Multi-ion mixed solution, preparation method and application thereof, and oral care product containing multi-ion mixed solution
阅读说明：本技术 一种多离子混合液及其制备方法与应用、含有该多离子混合液的口腔护理产品 (Multi-ion mixed solution, preparation method and application thereof, and oral care product containing multi-ion mixed solution ) 是由 关晴光 肖丽娟 李明 邹萍 范玉奇 于 2021-10-19 设计创作，主要内容包括：本发明涉及一种多离子混合液及其制备方法与应用、含有该多离子混合液的口腔护理产品,属于口腔护理技术领域。为解决现有固体粉状钙－硅基生物活性材料有效成分释放缓慢、流动性差的问题,本发明提供了一种多离子混合液的制备方法,包括将各原料组分混匀后置于一定加热温度下熔化得到均一混合物,将其在原加热温度的状态下置于常温水中,均一混合物在水中骤冷发生炸裂,冷却后过滤收集滤液即为多离子混合液。本发明提供了一种液态钙－硅基生物活性材料,可作为防龋坏、再矿化、抗牙本质敏感的特效活性物广泛应用于各种口腔护理产品,能有效的辅助治疗各种牙龈炎、牙周炎、牙髓炎等症状,而且使用安全、无毒,具有广阔的应用前景。(The invention relates to a multi-ion mixed liquid, a preparation method and application thereof, and an oral care product containing the multi-ion mixed liquid, and belongs to the technical field of oral care. The invention provides a preparation method of a multi-ion mixed solution, aiming at solving the problems of slow release and poor fluidity of active ingredients of the existing solid powdery calcium-silicon-based bioactive material. The invention provides a liquid calcium-silicon-based bioactive material, which can be widely applied to various oral care products as a specific active matter for preventing caries, remineralizing and resisting dentin sensitivity, can effectively assist in treating various symptoms such as gingivitis, periodontitis, pulpitis and the like, is safe and nontoxic to use, and has wide application prospect.)
1. The preparation method of the multi-ion mixed liquid is characterized by weighing the following raw materials in parts by weight: SiO 2230-50 parts of CaO, 10-30 parts of K210-20 parts of O and P2O52-8 parts of a multi-ion mixed solution, uniformly mixing the raw material components, placing the mixture at a certain heating temperature to melt the mixture to obtain a uniform mixture, placing the uniform mixture in normal-temperature water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering, and collecting filtrate to obtain the multi-ion mixed solution.
2. The method for preparing the multi-ion mixed solution according to claim 1, wherein the heating temperature is 1300 to 1800 ℃; the melting time is 50-100 min.
3. The method of claim 1 or 2, wherein the water at normal temperature is used in an amount of 600 to 1000 parts by weight per 100 parts by weight of the raw material.
4. A polyion-mixed solution produced by the method for producing a polyion-mixed solution according to any one of claims 1 to 3.
5. Use of the polyion mixed solution of claim 4 in the preparation of an oral care product.
6. Use of the polyionic mixed solution of claim 5 in the preparation of an oral care product comprising a mouthwash, toothpaste, tooth gel, or tooth paste.
7. An oral care product containing the polyion mixed solution of claim 4, wherein the oral care product is a mouthwash, and the oral care product comprises the following components in parts by weight: 1-50 parts of multi-ion mixed liquid, 1-20 parts of solubilizer, 0.1-1 part of sweetening agent, 0.1-1 part of stabilizer, 0.1-1 part of aromatic and 27-97.7 parts of pure water.
8. An oral care product containing the polyion mixed solution of claim 4, wherein the oral care product is toothpaste and comprises the following components in parts by weight: 1-10 parts of multi-ion mixed liquid, 10-80 parts of first solvent, 5-25 parts of friction agent, 0.5-5 parts of foaming agent, 0.1-1 part of thickening agent and 0.1-1 part of coloring agent.
9. An oral care product containing the polyion mixed solution of claim 4, wherein the oral care product is a tooth gel, and the oral care product comprises the following components in parts by weight: 1-10 parts of multi-ion mixed liquid, 40-85 parts of second solvent, 5-15 parts of thickening agent, 0.5-2 parts of preservative and 1-2 parts of penetrating agent.
10. An oral care product containing the polyion mixed solution of claim 4, wherein the oral care product is a tooth paste, and is characterized by comprising the following components in parts by weight: 10-30 parts of multi-ion mixed liquid, 10-30 parts of third solvent, 20-50 parts of thickening agent and 20-30 parts of film forming agent.
Technical Field
The invention belongs to the technical field of oral care, and particularly relates to a multi-ion mixed liquid, a preparation method and application thereof, and an oral care product containing the multi-ion mixed liquid.
