Refreshing and whitening toothpaste and preparation method thereof
By combining sodium dihydrogen pyrophosphate, hydrated silica, and color-correcting particles, this refreshing whitening toothpaste solves the safety and insignificant effects of existing teeth whitening methods, achieving highly efficient and long-lasting teeth whitening and stain removal while reducing the risk of teeth yellowing.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-28
- Publication Date
- 2026-04-21
AI Technical Summary
Existing teeth whitening methods have problems such as high safety risks, insignificant effects or poor compliance, especially limited effectiveness against deep intrinsic staining, and difficulty in maintaining teeth whiteness in the long term.
This refreshing whitening toothpaste combines a triple whitening approach: softening stains with disodium dihydrogen pyrophosphate, physical abrasion with hydrated silica, optical color correction with color-fixing particles, and forming a color-locking film after whitening. It also uses PVM/MA copolymer to prevent stains and reduce the risk of teeth yellowing.
It achieves highly efficient and long-lasting teeth whitening effects, significantly removes extrinsic and intrinsic stains, reduces the risk of teeth yellowing, and forms a color-locking film after use to maintain whiteness. It is also non-irritating to the oral cavity and has a high safety profile.
Smart Images
Figure SMS_1 
Figure SMS_2 
Figure SMS_3
Abstract
Description
Technical Field
[0001] This invention relates to the field of toothpaste technology, and in particular to a refreshing and whitening toothpaste and its preparation method. Background Technology
[0002] The color and appearance of teeth are important components of oral health and facial aesthetics. Naturally healthy teeth have a translucent, slightly yellowish to light yellow hue, primarily due to the optical effect of the color of the inner dentin showing through the outer translucent enamel. However, various intrinsic and extrinsic factors can cause tooth discoloration. For example, long-term consumption of coffee, tea, red wine, and tobacco can lead to pigment deposition (extrinsic staining); while changes in the color of the tooth's internal structure can be caused by tetracycline antibiotics, excessive fluoride intake, pulp necrosis, and age-related changes (intrinsic staining). Darkening or unevenness in tooth color not only affects personal appearance and social confidence but may also reflect, to some extent, oral hygiene conditions or historical health problems.
[0003] Currently, the teeth whitening method used on the market is chemical oxidation-reduction bleaching, with hydrogen peroxide or its precursors (such as silicon peroxide) as the representative active ingredient. The principle is that low-molecular-weight hydrogen peroxide penetrates into the enamel and even dentin, decomposing to produce highly reactive free radicals (such as hydroxyl radicals). These free radicals, through oxidation-reduction reactions, break down the complex macromolecular staining substances inside the teeth (usually containing conjugated double-bonded chromophores) into colorless small molecules, thereby achieving the purpose of decolorization. The whitening effect of chemical bleaching methods based on hydrogen peroxide is positively correlated with drug concentration, duration of action, and treatment frequency. However, while high-concentration hydrogen peroxide can take effect quickly, it significantly increases the risk of causing changes in the microstructure of the enamel surface, mineral loss, tooth sensitivity (pain from hot and cold stimuli), and chemical burns to the gingival soft tissue. While low-concentration products are safer, they often require a long period to show results, leading to poor patient compliance. Furthermore, they have limited effectiveness for deep, stubborn intrinsic staining (such as moderate to severe tetracycline staining), and color rebound is common after discontinuation.
[0004] Therefore, how to achieve a new whitening method that is efficient, long-lasting, and more biocompatible is an urgent problem to be solved. Summary of the Invention
[0005] To address the aforementioned technical problems, this invention provides a refreshing whitening toothpaste and its preparation method. By combining three whitening methods, it achieves teeth whitening and forms a color-locking film on the whitened tooth surface to prevent stains and reduce the risk of teeth yellowing.
[0006] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a refreshing whitening toothpaste, the raw materials of which include hydrated silica, disodium dihydrogen pyrophosphate, PVM / MA copolymer, color-correcting particles and additives; the color-correcting particles include mannitol, microcrystalline cellulose, CI 74160, cetyl alcohol, corn starch, ethyl cellulose and hydroxypropyl methyl cellulose.
[0007] In this invention, disodium dihydrogen pyrophosphate softens stains, chemically adsorbs and removes color, hydrated silica physically rubs the softened stains and unadsorbed spots, and color-correcting particles are added to correct color through optical principles. By combining these three methods, teeth whitening is achieved through multiple approaches. Furthermore, PVM / MA copolymer is added to form a color-locking film at the whitened interface, preventing stains and reducing the risk of teeth yellowing.
[0008] Preferably, the hydrated silica includes hydrated silica with a water absorption capacity of (0.85-1) mL / g, hydrated silica with a water absorption capacity of (2.4-2.6) mL / g, and hydrated silica with an oil absorption capacity of (0.4-1) mL / g. The (0.85-1) mL / g can be, for example, 0.85 mL / g, 0.90 mL / g, 0.95 mL / g, or 1 mL / g. The (2.4-2.6) mL / g can be, for example, 2.4 mL / g, 2.45 mL / g, 2.5 mL / g, 2.55 mL / g, or 2.6 mL / g. The (0.4-1) mL / g can be, for example, 0.4 mL / g, 0.5 mL / g, 0.6 mL / g, 0.7 mL / g, 0.8 mL / g, 0.9 mL / g, or 1 mL / g, etc.
