Anhydrous toothpaste and method of making same

Abstract

The application discloses anhydrous toothpaste and a preparation method thereof. The anhydrous toothpaste comprises a humectant, a thickening agent, an abrasive and an efficacy component; the humectant is composed of at least one of PEG 400 and propylene glycol and glycerol, and the amount of the glycerol is not more than 40% of the total weight of the anhydrous toothpaste; the thickening agent comprises microcrystalline cellulose; the abrasive is composed of at least one of calcium hydrogen phosphate dihydrate and calcium pyrophosphate and calcium hydrogen phosphate and hydrated silica, and the calcium hydrogen phosphate is the main abrasive; and the efficacy component comprises sodium monofluorophosphate and sodium phytate. The anhydrous toothpaste can improve the burning and irritating taste of the anhydrous toothpaste; the calcium hydrogen phosphate is used as the main abrasive, the sodium monofluorophosphate is used as a repairing and remineralizing component, the two components are compatible, the soluble fluorine concentration can be improved, and the tooth remineralization and acid erosion resistance can be ensured; and the microcrystalline cellulose thickening does not need to be neutralized and is resistant to high-speed shearing, so that the system damage caused by incompatible raw materials during the shelf life is avoided, and the stability is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the toothpaste technical field, in particular to a kind of anhydrous toothpaste and preparation method thereof. BACKGROUND

[0002] Toothpaste is a paste product composed of abrasives, humectants, foaming agents, thickening agents, fragrances, water and other additives, such as efficacy ingredients for improving oral health. With the improvement of living standards, people have higher and higher demands for toothpaste varieties and functions. Common abrasives for toothpaste include calcium carbonate, silicon dioxide and calcium hydrogen phosphate. Calcium hydrogen phosphate has low hardness, proper cleaning power without damaging teeth, and good polishing properties on tooth surface; toothpaste with calcium hydrogen phosphate as abrasive has good appearance gloss, little irritation to oral mucosa, and strong fragrance burst.

[0003] Anhydrous toothpaste is different from conventional aqueous toothpaste in thickening system, and requires that a stable colloid with certain viscosity and good thixotropy can be prepared without using water, so the preparation of anhydrous thickening system is the key to the preparation of anhydrous toothpaste. Commonly used thickening agents in toothpaste include thickening silica, binders (such as sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, xanthan gum, carrageenan, etc.), and high molecular polymers (such as carbomer, polyvinylpyrrolidone and its derivatives, etc.). However, there are fewer choices of thickening agents that can be used in anhydrous toothpaste, and carbomer is currently the main choice on the market. For example, CN 106511105 B “Anhydrous Toothpaste for Repairing Demineralized Tooth Enamel and Dentin and Preparation Method Thereof”, which uses carbomer as a thickening agent. Carbomer needs to be neutralized to thicken and is not resistant to high-speed shearing. In addition, toothpaste with carbomer as a thickening agent is prone to hardening and may cause poor experience of difficult extrusion during shelf life. In addition, anhydrous toothpaste has a certain burning sensation, which greatly affects the user experience.

[0004] Therefore, how to improve the stability of anhydrous toothpaste and reduce the burning sensation during use is still the focus and difficulty of research on anhydrous toothpaste. SUMMARY

[0005] The purpose of the present application is to provide an improved anhydrous toothpaste and a preparation method thereof.

[0006] To achieve the above-mentioned purpose, the present application adopts the following technical solutions:

[0007] The first aspect of the present application discloses an anhydrous toothpaste, comprising a humectant, a thickening agent, an abrasive agent and an efficacy component; the humectant is composed of at least one of sorbitol, PEG 400 and propylene glycol, and glycerol; the amount of the humectant is 45-55% of the total weight of the anhydrous toothpaste, wherein the amount of glycerol is less than or equal to 40% of the total weight of the anhydrous toothpaste; the thickening agent comprises microcrystalline cellulose; the abrasive agent is composed of at least one of calcium hydrogen phosphate dihydrate and calcium pyrophosphate, and calcium hydrogen phosphate and hydrated silica; the amount of calcium hydrogen phosphate is 20-25% of the total weight of the anhydrous toothpaste; the amount of hydrated silica is 3-10% of the total weight of the anhydrous toothpaste; the amount of calcium hydrogen phosphate dihydrate is 0-20% of the total weight of the anhydrous toothpaste; the amount of calcium pyrophosphate is 0-18% of the total weight of the anhydrous toothpaste; and the efficacy component comprises sodium monofluorophosphate and sodium phytate.

