Oral liquid composition comprising sodium fluoride, sodium metaphosphate, zinc salt, and chelating agent

The oral liquid composition stabilizes zinc ions using sodium fluoride, sodium metaphosphate, and a chelating agent to address stability and irritation issues, ensuring effective teeth whitening and plaque prevention with reduced oral discomfort.

WO2026095544A1PCT designated stage Publication Date: 2026-05-07LG HOUSEHOLD & HEALTH CARE LTD
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Patent Information

Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
LG HOUSEHOLD & HEALTH CARE LTD
Filing Date
2025-10-28
Publication Date
2026-05-07

AI Technical Summary

Technical Problem

Existing oral compositions containing sodium metaphosphate and zinc salts face issues with zinc ion stability and oral irritation due to the formation of precipitates and astringent action, limiting their effectiveness and user comfort.

Method used

An oral liquid composition comprising sodium fluoride, sodium metaphosphate, a zinc salt, and a chelating agent, specifically disodium ethylenediaminetetraacetic acid, is formulated to stabilize zinc ions through chelation, maintaining stability and minimizing irritation by preventing precipitate formation and optimizing pH conditions.

Benefits of technology

The composition effectively maintains zinc ion stability, prevents plaque formation, reduces bad breath, and minimizes oral irritation while enhancing teeth whitening efficacy and user satisfaction.

✦ Generated by Eureka AI based on patent content.

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Abstract

The oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent of the present invention maintains stability of zinc ions within the formulation while exhibiting an effect of reducing irritation in the oral cavity. Accordingly, the composition can be effectively used for: tooth whitening; prevention, alleviation, or treatment of dental caries, halitosis, and dental plaque; and irritation relief.
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Description

Oral liquid composition comprising sodium fluoride, sodium metaphosphate, zinc salt, and a chelating agent

[0001] The present invention relates to an oral liquid composition, specifically comprising sodium fluoride, sodium metaphosphate, a zinc salt, and a chelating agent, and to an oral liquid composition that maintains the stability of zinc ions within the formulation while minimizing irritation in the oral cavity.

[0002]

[0003] A bright, white smile greatly helps in building confident interpersonal relationships. Furthermore, a confident smile makes a first impression appear even more positive.

[0004] Recently, as interest in teeth whitening has grown beyond oral health, toothpaste formulations with teeth whitening effects are being released.

[0005] Teeth whitening is a dental procedure that makes teeth whiter and brighter without damaging teeth discolored by various causes, and recently, teeth whitening products that can be used at home are being developed.

[0006] While there are various types and methods of teeth whitening, most utilize high concentrations of hydrogen peroxide to bleach teeth by oxidizing staining agents; this method has been used in dentistry for over 100 years and its whitening effect has been proven. Peroxide acts as an oxidizing agent that alters or decomposes staining substances to achieve whitening; however, due to its high reactivity, there have been limitations in storage. Furthermore, the oxidation reaction using hydrogen peroxide is highly irritating and causes strong irritation if it comes into contact with the lips, gums, or tongue.

[0007] Accordingly, research on sodium metaphosphate is actively being conducted as an excellent ingredient for removing discoloration components and inhibiting and preventing re-discoloration as a substitute for hydrogen peroxide, but there was a problem in that as the content of sodium metaphosphate increased, it caused irritation in the oral cavity due to its characteristic astringent action.

[0008] In addition, zinc salts are known to be an ingredient that can prevent plaque formation and bad breath by inhibiting the growth of harmful bacteria in the oral cavity, and can protect against external stimuli by forming a protective film on the tooth surface.

[0009] However, in the case of formulations containing sodium metaphosphate and zinc salts, zinc ions (Zn) over time 2+ Phosphorus (P) in which ) is ionized - There were problems with reduced stability, such as the formation of precipitates when combined with ).

[0010]

[0011] Against this backdrop, the inventors, through diligent research efforts to solve these problems, confirmed that an oral composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent maintains the stability of zinc ions within the formulation while minimizing irritation in the oral cavity, thereby completing the present invention.

[0012]

[0013] The object of the present invention is to provide an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent.

[0014] Another objective of the present invention is to provide an oral product comprising an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent.

[0015] Another objective of the present invention is to provide a method for preparing an oral liquid composition comprising the step of stirring and mixing a chelating agent and a zinc salt in purified water.

[0016] Another objective of the present invention is to provide an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, zinc salt, and a chelating agent for use in teeth whitening, prevention or improvement of tooth decay, bad breath, and plaque, and irritation relief.

