Preparation method of tooth remineralization composition

Through a simplified preparation method, the dental remineralization composition is prepared by a one-step method using a nonionic surfactant emulsifier, which solves the problems of complicated steps and poor stability of intermediate products in the prior art, and achieves an efficient and stable dental remineralization effect.

CN120204058APending Publication Date: 2025-06-27XIAN UNIV OF SCI & TECH
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Patent Information

Application Number
CN202510325533.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-19
Publication Date
2025-06-27

AI Technical Summary

Technical Problem

The prior art When preparing dental remineralization compositions, the steps are cumbersome and the intermediate product has poor stability, which affects the quality and performance of the final product.

Method used

A stable water-in-water emulsion in oil was prepared by using both lipophilic and hydrophilic nonionic surfactants as emulsifiers, respectively, and an aqueous solution containing calcium ions and phosphate was added to the oil phase for emulsification.

Benefits of technology

The preparation process is simplified, the stability and quality of the product is improved, and the ability to release high concentrations of calcium ions and phosphates in the oral cavity, promoting teeth remineralization.

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Abstract

The invention discloses a preparation method of a tooth remineralization composition. According to the invention, an oleophylic nonionic surfactant and a hydrophilic nonionic surfactant are used as emulsifiers at the same time, and the emulsifiers are added into a non-polar or small-polarity substance for oral care to form an oil phase; under stirring, an aqueous solution containing phosphate radical, hydrogen phosphate radical or dihydrogen phosphate radical ions and an aqueous solution containing calcium ions are continuously added into two parts of oil phases for emulsification, a water-in-oil-in-water emulsion containing soluble calcium salt and a water-in-oil-in-water emulsion containing soluble phosphate are obtained through a one-step method, and the preparation process is simplified. When the toothpaste, the gel and the tooth strip disclosed by the invention are used, the water-in-oil-in-water emulsion is broken under the action of friction, massage and extrusion to release soluble calcium salt and soluble phosphate wrapped in an inner water phase, so that oral liquid contains calcium ions and phosphate radical or hydrogen phosphate radical or dihydrogen phosphate radical ions with relatively high concentration; the tooth remineralization rate can be improved.
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Description

Technical Field

[0001] The present invention relates to the fields of daily chemicals, oral hard tissue medical treatment, nursing, and cleaning, and particularly relates to a preparation method of a tooth remineralization composition. Background Art

[0002] The main inorganic components of enamel and dentin are hydroxyapatite. Generally, when pH < 5.5, hydroxyapatite will dissolve, leading to tooth demineralization. If the enamel continues to demineralize, it will also cause the exposure of dentinal tubules, thus inducing dentin hypersensitivity.

[0003] Saliva contains a certain concentration of calcium ions and phosphate ions. In the oral environment where pH > 5.5 and the concentrations of calcium ions and phosphate ions in saliva are relatively high, calcium phosphate will be formed in saliva, which helps the demineralized teeth to remineralize. However, under normal circumstances, the concentrations of calcium ions and phosphate ions in saliva are relatively low, and it is difficult to form a sufficient amount of hydroxyapatite, so the demineralized teeth cannot be effectively repaired.

[0004] Chinese Patent with Application No. CN202010089792.X discloses a preparation method of an enamel regeneration composition. This method involves encapsulating soluble calcium salts and soluble phosphates respectively as the inner aqueous phase of a solid particle-stabilized water-in-oil-in-water emulsion and adding it to toothpaste, enamel repair gel, or mouthwash. However, this preparation method uses a two-step process when preparing the water-in-oil-in-water emulsion containing soluble calcium salts or soluble phosphates: first, preparing an oil-in-water emulsion as an intermediate product, and then further preparing a water-in-oil-in-water emulsion. This method not only has cumbersome steps, but also the intermediate oil-in-water emulsion may have stability problems during storage and subsequent use, such as phenomena like stratification or demulsification, which will directly affect the quality and performance of the final product. Summary of the Invention

[0005] The purpose of the present invention is to provide an efficient and stable preparation method of a tooth remineralization composition that can accelerate tooth remineralization by simplifying the preparation process and increasing the concentrations of calcium ions and phosphate ions or hydrogen phosphate ions or dihydrogen phosphate ions in the oral cavity.

