JP7363815B2 - Oral composition - Google Patents

Description

The present invention relates to an oral composition that has excellent retention of tocopherol or a derivative thereof in the oral cavity, and also has good appearance stability and usability.

Tocopherol or its derivatives have a peripheral circulation promoting effect (blood circulation promoting effect) in the gingival tissue, and therefore are useful for preventing periodontal disease, and are widely incorporated into oral compositions such as dentifrices. In order to further enhance the effects of these ingredients, studies have been made to increase their retention in the oral cavity.

For example, Patent Document 1 (Japanese Unexamined Patent Publication No. 2008-120753) proposes a technique using hydroxyethyl cellulose as a non-anionic water-soluble polymer in order to improve the retention of vitamin E derivatives in the oral cavity. The retentivity in the oral cavity tends to decrease due to the influence of other ingredients, and problems may also arise in stability, such as the appearance of the preparation. On the other hand, Patent Document 2 (Japanese Unexamined Patent Publication No. 2012-97057) discloses that 1.4% by mass or more of xanthan gum and 1.4% by mass or more of an alkyl sulfate are used together in a specific ratio, and an amphoteric surfactant is used in combination. A technology has been proposed to improve the retention of medicinal ingredients such as vitamin E or its derivatives in the oral cavity by increasing the sustainability of foam during tooth brushing, but the relatively large amount of xanthan gum makes it difficult to store at low temperatures. Under such conditions, it may become difficult to extrude from the tube container, resulting in decreased usability.

Japanese Patent Application Publication No. 2008-120753 Japanese Patent Application Publication No. 2012-97057

The present invention was made in view of the above circumstances, and an object of the present invention is to provide an oral composition that has excellent retention of tocopherol or a derivative thereof in the oral cavity, and also has good appearance stability and usability.

As a result of intensive studies to achieve the above object, the present inventors added polyacrylate with a weight average molecular weight below a specific value to an oral composition containing a specific tocopherol or a derivative thereof. It has been found that when formulated in combination with molecular substances, tocopherol or its derivatives exhibit a remarkable retention effect in the oral cavity, exhibiting excellent retention in the oral cavity, and also being able to maintain good appearance stability and usability. . That is, in the present invention, (a) one or more selected from tocopherol and its ester with an organic acid, (b) one or more selected from xanthan gum, alginate, and carrageenan, and (c) a weight average molecular weight of 1, 000 to 20,000, the component (a) has excellent retention in the oral cavity, and liquid separation is suppressed even after high temperature storage, resulting in good appearance stability and low temperature storage. The present inventors have discovered that an oral composition that is easy to extrude from a storage container even after storage and has good usability can be obtained, and has thus come to form the present invention.

