Application of hydroxypropyl cassia gum in preparing tooth whitening agent, tooth whitening composition and anhydrous toothpaste

Abstract

The present invention provides an application of hydroxypropyl cassia gum in the preparation of a tooth whitening agent, a tooth whitening composition and anhydrous toothpaste, and relates to the technical field of toothpaste. The present invention provides an application of hydroxypropyl cassia gum in the preparation of a tooth whitening agent. The present invention also provides a tooth whitening composition, which comprises hydroxypropyl cassia gum and magnesium aluminum silicate. The hydroxypropyl cassia gum of the present invention forms an O—H…O hydrogen bond with the main functional groups contained in organic substances such as tea and coffee that stain teeth through hydroxyl groups, and a complex reaction occurs, so that the toothpaste of the present invention has the effect of reducing exogenous stains on teeth and whitening teeth.

Description

Technical Field

[0001] The invention relates to the technical field of toothpaste, in particular to application of hydroxypropyl cassia gum in preparing a tooth whitening agent, a tooth whitening composition and anhydrous toothpaste. Background Art

[0002] Traditional toothpastes are all water-based toothpastes. In the past decade, waterless toothpastes have gradually become popular. Because no water is added, the liquid ingredients in the formula are mainly glycerin, propylene glycol, and polyethylene glycol, and the free water content in the toothpaste is kept at a trace level, so the stability and effect of special functional ingredients such as bioglass, peroxide, and biological enzymes in the toothpaste can be ensured. With the increasing market demand for these special functional toothpastes, waterless toothpaste will have a leapfrog growth in the future, providing better product category support for the toothpaste industry to achieve high-quality development.

[0003] Teeth whitening problems are generally caused by exogenous tooth stains, which refer to the stains or calculus attached to the surface of people's teeth. The main reason is that there is a layer of salivary protein organic film on the surface of the teeth. This organic film is easily stained by these substances, which are usually organic substances containing conjugated chains, typically including heterocyclic atoms, carbonyl groups and benzene rings. If the stained film is not removed promptly and effectively, these stains will adhere firmly to the surface of the tooth enamel and easily develop into calculus or plaque that is more difficult to remove.

[0004] At present, the whitening schemes of teeth in the prior art include: 1. Oxidants or bleaching agents, both of which act on the surface of the teeth and react with the exogenous pigmentation on the surface, and the other part will diffuse into the pulp cavity to bleach the dentin, but once the calcium deposition is uneven, the color will be uneven after reacting with the oxidant. The other two are generally irritating and may cause tooth sensitivity. 2. Abrasives, through the physical action between the abrasive and the pigmentation on the surface of the teeth, it is caused to fall off. The physical whitening effect of the abrasive alone is limited. However, if its content is increased, the excessive friction will easily cause tooth wear, thereby causing other problems such as tooth allergy. 3. Chinese medicine composition as a whitening agent, but the color of the toothpaste prepared by adding Chinese medicine is generally darker, and long-term use is very likely to leave pigments on the toothbrush, and the paste itself is dark in color.

[0005] Therefore, there is an urgent need to develop a stable, mild and effective whitening agent that can stably exert its effect in toothpaste, help solve the problem of dentin sensitivity and promote tooth repair.

[0006] In view of this, the present invention is proposed. Summary of the invention

[0007] The object of the present invention is to provide an application of hydroxypropyl cassia gum in the preparation of a tooth whitening agent, a tooth whitening composition and anhydrous toothpaste. The hydroxypropyl cassia gum of the present invention forms an O—H…O hydrogen bond with the main functional groups contained in organic substances such as tea and coffee that stain teeth through hydroxyl groups, and a complex reaction occurs, so that the toothpaste of the present invention also has the effect of reducing exogenous stains on teeth and whitening teeth.

[0008] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0009] In a first aspect, the present invention provides a use of hydroxypropyl cassia gum in the preparation of a tooth whitening agent.

[0010] In a second aspect, the present invention provides a tooth whitening composition, comprising hydroxypropyl cassia gum and magnesium aluminum silicate.

[0011] Furthermore, the mass ratio of hydroxypropyl cassia gelatin to magnesium aluminum silicate is 1:(0.2-5), preferably 1:(1-3).

[0012] In a third aspect, the present invention provides an anhydrous toothpaste, wherein the anhydrous toothpaste comprises the following components by weight:

[0013]

[0014] Wherein, the whitening agent includes hydroxypropyl cassia gelatin, or the tooth whitening composition as described in the first aspect.

[0015] Furthermore, the anhydrous toothpaste also includes 0.3 to 3 parts of a thickener.

[0016] Preferably, the thickener comprises any one of carrageenan, polyvinyl pyrrolidone, alcohol-soluble hydroxypropyl guar gum, alcohol-soluble xanthan gum, and carbomer, or a combination of at least two thereof, preferably carrageenan and / or polyvinyl pyrrolidone.

[0017] Preferably, the mass ratio of carrageenan to polyvinyl pyrrolidone is (0.5-2):1.

[0018] Furthermore, the anhydrous toothpaste also includes 0 to 20 parts of a moisturizing agent, wherein the moisturizing agent does not include glycerin.

[0019] Preferably, the humectant comprises polyethylene glycol and / or propylene glycol, preferably a combination of polyethylene glycol and propylene glycol.

[0020] Preferably, the mass ratio of the polyethylene glycol to propylene glycol is (0.5-2):1.

