JP2010006720A - Liquid composition for cleaning denture - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a liquid composition for cleaning a denture, which exhibits excellent removal power and germicidal power to a denture biofilm even in a diluted state, gives a denture immersion liquid having high antiseptic power in use, excellent storage stability, effectively removes a denture biofilm of denture by a chemical method, disinfects a denture and cleanly maintains a denture. <P>SOLUTION: The concentration type liquid composition for cleaning a denture, which is diluted with water in use and applied to a denture, comprises (A) a polyglycerol fatty acid ester having an HLB value of 12-17, (B) a protease, (C) a cationic disinfectant and (D) water, wherein the composition is diluted with water to make the mass ratio of (A)/(C) to 2.5-15, the concentration of the component (A) to 0.03-0.5 mass% and the concentration of the component (C) to 0.005-0.1 mass% to be used. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention is a concentrated denture cleaning that is used after dilution, which exhibits excellent removal power and sterilization power for denture biofilms, is excellent in the sterilization power of denture immersion liquid, and has good storage stability The present invention relates to a liquid composition for use.

  In recent years, with the arrival of an aging society, the number of denture users tends to increase year by year. Denture users tend to accumulate food residue between the dentures and the oral mucosa and healthy teeth, and are placed in an environment in which oral microorganisms are more likely to propagate than healthy people.

  Denture stains include food residues, denture biofilms, tartar-like deposits, pigments and the like. Here, the denture biofilm is a biofilm in which oral microorganisms are fixed on the surface of the denture and aggregated together with products such as adhesive polysaccharides, saliva and serum components. Due to the presence of various microorganisms in this denture biofilm, denture stomatitis, halitosis and denture odor occur, or, for partial dentures, dental caries and periodontal disease of the remaining teeth are likely to occur.

  The microbiological characteristics of denture biofilms include a high proportion of Candida, but Candida is closely related to respiratory infections such as pulmonary candidiasis and aspiration pneumonia. Has been reported (see Non-Patent Documents 1 and 2). Therefore, it is important to keep the denture clean by removing the denture biofilm attached to the denture by daily care.

  As a method for removing the denture biofilm, there are mechanical removal by brushing and chemical removal by using a denture cleaning agent and a polishing agent. However, mechanical removal by brushing makes it difficult to completely remove the denture biofilm adhering to the narrow gap or denture surface. Therefore, it is effective to combine the two methods of mechanical removal and chemical removal. It is desirable as a safe care method.

  As denture cleaning agents marketed for the purpose of chemical removal, tablet-type and powder-type ones are mainly used. Generally, these detergents contain peroxides such as percarbonates and perborate, proteolytic enzymes (proteases), surfactants, chelating agents, etc. as cleaning ingredients. It uses a cleaning system that dissolves in water and removes the denture biofilm by the action of decomposing hydrogen peroxide and enzymes generated, and the action of surfactants and chelating agents. However, in such a cleaning system, a certain degree of bactericidal power is exhibited by the generated hydrogen peroxide, but the removal power against the denture biofilm is insufficient.

  In addition, the above-described solid type cleaning agent has a problem in that the amount used is adjusted according to the amount of liquid. In particular, tablet-type cleaning agents are packaged in a single unit, and the user is dissatisfied with the amount of use adjustment for cleaning partial dentures whose denture sizes vary greatly among users. Solid-type cleaning agents have such problems, while liquid preparations have the advantage of easy adjustment of the amount used. Furthermore, concentrated type preparations that are diluted with water according to the amount used at the time of use can reduce the volume of the container and reduce the volume of the container since it can be used only once compared with the case of using the stock solution preparation. And is advantageous in terms of storage space.

  However, the concentration-type preparation that is diluted with water at the time of use reduces the concentration of the ingredients depending on the mixing ratio of the preparation and water. The issue is whether to do this. Accordingly, there has been a demand for the development of a concentrated liquid composition that exhibits excellent removal power and sterilization power for denture biofilms with a concentrated liquid composition that is diluted with water at the time of use.

  Examples of components that remove denture biofilms and dental plaques include protease enzymes and surfactants, and biofilms can be effectively removed by using proteases and surfactants in combination. However, enzymes generally have low stability, and there is a problem that they are inactivated when stored for a long time in a liquid composition. In addition, depending on the type of surfactant used, the enzyme activity may be greatly reduced. Therefore, in order to maintain the quality as a product, it is important to use a surfactant that has little influence on enzyme stability in addition to excellent detergency. Nonionic surfactants are often used as surfactants with good enzyme stability.

  On the other hand, in order to exert a bactericidal power against denture biofilms, it is essential to add a bactericidal agent. However, surfactants such as nonionic surfactants formulated for imparting detergency and solubilizing oily components such as fragrances reduce the effectiveness of the bactericide to incorporate the bactericide into micelles. There is a problem. In addition, in a composition containing an anionic surfactant such as sodium lauryl sulfate, when a cationic bactericidal agent is used, there is a problem that the efficacy of the bactericidal agent is lost because a complex is formed. For this reason, it becomes important to set the kind of surfactant and its blending amount so as not to inhibit the efficacy of the bactericide as much as possible.

  As described above, in order to obtain a concentrated denture cleaning liquid composition that exhibits excellent removal and bactericidal power against denture biofilms, it is essential to add protease and bactericides. It is important to select surfactants with excellent detergency while demonstrating their properties, and to determine the concentration and mass ratio for each use, but with conventional technologies, proteases and fungicides are stable in liquid compositions. It has been difficult to mix and exhibit the above effects satisfactorily.

  A liquid composition containing a protease and a nonionic surfactant is known (see Patent Document 1). However, since this liquid composition does not contain a bactericidal component, it does not exert bactericidal power and is used for denture cleaning. It is insufficient as a composition.

  Moreover, although the composition which exhibits the outstanding bactericidal power with respect to the aggregate of microorganisms like a dental plaque is disclosed (refer patent document 2), this is a cationic bactericide and a specific nonionic surfactant. In combination, the excellent bactericidal effect is exhibited. This technology does not include protease as an essential component, and there is no description about the amount of the protease. Sufficient removal power against strong dirt such as denture biofilm is not demonstrated, and high bactericidal power and removal power against denture biofilm are exhibited. It is difficult to balance satisfaction. Further, it is not a concentrated type composition that is diluted at the time of use, and there is no description about improvement in appearance stability and protease stability of the composition.

  As a cosmetic composition with improved detergency while ensuring enzyme stability, a technique has been proposed in which a polyhydric alcohol-containing aqueous solution is mixed with a proteolytic enzyme, a surfactant, and a cationic fungicide (patent) In References 3 and 4, the selected surfactant is used as a cleaning component for contact lenses, and does not exhibit cleaning power against strong dirt such as a denture biofilm. In Example 3 described in Patent Documents 3 and 4, the cationic bactericide benzalkonium chloride is blended. The concentration of this cationic bactericide and the nonionic surfactant for the cationic bactericide In the range of the mass ratio, sufficient sterilizing power is not exhibited, and excellent sterilizing power for denture biofilm is not exhibited.

