CN111481453A - Desensitizing oral composition, preparation method and application thereof - Google Patents

Desensitizing oral composition, preparation method and application thereof Download PDF

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CN111481453A
CN111481453A CN202010368165.XA CN202010368165A CN111481453A CN 111481453 A CN111481453 A CN 111481453A CN 202010368165 A CN202010368165 A CN 202010368165A CN 111481453 A CN111481453 A CN 111481453A
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micron
oral composition
sized
calcium carbonate
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区志宏
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Yangzhou Perfect Daily Chemicals Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

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Abstract

The invention belongs to the technical field of oral products, and provides a desensitizing oral composition, and a preparation method and application thereof. The desensitizing oral composition of the present invention comprises micron grade hydroxyapatite coated calcium carbonate and micron grade precipitated silica. The mass fraction of the micron-sized hydroxyapatite coated calcium carbonate in the oral composition is 0.1-30%, and the mass fraction of the micron-sized precipitated silica in the oral composition is 0.1-30%. The invention provides a desensitization oral composition without sylvine and strontium salt, which has desensitization effect by adding the oral composition of micron-sized hydroxyapatite-coated calcium carbonate and micron-sized precipitated silica, and because the sizes of the materials of the two are smaller than the aperture (generally 3-5 microns) of a dental tubule, the oral composition can fill the dental tubule during tooth brushing and block the channel between the dental pulp nerve and the outside, so that the external cold, hot, sour and sweet taste cannot stimulate the dental nerve, and the desensitization oral composition can be used every day to achieve the effect of tooth desensitization.