Background
Caries is progressive lesion of tooth hard tissue caused by the combined action of multiple factors in oral cavity, is represented by inorganic demineralization and organic matter decomposition, and has an evolution process from color change to substantial lesion along with the development of disease course. Small white spots on teeth are indicative of demineralization, also called decalcification. The reason is that the exposed enamel surface is stripped of calcium and phosphorus, the oral hygiene is poor, and dental plaque or bacteria can slowly erode the enamel when being gathered to generate acid, so that the color of teeth is changed to be white or yellowish.
Dentin hypersensitivity is a common oral disease with high adult oral morbidity as an oral common disease and a frequently encountered disease, and is also one of the common causes of clinical toothache. The theory of fluid is that after dentin is exposed, the fluid in the tubule of dentin, i.e. dentin fluid, has a mechanical response to external stimuli. Dentin fluid flows from inside to outside when subjected to cold stimulation and from outside to inside when subjected to heat stimulation. Dentinal cell membranes are sensitive to this fluid flow and sudden pressure changes, which in turn cause relaxation and compression of dentinal cells and processes, which can cause pain symptoms by conduction through the surrounding pulp nerve endings. Therefore, reducing the diameter of the dentinal tubules and sealing the openings of the dentinal tubules to reduce and avoid fluid flow within the dentin is the fundamental approach to treating dentinal hypersensitivity.
Because the gingival atrophy leads anaerobic bacteria to be bred and diffused under the gingiva and invade the health of the gingiva and the periodontal tissue for a long time, various gingivitis, periodontitis and pulpitis symptoms are caused, the health of the gingiva is further harmed, the gingival atrophy is degraded, and teeth are loosened and fall off and lost in advance.
The treatment of caries, dentin hypersensitivity, gingivitis, periodontitis and pulpitis is closely related to the repair material, and the requirements on the oral repair material are continuously improved along with the deep understanding of the generation, formation, structure and function relationship, tissue wound healing and structural change rule of oral tissues.
Since the introduction of the concept of "bioactivity", the use of calcium-silicon based bioactive materials in the treatment of oral diseases has played a great role. However, such inorganic bioactive materials are generally applied in the form of solid powder, and the disadvantages of poor fluidity and slow release of active ingredients are increasingly highlighted while the physical properties are hard, so that in terms of clinical treatment requirements, application materials with strong fluidity, rapid release and rapid effect are always desired to be found, and the advantages of the existing application technologies are complemented.
Disclosure of Invention
In order to solve the problems of slow release and poor fluidity of the active ingredients of the existing solid powdery calcium-silicon-based bioactive material, the invention provides a multi-ion mixed solution, a preparation method and application thereof, and an oral care product containing the multi-ion mixed solution.
The technical scheme of the invention is as follows:
a preparation method of a multi-ion mixed solution comprises the following raw materials in parts by weight: SiO 2230-50 parts of CaO, 10-30 parts of K210-20 parts of O and P2O52-8 parts of a multi-ion mixed solution, uniformly mixing the raw material components, placing the mixture at a certain heating temperature to melt the mixture to obtain a uniform mixture, placing the uniform mixture in normal-temperature water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering, and collecting filtrate to obtain the multi-ion mixed solution.
Further, the heating temperature is 1300-1800 ℃; the melting time is 50-100 min.
Further, the water at normal temperature is used in an amount of 600 to 1000 parts by weight per 100 parts by weight of the raw material.
The invention provides a multi-ion mixed liquid prepared by the preparation method of the multi-ion mixed liquid.
The invention provides an application of a multi-ion mixed solution in preparation of an oral care product.
Further, the oral care products include mouthwashes, toothpastes, tooth gels, tooth strips.
An oral care product containing the multi-ion mixed solution provided by the invention is a mouthwash, and comprises the following components in parts by weight: 1-50 parts of multi-ion mixed liquid, 1-20 parts of solubilizer, 0.1-1 part of sweetening agent, 0.1-1 part of stabilizer, 0.1-1 part of aromatic and 27-97.7 parts of pure water.
Further, the solubilizer is one or a combination of several of glycerol, propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600 or polyethylene glycol 1000; the stabilizer is one or the combination of two of sodium benzoate and citric acid; the sweetening agent is one or a combination of more of sorbitol, xylitol, sucrose, trichlorogalactose, saccharin sodium or aspartame; the aromatic is essence extracted from natural plants.
Further, the preparation method of the mouthwash is as follows: mixing solubilizer, polyion mixed solution and appropriate amount of pure water, stirring, adding sweetener, stabilizer and aromatic, stirring, adding the rest pure water, and stirring.
The oral care product containing the multi-ion mixed solution provided by the invention is toothpaste and comprises the following components in parts by weight: 1-10 parts of multi-ion mixed liquid, 10-80 parts of first solvent, 5-25 parts of friction agent, 0.5-5 parts of foaming agent, 0.1-1 part of thickening agent and 0.1-1 part of coloring agent.
