CN115024990A - Bioactive glass-based anhydrous toothpaste for repairing dentin and preparation method thereof - Google Patents
Bioactive glass-based anhydrous toothpaste for repairing dentin and preparation method thereof Download PDFInfo
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- CN115024990A CN115024990A CN202210641447.1A CN202210641447A CN115024990A CN 115024990 A CN115024990 A CN 115024990A CN 202210641447 A CN202210641447 A CN 202210641447A CN 115024990 A CN115024990 A CN 115024990A
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- calcium carbonate
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- bioactive glass
- stirring
- dentin
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- 239000005313 bioactive glass Substances 0.000 title claims abstract description 52
- 239000000606 toothpaste Substances 0.000 title claims abstract description 45
- 229940034610 toothpaste Drugs 0.000 title claims abstract description 43
- 210000004268 dentin Anatomy 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 180
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 90
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 25
- 239000010452 phosphate Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 22
- 239000000049 pigment Substances 0.000 claims abstract description 20
- 239000000022 bacteriostatic agent Substances 0.000 claims abstract description 19
- 239000004088 foaming agent Substances 0.000 claims abstract description 19
- 235000003599 food sweetener Nutrition 0.000 claims abstract description 19
- 239000003906 humectant Substances 0.000 claims abstract description 19
- 239000003765 sweetening agent Substances 0.000 claims abstract description 19
- 239000002562 thickening agent Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims description 67
- 239000000203 mixture Substances 0.000 claims description 24
- 239000006072 paste Substances 0.000 claims description 17
- 235000005979 Citrus limon Nutrition 0.000 claims description 14
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 12
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 12
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 12
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 12
- 239000001488 sodium phosphate Substances 0.000 claims description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 12
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 12
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 12
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- 229920002674 hyaluronan Polymers 0.000 claims description 10
- 229960003160 hyaluronic acid Drugs 0.000 claims description 10
- 235000013399 edible fruits Nutrition 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 235000006679 Mentha X verticillata Nutrition 0.000 claims description 6
- 235000002899 Mentha suaveolens Nutrition 0.000 claims description 6
- 235000001636 Mentha x rotundifolia Nutrition 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 6
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 6
- 229960001631 carbomer Drugs 0.000 claims description 6
- 235000015110 jellies Nutrition 0.000 claims description 6
- 239000008274 jelly Substances 0.000 claims description 6
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 6
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 6
- 235000010234 sodium benzoate Nutrition 0.000 claims description 6
- 239000004299 sodium benzoate Substances 0.000 claims description 6
- 239000000811 xylitol Substances 0.000 claims description 6
- 235000010447 xylitol Nutrition 0.000 claims description 6
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical group OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 6
- 229960002675 xylitol Drugs 0.000 claims description 6
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- 244000248349 Citrus limon Species 0.000 claims description 4
- 239000001052 yellow pigment Substances 0.000 claims description 4
- 239000001056 green pigment Substances 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 239000001055 blue pigment Substances 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 20
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 244000131522 Citrus pyriformis Species 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 7
- 230000008439 repair process Effects 0.000 description 7
- 229920002385 Sodium hyaluronate Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229940010747 sodium hyaluronate Drugs 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000008368 mint flavor Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000004383 yellowing Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 210000005239 tubule Anatomy 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- -1 sodium hyaluronate modified calcium carbonate Chemical class 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 208000008312 Tooth Loss Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000005115 demineralization Methods 0.000 description 1
- 230000002328 demineralizing effect Effects 0.000 description 1
- 201000002170 dentin sensitivity Diseases 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000036347 tooth sensitivity Effects 0.000 description 1
- 230000036345 yellow teeth Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- A61K8/25—Silicon; Compounds thereof
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of toothpaste, and particularly relates to anhydrous toothpaste for repairing dentin based on bioactive glass and a preparation method thereof, wherein the anhydrous toothpaste comprises the following components in parts by mass: 5-10 parts of phosphate, 10-30 parts of multi-stage calcium carbonate, 5-8 parts of bioactive glass, 1-3 parts of thickening agent, 0.2-1.4 parts of foaming agent, 5-20 parts of humectant, 0.1-0.3 part of bacteriostatic agent, 0.01-0.03 part of sweetening agent, 0.01 part of pigment and 0.2-0.6 part of essence, wherein the multi-stage calcium carbonate is formed by combining light calcium carbonate with different particle sizes; and provides a specific preparation method. The invention solves the problem of poor repairing effect of the existing toothpaste, realizes multi-angle repairing by utilizing different particle diameters of the multi-stage calcium carbonate, and realizes complete adsorption effect aiming at different sizes of damage.
