CN102335111B - Powder toothpaste combination comprising Ag particles and manufacturing method thereof - Google Patents
Powder toothpaste combination comprising Ag particles and manufacturing method thereof Download PDFInfo
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- CN102335111B CN102335111B CN2011101930131A CN201110193013A CN102335111B CN 102335111 B CN102335111 B CN 102335111B CN 2011101930131 A CN2011101930131 A CN 2011101930131A CN 201110193013 A CN201110193013 A CN 201110193013A CN 102335111 B CN102335111 B CN 102335111B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- 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
Abstract
The invention relates to a powder toothpaste combination comprising Ag particles and a manufacturing method thereof, and in more detail, provides a powder toothpaste combination comprising Ag particles and a manufacturing method thereof advantaged by taking effect of sterilization via use of inherent property of a Ag ingredient having no side effect in the oral cavity, and taking effect of sterilization in short time, thereby taking effect of substantial sterilization as powder toothpaste for use, preventing decayed teeth and gum disease, and improving effect of eliminating bad breath. The powder toothpaste combination comprising Ag particles is formed via the following method: ingredients of Ag particles, a tooth plaque removing agent, a sterilization capability enhancing auxiliary agent, a sweet taste agent, a form-giving agent, a flavouring agent, a brightening agent, and a coloring agent are thrown into a mixer to form a powder mixture, the powder mixture is stirred and mixed while a Au particle colloidal solution is uniformly injected so as to perform coating and drying, and the powder toothpaste combination is formed.
Description
Technical field
The present invention relates to contain powder dentifrice composition and the manufacture method thereof of silver particles, relate in more detail utilize silver (Ag) thus the intrinsic character of composition plays bactericidal action with being free from side effects, and can play at short notice bactericidal action and be suitable for the powder dentifrice composition and the manufacture method thereof that contain silver particles that also can play substantial bactericidal action, caries prevention and gingival disease and can improve removing halitosis effect as powder toothpaste in the oral cavity.
Background technology
Generally, for the cleaning of oral cavity and tooth and the toothpaste that uses is widely used paste toothpaste, but use for a long time or the lid of opening pipe through certain hour, then the fore-end of pipe solidify and be not easy to extrude or out of use situation more.In addition, in use, the inner residual toothpaste of pipe can not be finished fully, inject the pipe of toothpaste as disposable pipe, can only throw away at every turn, so waste is serious, have the problem of environmental pollution.
In order to solve such problem, can use more meticulously toothpaste, and propose to reuse the liquid toothpaste of container.But such liquid toothpaste is when it uses, and has the problem that the liquid toothpaste compositions flows out easily and use is very inconvenient, waste is serious, so do not use in reality.
On the other hand, the scheme as for the problem that solves above-mentioned paste toothpaste and liquid toothpaste has proposed powder toothpaste recently.As such powder toothpaste, shown in " dentifrice composition that contains the germanium oxide powder " of Korean granted patent communique patent No. 10-0614685 number, propose to contain purity and be the germanium oxide powder more than 99%, thereby can improve the dentifrice composition of the descale effect of the dental calculus that utilizes the distinctive porous space of germanium oxide to remove dental surface.
And, shown in " the powder Chinese prescription toothpaste " of Korea S's publication communique publication number 10-2006-0102681 number, propose powder salt, bamboo salt, Pulvis Talci, Maifanitum, Chinese drugs powder brought into play the effect of removing dental plaque or protection oral cavity, and can protect adamantine powder toothpaste; " containing the powder toothpaste as the Maifanitum in far infrared irradiation source " that Korea S's publication communique publication number is 10-2006-0008509 number proposed to have brought into play from the powder toothpaste of effective effect of the far infrared of Maifanitum radiation.
In addition, shown in " manufacture method of the powder toothpaste of prevention and treatment periodontitis, dental caries, apicitis etc. " of special 1997-0069019 number of Korea S publication communique publication number, propose the salt-mixture powder, fried Semen Gleditsiae powder, Colophonium powder etc., the powder toothpaste of prevention and treatment tooth or gum disease, particularly periodontitis, dental caries, apicitis etc.
Yet, although removing the aspects such as effect and gum disease at descale effect, dental plaque, above-mentioned powder toothpaste in the past can bring into play separately certain effect, but because a little less than the sterilizing ability, can not expect sufficient effect so remove the removing of dental plaque in oral cavity and oral cavity bacterium.
For this reason, need to drop into the chemical additive that plays bactericidal action, therefore occured to cause stimulating the skin in responsive oral cavity or bringing dysgenic problem.For example, in toothpaste for bactericidal action widely used fluoride preparation, although can effectively play the dental caries of prophylaxis of teeth or the function of anti-bacteria, but relatively can not bring into play good bactericidal effect for the gingiva of supports tooth or the skin of inside, oral cavity, and existence brings unhappy problem owing to making tooth generation speckle or medicine taste to consumer.
In order to address the above problem, the applicant has proposed 2007-0048134 number disclosed powder dentifrice composition that contains silver particles of korean patent application.
