CN113827508A - Thickening agent, gargling toothpaste and preparation method thereof - Google Patents

Thickening agent, gargling toothpaste and preparation method thereof Download PDF

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CN113827508A
CN113827508A CN202111367906.3A CN202111367906A CN113827508A CN 113827508 A CN113827508 A CN 113827508A CN 202111367906 A CN202111367906 A CN 202111367906A CN 113827508 A CN113827508 A CN 113827508A
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toothpaste
percent
thickener
carbopol
high molecular
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CN113827508B (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

Abstract

The invention relates to the technical field of oral care, in particular to a thickening agent, gargling toothpaste and a preparation method thereof. The thickener of the present invention comprises: a) one or two of nonionic high molecular compound, acrylic acid bonded allyl sucrose or pentaerythritol allyl ether high molecular polymer; b) an inorganic gel. The invention adopts the compatibility of nonionic high molecular compounds, high molecular polymers of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and inorganic gel as the thickening agent, has synergistic effect, is applied to oral care products, improves the stability of the oral care products, and simultaneously enhances the dissolving capacity of the oral care products. The toothpaste containing the thickening agent can help tooth-sensitive people to relieve dentine sensitivity in terms of efficacy, and has the functions of gargling water and toothpaste in terms of using methods, so that the toothpaste has two purposes.

Description

Thickening agent, gargling toothpaste and preparation method thereof
Technical Field
The application relates to the technical field of oral care, in particular to a thickening agent, gargle toothpaste and a preparation method thereof.
Background
Many people suffer from tooth sensitivity, a condition commonly referred to as dentinal hypersensitivity (hypersensitive dentin), which is a common problem for adults. It is a transient pain caused by exposed dentin, usually in response to chemical, thermal, tactile or osmotic stimuli, and cannot be explained by any other tooth defect or pathology. Anti-sensitivity toothpastes are commonly used to alleviate tooth sensitivity, and the main ingredients for anti-sensitivity are potassium and strontium salts. Wherein the desensitization mechanism of the strontium salt is that the strontium salt is dissolved in water to form strontium ions which can react with calcium carbonate in dentin to generate strontium carbonate SrCO3Meanwhile, the calcium phosphate acts with hydroxyapatite of dentin to generate strontium hydroxyapatite, which blocks the open tubules of 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 dentin tubules to reduce the permeability of dentin and have affinity with nerve endings, improve the transmission of nerve impulses and relieve the pain of teeth.
The thickening agent is a key raw material in oral care products, 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 and prevent the separation of a solid phase component and a liquid phase component in the toothpaste, and is an important component for adjusting the stability of the toothpaste. However, common toothpastes generally have a high consistency, and conventional thickening systems such as sodium carboxymethylcellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum (xanthan gum), hydroxypropyl guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan, etc. are commonly used as thickening agents. The thickening agents ensure the stability of the paste, simultaneously ensure that the solubility of the paste is poor, and the paste containing anti-sensitive ingredients (strontium salt/potassium salt) is difficult to release strontium ions/potassium ions or has incomplete release and slow dissolution rate, thereby obviously reducing the anti-sensitive effect of the toothpaste.
Disclosure of Invention
Therefore, it is required to provide a thickening agent, which can enhance the dissolving capacity of the paste and promote the strontium ions to be completely dissociated while ensuring the stability of the toothpaste, thereby exerting the maximum dentin sensitivity resistance effect and effectively improving the sensitivity resistance effect of the toothpaste.
To achieve the above object, a first aspect of the present invention provides a thickener comprising: a) one or two of nonionic high molecular compound, acrylic acid bonded allyl sucrose or pentaerythritol allyl ether high molecular polymer; b) an inorganic gel.
As a further embodiment of the present invention, the thickener comprises, in weight percent: 25 to 30 percent of nonionic macromolecular compound, 25 to 30 percent of macromolecular 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 non-ionic high molecular 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, said high molecular weight polymer of acrylic-bonded allyl sucrose or pentaerythritol allyl ether is selected from the group consisting 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.
