution, stirred at a high speed of 13000r / min for 1.5h, dried after centrifugal separation, and then added to deionized water, stirred and dispersed evenly to obtain a treating agent with a solid content of 5wt%.

[0048] In the present invention, the flavoring agent is glycerol; the thickener is sodium alginate; and the clarifying agent is ZTC1+1-III clarifying agent.

[0049] Example 1

[0050] A highly effective antibacterial pet oral cleaning water, comprising an extract, an inactive ingredient, a synergist, an adjuvant and water, with a mass ratio of 50:10:3:5:500;

[0051] The preparation method of the pet oral cleaning water specifically comprises the following steps:

[0052] 1) Weigh the extract according to the formula into a beaker, add half the amount of water and stir to dissolve;

[0053] 2) Weigh the inactive ingredients according to the formula and add the remaining half of the water to dissolve;

[0054] 3) After mixing the solution obtained in step 1) and the solution obtained in step 2), a synergist is added, vacuuming to 50 Pa and maintaining for 10 min, then slowly releasing the pressure to normal pressure, then adding an auxiliary agent, stirring and mixing evenly, and then adjusting the pH to 7.0;

[0055] The weight proportions of the components in the extract are: 0.1 part of green tea extract, 0.5 part of Viola yedoensis extract, 1 part of pomegranate extract, 0.1 part of vanilla extract, 1 part of erythritol, and 1 part of oligofructose;

[0056] The weight parts of the inactive ingredients are: 1 part glycerin, 0.5 part citric acid, 0.2 part food grade sodium bicarbonate;

[0057] The weight proportions of each component in the auxiliary agent are: 1 part of flavoring agent, 1 part of thickener, and 1 part of clarifying agent.

[0058] Wherein, the preparation method of the synergist is as follows:

[0059] 1) Cut the silk cocoons into pieces and add them to a boiling sodium carbonate solution with a concentration of 0.5wt%, boil them for 60 minutes, then soak and wash them with distilled water for 10 minutes, repeat twice and then dry them to obtain degummed silk, then dissolve the degummed silk in a lithium bromide solution with a concentration of 9.2mol / L at 60°C according to a mass ratio of 1:6, cool to room temperature and filter, transfer to a dialysis bag after centrifugation, dialyze with ultrapure water for 3 days, and then put them into a polyethylene glycol solution with a concentration of 10wt% for concentration for 12 hours to obtain a silk fibroin solution;

[0060] 2) A silk fibroin solution, a chitosan solution and a gelatin solution with a mass fraction of 3% were mixed in equal volume ratios to obtain a mixed solution, and then hydroxyapatite was added to the mixed solution at 2% of the total mass of the mixed solution, and magnetic stirring was performed for 60 minutes. Then, 1 mL per well was transferred to a 48-well plate, pre-frozen at -20°C overnight, and then continued to be frozen at -80°C for 24 hours, and then vacuum freeze-dried for 48 hours to obtain a cylindrical freeze-dried scaffold. After freeze-drying, 2 mL of a cross-linking agent was added to each well, and the cross-linking agent consisted of an equal volume of 50 mL mol / L carbodiimide solution and 25mmol / L N-hydroxysuccinimide solution, cross-linked overnight at 4°C, then repeatedly washed with ethanol and deionized water, then soaked in 75wt% ethanol solution for 24h, and soaked in 1mol / L sodium hydroxide solution for 6h, washed repeatedly with deionized water, frozen at -20°C overnight again, then frozen at -80°C for 24h, and then freeze-dried in vacuum for 48h, the dried product was crushed and ground to obtain a granular porous carrier;

[0061] 3) Weigh maleic anhydride with a mass of 12% of chitosan mass, mix it evenly with chitosan, seal it in a container, place it in a 120° C. thermostat to react for 3 hours, and after the reaction is completed, wash the product with anhydrous ethanol to remove the color, continue to wash with pure water to a pH value of 7, then drop a 1.0 mol / L sodium hydroxide solution into the system to a pH value of 11.0, wash it by centrifugation to a pH value of 7.5, and dilute it with pure water to a concentration of 1wt%, to obtain an acylated chitosan dispersion;

[0062] 4) The acylated chitosan dispersion is placed in a container, and treated with a 22KHz ultrasonic generator at a power of 500W for 30 minutes with a 1s on / 1s off pulse to obtain a chitosan nanofiber dispersion. A porous carrier is then added to the chitosan nanofiber dispersion at a solid-liquid ratio of 1g:10mL, and ultrasonically dispersed at 300W for 1h, and then mechanically stirred at 1500r / min for 1h. After the treatment is completed, the dispersion is centrifuged, repeatedly washed with deionized water, and dried to obtain a synergist.