[0009] Preferably, the ingredients of the refreshing whitening toothpaste, by weight, include 15-20 parts hydrated silica, 0.5-3 parts disodium dihydrogen pyrophosphate, 0.01-0.1 parts PVM / MA copolymer, 0.1702-0.77 parts color-correcting particles, and 71.2217-95.5345 parts additives. The 15-20 parts can be, for example, 15, 16, 17, 18, 19, or 20 parts. The 0.5-3 parts can be, for example, 0.5, 1, 1.5, 2, 2.5, or 3 parts. The 0.01-0.1 parts can be, for example, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, or 0.1 parts. The 0.1702-0.77 parts can be, for example, 0.1702 parts, 0.2 parts, 0.25 parts, 0.3 parts, 0.35 parts, 0.4 parts, 0.45 parts, 0.5 parts, 0.55 parts, 0.6 parts, 0.65 parts, 0.7 parts, 0.75 parts, or 0.77 parts, etc. The 71.2217-95.5345 parts can be, for example, 71.2217 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, or 95.5345 parts, etc.
[0010] Preferably, the color-correcting particles comprise, by weight, 0.1-0.5 parts mannitol, 0.05-0.1 parts microcrystalline cellulose, 0.01-0.1 parts CI 74160, 0.005-0.03 parts cetyl alcohol, 0.005-0.03 parts corn starch, 0.0001-0.005 parts ethyl cellulose, and 0.0001-0.005 parts hydroxypropyl methylcellulose. The 0.1-0.5 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts. The 0.05-0.1 parts can be, for example, 0.05 parts, 0.06 parts, 0.07 parts, 0.08 parts, 0.09 parts, or 0.1 parts. The 0.01-0.1 parts can be, for example, 0.01 parts, 0.02 parts, 0.04 parts, 0.06 parts, 0.08 parts, or 0.1 parts, etc. The 0.005-0.03 parts can be, for example, 0.005 parts, 0.01 parts, 0.015 parts, 0.02 parts, 0.025 parts, or 0.03 parts, etc. The 0.0001-0.005 parts can be, for example, 0.0001 parts, 0.001 parts, 0.002 parts, 0.003 parts, 0.004 parts, or 0.005 parts, etc.
[0011] Preferably, the additives include any one or a combination of at least two of the following: humectants, solvents, foaming agents, fragrances, thickeners, oral care agents, taste modifiers, preservatives, pH adjusters, or colorants.
[0012] Preferably, the additives, by weight, comprise any one or a combination of at least two of the following: 31-41 parts humectant, 38-43 parts solvent, 1.121-4.43 parts foaming agent, 0.5-3 parts fragrance, 0.2005-1.803 parts thickener, 0.1-0.8 parts oral care agent, 0.1-0.5 parts taste improver, 0.1-0.5 parts preservative, 0.1-0.5 parts pH adjuster, or 0.0002-0.0015 parts colorant. The 31-41 parts can be, for example, 31, 32, 34, 36, 38, 40, or 41 parts. The 1.121-4.43 parts can be, for example, 1.121, 1.5, 2, 2.5, 3, 3.5, 4, or 4.43 parts. The 0.5-3 parts can be, for example, 0.5 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts, or 3 parts, etc. The 0.2005-1.803 parts can be, for example, 0.2005 parts, 0.4 parts, 0.6 parts, 0.8 parts, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, or 1.803 parts, etc. The 0.1-0.8 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, or 0.8 parts, etc. The 0.1-0.5 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts, etc. The 0.0002-0.0015 parts can be, for example, 0.0002 parts, 0.0004 parts, 0.0006 parts, 0.0008 parts, 0.001 parts, 0.0012 parts, 0.0014 parts, or 0.0015 parts, etc.
[0013] Preferably, the humectant comprises any one or a combination of at least two of sorbitol, xylitol, or polyethylene glycol-8, consisting of 30-35 parts. The 30-35 parts can be, for example, 30, 31, 32, 33, 34, or 35 parts. The 0.5-3 parts can be, for example, 0.5, 1, 1.5, 2, 2.5, or 3 parts.
[0014] Preferably, the solvent includes water.
[0015] Preferably, the foaming agent comprises any one or a combination of at least two of the following: sodium lauryl sulfate, 0.1-1 part cocamidopropyl betaine, 0.01-0.3 parts sodium chloride, 0.001-0.03 parts sodium benzoate, or 0.01-0.1 parts cetylpyridinium chloride. The 1-3 parts can be, for example, 1 part, 1.5 parts, 2 parts, 2.5 parts, or 3 parts. The 0.1-1 part can be, for example, 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, or 1 part. The 0.01-0.3 parts can be, for example, 0.01 part, 0.05 part, 0.1 part, 0.15 part, 0.2 part, 0.25 part, or 0.3 parts. The 0.001-0.03 parts can be, for example, 0.001 parts, 0.005 parts, 0.01 parts, 0.015 parts, 0.02 parts, 0.025 parts, or 0.03 parts, etc. The 0.01-0.1 parts can be, for example, 0.01 parts, 0.02 parts, 0.04 parts, 0.06 parts, 0.08 parts, or 0.1 parts, etc.
[0016] Preferably, the fragrance agent comprises 0.5-3 parts of fragrance. The 0.5-3 parts can be, for example, 0.5 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts, or 3 parts, etc.
