CN1714864A - Nano grade polypeptide anti-dental caries material and producing method and tooth-paste containing said material - Google Patents
Nano grade polypeptide anti-dental caries material and producing method and tooth-paste containing said material Download PDFInfo
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- CN1714864A CN1714864A CN 200510035181 CN200510035181A CN1714864A CN 1714864 A CN1714864 A CN 1714864A CN 200510035181 CN200510035181 CN 200510035181 CN 200510035181 A CN200510035181 A CN 200510035181A CN 1714864 A CN1714864 A CN 1714864A
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- hap
- cpp
- toothpaste
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- polypeptide anti
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Abstract
The composite nano microcrystal caries-preventing polypeptide material CPP/HAP is prepared through cross-linking nano microcrystal hydroxyapatite (HAP) and casein peptide phosphate (CPP) in a solution-ultrasonic dispersion process. The caries-preventing polypeptide material has improved use performance of nano microcrystal HAP, raised CPP compatibility, the re-mineralizing performance of CPP and re-depositing performance of HAP, so that it may be used in toothpaste to promote the re-mineralizing of teeth, prevent caries and repair enamel through the synergistic effect of HAP and CPP.
Description
Technical field
The present invention relates to a kind of toothpaste, especially a kind of nanometer anti-caries anti-biotic material and manufacture method thereof that can be used for toothpaste, and the toothpaste that contains described material.
Background technology
Dental caries a kind of chronic progressive external that to be dental hard tissue take place under the combined effect based on the multiple factor of antibacterial destroys disease, the existence that Streptococcus mutans etc. cause the dental caries antibacterial is the essential condition that dental caries takes place, the dental plaque that sticks on the tooth is antibacterial produces dental caries on facing an important oral environment, cariogenicity foods such as sucrose enter bacterial plaque, cariogenic bacteria in the bacterial plaque makes sugar fermentation produce acid, these acid stop for a long time at facing, with the hard tooth tissue dissolved destruction, make it demineralization and produce dental caries.In time remove cariogenic bacteria and dental plaque, regular maintenance oral cavity cleaning health reduces the absorption of cariogenicity food, strengthens the ability of dental surface opposing acid etching, is the requisite measure of control dental caries.
Toothpaste has become the necessary in people's daily life, and along with improving constantly of people's living standard, toothpaste is developed to curative effect-type by the common type that cleans the teeth, and the added medicine of curative effect-type medicated toothpaste mostly is Chinese herbal medicine and fluoride etc. at present.Facts have proved fluorine can with dental hard tissue the main component hydroxyapatite combine, form fluor-apatite, this fluor-apatite is insoluble in acid, can strengthen the ability of tooth opposing acid etching greatly, so fluoride can preventing decayed tooth.But because fluorine itself has suitable toxicity, the consumption of fluorine in toothpaste is subjected to strict restriction, and the absorption of excessive fluoride can cause filemot dental fluorosis, influences the bright and clean and attractive in appearance of dental surface, and serious also can cause fluorosis and skeletal fluorosis.
In view of this, provide a kind of anti-caries anti-biotic material that can be used for toothpaste that addresses the above problem and toothpaste thereof real for necessary.
Summary of the invention
The objective of the invention is to synthetic a kind of nano grade polypeptide anti-caries material, this nano material can promote the surface of damage and etching teeth remineralization, in time repairs bad facing of dental caries, recovers the bright and clean true qualities of whitening of tooth.This material is applied to toothpaste, and is safe and effective, and human body is but had no side effect, and makes toothpaste have good safe anticaries efficacy.
Another object of the present invention is to provide a kind of manufacture method of described nano grade polypeptide anti-caries material.
Another purpose of the present invention is to provide a kind of toothpaste of using described nano grade polypeptide preventing decayed tooth material.
For achieving the above object, the invention provides a kind of nano grade polypeptide anti-caries material, its by hydroxyapatite nano crystallite and phosphopeptide caseinate by crosslinked compound the making of solution-ultrasonic dispersion.
Described nano grade polypeptide anti-caries preparation methods is:
At first, preparation HAP dispersion liquid and CPP solution are dispersed in the HAP nano microcrystalline in the PEG400, form the dispersion liquid of concentration 20%-50%, with the ultrasonic grinding machine handle 10 minutes stand-by; To be scattered in the CPP of HAP identical weight in the propylene glycol, form dispersion liquid with the HAP same concentrations.