  A concentrated liquid composition containing a protease and a bactericidal agent has also been studied (see Patent Document 5). However, in this proposal, the mass ratio of the nonionic surfactant to the cationic bactericidal agent is described. In this case, although a good sterilizing power is exhibited, the cleaning power is insufficient, and thus the effect of removing the denture biofilm is weak. Moreover, in order to exhibit the bactericidal power, the bactericidal agent is mix | blended in high concentration, As a result, the fall of enzyme activity occurs and the removal power will fall remarkably. That is, such a technique has a problem that it is difficult to achieve both sterilization and removal.

  In addition, a two-component type cleaning solution in which a cleaning solution containing a nonionic surfactant and a protease is diluted with a diluting solution containing an ionic antibacterial agent has been studied (see Patent Document 6). However, this technology relates to cleaning for contact lenses, and within the scope of the contents described, it cannot exert sufficient cleaning power and sterilizing power against strong dirt such as denture biofilm. . In addition, when the technique is applied to cleaning dentures, a large amount of dilution solution is required. For this reason, it is inconvenient for the user in terms of use, carrying, and storage space.

  Furthermore, it has been difficult for a concentrated liquid composition diluted during conventional use to maintain good temporal stability during both high temperature storage and low temperature storage.

  As described above, the conventional technology has both excellent removal power and sterilization power for denture biofilms, excellent antiseptic power of denture immersion liquid, and also has good storage stability during high temperature storage and low temperature storage. It has been difficult to obtain a concentrated denture cleaning liquid composition.

JP 2002-69487 A JP-A-11-255629 JP 2000-273489 A JP 2001-114624 A JP-T-2003-530447 Japanese Patent No. 3697294 Prosthetic Journal 43: 636-639, 1999. Nihon University Dentistry 79,117-123,2005

  The present invention has been made in view of the above circumstances, and exhibits excellent removal power and bactericidal power for denture biofilms, and when immersed in dentures after dilution, has excellent antiseptic power of a denture soaking solution and stable storage An object of the present invention is to provide a concentrated liquid type denture cleaning liquid composition having good properties.

  As a result of intensive studies to achieve the above object, the present inventors have added (A) polyglycerin fatty acid as a nonionic surfactant to a concentrated denture cleaning liquid composition diluted with water and used. Ester, (B) protease, (C) cationic fungicide, (D) water is blended, and (A) polyglycerin fatty acid ester having an HLB value of 12 to 17 is selected as a polyglycerin fatty acid ester at a specific ratio. When blended and diluted with water so that the concentration of the polyglycerin fatty acid ester and the cationic bactericidal agent are in a specific range, it has excellent removal power against denture biofilm in the diluted state. Excellent sterilizing power is exerted on biofilms, and it is possible to achieve both excellent removal power and sterilizing power while diluting with water. If soaked dentures dilution, found that the denture immersion liquid has a high antiseptic, they were able to complete the present invention.

  Furthermore, (E) The sterilizing power with respect to a denture biofilm can be strengthened more by mix | blending isopropylmethylphenol and / or thymol.

  In particular, (A) 5 to 30% by mass of a polyglycerol fatty acid ester having a fatty acid residue having 8 to 16 carbon atoms and an average degree of polymerization of 6 to 12 as a polyglycerol fatty acid ester, and (D) 30 to 50 water. More stable storage stability, in particular composition, because it contains by mass%, further comprises (F) polyol, (G) pH adjuster, and pH at 25 ° C. is 6.0-8.5. Enzyme stability in a product, appearance stability in high temperature storage and low temperature storage can be further improved.

  When (G) phosphoric acid or a salt thereof is included as a pH adjuster, (H) at least one chelating agent selected from citrate, edetate and water-soluble polyphosphate is added to (B) protease / (H) The storage stability of a composition can be improved more by mix | blending a chelating agent with the mass ratio of 1-10.

  In addition, as described above, in the liquid composition for concentrated denture cleaning used by dilution in the prior art, the selected surfactant is not suitable for removing the denture biofilm, It is difficult to solve the above problems because the mixing amount of the nonionic surfactant with respect to the cationic bactericidal agent is not suitable, and it is difficult to solve the above problems. It has been difficult to achieve a balance between excellent removal power and sterilization power for the denture biofilm after dilution, and in addition, it is difficult to obtain a denture immersion liquid (dilution liquid) having high antiseptic power. On the other hand, the applicant can solve the above-mentioned problems by blending a specific polyoxyethylene alkyl ether, protease, cationic bactericidal agent, and water, diluting to an appropriate concentration and using it. It was proposed in Japanese Patent Application No. 2007-327184 that excellent removal power, bactericidal power, and antiseptic power of denture soaking solution are exhibited. As a result of further studies to solve the above problems, the present inventors have formulated a specific (A) polyglycerin fatty acid ester and components (B) to (D) as a new technique, and (A) Excellent removal with respect to denture biofilm by using a specific ratio of / (C) and diluting with water so that the concentrations of components (A) and (C) are in a specific range Thus, a concentrated liquid type denture cleaning liquid composition that exhibits strength and bactericidal power, has high antiseptic power of the denture soaking solution, and has good storage stability can be obtained.

Accordingly, the present invention provides the following denture cleaning liquid composition.
1. A concentrated denture cleaning liquid composition that is diluted with water and applied to a denture during use,
(A) Polyglycerin fatty acid ester having an HLB value of 12 to 17 (B) Protease (C) Cationic fungicide (D) Water is included, and the mass ratio of (A) / (C) is 2.5 to And diluted with water so that the concentration of the component (A) is 0.03 to 0.5% by mass and the concentration of the component (C) is 0.005 to 0.1% by mass. A liquid composition for cleaning dentures.
[2] The denture cleaning liquid composition according to [1], further comprising (E) isopropylmethylphenol and / or thymol.
Claim 3; (A) 5 to 30% by mass of polyglycerin fatty acid ester having a fatty acid residue having 8 to 16 carbon atoms and an average degree of polymerization of 6 to 12 as polyglycerin fatty acid ester, and (D) 30 water. The denture cleaning according to claim 1 or 2, further comprising ~ 50 mass%, further comprising (F) a polyol and (G) a pH adjusting agent, and having a pH at 25 ° C of 6.0 to 8.5. Liquid composition.
Claim 4; (G) the pH adjuster is phosphoric acid or a salt thereof; and (H) at least one chelating agent selected from (H) citrate, edetate and water-soluble polyphosphate (B) The denture cleaning liquid composition according to claim 3, wherein the protease / (H) chelating agent has a mass ratio of 1 to 10.

  The denture cleaning liquid composition of the present invention is a concentrated type that is applied to a denture by diluting with water at the time of use, and exhibits excellent removal power and sterilization power against a denture biofilm even in a diluted state. When dentures are soaked in the diluted solution, the denture soaking solution has high antiseptic properties, and the composition has good storage stability, and also has good storage stability and enzyme stability during high-temperature storage and low-temperature storage. The denture biofilm of denture can be effectively removed and sterilized by a chemical method, and the denture can be kept clean.