[0008] It should be noted that the anhydrous toothpaste of the present application optimizes the formula of the humectant, so that the amount of glycerol is controlled to be 40% or less, thereby improving the problem of burning and irritating taste of the anhydrous toothpaste; by using calcium hydrogen phosphate and / or calcium hydrogen phosphate dihydrate as the abrasive agent and sodium monofluorophosphate as the repair and remineralization efficacy component, the problem of incompatibility between calcium-containing abrasive agents such as calcium hydrogen phosphate and fluoride is improved in the anhydrous environment, the soluble fluoride concentration is improved, and the tooth remineralization and repair efficacy is ensured; by using microcrystalline cellulose as the thickening and suspending agent, the microcrystalline cellulose thickening does not need to be neutralized, and it is resistant to high-speed shearing, thereby avoiding the damage of high-speed shearing during the toothpaste preparation process to the thickening system of the paste; and the microcrystalline cellulose has good compatibility with calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate, calcium pyrophosphate and the like, thereby avoiding the damage of the formula system caused by the incompatibility of raw materials during the entire shelf life, and improving the stability of the toothpaste. In summary, the anhydrous toothpaste of the present application improves the burning and irritating taste of the conventional anhydrous toothpaste; not only has the effect of phosphorus and calcium abrasive agent for cleaning and removing stains, but also effectively ensures the tooth remineralization and repair efficacy due to the solution of the problem of incompatibility between calcium-containing abrasive agents and fluoride, thereby having better anti-cavity efficacy; and the anhydrous toothpaste of the present application has good toothpaste forming, paste shape and shape stability, does not produce water, and has good overall stability.

[0009] It should be further noted that the anhydrous toothpaste of the present application is key to optimizing and improving the humectant, thickening agent, abrasive agent and efficacy component; as for other components of the anhydrous toothpaste, such as surfactants, fragrances and additives, they can be referred to the existing anhydrous toothpaste; however, in the preferred scheme of the present application, the surfactants, fragrances and additives are particularly limited in order to ensure the performance of the anhydrous toothpaste.

[0010] In an implementation manner of the present application, the amount of sodium monofluorophosphate is 0.5-1.1% of the total weight of the anhydrous toothpaste.

[0011] In one implementation of the present application, the sodium phytate is used in an amount of 0.5-1.5% of the total weight of the anhydrous toothpaste.

[0012] In one implementation of the present application, the microcrystalline cellulose is used in an amount of 0.1-2% of the total weight of the anhydrous toothpaste.

[0013] In one implementation of the present application, the thickening agent further comprises cellulose gum and / or thickening type hydrated silica.

[0014] It should be noted that one of the keys of the present application is to use microcrystalline cellulose as a thickening agent for anhydrous toothpaste, and on this basis, microcrystalline cellulose can be used as the main thickening agent, and cellulose gum and / or thickening type hydrated silica commonly used can be additionally supplemented. It can be understood that the thickening type hydrated silica in the present application and the hydrated silica as an abrasive are different types of hydrated silica.

[0015] In one implementation of the present application, the anhydrous toothpaste of the present application further comprises a surfactant, a flavoring agent, and an additive.

[0016] In one implementation of the present application, the surfactant is sodium lauryl sulfate.

[0017] In one implementation of the present application, the surfactant is used in an amount of 1.5-2.5% of the total weight of the anhydrous toothpaste.

[0018] In one implementation of the present application, the anhydrous toothpaste further comprises a biological enzyme.

[0019] In one implementation of the present application, the biological enzyme is at least one of papain, dextranase, and lysozyme.

[0020] In one implementation of the present application, the biological enzyme is used in an amount of 0.01-0.5% of the total weight of the anhydrous toothpaste.

[0021] In one implementation of the present application, the flavoring agent is used in an amount of 0.5-2% of the total weight of the anhydrous toothpaste.

[0022] In one implementation of the present application, the additive is sucralose and / or sodium benzoate.

[0023] A second aspect of the present application discloses another anhydrous toothpaste, comprising a humectant composed of at least one of sorbitol, PEG 400, and propylene glycol, and glycerol; the humectant is used in an amount of 45-55% of the total weight of the anhydrous toothpaste, wherein the amount of glycerol is less than or equal to 40% of the total weight of the anhydrous toothpaste.

[0024] It should be noted that the anhydrous toothpaste disclosed in the second aspect of the present application is characterized in that the amount of glycerol is controlled at 40% or less by optimizing and improving the humectant, thereby improving the burning and irritating taste of the anhydrous toothpaste. It can be understood that other components of the anhydrous toothpaste of the present application, such as thickening agents, abrasives, efficacy ingredients, surfactants, fragrances and additives, can be referred to existing anhydrous toothpaste; however, in the preferred embodiments of the present application, these components are specially limited in order to ensure the performance of the anhydrous toothpaste. For example, in one implementation of the present application, the anhydrous toothpaste disclosed in the second aspect of the present application can refer to the anhydrous toothpaste disclosed in the first aspect of the present application for its thickening agent, abrasive, efficacy ingredient, surfactant, fragrance and additive.

[0025] The third aspect of the present application discloses another kind of anhydrous toothpaste, which comprises a thickening agent, the thickening agent comprising microcrystalline cellulose, and the amount of microcrystalline cellulose being 0.1-2% of the total weight of the anhydrous toothpaste.