Then, under agitation, the HAP dispersion liquid is slowly added in the CPP propylene glycol solution that is under the ultrasound wave effect;
Then, stirred compound about two hours down, cool and isolate solvent, heavy-gravity combination product airing at 150 ℃;
At last, CPP and HAP combination product are carried out vacuum drying 48 hours about 60 ℃, make CPP/HAP polypeptide nano preventing decayed tooth composite.
Wherein, described CPP comprises the phosphoric acid silk acyl group that 4～7 clusters exist, and its core texture is :-Ser (P)-Ser (P)-Ser (P)-Glu-Glu-(Ser: serine, Glu: glutamic acid, P: phosphate).Described phosphopeptide caseinate (CPP) is to be raw material with the bovine casein, with pancreatin or trypsin hydrolyzing casein, through the bioactive polypeptide made from extra care, purification is made of tool.
Described hydroxyapatite (HAP) nano microcrystalline adopts the sol-gel process preparation, is raw material with calcium salt, phosphate, and the mol ratio of control Ca/P is 1.67: 1.
The present invention further provides a kind of nano grade polypeptide anti-caries material toothpaste, comprised the lotion of toothpaste matrix components, described nano grade polypeptide anti-caries material toothpaste also comprises nano grade polypeptide anti-caries material, i.e. CPP/HAP nano grade polypeptide anti-caries material.The percentage by weight of described nano grade polypeptide anti-caries material in described toothpaste is 0.1%-20%.Below sketch the component of described toothpaste by several embodiment.
In one embodiment of the invention, each ingredients constitute total weight percent is in the described nano grade polypeptide anti-caries material toothpaste:
Glycerol 5% sorbitol 15%
CMC 1.0％ K
12 1.8％
CaHPO
4 40％ CPP/HAP 5.0％
Saccharin sodium 0.15% essence 1.2%
The deionized water surplus
In yet another embodiment of the present invention, each ingredients constitute total weight percent is in the described nano grade polypeptide anti-caries material toothpaste:
Glycerol 10% sorbitol 10%
CMC 1.1％ K
12 1.7％
CaCO
3 45％ CPP/HAP 3.0％
Saccharin sodium 0.2% essence 1.1%
The deionized water surplus
In yet another embodiment of the present invention, each ingredients constitute total weight percent is in the described nano grade polypeptide anti-caries material toothpaste:
Propylene glycol 5% sorbitol 20%
CMC 1.1％ K
12 1.8％
SiO
2 15％ CaHPO
4 25％
CPP/HAP 1.5% saccharin sodium 0.1%
Essence 1.0% deionized water surplus
In yet another embodiment of the present invention, each ingredients constitute total weight percent is in the described nano grade polypeptide anti-caries material toothpaste:
Propylene glycol 5% glycerol 10%
Sorbitol 10% CMC 1.2%
K
12 1.9％ SiO
2 5％
CaCO
3 35％ CPP/HAP 1.0％
Saccharin sodium 0.2% essence 1.0%
The deionized water surplus
In the present invention, CPP/HAP nano grade polypeptide anti-caries material, one side has been improved the serviceability of HAP nano microcrystalline, improves the compatibility of CPP; Because CPP itself has the remineralization effect, can impel HAP on the other hand in damaged enamel surface and inner deposition.CPP/HAP nano microcrystalline polypeptide anti-caries composite has compiled the remineralization effect of CPP and the resedimentation of HAP nano microcrystalline, both synergism, be applied in the toothpaste, can dual promotion remineralization of teeth, the effect of multiplication preventing decayed tooth, strengthen greatly for damaged adamantine repairing and anticaries action effect, have the incomparable safe application performance of traditional preventing decayed tooth material fluoride.
The specific embodiment
A kind of nano grade polypeptide anti-caries of the present invention material is by hydroxyapatite (molecular formula: Ca
10(PO
4)
6(OH)
2, being called for short HAP) and nano microcrystalline carries out crosslinked compound making with this natural polypeptides of phosphopeptide caseinate (Casein Phosphopeptides, abbreviation CPP).
Hydroxyapatite (HAP) nano microcrystalline is extremely similar to skeleton structure (comprising adamantine structure), has good biocompatibility, can form firm bonding with osseous tissue, at the attached knot in tooth defect surface, have good remineralization and repair whitening function easily.But the HAP nano microcrystalline of synthetic because easily reunite, intensity is low, fragility is big, has limited its application to a certain extent, therefore, need the serviceability of HAP nano microcrystalline is improved.