The powder dentifrice composition that contains silver particles that korean patent application proposes for 2007-0048134 number contains silver particles 0.0005～1 % by weight, hexadecylpyridinium chloride
Powder 0.1～5 % by weight, ubidecarenone (coenzyme Q10) powder 0.0001～2 % by weight, propolis extract powder 0.1～5 % by weight, hydroxyapatite powder 0.5～2 % by weight, sorbitol powder 2.0～30 % by weight and as excipient, be selected from silicon dioxide, moisture silicic acid, lactose, the titanium oxide more than one excipient powders 10～80 % by weight and consist of.
The powder dentifrice composition that contains silver particles like this utilizes the intrinsic bactericidal action of silver-colored composition and strengthens at intraoral sterilizing ability, thereby has played the effect of caries prevention and gum disease.And, be dissolved in sterile purified water with identical amount above-mentioned powder dentifrice composition after, pour in the test strain, after 1 minute time, measure remaining bacterium number, the result is determined as has excellent sterilizing ability and antibacterial ability.
But, above-mentioned sterilization and antibacterial ability test are the sterilizing abilities of in advance the powder dentifrice composition being measured after the long time is dissolved in solvent (sterile purified water), therefore as can be known owing to there not be consideration to contain characteristic in the use of powder dentifrice composition of silver particles, so compare the difference with suitable sterilizing ability when in fact using as the purposes of toothpaste.Namely, the powder dentifrice composition that will contain silver particles be not dissolved in advance solvent state under, carry out bactericidal assay according to identical method, as a result sterilization is compared remarkable reduction with antibacterial ability with the situation of having carried out in advance dissolving, therefore can not expect sufficient bactericidal effect when gargling.
Studied its reason, the powder dentifrice composition that the result contains particle is the toothpaste of powder morphology, so different from paste toothpaste or liquid toothpaste when gargling, the time that the material of needs performance sterilizing ability dissolves, but gargle owing to probably in 3 minutes, finishing, so can not bring into play sufficient sterilizing ability.The silver particles that particularly contains as the main component of bringing into play sterilizing ability is owing to be the natural materials of being free from side effects, have the skin that does not stimulate responsive oral cavity or bring harmful effect, to have got rid of the chemical substance of adding in addition in order sterilizing and not produce the advantage of medicine taste, but be not allow diffluent solid granulates, have certain limit in bactericidal action, therefore need to replenish it.
Summary of the invention
The present invention is conceived to solve above-mentioned problem in the past, purpose is to provide utilizes the intrinsic character of silver (Ag) composition to play bactericidal action with being free from side effects in the oral cavity, and can play bactericidal action at short notice, thereby even be suitable for the powder dentifrice composition that contains silver particles that also can play substantial bactericidal action, caries prevention and gingival disease and can improve removing halitosis effect as powder toothpaste.
Be characterised in that for the powder dentifrice composition that contains silver particles that reaches aforesaid purpose of the present invention, form by the following method the powder dentifrice composition that contains silver particles: will be by silver particles, scavenger for dental scar, sterilizing ability strengthens adjuvant, sweeting agent, excipient, fumet, above-mentioned each composition that brightening agent and coloring agent form is put into mixer and is formed mixture of powders, stir on one side, mix above-mentioned mixture of powders on one side equably the concentration of ejected silver (Ag) particle be that silver (Ag) the particle,colloid solution of 30～60ppm is coated with, and carry out drying and form; With respect to the weight of above-mentioned mixture of powders, above-mentioned silver (Ag) particle,colloid solution is 3～10 % by weight; Silver particles is as the antibacterial of anti-bacteria in the oral cavity, and its particle diameter is 10～200 mu m ranges, and contains with 0.0005～1.0 % by weight scope; Scavenger for dental scar contains and is selected from hexadecylpyridinium chloride
0.1 in～0.5 % by weight, sodium fluoride 0.01～0.05 % by weight, sodium monofluorophosphate 0.1～0.7 % by weight a kind or 2 kinds; Sterilizing ability strengthen adjuvant contain be selected from trichlorophenol 0.01～0.5 % by weight, Olibanum oil 0.01～0.5 % by weight, propolis extract powder 0.1～5 % by weight more than a kind; Sweeting agent contain be selected from xylitol powder 1.0～10 % by weight, saccharin sodium 0.01～1.0 % by weight, sorbitol powder 2.0～30 % by weight more than a kind; Excipient contain be selected from lactose 50.0～86.0 % by weight, silica 1 9.0～75.0 % by weight more than a kind; The surplus % by weight of stating each composition more than fumet, brightening agent, coloring agent form contains.
And, above-mentioned fumet contain be selected from minty note powder 1.0～5 % by weight, Herba Menthae Rotundifoliae powder 1.0～5.0 % by weight more than a kind, above-mentioned brightening agent contains the hydroxyapatite of 0.5～2 % by weight scope, and above-mentioned coloring agent contains the spirulina blue color of 0.001～1.0 % by weight scope.
On the other hand, above-mentioned silver (Ag) particle,colloid solution is characterised in that the process by 99.9% silver medal of electrolysis in distilled water (Ag) rod, carry out ionizing (Ag+), thus in distilled water, contain 0.001～0.015 micron about (μ m) silver (Ag) fundamental particle and form.
