CN111249165B - Lipophilic colloid stable water-in-oil emulsion and preparation method of product for repairing tooth enamel by using same - Google Patents
Lipophilic colloid stable water-in-oil emulsion and preparation method of product for repairing tooth enamel by using same Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/064—Water-in-oil emulsions, e.g. Water-in-silicone emulsions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/066—Multiple emulsions, e.g. water-in-oil-in-water
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/925—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of animal origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
Abstract
A water-in-oil emulsion with stable lipophilic colloid and its preparation method for repairing enamel product are disclosed, which are characterized by that the soluble calcium salt and soluble phosphate are respectively used as internal water phase of water-in-oil emulsion with stable lipophilic colloid for wrapping, and then added in the toothpaste, enamel repairing gel or gargle. The soluble calcium salt and soluble phosphate salt in the toothpaste, enamel repair gel or mouthwash prepared in this way can be stable for a long time at the same time. When the toothpaste, the enamel repair gel or the mouthwash is used, the lipophilic colloid-stable water-in-oil emulsion is broken under the actions of friction, extrusion and the like, and soluble calcium salt and soluble phosphate which are wrapped in the internal water phase are released, so that the oral liquid contains calcium ions and phosphate ions with higher concentration, and the remineralization rate of enamel can be improved.
Description
Technical Field
The invention belongs to the field of medical and daily chemical products, and particularly relates to a lipophilic colloid-stable water-in-oil emulsion and a preparation method thereof for repairing enamel products.
Background
Enamel is the hardest tissue of the human body. As the outermost layer of the tooth, enamel is subjected to various physical and chemical attacks, such as bite, abrasion and acid erosion from food and bacteria, and demineralization problems occur in which hydroxyapatite dissolves at pH < 5.5 to produce enamel.
Saliva contains calcium ions and phosphate ions, and the change of the pH value of the saliva is buffered to a certain extent, so that the dissolution of hydroxyapatite is inhibited. At pH > 5.5 and at higher concentrations of calcium and phosphorus ions, calcium phosphate is formed in the saliva, which remineralizes the demineralized teeth. However, in general, saliva contains low concentrations of calcium and phosphate ions, and it is difficult to form sufficient amounts of hydroxyapatite to repair demineralized enamel.
Calcium salt and phosphate are added into the toothpaste, so that the concentration of calcium ions and the concentration of phosphate ions in the oral cavity can be improved during tooth brushing, and the remineralization process of teeth is facilitated. When less soluble calcium salts and phosphate salts are added to the toothpaste, lower concentrations of calcium ions and phosphate ions can be provided. When calcium salt and phosphate with higher solubility are added into the toothpaste, because the solubility product of octacalcium phosphate, calcium hydrophosphate, hydroxyapatite and the like is smaller, calcium ions in the toothpaste and phosphate ions quickly react to form precipitates, so that the concentration of free calcium ions and phosphate ions contained in the toothpaste is still lower. Thus, by adding calcium and phosphate salts directly to toothpaste, the toothpaste is able to provide lower concentrations of free calcium and phosphate ions and a lower rate of remineralization of the enamel with limited brushing time and frequency.
