An oral care fluid and a method of preparing the same

Abstract

The application relates to the field of daily chemical products, and particularly discloses an oral care liquid and a preparation method thereof. The oral care liquid comprises the following raw materials in parts by weight: 0.003-0.02 parts of sodium hypochlorite, 1-5 parts of a humectant, 0.1-0.3 parts of menthol, 0.1-0.5 parts of PEG-400, 3-7 parts of citric acid, 0.01-0.5 parts of essence, 0.5-1 part of a suspending agent, 0.1-1 part of a long-acting antibacterial component, and 80-90 parts of purified water; the long-acting antibacterial component comprises a gelatin-chitosan self-assembled film and an antibacterial agent loaded on the gelatin-chitosan self-assembled film. The oral care liquid disclosed by the application can effectively kill Helicobacter pylori and other pathogenic bacteria in the oral cavity, has good and long-lasting antibacterial effect, solves periodontal problems such as dental plaque, periodontitis and gingivitis, and has the advantages of protecting oral health.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily chemical products, more particularly, it relates to an oral care solution and a preparation method thereof. BACKGROUND

[0002] Oral diseases are common diseases caused by various pathogenic bacteria in the oral cavity, which directly affect people's physical health. In particular, Helicobacter pylori exists in more than 50% of the world's population in the upper digestive system, which can cause halitosis, acid reflux, nausea, vomiting and other symptoms. People prevent the occurrence of oral diseases through oral care products. Oral care products mainly include toothpaste, mouthwash and breath fresheners. These products mainly play the roles of cleaning teeth, whitening teeth, removing dental plaque, killing harmful bacteria in the oral cavity, preventing dental caries, and cleaning breath. At the same time, they also play a positive role in the treatment of some oral diseases such as gingival inflammation.

[0003] A Chinese patent application with the application number CN2010105634594 discloses an oral care solution, which comprises, by weight ratio, medicinal plant extract 1%-20%, sodium molsulfonate 0.005-0.5%, functional components 0.1%-10%, antibacterial agent 0.01%-0.5%, solubilizer 1-15%, sweetener 0.01%-5%, thickening agent 1-20%, essence 0.01%-0.5%, ethanol 0.1%-5%, water 13%-90%, and pH regulator 0.001%-10%. The oral care solution has the effects of cleaning the oral cavity and teeth, relieving discomfort symptoms such as toothache and oral ulcer, and protecting oral health. However, the inventors found that the antibacterial agent in the oral care solution has a short action time, even if it kills part of the bacteria, new bacteria and microorganisms will soon breed, especially at night, the growth and reproduction of bacteria and microorganisms in the oral cavity is extremely fast, and the acidic metabolites produced thereby will still cause oral odor and dental caries. SUMMARY

[0004] In order to prolong the bacteriostatic long-acting property of the oral care solution, the present application provides an oral care solution and a preparation method thereof.

[0005] In a first aspect, the present application provides an oral care solution, which adopts the following technical solution:

[0006] An oral care solution comprises the following raw materials by weight: 0.003-0.02 parts of sodium hypochlorite, 1-5 parts of a humectant, 0.1-0.3 parts of menthol, 0.1-0.5 parts of PEG-400, 3-7 parts of citric acid, 0.01-0.5 parts of essence, 0.5-1 part of a suspending agent, 0.1-1 part of a long-acting antibacterial component, and 80-90 parts of purified water.

[0007] The long-acting antibacterial component comprises a gelatin-chitosan self-assembled membrane and an antibacterial agent loaded on the gelatin-chitosan self-assembled membrane.

[0008] By adopting the above technical scheme, the sodium hypochlorite, menthol and citric acid are used to prepare the oral care liquid, the sodium hypochlorite has a high-efficiency sterilization effect, the menthol has a cooling effect, the oral care liquid has a refreshing taste, a pure and long-lasting fragrance, can quickly eliminate oral odor and is suitable for a wide range of people; the long-acting antibacterial component comprises a gelatin-chitosan self-assembled membrane and an antibacterial agent loaded in the gelatin-chitosan self-assembled membrane, the gelatin-chitosan self-assembled membrane has a multi-layer structure, the antibacterial agent is loaded in the layer structure, the release rate of the antibacterial agent is delayed, the antibacterial durability is improved, the suspension agent is added in the oral care liquid, the adhesion of the oral care liquid is increased, the retention time of the long-acting antibacterial component in the oral cavity is improved, and the antibacterial time is prolonged.

[0009] Optionally, the antibacterial agent comprises an antibacterial plant extract and a silicone quaternary ammonium salt, and a mass ratio of the gelatin-chitosan self-assembled membrane, the antibacterial plant extract and the silicone quaternary ammonium salt is 1:0.3-0.5:0.05-0.1.

[0010] By adopting the above technical scheme, the antibacterial plant extract has a small drug resistance, is not easy to have residues and certain toxic side effects, has a high safety, the silicone quaternary ammonium salt has a positive charge, can adsorb pathogenic microorganisms such as bacteria, fungi and viruses with negative charges through electrostatic adsorption, makes the pathogenic microorganisms rupture and die, has a physical effect of killing pathogenic microorganisms and has no side effects on the human body and is safe to use.