Phosphopeptide caseinate (CPP) is a kind of natural polypeptides that extracts from milk; has physiologically active; the CPP molecule is made up of 20 to thirties amino acid residues; phosphoric acid silk acyl group comprising 4～7 clusters existence; its core texture is :-Ser (P)-Ser (P)-Ser (P)-Glu-Glu-(Ser: serine; Glu: glutamic acid, P: phosphoric acid).Discover that the CPP physiologically active shows that its unique texture can promote the absorption of human body to calcium, can promote damaged property enamel to mineralize again, calcium ion is combined in the dental caries place, thereby reaches anti-dental caries purpose.CPP is to the increasing experiment confirm of the adamantine remineralization effect quilt of damaged property, but find that also the remineralization effect of CPP is subjected to the influence of PH environment, can only promote the absorption of reactive amorphous calcium, if technology makes an addition to toothpaste with CPP routinely, the compatibility of CPP and other components of toothpaste is bad, and CPP loses activity easily.
CPP/HAP nano grade polypeptide anti-caries material of the present invention can adopt the preparation of solution-ultrasonic dispersion, but this nano material that is applied to toothpaste is not limited to this preparation method.Below further describe this preparation method.
The precursor of CPP/HAP polypeptide nano preventing decayed tooth composite comprises the nano microcrystalline of CPP and HAP.Wherein, described phosphopeptide caseinate (CPP) is to be raw material with the bovine casein, by biotechnology, and with pancreatin or trypsin hydrolyzing casein, the bioactive polypeptide of making through refining, purification of tool.Hydroxyapatite (HAP) nano microcrystalline can adopt the sol-gel process preparation, is raw material with calcium salt, phosphate, and the mol ratio of control Ca/P is 1.67: 1 in aqueous solution, with NH
4The pH value of OH control solution can make the HAP nano microcrystalline greater than 10.
In the present invention, Ca
2+Derive from lime nitrate, calcium chloride, calcium oxide or their mixture; PO4
3-Derive from dipotassium hydrogen phosphate, sodium hydrogen phosphate, diammonium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, Ammonium biphosphate, phosphoric acid, potassium phosphate, sodium phosphate, ammonium phosphate; OH
-Derive from calcium hydroxide, sodium hydroxide, potassium hydroxide.
The method for making of nano grade polypeptide anti-caries material of the present invention is below described:
1) preparation HAP dispersion liquid; The HAP nano microcrystalline is dispersed in the PEG400, forms the dispersion liquid of concentration 20%-50%, with the ultrasonic grinding machine handle 10 minutes stand-by;
2) preparation CPP solution; To be scattered in the CPP of HAP identical weight in the propylene glycol, form dispersion liquid with the HAP same concentrations;
3) under agitation, the HAP dispersion liquid is slowly added in the CPP propylene glycol solution that is under the ultrasound wave effect;
4) stirred compound about two hours down at 150 ℃, cool and isolate solvent, heavy-gravity combination product airing;
5) CPP and HAP combination product are carried out vacuum drying 48 hours about 60 ℃, make CPP/HAP polypeptide nano preventing decayed tooth composite.
Mastic matrix components in the toothpaste generally includes and mixes wetting agent, binding agent, abrasivus, foaming agent, sweeting agent, flavouring agent, functional agent and the deionized water of forming etc. by a certain percentage.In the present invention, described wetting agent can be glycerol, sorbitol, propylene glycol, diethylene glycol or Polyethylene Glycol, and described several wetting agents can be singly with also can severally being used in combination.Described binding agent can be sodium carboxymethyl cellulose, hydroxyethyl-cellulose, carrageenan or HANSHENGJIAO, and described several binding agents can singly be used, and also can severally be used in combination.Described abrasivus is calcium carbonate, calcium bicarbonate or silicon dioxide, described several abrasivuss can be singly with or several being used in combination.Described foaming agent is generally sodium lauryl sulphate.Described sweeting agent can be saccharin sodium.Described flavouring agent is an essence.
The functional agent of nano grade polypeptide anti-caries toothpaste of the present invention is a CPP/HAP nano grade polypeptide anti-caries material, can be added in the toothpaste with technology according to a conventional method, and addition is 0.1%-20% (by weight percentage).
Further set forth the component prescription of described nano grade polypeptide anti-caries toothpaste below in conjunction with several specific embodiments.