Disclosure of Invention
The invention aims to provide a lipophilic colloid-stable water-in-oil emulsion which can enable oral liquid to contain calcium ions and phosphate ions with higher concentration and can improve the remineralization rate of enamel, and a preparation method of the product for repairing the enamel.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) the preparation method of the lipophilic colloid stable water-in-oil emulsion containing soluble calcium salt and phosphate radical comprises the following steps:
according to the weight ratio of 0.1: 100-25: adding solid particles with the particle size of 0.1-1000000 nanometers, which can be dispersed in oil, into natural oil of plant, animal or mineral sources, which can be used for preparing water aqua and gel for oral treatment, or preparing toothpaste, mouthwash or enamel and oral repair gel, or synthetic oil processed by petrochemical products and natural extraction raw materials according to the mass ratio of 0.1: 1-15: 1, heating to 30-80 ℃, adding titanate and silicate into oil phase according to the mass ratio of titanate or silicate to oil, and uniformly stirring to form oil phase;
adding a substance which can be dissolved in water and alcohol substances and can generate free calcium ions or free phosphate ions into water to prepare an aqueous solution with the concentration of the calcium ions or the phosphate ions being 0.1-60%, and mixing the aqueous solution and the oil phase according to the weight ratio of 0.5: 9.5-1.5: mixing the components in a volume ratio of 0.5, placing the mixture on a high-speed dispersion machine, heating the mixture to 30-80 ℃, and stirring the mixture for 0.5-120 minutes at a speed of 10-24000 r/min to obtain lipophilic colloid stable water-in-oil emulsion containing soluble calcium salt or phosphate radical;
2) mouthwash, toothpaste or enamel repair gels containing soluble calcium salts or soluble phosphate salts are prepared as follows:
mixing a lipophilic colloidally stabilized water-in-oil emulsion containing soluble calcium salt and phosphate radical heated to 30-80 ℃ with a mouthwash base, toothpaste base or enamel repair gel base, stirring at 10-24000 rpm for 0.5-120 minutes to obtain a mouthwash, toothpaste or enamel repair gel containing soluble calcium salt and soluble phosphate radical, wherein the ratio of the amount of substance of calcium ions contained in the lipophilic colloidally stabilized water-in-oil emulsion containing soluble calcium salt to the amount of substance of phosphate ions contained in the lipophilic colloidally stabilized water-in-oil emulsion containing soluble phosphate radical is 5: 3, the mass ratio of the lipophilic colloid-stabilized water-in-oil emulsion containing soluble calcium salt and the lipophilic colloid-stabilized water-in-oil emulsion containing soluble phosphate to the mouthwash matrix, the toothpaste matrix or the enamel repair gel matrix is 1: 19 to 19: 1.
the solid particles in the step 1) are one or a mixture of at least two of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, polystyrene, polyacrylic resin, natural plant powder and surface-modified natural plant powder thereof, cellulose and functional group amphiphilic derivatives thereof;
the solid particles are one or a mixture of at least two of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite and zeolite which are modified by a silane coupling agent, a titanate coupling agent and a surfactant;
the surfactant used for modifying the solid particles is all amphiphilic substances used for oral cleaning and nursing products and a composition of the amphiphilic substances in any proportion, and comprises one or a mixture of at least two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium lauryl sulfate, dextran glycoside type nonionic surfactant and betaine.
The oil in the step 1) is one or a mixture of at least two of rapeseed oil, peanut oil, cannabis 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, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, fish oil, frog oil, snake oil, silicone oil, straight-chain alkanes, lipids and alcohols which are not mutually soluble with water.
The titanate is butyl titanate, isobutyl titanate or ethyl titanate;
the silicate ester is tetraethyl silicate or tetrabutyl silicate.
The substance capable of generating free calcium ions is one or a mixture of at least two of calcium chloride, calcium carbonate, calcium hydroxide, calcium oxide, calcium phosphate salts, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium hydrogen sulfate and calcium lactate.
The substance capable of generating free phosphate radical is one or the mixture of at least two 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.
Compared with the prior art, the invention has the following advantages:
the invention wraps the soluble calcium salt and the soluble phosphate respectively as the inner water phase of the water-in-oil emulsion with stable lipophilic colloid, and adds the water-in-oil emulsion into toothpaste, enamel repair gel or mouthwash. The soluble calcium salt and soluble phosphate salt in the toothpaste, enamel repair gel or mouthwash prepared in this way can be stable for a long time at the same time. When the toothpaste, the enamel repairing gel or the mouthwash is used, the water-in-oil-in-water emulsion with stable solid particles is broken under the actions of friction, extrusion and the like, and soluble calcium salt and soluble phosphate which are wrapped in the internal water phase are released, so that the oral liquid contains calcium ions and phosphate ions with higher concentration, and the remineralization rate of enamel can be improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
1) Preparation of lipophilic colloid-stabilized water-in-oil emulsion containing soluble calcium salt and phosphate
Adding 0.1 g of silicon dioxide and 5 ml of butyl titanate into 100 g of rapeseed oil, heating to 30 ℃, and uniformly stirring to obtain an oil phase. Then 20 ml of 0.1% calcium chloride solution or 0.1% sodium phosphate solution and 100 ml of rapeseed oil containing silicon dioxide and butyl titanate are heated to 80 ℃ for mixing, and a high-speed dispersion machine is used for stirring for 120 minutes at the speed of 1000 r/min, thus obtaining the lipophilic colloid stable water-in-oil emulsion containing two different ions.
