CN108542832A - A kind of antibacterial liquid tooth paste - Google Patents
A kind of antibacterial liquid tooth paste Download PDFInfo
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- CN108542832A CN108542832A CN201810755740.4A CN201810755740A CN108542832A CN 108542832 A CN108542832 A CN 108542832A CN 201810755740 A CN201810755740 A CN 201810755740A CN 108542832 A CN108542832 A CN 108542832A
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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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- 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
- A61K8/25—Silicon; 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
- A61K8/585—Organosilicon compounds
-
- 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
- A61K8/73—Polysaccharides
- A61K8/733—Alginic acid; Salts 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
-
- 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
Abstract
The present invention relates to a kind of antibacterial liquid tooth pastes, belong to field of oral care.The present invention is with sodium metasilicate, sulfuric acid is raw material, silica is made using the precipitation method, sodium chloride is as electrolyte, so that it is good with other constituent compatibilities in system, hydroxyapatite compounding is added and is used as rubbing agent, with mild dentifrice performance, with ethyl orthosilicate four water-calcium nitrate, dihydrogen phosphate is raw material, obtain bactericidal activity object, it contains sodium, calcium, phosphorus, silicon, dental hypersensitiveness and remineralization incipient dental caries can effectively be treated, with sodium alginate through cyanogen bromide-activated, chitosan mixing is added, it is modified through methoxy poly (ethylene glycol), obtain anti-protein adsorbent, protein is in negative electrical charge, hydroxyl repels each other in attachment proteins matter, make the protein of dental surface adsorb to reduce, improve size exclusion effect, improve cleaning of teeth degree, increase bacteria breed, tooth is formed and is protected.The present invention solves that current liquid viscosity is low, and active constituent is easy to run off, and the problem of fungistatic effect difference.
Description
Technical field
The present invention relates to field of oral care, and in particular to a kind of antibacterial liquid tooth paste.
Background technology
Traditional tooth paste product for brushing teeth and gargling is available commercially, and with a variety of different dosage form pins
It sells, such as：Ointment（paste）, powder, gel and viscous liquid, liquid etc., and have in processing and use various advantages and
It is insufficient.For example, due to including polishing ingredient in the composition, the easily damaged tooth of dentifrice composition of highly viscous ointment
The adamantine layer of tooth, and, it is difficult to the dentifrice composition is squeezed out by squeezing the container containing the composition, and in reality
The content being difficult in the fully utilize container, which results in wherein remain content to used as a result,
Container processing and subsequent environmental pollution.For powdered dentifrice composition, due to the particle point of toothpaste
Dissipate and splash and seem and be not convenient to use.For gel type dentifrice composition, it can be divided into containing polishing agent or not contain
The dentifrice composition of polishing agent, the viscosity height and bad dispersibility of gel type dentifrice composition, so as to cause the tooth of the composition
Bad dispersibility of the paste composition in the oral cavity of user, it is inconvenient to generate in use.Although in addition, the toothpaste of liquid form
Composition is currently widely used for flavorants of rinsing the mouth or be used as（breath freshener）, to inhibit to deform hammer
Bacterium（streptococcus mutans）With remove bad implication, but the deficiency of the dentifrice composition of liquid form is, by
It is low and easily flowing down in viscosity.Due to liquid composition shortage cleansing and also viscosity is low and easily flowing down
The problem of, therefore it can not show the toothbrushing effect for being enough to remove plaque or streptococcus mutans.
Invention content
The technical problems to be solved by the invention：Low for current liquid viscosity, active constituent is easy to run off, and fungistatic effect
The problem of difference, provides a kind of antibacterial liquid tooth paste.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of antibacterial liquid tooth paste, meter includes following component, 2 ~ 4 parts of foaming agents, 3 ~ 5 parts of moisturizer, 100 ~ 200 in parts by weight
Part water, 3 ~ 6 parts of Lotus Leafextracts, 3 ~ 6 parts of Honegsukle flower P.Es, which is characterized in that further include 5 ~ 10 parts of anti-protein adsorbents, 1 ~
3 parts of rubbing agents, 9 ~ 13 parts of bactericidal active agents；
The preparation method of the anti-protein adsorbent, includes the following steps：
（1）Take sodium alginate in mass ratio 1 ~ 3：50 ~ 90 are added ultra-pure water, and the bromination of sodium alginate quality 0.01 ~ 0.03% is added
Cyanogen is stirred 1 ~ 2h, adjusts pH to 10 ~ 11, and ultrafiltration takes ultrafiltrate in mass ratio 90 ~ 100：3 ~ 7 are added 3-（P- benzyl amino）-
1,2,4,5- tetrazine is stirred, and obtains stirring mixture；
（2）Take stirring mixture in mass ratio 1 ~ 3：90 ~ 100 are added ultra-pure water, and the matter for being stirred amount of substance 40 ~ 50% is added
The calcium chloride solution that amount score is 1.5% is stirred, and is added and is stirred the chitosan of amount of substance 40 ~ 50% and is stirred,
Mixture a must be stirred, stirring mixture a in mass ratio 1 ~ 3 is taken：8 ~ 12 are added the methoxy poly (ethylene glycol) that mass fraction is 0.5%
Solution is stirred to get anti-protein adsorbent.
