CN113827508B - Thickening agent, collutory toothpaste and preparation method of collutory toothpaste - Google Patents

Thickening agent, collutory toothpaste and preparation method of collutory toothpaste Download PDF

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Publication number
CN113827508B
CN113827508B CN202111367906.3A CN202111367906A CN113827508B CN 113827508 B CN113827508 B CN 113827508B CN 202111367906 A CN202111367906 A CN 202111367906A CN 113827508 B CN113827508 B CN 113827508B
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toothpaste
thickener
carbopol
high molecular
oral care
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CN113827508A (en
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黄强
蔡丽萍
沈章宁
陈万金
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Fujian Azalli Chemicals Co ltd
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Fujian Azalli 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • 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
    • 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
    • A61K8/26Aluminium; 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8123Compositions of homopolymers or copolymers of compounds having one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers, e.g. PVC, PTFE
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8158Homopolymers or copolymers of amides or imides, e.g. (meth) acrylamide; Compositions of derivatives of such polymers
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/48Thickener, Thickening system
    • 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
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention relates to the technical field of oral care, in particular to a thickening agent, a mouthwash toothpaste and a preparation method thereof. The thickener of the present invention includes: a) One or two of nonionic high molecular compounds, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymers; b) And (5) inorganic gel. The invention adopts the compatibility of nonionic high molecular compound, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymer and inorganic gel as a thickening agent, plays a role in synergy, is applied to oral care products, improves the stability of the oral care products and enhances the dissolving capacity of the oral care products. The toothpaste containing the thickener can help people with tooth sensitivity to relieve dentin sensitivity in efficacy, has the functions of mouthwash and toothpaste in the aspect of using methods, and realizes dual purposes of toothpaste.

Description

Thickening agent, collutory toothpaste and preparation method of collutory toothpaste
Technical Field
The application relates to the technical field of oral care, in particular to a thickening agent, a mouthwash toothpaste and a preparation method thereof.
Background
Many people suffer from tooth sensitivity, a condition commonly known as dentin hypersensitivity (hypersensitive dentin), a common problem for adults. It is a transient pain caused by exposed dentin, usually a response to chemical, thermal, tactile or osmotic stimuli, that cannot be explained by any other dental defect or pathology. Anti-sensitivity toothpastes are commonly used to alleviate tooth sensitivity, with potassium and strontium salts as the main ingredients of the anti-sensitivity. Wherein the desensitizing mechanism of the strontium salt is that the strontium salt is dissolved in water to form strontium ions, and the strontium ions can react with calcium carbonate in dentin to generate strontium carbonate SrCO 3 Hydroxy phosphorus ash simultaneously with dentinThe stone acts to produce hydroxy strontium apatite, blocking the tubules that open up the dentin. The desensitization mechanism of the potassium salt is that the potassium salt is dissolved in water to form potassium ions, and the potassium ions can enter dentinal tubules to reduce the permeability of dentin, and have an affinity effect with nerve endings, improve the transmission of nerve pulses and alleviate the pain of teeth.
The thickener is a key raw material in the oral care product, can enable the toothpaste to have proper viscosity and consistency, does not feel sticky, has good fluidity, swells in a liquid phase in the toothpaste to form a stable colloid so as to suspend a solid phase of the toothpaste, prevents separation of solid phase components and liquid phase components in the toothpaste, and is an important component for regulating the stability of the toothpaste. However, common toothpastes are generally higher in consistency, and commonly used thickening agents are sodium carboxymethylcellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum (xanthan gum), hydroxypropyl guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan, and other conventional thickening systems. These thickeners ensure paste stability and also make the paste solubility worse, and the paste containing anti-sensitive ingredients (strontium salt/potassium salt) is difficult to release strontium ions/potassium ions or is not fully released and the dissolution rate is too slow, thus the anti-sensitive effect of the toothpaste is obviously reduced.
Disclosure of Invention
Therefore, it is necessary to provide a thickener, which can enhance the dissolution ability of the paste while ensuring the stability of the toothpaste, and promote the strontium ions to be completely dissociated, thereby exerting the maximum dentin sensitivity resistance effect and effectively improving the sensitivity resistance effect of the toothpaste.
To achieve the above object, the first aspect of the present invention provides a thickener comprising: a) One or two of nonionic high molecular compounds, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymers; b) And (5) inorganic gel.