[0017]

[0018] The oral liquid composition of the present invention, comprising sodium fluoride (NaF), sodium metaphosphate, zinc salt, and a chelating agent, has the effect of maintaining the stability of zinc ions within the formulation while minimizing irritation in the oral cavity.

[0019]

[0020] Figure 1 shows the results of a qualitative analysis of a precipitate of Comparative Example 1 composition that does not contain disodium ethylenediaminetetraacetic acid, a chelating agent, according to one embodiment of the present invention.

[0021] Figure 2 shows the results of a qualitative analysis of the inorganic components of the precipitate of Comparative Example 1 composition, which does not contain disodium ethylenediaminetetraacetic acid, a chelating agent, according to one embodiment of the present invention.

[0022]

[0023] According to one embodiment of the present invention, an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent is provided.

[0024] In addition, according to one embodiment of the present invention, an oral product comprising the above-mentioned liquid composition for oral use is provided.

[0025] In addition, according to one embodiment of the present invention, a method for preparing an oral liquid composition is provided, comprising the step of stirring and mixing a chelating agent and a zinc salt in purified water.

[0026]

[0027] This is explained in detail as follows. Meanwhile, each description and embodiment disclosed in the present invention may be applied to each other description and embodiment. That is, all combinations of the various elements disclosed in the present invention fall within the scope of the present invention. Furthermore, the scope of the present invention should not be considered limited by the specific descriptions provided below.

[0028]

[0029] In the present invention, the liquid composition for oral use may be used interchangeably with oral care compositions, etc., and when used on teeth, it may refer to a composition capable of exhibiting a teeth whitening effect, a cavity prevention effect, and a plaque and bad breath prevention effect.

[0030] In addition, in the present invention, the oral liquid composition may refer to a composition provided in liquid form containing a solvent.

[0031] In addition, in the present invention, tooth whitening may mean removing or pushing out a substance that attaches to or penetrates the tooth surface and enamel to cause a discoloration effect, or removing the discoloration effect by modifying the chemical structure of said substance.

[0032] In addition, in the present invention, tooth decay refers to the destruction of tooth enamel or dentin by harmful bacteria, such as caries bacteria, resulting in holes and black decay, and can be used interchangeably with dental caries.

[0033] In addition, in the present invention, bad breath refers to an unpleasant odor emanating from the mouth due to volatile sulfur compounds (VSCs) produced by the decomposition of bacterial proteins in the mouth.

[0034] In addition, in the present invention, plaque refers to a microbial film or mass of bacteria growing on the surface of the mouth, and calcium ions present in saliva can combine with plaque to develop into tartar.

[0035] In addition, in the present invention, oral irritation or oral irritation may include any irritation phenomena, such as swelling, redness, pain, etc., that appear on teeth and gums.

[0036] In addition, the term "alleviation" in the present invention means that oral irritation, etc., as described above is reduced or alleviated, and can be understood as a broad concept including improvement, prevention, treatment, etc.

[0037]

[0038] One aspect of the present invention is an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent.

[0039] In the present invention, the chelating agent may stabilize zinc ions in the oral liquid composition.

[0040] In the present invention, sodium fluoride (NaF) is a component that can help prevent tooth decay by forming a film on the tooth surface, thereby preventing tooth decay caused by acid produced by tooth decay bacteria, and inhibiting the enzymatic activity of bacteria. When sodium fluoride (NaF) is included in an oral composition, it can exhibit effects such as strengthening tooth structure and increasing acid resistance.

[0041] The sodium fluoride (NaF) may be included in a ratio of 0.01 to 2.0 weight% relative to the total weight of the oral composition, specifically in a ratio of 0.02 weight%, and by providing an oral composition containing sodium fluoride (NaF) within the above-described range, a high caries prevention effect can be achieved.

[0042]

[0043] In the present invention, sodium metaphosphate is generally (NaPO3) n When the sodium metaphosphate is included in an oral liquid composition, it is a compound represented by the molecular formula, and compared to other polyphosphates, it may have a superior effect in removing coloring components and prevent discoloration.

