HK1138180B - Recalcification promoter and composition for oral cavity - Google Patents
Recalcification promoter and composition for oral cavity Download PDFInfo
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- HK1138180B HK1138180B HK10103393.5A HK10103393A HK1138180B HK 1138180 B HK1138180 B HK 1138180B HK 10103393 A HK10103393 A HK 10103393A HK 1138180 B HK1138180 B HK 1138180B
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Description
Technical Field
The present invention relates to an agent for promoting recalcification of dental enamel and an oral composition.
Background
Dental caries is caused by the formation of tartar due to the adhesion of dental caries bacteria to the tooth surface, and calcium and phosphorus are dissolved out from the right below of the tooth surface by the acid generated by the dental caries bacteria metabolizing food in tartar, so that the enamel is decalcified to form an initial dental caries state. Saliva has a function of recalcifying the decalcified portion by the action of calcium and phosphorus in the saliva to restore the original shape of the teeth. In addition, in order to promote recalcification, a dentifrice in which one of fluoride and calcium phosphate is blended with hydroxyapatite fine particles having a crystal structure similar to that of an inorganic component of a tooth is produced.
However, recalcification of the decalcified portion is insufficient if only saliva, fluoride, hydroxyapatite dentifrice is used. In addition, although chewing gums prepared by blending xylitol with calcium phosphate or calcium oligo-phosphate (calcium phosphate) have been produced to promote recalcification, recalcification of the decalcified portion is not sufficient when using chewing gums blended with xylitol or various calcium phosphates.
Therefore, research on improving the caries effect of hydroxyapatite is carried out, and the following proposals are proposed: an oral cavity dentifrice which can improve the effects of restoration, protection, prevention of caries, strengthening of dentin and whitening of fine irregularities on the tooth surface by blending hydroxyapatite having a particle diameter of 0.05 to 1.0 μm (see patent document 1); an oral composition containing low-crystalline hydroxyapatite and capable of preventing diseases and discomfort in the oral cavity by adsorbing the composition to bacteria in the oral cavity and removing bacteria (see patent document 2); 3DS household care (home care) agents for caries elimination, which contain low-crystalline or amorphous hydroxyapatite (see patent document 3).
Patent document 1: japanese laid-open patent publication No. 9-202717
Patent document 2: japanese patent laid-open No. 2001-122748
Patent document 3: japanese patent laid-open publication No. 2004-35416
Disclosure of Invention
Hydroxyapatite is generally known to promote recalcification of enamel, and is also described in patent documents 1 to 3, but it is not known that the recalcification effect of enamel shows a significant difference depending on the crystallinity of hydroxyapatite.
The present invention addresses the problem of providing an agent for promoting recalcification of tooth enamel which is extremely effective in promoting the recalcification of tooth enamel and positively suppressing dental caries, and an oral composition.
It is known that a low-crystalline hydroxyapatite can be obtained by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at a low temperature of 100 ℃ or lower, but a difference in function is not considered among hydroxyapatite such as low-crystalline hydroxyapatite, and it is considered that the difference in function is not so large. And in practical cases, from the viewpoint of drying time (production efficiency), drying is performed at 100 ℃.
However, the present inventors have surprisingly found that, without being limited by the production efficiency, when hydroxyapatite (amorphous hydroxyapatite) is produced by drying at a temperature lower than 100 ℃, such as room temperature to 70 ℃, and the function thereof is examined, the amorphous hydroxyapatite can dramatically promote recalcification of enamel, as compared with high-crystalline hydroxyapatite and low-crystalline hydroxyapatite obtained by drying at 100 ℃, and thus completed the present invention.
Namely, the present invention relates to: (1) an agent for promoting recalcification of enamel, which is characterized by containing amorphous hydroxyapatite and/or amorphous hydroxyapatite; (2) the agent for promoting recalcification of enamel according to the above (1), wherein the amorphous hydroxyapatite is a hydroxyapatite showing two peaks at 2 θ of 31 to 35 ° in X-ray diffraction; (3) the agent for promoting recalcification of enamel according to (2) above, wherein the amorphous hydroxyapatite is a hydroxyapatite showing an X-ray diffraction pattern shown in FIG. 2; (4) the accelerator for recalcification of enamel according to any one of (1) to (3), wherein the amorphous hydroxyapatite is a hydroxyapatite obtained by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at 10 to 70 ℃.