As a further embodiment of the present invention, the thickener comprises, in weight percent: 25 to 30 percent of nonionic high molecular compound, 25 to 30 percent of high molecular polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and 40 to 50 percent of inorganic gel.
As a further embodiment of the present invention, the thickener comprises, in weight percent: 20-40% of nonionic polymer compound and 60-80% of inorganic gel.
In a further embodiment of the present invention, the nonionic polymer compound is selected from one or more of polyvinylpyrrolidone, polytetrafluoroethylene amine, polyacrylamide, and polyethyleneimine.
As a further embodiment of the present invention, the high molecular polymer of acrylic acid-bonded allyl sucrose or pentaerythritol allyl ether is selected from one or more of Pemulen TR-1, pemulen TR-2, carbopol 1342, carbopol 934, carbopol 940, carbopol 941, carbopol 980, carbopol ETD 2020, carbopol AQUA SF-1, carbopol Ultrez 21, carbopol Ultrez 20.
As a further embodiment of the present invention, the inorganic gel is selected from one or more of magnesium lithium silicate, magnesium aluminum silicate, montmorillonite powder, sodium bentonite.
In a second aspect, the invention provides the use of a thickener according to the first aspect of the invention in the manufacture of an oral care product, the thickener being for use in the manufacture of an oral care product.
Preferably, the oral care implement comprises a toothpaste and a dental gel.
In a third aspect the present invention provides a mouthwash toothpaste comprising a thickener, abrasive, humectant, surfactant, strontium salt and/or potassium salt, acid base buffer, food grade flavour, preservative and water according to the first aspect of the present invention.
As a further embodiment of the invention, the friction agent is selected from calcium hydrogen phosphate, aluminium hydroxide or silica.
As a further embodiment of the present invention, the humectant is selected from one or more of glycerin, sorbitol, polyethylene glycol or propylene glycol.
As a further embodiment of the present invention, the surfactant is selected from one or more of anionic, cationic, amphoteric and nonionic surfactants, for example: poloxamers, sodium lauryl sulfate (sodium lauryl sulfate), sodium lauroyl sarcosinate, sodium sulfatase or cocamidopropyl betaine.
As a further embodiment of the present invention, the strontium salt is selected from strontium chloride, strontium acetate, and the potassium salt is selected from potassium nitrate, potassium citrate, potassium chloride, potassium bicarbonate or potassium oxalate.
As a further embodiment of the present invention, the acid-base buffer is selected from sodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium carbonate, sodium bicarbonate or sodium silicate.
As a further embodiment of the present invention, the flavour is selected from one or more of peppermint, spearmint oil, peppermint, menthyl lactate, peppermint and lemon flavour.
As a further embodiment of the present invention, the preservative is selected from one or more of methyl benzoate, ethyl benzoate, propyl benzoate, sodium benzoate, butyl benzoate, sorbic acid, potassium sorbate, sodium methyl parahydroxybenzoate, and sodium ethyl parahydroxybenzoate.
As a further embodiment of the present invention, the mouthwash toothpaste comprises the following components in weight percent:
0.4% -5% of thickening agent;
8% -25% of friction agent;
15% -75% of humectant;
2.5% -20% of surfactant;
strontium salt and/or potassium salt 0.2-3.8%;
0.1 to 1 percent of acid-base buffer;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
According to a fourth aspect of the present invention there is provided a method of preparing a mouthwash toothpaste according to the third aspect of the present invention, the method comprising the steps of:
(1) Uniformly mixing water and a surfactant to prepare a solution A;
(2) Uniformly mixing a humectant and a thickener to prepare a solution B;
(3) Uniformly mixing an abrasive, strontium salt and/or potassium salt and an acid-base buffer to prepare powder C;
(4) Sequentially adding the solution A, the solution B and the powder C into a container, uniformly mixing, vacuumizing, adding essence and preservative, stirring, homogenizing, and degassing to obtain the mouthwash toothpaste.