Description

Desensitizing oral composition, preparation method and application thereof
Technical Field
The invention relates to the technical field of oral products, in particular to a desensitization oral composition and a preparation method and application thereof.
Background
At present, scientific researches find that dentin sensitivity is caused by enamel loss due to tooth decay or mechanical abrasion, a tubule originally covered by the enamel is exposed outside, and dental pulp nerves in the tubule are stimulated by external cold, hot, sour and sweet and the like, so that people feel intolerable ache. The tubules can thus be filled with active substances.
The active substance adopted by the oral cavity product which is declared to have the tooth desensitizing or anti-allergic effect is basically 5 percent of potassium salt or 10 percent of strontium salt as the desensitizer. The technique of using potassium salt or strontium salt has obvious disadvantages of bitter and astringent feeling, strong covering to essence and great negative influence to mouth feeling. Because the potassium salt and the strontium salt have bitter taste and the salt product is easy to defoam, the air bubbles are less during tooth brushing, and the tooth brushing is not clean; in addition, the desensitizing effect of the salt is short in duration. The above disadvantages make the desensitization products not highly acceptable to consumers, and are not favorable for product popularization.
Disclosure of Invention
Aiming at the defects in the prior art, the desensitizing oral composition provided by the invention, as well as the preparation method and the application thereof, can fill up the dental tubules during tooth brushing, thereby achieving the effect of desensitizing the teeth.
In a first aspect, the present invention provides a desensitizing oral composition comprising micron-sized hydroxyapatite coated calcium carbonate and micron-sized precipitated silica.
Optionally, the mass fraction of the micron-sized hydroxyapatite coated calcium carbonate in the oral composition is 0.1-30%, and the mass fraction of the micron-sized precipitated silica in the oral composition is 0.1-30%.
Optionally, the range of the medium particle size D50 of the micron-sized hydroxyapatite-coated calcium carbonate is 1-10 micrometers, the range of the center particle size D50 of the micron-sized precipitated silica is 0.1-5 micrometers, and the range of the particle size D90 is not more than 8 micrometers.
Optionally, the composition comprises the following components in percentage by mass:
5% of PEG 400, 48% of sorbitol, 0.9% of thickening agent, 0.2% of saccharin sodium, 0.23% of sodium fluoride, 0.3% of titanium dioxide, 1% of micron-sized hydroxyapatite coated calcium carbonate, 6% of micron-sized precipitated silica, 10% of friction type silica, 2% of K12, 1% of essence, 0.15% of methyl hydroxybenzoate, 0.06% of propyl hydroxybenzoate and the balance of water.
Optionally, the composition comprises the following components in percentage by mass:
0.1 percent of saccharin sodium, 0.23 percent of sodium fluoride, 0.2 percent of essence, 0.1 percent of methyl hydroxybenzoate, 0.08 percent of propyl hydroxybenzoate, 5 percent of micron-sized hydroxyapatite coated calcium carbonate, 6 percent of micron-sized precipitated silicon dioxide and the balance of calcium hydrophosphate.
In a second aspect, the present invention provides a method of preparing a desensitizing oral composition comprising the steps of:
step S1: dissolving PEG-400, sorbitol, saccharin sodium and sodium fluoride in water to form a solution;
step S2: uniformly mixing titanium dioxide, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica, friction type silica, a thickening agent and K12, adding the solution obtained in the step S1, and uniformly stirring the mixture in a vacuum environment to form a paste;
step S3: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using the essence, adding into the paste obtained in the step S2, and uniformly stirring in vacuum to obtain the toothpaste.
In a third aspect, the present invention provides a method of preparing a desensitizing oral composition comprising the steps of:
step S1: uniformly mixing sodium fluoride, saccharin sodium, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica and calcium hydrophosphate to form a powdery mixture;
step S2: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using essence, spraying the mixture into the powder mixture obtained in the step S1 by using a sprayer, and uniformly stirring to obtain the dentifrice.
In a fourth aspect, the invention provides the use of a desensitizing oral composition according to the invention, which can be used to prepare a toothpaste or a dentifrice.
The invention has the beneficial effects that:
1. the invention provides a desensitization oral composition without sylvine and strontium salt, which has desensitization effect by adding the oral composition of micron-sized hydroxyapatite-coated calcium carbonate and micron-sized precipitated silica, and because the appearances of the materials of the two are similar to spherical shapes, and the size of the materials is smaller than the aperture (generally 3-5 microns) of a dental tubule, the oral composition can finish the work of filling the dental tubule during tooth brushing, block the channel between the dental pulp nerve and the outside, ensure that the outside cold, hot, sour and sweet can not stimulate the dental nerve, and can be used every day to achieve the effect of tooth desensitization.
2. The desensitizing oral composition provided by the invention does not contain potassium salt and strontium salt, has lasting effect on tooth desensitization, has no influence on the taste of the product, does not generate bitter taste, has rich foam, and is very suitable for popularization of the product.
3. The micron-sized hydroxyapatite coated calcium carbonate and the micron-sized precipitated silica adopted by the invention are safe and non-toxic, have different affinities for teeth, and can mutually promote the blocking effect on the dental tubules by matching use, thereby achieving the synergistic effect of desensitizing the teeth; and the micron-sized hydroxyapatite coated calcium carbonate is the same as the tooth material, and has excellent remineralization performance.
4. The micron-sized hydroxyapatite coated calcium carbonate and the micron-sized precipitated silica are combined, and through the combination of remineralization and mechanical blockage, the tooth can be effectively and durably desensitized.
5. The oral composition provided by the invention can be used for preparing various oral cleaning and nursing products for teeth, such as toothpaste, tooth powder and the like.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a schematic view of a scanning electron microscope of calcium carbonate coated with micron-sized hydroxyapatite used in the present invention;
FIG. 2 is a view of the microscopic state of a tooth before brushing the tooth with the toothpaste of example 1 after demineralization;
FIG. 3 is a view of the microscopic state of the teeth after demineralised teeth have been brushed with the toothpaste of example 1;
FIG. 4 is a view showing a microscopic state of teeth after toothbrushing with the toothpaste of example 4 for broken teeth;