[0017] Preferably, the thickener comprises any one or a combination of at least two of the following: 0.1-1 parts cellulose gum, 0.1-0.8 parts xanthan gum, or 0.0005-0.003 parts lecithin. The 0.1-1 parts can be, for example, 0.1 parts, 0.2 parts, 0.4 parts, 0.6 parts, 0.8 parts, or 1 part. The 0.1-0.8 parts can be, for example, 0.1 parts, 0.2 parts, 0.4 parts, 0.6 parts, or 0.8 parts. The 0.0005-0.003 parts can be, for example, 0.0005 parts, 0.001 parts, 0.002 parts, or 0.003 parts.
[0018] Preferably, the oral care agent comprises 0.1-0.8 parts of zinc citrate. The 0.1-0.8 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, or 0.8 parts, etc.
[0019] Preferably, the taste improver comprises 0.1-0.5 parts of sodium saccharin. The 0.1-0.5 parts may be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts.
[0020] Preferably, the preservative includes 0.1-0.5 parts of sodium benzoate. The 0.1-0.5 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts.
[0021] Preferably, the pH adjuster comprises 0.1-0.5 parts of sodium hydroxide. The 0.1-0.5 parts can be, for example, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts.
[0022] Preferably, the colorant comprises 0.0001-0.001 parts of CI 17200 and / or 0.0001-0.0005 parts of CI 42051. The 0.0001-0.001 parts can be, for example, 0.0001 parts, 0.0002 parts, 0.0004 parts, 0.0006 parts, 0.0008 parts, or 0.001 parts, etc. The 0.0001-0.0005 parts can be, for example, 0.0001 parts, 0.0002 parts, 0.0003 parts, 0.0004 parts, or 0.0005 parts, etc.
[0023] In a second aspect, the present invention provides a method for preparing the refreshing whitening toothpaste according to the first aspect, the method comprising stirring hydrated silica, disodium dihydrogen pyrophosphate, PVM / MA copolymer, color-correcting particles and additives to obtain the toothpaste.
[0024] Preferably, the preparation method further includes pretreatment.
[0025] Preferably, the pretreatment includes mixing a solvent, disodium dihydrogen pyrophosphate, flavoring agent, taste modifier, preservative, pH adjuster, lecithin, PVM / MA copolymer, cetylpyridinium chloride and colorant to obtain raw material 1, and mixing hydrated silica, cellulose gum, oral care agent and other foaming agents except cetylpyridinium chloride to obtain raw material 2.
[0026] Preferably, the preparation method includes mixing raw material 1 with a humectant other than xylitol, adding xanthan gum and mixing, then adding raw material 2 and mixing, and finally adding xylitol and color correction particles to obtain the final product.
[0027] Compared with the prior art, the present invention has at least the following beneficial effects: In this invention, disodium dihydrogen pyrophosphate softens stains, chemically adsorbs and removes color, hydrated silica physically rubs the softened stains and unadsorbed spots, and color-correcting particles are added for optical color correction. Combining these three methods achieves teeth whitening through multiple approaches. Furthermore, the addition of PVM / MA copolymer forms a color-locking film at the whitened interface, preventing stains and reducing the risk of yellowing. Experiments have shown that this fresh-smelling whitening toothpaste has a breath-freshening effect, significantly lowering the oral cavity temperature by 4.5°C, and is non-irritating to the oral mucosa, demonstrating high safety. Detailed Implementation
[0028] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.
[0029] The reagents used in the following examples were sourced from the following sources: Disodium dihydrogen pyrophosphate: Jiangsu Debang Duoling Health Technology Co., Ltd. PVM / MA copolymer: Ashland LLC; Mannitol: Chongqing Xiaowan Biotechnology Co., Ltd.; Microcrystalline cellulose: Chongqing Xiaowan Biotechnology Co., Ltd.; CI 74160: Chongqing Xiaowan Biotechnology Co., Ltd.; Cetyl alcohol: Chongqing Xiaowan Biotechnology Co., Ltd.; Corn starch: Chongqing Xiaowan Biotechnology Co., Ltd.; Ethyl cellulose: Chongqing Xiaowan Biotechnology Co., Ltd.; Hydroxypropyl methylcellulose: Chongqing Xiaowan Biotechnology Co., Ltd.; CI 17200: Sensient Cosmetic Technologies, UNICERT RED K7057-J; CI 42051: Neelikon Food Dyes and Chemicals Ltd., NEELICOL PATENT BLUEV; Fragrance: Givaudan Fragrance & Flavor (Shanghai) Co., Ltd., Dewdrop Lotus LC AAN56200 / 00.
[0030] Example 1 This embodiment describes the preparation of a refreshing and whitening toothpaste. The formulations of the refreshing whitening toothpaste prepared in Examples 1-3 are shown in Table 1.
[0031] Table 1 The preparation method of the refreshing and whitening toothpaste is as follows: Raw material 1 is obtained by mixing solvent, disodium dihydrogen pyrophosphate, flavoring agent, taste modifier, preservative, pH adjuster, lecithin, PVM / MA copolymer, cetylpyridinium chloride and colorant. Raw material 2 is obtained by mixing hydrated silica, cellulose gum, oral care agent and other foaming agents except cetylpyridinium chloride.
