Double-tube toothpaste and preparation method thereof

Abstract

The invention discloses double-tube toothpaste and a preparation method thereof, the double-tube toothpaste comprises calcium salt-containing toothpaste and fluorine-containing toothpaste which are separately stored, the calcium salt-containing toothpaste comprises a calcium salt abrasive, the fluorine-containing toothpaste comprises an anti-caries agent, and the anti-caries agent comprises fluoride. According to the application, the fluorine-calcium compatible double-effect repairing toothpaste can be provided.

Description

Technical Field

[0001] The present application relates to the technical field of daily chemical product production, and particularly to a dual-tube toothpaste and a preparation method thereof. Background Art

[0002] Toothpaste is an indispensable product in daily oral care, and is widely used for cleaning teeth, preventing dental caries, freshening breath, etc. With the continuous improvement of consumers' attention to oral health, various functional toothpaste products have emerged in the market, such as anti-sensitivity toothpaste, whitening toothpaste, antibacterial toothpaste, etc.

[0003] However, traditional toothpaste has certain limitations in formula design. It usually contains a single formula designed to meet specific oral care needs, and it is difficult to meet multiple functional requirements simultaneously. Moreover, it may be difficult for different components to be compatible and interact with each other. For example, some enzymes may be inactivated after being mixed with acidic components, resulting in loss of function. For example, fluoride may form insoluble complexes after being mixed with certain minerals (such as calcium salts), reducing the bioavailability of fluoride. In addition, with the accelerating pace of life, users often rush through the brushing process, resulting in too short brushing time and poor effect. Especially in the morning brushing, due to the tight pace of life, users tend to shorten the brushing time. However, after a night's sleep, bacteria in the oral cavity use the sugar in food residues to reproduce, leading to rapid growth of dental plaque. The saliva secretion decreases during sleep, and the self-regulating ability of the oral cavity weakens. The activities of bacteria in the oral cavity are very active, resulting in a more acidic oral environment, increasing the risk of dental caries and gum diseases. If the brushing time or effect is insufficient, in the long run, it will not only increase the incidence of dental caries, but also cause serious oral diseases such as gingivitis and periodontitis.

[0004] Therefore, there is an urgent need for a toothpaste with good fluoride-calcium compatibility and dual-effect repair. Summary of the Invention

[0005] To overcome the deficiencies of the prior art and solve the problems of general efficacy and poor fluoride-calcium compatibility in the existing toothpaste, the present application provides a dual-tube toothpaste and a preparation method thereof. The present application adopts the following technical solutions:

[0006] In the first aspect of the present application, a dual-tube toothpaste is disclosed, which includes a calcium salt-containing toothpaste and a fluoride-containing toothpaste stored separately and isolated from each other. The calcium salt-containing toothpaste includes a calcium salt abrasive, and the fluoride-containing toothpaste includes an anti-caries agent, and the anti-caries agent includes fluoride.

[0007] It should be noted that a double-tube toothpaste is a product containing two independent chambers for storing toothpastes of different formulas. When the user squeezes the toothpaste tube, the two toothpastes of different formulas will be squeezed out together. The double-tube toothpaste of the present application can effectively avoid the reduction of the bioavailability of fluoride and calcium salt abrasives caused by the combination of fluoride and calcium salt abrasives to form an insoluble complex by isolating the calcium salt abrasives in the calcium salt toothpaste and the fluoride in the fluoride toothpaste, thereby having good friction cleaning power and anti-caries function at the same time, thereby providing a toothpaste with good fluoride-calcium compatibility and dual-effect repair.

[0008] In one implementation of the present application, the fluoride-containing toothpaste includes a non-calcium salt abrasive, and the non-calcium salt abrasive includes silicon dioxide; the fluoride includes at least one of sodium monofluorophosphate, sodium fluoride, olafluor and stannous fluoride.

[0009] It should be noted that fluoride toothpaste can provide moderate friction cleaning power and enhance cleaning; fluoride can react with OH in hydroxyapatite in tooth enamel. - It is replaced by fluoroapatite with lower solubility and recrystallized on the apatite surface in the enamel. Fluoride can also promote the adhesion of calcium and phosphorus in saliva to the tooth surface, which helps to restore the damaged hydroxyapatite in the caries lesion site, thereby preventing caries and promoting the remineralization of enamel.

[0010] In one implementation of the present application, the calcium salt friction agent includes anhydrous calcium hydrogen phosphate and dihydrated calcium hydrogen phosphate.

[0011] It should be noted that calcium salt toothpaste uses dihydrated calcium phosphate (RDA40) and anhydrous calcium phosphate (RDA>100) as abrasives, which can achieve low friction and high cleaning, and help to quickly clean dental plaque. Dihydrated calcium phosphate is slightly soluble in water (the solubility product Ksp at room temperature is about 0.27×10 8 ), can provide a calcium source, and fluorine synergistic mineralization. In addition, the calcium-phosphate system has good rheological properties, which can match the rheological requirements of double-tube toothpaste extrusion and is easier to extrude.

[0012] In one implementation of the present application, the calcium salt-containing toothpaste includes calcium glycerophosphate.