[0011] Optionally, the preparation method of the long-acting antibacterial component comprises the following steps.

[0012] The antibacterial plant extract and the silicone quaternary ammonium salt are mixed with water respectively to prepare an antibacterial liquid and a silicone quaternary ammonium salt solution;

[0013] The gelatin-chitosan self-assembled membrane is soaked in the antibacterial liquid for 1.5-2 hours, taken out, washed with deionized water and then dried to prepare a pretreated self-assembled membrane;

[0014] The pretreated self-assembled membrane is cyclically immersed in an okra stock solution and dried to prepare an intermediate self-assembled membrane;

[0015] The intermediate self-assembled membrane is cyclically immersed in the silicone quaternary ammonium salt solution, deionized water and chitosan solution for 10-15 cycles to prepare the long-acting antibacterial component.

[0016] By adopting the technical scheme, firstly, the antibacterial plant extract is dissolved to prepare an antibacterial solution, and the antibacterial plant extract is loaded on the gelatin-chitosan self-assembled membrane through soaking. The antibacterial plant extract continuously enters the self-assembled membrane through diffusion, so that the loading amount continuously increases. Since the antibacterial plant extract is a hydrophilic substance and has strong diffusion capacity, the okra stock solution is used to form an okra membrane on the surface of the pretreated self-assembled membrane as a barrier layer to play a protective role. The antibacterial plant extract has to pass through the barrier layer to diffuse out of the self-assembled membrane, thereby slowing down the release rate of the antibacterial plant extract and prolonging the release time. Then, the organosilicon quaternary ammonium salt is loaded on the gelatin-chitosan self-assembled membrane loaded with the antibacterial plant extract. When the organosilicon quaternary ammonium salt solution is first immersed, the sticky okra membrane on the surface can load the organosilicon quaternary ammonium salt on the surface. When the organosilicon quaternary ammonium salt solution is immersed again, the organosilicon quaternary ammonium salt is loaded on the self-assembled membrane layer by layer under the action of chitosan. Therefore, after the long-acting antibacterial component enters the oral cavity, the organosilicon quaternary ammonium salt is gradually released from the multilayer chitosan membrane. After the multilayer chitosan membrane gradually dissolves in the oral cavity, the okra coating continuously dissolves to release the antibacterial plant extract inside, thereby prolonging the release time of the antibacterial component and improving the long-acting antibacterial property. In addition, the okra stock solution contains okra flavone components, which have the effects of clearing heat and detoxifying, anti-inflammatory and antibacterial, and analgesic, and can further improve the treatment effect of the oral care solution on oral problems such as oral ulcers and gum swelling and pain.

[0017] Optionally, the preparation method of the chitosan solution comprises the following steps: dissolving carbomer in ultrapure water to obtain a carbomer sol with a concentration of 1-3 wt%, adding chitosan, stirring uniformly, and adjusting the pH to 7-8. The mass ratio of carbomer to chitosan is 1-3:1.

[0018] By adopting the technical scheme, the carbomer swells to form an acidic viscous sol when it comes into contact with water, and the chitosan is only dissolved in an acidic medium to form a colloidal viscous substance. Therefore, the crosslinking of the two can obtain a good hydrogel with a delicate and smooth feeling, so that the surface of the long-acting antibacterial component has a delicate and smooth feeling, has a good coupling effect with the skin, reduces the foreign body sensation of the long-acting antibacterial component when it stays in the oral cavity, and improves the viscosity of the chitosan solution by the carbomer. The long-acting antibacterial component has good adhesion to the oral mucosa or the outer surface of the teeth, prolongs the retention time of the long-acting antibacterial component in the oral cavity, promotes the absorption of the antibacterial plant extract and the organosilicon quaternary ammonium salt by the oral mucosa and the gums around the teeth, and enhances the medicinal effect of the antibacterial component.

[0019] Optionally, the antibacterial plant extract comprises dandelion extract, honeysuckle flower extract, and salvia extract at a mass ratio of 0.3-0.7:0.1-0.4:1.

[0020] The sage extract has the effects of detoxification, swelling relief, oral cavity and tooth cleaning, and gum strengthening, and helps to relieve gum swelling and pain and oral cavity ulcer; the dandelion extract can clear heat, detoxify and relieve swelling, and can supplement the nutrients lost by teeth and gums, repair tooth enamel, tighten gums, prevent teeth from loosening and falling out, and relieve ulcer and gum swelling; the honeysuckle flower has the effects of clearing heat and detoxifying and dispelling wind-heat, and can relieve ulcer and gum swelling; and the sage extract, the dandelion extract and the honeysuckle flower extract have the effects of antibiosis and bacteriostasis.