Description
Technical Field
The invention belongs to the technical field of toothpaste, and particularly relates to anhydrous toothpaste for repairing dentin based on bioactive glass and a preparation method thereof.
Background
Toothpaste is an essential product in daily life. With the continuous improvement of living standard, the poor eating habit brings the health problem of oral cavity, especially the high sugar food. The high sugar remains in the oral cavity and is decomposed into acid, which can corrode tooth enamel and exposed dentin to produce demineralization of the enamel and dentin, seriously causing a series of diseases such as decayed teeth, tooth loss or tooth sensitivity and the like, and seriously affecting the health of people.
With the continuous development of toothpaste technology, anhydrous toothpaste is more and more emphasized by the characteristic of excellent stability of active substances, and meanwhile, the instability of the active substances in an aqueous environment is avoided, but the existing anhydrous toothpaste has a common repairing effect, particularly the fine part, and the treatment effect is difficult to achieve.
Description of the invention
Aiming at the problems in the prior art, the invention provides the anhydrous toothpaste for repairing dentin based on the bioactive glass, which solves the problem of poor repairing effect of the existing toothpaste, realizes multi-angle repair by utilizing different particle sizes of multi-stage calcium carbonate, and realizes complete adsorption effect aiming at different sizes of damages.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
an anhydrous toothpaste for restoring dentin based on bioactive glass comprises the following components in parts by mass:
5-10 parts of phosphate, 10-30 parts of multi-grade calcium carbonate, 5-8 parts of bioactive glass, 1-3 parts of thickening agent, 0.2-1.4 parts of foaming agent, 5-20 parts of humectant, 0.1-0.3 part of bacteriostatic agent, 0.01-0.03 part of sweetening agent, 0.01 part of pigment and 0.2-0.6 part of essence.
The phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, the proportion of the trisodium phosphate, the sodium dihydrogen phosphate and the disodium hydrogen phosphate is 1:2-3:3-4, the phosphate has good buffering performance, and the effect of effectively controlling pH is achieved, namely, the phosphate is slightly alkaline in the environment and can neutralize acid substances generated by high-sugar residues, so that the effect of improving the oral environment is achieved, and the influence caused by high-sugar acid conversion is effectively avoided. Meanwhile, the phosphate has phosphate radical and can be matched with free calcium ions to achieve the effect of repairing dentin; secondly, the acid and alkali of the phosphate is matched with the free state of the phosphate, so that a certain antibacterial effect is achieved in the tooth cleaning process.
The multistage calcium carbonate is formed by combining light calcium carbonate with different particle sizes, and the mass ratio of the multistage calcium carbonate is as follows: 5-10 parts of calcium carbonate with the diameter of 10-20 mu m, 5-10 parts of calcium carbonate with the diameter of 1-5 mu m and 1-3 parts of calcium carbonate with the diameter of 0.1-0.5 mu m. The calcium carbonate with different particle sizes is combined to form a multistage calcium carbonate system, the multistage calcium carbonate system can directly act on dentin surfaces with different damages, and can be deposited in different dentin areas by utilizing the matching of calcium carbonate with large particle sizes, medium particle sizes and small particle sizes based on the different particle sizes of the calcium carbonate, so that the deposition compactness of the dentin surfaces is improved, calcium ions and phosphate ions with higher concentration are provided for the subsequent biomineralization repairing dentin sheets, meanwhile, the calcium carbonate deposition with a low particle size structure can be used for the low particle size damages on dentin, the repairing can be completed in the early stage, and the excellent deposition repairing effect is achieved. From the aspect of the aperture of the dental tubule, calcium carbonate with large and medium particle diameters can form a dense repair effect to reduce the aperture of the dental tubule, and calcium carbonate with low particle diameter can enter from the gap between the calcium carbonate with large and medium particle diameters to block the dental tubule, so that the effect of thorough repair is achieved.