[0013] It should be noted that calcium glycerophosphate can increase the calcium and phosphorus content in tooth enamel, inhibit the demineralization of tooth enamel, enhance the remineralization of tooth enamel, change the acidity and alkalinity of the tooth enamel surface, and enhance the acid resistance of tooth enamel. In addition, calcium glycerophosphate can improve the absorption of fluoride. By adding an appropriate amount of calcium glycerophosphate to toothpaste, the absorption rate of fluoride by tooth enamel can be increased, and the fluoridation effect of strengthening the anti-demineralization of tooth enamel can be enhanced. Calcium glycerophosphate also has certain antibacterial activity and can inhibit the growth of some harmful bacteria in the oral cavity, especially the bacteria related to dental plaque and dental caries formation. Specifically, calcium glycerophosphate can maintain the pH of the oral cavity in a relatively neutral range, improve the acidic environment of the oral cavity, and reduce the damage of acid to tooth enamel. In addition, the calcium and phosphorus rich in calcium glycerophosphate can promote the remineralization of the tooth surface, repair early minor damages, and enhance the anti-caries ability of teeth. Calcium glycerophosphate can also act synergistically with fluoride to further improve the remineralization effect of teeth. Fluoride can combine with calcium and phosphorus ions to form more stable fluorapatite, which is more acid-resistant than hydroxyapatite and can better resist the occurrence of dental caries. Calcium glycerophosphate can combine with calcium salts in saliva to prevent them from depositing on the tooth surface, thereby reducing the formation of dental calculus. Calcium glycerophosphate can change the chemical properties of the tooth surface, reduce the adhesion of bacteria on it, and thus reduce the formation of dental plaque and dental calculus.

[0014] In summary, through calcium hydrogen phosphate dihydrate, calcium glycerophosphate and fluoride, the fluorine-calcium synergistic mineralization is achieved, playing a role in preventing caries and repairing.

[0015] In one implementation manner of the present application, the calcium salt-containing toothpaste or the fluoride-containing toothpaste further includes at least one of the following: freshener, gum protector, whitening agent, thickener, humectant, foaming agent, preservative, fragrance, sweetener, pearlescent agent, pigment; the freshener includes zinc citrate and zinc glycinate, the gum protector includes at least one of dipotassium glycyrrhizinate and allantoin, the whitening agent includes at least one of tetrasodium pyrophosphate, sodium hexametaphosphate and sodium tripolyphosphate, the thickener includes at least one of cellulose gum, xanthan gum, microcrystalline cellulose and chondrus crispus, and the humectant includes at least one of glycerol, sorbitol and polyethylene glycol.

[0016] It should be noted that the amino and carboxyl groups in zinc glycinate can combine with ammonia, acid, aldehyde and other odor molecules to achieve the deodorization effect. The activated zinc atoms can form chemical bonds with nitrogen and sulfur atoms in the odor, thus contributing to the complete elimination of odor. In addition, zinc ions can inhibit the growth of oral pathogens and reduce the generation of unpleasant gases. Zinc citrate has a very low solubility and can remain in the sewer, dental plaque, dental calculus and places inaccessible to the toothbrush after brushing. It slowly dissolves in saliva, gradually releases zinc ions and plays a lasting role in preventing the formation of dental calculus. In addition, zinc ions achieve the purpose of antibacterial and bactericidal effects by destroying the cell membrane function, denaturing bacterial proteins or enzymes, and destroying the cell division and reproduction ability, thereby inhibiting dental plaque. In summary, with the double zinc support of zinc glycinate and zinc citrate, it can play an immediate refreshing and long-lasting antibacterial role.

[0017] It should also be noted that dipotassium glycyrrhizinate can regulate the excitability of cholinergic nerves, resulting in reduced permeability of capillary walls and cell membranes, reduced inflammatory exudation, and inhibition of the formation and release of histamine and other toxic substances, thus achieving a good anti-inflammatory effect and relieving gum problems such as gum bleeding. Zinc ions can inhibit dental plaque, inhibit the development of dental calculus, especially the erosion of dental calculus on gum tissue at present; inhibit the growth of periodontitis pathogenic bacteria (such as Porphyromonas gingivalis, Fusobacterium nucleatum and Prevotella intermedia), reduce the production of toxic substances, and relieve gum and periodontal problems. In summary, double zinc and dipotassium glycyrrhizinate can synergistically enhance the effect and better relieve gum problems.

[0018] It should also be noted that allantoin has anti-inflammatory properties and can reduce the inflammatory response in gum tissue. It reduces symptoms such as gum swelling and bleeding by inhibiting the release of inflammatory mediators. It can also reduce the irritation of the oral mucosa, relieve pain and discomfort. For patients with oral ulcers and oral inflammation, allantoin can effectively shorten the healing time and relieve symptoms. Allantoin can also act synergistically with other components. For example, allantoin can promote the deposition of fluoride on the tooth surface, enhancing the acid resistance and caries resistance of teeth.

[0019] It should also be noted that using sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate as whitening agents can compete for pigment sites and enhance cleaning. Specifically, sodium tripolyphosphate can chelate metal ions such as calcium, iron and copper, reducing the deposition of these metal ions on the tooth surface, thereby inhibiting the attachment of pigments and proteins. By binding to minerals such as calcium and magnesium in saliva, sodium tripolyphosphate can also prevent the deposition and mineralization of these minerals in dental calculus, thus delaying the formation of dental calculus. Without the presence of dental calculus, pigment molecules lose an important attachment platform, reducing the possibility of tooth discoloration. In addition, sodium tripolyphosphate can act synergistically with other toothpaste ingredients to enhance the overall cleaning effect of the toothpaste. For example, it can help the abrasive better adhere to the tooth surface and improve its ability to remove dirt and pigments. Sodium pyrophosphate and sodium hexametaphosphate can inhibit the formation of calcium phosphate deposits and are effective anti-calculus agents, which can reduce dental calculus and exogenous pigments penetrating into dental calculus, playing a whitening role. Polyphosphates can also desorb salivary proteins from tooth enamel and inhibit the adsorption of proteins on its surface, reducing the formation of dental plaque or calculus, and thus reducing the deposition of pigments.