In addition, the present invention relates to: (5) an oral composition characterized by containing amorphous hydroxyapatite and/or amorphous hydroxyapatite; (6) the oral composition according to the above (5), wherein the amorphous hydroxyapatite is a hydroxyapatite showing two peaks at an X-ray diffraction 2 θ of 31 to 35 °; (7) the oral composition according to item (6) above, wherein the amorphous hydroxyapatite is hydroxyapatite showing an X-ray diffraction pattern shown in FIG. 2; (8) the oral composition according to any one of the above (5) to (7), wherein the amorphous hydroxyapatite is a hydroxyapatite obtained by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at 10 to 70 ℃; (9) the oral composition according to any one of the above (5) to (8), wherein the content of amorphous hydroxyapatite and/or amorphous hydroxyapatite is 0.01 to 50% by weight; (10) the oral composition according to any one of the above (5) to (9), wherein the composition is a dentifrice, a mouthwash or a chewing gum.
According to the agent for promoting recalcification of enamel and the composition for oral cavity of the present invention, recalcification of enamel can be promoted extremely effectively and dental caries can be suppressed positively.
Drawings
Figure 1 is an X-ray diffraction pattern of an amorphous hydroxyapatite powder of the invention (dried at 60 ℃).
Fig. 2 is an X-ray diffraction pattern of an amorphous hydroxyapatite powder (freeze-dried) according to the present invention.
Fig. 3 is an X-ray diffraction pattern of a low crystalline hydroxyapatite powder (dried at 100 ℃).
FIG. 4 is an X-ray diffraction pattern of a highly crystalline hydroxyapatite powder (calcined at 800 ℃ C.)
Fig. 5 is a photograph of the crown portion control surface and the treated surface, which is represented by a Contact Micrograph (CMR).
Fig. 6 is an explanatory view of the photograph shown in fig. 5.
Detailed Description
The agent for promoting recalcification of enamel and the composition for oral cavity of the present invention are not particularly limited as long as they contain amorphous hydroxyapatite and/or amorphous hydroxyapatite, and can more effectively promote recalcification of enamel than a composition containing highly crystalline hydroxyapatite and low crystalline hydroxyapatite obtained by drying at 100 ℃.
Hydroxyapatite is usually expressed in Ca10(PO4)6(OH)2The stoichiometric composition of (a) shows a feature that even when the molar ratio of Ca/P is not 1.67, the property of hydroxyapatite is exhibited and an apatite structure is obtained. The Ca/P molar ratio of hydroxyapatite can be controlled by controlling the mixing ratio of the salts of the raw materials and the synthesis conditions. For example, in the wet synthesis method of hydroxyapatite, if the aqueous solution is made alkaline with ammonia water or the like at the time of synthesis, the Ca/P molar ratio is increased; on the other hand, if the aqueous solution is made neutral or weakly acidic with a dilute acid, the Ca/P molar ratio can be lowered. In the enamel recalcification promoter and the oral composition of the present invention, hydroxyapatite having both stoichiometric composition and non-stoichiometric composition can be used, and hydroxyapatite having a Ca/P molar ratio of 1.56 to 1.68 can be used.
The X-ray diffraction pattern of the amorphous hydroxyapatite powder of the present invention (dried at 60 ℃) is shown in fig. 1, and the X-ray diffraction pattern of the amorphous hydroxyapatite powder of the present invention (freeze-dried) is shown in fig. 2. In addition, as a comparison, figure 3 shows the low crystalline hydroxyapatite powder (at 100 degrees C drying) X-ray diffraction pattern, figure 4 shows the high crystalline hydroxyapatite powder (at 800 degrees C calcination) X-ray diffraction pattern. An X-ray diffraction apparatus (MXP18VAHF) (manufactured by KOKAI マツクサイエンス) was used for the measurement.