  The present invention will be described in further detail below. The denture cleaning liquid composition of the present invention is a concentrated denture cleaning liquid composition that is diluted with water and applied to a denture when in use, (A) a polyglycerin fatty acid ester having an HLB value of 12 to 17, (B) Protease, (C) Cationic fungicide, (D) Water, (E) Isopropylmethylphenol and / or thymol, (F) Polyol, (G) pH adjuster, (H) Chelating agents and the like can be contained.

In the present invention, (A) a polyglycerin fatty acid ester having an HLB value of 12 to 17 is used from the viewpoints of the removal power, the bactericidal power and the antiseptic power of the denture soaking solution for the denture biofilm after dilution.
The HLB value of the polyglycerin fatty acid ester is 12 to 17, preferably 13 to 16, and more preferably 14 to 16. When the HLB value is less than 12, the sterilizing power against the denture biofilm after dilution and the antiseptic power of the denture soaking solution are reduced, and a problem in appearance stability due to a decrease in solubility in water occurs. Those exceeding 17 are generally not commercially available.
The HLB value of the polyglycerin fatty acid ester was calculated using the Atlas method (HLB value = 20 (1-S / A)), where S is the saponification value and A is the acid value of the fatty acid constituting the surfactant. Value.

  As such a polyglycerol fatty acid ester, a polyglycerol fatty acid ester having 8 to 18 carbon atoms in the fatty acid residue and having an average polymerization degree of 5 to 12 is preferably used. Specifically, decaglyceryl caprylate, decaglyceryl laurate, decaglyceryl myristate, decaglyceryl palmitate, decaglyceryl oleate, decaglyceryl stearate, hexaglyceryl caprylate, hexaglyceryl laurate, hexaglyceryl myristate, palmitic Hexaglyceryl acid, hexaglyceryl oleate, hexaglyceryl stearate, pentaglyceryl laurate, pentaglyceryl myristate, pentaglyceryl oleate, pentaglyceryl stearate, etc., Taiyo Kagaku Co., Ltd., Mitsubishi Chemical Foods Co., Ltd. A commercially available product can be used. Among them, it is preferable to use decaglyceryl caprylate, decaglyceryl laurate, decaglyceryl myristate, hexaglyceryl laurate, hexaglyceryl myristate, pentaglyceryl laurate, pentaglyceryl myristate, especially decaglyceryl caprylate, lauric acid It is more preferable to use decaglyceryl and decaglyceryl myristate.

  For example, decaglyceryl caprylate (Sunsoft Q-10Y, HLB17), decaglyceryl laurate (Sunsoft M-12J, HLB16), decaglyceryl laurate (Sunsoft Q-12Y, HLB17) manufactured by Taiyo Kagaku Co., Ltd. ), Decaglyceryl myristate (Sunsoft Q-14Y, HLB17), decaglyceryl oleate (Sunsoft Q-17Y, HLB16), decaglyceryl stearate (Sunsoft Q-18Y, HLB17), hexaglyceryl caprylate (Sun Soft Q-81F, HLB13), pentaglyceryl laurate (Sunsoft A-12E, HLB16), pentaglyceryl myristate (Sunsoft A-14E, HLB15), pentaglyceryl myristate (Sunsoft A-141E, HLB12), Pentaglyceryl oleate (Sunsoft A-17E, HLB15), Pentaglyceryl stearate (Sunsoft A-18E, HLB15), Decaglyceryl laurate (L-10D, HLB15), Laurin manufactured by Mitsubishi Chemical Foods, Inc. There are decaglyceryl acid (L-7D, HLB16), decaglyceryl myristate (M-10D, HLB15), etc., and these can be used alone or in combination of two or more.

(A) As the polyglycerol fatty acid ester, it is particularly preferable to use a fatty acid residue having 8 to 16, especially 10 to 14, and an average polymerization degree of 6 to 12, especially 8 to 10. Thus, in addition to the removal power against the denture biofilm, the bactericidal power and the antiseptic power of the denture soaking solution, it is possible to obtain a composition and an excellent protease stability. When the fatty acid residue has less than 8 carbon atoms, when oil-soluble fragrances and bactericides are blended, the appearance stability at high and low temperatures cannot be obtained sufficiently, or the stability of protease cannot be obtained sufficiently. There is. If it exceeds 16, the appearance stability at low temperatures may not be satisfactorily improved.
If the average degree of polymerization of the polyglycerol fatty acid ester is less than 6, the appearance stability at low temperatures may not be satisfactorily improved. If it exceeds 12, the appearance stability at high and low temperatures may not be sufficiently improved or sufficient protease stability may not be obtained when oil-soluble fragrances, bactericides and the like are blended.
Specific examples of the polyglycerin fatty acid ester having the carbon number of such fatty acid residues and the average degree of polymerization include decaglyceryl caprylate, decaglyceryl laurate, decaglyceryl myristate, decaglyceryl palmitate, hexaglyceryl caprylate, Those selected from hexaglyceryl laurate and hexaglyceryl myristate, particularly decaglyceryl caprylate, decaglyceryl laurate and decaglyceryl myristate are preferred.

  (A) The compounding quantity of polyglycerol fatty acid ester is suitable 2-50 mass% with respect to the whole composition from the point of the removal power with respect to the denture biofilm after dilution, the bactericidal power, and the preservative power of denture immersion liquid. . If the blending amount is less than 2% by mass, the removal power for the denture biofilm after dilution may not be satisfactorily exhibited, and if it exceeds 50% by mass, the effect of the cationic bactericidal agent after dilution decreases, The sterilizing power and the antiseptic power of the denture soaking solution may not be sufficiently exhibited. In addition, the stability of the protease in the composition is lowered, and the removal power for the denture biofilm after dilution may not be satisfactorily exhibited.

  In particular, the blending amount of the polyglycerin fatty acid ester is more preferably 5 to 30% by mass, particularly 8 to 25% by mass, whereby the storage stability of the composition and the stability of the protease can also be improved. If it is less than 5% by mass, the storage stability at high and low temperatures may not be improved satisfactorily when oil-soluble fragrances and bactericides are blended. If it exceeds 30% by mass, the stability under high and low temperature storage may not be achieved. In some cases, it is not possible to satisfactorily improve the properties, and in any case, a sufficient appearance stability improvement effect may not be obtained. In addition, the effect of improving the stability of the protease may not be sufficiently obtained.

Examples of the component (B) protease include microorganism-derived proteases, plant-derived proteases, animal-derived proteases, and the like, and are not particularly limited, but are preferably derived from microorganisms that can maintain activity in a washing solution. Protease, more preferably alkaline protease that maintains high activity in the washing solution. A protease preparation can also be used as the protease. Here, the protease preparation includes propylene glycol, glycerin, boric acid, formic acid, calcium, and water as a base in addition to protease.
Specific examples include Evalase 16L, Savinase 16L, Cannase, Clearlens Pro (Novozymes), Purefect L, Alkaline Protease GL440 (GENENCOR), Properase L (GENENCOR), etc. Among them, Evaluase 16L and Savinase 16L are preferable. is there. The titer of Evalase 16L is 16 EPU / g or more, usually 16-20 EPU / g. Moreover, the titer of sabinase 16L is 16 KNPU / g or more, usually 16 to 20 KNPU / g.

