CN117982361A - Submicron whitening toothpaste for inhibiting dental plaque and preparation method thereof - Google Patents
Submicron whitening toothpaste for inhibiting dental plaque and preparation method thereof Download PDFInfo
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- CN117982361A CN117982361A CN202410396413.XA CN202410396413A CN117982361A CN 117982361 A CN117982361 A CN 117982361A CN 202410396413 A CN202410396413 A CN 202410396413A CN 117982361 A CN117982361 A CN 117982361A
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- 239000000606 toothpaste Substances 0.000 title claims abstract description 56
- 229940034610 toothpaste Drugs 0.000 title claims abstract description 49
- 230000002087 whitening effect Effects 0.000 title claims abstract description 46
- 208000002064 Dental Plaque Diseases 0.000 title claims abstract description 20
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- QCZAWDGAVJMPTA-RNFRBKRXSA-N ClC1=CC=CC(=N1)C1=NC(=NC(=N1)N[C@@H](C(F)(F)F)C)N[C@@H](C(F)(F)F)C Chemical compound ClC1=CC=CC(=N1)C1=NC(=NC(=N1)N[C@@H](C(F)(F)F)C)N[C@@H](C(F)(F)F)C QCZAWDGAVJMPTA-RNFRBKRXSA-N 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 229940068475 zinc citrate Drugs 0.000 claims abstract description 20
- 235000006076 zinc citrate Nutrition 0.000 claims abstract description 20
- 239000011746 zinc citrate Substances 0.000 claims abstract description 20
- WGIWBXUNRXCYRA-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WGIWBXUNRXCYRA-UHFFFAOYSA-H 0.000 claims abstract description 18
- 239000003906 humectant Substances 0.000 claims abstract description 17
- 239000004088 foaming agent Substances 0.000 claims abstract description 13
- 235000003599 food sweetener Nutrition 0.000 claims abstract description 13
- 239000003765 sweetening agent Substances 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 13
- XGRSAFKZAGGXJV-UHFFFAOYSA-N 3-azaniumyl-3-cyclohexylpropanoate Chemical compound OC(=O)CC(N)C1CCCCC1 XGRSAFKZAGGXJV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960004711 sodium monofluorophosphate Drugs 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 12
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 claims description 12
- 239000000049 pigment Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 10
- 239000003755 preservative agent Substances 0.000 claims description 10
- 230000002335 preservative effect Effects 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 229920005862 polyol Polymers 0.000 claims description 8
- 150000003077 polyols Chemical class 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 239000000084 colloidal system Substances 0.000 claims description 6
- 229940117955 isoamyl acetate Drugs 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- 229940083982 sodium phytate Drugs 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical group OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical group O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 229940085605 saccharin sodium Drugs 0.000 claims description 2
- 108700004121 sarkosyl Proteins 0.000 claims description 2
- 229960004029 silicic acid Drugs 0.000 claims description 2
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 claims description 2
- 229940045885 sodium lauroyl sarcosinate Drugs 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 239000000230 xanthan gum Substances 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 235000010493 xanthan gum Nutrition 0.000 claims description 2
- 229940082509 xanthan gum Drugs 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 1
- 210000000214 mouth Anatomy 0.000 abstract description 8
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract description 5
- 244000052616 bacterial pathogen Species 0.000 abstract description 3
- 208000002925 dental caries Diseases 0.000 abstract description 2
- 208000028169 periodontal disease Diseases 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 31
- 238000012360 testing method Methods 0.000 description 15
- 239000000523 sample Substances 0.000 description 13
- 230000000844 anti-bacterial effect Effects 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000005764 inhibitory process Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 241000605862 Porphyromonas gingivalis Species 0.000 description 4
- 241000194019 Streptococcus mutans Species 0.000 description 4
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 229960003500 triclosan Drugs 0.000 description 4
- -1 2% PVM/MA Chemical compound 0.000 description 3
- 208000006558 Dental Calculus Diseases 0.000 description 3
- 206010020751 Hypersensitivity Diseases 0.000 description 3
- 206010044029 Tooth deposit Diseases 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 208000026935 allergic disease Diseases 0.000 description 3
- 230000007815 allergy Effects 0.000 description 3
- 230000003266 anti-allergic effect Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 210000004262 dental pulp cavity Anatomy 0.000 description 2
- 210000004268 dentin Anatomy 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005660 hydrophilic surface Effects 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 230000007830 nerve conduction Effects 0.000 description 2