Example one
Contain described in the present embodiment that the shared total weight percent of each component is in the toothpaste of nano grade polypeptide anti-caries material:
Glycerol 5% sorbitol 15%
CMC 1.0％ K
12 1.8％
CaHPO
4 40％ CPP/HAP 5.0％
Saccharin sodium 0.15% essence 1.2%
The deionized water surplus
Example two
Contain described in the present embodiment that the shared total weight percent of each component is in the toothpaste of nano grade polypeptide anti-caries material:
Glycerol 10% sorbitol 10%
CMC 1.1％ K
12 1.7％
CaCO
3 45％ CPP/HAP 3.0％
Saccharin sodium 0.2% essence 1.1%
The deionized water surplus
Example three
Contain described in the present embodiment that the shared total weight percent of each component is in the toothpaste of nano grade polypeptide anti-caries material:
Propylene glycol 5% sorbitol 20%
CMC 1.1％ K
12 1.8％
SiO
2 15％ CaHPO
4 25％
CPP/HAP 1.5% saccharin sodium 0.1%
Essence 1.0% deionized water surplus
Example four
Close described in the present embodiment that the shared total weight percent of each component is in the toothpaste of nano grade polypeptide anti-caries material:
Propylene glycol 5% glycerol 10%
Sorbitol 10% CMC 1.2%
K
12 1.9％ SiO
2 5％
CaCO
3 35％ CPP/HAP 1.0％
Saccharin sodium 0.2% essence 1.0%
The deionized water surplus
In the present invention, meter level polypeptide anti-caries material in the CPP/HAP, one side has been improved the serviceability of HAP nano microcrystalline, improves the compatibility of CPP; Because CPP itself has the remineralization effect, can impel HAP on the other hand in damaged enamel surface and inner deposition.CPP/HAP nano microcrystalline polypeptide anti-caries composite has compiled the remineralization effect of CPP and the resedimentation of HAP nano microcrystalline, both synergism, be applied in the toothpaste, can dual promotion remineralization of teeth, the effect of multiplication preventing decayed tooth, strengthen greatly for damaged adamantine repairing and anticaries action effect, have the incomparable safe application performance of traditional preventing decayed tooth material fluoride.
Above disclosedly only be the preferred embodiment of nano grade polypeptide anti-caries material of the present invention, can not limit the present invention's interest field certainly with this, therefore the equivalent variations of being done according to the present patent application claim still belongs to the scope that the present invention is contained.
Claims (10)
1. nano grade polypeptide anti-caries material is characterized in that: it carries out crosslinked compound making by hydroxyapatite nano crystallite (HAP) and phosphopeptide caseinate (CPP).
2. the nano grade polypeptide anti-caries material of stating as claim 1, it is characterized in that: described nano grade polypeptide anti-caries material is prepared from by solution-ultrasonic dispersion, and its preparation method is:
At first, preparation HAP dispersion liquid and CPP solution are dispersed in the HAP nano microcrystalline in the PEG400, form the dispersion liquid of concentration 20%-50%, with the ultrasonic grinding machine handle 10 minutes stand-by; To be scattered in the CPP of HAP identical weight in the propylene glycol, form dispersion liquid with the HAP same concentrations.
Then, under agitation, the HAP dispersion liquid is slowly added in the CPP propylene glycol solution that is under the ultrasound wave effect;
Then, stirred compound about two hours down, cool and isolate solvent, heavy-gravity combination product airing at 150 ℃;
At last, CPP and HAP combination product are carried out vacuum drying 48 hours about 60 ℃, make CPP/HAP polypeptide nano preventing decayed tooth composite.
3. nano grade polypeptide anti-caries material as claimed in claim 1 or 2; it is characterized in that: described phosphopeptide caseinate (CPP) comprises the phosphoric acid silk acyl group that 4～7 clusters exist; its core texture is :-Ser (P)-Ser (P)-Ser (P)-Glu-Glu-(Ser: serine; Glu: glutamic acid, P: phosphate).
4. nano grade polypeptide anti-caries material as claimed in claim 1 or 2 is characterized in that: described hydroxyapatite nano crystallite (HAP) adopts sol-gel processing synthetic.
5. a nano grade polypeptide anti-caries material toothpaste comprises the lotion of toothpaste matrix components, it is characterized in that: described nano grade polypeptide anti-caries material toothpaste also comprises nano grade polypeptide anti-caries material, i.e. CPP/HAP nano grade polypeptide anti-caries material.
6. nano grade polypeptide anti-caries material toothpaste as claimed in claim 5 is characterized in that: the percentage by weight of described nano grade polypeptide anti-caries material in described toothpaste is 0.1%-20%.
7. nano grade polypeptide anti-caries material toothpaste as claimed in claim 5, it is characterized in that: the shared total weight percent of each component is in the described toothpaste:
Glycerol 5% sorbitol 15%
CMC 1.0％ K
12 1.8％
CaHPO
4 40％ CPP/HAP 5.0％
Saccharin sodium 0.15% essence 1.2%
The deionized water surplus.