Compared with the prior art, the technical scheme has the following beneficial effects:
the invention adopts nonionic high molecular compound, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymer and inorganic gel as thickener to play a role of synergy, and is applied to oral care products, thus improving the stability of the oral care products and enhancing the dissolving capacity of the oral care products, and the invention is specifically characterized in that: on one hand, the method can accelerate the dissociation of strontium ions, promote the strontium ions to be completely dissociated, and promote the anti-sensitivity toothpaste containing the strontium ions to exert the maximum anti-dentin sensitivity effect; on the other hand, the toothpaste or the dental gel is quickly dissolved in a proper amount of water, can be used as mouthwash, has simpler and more convenient use method, and realizes the dual purposes of toothpaste and dental gel. The toothpaste containing the thickener can help people with tooth sensitivity to relieve dentin sensitivity in efficacy, and also has the functions of mouthwash and toothpaste in the aspect of using methods.
Detailed Description
In order to describe the technical content, constructional features, achieved objects and effects of the technical solution in detail, the following description is made in detail with reference to specific embodiments. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified. The experimental methods in the following examples are conventional methods unless otherwise specified.
First, a thickener according to a first aspect of the present invention is described, which comprises: a) One or two of nonionic high molecular compounds, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymers; b) And (5) inorganic gel.
The invention adopts the compatibility of nonionic high molecular compound, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymer and inorganic gel as a thickening agent, plays a role in synergy, is applied to oral care products, and can enhance the dissolving capacity of the oral care products while improving the stability of the oral care products. Compared with single thickener or mixture thereof in traditional thickening systems such as sodium carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum, guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan and the like, the composition of nonionic high molecular compound, high molecular polymer of acrylic acid bonding allyl sucrose or pentaerythritol allyl ether and inorganic gel has more proper viscosity, can maintain stable paste shape under normal state after being applied to toothpaste or dental gel, can be quickly dissolved after being applied to oral cavity or meeting water, improves the dissolution efficiency of strontium salt/potassium salt, and effectively relieves tooth sensitivity.
In an embodiment of the present invention, the thickener includes, in weight percent: 25 to 30 percent of nonionic high molecular compound, 25 to 30 percent of high molecular polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and 40 to 50 percent of inorganic gel.
In an embodiment of the present invention, the thickener includes, in weight percent: 20-40% of nonionic polymer compound and 60-80% of inorganic gel.
In the embodiment of the invention, the nonionic polymer compound is selected from one or a combination of more of polyvinylpyrrolidone, polytetrafluoroethylene amine, polyacrylamide and polyethyleneimine.
In an embodiment of the present invention, the high molecular polymer of acrylic acid-bonded allyl sucrose or pentaerythritol allyl ether is selected from one or more of Pemulen TR-1, pemulen TR-2, carbopol 1342, carbopol 934, carbopol 940, carbopol 941, carbopol 980, carbopol ETD 2020, carbopol AQUA SF-1, carbopol Ultrez 21, carbopol Ultrez 20.
In an embodiment of the present invention, the inorganic gel is selected from one or more of lithium magnesium silicate, magnesium aluminum silicate, montmorillonite powder, and sodium bentonite.
In a second aspect, the invention provides the use of a thickener according to the first aspect of the invention in the manufacture of an oral care product, the thickener being for use in the manufacture of an oral care product.
Preferably, the oral care implement comprises a toothpaste and a dental gel.
In a third aspect the present invention provides a mouthwash toothpaste comprising a thickener, abrasive, humectant, surfactant, strontium salt and/or potassium salt, acid base buffer, food grade flavour, preservative and water according to the first aspect of the present invention.
The toothpaste containing the thickener can keep good stability, the paste is not water-separated in the shelf life, and can be quickly dissolved after entering into the oral cavity or meeting water, and the dissolution of strontium ions is accelerated, so that tooth sensitivity is effectively relieved. The tooth paste capable of gargling provided by the invention can help people with tooth sensitivity to relieve dentin sensitivity in efficacy, has functions of mouthwash and toothpaste in the aspect of using method, is more convenient in using method, and realizes dual purposes of toothpaste.
In an embodiment of the present invention, the friction agent is selected from the group consisting of dibasic calcium phosphate, aluminum hydroxide, and silicon dioxide.
In an embodiment of the present invention, the humectant is selected from one or more of glycerin, sorbitol, polyethylene glycol or propylene glycol.
In an embodiment of the invention, the surfactant is selected from one or more of anionic, cationic, amphoteric and nonionic surfactants, such as poloxamer, sodium lauryl sulfate (sodium lauryl sulfate), sodium lauroyl sarcosinate, sodium sulfanate or cocamidopropyl betaine.