[0006] To achieve the above purpose, the present invention provides the following technical solutions:

[0007] A preparation method of a tooth remineralization composition, comprising the following steps:

[0008] 1) Prepare a water-in-oil-in-water emulsion containing soluble calcium salts:

[0009] A mixture of a lipophilic nonionic surfactant and a hydrophilic nonionic surfactant that can be used in medical and oral care is added to a nonpolar or less polar substance that can be used in oral care at a mass ratio of (0.2 - 20):100, and heated to 25°C - 95°C, and stirred evenly to form an oil phase A;

[0010] A soluble substance that can provide free calcium ions is added to water to make an aqueous solution A with a calcium ion concentration of 0.1% - 60%;

[0011] At 25°C - 95°C, at a stirring rate of 100 revolutions per minute to 16,000 revolutions per minute, aqueous solution A is added to oil phase A within 2 to 60 minutes at a volume ratio of (3:7) - (9.5:0.5), and then stirred continuously for 10 to 60 minutes to obtain a water-in-oil-in-water emulsion containing soluble calcium salt;

[0012] 2) Preparation of a water-in-oil-in-water emulsion containing soluble phosphate:

[0013] A mixture of a lipophilic nonionic surfactant and a hydrophilic nonionic surfactant that can be used in medical and oral care is added to a nonpolar or less polar substance that can be used in oral care at a mass ratio of (0.2 - 20):100, and heated to 25°C - 95°C, and stirred evenly to form an oil phase B;

[0014] A soluble substance that can provide free phosphate, hydrogen phosphate or dihydrogen phosphate ions is added to water to make an aqueous solution B with a total concentration of phosphate, hydrogen phosphate or dihydrogen phosphate ions of 0.1% - 60%;

[0015] At 25°C - 95°C, at a stirring rate of 100 revolutions per minute to 16,000 revolutions per minute, aqueous solution B is added to oil phase B within 2 to 60 minutes at a volume ratio of (3:7) - (9.5:0.5), and then stirred continuously for 10 to 60 minutes to obtain a water-in-oil-in-water emulsion containing soluble phosphate;

[0016] The mass ratio of the lipophilic nonionic surfactant and the hydrophilic nonionic surfactant that can be used in medical and oral care in the above steps 1 and 2) is 1:19 to 19:1;

[0017] The nonpolar or less polar substance that can be used in oral care in the above steps 1 and 2) is one or at least two of rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, mutton tallow, chicken oil, snake oil, frog oil, fish oil, nonpolar or less polar compounds that are non-toxic to the human body and are processed from petroleum, natural gas, and coal;

[0018] 3) The preparation method of toothpaste, dental restoration gel, dental restoration dental patch or teeth whitening patch that simultaneously contains soluble calcium salt and soluble phosphate is as follows:

[0019] Mix the water-in-oil-in-water emulsion containing soluble calcium salt heated to 25°C to 90°C, the water-in-oil-in-water emulsion containing soluble phosphate, and toothpaste matrix, dental restoration gel matrix, dental patch gel matrix without peroxide or dental patch gel matrix containing peroxide used for teeth whitening, and stir at a rate of 50 revolutions per minute to 20,000 revolutions per minute for 1 minute to 160 minutes to obtain toothpaste, dental restoration gel or gel for dental patch that simultaneously contains soluble calcium salt and soluble phosphate. Among them, the gel for dental patch is compounded with a soft film layer and a backing layer by a known method to prepare a dental restoration dental patch or teeth whitening patch. What is finally obtained is a tooth remineralization composition, including toothpaste, dental restoration gel, dental restoration dental patch or teeth whitening patch; the molar ratio of calcium ions contained in the water-in-oil-in-water emulsion containing soluble calcium salt to the amount of phosphate ions, hydrogen phosphate ions or dihydrogen phosphate ions contained in the water-in-oil-in-water emulsion containing soluble phosphate is 5:3, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the toothpaste matrix, dental restoration gel matrix or dental patch gel matrix is 0.01:19.99 to 19.5:0.5.

