CN106074195B - A kind of hydroxyl apatite and the toothpaste of calcium carbonate and preparation method thereof - Google Patents
A kind of hydroxyl apatite and the toothpaste of calcium carbonate and preparation method thereof Download PDFInfo
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- CN106074195B CN106074195B CN201610539053.XA CN201610539053A CN106074195B CN 106074195 B CN106074195 B CN 106074195B CN 201610539053 A CN201610539053 A CN 201610539053A CN 106074195 B CN106074195 B CN 106074195B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds thereof
- A61K8/21—Fluorides; Derivatives thereof
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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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Abstract
The toothpaste of hydroxyl apatite and calcium carbonate of the present invention includes nano-grade hydroxy apatite, micron order calcium carbonate and fluoride；The partial size of nano-grade hydroxy apatite is less than 100 nm, the partial size of micron order calcium carbonate is 0.1 μm ~ 10 μm, mass concentration of the fluorine element in hydroxy agustite tooth-paste is not more than 8.0wt% in fluoride, the mass content of nano-grade hydroxy apatite is not more than 20wt%, and the mass ratio of micron order calcium carbonate and nano-grade hydroxy apatite is 1/10 ~ 10:1.When the toothpaste of the hydroxyl apatite and calcium carbonate uses, demineralization enamel and demineralization dentine piece is helped to carry out biomineralization, repairing dental enamel surface and diminution dentine facing canaliculi dentales aperture, or even block dentinal tubule or deposit hydroxyapatite layer in dentin surface.At the same time, fluoride hydrolysis generates fluorine ion, promotes the mineralization process of hydroxyapatite in tooth, significantly improves the toothpaste to the repair function of enamel and dentine.
Description
Technical field
The invention belongs to life chemical product technical fields, and in particular to one kind, which has, repairs demineralization enamel and demineralization tooth sheet
The toothpaste and preparation method thereof containing nano-grade hydroxy apatite and micron order calcium carbonate of matter.
Background technique
Toothpaste has become the necessity in people's daily life.As the improvement of people's living standards, bad diet knot
The generation of structure, the intake of sugared high-content threaten the oral health of people.High sugar, especially sucrose, remain in oral cavity, are divided
Solution is at acid, the dentine for corroding tooth enamel and being exposed to surface, and the demineralization for generating enamel and dentine is seriously made
At some column diseases such as saprodontia, tooth loss or sensitivity of tooth, people's health is seriously affected.So a can repair of research and development takes off
The toothpaste of mine enamel surface and dentine has very important significance.
Hydroxyapatite has good biocompatibility and bioactivity and the main component of dentine sclerous tissues,
It is thus widely applied in formulation of tooth-paste, promotes the reparation of enamel and dentine.Micron order calcium carbonate then can be tooth
It repairs and calcium ion is provided, can also improve the pH value of microenvironment, be conducive to the reparation of tooth, but since it does not have with dental surface
There is stronger suction-operated, is difficult to deposit to dental surface.
Summary of the invention
For this purpose, the present invention finds the synergistic effect of nano-grade hydroxy apatite and micron order calcium carbonate in toothpaste, thus
There is provided it is a kind of can effectively repair demineralization enamel and demineralization dentine containing nano-grade hydroxy apatite and micron order calcium carbonate
Toothpaste and preparation method thereof.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of toothpaste containing nano-grade hydroxy apatite and micron order calcium carbonate of the present invention includes micron order carbonic acid
Calcium, nanometer hydroxyapatite and fluoride；
The partial size of the nano-grade hydroxy apatite is less than 100nm, the partial size of the micron order calcium carbonate be 38 μm and its
Below；
Mass concentration of the fluorine element in the hydroxy agustite tooth-paste is not more than 0.1wt% in the fluoride, described
The mass content of nano-grade hydroxy apatite is not more than 20wt%, the micron order calcium carbonate and the nano-grade hydroxy apatite
Mass ratio be 1:10~10:1.
The partial size of the micron order calcium carbonate is 13 μm and its hereinafter, the partial size of the nano-grade hydroxy apatite is 30nm
~80nm.
The mass ratio of the micron order calcium carbonate and the nanometer hydroxyapatite is 1:2~4:1, and the micron order carbon
The mass content of sour calcium is 4wt%~30wt%.
The mass content of the micron order calcium carbonate is 4wt%, and the mass content of the nano-grade hydroxy apatite is
4wt%, and calcium carbonate crystal form is calcite phase.
The fluoride is sodium fluoride and/or sodium monofluorophosphate, and fluorine element is in the hydroxyapatite in the fluoride
Mass concentration in toothpaste is not more than 0.1wt%.
Preferably, further include rubbing agent, thickener, moisturizer, sweetener, bacteriostatic agent, foaming agent, essence, in pigment
It is at least one.