The step（1）It is middle stirring mixture the condition that is stirred be：It is stirred 18 in 25 ~ 30 DEG C ~ for 24 hours.
The preparation method of the rubbing agent, includes the following steps：
Take sodium metasilicate in mass ratio 1 ~ 3：8 ~ 12 addition deionized waters are stirred, and the sodium chloride of sodium metasilicate quality 2 ~ 5% is added,
65 ~ 70 DEG C are warming up to, the sulfuric acid for adding sodium metasilicate quality 20 ~ 30% is stirred, and adds the carbonic acid of sulfuric acid quality 40 ~ 60%
Hydrogen sodium mixes, and obtains mixture, takes mixture in mass ratio 2 ~ 5：1 ~ 3 is added hydroxyapatite mixing to get rubbing agent.
The preparation method of the bactericidal active agent, includes the following steps：
Take ethyl orthosilicate in mass ratio 4 ~ 7：2 ~ 4 are added four water-calcium nitrate mixing, obtain mixture a, take mixture a in mass ratio
1~3：8 ~ 10 are added ethyl alcohol, adjust pH to 1 ~ 2, are stirred, obtain mixed liquor a, take dihydrogen phosphate in mass ratio 1 ~ 3：7~10
Deionized water is added, the polyethylene glycol-1000 0 for adding dihydrogen phosphate quality 10 ~ 20% is stirred 1 ~ 2h, obtains mixed liquor
B takes mixed liquor a in mass ratio 3 ~ 5：It is stirred in 1 ~ 4 addition mixed liquor b, obtains stirring mixture, pH to 10 is adjusted with ammonium hydroxide
~ 11,1 ~ 2h is stood, centrifugation takes pellet frozen drying to get bactericidal active agent.
It is described stirring mixture the condition that is stirred be：It is stirred 40 ~ 60min in 40 ~ 50 DEG C.
The foaming agent is：Take sodium N-lauroyl sarcosinate in mass ratio 3 ~ 5：1 ~ 3, which is added coconut oil propyl betaine, mixes
Close to get.
The moisturizer：Take sorbierite in mass ratio 2 ~ 5：1~3：2 ~ 5 are added xylitol, carboxymethyl cellulose mixing, i.e.,
.
Compared with other methods, advantageous effects are the present invention：
（1）Silica is made using sodium metasilicate, sulfuric acid as raw material, using the precipitation method in the present invention, introduces sodium chloride as electrolyte,
Enhance the transparency, the abrasive material of residuite is done in liquid tooth paste, it has chemical inertness, only absorbs minimal amount of liquid tooth paste
Function ingredients so that it is very good with other constituent compatibilities in toothpaste system, and hydroxyapatite compounding is added as friction
Agent has mild dentifrice performance, enamel can be protected not to be destroyed, and repairing dental enamel realizes remineralization of teeth；
（2）Ethyl orthosilicate four water-calcium nitrate of the present invention, dihydrogen phosphate are raw material, and bactericidal activity object is prepared, contains
Sodium, calcium, phosphorus, silicon composition, can effectively treat dental hypersensitiveness and remineralization incipient dental caries, bactericidal activity object meets water can be quick
Dissolving discharges silicon ion, forms gel layer in dental surface, subsequent calcium phosphorus precipitation wherein blocks dentinal tubule, and formation is coagulated
Glue-line has effectively lockked the active constituent in liquid tooth paste, and sodium that bactericidal activity object is released, calc-alkaline ion can be in winks
Between increase solution ph, increase osmotic pressure, change the ability that bacterium adjusts the outer water balance of intracellular, cause harmful bacteria in oral cavity de-
Water is dead, achievees the purpose that sterilization；
（3）The present invention, through cyanogen bromide-activated, can be grafted with sodium alginate in sodium alginate hydroxyl group sites, and it is poly- to add shell
Sugar mixing, modifies through methoxy poly (ethylene glycol), obtains anti-protein adsorbent, the residue adhered on tooth contains abundant albumen
Matter introduces methoxy poly (ethylene glycol), after brushing teeth, hydrophilic hydroxyl groups is rich in anti-protein adsorbent, can be formed a film in dental surface, and egg
White matter is when Fungicidal active substance increases the pH value of liquid tooth paste so that intraoral pH is more than the isoelectric point of protein so that
The protein of adherency is in negative electrical charge, and hydroxyl repels each other in attachment proteins matter, so that the protein absorption of dental surface is reduced, is carried
High size exclusion effect, improves the cleannes of tooth, plays anti-protein adsorption outstanding, and increase bacteria breed can
Can, tooth is formed and is protected.