[0044] The above sodium metaphosphate may include sodium hexametaphosphate (SHMP). The sodium hexametaphosphate (SHMP) can prevent discoloration by pushing out and removing staining substances from the tooth surface, and then adsorbing to the tooth surface to block the staining substances. Although phosphates containing sodium metaphosphate are known for use in teeth whitening, there was a problem in that if the pH conditions and content ranges according to the type of phosphate were not met, it could cause a decrease in whitening efficacy, a decline in usability, and oral irritation. However, in one embodiment of the present invention, appropriate pH conditions and an optimal content range for including sodium hexametaphosphate (SHMP) in an oral liquid composition were derived. Specifically, to enhance the effect of removing coloring substances, it was derived that the sodium hexametaphosphate (SHMP) can be included in a ratio of 1 to 3.5 weight%, specifically 1 to 3.0 weight%, more specifically 1.5 to 2.5 weight%, and most specifically 2 weight% relative to the total weight of the oral liquid composition of the present invention under pH conditions of 4 to 6. When sodium hexametaphosphate (SHMP) is added to the oral liquid composition of the present invention under the above pH conditions and content, it can exhibit excellent coloring component removal and coloring prevention effects while having less irritation and high user satisfaction.

[0045]

[0046] In the present invention, the zinc salt may include zinc gluconate. The zinc gluconate has the effect of protecting teeth from external stimuli by forming a protective film on the tooth surface. In addition, toothpaste containing zinc gluconate is known to have an effect of preventing or improving bad breath by inhibiting volatile sulfur compounds (VSCs), which are bad breath components generated during saliva fermentation, and by effectively removing VSCs derived from harmful oral bacteria such as P. gingivalis, S. mutans, and F. nucleatum (Choi et al., Reduction of oral malodor with toothpaste containing zinc gluconate, tetrasodium pyrophosphate and supercritical CO2 extract of magnolia, 2022).

[0047] The zinc gluconate above may be included in a ratio of 0.01 to 1.0 weight%, specifically 0.05 to 0.5 weight%, more specifically 0.1 to 0.4 weight%, even more specifically 0.1 to 0.3 weight%, and most specifically 0.15 weight% relative to the total weight of the oral liquid composition of the present invention, but is not limited thereto. By providing zinc gluconate in the oral liquid composition within the above-described range, excellent plaque formation prevention and bad breath prevention effects can be exhibited without affecting the whitening effect of sodium fluoride (NaF) and sodium metaphosphate.

[0048]

[0049] In the present invention, a chelating agent refers to a ligand capable of forming a coordinate bond with a metal ion at two or more sites, and the chelating agent can stabilize zinc ions in the composition.

[0050] In addition, in the present invention, "zinc ion stabilization" refers to zinc ions (Zn) within the composition. 2+ ) forms a chelate through coordination bonding with a chelating agent, and phosphorus ions (P - It prevents binding with ) and precipitation formation, and thereby zinc ions (Zn 2+ It means maintaining the content of ) stably.

[0051] In the case where a conventional oral liquid composition contains sodium metaphosphate and zinc salt, zinc ions (Zn) over time 2+ ) Phosphorus ions (P) in this composition - There was a problem in that the stability of zinc ions was reduced, such as the formation of a white precipitate upon combining with ). However, in one embodiment of the present invention, when an oral liquid composition is prepared by stirring and dissolving a chelating agent with a zinc salt and then mixing it with sodium metaphosphate, the phosphorus ions (P) dissolved in the sodium metaphosphate - Due to ), even under pH conditions of 5 or lower, zinc ions (Zn) in the composition 2+ The content of ) can be stably maintained, and it was confirmed that no precipitate precipitates when verifying stability over accelerated time; accordingly, zinc ions (Zn 2+ It was confirmed that the excellent plaque formation and bad breath prevention effects of ) can be maintained.

[0052] The above chelating agent may include disodium ethylenediaminetetraacetic acid (disodium EDTA).

[0053] The above-mentioned disodium ethylenediaminetetraacetic acid is a sodium salt of ethylenediaminetetraacetic acid (EDTA), which acts as a chelating agent binding to divalent metal ions such as calcium and magnesium. It is known to have a metal ion chelating effect that prevents oxidizing substances causing corrosion and rancidity of the composition, as well as an effect that controls viscosity. Furthermore, the above-mentioned disodium ethylenediaminetetraacetic acid may be included in a ratio of 0.1 to 1.5 weight%, specifically 0.1 to 1.2 weight%, and more specifically 0.1 to 1 weight%, relative to the total weight of the oral liquid composition of the present invention. By providing the above-mentioned disodium ethylenediaminetetraacetic acid to the oral liquid composition within the aforementioned range, zinc ions (Zn) within the composition 2+ It can stabilize ) while also exhibiting low stimulation.