As shown in fig. 4, the highly crystalline hydroxyapatite was completely separated into four peaks at a peak 2 θ of 31 to 35 °, indicating high crystallinity. As shown in fig. 3, among the four peaks, two peaks near 31 to 33 ° 2 θ of the low-crystalline hydroxyapatite overlap each other and are not completely separated, indicating that the crystallinity is low. As shown in fig. 1, the peak of the amorphous hydroxyapatite of the present invention in the vicinity of 31 to 35 ° 2 θ is a broad peak, indicating that the hydroxyapatite is amorphous, as compared to these X-ray diffraction patterns. As shown in fig. 2, the three peaks of the amorphous hydroxyapatite of the present invention near 31 to 34 ° 2 θ overlap each other, indicating that the hydroxyapatite is substantially amorphous (amorphized) although low crystallization is started.
That is, the dry amorphous hydroxyapatite of the present invention shows one broad peak at 2 θ of 31 to 35 ° in X-ray diffraction, and the dry amorphous apatite of the present invention shows two peaks at 2 θ of 31 to 35 ° in X-ray diffraction.
As described above, unlike crystalline hydroxyapatite, amorphous hydroxyapatite and amorphous hydroxyapatite according to the present invention are not hydroxyapatite having a complete crystal structure, but have a structure that exhibits a weak diffraction degree even in an X-ray diffraction pattern. Further, the amorphous hydroxyapatite and the amorphous hydroxyapatite of the present invention have a specific surface area of 60m by the BET method2And about/g.
The amorphous hydroxyapatite and the method for producing an amorphous hydroxyapatite according to the present invention are not particularly limited as long as they can be produced by a method for producing a hydroxyapatite showing the X-ray diffraction pattern, and for example, they can be produced by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at a predetermined temperature. The reaction of the calcium salt and the phosphate can be carried out, for example, by keeping a mixed solution of the calcium salt and the phosphate at room temperature for 2 to 3 days. Examples of the calcium salt include common calcium salts such as calcium hydroxide, calcium acetate, calcium carbonate, calcium chloride, calcium citrate, and calcium lactate; examples of the phosphate include common phosphates such as phosphoric acid, ammonium phosphate, sodium phosphate, potassium phosphate, pyrophosphoric acid, and sodium hexametaphosphate.
The amorphous hydroxyapatite of the present invention may be, for example, a suspension (reaction solution) within one week after preparation and a dried product obtained by freeze-drying the suspension, and the freeze-drying is usually performed within one week, preferably within 3 days, from the preparation of the suspension, depending on the solution temperature and storage temperature at the time of production.
The amorphous hydroxyapatite of the present invention may be, for example, a suspension (reaction solution) which is prepared and then stored for more than one week, or a dried product obtained by drying the prepared suspension at a temperature of 10 to 70 ℃, preferably 40 to 70 ℃, or the prepared suspension may be stored at room temperature or lower for a long period of time and then dried. Therefore, the method is easy to manufacture and store, and is suitable for industrialization.
The amorphous hydroxyapatite can be obtained by mechanically finely pulverizing a low-crystalline hydroxyapatite powder or a suspension thereof. The mechanical micro-pulverization can be carried out by using a bead mill, a sand mill, a high-speed impact pulverizer, or a high-pressure wet micronizing device. Examples of the bead mills and sand mills include ビスコミル available from アイメツクス (manufactured by LTD), グレンミル available from Seikagaku corporation, (ダイノミル available from LTD シンマルエンタ - プライゼス), アニラ - ミル available from Mitsui mine (manufactured by LTD アニラ - ミル), sand mills available from Tokuai industries (manufactured by LTD コトブキ), and the like; examples of the high-speed impact mill include みづほ industrial ultrahigh-pressure homogenizer (homogenerizer); examples of the high-pressure wet type micronizing apparatus include ナノマイザ available from ナノマイザ Kabushiki Kaisha and a micronizing apparatus available from スギノマシン Kabushiki Kaisha. In addition, when wet grinding is performed, the hydroxyapatite may be dried at 10 to 70 ℃, preferably 40 to 70 ℃, and the X-ray diffraction pattern of the powder is the same as that shown in fig. 2.