[0026] It should be noted that the anhydrous toothpaste disclosed in the third aspect of the present application is characterized in that the microcrystalline cellulose is creatively used as the main thickening agent in the system of the anhydrous toothpaste to improve the stability of the anhydrous toothpaste; on this basis, the thickening agent of the present application can also comprise cellulose gum and / or thickening hydrous silica. The microcrystalline cellulose thickening does not need to be neutralized and is resistant to high-speed shearing, avoiding the damage of the high-speed shearing in the toothpaste making process to the thickening system of the paste body; and the microcrystalline cellulose has good compatibility with other components, avoiding the destruction of the formula system due to the incompatibility of raw materials during the entire shelf life, thereby improving the stability of the toothpaste. It can be understood that other components of the anhydrous toothpaste of the present application, such as humectants, abrasives, efficacy ingredients, surfactants, fragrances and additives, can be referred to existing anhydrous toothpaste; however, in the preferred embodiments of the present application, these components are specially limited in order to ensure the performance of the anhydrous toothpaste. For example, in one implementation of the present application, the anhydrous toothpaste disclosed in the third aspect of the present application can refer to the anhydrous toothpaste disclosed in the first aspect of the present application for its humectant, abrasive, efficacy ingredient, surfactant, fragrance and additive.

[0027] The fourth aspect of the present application discloses another kind of anhydrous toothpaste, which comprises an abrasive and an efficacy ingredient, the abrasive being composed of at least one of dicalcium phosphate dihydrate, calcium pyrophosphate, dicalcium phosphate and hydrous silica; the amount of dicalcium phosphate being 20-25% of the total weight of the anhydrous toothpaste; the amount of hydrous silica being 3-10% of the total weight of the anhydrous toothpaste; the amount of dicalcium phosphate dihydrate being 0-20% of the total weight of the anhydrous toothpaste; the amount of calcium pyrophosphate being 0-18% of the total weight of the anhydrous toothpaste; and the efficacy ingredient comprising sodium monofluorophosphate and sodium phytate.

[0028] It should be noted that the anhydrous toothpaste of the present application is characterized in that calcium hydrogen phosphate and / or calcium hydrogen phosphate dihydrate are used as abrasives, and sodium monofluorophosphate is used as a remineralization component, which improves the incompatibility of calcium hydrogen phosphate and fluoride in anhydrous environment, increases the concentration of soluble fluoride, and thus guarantees the remineralization effect. The anhydrous toothpaste of the present application not only has the effect of removing stains by phosphorus calcium abrasives, but also effectively guarantees the remineralization effect due to the solution of the incompatibility of calcium abrasives and fluoride, thereby having better anti-cavity effect. It can be understood that other components of the anhydrous toothpaste of the present application, such as humectants, thickeners, surfactants, fragrances and additives, can refer to existing anhydrous toothpaste; however, in the preferred embodiment of the present application, in order to ensure the performance of the anhydrous toothpaste, these components are specially limited. For example, in one implementation of the present application, the anhydrous toothpaste disclosed in the fourth aspect of the present application can refer to the anhydrous toothpaste disclosed in the first aspect of the present application.

[0029] The fifth aspect of the present application discloses a preparation method of the anhydrous toothpaste of the present application, comprising the following steps:

[0030] (1) Weigh the glycerol, add the thickener to the glycerol, stir and disperse uniformly, heat to homogenize to colloidal swelling, and after cooling, add other humectants and disperse uniformly; wherein the thickener mainly refers to microcrystalline cellulose;

[0031] (2) Mix other components except fragrances to form a mixed powder, add the mixed powder to the mixture of microcrystalline cellulose and humectants obtained in step (1), and after the mixed powder is wetted, stir uniformly;

[0032] (3) Add fragrances to the product of step (2) and stir uniformly to obtain the anhydrous toothpaste of the present application.

[0033] It should be noted that microcrystalline cellulose is usually used as a thickener for toothpaste with water, because in the presence of water, microcrystalline cellulose can be well dissolved, thereby ensuring toothpaste formation, ensuring toothpaste shape, and ensuring shape stability without water. In the anhydrous toothpaste system, microcrystalline cellulose is usually not used. The present application creatively improves and optimizes the preparation method, so that microcrystalline cellulose can also be used in the anhydrous system of the present application, and the toothpaste formation, paste shape and shape stability can be guaranteed without water.

[0034] In one implementation of the present application, the temperature for heating to homogenize to colloidal swelling in step (1) is 70-85°C.

[0035] In one implementation of the present application, the stirring condition in step (2) is 1000 r / min, and the stirring time is 15-25 min.

[0036] In an implementation form of the present application, the stirring condition of step (3) is 1000 r / min for 10-20 min.

[0037] In an implementation form of the present application, the preparation method further comprises, after the flavor is added and stirred uniformly in step (3), stopping the dispersion disc, scraping the plate slowly, and filling while the paste is stirred by the residual heat.