Polyacrylic acid or its salt is known as a binder for oral compositions, but generally crosslinked polyacrylic acid or its salt with a weight average molecular weight of 100,000 or more, usually about 300,000, is used. ing. In contrast, in the present invention, (c) a low weight average molecular weight polyacrylate having a weight average molecular weight of 20,000 or less, preferably a linear polyacrylate, is used in combination with component (b). It has been found that this has the effect of increasing the retention of component (a) in the oral cavity, thereby providing excellent retention in the oral cavity while maintaining good appearance stability and usability as described above. did. By combining components (a), (b), and (c), the retention of component (a) in the oral cavity can be improved without increasing the amount of water-soluble polymeric substances such as xanthan gum. It was possible to provide the above-mentioned particularly remarkable effects. Such effects can be achieved by using polyacrylates that do not use component (c) and instead have a weight average molecular weight of over 20,000, or polyacrylic salts that have a weight average molecular weight of 20,000 or less but are not in the form of salts. This could not be achieved using acids.
As is clear from the results of the comparative examples described below, if component (c) is not contained, even if component (b) is contained and polyacrylate with a weight average molecular weight of 300,000 is contained, ( a) The retention of the component in the oral cavity was poor (Comparative Examples 1 and 3). In this case, Comparative Example 1, which does not contain polyacrylate, has poor appearance stability (no liquid separation) after high-temperature storage, and Comparative Example 3, which contains polyacrylate with a weight average molecular weight of 300,000, The ease of extrusion from the container after storage at low temperatures was also poor. If component (b) is not contained, even if component (c) is contained and an inorganic binder (silicic anhydride (thickening)) is contained, the retention of component (a) in the oral cavity will be poor; The appearance stability (no liquid separation) after high temperature storage was also poor (Comparative Example 2).
Furthermore, if it does not contain component (c), even if it contains polyacrylic acid with a weight average molecular weight of 20,000 or less together with component (b), the retention of component (a) in the oral cavity will be poor. there were.
On the other hand, in the oral compositions containing the components (a), (b), and (c) of the present invention shown in Examples, the component (a) remains in the oral cavity at a high rate; The retention of the ingredients in the oral cavity was excellent, and the appearance stability (no liquid separation) after high-temperature storage and ease of extrusion from the container after low-temperature storage were also good.
Patent Document 2 describes the improvement of oral retention of vitamin E or its derivatives by a combination of xanthan gum, alkyl sulfate, and an amphoteric surfactant. In contrast, the present invention discloses (b) and Component (c) improves the retention of component (a) in the oral cavity, and also ensures stability in appearance and usability after storage at low temperatures.

Therefore, the present invention provides the following oral composition.
[1]
(a) one or more selected from tocopherol and its ester with an organic acid;
(b) an oral composition containing one or more selected from xanthan gum, alginate, and carrageenan; and (c) a polyacrylate having a weight average molecular weight of 1,000 to 20,000.
[2]
The oral composition according to [1], wherein component (a) is selected from tocopherol, tocopherol acetate, and tocopherol nicotinate.
[3]
The oral composition according to [1] or [2], wherein the polyacrylate has a weight average molecular weight of 5,000 or more and 10,000 or less.
[4]
The oral composition according to any one of [1] to [3], wherein (c)/(b) is 0.1 to 3 as a mass ratio.
[5]
The oral composition according to any one of [1] to [4], wherein ((b)+(c))/(a) is 1 to 30 as a mass ratio.
[6]
For the oral cavity according to any one of [1] to [5], wherein the content of the component (b) is 0.4 to 1.4% by mass, and the content of the component (c) is 0.1 to 2% by mass. Composition.
[7]
The oral composition according to any one of [1] to [6], wherein the content of component (a) is 0.05 to 1% by mass.
[8]
The oral cavity composition according to any one of [1] to [7], which is a dentifrice composition.

According to the present invention, it is possible to provide an oral composition that has excellent retention of component (a) in the oral cavity and has good appearance stability and usability. The oral composition of the present invention fully exhibits the medicinal effects of component (a), and is effective in preventing or suppressing periodontal diseases such as gingivitis and periodontitis.

The present invention will be explained in more detail below. The oral composition of the present invention comprises (a) one or more selected from tocopherol and its ester with an organic acid, (b) one or more selected from xanthan gum, alginate, and carrageenan, and (c) a weight average and a polyacrylate having a molecular weight of 1,000 or more and 20,000 or less.