  (B) The amount of the protease is appropriately adjusted according to the titer, but it is 0 with respect to the entire composition from the viewpoint of the ability to remove and sterilize the denture biofilm after dilution, or the stability of the composition. 0.1 to 5.0% by mass, particularly 0.5 to 2.0% by mass is preferable, and 0.5 to 1.2% by mass is more preferable particularly when Evalase 16L or Sabinase 16L is used. If the blending amount is less than 0.1% by mass, the removal power and sterilization power for the denture biofilm after dilution may not be satisfactorily exhibited. The removal power and sterilization power of denture biofilms may not be satisfactorily exhibited. Moreover, a problem may arise in the external appearance stability of a composition.

  (C) Cationic fungicides include bisguanides such as chlorhexidine hydrochloride and chlorhexidine gluconate, and quaternary ammoniums such as benzethonium chloride, benzalkonium chloride, cetylpyridinium chloride, etc., preferably quaternary. Ammonium compounds such as benzethonium chloride, benzalkonium chloride, and cetylpyridinium chloride are preferable, and benzethonium chloride is particularly preferable in terms of bactericidal power against denture biofilms. One of the above cationic fungicides may be used alone, or two or more thereof may be used in combination.

  (C) The compounding quantity of a cationic disinfectant is 0.2- with respect to the whole composition from the point of the bactericidal power with respect to the denture biofilm after dilution, the preservative power of denture immersion liquid, and also the stability of a composition. 10% by mass, particularly 1.0 to 5.0% by mass is preferable. When the blending amount is less than 0.2% by mass, the bactericidal power against the denture biofilm after dilution and the antiseptic power of the denture soaking solution may not be satisfactorily exhibited. In some cases, the removal power of the diluted biofilm after dilution is not satisfactorily exhibited. In addition, problems such as discoloration may occur under high temperature storage of the composition.

  In the present invention, the mass ratio of (A) polyglycerin fatty acid ester to (C) cationic fungicide is (A) / (C) of 2. from the viewpoint of the removal power and the bactericidal power against the denture biofilm after dilution. It is the range of 5-15, Preferably it is the range of 4-12, More preferably, it is the range of 5-10. If the mass ratio of (A) / (C) is less than 2.5, the removal power for the denture biofilm after dilution is weak, and if it exceeds 15, the uptake of the cationic fungicide into the micelle increases. The sufficient sterilizing power against the diluted denture biofilm and the sufficient antiseptic power in the denture soaking solution cannot be exhibited.

  The denture cleaning liquid composition of the present invention is obtained by blending (D) water, and the water content (moisture content) is the removal power, the bactericidal power and the antiseptic of the denture soaking solution for the denture biofilm after dilution. From the point of force, it can be 30 to 97% by mass with respect to the total amount of the composition, but in addition to the removal power against the denture biofilm after dilution, the bactericidal power and the antiseptic power of the denture soaking solution, From the viewpoint of enhancing the stability of the protease and the appearance stability during low-temperature storage, the water content is preferably 30 to 50% by mass, particularly preferably 35 to 45% by mass. If the water content is less than 30% by mass, the composition may be precipitated under low temperature storage, resulting in poor appearance stability. If it exceeds 97% by mass, the removal ability and sterilization power against the denture biofilm after dilution And the antiseptic power of the denture soaking solution may not be satisfactorily exhibited. Moreover, when it exceeds 50 mass%, the stability of the protease in the composition may be inferior. In this case, the water content of the composition includes water contained in each component such as a glycerin liquid blended in the composition.

  The denture cleaning liquid composition of the present invention is a concentrated type preparation that is used after dilution, and the denture can be cleaned by immersing the denture in a diluted solution obtained by diluting with water such as tap water or purified water. However, in this case, the dilution ratio of the denture cleaning liquid composition with water is from 5 to 500 times, particularly from 25 to 200 times, especially from 50 to 200 times, from the viewpoint of usability and solubility. Dilution is preferred.

  In the denture cleaning liquid composition of the present invention, the diluted solution diluted at the above dilution ratio can be used as a denture immersion solution, and in this case, the concentration of each component in the diluted solution is diluted so as to be in the following range. In particular, in the present invention, the concentration of the component (A) in the diluent is 0.03 to 0.5% by mass, and the concentration of the component (C) is 0.005 to 0.1. It is necessary to dilute the composition with water so as to be in mass% in order to exhibit excellent removal power and sterilization power against denture biofilm and high antiseptic power in denture immersion liquid.

The concentration of each component during use will be described in further detail below.
(A) The concentration in the diluting liquid when polyglycerin fatty acid ester is used (after dilution) is 0.03 to 0.03 of the whole diluting liquid from the viewpoint of the removal power against the denture biofilm, the sterilizing power, and the antiseptic power of the denture immersion liquid. It is 0.5 mass%, More preferably, it is 0.1-0.3 mass%. When the concentration after dilution is less than 0.03% by mass, the removal power and sterilization power against the denture biofilm become insufficient, and when it exceeds 0.5% by mass, the biocidal power against the denture biofilm and the antiseptic power of the denture soaking solution This is not preferable because of a decrease in the thickness.

  In the present invention, nonionic surfactants other than the above (A) polyglycerin fatty acid ester, particularly polyoxyethylene alkyl having an ethylene oxide average addition mole number of 10 to 20 and an alkyl group having 12 to 20 carbon atoms. Ether may not be blended, but (A) when the concentration of the polyglycerol fatty acid ester in the diluted solution at the time of use (after dilution) is 0.03 to 0.1% by mass of the entire diluted solution. Is a polyoxyethylene alkyl ether having an ethylene oxide average addition mole number of 10 to 20 and an alkyl group having 12 to 20 carbon atoms in order to improve the removal power and sterilization power of the denture biofilm. It can mix | blend together.

  In this case, the alkyl group of (A ′) polyoxyethylene alkyl ether has preferably 12 to 20, particularly 12 to 16, particularly 12 or 14, and a single carbon number or different carbon. A number of them may be used in combination, for example, as a mixture of 12 and 14 carbon atoms. If the number of carbon atoms is less than 12, the removal power and bactericidal power for denture biofilms may not be sufficiently improved due to weak surface activity. The antibacterial power against the above and the preservative power of the denture soaking solution are not improved, and the blending effect may not be sufficiently obtained. Moreover, solubility may deteriorate and storage stability may be reduced.

  Moreover, the ethylene oxide average added mole number of polyoxyethylene alkyl ether is preferably 10 to 20, particularly 12 to 18, and particularly preferably 12 to 15. If the average number of added moles is less than 10, the effectiveness of the cationic bactericidal agent is lowered, the bactericidal power against the denture biofilm and the antiseptic power of the denture soaking solution are lowered, and the blending effect may not be sufficiently obtained. Moreover, solubility may deteriorate and storage stability may be reduced. If it exceeds 20, the removal power and sterilization power for the denture biofilm may not be sufficiently improved.