[0021] Furthermore, the anhydrous toothpaste also includes 10 to 30 parts of abrasives.

[0022] Preferably, the abrasive comprises any one of hydrated silica, calcium hydrogen phosphate, calcium pyrophosphate or calcium citrate, or a combination of at least two thereof.

[0023] Furthermore, the anhydrous toothpaste also includes 1 to 3 parts of a foaming agent.

[0024] Preferably, the foaming agent comprises sodium lauryl sulfate and / or sodium lauroyl sarcosinate.

[0025] Furthermore, the anhydrous toothpaste also includes 0.3 to 2 parts of flavor.

[0026] Furthermore, the anhydrous toothpaste also includes 0.1 to 0.5 parts of sweetener.

[0027] Preferably, the sweetener includes any one of saccharin sodium, sucralose or dipotassium glycyrrhizinate, or a combination of at least two thereof.

[0028] Furthermore, the anhydrous toothpaste also includes 0.05 to 0.4 parts of preservatives.

[0029] Preferably, the preservative comprises any one of paraben, sodium benzoate or potassium sorbate, or a combination of at least two thereof.

[0030] In a fourth aspect, the present invention provides a method for preparing the anhydrous toothpaste as described in the third aspect, the preparation method comprising the following steps:

[0031] The raw materials in the anhydrous toothpaste are mixed and homogenized to obtain the anhydrous toothpaste.

[0032] Furthermore, the preparation method of the anhydrous toothpaste comprises the following steps:

[0033] dissolving fluoride, sweetener, and preservative in part of the glycerol to obtain a pre-dissolved solution;

[0034] Dispersing hydroxypropyl cassia gelatin and a thickener in a moisturizer to obtain a pre-dispersion liquid;

[0035] After preheating the remaining glycerin, add the pre-dissolved liquid and the pre-dispersed liquid, stir and let stand to obtain a toothpaste gum base;

[0036] The toothpaste base, magnesium aluminum silicate, calcium phosphosilicate, abrasive and foaming agent are mixed, and the mixture is homogenized for the first time in a vacuum environment. Then, the vacuum is turned off to inhale the flavor, and the mixture is homogenized for the second time in a vacuum environment to obtain the anhydrous toothpaste.

[0037] Preferably, the part of glycerol accounts for 30-80% of the total mass of the glycerol.

[0038] Preferably, the preheating temperature of the remaining glycerol is 55-65°C.

[0039] Preferably, the stirring speed is 800-1000 rpm, and the stirring time is 40-80 min.

[0040] Preferably, the standing time is 12 to 36 hours.

[0041] Preferably, the pressure of the first homogenization treatment is -0.098 to -0.090 MPa, the rotation speed of the first homogenization treatment is 800 to 1200 rpm, and the time of the first homogenization treatment is 20 to 40 min.

[0042] Preferably, the pressure of the second homogenization treatment is -0.095 to -0.092 MPa, the rotation speed of the second homogenization treatment is 800 to 1200 rpm, and the time of the second homogenization treatment is 10 to 20 min.

[0043] Compared with the prior art, the present invention has the following beneficial effects:

[0044] (1) The present invention finds that in addition to having a thickening effect, hydroxypropyl cassia gum can also form O—H…O hydrogen bonds with the main functional groups contained in organic substances such as tea and coffee that cause tooth staining through the hydroxyl groups, thereby causing a complexation reaction, so that the toothpaste of the present invention also has the effect of reducing exogenous tooth stains and whitening teeth.

[0045] (2) The tooth whitening composition of the present invention contains hydroxypropyl cassia gum and magnesium aluminum silicate, which cooperate with each other to have a synergistic effect. During the brushing process, they can quickly combine with tooth stains, dental plaques, and tartar on the tooth surface, and can further improve the ability to reduce exogenous tooth stains and whiten teeth.

[0046] (3) The waterless toothpaste of the present invention uses a tooth whitening composition as a whitening agent to achieve the effect of reducing exogenous tooth stains and whitening teeth; calcium phosphosilicate and fluoride are added to have the effects of preventing caries, resisting dentin sensitivity, inhibiting dental plaque, and reducing gingivitis; glycerin is used as the main component, and hydroxypropyl cassia gelatin can form a high-viscosity solution in glycerin to further improve the thickening effect and thickening stability. DETAILED DESCRIPTION

[0047] Unless otherwise defined herein, scientific and technical terms used in conjunction with the present invention shall have the meanings commonly understood by those of ordinary skill in the art. The meaning and scope of the terms should be clear, however, in the case of any potential ambiguity, the definitions provided herein take precedence over any dictionary or external definitions. In this application, unless otherwise stated, the use of "or" means "and / or". In addition, the use of the term "including" and other forms is non-limiting.

[0048] It should be noted that specific details are described in the following description to facilitate a full understanding of the present invention. However, the present invention can be implemented in a variety of other ways different from those described herein, and those skilled in the art can make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0049] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0050] In a first aspect, the present invention provides a use of hydroxypropyl cassia gum in the preparation of a tooth whitening agent.

[0051] Wherein, the structural formula of the hydroxypropyl cassia gelatin is as follows:

[0052]

[0053] Where R is H or

[0054] The present invention unexpectedly discovered that in addition to having a thickening effect, hydroxypropyl cassia gum can also form O—H…O hydrogen bonds with the main functional groups contained in organic substances such as tea and coffee that stain teeth through hydroxyl groups, resulting in a complex reaction, so that the toothpaste of the present invention also has the effect of reducing exogenous tooth stains and whitening teeth.