[0063] Example 2

[0064] A highly effective antibacterial pet oral cleaning water, comprising an extract, an inactive ingredient, a synergist, an adjuvant and water, with a mass ratio of 60:15:5:7:700;

[0065] The preparation method of the pet oral cleaning water specifically comprises the following steps:

[0066] 1) Weigh the extract according to the formula into a beaker, add half the amount of water and stir to dissolve;

[0067] 2) Weigh the inactive ingredients according to the formula and add the remaining half of the water to dissolve;

[0068] 3) After mixing the solution obtained in step 1) and the solution obtained in step 2), a synergist is added, the vacuum is evacuated to 70 Pa, and the pressure is maintained for 15 minutes, and then the pressure is slowly released to normal pressure, and then an auxiliary agent is added, and the mixture is stirred and mixed uniformly, and then the pH is adjusted to 7.0;

[0069] The weight proportions of the components in the extract are: 0.3 parts of green tea extract, 0.8 parts of Viola yedoensis extract, 1.5 parts of pomegranate extract, 0.3 parts of vanilla extract, 2 parts of erythritol, and 2 parts of oligofructose;

[0070] The weight parts of the inactive ingredients are: 2 parts of glycerin, 0.8 parts of citric acid, and 0.4 parts of food-grade sodium bicarbonate;

[0071] The weight proportions of the components in the auxiliary agent are: 1.5 parts of flavoring agent, 1.5 parts of thickener, and 1.5 parts of clarifying agent.

[0072] Wherein, the preparation method of the synergist is as follows:

[0073] 1) Cut the silk cocoons into pieces and add them to a boiling sodium carbonate solution with a concentration of 0.7wt%, boil them for 70min, then soak and wash them with distilled water for 20min, repeat 3 times and dry them to obtain degummed silk, then dissolve the degummed silk in a lithium bromide solution with a concentration of 9.5mol / L at 62°C according to a mass ratio of 1:7, cool them to room temperature and filter them, transfer them to a dialysis bag after centrifugation, dialyze them with ultrapure water for 4d, and then put them into a polyethylene glycol solution with a concentration of 12wt% for concentration for 13h to obtain a silk fibroin solution;

[0074] 2) A silk fibroin solution, a chitosan solution and a gelatin solution with a mass fraction of 4% were mixed in equal volumes to obtain a mixed solution, and then hydroxyapatite was added to the mixed solution at 3% of the total mass of the mixed solution, and magnetic stirring was performed for 70 minutes. Then, 1 mL per well was transferred to a 48-well plate, pre-frozen at -25°C overnight, and then continued to be frozen at -85°C for 26 hours, and then vacuum freeze-dried for 52 hours to obtain a cylindrical freeze-dried scaffold. After freeze-drying, 2.5 mL of a cross-linking agent was added to each well, and the cross-linking agent consisted of an equal volume of 55 mL mol / L carbodiimide solution and 26mmol / L N-hydroxysuccinimide solution, cross-linked overnight at 5°C, then repeatedly washed with ethanol and deionized water, then soaked in 76wt% ethanol solution for 26h, and soaked in 1.5mol / L sodium hydroxide solution for neutralization for 8h, after repeated washing with deionized water, frozen at -25°C overnight again, then continued to freeze at -85°C for 26h, and then vacuum freeze-dried for 52h, the dried product was crushed and ground to obtain a granular porous carrier;

[0075] 3) Weigh maleic anhydride with a mass of 18% of chitosan mass, mix it evenly with chitosan, seal it in a container, place it in a constant temperature box at 123° C. for 4 hours, and after the reaction is completed, wash the product with anhydrous ethanol to remove the color, continue to wash with pure water until the pH value is 7, then drip a 1.2 mol / L sodium hydroxide solution into the system until the pH value is 11.5, wash it by centrifugation until the pH value is 7.8, and dilute it with pure water to a concentration of 1.5wt% to obtain an acylated chitosan dispersion;

[0076] 4) The acylated chitosan dispersion is placed in a container, and treated with a 23KHz ultrasonic generator at a power of 550W and a 1s on / 1s off pulse for 40min to obtain a chitosan nanofiber dispersion. A porous carrier is then added to the chitosan nanofiber dispersion at a solid-liquid ratio of 1g:15mL, and ultrasonically dispersed at 400W for 1.5h, and then mechanically stirred at 1800r / min for 1.5h. After the treatment is completed, centrifugation is performed, and the synergist is obtained after repeated washing with deionized water and drying.