8. nano grade polypeptide anti-caries material toothpaste as claimed in claim 5, it is characterized in that: the shared total weight percent of each component is in the described toothpaste:
Glycerol 10% sorbitol 10%
CMC 1.1％ K
12 1.7％
CaCO
3 45％ CPP/HAP 3.0％
Saccharin sodium 0.2% essence 1.1%
The deionized water surplus.
9. nano grade polypeptide anti-caries material toothpaste as claimed in claim 5, it is characterized in that: the shared total weight percent of each component is in the described toothpaste:
Propylene glycol 5% sorbitol 20%
CMC 1.1％ K
12 1.8％
SiO
2 15％ CaHPO
4 25％
CPP/HAP 1.5% saccharin sodium 0.1%
Essence 1.0% deionized water surplus.
10. nano grade polypeptide anti-caries material toothpaste as claimed in claim 5, it is characterized in that: the shared total weight percent of each component is in the described toothpaste:
Propylene glycol 5% glycerol 10%
Sorbitol 10% CMC 1.2%
K
12 1.9％ SiO
2 5％
CaCO
3 35％ CPP/HAP 1.0％
Saccharin sodium 0.2% essence 1.0%
The deionized water surplus.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100351812A CN100469389C (en) | 2005-06-15 | 2005-06-15 | Nano grade polypeptide anti-dental caries material and producing method and tooth-paste containing said material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100351812A CN100469389C (en) | 2005-06-15 | 2005-06-15 | Nano grade polypeptide anti-dental caries material and producing method and tooth-paste containing said material |
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| Publication Number | Publication Date |
|---|---|
| CN1714864A true CN1714864A (en) | 2006-01-04 |
| CN100469389C CN100469389C (en) | 2009-03-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITNA20110016A1 (en) * | 2011-03-24 | 2012-09-25 | Francesco Addeo | PREPARATION OF A PRODUCT CONSISTING OF IMMOBILIZED PHOSPHOPEPTIDES ON HYDROXYAPATITIS FOR NUTRACEUTICAL AND (OTHER) INNOVATIVE AIMS |
| CN103096866A (en) * | 2010-03-19 | 2013-05-08 | 墨尔本大学 | Kit and method for detecting porous dental hydroxy apatite |
| CN107411975A (en) * | 2017-03-28 | 2017-12-01 | 常州大学 | A kind of preparation method of carious tooth filling patching material |
| CN107715172A (en) * | 2017-11-08 | 2018-02-23 | 江苏华友装饰工程有限公司 | A kind of preparation method of bone bionic composite material |
| CN113456521A (en) * | 2021-09-01 | 2021-10-01 | 中国人民解放军总医院第一医学中心 | Oral care composition containing peptide and preparation method thereof |
| CN115778838A (en) * | 2022-12-23 | 2023-03-14 | 重庆登康口腔护理用品股份有限公司 | Enhanced-effect oral care composition, application thereof and oral care product containing composition |
-
2005
- 2005-06-15 CN CNB2005100351812A patent/CN100469389C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103096866A (en) * | 2010-03-19 | 2013-05-08 | 墨尔本大学 | Kit and method for detecting porous dental hydroxy apatite |
| CN103096866B (en) * | 2010-03-19 | 2016-07-06 | 先锋技术有限责任公司 | The detection method of porous dental hydroxy apatite and test kit |
| US11400027B2 (en) | 2010-03-19 | 2022-08-02 | Incisive Technologies Pty Ltd | Kit and method for detecting porous dental hydroxyapatite |
| ITNA20110016A1 (en) * | 2011-03-24 | 2012-09-25 | Francesco Addeo | PREPARATION OF A PRODUCT CONSISTING OF IMMOBILIZED PHOSPHOPEPTIDES ON HYDROXYAPATITIS FOR NUTRACEUTICAL AND (OTHER) INNOVATIVE AIMS |
| CN107411975A (en) * | 2017-03-28 | 2017-12-01 | 常州大学 | A kind of preparation method of carious tooth filling patching material |
| CN107715172A (en) * | 2017-11-08 | 2018-02-23 | 江苏华友装饰工程有限公司 | A kind of preparation method of bone bionic composite material |
| CN113456521A (en) * | 2021-09-01 | 2021-10-01 | 中国人民解放军总医院第一医学中心 | Oral care composition containing peptide and preparation method thereof |
| CN115778838A (en) * | 2022-12-23 | 2023-03-14 | 重庆登康口腔护理用品股份有限公司 | Enhanced-effect oral care composition, application thereof and oral care product containing composition |
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| Publication number | Publication date |
|---|---|
| CN100469389C (en) | 2009-03-18 |
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