  Examples of such polyoxyethylene alkyl ethers include polyoxyethylene lauryl ether (EO average addition mole number 15), polyoxyethylene myristyl ether (EO average addition mole number 15), and polyoxyethylene alkyl (C12,14) ether. (EO average added mole number 15) and the like can be used, and one of these can be used alone or in combination of two or more, and polyoxyethylene lauryl ether (EO average added mole number 15) is particularly preferable. Used for. These polyoxyethylene alkyl ethers can be obtained from, for example, Nippon Emulsion Co., Ltd. or Lion Chemical Co., Ltd.

  In addition, when mix | blending (A ') polyoxyethylene alkyl ether, the compounding quantity is 2-50 mass% of the total amount of (A) polyglycerin fatty acid ester and (A') polyoxyethylene alkyl ether, and especially 5-5. The range which becomes 30 mass% is preferable, and it is more preferable to set it as 8-15 mass%.

Also, the mass ratio ((A) + (A) of the total amount of (A) polyglycerin fatty acid ester, (A ′) polyoxyethylene alkyl ether ((A) + (A ′)) and (C) cationic fungicide ')) / (C) is preferably in the range of 2.5 to 10, particularly 2.5 to 8, from the viewpoint of removal power and sterilization power for denture biofilms.
Furthermore, when (A ′) polyoxyethylene alkyl ether is blended, the total concentration of (A) polyglycerin fatty acid ester and (A ′) polyoxyethylene alkyl ether in the diluted solution is 0.03 to 0.5 mass. % Is preferable.

  (B) When using protease (after dilution), the concentration in the dilute solution is particularly when Evalase 16L or Sabinase 16L is used from the viewpoint of removal power against denture biofilm, sterilization power and antiseptic power of denture soaking solution. Is preferably 0.001 to 0.02 mass% of the whole diluted solution, and more preferably 0.005 to 0.015 mass%. When it is less than 0.001% by mass, the removal power and sterilization power against the denture biofilm are insufficient, and when it exceeds 0.02% by mass, the effect of the cationic biocide is reduced. The antiseptic power of may not be fully demonstrated.

  (C) The concentration in the diluted solution at the time of use (after dilution) of the cationic disinfectant is 0.005 to the entire diluted solution from the viewpoint of the removal power against the denture biofilm, the sterilizing power, and the antiseptic power of the denture soaking solution. It is 0.1 mass%, it is preferable that it is 0.01-0.05 mass%, and it is more preferable that it is 0.02-0.04 mass%. When the amount is less than 0.005% by mass, sufficient bactericidal power against the denture biofilm and preservative power in the immersion liquid are not exhibited. When the amount exceeds 0.1% by mass, the action of the protease is inhibited and the biofilm is sufficiently removed from the denture biofilm. The power cannot be demonstrated.

  Moreover, the mass ratio in the diluted solution at the time of use (after dilution) of (B) protease and (C) cationic fungicide is the point of the bactericidal power against denture biofilm, the removal power, and the antiseptic power of the denture immersion liquid. In particular, when Evalase 16L or Sabinase 16L is used, the mass ratio of (B) / (C) is preferably in the range of 0.2 to 2, particularly in the range of 0.3 to 1.0. More preferably. When the mass ratio of (B) / (C) is less than 0.2, the cationic bactericidal agent may inhibit the protease, and the removal ability against the denture biofilm may not be sufficiently exerted. May inhibit the effect of the cationic bactericidal agent, and the bactericidal power against the denture biofilm and the antiseptic power in the denture soaking solution may not be sufficiently exhibited.

  The denture cleaning liquid composition of the present invention contains the components (A) to (D) as described above, and can further contain (E) isopropylmethylphenol and / or thymol, Thereby, the bactericidal power with respect to the denture biofilm after dilution can be strengthened. In particular, when the concentration of the (C) cationic fungicide at the time of use (after dilution) is 0.01% by mass or less, or when the concentration of the (A) polyglycerol fatty acid ester is 0.2% by mass or more, When the mass ratio of A) / (C) is 7 or more, in order to enhance the bactericidal power against the diluted denture biofilm, in addition to (C) the cationic bactericidal agent, (E) isopropyl It is preferable to blend methylphenol and / or thymol. These isopropylmethylphenol and thymol may be used alone or in combination of two.

  When the component (E) is blended, the total blending amount of the fungicide of the component (E) is the enhancement of the bactericidal power against the denture biofilm after dilution and the appearance stability when the composition is stored at high and low temperatures. From 0.5 to 2.0% by mass of the entire composition, particularly 0.8 to 1.5% by mass is preferable. If it is less than 0.5% by mass, the effect of enhancing the bactericidal power against denture biofilms is weak, and if it exceeds 2.0% by mass, discoloration during high-temperature storage may occur remarkably, or appearance stability during low-temperature storage may deteriorate. is there.

  Further, when the component (E) is blended, the concentration in the diluting solution when the fungicide of the component (E) is used (dilute) is preferably 0.001 to 0.1% by mass. It is more preferable that it is 005-0.05 mass%. If it is less than 0.001% by mass, the effect of enhancing the bactericidal power against denture biofilms is weak. If it exceeds 0.1% by mass, the solution becomes cloudy at the time of dilution or the denture material (resin) is made by repeatedly immersing dentures. Alteration may occur.

  The denture cleaning liquid composition of the present invention further comprises (F) a polyol and (G) a pH adjuster in order to enhance the storage stability of the whole composition (appearance stability of the composition, protease stability). can do.

  Examples of the (F) polyol used in the present invention include 1,3-butylene glycol, glycerin, propylene glycol, ethylene glycol, polypropylene glycol, polyethylene glycol, and sugar alcohols such as erythritol and sorbit. Among these, glycerin, propylene glycol, and polyethylene glycol are preferably used from the viewpoint of protease stability, and glycerin is particularly preferable. These polyols may be used alone or in combination of two or more.

  In the case of blending (F) polyol, the blending amount of (F) polyol in the composition of the present invention is not particularly limited, but is 20 to 60% by mass in total with respect to the total amount of the composition in terms of protease stability. Preferably, 30-50 mass% is more preferable. If it is less than 20% by mass, the stability of the protease may not be improved, and if it exceeds 60% by mass, the appearance stability during low-temperature storage may be inferior.

  Furthermore, when mix | blending (F) polyol, it is preferable that the density | concentration in the dilution liquid at the time of use of (F) polyol (at the time of dilution) is 0.04-12 mass%.

  The composition of the present invention preferably has a pH at 25 ° C. of 6.0 to 8.5, particularly 6.5 to 8.0, preferably 7.0 to 7.7 in terms of appearance stability and protease stability. 8 is more preferable. If the pH at 25 ° C. is less than 6.0, the stability of the protease is low, and if it exceeds 8.5, discoloration of the high-temperature storage product occurs, resulting in poor appearance stability or repeated denture soaking. Degeneration of denture material (resin) may occur. In addition, as a means of pH adjustment, (G) pH adjuster can be mix | blended as needed. Examples of the pH adjuster in this case include sodium hydroxide, hydrochloric acid, phosphoric acid or a salt thereof, citric acid or a salt thereof, sodium carbonate, sodium bicarbonate, boric acid or a salt thereof. Among these, it is preferable to use sodium hydroxide, hydrochloric acid, phosphoric acid or a salt thereof, citric acid or a salt thereof. Examples of the phosphate include sodium monohydrogen phosphate, potassium monohydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, trisodium phosphate and the like. Examples of the citrate include sodium citrate, calcium citrate, and tripotassium citrate. The blending amount of these pH adjusters only needs to be able to adjust the pH to the above range.