- 210000001640 nerve ending Anatomy 0.000 description 2
- 210000002569 neuron Anatomy 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 159000000001 potassium salts Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 210000003296 saliva Anatomy 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 206010006326 Breath odour Diseases 0.000 description 1
- 208000032139 Halitosis Diseases 0.000 description 1
- 208000005888 Periodontal Pocket Diseases 0.000 description 1
- 208000010641 Tooth disease Diseases 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000022 bacteriostatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 206010006514 bruxism Diseases 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 201000002170 dentin sensitivity Diseases 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000006916 nutrient agar Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 230000003239 periodontal effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000036347 tooth sensitivity Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Cosmetics (AREA)
Abstract
The invention relates to the technical field of oral care products, in particular to submicron whitening toothpaste for inhibiting dental plaque and a preparation method thereof; the submicron whitening toothpaste comprises the following components in percentage by weight: 0.1 to 1 percent of submicron sphere, 0.1 to 2 percent of PVM/MA, 0.01 to 0.1 percent of zinc citrate, 0.7 to 0.8 percent of sodium monofluorophosphate, 0.5 to 3.5 percent of whitening agent, 15 to 25 percent of friction agent, 1.5 to 3 percent of foaming agent, 45 to 60 percent of humectant, 0.5 to 2 percent of thickening agent, 1.0 to 1.5 percent of essence, 0.1 to 1 percent of sweetener and the balance of water; the submicron spheres and PVM/MA in the invention sequentially wrap zinc citrate and form a film to be adhered on the surfaces of teeth and gums, slowly release zinc ions in the oral cavity, inhibit the growth and reproduction of various pathogenic bacteria causing dental caries and periodontal diseases in the oral cavity, and inhibit the generation of dental plaque.
Description
Technical Field
The invention relates to the technical field of oral care products, in particular to submicron whitening toothpaste for inhibiting dental plaque and a preparation method thereof.
Background
Toothpaste is a common cleaning product in daily life and has a long history. With the continuous development of science and technology, technological equipment is continuously improved and perfected, various types of toothpastes are continuously developed, the quality and grade of products are continuously improved, the types of toothpastes are developed into complete types and functions from single clean toothpastes, and the requirements of different levels of consumption are met.
Plaque is a bacterial ecological environment that exists in the tooth surface or periodontal pocket where bacteria grow, develop and decay and undergo complex metabolic activities of matter that under certain conditions, bacteria and their products will destroy the teeth and periodontal tissue. Plaque is a soft, unmineralized colony of bacteria that adheres to tooth surfaces and is not readily noticeable in small amounts. However, with the increase of time, bacterial plaque is not removed in time, which causes stubborn spots and stains which cannot be removed by daily oral care, and the surfaces of teeth lose luster and turn yellow and dark.
The existing toothpaste is basically used for grinding teeth through a friction agent to realize cleaning and whitening, and essence is added to enable the toothpaste to freshen breath, but the inside of an oral cavity is provided with a complex colony environment, teeth can be cleaned only by grinding common toothpaste and only temporarily by the essence, but the colony environment of the oral cavity cannot be changed, if the colony environment of the oral cavity is unbalanced, the problems of dental caries, dental plaque, halitosis and the like can be caused, and the dental plaque cannot be cleaned by the existing grinding type toothpaste.
Therefore, development of a composition which can effectively remove dental plaque and has an important effect on preventing the occurrence of oral problems associated with dental plaque.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide submicron whitening toothpaste capable of effectively inhibiting dental plaque.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
a submicron whitening toothpaste for inhibiting dental plaque comprises the following components in percentage by weight: 0.1 to 1 percent of submicron sphere, 0.1 to 2 percent of PVM/MA, 0.01 to 0.1 percent of zinc citrate, 0.76 percent of sodium monofluorophosphate, 0.5 to 3.5 percent of whitening agent, 15 to 25 percent of friction agent, 1.5 to 3 percent of foaming agent, 45 to 60 percent of humectant, 0.5 to 2 percent of thickening agent, 1.0 to 1.5 percent of essence, 0.1 to 1 percent of sweetener and the balance of water.