In an embodiment of the present invention, the strontium salt is selected from strontium chloride and strontium acetate, and the potassium salt is selected from potassium nitrate, potassium citrate, potassium chloride, potassium bicarbonate or potassium oxalate. The strontium salt and potassium salt may be mixed in any ratio.
In an embodiment of the present invention, the acid-base buffer is selected from sodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium carbonate, sodium bicarbonate, or sodium silicate.
In the embodiment of the invention, the essence is one or more selected from peppermint, spearmint oil, peppermint, menthyl lactate, peppermint and lemon essence.
In the embodiment of the invention, the preservative is selected from one or more of methyl benzoate, ethyl benzoate, propyl benzoate, sodium benzoate, butyl benzoate, sorbic acid, potassium sorbate, sodium methyl parahydroxybenzoate and sodium ethyl parahydroxybenzoate.
Of course, in some embodiments of the present invention, sweeteners may also be added to the collutoble toothpaste. The sweetener may be selected from saccharin, glucose, sucrose, lactose, maltose, fructose, aspartame, sodium cyclamate, D-tryptophan, dihydrochalcones, acesulfame, or a mixture thereof. Pigments such as lemon yellow, brilliant blue, allure red, carmine, etc. may also be added.
In some embodiments of the present invention, green tea extract, spilanthes extract, ginseng extract, licorice extract, etc. may also be added to the collutoble toothpaste to induce an increase in saliva production in the mouth, helping the toothpaste to dissolve rapidly in the mouth.
The toothpaste of the invention can be added with various additives such as pigment, lemon yellow, brilliant blue, allure red, carmine and the like according to actual requirements; tea polyphenols; lactobacillus; enzymes, and the like.
In the embodiment of the invention, the collutory toothpaste comprises the following components in percentage by weight:
0.4% -5% of thickening agent;
8% -25% of friction agent;
15% -75% of humectant;
2.5% -20% of surfactant;
strontium salt and/or potassium salt 0.2-3.8%;
0.1 to 1 percent of acid-base buffer;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
According to a fourth aspect of the present invention there is provided a method of preparing a mouthwash toothpaste according to the third aspect of the present invention, the method comprising the steps of:
(1) Uniformly mixing water and a surfactant to prepare a solution A;
(2) Uniformly mixing a humectant and a thickener to prepare a solution B;
(3) Uniformly mixing an abrasive, strontium salt and/or potassium salt and an acid-base buffer to prepare powder C;
(4) Sequentially adding the solution A, the solution B and the powder C into a container, uniformly mixing, vacuumizing, adding essence and preservative, stirring, homogenizing, and degassing to obtain the mouthwash toothpaste.
Example 1 thickening agent
A thickener comprising, in weight percent: 25% carbopol 980 and 75% lithium magnesium silicate RD-1 gum.
Example 2 thickening agent
A thickener comprising, in weight percent: 20% polyvinylpyrrolidone PVP K90 and 80% lithium magnesium silicate RD-1 gum.
Example 3 thickening agent
A thickener comprising, in weight percent: 25% polyvinylpyrrolidone PVP K90, 25% carbopol 934 and 50% lithium magnesium silicate RD-1 gum.
Example 4 thickening agent
A thickener comprising, in weight percent: 30% polyethylenimine and 70% magnesium aluminum silicate.
Example 5 thickening agent
A thickener comprising, in weight percent: 20% of polytetrafluoroethylene amine and 80% of sodium bentonite.
Example 6 thickening agent
A thickener comprising, in weight percent: 30% polyvinylpyrrolidone PVP K90, 30% carbopol 940 and 40% lithium magnesium silicate RD-1 gum.
Example 7 thickening agent
A thickener comprising, in weight percent: 40% polyacrylamide and 60% magnesium aluminum silicate.
Example 8 thickening agent
A thickener comprising, in weight percent: 35% of polytetrafluoroethylene amine and 65% of montmorillonite powder.
Example 9 thickening agent
A thickener comprising, in weight percent: 28% polyvinylpyrrolidone PVP K90, 30% carbopol 941 and 42% magnesium aluminum silicate.
Example 10 thickening agent
A thickener comprising, in weight percent: 28% Pemulen TR-1 and 72% lithium magnesium silicate RD-1 gum.