[0038] With the above technical solution, the present application has the following beneficial effects:

[0039] The anhydrous toothpaste of the present application controls the amount of glycerol to be 40% or less, which can improve the burning and irritating taste of the anhydrous toothpaste, and give the product a clean and soft brushing experience. The calcium hydrogen phosphate is used as the main abrasive, and the sodium monofluorophosphate is used as the component for repairing and remineralizing. The anhydrous environment can improve the incompatibility of the calcium-containing abrasive and the fluoride, increase the soluble fluoride concentration, ensure the tooth remineralization and repair effect, and improve the fluoride utilization rate by supplementing calcium ions and phosphate ions, thereby improving the tooth remineralization and acid erosion resistance. The microcrystalline cellulose is used as the thickening agent, which does not need to be neutralized and is resistant to high-speed shearing, thereby avoiding the damage of high-speed shearing to the paste thickening system during the paste preparation process. Moreover, the microcrystalline cellulose has good compatibility with the calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate, and calcium pyrophosphate, thereby avoiding the damage of the incompatibility of raw materials to the formula system during the whole shelf life, and improving the stability of the anhydrous toothpaste. DETAILED DESCRIPTION

[0040] The existing anhydrous toothpaste generally has poor stability and burning sensation during use. Moreover, due to the incompatibility of the calcium-containing abrasive and the fluoride, the anhydrous toothpaste has low anti-cavity effect.

[0041] To solve the above problems, the present application creatively develops a new anhydrous toothpaste, which comprises a humectant, a thickening agent, an abrasive, and an efficacy component. The humectant is composed of at least one of sorbitol, PEG 400, and propylene glycol, and glycerol. The amount of the humectant is 45-55% of the total weight of the anhydrous toothpaste, and the amount of glycerol is less than or equal to 40% of the total weight of the anhydrous toothpaste. The thickening agent comprises microcrystalline cellulose. The abrasive is composed of at least one of calcium hydrogen phosphate dihydrate and calcium pyrophosphate, and calcium hydrogen phosphate and hydrous silicon stone. The amount of calcium hydrogen phosphate is 20-25% of the total weight of the anhydrous toothpaste. The amount of hydrous silicon stone is 3-10% of the total weight of the anhydrous toothpaste. The amount of calcium hydrogen phosphate dihydrate is 0-20% of the total weight of the anhydrous toothpaste. The amount of calcium pyrophosphate is 0-18% of the total weight of the anhydrous toothpaste. The efficacy component comprises sodium monofluorophosphate and sodium phytate.

[0042] Fluoride is a recognized anticaries ingredient, in the conventional aqueous formula, calcium-containing abrasives will react with fluoride to form precipitates, thereby greatly reducing the soluble fluoride with anticaries effect. The present application research found that in the anhydrous system, calcium and phosphate and fluoride will not react, and also has good compatibility; therefore, the present application creatively proposes to use calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate and / or calcium pyrophosphate as the abrasive, sodium monofluorophosphate as the repair remineralization efficacy ingredient; so that the anhydrous toothpaste of the present application not only has the effect of cleaning and removing stains of phosphorus calcium abrasive, but also can effectively protect the tooth remineralization repair effect due to the solution of the problem of incompatibility of calcium abrasive and fluoride, thereby having better anticaries effect. The anhydrous toothpaste formula of the present application uses calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate and / or calcium pyrophosphate as the abrasive, and sodium monofluorophosphate as the repair remineralization efficacy ingredient, on the one hand, the anhydrous environment improves the incompatibility of calcium-containing abrasives (calcium hydrogen phosphate) and fluoride, increases the concentration of soluble fluoride, and ensures the tooth remineralization repair effect, on the other hand, by supplementing calcium ions and phosphate ions, the utilization rate of fluoride is improved, and the tooth remineralization and acid erosion resistance are improved as a whole.

[0043] The anhydrous toothpaste formula of the present application, unlike the conventional anhydrous toothpaste formula which needs to be neutralized and thickened by carbomer, the present application uses microcrystalline cellulose as the main thickening agent, which does not need to be neutralized and is resistant to high-speed shearing, avoiding the damage of high-speed shearing during the toothpaste preparation process to the thickening system of the paste; microcrystalline cellulose has good compatibility with calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate and calcium pyrophosphate, avoiding the destruction of the formula system due to the incompatibility of raw materials during the whole shelf life, and improving the stability of the toothpaste.

[0044] It should be noted that microcrystalline cellulose is usually used in aqueous toothpaste, not in anhydrous toothpaste; because in the presence of water, microcrystalline cellulose can be well dissolved, thereby exerting its performance. The present application research found that by improving and optimizing the preparation method, microcrystalline cellulose can also be used in the anhydrous toothpaste of the present application, and can ensure the toothpaste forming, ensure the shape and shape stability of the paste, and not out of water.

