WO2023008985A1 - Abrasive composition including enzymatically treated, ground pear for companion animal toothpaste and pet toothpaste composition comprising same - Google Patents

Abstract

The present invention relates to a method for preparing an abrasive composition for companion animal toothpaste and a toothpaste composition, prepared thereby, for companion animals, the method comprising the steps of: (a) thermally treating crushed pear, filtering out the pear juice, and drying the residue to obtain a ground pear powder; (b) pulverizing the ground pear powder and screening the pulverized powder by size to select ground pear powder that can pass through a 30 mesh, but cannot through a 60 mesh; (c) reacting the selected ground pear powder with an alcohol to obtain a precipitate; and (d) enzymatically treating the precipitate with Aspergillus niger-derived rapidase, removing the supernatant from the enzymatically treated matter, and drying the precipitate with hot air. Thus, the toothpaste composition exhibits remarkably better effects, such as proper abrasion of animal teeth, prevention and removal of dental plaques and calculus, and suppression of gingivitis, than conventional commercially available animal toothpastes or toothpastes having a ground pear ingredient simply introduced thereto. Employing natural materials, the toothpaste composition is harmless to companion animals such as dogs or cats even when they ingest the toothpaste ingredients during tooth brushing.

Description

Toothpaste abrasive composition for companion animals containing pear enzyme treatment and toothpaste composition for companion animals containing the same

The present invention relates to a toothpaste abrasive composition for companion animals containing a pear enzyme-treated material and a toothpaste composition for companion animals containing the same, and more particularly, to a toothpaste abrasive material for companion animals containing a pear enzyme-treated material containing stone cells. It relates to a composition and a toothpaste composition for companion animals comprising the same.

Stone cells are also called reinforcing cells or sclerenchyma cells, and have shorter, thicker, irregular, and very hard secondary cell walls than fibrous cells. Stone cells are found in fruit tissues, especially in the pulp of the genus Pyrus. Stone cells are a type of lignification in which lignin is deposited on cell walls in tissues, and it is known that they serve as a framework for fixing cell walls so that they do not change in shape by strengthening cell walls.

The main component of stone cells in pear fruits was studied by Ranadive and Haard in Western pears a long time ago. It is known to contain 18 to 35% of lignin, which is not present in the primary cell wall. In addition, the main units of lignin are vanillin and syringaldehyde.

On the other hand, toothpaste for companion animals is a kind of tooth cleaner for preventing or removing food debris, bacterial film, plaque, calculus, etc. attached to teeth, and may contain ingredients that prevent tooth decay or bad breath by delivering ingredients effective in preventing tooth decay. there is. Toothpaste includes a liquid type with low viscosity, a paste type with high viscosity, and a powder type, but the paste type is mainly used. On the other hand, the components of pet toothpaste are an abrasive composition that physically removes debris attached to animal teeth, a surfactant that helps effectively remove debris that is firmly attached to animal teeth, and water that has an appropriate viscosity and can maintain its shape. An excipient that helps to prevent hardening and a moisturizer that prevents hardening are the main components, and an abrasive composition such as a flavoring agent, a sweetener, a preservative, a colorant, etc. may be included so that there is no objection when brushing animals.

Although the role of the abrasive composition for animal toothpaste is to physically remove debris on the tooth surface, the degree of abrasion of the abrasive composition is important because it can abrade tooth enamel or dentin. Representative abrasive compositions include monocalcium hydrogen phosphate, precipitated calcium carbonate, silica, and insoluble sodium metaphosphate. These abrasive compositions have a problem in that tooth enamel can be worn because their hardness is higher than that of apatite carbonate, a component of tooth enamel. . In addition, since the currently used abrasive compositions have an average particle diameter of 10 to 30 μm, for effective polishing, the addition amount should be 40% or more in weight ratio and the brushing time should be increased.

On the other hand, in order to solve the above problems, toothpaste compositions containing natural products have been developed. Conventionally developed oral compositions such as toothpaste have been disclosed that include plant extracts such as green tea extract, moth extract, horsetail extract, and myrrh extract in walnut shell powder, which are effective in removing plaque and preventing gum disease. , In the case of walnut shell powder particles, the surface is very rough, so the enamel of teeth can be worn, and since most of the walnut shell powder is imported, there is a problem in that expensive costs are required when used for polishing purposes.

In addition, a toothpaste composition comprising a vegetable abrasive composition obtained by freeze-drying a component containing fibers of plant leaves, stems, and fruit peels and then pulverizing the fiber powder with a starch solution or polymer and coating is disclosed. Since the polishing effect cannot be greatly improved with the same vegetable abrasive composition alone, there is a problem in that an abrasive composition composed of chemical components such as silica, potassium carbonate, sodium bicarbonate, calcium monohydrogen phosphate, and alumina must be included.

The object of the present invention is that the effects such as proper polishing of animal teeth, prevention and removal of plaque and calculus, and inhibition of gingivitis are remarkably superior to conventional commercial animal toothpaste or toothpaste simply introducing pear peel components, and brushing teeth by using natural materials It is an object of the present invention to provide a toothpaste abrasive composition for companion animals containing an enzyme-treated pear shell containing stone cells harmless to a living body even when companion animals such as dogs or cats consume toothpaste components, and a toothpaste composition for companion animals containing the same.

Another object of the present invention is to select the abrasive composition components using pear shells by particle size without using complicated processes or harmful chemicals, and only by performing alcohol treatment and enzyme treatment to improve the polishing effect of animal teeth, gingivitis , A method for producing a toothpaste abrasive composition for companion animals comprising an enzyme-treated product of pear shell containing stone cells that is significantly superior to conventional commercial animal toothpaste or toothpaste simply introducing pear shell components in plaque and calculus inhibitory effect, and a companion animal composition comprising the same It is to provide a method for preparing a toothpaste composition for animals.

According to one aspect of the present invention,

(a) heat-treating the pear pulverized solution, filtering to remove the pear juice, and drying the by-product to obtain pear pear powder;

(B) after pulverizing the pear powder, passing through a 30-mesh mesh and screening to a size that does not pass through a 60-mesh mesh to obtain a screened pear powder;

(c) reacting the selected pear powder with alcohol to obtain a precipitate; and

(d) enzymatically treating the precipitate with Aspergillus niger-derived rapidase, removing the supernatant from the enzymatically treated product and drying the precipitate with hot air; A method for preparing a dentifrice abrasive composition is provided.