Preferred toothpaste includes the component of following mass percent:
The micron order calcium carbonate 2wt%~40wt%,
Nano-grade hydroxy apatite 1wt%~the 20wt%,
Rubbing agent 2wt%~the 40wt%,
Thickener 0.02wt%~the 8wt%,
Moisturizer 1wt%~the 50wt%,
Sweetener 0.001wt%~the 0.1wt%,
Bacteriostatic agent 0.004wt%~the 0.1wt%,
Foaming agent 0.1wt%~the 5wt%,
Fluoride 0wt%~the 2wt%,
Essence 0.6wt%~the 3wt%,
Pigment 0wt%~the 0.01wt%.
Preferably, the rubbing agent is at least one of silica, calcium phosphate dibasic dihydrate or calcium carbonate；The increasing
Thick dose is at least one of xanthan gum, carragheen or sodium carboxymethylcellulose；The moisturizer is glycerol, sorbierite or poly- second
At least one of glycol 400；The sweetener is at least one of saccharin, Sucralose or xylitol；The bacteriostatic agent
For at least one of zinc citrate, sodium benzoate or methylparaben；The foaming agent is lauryl sodium sulfate, cocounut oil acyl
At least one of amine propyl betaine or sodium lauroyl sarcosine；The essence is Mint Essence；The pigment is fruit green
At least one of element, allured red pigment, bright blue pigment or lemon yellow pigment.
Preferred formula includes: dicalcium phosphate dihydrate 12wt%, carragheen 0.8wt%, glycerol 28wt%, Sucralose
0.1wt%, zinc citrate 0.05wt%, lauryl sodium sulfate 2wt%, sodium monofluorophosphate 0.76wt%, essence 1.25wt%,
Pigment 0.005wt%, hydrated SiO 2 10wt%, micron order calcium carbonate 4wt%, nanometer hydroxyapatite 4wt%；
The micron order calcium carbonate is calcite crystal form, filters by 1200 mesh sieve that average grain diameter is 13 μm or less；
The average grain diameter 60nm of the nano-grade hydroxy apatite.
The preparation method of hydroxy agustite tooth-paste of the present invention, which comprises the steps of:
The recipe ingredient of the toothpaste is placed in 200rpm~1000rpm in blender and stirs 20min~60min；
Vacuum outgas is at paste.
The above technical solution of the present invention has the following advantages over the prior art:
It include micron order carbon 1. containing nano-grade hydroxy apatite and micron order calcium carbonate toothpaste described in the embodiment of the present invention
Sour calcium, nanometer hydroxyapatite and fluoride；The partial size of the nanometer hydroxyapatite is less than 100nm, the micron hydroxyl phosphorus
The partial size of lime stone is less than 13 μm；Mass concentration of the fluorine element in the hydroxy agustite tooth-paste is not more than in the fluoride
The mass content of 0.1wt%, the nano-grade hydroxy apatite are not more than 20wt%, the micron order calcium carbonate and the nanometer
The mass ratio of hydroxyapatite is 1:10~10:1.The toothpaste is in use, remaining micro-calcium carbonate and nano hydroxyapatite
Lime stone synergistic effect, can sustained release calcium ion and phosphate anion, improve microenvironment pH value, help demineralization enamel surface
Biomineralization, repairing dental enamel and dentine piece are carried out with demineralization dentine piece, reduces canaliculi dentales aperture, or even blocking dentine
Tubule deposits hydroxyapatite layer in dentin surface.
2. the preparation method of toothpaste of the present invention, simple process, lotion is uniform and stable, is easy to industrialization.