Further, the multistage calcium carbonate is pretreated before use, the pretreatment of the multistage calcium carbonate comprises a1, the multistage calcium carbonate is placed into an ethanol water solution for ultrasonic cleaning for 50min, the ethanol is added after filtration for washing for 20min, and the clean multistage calcium carbonate is obtained after drying, wherein the volume ratio of ethanol to water in the ethanol water solution is 3:2, the ultrasonic frequency of the ultrasonic cleaning is 50kHz, the temperature is 30 ℃, the mass ratio of the multistage calcium carbonate to the ethanol water solution is 5:1, the mass ratio of ethanol to the multistage calcium carbonate in the cleaning is 3:1, and the drying temperature is 80 ℃, ethanol water is used for ultrasonic cleaning, the large surface of the light calcium carbonate is rapidly cleaned, and the surface of the light calcium carbonate is clean; a2, adding sodium hyaluronate into water, stirring uniformly, adding multistage calcium carbonate, carrying out ultrasonic treatment for 30min, filtering, and airing to obtain sodium hyaluronate modified calcium carbonate, wherein the concentration of sodium hyaluronate in water is 2%, the stirring speed is 500r/min, the concentration of multistage calcium carbonate in a solution is 400g/L, the ultrasonic frequency is 50kHz, and the temperature is normal temperature. Hyaluronic acid is used as a modifier of calcium carbonate, can be uniformly dispersed in a solution by matching with the solubility of the hyaluronic acid in water, and is uniformly attached to the specific surface of calcium carbonate, namely, the large specific surface of light calcium carbonate is adsorbed by molecules of hyaluronic acid, so that the surface modification is realized. The molecular chain of hyaluronic acid in water is completely opened, and the hyaluronic acid is completely attached in the ultrasonic process, so that the porous structure in the light sodium carbonate is ensured to be attached. In the using process, molecular chains are opened when water molecules are encountered in the hyaluronic acid, and the effect of impurity adsorption is achieved by utilizing a certain negative electricity characteristic of the hyaluronic acid aqueous solution. In the last step, the porous calcium carbonate has good friction characteristics, a friction effect with multiple particle sizes is formed, impurities on the surface of dentin are removed, friction is loosened, the impurities are fixed by the adsorption force of hyaluronic acid, and a temporary removal effect is achieved; and secondly, the hyaluronic acid is attached to the surface of the calcium carbonate, is separated in the friction process, is in a free state, acts on the gum and improves the cell activity of the gum.
The bioactive glass is strontium-reinforced bioactive glass. The bioactive glass is silicate glass consisting of silicon dioxide, sodium oxide, calcium oxide and phosphorus pentoxide, the surface state of the bioactive glass can be converted into a hydroxyapatite carbonate structure with the passage of time, excellent bioactivity is shown, and a bonding interface is provided. The bioactive glass has an excellent repair system which can not only directly act on dentin, but also act on the connection between dentin and soft tissue. In the overall repairing process, the bioactive glass is used as a repairing main material, the multi-stage calcium carbonate is used as an auxiliary material, multiple repairing effects are formed, stable synergy can be formed by matching partial homogenization of the multi-stage calcium carbonate and the bioactive glass, and the gap repairing specificity of the low-particle-size calcium carbonate is assisted, so that the complete repairing effect is achieved.
The thickening agent adopts carbomer.
The foaming agent adopts sodium dodecyl sulfate.
The humectant adopts glycerin or polyethylene glycol 400.
The bacteriostatic agent adopts sodium benzoate.
The sweetener is xylitol.
The pigment is one of fruit green pigment, brilliant blue pigment or lemon yellow pigment.