In step (a), the heat treatment may be performed at 100 to 140 °C.

In step (c), the alcohol may be a lower alcohol having 1 to 4 carbon atoms.

The alcohol may be an aqueous solution of ethanol at a concentration of 40 to 50%.

In step (d), the Aspergillus niger-derived rapidase may be added in an amount of 0.01 to 0.15 wt% of solids.

In step (d), the Aspergillus niger derived rapidase is cellulase, hemicellulase, beta-glucanase and pectinase ( pectinase).

In step (d), the enzymatic treatment may be performed at 35 to 40° C. for 8 to 20 hours.

In step (d), the hot air drying may be performed at 50 to 70° C. for 10 to 20 hours.

According to another aspect of the present invention,

A toothpaste abrasive composition for companion animals prepared according to the manufacturing method of the abrasive composition for animal toothpaste is provided.

The toothpaste abrasive composition for companion animals may have a total dietary fiber content of 75 to 85% (w/v).

The toothpaste abrasive composition for companion animals may have an insoluble dietary fiber content of 65 to 80% (w/v).

The stone cell content may be 85 to 95% based on the total weight of the insoluble dietary fiber.

The toothpaste abrasive composition for companion animals may have a water absorption capacity of 1.2 to 2 ml/g based on the passage of 1 to 24 hours.

According to another aspect of the present invention,

A toothpaste composition for companion animals is provided, including the toothpaste abrasive composition for companion animals prepared according to the manufacturing method of the toothpaste abrasive composition for companion animals.

The toothpaste composition for companion animals may have a moisture content of 25 to 35%.

The toothpaste composition for companion animals may include 3 to 15 wt% of the toothpaste abrasive composition for companion animals based on the total weight.

The toothpaste composition for companion animals may be used to remove or inhibit gingivitis, plaque or calculus.

The toothpaste abrasive composition for companion animals comprising the enzyme-treated pear shell containing stone cells of the present invention and the toothpaste composition for companion animals containing the same are suitable for polishing animal teeth, preventing and removing plaque and calculus, suppressing gingivitis and The same effect is significantly superior to conventional commercial animal toothpaste or toothpaste that simply introduces pear pear components, and by using natural ingredients, there is an effect that is harmless to the body even if companion animals such as dogs and cats ingest toothpaste components when brushing teeth.

The manufacturing method of a toothpaste abrasive composition for companion animals containing an enzymatically treated product of pears containing stone cells and the manufacturing method of a toothpaste composition for companion animals including the same of the present invention are complex processes or harmful Simple introduction of conventional commercial animal toothpaste or pear-shell components to prevent polishing of animal teeth, gingivitis, plaque, and calculus, without using chemical products, by sorting the pear material by particle size, and by performing alcohol treatment and enzyme treatment. Significantly better than toothpaste.

1 is a photograph of a functional toothpaste for companion animals according to Examples 1 to 3 and Comparative Example 1.

2 is a stereomicrograph after staining of a pear shell powder sample according to Experimental Example 1.

Figure 3 is a standard curve according to the dyed photograph and color difference value according to the stone cell concentration for examining stone cell purity in Experimental Example 1.

4 shows a polishing process using beagle teeth according to Experimental Example 4.

5 is a 3D-OP surface shape photograph of a tooth before and after using the toothpaste according to Experimental Example 4;

6 is a photograph of performing scaling and brushing according to Experimental Example 5.

7 is a photograph of fecal evaluation criteria according to Experimental Example 5.

8 is a result of measuring the gingival index (GI), plaque index (PI), and calculus index (CI) of an untreated control group without brushing according to Experimental Example 5.

Figure 9 is a gingival index (GI), plaque index (PI), calculus index in the teeth of the experimental beagle treated with the commercial animal toothpaste (containing 5% walnut shell) of Comparative Example 3 according to Experimental Example 5 and the toothpaste of Example 3. It is the result of measuring (CI).

10 is a photograph showing the dental condition of a beagle after 4 weeks of brushing using the non-treatment according to Experimental Example 5, the commercial animal toothpaste containing walnut shells of Comparative Example 3, and the functional toothpaste of Example 3.

11 is a fecal evaluation result according to Experimental Example 5.

Since the present invention can apply various transformations and have various embodiments, specific embodiments will be illustrated in the drawings and described in detail in the detailed description. However, it should be understood that this is not intended to limit the present invention to specific embodiments, and includes all transformations, equivalents, and substitutes included in the spirit and scope of the present invention. In describing the present invention, if it is determined that a detailed description of related known technologies may obscure the gist of the present invention, the detailed description will be omitted.

Terms used in this application are only used to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, the terms "include" or "have" are intended to designate that there is a feature, number, step, operation, component, part, or combination thereof described in the specification, but one or more other features It should be understood that the presence or addition of numbers, steps, operations, components, parts, or combinations thereof is not precluded.

Hereinafter, a method for producing a toothpaste abrasive composition for companion animals containing the enzyme-treated pear shell of the present invention will be described.

First, the pear pulverized liquid is heat-treated, filtered to remove pear juice, and the by-product is dried to obtain pear pear powder (step a).

The heat treatment is preferably performed at 100 to 140 °C, more preferably at 110 to 130 °C, and even more preferably at 115 to 125 °C.

The filtration is preferably performed 2 to 3 times using a non-woven fabric to remove pear juice.

Thereafter, the pear powder is pulverized and then passed through a 30 mesh mesh and screened to a size that does not pass through a 60 mesh mesh to obtain a sorted pear shell powder (step b).

The selected pear powder is preferably selected to a size that passes through a 30 mesh mesh and does not pass through a 60 mesh mesh, more preferably a size that passes through a 30 mesh mesh and does not pass through a 50 mesh mesh, even more preferably Preferably, it can be used by selecting a size that passes through a 30 mesh network and does not pass through a 50 mesh network. In the case of selecting the size of such particles, the polishing performance can be improved by increasing the density of stone cells.

If the particle size is less than 30 mesh, the particle size of the pear component may cause a foreign body feeling or damage the teeth, and if it exceeds 60 mesh, the particle size is too small and the abrasive performance for pet toothpaste may deteriorate.