[0045] In addition, the present application research found that the burning and irritating taste of the existing anhydrous toothpaste is mainly due to the excessive amount of glycerol; therefore, the present application scientifically designs the moisturizing agent ratio, and controls the glycerol addition amount within 40%, which improves the burning and irritating taste of the conventional anhydrous formula with high addition amount of glycerol.

[0046] The present application will be further described in detail through specific examples. The following examples only further illustrate the present application and should not be construed as limiting the present application.

[0047] If not specifically indicated, the technical means used in the examples is the conventional means familiar to those skilled in the art.

[0048] Examples

[0049] The anhydrous toothpaste of the present example comprises a humectant, a thickening agent, an abrasive agent and an efficacy ingredient, as well as conventional surfactants, fragrances and additives.

[0050] The humectant of the present example is composed of at least one of sorbitol, PEG 400 and propylene glycol, and glycerol; the humectant is used in an amount of 45-55% of the total weight of the anhydrous toothpaste, wherein the amount of glycerol is less than or equal to 40% of the total weight of the anhydrous toothpaste; the thickening agent comprises microcrystalline cellulose, and can further comprise cellulose gum and / or thickening type hydrated silica; the microcrystalline cellulose is used in an amount of 0.1-2% of the total weight of the anhydrous toothpaste; the abrasive agent is composed of at least one of calcium hydrogen phosphate dihydrate, calcium pyrophosphate, and calcium hydrogen phosphate and hydrated silica; the calcium hydrogen phosphate is used in an amount of 20-25% of the total weight of the anhydrous toothpaste; the hydrated silica is used in an amount of 3-10% of the total weight of the anhydrous toothpaste; the calcium hydrogen phosphate dihydrate is used in an amount of 0-20% of the total weight of the anhydrous toothpaste; the calcium pyrophosphate is used in an amount of 0-18% of the total weight of the anhydrous toothpaste; the efficacy ingredient comprises sodium monofluorophosphate and sodium phytate, the sodium monofluorophosphate is used in an amount of 0.5-1.1% of the total weight of the anhydrous toothpaste, and the sodium phytate is used in an amount of 0.5-1.5% of the total weight of the anhydrous toothpaste.

[0051] The surfactant of the present example is sodium lauryl sulfate; the surfactant is used in an amount of 1.5-2.5% of the total weight of the anhydrous toothpaste; the fragrance is used in an amount of 0.5-2% of the total weight of the anhydrous toothpaste; the additive is sucralose and / or sodium benzoate. In addition, the anhydrous toothpaste of the present example can further comprise a biological enzyme according to needs, the biological enzyme can be at least one of papain, dextranase and lysozyme, and the present example specifically adopts lysozyme; the biological enzyme is used in an amount of 0.01-0.5% of the total weight of the anhydrous toothpaste.

[0052] According to the above formula, different anhydrous toothpastes are prepared according to the specific amount of Table 1, and a comparative test is set, which is shown in Table 1.

[0053] Table 1: Anhydrous toothpastes of different formulas (amount of each component is % of the total weight of the anhydrous toothpaste)

[0054]

[0055] The preparation method of the anhydrous toothpaste of the present example comprises:

[0056] Preparation of Comparative Examples 1 and 2: PEG 400 and propylene glycol were weighed, and carbomer was pre-dispersed in the PEG 400 and propylene glycol solution; the colloidal dispersion was added to hot glycerol (60±5℃), and stirred rapidly until the colloid was fully swollen; the uniformly mixed powder (friction agent, soluble salt) was slowly added (powder did not fly out) under low-speed stirring, and after the powder was fully wetted, the stirring speed was increased to 2000r / min, and stirring was performed for 20 min, during which the bottom powder was stirred evenly with a spoon. Stopping stirring, adding surface active agent, essence, and slowly starting stirring until the powder was fully wetted, and the stirring speed was increased to 1000r / min, and stirring was performed for about 15 min. During this period, the bottom powder was stirred evenly with a spoon. While the paste was still hot, air was extracted, and the product was filled.

[0057] Preparation of Test Examples 1 to 6: Glycerol was weighed, and microcrystalline cellulose 268 was added to the glycerol and stirred to disperse evenly; 70-85℃ heating was performed until the paste was swollen, and after cooling, other humectants were added and dispersed evenly; the uniformly mixed powder was slowly added, and after the powder was wetted, the stirring speed was controlled at 1000r / min, and stirring was performed for 20 min; essence, biological enzyme and other components were added, the stirring speed was controlled at 1000r / min, and stirring was performed for 15 min. During this period, the bottom powder was stirred evenly with a spoon. While the paste was still hot, air was extracted, and the product was filled.