[0020] Furthermore, the lipophilic non-ionic surfactant that can be used in medical and oral care includes but is not limited to one or a mixture of more than one of Span40, Span60, and Span80.

[0021] Furthermore, the hydrophilic non-ionic surfactant that can be used in medical and oral care includes but is not limited to one or a mixture of more than one of Tween40, Tween60, and Tween80.

[0022] Furthermore, the soluble substance that can provide free calcium ions is one or a mixture of at least two of calcium chloride, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, and calcium acetate.

[0023] Furthermore, the soluble substance that can provide free phosphate ions, hydrogen phosphate ions or dihydrogen phosphate ions is one or a mixture of at least two of potassium phosphate, sodium phosphate, ammonium phosphate, potassium hydrogen phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, and ammonium dihydrogen phosphate.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The present invention simplifies the preparation process by using both lipophilic nonionic surfactants and hydrophilic nonionic surfactants as emulsifiers. The emulsifiers are added to nonpolar or less polar substances that can be used for oral care to form an oil phase. During stirring, an aqueous solution containing phosphate ions, hydrogen phosphate ions, or dihydrogen phosphate ions and an aqueous solution containing calcium ions are continuously added to two portions of the oil phase for emulsification, respectively, to obtain a water-in-oil-in-water emulsion containing soluble calcium salts and a water-in-oil-in-water emulsion containing soluble phosphates in one step. Compared with the existing two-step method for preparing a water-in-oil-in-water emulsion containing soluble calcium salts or soluble phosphates, the preparation process is simplified. When using the toothpaste, gel, and dental patch of the present invention, the water-in-oil-in-water emulsion breaks under the action of friction, massage, and extrusion, releasing the soluble calcium salts and soluble phosphates encapsulated in the inner aqueous phase, so that the oral liquid contains a high concentration of calcium ions and phosphate ions, hydrogen phosphate ions, or dihydrogen phosphate ions, which can increase the rate of tooth remineralization. Detailed Embodiments

[0026] To make the above objects, features, and advantages of the present invention more obvious and understandable, the present invention will be described in detail below with reference to specific embodiments.

[0027] Example 1:

[0028] 1) Preparation of a water-in-oil-in-water emulsion containing soluble calcium salts:

[0029] A mixture of Span40 and Tween40 was added to rapeseed oil at a mass ratio of 0.2:100 and heated to 25°C, and stirred evenly to form oil phase A, where the mass ratio of Span40 to Tween40 was 1:19;

[0030] Calcium chloride was added to water to make an aqueous solution A with a calcium ion concentration of 60%;

[0031] At 95°C and a stirring rate of 16,000 revolutions per minute, aqueous solution A was added to oil phase A at a volume ratio of 3:7 within 2 minutes, and then stirred for another 10 minutes to obtain a water-in-oil-in-water emulsion containing soluble calcium salts.

[0032] 2) Preparation of a water-in-oil-in-water emulsion containing soluble phosphates:

[0033] A mixture of Span40 and Tween40 was added to rapeseed oil at a mass ratio of 0.2:100 and heated to 95°C, and stirred evenly to form oil phase B, where the mass ratio of Span40 to Tween40 was 1:19;

[0034] Potassium phosphate was added to water to make an aqueous solution B with a total phosphate ion concentration of 60%;

[0035] At 25°C, with a stirring rate of 16,000 revolutions per minute, aqueous solution B was added to oil phase B in a volume ratio of 3:7 within 2 minutes, and then stirring was continued for 10 minutes to obtain a water-in-oil-in-water emulsion containing soluble phosphate.