Detailed description of the invention
Fig. 1 be comparative example toothpaste 1, in embodiment toothpaste 2 and 3 micron order calcium carbonate scanning electron microscope (SEM) figure；
Fig. 2 is scanning electron microscope (SEM) figure of nano-grade hydroxy apatite in embodiment toothpaste 2,3 and comparative example toothpaste 4；
Fig. 3 is that starting baseline, acid attack and toothpaste treated the surface micro-vickers hardness of enamel in experimental example 1 become
Change histogram (10 enamel of every group of sample).English alphabet indicates the statistics between the micro-vickers hardness of different enamel groups
Learn difference (mark letter is different, then p value < 0.05, and there are the differences of statistical significance)；
Fig. 4 a is scanning electron microscope (SEM) figure of the enamel surface after polishing；
Fig. 4 b is scanning electron microscope (SEM) figure of acid eroded enamel surface；
Fig. 4 c is scanning electron microscope (SEM) figure of SOF treated enamel surface；
Fig. 4 d is scanning electron microscope (SEM) figure of treated the enamel surface of toothpaste 1；
Fig. 4 e is scanning electron microscope (SEM) figure of treated the enamel surface of toothpaste 2；
Fig. 4 f is scanning electron microscope (SEM) figure of treated the enamel surface of toothpaste 3；
Fig. 4 g is scanning electron microscope (SEM) figure of treated the enamel surface of toothpaste 4；
Fig. 5 a is scanning electron microscope (SEM) figure of dentine sample after 36wt% phosphate aqueous solution corrodes 2min；
Fig. 5 b is SEM picture of the dentine sample after Mouthsimulator saliva (SOF) is handled 6 times；
Fig. 5 c is SEM picture of the dentine sample after comparative example toothpaste 1 is handled 6 times；
Fig. 5 d is SEM picture of the dentine sample after embodiment toothpaste 2 is handled 6 times；
Fig. 5 e is SEM picture of the dentine sample after embodiment toothpaste 3 is handled 6 times；
Fig. 5 f is SEM picture of the dentine sample after comparative example toothpaste 4 is handled 6 times；
Fig. 5 g is SEM picture of the dentine sample after Mouthsimulator saliva (SOF) is handled 14 times；
Fig. 5 h is SEM picture of the dentine sample after comparative example toothpaste 1 is handled 14 times；
Fig. 5 i is SEM picture of the dentine sample after embodiment toothpaste 2 is handled 14 times；
Fig. 5 j is SEM picture of the dentine sample after embodiment toothpaste 3 is handled 14 times；
Fig. 5 k is SEM picture of the dentine sample after comparative example toothpaste 4 is handled 14 times；
Fig. 6 a is the graph of pore diameter distribution of dentine sample dentinal tubule after 36wt% phosphate aqueous solution corrodes 2min；
Fig. 6 b is the graph of pore diameter distribution of dentine sample dentinal tubule after Mouthsimulator saliva (SOF) is handled 6 times；
Fig. 6 c is the graph of pore diameter distribution of dentine sample dentinal tubule after comparative example toothpaste 1 is handled 6 times；
Fig. 6 d is the graph of pore diameter distribution of dentine sample dentinal tubule after embodiment toothpaste 2 is handled 6 times；
Fig. 6 e is the graph of pore diameter distribution of dentine sample dentinal tubule after embodiment toothpaste 3 is handled 6 times；
Fig. 6 f is the graph of pore diameter distribution of dentine sample dentinal tubule after comparative example toothpaste 4 is handled 6 times；
Fig. 6 g is the pore-size distribution of dentine sample dentinal tubule after Mouthsimulator saliva (SOF) is handled 14 times
Figure；
Fig. 6 h is the graph of pore diameter distribution of dentine sample dentinal tubule after comparative example toothpaste 1 is handled 14 times；
Fig. 6 i is the graph of pore diameter distribution of dentine sample dentinal tubule after embodiment toothpaste 2 is handled 14 times；
Fig. 6 j is the graph of pore diameter distribution of dentine sample dentinal tubule after embodiment toothpaste 3 is handled 14 times；
Fig. 6 k is the graph of pore diameter distribution of dentine sample dentinal tubule after comparative example toothpaste 4 is handled 14 times；
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with the drawings and specific embodiments
The present invention is described further.The present invention can be embodied in many different forms, and should not be construed as limited to herein
The embodiment of elaboration.On the contrary, these embodiments are provided, so that the disclosure will be thorough and complete, and will be of the invention
Design is fully conveyed to those skilled in the art, and the present invention will only be defined by the appended claims.
Comparative example toothpaste 1
The present embodiment provides a kind of hydroxy agustite tooth-pastes, by percentage to the quality, are made of following raw materials according:
Dicalcium phosphate dihydrate 12wt%, hydrated SiO 2 10wt%, carragheen 2wt%, glycerol 28wt%, Sucralose
0.1wt%, zinc citrate 0.05wt%, lauryl sodium sulfate 2wt%, sodium monofluorophosphate 0.76wt%, Mint Essence
1.25wt%, lemon yellow pigment 0.005wt%, micron order calcium carbonate 8.0wt%, surplus are deionized water.
The preparation method of the hydroxy agustite tooth-paste, includes the following steps:
S1, said components are placed in 800rpm stirring 40min in blender；
S2, vacuum outgas are at paste.
Micron order calcium carbonate is 1200 mesh calcites, as shown in Figure 1.
Embodiment toothpaste 2
The present embodiment provides one kind to contain nano-grade hydroxy apatite and micron order calcium carbonate toothpaste, by percentage to the quality,
It is made of following raw materials according:
Dicalcium phosphate dihydrate 12wt%, carragheen 2wt%, glycerol 28wt%, Sucralose 0.1wt%, zinc citrate
0.05wt%, lauryl sodium sulfate 2wt%, sodium monofluorophosphate 0.76wt%, Mint Essence 1.25wt%, lemon yellow pigment
0.005wt%, hydrated SiO 2 10wt%, micron order calcium carbonate 6wt%, nano-grade hydroxy apatite 2wt%, surplus are to go
Ionized water.