In the present invention, the mesh unit was based on KS A 5101 (a unit representing particle size by a standard sieve), and the mesh and micrometer (μm) unit conversion table according to this is shown in Table 1 below.

Next, the selected pear powder is reacted with alcohol to obtain a precipitate (step c).

In step (c), the alcohol is preferably a lower alcohol having 1 to 4 carbon atoms, more preferably a 40 to 50% aqueous ethanol solution, and even more preferably a 43 to 47% concentration It may be an aqueous solution of ethanol.

The reaction with the alcohol is preferably carried out while stirring at a speed of 100 to 140 rpm at 20 to 30 ° C., and more preferably reacted while stirring at a speed of 110 to 130 rpm at 23 to 27 ° C. to accelerate the reaction.

Finally, after enzymatically treating the precipitate with Aspergillus niger-derived rapidase, the supernatant is removed from the enzymatically treated product and the precipitate is dried with hot air (step d).

The Aspergillus niger derived rapidase is a complex containing cellulase, hemicellulase, β-glucanase and pectinase. is an enzyme

The Aspergillus niger-derived rapidase is preferably added in an amount of 0.01 to 0.15 wt% of solids, more preferably 0.05 to 0.13 wt%, and still more preferably 0.08 to 0.12 wt%. It can be added in wt% amount.

As the buffer solution, sodium acetate, sodium phosphate, 2-ethanesulfonic acid (PIPES), water, etc. may be used, and sodium acetate may be preferably used.

The enzymatic treatment is preferably performed at 35 to 40° C. for 10 to 20 hours. In this case, when the abrasive composition, which has the highest enzyme activity and is an enzyme-treated product, is used in toothpaste for companion animals, the abrasive effect, gingivitis, plaque, and calculus inhibitory effect can be increased.

The obtained enzyme-treated material is centrifuged to obtain a precipitate, which can be used as a functional abrasive composition of toothpaste for companion animals.

The hot air drying is preferably performed at 50 to 70°C for 10 to 20 hours, more preferably at 55 to 65°C for 13 to 18 hours.

The present invention provides a toothpaste abrasive composition for companion animals prepared according to the manufacturing method of the toothpaste abrasive composition for companion animals.

The toothpaste abrasive composition for companion animals may have a total dietary fiber content of 75 to 85% (w/v). Here, total dietary fiber means the content including insoluble dietary fiber and soluble dietary fiber.

In addition, the toothpaste abrasive composition for companion animals may have an insoluble dietary fiber content of 65 to 80% (w/v), preferably 70 to 75% (w/v). Here, the water-soluble dietary fiber content is the total dietary fiber content minus the insoluble dietary fiber content, and since water-soluble dietary fiber has high water absorption, it may reduce formulation stability when used as a toothpaste component, so a formulation with a low water-soluble dietary fiber content It can be advantageous to improve stability.

In addition, the content of stone cells in the total amount of insoluble dietary fiber may be 85 to 95%, preferably 90 to 93%. Here, stone cells can be defined as components containing lignocellulose and ligne. When the stone cell content is within the above range, polishing performance can be remarkably improved when used as an abrasive composition of toothpaste for companion animals.

The high stone cell content in the total amount of insoluble dietary fiber in the toothpaste abrasive composition for companion animals of the present invention is because cellulose, hemicellulose, etc. other than stone cells are removed by the enzyme treatment.

The toothpaste abrasive composition for companion animals may have a water absorption capacity of 1.2 to 2 ml/g, preferably 1.4 to 1.6 ml/g, based on the lapse of 1 to 24 hours. This low water absorption capacity seems to be due to the high purity of stone cells, and there is an effect of preventing formulation stability deterioration due to water absorption during toothpaste manufacturing.

The present invention provides a toothpaste composition for companion animals comprising the toothpaste abrasive composition for companion animals.

In addition, the toothpaste composition for companion animals preferably has a moisture content of 25 to 35%, more preferably 27 to 30%.

The toothpaste composition for companion animals preferably contains 3 to 15 wt% of the toothpaste abrasive composition for companion animals, more preferably 5 to 10 wt%, based on the total weight. If it is included in less than 3wt%, the abrasive effect, gingivitis, plaque and calculus inhibitory effect may be reduced, and if it exceeds 15wt%, the tooth surface may be damaged or the gums may be irritated or damaged.

The toothpaste composition for companion animals may be selected from cream, powder, paste, gel and liquid types.

The toothpaste composition for companion animals may be used for removing or inhibiting gingivitis, plaque or calculus.

The toothpaste composition for companion animals of the present invention may include a detergent together with the toothpaste abrasive composition for companion animals.

Conventional surfactants may be used as the cleaning agent. These detergents prevent foreign substances separated from the tooth surface during brushing from adhering to the tooth surface again, and function to ensure that they are completely discharged from the mouth during brushing. These detergents include alkyl sulfates, olefin sulfonates, monoglyceride sulfonates, etc. Anionic surfactants such as polyoxyethylene sorbitan fatty acid ester, polyoxyethylene castor oil, glycerin fatty acid ester, nonionic surfactants such as alkylolamide, and amphoteric surfactants such as Pluronic F-108. can

All of these detergents are listed by way of example, and in addition to these, various kinds of detergents having surface activity can be used as long as they are not harmful to animals.

In addition, an excipient may be used to increase the weight or form a paste, etc., and an excipient means an orally acceptable carrier.

The toothpaste composition may further include xylitol, a fluorine compound, or a caries preventing component composed of a mixture of two or more thereof in an amount of 0.1 to 5% by weight based on the total weight of the toothpaste composition. The xylitol is obtained from a natural substance such as a birch tree extract, and is known to be effective in preventing tooth decay by suppressing the propagation of bacteria while having a sweet taste but not containing sugar. The xylitol can also be used as a sweetener. Fluorine compounds have also been known to be effective in preventing tooth decay for a long time, and are known to those skilled in the art to easily purchase and use them.

In addition, in the toothpaste composition for companion animals of the present invention, other wetting agents, binders, foaming agents, sweeteners, flavoring agents, coloring agents, or auxiliary components consisting of a mixture of two or more of them are present in an amount of 0.1 to 50% by weight based on the total weight of the toothpaste composition. More may be included. These wetting agents, foaming agents, sweetening agents, flavoring agents, and coloring agents are also things that can be understood as known enough to be easily purchased and used by those skilled in the art of toothpaste manufacturing.