  When a phosphoric acid such as sodium monohydrogen phosphate or sodium dihydrogen phosphate or a salt thereof is added as a pH adjuster among these, (H) in terms of protease stability and appearance stability. Preferably, at least one chelating agent selected from citrate, edetate and water-soluble polyphosphate is used in combination. When a chelating agent selected from citrate, edetate and water-soluble polyphosphate is added, when (B) protease, especially Evalase 16L or Sabinase 16L is used, (B) calcium contained in the protease raw material It can be prevented that phosphoric acid or a salt thereof reacts to precipitate an insoluble matter, resulting in an appearance problem.

  As a chelating agent, for example, sodium citrate, sodium edetate (EDTA-2Na), sodium tripolyphosphate, etc. can be blended, and sodium citrate is particularly remarkable in terms of protease stability and appearance stability during storage at high and low temperatures. It is more preferably used because of its superiority. In addition, about citrate, you may mix | blend for any purpose of a pH adjuster and a chelating agent.

  In this case, when phosphoric acid or a salt thereof is blended as a pH adjuster, the blending amount is 0.1 to 1. of the entire composition from the viewpoint of pH stability, protease stability and appearance stability of the composition. 0 mass% is preferable and 0.2-0.5 mass% is more preferable. If it is less than 0.1% by mass, the stability of the pH may decrease and the stability of the protease may decrease. If it exceeds 1.0% by mass, orientation and discoloration may occur during storage at high or low temperatures.

  Moreover, when mix | blending (H) chelating agent, 0.1-1.0 mass% of the whole composition is preferable from the point of the stability of protease, and the external appearance stability, 0.2-0 More preferable is 5% by mass. If it is less than 0.1% by mass, the effect of suppressing the occurrence of orientation during high-temperature and low-temperature storage may be low, and if it exceeds 1.0% by mass, the stability of the protease may be reduced.

  In addition, when blending (H) chelating agent, mass ratio of (B) protease and (H) chelating agent in the composition (from the viewpoint of protease stability and appearance stability at high temperature storage and low temperature storage ( (B) / (H)) is preferably in the range of 1-10, more preferably in the range of 2-5. If it is less than 1, the protease stability may be lowered, and if it is more than 10, orientation or the like may occur during high-temperature storage and low-temperature storage, and appearance stability may be reduced.

  In the denture cleaning liquid composition of the present invention, other known components can be further blended as necessary in addition to the above components as long as the effects of the present invention are not hindered. Optional ingredients include, for example, fragrances, solvents other than polyols, colorants, cationic fungicides, other fungicides other than isopropylmethylphenol and thymol, (A) polyglycerin fatty acid esters, and (A ′) polypropylene alkyl. Surfactants such as nonionic surfactants other than ether can be used.

  As perfumes, spearmint oil, peppermint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, Natural flavors such as lime oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, cinnamon bark oil, and menthol, Menthone, Carvone, Ethylbutyrate, Vanillin, Ethylmaltol, Anethole, Methyl salicylate, Synamic aldehyde, Cineol, Eugenol, Ethylvanillin, Maltol, Limonene, Citronellol, Linalol, Linalyl acetate, Menthyl acetate, Pine , Octyl aldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ginger oleoresin, creosole, dl-camphor, etc., single fragrance, ethyl acetate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycy Known fragrances used in oral compositions such as single fragrances such as dating, undecalactone, hexanal, ethyl alcohol, propyl alcohol, butanol, isoamyl alcohol and / or various blended fragrances including natural fragrances can be used. .

  In the denture cleaning liquid composition of the present invention, a refreshing feeling can be imparted by blending a fragrance, and the user can more comfortably clean the denture or feel a refreshing feeling when the denture is attached. it can. It is preferable to mix 1 to 4% by mass of the fragrance from the viewpoint of refreshing feeling and appearance stability. When the blending amount is less than 1% by mass, the refreshing feeling and the refreshing feeling may be insufficient when the denture is mounted. If it exceeds 4% by mass, for example, even if 30% by mass of polyoxyethylene alkyl ether is blended, good appearance stability may not be maintained, or discoloration of a high-temperature storage product may occur remarkably.

  In the composition of the present invention, ethanol can be blended as a solvent in order to dissolve hardly soluble components such as oil-soluble fragrances and isopropylmethylphenol. When ethanol is blended, it is preferably blended in the composition in an amount of 4 to 20% by mass, more preferably 6 to 12% by mass. When ethanol is blended in the above concentration range, fragrances, oil-soluble components such as isopropylmethylphenol and thymol are easily dissolved, and the stability of the protease is not inhibited.

  As colorants, Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green No. 3 etc. Legal dye, caramel dye, safflower dye, gardenia dye, cochineal dye, anato dye, mica titanium, titanium oxide and the like.

  In the present invention, in addition to the above (C) cationic fungicide, (E) isopropylmethylphenol and / or thymol, as other fungicides, triclosan, benzoic acid or a salt thereof, salicylic acid or an ester thereof or a salt thereof, Parabens, phenol and the like can be used.

  Examples of the surfactant include other nonionic surfactants such as polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil, sugar alcohol fatty acid esters such as sucrose fatty acid ester, alkylol amide, polyoxyethylene sorbitan monostearate. Polyoxyethylene sorbitan fatty acid ester such as rate, sorbitan fatty acid ester, glycerin fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene glycol fatty acid ester, polyethylene glycol fatty acid ester, polyoxyethylene polyoxypropylene glycol, lauric acid mono- or diethanolamine Fatty acid diethanolamide, polyoxyethylene alkylphenyl ether, etc. can be blended. In addition, as for the compounding quantity of these other surfactant, mass ratio of the nonionic surfactant in the composition containing the said (A) polyglycerol fatty acid ester and (C) cationic disinfectant is 2. In the range which does not exceed 5-15, it can be set as 0-2 mass% of the whole composition, especially 0.1-1 mass%.

  Moreover, there is no restriction | limiting in particular as a container which accommodates this invention composition, Usually, it can be filled and used for the container currently applied to the composition for oral cavity. Specifically as such a container, a polyethylene layer, an ethylene methacrylic acid copolymer layer, a polyethylene terephthalate layer, an aluminum layer, a glass vapor deposition layer, a polyvinyl alcohol layer, an ethylene vinyl alcohol copolymer layer, an acrylonitrile copolymer layer, Laminate containers made of paper, recycled plastic layers, etc., or polyethylene containers, polyethylene terephthalate containers, polypropylene containers, etc. can be used. Tube containers, dispensers containers with mechanical or differential pressure, film packaging containers such as pillow packaging, etc. Various containers usually used as the composition can be used. A polyethylene terephthalate container is preferable.