[0077] Example 3

[0078] A highly effective antibacterial pet oral cleaning water, comprising an extract, an inactive ingredient, a synergist, an adjuvant and water, with a mass ratio of 70:20:8:10:800;

[0079] The preparation method of the pet oral cleaning water specifically comprises the following steps:

[0080] 1) Weigh the extract according to the formula into a beaker, add half the amount of water and stir to dissolve;

[0081] 2) Weigh the inactive ingredients according to the formula and add the remaining half of the water to dissolve;

[0082] 3) After mixing the solution obtained in step 1) and the solution obtained in step 2), a synergist is added, vacuuming to 80 Pa and maintaining for 20 min, then slowly releasing the pressure to normal pressure, then adding an auxiliary agent, stirring and mixing evenly, and then adjusting the pH to 7.0;

[0083] The weight proportions of the components in the extract are: 0.5 parts of green tea extract, 1 part of Viola yedoensis extract, 2 parts of pomegranate extract, 0.5 parts of vanilla extract, 3 parts of erythritol, and 3 parts of oligofructose;

[0084] The weight parts of the inactive ingredients are: 3 parts of glycerin, 1.2 parts of citric acid, and 0.6 parts of food-grade sodium bicarbonate;

[0085] The weight proportions of each component in the auxiliary agent are: 2 parts of flavoring agent, 2 parts of thickener, and 2 parts of clarifying agent.

[0086] Wherein, the preparation method of the synergist is as follows:

[0087] 1) Cut the silk cocoons into pieces and add them to a boiling sodium carbonate solution with a concentration of 0.8wt%, boil them for 80min, then soak and wash them with distilled water for 30min, repeat 5 times and dry them to obtain degummed silk, then dissolve the degummed silk in a lithium bromide solution with a concentration of 9.8mol / L at 65°C according to a mass ratio of 1:8, cool them to room temperature and filter them, transfer them to a dialysis bag after centrifugation, dialyze them with ultrapure water for 5d, and then put them into a polyethylene glycol solution with a concentration of 13wt% for concentration for 15h to obtain a silk fibroin solution;

[0088] 2) A silk fibroin solution, a chitosan solution and a gelatin solution with a mass fraction of 5% were mixed in equal volumes to obtain a mixed solution, and then hydroxyapatite was added to the mixed solution at 5% of the total mass of the mixed solution, and magnetic stirring was performed for 80 minutes. Then, 1 mL per well was transferred to a 48-well plate, pre-frozen at -30°C overnight, and then continued to be frozen at -90°C for 30 hours, and then vacuum freeze-dried for 60 hours to obtain a cylindrical freeze-dried scaffold. After freeze-drying, 3 mL of a cross-linking agent was added to each well, and the cross-linking agent consisted of an equal volume of 60 mL mol / L carbodiimide solution and 28mmol / L N-hydroxysuccinimide solution, cross-linked at 6°C overnight, then repeatedly washed with ethanol and deionized water, then soaked in 78wt% ethanol solution for 30h, and soaked in 2mol / L sodium hydroxide solution for 10h, washed repeatedly with deionized water, frozen at -30°C overnight again, then frozen at -90°C for 30h, and then freeze-dried in vacuum for 60h, the dried product was crushed and ground to obtain a granular porous carrier;

[0089] 3) Weigh maleic anhydride with a mass of 20% of the mass of chitosan, mix it evenly with chitosan, seal it in a container, place it in a constant temperature box at 125° C. to react for 5 hours, and after the reaction is completed, wash the product with anhydrous ethanol to remove the color, continue to wash with pure water until the pH value is 7, then drip a 1.5 mol / L sodium hydroxide solution into the system until the pH value is 11.5, wash it by centrifugation until the pH value is 7.8, and dilute it with pure water to a concentration of 2wt% to obtain an acylated chitosan dispersion;

[0090] 4) The acylated chitosan dispersion is placed in a container, and treated with a 25KHz ultrasonic generator at a power of 600W for 1s on / 1s off pulse for 50min to obtain a chitosan nanofiber dispersion. A porous carrier is then added to the chitosan nanofiber dispersion at a solid-liquid ratio of 1g:20mL, and ultrasonically dispersed at 500W for 2h, and then mechanically stirred at 2000r / min for 2h. After the treatment is completed, the dispersion is centrifuged, repeatedly washed with deionized water, and dried to obtain a synergist.