As a further embodiment of the present invention, the inorganic gel is selected from the group consisting of one or more of lithium magnesium silicate, magnesium aluminum silicate, montmorillonite powder, sodium bentonite, and combinations thereof.
In a second aspect, the present invention provides the use of a thickener according to the first aspect of the invention in the manufacture of an oral care product, for use in the manufacture of an oral care product.
Preferably, the oral care products include toothpastes and dental gels.
In a third aspect the present invention provides a collutory toothpaste comprising a thickener according to the first aspect of the present invention, an abrasive agent, a humectant, a surfactant, a strontium and/or potassium salt, an acid-base buffer, a food grade flavour, a preservative and water.
As a further embodiment of the invention, the abrasive is selected from calcium hydrogen phosphate, aluminium hydroxide or silica.
As a further embodiment of the invention, the humectant is selected from one or more of glycerin, sorbitol, polyethylene glycol or propylene glycol.
As a further embodiment of the invention, the surfactant is selected from one or more of anionic, cationic, amphoteric and nonionic surfactants, for example: poloxamer, sodium lauryl sulfate (sodium lauryl sulfate), sodium lauroyl sarcosinate, sodium thiosulfonate, 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 essence is selected from one or more of peppermint, spearmint oil, peppermint, menthyl lactate, peppermint, lemon essence.
As a further embodiment of the present invention, the preservative is selected from one or more of methyl paraben, ethyl paraben, propyl paraben, sodium benzoate, butyl paraben, sorbic acid, potassium sorbate, sodium methyl paraben and sodium ethyl paraben.
As a further embodiment of the invention, the collutory toothpaste comprises the following components, in weight percent:
0.4 to 5 percent of thickening agent;
8 to 25 percent of a friction agent;
15 to 75 percent of humectant;
2.5 to 20 percent of surfactant;
strontium salt and/or sylvite 0.2% -3.8%;
0.1 to 1 percent of acid-base buffering agent;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
In a fourth aspect, the present invention provides a process for preparing a collutory toothpaste according to the third aspect of the present invention, comprising the steps of:
(1) uniformly mixing water and a surfactant to prepare a solution A;
(2) uniformly mixing the humectant and the thickener to prepare a solution B;
(3) uniformly mixing a friction agent, strontium salt and/or potassium salt and an acid-base buffering agent 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 gargle toothpaste.
Different from the prior art, the technical scheme has the following beneficial effects:
the invention adopts the compatibility of nonionic high molecular compounds, high molecular polymers of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether 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 simultaneously enhances the dissolving capacity of the oral care products, and is specifically embodied in that: on one hand, the release of strontium ions can be accelerated, the strontium ions can be promoted to be completely released, and the anti-sensitive toothpaste containing the strontium ions can be promoted to have the maximum anti-dentin sensitivity effect; on the other hand, the toothpaste or the tooth gel is quickly dissolved in a proper amount of water and can be used as mouthwash, the use method is simpler and more convenient, and the dual purposes of the toothpaste and the tooth gel are realized. The toothpaste containing the thickening agent can help tooth-sensitive people to relieve dentine sensitivity, and has the functions of gargling water and toothpaste in the aspect of using methods.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the technical means in detail, the following detailed description is given with reference to specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified. The experimental procedures in the following examples are conventional unless otherwise specified.
First, a thickener according to a first aspect of the present invention is explained, which comprises: a) one or two of nonionic high molecular compound, acrylic acid bonded allyl sucrose or pentaerythritol allyl ether high molecular polymer; b) an inorganic gel.
The invention adopts the compatibility of nonionic high molecular compounds, high molecular polymers of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and inorganic gel as the thickening agent, has synergistic effect, is applied to oral care products, improves the stability of the oral care products, and simultaneously can enhance the dissolving capacity of the oral care products. Compared with a single thickening agent or a mixture thereof in a traditional thickening system such as sodium carboxymethylcellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum, guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan and the like, the composition of the nonionic polymer compound, the high polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether and the inorganic gel has more proper viscosity, can maintain a stable paste shape under a normal state after being applied to toothpaste or dental gel, can be quickly dissolved after being applied to an oral cavity or meeting water, improves the dissolving efficiency of strontium salt/potassium salt, and effectively relieves tooth sensitivity.