[0054]

[0055] In the present invention, the pH of the oral liquid composition may be 4 to 6, specifically 4 to 5.5, and most specifically 4 to 5. The oral liquid composition of the present invention may exhibit the best stain removal effect under the above pH range conditions. In particular, under the above-mentioned pH range conditions, the stain removal effect and stain prevention effect of sodium hexametaphosphate (SHMP) included in the oral liquid composition may be enhanced. Under the above-mentioned pH range conditions, the sodium ions or hydrogen ions of sodium hexametaphosphate (SHMP) form a strong affinity with calcium ions exposed on the tooth surface, adhering to the tooth enamel surface. This destroys the pellicle on the enamel, pushes out and removes contaminants causing staining, and forms a sodium hexametaphosphate (SHMP) coating film on the tooth surface, thereby exhibiting an excellent effect in preventing new extrinsic staining. Therefore, an appropriate pH range condition is required for appropriate binding strength with metal ions. For example, if the pH of the oral liquid composition is lower than 4, sodium hexametaphosphate (SHMP) decomposes, reducing the active ingredient that exerts a whitening effect, and thus reducing the ability of sodium hexametaphosphate (SHMP) to bind with metal ions, whereas if the pH of the oral liquid composition is higher than 6, the binding of sodium hexametaphosphate (SHMP) may be inhibited due to increased competition for metal ions, so the whitening effect may be best within the above-described pH range conditions.

[0056] In addition, a pH adjuster may be additionally included to maintain the pH of the oral liquid composition at 4 to 6 by implementing a pH buffering system. The pH adjuster may include one or more of citric acid, sodium citrate, tartaric acid, sodium tartrate, phosphoric acid, sodium phosphate, sodium acid pyrophosphate, sodium saccharin, calcium lactate, sodium monophosphate, sodium triphosphate, potassium monophosphate, potassium triphosphate, sodium bicarbonate, potassium pyrophosphate, etc. The pH adjuster may be included in a ratio of 0.01 to 2.0 weight%, specifically 0.01 to 1.0 weight%, and more specifically 0.01 to 0.5 weight% relative to the total weight of the oral liquid composition. If the oral liquid composition contains less than 0.01 weight% of the pH adjuster, a pH buffering effect cannot be expected, and if it contains more than 2 weight% of the pH adjuster, a decrease in usability may occur.

[0057]

[0058] In the present invention, the liquid composition for oral use may additionally include one or more selected from the group consisting of surfactants, humectants, flavoring agents, sweeteners, preservatives, binders, foaming agents, whitening agents, fragrances, colorants, solubilizers, and solvents.

[0059] Surfactants are ingredients characterized by possessing both hydrophobic and hydrophilic properties within a single molecule; they effectively remove organic substances contaminated by greasy foods and assist in the cleaning of pellicles. In the case of sodium hexametaphosphate, it forms a coating film on the tooth surface due to its high affinity for calcium ions present on the tooth surface; however, since the presence of organic contaminants hinders effective contact with the tooth surface, using a surfactant to remove them can enhance the stain removal and inhibition effects.

[0060] In addition, the surfactant may be included in a ratio of 0.01 to 4 weight%, specifically 0.01 to 3 weight%, more specifically 0.01 to 2 weight%, and most specifically 0.01 to 1.5 weight% relative to the total weight of the oral liquid composition. Since surfactants have a contact affinity with oral mucosa as well as tooth surfaces, including an excess amount of 3.0 weight% or more may cause oral irritation. Therefore, by providing the surfactant to the oral liquid composition within the above-described range, the stain removal and inhibition effects can be enhanced without oral irritation.

[0061] A humectant is a component that prevents the liquid composition for oral use from drying out and maintains a moist state. The humectant may include, but is not limited to, one or more selected from the group consisting of polyethylene glycol, glycerol, propylene glycol, ethylene glycol, polypropylene glycol, sorbitol, and mixtures thereof. Specifically, it may include one or more selected from the group consisting of polyethylene glycol 200 to 600, glycerol, propylene glycol, ethylene glycol, polypropylene glycol, and mixtures thereof. Furthermore, as a liquid humectant, petroleum-based oils, animal and vegetable oils, synthetic lubricants, etc., may be used, and liquid polyols may be used in terms of the stability of the composition and excellent usability. Alternatively, the wetting agent is not limited to liquid polyols and may also include high molecular weight polyols such as polyethylene glycol and polypropylene glycol, which have a polymeric form and can exist as a solid at room temperature due to intramolecular interactions of the polymer at a certain molecular weight or higher, but can be liquefied by controlling the manufacturing temperature and maintained in a stable state after commercialization.