And, be coated with above-mentioned silver (Ag) particle,colloid solution and drying after, can also contain the angelica powder, with respect to the total weight of above-mentioned mixture of powders, above-mentioned angelica powder is 1～10 % by weight scope.
Manufacture method for the powder dentifrice composition that contains silver particles that reaches aforesaid purpose of the present invention, possess: powder composition preparation process, namely, prepare respectively as the antibacterial that suppresses oral cavity bacterium, particle diameter is 10～200 mu m ranges and the silver particles that contains with 0.0005～1.0 % by weight scope, contain to be selected from hexadecylpyridinium chloride
0.1～0.5 % by weight, sodium fluoride 0.01～0.05 % by weight, 1 kind or 2 kinds scavenger for dental scar in sodium monofluorophosphate 0.1～0.7 % by weight, contain and be selected from trichlorophenol 0.01～0.5 % by weight, Olibanum oil 0.01～0.5 % by weight, the sterilizing ability more than a kind in propolis extract powder 0.1～5 % by weight strengthens adjuvant, contain and be selected from xylitol powder 1.0～10 % by weight, saccharin sodium 0.01～1.0 % by weight, the sweeting agent more than a kind in sorbitol powder 2.0～30 % by weight, contain and be selected from lactose 50.0～86.0 % by weight, the excipient more than a kind in silica 1 9.0～75.0 % by weight, and the fumet that contains with the surplus % by weight of above-mentioned each composition, brightening agent, coloring agent.
And, the manufacture method that contains the powder dentifrice composition of silver particles also comprises: the solution preparation process, in electrolysis bath, inject sterile purified water, purity is set is 99.9% silver (Ag) rod, the concentration of preparing silver (Ag) particle by electrolytic process is silver (Ag) the particle,colloid solution of 30～60ppm; Mixture forms step, forms mixture of powders on one side make above-mentioned each powder composition of preparing in the above-mentioned powder preparation process drop into mixer by 20～30 purpose sieves on one side; Application step, spray above-mentioned silver (Ag) particle,colloid solution while stirring, mix described mixture of powders, so that with respect to the weight of above-mentioned mixture of powders, above-mentioned silver (Ag) particle,colloid solution is 3～10 % by weight scopes, thereby is coated with on the surface of above-mentioned each powder composition; And drying steps, the mixture of powders that has been coated with above-mentioned silver (Ag) particle,colloid solution in the above-mentioned application step is carried out drying.
And, implement above-mentioned drying steps after, also comprise the angelica powders mixing, described angelica powders mixing comprises: drop into the angelica powder, so that with respect to all weight of above-mentioned mixture of powders, above-mentioned angelica powder is 1～10 % by weight scope, and evenly mix.
Utilization is strengthened intraoral sterilizing ability according to the above-mentioned powder dentifrice composition that contains silver particles of the present invention by the intrinsic bactericidal action of silver-colored composition, can improve the preventive effect of dental caries and gum disease, and owing to has added hexadecylpyridinium chloride
, so sterilizing ability and removing halitosis effect further improve.
Particularly, the powder dentifrice composition of silver particles that contains according to the present invention is with the bactericidal action excellence, after the mode that the preventive effect of dental caries and gum disease improves makes up mixture of powders, be scope about 30～60ppm with the concentration of silver (Ag) particle, the size of particle is that 0.001～0.015 micron silver (Ag) particle,colloid solution coat about (μ m) is in each powder composition and carry out drying, so that can carry out bactericidal action at short notice, thereby be suitable for the effect that also can play substantial bactericidal action even have as powder toothpaste.
The specific embodiment
Below, utilize the manufacturing technology of powder toothpaste to describe in detail according to the powder dentifrice composition that contains silver particles of the present invention, utilize for those skilled in the art structure that prior art in the past learns easily and the detailed description of effect and effect thereof to carry out simple declaration or omission, will describe centered by the part related to the present invention.
The powder dentifrice composition that contains silver particles according to the present invention is will strengthen all the components that adjuvant, sweeting agent, excipient, fumet, brightening agent and coloring agent consist of by the silver particles that contain as the antibacterial that suppresses oral cavity bacterium, scavenger for dental scar, sterilizing ability to drop in the mixer and form mixture of powders, while stir, mix this mixture of powders equably the concentration of ejected silver (Ag) particle be that silver (Ag) the particle,colloid solution of 30～60ppm is coated with, and carry out drying and form; With respect to the weight of mixture of powders, above-mentioned silver (Ag) particle,colloid solution is 3～10 % by weight.
Below, each composition that forms mixture of powders is specifically studied.
The character that above-mentioned silver particles becomes branch to have owing to silver (Ag) makes at intraoral sterilizing ability and strengthens, anti-bacteria propagation, play the effect of removing dental plaque and prevention disease in mouth, the bactericidal action of such silver particles is the metabolism such as the breathing that acts on antibacterial of silver ion (Ag+) that argent discharges, digestion and play bactericidal action.
And silver (Ag) uses as the interpolation material of the traditional Chinese medical science or therapeutic appliance etc. since ancient times, and in the modern times, is carrying out effort and research that this silver is more diversely utilized.In addition, silver (Ag) plays the function of the natural bactericidal agent of being free from side effects, in addition, activation skin physiology function and cell regeneration function, play recovery and the Detoxication of the gingival cell of damage, out cation makes the secretion of hormone smooth and easy from silver, plays the effect of keeping intraoral skin health.