In the embodiment of the invention, the thickener comprises the following components in percentage by weight: 25 to 30 percent of nonionic macromolecular compound, 25 to 30 percent of macromolecular polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether, and 40 to 50 percent of inorganic gel.
In the embodiment of the invention, the thickener comprises the following components in percentage by weight: 20-40% of non-ionic high molecular compound and 60-80% of inorganic gel.
In the embodiment of the present invention, the nonionic polymer compound is selected from one or more of polyvinylpyrrolidone, polytetrafluoroethylene amine, polyacrylamide, and polyethyleneimine.
In the embodiment of the invention, the high molecular polymer of acrylic 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 and Carbopol Ultrez 20.
In the embodiment of the 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 present invention provides the use of a thickener according to the first aspect of the invention in the manufacture of an oral care product, for use in the manufacture of an oral care product.
Preferably, the oral care products include toothpastes and dental gels.
In a third aspect the present invention provides a collutory toothpaste comprising a thickener according to the first aspect of the present invention, an abrasive agent, a humectant, a surfactant, a strontium and/or potassium salt, an acid-base buffer, a food grade flavour, a preservative and water.
The toothpaste containing the thickening agent can keep good stability, the paste is not separated in the shelf life, and can be quickly dissolved after entering a cavity or meeting water, so that the dissolution of strontium ions is accelerated, and the tooth sensitivity is effectively relieved. The gargle toothpaste provided by the invention can help tooth-sensitive people to relieve dentine sensitivity in terms of efficacy, has the functions of gargle and toothpaste in terms of a using method, is more convenient and fast to use, and realizes dual purposes of toothpaste and toothpaste.
In an embodiment of the invention, the abrasive is selected from calcium hydrogen phosphate, aluminium hydroxide or silicon dioxide.
In the embodiment of the 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 thiosulfonate or cocamidopropyl betaine.
In the embodiment of the 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 the potassium salt can be mixed according to any proportion.
In the 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 selected from one or more of mint, spearmint oil, peppermint, menthyl lactate, refreshing mint and lemon essence.
In the embodiment of the invention, the preservative is selected from one or more of methyl paraben, ethyl paraben, propyl paraben, sodium benzoate, butyl paraben, sorbic acid, potassium sorbate, sodium methyl paraben and sodium ethyl paraben.
Of course, in some embodiments of the present invention, sweeteners may also be added to the colludable toothpaste. The sweetener can be selected from saccharin, glucose, sucrose, lactose, maltose, fructose, aspartame, sodium cyclamate, D-tryptophan, dihydrochalcone, and acesulfame. Pigments such as lemon yellow, brilliant blue, allura red, carmine, etc. may also be added.
In some embodiments of the present invention, green tea extract, spicebush flower extract, ginseng extract, licorice extract, etc. may also be added to the collutory toothpaste to induce an increase in saliva production in the oral cavity and to help the toothpaste dissolve rapidly in the oral cavity.
The toothpaste of the invention can be added with various additives according to the actual requirements, such as pigments, lemon yellow, brilliant blue, allure red, carmine and the like; 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 to 5 percent of thickening agent;
8 to 25 percent of a friction agent;
15 to 75 percent of humectant;
2.5 to 20 percent of surfactant;
strontium salt and/or sylvite 0.2% -3.8%;
0.1 to 1 percent of acid-base buffering agent;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
In a fourth aspect, the present invention provides a process for preparing a collutory toothpaste according to the third aspect of the present invention, comprising the steps of:
(1) uniformly mixing water and a surfactant to prepare a solution A;
(2) uniformly mixing the humectant and the thickener to prepare a solution B;
(3) uniformly mixing a friction agent, strontium salt and/or potassium salt and an acid-base buffering agent 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 gargle 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% polyethyleneimine 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 aluminium 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-tooth pastes
The 10 kinds of collutory toothpaste are prepared according to the following preparation method, the thickening agents in the embodiments 1-10 are respectively adopted to prepare the toothpaste in the embodiments 11-20, and the specific formula is shown in table 1.