Preferably, the submicron spheres are made by the following method:
S1: adding a silane coupling agent, silica colloid particles and isoamyl acetate into water, and stirring to form emulsion;
S2: heating the emulsion to a temperature higher than 60 ℃, and adding persulfate as an initiator to initiate polymerization;
s3: and drying to obtain a powdery product which is the submicron sphere.
Preferably, the stirring time in the step S1 is 15 to 25 hours, and the polymerization time in the step S3 is 10 to 15 hours.
Preferably, the particle size of the silica colloid particles is 30 to 40 nm.
Preferably, the whitening agent is at least one selected from pearl powder, sodium phytate, tetrapotassium pyrophosphate and tetrasodium pyrophosphate.
Preferably, the friction agent is hydrated silica; the foaming agent consists of sodium lauryl sulfate and sodium lauroyl sarcosinate.
Preferably, the humectant is selected from at least one of sorbitol, glycerin, and polydiethanol-8; the thickener consists of cellulose gum and xanthan gum; the sweetener is saccharin sodium.
Preferably, the composition further comprises the following components in percentage by weight: 0.1 to 0.3 percent of preservative and 0.1 to 0.5 percent of pigment.
The invention also aims to provide a preparation method of the submicron whitening toothpaste, which comprises the following steps of dispersing a thickener into a humectant to form a polyol phase; dissolving sweetener in water and humectant to form water phase; mixing the water phase and the polyol phase, and grinding and homogenizing for 10-15 minutes to obtain uniform glue; then adding a whitening agent, an abrasive, zinc citrate, sodium monofluorophosphate and PVM/MA, grinding and homogenizing for 20-25 minutes; and adding the foaming agent, stirring for 10-15 minutes in vacuum, adding the preservative, the submicron spheres, the essence and the pigment, stirring for 5-10 minutes in vacuum, closing stirring, and breaking vacuum to obtain the submicron whitening toothpaste.
The application has the following beneficial effects:
(1) The invention combines submicron spheres, PVM/MA (methyl vinyl ether/maleic anhydride copolymer) and zinc citrate, the PVM/MA wraps the zinc citrate and forms a film to adhere on the surfaces of teeth and gums, zinc ions are slowly released in the oral cavity, various bacteria causing saw teeth and periodontal diseases are killed, and the generation of dental plaque is inhibited; the submicron sphere has a hydrophobic cavity and a hydrophilic surface, and can further wrap PVM/MA which is hydrophobic and wraps zinc citrate, so as to form a slow release body with a double-layer wrapping structure, and prolong the action time and the utilization rate of zinc ions; the three components are synergistic, can continuously inhibit the growth and reproduction of harmful microorganisms in the oral cavity, inhibit the generation of dental plaque, and is nontoxic and harmless to human bodies.
(2) The submicron spheres prepared by the invention take isoamyl acetate as a template, the template is removed in the drying process, the conditions are mild, and the operation is simple and convenient; compared with the conventional preparation method of the submicron spheres, the subsequent module removing process is omitted, and the shell layer is not damaged; in addition, the isoamyl acetate can leave nano-pore channels in the shell layer in the volatilization process, so that the submicron spheres have larger specific surface area, and the encapsulation rate of PVM/MA is improved.
(3) The whitening agent disclosed by the invention grinds teeth by using pearl powder, and rubs off dirt and pigment on the surfaces of the teeth, so that the whitening effect is achieved; complexing sodium phytate with dental calculus component to avoid or relieve dental calculus, and separating dental calculus from tooth surface; removing pigment component adsorption by tetrapotassium pyrophosphate and tetrasodium pyrophosphate, softening color spots, cleaning and whitening; in addition, potassium ions in tetrapotassium pyrophosphate are wrapped by the single-layer or double-layer structure, so that the residual saliva in the root canal of the tooth is prevented from flushing, the potassium salt is delivered into neurons and nerve endings in a sufficient concentration, thereby preventing nerve conduction, relieving pain and preventing tooth allergy.
Detailed Description
The present invention will be further described with reference to examples, but the scope of the invention as claimed is not limited to the scope expressed by the examples.