Further, the first solvent is one or a combination of more of water, glycerol, propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600 or polyethylene glycol 1000; the solvent also acts as a humectant; the friction agent is one or a combination of more of calcium carbonate, calcium hydrophosphate, calcium pyrophosphate, tricalcium phosphate, silicon dioxide, aluminum silicate, aluminum hydroxide, alumina, zeolite, silicic acid or kaolin; the foaming agent is one or a combination of sodium dodecyl sulfate, sodium lauroyl sarcosinate or polyglycerol ester; the thickening agent is one or a combination of more of carbomer, xanthan gum, modified guar gum, carrageenan, methylcellulose, carboxymethyl cellulose, sodium carboxymethyl cellulose, hydroxyethyl cellulose or hydroxypropyl methyl cellulose; the colorant is non-nano titanium dioxide or natural pigment.
Further, the preparation method of the toothpaste comprises the following steps: weighing the raw materials according to a formula, adding a first solvent into a preparation tank, adding a thickening agent in a fractional manner, stirring and homogenizing, heating to a certain temperature of 40-60 ℃ while stirring, adding one third of a friction agent, fully stirring uniformly, sequentially adding a foaming agent, a coloring agent and a multi-ion mixed solution, adding the rest two thirds of the friction agent in a fractional manner after stirring uniformly, homogenizing, stopping heating, vacuumizing and stirring uniformly, degassing, standing and filling to obtain the composite material.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth gel and comprises the following components in parts by weight: 1-10 parts of multi-ion mixed liquid, 40-85 parts of second solvent, 5-15 parts of thickening agent, 0.5-2 parts of preservative and 1-2 parts of penetrating agent.
Further, the second solvent is one or a combination of several of glycerol, propylene glycol, ethanol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, or polyethylene glycol 1000, and in this embodiment, the solvent simultaneously functions as a humectant; the thickening agent is one or a combination of more of sodium carboxymethylcellulose, hydroxypropyl methylcellulose, polyvinylpyrrolidone, gelatin or carbomer; the preservative is one or a combination of more of parabens, benzoic acid, sodium benzoate, sorbic acid or benzalkonium bromide; the penetrant is one or more of azone, sialone, laurocapram, oleum Menthae Dementholatum, Borneolum Syntheticum, oleum Eucalypti or oleum Terebinthinae.
Further, the preparation method of the tooth gel comprises the following steps: adding the thickening agent into one third of the second solvent for pre-dispersion, and uniformly stirring to obtain a feed liquid A; adding the multi-ion mixed solution into two thirds of the second solvent, and stirring and fully dissolving to obtain a feed liquid B; transferring the material liquid B into the material liquid A, and stirring the material liquid B and the material liquid A uniformly; slowly adding antiseptic and penetrant into the mixed solution, vacuum stirring, degassing, standing, and packaging.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth paste and comprises the following components in parts by weight: 10-30 parts of multi-ion mixed liquid, 10-30 parts of third solvent, 20-50 parts of thickening agent and 20-30 parts of film forming agent.
Further, the third solvent is one or a combination of several of glycerin, propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, and polyethylene glycol 1000, and in this embodiment, the solvent simultaneously functions as a humectant; the thickening agent is one or a combination of more of sodium carboxymethylcellulose, hydroxypropyl methylcellulose, gelatin or carbomer; the film forming agent is one or a combination of polyvinyl alcohol, polyvinylpyrrolidone or acrylic resin.
Further, the preparation method of the tooth paste comprises the following steps: weighing the raw materials according to the formula of the tooth paste, adding a third solvent into a preparation tank, adding a thickening agent in several times, stirring and homogenizing, heating to 40-60 ℃ while stirring, sequentially adding a film-forming agent and a multi-ion mixed solution, homogenizing, stopping heating, vacuumizing and stirring to be uniform, and directly preparing the tooth paste from the obtained viscous colloid by continuous processes of coating, slitting, indentation, waste collection, cutting and the like.
The invention has the beneficial effects that:
the preparation method of the multi-ion mixed liquid provided by the invention can provide the liquid calcium-silicon-based bioactive material meeting the fluidity requirement, the multi-ion mixed liquid is rich in free calcium ions, phosphate ions and silicate ions, can provide a stable and sufficient ion reservoir for teeth, can form a calcium and phosphorus ion rich environment in a local oral environment, can improve the content of calcium and phosphorus in the enamel, inhibit enamel demineralization, improve enamel remineralization, change the acid-base property of the enamel surface and enhance the acid-resistant capability of the teeth.