The preparation method of the gargle toothpaste comprises the following steps:
(1) uniformly mixing water and a surfactant to prepare a solution A;
(2) uniformly mixing the humectant and the thickener to prepare a solution B;
(3) uniformly mixing a friction agent, strontium salt and/or potassium salt and an acid-base buffering agent 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 gargle toothpaste.
TABLE 1 mouthwash-rinse dentifrice formulations of examples 11-20
Figure BDA0003361527750000101
Figure BDA0003361527750000111
Comparative examples 1-9 toothpaste
This comparative example provides 9 different formulations of toothpaste, the specific formulation being 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 the humectant and the thickener to prepare a solution B;
(3) uniformly mixing a friction agent, strontium salt and/or potassium salt and an acid-base buffering agent 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 gargle toothpaste.
TABLE 2 toothpaste formulations for comparative examples 1-9
Figure BDA0003361527750000121
Figure BDA0003361527750000131
And (3) performance testing:
in order to compare the comprehensive performance of the gargle toothpastes of examples 11 to 20 and the toothpastes of comparative examples 1 to 9, the viscosity, stability and dissolution efficiency of the gargle toothpastes of examples 11 to 20 and the toothpastes of comparative examples 1 to 9 were tested, and the test results are shown in table 3.
Table 3 results of performance testing
Figure BDA0003361527750000132
Figure BDA0003361527750000141
As shown in table 3, compared with a single thickener or a mixture thereof in a 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 present invention adopts a nonionic polymer compound, a polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether, and an inorganic gel in combination as a thickener, has a more suitable viscosity, can well maintain stability and paste fineness during a shelf life, and does not divide water, does not return coarse during a shelf life, or only slightly divides water during a shelf life. Compared with comparative examples 1-5, comparative example 6 adopts the compounding of sodium carboxymethylcellulose (CMC) and carrageenan as the thickening agent, and has a good dentin sensitivity resistant effect; compared with comparative examples 1-6, the high molecular polymer (carbomer Carbopol 940) of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether, the inorganic gel (magnesium lithium silicate RD-1 glue) and the non-ionic high molecular compound (polyvinylpyrrolidone PVP K90) are respectively added in comparative examples 7-9, so that the performance is stable, and the dissolving speed is remarkably improved. Compared with comparative examples 1-5, the gargle toothpaste containing 2.0-5.0% of the thickening agent has stable performance, but has higher dissolution speed, can release strontium salt/sylvite more quickly, improves the use efficiency of the toothpaste, and fully exerts the anti-sensitivity effect of the toothpaste; compared with comparative examples 6-9, the gargle toothpaste containing 0.4% -2.0% of the thickening agent disclosed by the invention has relatively stable performance, and has a higher dissolution speed, so that strontium salt/potassium salt can be released more quickly, the use efficiency of the toothpaste is improved, and the anti-sensitivity effect of the toothpaste is fully exerted. In addition, the gargle toothpaste provided by the invention can help tooth-sensitive people to relieve dentine sensitivity, has the functions of gargle and toothpaste in the aspect of a using method, is more convenient and fast to use, and realizes dual purposes of toothpaste and toothpaste.
Test example 2 anti-sensitivity test of mouthwash toothpaste
In order to verify the tooth sensitivity resisting effect of the mouthwash toothpaste, examples 11-13, examples 15 and 17, comparative examples 1 and 6-9 were selected for clinical tests. The study was a randomized, double-blind, control, parallel clinical study. Patients with dentinal hypersensitivity (sensitive to touch, cold, hot, sour and sweet stimuli) were selected for clinical treatment, 298 subjects participated in a baseline examination, and 270 subjects completed the entire study for 8 weeks, each index being completed by the same subject. A total of 28 subjects were withdrawn halfway, the data not being included in the statistical analysis, the reason for the withdrawal of subjects was not related to the product of the study, and the baseline status of the subjects who completed the trial is shown in table 4.
TABLE 4 basic conditions of the subjects
Figure BDA0003361527750000151
The test verifies the tooth sensitivity resistance effect of the mouthwash toothpaste disclosed by the invention by adopting a probing sensitivity evaluation method and a cold air blowing sensitivity evaluation method.