Example 1
The submicron whitening toothpaste for inhibiting dental plaque comprises the following components in percentage by weight: 0.1% of submicron sphere, 0.1% of PVM/MA, 0.01% of zinc citrate, 0.76% of sodium monofluorophosphate, 0.5% of whitening agent, 15% of friction agent, 2.0% of foaming agent, 57% of humectant, 1.0% of thickening agent, 1.1% of essence, 0.2% of sweetener, 0.15% of preservative, 0.1% of pigment and the balance of deionized water.
The submicron spheres are prepared by the following method:
S1: adding a silane coupling agent, silica colloid particles and isoamyl acetate into water, and stirring to form emulsion;
S2: heating the emulsion to a temperature higher than 60 ℃, and adding persulfate as an initiator to initiate polymerization;
s3: and drying to obtain a powdery product which is the submicron sphere.
S1: adding 5mL of silane coupling agent KH-560, 7mL of silica colloid particle dispersion liquid with the particle size of 30-40 nanometers and 10mL of isoamyl acetate into 400mL of deionized water, and stirring at 15 ℃ for 15 hours to form emulsion;
S2: introducing nitrogen gas into the emulsion for discharging oxygen for 30 minutes, heating to 65 ℃, adding 100mg of potassium persulfate to initiate polymerization, and continuing the polymerization for 10 hours;
S3: and (3) centrifugally separating the emulsion, washing the emulsion with ethanol for 3 times, dispersing the emulsion in deionized water, and freeze-drying the emulsion to obtain white powdery solid, namely submicron spheres with hydrophobic cavities and hydrophilic surfaces.
The preparation method of the submicron whitening toothpaste comprises the following steps: dispersing a thickener into a humectant to form a polyol phase; dissolving sweetener in water and humectant to form water phase; mixing the water phase and the polyol phase, and grinding and homogenizing for 10-15 minutes to obtain uniform glue; then adding a whitening agent, an abrasive, zinc citrate, sodium monofluorophosphate and PVM/MA, grinding and homogenizing for 20-25 minutes; and adding the foaming agent, stirring for 10-15 minutes in vacuum, adding the preservative, the submicron spheres, the essence and the pigment, stirring for 5-10 minutes in vacuum, closing stirring, and breaking vacuum to obtain the submicron whitening toothpaste capable of effectively inhibiting dental plaque.
Example 2
The submicron whitening toothpaste for inhibiting dental plaque comprises the following components in percentage by weight: 1% of submicron sphere, 2% of PVM/MA, 0.1% of zinc citrate, 0.76% of sodium monofluorophosphate, 3.5% of whitening agent, 20% of friction agent, 3% of foaming agent, 52% of humectant, 1.2% of thickening agent, 1.2% of essence, 0.15% of sweetener, 0.2% of preservative, 0.2% of pigment and the balance of deionized water.
The preparation method of the submicron spheres of this example is the same as that of example 1.
The preparation method of the submicron whitening toothpaste of this example is the same as that of example 1.
Example 3
The submicron whitening toothpaste for inhibiting dental plaque comprises the following components in percentage by weight: 1% of submicron sphere, 2% of PVM/MA, 0.1% of zinc citrate, 0.76% of sodium monofluorophosphate, 2.3% of whitening agent, 25% of friction agent, 2.4% of foaming agent, 49% of humectant, 0.8% of thickening agent, 1.3% of essence, 0.18% of sweetener, 0.2% of preservative, 0.3% of pigment and the balance of deionized water.
The preparation method of the submicron spheres of this example is the same as that of example 1.
The preparation method of the submicron whitening toothpaste of this example is the same as that of example 1.
Example 4
The submicron whitening toothpaste for inhibiting dental plaque comprises the following components in percentage by weight: 0.5% of submicron sphere, 1% of PVM/MA, 0.1% of zinc citrate, 0.76% of sodium monofluorophosphate, 2.3% of whitening agent, 25% of friction agent, 2.4% of foaming agent, 49% of humectant, 1% of thickening agent, 1.3% of essence, 0.18% of sweetener, 0.2% of preservative, 0.5% of pigment and the balance of deionized water.
The preparation method of the submicron spheres of this example is the same as that of example 1.