[0055] In a second aspect, the present invention provides a tooth whitening composition, comprising hydroxypropyl cassia gum and magnesium aluminum silicate.

[0056] In the present invention, magnesium aluminum silicate is also added to the tooth whitening composition. Magnesium aluminum silicate is a purified and modified natural mineral material with a porous interior, a large specific surface area, and high surface activity. It has excellent adsorption properties and can quickly combine with tooth stains, dental plaque, and tartar on the tooth surface during brushing, and then be removed by rinsing the mouth. Hydroxypropyl cassia gum and magnesium aluminum silicate cooperate with each other to have a synergistic effect, which is beneficial to enhance the solubility and adsorption capacity of toothpaste on tooth stains, and can reduce the impact on the stability of toothpaste formula. After the two are combined, the removal of tooth stains and plaque on teeth is significantly improved, and the tooth cleaning ability is significantly improved. While achieving the effect of tooth whitening, it avoids the damage of general whitening agents to teeth and gums.

[0057] In an optional embodiment, the mass ratio of hydroxypropyl cassia gelatin to magnesium aluminum silicate is 1:(0.2-5), for example, it can be 1:0.2, 1:0.4, 1:0.6, 1:0.8, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, 1:3.5, 1:4, 1:5, etc.

[0058] In a preferred embodiment, the mass ratio of hydroxypropyl cassia gelatin to magnesium aluminum silicate is 1:(1-3).

[0059] In the present invention, by further optimizing the ratio of hydroxypropyl cassia gelatin and magnesium aluminum silicate, the ability of the gelatin to quickly combine with stains, plaque and tartar on the tooth surface during tooth removal can be further improved, thereby further improving the effect of removing exogenous stains and whitening teeth.

[0060] In a third aspect, the present invention provides an anhydrous toothpaste, wherein the anhydrous toothpaste comprises the following components by weight:

[0061]

[0062] Wherein, the whitening agent includes hydroxypropyl cassia gelatin, or the tooth whitening composition as described in the first aspect.

[0063] In the anhydrous toothpaste, the added amount of the whitening agent is 0.5 to 5 parts, for example, it can be 0.5 parts, 1 parts, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, etc.

[0064] In the present invention, the anhydrous toothpaste contains 0.5 to 5 parts of hydroxypropyl cassia gum, or 0.5 to 5 parts of the above-mentioned tooth whitening composition containing hydroxypropyl cassia gum and magnesium aluminum silicate as a whitening agent. At this added amount, the whitening agent can fully enhance the effect of toothpaste in whitening teeth.

[0065] In the anhydrous toothpaste, the added amount of calcium phosphosilicate is 5 to 15 parts, for example, it can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc.

[0066] In the anhydrous toothpaste, the content of fluoride is 0.05 to 0.15 parts, for example, it can be 0.05 parts, 0.06 parts, 0.08 parts, 0.09 parts, 0.10 parts, 0.11 parts, 0.12 parts, 0.13 parts, 0.14 parts, 0.15 parts, etc.

[0067] In an optional embodiment, the fluoride includes any one of sodium fluoride, sodium monofluorophosphate, stannous fluoride, strontium fluoride, potassium fluoride or olaflur, or a combination of at least two thereof.

[0068] In the present invention, 5 to 15 parts of calcium phosphosilicate are added and used in combination with 0.05 to 0.15 parts of fluoride. The two cooperate with each other and synergistically enhance the efficacy of the anhydrous toothpaste in preventing caries, resisting dentin sensitivity, inhibiting dental plaque, and alleviating gingivitis.

[0069] Among them, compared with the traditional biological glass sodium calcium phosphosilicate, calcium phosphosilicate has the following three advantages:

[0070] (1) The pH value of calcium phosphosilicate ranges from 7.4 to 9.8, and the pH value of sodium calcium phosphosilicate ranges from 11 to 13; sodium calcium phosphosilicate is a strong alkaline system and is highly irritating when used in toothpaste. When acting on the human body, it will damage normal cells and tissues while repairing them. Calcium phosphosilicate materials are mild and non-irritating, and are not cytotoxic when used in toothpaste. (2) The specific surface area of ​​calcium phosphosilicate can reach more than 300㎡ / g, which is nearly 300 times that of sodium calcium phosphosilicate (specific surface area 1.5 to 2.0㎡ / g); the ultra-large specific surface area can further promote the in situ formation of hydroxyapatite, promote tooth and bone repair, and is more conducive to cell climbing and orderly tissue growth. (3) Calcium phosphosilicate can further inhibit dental plaque and reduce gingivitis.

[0071] In the anhydrous toothpaste, the content of glycerin is 50 to 70 parts, for example, it can be 50 parts, 52 parts, 55 parts, 58 parts, 60 parts, 62 parts, 65 parts, 68 parts, 70 parts, etc.

[0072] In an optional embodiment, the anhydrous toothpaste also includes 0.3 to 3 parts of a thickener, for example, 0.3 parts, 0.6 parts, 1 parts, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, 3 parts, etc.

[0073] In an optional embodiment, the thickener includes any one of carrageenan, polyvinyl pyrrolidone, alcohol-soluble hydroxypropyl guar gum, alcohol-soluble xanthan gum, and carbomer, or a combination of at least two thereof, preferably carrageenan and / or polyvinyl pyrrolidone.