[0020] In one implementation of the present application, by weight, the calcium salt-containing toothpaste includes: 20 to 60 parts of the calcium salt abrasive, 0.1 to 5 parts of calcium glycerophosphate, 0.2 to 10 parts of the freshener, 0.01 to 10 parts of the gum protector, 0.01 to 10 parts of the whitening agent, 0.1 to 15 parts of the thickener, 5 to 50 parts of the humectant, 0.1 to 10 parts of the foaming agent, and 2 to 30 parts of water. It should be noted that the calcium salt-containing toothpaste with this formulation has good stripability and extrusion performance, and can produce good efficacy, including cleaning, anti-caries, freshening, whitening, etc.

[0021] In one implementation of the present application, by weight, the calcium salt-containing toothpaste includes: 10 to 40 parts of anhydrous calcium hydrogen phosphate, 10 to 40 parts of calcium hydrogen phosphate dihydrate, 0.1 to 5 parts of calcium glycerophosphate, 0.01 to 5 parts of zinc citrate, 0.01 to 5 parts of zinc glycinate, 0.01 to 5 parts of dipotassium glycyrrhizinate, 0.01 to 5 parts of allantoin, 0.1 to 5 parts of sodium pyrophosphate, 0.01 to 5 of carboxymethyl cellulose, 0.01 to 5 of xanthan gum, 0.1 to 5 of microcrystalline cellulose, 5 to 40 parts of sorbitol, 1 to 30 parts of glycerol, 1 to 20 parts of PEG-8.

[0022] In one implementation of the present application, by weight parts, the fluoride toothpaste includes: 10 to 50 parts of silica, 0.1 to 5 parts of the fluoride, 0.01 to 10 parts of the gingiva protector, 0.01 to 10 parts of the whitening agent, 0.01 to 10 parts of the thickening agent, 10 to 80 parts of the humectant, 0.1 to 10 parts of the foaming agent, 0.001 to 1 part of the pearlescent agent, 0.0001 to 1 part of the pigment, and 2 to 30 parts of water. It should be noted that the calcium salt toothpaste of this formula can have both good stripability and extrusion performance, and can produce good efficacy functions, including cleaning, anti-caries, gingiva protection, whitening, etc.

[0023] In one implementation of the present application, the fluoride toothpaste contains: 10 to 50 parts of silica, 0.1 to 5 parts of sodium monofluorophosphate, 0.01 to 5 parts of dipotassium glycyrrhizinate, 0.1 to 5 parts of sodium hexametaphosphate, 0.1 to 5 parts of pentasodium triphosphate, 0.01 to 5 parts of xanthan gum, 0.01 to 5 parts of chondrus crispus, 10 to 70 parts of sorbitol, 1 to 30 parts of glycerol, 1 to 30 parts of PEG400, 0.001 to 1 part of mica, 0.0001 to 1 part of pigment.

[0024] It should be noted that the dual-tube toothpaste of the present application adopts a dual-phosphorus-calcium friction system + silica friction system, as well as calcium glycerophosphate and fluoride, which synergistically enhance the effects of rapid cleaning and anti-caries; adopts a dual-zinc component of zinc citrate and zinc glycinate, which can help quickly clean up the accumulated unpleasant odor; adopts dipotassium glycyrrhizinate and allantoin for gingiva protection and repair; adopts sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate for complexing and whitening; adopts a thickening system with good rheology, which is beneficial to the extrusion of the dual-tube packaging material. In addition, the components in the present application synergistically enhance the effects and jointly improve the efficacy of the toothpaste. The dual-tube toothpaste of the present application is especially suitable for the scenario where rapid brushing is required in the morning, can quickly clean, remove the dental plaque accumulated at night, can immediately freshen the breath and have a long-term antibacterial effect, can protect and nourish the gingiva, can prevent caries, repair, resist dental calculus and whiten, and has the advantages of high efficiency, multiple effects and good fluorine-calcium compatibility.

[0025] The second aspect of the present application discloses a preparation method of a dual-tube toothpaste, including the following steps: separately preparing a calcium salt toothpaste and a fluoride toothpaste: adding a thickening agent to a part of the humectant, homogenizing to obtain a glue, adding the remaining components, stirring at room temperature, and performing vacuum degassing to obtain a paste, namely obtaining the calcium salt toothpaste and the fluoride toothpaste respectively; then, filling the calcium salt toothpaste and the fluoride toothpaste into the dual tubes respectively.

[0026] The beneficial effects of the present application are as follows:

[0027] The dual-tube toothpaste of the present application can effectively avoid the reduction of the bioavailability of fluoride and calcium salt abrasives caused by the combination of fluoride in the fluoride-containing toothpaste and calcium salt abrasives in the calcium salt-containing toothpaste by storing the calcium salt abrasives in the calcium salt-containing toothpaste and the fluoride separately. Furthermore, it can simultaneously have good friction cleaning power and anti-caries function. Thus, a toothpaste with good fluorine-calcium compatibility and dual-effect repair can be provided. Detailed implementation manners

[0028] The present invention will be further described in detail below through specific implementation manners. In the following implementation manners, many detailed descriptions are provided to enable a better understanding of the present application. However, those skilled in the art can easily recognize that some of the features can be omitted in different situations, or can be replaced by other materials or methods. In some cases, some operations related to the present application are not shown or described in the specification to avoid overwhelming the core part of the present application with excessive descriptions. For those skilled in the art, it is not necessary to describe these related operations in detail, and they can fully understand the related operations based on the description in the specification and the general technical knowledge in the art.