The multi-ion mixed solution provided by the invention can be used as a specific active substance for preventing decayed teeth, remineralizing and resisting dentin sensitivity, can be widely applied to various oral care products such as toothpaste, mouthwash, tooth gel, tooth paste and the like, is safe and nontoxic to use, and has wide application prospect. The polyionic mixed solution can function to effectively remineralize enamel and/or dentin lesions, block exposed dentin and/or cementum tubules that mask sensitivity during use; repairing worn and/or eroded enamel surfaces; and enhancing the ability of contacting and adjacent tooth structures to resist acid erosion, anticaries, and dentinal hypersensitivity. The multi-ion mixed liquid can induce calcium and phosphorus to deposit on the surface of a bone, can promote calcium and phosphorus in saliva to attach on the surface of teeth, remineralize the surface of the teeth, change the acid-base property of the surface of enamel, enhance the acid-resistant capability of the teeth, obviously improve the density of remineralized dentin, strengthen the teeth, prevent looseness, effectively resist the stimulation of dental plaque, tartar and the like, and can effectively assist in treating various symptoms such as gingivitis, periodontitis, pulpitis and the like.
Drawings
FIG. 1 is a scanning electron micrograph of tubules of a test group treated with a multi-ionic liquid mixture prepared in example 4;
FIG. 2 is a scanning electron micrograph of a control tubule not treated with a multi-ion mixture;
FIG. 3 is a scanning electron micrograph of tubules of a test group after treatment with mouthwash prepared according to example 8;
FIG. 4 is a scanning electron micrograph of tubules of a control group not treated with mouthwash;
FIG. 5 is a scanning electron micrograph of tubules of a test group after treatment with the toothpaste prepared in example 11;
FIG. 6 is a scanning electron micrograph of tubules of a control group not treated with toothpaste;
FIG. 7 is a scanning electron micrograph of tubules of a test group after tooth gel treatment prepared in example 14;
FIG. 8 is a scanning electron micrograph of tubules of a control group not treated with tooth gel;
FIG. 9 is a scanning electron micrograph of tubules of a test group after treatment of a dental tape prepared in example 17;
FIG. 10 is a scanning electron micrograph of a control tubule without a tooth paste treatment.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2230 portions of CaO, 10 portions of CaO and K2O10 parts and P2O52 parts by weight of raw materials are evenly mixed and then are placed at 1300 ℃ for melting for 100min to obtain a uniform mixture, and the ratio of 600 parts by weight of water to 100 parts by weight of raw materialsFor example, preparing normal temperature pure water, placing the obtained homogeneous mixture in normal temperature pure water at the original heating temperature, quenching the homogeneous mixture in water to crack, cooling, filtering, and collecting filtrate to obtain the polyion mixed solution.
Example 2
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2235 parts of CaO15 parts of K2O12 parts and P2O53 parts, uniformly mixing all the raw material components, placing the mixture at the heating temperature of 1400 ℃ for melting for 90min to obtain a uniform mixture, preparing normal-temperature pure water according to the proportion that 700 parts by weight of water is used for every 100 parts by weight of raw materials, placing the obtained uniform mixture in the normal-temperature pure water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering and collecting filtrate to obtain the multi-ion mixed solution.
Example 3
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2240 parts of CaO, 20 parts of CaO and K2O15 parts and P2O54 parts, uniformly mixing all the raw material components, placing the mixture at the heating temperature of 1500 ℃ for melting for 80min to obtain a uniform mixture, preparing normal-temperature pure water according to the proportion that 800 parts by weight of water is used for every 100 parts by weight of raw materials, placing the obtained uniform mixture in the normal-temperature pure water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering and collecting filtrate to obtain the multi-ion mixed solution.
Example 4
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2245 parts of CaO, 25 parts of CaO and K2O16 parts and P2O55 parts by weight, uniformly mixing the raw material components, placing the mixture at 1600 ℃ for melting for 70min to obtain a uniform mixture, preparing normal-temperature pure water according to the proportion that 900 parts by weight of water is used for each 100 parts by weight of raw material, placing the uniform mixture in the normal-temperature pure water at the original heating temperature, and quenching the uniform mixture in the water for fryingCracking, cooling, filtering and collecting filtrate to obtain the multi-ion mixed liquor.
Example 5
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2248 parts of CaO, 28 parts of CaO and K2O18 parts and P2O56 parts, uniformly mixing the raw material components, placing the mixture at the heating temperature of 1700 ℃ for melting for 60min to obtain a uniform mixture, preparing normal-temperature pure water according to the proportion that 1000 parts by weight of water is used for each 100 parts by weight of raw material, placing the obtained uniform mixture in the normal-temperature pure water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering and collecting filtrate to obtain the multi-ion mixed solution.