  In order to wash dentures with the concentrated denture cleaning liquid composition of the present invention, for example, the composition of the present invention is put in a container such as a cup, and the composition is diluted with tap water or purified water to obtain a diluted solution. It is only necessary to prepare and soak the denture overnight, and after soaking, the denture can be taken out and rinsed with water before being mounted. It is more effective to remove the dirt lightly with a toothbrush or the like and then immerse the denture in the diluent.

  EXAMPLES Hereinafter, although an experimental example, an Example, and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples,% means mass% unless otherwise specified. The compounding amount of each compounding component in the compounded product (denture cleaning liquid composition) in the table indicates the amount converted into a pure component for the components (A), (C) and (F). Moreover, since the sodium hydroxide mix | blended as a pH adjuster in Table 1,3,5,7 is a trace amount, the compounding quantity was considered to be zero and (D) moisture content was computed.

Moreover, the following were used as each component of a raw material.
Decaglyceryl laurate (HLB16); manufactured by Taiyo Kagaku (trade name Sunsoft M-12J)
Decaglyceryl laurate (HLB17); manufactured by Taiyo Kagaku Co., Ltd. (trade name Sunsoft Q-12Y)
Decaglyceryl myristate (HLB15); manufactured by Mitsubishi Chemical Foods Co., Ltd. (trade name Ryoto Polyglycerester M-10D)
Decaglyceryl caprylate (HLB17); manufactured by Taiyo Kagaku Co., Ltd. (trade name Sunsoft Q-10Y)
Pentaglyceryl myristate (HLB12); manufactured by Taiyo Kagaku (trade name Sunsoft A-141E)
Polyoxyethylene (POE) lauryl ether (ethylene oxide (EO) addition mole number 15); manufactured by Nippon Emulsion Co., Ltd. (trade name EMALEX 715)
Decaglyceryl trilaurate (HLB10) (comparative product); manufactured by Taiyo Kagaku Co., Ltd. (trade name Sunsoft Q-123Y)
Sucrose stearate ester (HLB15) (comparative product); manufactured by Mitsubishi Chemical Foods Corporation (trade name Ryoto Sugar Ester S-1570)
Alkyl (C12,14) glycoside (comparative product); manufactured by Henkel (trade name Plantacare 2000UP)

Protease; manufactured by Novozymes (trade name Evalase 16L)
Novozymes (trade name Sabinase 16L)
Benzethonium chloride; manufactured by Mitsui Lifetech Co., Ltd. (trade name Hyamine)
Cetylpyridinium chloride; benzalkonium chloride manufactured by Wako Pure Chemical Industries, Ltd .; chlorhexidine chloride manufactured by Nippon Oil & Fats Co., Ltd .; alkyl chloride (C12,14) diaminoglycine (comparative product) manufactured by Wako Pure Chemical Industries, Ltd .; Sanyo Made by Kasei Co., Ltd. (trade name Levon LAG-40, 40% product)
Photosensitive element 201 (comparative product); manufactured by Koseisha
Isopropyl methylphenol; Osaka Chemical Co., Ltd. thymol; Osaka Kasei Co., Ltd. glycerin; Sakamoto Pharmaceutical Co., Ltd. (85% product)
Propylene glycol; Showa Denko Co., Ltd. sorbit; 70% sorbite solution, Towa Kasei Kogyo Co., Ltd. erythritol; Mitsubishi Chemical Foods Co., Ltd. sodium monohydrogen phosphate and sodium dihydrogen phosphate; Taihei Chemical Industry Co., Ltd. Sodium citrate manufactured by Iwata Chemical Co., Ltd. Other optional ingredients: All used are Japanese Pharmacopoeia or quasi-drug raw material compliant products.

[Examples and Comparative Examples]
Preparations of the compositions shown in the following Tables 1, 3, 5, 7, 9, 11, and 13 (denture cleaning liquid compositions) were prepared by the following manufacturing method, and the denture biofilm removal power, bactericidal power, The antiseptic power and storage stability of the denture soaking solution were evaluated. The results are shown in Tables 2, 4, 6, 8, 10, 12, and 14.
<Production method>
(1) A phase was prepared by mixing and dissolving water-soluble components such as a cationic bactericide, polyol, and protease in purified water. A pH adjuster was added if necessary.
(2) Ethanol and heated and melted polyglycerin fatty acid ester were mixed to prepare B phase. In the case of addition, oil-soluble components such as fragrance, isopropylmethylphenol, and thymol were added.
(3) The B phase was added to and mixed with the A phase while stirring to obtain a denture cleaning liquid composition.

<PH measurement method>
The value after 3 minutes at 25 ° C. with a pH meter (manufactured by Toa Denpa Kogyo Co., Ltd., HM-30V) and a pH electrode (manufactured by Toa Denpa Kogyo Co., Ltd., GST-5421C) for the blended product transferred to a glass container. Was measured.

<Measurement method of HLB value>
The HLB value of the polyglycerin fatty acid ester of component (A) is calculated using the Atlas method (HLB value = 20 (1-S / A)) where S is the saponification value and A is the acid value of the fatty acid constituting the surfactant. did.

<Preparation of sample solution>
In order to achieve the dilution ratios shown in Tables 2, 4, 6, and 8 in the following Tables 1, 3, 5, and 7 (liquid compositions for cleaning dentures), they were diluted with tap water. This diluted solution was used as a sample solution in the following Test Examples 1 to 3. The volume of the sample solution (diluted solution) used for the test was 1.8 mL.

Test Example 1 Removal power test for denture biofilm In order to verify the removal power of the denture cleaning liquid composition of the present invention for a denture biofilm, a denture biofilm model was created and evaluated in vitro.

<Denture biofilm model creation method>
A 1 × 1 cm polymerized acrylic plate was placed in a 24-well plate, and 0.5 mL of a 0.5% mucin solution and 0.5% albumin solution mixture was placed there and allowed to stand at 37 ° C. for 1 hour. After 1 hour, the mucin albumin solution was removed. Next, 50 μL each of Candida albicans (Candida albicans IFO1594) and Streptococcus mutans (Streptococcus mutans ATCC25175) were collected from the precultured bacterial solution and dispersed in PBS (turbidity OD = 1.0 concentration at 660 nm). And allowed to stand at 37 ° C. for 2 hours. Thereafter, 1.8 mL of tributicase soy broth (TSB) medium was added and cultured at 37 ° C. for 20 hours to prepare a denture biofilm. After 20 hours, the medium was removed from the well, and 1 mL of water was added for washing, and the operation of removing water was repeated twice.

<Removal power test>
The denture biofilm model prepared by the above method was placed in a new 24-well plate and immersed in 1.8 mL of the sample solution overnight. The next day, after shaking the plate to remove the broken denture biofilm, the sample solution was removed and washing with 1 mL of water was repeated twice. The acrylic plate was transferred to a test tube, and the biofilm was peeled and dispersed in water with ultrasound and vortex, and the turbidity (OD = 660 nm) was measured (OD sample). As a control, turbidity (OD control) was similarly measured for a biofilm immersed in water overnight, and the denture biofilm removal rate was calculated according to the following formula. This test was measured three times, the average value was obtained, and the removal power against denture biofilm was evaluated according to the following criteria.
Removal rate (%) = {(OD control−OD sample) / OD control} × 100

<Evaluation criteria>
Denture biofilm removal rate 80% or more: ◎
６０ 60% or more and less than 80%: ○
５０ 50% to less than 60%: △
未 満 Less than 50%: ×

Test Example 2 Bactericidal power test for denture biofilm In order to verify the bactericidal power of the liquid composition for denture cleaning of the present invention to microorganisms in the denture biofilm, a denture biofilm model was created and evaluated in vitro.