[0021] Optionally, the preparation method of the gelatin-chitosan self-assembled film is as follows:

[0022] The gelatin is dissolved in distilled water to prepare a gelatin solution, and the chitosan is dissolved in acetic acid to prepare a chitosan solution;

[0023] The glass sheet is sequentially immersed in the gelatin solution, deionized water and the chitosan solution for 10-20 times, and is air-dried at room temperature, peeled off and cut to prepare the gelatin-chitosan self-assembled film.

[0024] Through the above technical scheme, the chitosan is edible, the gelatin can form a film with good mechanical properties, the self-assembled film of the gelatin and the chitosan is prepared through electrostatic deposition, the cycle number is 10-20 times, the outer layer of the prepared gelatin-chitosan self-assembled film is the chitosan layer, the chitosan itself has good antibacterial and hydrophobic properties, has a good killing effect on common pathogenic bacteria, and the cutting size is controlled to reduce the foreign body sensation of the gelatin-chitosan self-assembled film when retained in the oral cavity.

[0025] Optionally, the humectant is at least one of xylitol, sorbitol and lactitol.

[0026] Through the above technical scheme, the humectant in the oral care solution can prevent the damage of the skin in the oral cavity and promote the repair of the damaged skin, thereby protecting the gums, delaying the oral mucosa, relieving toothache, gum bleeding, oral ulcer, gingivitis, periodontitis, sore throat and other uncomfortable symptoms, and making the oral cavity healthier.

[0027] Optionally, the suspending agent is at least one of polyvinylpyrrolidone, carbomer, sodium carboxymethyl cellulose, algin and xanthan gum.

[0028] Through the above technical scheme, polyvinylpyrrolidone, carbomer, sodium carboxymethyl cellulose, algin and xanthan gum and the like are added to the oral care solution as suspending agents, which can effectively improve the texture uniformity of the oral care solution, improve the dispersion uniformity of the long-acting antibacterial component in the oral care solution, improve the adhesion of the oral care solution to the oral mucosa and the tooth surface, increase the retention time of the long-acting antibacterial component in the oral cavity, and achieve a long-lasting bacteriostatic effect.

[0029] Optionally, the oral care liquid further comprises 1-3 parts by weight of mussel mucin.

[0030] By adopting the technical scheme, the mussel mucin has high strength, high toughness and water resistance, belongs to macromolecular protein, has the effect of forming a micro non-continuous adhesive film on a local site to effectively protect a wound surface and promote wound healing, has hydrophobic effect and is not easily taken into the body by saliva in the oral cavity, increases the retention time of the oral care liquid in the oral cavity, prolongs the antibacterial persistence of the antibacterial component, effectively kills bacteria in the oral cavity, and thus has a good removal effect on halitosis caused by bacteria in the oral cavity.

[0031] In a second aspect, the application provides a preparation method of the oral care liquid, which adopts the following technical scheme:

[0032] The preparation method of the oral care liquid comprises the following steps:

[0033] The moisturizing agent, PEG-400, sodium hypochlorite, menthol, citric acid and essence are mixed to prepare component A;

[0034] The purified water, suspending agent and long-acting antibacterial component are uniformly mixed to prepare component B;

[0035] The components A and B are uniformly mixed, and the pH value is adjusted to 5-7 to prepare the oral care liquid.

[0036] By adopting the technical scheme, the oral care liquid is prepared by a simple raw material mixing method, has good antibacterial persistence, freshens breath, relieves pain, stops bleeding, has anti-inflammatory effect, protects gum health, reduces gum bleeding and lightens dental plaque.

[0037] In summary, the application has the following beneficial effects:

[0038] 1. Since the long-acting antibacterial component, suspending agent and other components are added in the oral care liquid, the long-acting antibacterial component stays in the oral cavity for a long time, has a long antibacterial effect, has a good effect when used before sleep, can effectively kill Helicobacter pylori and other pathogenic bacteria in the oral cavity, eliminate oral odor, relieve toothache symptoms, keep teeth white, solve periodontal problems such as dental plaque, periodontitis and gingivitis, and keep the oral cavity clean and hygienic, healthy teeth and gums, and reduce the occurrence of dental caries and oral diseases.

[0039] 2. In the application, the adherent type thin film chitosan is used as the outer layer and the quick-dissolving okra film is used as the barrier layer when the long-acting antibacterial component is prepared, the long-acting antibacterial component stays in the oral cavity for a long time, and when the chitosan film in the outer layer dissolves, the okra film can quickly dissolve under the action of saliva to release the antibacterial plant extract inside, so as to achieve antibacterial continuity and persistence.

[0040] 3, The carbomer is preferably used in the application to improve the viscosity of the chitosan solution, increase the retention time of the long-acting antibacterial component in the oral cavity, and add mussel mucin to the oral care liquid to improve the healing effect of the oral care liquid on damaged skin such as oral ulcers. DETAILED DESCRIPTION

[0041] Preparation Example 1 of gelatin-chitosan self-assembled film

[0042] Dissolve 1.25 kg of gelatin in distilled water to prepare a gelatin solution with a concentration of 1.25 wt%, and dissolve 1.75 kg of chitosan in 1% acetic acid by volume to prepare a chitosan solution with a concentration of 1.75 wt%.