[0029] In addition, the features, operations or characteristics described in the specification can be combined in any appropriate manner to form various implementation manners. At the same time, the steps or actions in the method description can also be reordered or adjusted in an obvious manner for those skilled in the art. Therefore, the various sequences in the specification are only for clearly describing a certain embodiment and do not mean a necessary sequence, unless it is stated that a certain sequence must be followed.

[0030] Brushing teeth is often ignored by users. Especially in the morning, due to sleepiness and haste, the brushing time is short and the effect is poor, which easily leads to frequent dental problems. In view of this, the present application provides a dual-tube toothpaste that is efficient, multifunctional and has good fluorine-calcium compatibility. The dual-tube toothpaste of the present application has multiple effects such as rapid cleaning, anti-caries, instant fresh breath, long-term antibacterial, gum care, and whitening. Moreover, the components are stable with each other and have good fluorine-calcium compatibility. It is especially suitable for the scenario where users need to brush their teeth quickly in the morning. It can quickly clean, remove the dental plaque accumulated at night, can instantly freshen the breath and have long-term antibacterial effect, can care for the gums, can prevent caries and repair, resist dental calculus, and whiten teeth. It has the advantages of high efficiency, multiple effects and good fluorine-calcium compatibility. In addition, the components in the present application synergistically enhance the effect and jointly improve the efficacy of the toothpaste.

[0031] The present application relates to a dual-tube toothpaste and a preparation method thereof. A dual-tube toothpaste is a toothpaste product containing two independent chambers for storing toothpaste with different formulations. When the user squeezes the toothpaste tube body, the toothpaste with two different formulations will be extruded together. The discharge ratio can be designed according to requirements. For example, it can be discharged at a ratio of 1:1.

[0032] In a specific embodiment, the dual-tube toothpaste includes a calcium salt-containing toothpaste and a fluoride-containing toothpaste that are separately stored and isolated.

[0033] In a specific embodiment, the calcium salt-containing toothpaste includes a calcium salt abrasive, and the fluoride-containing toothpaste includes a non-calcium salt abrasive. The calcium salt abrasive may include at least one of calcium carbonate, dicalcium hydrogen phosphate, and calcium pyrophosphate. Preferably, the calcium salt abrasive is anhydrous dicalcium hydrogen phosphate and dicalcium hydrogen phosphate dihydrate. The non-calcium salt abrasive may include silica. The fluoride-containing toothpaste further includes a fluoride anti-caries agent, and the fluoride includes at least one of sodium monofluorophosphate, sodium fluoride, orafluor, and stannous fluoride. Preferably, the fluoride is sodium monofluorophosphate. Using sodium monofluorophosphate as the fluoride can provide both fluorine and phosphorus, further promoting the remineralization of teeth.

[0034] In a specific embodiment, the calcium salt-containing toothpaste may further include calcium glycerophosphate.

[0035] In a specific embodiment, the calcium salt-containing toothpaste or the fluoride-containing toothpaste may further include at least one of the following: freshener, gingiva protector, whitening agent, thickener, humectant, foaming agent, preservative, fragrance, sweetener, pearlescent agent, pigment.

[0036] In a specific embodiment, the freshener may include zinc citrate and zinc glycinate.

[0037] In a specific embodiment, the gingiva protector may include at least one of dipotassium glycyrrhizinate and allantoin.

[0038] In a specific embodiment, the whitening agent may include at least one of sodium pyrophosphate tetrasodium, sodium tripolyphosphate, and sodium hexametaphosphate.

[0039] In a specific embodiment, the thickener may include at least one of cellulose gum, xanthan gum, microcrystalline cellulose, and chondrus crispus. It should be noted that in order to match the extrusion rheology of the dual-tube packaging material, a thickener with good rheological properties needs to be used, considering the overall rheological properties.

[0040] In a specific embodiment, the humectant may include at least one of glycerol, sorbitol, and polyethylene glycol.

[0041] In a specific embodiment, the pearlescent agent may include mica.

[0042] In a specific embodiment, the foaming agent may include at least one of sodium lauryl sulfate, cocamidopropyl betaine, sodium lauroyl sarcosinate, disodium lauroyl glutamate, disodium cocoyl glutamate, sodium methyl lauroyl taurate, sodium methyl cocoyl taurate, and sodium cocoyl methyl taurate.

[0043] In a specific embodiment, the preservative may include ethylparaben, benzoic acid, sodium benzoate, and potassium sorbate. The preservative may also be selected from other edible antibacterial substances, which will not be elaborated herein one by one.

[0044] In a specific embodiment, the fragrance may include at least one of essence, natural essential oil, and natural extract. The essence is an edible essence, which may include at least one of bergamot essence, eucalyptus essence, citrus essence, lemon essence, peppermint essence, mint essence, menthol, licorice essence, wintergreen essence, tobacco essence, coffee essence, vanilla essence, lime essence, apple essence, peach essence, mango essence, cherry essence, blueberry essence, strawberry essence, cola essence, cinnamon essence, vanillin essence, and watermelon essence. The essence may also be other types of edible essences, which will not be elaborated herein one by one.

[0045] In a specific embodiment, the sweetener may include xylitol, sorbitol, mannitol, erythritol, lactitol, maltitol, isomaltulose, hydrogenated starch hydrolysate, erythritol, maltotriitol, aspartame, acesulfame potassium, sodium saccharin, sucralose, neotame, sodium cyclamate, alitame, stevioside, arabitol, and mogroside. The sweetener may also be selected from other edible substances, which will not be elaborated herein one by one.