Micron order calcium carbonate is 1200 mesh calcites, less than 13 μm, as shown in Figure 1；The average grain of nanometer hydroxyapatite
Diameter is 60nm, as shown in Figure 2.
The preparation method of the toothpaste, includes the following steps:
S1, said components are placed in 800rpm stirring 40min in blender；
S2, vacuum outgas are at paste.
Embodiment toothpaste 3
The present embodiment provides one kind to contain nano-grade hydroxy apatite and micron order calcium carbonate toothpaste, by percentage to the quality,
It is made of following raw materials according:
Dicalcium phosphate dihydrate 12wt%, carragheen 2wt%, glycerol 28wt%, Sucralose 0.1wt%, zinc citrate
0.05wt%, lauryl sodium sulfate 2wt%, sodium monofluorophosphate 0.76wt%, Mint Essence 1.25wt%, lemon yellow pigment
0.005wt%, hydrated SiO 2 10wt%, micron order calcium carbonate 4wt%, nano-grade hydroxy apatite 4wt%, surplus are to go
Ionized water.
Micron order calcium carbonate is 1200 mesh calcites, less than 13 μm, as shown in Figure 1；The average grain of nanometer hydroxyapatite
Diameter is 60nm, as shown in Figure 2.
The preparation method of the toothpaste, includes the following steps:
S1, said components are placed in 100rpm stirring 20min in blender；
S2, vacuum outgas are at paste.
Comparative example toothpaste 4
The present embodiment provides a kind of hydroxy agustite tooth-pastes, by percentage to the quality, are made of following raw materials according:
Dicalcium phosphate dihydrate 12wt%, carragheen 2wt%, glycerol 28wt%, Sucralose 0.1wt%, zinc citrate
0.05wt%, lauryl sodium sulfate 2wt%, sodium monofluorophosphate 0.76wt%, Mint Essence 1.25wt%, lemon yellow pigment
0.005wt%, hydrated SiO 2 10wt%, micron order calcium carbonate 0.0wt%, nano-grade hydroxy apatite 8.0wt%, surplus
For deionized water.
Micron order calcium carbonate is 1200 mesh calcites, less than 13 μm, as shown in Figure 1；The average grain of nanometer hydroxyapatite
Diameter is 60nm, as shown in Figure 2.
The preparation method of the hydroxy agustite tooth-paste, includes the following steps:
S1, said components are placed in 800rpm stirring 60min in blender；
S2, vacuum outgas are at paste.
The external reparative experiment of 1 demineralization enamel of experimental example
Mouthsimulator saliva (SOF), specific ingredient are as follows: 137.35mM NaCl, 4.17mM NaHCO3,3.01mM
KCl、7.17mM K2HPO4·3H2O、1.53mM MgCl2·6H2O、20.00mM HCl、0.90mM CaCl2、0.51mM
Na2SO4 and Tris tune pH value is to 7.0.
Baurodont is cut using low-speed diamond cutting machine (SYJ-160 low-speed diamond cutting machine), is prepared with a thickness of 2mm's
Enamel piece, then the silicon carbide waterproof abrasive paper polishing grinding respectively through 200,400,1000,2000 and 4000 mesh are flat to surface-brightening
It is whole；It is finally polished smooth with 3M polishing paper (3 microns), and is cleaned by ultrasonic 3min in deionized water, it is spare.It is hard using micro Vickers
Spend instrument (HV-1000Z type, load 500gf, 15 seconds) measure enamel surface micro-vickers hardness, according to hardness, select suitable tooth
Enamel specimen, and 5 groups are randomly divided into, every group 10.It is smooth in every group of enamel piece insertion oral cavity elastomeric material (Shanghai dove board)
Enamel is face-up, pre-processes 10min demineralization through 1.0% aqueous citric acid solution, then carries out micro-vickers hardness test.Toothpaste
Handling demineralization enamel, specific step is as follows: weighing 5.0g SOF, comparative example toothpaste 1, embodiment toothpaste 2, embodiment toothpaste 3
Add the stirring of 10.0g deionized water that solution or toothpaste slurries are made respectively with comparative example toothpaste 4, and is poured on 5 groups embedded with enamel sample
It is quiet to put 2min on the elastomeric material of product；Then, it is rinsed 3 times with 20mL deionized water, is put into 20ml Mouthsimulator saliva and soaks
Bubble；Then, it is by the constant rate of speed that the container containing Mouthsimulator saliva and enamel elastomeric material is placed in 37 DEG C
4h in the constant temperature oscillator (THZ-98A) of 150rpm.Processing enamel specimen 3 times daily, the mistake in 37 DEG C of Mouthsimulator salivas
Night.When handling sample number is 14 times, enamel specimen is taken out, carries out micro-vickers hardness test, and every group of taking-up enamel
It is a piece of, it separately respectively takes normal enamel piece and demineralization enamel a piece of, after all drying, saves, for scanning electron microscope mirror SEM
(Hitachi S-3400N) phenetic analysis enamel surface repairs situation.