In addition, titanium dioxide or the like may be used to improve whitening. If the auxiliary components are included in less than 0.1% by weight based on the total weight of the toothpaste composition, there may be a problem in that it is difficult to form an appropriate toothpaste by these auxiliary components, and conversely, even if it exceeds 50% by weight, other There may be a problem that causes a lack of content of components.

On the other hand, a humectant is an essential base component for making toothpaste formulations, and prevents toothpaste from drying and solidifying when exposed to air, provides gloss to the surface of toothpaste, and also serves to give a sweetening effect when brushing teeth depending on the type. In addition, the binder serves to prevent separation between the solid powder component and the liquid component. Any type of water-soluble polymer can be used, and commonly used ingredients include sodium carboxymethylcellulose synthesized from cellulose of trees, carrageenan extracted from seaweed, and xanthan gum obtained from metabolism of microorganisms. . In addition, the foaming agent enhances the feeling of use of the product, helps in cleaning, and quickly disperses and penetrates other active ingredients, and reduces interfacial tension to easily remove foreign substances in the oral cavity. As the foaming agent, sodium lauryl sulfate, which is an anionic surfactant, polyoxyethylene-polyoxypropylene copolymer (poloxamer), polyoxyethylene hydrogenated castor oil, polyoxyethylene sorbitan fatty acid ester, and the like may be used.

In addition to the above ingredients, spices, sweeteners, colorings, etc. may be used to improve the feeling of use. As spices used for this purpose, it is common for animals to consume even a small amount when brushing their teeth, so it is essential to use edible spices. Saccharin sodium and stevioside are used as the sweetening agent, and food coloring is preferably used as the colorant.

The present invention provides a method for manufacturing a toothpaste composition for companion animals, including a method for manufacturing a toothpaste abrasive composition for companion animals.

Examples of the present invention will be described below, but the scope of the present invention is not limited thereto.

[Example]

Preparation Example 1: Preparation of pear shell powder

100 g of the pear pulverized liquid was heated at 120 ° C. for 3 hours under high pressure and filtered twice through a non-woven fabric to prepare pear juice, and then pear pear powder, a remaining by-product, was obtained, and the lightness was measured as 60.2 - 65.4.

Preparation Example 2: Selected pear shell powder

After pulverizing the pear powder prepared in Preparation Example 1 with a blender, only the 30 to 60 mesh size in which stone cells are dense was selected to prepare a selected pear powder.

Preparation Example 3: Enzyme-treated animal toothpaste abrasive

The selected pear powder prepared according to Preparation Example 2 was treated with ethanol and enzyme.

Specifically, in the ethanol treatment, 10 g of the sample was reacted at 120 rpm at 25 ° C. for 1 hour in a 45% ethanol aqueous solution contained in a 1 L Erlenmeyer flask to dissolve stone cells and dietary fiber. Thereafter, centrifugation was performed at 8,000 rpm for 10 minutes, and the supernatant was removed at 4°C. Thereafter, it was washed twice with water, and residual ethanol components were removed by centrifugation.

Next, the ethanol-treated selected pear powder was subjected to enzyme treatment. Enzyme treatment is performed by adding 0.1% by weight of cellulase to the Aspergillus niger-derived Rapidase, and then using sodium acetate buffer (0.01M, pH 5.0). ) was added in 450 ml and reacted for 15 hours at a speed of 80 rpm at 37 ° C. After centrifugation, the supernatant was completely removed and dried at 60 ° C. for 15 hours.

Example 1: Preparation of functional toothpaste for companion animals containing pear shell powder

A functional toothpaste containing the pear shell powder of Preparation Example 1 was prepared with the composition shown in Table 2 below, and the abrasive composition component included 5 wt% of the pear shell powder instead of 5 wt% of the cellulose gum of the commercial animal toothpaste.

Example 2: Preparation of functional toothpaste for companion animals containing selected pear powder

A functional toothpaste was prepared under the same conditions as in Example 1, except that the selected pear powder of Preparation Example 2 was included instead of the pear powder of Preparation Example 1.

Example 3: Preparation of functional toothpaste for companion animals containing enzymatically treated animal toothpaste abrasives

A functional toothpaste was prepared under the same conditions as in Example 1, except that the enzyme-treated animal toothpaste abrasive of Preparation Example 3 was included instead of the pear shell powder of Preparation Example 1.

Comparative Example 1: Commercial Cellulose Gum Animal Toothpaste

A commercial animal toothpaste was prepared, and one containing cellulose gum as an abrasive composition component was prepared.

Comparative Example 2: Commercial High Concentration Cellulose Gum Animal Toothpaste

A commercial animal toothpaste was prepared, and a product with high abrasive performance was prepared by containing 10 wt% of cellulose gum instead of 5 wt% as an abrasive composition component.

Comparative Example 3: Commercial Walnut Shell Animal Toothpaste

A commercial animal toothpaste was prepared, and one containing walnut shell powder instead of cellulose gum as an abrasive composition component was prepared.

Ingredients	Content (wt%)
Abrasive Composition Ingredients	5 to 10
Water	dose
Glycerin	9-11
PEG-40 Hydrogenated Castor Oil	1.23
Hydrolyzed Collagen	12.5
Fragrance	dose
Enzyme-modified steviol glycosides	8 to 12
Citric Acid	0.09 to 0.13
Potassium Sorbate	0.8~1.2
Zinc citrate	0.004~0.01
Sodium Benzoate	0.004~0.01
Menthol	dose
Butylene Glycol	1~2
Enzymatically Modified Rutin	4-7
entire	100

Examples 1 to 3, and Comparative Examples 1 to 3 are shown in Fig. 1 a photograph of the functional toothpaste for companion animals prepared respectively.

[Experimental Example]

Experimental Example 1: stone cell purity analysis

Dietary fiber was analyzed according to the method of Prosky et al. (1988). For the content of insoluble dietary fiber (IDF), 1 g of the sample was turbid in 50 ml of phosphate buffer (pH 6.0), heat-resistant α-amylase at 95 ° C, and protease at 60 ° C. and amyloglucosidase were sequentially treated with enzymes. After filtering the enzyme-treated sample in constant weight diatomaceous earth, the filtered residue was washed with 75% ethanol, 95% ethanol and acetone, and dried for 12 hours, and the value was measured excluding protein and ash content. In addition, for soluble dietary fiber (SDF), 95% ethanol at 60 ° C was added in a ratio of 1: 4 to the filtrate filtered through diatomaceous earth, reacted for 1 hour, and then filtered again to measure the dry weight of the remaining residue. .