Preferably, silver particles is that adding purity is the native silver that 99.9% argent (Ag) forms particle diameter 10～200 μ m.
In addition, the content of silver particles is 0.0005～1 % by weight with respect to the total weight of above-mentioned mixture of powders preferably, this reason can be learnt by experiment: if be that then sterilizing ability significantly weakens below 0.0005 % by weight, thereby can not bring into play the preventive effect of removing dental plaque and disease in mouth; If when its weight surpassed 1 % by weight, even appended its content, bactericidal effect can further not increase yet.
Scavenger for dental scar can be suitable for hexadecylpyridinium chloride
(CPC), the inhibition oral cavity bacterium of sodium fluoride, sodium monofluorophosphate and so on and remove dental plaque, and performance disease in mouth prevention and remove the composition of the effect of halitosis.Its content preferably contains hexadecylpyridinium chloride with respect to the total weight of above-mentioned mixture of powders
(CPC) one kind or two or more in 0.1～0.5 % by weight, sodium fluoride 0.01～0.05 % by weight, sodium monofluorophosphate 0.1～0.7 % by weight.
Sterilizing ability strengthens the natural antibiotics that adjuvant can be suitable for trichlorophenol, Olibanum oil, propolis extract and so on.At this moment, preferred mixed phase is for the overall weight of above-mentioned mixture of powders, in trichlorophenol 0.01～0.5 % by weight, Olibanum oil 0.01～0.5 % by weight, propolis extract powder 0.1～5 % by weight more than a kind.
Sweeting agent is to select from can xylitol, saccharin sodium and the sorbitol powder of caries prevention and contain, preferably contain in xylitol powder 1.0～10 % by weight, saccharin sodium 0.01～1.0 % by weight, sorbitol powder 2.0～30 % by weight more than a kind.
Excipient is the material that adds in order to form powder toothpaste with certain form, preferably contain in lactose 50.0～86.0 % by weight, silica 1 9.0～75.0 % by weight more than a kind.
Fumet is to select a kind and contain from minty note powder 1.0～5 % by weight, Herba Menthae Rotundifoliae powder 1.0～5.0 % by weight.
The applicable hydroxyapatite (Hydroxyapatite) that consists of the main constituent of human skeleton and tooth enamel of brightening agent, play the fine damaged part of filling tooth, so that the smooth and glossiness effect of tooth, the scope of its content is 0.5～2 % by weight scope.
The extraction that coloring agent contains 0.001～1.0 % by weight scope is from the spirulina blue color of spirulina (spirulina) and consist of.Spirulina is dark green blue algae, the a kind of of cyanobacteria, it is the spiral type prokaryotic micro-organisms that does not have the spring-like of cell wall, contain a large amount of vitamin, so sulfonation is excellent, improve the resistance that oral cavity bacterium is infected, thereby raising immunity, prevent intraoral gum disease, have powerful bactericidal action as chlorophyllous CHLOROPHYLLINE, so be the material that suppresses oral cavity bacterium propagation.
Above-mentioned silver (Ag) particle,colloid solution is to form by the following method, namely, in distilled water, by electrolytic process ionizing (Ag+), make distilled water contain 0.001～0.015 micron silver (Ag) fundamental particle about (μ m) 99.9% silver medal (Ag) rod.
On the other hand, the powder dentifrice composition that contains silver particles according to the present invention can also contain the angelica powder.With regard to the angelica powder, when containing less than 1 % by weight, limited in the utilization of effective ingredient; Be 10 % by weight when above, impair as the frankness sense of toothpaste or use sense that therefore with respect to the total weight of mixture of powders, the angelica powder is 1～10 % by weight scope.
Angelica the sea water in the seashore of Korea S or area, island in one's power seashore or mud bank, salt pan around in flakes growth, owing to be the grass that plump and every joint is all given prominence to, so be also referred to as " fat joint ", 1 year this plant of SHENGCAO that belongs to Chenopodiaceae (chenopodiaceae) at botany classification, as land plant, contain abundant, be dissolved in the various mineral such as the calcium take salt as representative in the sea water, enzyme, potassium, ferrum, phosphorus, thereby to tooth or effectively effect of gingiva performance.
And, the angelica powder can utilize the heating extraction mode extract and powdered after drop into, but in the present embodiment, in order not destroy the effective crude drug composition that contains in the angelica, the angelica of collecting is cleaned, carry out lyophilization, fragmentation drops into the angelica of powdered.
Particularly in order not destroy the effective crude drug composition that contains in the angelica, importantly as described below, behind drying steps, drop in addition, it is not exposed in the steam.
And each the powder composition that forms mixture of powders preferably can pass through the granularity of the degree of 20～50 purpose sieves (drainage screen).
Below, the manufacture method according to the powder dentifrice composition that contains silver particles of preferred implementation of the present invention is described.