Component (a) is tocopherol or a tocopherol derivative, and as the tocopherol derivative, an ester of tocopherol with an organic acid can be used. These may be used alone, or two or more selected from these may be used in combination. Component (a) is a medicinal component that promotes blood flow and repairs tissue, and is an effective component for preventing or suppressing periodontal diseases such as gingivitis and periodontitis.
Examples of tocopherols include d-α-tocopherol, dl-α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol.
Further, as the ester of tocopherol with an organic acid, esters of the above-mentioned tocopherol with organic acids such as acetic acid, nicotinic acid, succinic acid, and linolenic acid, and salts thereof can be used. Specifically, tocopherol acetates such as d-α-tocopherol acetate and dl-α-tocopherol acetate, tocopherol nicotinic esters such as d-α-tocopherol nicotinate and dl-α-tocopherol nicotinate, and d-succinate. Examples include tocopherol succinate esters such as α-tocopherol and dl-α-tocopherol succinate, tocopherol linolenic esters such as d-α-tocopherol linolenate and dl-α-tocopherol linolenate, and tocopherol calcium succinate. Among these, tocopherol acetate, tocopherol nicotinate, and especially tocopherol acetate are preferred from the viewpoint of retention in the oral cavity.
Ingredients (a) can be those that comply with the old cosmetic raw material standards (cosmetic raw materials) or quasi-drug raw material standards 2006, and are manufactured by DSM Nutrition Japan Co., Ltd., Eisai Food Chemical Co., Ltd., and BASF. Commercial products such as those manufactured by Japan Co., Ltd. can be used.

In terms of effectiveness and taste, the blending amount of component (a) is preferably 0.05 to 1% (mass%, hereinafter the same) of the entire composition, more preferably 0.08 to 1.0%, and .1 to 0.5% is more preferable. Within the above range, the retention in the oral cavity is sufficiently improved, the composition is sufficiently solubilized, the appearance is stable even after high-temperature storage, and the taste is good.

Component (b) is one or more selected from xanthan gum, alginate, and carrageenan. These are anionic water-soluble polymeric substances that contribute to improving the retention of component (a) in the oral cavity.
As the alginate, an alkali metal salt such as a sodium salt of alginic acid can be used, and sodium alginate is preferable.
Component (b) is preferably xanthan gum or carrageenan, more preferably xanthan gum, from the viewpoint of the retention of component (a) in the oral cavity.
As the component (b), commercially available products such as those manufactured by CP Kelco, Kimica Co., Ltd., and Sansho Co., Ltd. can be used.
The blending amount of component (b) is preferably 0.4 to 1.4%, more preferably 0.6 to 1.0% of the total composition. When the blending amount is 0.4% or more, the retention of component (a) in the oral cavity is sufficiently excellent, and the appearance stability after high-temperature storage is sufficiently obtained. When the content is 1.4% or less, ease of extrusion from the container after storage at low temperature can be sufficiently maintained.

Component (c) is a polyacrylate having a weight average molecular weight (Mw) of 1,000 or more and 20,000 or less. Component (c) has the effect of improving the retention of component (a) in the oral cavity, and also contributes to suppressing liquid separation after high-temperature storage and ensuring ease of extrusion from a container after low-temperature storage.
The polyacrylate as the component (c) has a weight average molecular weight of 1,000 or more, preferably 5,000 or more, particularly 6,000 or more, from the viewpoint of the retention property in the oral cavity and the appearance stability of the component (a). or more, and 20,000 or less, preferably 10,000 or less, particularly 8,000 or less. If the weight average molecular weight is less than 1,000, the effect of improving the retention of component (a) in the oral cavity will be poor, and the appearance stability after high temperature storage will be poor. When it exceeds 20,000, the effect of improving the retention of the component (a) in the oral cavity decreases, and the retention of the component (a) in the oral cavity is not sufficiently obtained.
The weight average molecular weight of the polyacrylate as component (c) is preferably 5,000 to 20,000, more preferably 5,000 to 10,000 in terms of the retention of component (a) in the oral cavity. be.