(1) Evaluation of sensitivity to probing
A calibrated model 2000A yeapple electron pressure sensitive probe (yeapple research, Pittsford, NY) was used. The instrument can quantitatively measure the pressure (in grams) applied to the tooth surface. To test sensitivity, a probe is placed in contact with dentin exposed on the buccal surface of a selected tooth, placed at the enamel junction, probed using an initial preset amount of 10 grams of force, and then increased by 10 grams of force each time until the subject indicates an uncomfortable sensation with a maximum force of 80 grams. A high value of the probing force indicates a low level of tooth sensitivity.
(2) Evaluation of Cold air blowing sensitivity
An 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 an air compressor is 55-65 p.s.i., the blowing temperature is 19-21 ℃, and fingers are placed on adjacent teeth during blowing so as to avoid influencing the accuracy of results. The results were evaluated using the Schiff cold air sensitivity index and scored as follows: 0 ═ teeth and subjects did not respond to air stimuli; 1 ═ tooth and subject responded to air stimulation, but did not request cessation of stimulation; 2 ═ tooth and subject respond to air stimuli, requesting cessation or removal of stimuli; 3 ═ teeth and subjects responded to air irritation; the stimulus causes pain and the request stops. A low score for this parameter indicates a reduced sensitivity.
(3) The statistical analysis method comprises the following steps:
in this test, statistical analysis was performed on the obtained data using one-way analysis of variance (ANOVA) and t-test of SPSS16.0 statistical software, and using two-sided test, the test level α was 0.05.
The baseline, week 4, and week 8 examinations of subjects participating in the exploratory sensitivity test are shown in table 5. In the baseline examination, the average number of the probing sensitivity indexes of each group has no statistical difference; at week 4, there was no statistical difference between groups; at week 8, examples 11, 12, 13, 15, 17, and 6-9 all showed significant statistical differences compared to comparative example 1. Wherein, the average number of the probing tooth sensitivity indexes of the example 11 is reduced by 39.82 percent compared with the average number of the probing tooth sensitivity indexes of the comparative example 1, the average number of the probing tooth sensitivity indexes of the example 12 is reduced by 32.75 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the example 13 is reduced by 41.70 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the example 15 is reduced by 26.06 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the example 17 is reduced by 26.35 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the comparative example 6 is reduced by 22.53 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the comparative example 7 is reduced by 25.59 percent compared with the comparative example 1, the average number of the probing tooth sensitivity indexes of the comparative example 8 is reduced by 25.12 percent compared with the comparative example 1, and the average number of the probing tooth sensitivity indexes of the comparative example 9 is reduced by 24.27 percent compared with the comparative example 1.
TABLE 5 evaluation results of probing sensitivity
Figure BDA0003361527750000171
Figure BDA0003361527750000181
*P<0.05
The baseline, week 4, and week 8 examinations of subjects participating in cold air blowing are shown in table 6. In the baseline examination, the cold air blowing sensitivity value average of each group has no statistical difference; at week 4, there was no statistical difference between groups; at week 8, examples 11, 12, 13, 15, 17, and 6-9 all showed significant statistical differences compared to comparative example 1. Wherein, the average of the cold air blowing sensitivity values of the example 11 is reduced by 46.15% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the example 12 is reduced by 35.90% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the example 13 is reduced by 41.03% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the example 15 is reduced by 32.05% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the example 17 is reduced by 30.77% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the comparative example 6 is reduced by 26.92% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the comparative example 7 is reduced by 30.77% compared with that of the comparative example 1, the average of the cold air blowing sensitivity values of the comparative example 8 is reduced by 30.77% compared with that of the comparative example 1, and the average of the cold air blowing sensitivity values of the comparative example 9 is reduced by 29.49% compared with that of the comparative example 1.