The manufacture method that contains the powder dentifrice composition of silver particles according to the present invention is carried out following steps successively: prepare silver particles, scavenger for dental scar, sterilizing ability strengthens adjuvant, sweeting agent, excipient and the fumet that contains with the surplus % by weight of above-mentioned each powder composition, brightening agent, the powder composition preparation process of coloring agent, prepare the solution preparation process of silver (Ag) particle,colloid solution, the mixture that forms mixture of powders forms step, at the application step of the surface coated of powder composition silver (Ag) particle,colloid solution, the drying steps of dry powder mixture.
At first, in powder composition preparation process, prepare respectively as mentioned above: as the antibacterial that suppresses oral cavity bacterium, with the silver particles that 0.0005～1.0 % by weight scope contains, contain and be selected from hexadecylpyridinium chloride
0.1～0.5 % by weight, sodium fluoride 0.01～0.05 % by weight, 1 kind or 2 kinds scavenger for dental scar in sodium monofluorophosphate 0.1～0.7 % by weight, contain and be selected from trichlorophenol 0.01～0.5 % by weight, Olibanum oil 0.01～0.5 % by weight, the sterilizing ability more than a kind in propolis extract powder 0.1～5 % by weight strengthens adjuvant, contain and be selected from xylitol powder 1.0～10 % by weight, saccharin sodium 0.01～1.0 % by weight, the sweeting agent more than a kind in sorbitol powder 2.0～30 % by weight, contain and be selected from lactose 50.0～86.0 % by weight, the excipient more than a kind in silica 1 9.0～75.0 % by weight, and the fumet that contains with the surplus % by weight of described each composition, brightening agent, coloring agent.
The solution preparation process is to inject sterile purified water in electrolysis bath, purity be set be 99.9% silver (Ag) rod, the concentration of preparing silver (Ag) particle by electrolytic process is the step of silver (Ag) the particle,colloid solution of 30～60ppm, be that 99.9% silver (Ag) rod is arranged on electrolysis bath and implements electrolysis as can be known with purity, after the silver-colored composition ionizing of silver (Ag) rod, when its concentration reaches roughly the 30ppm left and right sides, particlized and being present in the distilled water then, begin to form colloid solution, when surpassing 60ppm, then not only silver particles precipitates, and particle mutually combines its size increase.
And, in the present embodiment, if electrolysis is scope about 30～60ppm to the concentration of silver (Ag) particle, the size of the silver particles that then contains in the sterile purified water is about 0.001～0.015 micron (μ m), by using the little fundamental particle of such particle diameter, when gargling, can more promptly play bactericidal action.
It is to make each powder composition of preparing in the above-mentioned powder composition preparation process put into the step that forms mixture of powders in the mixer on one side by sieve on one side that mixture forms step, at first, with scavenger for dental scar, sterilizing ability strengthen adjuvant, sweeting agent and excipient about with 30 orders the drainage screen filtration and drop into, mix, for the second time a kind in minty note powder, the Herba Menthae Rotundifoliae powder and spirulina blue color are filtered with 30 mesh sieves and behind the input mixer, mixed 90～120 minutes with 15～25rpm, then each composition evenly distributes gradually.
Application step is silver (Ag) the particle,colloid solution of preparing in the above-mentioned mixture of powders sprayed solution preparation process while stirring, mixing, so that with respect to the weight of mixture of powders, above-mentioned silver (Ag) particle,colloid solution 3～10 % by weight scopes, thereby the step that is coated with on the surface of each powder composition is carried out to the mode of jet surface silver (Ag) particle,colloid solution of the mixture of powders that stirs, mixes with the automatic sprayer that utilizes the ormal weight of can spraying.
And, the reasons that the input weight of silver (Ag) particle,colloid solution is decided to be 3～10 amount % scopes are: if its weight surpasses 10 % by weight with respect to the weight of mixture of powders, each the powder composition that then causes forming mixture of powders condenses into mutually bulk, so not only need through once other broken step, and dry too much time, the problems such as each powder composition interreaction of needing.And the input weight of silver (Ag) particle,colloid solution is during less than 3 % by weight, because its amount is too small and can not mixture of powders all be sprayed evenly distributedly, so can not expect effective effect.
Drying steps be will be coated with in the application step step of mixture of powders drying of silver (Ag) particle,colloid solution, this drying steps can or spray hot blast and selects in the hot air drying that carries out and carry out at the heat drying that carry out to the mixer heating.
After such drying steps finished, the distilled water that contains in silver (Ag) particle,colloid solution all evaporated, and fine silver (Ag) fundamental particle remains on each powder particle that consists of mixture of powders.
After above-mentioned drying steps finishes, the powder composition that forms is filled in the regulation container, packs, then finished the manufacture process according to powder dentifrice composition of the present invention.
On the other hand, contain in the situation of angelica powder, also carry out the angelica powders mixing.The angelica powders mixing is that the angelica powder of preparing by powder composition preparation process is put in the mixture of powders that has carried out drying steps, again carry out Agitation and mixing, the step that it is distributed equably, at this moment, with respect to all weight of mixture of powders, the angelica powder of input is 1～10 % by weight scope.
On the other hand, simple declaration by above-mentioned manufacture process manufacturing according to the using method that contains the powder dentifrice composition of silver particles of the present invention.