The weight average molecular weight was measured by GPC (gel permeation chromatography) using the method and measurement conditions described in Japanese Patent No. 5740859. Specifically, it is shown below (the same applies below).
Method for measuring weight average molecular weight;
The weight average molecular weight is a value measured using a gel permeation chromatograph/multi-angle laser light scattering detector (GPC-MALLS) under the following conditions.
Mobile phase: 0.3M _NaClO4
NaN ₃ aqueous solution column: TSKgelα-M 2 pre-column: TSKguardcolumn α
Standard substance: polyethylene glycol

The polyacrylate as the component (c) is preferably a linear polyacrylate (non-crosslinked polyacrylate) from the viewpoint of the retention of the component (a) in the oral cavity.
As the salt, monovalent salts are preferred, alkali metal salts or ammonium salts are more preferred, alkali metal salts such as sodium salts and potassium salts are still more preferred, and sodium salts are particularly preferred.
As such polyacrylates, commercial products sold by Polyscience Co., Ltd. and Toagosei Co., Ltd. can be used.
Specific commercial products include sodium polyacrylate (Mw: 1,000); linear, manufactured by Polyscience; sodium polyacrylate (Mw: 6,000); linear, manufactured by Toagosei Co., Ltd. , AC-10NP, AC-10NPD, Aron T-50, sodium polyacrylate (Mw: 8,000); linear, manufactured by Polyscience, sodium polyacrylate (Mw: 20,000); linear , manufactured by Toagosei Co., Ltd., Aron A-20UN, etc. can be used.

In addition, the polyacrylate of component (c) has a weight average molecular weight lower than the crosslinked polyacrylate of the binder normally used in dentifrices, and is a polyacrylate salt known as a binder. It is different from

The amount of component (c) to be blended is preferably 0.1 to 2% of the total composition, more preferably 0.3 to 1.0%, and even more preferably 0.4 to 0.8%. When the content is 0.1% or more, the retention of component (a) in the oral cavity is sufficiently improved, and the appearance stability after high-temperature storage is sufficiently obtained. When it is 2% or less, the influence of the taste of component (c) itself can be sufficiently prevented.

Further, in the present invention, (c)/(b), which indicates the quantitative ratio of component (b) to component (c), is preferably 0.1 to 3 as a mass ratio, more preferably 0.3 to 1. 5, more preferably 0.5 to 1.0. When the mass ratio of (c)/(b) is within the above range, the retention of component (a) in the oral cavity is better, and the appearance stability after high temperature storage (no liquid separation) and after low temperature storage are improved. Easier to extrude from the container.

Furthermore, ((b)+(c))/(a), which indicates the quantitative ratio of component (a) to components (b) and (c), is preferably 1 to 30 as a mass ratio, more preferably 1. -20, more preferably 1-16. When the mass ratio of ((b)+(c))/(a) is within the above range, the retention of the component (a) in the oral cavity is better, and the appearance stability after high temperature storage (no liquid separation). ) and easier to extrude from the container after storage at low temperature.
In the present invention, in particular, when the mass ratio of (c)/(b) and the mass ratio of ((b)+(c))/(a) are each within the above ranges, the oral cavity of the component (a) It is especially preferable because it further improves the internal retention property, and further improves the appearance stability (no liquid separation) after high temperature storage and the ease of extrusion from the container after low temperature storage.

The oral composition of the present invention can be prepared into a paste, gel, or liquid dentifrice (toothpaste, gel dentifrice, liquid dentifrice, liquid dentifrice, etc.), mouthwash, mouth spray, liniment, patch, etc. However, it is particularly suitable as a dentifrice composition, especially a toothpaste composition. In this case, in addition to the above-mentioned components, known components other than the above-mentioned components may be added as an optional component depending on the dosage form and the like. It is preferable to add optional components within a range that does not impede the effects of the present invention. Specifically, dentifrice compositions such as toothpaste can contain abrasives, binders, thickeners, surfactants, sweeteners, preservatives, colorants, fragrances, active ingredients, etc. It can be prepared in a conventional manner by mixing the ingredients with water. The amounts shown below are based on the entire composition.