2) Preparation of toothpaste containing soluble calcium salt and soluble phosphate
Heating 0.5 g of lipophilic colloid-stabilized water-in-oil emulsion containing soluble calcium salt, lipophilic colloid-stabilized water-in-oil emulsion containing soluble phosphate and 9.5 g of toothpaste base to 30 deg.C, mixing, and dispersing with high speed disperser at 24000 rpm for 0.5 min to obtain toothpaste product; or mixing 0.5 g of a lipophilic colloidally stabilized water-in-oil emulsion containing a soluble calcium salt or phosphate with 9.5 g of a toothpaste base containing another salt (when the aqueous phase of the lipophilic colloidally stabilized water-in-oil emulsion contains a calcium salt; when the aqueous phase of the lipophilic colloidally stabilized water-in-oil emulsion contains a phosphate; the toothpaste base contains a calcium salt) by heating to 30 ℃ and dispersing at a rate of 24000 rpm for 0.5 minute by a high speed dispersing machine to obtain a finished toothpaste wherein the ratio of the amount of calcium ion-containing substance contained in the lipophilic colloidally stabilized water-in-oil emulsion containing a soluble calcium salt to the amount of phosphate ion-containing substance contained in the lipophilic colloidally stabilized water-in-oil emulsion containing a soluble phosphate is 5: 3.
enamel remineralization tests show that the enamel remineralization rate of the enamel in the embodiment is 30 and 35 times that of the common hydroxyapatite-containing toothpaste.
Example 2
This example is the same as example 1, except that: the solid particles are all organic, inorganic and natural polymers which can be used in oral cleaning and nursing products except silica particles, including but not limited to aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, polystyrene, polyacrylic resin, natural plant powder and surface modified natural plant powder thereof, one of cellulose and functional group amphiphilic derivatives thereof, or silica, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, magnesium oxide, calcium hydroxide, zinc oxide, polyethylene, calcium hydroxide, calcium carbonate, and/calcium carbonate, and/magnesium carbonate, calcium carbonate, or magnesium carbonate, The modified polypropylene composite material comprises at least two mixed particles of polystyrene, polyacrylic resin, natural plant powder and surface-modified natural plant powder thereof, cellulose and functional group amphiphilic derivatives thereof, or one or more mixed particles of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, kieselguhr, montmorillonite, hydrotalcite, mica, attapulgite and zeolite, which are modified by a silane coupling agent, a titanate coupling agent and a surfactant; the surfactant used for modifying the solid particles is one of or a mixture of at least two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium lauryl sulfate, dextran glycoside nonionic surfactant, betaine and the like; the soluble calcium salt is a substance capable of directly providing or degrading free calcium ions and comprises one of but not limited to calcium carbonate, calcium hydroxide, calcium oxide, calcium phosphate salts, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium hydrogen sulfate and calcium lactate, or a mixture of at least two of calcium chloride, calcium carbonate, calcium hydroxide, calcium oxide, calcium phosphate salts, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium hydrogen sulfate and calcium lactate; the soluble phosphate is one of 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 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; the oil is any nonpolar material which can be used for oral care including, but not limited to peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil (linseed oil), grape seed oil, walnut oil, peony seed oil, coconut oil, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, all fish oils, frog oil, snake oil, silicone oil, straight chain alkanes, lipids, alcohols immiscible with water, or rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil (linseed oil), grape seed oil, walnut oil, peony seed oil, coconut oil, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, all fish oils, frog oil, snake oil, silicone oil, sesame oil, linseed oil, sesame oil, linseed oil, lard, beef tallow, and the like, A mixed oil of at least two of straight-chain hydrocarbons, lipids and water-immiscible alcohols.
Enamel remineralization tests show that the rate of enamel remineralization in this example is 25-60 times that of a conventional hydroxyapatite-containing toothpaste.
Example 3
1) Lipophilic colloid-stabilized water-in-oil emulsions containing soluble calcium salts, phosphates are prepared.
Adding 0.5 g of calcium carbonate and 0.3 g of ethyl orthosilicate into 2 g of sunflower seed oil, heating to 80 ℃, and uniformly stirring to obtain an oil phase. Then 1.5 ml of 60 percent calcium nitrate solution or potassium dihydrogen phosphate solution and 1 ml of sunflower seed oil containing calcium carbonate and ethyl orthosilicate are heated to 30 ℃ for mixing, and stirred for 0.5 minute at the speed of 24000 r/min by a high-speed dispersion machine, so as to respectively obtain two lipophilic colloid-stable water-in-oil emulsions of which the water phases respectively contain calcium ions or phosphate ions.