[0046] In a specific embodiment, by weight, the calcium salt toothpaste may include 20 to 60 parts of calcium salt abrasives. For example, the calcium salt toothpaste may include 20, 30, 40, 50, or 60 parts of calcium salt abrasives. Preferably, the calcium salt toothpaste may include 10 to 40 parts of anhydrous calcium hydrogen phosphate and 10 to 40 parts of calcium hydrogen phosphate dihydrate. For example, the calcium salt toothpaste may include 10, 20, 30, or 40 parts of anhydrous calcium hydrogen phosphate and 10, 20, 30, or 40 parts of calcium hydrogen phosphate dihydrate.

[0047] In a specific embodiment, by weight, the calcium salt toothpaste may include 0.1 to 5 parts of calcium glycerophosphate. For example, the calcium salt toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of calcium glycerophosphate.

[0048] In a specific embodiment, by weight, the calcium salt toothpaste may include 0.2 to 10 parts of freshener. For example, the calcium salt toothpaste may include 0.2, 0.5, 1, 3, 5, 8, or 10 parts of freshener. Preferably, the calcium salt toothpaste may include 1 to 10 parts of freshener. Preferably, the calcium salt toothpaste may include 0.5 to 5 parts of zinc glycinate and 0.5 to 5 parts of zinc citrate. For example, the calcium salt toothpaste may include 0.5, 1, 2, 3, 4, or 5 parts of zinc glycinate and 0.5, 1, 2, 3, 4, or 5 parts of zinc citrate.

[0049] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.01 to 10 parts of a gum care agent. For example, the calcium salt-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a gum care agent. Preferably, the calcium salt-containing toothpaste may include 0.01 to 5 parts of dipotassium glycyrrhizinate and 0.01 to 5 parts of allantoin. For example, the calcium salt-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of dipotassium glycyrrhizinate and 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of allantoin.

[0050] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.01 to 10 parts of a whitening agent. For example, the calcium salt-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a whitening agent. Preferably, the calcium salt-containing toothpaste may include 0.1 to 5 parts of tetrasodium pyrophosphate. For example, the calcium salt-containing toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of tetrasodium pyrophosphate.

[0051] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.1 to 15 parts of a thickening agent. For example, the calcium salt-containing toothpaste may include 0.1, 0.5, 1, 3, 5, 8, 10, 13, or 15 parts of a thickening agent. Preferably, the calcium salt-containing toothpaste may include 0.01 to 5 of carboxymethyl cellulose, 0.01 to 5 of xanthan gum, and 0.1 to 5 of microcrystalline cellulose. For example, the calcium salt-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of carboxymethyl cellulose, 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of xanthan gum, and 0.1, 0.5, 1, 2, 3, 4, or 5 parts of microcrystalline cellulose.

[0052] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 5 to 50 parts of a humectant. For example, the calcium salt-containing toothpaste may include 5, 10, 20, 30, 40, or 50 parts of a humectant. Preferably, the calcium salt-containing toothpaste may include 5 to 40 parts of sorbitol, 1 to 30 parts of glycerol, and 1 to 20 parts of PEG-8. For example, the calcium salt-containing toothpaste may include 5, 10, 20, 30, or 40 parts of sorbitol, 1, 5, 10, 20, or 30 parts of glycerol, and 1, 5, 10, or 20 parts of PEG-8.

[0053] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.1 to 10 parts of a foaming agent. For example, the calcium salt-containing toothpaste may include 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a foaming agent.

[0054] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 2 to 30 parts of water. For example, the calcium salt-containing toothpaste may include 2, 5, 10, 15, 20, 25, or 30 parts of water.

[0055] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.01 to 5 parts of a sweetening agent. For example, the calcium salt-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of a sweetening agent.

[0056] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.1 to 5 parts of a flavoring agent. For example, the calcium salt-containing toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of a flavoring agent.

[0057] In a specific embodiment, by weight parts, the calcium salt-containing toothpaste may include 0.1 to 5 parts of a preservative. For example, the calcium salt-containing toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of a preservative.

[0058] In a specific embodiment, by weight parts, the fluoride-containing toothpaste may include 10 to 50 parts of silica. For example, the fluoride-containing toothpaste may include 10, 15, 20, 25, 30, 35, 40, 45, or 50 parts of silica.

[0059] In a specific embodiment, by weight parts, the fluoride-containing toothpaste may include 0.1 to 5 parts of a fluoride. Preferably, the fluoride-containing toothpaste may include 0.1 to 5 parts of sodium monofluorophosphate. For example, the fluoride-containing toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of sodium monofluorophosphate.

[0060] In a specific embodiment, by weight parts, the fluoride-containing toothpaste may include 0.01 to 10 parts of a gingiva protector. For example, the fluoride-containing toothpaste may include 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a gingiva protector. Preferably, the fluoride-containing toothpaste may include 0.01 to 5 parts of dipotassium glycyrrhizinate. For example, the fluoride-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of dipotassium glycyrrhizinate.

[0061] In a specific embodiment, by weight parts, the fluoride-containing toothpaste may include 0.01 to 10 parts of a whitening agent. For example, the fluoride-containing toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a whitening agent. Preferably, the fluoride-containing toothpaste may include 0.1 to 5 parts of sodium hexametaphosphate and 0.1 to 5 parts of sodium tripolyphosphate. For example, the fluoride-containing toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of sodium hexametaphosphate and 0.1, 0.5, 1, 2, 3, 4, or 5 parts of sodium tripolyphosphate.

[0062] In a specific embodiment, by weight parts, the fluoride toothpaste may include 0.01 to 10 parts of a thickening agent. For example, the fluoride toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a thickening agent. Preferably, the fluoride toothpaste may include 0.01 to 5 parts of xanthan gum and 0.01 to 5 parts of Chondrus crispus. For example, the fluoride toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of xanthan gum and 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of Chondrus crispus.