[0036] 3) Prepare toothpaste containing both soluble calcium salt and soluble phosphate

[0037] The water-in-oil-in-water emulsion containing soluble calcium salt heated to 25°C, the water-in-oil-in-water emulsion containing soluble phosphate, and the toothpaste matrix were mixed and stirred at a rate of 20,000 revolutions per minute for 1 minute to obtain toothpaste containing both soluble calcium salt and soluble phosphate. The molar ratio of calcium ions contained in the water-in-oil-in-water emulsion containing soluble calcium salt to the molar amount of phosphate ions contained in the water-in-oil-in-water emulsion containing soluble phosphate is 5:3, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the toothpaste matrix is 0.01:19.99.

[0038] Example 2:

[0039] This example is the same as Example 1, and the difference from Example 1 is that

[0040] The Tween series nonionic surfactants used include but are not limited to one of Tween 60 and Tween 80, or a mixture of multiple of Tween 40, Tween 60, and Tween 80;

[0041] The Span series nonionic surfactants used include but are not limited to one of Span 60 and Span 80, or a mixture of multiple of Span 40, Span 60, and Span 80;

[0042] All non-polar substances that can be used for oral care are one of peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, mutton tallow, chicken oil, snake oil, frog oil, fish oil, non-toxic non-polar or less polar compounds processed from petroleum, natural gas, and coal, or a mixed oil of at least 2 of rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, mutton tallow, chicken oil, snake oil, frog oil, fish oil, non-toxic non-polar or less polar compounds processed from petroleum, natural gas, and coal;

[0043] The soluble substance capable of providing free calcium ions is one of calcium nitrate, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, calcium acetate, or a mixture of at least two of calcium chloride, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, calcium acetate;

[0044] The soluble substance capable of providing free phosphate, hydrogen phosphate or dihydrogen phosphate is one of sodium phosphate, ammonium phosphate, potassium hydrogen phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, or a mixture of at least two of potassium phosphate, sodium phosphate, ammonium phosphate, potassium hydrogen phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate.

[0045] Example 3:

[0046] 1) Prepare an oil-in-water-in-water emulsion containing a soluble calcium salt:

[0047] Add a mixture of Span60 and Tween60 to peanut oil at a mass ratio of 20:100, heat to 95 °C, and stir evenly to form oil phase A, where the mass ratio of Span60 to Tween60 is 19:1;

[0048] Add calcium nitrate to water to make an aqueous solution A with a calcium ion concentration of 60%;

[0049] At 25 °C, at a stirring rate of 100 revolutions per minute, add aqueous solution A to oil phase A at a volume ratio of 9.5:0.5 within 60 minutes, and then continue to stir for 60 minutes to obtain an oil-in-water-in-water emulsion containing a soluble calcium salt.

[0050] 2) Prepare an oil-in-water-in-water emulsion containing a soluble phosphate:

[0051] Add a mixture of Span60 and Tween60 to peanut oil at a mass ratio of 20:100, heat to 25 °C, and stir evenly to form oil phase B, where the mass ratio of Span60 to Tween60 is 19:1;

[0052] Add sodium phosphate to water to make an aqueous solution B with a total phosphate ion concentration of 60%;

[0053] At 95 °C, at a stirring rate of 100 revolutions per minute, add aqueous solution B to oil phase B at a volume ratio of 9.5:0.5 within 60 minutes, and then continue to stir for 60 minutes to obtain an oil-in-water-in-water emulsion containing a soluble phosphate.

[0054] 3) Prepare a dental restoration gel containing both a soluble calcium salt and a soluble phosphate

[0055] An oil-in-water-in-water emulsion containing a soluble calcium salt, an oil-in-water-in-water emulsion containing a soluble phosphate, and a dental restoration gel matrix, which are heated to 90 °C, are mixed and stirred at a rate of 50 revolutions per minute for 160 minutes to obtain a dental restoration gel containing both a soluble calcium salt and a soluble phosphate. The molar ratio of calcium ions contained in the oil-in-water-in-water emulsion containing the soluble calcium salt to the molar amount of phosphate ions contained in the oil-in-water-in-water emulsion containing the soluble phosphate is 5:3, and the mass ratio of the oil-in-water-in-water emulsion containing the soluble calcium salt and the oil-in-water-in-water emulsion containing the soluble phosphate to the dental restoration gel matrix is 19.5:0.5.