[0043] After washing the glass sheet with deionized water for 15 min, immerse it in the gelatin solution for 2 min, take it out and immerse it in deionized water for 1 min, then take it out and immerse it in the chitosan solution for 2 min. Repeat the immersion in the gelatin solution-deionized water-chitosan solution for 20 times, and air dry at room temperature for 30 min. Then, peel off the formed film from the glass sheet, cut it into squares with a length of 3 mm, and obtain the gelatin-chitosan self-assembled film.

[0044] Preparation Example 1 of okra stock solution

[0045] After removing the head of fresh okra, crush it, add 2 times the mass of water to the crushed okra, mix well, adjust the pH to 4 with 10% hydrochloric acid, and incubate at 50°C for 120 min. Then, filter and centrifuge at 4°C and 4000 r / min for 15 min. Take the supernatant to obtain the okra stock solution.

[0046] Preparation Example 1 of long-acting antibacterial component

[0047] Preparation Example 1: (1) Mix 0.5 kg of antibacterial plant extract and 0.1 kg of organosilicon quaternary ammonium salt with water to prepare an antibacterial solution with a concentration of 5 wt% and an organosilicon quaternary ammonium salt solution with a concentration of 1 wt%, respectively. The antibacterial plant extract includes dandelion extract, honeysuckle extract, and sage extract with a mass ratio of 0.7:0.4:1.

[0048] (2) Soak 1 kg of gelatin-chitosan self-assembled film in the antibacterial solution, immerse at 40°C for 2 h, take it out, immerse it in deionized water for 2 min, and then dry it with N2. Thus, a pretreated self-assembled film is obtained. The gelatin-chitosan self-assembled film is prepared according to Preparation Example 1 of gelatin-chitosan self-assembled film.

[0049] (3) the pretreated self-assembled membrane is cyclically immersed in okra stock solution at room temperature, and the intermediate self-assembled membrane is prepared after 3 times of cyclic immersion, the okra stock solution immersion time is 3 min, and the okra stock solution is prepared according to the preparation example 1 of the okra stock solution;

[0050] (4) the intermediate self-assembled membrane is sequentially immersed in the organosilicon quaternary ammonium salt solution, deionized water and chitosan solution, which is one cycle, and the process is repeated for 15 cycles, and then the long-acting antibacterial component is prepared after nitrogen blowing drying, the organosilicon quaternary ammonium salt solution immersion time is 15 min, the deionized water immersion time is 3 min, and the chitosan solution immersion time is 15 min, and the chitosan solution concentration is 1 g / L, which is prepared by dispersing chitosan in 1% acetic acid, and the pH is 8.

[0051] Preparation Example 2: (1) 0.3 kg of antibacterial plant extract and 0.05 kg of organosilicon quaternary ammonium salt are mixed with water to prepare an antibacterial solution with a concentration of 3 wt% and an organosilicon quaternary ammonium salt solution with a concentration of 0.5 wt%, respectively, and the antibacterial plant extract includes dandelion extract, honeysuckle flower extract and salvia extract with a mass ratio of 0.3:0.1:1;

[0052] (2) 1 kg of gelatin-chitosan self-assembled membrane is immersed in the antibacterial solution, immersed at 40°C for 1.5 h, taken out, immersed in deionized water for 2 min, and then dried with N2 to prepare a pretreated self-assembled membrane, and the gelatin-chitosan self-assembled membrane is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled membrane;

[0053] (3) the pretreated self-assembled membrane is cyclically immersed in okra stock solution at room temperature, and the intermediate self-assembled membrane is prepared after 3 times of cyclic immersion, the okra stock solution immersion time is 3 min, and the okra stock solution is prepared according to the preparation example 1 of the okra stock solution;

[0054] (4) the intermediate self-assembled membrane is sequentially immersed in the organosilicon quaternary ammonium salt solution, deionized water and chitosan solution, which is one cycle, and the process is repeated for 15 cycles, and then the long-acting antibacterial component is prepared after nitrogen blowing drying, the organosilicon quaternary ammonium salt solution immersion time is 15 min, the deionized water immersion time is 3 min, and the chitosan solution immersion time is 15 min, and the chitosan solution concentration is 1 g / L, which is prepared by dispersing chitosan in 1% acetic acid, and the pH is 8.

[0055] Preparation Example 3: (1) 0.5 kg of antibacterial plant extract is mixed with water to prepare an antibacterial solution with a concentration of 5 wt%, and the antibacterial plant extract includes dandelion extract, honeysuckle flower extract and salvia extract with a mass ratio of 0.7:0.4:1;

[0056] (2) Soak 1 kg of the gelatin-chitosan self-assembled film in the antibacterial solution, immerse at 40 °C for 2 h, take out, immerse in deionized water for 2 min, and then dry with N2 to obtain a pretreated self-assembled film, wherein the gelatin-chitosan self-assembled film is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled film.