[0032] Add ingredient 1 and humectant (excluding xylitol) to the main pot and mix evenly at 45°C. Add ingredient 2 and mix evenly at 45°C. Then add xylitol and color correction particles to the main pot and mix evenly at 45°C to obtain the final product.
[0033] Example 4 This embodiment prepares a refreshing whitening toothpaste. The only difference between this embodiment and Example 1 is that the hydrated silica with a water absorption capacity of 0.9 mL / g is not added, and the hydrated silica with a water absorption capacity of 0.9 mL / g is distributed according to the ratio in Example 1 to the hydrated silica with a water absorption capacity of 2.5 mL / g and the hydrated silica with an oil absorption capacity of 0.6 mL / g. All other aspects are the same as in Example 1.
[0034] Example 5 This embodiment prepares a refreshing whitening toothpaste. The only difference between this embodiment and Example 1 is that the hydrated silica with a water absorption capacity of 0.9 mL / g is not added, and the hydrated silica with an oil absorption capacity of 0.6 mL / g is distributed according to the ratio in Example 1 to the hydrated silica with a water absorption capacity of 2.5 mL / g and the hydrated silica with a water absorption capacity of 0.9 mL / g. All other aspects are the same as in Example 1.
[0035] Example 6 This embodiment prepares a refreshing and whitening toothpaste, which differs from Example 1 only in that the amount of hydrated silica with an oil absorption capacity of 0.6 mL / g added is 10 parts, the amount of hydrated silica with an oil absorption capacity of 2.5 mL / g added is 7 parts, the amount of hydrated silica with an water absorption capacity of 0.9 mL / g added is 7 parts, the amount of disodium dihydrogen pyrophosphate added is 0.1 parts, the amount of PVM / MA copolymer added is 0.3 parts, the amount of mannitol added is 0.8 parts, the amount of microcrystalline cellulose added is 0.3 parts, the amount of CI 74160 added is 0.001 parts, the amount of cetyl alcohol added is 0.001 parts, the amount of corn starch added is 0.01 parts, and the amount of hydroxypropyl methylcellulose added is 0.01 parts. The rest is the same as in Example 1.
[0036] Example 7 This embodiment prepares a refreshing and whitening toothpaste, which differs from Example 1 only in that the amount of hydrated silica with an oil absorption capacity of 0.6 mL / g added is 7 parts, the amount of hydrated silica with an oil absorption capacity of 2.5 mL / g added is 3 parts, the amount of hydrated silica with an water absorption capacity of 0.9 mL / g added is 1 part, the amount of disodium dihydrogen pyrophosphate added is 5 parts, the amount of PVM / MA copolymer added is 0.05 parts, the amount of mannitol added is 0.05 parts, the amount of microcrystalline cellulose added is 0.01 parts, the amount of CI 74160 added is 0.2 parts, the amount of cetyl alcohol added is 0.05 parts, the amount of corn starch added is 0.001 parts, and the amount of hydroxypropyl methylcellulose added is 0.00001 parts. The rest is the same as in Example 1.
[0037] Comparative Example 1 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that it does not include 7 parts of hydrated silica with an oil absorption capacity of 0.6 mL / g, 2.5 mL / g of hydrated silica, and 0.9 mL / g of hydrated silica. The above mass parts are distributed to disodium dihydrogen pyrophosphate, PVM / MA copolymer, and color correction particles according to the proportions in Example 1. All other aspects are the same as in Example 1.
[0038] Comparative Example 2 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that disodium dihydrogen pyrophosphate is not added, and the above-mentioned mass proportions are allocated to hydrated silica, PVM / MA copolymer, and color-correcting particles according to the proportions in Example 1. All other aspects are the same as in Example 1.
[0039] Comparative Example 3 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that it does not contain PVM / MA copolymer, and the above-mentioned mass proportions are allocated to hydrated silica, disodium dihydrogen pyrophosphate, and color-correcting particles according to the proportions in Example 1. All other aspects are the same as in Example 1.
[0040] Comparative Example 4 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that it does not contain color-correcting particles, and the above-mentioned mass proportions are allocated to hydrated silica, disodium dihydrogen pyrophosphate, and PVM / MA copolymer according to the proportions in Example 1. All other aspects are the same as in Example 1.
[0041] Comparative Example 5 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that microcrystalline cellulose is not added, and the above-mentioned mass proportions are allocated to mannitol, CI 74160, cetyl alcohol, corn starch, ethyl cellulose, and hydroxypropyl methylcellulose according to the proportions in Example 1. The rest is the same as in Example 1.
[0042] Comparative Example 6 This comparative example of preparing a refreshing whitening toothpaste differs from Example 1 only in that cetyl alcohol is not added, and the above-mentioned mass proportions are allocated to mannitol, CI 74160, microcrystalline cellulose, corn starch, ethyl cellulose, and hydroxypropyl methylcellulose according to the proportions in Example 1. The rest is the same as in Example 1.
[0043] Test Example 1 This test case examines the whitening effect of Fresh Whitening Toothpaste. (1) Whitening effect after brushing teeth for three days A strong, acquired tartar exists on the surface of teeth. Bacteria break down food on teeth or consume dark-colored foods or beverages in our daily diet, such as black tea, soy sauce, chocolate, and coffee, which stain this acquired tartar and gradually accumulate to form extrinsic stains that are difficult to remove. This test case uses bovine teeth as a substrate. The teeth are cut, inlaid with resin, and polished to create regular abrasive blocks. These blocks are then artificially stained to obtain extrinsic stains. By simulating the brushing process, a colorimeter is used to measure the color difference in the teeth to evaluate the toothpaste's ability to remove extrinsic stains.