Fig. 3 is that starting baseline, acid attack and toothpaste treated the surface micro-vickers hardness of enamel change histogram
And its results of statistical analysis.On starting baseline, SOF, comparative example toothpaste 1, embodiment toothpaste 2, embodiment toothpaste 3 and comparison
Example toothpaste 45 groups of enamel average micro-vickers hardness be respectively 291.0 ± 9.0HV, 285.0 ± 12.9HV, 286.5 ±
15.0HV, 282.4 ± 13.4HV and 281.8 ± 10.9HV (Fig. 3), and one-way analysis of variance (Anova, Tukey) shows 5 groups
Not there is significant difference between the surface micro-vickers hardness of enamel.After 1% lemon acid attack, SOF, toothpaste 1,2,
The average micro-vickers hardness of 3 and 45 groups of enamel be reduced to be 190.2 ± 10.3HV, 188.7 ± 10.7HV, 186.2 ±
11.7HV, 184.7 ± 12.2HV and 184.9 ± 9.5HV；One-way analysis of variance (Anova, Tukey) shows 5 groups of enamel
Not there is significant difference between the micro-vickers hardness of surface.After SOF or toothpaste are handled enamel piece 14 times, SOF, toothpaste
1, the average micro-vickers hardness of 2,3 and 45 groups of enamel is improved to being 199.6 ± 8.2HV, 207.7 ± 12.6HV, 219.6
± 16.0HV, 229.3 ± 17.0HV and 210.0 ± 6.9HV.It is arranged from high to low by enamel surface micro-vickers hardness, sample
Product group is followed successively by 3 groups of toothpaste, 2 groups of toothpaste, 4 groups of toothpaste, 1 group of toothpaste and SOF group.Each group enamel microhardness statisticallys analyze such as
Under: significant difference is not present between SOF group, 1 group of toothpaste and 4 groups of toothpaste；Containing 6.0% micron order calcium carbonate and 2.0% nanoscale
2 groups of the toothpaste of hydroxyapatite, compared with SOF group, there are the significant difference of statistical significance (p value < 0.05)；It is micro- containing 4.0%
3 groups of toothpaste of meter level calcium carbonate and 4.0% nano-grade hydroxy apatite compare one by one with SOF group, 1 group of toothpaste and 4 groups of toothpaste,
There is the significant difference (p value < 0.05) of statistical significance.
Fig. 4 is the Electron micrographs picture of starting normal, acid attack and toothpaste treated enamel surface.It is normal to throw
Enamel surface after light is smooth, smooth (Fig. 4 a)；Acid eroded enamel surface defect, it is rugged, it is largely distributed several
The hole (Fig. 4 b) of micron size；After SOF is handled 14 times, fish scale-shaped is presented in enamel surface, and micro-crack size is 1~2 micron
(Fig. 4 c)；After the processing of toothpaste 1, sand dune shape is presented in enamel surface, and partial region is relatively flat (Fig. 4 d)；In the processing of toothpaste 2
Afterwards, there is a certain amount of deposit in enamel surface, and plane is more smooth, distributed certain micro- hole (Fig. 4 e)；In toothpaste 3
After processing, enamel surface also has certain deposit, and plane is quite smooth, and than sparse, the size in hole is about 1 micron in micro- hole
(Fig. 4 f)；After the processing of toothpaste 4, enamel surface also has a small amount of deposit, is in sand dune shape, cheats also small 1~2 micron (Fig. 4 g).
After acid attack, enamel surface becomes rugged, and surface micro-vickers hardness is reduced within the scope of 180~190HV.
Because the low ph value of citric acid causes hydroxyapatite to dissolve, the demineralization of enamel surface is formed, the hydroxyapatite on surface lacks
It loses or density reduces.In hydroxyapatite course of dissolution, calcium ion, hydroxide ion and phosphate anion are successively lost.