[0062] Solubilizers are used to help dissolve components that are not easily soluble in water. Examples of solubilizers that may be used include poloxamer, HCO-40, liquid olive oil, polysorbate, and PEG-40 hydrogenated castor oil.

[0063] Flavoring agents are used to maintain a fresh sensation by remaining in the oral cavity and continuously releasing a scent, and for effects such as cleanliness and the elimination of bad breath. Flavoring agents may include mints such as peppermint and spearmint, wintergreen, methyl salicylate, eugenol, melon, strawberry, orange, vanillin, etc.

[0064] Sweeteners may be added to overcome the basic taste that the formulation may have. Sweeteners can serve to sustain saliva production by remaining in the oral cavity and continuously providing a taste. As sweeteners, one or more types of saccharin, sucralose, sugar, xylitol, sorbitol, lactose, mannitol, maltitol, erythritol, aspartame, taurine, saccharin salts, D-tryptophan, stevioside, enzyme-treated stevia, etc., may be used.

[0065] Benzoic acid, methylparaben, propylparaben, sodium benzoate, etc. can be used as preservatives.

[0066] A solvent is a substance that dissolves a solute in a formulation and can be used interchangeably with a solvent. Purified water and alcohols with 1 to 4 carbon atoms, such as methanol and ethanol, may be used as solvents.

[0067]

[0068] Another aspect of the present invention is an oral product comprising an oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, zinc salt, and a chelating agent.

[0069] The oral product of the present invention may be one or more selected from the group consisting of liquid toothpaste, oral spray, oral rinse, oral ointment, oral rinse, and gargling product, but is not limited thereto.

[0070] In the present invention, the oral product may be distributed by storing the oral liquid composition of the present invention in a container. The container may be provided to include an applicator, such as a brush or tip, capable of applying the composition, and if necessary, the applicator may be provided separately from the container. Additionally, an instruction manual describing the method of use may be provided together with the container or the composition.

[0071] Suitable additives, carriers, etc., may be additionally included in the oral liquid composition for application to the above oral product, and said additives and carriers, etc., may be appropriately selected and combined by those skilled in the art.

[0072] Oral products manufactured using the composition of the present invention can be manufactured using methods commonly used in the industry.

[0073]

[0074] Another aspect of the present invention is a method for preparing an oral liquid composition comprising the step of stirring and mixing a chelating agent and a zinc salt in purified water.

[0075] The above terms "sodium fluoride (NaF)," "sodium metaphosphate," "zinc salt," "chelating agent," and "zinc ion stabilization" are as described in the above oral liquid composition, and the specific composition of the method for manufacturing the oral liquid composition will be described below.

[0076] In the present invention, stirring and mixing the chelating agent and the zinc salt in purified water in the above step is performed so that zinc ions (Zn) within the composition are formed by the formation of a chelate through the coordination bonding of the chelating agent and the zinc salt. 2+ ) is a person (P - The purpose is to prevent binding with ) and forming precipitates, thereby inducing stabilization of zinc ions within the composition.

[0077] In one embodiment of the present invention, a liquid oral composition was prepared by stirring and mixing a chelating agent and a zinc salt in purified water, then stirring and mixing with sodium metaphosphate or stirring and mixing together. As a result of confirming the stability of zinc ions in the composition, it was confirmed that the composition prepared by stirring and mixing the chelating agent and the zinc salt together with sodium metaphosphate showed that zinc ions combined with phosphorus to form a precipitate and the zinc ion content decreased under pH 4 to 5 conditions, whereas the composition prepared by stirring and mixing the chelating agent and the zinc salt in purified water and then stirring and mixing with sodium metaphosphate showed a higher zinc ion content and no precipitate formed under pH 4 to 5 conditions, thus confirming that the stabilization of zinc ions was superior. Furthermore, it was confirmed that it is possible to exhibit low irritation and improved user satisfaction while maintaining the stability of zinc ions.

[0078]

[0079] In the foregoing, a zinc ion-stabilized liquid oral composition according to one embodiment of the present invention was examined. Below, based on experimental examples and results of the liquid oral compositions according to the examples and comparative examples, the advantageous effects of the present invention are confirmed.