The essence adopts mint essence.
The preparation method of the anhydrous toothpaste comprises the following steps:
step 1, uniformly stirring phosphate, multilevel calcium carbonate and bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 30-40 min;
step 2, adding the humectant, the thickener and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature to form a colloidal mixture, wherein the constant-temperature stirring temperature is 70 ℃, and the stirring speed is 500-;
step 3, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 4, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of the vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor repairing effect of the existing toothpaste, realizes multi-angle repairing by utilizing different particle diameters of the multi-stage calcium carbonate, and realizes complete adsorption effect aiming at different sizes of damage.
2. The invention utilizes the repairing performance of the bioactive glass to realize the high-efficiency repair of dentin, and simultaneously, the matching of the low particle size of calcium carbonate is matched to achieve the aim of deep repair, thereby realizing the complete repair of dentin.
3. The method provided by the invention has the advantages of simple process, uniform and stable paste and easy industrialization.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
An anhydrous toothpaste for restoring dentin based on bioactive glass comprises the following components in parts by mass:
5 parts of phosphate, 10 parts of multi-stage calcium carbonate, 5 parts of bioactive glass, 1 part of thickening agent, 0.2 part of foaming agent, 5 parts of humectant, 0.1 part of bacteriostatic agent, 0.01 part of sweetening agent, 0.01 part of pigment and 0.2 part of essence.
The phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the ratio of the trisodium phosphate, the sodium dihydrogen phosphate and the disodium hydrogen phosphate is 1:2: 3.
The multistage calcium carbonate is formed by combining light calcium carbonate with different particle sizes, and the mass ratio of the multistage calcium carbonate is as follows: 5 parts of 10-20 mu m calcium carbonate, 5 parts of 1-5 mu m calcium carbonate and 1 part of 0.1-0.5 mu m calcium carbonate.
The bioactive glass is strontium-reinforced bioactive glass.
The thickening agent adopts carbomer.
The foaming agent adopts sodium dodecyl sulfate.
The humectant adopts glycerin.
The bacteriostatic agent adopts sodium benzoate.
The sweetener is xylitol.
The pigment is fruit green pigment.
The essence adopts mint essence.
The preparation method of the anhydrous toothpaste comprises the following steps:
step 1, uniformly stirring phosphate, multilevel calcium carbonate and bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 30 min;
step 2, adding the humectant, the thickener and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature of 70 ℃ to form a colloidal mixture, wherein the stirring speed is 500 r/min;
step 3, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 4, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of the vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
The stability test is as follows:
initial state | 1 week | Half a month | 1 month | 3 months old | |
Appearance of the product | Fruit green | Fruit green | Fruit green | Fruit green | Fruit green |
Fragrant mint flavor | Is normal | Is normal | Is normal | Is normal | Is normal |
Amount of foam mm | 130 | 130 | 135 | 125 | 135 |
Thickness mm | 12 | 12 | 15 | 12 | 12 |
Stability of | Is normal and normal | Is normal | Is normal | Is normal | Is normal |
In the accelerated ageing test at 45 ℃, the paste did not develop oil for 3 months.
Example 2
An anhydrous toothpaste for restoring dentin based on bioactive glass comprises the following components in parts by mass:
10 parts of phosphate, 30 parts of multi-stage calcium carbonate, 8 parts of bioactive glass, 3 parts of thickening agent, 1.4 parts of foaming agent, 20 parts of humectant, 0.3 part of bacteriostatic agent, 0.03 part of sweetening agent, 0.01 part of pigment and 0.6 part of essence.
The phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the ratio of the trisodium phosphate, the sodium dihydrogen phosphate and the disodium hydrogen phosphate is 1:3: 4.
The multistage calcium carbonate is formed by combining light calcium carbonate with different particle sizes, and the mass ratio of the multistage calcium carbonate is as follows: 10 parts of 10-20 mu m calcium carbonate, 10 parts of 1-5 mu m calcium carbonate and 3 parts of 0.1-0.5 mu m calcium carbonate.