[0063] In a specific embodiment, by weight parts, the fluoride toothpaste may include 10 to 80 parts of a humectant. For example, the fluoride toothpaste may include 10, 15, 20, 30, 40, 50, 60, 70, or 80 parts of a humectant. Preferably, the fluoride toothpaste may include 10 to 70 parts of sorbitol, 1 to 30 parts of glycerol, and 1 to 30 parts of PEG400. For example, the fluoride toothpaste may include 10, 15, 20, 30, 40, 50, 60, or 70 parts of sorbitol, 1, 5, 10, 15, 20, 25, or 30 parts of glycerol, and 1, 5, 10, 15, 20, 25, or 30 parts of PEG400.

[0064] In a specific embodiment, by weight parts, the fluoride toothpaste may include 0.1 to 10 parts of a foaming agent. For example, the fluoride toothpaste may include 0.1, 0.5, 1, 3, 5, 8, or 10 parts of a foaming agent.

[0065] In a specific embodiment, by weight parts, the fluoride toothpaste may include 0.001 to 1 part of a pearlescent agent. Preferably, the fluoride toothpaste may include 0.001 to 1 part of mica. For example, the fluoride toothpaste may include 0.001, 0.005, 0.01, 0.05, 0.1, 0.5, or 1 part of mica.

[0066] In a specific embodiment, by weight parts, the fluoride toothpaste may include 0.0001 to 1 part of a pigment. For example, the fluoride toothpaste may include 0.0001, 0.0005, 0.001, 0.005, 0.01, 0.05, 0.1, 0.5, or 1 part of a pigment.

[0067] In a specific embodiment, by weight parts, the fluoride toothpaste may include 2 to 30 parts of water. For example, the fluoride toothpaste may include 2, 5, 10, 15, 20, 25, or 30 parts of water.

[0068] In a specific embodiment, by weight parts, the fluoride toothpaste may include 0.01 to 5 parts of a sweetening agent. For example, the fluoride toothpaste may include 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, or 5 parts of a sweetening agent.

[0069] In a specific embodiment, by weight, the fluoride toothpaste may include 0.1 to 5 parts of a flavoring agent. For example, the fluoride toothpaste may include 0.1, 0.5, 1, 2, 3, 4, or 5 parts of a flavoring agent.

[0070] In a specific embodiment, by weight, the fluoride toothpaste may include 0.01 to 5 parts of a preservative.

[0071] In a specific embodiment, a method for preparing a dual-tube toothpaste is provided, including: separately preparing a calcium salt toothpaste and a fluoride toothpaste: Step S100: Add a thickening agent to a part of a humectant, homogenize to obtain a glue, add the efficacy components dissolved by pre-microheating and the remaining components, stir at room temperature, and perform vacuum degassing to obtain a paste, thereby separately obtaining the calcium salt toothpaste and the fluoride toothpaste; Step S200: Fill the calcium salt toothpaste and the fluoride toothpaste into two tubes respectively.

[0072] In a specific embodiment, in Step S100, the temperature when preparing the glue may be 50°C to 60°C. For example, in Step S100, the temperature may be 50°C, 55°C, or 60°C.

[0073] In a specific embodiment, in Step S100, the heating temperature of the efficacy components dissolved by pre-microheating is 50°C to 60°C.

[0074] In a specific embodiment, in Step S100, when adding the thickening agent to a part of the humectant and stirring, the conditions for uniform stirring are: stirring speed 2000 to 4000 r / min, stirring time 10 to 30 min. For example, in Step S100, the conditions for uniform stirring are: the stirring speed may be 800 r / min, 3000 r / min, or 4000 r / min, and the stirring time may be 10 min, 20 min, or 30 min.

[0075] In a specific embodiment, in Step S100, the conditions for stirring at room temperature are: stirring speed 2000 to 4000 r / min, stirring time 10 to 15 min.

[0076] The present application will be further described in detail below through specific examples and comparative examples. The following examples and comparative examples are only for further illustration of the present application and should not be construed as a limitation of the present application. In this embodiment, unless otherwise specified, the raw materials, reagents, and instruments used are all commercially available, and the experimental operations are carried out in accordance with the product instructions and conventional experimental specifications.

[0077] Preparation of the dual-tube toothpaste of Example 1, Example 2, Comparative Example 1, and Comparative Example 2:

[0078] Preparation of calcium salt toothpaste and fluoride toothpaste: weigh the corresponding amount of thickener and moisturizer, stir at 3000r / min for 20min until uniform dispersion; add the remaining components, use a propeller mixer to stir at 2000r / min for 15min at room temperature until the paste is fine and uniform, and vacuum degas to obtain toothpaste paste. Fill the calcium salt toothpaste and fluoride toothpaste into a double-tube pipe with a 1:1 discharge ratio.

[0079] The formula of the calcium salt toothpaste of each embodiment and comparative example is as follows:

[0080]

[0081] The formula of the fluoride toothpaste of each embodiment and comparative example is as follows:

[0082]

[0083]

[0084] Efficacy test:

[0085] 1. Bad breath removal test

[0086] 1. Experimental Grouping

[0087] Sample group: Example 1 double tube toothpaste

[0088] Control group: double tube toothpaste of comparative example 1 or comparative example 2

[0089] 2. Experimental Methods

[0090] (1) Cultivation of membrane: 14 g of saliva from four volunteers was collected and mixed in a 50 mL centrifuge tube. Ten 10 mL centrifuge tubes were taken, and one hydroxyapatite (HAP) sheet and 1 mL of saliva were added to each centrifuge tube so that the HAP sheet was immersed in the saliva. The centrifuge tubes were then placed in a 37°C constant temperature water bath for overnight incubation to form an acquired membrane on the surface of the HAP sheet. The centrifuge tubes were removed from the water bath the next day and the saliva was removed.