The character that contains the powder dentifrice composition of silver particles according to the present invention is the Powdered of light gray or nattierblue, must be attached to the toothpaste of paste in the past and used, but owing to also can play fully bactericidal action in the time of gargling of short time, therefore can use separately according to pulverous compositions of present embodiment.
Below, expression is according to preferred embodiment of the present invention, and such embodiment is in order to help understanding of the present invention and illustrative, and scope of the present invention is not limited to following embodiment.And, at first, mixture of powders is carried out experiment for the in vitro antibacterial ability of harmful bacteria, and halitosis is removed in experiment, dental plaque is removed ability and used sense, and then experiment has been coated with the in vitro antibacterial ability to harmful bacteria behind silver (Ag) particle,colloid solution.
Below, specific embodiment is described.
(mixture of powders 1)
As shown in table 1 below, will be as silver particles (native silver) 0.0005 % by weight of antibacterial, as trichlorophenol 0.1 % by weight, Olibanum oil 0.1 % by weight, propolis extract 1.0 % by weight of sterilizing ability enhancing adjuvant, as the hexadecylpyridinium chloride of scavenger for dental scar
0.1 % by weight, xylitol 5 % by weight, saccharin sodium 0.002 % by weight as sweeting agent, lactose 85.98 % by weight as excipient, minty note powder 5.0 % by weight, Herba Menthae Rotundifoliae powder 2.0 % by weight as fumet, as hydroxyapatite 0.3 % by weight of brightening agent, mix and the dentifrice composition that makes powder as spirulina blue color 0.4 weight of coloring agent.
(mixture of powders 2)
As shown in table 1 below, will be as silver particles (native silver) 0.5 % by weight of antibacterial, as trichlorophenol 0.2 % by weight, propolis extract 1.5 % by weight of sterilizing ability enhancing adjuvant, as the hexadecylpyridinium chloride of scavenger for dental scar
0.2 % by weight, xylitol 3 % by weight, sorbitol powder 20 % by weight as sweeting agent, lactose 67.90 % by weight as excipient, minty note powder 5.0 % by weight, Herba Menthae Rotundifoliae powder 1.0 % by weight as fumet, as hydroxyapatite 0.5 % by weight of brightening agent, mix and the dentifrice composition that makes powder as spirulina blue color 0.4 weight of coloring agent.
(mixture of powders 3)
As shown in table 1 below, will be as silver particles (native silver) 1.0 % by weight of antibacterial, as trichlorophenol 0.3 % by weight, propolis extract 3 % by weight of sterilizing ability enhancing adjuvant, as the hexadecylpyridinium chloride of scavenger for dental scar
0.4 % by weight, saccharin sodium 0.03 % by weight, sorbitol powder 20 % by weight as sweeting agent, lactose 49.17 % by weight, silicon dioxide 20.0 % by weight as excipient, minty note powder 5.0 % by weight as fumet, as hydroxyapatite 0.7 % by weight of brightening agent, mix as spirulina blue color 0.4 weight of coloring agent and made the powder dentifrice composition.
(mixture of powders 4)
As shown in table 1 below, will be as silver particles (native silver) 1.2 % by weight of antibacterial, as trichlorophenol 0.5 % by weight, Olibanum oil 0.4 % by weight, propolis extract 4 % by weight of sterilizing ability enhancing adjuvant, as the hexadecylpyridinium chloride of scavenger for dental scar
0.5 % by weight, xylitol 10 % by weight, sorbitol powder 20 % by weight as sweeting agent, lactose 55.00 % by weight as excipient, minty note powder 2.0 % by weight, Herba Menthae Rotundifoliae powder 5 % by weight as fumet, as hydroxyapatite 1.0 % by weight of brightening agent, mix and the dentifrice composition that makes powder as spirulina blue color 0.4 weight of coloring agent.
(mixture of powders 5)
As shown in table 1 below, will be as sorbitol powder 20 % by weight of sweeting agent, lactose 73.10 % by weight as excipient, minty note powder 1.0 % by weight, Herba Menthae Rotundifoliae powder 5.0 % by weight as fumet, as hydroxyapatite 0.5 % by weight of brightening agent, mix and the dentifrice composition that makes powder as spirulina blue color 0.4 % by weight of coloring agent.
(mixture of powders 6)
As shown in table 1 below, will be as sorbitol powder 20 % by weight of sweeting agent, as lactose 74.10 % by weight of excipient, as minty note powder 5.0 % by weight of fumet, as hydroxyapatite 0.5 % by weight of brightening agent, mix and the toothpaste that makes powder as spirulina blue color 0.4 % by weight of coloring agent.
Table 1
Experimental example 1
Following experimental example 1 be each mixture of powders of experiment table 1 to the antibacterial ability of the organism of oral cavity harmful bacteria, the test strain that uses this moment has been suitable for and has made tooth send out Streptococcus mutans (Streptococcus mutans cariogenic; NCTC 10449), make companion actinomycetes Actinobacillus (the Actinobacillus actinomycetemcomitans of tooth generation periodontal; ATCC 29522) and Capnocytophaga ochracea (Capnocytophaga ochracea; ATCC 27827), make Fusobacterium nucleatum (the Fusobacterium nucleatum of tooth generation periodontal and halitosis; ATCC 25586).