fig. 5 is a view showing a microscopic state of teeth after toothbrushing with the toothpaste of example 1 for broken teeth.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The micron-sized hydroxyapatite-coated calcium carbonate adopted in the application is a product purchased from OMYA INTERNATIONA L AG "
Figure BDA0002477244050000041
100-OG ", which is specifically Functionalized calcium carbonate or calcium carbonate applications (i.e., Functionalized calcium carbonate for oral care applications), wherein the hydroxyapatite content is 85% and the calcium carbonate content is 15%. The specific surface area is 5.5 μm and 110m2The apparent density is 0.15g/ml, and the drying weight loss is 4 percent at 200 ℃ for 4 h.
The range of the medium particle size D50 of the micron-sized hydroxyapatite coated calcium carbonate adopted by the application is 1-10 microns, and preferably 5.5 microns. Fig. 1 is a scanning electron microscope schematic diagram of calcium carbonate coated with micron-sized hydroxyapatite adopted by the invention. Referring to fig. 1, it can be seen that the calcium carbonate coated with micron-sized hydroxyapatite is a loose spherical structure, has a large specific surface area, is easily adhered to defective enamel, and has the effect of remineralization; in addition, the micron-sized hydroxyapatite coated calcium carbonate can mineralize and repair enamel and block small dental orifices, so that the originally exposed dental nerves are blocked, and the tooth desensitization effect is achieved.
The range of the center particle size D50 of the micron-sized precipitated silica is 0.1-5 microns, and the range of the particle size D90 is not more than 8 microns. The micron-sized precipitated silica has smaller particle size than the dental tubules, so that the mouth of the dental tubules can be blocked, the original exposed dental nerves are blocked, and the dental pulp nerves in the dental tubules are prevented from being stimulated by external cold, hot, sour and sweet and the like to generate pain sensation.
In addition, the calcium carbonate coated by the micron-sized hydroxyapatite which is one of the active ingredients in the invention can be calcium carbonate or other calcium-containing compounds. The other active ingredient micron-sized precipitated silica comprises micron-sized silica which has the central particle size D50 of 0.1-5 microns and the particle size D90 of less than or equal to 8 microns and is prepared by various chemical precipitation methods.
Example 1
Example 1 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000051
the total of all the components is 100 percent.
The preparation method of the desensitization toothpaste comprises the following steps:
step S1: dissolving PEG-400, sorbitol, saccharin sodium and sodium fluoride in water to form a solution;
step S2: uniformly mixing titanium dioxide, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica, friction type silica, a thickening agent and K12, adding the solution obtained in the step S1, and uniformly stirring the mixture in a vacuum environment to form a paste;
step S3: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using the essence, adding into the paste obtained in the step S2, and uniformly stirring in vacuum to obtain the toothpaste.
Example 2
Example 2 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000061
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 3
Example 3 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000062
Figure BDA0002477244050000071
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 4
Example 4 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000072
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 5
Example 5 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000081
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 6
Example 6 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000082
Figure BDA0002477244050000091
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 7
Example 7 provides a desensitizing toothpaste comprising the following components in parts by mass:
Figure BDA0002477244050000092
the total of all the components is 100 percent.
The preparation method is the same as that of example 1.
Example 8
Example 8 provides a desensitizing dentifrice comprising the following components in mass fractions:
Figure BDA0002477244050000101
the total of all the components is 100 percent.
The preparation method of the desensitization toothpaste comprises the following steps:
step S1: uniformly mixing sodium fluoride, saccharin sodium, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica and calcium hydrophosphate to form a powdery mixture;
step S2: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using essence, spraying the mixture into the powder mixture obtained in the step S1 by using a sprayer, and uniformly stirring to obtain the dentifrice.
Example 9
Fig. 2 is a view showing a microscopic state of a tooth before brushing the tooth with the toothpaste of example 1 after demineralizing the tooth. Referring to fig. 2, it can be seen that the tooth surface is partially concave, indicating that it is in a demineralised state. Fig. 3 is a view showing a microscopic state of the teeth after demineralised teeth were brushed with the toothpaste of example 1. Referring to fig. 3, it can be seen that the tooth surface demineralization sites have been substantially filled, indicating a greater capacity for restoration and remineralization.
Fig. 4 is a view showing a microscopic state of teeth after toothbrushing with the toothpaste of example 4 using the broken teeth. Referring to fig. 4, since the enamel on the tooth was worn away, most of the tubules on the surface were seen to be bare after brushing the surface with the toothpaste of example 4. Fig. 5 is a view showing a microscopic state of teeth after toothbrushing with the toothpaste of example 1 for broken teeth. Referring to fig. 5, it can be seen that the surface has been mostly filled and sealed by the filling.
Example 10
This example compares the desensitizing toothpastes prepared in example 1, example 2 and example 3 respectively. 90 people with oral cavity sensitivity problems are collected for testing, the testing is divided into 3 groups, each group comprises 30 people, 3 groups of testers respectively use the desensitizing toothpaste of the embodiment 1-3 to brush teeth for one month, and the using effect of each person is counted after one month, which is specifically shown in table 1.
TABLE 1
Figure BDA0002477244050000111
As can be seen from the data in Table 1, the micron-sized hydroxyapatite coated calcium carbonate and the micron-sized precipitated silica are effective in dentin desensitization, and the desensitization effect of the toothpaste with the micron-sized hydroxyapatite coated calcium carbonate and the micron-sized precipitated silica added is obviously higher than that of the toothpaste with one of the active ingredients added separately.
According to the application, the micron-sized hydroxyapatite is coated with the calcium carbonate and the micron-sized precipitated silica, so that the tooth demineralization surface can be restored and remineralized and the exposed dental tubules can be plugged simultaneously, the effect of plugging the dental nerves in a large-area microcosmic manner is achieved, and the tooth desensitization effect is very obvious.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.