2) Preparation of enamel restoration gel containing soluble calcium salt and soluble phosphate
Heating 4 g of lipophilic colloid-stabilized water-in-oil emulsion containing soluble calcium salt, 0.2 g of lipophilic colloid-stabilized water-in-oil emulsion containing soluble phosphate and 0.2 g of enamel repairing gel to 80 ℃ for mixing or directly mixing the two or mixing one of the two with a repairing gel matrix containing one ion out of forest, and stirring the mixture for 120 minutes at the speed of 300 revolutions per minute by using a high-speed disperser to obtain a finished toothpaste product containing both soluble calcium salt and soluble phosphate. The ratio of the amount of the substance containing calcium ions in the water-in-oil-in-water emulsion containing a soluble calcium salt to the amount of the substance containing phosphate ions in the water-in-oil-in-water emulsion containing a soluble phosphate salt is 5: 3.
enamel remineralization experiments showed that the enamel remineralization rate of this example was 45 times that of the conventional hydroxyapatite-containing toothpaste.
Example 4
This example is the same as example 3, except that: the solid particles used in the oral care composition include, but are not limited to, silica, alumina, bioactive glass, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomaceous earth, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, polystyrene, polyacrylic resin, natural plant powder and surface-modified natural plant powder thereof, cellulose and one of its functional group-containing amphiphilic derivatives, and mixed particles thereof, or silica, alumina, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomaceous earth, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, polystyrene, and mixtures thereof, The modified natural plant material comprises polyacrylic resin, natural plant powder and surface-modified natural plant powder thereof, and mixed particles of at least two of cellulose and functional group amphiphilic derivatives thereof, or one of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite and zeolite and mixed particles of at least two of the silicon dioxide, the aluminum oxide, the bioactive glass, the calcium carbonate, the calcium silicate, the calcium phosphate, the hydroxyapatite, the zinc oxide, the titanium dioxide, the magnesium carbonate, the magnesium hydroxide, the diatomite, the montmorillonite, the hydrotalcite, the mica, the attapulgite and the zeolite, which are modified by a silane coupling agent, a titanate coupling agent and a surfactant; the surfactant used for modifying the solid particles is one of or a mixture of at least two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium lauryl sulfate, dextran glycoside nonionic surfactant and betaine; the soluble calcium salt is a substance capable of directly providing or degrading free calcium ions and comprises one of but not limited to calcium carbonate, calcium hydroxide, calcium oxide, calcium phosphate salts, calcium gluconate, calcium bicarbonate, calcium hydrogen sulfate and calcium lactate, or a mixture of at least two of calcium chloride, calcium carbonate, calcium hydroxide, calcium oxide, calcium phosphate salts, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium hydrogen sulfate and calcium lactate; the soluble phosphate is one of sodium phosphate, ammonium phosphate, potassium monohydrogen phosphate, sodium monohydrogen phosphate, ammonium monohydrogen phosphate, sodium dihydrogen phosphate and ammonium dihydrogen phosphate, or a mixture of at least two 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; the oil is any nonpolar material which can be used for oral care including, but not limited to, rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, soybean oil, sesame oil, linseed oil (linseed oil), grape seed oil, walnut oil, peony seed oil, coconut oil, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, all fish oils, frog oil, snake oil, silicone oil, straight chain alkanes, lipids, alcohols immiscible with water, or rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil (linseed oil), grape seed oil, walnut oil, peony seed oil, coconut oil, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, all fish oils, frog oil, snake oil, silicone oil, sesame oil, linseed oil, sesame oil, linseed oil, lard, beef tallow, and the like, A mixed oil of at least two of straight-chain hydrocarbons, lipids, and water-immiscible alcohols; the precursor of the lipophilic colloid is titanate or silicate and their mixed esters.
Enamel remineralization tests show that the enamel remineralization rate of the present example is 23-83 times that of the common hydroxyapatite-containing toothpaste.