Example 6
The embodiment provides a preparation method of a multi-ion mixed solution, which specifically comprises the following raw materials in parts by weight: SiO 2250 parts of CaO, 30 parts of CaO and K2O20 parts and P2O58 parts, uniformly mixing all the raw material components, placing the mixture at a heating temperature of 1800 ℃ for melting for 50min to obtain a uniform mixture, preparing normal-temperature pure water according to the proportion that 800 parts by weight of water is used for every 100 parts by weight of raw materials, placing the obtained uniform mixture in the normal-temperature pure water at the original heating temperature, quenching the uniform mixture in the water to crack, cooling, filtering and collecting filtrate to obtain the multi-ion mixed solution.
The multi-ion mixed liquid prepared in the embodiments 1 to 6 of the present invention is rich in free calcium ions, phosphate ions and silicate ions, and can provide a stable and sufficient ion reservoir for teeth, form an environment rich in calcium and phosphorus ions in a local oral environment, increase calcium and phosphorus contents in enamel, inhibit enamel demineralization, improve enamel remineralization, change the acid-base property of enamel surface, and enhance the acid-resistant ability of teeth.
Silicate ions can induce calcium and phosphorus to deposit on the surface of the bone in a physiological environment, can promote calcium and phosphorus in saliva to be attached to the surface of teeth, is beneficial to the continuous maturation of enamel after the teeth sprout and the recovery of apatite damaged at the lesion part of the decayed teeth, promotes the remineralization of decayed teeth, obviously improves the density of remineralized dentin, remineralizes softened dentin, recovers the original functions of the softened dentin and achieves the aim of treating the decayed teeth.
Calcium ions and phosphate ions can perform a coagulation reaction on the surface of dentin and around dentin tubules, the generated apatite sediment is relatively stable and insoluble and cannot be washed away by saliva or acid soft drinks, and the apatite sediment is finally converted into hydroxyapatite in the dentin tubules, so that the dentin tubules are deposited and blocked, the dental pulp is prevented from being stimulated by foreign substances, and the dentin hypersensitivity is improved.
The multi-ion mixed liquid prepared in the embodiments 1 to 6 of the invention can be used as a specific active substance for preventing caries, remineralization and dentin sensitivity, can be widely applied to various oral care products such as toothpaste, mouthwash, tooth gel, tooth paste and the like, and has safe use, no toxicity and wide application prospect.
Example 7
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a mouthwash having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
An oral care product containing the multi-ion mixed solution provided by the invention is a mouthwash, and comprises the following components in parts by weight: 1 part of multi-ion mixed liquid, 1 part of glycerol, 0.1 part of sorbitol, 0.1 part of sodium benzoate, 0.1 part of mint essence and 97.7 parts of pure water.
In this embodiment, the glycerin may be replaced with one or more of propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, and polyethylene glycol 1000.
Sodium benzoate may be replaced with citric acid or a combination of both in this example.
In the embodiment, the sorbitol can be replaced by one or a combination of more of xylitol, sucrose, trichlorogalactose, saccharin sodium or aspartame.
In the embodiment, the mint essence can be replaced by other common natural plant extracts in the market.
The preparation method of the mouthwash in this example is as follows: mixing glycerol, polyion mixed solution and appropriate amount of pure water, stirring, adding sorbitol, sodium benzoate and herba Menthae essence, stirring, adding the rest pure water, and stirring.
Example 8
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a mouthwash having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
An oral care product containing the multi-ion mixed solution provided by the invention is a mouthwash, and comprises the following components in parts by weight: 30 parts of multi-ion mixed liquid, 10 parts of propylene glycol, 0.5 part of xylitol, 0.5 part of citric acid, 0.5 part of green tea essence and 58.5 parts of pure water.
The preparation method of the mouthwash in this example is as follows: mixing propylene glycol, multi-ion mixed solution and appropriate amount of pure water, stirring, adding xylitol, citric acid and green tea essence, stirring, adding the rest pure water, and stirring.
Example 9
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a mouthwash having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
An oral care product containing the multi-ion mixed solution provided by the invention is a mouthwash, and comprises the following components in parts by weight: 50 parts of multi-ion mixed liquid, 20 parts of sorbitol, 1 part of aspartame, 1 part of citric acid, 1 part of apple essence and 27 parts of pure water.
The preparation method of the mouthwash in this example is as follows: mixing sorbitol, polyion mixed solution and appropriate amount of pure water, stirring, adding aspartame, citric acid and apple essence, stirring, adding the rest pure water, and stirring.
Example 10
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a toothpaste having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is toothpaste and comprises the following components in parts by weight: 1 part of polyion mixed liquid, 10 parts of water, 5 parts of calcium carbonate, 0.5 part of sodium dodecyl sulfate, 0.1 part of carbomer and 0.1 part of non-nanoscale titanium dioxide.
In this embodiment, the first solvent also functions as a humectant, and the water may be replaced by one or a combination of more of glycerin, propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, or polyethylene glycol 1000.