Specific implementation mode
Rubbing agent：Take sodium metasilicate in mass ratio 1 ~ 3：8 ~ 12 are added deionized water, are stirred 20 ~ 30min, and silicic acid is added
The sodium chloride of sodium quality 2 ~ 5% is warming up to 65 ~ 70 DEG C, adds the sulfuric acid that the mass fraction of sodium metasilicate quality 20 ~ 30% is 80%,
It is stirred 30 ~ 40min, the sodium bicarbonate mixing for the sulfuric acid quality 40 ~ 60% that mass fraction is 80% is added, obtains mixture,
Take mixture in mass ratio 2 ~ 5：1 ~ 3 is added hydroxyapatite mixing to get rubbing agent.
Foaming agent：Take sodium N-lauroyl sarcosinate in mass ratio 3 ~ 5：1 ~ 3 is added the mixing of coconut oil propyl betaine, i.e.,
.
Moisturizer：Take sorbierite in mass ratio 2 ~ 5：1~3：2 ~ 5 be added xylitols, carboxymethyl cellulose mixing to get.
Bactericidal active agent：Take ethyl orthosilicate in mass ratio 4 ~ 7：2 ~ 4 are added four water-calcium nitrate mixing, obtain mixture a, take
Mixture a in mass ratio 1 ~ 3：8 ~ 10 are added the ethyl alcohol of mass fraction 80%, adjust pH to 1 ~ 2, are stirred 30 ~ 50min, obtain
Mixed liquor a takes dihydrogen phosphate in mass ratio 1 ~ 3：7 ~ 10 are added deionized water, add dihydrogen phosphate quality 10 ~ 20%
Polyethylene glycol-1000 0 is stirred 1 ~ 2h, obtains mixed liquor b, takes mixed liquor a in mass ratio 3 ~ 5：1 ~ 4 is added in mixed liquor b, in
40 ~ 50 DEG C are stirred 40 ~ 60min, obtain stirring mixture, and pH to 10 ~ 11 is adjusted with ammonium hydroxide, stand 1 ~ 2h, and centrifugation takes precipitation
Freeze-drying is to get bactericidal active agent.
Anti- protein adsorbent：（1）Take sodium alginate in mass ratio 1 ~ 3：50 ~ 90 are added ultra-pure water, and sodium alginate matter is added
The cyanogen bromide of amount 0.01 ~ 0.03% is stirred 1 ~ 2h, adjusts pH to 10 ~ 11, and ultrafiltration takes ultrafiltrate in mass ratio 90 ~ 100：3~
7 are added 3-（P- benzyl amino）- 1,2,4,5- tetrazines, it is stirred 18 in 25 ~ 30 DEG C ~ for 24 hours, obtain stirring mixture；
（2）Take stirring mixture in mass ratio 1 ~ 3：90 ~ 100 are added ultra-pure water, and the matter for being stirred amount of substance 40 ~ 50% is added
The calcium chloride solution that score is 1.5% is measured, 20 ~ 30min is stirred, adds the chitosan for being stirred amount of substance 40 ~ 50%,
It is stirred 1 ~ 2h, mixture a must be stirred, takes stirring mixture a in mass ratio 1 ~ 3：8 ~ 12 are added mass fraction as 0.5%
Methoxy poly (ethylene glycol) solution is stirred 1 ~ 3h to get anti-protein adsorbent.