Examples of the abrasive include silica-based abrasives such as anhydrous silicic acid, crystalline silica, amorphous silica, silica gel, and aluminosilicate, tribasic calcium phosphate, quaternary calcium phosphate, calcium hydrogen phosphate anhydrate, and calcium hydrogen phosphate. Calcium phosphate abrasives such as dihydrate, zeolite, calcium pyrophosphate, calcium carbonate, sodium hydrogen carbonate, aluminum hydroxide, alumina, magnesium carbonate, tribasic magnesium phosphate, zirconium silicate, hydroxyapatite, synthetic resin abrasives can be mentioned. These can be used alone or in combination of two or more, but from the viewpoint of usability, among them, silica-based abrasives such as inorganic abrasives such as silicic anhydride, calcium phosphate-based abrasives, and especially silicic anhydride. is preferable (the blending amount is usually 5 to 60%, and 10 to 55% in the case of toothpaste).

Examples of the binder include organic binders other than component (b) and inorganic binders such as silica gel, aluminum silica gel, Veegum, and Laponite (the amount is usually 0.3 to 10%). (The amount of inorganic binder added is preferably 1 to 5%).
In addition, in the present invention, since component (b) also acts as a binder, it is not necessary to mix any organic binder other than component (b) (blending amount: 0%).

Examples of thickeners include sugar alcohols such as sorbitol, maltitol, lactitol, and erythritol, and polyhydric alcohols such as propylene glycol (the amount blended is usually 5 to 70%).

The surfactant may include an anionic surfactant, a nonionic surfactant, and an amphoteric surfactant. These can be used alone or in combination of two or more.
Examples of the anionic surfactant include alkyl sulfates having an alkyl group having 12 to 14 carbon atoms, acylamino acid salts, acyl taurine salts, and the like. The acyl group of the acylamino acid salt and the acyl taurine salt preferably has 12 to 14 carbon atoms, particularly 12 carbon atoms.
Specifically, examples of alkyl sulfates include lauryl sulfate and myristyl sulfate; examples of acylamino acid salts include acyl glutamates such as lauroyl glutamate and myristoyl glutamate; and acyl sarcosine salts such as lauroyl sarcosine salt; Examples of the salt include lauroylmethyltaurine salt. The salt is preferably an alkali metal salt such as sodium salt or potassium salt. Particularly preferred are alkyl sulfates, acyl sarcosine salts, and acyl taurine salts. Among these, anionic surfactants having a hydrocarbon group having 12 carbon atoms (lauryl group) are preferred, and alkyl sulfates (sodium salts) are particularly preferred because they are superior in taste to other surfactants. .
Nonionic surfactants include, for example, polyoxyethylene alkyl ethers, polyoxyethylene-polyoxypropylene block copolymers, polyoxyethylene hydrogenated castor oil, polyoxyethylene ethers of glycerin esters, sucrose fatty acid esters, and alkylolamides. , sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, and glycerin fatty acid ester. Among these, polyoxyethylene alkyl ether, polyoxyethylene hydrogenated castor oil, alkylolamide, and sorbitan fatty acid ester are preferred in terms of versatility. The polyoxyethylene alkyl ether preferably has an alkyl chain of 14 to 30 carbon atoms and an average number of added moles of ethylene oxide (average added EO) of 3 to 30. The polyoxyethylene hydrogenated castor oil preferably has an average added EO of 5 to 100, more preferably 20 to 60. The alkylolamide preferably has 12 to 14 carbon atoms in the alkyl chain. In the sorbitan fatty acid ester, the fatty acid preferably has 12 to 18 carbon atoms. The polyoxyethylene sorbitan fatty acid ester preferably has a fatty acid having 16 to 18 carbon atoms and an average added EO of 10 to 40.
Examples of the amphoteric surfactant include acylaminoacetic acid betaine and fatty acid amidopropyl betaine having an acyl group having 12 to 14 carbon atoms. Examples of the acylaminoacetic acid betaine include lauroyl dimethylaminoacetic acid betaine, and examples of the fatty acid amidopropyl betaine include coconut oil fatty acid amidopropyl betaine.