In this embodiment, the calcium carbonate can be replaced by one or more of calcium hydrogen phosphate, calcium pyrophosphate, tricalcium phosphate, silicon dioxide, aluminum silicate, aluminum hydroxide, alumina, zeolite, silicic acid, or kaolin.
In this embodiment, sodium lauryl sulfate may be replaced by one or more of sodium lauroyl sarcosinate or polyglycerol ester.
In the embodiment, the carbomer can be replaced by one or a combination of more of xanthan gum, modified guar gum, carrageenan, methylcellulose, carboxymethyl cellulose, sodium carboxymethyl cellulose, hydroxyethyl cellulose or hydroxypropyl methyl cellulose.
The non-nanoscale titanium dioxide in this embodiment can be replaced by commercially available natural pigments.
The preparation method of the toothpaste of the embodiment is as follows: weighing the raw materials according to a formula, adding water into a preparation tank, adding carbomer in portions, stirring and homogenizing, heating to a certain temperature of 50 ℃ while stirring, adding one third of calcium carbonate, fully and uniformly stirring, sequentially adding sodium dodecyl sulfate, non-nanoscale titanium dioxide and multi-ion mixed liquid, adding the rest two thirds of calcium carbonate in portions after uniformly stirring, homogenizing, stopping heating, vacuumizing and stirring uniformly, degassing, standing and filling to obtain the calcium carbonate.
Example 11
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a toothpaste having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is toothpaste and comprises the following components in parts by weight: 5 parts of multi-ion mixed liquid, 50 parts of propylene glycol, 15 parts of calcium hydrophosphate, 3 parts of sodium lauroyl sarcosinate, 0.5 part of xanthan gum and 0.5 part of non-nano titanium dioxide.
The preparation method of the toothpaste of the embodiment is as follows: weighing the raw materials according to a formula, adding propylene glycol into a preparation tank, adding xanthan gum in a fractional manner, stirring and homogenizing, heating to a certain temperature of 40 ℃ while stirring, adding one third of calcium hydrophosphate, fully and uniformly stirring, then sequentially adding sodium lauroyl sarcosinate, non-nanoscale titanium dioxide and multi-ion mixed liquid, adding the rest two thirds of calcium hydrophosphate in a fractional manner after uniformly stirring, homogenizing, stopping heating, vacuumizing and stirring uniformly, degassing, standing and filling to obtain the product.
Example 12
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a toothpaste having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is toothpaste and comprises the following components in parts by weight: 10 parts of multi-ion mixed liquid, 80 parts of sorbitol, 25 parts of silicon dioxide, 5 parts of polyglycerol ester, 1 part of carrageenan and 1 part of non-nano titanium dioxide.
The preparation method of the toothpaste of the embodiment is as follows: weighing the raw materials according to a formula, adding sorbitol into a preparation tank, adding carat in portions, stirring and homogenizing, heating to a certain temperature of 60 ℃ while stirring, adding one third of silicon dioxide, fully and uniformly stirring, sequentially adding polyglycerol ester, non-nanoscale titanium dioxide and multi-ion mixed liquid, adding the rest two thirds of silicon dioxide in portions after uniformly stirring, homogenizing, stopping heating, vacuumizing and stirring uniformly, degassing, standing and filling to obtain the product.
Example 13
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a tooth gel having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth gel and comprises the following components in parts by weight: 1 part of multi-ion mixed solution, 40 parts of glycerol, 5 parts of sodium carboxymethyl cellulose, 0.5 part of parabens and 1 part of azone.
In this embodiment, the second solvent simultaneously functions as a humectant, and the glycerin may be replaced with one or a combination of more of propylene glycol, ethanol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, or polyethylene glycol 1000.
In this embodiment, one or more of sodium carboxymethylcellulose, hydroxypropylmethylcellulose, polyvinylpyrrolidone, gelatin, and carbomer may be used.
In this embodiment, one or more of parabens, benzoic acid, sodium benzoate, sorbic acid, and benzalkonium bromide are used in combination.
In this embodiment, azone may be replaced by one or more of sialone, laurocapram, peppermint oil, borneol, eucalyptus oil, and turpentine.
The preparation method of the tooth gel of this example is as follows: putting sodium carboxymethylcellulose into one third of glycerol for pre-dispersion, and stirring uniformly to obtain feed liquid A; adding the multi-ion mixed solution into two thirds of glycerol, and stirring and fully dissolving to obtain feed liquid B; transferring the material liquid B into the material liquid A, and stirring the material liquid B and the material liquid A uniformly; slowly adding the parabens and azone into the mixed solution, stirring uniformly in vacuum, degassing, standing and filling to obtain the product.
Example 14
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a tooth gel having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth gel and comprises the following components in parts by weight: 5 parts of multi-ion mixed liquid, 50 parts of propylene glycol, 10 parts of hydroxypropyl methyl cellulose, 1 part of benzoic acid and 1.5 parts of peppermint oil.