The total dietary fiber (TDF) content was calculated as the sum of the insoluble and soluble dietary fiber content of the residue.

Stone cells can be defined as those containing lignocellulose and lignin, and a staining method that can be distinguished from insoluble dietary fibers composed of simple cellulose or hemicellulose is required. Kwon et al. (2016). According to the method, Wiesner staining solution was composed of 2% phloroglucinol, 20% ethanol, and 20% hydrochloric acid (HCl), and was left for about 2 hours after preparation.

2% Phloroglucinol-HCl staining solution was added to the pear powder of Preparation Example 1, the selected pear powder of Preparation Example 2, and the enzymatically treated abrasive powder sample of Preparation Example 3, and then stained at room temperature for 1 hour at 100 rpm and then stained 2.5 times under a stereomicroscope. The enlarged observation results are shown in FIG. 2 . According to this, stone cells (lignocellulose + lignin) are red, and other insoluble dietary fibers, cellulose and hemicellulose, are brown, so stone cells can be distinguished.

On the other hand, for the quantification of stone cells, the redness value (a-value) was measured using a colorimeter, and the stone cell content contained in the insoluble dietary fiber powder was quantified using a standard curve to which the concentration and redness value of stone cells were applied. .

For reference, the standard curve to which the dyed photo and the redness value according to the stone cell concentration are applied is shown in FIG. 3, and the color difference value for each component content is shown in Table 3 below. Here, the stone cell concentration can be measured according to the a value.

Concentration (mg/mL)	L	a	b		c
0	2.47±0.04	0.08±0.03	-1.09±0.08	1.09±0.09
One	4.66±0.02	2.95±0.06	-1.49±0.06	3.31±0.08
3	5.35±0.06	3.92±0.06	-1.65±0.05	4.25±0.07
5	8.03±0.05	7.97±0.09	-1.15±0.04	8.05±0.09
10	6.91±0.07	10.79±0.20	-0.93±0.09	10.83±0.21
20	7.02±0.16	16.23±0.01	-0.77±0.01	16.25±0.40
30	7.57±0.06	17.93±0.05	0.50±0.05	17.93±0.31
40	6.69±0.06	18.69±0.02	0.39±0.02	18.69±0.19
50	7.49±0.06	19.36±0.05	0.59±0.05	19.37±0.27
70	7.31±0.06	19.39±0.05	0.25±0.05	19.39±0.11
100	8.51±0.02	20.00±0.02	0.73±0.02	20.01±0.01

The results measured accordingly are shown in Table 4 below.

type	total dietary fiber (wt%)	Insoluble fiber content (%)	Stone cell content in insoluble dietary fiber (%)	Water absorption capacity (㎖/g)
				1 h	3h	24h
Preparation Example 1	64.38b	16.21c	25.20c	16.55a	17.93a	19.18a
Preparation Example 2	69.74b	46.41b	66.67b	2.91bc	2.80bc	3.26b
Preparation Example 3	78.08a	72.21a	92.26a	1.36e	1.430d	1.54d

According to this, the enzyme-treated animal toothpaste abrasive of Preparation Example 3 had a high stone cell purity of 92%, and the pear shell powder of Preparation Example 1 had a relatively low stone cell content and dietary fiber accounted for most of it at 75%. When used as a toothpaste, the water absorption capacity that causes formulation instability was calculated according to Equation 1 below.

[Equation 1]

Water absorption capacity (SC) (㎖ / g) = (V _wet -V _dry ) / W _dry

Here, V _wet represents the volume of the hydrated sample, V _dry represents the volume of the dry sample, and W _wet represents the mass of the dry sample.

According to this, the pear shell powder of Preparation Example 1 having a relatively high water-soluble dietary fiber ratio and a low stone cell content had a very high water absorption capacity of 19 ml / g, and the selected pear shell powder of Preparation Example 2 had 3.2 ml / g, Preparation Example The enzymatically treated abrasive for animal toothpaste showed very low water absorption even after 24 hours with 1.5 ml/g of germ cell B. As can be seen in the microscopic image, it seems to be due to the high purity of the stone cells that are red. If the water absorption capacity is low, it may have high formulation stability.

Experimental Example 2: Quality analysis of functional toothpaste for companion animals

As for the quality characteristics of the functional toothpastes of Examples 1 to 3 and Comparative Example 1, pH, color, sugar, and acidity were measured.

Chromaticity was measured by partially modifying the method of Hur and Kim (2018). L (Lightness), a (Redness), b (yellowness), and ΔE (Total color difference) were measured using a color difference meter (Handheld color spectrophotometer 45/0 NS 800, Shenzhen 3nh Technology Co., Ltd, Shenzhen, China). . The chromaticity values of the standard whiteboard were L=96.39, a=-0.43, and b=1.33, and were calculated according to Equation 2 below.

[Equation 2]

ΔE=[(LL ₀ )2-(aa ₀ )2-(bb ₀ )2]1/2

Sugar content, pH, and acidity were measured after dissolving 1 g of the sample in distilled water at 10% (v/v). Sugar content was measured with a refractometer (Digital hand-held PAL-1, ATAGO Co., Ltd, Tokyo, Japan) for the dissolved sample. The pH of the dissolved sample was measured using a pH meter (Benchtop pH Meter, Mettler Toledo, Columbus, Ohio, USA). Acidity was titrated with 0.1 N NaOH after adding two or three drops of 1% (v/v) phenolphthalein (Junsei chemical Co., Ltd, Tokyo, Japan) to the dissolved sample. When shaking, the indicator lasted for 20 to 30 seconds in a bright red color as the end point, and after measuring the NaOH consumption, the total acidity of the sample was converted into citric acid.