The amount of surfactant added is usually 0.01 to 15%, particularly 0.01 to 10%.
The amount of anionic surfactant to be blended is preferably 0.1 to 3%, particularly 0.5 to 2%. The amount of alkyl sulfate added may be 1.2% or less, particularly 1.0% or less, and even 0.8% or less. The content of the nonionic surfactant is preferably 0.01 to 10%. The blending amount of the amphoteric surfactant is preferably 0 to 3%.

Sweeteners include saccharin sodium, stevioside, dipotassium glycyrrhizinate, perillartine, thaumatin, neohesperidyl dihydrochalcone, and asparatylphenylalanine methyl ester.
Examples of preservatives include paraoxybenzoic acid ester and sodium benzoate.
Examples of the coloring agent include Blue No. 1, Yellow No. 4, and titanium dioxide.

Fragrances include peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime. Oil, lavender oil, rosemary oil, laurel oil, chamomile oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, iris concrete, absolute peppermint. , absolute rose, orange flower, and other natural fragrances, and fragrances obtained by processing these natural fragrances (cutting the front reservoir, cutting the rear reservoir, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.), and Menthol, carvone, anethole, methyl salicylate, cinnamic aldehyde, 3-l-menthoxypropane-1,2-diol, linalool, linaryl acetate, limonene, menthone, menthyl acetate, N-substituted-paramenthane-3-carboxamide, Pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allylcyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, isoamyl alcohol , hexenol, dimethyl sulfide, cyclotene, furfural, trimethylpyrazine, ethyl lactate, ethyl thioacetate, and other individual flavors, as well as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, Known flavoring materials used in oral compositions can be used, such as blended flavorings such as mixed fruit flavors and tropical fruit flavors, and are not limited to the flavorings in the Examples.
Further, it is preferable that the above fragrance material is used in an amount of 0.000001 to 1% of the total composition. It is preferable to use 0.001 to 2.0% of the fragrance material in the composition as a fragrance material using the above fragrance material.

Optional active ingredients include nonionic disinfectants such as isopropylmethylphenol; cationic disinfectants such as cetylpyridinium chloride; dextranase, mutanase, lysozyme, amylase, protease, lytic enzyme, SOD (superoxide dismutase), etc. enzymes; alkali metal monofluorophosphates such as sodium monofluorophosphate and potassium monofluorophosphate; fluorides such as sodium fluoride and stannous fluoride; tranexamic acid, epsilon aminocaproic acid, allantoin, allantoin chlorhydroxy aluminum , anti-inflammatory agents such as dihydrocholesterol, glycyrrhizic acid, and glycyrrhetinic acid; hypersensitivity improving agents such as potassium nitrate and aluminum lactate; glycerophosphate, chlorophyll, sodium chloride, and zinc compounds such as zinc chloride, zinc oxide, and zinc citrate; Copper compounds such as copper gluconate and copper sulfate; vitamins such as vitamin A, B group vitamins, and vitamin C; and crude drugs such as Auricula japonica and tea. These active ingredients can be used alone or in combination of two or more, and can be blended in an effective amount within a range that does not impede the effects of the present invention.

The pH (25° C.) of the oral composition may be within the normal range, preferably 5 to 9, particularly 6 to 8. Note that the pH may be adjusted by adding a known pH adjuster, for example, hydrochloric acid or an alkali metal hydroxide such as sodium hydroxide can be used.

EXAMPLES Hereinafter, the present invention will be specifically explained with reference to Examples and Comparative Examples, but the present invention is not limited to the Examples below. In addition, in the following examples, % indicates mass % unless otherwise specified.

[Examples, comparative examples]
Dentifrice compositions (toothpastes) having the compositions shown in Tables 1 to 3 were prepared by conventional methods and evaluated by the following methods. The results are also listed in Tables 1 to 3.