Examples 11 to 20 mouthwash toothpaste
10 kinds of collutory toothpastes were prepared according to the following preparation methods, examples 11 to 20, using the thickeners of examples 1 to 10, respectively, and specific formulations are shown in Table 1.
The preparation method of the collutory toothpaste comprises the following steps:
(1) Uniformly mixing water and a surfactant to prepare a solution A;
(2) Uniformly mixing a humectant and a thickener to prepare a solution B;
(3) Uniformly mixing an abrasive, strontium salt and/or potassium salt and an acid-base buffer to prepare powder C;
(4) Sequentially adding the solution A, the solution B and the powder C into a container, uniformly mixing, vacuumizing, adding essence, preservative and other ingredients, stirring, homogenizing and degassing to obtain the mouthwash toothpaste.
TABLE 1 mouthwash toothpaste formulations of examples 11-20
Comparative examples 1 to 9 toothpastes
This comparative example provides 9 different formulations of toothpaste, the specific formulations are shown in table 2.
The preparation method of the traditional toothpaste comprises the following steps:
(1) Uniformly mixing water and a surfactant to prepare a solution A;
(2) Uniformly mixing a humectant and a thickener to prepare a solution B;
(3) Uniformly mixing an abrasive, strontium salt and/or potassium salt and an acid-base buffer to prepare powder C;
(4) Sequentially adding the solution A, the solution B and the powder C into a container, uniformly mixing, vacuumizing, adding essence, preservative and other ingredients, stirring, homogenizing and degassing to obtain the mouthwash toothpaste.
Table 2 toothpaste formulations of comparative examples 1-9
Performance test:
for the purpose of comparing the overall properties of the mouthwash toothpastes of examples 11 to 20 and the toothpastes of comparative examples 1 to 9, the mouthwash toothpastes of examples 11 to 20 and the toothpastes of comparative examples 1 to 9 were tested for viscosity, stability and dissolution efficiency, and the test results are shown in Table 3.
TABLE 3 Performance test results
As shown in Table 3, compared with the single thickener or the mixture thereof in the traditional thickening system such as sodium carboxymethylcellulose CMC, hydroxyethyl cellulose HEC, xanthan gum, guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan and the like, the collutory toothpaste of the invention adopts the compatibility of nonionic high molecular compound, acrylic acid bonding allyl sucrose or pentaerythritol allyl ether high molecular polymer and inorganic gel as the thickener, has more proper viscosity, can better maintain stability in the quality guarantee period, has fine paste, does not separate water, does not return coarse in the quality guarantee period, or only slightly separates water. Compared with comparative examples 1-5, comparative example 6 adopts the compounding of sodium carboxymethylcellulose CMC and carrageenan as a thickening agent, and has better dentin sensitivity resisting effect; compared with comparative examples 1 to 6, the high molecular polymer (carbomer Carbopol 940), inorganic gel (lithium magnesium silicate RD-1 gum) and nonionic high molecular compound (polyvinylpyrrolidone PVP K90) of comparative examples 7 to 9 respectively added with acrylic acid bonded allyl sucrose or pentaerythritol allyl ether have more stable performance and remarkably improved dissolution rate. Compared with comparative examples 1-5, the mouthwash toothpaste containing 2.0% -5.0% of the thickener of the invention has stable performance, but has a faster dissolution rate, can release strontium salt/potassium salt more quickly, improves the service efficiency of the toothpaste, and fully exerts the anti-sensitivity effect of the toothpaste; compared with comparative examples 6-9, the mouthwash toothpaste containing 0.4% -2.0% of the thickener of the invention has stable performance, has higher dissolution rate, can release strontium salt/potassium salt more quickly, improves the use efficiency of the toothpaste, and fully exerts the anti-sensitivity effect of the toothpaste. In addition, the tooth paste capable of gargling provided by the invention can help people with tooth sensitivity to relieve dentin sensitivity in efficacy, has functions of mouthwash and toothpaste in the aspect of using method, is more convenient in using method, and realizes dual purposes of toothpaste.
Test example 2 mouthwash toothpaste sensitivity test
To verify the anti-tooth sensitivity effect of the mouthwash toothpastes of the present invention, clinical tests were performed by selecting examples 11 to 13, examples 15 and 17, and comparative examples 1, comparative examples 6 to 9. The study was a randomized, double-blind, control, parallel clinical study. Patients with dentinal sensitivity (sensitivity to touch, cold, hot, sour, and sweet stimuli) were selected for clinical treatment, 298 subjects were enrolled in a baseline examination, and 270 subjects completed a total of 8 weeks of study, with each index completed by the same subject. The data were not included in the statistical analysis for a total of 28 subjects, and the reason for the subjects' mid-withdrawal was independent of the study product, and the basic status of the subjects who completed the trial is shown in table 4.