[0074] In an optional embodiment, the thickener is carrageenan and / or polyvinyl pyrrolidone.

[0075] In a preferred embodiment, the thickener is a combination of carrageenan and polyvinyl pyrrolidone.

[0076] In an optional embodiment, the mass ratio of carrageenan to polyvinyl pyrrolidone is (0.5-2):1, for example, it can be 0.5:1, 0.6:1, 0.8:1, 1:1, 1.2:1, 1.4:1, 1.6:1, 1.8:1, 2:1, etc.

[0077] In an optional embodiment, the anhydrous toothpaste further includes 0 to 20 parts of a moisturizer, wherein the moisturizer does not include glycerin; for example, it may be 0 parts, 2 parts, 4 parts, 6 parts, 8 parts, 10 parts, 15 parts, 20 parts, etc.

[0078] In an alternative embodiment, the humectant comprises polyethylene glycol and / or propylene glycol.

[0079] In a preferred embodiment, the humectant is a combination of polyethylene glycol and propylene glycol.

[0080] In an optional embodiment, the mass ratio of polyethylene glycol to propylene glycol is (0.5-2):1, for example, it can be 0.5:1, 0.6:1, 0.8:1, 1:1, 1.2:1, 1.4:1, 1.6:1, 1.8:1, 2:1, etc.

[0081] In an optional embodiment, the anhydrous toothpaste further includes 10 to 30 parts of abrasives, for example, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, etc.

[0082] In an optional embodiment, the abrasive includes any one of hydrated silica, calcium hydrogen phosphate, calcium pyrophosphate or calcium citrate, or a combination of at least two thereof.

[0083] In an optional embodiment, the anhydrous toothpaste further includes 1 to 3 parts of foaming agent, for example, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, 3 parts, etc.

[0084] In an optional embodiment, the foaming agent includes sodium lauryl sulfate and / or sodium lauroyl sarcosinate.

[0085] In an optional embodiment, the anhydrous toothpaste further includes 0.3 to 2 parts of flavor, for example, 0.3 parts, 0.4 parts, 0.6 parts, 0.8 parts, 1 parts, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, etc.

[0086] In an optional embodiment, the anhydrous toothpaste further includes 0.1 to 0.5 parts of a sweetener, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, etc.

[0087] In an optional embodiment, the sweetener includes any one of saccharin sodium, sucralose or dipotassium glycyrrhizinate, or a combination of at least two thereof.

[0088] In an optional embodiment, the anhydrous toothpaste further includes 0.05 to 0.4 parts of preservatives, for example, 0.05 parts, 0.06 parts, 0.08 parts, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, etc.

[0089] In an optional embodiment, the preservative includes any one of paraben, sodium benzoate or potassium sorbate, or a combination of at least two thereof.

[0090] In a fourth aspect, the present invention provides a method for preparing the anhydrous toothpaste as described in the third aspect, the preparation method comprising the following steps:

[0091] The raw materials in the anhydrous toothpaste are mixed and homogenized to obtain the anhydrous toothpaste.

[0092] In an optional embodiment, the method for preparing the anhydrous toothpaste comprises the following steps:

[0093] dissolving fluoride, sweetener, and preservative in part of the glycerol to obtain a pre-dissolved solution;

[0094] Dispersing hydroxypropyl cassia gelatin and a thickener in a moisturizer to obtain a pre-dispersion liquid;

[0095] After preheating the remaining glycerin, add the pre-dissolved liquid and the pre-dispersed liquid, stir and let stand to obtain a toothpaste gum base;

[0096] The toothpaste base, magnesium aluminum silicate, calcium phosphosilicate, abrasive and foaming agent are mixed, and the mixture is homogenized for the first time in a vacuum environment. Then, the vacuum is turned off to inhale the flavor, and the mixture is homogenized for the second time in a vacuum environment to obtain the anhydrous toothpaste.

[0097] In an optional embodiment, the portion of glycerol accounts for 30-80% of the total mass of the glycerol, for example, it may be 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, etc.

[0098] In an optional embodiment, the preheating temperature of the remaining glycerol is 55-65°C, for example, it can be 55°C, 56°C, 57°C, 58°C, 59°C, 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, etc.

[0099] In an optional embodiment, the stirring speed is 800-1000rpm, for example, it can be 800rpm, 820rpm, 840rpm, 860rpm, 880rpm, 900rpm, 920rpm, 940rpm, 960rpm, 980rpm, 1000rpm, etc., and the stirring time is 40-80min, for example, it can be 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, 80min, etc.

[0100] In an optional embodiment, the standing time is 12 to 36 hours, for example, it can be 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24 hours, 26 hours, 28 hours, 30 hours, 32 hours, 34 hours, 36 hours, etc.

[0101] In an optional embodiment, the pressure of the first homogenization treatment is -0.098 to -0.090 MPa, for example, it can be -0.098 MPa, -0.097 MPa, -0.096 MPa, -0.095 MPa, -0.094 MPa, -0.093 MPa, -0.092 MPa, -0.091 MPa, -0.090 MPa, etc. The rotation speed of the first homogenization treatment is 800 to 1200 rpm, for example, it can be 800 rpm, 850 rpm, 900 rpm, 950 rpm, 1000 rpm, 1050 rpm, 1100 rpm, 1150 rpm, 1200 rpm, etc. The time of the first homogenization treatment is 20 to 40 min, for example, it can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, etc.