<Bactericidal test>
Put the denture biofilm model created by the above method into a new 24-well plate, soak it overnight in 1.8 mL of sample solution, shake the plate the next day to remove the broken biofilm, remove the sample solution and wash with water Was repeated twice. The acrylic plate was transferred to a test tube, the biofilm was peeled and dispersed in PBS with ultrasound and vortex, and then diluted serially with PBS. After 100 μL of each diluted solution was smeared on tributicase soy agar (TSA) medium and cultured at 37 ° C. for 4 days, the number of colonies was counted as the number of remaining bacteria, and the bactericidal effect was evaluated according to the following evaluation criteria. The number of colonies was similarly measured for a biofilm immersed in water overnight as a control. This test was performed twice, the average value was calculated | required, and the bactericidal power with respect to a denture biofilm was evaluated by the following evaluation criteria.

<Evaluation criteria>
The number of colonies was measured and evaluated by the number of bacteria reduced with respect to the control (water).
Decreasing number of bacteria = control (water) number of bacteria−number of sample treated bacteria 0 to 10: ×
11 to 100: △
101-1000: ○
1001-: ◎

Test Example 3 Preservative Power Test In order to verify the preservative power during denture immersion in the diluted solution of the denture cleaning liquid composition of the present invention, a denture biofilm model was created and evaluated in vitro.

<Preservation test>
The denture biofilm model prepared by the above method is placed in a new 24-well plate, immersed in 1.8 mL of the sample solution overnight, and 40 μL of the immersion solution is collected the next day, and a soybean / casein digest (SCDLP) liquid medium supplemented with lecithin / polysorbate Diluted 100 times. 100 μL of the diluted solution was smeared on an SCDLP agar medium and cultured at 37 ° C. for 4 days, and the number of colonies was counted as the number of remaining bacteria. This test was performed twice, the average value was calculated | required, and the preservative power in denture immersion was evaluated by the following evaluation criteria.

<Evaluation criteria>
The number of colonies was measured and evaluated based on the number of grown bacteria.
0: ◎
1 to 50: ○
51-300: △
301-: x

  From the results of Tables 1 to 4, it was found that the denture cleaning liquid composition of the present invention was excellent in the removal power against the denture biofilm, the bactericidal power, and the antiseptic power of the denture immersion liquid. On the other hand, from the results of Tables 5 to 8, when any of the essential components of the present invention is not contained, (A) polyglycerin fatty acid ester or (C) cationic fungicide is used (when diluted). ) Concentration is outside the predetermined range, or when the mass ratio of (A) / (C) is outside the predetermined range, the removal power against the denture biofilm, the bactericidal power, and the antiseptic power of the denture soaking solution It was found that sufficient effects were not exhibited in any of the points.

Test Example 4 Storage Stability Test Regarding the blended products (denture cleaning liquid composition) shown in Tables 9, 11, and 13, the storage stability of the denture cleaning liquid composition was evaluated by the following method. Moreover, the removal power with respect to a denture biofilm, the bactericidal power, and the antiseptic power of denture immersion liquid were evaluated about the dilution liquid of the compounded product (denture cleaning liquid composition) like the above. The results are shown in Tables 10, 12, and 14.

<Evaluation Method> Appearance Stability About 40 g of the sample (formulated product) was stored in a 50 mL transparent PET container for 1 month under high temperature (50 ° C.) and low temperature (−10 ° C.) conditions. The sample after storage was allowed to stand at room temperature for 1 day, and then the appearance change (precipitate / liquid separation / discoloration) was evaluated. Enzyme activity was measured and storage stability was evaluated.

<Evaluation criteria>
No change is observed in any of precipitate, liquid separation and discoloration: ◎
Slight changes are observed in any of the items of sediment, liquid separation, and discoloration, but there is no problem: ○
Changes are observed in any of the items of sediment, liquid separation, and discoloration: △
Changes are observed in any of precipitates, liquid separation, and discoloration: ×

<Evaluation Method> Enzyme Stability About 20 g of the sample (formulated product) was stored in a 20 mL glass vial at 40 ° C. for 1 month. The sample after storage was allowed to stand at room temperature for 1 day, and then enzyme activity was measured to evaluate storage stability. As a method for measuring enzyme activity, peptidyl p-nitroaniline was used as a substrate, and the increase rate of p-nitroaniline released by hydrolysis was determined by measuring the absorbance at 405 nm.

<Evaluation criteria>
Residual rate of enzyme after storage for 1 month at 40 ° C 80% or more: ◎
７０ 70% or more and less than 80%: ○
〃 50% to less than 70%: △
未 満 Less than 50%: ×

  From the results of Tables 9 to 14, the denture cleaning liquid composition of the present invention is excellent in removal power, sterilization power and antiseptic power of denture soaking solution for the denture biofilm after dilution, and in particular, the component (A) has 8 carbon atoms. It is an ester of polyglycerin having a fatty acid of ˜16 and an average degree of polymerization of 6 to 12, the blending amount of which is 5 to 30% by mass, (D) a water content of 30 to 50% by mass, and (F) a polyol, ( G) It was found that those containing a pH adjuster and having a pH of 6.0 to 8.5 were superior in appearance stability and protease stability during high-temperature storage and low-temperature storage of the blended product before dilution.

Claims (4)

A concentrated denture cleaning liquid composition that is diluted with water and applied to a denture during use,
(A) Polyglycerin fatty acid ester having an HLB value of 12 to 17 (B) Protease (C) Cationic fungicide (D) Water is included, and the mass ratio of (A) / (C) is 2.5 to And diluted with water so that the concentration of component (A) is 0.03 to 0.5% by mass and the concentration of component (C) is 0.005 to 0.1% by mass. A liquid composition for cleaning dentures.   The denture cleaning liquid composition according to claim 1, further comprising (E) isopropylmethylphenol and / or thymol.   (A) 5 to 30% by mass of polyglycerin fatty acid ester having a fatty acid residue of 8 to 16 carbon atoms and an average polymerization degree of 6 to 12 as polyglycerin fatty acid ester, and (D) 30 to 50% by mass of water The denture cleaning liquid composition according to claim 1 or 2, further comprising (F) a polyol and (G) a pH adjuster, and having a pH of 6.0 to 8.5 at 25 ° C. .   (G) The pH adjuster is phosphoric acid or a salt thereof, and (H) at least one chelating agent selected from citrate, edetate and water-soluble polyphosphate is added to (B) protease / (H 4. The denture cleaning liquid composition according to claim 3, wherein the chelating agent has a mass ratio of 1 to 10.