A kind of antibacterial liquid tooth paste, according to the mass fraction, take 5 ~ 10 parts of anti-protein adsorbents, 1 ~ 3 part of rubbing agent, 2 ~ 4 parts
Foaming agent, 3 ~ 5 parts of moisturizer, 9 ~ 13 parts of bactericidal active agents, 100 ~ 200 parts of water, 3 ~ 6 parts of Lotus Leafextracts, 3 ~ 6 portions of honeysuckles carry
Object is taken, 30 ~ 60 DEG C is warming up to and is stirred 1 ~ 3h to get liquid tooth paste.
Embodiment 1
Rubbing agent：Take sodium metasilicate in mass ratio 1：8 are added deionized water, are stirred 20min, and the chlorine of sodium metasilicate quality 2% is added
Change sodium, be warming up to 65 DEG C, adds the sulfuric acid that the mass fraction of sodium metasilicate quality 20% is 80%, be stirred 30min, add
The sodium bicarbonate mixing for the sulfuric acid quality 40% that mass fraction is 80%, obtains mixture, takes mixture in mass ratio 2：1 is added hydroxyl
Apatites mixed is to get rubbing agent.
Foaming agent：Take sodium N-lauroyl sarcosinate in mass ratio 3：1 be added coconut oil propyl betaine mixing to get.
Moisturizer：Take sorbierite in mass ratio 2：1：2 be added xylitols, carboxymethyl cellulose mixing to get.
Bactericidal active agent：Take ethyl orthosilicate in mass ratio 4：2 are added four water-calcium nitrate mixing, obtain mixture a, take mixing
Object a in mass ratio 1：8 are added the ethyl alcohol of mass fraction 80%, adjust pH to 1, are stirred 30min, obtain mixed liquor a, take phosphoric acid
Hydrogen diamino in mass ratio 1：7 are added deionized water, and the polyethylene glycol-1000 0 for adding dihydrogen phosphate quality 10% is stirred
1h obtains mixed liquor b, takes mixed liquor a in mass ratio 3：1 is added in mixed liquor b, is stirred 40min in 40 DEG C, must be stirred
Object adjusts pH to 10 with ammonium hydroxide, stands 1h, and centrifugation takes pellet frozen drying to get bactericidal active agent.
Anti- protein adsorbent：（1）Take sodium alginate in mass ratio 1：50 are added ultra-pure water, and sodium alginate quality is added
0.01% cyanogen bromide is stirred 1h, adjusts pH to 10, and ultrafiltration takes ultrafiltrate in mass ratio 90：3 are added 3-（P- benzyl amino）-
1,2,4,5- tetrazine is stirred 18h in 25 DEG C, obtains stirring mixture；
（2）Take stirring mixture in mass ratio 1：90 are added ultra-pure water, and the mass fraction that addition is stirred amount of substance 40% is
1.5% calcium chloride solution, is stirred 20min, adds the chitosan for being stirred amount of substance 40%, is stirred 1h, obtains
Mixture a is stirred, stirring mixture a in mass ratio 1 is taken：8 are added the methoxy poly (ethylene glycol) solution that mass fraction is 0.5%, stir
Mixing 1h is mixed to get anti-protein adsorbent.
A kind of antibacterial liquid tooth paste takes 5 parts of anti-protein adsorbents, 1 part of rubbing agent, 2 parts of foaming agents, 3 according to the mass fraction
It is mixed to be warming up to 30 DEG C of stirrings for part moisturizer, 9 parts of bactericidal active agents, 100 parts of water, 3 parts of Lotus Leafextracts, 3 parts of Honegsukle flower P.Es
1h is closed to get liquid tooth paste.
Embodiment 2
Rubbing agent：Take sodium metasilicate in mass ratio 2：11 are added deionized water, are stirred 25min, and sodium metasilicate quality 3% is added
Sodium chloride is warming up to 67 DEG C, adds the sulfuric acid that the mass fraction of sodium metasilicate quality 25% is 80%, is stirred 35min, then add
The sodium bicarbonate mixing for entering the sulfuric acid quality 50% that mass fraction is 80%, obtains mixture, takes mixture in mass ratio 3：2 are added hydroxyl
Base apatites mixed is to get rubbing agent.