Claims (8)
1. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for modifying dental enamel products, comprising the steps of:
1) the preparation method of the lipophilic colloid stable water-in-oil emulsion containing soluble calcium salt and phosphate radical comprises the following steps:
according to the proportion of 0.1: 100-25: 100, adding solid particles with the particle size of 0.1-1000000 nanometers which can be dispersed in grease into water aqua or gel which can be used for preparing oral treatment, or natural grease which is used for preparing toothpaste or mouthwash, or tooth enamel or oral repair gel and is derived from plants, animals or minerals, or synthetic grease processed by petrochemical products and natural extraction raw materials, heating to 30-80 ℃, adding titanate or silicate into oil phase according to the mass ratio of 0.1: 1-15: 1, and stirring uniformly to form oil phase A;
adding a substance which can be dissolved in water and alcohol substances and can generate free calcium ions or free phosphate ions into water to prepare an aqueous solution with the concentration of the calcium ions or the phosphate ions of 0.1-60%, and mixing the aqueous solution and the oil phase A according to the weight ratio of 0.5: 9.5-1.5: mixing at a volume ratio of 0.5, placing on a high-speed dispersion machine, heating to 30-80 ℃, stirring at 10-24000 r/m for 0.5-120 minutes to obtain lipophilic colloid-stable water-in-oil emulsion A containing soluble calcium salt and lipophilic colloid-stable water-in-oil emulsion B containing phosphate radical;
2) mouthwash, toothpaste or enamel repair gels containing soluble calcium salts or soluble phosphate salts are prepared as follows:
mixing a lipophilic colloidally stabilized water-in-oil emulsion A containing soluble calcium salt and a lipophilic colloidally stabilized water-in-oil emulsion B containing phosphate which are heated to 30-80 ℃, with a mouthwash base, a toothpaste base or an enamel repair gel base, stirring for 0.5-120 minutes at 10-24000 r/min to obtain the mouthwash, toothpaste or enamel repair gel containing soluble calcium salt and soluble phosphate, wherein the ratio of the amount of calcium ion substances contained in the lipophilic colloidally stabilized water-in-oil emulsion A containing soluble calcium salt to the amount of phosphate ion substances contained in the lipophilic colloidally stabilized water-in-oil emulsion B containing soluble phosphate is 5: 3, the mass ratio of the total amount of lipophilic colloidally stabilized water-in-oil emulsion a containing soluble calcium salt and lipophilic colloidally stabilized water-in-oil emulsion B containing soluble phosphate to mouthwash base, toothpaste base or enamel repair gel base is 1: 19 to 19: 1.
2. a method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 1 characterised in that: the solid particles in the step 1) are one or a mixture of at least two of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite, zeolite, polyethylene, polystyrene, polyacrylic resin, natural plant powder and surface-modified natural plant powder thereof, cellulose and functional group amphiphilic derivatives thereof.
3. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 1 characterised in that: the solid particles in the step 1) are one or a mixture of at least two of silicon dioxide, aluminum oxide, bioactive glass, calcium carbonate, calcium silicate, calcium phosphate, hydroxyapatite, zinc oxide, titanium dioxide, magnesium carbonate, magnesium hydroxide, diatomite, montmorillonite, hydrotalcite, mica, attapulgite and zeolite which are modified by a silane coupling agent, a titanate coupling agent and a surfactant.
4. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 3, characterised in that: the surfactant used for modifying the solid particles is all amphiphilic substances used for oral cleaning and nursing products and a composition of the amphiphilic substances in any proportion, and comprises one or a mixture of at least two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, dextran glycoside type nonionic surfactant and betaine.
5. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 1 characterised in that: the oil in the step 1) is one or a mixture of at least two of rapeseed oil, peanut oil, cannabis 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, edible paraffin, turpentine oil, lard, beef tallow, mutton fat, fish oil, frog oil, snake oil and organic silicone oil.
6. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 1 characterised in that: the titanate is butyl titanate, isobutyl titanate or ethyl titanate; the silicate ester is tetraethyl silicate or tetrabutyl silicate.
7. A method of preparing a lipophilic colloid-stabilized water-in-oil emulsion for restorative enamel products according to claim 1, characterized in that: the substance capable of generating free calcium ions is one or a mixture of at least two of calcium chloride, calcium hydroxide, calcium nitrate, calcium gluconate, calcium hydrogen sulfate and calcium lactate.
8. A method of preparing a lipophilic colloidally stabilized water-in-oil emulsion for restorative enamel products according to claim 1 characterised in that: the substance capable of generating free phosphate radical is one or the mixture of at least two 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.
Priority Applications (1)
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| CN111249165A (en) | 2020-06-09 |
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