[0044] Caries-free bovine teeth were selected, and the teeth were cleaned and sterilized. The teeth were then soaked alternately in 1% hydrochloric acid, saturated sodium carbonate, and 1% phytic acid for 1 minute each, rinsed thoroughly, and then immersed in a prepared staining solution for 48 hours. The staining source was a mixture of black tea, coffee, soy sauce, and ferric chloride. After removing the teeth from the staining solution, they were rinsed, dried, and the whiteness of the enamel surface of each tooth was measured using a colorimeter. The teeth were randomly divided into a sample group and a control group, with 8 teeth in each group. The sample group consisted of toothpastes prepared according to the above-described examples and comparative examples, respectively. Difference analysis software was used to test for differences, requiring no significant difference between the two groups. A negative control toothpaste was prepared by adding 10 g of calcium pyrophosphate to 50 g of 5.2% carboxymethyl cellulose solution. Sample toothpaste paste and control toothpaste paste were prepared at a 1:3 ratio. The sample group and control group were brushed 50 times at a frequency of 100 r / min with a vertical pressure of 150 g to simulate one brushing session. After simulating one brushing session, the tooth blocks were rinsed clean and dried, and the whiteness of the enamel surface was measured using a colorimeter. The sample group and control group, with their whiteness values measured, were then brushed again 250 times (a total of 300 times) at a vertical pressure of 150 g and a frequency of 100 r / min to simulate brushing for 3 days. After simulating 3 days of brushing, the tooth blocks were rinsed clean and dried, and the whiteness of the enamel surface was measured using a colorimeter. The specific results are shown in Table 2.
[0045] Table 2 The experimental results above show that the difference in whiteness value before and after brushing with the whitening toothpaste prepared in this invention is significantly greater than that in the negative control group. Comparing Example 1 with the negative control group, it was found that whitening and stain removal improved by 170% after one use and by 271% after three days. This indicates that the tested toothpaste sample can remove exogenous stains caused by a mixture of tea stains, coffee stains, soy sauce stains, etc., and has whitening and stain removal effects.
[0046] (2) Whitening effect after brushing teeth for seven days - 5 Caries-free bovine teeth were selected, and cleaned and sterilized tooth blocks were prepared. The tooth blocks were then soaked alternately in 1% hydrochloric acid, saturated sodium carbonate, and 1% phytic acid for 1 minute each. After rinsing, they were immersed in a prepared staining solution for 48 hours. The staining source was a mixture of black tea, coffee, soy sauce, and ferric chloride. After removing the tooth blocks from the staining solution, they were rinsed, dried, and the whiteness of the enamel surface of each tooth block was measured using a colorimeter. The tooth blocks were randomly divided into a sample group and a control group, with 8 blocks in each group. A difference test was performed using analysis software, requiring no significant difference between the two groups. A sample toothpaste paste was prepared according to a toothpaste-to-water ratio of 1:1.6. The toothpaste used was prepared in Example 1. The sample toothpaste paste and the control (water) were used to brush the sample group and the control group 700 times at a frequency of 100 times / min to simulate brushing for 7 days. After rinsing and drying, the whiteness of the enamel surface of the tooth blocks was measured using a colorimeter. The difference in whiteness before and after simulated brushing was calculated for both the sample group and the control group. Analyze whether the differences between the two groups are significant. Sex differences were investigated, and the whitening factor (difference in whiteness value before and after brushing in the sample group / difference in whiteness value before and after brushing in the control group) and color enhancement (color chart readings and color values: 1→B1, 2→A1, 3→B2, 4→D2, 5→A2, 6→C1, 7→C2, 8→D3, 9→A3, 10→D4, 11→B3, 12→A3.5, 13→B4, 14→C3, 15→A4, 16→C4) were calculated. The specific results are shown in Tables 3 and 4.
[0047] Table 3 Table 4 The toothpaste prepared according to this invention was compared with the control group. The difference in whiteness value before and after simulated brushing in the sample group was greater than that in the control group. The difference between the two groups was statistically significant (P < 0.05). This indicates that the tested toothpaste sample can remove exogenous stains caused by mixed stains such as tea stains, coffee stains, and soy sauce stains. It has the effect of whitening and stain removal. After 7 days of use, the whitening and stain removal effect was improved by 475%, which is 3.5 shades brighter.