The recalcification accelerator of the present invention contains amorphous hydroxyapatite and amorphous hydroxyapatite in an amount of, for example, 50 to 100 wt%, preferably 75 to 100 wt%, and more preferably 80 to 99 wt% of the total amount of the compounding ingredients. The content of the amorphous hydroxyapatite and the amorphized hydroxyapatite in the oral composition of the present invention is, for example, 0.01 to 50% by weight, preferably 0.1 to 30% by weight of the total composition, from the viewpoints of caries prevention effect, production cost, and feeling of use.
The recalcification promoter and the oral composition of the present invention may contain, in addition to amorphous hydroxyapatite and amorphous hydroxyapatite, a polishing agent, a humectant, a foaming agent, a thickener, a preservative, a flavor, a sweetener, various medicinal components, and the like, which are commonly used additives, in the oral composition. Specific examples of these components are shown below. The amount of these optional components may be appropriately used within a pharmaceutically acceptable range without impairing the effect of the present invention.
Grinding agent: calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate, tricalcium phosphate, silica, aluminum silicate, aluminum hydroxide, alumina, zeolite, titanium oxide, zirconium silicate, and the like.
Wetting agent: glycerin, propylene glycol, polyethylene glycol, sorbitol, xylitol, and the like.
Foaming agent: sodium lauryl sulfate, sodium N-lauroyl sarcosinate, nonionic surfactants, and the like.
Thickening agent: hydroxyethyl cellulose, sodium carboxymethyl cellulose, carrageenan (carrageenan), carboxyvinyl polymers, xanthan gum (xanthan gum), gelatin, pullulan, sodium alginate, and the like.
Preservative: parabens, alkyldiaminoethyl glycinate hydrochloride, methylparaben, ethylparaben, sodium benzoate, and the like.
Spice: menthol, peppermint oil, lemon oil, eucalyptus oil, and the like.
A sweetening agent: saccharin sodium, stevia extract, aspartame, etc.
Other effective components: allantoin, tocopheryl acetate, isopropyl phenol, beta-glycyrrhetinic acid, triclosan, chlorhexidine, dextranase, chlorophyll, flavonoids, tranexamic acid, hinokitiol, and the like.
Specific examples of the oral composition of the present invention include: dentifrices such as toothpaste, tooth powder, liquid toothpaste, mouth wash, chewing gum, etc.
In the production of the recalcification accelerator and the oral composition of the present invention, amorphous hydroxyapatite, and other additives may be added in any process of the production process. The oral composition of the present invention may be prepared by blending the recalcification promoter of the present invention.
Examples
Hereinafter, examples and test examples of the present invention will be described, and examples used as recalcification tests are described in the following examples, but the scope of the present invention is not limited thereto.
(preparation of amorphous hydroxyapatite)
A phosphate solution was added dropwise to a calcium hydroxide solution being stirred, the mixed solution was stored at room temperature for 3 days, and the suspension was freeze-dried to obtain amorphous hydroxyapatite. The amorphous hydroxyapatite thus obtained had a maximum particle diameter of about 0.8 μm, a minimum particle diameter of about 0.03 μm and an average particle diameter of about 0.08. mu.m. The particle size was measured using an マイクロトラツク 7340UPA particle size distribution meter (manufactured by Nikkiso Co., Ltd.). Further, the X-ray diffraction pattern thereof is shown in FIG. 1.
(preparation of amorphous hydroxyapatite)
A phosphate solution was added dropwise to a calcium hydroxide solution under stirring, the mixed solution was stored at room temperature for 3 days, and the suspension was air-dried at 60 ℃ for 24 hours to obtain amorphous hydroxyapatite. The maximum particle size of the resulting amorphous hydroxyapatite was about 0.8 μm, the minimum particle size was about 0.03 μm, and the average particle size was about 0.08. mu.m. The X-ray diffraction pattern is shown in FIG. 2.
(preparation of Low-crystalline hydroxyapatite)
The suspension obtained above was dried at 100 ℃ for 2 hours to obtain low-crystalline hydroxyapatite. The obtained low-crystalline hydroxyapatite had a maximum particle diameter of about 10 μm, a minimum particle diameter of about 0.05 μm, and an average particle diameter of about 1.2. mu.m. The X-ray diffraction pattern is shown in FIG. 3.