The preparation method of the submicron whitening toothpaste of this example is the same as that of example 1.
The content of the components in examples 1 to 4 is shown in Table 1 below:
Table 1 Table of the formulations of submicron whitening toothpastes in examples 1 to 4
Comparative example 1
A toothpaste having a composition that differs from example 3 in that the PVM/MA is replaced with an equal amount of deionized water (i.e., 2% PVM/MA is omitted).
The preparation method of the submicron spheres of this comparative example is the same as in example 1.
The toothpaste of this comparative example was prepared in the same manner as in example 1 (when a component was absent, the component was omitted).
Comparative example 2
A toothpaste having a composition that differs from example 3 in that the sub-micron spheres are replaced with an equal amount of deionized water (i.e., 1% of the sub-micron spheres are omitted).
The toothpaste of this comparative example was prepared in the same manner as in example 1 (when a component was absent, the component was omitted).
Comparative example 3
A toothpaste having a composition that differs from example 3 in that 3% deionized water is used instead of PVM/MA and submicron spheres (i.e., 2% PVM/MA and 1% submicron spheres are omitted simultaneously).
The toothpaste of this comparative example was prepared in the same manner as in example 1 (when a component was absent, the component was omitted).
Comparative example 4
A toothpaste having a composition that differs from example 3 in that 3.1% triclosan is used in place of PVM/MA, submicron spheres and zinc citrate (i.e., 2% PVM/MA, 1% submicron spheres and 0.1% zinc citrate are omitted simultaneously, and 3.1% triclosan is supplemented).
The preparation method of the toothpaste of the comparative example comprises the following steps: dispersing a thickener into a humectant to form a polyol phase; dissolving sweetener in water and humectant to form water phase; mixing the water phase and the polyol phase, and grinding and homogenizing for 10-15 minutes to obtain uniform glue; then adding a whitening agent, an abrasive agent and sodium monofluorophosphate, and grinding and homogenizing for 20-25 minutes; and adding the foaming agent, stirring for 10-15 minutes in vacuum, adding the preservative, the essence and the pigment, stirring for 5-10 minutes in vacuum, closing stirring, and breaking vacuum to obtain the finished product.
Antibacterial test
The toothpaste prepared in examples 1 to 4 and comparative examples 1 to 4 were used for antibacterial tests according to the antibacterial test method of "sterilizing technical Specification" 2.1.8.
Preparation of antibacterial tablets: in a clean sterile plate, the raw paste of the bacteriostat is prepared into discs (blocks) with the diameter of 5mm and the thickness of not more than 4mm, and each 4 discs are combined.
Inoculation of test bacteria: dipping a sterile cotton swab into test bacterial suspension with the concentration of 5 x 10 5cfu/ml～5*106 cfu/ml, uniformly smearing the test bacterial suspension on the surface of a nutrient agar culture medium flat plate for 3 times, rotating the flat plate for 60 degrees every 1 time, smearing the cotton swab around the edge of the flat plate for one circle, covering the flat plate, and drying at room temperature for 5min.
Sticking and placing a bacteriostatic agent sample wafer: 1 bacteria-contaminated flat plate is attached to each test, and 4 test pieces of the same test group are attached to each flat plate. The sample piece was attached to the surface of the plate using sterile forceps. The distance between the centers of the sample pieces is more than 25mm, and the distance between the centers of the sample pieces and the periphery of the flat plate is more than 15 mm. After the sticking, the sample wafer is lightly pressed by sterile forceps to be tightly attached to the surface of the flat plate. The plates were covered and incubated in a 37℃incubator for 12h, 24h, 48 h. The diameter of the inhibition ring was measured with a vernier caliper, recorded and the average value calculated.
The strain tested at this time selects common oral pathogenic bacteria: streptococcus mutans and Porphyromonas gingivalis.
Bacteriostasis test evaluation criteria: when the diameter of the bacteriostasis ring is larger than 7mm, the bacteriostasis ring is judged to have bacteriostasis; and when the diameter of the inhibition ring is smaller than or equal to 7mm, judging that no inhibition effect exists.