[0057] Preparation example 4: (1) Mix 0.5 kg of the antibacterial plant extract and 0.1 kg of the organosilicon quaternary ammonium salt with water respectively to prepare an antibacterial solution with a concentration of 5 wt% and an organosilicon quaternary ammonium salt solution with a concentration of 1 wt%, wherein the antibacterial plant extract comprises dandelion extract, honeysuckle flower extract and salvia extract at a mass ratio of 0.7:0.4:1.

[0058] (2) Soak 1 kg of the gelatin-chitosan self-assembled film in the antibacterial solution, immerse at 40 °C for 2 h, take out, immerse in deionized water for 2 min, and then dry with N2 to obtain a pretreated self-assembled film, wherein the gelatin-chitosan self-assembled film is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled film.

[0059] (3) Cyclically immerse the pretreated self-assembled film in the okra stock solution at room temperature for 3 times to obtain an intermediate self-assembled film, wherein the immersion time of the okra stock solution is 5 min, and the okra stock solution is prepared according to the preparation example 1 of the okra stock solution.

[0060] Preparation example 4: (1) Mix 0.5 kg of the antibacterial plant extract and 0.1 kg of the organosilicon quaternary ammonium salt with water respectively to prepare an antibacterial solution with a concentration of 5 wt% and an organosilicon quaternary ammonium salt solution with a concentration of 1 wt%, wherein the antibacterial plant extract comprises dandelion extract, honeysuckle flower extract and salvia extract at a mass ratio of 0.7:0.4:1.

[0061] (2) Soak 1 kg of the gelatin-chitosan self-assembled film in the antibacterial solution, immerse at 40 °C for 2 h, take out, immerse in deionized water for 2 min, and then dry with N2 to obtain a pretreated self-assembled film, wherein the gelatin-chitosan self-assembled film is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled film.

[0062] (3) Cyclically immerse the pretreated self-assembled film in the organosilicon quaternary ammonium salt solution, deionized water and chitosan solution in sequence, which is one cycle, and repeat for 15 cycles, and then dry with N2, wherein the immersion time of the organosilicon quaternary ammonium salt solution is 15 min, the immersion time of the deionized water is 3 min, and the immersion time of the chitosan solution is 15 min, to obtain a long-acting antibacterial component, wherein the concentration of the chitosan solution is 1 g / L, which is prepared by dispersing chitosan in acetic acid with a volume fraction of 1%, and the pH is 8.

[0063] Preparation example 6: (1) Mix 0.1 kg of the organosilicon quaternary ammonium salt with water to prepare an organosilicon quaternary ammonium salt solution with a concentration of 1 wt%.

[0064] (2) Soak 1 kg of the gelatin-chitosan self-assembled film in the organic silicon quaternary ammonium salt solution, immerse at 40°C for 2 h, take out, immerse in deionized water for 2 min, and dry with N2 to obtain the long-acting antibacterial component. The gelatin-chitosan self-assembled film is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled film.

[0065] Preparation example 7: (1) Mix 0.5 kg of the antibacterial plant extract and 0.1 kg of the organic silicon quaternary ammonium salt with water respectively to prepare an antibacterial solution with a concentration of 5 wt% and an organic silicon quaternary ammonium salt solution with a concentration of 1 wt%. The antibacterial plant extract comprises dandelion extract, honeysuckle flower extract, and salvia extract at a mass ratio of 0.7:0.4:1.

[0066] (2) Soak 1 kg of the gelatin-chitosan self-assembled film in the mixture of the antibacterial solution and the organic silicon quaternary ammonium salt solution, immerse at 40°C for 2 h, take out, immerse in deionized water for 2 min, and dry with N2 to obtain the long-acting antibacterial component. The gelatin-chitosan self-assembled film is prepared according to the preparation example 1 of the gelatin-chitosan self-assembled film. The chitosan solution has a concentration of 1 g / L and is prepared by dispersing chitosan in acetic acid with a volume fraction of 1%. The pH is adjusted to 8.

[0067] Preparation example 8: The difference from the preparation example 1 is that the preparation method of the chitosan solution in step (4) is as follows: dissolve carbomer in ultrapure water to obtain a 3 wt% carbomer sol, add 1 kg of chitosan, stir uniformly, and adjust the pH to 8 with triethanolamine. The mass ratio of carbomer to chitosan is 3:1.

[0068] Preparation example 9: The difference from the preparation example 1 is that the preparation method of the chitosan solution in step (4) is as follows: dissolve carbomer in ultrapure water to obtain a 1 wt% carbomer sol, add 1 kg of chitosan, stir uniformly, and adjust the pH to 7 with triethanolamine. The mass ratio of carbomer to chitosan is 1:1.

[0069] Example

[0070] Example 1: An oral care solution, the amounts of raw materials of which are shown in Table 1. The humectant is xylitol, the flavor is lemon flavor, the suspending agent is polyvinylpyrrolidone, and the long-acting antibacterial component is prepared according to the preparation example 1 of the long-acting antibacterial component.