(preparation of highly crystalline hydroxyapatite)
And calcining a part of the obtained low-crystallinity hydroxyapatite in air at 800 ℃ for 2 hours to obtain the high-crystallinity hydroxyapatite. The obtained highly crystalline hydroxyapatite had a maximum particle diameter of about 40 μm, a minimum particle diameter of about 0.1 μm, and an average particle diameter of about 3.7. mu.m. The X-ray diffraction pattern is shown in FIG. 4.
(production of oral composition for examples and comparative examples)
Dentifrices, mouthwashes, and chewing gums having the following compositions were manufactured according to a conventional method. Examples 1 to 12 are dentifrices, examples 13 to 20 are mouthwashes, and examples 21 to 30 are chewing gums. Examples 1 to 6, examples 13 to 16, and examples 21 to 25 are examples using amorphous hydroxyapatite; examples 7 to 12, examples 17 to 20 and examples 26 to 30 are examples using amorphous hydroxyapatite. In the comparative examples, comparative examples 1 to 12 are dentifrices, comparative examples 13 to 20 are mouthwashes, and comparative examples 21 to 30 are chewing gums. Among them, comparative examples 1 to 6, comparative examples 13 to 16, and comparative examples 21 to 25 are examples using low crystalline hydroxyapatite; comparative examples 7 to 12, comparative examples 17 to 20, and comparative examples 26 to 30 are examples using highly crystalline hydroxyapatite.
[ Table 1]
Tooth cleaning agent
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Amorphous hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 30.0 | 50.0 |
| Glycerol | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 |
| Polyethylene glycol | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Xanthan gum | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Hydroxyethyl cellulose | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Menthol | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 2]
Tooth cleaning agent
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | |
| Amorphous hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 30.0 | 50.0 |
| Glycerol | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 |
| Polyethylene glycol | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Xanthan gum | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Hydroxyethyl cellulose | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Menthol | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 3]
Tooth cleaning agent
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Low crystalline hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 30.0 | 50.0 |
| Glycerol | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 |
| Polyethylene glycol | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Xanthan gum | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Hydroxyethyl cellulose | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Menthol | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 4]
Tooth cleaning agent
| Comparative example 7 | Comparative example 8 | Comparative example 9 | Comparative example 10 | Comparative example 11 | Comparative example 12 | |
| High crystalline hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 30.0 | 50.0 |
| Glycerol | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 | 20.0 |
| Polyethylene glycol | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Xanthan gum | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Hydroxyethyl cellulose | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Menthol | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 5]
Gargle
| Example 13 | Example 14 | Example 15 | Example 16 | |
| Amorphous hydroxyapatite | 0.001 | 0.01 | 0.1 | 2.0 |
| Ethanol | 10.0 | 10.0 | 10.0 | 10.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 |
| Glycerol | 10.0 | 10.0 | 10.0 | 10.0 |
| Menthol | 0.4 | 0.4 | 0.4 | 0.4 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 6]
Gargle
| Example 17 | Example 18 | Example 19 | Example 20 | |
| Amorphous hydroxyapatite | 0.001 | 0.01 | 0.1 | 2.0 |
| Ethanol | 10.0 | 10.0 | 10.0 | 10.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 |
| Glycerol | 10.0 | 10.0 | 10.0 | 10.0 |
| Menthol | 0.4 | 0.4 | 0.4 | 0.4 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 7]
Gargle
| Comparative example 13 | Comparative example 14 | Comparative example 15 | Comparative example 16 | |
| Low crystalline hydroxyapatite | 0.001 | 0.01 | 0.1 | 2.0 |