[0102] In an optional embodiment, the pressure of the second homogenization treatment is -0.095 to -0.092 MPa, for example, it can be -0.095 MPa, -0.094 MPa, -0.093 MPa, -0.092 MPa, etc., the rotation speed of the second homogenization treatment is 800 to 1200 rpm, for example, it can be 800 rpm, 850 rpm, 900 rpm, 950 rpm, 1000 rpm, 1050 rpm, 1100 rpm, 1150 rpm, 1200 rpm, etc., and the time of the second homogenization treatment is 10 to 20 min, for example, it can be 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, etc.

[0103] The present invention is further described below by way of examples. Unless otherwise specified, the materials in the examples are prepared according to existing methods or directly purchased from the market.

[0104] Example 1

[0105] This embodiment provides an anhydrous toothpaste, which comprises the following components by weight:

[0106]

[0107]

[0108] The anhydrous toothpaste is prepared by the following steps:

[0109] (1) adding a sweetener, a preservative, and a fluoride to 45 parts of glycerol and dissolving them at 65° C. within 8 hours to obtain a pre-dissolved solution;

[0110] (2) adding hydroxypropyl cassia gelatin and a thickener to a moisturizer, and then pre-dispersing at a rotation speed of 1200 rpm for 90 minutes to obtain a pre-dispersion liquid;

[0111] (3) heating the remaining glycerin to 60° C., adding the pre-dispersed liquid and the pre-dissolved liquid, and stirring at 1000 rpm for 60 min to obtain a toothpaste gum base;

[0112] (4) Cover the toothpaste base and place it at room temperature for 24 hours;

[0113] (5) adding the toothpaste base after standing to the paste making pot, and then adding magnesium aluminum silicate, calcium phosphosilicate, abrasive and foaming agent to the paste making pot, evacuating, starting stirring and scraping, and then homogenizing at a speed of 1000 rpm for 30 minutes at -0.095 MPa;

[0114] (6) Turn off the vacuum and inhale the essence;

[0115] (7) Turn on the vacuum, and continue homogenizing at -0.095 MPa and 1000 rpm for 15 min to obtain a finished paste; the finished paste is poured into a toothpaste tube.

[0116] Example 2

[0117] This embodiment provides an anhydrous toothpaste, which comprises the following components by weight:

[0118]

[0119]

[0120] The anhydrous toothpaste is prepared by the following steps:

[0121] (1) adding a sweetener, a preservative, and a fluoride to 50 parts of glycerol and dissolving them at 65° C. within 8 hours to obtain a pre-dissolved solution;

[0122] (2) adding hydroxypropyl cassia gelatin and a thickener to a moisturizer, and then pre-dispersing at a rotation speed of 1200 rpm for 90 minutes to obtain a pre-dissolved solution;

[0123] (3) heating the remaining glycerol to 60° C., adding the pre-dispersed liquid and the pre-dissolved liquid, and stirring at 1000 rpm for 60 min to obtain a toothpaste gum base;

[0124] (4) Cover the toothpaste base and place it at room temperature for 24 hours;

[0125] (5) adding the toothpaste base after standing to the paste making pot, and then adding magnesium aluminum silicate, calcium phosphosilicate, abrasive and foaming agent to the paste making pot, evacuating, starting stirring and scraping, and then homogenizing at a speed of 1000 rpm for 30 minutes at -0.095 MPa;

[0126] (6) Turn off the vacuum and inhale the essence;

[0127] (7) Turn on the vacuum, and continue homogenizing at -0.096 MPa and 1000 rpm for 15 min to obtain a finished paste; the finished paste is poured into a toothpaste tube.

[0128] Example 3

[0129] This embodiment provides an anhydrous toothpaste, which comprises the following components by weight:

[0130]

[0131]

[0132] The anhydrous toothpaste is prepared by the following steps:

[0133] (1) adding a sweetener, a preservative, and a fluoride to 40 parts of glycerol and dissolving them at 65° C. within 8 hours to obtain a pre-dissolved solution;

[0134] (2) adding hydroxypropyl cassia gelatin and a thickener to a moisturizer, and then pre-dispersing at a rotation speed of 1200 rpm for 90 minutes to obtain a pre-dissolved solution;

[0135] (3) heating the remaining glycerin to 60° C., adding the pre-dispersed liquid and the pre-dissolved liquid, and stirring at 1000 rpm for 60 min to obtain a toothpaste gum base;

[0136] (4) Cover the toothpaste base and place it at room temperature for 24 hours;

[0137] (5) adding the toothpaste base after standing to the paste making pot, and then adding magnesium aluminum silicate, calcium phosphosilicate, abrasive and foaming agent to the paste making pot, evacuating, starting stirring and scraping, and then homogenizing at a speed of 1000 rpm for 30 minutes at -0.095 MPa;

[0138] (6) Turn off the vacuum and inhale the essence;

[0139] (7) Turn on the vacuum, and continue homogenizing at -0.095 MPa and 1000 rpm for 15 min to obtain a finished paste; the finished paste is poured into a toothpaste tube.

[0140] Example 4

[0141] This embodiment provides an anhydrous toothpaste, which is different from Example 1 only in that the content of hydroxypropyl cassia gelatin is reduced to 0.5 parts, and the content of magnesium aluminum silicate is reduced to 0.3 parts. Other components, contents and preparation methods are exactly the same as those in Example 1.