[0091] (2) Sample preparation: toothpaste (outer core and inner core mixed in a mass ratio of 1:1) and water in a mass ratio of 1:1.6 were thoroughly mixed to form a uniform slurry.

[0092] (3) Treatment of test samples: 10 cultured HAP sheets were randomly divided into a sample group and a control group, with 5 sheets in each group. The HAP sheets in the sample group were soaked in 5 mL of toothpaste slurry for 30 seconds, taken out and placed in a headspace bottle, with 1 sheet in each bottle.

[0093] (4) Preparation of saliva culture medium solution: Weigh 0.75 g of thioglycollate medium, add 25 g of deionized water, heat and stir to dissolve it to obtain the culture medium stock solution. Collect 26 g of saliva from 4 volunteers, mix it evenly and store it in a 50 mL centrifuge tube. Prepare the saliva culture medium solution according to the ratio of culture medium stock solution: deionized water: saliva (1.6:13.4:85), mix it evenly and set aside.

[0094] (5) Culturing for gas production: Add 3 mL of saliva culture medium solution to each headspace vial, seal it and place it in a water bath at 37 °C for 16 hours to produce volatile sulfide gas. Take out the cultured headspace vials from the water bath the next day.

[0095] (6) Quantitative detection of methanethiol: Place the headspace vial in a headspace sampler, and determine the peak area of methanethiol in the gas in the headspace vial by gas chromatography - flame photometric detector, and calculate the logarithm of the peak area.

[0096] 3. Evaluation method

[0097] Use SPSS 27.0 statistical software, and use the Shapiro - Wilk test to check the normality of the logarithm of the peak area. If P > 0.05, it is normally distributed, and a t - test is performed with a significance level of α = 0.05. If P < 0.05, it is non - normally distributed, and a Wilcoxon rank - sum test is performed with a significance level of α = 0.05.

[0098] Methanethiol is one of the characteristic substances of bad breath. The less the amount of methanethiol, the better the effect of removing bad breath. If the value of the sample group is less than that of the control group, and the difference between groups is statistically significant (P < 0.05), it indicates that after 16 - hour co - culture with saliva, the sample group can reduce the production of methanethiol, and has the effect of freshening breath and preventing bad breath.

[0099] 4. Test data and statistical results

[0100]

[0101] Note: When the peak area < 100, define lg(A) as 0.

[0102] 5. Conclusion

[0103] Compared with the control group, after 16 - hour co - culture with saliva, the sample group can reduce the production of methanethiol, and the difference between groups is statistically significant (P < 0.05). It can be considered that the dual - tube toothpaste of Example 1 has the effect of freshening breath and preventing bad breath for 16 hours.

[0104] II. Anti - caries test

[0105] 2.1 Test grouping

[0106] The experiment was divided into 3 groups, Comparative Example 1 and Comparative Example 2: After the bovine teeth were cleaned with deionized water, they were immersed in the saliva of the subjects for 12 h; Example 1: After the bovine teeth were cleaned with deionized water, the bovine teeth were treated with the sample in the conventional brushing method, and then after rinsing off the sample and foam on the surface of the bovine teeth with deionized water, they were immersed in the saliva of the subjects for 12 h.

[0107] 2.2 Saliva preparation

[0108] The saliva of the subjects was collected 1 h before the experiment.

[0109] 2.3 Operating steps

[0110] (1) Take 18 bovine teeth and randomly divide them into Comparative Example 1, Comparative Example 2 and Example 1, with 6 pieces in each group.

[0111] (2) Take about 0.5 g of toothpaste and place it on the surface of the bovine teeth, and use an ordinary toothbrush to simulate brushing for 3 min. After rinsing off the toothpaste foam on the surface of the bovine teeth with deionized water, place them in the saliva of the subjects and soak for 12 h.

[0112] (3) Take out the bovine teeth and quantify the total fluorine remaining on the surface of the bovine teeth according to the determination method of the total fluorine content in GB / T8372-2017 "Toothpaste".

[0113] 2.4 Test results

[0114]

[0115]

[0116] 2.5 Conclusion

[0117] In Example 1, after simulating brushing and soaking in saliva for 12 hours, the total fluorine residue on the surface of the bovine teeth was 0.27 μg / tooth, which has a longer-lasting effect on preventing dental caries compared with Comparative Example 1 and Comparative Example 2.

[0118] III. Tooth enamel protection test

[0119] 3.1 Test grouping

[0120] The experiment was divided into 3 groups, the test group: Example 1; the blank control group: Comparative Example 1, Comparative Example 2.

[0121] The outermost enamel of the tooth is the hardest tissue in the human body. Due to poor oral hygiene, excessive deposition of acidic substances inside the body, etc., white or yellowish-brown spots appear on the tooth surface. The spots will gradually increase, and even lead to the demineralization phenomenon where the tooth develops cracks. Daily use of toothpaste with the function of preventing demineralization helps reduce tooth demineralization. Therefore, in this experiment, a bovine tooth model was used as the substrate. First, the bovine tooth model was soaked in toothpaste paste, and then acid etching treatment (or "acid corrosion") was carried out on it. The microhardness tester was used to measure the change in the surface hardness of the enamel before and after the treatment, so as to evaluate the anti-demineralization effect of the toothpaste on the enamel. The results and analysis are shown in the following table.