The test results are shown in tables 2 to 4 below:
TABLE 2 diameter data of inhibition zone after 12h of incubation
| Group of | Streptococcus mutans | Porphyromonas gingivalis |
| Example 1 | 14.6 | 12.2 |
| Example 2 | 17.6 | 15.1 |
| Example 3 | 17.0 | 14.5 |
| Example 4 | 15.9 | 13.7 |
| Comparative example 1 | 10.8 | 8.3 |
| Comparative example 2 | 9.7 | 5.1 |
| Comparative example 3 | 5.3 | 4.6 |
| Comparative example 4 | 16.8 | 13.8 |
TABLE 3 diameter data of inhibition zone after 24h of incubation
| Group of | Streptococcus mutans | Porphyromonas gingivalis |
| Example 1 | 13.4 | 10.1 |
| Example 2 | 16.6 | 13.9 |
| Example 3 | 15.8 | 13.4 |
| Example 4 | 13.7 | 11.6 |
| Comparative example 1 | 9.1 | 7.7 |
| Comparative example 2 | 8.2 | 6.2 |
| Comparative example 3 | 3.1 | 2.2 |
| Comparative example 4 | 14.5 | 11.6 |
TABLE 4 diameter data of inhibition zone after 48h of culture
| Group of | Streptococcus mutans | Porphyromonas gingivalis |
| Example 1 | 12.2 | 8.9 |
| Example 2 | 15.4 | 12.6 |
| Example 3 | 14.6 | 12.1 |
| Example 4 | 10.5 | 8.4 |
| Comparative example 1 | 6.8 | 5.5 |
| Comparative example 2 | 5.8 | 3.9 |
| Comparative example 3 | 0.4 | * |
| Comparative example 4 | 7.2 | 5.8 |
Note that: the "×" in table 4 indicates that the diameter of the zone of inhibition could not be detected.
As can be seen from Table 2, after 12 hours of culture, the antibacterial effect of the toothpaste in examples 1-4 is equivalent to that of the toothpaste in comparative example 4, and is obviously better than that of the toothpaste in comparative examples 1-3, which shows that the submicron sphere, PVM/MA and zinc citrate compound can replace triclosan with potential safety hazard and has good inhibition effect on oral pathogenic bacteria.
As can be seen from Table 3, after 24 days of culture, the antibacterial effect of the toothpaste of examples 1-4 is significantly better than that of the toothpaste of comparative example 4, and is significantly better than that of the toothpaste of comparative examples 1-3, which means that the submicron sphere, PVM/MA and zinc citrate compound can prolong the action time of zinc ions, and the three synergistically cooperate to continuously inhibit the growth and propagation of harmful microorganisms in the oral cavity and inhibit the generation of dental plaque.
As can be seen from Table 4, after 48 days of culture, the antibacterial effect of the toothpastes in examples 1 to 4 is significantly better than that of the toothpastes in comparative examples 1 to 4, which means that the combination of submicron spheres, PVM/MA and zinc citrate can prolong the action time of zinc ions, and the three are synergistic, and can still effectively exert the antibacterial effect after 48 hours, but neither triclosan nor zinc citrate can effectively inhibit the antibacterial effect when any of the submicron spheres or PVM/MA is lacked.
Antiallergic test
The test method comprises the following steps: the test was performed by selecting 70 subjects with oral allergy and discomfort, half of each of men and women, ages 25 to 45 years, and average ages 30 years. The toothpastes prepared in examples 1 to 4 and comparative examples 1 to 3 of the present invention were used for brushing teeth, respectively, 10 persons in each group were randomly divided into 7 groups, and brushing teeth was performed once a day in the morning and at the evening, and after continuous use for 2 months, a probe sensitivity test was performed to calculate average score.
The probe sensitivity test was: the tooth sensitivity index was tested using an electronic pressure sensitive probe that contacted the dentin exposed on the buccal surface of the selected tooth and placed at the enamel dentin junction, and the force of the probe contact was set at 50g.
The judgment score is: 0: the probe is contacted without any pain; 1: slightly uncomfortable contact of the probe, basically no pain; 2: the probe has pain feeling when in contact, but can still endure; 3: the probe is in contact with severe pain and cannot be tolerated.