[0056] Example 4:

[0057] This example is the same as Example 3, and the difference from Example 3 is that

[0058] The Tween series of non-ionic surfactants used include, but are not limited to, one of Tween 40 and Tween 80, or a mixture of multiple of Tween 40, Tween 60, and Tween 80;

[0059] The Span series of non-ionic surfactants used include, but are not limited to, one of Span 40 and Span 80, or a mixture of multiple of Span 40, Span 60, and Span 80;

[0060] All non-polar substances that can be used for oral care are one of rapeseed oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, mutton tallow, chicken oil, snake oil, frog oil, fish oil, non-toxic non-polar or less polar compounds prepared from petroleum, natural gas, and coal, or a mixed oil of at least two of rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, mutton tallow, chicken oil, snake oil, frog oil, fish oil, non-toxic non-polar or less polar compounds prepared from petroleum, natural gas, and coal;

[0061] The soluble substances that can provide free calcium ions used are one of calcium chloride, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, and calcium acetate, or a mixture of at least two of calcium chloride, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, and calcium acetate;

[0062] The soluble substance capable of providing free phosphate, hydrogen phosphate or dihydrogen phosphate used is one of potassium phosphate, ammonium phosphate, monopotassium hydrogen phosphate, monosodium hydrogen phosphate, monoammonium hydrogen phosphate, dipotassium dihydrogen phosphate, disodium dihydrogen phosphate, diammonium dihydrogen phosphate, or a mixture of at least two of potassium phosphate, sodium phosphate, ammonium phosphate, monopotassium hydrogen phosphate, monosodium hydrogen phosphate, monoammonium hydrogen phosphate, dipotassium dihydrogen phosphate, disodium dihydrogen phosphate, diammonium dihydrogen phosphate.

[0063] Example 5:

[0064] 1) Prepare an oil-in-water-in-water emulsion containing a soluble calcium salt:

[0065] Add a mixture of Span80 and Tween80 to peanut oil at a mass ratio of 10:100, heat to 50 °C, and stir evenly to form oil phase A, where the mass ratio of Span80 to Tween80 is 1:1;

[0066] Add calcium nitrate to water to make an aqueous solution A with a calcium ion concentration of 10%;

[0067] At 30 °C, at a stirring rate of 8000 revolutions per minute, add aqueous solution A to oil phase A at a volume ratio of 9:1 within 30 minutes, and then continue to stir for 30 minutes to obtain an oil-in-water-in-water emulsion containing a soluble calcium salt.

[0068] 2) Prepare an oil-in-water-in-water emulsion containing a soluble phosphate:

[0069] Add a mixture of Span80 and Tween80 to peanut oil at a mass ratio of 10:100, heat to 30 °C, and stir evenly to form oil phase B, where the mass ratio of Span80 to Tween80 is 1:1;

[0070] Add sodium phosphate to water to make an aqueous solution B with a total phosphate ion concentration of 10%;

[0071] At 50 °C, at a stirring rate of 8000 revolutions per minute, add aqueous solution B to oil phase B at a volume ratio of 9:1 within 30 minutes, and then continue to stir for 30 minutes to obtain an oil-in-water-in-water emulsion containing a soluble phosphate.

[0072] 3) Prepare a dental patch gel containing a soluble calcium salt and a soluble phosphate:

[0073] An oil-in-water-in-water emulsion containing a soluble calcium salt, an oil-in-water-in-water emulsion containing a soluble phosphate, and a tooth patch gel matrix without peroxide are mixed and stirred at a rate of 10,000 revolutions per minute for 80 minutes to obtain a gel for tooth patch containing both a soluble calcium salt and a soluble phosphate. The molar ratio of calcium ions contained in the oil-in-water-in-water emulsion containing a soluble calcium salt to the molar amount of phosphate ions contained in the oil-in-water-in-water emulsion containing a soluble phosphate is 5:3, and the mass ratio of the oil-in-water-in-water emulsion containing a soluble calcium salt and the oil-in-water-in-water emulsion containing a soluble phosphate to the tooth patch gel matrix is 3:7.