[0058] The anhydrous toothpaste prepared according to Table 1 was subjected to the following tests:

[0059] 1. Stability test

[0060] The filled toothpaste was placed at room temperature, in an oven (temperature controlled at 45±2℃), and in a refrigerator (4±2℃), and at the start, one week, two weeks, one month, two months, and three months, the sensory and physicochemical indicators were tested according to GB / T 8372-2017 Toothpaste.

[0061] 2. Fluoride ion concentration test

[0062] The fluoride ion concentration of the samples at different time points and in different environments was tested according to GB / T 8372-2017 Toothpaste.

[0063] 3. Whitening test method

[0064] The whitening was tested by removing exogenous stains.

[0065] Preparation of tooth enamel samples: bovine teeth were cut into 5mm*5mm tooth enamel blocks, embedded in polymethyl methacrylate resin, and the tooth enamel surface was polished with water-wetted 180-mesh sandpaper. The tooth enamel surface was polished flat, the sample was washed with water, and the tooth enamel surface was polished smooth with water-wetted 600-mesh sandpaper.

[0066] Acid etching: immerse the enamel block in 1% hydrochloric acid, stir for 1 minute, take out and dry the residual liquid with a paper towel, then immerse in a saturated sodium carbonate solution, stir for 1 minute, take out and dry the residual liquid with a paper towel; then immerse in 1% phytic acid solution, stir for 1 minute, take out and dry the residual liquid with a paper towel.

[0067] Staining of the enamel sample: Staining solution composition: mucin 2.5 g / L, coffee 4.0 g / L, soy sauce 4.0 g / L, black tea 4.0 g / L, ferric chloride 0.05 g / L. Staining solution preparation: dissolve mucin with hot water, then add the above staining solution components, stir well, and store at 2-8°C for standby use. The shelf life of the staining solution is 3 days. The acid-etched enamel block is placed in a staining machine for staining, and the staining is continued for 12 days.

[0068] Whiteness value test of the stained enamel sample: number and mark the stained enamel blocks, measure the enamel whiteness value (L* before brushing) with a color difference meter, select enamel blocks with L* values between 30-50, and randomly divide them into groups for brushing treatment with the test substance.

[0069] Simulate the brushing process: Toothpaste slurry preparation: weigh a certain amount of toothpaste to be tested and deionized water according to the ratio of 1:1.6 (toothpaste:water), and stir to form a uniform toothpaste slurry for standby use. Place the slurry enamel block into the fixed slot of the brushing machine, with the enamel block protruding about 2 mm, and the bristles directly touching the enamel surface. The total weight of the toothbrush head and stem is 150 g. Weigh 70 g of the toothpaste slurry into the rubbing liquid bottle, fix the rubbing liquid bottle on the brushing machine, and immerse the toothpaste slurry in the enamel block. Brush back and forth 800 times, take out the enamel block, rinse it with water, and dry it.

[0070] Determine the enamel whiteness value L* after brushing.

[0071] Calculate the difference between L* values before and after brushing.

[0072] ΔL* = L* after - L* before

[0073] 4. Repair test method

[0074] The repair efficacy is determined by the enamel repair (remineralization) effect in vitro test method.

[0075] Enamel sample preparation: select bovine teeth, cut into 5mm*5mm size, and embed in dental resin. Under water cooling conditions, use a P180 grinding wheel on a grinding machine to polish the enamel surface of the tooth block to expose the surface completely, and the surface of the tooth block is level. Then use P600-6μm-1μm-0.5μm grinding wheels for polishing. The prepared tooth block is stored in deionized water for standby use.

[0076] Preparation of artificial saliva: Weigh 0.246 g of calcium nitrate, 0.122 g of potassium dihydrogen phosphate, 8.394 g of potassium chloride, 20.920 g of bis(2-hydroxyethyl) aminotris(hydroxymethyl) methane into a 1 L beaker, add 800 mL of deionized water, stir well to dissolve, then add 5 μL of 1% sodium fluoride solution, adjust the pH value to 7.0 ± 0.05 with 1 mol / L HC1. Transfer this solution to a 1 L volumetric flask and dilute to the mark with deionized water.

[0077] Preparation of demineralization solution: Weigh 5 g of citric acid into a 500 mL volumetric flask, add deionized water to 500 mL, shake well and use.

[0078] Screening of enamel specimens: The hardness of the enamel specimens was measured using a Vickers hardness tester (pressure 300 g, loading time 5 s). Four points were measured for each specimen and the average value was recorded as H0. Specimens with a hardness of 300-330 were selected and randomly divided into groups according to surface hardness, with 8 specimens in each group.

[0079] Preparation of toothpaste slurry: Weigh a certain amount of toothpaste to be tested and deionized water according to the ratio of 1:3 (toothpaste:water), stir well and avoid foam generation. At least 5 mL of toothpaste slurry is required for each enamel specimen.

[0080] Demineralization treatment: The enamel specimens were immersed in a 1% citric acid solution at a temperature of 37°C ± 2°C. A propeller was kept 5 cm above the enamel specimens at a stirring speed of 60 r / min for 30 min. Then the specimens were thoroughly washed with deionized water and dried. The hardness of the demineralized enamel was tested and the hardness value was recorded as H1.