The test results are shown in Table 5 below:
Table 5 antiallergic score data
| Group of | Average distribution before use | Average after use |
| Example 1 | 2.7 | 0.9 |
| Example 2 | 2.8 | 0.7 |
| Example 3 | 2.7 | 0.8 |
| Example 4 | 2.8 | 0.9 |
| Comparative example 1 | 2.6 | 1.3 |
| Comparative example 2 | 2.7 | 1.1 |
| Comparative example 3 | 2.8 | 2.6 |
As shown in Table 5, the toothpaste prepared by the invention has good antiallergic effect, potassium ions in tetrapotassium pyrophosphate are coated by PVM/MA or (and) submicron spheres in a single layer or double layers, and the potassium salts are prevented from being scoured by remained saliva in a root canal, so that the potassium salts are delivered into neurons and nerve endings in a sufficient concentration, thereby preventing nerve conduction, relieving pain and preventing tooth allergy.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (9)
1. The submicron whitening toothpaste for inhibiting dental plaque is characterized by comprising the following components in percentage by weight: 0.1 to 1 percent of submicron sphere, 0.1 to 2 percent of PVM/MA, 0.01 to 0.1 percent of zinc citrate, 0.7 to 0.8 percent of sodium monofluorophosphate, 0.5 to 3.5 percent of whitening agent, 15 to 25 percent of friction agent, 1.5 to 3 percent of foaming agent, 45 to 60 percent of humectant, 0.5 to 2 percent of thickening agent, 1.0 to 1.5 percent of essence, 0.1 to 1 percent of sweetener and the balance of water.
2. The submicron whitening toothpaste according to claim 1, characterized in that the submicron spheres are prepared by the following method:
S1: adding a silane coupling agent, silica colloid particles and isoamyl acetate into water, and stirring to form emulsion;
S2: heating the emulsion to a temperature higher than 60 ℃, and adding persulfate as an initiator to initiate polymerization;
s3: and drying to obtain a powdery product which is the submicron sphere.
3. The submicron whitening toothpaste according to claim 2, characterized in that the stirring time in step S1 is 15 to 25 hours, and the polymerization time in step S3 is 10 to 15 hours.
4. The submicron whitening toothpaste according to claim 2, characterized in that the particle diameter of the silica colloid particles is 30-40 nm.
5. The submicron whitening toothpaste according to claim 1, wherein the whitening agent is selected from at least one of pearl powder, sodium phytate, tetrapotassium pyrophosphate, tetrasodium pyrophosphate.
6. The submicron whitening toothpaste according to claim 1, characterized in that the abrasive is hydrated silica; the foaming agent consists of sodium lauryl sulfate and sodium lauroyl sarcosinate.
7. The submicron whitening toothpaste according to claim 1, characterized in that the humectant is selected from at least one of sorbitol, glycerin, polydiethanol-8; the thickener consists of cellulose gum and xanthan gum; the sweetener is saccharin sodium.
8. The submicron whitening toothpaste according to claim 1, characterized by further comprising the following ingredients in weight percent: 0.1 to 0.3 percent of preservative and 0.1 to 0.5 percent of pigment.
9. A method of preparing a submicron whitening toothpaste according to any of claims 1 to 8, characterized in that a thickener is dispersed in a humectant to form a polyol phase; dissolving sweetener in water and humectant to form water phase; mixing the water phase and the polyol phase, and grinding and homogenizing for 10-15 minutes to obtain uniform glue; then adding a whitening agent, an abrasive, zinc citrate, sodium monofluorophosphate and PVM/MA, grinding and homogenizing for 20-25 minutes; and adding the foaming agent, stirring for 10-15 minutes in vacuum, adding the preservative, the submicron spheres, the essence and the pigment, stirring for 5-10 minutes in vacuum, closing stirring, and breaking vacuum to obtain the submicron whitening toothpaste.
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| CN103962074A (en) * | 2014-02-28 | 2014-08-06 | 中国科学院化学研究所 | Hollow sub-microsphere as well as preparation method and application thereof |
| CN104997662A (en) * | 2015-06-17 | 2015-10-28 | 烟台新时代健康产业日化有限公司 | Composition for inhibiting dental plaque and application thereof |
| CN106619187A (en) * | 2017-01-24 | 2017-05-10 | 广州薇美姿实业有限公司 | Composition for preventing dental calculus and application |
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