[0142] Example 5

[0143] This embodiment provides an anhydrous toothpaste, which is different from Example 1 only in that the content of hydroxypropyl cassia gelatin is reduced to 0.5 parts, and the content of magnesium aluminum silicate is increased to 1.8 parts. Other components, contents and preparation methods are exactly the same as those in Example 1.

[0144] Example 6

[0145] This comparative example provides an anhydrous toothpaste, which differs from Example 1 only in that magnesium aluminum silicate is not added, and the content of hydroxypropyl cassia gelatin is increased to 1 part. Other components, contents and preparation methods are completely consistent with those in Example 1.

[0146] Example 7

[0147] This embodiment provides an anhydrous toothpaste, which is different from the embodiment 1 only in that no fluoride is added, the content of calcium phosphosilicate is increased to 10.1 parts, and the other components, contents and preparation methods are completely consistent with those in the embodiment 1.

[0148] Example 8

[0149] This embodiment provides an anhydrous toothpaste, which is different from Embodiment 1 only in that the glycerol content is reduced to 50 parts and the propylene glycol content is increased to 12 parts. The other components, contents and preparation methods are completely consistent with those in Embodiment 1.

[0150] Example 9

[0151] This embodiment provides an anhydrous toothpaste, which is different from Embodiment 1 only in that the moisturizing agent is 4 parts of propylene glycol, and the other components, contents and preparation methods are exactly the same as those in Embodiment 1.

[0152] Example 10

[0153] This embodiment provides an anhydrous toothpaste, which is different from the embodiment 1 only in that the moisturizing agent is 4 parts of polyethylene glycol 600, and the other components, contents and preparation methods are completely consistent with those in the embodiment 1.

[0154] Embodiment 11

[0155] This embodiment provides an anhydrous toothpaste, which is different from Embodiment 1 only in that the thickener is 0.5 parts of carrageenan and 0.5 parts of carbomer, and the other components, contents and preparation methods are exactly the same as those in Embodiment 1.

[0156] Example 12

[0157] This embodiment provides an anhydrous toothpaste, which is different from Embodiment 1 only in that the thickener is 0.5 parts of xanthan gum and 0.5 parts of hydroxypropyl guar gum, and the other components, contents and preparation methods are exactly the same as those in Embodiment 1.

[0158] Comparative Example 1

[0159] This comparative example provides an anhydrous toothpaste, which differs from Example 1 only in that hydroxypropyl cassia gelatin is not added, and the content of aluminum magnesium silicate is increased to 1 part. Other components, contents and preparation methods are exactly the same as those in Example 1.

[0160] Comparative Example 2

[0161] This comparative example provides an anhydrous toothpaste, which is different from Example 1 only in that hydroxypropyl cassia gelatin is not added, the content of hydrated silica is increased to 20.7 parts, and other components, contents and preparation methods are completely consistent with those in Example 1.

[0162] Comparative Example 3

[0163] This comparative example provides an anhydrous toothpaste, which is different from Example 1 only in that hydroxypropyl cassia gelatin is replaced with an equal mass of sodium sulfite, and other components, contents and preparation methods are completely consistent with those in Example 1.

[0164] Comparative Example 4

[0165] This comparative example provides an anhydrous toothpaste, which is different from Example 1 only in that hydroxypropyl cassia gelatin is replaced with an equal mass of hydrogen peroxide, and other components, contents and preparation methods are completely consistent with those in Example 1.

[0166] Comparative Example 5

[0167] This comparative example provides an anhydrous toothpaste, which is different from Example 1 only in that hydroxypropyl cassia gelatin is replaced with an equal mass of xylanase, and other components, contents and preparation methods are completely consistent with those in Example 1.

[0168] Comparative Example 6

[0169] This comparative example provides an anhydrous toothpaste, which is different from Example 1 only in that hydroxypropyl cassia gelatin is replaced with an equal mass of sodium phytate, and other components, contents and preparation methods are completely consistent with those in Example 1.

[0170] Test Example 1

[0171] In vitro whitening effect simulation test

[0172] Test samples: the anhydrous toothpaste samples and blank control toothpaste provided in Examples 1 to 12, and the anhydrous toothpaste samples and blank control toothpaste provided in Comparative Examples 1 to 6.

[0173] Test method:

[0174] (1) Preparation of dye solution: Weigh 2 g of black tea and 1 g of gastric mucin, add 200 mL of hot water to brew, and filter out the tea leaves with filter paper after the tea has cooled. Then add 2 g of coffee and 5 mL of soy sauce to the filtered and cooled tea and fully dissolve and mix.

[0175] (2) Staining: Immerse the tooth in the prepared staining solution. After staining, rinse the staining solution off the surface and dry it to ensure that the color adheres firmly. After staining, use a spectrophotometer to measure the whiteness value (L 1 *).

[0176] (3) Toothbrushing: Weigh a certain amount of the toothpaste to be tested and deionized water in a ratio of 1:1.6 (toothpaste: water), stir evenly to form a toothpaste slurry for use. The preparation method of the control toothpaste slurry is the same. Set the reciprocating frequency of the brush grinder to 100r / min, add an appropriate amount of the toothpaste slurry to be tested to each slurry cup so that it immerses the tooth module. Start the machine and brush your teeth back and forth 800 times. After finishing, rinse and wipe off the surface moisture, and measure the whiteness value (L) of the teeth within 10 minutes. 2 *).