[0080]

[0081] Experimental Example 1: Preparation of the composition of the example and preparation example

[0082] An oral liquid composition comprising sodium metaphosphate (SHMP), sodium fluoride (NaF), zinc gluconate, and disodium ethylenediaminetetraacetic acid was prepared as follows.

[0083] Specifically, zinc gluconate and disodium ethylenediaminetetraacetic acid were stirred and mixed in purified water, and after sufficiently stirring and solubilizing the fragrance, ethanol, and solubilizing agent, the remaining components, including sodium fluoride, glycerin, phosphoric acid, sodium citrate, sodium saccharin, sodium hexametaphosphate (SHMP), and disodium phosphate (SAPP), were added and stirred for about 30 minutes to prepare a composition. At this time, poloxamer and HCO-40 were used as solubilizing agents.

[0084] The specific components and content of Example 1 are shown in Table 1 below as a representative example. Subsequently, the example and comparative example compositions used in the experiment were prepared by varying the type and content of the chelating agent and whether the chelating agent and zinc salt were pre-stirred in the above manufacturing method.

[0085] Ingredient Name Example 1 NaF 0.02 Glycerin 6 Ethanol 7 Fragrance 0.22 Phosphate 0.1 Sodium Citrate 0.01 Sodium Saccharin 0.04 Solubilizer 1 SHMP 2 SAPP 0.2 Disodium EDTA 0.15 Zinc Gluconate 0.15 Water Purification Amount Appropriate Amount Total 100

[0086]

[0087] Experimental Example 2: Confirmation of the effect of adding a chelating agent to the composition

[0088] Unlike Example 1, Comparative Example 1 was prepared without disodium ethylenediaminetetraacetic acid, which is a chelating agent, and the precipitate was qualitatively analyzed using FT-IR spectroscopy and SEM-EDS analysis methods, and the results are shown in FIGS. 1 and 2.

[0089] At this time, an FT-IR instrument (PerkinElmer, Spectrum Two) was used to confirm whether the precipitate matched zinc gluconate, and to confirm the inorganic components of the precipitate, measurements were taken using a scanning electron microscope (Hitachi, S-4800) equipped with an energy dispersive spectrometer (HORIBA, EMAX x-act).

[0090] As a result, as can be seen in Figure 1, if the precipitate were zinc gluconate, the two graphs should match, but since they do not match, it was confirmed that the precipitate is not zinc gluconate.

[0091] And, as can be seen in Figure 2, phosphorus (P), zinc (Zn), and oxygen (O) were detected in the precipitate, so it was confirmed that the precipitate was formed by the combination of phosphorus and zinc.

[0092] Therefore, in the case of a composition containing sodium metaphosphate and zinc gluconate, as time passes, zinc ions (Zn 2+ Phosphorus (P) that is ionized within this composition - While the stability of zinc ions is reduced because a white precipitate forms upon combination with ), a composition additionally containing a chelating agent forms a chelate through coordinate bonding with zinc ions, thereby [releasing] the zinc ions (Zn 2+ Maintaining the ionization of ), and phosphorus (P - It was confirmed that zinc ions can be stabilized within the composition by preventing precipitation through reaction with ).

[0093]

[0094] Experimental Example 3: Confirmation of formulation stability, irritation, and satisfaction with usability

[0095] 3-1. Confirmation of Formulation Stability

[0096] Accelerated stability tests were performed at a pH of 5 or lower according to the type of chelating agent when preparing an oral liquid composition.

[0097] The above accelerated time-lapse stability test was conducted to verify the stability of the oral liquid composition within its shelf life (3 years) in the short term. Specifically, the composition was placed in a transparent container and stored in a chamber maintained at room temperature and 50°C for 4 weeks to check the stability of the formulation (pH, presence or absence of precipitate) at the beginning and after 4 weeks, and this is shown in Table 2 below.

[0098] At this time, the compositions of Example 1 and Comparative Examples 2 to 4 were prepared with only the chelating agent used being different, while the remaining composition and content were identical.