[0081] Test cycle: The toothpaste slurry was soaked in the tooth block for 3 minutes, then the tooth block was thoroughly washed with deionized water, soaked in artificial saliva for 3 hours, then the toothpaste slurry was soaked in the tooth block for 3 minutes, and the tooth block was thoroughly washed with deionized water. Finally, the tooth block was soaked in artificial saliva overnight, and the above operation was repeated for a total of 8 cycles. Except for the washing step, the soaking treatment was carried out in a water bath at 37°C ± 2°C.

[0082] Hardness test: The hardness of the treated enamel specimens was measured using a Vickers hardness tester (pressure 300 g, loading time 5 s), and the hardness value was recorded as H2.

[0083] The hardness recovery rate R of each tooth block was calculated as (H2-H1) / (H0-H1) x 100%.

[0084] 5. Consumer test

[0085] The consumer test (taste, appearance) was conducted using a consumer blind test method.

[0086] Consumer test blind test index contains paste appearance, fragrance burst, heat when brushing, overall taste index preference score, score 1-10, the smaller the score, the lower the preference for this index, the higher the score, the higher the preference for this index.

[0087] 40 volunteers were recruited, and the researchers introduced the purpose of the test and the details of the study to the volunteers. According to the test results, the volunteers were randomly divided into 8 groups, and they brushed their teeth twice a day in the morning and evening. After 14 days, the volunteers self-evaluated their feelings after using the toothpaste.

[0088] The results of the above tests are shown in Table 2, and the detailed stability test results of some tests are shown in Table 3.

[0089] Table 2 Test results of anhydrous toothpaste

[0090] Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Test 1 Test 2 Test 3 Test 4 Stability Unstable Unstable Stable Stable Stable Stable Stable Stable Fluoride ion concentration 630 ppm 620 ppm 900 ppm 700 ppm 910 ppm 920 ppm 910 ppm 900 ppm Whitening efficacy (ΔL*) 14.2 14.5 14.2 15.8 15.7 15.1 15.7 15.2 Repair efficacy (%) 15.56 18.88 30.05 22.33 29.89 30.12 29.88 30.01 Cream appearance 7 points 6 points 8 points 8 points 8 points 9 points 9 points 9 points Fragrance burst 8 points 6 points 8 points 8 points 8 points 9 points 8 points 9 points Preference for heat when brushing 5 points 7 points 5 points 9 points 8 points 8 points 8 points 8 points Overall preference for taste 6 points 6 points 7 points 8 points 8 points 9 points 8 points 9 points

[0091] In Table 2, the stability results are the results of 3 months at room temperature, the fluoride ion concentration results are measured after 3 months in an oven at 45±2℃, and the remaining test items are tested after the toothpaste is placed at room temperature for one week; the higher the score of the heat preference when brushing, the lower the burning and irritating taste of the toothpaste.

[0092] Table 3 Test results of anhydrous toothpaste stability test 2

[0093]

[0094] Table 3 is the stability test results of anhydrous toothpaste in test 2. The stability of anhydrous toothpaste in test 1, test 3 and test 4 is equivalent to that in test 2, and is not repeated here. In Table 3, "appearance" includes product color, paste smoothness, bar formation, color stability, and liquid transparency; "paste stability" description includes paste water separation, shell removal, stability, and whether particles are precipitated, changes in transparency, etc.; "normal" means that the characteristics of the anhydrous toothpaste have not changed, and meet the normal properties of anhydrous toothpaste.

[0095] The results of Table 2 and Table 3 show that the test example toothpaste of this example has good stability for 3 months; the comparative example 1 and the comparative example 2 show unstable paste after being placed at room temperature for 3 months; the comparative example 3 and the comparative example 4 have good paste stability, but have poor performance in other aspects, for example, the comparative example 3 has low preference for heat sensation during brushing, and the comparative example 4 has low fluoride ion concentration; the microcrystalline cellulose used as the thickening agent can impart good viscosity and thixotropic properties to the toothpaste, and has better compatibility with fluoride than the carbomer; the use of calcium hydrogen phosphate and / or calcium hydrogen phosphate dihydrate, and calcium pyrophosphate and the like as the abrasive agent can impart obvious advantages to the paste appearance, fragrance burst, overall mouthfeel, and whitening effect compared with toothpaste using stone powder as the main abrasive agent; there is no obvious difference in the whitening effect with different proportions of phosphorus calcium combination, and the whitening effect is enhanced with the increase of the addition amount within the normal addition amount range; the burning sensation (irritation) of the mouth during brushing of the anhydrous toothpaste with the glycerol addition amount of 30-40% is comparable to that of the conventional aqueous toothpaste, and is obviously superior to that of the anhydrous toothpaste with the glycerol addition amount of about 50%; from the repair efficacy data, the anhydrous phosphorus calcium fluoride-containing system is obviously superior to the aqueous double phosphorus calcium system, the anhydrous stone powder system, and the anhydrous phosphorus calcium + carbomer system.