[0177] The specific test results are shown in Table 1:

[0178] Table 1

[0179]

[0180]

[0181] As shown in Table 1, the ΔL* value of each sample toothpaste is greater than the ΔL* value of the control group toothpaste, and the comparison of the ΔL* values ​​of the two groups is statistically significant (P<0.05), which shows that the toothpaste of the present invention has the effect of reducing exogenous stains on teeth and whitening teeth. In particular, from the comparison of Example 1 and Comparative Examples 1 to 6, it can be seen that the application of the hydroxypropyl cassia gum in the preparation of tooth whitening agents has a whitening effect that is significantly better than that of other whitening agents.

[0182] Test Example 2

[0183] Actual test of stain removal and whitening effect

[0184] Test samples: the anhydrous toothpaste samples provided in Examples 1 to 12 and the anhydrous toothpaste samples provided in Comparative Examples 1 to 6.

[0185] Test method: Volunteers were divided into 18 groups, with 10 people in each group. They used the above samples to brush their teeth, once in the morning and once in the evening every day. The stain index LSI was tested before use and after continuous use for 3 months.

[0186] LSI scoring method, the specific scoring rules are as follows:

[0187] 0 points - no stains are present;

[0188] 1 point: The stain size does not exceed 1 / 3 of the tooth surface; the degree is mild stain (yellow or brown);

[0189] 2 points: the stain size does not exceed 2 / 3 of the tooth surface; the degree is moderate stain (medium brown);

[0190] 3 points: The stain is larger than 2 / 3 of the tooth surface; the degree of stain is severe (dark brown or black).

[0191] The LSI values ​​of the subjects before use and after 3 months of use were counted, the average LSI values ​​before use and after 3 months of use were calculated, and then the LSI reduction rate of the pigmentation index was calculated.

[0192] The reduction rate of the stain index LSI (%) = [average LSI before use - average LSI after 3 months of use] / average LSI before use × 100%.

[0193] The specific test results are shown in Table 2:

[0194] Table 2

[0195]

[0196] As shown in Table 2, after using the whitening and anti-caries toothpaste of Examples 1 to 12 for 3 months, the LSI value is significantly reduced, reaching more than 26%, indicating that the anhydrous toothpaste provided by the present invention has the effect of reducing exogenous stains on teeth and whitening teeth. In particular, from the comparison between Example 1 and Comparative Examples 1 to 6, it can be seen that the application of the hydroxypropyl cassia gum in the preparation of tooth whitening agents has a significantly better whitening effect than other whitening agents.

[0197] Test Example 3

[0198] Allergy test

[0199] Test samples: the anhydrous toothpaste samples provided in Examples 1 to 12 and the anhydrous toothpaste samples provided in Comparative Examples 1 to 6;

[0200] Test method:

[0201] (1) Preparation of dentin slices: Select freshly extracted bovine teeth without cracks or damage, clean them thoroughly and store them in formaldehyde solution for later use. Cut to obtain a flat dentin exposure area with a thickness of 2 to 3 mm. Polish the dentin slice to form a uniform, flat and smooth surface, and clean it with pure water ultrasonically. Place the dentin in 10% citric acid for 2 minutes, rinse with a large amount of pure water and then clean it with ultrasonic waves. The etching step is repeated 3 times to obtain a dentin slice with open dentinal tubules.

[0202] (2) Fix the dentin slices on a glass slide, place 0.2g of the corresponding test sample on each dentin slice, evenly apply it on the surface of the dentin slice, moisten it with pure water, scrub it with a toothbrush for 2 minutes, let it stand for 2 minutes, and gently rinse it with pure water to remove the test sample on the surface. The dentin slices in the control group were only scrubbed with a toothbrush dipped in pure water, scrubbed with a toothbrush for 2 minutes, and let it stand for 2 minutes. After treatment, the dentin slices were stored in artificial saliva and stored in a constant temperature water bath at 37°C. Continuously scrub for 7 days, twice a day.

[0203] (3) After the dentin slices were dried, three different areas of each dentin slice were randomly selected for observation using a scanning electron microscope (SEM) (magnification was 2000 times). The area of ​​the unplugged area of ​​the dentinal tubules was calculated, and then the plugging rate (Plugging rate, PR) of the dentinal tubules in each experimental group was calculated. Plugging rate (PR, %) = (open dentinal tubule area of ​​the control group - open dentinal tubule area of ​​the experimental group) / open dentinal tubule area of ​​the control group.

[0204] The specific test results are shown in Table 3:

[0205] Table 3

[0206]

[0207]

[0208] As shown in Table 3 above, the occlusion rate of dentinal tubules was calculated by image analysis, and the results showed that the unoccluded area of ​​dentinal tubules in the experimental group was significantly smaller than that in the control group, and was statistically significant (P<0.05). The waterless toothpaste of the present invention has a good anti-allergic effect, plays a good anti-allergic analgesic and stabilizing effect, and relieves the symptoms of dentin sensitivity, or even eliminates them.

[0209] Test Example 4

[0210] Caries (Enamel Restoration) Test

[0211] Test samples: the anhydrous toothpaste samples provided in Examples 1 to 12 and the anhydrous toothpaste samples provided in Comparative Examples 1 to 6.

[0212] Test method:

[0213] (1) Demineralization: Select fresh calf front teeth without cracks, caries, or stains, cut, clean, polish, and set aside. Treat the ex vivo bovine teeth with 1% lactic acid solution twice a day for 2 minutes each time for a total of 2 weeks, and place them in 37°C artificial saliva during the interval.