Above-mentioned test strain is taken out from freezing keeping state, after being inoculated in nutrient broth (Nutrient broth), in 37 ℃ culture medium, cultivated 48 hours, after pre-incubated like this each test organisms liquid is inoculated in the nutrient broth of 100ml with 1% (v/v), after in culture medium, again cultivating 12-20 hour, be used for experiment.
In order to test, the initial value of suitable bacterial population (bacterial suspension number) is 106～107cell/ml, for this reason, from pre-incubated bacterium liquid, respectively get the sterile purified water that 1ml puts into respectively in advance the 100ml of sterilization, this as stock solution, is utilized after progressively dilution method dilutes, to be coated on separately on the solid medium, it was cultivated 24 hours, the colony of regeneration is counted, obtain the initial stage inoculum density.
On the other hand, the preparation of experimental liquid is that the compositions that mixture of powders 1～6 described above prepares like that is mixed in the sterile purified water with identical amount, prepares through long-time dissolving.
And, each experimental liquid of above-mentioned preparation is respectively got 1ml pour into respectively in each test strain of having adjusted the initial stage inoculum density, after 1 minute time, measure remaining bacterium number.The mensuration of bacterium number is carried out by the following method, namely, the stock solution that reclaims is diluted by dilution method progressively, be coated on the dull and stereotyped training base according to each extension rate, after in culture machine, cultivating, bacterium colony of each dull and stereotyped training base is counted, according to the minimizing of the bacterium number of remaining bacterium number whether to be determined, thereby measure antibacterial ability.By the concentration of such method utilization to the remaining bacterium number of initial stage inoculum density, obtain bacteriostasis rate (%) with percentage rate, with this bacteriostasis rate (%) arrangement antibacterial ability (sterilizing ability), then as described in Table 2.
Table 2
As shown in table 2, example 1 as can be known by experiment: the content of silver particles is in the following comparative example 1 of 0.0005 % by weight, sterilizing ability for all test strains is significantly low, when making the content of silver particles increase to 1 % by weight from 0.0005 % by weight, sterilizing ability increases gradually, when surpassing 1 % by weight, sterilizing ability does not change.In addition, do not contain as can be known hexadecylpyridinium chloride fully
Mixture of powders 5 and 6 sterilizing ability significantly low.
As a result, the content that can confirm silver particles is 0.0005 % by weight～1 % by weight, contains hexadecylpyridinium chloride
In the situation, sterilizing ability is excellent.
Experimental example 2
Following experimental example 2 is the compositionss to the mixture of powders 1～6 of making according to the ratio of components of above-mentioned table 1 expression, use with each 10 object by name of men and women of growing up respectively, to removing halitosis, remove dental plaque, using sense to implement organoleptic examination, its meansigma methods is shown in following table 3 according to 5 point scale methods.
Table 3
| Inspection item | Mixture of powders 1 | Mixture of powders 2 | Mixture of powders 3 | Mixture of powders 4 | Mixture of powders 5 | Mixture of powders 6 |
| Remove halitosis | 1.2 | 3.9 | 4.5 | 3.9 | 0.8 | 0.8 |
| Remove dental plaque | 3.0 | 4.1 | 4.7 | 4.6 | 1.4 | 1.4 |
| Use sense | 4.2 | 4.1 | 4.0 | 3.9 | 3.1 | 3.2 |
| On average | 2.73 | 4.03 | 4.50 | 4.13 | 1.76 | 1.80 |
＜very 5,4, general 3, differ from 2, non-constant 1 〉
As shown in table 3, by above-mentioned experimental example 3 as can be known: the content right along with silver particles increases, and removes dental plaque and removes the halitosis raising, but use sense to reduce gradually, does not particularly add hexadecylpyridinium chloride
Mixture of powders 5 and 6 in, remove halitosis and remove the dental plaque effect significantly low.
As a result, example 3 can confirm that the content of silver particles is 0.0005 % by weight～1 % by weight, contains hexadecylpyridinium chloride by experiment
Situation under, can remove halitosis, remove dental plaque and use sense all to satisfy.
Experimental example 3
Following experimental example 3 is to confirm as in the sample of antibacterial ability excellence to select mixture of powders 2 in each mixture of powders of table 1, the silver colloidal solution that concentration is different (20ppm, 30ppm, 50ppm, 60ppm, 70ppm) take with respect to the weight of mixture of powders 2 as the amount of 3 % by weight is coated with prepare after, carry out the in vitro sterilizing ability experiment to the oral cavity harmful bacteria, the result has obtained the result shown in the table 4.Experimental example 3 is to carry out according to the method identical with above-mentioned experimental example 1, but, to put in the sterile purified water with identical amount with the powder dentifrice composition that the mode that can confirm sterilizing ability when actual the gargling is made, but unlike experimental example 1, wait until fully dissolving, but each experimental liquid that will prepare immediately after stirring is respectively got 1ml and is poured into respectively in each test strain of having adjusted the initial stage inoculum density, after 1 minute time, measure remaining bacterium number.The mensuration of bacterium number is carried out by the following method, namely, the stock solution that reclaims is diluted by dilution method progressively, be coated on the dull and stereotyped training base according to each extension rate, after in culture machine, cultivating, bacterium colony of each dull and stereotyped training base is counted, according to the minimizing of the bacterium number of remaining bacterium number whether to be determined, thereby measure antibacterial ability.By such method utilization to the concentration of the remaining bacterium number of initial stage inoculum density with, percentage rate is obtained bacteriostasis rate (%), with this bacteriostasis rate (%) arrangement antibacterial ability (sterilizing ability).