[0091] Comparative Example 1: This comparative example is substantially the same as Example 1, except that it does not contain a synergist.

[0092] Comparative Example 2: This comparative example is substantially the same as Example 1, except that, in the preparation of the synergist, step 1) is omitted.

[0093] Comparative Example 3: This comparative example is basically the same as Example 1, except that step 2) is omitted in the preparation of the synergist.

[0094] Comparative Example 4: This comparative example is basically the same as Example 1, except that step 3) is omitted in the preparation of the synergist.

[0095] Comparative Example 5: This comparative example is basically the same as Example 1, except that step 4) is omitted in the preparation of the synergist.

[0096] Test experiment:

[0097] The preparation methods provided in Examples 1 to 3 and Comparative Examples 1 to 5 were respectively used to prepare oral cleaning water samples; 90 experimental dogs with the same growth environment, feeding conditions, age, and breed were randomly divided into 9 groups, with 10 dogs in each group. The oral cleaning water samples of Examples 1 to 3 and Comparative Examples 1 to 5 were used once a day, and the control group was used with an equal amount of physiological saline once a day for 3 consecutive days; oral swabs were taken for colony culture, and the bacterial culture results before and after the experiment were observed, as shown in Table 1 (the values ​​are colony counts).

[0098] Table 1

[0099]

[0100] It can be seen from Table 1 that the pet oral cleaning water of the present invention can effectively inhibit the growth of bacteria, can achieve long-term antibacterial and anti-bad breath effects, can better inhibit bacteria and prevent caries, prevent the formation of dental plaque, and prevent the occurrence of gingivitis and gingivitis.

[0101] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A highly effective antibacterial pet oral cleaning water. It is characterized in that The pet oral cleaning water comprises an extract, an inactive ingredient, a synergist, an adjuvant and water; The extract comprises green tea extract, Viola yedoensis extract, pomegranate extract, vanilla extract, erythritol, and oligofructose; The inactive ingredients include glycerin, citric acid, and food-grade sodium bicarbonate; The auxiliary agents include flavoring agents, thickeners and clarifying agents.

2. A highly effective antibacterial pet oral cleaning water according to claim 1, It is characterized in that The flavoring agent is at least one of glycerol, mannitol and saccharin sodium; The thickener is at least one of sodium alginate, sodium carboxymethyl cellulose and sodium carboxymethyl starch; The clarifier is ZTC1+1-III clarifier.

3. The highly effective antibacterial pet oral cleaning water according to claim 1, It is characterized in that In the pet oral cleaning water, the mass ratio of the extract, the inactive ingredient, the synergist, the adjuvant and the water is (50-70): (10-20): (3-8): (5-10): (500-800); The weight proportions of the components in the extract are: 0.1-0.5 parts of green tea extract, 0.5-1 parts of Viola yedoensis extract, 1-2 parts of pomegranate extract, 0.1-0.5 parts of vanilla extract, 1-3 parts of erythritol, and 1-3 parts of oligofructose; The weight parts of the inactive ingredients are: 1 to 3 parts of glycerin, 0.5 to 1.2 parts of citric acid, and 0.2 to 0.6 parts of food-grade sodium bicarbonate; The weight proportions of the components in the auxiliary agent are: 1 to 2 parts of flavor corrector, 1 to 2 parts of thickener, and 1 to 2 parts of clarifier.