Foaming agent：Take sodium N-lauroyl sarcosinate in mass ratio 4：2 be added coconut oil propyl betaine mixing to get.
Moisturizer：Take sorbierite in mass ratio 3：2：3 be added xylitols, carboxymethyl cellulose mixing to get.
Bactericidal active agent：Take ethyl orthosilicate in mass ratio 5：3 are added four water-calcium nitrate mixing, obtain mixture a, take mixing
Object a in mass ratio 2：9 are added the ethyl alcohol of mass fraction 80%, adjust pH to 1.5, are stirred 40min, obtain mixed liquor a, take phosphorus
Sour hydrogen diamino in mass ratio 2：9 are added deionized water, and the stirring of polyethylene glycol-1000 0 for adding dihydrogen phosphate quality 15% is mixed
1.5h is closed, mixed liquor b is obtained, takes mixed liquor a in mass ratio 4：3 are added in mixed liquor b, are stirred 45min in 45 DEG C, must stir
Mixture adjusts pH to 10.5 with ammonium hydroxide, stands 1.5h, and centrifugation takes pellet frozen drying to get bactericidal active agent.
Anti- protein adsorbent：（1）Take sodium alginate in mass ratio 2：70 are added ultra-pure water, and sodium alginate quality is added
0.02% cyanogen bromide is stirred 1.5h, adjusts pH to 10.5, and ultrafiltration takes ultrafiltrate in mass ratio 95：4 are added 3-（P- benzyl ammonia
Base）- 1,2,4,5- tetrazines are stirred 20h in 27 DEG C, obtain stirring mixture；
（2）Take stirring mixture in mass ratio 2：95 are added ultra-pure water, and the mass fraction that addition is stirred amount of substance 45% is
1.5% calcium chloride solution, is stirred 25min, adds the chitosan for being stirred amount of substance 45%, is stirred 1.5h,
Mixture a must be stirred, stirring mixture a in mass ratio 2 is taken：The methoxy poly (ethylene glycol) that 10 addition mass fractions are 0.5% is molten
Liquid is stirred 2h to get anti-protein adsorbent.
A kind of antibacterial liquid tooth paste takes 7 parts of anti-protein adsorbents, 2 parts of rubbing agents, 3 parts of foaming agents, 4 according to the mass fraction
Part moisturizer, 11 parts of bactericidal active agents, 150 parts of water, 5 parts of Lotus Leafextracts, 5 parts of Honegsukle flower P.Es, are warming up to 50 DEG C of stirrings
2h is mixed to get liquid tooth paste.
Embodiment 3
Rubbing agent：Take sodium metasilicate in mass ratio 3：12 are added deionized water, are stirred 30min, and sodium metasilicate quality 5% is added
Sodium chloride is warming up to 70 DEG C, adds the sulfuric acid that the mass fraction of sodium metasilicate quality 30% is 80%, is stirred 40min, then add
The sodium bicarbonate mixing for entering the sulfuric acid quality 60% that mass fraction is 80%, obtains mixture, takes mixture in mass ratio 5：3 are added hydroxyl
Base apatites mixed is to get rubbing agent.
Foaming agent：Take sodium N-lauroyl sarcosinate in mass ratio 5：3 be added coconut oil propyl betaine mixing to get.
Moisturizer：Take sorbierite in mass ratio 5：3：5 be added xylitols, carboxymethyl cellulose mixing to get.
Bactericidal active agent：Take ethyl orthosilicate in mass ratio 7：4 are added four water-calcium nitrate mixing, obtain mixture a, take mixing
Object a in mass ratio 3：10 are added the ethyl alcohol of mass fraction 80%, adjust pH to 2, are stirred 50min, obtain mixed liquor a, take phosphoric acid
Hydrogen diamino in mass ratio 3：10 are added deionized water, and the stirring of polyethylene glycol-1000 0 for adding dihydrogen phosphate quality 20% is mixed
2h is closed, mixed liquor b is obtained, takes mixed liquor a in mass ratio 5：4 are added in mixed liquor b, and 60min is stirred in 50 DEG C, must stir mixed
Object is closed, pH to 11 is adjusted with ammonium hydroxide, stands 2h, centrifugation takes pellet frozen drying to get bactericidal active agent.