[0074] 4) Preparation of a tooth repair patch

[0075] Then, the gel for tooth patch is compounded with a soft film layer and a backing layer by a known method to prepare a tooth repair patch.

[0076] Example 6:

[0077] 1) Preparation of an oil-in-water-in-water emulsion containing a soluble calcium salt:

[0078] A mixture of Span40 and Tween 60 is added to camellia oil at a mass ratio of 1:100, heated to 60 °C, and stirred evenly to form oil phase A, where the mass ratio of Span40 to Tween 60 is 15:1;

[0079] Calcium nitrate is added to water to make an aqueous solution A with a calcium ion concentration of 10%;

[0080] At 80 °C, at a stirring rate of 1000 revolutions per minute, aqueous solution A is added to oil phase A at a volume ratio of 3:1 within 50 minutes, and then stirred for another 50 minutes to obtain an oil-in-water-in-water emulsion containing a soluble calcium salt.

[0081] 2) Preparation of an oil-in-water-in-water emulsion containing a soluble phosphate:

[0082] A mixture of Span40 and Tween 60 is added to camellia oil at a mass ratio of 1:100, heated to 80 °C, and stirred evenly to form oil phase B, where the mass ratio of Span40 to Tween 60 is 15:1;

[0083] Sodium phosphate is added to water to make an aqueous solution B with a total phosphate ion concentration of 10%;

[0084] At 60 °C, at a stirring rate of 1000 revolutions per minute, aqueous solution B is added to oil phase B at a volume ratio of 3:1 within 50 minutes, and then stirred for another 50 minutes to obtain an oil-in-water-in-water emulsion containing a soluble phosphate.

[0085] 3) Preparation of a gel for tooth patch containing a soluble calcium salt and a soluble phosphate:

[0086] Mix the water-in-oil-in-water emulsion containing soluble calcium salt heated to 45°C, the water-in-oil-in-water emulsion containing soluble phosphate, and the tooth patch gel matrix without peroxide, and stir at a rate of 100 revolutions per minute for 120 minutes to obtain a gel for tooth patch containing both soluble calcium salt and soluble phosphate. The molar ratio of calcium ions contained in the water-in-oil-in-water emulsion containing soluble calcium salt to the molar amount of phosphate ions contained in the water-in-oil-in-water emulsion containing soluble phosphate is 5:3, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the tooth patch gel matrix is 2:1.

[0087] 4) Prepare the teeth-whitening tooth patch

[0088] Then, use a well-known method to compound the gel for tooth patch with the soft film layer and the backing layer to prepare the teeth-whitening tooth patch.

[0089] Example 7:

[0090] This example is the same as Example 6, except that the mass ratio of Span 40 to Tween 60 is 3:7, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the tooth patch gel matrix is 1:2.

[0091] Example 8:

[0092] This example is the same as Example 6, except that the mass ratio of Span 40 to Tween 60 is 7:3, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the tooth patch gel matrix is 19:1.