In SOF group, fish scale-shaped is presented in enamel surface, and surface micro-vickers hardness has to fraction of promotion, is not obtained adequately
Mineralising reparation illustrates calcium ion present in SOF solution and phosphate anion supersaturation, is made by hydroxylapatite biology mineralising
With repairing dental enamel surface can be helped, but repairing effect is limited to calcium ion and phosphate anion a small amount of in solution；In tooth
In 1 group of cream, the micron order calcium carbonate in toothpaste can provide certain calcium concentration, help to improve environmental pH；Sodium monofluorophosphate
It can promote dental hydroxy apatite mineralising, so enamel surface obtains effectively mineralising, sand dune shape, part area is presented in surface
Domain is relatively flat, and micro-vickers hardness is highly improved；In 2 groups of toothpaste, enamel surface obtains active and effective mine
Change, compared with SOF group, micro-vickers hardness is significantly improved；In 3 groups of toothpaste, with SOF group, 1 group of toothpaste and 4 groups of toothpaste
Enamel compare, surface micro-vickers hardness obtains being obviously improved for statistical significance, and enamel surface obtains best mine
Change and repair, and the deposit on surface is also most, illustrates the mutual of 4.0% micron order calcium carbonate and 4.0% nano-grade hydroxy apatite
Match, generates synergistic effect, optimal mass ratio is 1:1, the maximum amount of tosca is formed in enamel surface, subsequent
During, sustained release calcium ion and phosphate radical, preferably repairing dental enamel surface；In 4 groups of toothpaste, enamel dimensional microstructure
Family name's hardness is greatly improved, and surface is also relatively flat, illustrates that nanometer hydroxyapatite and single fluorapatite can be helped effectively
Demineralization enamel surface mineralising.
The external reparative experiment of 2 demineralization dentine of experimental example
The healthy third molar (patient's informed consent) extracted by correction is collected in stomatological hospital, is sufficiently cleaned up and is put into
In 0.5wt% thymol aqueous solution.Thickness is prepared using low-speed diamond cutting machine (SYJ-160 low-speed diamond cutting machine)
Silicon carbide waterproof abrasive paper polishing grinding for the dentine thin slice of 2mm, then respectively through 200,400,1000,2000 and 4000 mesh is to table
Face light is smooth；It is finally polished smooth with 3M polishing paper (3 microns), and is cleaned by ultrasonic 3min in deionized water, it is spare.
Before use, every dentine piece, which is put into demineralization in 36wt% phosphate aqueous solution, handles 2min, deionized water is then used
3min is rinsed, taking out sample before 3 dentine do toothpaste processing, to be used as phenetic analysis, residue is randomized into 5 groups, every group 6.
Dentine piece is fixed in oral cavity elastomeric material (Shanghai dove board), and dentine is face-up.Toothpaste handles the specific of dentine sample
Steps are as follows: weighing 5.0g SOF, experimental group toothpaste 1,2,3 and 4 respectively plus aqueous solution or tooth is made in the stirring of 10.0g deionized water
Cream slurries, and be poured on 5 groups of elastomeric materials embedded with dentine sample, with soft bristle tooth brush (bright and clear jade-like stone profit toothbrush) manual light brush
1min, it is quiet to put 1min；Then, it is rinsed 3 times with 20mL deionized water, is put into 20ml Mouthsimulator saliva and impregnates；Then, will contain
The constant rate of speed for having the container of Mouthsimulator saliva and dentine piece to be placed in 37 DEG C is the constant temperature oscillator (THZ- of 150rpm
4h in 98A).Processing dentine sample 3 times daily, and after third time processing, in 37 DEG C of Mouthsimulator salivas overnight.Work as place
When to manage sample number be 6,14 times, take out 3 dentine samples, after drying and processing, save, for scanning electron microscope mirror SEM (day
Vertical S-3400N) phenetic analysis dentin surface deposition and dentinal tubule diameter change situation (before characterization, dentine sample
Product surface vacuum is gold-plated) and final dentine sample surfaces progress X-ray elemental analysis (20KeV).Schemed according to sample SEM
Piece, measurement dentinal tubule aperture (canaliculi dentales diameter measuring method: by dentinal tubule center and reach tubule both sides most
Short distance, and measure number and be greater than 120, take the average value of 3 dentine canaliculi dentales).
In Electron micrographs picture, acid eroded dentin surface is smooth, and surface canaliculi dentales are all exposed,
Average pore size is 3.89 ± 0.54 μm (Fig. 5 a and Fig. 6 a).Different processing brings the variation of multiplicity: SOF to the dentine of demineralization
After processing 6 times or 14 times, dentin surface is still smooth, but canaliculi dentales aperture becomes smaller, respectively 3.58 ± 0.52 μm of (Fig. 5 b
With Fig. 6 b) and 3.32 ± 0.52 μm (Fig. 5 g and Fig. 6 g)；After toothpaste 1 is handled 6 times or 14 times, there is certain deposition in dentin surface
Object, canaliculi dentales aperture also become smaller, and respectively 3.44 ± 0.46 μm (Fig. 5 c and Fig. 6 c) and 3.08 ± 0.44 μm (Fig. 5 h and Fig. 6 h)；
After toothpaste 2 is handled 6 times or 14 times, there is deposit in dentin surface, and canaliculi dentales aperture also becomes smaller, and respectively 3.28 ± 0.52 μm
(Fig. 5 d and Fig. 6 d) and 2.76 ± 0.46 μm (Fig. 5 i and Fig. 6 i)；After toothpaste 3 is handled 6 times or 14 times, there is particle in dentin surface
Shape deposit, a small amount of canaliculi dentales be blocked, canaliculi dentales aperture also becomes smaller, respectively 3.10 ± 0.50 μm (Fig. 5 e and Fig. 6 e) and
2.56 ± 0.56 μm (Fig. 5 j and Fig. 6 j)；After toothpaste 4 is handled 6 times or 14 times, there are graininess deposit, canaliculi dentales in dentin surface
Aperture also becomes smaller, and respectively 3.31 ± 0.49 μm (Fig. 5 f and Fig. 6 f) and 2.93 ± 0.56 μm (Fig. 5 k and Fig. 6 k).According to diminution
The effect of canaliculi dentales, successively sequence was toothpaste 3, toothpaste 2, toothpaste 4,1 and of toothpaste respectively from toothpaste and SOF is tested to weak arrangement by force
SOF。
In dentine semiquantitative surface elemental analysis result (voltage 20eKv), acid attack dentine, SOF group, toothpaste 1
Handled in group, 2 groups of toothpaste, 3 groups of toothpaste and 4 groups of toothpaste 14 Ci Hou dentin surface calcium-phosphorus ratios respectively may be about 0.2,0.7,1.1,2,
1.8 and 1.5.