Anti- protein adsorbent：（1）Take sodium alginate in mass ratio 3：90 are added ultra-pure water, and sodium alginate quality is added
0.03% cyanogen bromide is stirred 2h, adjusts pH to 11, and ultrafiltration takes ultrafiltrate in mass ratio 100：7 are added 3-（P- benzyl ammonia
Base）- 1,2,4,5- tetrazines, are stirred for 24 hours in 30 DEG C, obtain stirring mixture；
（2）Take stirring mixture in mass ratio 3：100 are added ultra-pure water, and the mass fraction that addition is stirred amount of substance 50% is
1.5% calcium chloride solution, is stirred 30min, adds the chitosan for being stirred amount of substance 50%, is stirred 2h, obtains
Mixture a is stirred, stirring mixture a in mass ratio 3 is taken：12 are added the methoxy poly (ethylene glycol) solution that mass fraction is 0.5%,
3h is stirred to get anti-protein adsorbent.
A kind of antibacterial liquid tooth paste, according to the mass fraction, take 10 parts of anti-protein adsorbents, 3 parts of rubbing agents, 4 parts of foaming agents,
5 parts of moisturizer, 13 parts of bactericidal active agents, 200 parts of water, 6 parts of Lotus Leafextracts, 6 parts of Honegsukle flower P.Es are warming up to 60 DEG C of stirrings
3h is mixed to get liquid tooth paste.
Comparative example 1：It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking anti-protein adsorbent.
Comparative example 2：It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking rubbing agent.
Comparative example 3：It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking bactericidal active agent.
Comparative example 4：The liquid tooth paste of Guangzhou company production.
The liquid tooth paste of above-described embodiment 1-3 and comparative example 1-4 is detected respectively, case and method choice
1）Selecting object
1. age 18-65 Sui, remaining tooth >=16 tooth in mouth, no systemic disease, blood routine, blood platelet, clotting time and bleeding time are normal
Simple gingivitis；2. mouth cavity medicine or gargle were not used in 1 month, do not received dental care in 3 months；3. excluding
There are allergies and pregnant woman and nursing period personnel to each component in this product, chooses number 90.
2）90 experimenters are divided into three groups by grouping using the random packet mode of multicenter（Every group 30）.
3）Liquid tooth paste made from test specimen source 1-3 of the embodiment of the present invention and comparative example 1-4.
4）Test method 7 days is a cycle, totally 28 days, i.e. four periods；The daily gargle body toothpaste of subject 2 times,
Each 1ml；.
5）Observation index
5.1）Subjective symptoms
Show as gum redness, bleeding, pain, halitosis, occlusion discomfort etc.；Halitosis be divided into without, it is light, in, again；Slight halitosis：
Feel halitosis, other people can't smell；Moderate halitosis：Other people can smell halitosis when speaking；Severe halitosis：Other people can hear when silent
To halitosis；Gum pain is divided into nothing, light, neutralization weight.
5.2）Clinical indexes
To the areas subject oral cavity Fen Liuge, free 6 tooth positions record each tooth with 11,16,26,31,36,46 for index tooth respectively
Various bacteriums.
5.3）Observing time
Using being both needed to do blood routine, blood platelet, clotting time and bleeding time inspection before sample, all observation items are both needed to using subject
Before sample, using 7 days after sample, be examined in, and recorded by same doctor within 14 days, 21 days, 28 days.
6）Laboratory observation index
6.1）Sampling method
It samples before using sample and using 4 weeks after sample, by facing every wet, normal saline flushing, drying, is put with sterile key
Enter gingival pocket or oral pocket bottom, gently scrape facing, scrape a little bacterial plaque, is placed in the test tube for containing dilution.By above-mentioned bacterium solution point
Rear smear is not broken up, standby inspection.
6.2）Dark-field microscope is observed
By Mous classification, subgingival microbe is divided into following 4 class；Coccus（C）, active bacterium（M）, conveyor screw（S）With other bacterium
（O）；Amplify 1000 times under dark-field microscope, randomly choose 3 visuals field, by being added after above-mentioned 4 class differential counting bacterium, unites
Count antibacterial percentage；The above job requirement is completed after making a collection of specimens in 1h.
Testing result such as the following table 1.
Table 1：
In summary, antibacterial liquid dentifrice liquid viscosity of the invention is high, and active constituent not easily runs off, and good antimicrobial effect, value
It must promote the use of.