Table 4 basic conditions of the subject
The test adopts an evaluation method of detection sensitivity and an evaluation method of cold air blowing sensitivity to verify the tooth sensitivity resistance effect of the mouthwash toothpaste.
(1) Evaluation of sensitivity to detection
A calibrated model 2000A Yeaple electronic pressure sensitive probe (Yeaple research, pittsford, NY) was used. The instrument can quantitatively measure the pressure (grams) applied to the tooth surface. In testing sensitivity, the probe was placed in contact with exposed dentin on the buccal surface of the selected tooth, at the enamel boundary, using an initial pre-set amount of 10 gram force probe, followed by 10 gram force increments each time until the subject indicated an uncomfortable sensation with a maximum force of 80 grams. A high value of the detection force indicates a low level of tooth sensitivity.
(2) Evaluation of Cold air blowing sensitivity
The air gun of the dental comprehensive treatment table is used for blowing and spraying for 1 second at a distance of 1cm away from sensitive teeth, the pressure of the air compressor is 55-65 p.s.i., the blowing temperature is 19-21 ℃, and fingers are placed on adjacent teeth during blowing to avoid influencing the accuracy of results. The evaluation was carried out with the Schiff cold air sensitivity index, and the score was as follows: 0 = tooth and subject do not respond to air stimulus; 1 = tooth and subject respond to air stimulus but do not request cessation of stimulus; 2 = teeth and subject respond to air stimulus, requesting to stop stimulus or remove stimulus; 3 = tooth and subject response to air stimulus; the stimulus causes pain and requests cessation. A low score for this parameter indicates a reduced sensitivity.
(3) The statistical analysis method comprises the following steps:
in this test, the data obtained were statistically analyzed using one-way analysis of variance (ANOVA) and t-test of SPSS16.0 statistical software, and using a two-sided test, the test level α was 0.05.
The baseline, week 4, week 8 exams for subjects enrolled in the probe sensitivity test are shown in table 5. In the baseline examination, there was no statistical difference between the average of the diagnostic sensitivity indexes of each group; at week 4, there was no statistical difference between groups; at week 8, example 11, example 12, example 13, example 15, example 17, and comparative examples 6-9 all showed significant statistical differences compared to comparative example 1. Wherein, example 11 is reduced by 39.82% from the average of the comparative example 1, example 12 is reduced by 32.75% from the average of the comparative example 1, example 13 is reduced by 41.70% from the average of the comparative example 1, example 15 is reduced by 26.06% from the average of the comparative example 1, example 17 is reduced by 26.35% from the average of the comparative example 1, comparative example 6 is reduced by 22.53% from the average of the comparative example 1, comparative example 7 is reduced by 25.59% from the average of the comparative example 1, comparative example 8 is reduced by 25.12% from the average of the comparative example 1, and comparative example 9 is reduced by 24.27% from the average of the comparative example 1.
TABLE 5 evaluation results of detection sensitivity
*P<0.05
The baseline, 4 th week, 8 th week of examination of the subjects taking part in the cool air blow are shown in table 6. In the baseline inspection, there is no statistical difference between the averages of the cold air blowing sensitivity values of each group; at week 4, there was no statistical difference between groups; at week 8, example 11, example 12, example 13, example 15, example 17, and comparative examples 6-9 all showed significant statistical differences compared to comparative example 1. Wherein, the average value of the cold air blowing sensitivity value of the example 11 is reduced by 46.15% compared with that of the comparative example 1, the average value of the cold air blowing sensitivity value of the example 12 is reduced by 35.90% compared with that of the comparative example 1, the average value of the cold air blowing sensitivity value of the example 13 is reduced by 41.03% compared with that of the comparative example 1, the average value of the cold air blowing sensitivity value of the example 15 is reduced by 32.05%, the average value of the cold air blowing sensitivity value of the example 17 is reduced by 30.77% compared with that of the comparative example 1, the average value of the cold air blowing sensitivity value of the comparative example 6 is reduced by 26.92%, the average value of the cold air blowing sensitivity value of the comparative example 7 is reduced by 30.77% compared with that of the comparative example 1, the average value of the cold air blowing sensitivity value of the comparative example 8 is reduced by 30.77% compared with that of the cold air blowing sensitivity value of the comparative example 1, and the average value of the cold air blowing sensitivity value of the comparative example 9 is reduced by 29.49%.