4. The highly effective antibacterial pet oral cleaning water according to claim 1, It is characterized in that The preparation method of the synergist is as follows: 1) Weigh maleic anhydride, mix it with chitosan, seal it in a container, place it in a thermostat at 120-125° C. for reaction for 3-5 hours, after the reaction is completed, wash the product with anhydrous ethanol to remove the color, continue to wash with pure water until the pH value is 7, then drip sodium hydroxide solution into the system until the pH value is 11.0-11.5, wash it by centrifugation until the pH value is 7.5-7.8, and dilute it with pure water to a concentration of 1-2wt% to obtain an acylated chitosan dispersion; 2) The acylated chitosan dispersion is placed in a container, and treated with a 22-25KHz ultrasonic generator at a power of 500-600W and a 1s on / 1s off pulse for 30-50min to obtain a chitosan nanofiber dispersion. A porous carrier is then added to the chitosan nanofiber dispersion at a solid-liquid ratio of 1g: (10-20)mL, and ultrasonically dispersed for 1-2h, and then mechanically stirred for 1-2h. After the treatment is completed, the dispersion is centrifuged, repeatedly washed with deionized water, and dried to obtain a synergist.

5. The highly effective antibacterial pet oral cleaning water according to claim 4, It is characterized in that In step 1), the mass of the maleic anhydride is 12-20% of the mass of the chitin; The concentration of the sodium hydroxide solution is 1.0-1.5 mol / L.

6. The highly effective antibacterial pet oral cleaning water according to claim 4, It is characterized in that In step 2), the power of the ultrasonic dispersion is 300-500W; The rotation speed of the mechanical stirring is 1500-2000r / min.

7. The highly effective antibacterial pet oral cleaning water according to claim 4, It is characterized in that The preparation method of the porous carrier is as follows: 1) Cut the silk cocoons into pieces and add them to a boiling sodium carbonate solution, boil for 60 to 80 minutes, then soak and wash them with distilled water for 10 to 30 minutes, repeat 2 to 5 times and then dry them to obtain degummed silk, then dissolve the degummed silk in a lithium bromide solution at 60 to 65° C. in a mass ratio of 1:(6 to 8), cool to room temperature and filter, transfer to a dialysis bag after centrifugation, dialyze with ultrapure water for 3 to 5 days, and then put them into a polyethylene glycol solution for concentration for 12 to 15 hours to obtain a silk fibroin solution; 2) A silk fibroin solution, a chitosan solution and a gelatin solution with a mass fraction of 3 to 5% were mixed in equal volume ratios to obtain a mixed solution, and then hydroxyapatite was added to the mixed solution according to 2 to 5% of the total mass of the mixed solution, and magnetic stirring was performed for 60 to 80 minutes, and then 1 mL per well was transferred to a 48-well plate, and pre-frozen overnight at -20 to -30°C, and then continued to be frozen at -80 to -90°C for 24 to 30 hours, and then vacuum freeze-dried for 48 to 60 hours to obtain a cylindrical freeze-dried scaffold, and each well after freeze-drying Add 2-3 mL of a cross-linking agent, cross-link overnight at 4-6° C., then wash repeatedly with ethanol and deionized water, then soak in a 75-78 wt% ethanol solution for 24-30 hours, and soak in a 1-2 mol / L sodium hydroxide solution for neutralization for 6-10 hours, after repeated washing with deionized water, freeze again at -20--30° C. overnight, then continue freezing at -80--90° C. for 24-30 hours, and then freeze-dry in vacuum for 48-60 hours, and grind the dried product to obtain a granular porous carrier.

8. The highly effective antibacterial pet oral cleaning water according to claim 7, It is characterized in that In step 1), the concentration of the sodium carbonate solution is 0.5-0.8 wt %; The concentration of the lithium bromide solution is 9.2-9.8 mol / L; The concentration of the polyethylene glycol solution is 10-13 wt %.

9. The highly effective antibacterial pet oral cleaning water according to claim 7, It is characterized in that In step 2), the cross-linking agent is composed of equal volumes of 50-60 mmol / L carbodiimide solution and 25-28 mmol / L N-hydroxysuccinimide solution.

10. A method for preparing a highly effective antibacterial pet oral cleaning water according to any one of claims 1 to 9, It is characterized in that The specific steps include: 1) Weigh the extract according to the formula into a beaker, add half the amount of water and stir to dissolve; 2) Weigh the inactive ingredients according to the formula and add the remaining half of the water to dissolve; 3) After mixing the solution obtained in step 1) and the solution obtained in step 2), a synergist is added, and the vacuum is evacuated to 50-80 Pa and maintained for 10-20 min, and then the pressure is slowly released to normal pressure, and then an auxiliary agent is added, and the mixture is stirred and mixed evenly, and then the pH is adjusted to 7.0.

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