The bioactive glass is strontium-reinforced bioactive glass.
The thickening agent adopts carbomer.
The foaming agent adopts sodium dodecyl sulfate.
The humectant adopts polyethylene glycol 400.
The bacteriostatic agent adopts sodium benzoate.
The sweetener is xylitol.
The pigment is lucan pigment.
The essence adopts mint essence.
The preparation method of the anhydrous toothpaste comprises the following steps:
step 1, uniformly stirring phosphate, multilevel calcium carbonate and bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 40 min;
step 2, adding the humectant, the thickener and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature to form a colloidal mixture, wherein the constant-temperature stirring temperature is 70 ℃, and the stirring speed is 800 r/min;
step 3, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 4, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of the vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
The stability test is as follows:
initial state | 1 week | Half a month | 1 month | 3 months old | |
Appearance of the product | Light blue color | Brilliant blue color | Brilliant blue color | Light blue color | Brilliant blue color |
Fragrant mint flavor | Is normal | Is normal | Is normal and normal | Is normal | Is normal |
Foam amount mm | 115 | 120 | 125 | 120 | 120 |
Thickness mm | 9 | 12 | 12 | 12 | 12 |
Stability of | Is normal | Is normal | Is normal | Is normal | Is normal |
In the accelerated ageing test at 45 ℃, the paste did not develop oil for 3 months.
Example 3
An anhydrous toothpaste for restoring dentin based on bioactive glass comprises the following components in parts by mass:
8 parts of phosphate, 20 parts of multi-stage calcium carbonate, 7 parts of bioactive glass, 2 parts of thickening agent, 1 part of foaming agent, 10 parts of humectant, 0.2 part of bacteriostatic agent, 0.02 part of sweetening agent, 0.01 part of pigment and 0.4 part of essence.
The phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the ratio of the trisodium phosphate, the sodium dihydrogen phosphate and the disodium hydrogen phosphate is 1:3: 3.
The multistage calcium carbonate is formed by combining light calcium carbonate with different particle sizes, and the mass ratio of the multistage calcium carbonate is as follows: 8 parts of 10-20 mu m calcium carbonate, 8 parts of 1-5 mu m calcium carbonate and 2 parts of 0.1-0.5 mu m calcium carbonate.
The bioactive glass adopts strontium strengthened bioactive glass.
The thickening agent adopts carbomer.
The foaming agent is sodium dodecyl sulfate.
The humectant adopts glycerin.
The bacteriostatic agent adopts sodium benzoate.
The sweetener is xylitol.
The pigment is lemon yellow pigment.
The essence adopts mint essence.
The preparation method of the anhydrous toothpaste comprises the following steps:
step 1, uniformly stirring phosphate, multilevel calcium carbonate and bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 30 min;
step 2, adding the humectant, the thickening agent and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature of 70 ℃ at a stirring speed of 800r/min to form a colloidal mixture;
step 3, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 4, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of the vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
The stability test is as follows:
initial state | 1 week old | Half a month | 1 month | 3 months old | |
Appearance of the product | Lemon yellow | Lemon yellow | Lemon yellow | Lemon yellow | Lemon yellow |
Fragrant mint flavor | Is normal | Is normal | Is normal | Is normal | Is normal |
Amount of foam mm | 125 | 120 | 125 | 130 | 130 |
Thickness mm | 12 | 15 | 15 | 12 | 12 |
Stability of | Is normal | Is normal | Is normal | Is normal | Is normal and normal |
In the accelerated ageing test at 45 ℃, the paste did not produce oil for 3 months.
Example 4
An anhydrous toothpaste for restoring dentin based on bioactive glass comprises the following components in parts by mass:
8 parts of phosphate, 20 parts of multi-stage calcium carbonate, 7 parts of bioactive glass, 2 parts of thickening agent, 1 part of foaming agent, 10 parts of humectant, 0.2 part of bacteriostatic agent, 0.02 part of sweetening agent, 0.01 part of pigment and 0.4 part of essence.
The phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the ratio of the trisodium phosphate to the sodium dihydrogen phosphate to the disodium hydrogen phosphate is 1:3: 3.
The multistage calcium carbonate is formed by combining light calcium carbonate with different particle sizes, and the mass ratio of the multistage calcium carbonate is as follows: 8 parts of 10-20 mu m calcium carbonate, 8 parts of 1-5 mu m calcium carbonate and 2 parts of 0.1-0.5 mu m calcium carbonate.
The bioactive glass adopts strontium strengthened bioactive glass.
The thickening agent adopts carbomer.
The foaming agent adopts sodium dodecyl sulfate.
The humectant adopts glycerin.
The bacteriostatic agent adopts sodium benzoate.
The sweetener is xylitol.
The pigment is lemon yellow pigment.
The essence adopts mint essence.
The preparation method of the anhydrous toothpaste comprises the following steps:
step 1, pretreatment of multilevel calcium carbonate: a1, placing the multilevel calcium carbonate into an ethanol water solution, ultrasonically cleaning for 50min, filtering, adding ethanol, washing for 20min, drying to obtain clean multilevel calcium carbonate, the volume ratio of ethanol to water in the ethanol water solution is 3:2, the ultrasonic frequency of ultrasonic cleaning is 50kHz, the temperature is 30 ℃, the mass ratio of the multilevel calcium carbonate to the ethanol water solution is 5:1, the mass ratio of the ethanol to the multilevel calcium carbonate in washing is 3:1, the drying temperature is 80 ℃, a2, adding the sodium hyaluronate into water, stirring uniformly, then adding multilevel calcium carbonate for ultrasonic treatment for 30min, filtering and drying to obtain sodium hyaluronate modified calcium carbonate, the concentration of the sodium hyaluronate in water is 2 percent, the stirring speed is 500r/min, the concentration of the multistage calcium carbonate in the solution is 400g/L, the ultrasonic frequency is 50kHz, and the temperature is normal temperature;
step 2, uniformly stirring the phosphate, the multilevel calcium carbonate and the bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 30 min;
step 3, adding the humectant, the thickening agent and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature of 70 ℃ at a stirring speed of 800r/min to form a colloidal mixture;
step 4, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 5, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
The stability test is as follows:
initial state | 1 week | Half a month | 1 month | 3 months old | |
Appearance of the product | Lemon yellow | Lemon yellow | Lemon yellow | Lemon yellow | Lemon yellow |
Fragrant mint flavour | Is normal | Is normal | Is normal | Is normal | Is normal |
Amount of foam mm | 135 | 135 | 135 | 130 | 135 |
Thickness mm | 12 | 15 | 15 | 15 | 15 |
Stability of | Is normal | Is normal | Is normal and normal | Is normal | Is normal |
In the accelerated ageing test at 45 ℃, the paste did not develop oil for 3 months.
The tests were carried out using examples 3 and 4 as test examples and a commercial toothpaste containing bioactive glass as a comparative example (a dental care cream). Dividing 40 volunteers with red and swollen gums and yellow teeth into four groups, wherein three groups respectively adopt the toothpastes of example 3, example 4 and comparative example to brush teeth three times a day, and finally, the group is only rinsed with clear water; the volunteers who used the toothpastes of examples 3 and 4 all exhibited significant relief of gum redness, primarily improved tooth yellowing, completely disappeared redness after 7 days, significantly improved tooth yellowing, and teeth were whitened. After 14 days, teeth are obviously whitened, and yellow spots basically disappear; the volunteers adopting the comparative example have obvious red swelling and red swelling relief in 7 days, the tooth yellowing is improved, the tooth yellowing is obviously improved after 14 days, and meanwhile, the yellow spots are obviously reduced; the volunteers who gargle improved redness after 10 days, resolved slowly, and remained yellow after 14 days.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. An anhydrous toothpaste for repairing dentin based on bioactive glass, which is characterized in that: the mass ratio is as follows:
5-10 parts of phosphate, 10-30 parts of multi-stage calcium carbonate, 5-8 parts of bioactive glass, 1-3 parts of thickening agent, 0.2-1.4 parts of foaming agent, 5-20 parts of humectant, 0.1-0.3 part of bacteriostatic agent, 0.01-0.03 part of sweetening agent, 0.01 part of pigment and 0.2-0.6 part of essence; the multilevel calcium carbonate is formed by combining light calcium carbonate with different particle sizes.
2. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: the phosphate is a composition of trisodium phosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the ratio of the trisodium phosphate to the sodium dihydrogen phosphate to the disodium hydrogen phosphate is 1:2-3: 3-4.
3. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: the multistage calcium carbonate comprises the following components in percentage by mass: 5-10 parts of calcium carbonate with the diameter of 10-20 mu m, 5-10 parts of calcium carbonate with the diameter of 1-5 mu m and 1-3 parts of calcium carbonate with the diameter of 0.1-0.5 mu m.
4. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 3, wherein: before the multilevel calcium carbonate is used, hyaluronic acid modification pretreatment is carried out.
5. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: the bioactive glass is strontium-reinforced bioactive glass.
6. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: carbomer is adopted as the thickening agent, and sodium dodecyl sulfate is adopted as the foaming agent; the humectant adopts glycerin or polyethylene glycol 400.
7. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: the bacteriostatic agent adopts sodium benzoate; the sweetener is xylitol.
8. The bioactive glass dentin-restoring anhydrous toothpaste according to claim 1, wherein: the pigment is one of fruit green pigment, brilliant blue pigment or lemon yellow pigment.
9. The bioactive glass restorative dentin-based anhydrous toothpaste according to claim 1, wherein: the essence adopts mint essence.
10. The bioactive glass restorative dentin-based anhydrous toothpaste according to claim 1, wherein: the preparation method of the anhydrous toothpaste comprises the following steps:
step 1, uniformly stirring phosphate, multilevel calcium carbonate and bioactive glass to form a mixture, wherein the stirring speed is 500r/min, and the stirring time is 30-40 min;
step 2, adding the humectant, the thickener and the foaming agent into a homogenizer, uniformly stirring, and stirring at a constant temperature to form a colloidal mixture, wherein the constant-temperature stirring temperature is 70 ℃, and the stirring speed is 500-;
step 3, adding the mixture into the mixed jelly, vacuumizing and stirring to form a prefabricated paste, wherein the vacuumizing and stirring vacuum degree is-0.01 MPa to-0.05 MPa, and the time is 40 min;
and 4, sequentially adding the bacteriostatic agent, the pigment, the sweetening agent and the essence into the prefabricated paste, and continuously stirring in vacuum to obtain the anhydrous toothpaste, wherein the vacuum degree of the vacuum stirring is-0.04 MPa to-0.07 MPa, and the time is 30 min.
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CN101500622A (en) * | 2006-06-16 | 2009-08-05 | 帝国创新有限公司 | Bioactive glass |
US20120020898A1 (en) * | 2009-04-01 | 2012-01-26 | Colgate-Palmolive Company | Non-aqueous dentifrice composition with bioacceptable and bioactive glass and methods of use and manufacture thereof |
CN106511105A (en) * | 2017-01-10 | 2017-03-22 | 杭州皎洁口腔保健用品有限公司 | Anhydrous toothpaste repairing demineralized enamel and dentin and preparation method thereof |
CN111093604A (en) * | 2017-08-18 | 2020-05-01 | 荷兰联合利华有限公司 | Oral care compositions |
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CN101500622A (en) * | 2006-06-16 | 2009-08-05 | 帝国创新有限公司 | Bioactive glass |
US20120020898A1 (en) * | 2009-04-01 | 2012-01-26 | Colgate-Palmolive Company | Non-aqueous dentifrice composition with bioacceptable and bioactive glass and methods of use and manufacture thereof |
CN106511105A (en) * | 2017-01-10 | 2017-03-22 | 杭州皎洁口腔保健用品有限公司 | Anhydrous toothpaste repairing demineralized enamel and dentin and preparation method thereof |
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