Claims (7)
1. a kind of antibacterial liquid tooth paste, meter in parts by weight includes following component, 2 ~ 4 parts of foaming agents, 3 ~ 5 parts of moisturizer, 100 ~
200 parts of water, 3 ~ 6 parts of Lotus Leafextracts, 3 ~ 6 parts of Honegsukle flower P.Es, which is characterized in that further include 5 ~ 10 parts of anti-protein adsorptions
Agent, 1 ~ 3 part of rubbing agent, 9 ~ 13 parts of bactericidal active agents；
The preparation method of the anti-protein adsorbent, includes the following steps：
（1）Take sodium alginate in mass ratio 1 ~ 3：50 ~ 90 are added ultra-pure water, and the bromination of sodium alginate quality 0.01 ~ 0.03% is added
Cyanogen is stirred 1 ~ 2h, adjusts pH to 10 ~ 11, and ultrafiltration takes ultrafiltrate in mass ratio 90 ~ 100：3 ~ 7 are added 3-（P- benzyl amino）-
1,2,4,5- tetrazine is stirred, and obtains stirring mixture；
（2）Take stirring mixture in mass ratio 1 ~ 3：90 ~ 100 are added ultra-pure water, and the matter for being stirred amount of substance 40 ~ 50% is added
The calcium chloride solution that amount score is 1.5% is stirred, and is added and is stirred the chitosan of amount of substance 40 ~ 50% and is stirred,
Mixture a must be stirred, stirring mixture a in mass ratio 1 ~ 3 is taken：8 ~ 12 are added the methoxy poly (ethylene glycol) that mass fraction is 0.5%
Solution is stirred to get anti-protein adsorbent.
2. antibacterial liquid tooth paste according to claim 1, which is characterized in that the step（1）Middle stirring mixture stirs
Mixing mixing condition is：It is stirred 18 in 25 ~ 30 DEG C ~ for 24 hours.
3. antibacterial liquid tooth paste according to claim 1, which is characterized in that the preparation method of the rubbing agent, including such as
Lower step：
Take sodium metasilicate in mass ratio 1 ~ 3：8 ~ 12 addition deionized waters are stirred, and the sodium chloride of sodium metasilicate quality 2 ~ 5% is added,
65 ~ 70 DEG C are warming up to, the sulfuric acid for adding sodium metasilicate quality 20 ~ 30% is stirred, and adds the carbonic acid of sulfuric acid quality 40 ~ 60%
Hydrogen sodium mixes, and obtains mixture, takes mixture in mass ratio 2 ~ 5：1 ~ 3 is added hydroxyapatite mixing to get rubbing agent.
4. antibacterial liquid tooth paste according to claim 1, which is characterized in that the preparation method of the bactericidal active agent, packet
Include following steps：
Take ethyl orthosilicate in mass ratio 4 ~ 7：2 ~ 4 are added four water-calcium nitrate mixing, obtain mixture a, take mixture a in mass ratio
1~3：8 ~ 10 are added ethyl alcohol, adjust pH to 1 ~ 2, are stirred, obtain mixed liquor a, take dihydrogen phosphate in mass ratio 1 ~ 3：7~10
Deionized water is added, the polyethylene glycol-1000 0 for adding dihydrogen phosphate quality 10 ~ 20% is stirred 1 ~ 2h, obtains mixed liquor
B takes mixed liquor a in mass ratio 3 ~ 5：It is stirred in 1 ~ 4 addition mixed liquor b, obtains stirring mixture, pH to 10 is adjusted with ammonium hydroxide
~ 11,1 ~ 2h is stood, centrifugation takes pellet frozen drying to get bactericidal active agent.
5. antibacterial liquid tooth paste according to claim 1, which is characterized in that the stirring mixture is stirred condition
For：It is stirred 40 ~ 60min in 40 ~ 50 DEG C.
6. antibacterial liquid tooth paste according to claim 1, which is characterized in that the foaming agent is：Take lauroyl flesh ammonia
Sour sodium in mass ratio 3 ~ 5：1 ~ 3 be added coconut oil propyl betaine mixing to get.
7. antibacterial liquid tooth paste according to claim 1, which is characterized in that the moisturizer：Take sorbierite in mass ratio 2
~5：1~3：2 ~ 5 be added xylitols, carboxymethyl cellulose mixing to get.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112999104A (en) * | 2021-03-04 | 2021-06-22 | 福建英嘉医疗科技有限公司 | Antibacterial ion active agent for protecting teeth and preparation method thereof |
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Application publication date: 20180918 |