In actual treatment process, the diminution in demineralization dentin surface canaliculi dentales aperture is biomineralization as a result, being
Active matter provides calcium ion, phosphate anion in toothpaste, under the influence of fluorine ion and pH environment, forms hydroxyapatite phase substance
Result.Here active matter includes SOF solution, calcium carbonate and hydroxyapatite.After acid attack, dentin surface or its surface
In exposed canaliculi dentales, demineralization dentine is repaired in the micron order and nano-scale particle being easy in deposition toothpaste, help.Final
As a result in, the remineralization efficacy of 1,2,3 and 4 pair of demineralization dentine of toothpaste will be got well than SOF solution, show the micron order in toothpaste
Calcium carbonate, nano-grade hydroxy apatite and single fluorapatite serve, and can bring significantly mineralising repairing effect.Toothpaste 1,
2, in 3 and 4 groups, toothpaste 3 of the discovery containing 4.0% micron order calcium carbonate and 4.0% nano-grade hydroxy apatite is to demineralization dentine
Remineralization efficacy it is best, than containing 8.0% micron order calcium carbonate 1 group of toothpaste and containing the toothpaste 4 of 8.0% nano-grade hydroxy apatite
Group will be got well, and be implied in toothpaste 3, and synergistic effect may be present in 4% micron order calcium carbonate and 4% nano-grade hydroxy apatite,
Advantage deposition in surface adjusts solution environmental pH value and during subsequent, also for the mineralising of tooth provide more calcium ions and
Phosphate anion.The best in quality ratio of its micro-calcium carbonate and nano-grade hydroxy apatite is 1:1.Toothpaste handles 14 backteeth
Essential semi-quantitative elemental analysis is the result shows that the toothpaste 2 and 3 containing micron order calcium carbonate and nano-grade hydroxy apatite is processed
Dentin surface calcium-phosphorus ratio, than other group it is high, it is also higher than the calcium-phosphorus ratio numerical value 1.67 of hydroxyapatite, illustrate that there are micro-
The deposition of meter level calcium carbonate, and the deposition of these calcium carbonate is generated under the collaboration help of nanometer hydroxyapatite
's.Trace it to its cause may be micron order calcium carbonate and nano-grade hydroxy apatite particle surface different charge adsorption effect.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (5)
1. a kind of toothpaste containing nano-grade hydroxy apatite and micron order calcium carbonate, which is characterized in that include nano-grade hydroxy phosphorus
Lime stone, micron order calcium carbonate and fluoride；The partial size of the nano-grade hydroxy apatite is 30nm~80nm, the nanoscale hydroxyl
The mass content of base apatite is 4wt%, and the partial size of the micron order calcium carbonate is 13 μm and its hereinafter, the micron order carbonic acid
The mass content of calcium is 4wt%, and calcium carbonate crystal form is calcite phase；The fluoride be sodium fluoride and/or sodium monofluorophosphate,
Mass concentration of the fluorine element in the toothpaste is not more than 0.1wt% in the fluoride.
2. toothpaste according to claim 1, which is characterized in that further include rubbing agent, thickener, moisturizer, sweetener, suppression
At least one of microbial inoculum, foaming agent, essence, pigment.
3. toothpaste according to claim 2, which is characterized in that the rubbing agent be silica, dicalcium phosphate dihydrate or
At least one of calcium carbonate；The thickener is at least one of xanthan gum, carragheen or sodium carboxymethylcellulose；It is described
Moisturizer is at least one of glycerol, sorbierite or polyethylene glycol 400；The sweetener is saccharin, Sucralose or xylose
At least one of alcohol；The bacteriostatic agent is at least one of zinc citrate, sodium benzoate or methylparaben；The foaming
Agent is at least one of lauryl sodium sulfate, Cocoamidopropyl betaine or sodium lauroyl sarcosine；The essence is
Mint Essence；The pigment is at least one of light green pigment, allured red pigment, bright blue pigment or lemon yellow pigment.