[0096] The anhydrous toothpaste of this example, which is the toothpaste of this scheme with the microcrystalline cellulose thickening, scientific design of the moisturizing agent ratio, and the phosphorus calcium fluoride-containing system, can effectively improve the paste mouthfeel, brighten the paste appearance, and synergistically promote the whitening and repair efficacy.

[0097] The above content is a further detailed description of the present application in combination with specific embodiments, and cannot be deemed to limit the specific implementation of the present application to these descriptions. For ordinary skilled persons in the technical field to which the present application belongs, some simple deductions or substitutions can be made without departing from the concept of the present application.

Claims

1. An anhydrous toothpaste, characterized in that: Including moisturizers, thickeners, abrasives, and active ingredients; The moisturizer is composed of at least one of sorbitol, PEG 400 and propylene glycol, together with glycerin; The amount of the humectant used is 45-55% of the total weight of the anhydrous toothpaste, wherein the amount of glycerin used is less than or equal to 40% of the total weight of the anhydrous toothpaste; The thickener includes microcrystalline cellulose; The friction agent is composed of at least one of calcium hydrogen phosphate dihydrate and calcium pyrophosphate, together with calcium hydrogen phosphate and hydrated silica. The amount of dicalcium phosphate used is 20-25% of the total weight of the anhydrous toothpaste; The amount of hydrated silica used is 3-10% of the total weight of the anhydrous toothpaste; The amount of the calcium hydrogen phosphate dihydrate used is 0-20% of the total weight of the anhydrous toothpaste; The amount of calcium pyrophosphate used is 0-18% of the total weight of the anhydrous toothpaste; The active ingredients include sodium monofluorophosphate and sodium phytate.

2. The anhydrous toothpaste according to claim 1, characterized in that: The amount of sodium monofluorophosphate used is 0.5-1.1% of the total weight of the anhydrous toothpaste.

3. The anhydrous toothpaste according to claim 1, characterized in that: The amount of sodium phytate used is 0.5-1.5% of the total weight of the anhydrous toothpaste.

4. The anhydrous toothpaste according to claim 1, characterized in that: The amount of microcrystalline cellulose used is 0.1-2% of the total weight of the anhydrous toothpaste.

5. The anhydrous toothpaste according to claim 1, characterized in that: The thickener also includes cellulose gum and / or thickening hydrated silica.

6. The anhydrous toothpaste according to any one of claims 1-5, characterized in that: It also includes surfactants, fragrances, and additives.

7. The anhydrous toothpaste according to claim 6, characterized in that: The surfactant is sodium lauryl sulfate.

8. The anhydrous toothpaste according to claim 7, characterized in that: The amount of surfactant used is 1.5-2.5% of the total weight of the anhydrous toothpaste.

9. The anhydrous toothpaste according to claim 6, characterized in that: The anhydrous toothpaste also includes biological enzymes.

10. The anhydrous toothpaste according to claim 9, characterized in that: The bioenzyme is at least one of papain, glucanase, and lysozyme.

11. The anhydrous toothpaste according to claim 10, characterized in that: The amount of the bio-enzyme used is 0.01-0.5% of the total weight of the anhydrous toothpaste.

12. The anhydrous toothpaste according to claim 6, characterized in that: The amount of the fragrance used is 0.5-2% of the total weight of the anhydrous toothpaste.

13. The anhydrous toothpaste according to claim 6, characterized in that: The additive is sucralose and / or sodium benzoate.

14. The method for preparing anhydrous toothpaste according to any one of claims 1-13, characterized in that: Includes the following steps, (1) Weigh out glycerin, add thickener to glycerin, stir and disperse evenly, heat to homogenize until the colloid swells, cool and add other humectants and disperse evenly; (2) Mix all components except fragrance evenly to form a mixed powder. Add the mixed powder to the mixture of microcrystalline cellulose and humectant obtained in step (1). After the mixed powder is moistened, stir evenly. (3) Add fragrance to the product of step (2) and stir evenly to obtain the anhydrous toothpaste.

15. The preparation method according to claim 14, characterized in that: In step (1), the temperature at which the homogenized material is heated to the point of swelling of the colloid is 70-85℃.

16. The preparation method according to claim 14, characterized in that: In step (2), the conditions for uniform mixing are 1000 r / min and 15-25 min.

17. The preparation method according to claim 14, characterized in that: In step (3), the conditions for uniform mixing are 1000 r / min and 10-20 min.

18. The preparation method according to any one of claims 14-17, characterized in that: It also includes adding fragrance in step (3) and stirring evenly, stopping the dispersion plate, and while the paste is still hot from stirring, slowly stirring with a scraper to remove air and filling.

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