TABLE 6 evaluation results of Cold air blowing sensitivity
Figure BDA0003361527750000182
Figure BDA0003361527750000191
*P<0.05
The clinical treatment results show that, compared with the comparative example 1, the comparative example 6 adopts the compounding of the sodium carboxymethylcellulose CMC and the carrageenan as the thickening agent, and has better dentin sensitivity resistance effect. In comparative examples 7-9, a high molecular polymer (carbomer Carbopol 940) of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether, an inorganic gel (lithium magnesium silicate RD-1 glue) and a non-ionic high molecular compound (polyvinylpyrrolidone PVP K90) are respectively adopted to be compounded with the traditional glue, and compared with comparative examples 1 and 6, the dentin sensitivity resistant effect is better. However, the collutory toothpaste provided by the present invention (examples 11 to 13, 15, and 17) uses a nonionic polymer compound, a polymer of acrylic acid-bonded allyl sucrose or pentaerythritol allyl ether, and an inorganic gel in combination as a thickener, and has a better dentin sensitivity resistance than a single thickener or a mixture thereof in a conventional thickening system such as sodium carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), xanthan gum, guar gum, carboxymethyl hydroxypropyl cellulose, carrageenan, or a mixture of a polymer of acrylic acid-bonded allyl sucrose or pentaerythritol allyl ether, an inorganic gel, and a mixture of a nonionic polymer compound and a conventional thickening system. The collutory toothpaste provided by the present invention has no side effects observed in the clinical study.
It should be noted that, although the above embodiments have been described herein, the scope of the present invention is not limited thereby, and the technical parameters not described in detail herein may be changed within the range of the listed parameters, so that the technical effects similar to or similar to the above embodiments can be obtained, and still fall within the scope of the present invention. Therefore, based on the innovative concepts of the present invention, the technical solutions of the present invention can be directly or indirectly applied to other related technical fields by making changes and modifications to the embodiments described herein or by using equivalent structures or equivalent processes performed in the present specification, and are included in the scope of the present invention.

Claims (10)

1. A thickener, comprising: a) one or two of nonionic high molecular compound, acrylic acid bonded allyl sucrose or pentaerythritol allyl ether high molecular polymer; b) an inorganic gel.
2. Thickener according to claim 1, comprising, in weight percent: 25 to 30 percent of nonionic macromolecular compound, 25 to 30 percent of macromolecular polymer of acrylic acid bonded allyl sucrose or pentaerythritol allyl ether, and 40 to 50 percent of inorganic gel.
3. Thickener according to claim 1, comprising, in weight percent: 20-40% of non-ionic high molecular compound and 60-80% of inorganic gel.
4. The thickener according to claim 1, wherein the nonionic polymer compound is selected from one or more of polyvinylpyrrolidone, polytetrafluoroethylene amine, polyacrylamide and polyethyleneimine.
5. Thickener according to claim 1, wherein the high molecular weight polymer of acrylic-bonded allyl sucrose or pentaerythritol allyl ether is selected from the group consisting 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 Ultrez20 in combination of one or more thereof.
6. The thickener of claim 1, wherein the inorganic gel is selected from the group consisting of lithium magnesium silicate, magnesium aluminum silicate, montmorillonite powder, sodium bentonite, and combinations thereof.
7. Use of a thickener according to any of claims 1 to 6 in the manufacture of an oral care product, wherein the thickener is used in the manufacture of an oral care product;
preferably, the oral care products include toothpastes and dental gels.
8. A collutory toothpaste, comprising the thickener, abrasive, humectant, surfactant, strontium salt and/or potassium salt according to any one of claims 1 to 6, acid-base buffer, food grade flavor, preservative and water.
9. The colludable toothpaste according to claim 8, comprising the following components in weight percent:
0.4 to 5 percent of thickening agent;
8 to 25 percent of a friction agent;
15 to 75 percent of humectant;
2.5 to 20 percent of surfactant;
strontium salt and/or sylvite 0.2% -3.8%;
0.1 to 1 percent of acid-base buffering agent;
1.0 to 3.0 percent of food-grade essence;
0.1 to 0.4 percent of preservative;
the balance of water.
10. A process for preparing a gargle toothpaste according to claim 8 comprising the steps of:
(1) uniformly mixing water and a surfactant to prepare a solution A;
(2) uniformly mixing the humectant and the thickener to prepare a solution B;
(3) uniformly mixing a friction agent, strontium salt and/or potassium salt and an acid-base buffering agent 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 gargle toothpaste.
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