(1) Method for evaluating the retention of tocopherol or its derivatives in the oral cavity The skin of a 7-week-old male hairless mouse cut into 1.5 cm squares (Japan SLC Co., Ltd.; Labo Skin) was placed in a 6-well plate, and artificial saliva ( 5mL of 50mM KCl, 1mM CaCl ₂ , 0.1mM MgCl ₂ , 1mM KH ₂ PO ₄ , pH 7.0) was added, and the mixture was allowed to stand for 2 hours. A glass frame was placed on the skin so that the permeation area (approximately 0.8 cm ² ) was constant, and 300 μL of a solution obtained by diluting 5 g of the dentifrice composition of each example 3 times with artificial saliva was injected. It was left standing for a minute. Thereafter, the diluted solution was discarded, 5 mL of water was added, and the solution was washed using a shaker at 160 rpm for 1 minute. The above washing was repeated twice in total.
The washing solution was discarded, the skin was collected in a tube, 1 mL of ethanol (EtOH 90%) was added, and extraction was performed using a vortex mixer for 5 minutes. Collect the extract, dilute it 1:1 with methanol, and then quantify tocopherol or its derivatives (component (a)) using HPLC (high performance liquid chromatography, using the following equipment) using the absolute calibration curve method according to the test conditions below. did.
<Used equipment>
・Pump: Shimadzu Corporation, LC-20AD
・Sample introduction section: Shimadzu Corporation, SIL-20AC
・Detector: Shimadzu Corporation, SPD-20A
・Column constant temperature bath: Shimadzu Corporation, CTO-20AC
・Eluent flow rate: 1mL/min
<Test condition>
・Detector: Ultraviolet absorption photometer (measurement wavelength: 273 nm)
・Column: COSMOSIL 5C ₁₈ -MS-II
・Column temperature: 40℃
- Eluent: methanol As a control, the quantitative value of tocopherol or its derivative when treated with the dentifrice composition of Comparative Example 1 is set as 100%, and the intraoral concentration of component (a) when treated with each dentifrice composition. The retention rate (%) was calculated. However, in the control products of Examples 16 and 17, component (a) of Comparative Example 1 was changed to tocopherol nicotinate (same substance as in Example 16) and tocopherol (same substance as in Example 17). Furthermore, in the control products of Examples 18 and 19, the amount of tocopherol acetate in Comparative Example 1 was changed to 0.5% (same amount as Example 18) and 1.0% (same amount as Example 19).
Regarding the retention property of tocopherol or its derivative (component (a)) in the oral cavity, an oral retention rate of 110% or more is considered to be excellent and passed, and a retention rate of 120% or more is considered to be excellent and 130%. Those above were judged to be even better, and those of 140% or more were judged to be the most excellent.

(2) Evaluation method for appearance stability (no liquid separation) after high temperature storage 50 g of the dentifrice composition was filled into a laminated tube container with a diameter of 8 mm, and three bottles of each composition were stored at 50° C. for one month. After leaving it at room temperature, extrude 10 cm of the dentifrice composition from the tube container onto a straw paper, observe the state of liquid separation at the mouth of the container, and measure the length of the liquid if any liquid oozes out onto the straw paper. The degree of liquid separation was evaluated using the following scoring criteria.
The average value of the three evaluation points was calculated, and the appearance stability (absence of liquid separation) after high-temperature storage was determined according to the following evaluation criteria.
Scoring criteria: 4 points: No liquid separation was observed at all when extruded. 3 points: There was almost no liquid separation (less than 1 cm) when extruded, which caused problems in use.
No problem 2 points; When extruded, a liquid separation of 1 to 2 cm is observed at the mouth. 1 point; When extruded, a liquid separation of more than 2 cm is observed at the mouth. Evaluation criteria: ◎: 3.5 points or more 4 .0 points or less ○: 3.0 points or more and less than 3.5 points △: 2.0 points or more and less than 3.0 points ×: less than 2.0 points