The results of analyzing the quality characteristics of the functional dentifrices of Examples 1 to 3 and Comparative Example 1 measured in this way are shown in Table 5 below.

division	pH	acidity (%)	Sugar content (°brix)	chromaticity
				L*	a*	b*	ΔE*
Comparative Example 1	4.97a	0.36c	15.0d	4.34d	0.03d	-1.96d	92.42a
Example 1	4.87b	0.49a	17.7a	19.38c	4.30a	9.60a	77.91b
Example 2	4.94ab	0.43b	15.5b	29.32b	10.32b	19.02b	70.49c
Example 3	5.00a	0.34c	15.2c	32.91a	12.92c	21.77c	68.30d

According to this, the functional toothpaste for companion animals of Comparative Example 1 showed a sugar content of about 15 ° brix, similar to Examples 2 and 3, and the functional toothpaste for pets of Example 1 had a sugar content of 17.7 ° brix, which was relatively low. It was high. The L value, which is the brightness in the chromaticity of the sample, was 4.34 for the toothpaste of Comparative Example 1, 29.32 for the toothpaste of Example 2, 32.91 for the toothpaste of Example 3, and 19.38 for the toothpaste of Example 1. The toothpaste of Example 3 was the highest. The redness a value was 0.03 for the commercial animal toothpaste of Comparative Example 1, 10.32 for the toothpaste of Example 2, 12.92 for the toothpaste of Example 3, and 4.30 for the toothpaste of Example 1 1. toothpaste was the highest. The yellowness b value was -1.96 for the commercial animal toothpaste of Comparative Example 1, 19.02 for the toothpaste of Example 2, 21.77 for the toothpaste of Example 3, and 9.60 for Example 1. The higher the stone cell content, the higher the yellowness, which is its own color. appear. The ΔE value, which means the color difference between total brightness and saturation, was 92.42 for the commercial animal toothpaste of Comparative Example 1, 70.49 for the toothpaste of Example 2, 68.30 for the toothpaste of Example 3, and 77.91 for Example 1.

Experimental Example 3: Formulation stability analysis of functional toothpaste for companion animals

For the formulation stability analysis of the functional dentifrices of Examples 1 to 3 and Comparative Example 1, adhesion, moisture content, specific gravity, and water absorption were measured.

Gumminess was measured using a texture meter (XforceP, Zwick Roell Co., Germany), and the measurement condition was to attach a probe with a diameter of 15 mm at a start position speed of 5 mm/s, once The compression ratio was set to 70% at the time of measurement and 20% at the time of measurement when measuring twice.

Moisture content (%) was measured according to the loss on drying test method. 1 g of sample was precisely weighed, dried at 105 ° C. for 4 hours, left in a desiccator to cool, and then calculated according to Equation 3 below.

[Equation 3]

Moisture content (%) = {1-weight after drying (g)/weight of sample (g)} × 100

Density was calculated according to Equation 4 below by putting the sample into a container of known capacity and measuring its weight.

[Equation 4]

Density (g/mL) = sample weight (g)/container (mL)

Swelling Capacity is measured by mixing 1 g of sample with 20 ml of water (1:20, w/v) and then leaving it at 4 ° C. It was measured according to Equation 1 above.

The formulation stability measurement results according to this are shown in Table 6 below.

toothpaste	stickiness (g. sec)	Moisture rate (%)	density (g/ml)	Water absorption capacity (㎖/g)
				1 h	3h	24h
Comparative Example 1	156.9d	30.93b	1.45a	1.03c	1.07d	1.20d
Example 1	397.2a	58.37a	1.32b	2.77a	4.12a	4.58a
Example 2	250.2b	28.88c	1.43a	1.57b	1.52b	1.83b
Example 3	173.3c	28.43c	1.44a	1.27c	1.28c	1.42c

According to this, the adhesiveness of the toothpaste of Example 1 containing a lot of dietary fiber was the highest at 397, and the toothpaste of Example 3, which had a high content of stone cells, was similar in adhesiveness to the commercial animal toothpaste of Comparative Example 1, resulting in marketability. appeared to be high. In addition, the toothpaste of Example 1 having a high dietary fiber content was 58.3%, and the remaining toothpastes were 28 to 30%. It showed about 28% lower content than the toothpaste of Example 1. Density showed little difference between samples, and the water absorption capacity that causes the layer separation of the toothpaste and the expansion of the formulation was the lowest for the toothpaste of Example 3, which was about 1.4 even after 24 hours, similar to the commercial animal toothpaste 1.2 of Comparative Example 1. value was indicated. That is, the toothpaste of Example 3 exhibiting low adhesiveness, moisture content, and water absorption capacity as a whole exhibited a high formulation stability similar to that of the commercial animal toothpaste of Comparative Example 1.

Experimental Example 4: Analysis of polishing effect of functional toothpaste for companion animals

In order to investigate the polishing effect of the functional toothpaste of Examples 1 to 3 and the commercial functional toothpaste of Comparative Example 2, which contains 10% cellulose gum and has high polishing performance, the teeth of a 12-month-old beagle were extracted and used through a 3D-OP machine. Teeth and parts with similar roughness were selected and the polishing effect analysis experiment was performed.

To measure the abrasiveness of the toothpastes, first, 10 g of the sample toothpaste was applied thinly with a spatula on the satin non-woven fabric of Semi-Automatic Grinders/Polishers (Met Prep 3™ PH-4, Allied High Tech Products, Rancho Domingues, CA, USA). After marking the tooth area to be tested by 3x3cm, brushing was performed 3,000 times with a reciprocating motion of about 50 rows per minute. 3D Optical Profiler, NV-E1000; Nano System Co., Daejeon, Korea), the degree of change in roughness after fixing with rubber clay was investigated In addition, the polishing effect was determined through the arithmetic mean roughness (Ra) within the reference area. Before and after toothpaste samples were compared and measured. A photograph of the surface shape is shown in FIG. 5 .

toothpaste	before polishing		after polishing		Roughness (㎛) Ra(AB)	polishing effect (%)
	Ra(A)	average	Ra(B)	average
Comparative Example 2 (cellulose 10%)	4.47, 4.41, 4.36	4.41	3.78, 3.79, 3.79	3.79	0.62	14.06
Example 1	6.20, 6.02, 5.66	5.96	4.91, 4.59, 4.77	4.76	1.20	20.13
Example 2	6.67, 6.63, 6.69	6.66	4.51, 4.50, 4.64	4.55	2.11	31.68
Example 3	5.24, 5.44, 5.52	5.40	3.01, 2.97, 3.30	3.09	2.31	42.78

According to this, the polishing effect was 14.0% for the commercial animal toothpaste of Comparative Example 2, 20.1% for the toothpaste of Example 1, and 31.6 or 42.7% for the toothpaste of Examples 2 and 3, respectively. That is, the toothpaste of the present invention containing high-purity stone cells showed a higher polishing effect than the commercial animal toothpaste of Comparative Example 2 with a high abrasive composition content or the toothpaste of Example 1 with a relatively low content of stone cells. .