4. toothpaste according to claim 3 is, characterized by comprising: dicalcium phosphate dihydrate 12wt%, carragheen
0.8wt%, glycerol 28wt%, Sucralose 0.1wt%, zinc citrate 0.05wt%, lauryl sodium sulfate 2wt%, single fluorine
Sodium phosphate 0.76wt%, essence 1.25wt%, pigment 0.005wt%, hydrated SiO 2 10wt%, micron order calcium carbonate
4wt%, nanometer hydroxyapatite 4wt%；The micron order calcium carbonate is calcite crystal form, filters by 1200 mesh sieve, puts down
Equal partial size is 13 μm or less；The average grain diameter 60nm of the nano-grade hydroxy apatite.
5. a kind of preparation method of the described in any item toothpaste of claim 1-4, which comprises the steps of: by institute
The recipe ingredient for stating toothpaste is placed in 200rpm~1000rpm in blender and stirs 20min~60min；Vacuum outgas is at paste.
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| CN106511105B (en) * | 2017-01-10 | 2020-04-21 | 杭州皎洁口腔保健用品有限公司 | Anhydrous toothpaste for repairing demineralized enamel and dentin and preparation method thereof |
| CN107157785A (en) * | 2017-05-18 | 2017-09-15 | 中国人民解放军第四军医大学 | A kind of remineralization of teeth toothpaste and preparation method thereof |
| CN107625659B (en) * | 2017-09-04 | 2020-06-26 | 美晨集团股份有限公司 | Whitening toothpaste and preparation method thereof |
| CN108272646A (en) * | 2018-04-11 | 2018-07-13 | 佳木斯大学 | A kind of antibacterial toothpaste and preparation method thereof of hydroxyl apatite |
| CN110403851B (en) * | 2019-08-29 | 2022-03-08 | 无锡青禾小贝科技有限公司 | Anti-allergy toothpaste |
| CN112891234B (en) * | 2019-12-03 | 2022-11-08 | 谭生龙 | Biphase calcium-phosphorus material and toothpaste containing biphase calcium-phosphorus material |
| CN111481453A (en) * | 2020-04-30 | 2020-08-04 | 扬州倍加洁日化有限公司 | Desensitizing oral composition, preparation method and application thereof |
| CN111888304B (en) * | 2020-09-16 | 2021-01-26 | 白银香生物科技有限公司 | Anti-inflammation and anti-allergy toothpaste and preparation method thereof |
| CN113425610A (en) * | 2021-07-19 | 2021-09-24 | 厦门金特康生物科技有限公司 | Toothpaste and preparation method thereof |
| CN114886782B (en) * | 2022-05-07 | 2023-06-16 | 深圳市博威凯特科技有限公司 | Active calcium compound based on nano hydroxyapatite and preparation method and application thereof |
| CN114931540B (en) * | 2022-06-06 | 2023-07-14 | 云南白药集团健康产品有限公司 | Carboxymethyl bagasse-containing composite material and preparation method and application thereof |
| CN114796064B (en) * | 2022-06-06 | 2023-07-18 | 云南白药集团健康产品有限公司 | Bagasse calcium phosphate composite material, and preparation method and application thereof |
| CN115844737A (en) * | 2022-12-31 | 2023-03-28 | 广西信业生物技术有限公司 | Preparation method of bioactive mineral material for repairing enamel calcium |
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| WO2015150011A1 (en) * | 2014-03-31 | 2015-10-08 | Omya International Ag | Surface-reacted calcium carbonate for remineralisation and whitening of teeth |
| CN105640788A (en) * | 2016-01-27 | 2016-06-08 | 杭州皎洁口腔保健用品有限公司 | Hydroxyapatite toothpaste and preparation method thereof |
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| WO2015150011A1 (en) * | 2014-03-31 | 2015-10-08 | Omya International Ag | Surface-reacted calcium carbonate for remineralisation and whitening of teeth |
| CN105640788A (en) * | 2016-01-27 | 2016-06-08 | 杭州皎洁口腔保健用品有限公司 | Hydroxyapatite toothpaste and preparation method thereof |
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Address after: 311305 building 3, 268 Dakang Road, Qingshanhu science and Technology City, Lin'an District, Hangzhou City, Zhejiang Province Patentee after: HANGZHOU JIAOJIE ORAL HEALTH CARE PRODUCTS Co.,Ltd. Address before: Building 15, No. 2, Huafeng Road, Shiqiao Street, Xiacheng District, Hangzhou, Zhejiang 310022 Patentee before: HANGZHOU JIAOJIE ORAL HEALTH CARE PRODUCTS Co.,Ltd. |