Claims (8)

1. A desensitizing oral composition comprising micron grade hydroxyapatite coated calcium carbonate and micron grade precipitated silica.
2. The desensitizing oral composition according to claim 1, wherein said micron-sized hydroxyapatite coated calcium carbonate is present in the oral composition at a weight fraction of 0.1% to 30% and said micron-sized precipitated silica is present in the oral composition at a weight fraction of 0.1% to 30%.
3. The desensitizing oral composition according to claim 1, wherein said micron-sized hydroxyapatite coated calcium carbonate has a median particle size D50 ranging from 1 to 10 microns, said micron-sized precipitated silica has a central particle size D50 ranging from 0.1 to 5 microns, and a particle size D90 ranging from 8 microns or less.
4. The desensitizing oral composition according to any one of claims 1 to 3, comprising the following components in mass fractions:
5% of PEG 400, 48% of sorbitol, 0.9% of thickening agent, 0.2% of saccharin sodium, 0.23% of sodium fluoride, 0.3% of titanium dioxide, 1% of micron-sized hydroxyapatite coated calcium carbonate, 6% of micron-sized precipitated silica, 10% of friction type silica, 2% of K12, 1% of essence, 0.15% of methyl hydroxybenzoate, 0.06% of propyl hydroxybenzoate and the balance of water.
5. The desensitizing oral composition according to any one of claims 1 to 3, comprising the following components in mass fractions:
0.1 percent of saccharin sodium, 0.23 percent of sodium fluoride, 0.2 percent of essence, 0.1 percent of methyl hydroxybenzoate, 0.08 percent of propyl hydroxybenzoate, 5 percent of micron-sized hydroxyapatite coated calcium carbonate, 6 percent of micron-sized precipitated silicon dioxide and the balance of calcium hydrophosphate.
6. A method of preparing a desensitizing oral composition according to claim 4, comprising the steps of:
step S1: dissolving PEG-400, sorbitol, saccharin sodium and sodium fluoride in water to form a solution;
step S2: uniformly mixing titanium dioxide, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica, friction type silica, a thickening agent and K12, adding the solution obtained in the step S1, and uniformly stirring the mixture in a vacuum environment to form a paste;
step S3: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using the essence, adding into the paste obtained in the step S2, and uniformly stirring in vacuum to obtain the toothpaste.
7. A method of preparing a desensitizing oral composition according to claim 5, comprising the steps of:
step S1: uniformly mixing sodium fluoride, saccharin sodium, micron-sized hydroxyapatite-coated calcium carbonate, micron-sized precipitated silica and calcium hydrophosphate to form a powdery mixture;
step S2: and (4) dissolving methyl hydroxybenzoate and propyl hydroxybenzoate by using essence, spraying the mixture into the powder mixture obtained in the step S1 by using a sprayer, and uniformly stirring to obtain the dentifrice.
8. Use of a desensitizing oral composition according to claim 6 or 7 for the preparation of a toothpaste or a tooth powder.
CN202010368165.XA 2020-04-30 2020-04-30 Desensitizing oral composition, preparation method and application thereof Withdrawn CN111481453A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112618392A (en) * 2021-01-22 2021-04-09 广州舒客实业有限公司 Oral care compositions comprising bioactive materials and spherical silica

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Publication number Priority date Publication date Assignee Title
CN101889964A (en) * 2009-05-20 2010-11-24 广州薇美姿个人护理用品有限公司 Desensitizing toothpaste
CN106074195A (en) * 2016-07-06 2016-11-09 杭州皎洁口腔保健用品有限公司 A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101889964A (en) * 2009-05-20 2010-11-24 广州薇美姿个人护理用品有限公司 Desensitizing toothpaste
CN106074195A (en) * 2016-07-06 2016-11-09 杭州皎洁口腔保健用品有限公司 A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof

Non-Patent Citations (1)

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Title
佚名: "ozel Dis Macunlari icin cok Amacli Mineraller", 《HTTPS://WWW.TURKCHEM.NET/OZEL-DIS-MACUNLARI-ICIN-COK-AMACLI-MINERALLER.HTML》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112618392A (en) * 2021-01-22 2021-04-09 广州舒客实业有限公司 Oral care compositions comprising bioactive materials and spherical silica

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Application publication date: 20200804