[0122] Anti-demineralization test results (16h)

[0123]

[0124]

[0125] Analysis of significant differences (16h)

[0126]

[0127] 3.2 Experimental conclusions

[0128] Under the conditions of this experiment, for the bovine tooth model soaked and acid-etched in the test group, after being placed in artificial saliva for 16 hours, the decrease value of the enamel hardness (AHV) was significantly less than that of the control group in the same test, and there was a significant difference between the two groups (p < 0.001). Moreover, the test group improved the anti-acid-etching ability and the effect of protecting the enamel by about 1.3 times compared with the control group 1 and the control group 2. It shows that the test group has the effect of preventing enamel demineralization for 16 hours, and to a certain extent, enhancing the tooth acid-etching ability and preventing enamel demineralization.

[0129] The above content is a further detailed description of the present application in combination with specific implementation manners. It cannot be determined that the specific implementation of the present application is only limited to these descriptions. For those of ordinary skill in the technical field to which the present application belongs, without departing from the concept of the present application, several simple deductions or substitutions can still be made.

Claims

1. A double-tube toothpaste, characterized in that, It includes a calcium salt-containing toothpaste and a fluoride-containing toothpaste stored separately and isolated. The calcium salt-containing toothpaste includes a calcium salt abrasive, and the fluoride-containing toothpaste includes an anti-caries agent, and the anti-caries agent includes fluoride.

2. The double-tube toothpaste according to claim 1, wherein The fluoride-containing toothpaste includes a non-calcium salt abrasive, and the non-calcium salt abrasive includes silica; the fluoride includes at least one of sodium monofluorophosphate, sodium fluoride, orafluor, and stannous fluoride.

3. The dual-tube toothpaste according to claim 1, characterized in that, The calcium salt abrasive includes anhydrous calcium hydrogen phosphate and calcium hydrogen phosphate dihydrate.

4. The double-tube toothpaste according to any one of claims 1 to 3, characterized in that, The calcium salt-containing toothpaste includes calcium glycerophosphate.

5. The dual-tube toothpaste according to claim 1, wherein The calcium salt-containing toothpaste or the fluoride-containing toothpaste further includes at least one of the following: a freshener, a gum protector, a whitening agent, a thickener, a humectant, a foaming agent, a preservative, an aromatic agent, a sweetener, a pearlescent agent, a pigment; the freshener includes zinc citrate and zinc glycinate, the gum protector includes at least one of dipotassium glycyrrhizinate and allantoin, the whitening agent includes at least one of tetrasodium pyrophosphate, sodium hexametaphosphate, and sodium tripolyphosphate, the thickener includes at least one of cellulose gum, xanthan gum, chondrus crispus, and microcrystalline cellulose, and the humectant includes at least one of glycerol, sorbitol, and polyethylene glycol.

6. The dual-tube toothpaste according to claim 5, wherein By weight, the calcium salt-containing toothpaste includes: 20 to 60 parts of the calcium salt abrasive, 0.1 to 5 parts of calcium glycerophosphate, 0.2 to 10 parts of the freshener, 0.01 to 10 parts of the gum protector, 0.01 to 10 parts of the whitening agent, 0.1 to 15 parts of the thickener, 5 to 50 parts of the humectant, 0.1 to 10 parts of the foaming agent, and 2 to 30 parts of water.

7. The dual-tube toothpaste according to claim 6, wherein By weight, the calcium salt-containing toothpaste includes: 10 to 40 parts of anhydrous calcium hydrogen phosphate, 10 to 40 parts of calcium hydrogen phosphate dihydrate, 0.1 to 5 parts of calcium glycerophosphate, 0.01 to 5 parts of zinc citrate, 0.01 to 5 parts of zinc glycinate, 0.01 to 5 parts of dipotassium glycyrrhizinate, 0.01 to 5 parts of allantoin, 0.1 to 5 parts of tetrasodium pyrophosphate, 0.01 to 5 of carboxymethyl cellulose, 0.01 to 5 of xanthan gum, 0.1 to 5 of microcrystalline cellulose, 5 to 40 parts of sorbitol, 1 to 30 parts of glycerol, 1 to 20 parts of PEG-8.

8. The double-tube toothpaste according to claim 5, wherein, By weight, the fluoride-containing toothpaste includes: 10 to 50 parts of silica, 0.1 to 5 parts of the fluoride, 0.01 to 10 parts of the gum protector, 0.01 to 10 parts of the whitening agent, 0.01 to 10 parts of the thickener, 10 to 80 parts of the humectant, 0.1 to 10 parts of the foaming agent, 0.001 to 1 part of the pearlescent agent, 0.0001 to 1 part of the pigment, and 2 to 30 parts of water.

9. The dual-tube toothpaste according to claim 8, wherein By weight parts, the fluoride toothpaste contains: 10 to 50 parts of silica, 0.1 to 5 parts of sodium monofluorophosphate, 0.01 to 5 parts of dipotassium glycyrrhizinate, 0.1 to 5 parts of sodium hexametaphosphate, 0.1 to 5 parts of pentasodium triphosphate, 0.01 to 5 parts of xanthan gum, 0.01 to 5 parts of chondrus crispus, 10 to 70 parts of sorbitol, 1 to 30 parts of glycerol, 1 to 30 parts of PEG400, 0.001 to 1 part of mica, and 0.0001 to 1 part of pigment.

10. A method for preparing a dual-tube toothpaste according to any one of claims 1 to 9, characterized in that, It includes: Prepare the calcium salt toothpaste and the fluoride toothpaste respectively: Add the thickener to part of the humectant, homogenize to obtain a glue, add the remaining components, stir at room temperature, and degas under vacuum to obtain a paste, thereby obtaining the calcium salt toothpaste and the fluoride toothpaste respectively; Subsequently, fill the calcium salt toothpaste and the fluoride toothpaste into two tubes respectively.

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