[0071] The preparation method of the above oral care solution comprises the following steps:

[0072] S1, mix the humectant, PEG-400, sodium hypochlorite, menthol, citric acid, and flavor to obtain component A;

[0073] S2, mix the purified water, mucin, and long-acting antibacterial component uniformly to obtain component B;

[0074] S3, mixing the A component and the B component uniformly, adjusting the pH value to 7, to prepare the oral care liquid.

[0075] Table 1: Raw material usage in the oral care liquid of Examples 1-5

[0076]

[0077]

[0078] Example 2: An oral care liquid, which is different from Example 1 in that the raw material usage is shown in Table 1, and the long-acting antibacterial component is made from the preparation example 2 of the long-acting antibacterial component.

[0079] Example 3: An oral care liquid, which is different from Example 1 in that the raw material usage is shown in Table 1.

[0080] Examples 4-5: An oral care liquid, which is different from Example 1 in that the raw material further includes the mussel myoglobin in the usage shown in Table 1, and the molecular weight of the mussel myoglobin is 100 KDa, and the mussel myoglobin is mixed uniformly with the A component and the B component to prepare the oral care liquid.

[0081] Example 6: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is made from the preparation example 3 of the long-acting antibacterial component.

[0082] Example 7: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is made from the preparation example 4 of the long-acting antibacterial component.

[0083] Example 8: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is made from the preparation example 5 of the long-acting antibacterial component.

[0084] Example 9: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is made from the preparation example 6 of the long-acting antibacterial component.

[0085] Example 10: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is made from the preparation example 7 of the long-acting antibacterial component.

[0086] Example 11: An oral care liquid, which is different from Example 5 in that the long-acting antibacterial component is made from the preparation example 8 of the long-acting antibacterial component.

[0087] Example 12: An oral care liquid, which is different from Example 5 in that the long-acting antibacterial component is made from the preparation example 9 of the long-acting antibacterial component.

[0088] Comparative Example

[0089] Comparative Example 1: An oral care liquid, which is different from Example 1 in that the long-acting antibacterial component is a silicone quaternary ammonium salt.

[0090] Comparative Example 2: An oral care liquid, which is different from Example 1 in that no suspending agent is added.

[0091] Comparative Example 3: An oral care liquid deionized water 100 parts, ethanol 5 parts, surfactant (see Table 1 for surfactant types) 0.2 parts, xylitol 0.3 parts, sorbitol 2 parts, plant extract 5 parts, magnesium lithium silicate 0.8 parts, berberine 0.12 parts. Ethanol, surfactant, xylitol, sorbitol, plant extract, magnesium lithium silicate, berberine are sequentially added to the deionized water and mixed uniformly to obtain the oral care liquid. The plant extract is prepared by the following method: gallnut, pomegranate peel, clove are mixed in a mass ratio of 2:3:5, crushed through a 60 mesh sieve to obtain plant raw materials; the plant raw materials are extracted with 40% ethanol aqueous solution (i.e. an ethanol aqueous solution with a volume fraction of ethanol of 40%) at a material to liquid mass ratio of 1:20 at a temperature of 25°C for 24 hours, filtered with 300 mesh filter cloth, the filtrate is centrifuged at 4000 rpm for 15 minutes, the supernatant is concentrated by rotary evaporation, the supernatant is concentrated to 10% of the original volume to obtain a concentrated solution, the concentrated solution is vacuum freeze-dried to obtain the product, the material thickness is controlled to be 6 mm, the pre-freezing temperature is set to -25°C, the sample temperature is maintained for 2 hours after the sample temperature drops to the set temperature, the sublimation temperature is set to 10°C, the desorption temperature is set to 35°C, the vacuum degree is 15 pa, and the drying time is 12 hours.

[0092] Performance detection test

[0093] I. The oral care liquid is prepared according to the method in the examples and comparative examples, and the performance of the oral care liquid is detected according to the following method, and the detection results are recorded in Table 2.

[0094] Bacteriostatic long-acting property detection: 150 patients with oral gingivitis were selected and randomly divided into 15 groups, 10 people in each group, and the oral care liquids prepared from Examples 1-12 and Comparative Examples 1-3 were used, with a use amount of 25 g each time. After using the oral care liquid, the oral flora (with Helicobacter pylori, Lactobacillus acidophilus, and Porphyromonas gingivalis as detection targets) was detected every 6 hours for a total of 12 hours.

[0095] Table 2

[0096]

[0097]

[0098] From the data in Examples 1-3 and Table 2, it can be seen that different amounts of raw materials were used in Examples 1-3, and the long-acting antibacterial components were prepared using the long-acting antibacterial component preparation example 1 and the long-acting antibacterial component preparation example 2, and thus the oral care liquid prepared using the long-acting antibacterial components has a high initial antibacterial rate, and still maintains a high antibacterial rate at 12 h. Taking Example 1 as an example, the decrease rate of the bacteriostatic rate of H. pylori at 12 h is (99.92-96.81) / 99.92=3.12%, and thus the oral care liquid has the advantages of long antibacterial duration and long-lasting bacteriostatic effect.