(3) Evaluation method for ease of extrusion from a container after low temperature storage 50 g of the dentifrice composition was filled into a laminated tube container with a diameter of 8 mm, and three bottles of each composition were stored at -5° C. for one month. After being left at room temperature, the dentifrice composition was extruded from the tube container, and the ease of extrusion from the container was evaluated according to the following scoring criteria.
The average value of the three evaluation scores was calculated, and the ease of extrusion from the container after storage at low temperature was determined according to the following evaluation criteria.
Rating criteria: 4 points; Can be pushed out smoothly from the tube container. 3 points; Can be pushed out from the tube container somewhat smoothly. 2 points; Slightly difficult to push out from the tube container. 1 point; Difficult to push out from the tube container. Evaluation criteria: ◎: 3.5 points or more 4 points. .0 points or less ○: 3.0 points or more and less than 3.5 points △: 2.0 points or more and less than 3.0 points ×: less than 2.0 points

Details of the raw materials used are shown below.
(a) Component Tocopherol acetate dl-α-tocopherol acetate, manufactured by DSM Nutrition Japan Co., Ltd. Tocopherol nicotinate Vitamin E Nicotinate, manufactured by BASF Japan Co., Ltd. Tocopherol dl-α-tocopherol, manufactured by BASF Japan Co., Ltd. (b) Ingredients Xanthan gum Monarto gum DA, manufactured by CP Kelco Sodium alginate Kimiloid, manufactured by Kimica Co., Ltd. Carrageenan GENUVISCO (registered trademark) J-J, manufactured by Sansho Co., Ltd. (c) Component Sodium polyacrylate (Mw: 1,000)
Linear, sodium polyacrylate (Mw: 1,000), manufactured by Polyscience, sodium polyacrylate (Mw: 6,000)
Linear, Jurimer AC-10NP, manufactured by Toagosei Co., Ltd. Sodium polyacrylate (Mw: 8,000)
Linear, sodium polyacrylate (Mw: 8,000), manufactured by Polyscience, sodium polyacrylate (Mw: 20,000)
Linear, Aron A-20UN, Toagosei Co., Ltd. sodium polyacrylate (Mw: 300,000) (comparison product)
Crosslinked type, sodium polyacrylate (Mw: 300,000), manufactured by Polyscience

Claims (8)

(a) one or more selected from tocopherol and its ester with an organic acid;
(b) contains one or more selected from xanthan gum, alginate, and carrageenan, and (c) polyacrylate having a weight average molecular weight of 5,000 to 10,000 , and the content of component (b) is 0. .4 to 1.4% by mass, the content of component (c) is 0.1 to 2% by mass, and (c)/(b) indicates the quantitative ratio of component (b) to component (c). is 0.1 to 3 as a mass ratio, and ((b) + (c))/(a), which indicates the quantitative ratio of component (a) to components (b) and (c), is as a mass ratio. An oral composition having a rating of 1 to 30 . The oral composition according to claim 1, wherein component (a) is selected from tocopherol, tocopherol acetate, and tocopherol nicotinate. The oral composition according to claim 1 or 2, wherein the polyacrylate has a weight average molecular weight of 6,000 or more and 8,000 or less. The oral cavity according to any one of claims 1 to 3, wherein (c)/(b) indicating the quantitative ratio of the component (b) to the component (c) is 0.3 to 1.5 as a mass ratio. Composition. The oral composition according to claim 4, wherein the content of component (b) is 0.6 to 1.0% by mass, and the content of component (c) is 0.3 to 1.0% by mass. Any one of claims 1 to 5 , wherein ((b)+(c))/(a), which represents the quantitative ratio of components (b) and (c) to component (a), is 1 to 20 as a mass ratio. Oral composition according to item 1. The oral composition according to any one of claims 1 to 6, wherein the content of component (a) is 0.05 to 1% by mass. The oral composition according to any one of claims 1 to 7, which is a dentifrice composition.