Table 4
Example 3 fact as can be known is by experiment, and is as shown in table 4, is coated with in the situation of silver particles colloid solution, irrelevant with ratio, can relatively play effective bactericidal action in the short time.
But the concentration that can learn silver particles colloid solution is in the situation that 30ppm is following or 60ppm is above, the fact that the sterilizing ability of all test strains all descends.Former thereby speech with regard to it, the concentration of silver particles colloid solution is that 30ppm is when following, be judged as for the concentration of bactericidal action and cross low and can not carry out sufficient bactericidal action, the concentration of silver particles colloid solution is that 60ppm is when above, the size that is judged as along with silver particles becomes large relatively, little with the contact area of test strain, so sterilizing ability reduces.
By above-mentioned explanation the aforesaid powder dentifrice composition and the manufacture method thereof that contain silver particles according to preferred implementation of the present invention has been described, but this only illustrates, and those skilled in the art should be able to understand well in the scope that does not break away from technological thought of the present invention can carry out various variations and change.
Claims (2)
1. manufacture method that contains the powder dentifrice composition of silver particles wherein, comprising:
Powder composition preparation process, prepare respectively as the antibacterial that suppresses oral cavity bacterium, particle diameter is 10～200 mu m ranges and the silver particles that contains with 0.0005～1.0 % by weight scope, contain to be selected from hexadecylpyridinium chloride
0.1～0.5 % by weight, sodium fluoride 0.01～0.05 % by weight, 1 kind or 2 kinds scavenger for dental scar in sodium monofluorophosphate 0.1～0.7 % by weight, contain and be selected from trichlorophenol 0.01～0.5 % by weight, Olibanum oil 0.01～0.5 % by weight, the sterilizing ability more than a kind in propolis extract powder 0.1～5 % by weight strengthens adjuvant, contain and be selected from xylitol powder 1.0～10 % by weight, saccharin sodium 0.01～1.0 % by weight, the sweeting agent more than a kind in sorbitol powder 2.0～30 % by weight, contain and be selected from lactose 50.0～86.0 % by weight, the excipient more than a kind in silica 1 9.0～75.0 % by weight, and the fumet that contains with the surplus % by weight of described each composition, brightening agent, coloring agent, and the content sum of each composition is 100 % by weight;
The solution preparation process injects sterile purified water in electrolysis bath, purity is set is 99.9% silver rod, and the concentration of preparing silver particles by electrolytic process is the silver particles colloid solution of 30～60ppm;
Mixture forms step, forms mixture of powders on one side make described each powder composition of preparing in the described powder preparation process drop into mixer by 20～30 purpose sieves on one side;
Application step, spray described silver particles colloid solution while stirring, mix described mixture of powders, so that with respect to the weight of described mixture of powders, described silver particles colloid solution is 3～10 % by weight scopes, thereby is coated with on the surface of described each powder composition; And
Drying steps carries out drying with the mixture of powders that has been coated with described silver particles colloid solution in the described application step.
2. the manufacture method that contains the powder dentifrice composition of silver particles according to claim 1, wherein, after implementing described drying steps, also comprise the angelica powders mixing, described angelica powders mixing comprises: drop into the angelica powder, so that with respect to all weight of described mixture of powders, described angelica powder is 1～10 % by weight scope, and evenly mix.
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| CN109475473A (en) * | 2016-07-14 | 2019-03-15 | 荷兰联合利华有限公司 | Oral care composition comprising the composite material granular containing cationic germicide |
| CN106214502A (en) * | 2016-08-22 | 2016-12-14 | 重庆千贸实业有限公司 | Toothpaste |
| EP3843692A1 (en) * | 2018-08-28 | 2021-07-07 | 3M Innovative Properties Company | Aqueous oral care solutions, methods, kits, and tooth surfaces having a coating derived from the oral care solution |
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| CN1433751A (en) * | 2003-01-24 | 2003-08-06 | 武汉大学 | Nano colloidal silver toothpaste |
| CN101547679A (en) * | 2006-12-08 | 2009-09-30 | 金基暎 | Liquid-type dentifrice composition contained silver particles and mousse-type dentifrice using the same |
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| KR100494287B1 (en) * | 2002-12-10 | 2005-06-13 | 김기영 | Manufacturing method of tooth paste contained silver particles |
| KR20080101954A (en) * | 2007-05-17 | 2008-11-24 | 김기영 | Powder-type dentifrice composition contained silver particles |
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| CN1433751A (en) * | 2003-01-24 | 2003-08-06 | 武汉大学 | Nano colloidal silver toothpaste |
| CN101547679A (en) * | 2006-12-08 | 2009-09-30 | 金基暎 | Liquid-type dentifrice composition contained silver particles and mousse-type dentifrice using the same |
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