[0048] Test Example 2 This test case examines the whitening effect of the Fresh & Brightening Toothpaste on removing yellowing. (1) The effect of brushing teeth for seven days to remove yellowing Caries-free bovine teeth were selected, and cleaned and sterilized tooth blocks were prepared. The tooth blocks were then soaked alternately in 1% hydrochloric acid, saturated sodium carbonate, and 1% phytic acid for 1 minute each, rinsed thoroughly, and then immersed in the prepared staining solution for 48 hours. The staining sources used in this experiment were mixtures of tea, coffee, soy sauce, alcohol, cola, fruit juice, milk tea, chocolate, and hot sauce. After removing the tooth blocks from the staining solution, rinsing and drying them, the yellowness value of the enamel surface of each tooth block was measured using a colorimeter. The tooth blocks were randomly divided into a sample group and a control group, with 8 blocks in each group. Difference analysis software was used to perform a difference test, requiring no significant difference between the two groups. Sample toothpaste paste was prepared according to a toothpaste-to-water ratio of 1:1.6. The sample groups were the toothpastes prepared in the above-mentioned examples and comparative examples, respectively. The sample toothpaste paste and the negative control toothpaste paste were used to brush the sample group and the control group 50 times at a frequency of 100 times / min, respectively, to simulate one brushing session. After rinsing and drying, the yellowness value of the enamel surface of the tooth blocks was measured using a colorimeter. The sample toothpaste paste and the negative control toothpaste paste were then used to brush the sample group and the control group 250 times at a frequency of 100 times / min, respectively (a total of 300 brushing sessions), to simulate brushing for 3 days. After rinsing and drying, the yellowness value of the enamel surface of the tooth blocks was measured using a colorimeter. The sample toothpaste paste and the negative control toothpaste paste were then used to brush the sample group and the control group 400 times at a frequency of 100 times / min, respectively (a total of 700 brushing sessions), to simulate brushing for 7 days. After rinsing and drying, the yellowness value of the enamel surface of the tooth blocks was measured using a colorimeter. The specific results are shown in Table 5.
[0049] Table 5 The above experiments show that the fresh whitening toothpaste prepared by the present invention has a significant yellowing removal effect. Taking Example 1 and the negative control group as examples, the yellowing value reduction rate was 187.6% after one use, 264.5% after 3 days of use, and 309.4% after 7 days of use.
[0050] (2) Yellowing removal effect after 18 hours Caries-free bovine teeth were selected, and enamel specimens were cleaned and sterilized. After rinsing and drying the tooth blocks, the yellowness value of the enamel surface of each tooth block was measured using a colorimeter. Tooth blocks with similar yellowness values were randomly assigned to the sample group and control group, with 8 tooth blocks in each group. Sample toothpaste paste was prepared at a toothpaste-to-water ratio of 1:1.6. The sample group used the toothpaste prepared in Example 1. Both the sample toothpaste paste and the control group were used to simulate brushing teeth 800 times at 100 brushes / min. After rinsing and drying the tooth blocks, the yellowness value of the enamel surface of each tooth block was measured using a colorimeter. The tooth blocks were then rinsed and stained in a prepared staining solution for 18 hours. The staining sources used were tea, coffee, soy sauce, alcohol, cola, fruit juice, milk tea, chocolate, and hot sauce. After removing the tooth blocks from the staining solution, rinsing and drying them, the yellowness value of the enamel surface of each tooth block was measured using a colorimeter. Specific results are shown in Table 6.
[0051] Table 6 Test Example 3 This test case examines the anti-tartar and gloss-enhancing effects of Fresh & White toothpaste. (89) (1) Anti-calculus test When thick dental plaque is present, calcium and phosphate in saliva accumulate locally, gradually forming (hydroxyapatite)phosphate minerals, i.e., tartar. Under constant pH conditions, using hydroxyapatite powder as seed crystals, calcium and phosphorus elements in artificial saliva react on the seed crystal surface to form (hydroxyapatite)phosphate precipitates, simulating the plaque calcification process in tartar formation. By measuring the calcium concentration in the artificial saliva, the inhibition rate of the sample against tartar was calculated.
[0052] Accurately weigh 50 mg of hydroxyapatite powder and place it in a 10 mL centrifuge tube. Divide the tubes into a sample group, a negative control group, and a positive control group. The sample group consisted of toothpaste prepared in Example 1, with three replicates for each experimental group. Weigh 10 g of toothpaste into a beaker, add 30 g of water to prepare a 25% toothpaste paste solution, stir well, and centrifuge at 10000 r / min for 15 min. Collect the supernatant for later use. Add 5 mL of physiological saline to each hydroxyapatite powder tube, shake for 1 min, and centrifuge at 10000 r / min for 10 min. Slowly discard the supernatant using a pipette. Add 5 mL of toothpaste supernatant, water, and 5% sodium pyrophosphate solution to the centrifuge tubes of the sample group, negative control group (water), and positive control group (sodium pyrophosphate), respectively. Shake for 1 min, centrifuge at 10000 r / min for 10 min, and slowly discard the supernatant using a pipette. Then add 5 mL of physiological saline to the centrifuge tube, shake for 1 min, centrifuge at 10000 r / min for 10 min, slowly discard the supernatant with a pipette, add another 5 mL of physiological saline and repeat the above steps twice. Add another 5 mL of physiological saline to the centrifuge tube and vortex for 1 min to obtain a uniformly dispersed hydroxyapatite suspension.
[0053] Measure 100 mL of artificial saliva into a 200 mL beaker. Place the beaker on a temperature-controlled magnetic stirrer. Once the artificial saliva reaches 37°C, transfer the prepared hydroxyapatite suspension to the beaker to begin the reaction. Continuously add 0.01 mol / L sodium hydroxide solution to the beaker to maintain a constant pH of 7.4. Allow the reaction to proceed for 30 min. Immediately after the 30-minute mark, remove 10 mL of the solution from the beaker, filter it through a 0.22 μm filter membrane, and then proceed with the analysis.
[0054] The formation process of hydroxyapatite crystals is as follows: .