Experimental Example 5: Analysis of calculus and plaque production inhibitory ability of functional toothpaste for companion animals

A total of 12 experimental beagles were acclimatized in the laboratory for one week, then anesthetized to perform scaling to remove calculus, and left untreated for 4 weeks. Thereafter, 6 animals used commercial animal toothpaste (containing 5% walnut shells) and 6 animals brushed twice a day for 4 weeks using the toothpaste of Example 3 (Verbac C.E.T. Periaid dental brush) to check the degree of gingival inflammation, plaque, calculus, and feces. It was investigated, and a photograph of performing the scaling and brushing is shown in FIG. 6.

The remaining calculus content was qualitatively evaluated through the staining method. the irradiated area Measurements were taken at 3 sites per tooth (distal buccal, mesibuccal, buccal) of the left and right maxillary third incisors, maxillary and mandibular canines, maxillary and mandibular 3rd and 4th premolars, and maxillary and mandibular first molars. At week 0, gingivitis, plaque, and calculus evaluation progress evaluation was performed, and gingivitis, plaque and calculus removal (scale & polish) were performed under anesthesia, and fecal evaluation was performed twice a week. Gingivitis, plaque, and calculus were evaluated at weeks 2 and 4 and fecal evaluation twice a week. Brushing is performed once/day for 4 weeks, and the clinical indices evaluated at this time are the Gingival Index (GI), Plaque Index (PI), and Calculus Index (CI), and the evaluation criteria are as follows. The data obtained in all experiments were verified for significance with the Multiple Mann-Whitney test, and these values were expressed as mean ± SD values, and significance was determined as significant when the p value was less than 0.05 did

* Evaluation of gingival inflammation (GI)

The gingival inflammation status was scored using the Silness and Loe Cingival Index in the following way.

0: normal teeth

1: mild inflammation; Minor color change, mildly inflamed gingiva that is slightly swollen but does not bleed with mild irritation

2: moderate inflammation; Inflamed gingiva that is red, swollen and bleeds with minor irritation

3: severe inflammation; Gingival inflammation that has progressed to the point where marked redness, swelling, and ulceration appear and spontaneous bleeding occurs.

Gingival Inflammation Index (GI) = sum of total scores / total number of gums examined

Verdict: 0.1-1.0 (mild), 1.1-2.0 (moderate), 2.1-3.0 (severe)

* Plaque evaluation (CI)

Supragingival plaque coverage and plaque thickness were evaluated using the Turesky-Quigley-Hein Plaque index. Each tooth surface was stained with a red colorant (Erythrosin, sultan, USA) and scored in the following way. Scores are according to Table 7 below.

Plaque index (PI) = sum of (coverage * thickness) / total number of tooth surfaces examined

* Tartar Assessment (PI)

Supragingival calculus coverage and calculus thickness were scored using the Warrick and Gorrel method as follows. Scores are according to Table 8.

*Gingival Inflammation Index (GI) = sum of total scores / total number of gums examined

Verdict: 0.1-1.0 (mild), 1.1-2.0 (moderate), 2.1-3.0 (severe)

* Fecal evaluation

Fecal evaluation was performed twice a week according to the Waltham Faeces Scoring system. The Waltham Faeces Scoring system evaluation criteria, which are stool evaluation criteria, are shown in FIG. 7 .

The results of measuring the gingival index (GI), plaque index (PI), and calculus index (CI) of the untreated control group without brushing are shown in FIG. 8 .

According to this, the gingival index (GI) was measured as 0.37 at the 0th week, 1.08 at the 2nd week, and 1.23 at the 4th week. Plaque index (PI) was measured as 0 at week 0, 2.96 at week 2, and 5.53 at week 4. In addition, the calculus index (CI) was measured as 0 at week 0, 1.94 at week 2, and 3.00 at week 4. In other words, compared to the 0th week, the gingival inflammation index, plaque index, and calculus index significantly increased in the 2nd and 4th weeks in the untreated control group.

On the other hand, the gingival index (GI), plaque index (PI), calculus index (CI) were measured in the teeth of experimental beagles treated with the commercial animal toothpaste of Comparative Example 3 (containing 5% walnut shell) and the toothpaste of Example 3. The results are shown in FIG. 9 .

According to this, the gingival index (GI) at 2 weeks was measured as 1.08 in the control group, 0.65 in the group brushed using the toothpaste of Example 3, and 0.83 in the group using the commercial animal toothpaste containing walnut shells. In addition, the 4th week untreated control group was measured at 1.23, the group brushing using the toothpaste of Example 3 was 0.61, and the group using the commercial animal toothpaste containing walnut shells of Comparative Example 3 was measured at 1.02. Compared to the untreated control group, the commercial animal toothpaste containing walnut shells of Comparative Example 3 decreased the gingivitis level only at the 2nd week, and the gingivitis level of the toothpaste of Example 3 significantly decreased significantly at the 2nd and 4th weeks.

In addition, plaque index (PI) was measured at 2.96 in the untreated control group at 2 weeks, 3.70 in the group brushed using the toothpaste of Example 3, and 3.36 in the group using the commercial animal toothpaste containing walnut shells of Comparative Example 3. has been measured In addition, the 4th week untreated control group was measured at 5.53, the group using the toothpaste of Example 3 was measured at 4.12, and the group using the commercial animal toothpaste containing walnut shells of Comparative Example 3 was measured at 4.67. That is, the group using the toothpaste of Example 3 tended to have a slightly lower plaque index (PI) at 4 weeks compared to the group using the commercial animal toothpaste containing walnut shells of Comparative Example 3.