The preparation method of the tooth gel of this example is as follows: putting hydroxypropyl methyl fiber into one third of propylene glycol for pre-dispersion, and uniformly stirring to obtain feed liquid A; adding the multi-ion mixed solution into one third of dipropylene glycol, and stirring and fully dissolving to obtain a feed liquid B; transferring the material liquid B into the material liquid A, and stirring the material liquid B and the material liquid A uniformly; slowly adding benzoic acid and oleum Menthae Dementholatum into the mixed solution, vacuum stirring, degassing, standing, and packaging.
Example 15
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin hypersensitivity, and a tooth gel having the efficacy of preventing caries, remineralization and dentin hypersensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth gel and comprises the following components in parts by weight: 10 parts of polyion mixed liquid, 85 parts of ethanol, 15 parts of polyvinylpyrrolidone, 2 parts of sodium benzoate and 2 parts of borneol.
The preparation method of the tooth gel of this example is as follows: putting polyvinylpyrrolidone into one third of ethanol for pre-dispersion, and uniformly stirring to obtain feed liquid A; adding the multi-ion mixed solution into two thirds of ethanol, and stirring and fully dissolving to obtain feed liquid B; transferring the material liquid B into the material liquid A, and stirring the material liquid B and the material liquid A uniformly; slowly adding sodium benzoate and Borneolum Syntheticum into the mixed solution, vacuum stirring, degassing, standing, and packaging.
Example 16
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin sensitivity, and a dental patch having the efficacy of preventing caries, remineralization and dentin sensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth paste and comprises the following components in parts by weight: 10 parts of polyion mixed solution, 10 parts of glycerol, 20 parts of sodium carboxymethylcellulose and 20 parts of polyvinyl alcohol.
In this embodiment, the second solvent simultaneously functions as a humectant, and the glycerin may be replaced with one or a combination of more of propylene glycol, sorbitol, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, polyethylene glycol 600, or polyethylene glycol 1000.
In the embodiment, one or more of sodium carboxymethylcellulose, hydroxypropyl methylcellulose, gelatin and carbomer are combined;
in this embodiment, the polyvinyl alcohol may be replaced by one or a combination of several of polyvinylpyrrolidone and acrylic resin.
The preparation method of the tooth paste of the embodiment is as follows: weighing the raw materials according to the formula of the tooth paste, adding glycerol into a preparation tank, adding sodium carboxymethylcellulose in several times, stirring and homogenizing, heating to 40 ℃ while stirring, sequentially adding polyvinyl alcohol and polyion mixed liquid, homogenizing, stopping heating, vacuumizing and stirring to be uniform, and directly preparing the tooth paste from the obtained viscous colloid by continuous processes of coating, slitting, indentation, waste recycling, cutting and the like.
Example 17
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin sensitivity, and a dental patch having the efficacy of preventing caries, remineralization and dentin sensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth paste and comprises the following components in parts by weight: 20 parts of multi-ion mixed liquid, 20 parts of propylene glycol, 30 parts of hydroxypropyl methylcellulose and 25 parts of polyvinylpyrrolidone.
The preparation method of the tooth paste of the embodiment is as follows: weighing the raw materials according to the formula of the tooth paste, adding propylene glycol into a preparation tank, adding hydroxypropyl methylcellulose in several times, stirring and homogenizing, heating to 50 ℃ while stirring, sequentially adding polyvinylpyrrolidone and multi-ion mixed liquid, homogenizing, stopping heating, vacuumizing and stirring to be uniform, and directly preparing the tooth paste from the obtained viscous colloid by continuous processes of coating, slitting, indentation, waste collection, cutting and the like.
Example 18
In this embodiment, the multi-ion mixed solution prepared by the preparation method of example 4 is added to an oral care product as a specific active substance for preventing caries, remineralization and dentin sensitivity, and a dental patch having the efficacy of preventing caries, remineralization and dentin sensitivity is provided.
The oral care product containing the multi-ion mixed solution provided by the invention is a tooth paste and comprises the following components in parts by weight: 30 parts of multi-ion mixed liquid, 30 parts of sorbitol, 50 parts of gelatin and 30 parts of acrylic resin.
The preparation method of the tooth paste of the embodiment is as follows: weighing the raw materials according to the formula of the tooth paste, adding sorbitol into a preparation tank, adding gelatin in several times, stirring and homogenizing, heating to 60 ℃ while stirring, sequentially adding acrylic resin and multi-ion mixed liquid, homogenizing, stopping heating, vacuumizing and stirring to be uniform, and directly preparing the tooth paste from the obtained viscous colloid by continuous processes of coating, slitting, indentation, waste collection, cutting and the like.