[0099] Classification Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Raw Material Composition NaF (%) 0.02 0.02 0.02 0.02 SHMP (%) 2 2 2 Zinc Gluconate (%) 0.15 0.15 0.15 0.15 Chelating Agent (0.15%) Disodium EDTA TSPPTKPP EDTA Accelerated Time Initial pH 4.65 65.54 Weeks 50 ℃ pH 4.5 4.7 65 Presence of Precipitate None Presence Presence None

[0100] As a result of conducting a comparative evaluation based on a chelating agent having a blocking function for polyvalent metal ions, as can be seen in Table 5 above, in the case of Example 1 containing disodium ethylenediaminetetraacetic acid (Disodium EDTA), the initial pH and the pH change pattern over accelerated time satisfied the conditions of 4 to 5 and no precipitate was formed; however, in the case of Comparative Examples 2 to 4 containing tetrasodium pyrophosphate (TSPP), tetrapotassium pyrophosphate (TKPP), and ethylenediaminetetraacetic acid (EDTA), it was confirmed that the pH change pattern did not satisfy the conditions of 4 to 5 or precipitate was formed. Therefore, it was confirmed that disodium ethylenediaminetetraacetic acid is the most suitable chelating agent for preparing the oral liquid composition of the present invention.

[0101]

[0102] Next, the stability of the formulation was checked according to the content of disodium ethylenediaminetetraacetic acid and whether the chelating agent and zinc salt were stirred.

[0103] Specifically, the composition was placed in a transparent container and stored at room temperature and in a 50°C maintaining chamber for 4 weeks to check the stability of the formulation (pH, zinc ion content, presence or absence of precipitate) at the beginning and after 4 weeks, and the results are shown in Tables 3 and 4 below.

[0104] In this case, the compositions of the example and comparative example were prepared identically in composition and content, differing only in the content of the chelating agent or whether pre-stirring with the zinc salt occurred during preparation.

[0105] Classification Comparative Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 5 Disodium EDTA, Zinc Gluconate Stirring Status (Y / N) NYYYYY Raw Material Composition NaF (%) 0.0 20.0 20.0 20.0 20.0 20.0 SHMP (%) 222222 Zinc Gluconate (%) 0.1 50.1 50.1 50.1 50.1 50.1 Disodium EDTA (%) 00.1 0.2 0.5 12 pH Initial 4.6 4.5 4.5 4.6 4.6 50℃ 4 weeks 5.0 4.7 4.5 4.5 4.5 4.5 Overtime (50℃ 4 weeks) Zinc Analysis (%) 15 86 105 102 101 100 Presence of Precipitate Presence

[0106] Classification Comparative Example 6 Comparative Example 7 Comparative Example 8 Comparative Example 9 Comparative Example 10 Disodium EDTA, Zinc Gluconate Stirring Status (Y / N) NNNNN Raw Material Composition NaF (%) 0.0 20.0 20.0 20.0 20.0 SHMP (%) 22222 Zinc Gluconate (%) 0.1 50.1 50.1 50.1 50.1 Disodium EDTA (%) 0.1 0.2 0.5 12 pH Initial 4.6 4.6 4.5 4.5 4.5 50°C 4 Weeks 5.0 4.9 4.8 4.8 4.9 Over Time (50°C 4 Weeks) Zinc Analysis (%) 33 52 58 65 68 Presence of Precipitate None None None None None

[0107] Upon verification, as can be seen in Tables 3 and 4 above, it was confirmed that when a 4-week accelerated time test was conducted, a white precipitate formed and the pH increased in Comparative Example 5, which did not contain disodium ethylenediaminetetraacetic acid, and in particular, zinc ions (Zn 2+ ) decreases rapidly, causing zinc ions (Zn 2+ It was confirmed that the stability of ) is significantly low.

[0108] In contrast, no precipitate was generated in compositions containing disodium ethylenediaminetetraacetic acid; however, in cases where zinc gluconate and disodium ethylenediaminetetraacetic acid are prepared without prior stirring, as in Comparative Examples 6 to 10, zinc ions (Zn) after time 2+ It was confirmed that the content of ) decreased and the pH increased slightly.

[0109] However, in the case of Examples 2 to 5, which were prepared by pre-stirring zinc gluconate and disodium ethylenediaminetetraacetic acid while containing disodium ethylenediaminetetraacetic acid, no precipitate was generated and the pH condition of 4 to 5 was satisfied, so that the zinc ions (Zn) in the formulation 2+ It was confirmed that the stability of ) is excellent.

[0110] Based on these results, when disodium ethylenediaminetetraacetic acid is included in a ratio of 0.1 to 1 weight% and pre-stirred with zinc gluconate, no precipitate is formed even under pH 4 to 5 conditions, and zinc ions (Zn 2+ Since the content of ) can be stably maintained, the zinc ion (Zn) in the composition 2+ It was confirmed that the stability of ) can be improved.