Table 6 evaluation results of cold air blowing sensitivity
*P<0.05
The clinical treatment results show that compared with comparative example 1, comparative example 6 adopts the compound of CMC and carrageenan as a thickening agent, and has better dentin sensitivity resisting effect. In comparative examples 7 to 9, a polymer (carbomer Carbopol 940) having acrylic acid bonded with allyl sucrose or pentaerythritol allyl ether, an inorganic gel (magnesium lithium silicate RD-1 gum), and a nonionic polymer compound (polyvinylpyrrolidone PVP K90) were compounded with a conventional gum, respectively, which had a better dentin sensitivity resistance effect than comparative examples 1 and 6. However, the collutory toothpaste (examples 11 to 13, 15 and 17) provided by the invention adopts the nonionic polymer, the acrylic acid bonding allyl sucrose or pentaerythritol allyl ether polymer and inorganic gel as the thickener, and has better anti-dentin sensitivity effect compared with the single thickener or the mixture of the single thickener in the traditional thickening system such as sodium carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum, guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan and the like, or the mixture of the acrylic acid bonding allyl sucrose or pentaerythritol allyl ether polymer, inorganic gel and the mixture of the nonionic polymer and the traditional thickening system. No adverse effects were observed in the present clinical study with the collutory toothpaste provided by the present invention.
It should be noted that, although the foregoing embodiments have been described herein, the scope of the invention is not limited thereto, and technical parameters that are not described in detail may still be the same as or similar to the above embodiments when they are changed within the scope of the invention, and still fall within the scope of the invention. Therefore, changes and modifications to the embodiments described herein, or equivalent structures or equivalent flow transformations by employing the principles of the present invention, based on the innovative concepts of the present invention, will be apparent to those skilled in the art and will be encompassed by the present invention as described herein.

Claims (5)

1. The thickener is characterized by comprising, by weight, 25% -30% of a nonionic high molecular compound, 25% -30% of a high molecular polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and 40% -50% of inorganic gel, wherein the nonionic high molecular compound is selected from any one or a combination of more of polyvinylpyrrolidone, polytetrafluoroethylene amine, polyacrylamide and polyethyleneimine; the high molecular polymer of acrylic acid bonding allyl sucrose or pentaerythritol allyl ether is selected from one or more of Pemulen TR-1, pemulen TR-2, carbopol 1342, carbopol 934, carbopol 940, carbopol 941, carbopol 980, carbopol ETD 2020, carbopol AQUA SF-1, carbopol Ultrez 21 and Carbopol Ultrez 20; the inorganic gel is selected from one or more of lithium magnesium silicate, magnesium aluminum silicate, montmorillonite powder and sodium bentonite.
2. Use of the thickener of claim 1 for the preparation of an oral care product, wherein the thickener is used for the preparation of an oral care product; the oral care products include toothpastes and dental gels.
3. A collutoble toothpaste comprising a thickener, a friction agent, a humectant, a surfactant, a strontium salt and/or potassium salt, an acid-base buffer, a food grade flavour, a preservative and water according to claim 1.
4. A mouthwash toothpaste according to claim 3, comprising the following components in weight percent:
0.4% -5% of thickening agent;
8% -25% of friction agent;
15% -75% of humectant;
2.5% -20% of surfactant;
strontium salt and/or potassium salt 0.2-3.8%;
0.1 to 1 percent of acid-base buffer;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
5. The method of preparing a mouthwash toothpaste according to claim 4, comprising the steps of:
(1) Uniformly mixing water and a surfactant to prepare a solution A;
(2) Uniformly mixing a humectant and a thickener to prepare a solution B;
(3) Uniformly mixing an abrasive, strontium salt and/or potassium salt and an acid-base buffer to prepare powder C;
(4) Sequentially adding the solution A, the solution B and the powder C into a container, uniformly mixing, vacuumizing, adding essence and preservative, stirring, homogenizing, and degassing to obtain the mouthwash toothpaste.
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