Calculus index (CI) was measured at 1.94 in the untreated control group at 2 weeks, 0.80 in the group brushed using the toothpaste of Example 3, and 1.00 in the group using commercial animal toothpaste containing walnut shells in Comparative Example 3. . In addition, the untreated control group at 4 weeks was measured at 3.00, the calculus index of the group brushed using the toothpaste of Example 3 was 1.77, and the group using the commercial animal toothpaste containing walnut shells of Comparative Example 3 was measured at 2.53. That is, compared to the untreated control group, the group using the toothpaste of Example 3 showed a significant decrease in calculus index (CI) in both the 2nd and 4th weeks. As a result, at 4 weeks, when using the commercial animal toothpaste containing walnut shells of Comparative Example 3 and the toothpaste of Example 3, compared to untreated, the gingivitis level was reduced by 23% or 39.9%, the plaque index was reduced by 15.6%, 25.5%, and calculus. The index was significantly increased by 15.7% and 41.0%, respectively, and compared to the walnut shell-containing toothpaste of Comparative Example 3, the toothpaste of Example 3 of the present invention was found to be particularly effective in inhibiting gingivitis and calculus.

On the other hand, a photograph showing the dental condition of the beagle after 4 weeks of brushing using the untreated, commercial animal toothpaste containing walnut shells of Comparative Example 3 and the functional toothpaste of Example 3 is shown in FIG. 10 . When compared with the naked eye, when the functional toothpaste of Example 3 of the present invention was applied, the condition of the teeth seemed as clean as possible.

In addition, the results of evaluating feces according to the Waltham Faeces Scoring system are shown in FIG. 11 . There was no significant difference between the groups brushed with the control group, the toothpaste of Example 3 and the toothpaste of Comparative Example 3.

Although the embodiments of the present invention have been described above, those skilled in the art can add, change, delete, or add components within the scope not departing from the spirit of the present invention described in the claims. The present invention can be variously modified and changed by the like, and this will also be said to be included within the scope of the present invention.

The toothpaste abrasive composition for companion animals comprising the enzyme-treated pear shell containing stone cells of the present invention and the toothpaste composition for companion animals containing the same are suitable for polishing animal teeth, preventing and removing plaque and calculus, suppressing gingivitis and The same effect is significantly superior to conventional commercial animal toothpaste or toothpaste that simply introduces pear pear components, and by using natural ingredients, there is an effect that is harmless to the body even if companion animals such as dogs and cats ingest toothpaste components when brushing teeth.

The manufacturing method of a toothpaste abrasive composition for companion animals containing an enzymatically treated product of pears containing stone cells and the manufacturing method of a toothpaste composition for companion animals including the same of the present invention are complex processes or harmful Simple introduction of conventional commercial animal toothpaste or pear-shell components to prevent polishing of animal teeth, gingivitis, plaque, and calculus, without using chemical products, by sorting the pear material by particle size, and by performing alcohol treatment and enzyme treatment. Significantly better than toothpaste.

Claims (17)

1. (a) heat-treating the pear pulverized solution, filtering to remove the pear juice, and drying the by-product to obtain pear pear powder;

   (B) pulverizing the pear powder and then passing through a 30 mesh mesh and screening to a size that does not pass through a 60 mesh mesh to obtain a sorted pear shell powder;

   (c) reacting the selected pear powder with alcohol to obtain a precipitate; and

   (d) enzymatically treating the precipitate with Aspergillus niger-derived rapidase, removing the supernatant from the enzymatically treated product and drying the precipitate with hot air; A method for preparing a toothpaste abrasive composition.
2. According to claim 1,

   In step (a), the heat treatment is a method for producing a toothpaste abrasive composition for companion animals, characterized in that carried out at 100 to 140 ℃.
3. According to claim 1,

   In step (c), the alcohol is a method for producing a toothpaste abrasive composition for companion animals, characterized in that the lower alcohol having 1 to 4 carbon atoms.
4. According to claim 3,

   The method for producing a toothpaste abrasive composition for companion animals, characterized in that the alcohol is an aqueous solution of ethanol at a concentration of 40 to 50%.
5. According to claim 1,

   In step (d), the Aspergillus niger-derived rapidase is added in an amount of 0.01 to 0.15 wt% of solids. Method for producing a toothpaste abrasive composition for pets.
6. According to claim 1,

   In step (d), the Aspergillus niger derived rapidase is cellulase, hemicellulase, beta-glucanase and pectinase ( Method for producing a toothpaste abrasive composition for companion animals, characterized in that it is a complex enzyme containing pectinase).
7. According to claim 1,

   In step (d), the enzyme treatment is a method for producing a toothpaste abrasive composition for companion animals, characterized in that carried out at 35 to 40 ℃ for 8 to 20 hours.
8. According to claim 1,

   In step (d), the method for producing a toothpaste abrasive composition for companion animals, characterized in that the hot air drying is performed at 50 to 70 ° C. for 10 to 20 hours.
9. A toothpaste abrasive composition for companion animals prepared according to any one of claims 1 to 8.
10. According to claim 9,

    The toothpaste abrasive composition for companion animals is a toothpaste abrasive composition for companion animals, characterized in that the total dietary fiber content is 75 to 85% (w / v).
11. According to claim 9,

    The toothpaste abrasive composition for companion animals is a toothpaste abrasive composition for companion animals, characterized in that the insoluble dietary fiber content is 65 to 80% (w / v).
12. According to claim 11,

    A toothpaste abrasive composition for companion animals, characterized in that the stone cell content is 85 to 95% based on the total weight of the insoluble dietary fiber.
13. According to claim 11,

    The toothpaste abrasive composition for companion animals, characterized in that the water absorption capacity is 1.2 to 2㎖ / g based on the passage of 1 to 24 hours.
14. A toothpaste composition for companion animals comprising the toothpaste abrasive composition for companion animals prepared according to any one of claims 1 to 8.
15. According to claim 14,

    The companion animal toothpaste composition is a toothpaste composition for companion animals, characterized in that the moisture content is 25 to 35%.
16. According to claim 14,

    The companion animal toothpaste composition is a companion animal toothpaste composition, characterized in that it comprises 3 to 15wt% of the companion animal toothpaste abrasive composition with respect to the total weight.
17. According to claim 14,

    The companion animal toothpaste composition is a companion animal toothpaste composition, characterized in that for gingivitis, plaque or calculus removal or inhibition.

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