Claims

1. A method for preparing a tooth remineralization composition, characterized in that: The following steps are involved: 1) Preparation of a water-in-oil-in-water emulsion containing a soluble calcium salt: A mixture of a lipophilic nonionic surfactant and a hydrophilic nonionic surfactant that can be used for medical and oral care is added to a nonpolar or less polar substance that can be used for oral care in a mass ratio of (0.2-20):100, heated to 25° C.-95° C., and stirred to form an oil phase A; A soluble substance capable of providing free calcium ions is added into water to prepare an aqueous solution A having a calcium ion concentration of 0.1% to 60%; At 25° C. to 95° C., at a stirring rate of 100 rpm to 16,000 rpm, adding aqueous solution A to oil phase A in a volume ratio of (3:7) to (9.5:0.5) within 2 to 60 minutes, and then continuing to stir for 10 to 60 minutes to obtain a water-in-oil-in-water emulsion containing a soluble calcium salt; 2) Preparation of water-in-oil-in-water emulsion containing soluble phosphate: A mixture of a lipophilic nonionic surfactant and a hydrophilic nonionic surfactant that can be used for medical and oral care is added to a nonpolar or less polar substance that can be used for oral care in a mass ratio of (0.2-20):100, heated to 25° C.-95° C., and stirred to form an oil phase B; A soluble substance capable of providing free phosphate, hydrogen phosphate or dihydrogen phosphate ions is added into water to prepare an aqueous solution B having a total concentration of phosphate, hydrogen phosphate or dihydrogen phosphate ions of 0.1% to 60%; At 25° C. to 95° C., at a stirring rate of 100 rpm to 16,000 rpm, adding aqueous solution B to oil phase B in a volume ratio of (3:7) to (9.5:0.5) within 2 to 60 minutes, and then continuing to stir for 10 to 60 minutes to obtain a water-in-oil-in-water emulsion containing a soluble phosphate; The mass ratio of the lipophilic nonionic surfactant and the hydrophilic nonionic surfactant that can be used for medical treatment and oral care in steps 1 and 2) is 1:19 to 19:1; The non-polar or less polar substance that can be used for oral care in steps 1 and 2) is rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil, grape seed oil, walnut oil, peony seed oil, coconut oil, lard, beef tallow, sheep fat, chicken fat, snake oil, frog oil, fish oil, or a non-polar or less polar compound that is non-toxic to the human body and is processed using petroleum, natural gas, or coal as raw materials, or a mixed oil of at least two of them; 3) The preparation method of toothpaste, tooth repair gel, tooth repair tooth paste or tooth whitening tooth paste containing both soluble calcium salt and soluble phosphate is as follows: A water-in-oil-in-water emulsion containing a soluble calcium salt, a water-in-oil-in-water emulsion containing a soluble phosphate, and a toothpaste base, a tooth repair gel base, a tooth paste gel base without peroxide, or a tooth paste gel base containing peroxide for tooth whitening, which are heated to 25° C. to 90° C., are mixed, and stirred at a rate of 50 rpm to 20,000 rpm for 1 minute to 160 minutes to obtain a toothpaste, a tooth repair gel, or a tooth paste gel containing both a soluble calcium salt and a soluble phosphate, wherein the tooth paste gel is compounded with a soft film layer and a base lining layer by a known method to prepare a tooth repair tooth paste or a tooth whitening tooth paste. The final product is a tooth remineralization composition, including toothpaste, tooth repair gel, tooth repair tooth patch or tooth whitening tooth patch; wherein the ratio of the amount of calcium ion contained in the water-in-oil-in-water emulsion containing soluble calcium salt to the amount of phosphate, hydrogen phosphate or dihydrogen phosphate ion contained in the water-in-oil-in-water emulsion containing soluble phosphate is 5:3, and the mass ratio of the water-in-oil-in-water emulsion containing soluble calcium salt and the water-in-oil-in-water emulsion containing soluble phosphate to the toothpaste base, tooth repair gel base or tooth patch gel base is 0.01:19.99 to 19.5:0.

5.

2. The method for preparing a tooth remineralization composition according to claim 1, characterized in that: The lipophilic nonionic surfactant that can be used for medical treatment and oral care includes one or more mixtures of Span40, Span60, and Span80.

3. The method for preparing a tooth remineralization composition according to claim 1, characterized in that: The hydrophilic nonionic surfactant that can be used for medical treatment and oral care includes one or more mixtures of Tween 40, Tween 60 and Tween 80.

4. The method for preparing a tooth remineralization composition according to claim 1, characterized in that: The soluble substance capable of providing free calcium ions is one of calcium chloride, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium bisulfate, calcium lactate, calcium citrate, and calcium acetate, or a mixture of at least two of them.

5. The method for preparing a tooth remineralization composition according to claim 1, characterized in that: The soluble substance capable of providing free phosphate, hydrogen phosphate or dihydrogen phosphate is one of potassium phosphate, sodium phosphate, ammonium phosphate, potassium monohydrogen phosphate, sodium monohydrogen phosphate, ammonium monohydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate and ammonium dihydrogen phosphate, or a mixture of at least two of them.

Citation Information

Patent Citations

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