[0099] Compared with Example 1, the mussel myoglobin was further added to the oral care liquid in Example 4 and Example 5, and the initial antibacterial rate of the oral care liquid prepared in Example 4 and Example 5 does not change much compared with Example 1, but the bacteriostatic rates of H. pylori, L. acidophilus and P. gingivalis are still good after 6 h and 12 h, and the decrease rate of the bacteriostatic rate of H. pylori at 12 h relative to the initial time is (99.98-97.21) / 99.98=2.77%, and thus it can be seen that the mussel myoglobin improves the antibacterial durability of the oral care liquid.

[0100] The long-acting antibacterial component prepared in Example 6 uses the long-acting antibacterial component prepared in the long-acting antibacterial component preparation example 3, and the long-acting antibacterial component preparation example 3 does not add the organosilicon quaternary ammonium salt and does not dip the okra stock solution, and Table 2 shows that the oral care liquid prepared in Example 6 has a good initial bacteriostatic rate, but the bacteriostatic rate decreases significantly as time goes on, indicating that the antibacterial plant extract releases quickly and the antibacterial durability decreases.

[0101] The long-acting antibacterial component prepared in Example 7 uses the long-acting antibacterial component prepared in the long-acting antibacterial component preparation example 4, and the long-acting antibacterial component preparation example 4 does not add the organosilicon quaternary ammonium salt but dips the okra stock solution, and compared with Example 1, the initial antibacterial rate of the oral care liquid prepared in Example 7 decreases, but because the okra stock solution is used as a barrier layer, the long-acting antibacterial property is similar to that of Example 1, and taking H. pylori as an example, the decrease rate of the bacteriostatic rate at 12 h relative to the initial time is (98.35-95.25) / 98.35=3.15%.

[0102] The long-acting antibacterial component prepared in Example 8 uses the long-acting antibacterial component prepared in the long-acting antibacterial component preparation example 5, and the long-acting antibacterial component preparation example 5 does not dip the okra stock solution, and the self-assembled film is first dipped in the antibacterial solution and then dipped in the organosilicon quaternary ammonium salt solution, and compared with Example 1, the initial antibacterial rate increases, but the long-acting antibacterial property weakens, indicating that the organosilicon quaternary ammonium salt and the antibacterial plant extract produce antibacterial effect together at the initial time, but the antibacterial effect decreases as time goes on.

[0103] The long-acting antibacterial component prepared in Example 9 using the long-acting antibacterial component prepared in Preparation Example 6, wherein no antibacterial plant was added and only the self-assembled film was immersed in the silicone quaternary ammonium salt solution, has a good initial antibacterial rate, but the antibacterial rate decreases over time, indicating that the addition of the antibacterial plant extract and the immersion of the okra stock solution as the barrier layer can significantly improve the release time of the antibacterial plant extract and prolong the antibacterial durability.

[0104] Example 10 uses the long-acting antibacterial component prepared in Preparation Example 7 compared to Example 1, and the oral care solution prepared in Example 10 has a higher initial antibacterial rate, but the antibacterial rate decreases over time.

[0105] In Example 11 and Example 12, not only are the long-acting antibacterial components prepared in Preparation Example 8 and Preparation Example 9 used, respectively, but mussel mucin is also added. Compared to Example 5, the initial antibacterial rate of the oral care solution prepared in Example 11 and Example 12 does not change much, but the antibacterial rate of each type of bacteria is still high after 6h and 12h. Taking the antibacterial rate of Helicobacter pylori in Example 11 at 12h as an example, the decrease rate of the antibacterial rate is (99.99-98.28) / 99.99=1.7%, which shows that the antibacterial effect is more long-acting than that in Example 5.

[0106] Comparative Example 1 uses silicone quaternary ammonium salt as a long-acting antibacterial component compared to Example 1. Comparative Example 1 has a similar initial antibacterial rate to Example 1, but the antibacterial rate decreases significantly over time, indicating that the use of silicone quaternary ammonium salt as the only antibacterial component has little effect on improving the long-acting antibacterial effect of the oral care solution.

[0107] Comparative Example 2 does not add a suspending agent compared to Example 1, and Table 2 shows that the initial antibacterial effect of the oral care solution prepared in Comparative Example 2 is good, but the long-acting antibacterial effect decreases.

[0108] Comparative Example 3 is an oral care solution prepared by the prior art, which has a good initial antibacterial effect, but the antibacterial long-acting effect is not as good as the present application.

[0109] II. The oral care solution is prepared according to the methods in the examples and comparative examples, and the performance of the oral care solution is detected according to the following methods, and the detection results are recorded in Table 3.

[0110] Use effect detection: 150 patients with oral ulcer were selected, the symptoms were: multiple ulcer surfaces of different sizes appeared on the oral mucosa, the patients felt pain, which affected their diet and caused repeated attacks. The 150 patients were divided into 15 groups, 10 people in each group. The 15 groups of patients used the oral care liquids prepared by Examples 1-12 and Comparative Examples 1-3, respectively. The oral care liquids were used for gargling at 8 am, 12 pm and 6 pm every day, and the use was continued for 2 weeks. The use effect was counted. Recovery was defined as the symptoms disappearing, the ulcer surface healing, and the pain significantly reducing. Invalid was defined as the quality of the oral care liquid before and after use being obviously improved. The number of recovered, effective and invalid patients was counted.