| Ethanol | 10.0 | 10.0 | 10.0 | 10.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 |
| Glycerol | 10.0 | 10.0 | 10.0 | 10.0 |
| Menthol | 0.4 | 0.4 | 0.4 | 0.4 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 8]
Gargle
| Comparative example 17 | Comparative example 18 | Comparative example 19 | Comparative example 20 | |
| High crystalline hydroxyapatite | 0.001 | 0.01 | 0.1 | 2.0 |
| Ethanol | 10.0 | 10.0 | 10.0 | 10.0 |
| Sodium dodecyl sulfate | 1.0 | 1.0 | 1.0 | 1.0 |
| Glycerol | 10.0 | 10.0 | 10.0 | 10.0 |
| Menthol | 0.4 | 0.4 | 0.4 | 0.4 |
| Purified water | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 9]
Chewing gum
| Example 21 | Example 22 | Example 23 | Example 24 | Example 25 | |
| Amorphous hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 20.0 |
| Rubber base (gum base) | 28.0 | 28.0 | 28.0 | 28.0 | 28.0 |
| Xylitol, its preparation method and use | 30.0 | 30.0 | 30.0 | 25.0 | 25.0 |
| Isomalt (パラチニツト, palatinit) | 21.0 | 21.0 | 21.0 | 10.0 | 10.0 |
| Maltitol | 3.8 | 3.8 | 3.8 | 3.8 | 3.8 |
| Softening agent | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Perfume | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Reducing maltose syrup | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 10]
Chewing gum
| Example 26 | Example 27 | Example 28 | Example 29 | Example 30 | |
| Amorphous hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 20.0 |
| Glue matrix | 28.0 | 28.0 | 28.0 | 28.0 | 28.0 |
| Xylitol, its preparation method and use | 30.0 | 30.0 | 30.0 | 25.0 | 25.0 |
| Isomalt (パラチニツト) | 21.0 | 21.0 | 21.0 | 10.0 | 10.0 |
| Maltitol | 3.8 | 3.8 | 3.8 | 3.8 | 3.8 |
| Softening agent | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Perfume | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Reducing maltose syrup | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 11]
Chewing gum
| Comparative example 21 | Comparative example 22 | Comparative example 23 | Comparative example 24 | Comparative example 25 | |
| Low crystalline hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 20.0 |
| Glue matrix | 28.0 | 28.0 | 28.0 | 28.0 | 28.0 |
| Xylitol, its preparation method and use | 30.0 | 30.0 | 30.0 | 25.0 | 25.0 |
| Isomalt (パラチニツト) | 21.0 | 21.0 | 21.0 | 10.0 | 10.0 |
| Maltitol | 3.8 | 3.8 | 3.8 | 3.8 | 3.8 |
| SoftAgent for chemical treatment | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Perfume | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Reducing maltose syrup | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ Table 12]
Chewing gum
| Comparative example 26 | Comparative example 27 | Comparative example 28 | Comparative example 29 | Comparative example 30 | |
| High crystalline hydroxyapatite | 0.1 | 1.0 | 5.0 | 10.0 | 20.0 |
| Glue matrix | 28.0 | 28.0 | 28.0 | 28.0 | 28.0 |
| Xylitol, its preparation method and use | 30.0 | 30.0 | 30.0 | 25.0 | 25.0 |
| Isomalt (パラチニツト) | 21.0 | 21.0 | 21.0 | 10.0 | 10.0 |
| Maltitol | 3.8 | 3.8 | 3.8 | 3.8 | 3.8 |
| Softening agent | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Perfume | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Reducing maltose syrup | The remaining part | The remaining part | The remaining part | The remaining part | The remaining part |
| Meter | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
[ recalcification promotion test ]
The recalcification promoting effect was confirmed by using a previously prepared artificial incipient caries test specimen. The artificial early caries test sample is prepared by the following method: after removing dirt and deposits on the enamel surface by removing the crown part of a tooth using a person who has not undergone dental preservation or repair treatment, a window of 3.5X 3.0mM was made in the test site on the enamel surface using NailEname, and the window was set to 0.1M lactic acid buffer (pH4.5, 3.0mM CaCl) at 37 ℃2、1.8mM KH2PO40.5% CMC) for 7 days, thereby producing artificial incipient caries. In addition, within a window of 3.5 × 3.0mm, half of the crown apex side was masked with a Nail envelope, and the portion was set as a comparison target portion (control). Preparing the substance to be tested, and taking the suspension solution of the substance and artificial saliva as a test solution for dentifrice and mouthwash; chewing gum is prepared by extracting water-soluble components from various test substances after micronization, and using a suspension of the water-soluble components and artificial saliva as a test solution.