[0055] A calcium standard curve was prepared with concentrations of 0 mg / L, 0.5 mg / L, 1.0 mg / L, 2.0 mg / L, 4.0 mg / L, and 6.0 mg / L at calibration points. The calcium concentration C in the solution was obtained from the calibration curve, and the calculus inhibition rate R was calculated. .in It is 29.790. It is 20.443. The value was 29.483, and the specific test results are shown in Table 7.
[0056] in, It is the concentration of the sample group. This is the concentration of the negative control group. This is the concentration of the positive control group.
[0057] Table 7 A comparative experiment was conducted using the toothpaste prepared according to the present invention with negative and positive control samples. By simulating crystal growth inhibitors, the deposition of phosphorus and calcium in saliva on the tooth surface was inhibited to form minerals such as hydroxyapatite. The results showed that compared with the positive control, the tartar inhibition rate of the sample group was 103.4%, which has the effect of anti-tartar.
[0058] (2) Gloss test Caries-free bovine teeth were selected, cleaned, and sterilized. The tooth blocks were then polished to a standard surface roughness (Ra≤0.2μm) using a polishing machine, or tooth blocks with similar surface roughness were selected. The initial surface gloss of the tooth blocks was measured and recorded as Ginitial. Ten tooth blocks with similar gloss were selected and randomly divided into a sample group and a control group. Toothpaste paste was prepared at a toothpaste:water ratio of 1:1.6. The sample group used the toothpaste prepared in Example 1. Under a load of 150 g, the tooth blocks were brushed 300 times at 100 r / min to simulate brushing for 3 days. The tooth blocks were then removed, dried, and the surface gloss of the tooth blocks after brushing was measured and recorded as Gpost-treatment. Deionized water was used simultaneously as the control group, and the tooth blocks underwent the same treatment. Specific results are shown in Table 8. Table 8 The above experiments show that the toothpaste prepared by this invention can significantly improve the gloss of teeth. Compared with the control group, the gloss is increased by 2.1 times after 3 days of use.
[0059] Test Example 4 This test case examines the breath-freshening effect of the Fresh Whitening Toothpaste. The main components of halitosis are volatile sulfur compounds (VSCs), including methanethiol, hydrogen sulfide, and dimethyl sulfide. These are produced by various factors, with approximately 90% originating in the oral cavity. This experiment simulates the use of oral care products in vitro, cultivating volunteers to produce volatile sulfur compounds from their salivary secretions, and measuring methanethiol and other components to evaluate the effectiveness of breath freshening.
[0060] Saliva samples were obtained from volunteers. Hydroxyapatite tablets were cultured overnight to form an acquired biofilm. The hydroxyapatite tablets were then immersed in toothpaste prepared in the above-described examples and comparative examples for 2 minutes. After immersion, the tablets were placed in headspace vials, and 3 mL of saliva culture medium was added. The samples were cultured for 12 hours, and gas chromatography analysis was performed to obtain the methanethiol peak area. lg(methanethiol peak area) was then calculated. The hydroxyapatite tablets in the blank control group were immersed in deionized water, with the remaining steps identical to those described above. Significant differences between each group and the blank control group were calculated, and the specific results are shown in Table 9.
[0061] Table 9 The results above show that the toothpaste prepared in this invention, after being co-cultured with saliva for 24 hours, can reduce the production of methanethiol and has a 24-hour fresh breath effect.
[0062] Test Example 5 This test case explores the effects of Fresh & Whitening Toothpaste on oral health. (1) Detection of oral mucosal stimulation effect The toothpaste prepared in Example 1 was used in an experiment with three SPF-grade golden hamsters, each weighing 100 g. Before the experiment, a suitable 3-4 mm collar was fitted to each animal to ensure normal eating and breathing while preventing the cotton ball from dislodging from the mouth. Before administering the sample, the collar was removed, and the cheek pouches were turned inside out and rinsed with physiological saline to check for any abnormalities. A 5 mm cotton ball soaked in the sample was placed in one cheek pouch of the animal, while the other cheek pouch remained untreated as a control. The sample was allowed to contact the hamster's oral mucosa for 5 minutes. After contact, the collar and cotton ball were removed, and the cheek pouches were rinsed with physiological saline, taking care not to contaminate the other side. If necessary, the collar was reattached, and the animal was returned to its cage. This sampling procedure was repeated every hour for a total of 4 hours. After removing the sample, the test cheek pouch and the control cheek pouch were visually compared. The scores were summed and divided by the total number of observations to obtain the average score for each animal. This observation was helpful for histological evaluation. Twenty-four hours after the last contact, the cheek pouches were visually observed. The hamsters were euthanized painlessly, and tissue samples from representative areas of the cheek pouches were taken, fixed in tissue fixative, prepared into tissue sections, stained with hematoxylin and eosin (HE), and then histologically evaluated. The specific results are shown in Table 10.
[0063] Table 10 The results above show that the toothpaste prepared in this invention has no irritant effect on the oral mucosa of golden hamsters.
[0064] (2) Oral cooling This test measured the skin surface temperature of 30 healthy subjects before and after using the test sample, allowing for subject self-assessment and verifying the efficacy of the toothpaste prepared in Example 1. The ratio of male to female subjects was 3:7, their ages ranged from 20 to 59 years, and the recruitment target was 40 years old. A total of 33 subjects were screened and enrolled, with 3 failing to complete the test, resulting in 30 valid participants for data analysis. Infrared thermal imaging was used to detect skin surface temperature inside the oral cavity; a lower measurement value indicated a lower skin surface temperature. Specific test time points and content are shown in Table 11, and specific test results are shown in Table 12.