[0111]

[0112] 3-2. Verification of Satisfaction with Irritation and Usability

[0113] Sensory evaluation according to the content of disodium ethylenediaminetetraacetic acid was confirmed in terms of irritation and satisfaction with use. Specifically, 20 participants were asked to use each composition with sufficient time intervals, and then a survey was conducted on irritation and satisfaction with use.

[0114] At this time, the survey evaluation involved providing each applicant with a comparative example composition to use, and then having them express on a 5-point scale whether they felt stimulation during use and to what extent they were satisfied with the sensation of use, which is shown in Table 5 below.

[0115] At this time, the closer the stimulation evaluation is to 5 points, the higher the stimulation, and the closer the satisfaction evaluation is to 5 points, the higher the satisfaction.

[0116] Classification Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 Comparative Example 9 Comparative Example 10 User Experience Satisfaction 4.5 4.6 4.2 3.7 3.1 2.3 1.5 3.2 3.5 3.2 3.0 1.4 Irritation 2 2.1 2.2 2.6 2 3.5 1.9 2.1 2.2 8 3.7

[0117] As a result, as can be seen in Table 5 above, when 0.1 to 1% of disodium ethylenediaminetetraacetic acid is included (Examples 1 to 5), an irritation sensation of less than 3 points and a satisfaction of 3 points or more of usability are shown, whereas when disodium ethylenediaminetetraacetic acid is not included (Comparative Example 1), when an excess amount of 2% is included (Comparative Example 5), or when the chelating agent and zinc salt are not stirred (Comparative Examples 6 to 10), a high irritation sensation and a low satisfaction of usability are shown.

[0118] Consequently, as in the present invention, when containing an appropriate amount of disodium ethylenediaminetetraacetic acid and pre-dispersing with a zinc salt followed by stirring, the zinc ions (Zn) satisfy the pH 4 to 5 condition. 2+It was confirmed that it maintains the stability of ) while exhibiting low irritation and high user satisfaction.

[0119]

[0120] From the foregoing description, those skilled in the art to which the present invention pertains will understand that the present invention may be implemented in other specific forms without altering its technical concept or essential features. In this regard, the embodiments described above should be understood as illustrative in all respects and not restrictive. The scope of the present invention should be interpreted as including all modifications or variations derived from the meaning and scope of the claims set forth below and their equivalents, rather than from the detailed description above.

Claims

1. An oral liquid composition comprising sodium fluoride (NaF), sodium metaphosphate, a zinc salt, and a chelating agent.

2. In Paragraph 1, A composition in which the above-mentioned chelating agent stabilizes zinc ions in the above-mentioned oral liquid composition.

3. In Paragraph 1, A composition in which the above sodium metaphosphate comprises sodium hexametaphosphate (SHMP).

4. In Paragraph 1, A composition in which the zinc salt comprises zinc gluconate.

5. In Paragraph 1, The above chelating agent includes disodium ethylenediaminetetraacetic acid (Disodium EDTA), and A composition comprising the above disodium ethylenediaminetetraacetic acid in a ratio of 0.1 to 1.5 weight% relative to the total weight of the composition.

6. In Paragraph 1, A composition having a pH of 4 to 5 of the above-mentioned liquid composition for oral use.

7. In Paragraph 1, The above-mentioned oral liquid composition further comprises one or more selected from the group consisting of surfactants, humectants, flavoring agents, sweeteners, preservatives, binders, foaming agents, whitening agents, fragrances, colorants, solubilizers, and solvents.

8. In Paragraph 1, The above-mentioned liquid oral composition is a composition having one or more uses selected from the group consisting of teeth whitening, prevention or improvement of cavities, prevention or improvement of bad breath, prevention or improvement of plaque, and irritation relief.

9. An oral product comprising an oral liquid composition according to any one of paragraphs 1 to 8.

10. In Paragraph 9, The above oral product is one or more selected from the group consisting of liquid toothpaste, oral spray, mouthwash, oral ointment, mouthwash, and gargling product.

11. A method for preparing an oral liquid composition comprising the step of stirring and mixing a chelating agent and a zinc salt in purified water.

12. In Paragraph 11, A method of manufacturing in which the zinc salt comprises zinc gluconate.

13. In Paragraph 11, The above chelating agent includes disodium ethylenediaminetetraacetic acid (Disodium EDTA), and A method of manufacturing, wherein the disodium ethylenediaminetetraacetic acid is included in a ratio of 0.1 to 1.5 weight% relative to the total weight of the composition.

Citation Information

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