The multi-ion mixed solution has the effects of preventing caries, remineralizing and resisting dentin sensitivity and is proved by experiments:
the important function of the dentin tubule blocking type dental material is to partially or completely block open dentin tubules, thereby achieving the effect of reducing tooth sensitivity. Dentinal hypersensitivity is a condition of transient, sharp pain that occurs when exposed dentin is subjected to stimuli such as temperature, mechanical or chemical stimuli. The opening of the dentinal tubules at the exposed dentinal surface is a critical factor in dentinal sensitivity, and a more direct cause is dentinal permeability at the exposed site. According to the well-accepted hydrodynamics for explaining dentin hypersensitivity, external factors stimulate exposed dentin to cause non-directional flow of dentinal tubule fluid, mechanically agitate the contents of the pulp, indirectly excite free nerve endings, and produce pain sensation. According to this theory, it has been shown that reducing the permeability of dentin is effective in relieving dentin hypersensitivity, and sealing or occluding dentinal tubules is a direct means of reducing dentin permeability. Thus, evaluation of the dentinal tubule blocking effect allows indirect evaluation of its tooth desensitizing effect.
Dentinal tubule clogging rate test method (scanning electron microscope observation method)
The principle is as follows: and observing and recording the number of unblocked dentinal tubules of the dentin sheet after the dentin sheet is treated by the test sample by adopting a scanning electron microscope, simultaneously recording the number of the open dentinal tubules of the mouth of the dentin sheet of the control group, and obtaining the blockage rate of the dentinal tubules by calculating, thereby evaluating the effect of the sample on the blockage of the dentinal tubules.
Preparation of human dentin tablets: fresh extracted carious molars (preferably third molars from 16-40 years old, if possible) are selected, the tartar and attached soft tissue are removed with a hand-held instrument, soaked in 70% ethanol for at least 15min or left in 0.5% chloramine T solution for up to 1 week, then stored in distilled water and left at 4 ℃ for no more than 1 month. Cutting dentin sheets with thickness of (0.5 + -0.05) mm at the widest part of the dental crown, below occlusal enamel and above occlusal boundary of dental pulp cavity at an angle perpendicular to the long axis of the tooth under water cooling with a low-speed cutter. In order to ensure as uniform a permeability of the dentin lamellae as possible, the acquisition positions of the dentin lamellae should be as uniform as possible, so that usually only one dentin lamella can be acquired per individual tooth.
Each piece of the obtained human dentin sheet was cut symmetrically into two halves, one of which was used as a test group and the other was used as a control group. The test pieces of the test group and the control group of each parallel test are all from the same dentin sheet.
The test procedure was as follows:
(1) processing of dentin sheets: all test and control dentin sheets were double-side acid-etched with 35% (w/w) phosphoric acid solution for 30s to remove the staining layer, rinsed with deionized water, and ultrasonically cleaned in deionized water for 5 min.
(2) Use of the sample: the distal medullary surface of the test group dentin discs was treated with the test samples in a manner simulating the operation in actual use. The test samples in this experiment were the multi-ion mixture prepared in example 4, the mouthwash provided in example 8, the toothpaste provided in example 11, the tooth gel provided in example 14, and the tooth paste provided in example 17; wherein the test groups are respectively soaked in the multi-example mixed liquor for 21min, the use condition of the test groups in 7 days is simulated, and the test groups are washed and dried by clear water; soaking in mouthwash for 90min, simulating the use condition for 30 days, washing with clear water, and drying; tooth brushing of the toothpaste is carried out for 90 minutes, the use condition of the toothpaste is simulated for 30 days, and then the toothpaste is washed and dried by clear water; the tooth gel is applied to gingival margin for 60 min; the tooth paste is adhered on the surface of the tooth for 39 min; the control group was a blank control without treatment of the test sample.
(3) And (3) observing by a scanning electron microscope: after the test group dentin strips and the control group dentin strips were sufficiently dried, the blockage of dentinal tubules of the test group dentin strips and the control group dentin strips were observed under a scanning electron microscope (1000 times or 1500 times), respectively. When observing, the selected positions of the dentin sheets of the test group and the control group are symmetrical areas.
As can be seen from the comparison of the pictures in figures 1-10, the multi-ion solution provided by the invention, the mouthwash, the toothpaste, the tooth gel and the tooth paste containing the multi-ion solution can block the dentinal tubules on the dentin sheet, and the existing standard considers that the blockage rate of the dentinal tubules reaches more than 70 percent, namely the dentinal sheet has desensitization effect; the blockage rate of dentinal tubules of the product provided by the invention can reach more than 90%, and the desensitization effect is obvious. This shows that the polyion mixed liquor provided by the invention can effectively block and shield dentin and/or dentin tubules causing sensitive exposure, and plays a role in resisting dentin sensitivity.
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