[0111] Table 3

[0112] Item Number of Recovered Effective Number Invalid Number Example 1 10 4 1 Example 2 9 5 1 Example 3 10 4 1 Example 4 11 3 1 Example 5 12 2 1 Example 6 10 1 4 Example 7 9 3 3 Example 8 8 3 4 Example 9 9 3 3 Example 10 8 2 5 Example 11 13 1 1 Example 12 14 1 0 Comparative Example 1 3 4 8 Comparative Example 2 6 3 6 Comparative Example 3 5 5 5

[0113] As can be seen from Table 1, the number of recovered and effective patients in Examples 1-5 is large, and the number of invalid patients is small. The number of invalid patients in Examples 6-10 is increased, which indicates that the long-acting antibacterial component prepared by Preparation Example 1 and Preparation Example 2 of the present application can improve the bacteriostatic, anti-inflammatory and oral health protection effects of the oral care liquid. The oral care liquid prepared by Example 11 and Example 12 has good bacteriostatic and anti-inflammatory effects, and can quickly restore the oral mucosa. The oral care liquid prepared by Comparative Examples 1-3 has a lower oral protection effect than the present application.

[0114] The specific embodiments are only an explanation of the present application, and are not a limitation of the present application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the present specification, as long as the modifications are within the scope of the claims of the present application.

Claims

1. An oral care solution, characterized in that, The pH is 5-7, and the raw materials include the following parts by weight: 0.003-0.02 parts sodium hypochlorite, 1-5 parts humectant, 0.1-0.3 parts menthol, 0.1-0.5 parts PEG-400, 3-7 parts citric acid, 0.01-0.5 parts fragrance, 0.5-1 part suspending agent, 0.1-1 part long-lasting antibacterial component, and 80-90 parts purified water; The long-acting antibacterial component includes a gelatin-chitosan self-assembled membrane and an antibacterial agent loaded on the gelatin-chitosan self-assembled membrane; The antibacterial agent comprises antibacterial plant extracts and organosilicon quaternary ammonium salts, wherein the mass ratio of the gelatin-chitosan self-assembled membrane, the antibacterial plant extracts, and the organosilicon quaternary ammonium salts is 1:0.3-0.5:0.05-0.1; The preparation method of the long-acting antibacterial component includes the following steps: Antibacterial plant extracts and organosilicon quaternary ammonium salts were mixed with water to prepare antibacterial liquid and organosilicon quaternary ammonium salt solution, respectively. The gelatin-chitosan self-assembled membrane was immersed in an antibacterial solution for 1.5-2 hours, then removed, rinsed with deionized water, and dried to obtain a pretreated self-assembled membrane. The pretreated self-assembled membrane was circulated and impregnated in okra stock solution and dried to obtain an intermediate self-assembled membrane. The intermediate self-assembled membrane was sequentially immersed in organosilicon quaternary ammonium salt solution, deionized water and chitosan solution. This constitutes one cycle. After 10-15 cycles, the membrane was dried to obtain a long-lasting antibacterial component. The chitosan solution is prepared by dissolving carbomer in ultrapure water to obtain a carbomer sol with a concentration of 1-3 wt%, adding chitosan, stirring evenly, adjusting the pH to 7-8, and the mass ratio of carbomer to chitosan is 1-3:

1. The antibacterial plant extracts include dandelion extract, honeysuckle flower extract, and sage extract in a mass ratio of 0.3-0.7:0.1-0.4:

1. The method for preparing the gelatin-chitosan self-assembled membrane is as follows: Gelatin is dissolved in distilled water to make a gelatin solution, and chitosan is dissolved in acetic acid to make a chitosan solution. The glass slide was sequentially immersed in gelatin solution, deionized water and chitosan solution for 10-20 times, air-dried at room temperature, peeled and cut to obtain a gelatin-chitosan self-assembled membrane. The suspending agent is selected from at least one of polyvinylpyrrolidone, carbomer, sodium carboxymethyl cellulose, alginate, and xanthan gum.

2. The oral care solution according to claim 1, characterized in that, The humectant is selected from at least one of xylitol, sorbitol and lactitol.

3. The oral care solution according to claim 1, characterized in that, The oral care solution also includes 1-3 parts by weight of mussel adhesive protein.

4. The method for preparing the oral care solution according to any one of claims 1-3, characterized in that, Includes the following steps: Component A is prepared by mixing moisturizer, PEG-400, sodium hypochlorite, menthol, citric acid and fragrance; Component B is prepared by uniformly mixing purified water, suspending agent, and long-acting antibacterial component. Mix components A and B thoroughly and adjust the pH to 5-7 to obtain an oral care solution.

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