[0214] (2) Remineralization: Apply the solution on a toothbrush and use a toothbrush to brush the pretreated ex vivo tooth slices for 2 minutes, twice a day for 2 weeks. During the intermittent period, place the slices in artificial saliva at 37°C.

[0215] (3) The enamel repair effect was evaluated by hardness measurement test. In order to evaluate the effect of the test samples (prepared toothpaste) in the embodiments and comparative examples on the surface hardness of teeth, the surface hardness of the isolated tooth slices was measured by Vickers hardness tester (VH1102, Buehler).

[0216] The test results are shown in Table 4 below:

[0217] Table 4

[0218]

[0219]

[0220] As shown in Table 4 above, after using the anhydrous toothpaste of the present invention for 2 weeks, the surface hardness of the tooth pieces increased significantly, which fully demonstrates that the anhydrous toothpaste of the present invention can effectively release calcium and phosphorus ions, thereby promoting tooth repair.

[0221] Test Example 5

[0222] Test for inhibiting dental plaque and alleviating gingivitis

[0223] Test samples: the anhydrous toothpaste samples and blank toothpaste provided in Examples 1 to 12, and the anhydrous toothpaste samples and blank toothpaste provided in Comparative Examples 1 to 6.

[0224] Test method:

[0225] Volunteer subjects who met the criteria were selected and divided into 18 groups, each of which was divided into a test group and a control group, and the toothpaste of the present invention was used respectively. The method of use was: brush teeth once in the morning and evening every day, each time for at least 3 minutes, for 3 consecutive months. After using the toothpaste and toothbrush for 1.5 months and 3 months, the subjects' dental plaque and gingivitis conditions were re-evaluated according to the baseline examination procedure.

[0226] (1) Plaque index (PI) and inspection method:

[0227] Supragingival plaque was evaluated using the Quigley-Hein modified Turesky plaque index. Supragingival plaque was stained and recorded according to the following criteria:

[0228] 0 = no plaque;

[0229] 1 = scattered plaque is present at the cervical margin;

[0230] 2 = a continuous thin band of plaque (up to 1 mm wide) is visible at the cervical margin;

[0231] 3 = The plaque zone at the cervical part of the tooth is larger than 1 mm but less than 1 / 3 of the tooth surface;

[0232] 4 = plaque covers 1 / 3 to 2 / 3 of the tooth surface;

[0233] 5 = Plaque covers more than 2 / 3 of the tooth surface.

[0234] (2) Gingivitis Index (GI) and examination methods:

[0235] Gingivitis was measured using the modified Loe-Silness gingivitis index, which measured gingival condition before staining to measure plaque index. The gingivitis counting method and standard are as follows:

[0236] 0 = no gingivitis;

[0237] 1 = mild gingivitis, with slight changes in gum color and texture, but no bleeding on probing;

[0238] 2 = moderate inflammation, the gums are shiny, red, swollen, hyperplastic, and bleeding on probing;

[0239] 3 = Severe inflammation, with obvious redness and hyperplasia of the gums, and spontaneous bleeding.

[0240] Evaluation criteria:

[0241] The comparison of the final values ​​of various indicators between the control group and the experimental group should meet the requirement of (control - experimental) / control ≥ 12% and be statistically significant.

[0242] The examination results show that there is no statistically significant difference in the baseline indicators of gender, average age, gingivitis index and plaque index between the test group and the control group, and the baselines are comparable. The specific test results are shown in Table 5 below:

[0243] Table 5

[0244]

[0245]

[0246]

[0247] As shown in Table 5 above, after using the waterless toothpaste of the present invention for 3 months, the gingival index (GI) and plaque index (PLI) were significantly reduced, and the difference was statistically significant, which fully demonstrated that the waterless toothpaste of the present invention can effectively prevent and treat gingivitis, reduce gingival inflammation, gingival bleeding, and gingival swelling and pain.

[0248] Test Example 6

[0249] Physical and chemical indicators, microbiological indicators testing

[0250] Test sample: the anhydrous toothpaste sample provided in Example 1.

[0251] Test method:

[0252] Physical and chemical indexes and microbiological indexes were tested according to the requirements of the test standard "Toothpaste (GB / T 8372-2017)". Evaluators with relevant sensory evaluation experience were selected to conduct a test brushing evaluation on the taste of the toothpaste; at the same time, the sample toothpaste was subjected to shelf stability observation in a 45℃ oven and a -18℃ refrigerator.

[0253] Among them, the quality index and test standard comparison table of anhydrous toothpaste samples are shown in Table 6 below:

[0254] Table 6

[0255]

[0256]

[0257] Among them, the sensory evaluation of the anhydrous toothpaste samples is shown in Table 7 below:

[0258] Table 7

[0259]

[0260] From the quality index test results in Tables 6 to 7, it can be seen that the sample toothpaste has met the requirements of the test standard "Toothpaste (GB / T8372-2017)". From the sensory evaluation results in Table 7, it can be seen that the sample toothpaste has a moderate consistency, has the unique heating feeling of anhydrous toothpaste, can be quickly dispersed in the mouth, has a clean mouthfeel after brushing, and has a long-lasting fragrance. At the same time, the sample toothpaste has been tested in a 45℃ oven for 3 months and in a -8℃ refrigerator for 1 month. After returning to room temperature, there is no abnormality in the paste, and the stability meets the requirements of mass production.

[0261] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. Application of hydroxypropyl cassia gel in the preparation of a tooth whitening agent.

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