[0065] Table 11 Table 12 Compared with before using the sample, the oral cavity temperature decreased significantly by 4.5°C immediately after brushing and rinsing with water using the test sample (toothpaste prepared in Example 1).
[0066] In summary, this invention achieves teeth whitening through a combination of three whitening methods, and forms a color-locking film on the whitened tooth surface to prevent stains and reduce the risk of teeth yellowing. The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.
Claims
1. A refreshing and whitening toothpaste, characterized in that, The ingredients of the fresh whitening toothpaste include hydrated silica, disodium dihydrogen pyrophosphate, PVM / MA copolymer, color-correcting particles, and additives. The color-correcting particles include mannitol, microcrystalline cellulose, CI 74160, cetyl alcohol, corn starch, ethyl cellulose, and hydroxypropyl methyl cellulose.
2. The refreshing and whitening toothpaste according to claim 1, characterized in that, The hydrated silica includes hydrated silica with a water absorption of (0.85-1) mL / g, hydrated silica with a water absorption of (2.4-2.6) mL / g, and hydrated silica with an oil absorption of (0.4-1) mL / g; Preferably, the ingredients of the refreshing whitening toothpaste include, by weight, 15-20 parts hydrated silica, 0.5-3 parts disodium dihydrogen pyrophosphate, 0.01-0.1 parts PVM / MA copolymer, 0.1702-0.77 parts color-correcting particles, and 71.2217-95.5345 parts additives; Preferably, the color-correcting particles comprise, by weight, 0.1-0.5 parts mannitol, 0.05-0.1 parts microcrystalline cellulose, 0.01-0.1 parts CI 74160, 0.005-0.03 parts cetyl alcohol, 0.005-0.03 parts corn starch, 0.0001-0.005 parts ethyl cellulose, and 0.0001-0.005 parts hydroxypropyl methylcellulose.
3. The refreshing and whitening toothpaste according to claim 1 or 2, characterized in that, The additives include any one or a combination of at least two of the following: humectants, solvents, foaming agents, fragrances, thickeners, oral care agents, taste modifiers, preservatives, pH adjusters, or colorants.
4. The refreshing and whitening toothpaste according to claim 3, characterized in that, The additives, by weight, include any one or a combination of at least two of the following: 31-41 parts humectant, 38-43 parts solvent, 1.121-4.43 parts foaming agent, 0.5-3 parts fragrance, 0.2005-1.803 parts thickener, 0.1-0.8 parts oral care agent, 0.1-0.5 parts taste improver, 0.1-0.5 parts preservative, 0.1-0.5 parts pH adjuster, or 0.0002-0.0015 parts colorant.
5. The refreshing and whitening toothpaste according to claim 3 or 4, characterized in that, The moisturizer comprises any one or a combination of at least two of the following: 30-35 parts sorbitol, 0.5-3 parts xylitol, or 0.5-3 parts polyethylene glycol-8. Preferably, the solvent includes water; Preferably, the foaming agent comprises any one or a combination of at least two of the following: 1-3 parts sodium lauryl sulfate, 0.1-1 parts cocamidopropyl betaine, 0.01-0.3 parts sodium chloride, 0.001-0.03 parts sodium benzoate, or 0.01-0.1 parts cetylpyridinium chloride.
6. The refreshing whitening toothpaste according to any one of claims 3-5, characterized in that, The fragrance agent comprises 0.5-3 parts of fragrance essence; Preferably, the thickener comprises any one or a combination of at least two of the following: 0.1-1 parts cellulose gum, 0.1-0.8 parts xanthan gum, or 0.0005-0.003 parts lecithin; Preferably, the oral care agent comprises 0.1-0.8 parts of zinc citrate; Preferably, the taste improver comprises 0.1-0.5 parts of sodium saccharin.
7. The refreshing whitening toothpaste according to any one of claims 3-6, characterized in that, The preservative includes 0.1-0.5 parts sodium benzoate; Preferably, the pH adjuster comprises 0.1-0.5 parts of sodium hydroxide; Preferably, the colorant comprises 0.0001-0.001 parts of CI 17200 and / or 0.0001-0.0005 parts of CI 42051.
8. A method for preparing a refreshing whitening toothpaste according to any one of claims 1-7, characterized in that, The preparation method includes stirring hydrated silica, disodium dihydrogen pyrophosphate, PVM / MA copolymer, color correction particles and additives to obtain the product.
9. The method for preparing the refreshing and whitening toothpaste according to claim 8, characterized in that, The preparation method further includes pretreatment; Preferably, the pretreatment includes mixing a solvent, disodium dihydrogen pyrophosphate, flavoring agent, taste modifier, preservative, pH adjuster, lecithin, PVM / MA copolymer, cetylpyridinium chloride and colorant to obtain raw material 1, and mixing hydrated silica, cellulose gum, oral care agent and other foaming agents except cetylpyridinium chloride to obtain raw material 2.
10. The method for preparing the refreshing and whitening toothpaste according to claim 9, characterized in that, The preparation method includes mixing raw material 1 with a humectant other than xylitol, adding xanthan gum and mixing, then adding raw material 2 and mixing, and finally adding xylitol and color correction particles to obtain the final product.