The recalcification promotion test was performed by: after immersing the artificial incipient caries test body prepared as described above in each test solution for 24 hours, the test body was cut into a thickness of about 500 μm in a state parallel to the tooth axis by a micro cutter, and then, an artificial grindstone was used under water injection conditions (り rubstone) and a natural grindstone to grind the chips into parallel thin chips about 100 μm thick. After grinding, in order to confirm the recalcification effect of the teeth, a contact type display was photographedA microcapillary photograph (CMR) (see fig. 5 and 6) was taken to analyze the recalcification effect of the artificial primary caries site with a computer.
The image analysis of the computer adopts the following modes: the amount of recalcified inorganic material was calculated according to The formula of Angmer et al (B.angmer, D.Carlstromand J.E. Glas: students on ultrasound of Dental Enemel IV: The standardization of normal Human Ename, J.ultrastruture.Res.8, 12-23, 1963); the amount of inorganic lost Δ Z (vol.% inorganic. μm) for the control and treated sides of each section was calculated according to the method of Damto et al (F.A. Damato, R.Stang and K.W. Stephen: Effect of fluorine concentration on regeneration of Carious engineering: an in vitro pH-Cycling Study, Caries Res, 24, 174-. In addition, the recalcification rate was calculated by the following formula.
[ number 1]
Table 13 shows the results of confirming the recalcification promoting effect of the oral composition by the recalcification promoting test method.
[ Table 13]
As shown in table 13, it was found that the oral composition containing amorphous hydroxyapatite or amorphized hydroxyapatite according to the example of the present invention dramatically improved the recalcification rate of enamel, compared to the oral composition containing highly crystalline hydroxyapatite or lowly crystalline hydroxyapatite according to the comparative example. That is, even when all of the examples are compared, the oral composition containing amorphous hydroxyapatite or amorphous hydroxyapatite according to the example of the present invention shows a recalcification rate of 2 times or more, as compared with the oral composition containing low crystalline hydroxyapatite, indicating that the oral composition has an extremely excellent effect.
Claims (8)
1. An accelerating agent for recalcification of enamel, characterized by comprising an amorphous hydroxyapatite which shows two peaks at 2 θ =31 to 35 ° in X-ray diffraction.
2. An agent for accelerating recalcification of tooth enamel according to claim 1, wherein the amorphous hydroxyapatite is hydroxyapatite showing an X-ray diffraction pattern shown in fig. 2.
3. An accelerator for recalcification of tooth enamel according to claim 1 or 2, wherein the amorphous hydroxyapatite is a hydroxyapatite obtained by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at a temperature of 10 to 70 ℃.
4. An oral composition comprising an amorphous hydroxyapatite which shows two peaks at 2 θ =31 to 35 ° in X-ray diffraction.
5. The oral composition according to claim 4 wherein the amorphous hydroxyapatite is hydroxyapatite exhibiting an X-ray diffraction pattern as shown in figure 2.
6. The oral composition according to claim 4 or 5, wherein the amorphous hydroxyapatite is a hydroxyapatite obtained by reacting a calcium salt with a phosphate in an aqueous solution and drying the reaction product at a temperature of 10 to 70 ℃.
7. The oral composition according to claim 4, wherein the amorphous hydroxyapatite is contained in an amount of 0.01 to 50 wt%.
8. The oral composition of claim 4 wherein the oral composition is a dentifrice, mouthwash or chewing gum.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007103135A JP5553396B2 (en) | 2007-04-10 | 2007-04-10 | Remineralization accelerator and oral composition |
| JP2007-103135 | 2007-04-10 | ||
| PCT/JP2008/000909 WO2008126410A1 (en) | 2007-04-10 | 2008-04-08 | Recalcification promoter and composition for oral cavity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| HK1138180A1 HK1138180A1 (en) | 2010-08-20 |
| HK1138180B true HK1138180B (en) | 2013-12-20 |
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