KR101311011B1 - Aqueous mastic dispersion and process for producing the same - Google Patents

Abstract

The present invention relates to a mastic aqueous dispersion formed by dispersing mastic in water and a method for producing the mastic. More specifically, mastic having an average particle diameter of 0.1 to 50 nm by dynamic light scattering is dispersed, and an organic solvent is dispersed. It relates to a mastic aqueous dispersion containing less than 0.03% by weight. The mastic aqueous dispersion of the present invention is a mastic evenly dispersed in water, it can be easily used in a product for preventing or treating diseases such as oral cavity, stomach, even in a small amount.

Description

Mastic aqueous dispersion and its manufacturing method {Aqueous mastic dispersion and process for producing the same}

The present invention relates to a mastic aqueous dispersion formed by dispersing mastic in water and a method of manufacturing the same.

Mastic is a sap extract of the pistacia lentiscus tree native to the southern part of the Greek island of Chios in the Aegean Sea. It is a health food that has been used to promote health, especially the health of the digestive system.

Mastic has made Mastic Gum in Korea since it was first announced in 1998 that mastic possesses strong antibacterial activity against pylori, which causes stomach and duodenal ulcers (Ref. 1). When applied to patients with pylori gastritis, it has been reported that the density of pylori decreases and improves gastritis (Ref. 2), and is currently known to be effective for gastric and duodenal ulcers and gastritis.

In addition, it is known that mastic has an effect of reducing bacterial growth and oral plaque formation in oral saliva (Ref. 3), and toothpaste forms containing mastic itself are sold in Korea. Therefore, due to the effects of the mastic as mentioned above, a lot of research on the utilization of the mastic has been in progress.

On the other hand, since the mastic having excellent efficacy on gastrointestinal and oral diseases is insoluble (less than 0.01% of solubility), the mastic is dissolved in a solid state or oil and used as a result. There is a disadvantage that cannot be applied to the hydrate. In order to solve this problem, mastic must be dissolved in water or dispersed in water. However, due to the inherent property of mastic that is insoluble in water, it has been somewhat difficult to be usefully used.

Reference 1: Huwez FU, Thirlwell D, Cockayne A, Ala'Aldeen DA .; Mastic gum kills Helicobacter pylori .; N Engl J Med. 24: 339 (26): 1946, 1998.

Reference 2: Noh Im-hwan, Nam Seung-woo, Myeong Na Hye, Kim Jung Taek, Shin Ji Hyun; Effect of Mastic Gum on Helicobacter pylori gastritis; Journal of the Korean Society of Gastroenterology 41: 277-283, 2003.

Reference 3: Takahashi K, Fukazawa M, Motohira H, Ochiai K, Nishikawa H, Miyata T; A pilot study on antiplaque effects of mastic chewing gum in the oral cavity; J Periodontol. 74 (4): 501-505, 2003.

Accordingly, the present inventors have tried to solve the above problems, and after sequentially adding organic solvents such as acetone and water to the mastic having insolubility in water, the mastic is uniformly dispersed in water by selectively removing the organic solvent. It was confirmed that the made mastic aqueous dispersion could be obtained.

Accordingly, an object of the present invention is to provide a mastic aqueous dispersion in which mastic is uniformly dispersed in water.

Another object of the present invention to provide a method for producing the mastic aqueous dispersion.

It is another object of the present invention to provide a food supplement, animal feed, food, pharmaceutical or cosmetic formulation comprising a mastic aqueous dispersion.

According to an aspect of the present invention for achieving the above object, the present invention is a mastic aqueous dispersion formed by dispersing mastic having an average particle diameter (D ₅₀ ) of 0.1 to 50nm by water in the dynamic light scattering method, The stick aqueous dispersion provides a mastic aqueous dispersion containing less than 0.03% by weight of an organic solvent.

According to a preferred embodiment of the present invention, the content of the mastic is 0.1 to 5% by weight based on the total mastic aqueous dispersion.

According to another preferred embodiment of the present invention, the dispersion degree [(D ₅₀ ) / (D _TEM )] of the mastic aqueous dispersion is 5.0 or less.

According to another preferred embodiment of the present invention, the organic solvent is diethyl ether, methyl propyl ether, diisopropyl ether, methyl t-butyl ether, divinyl ether acetone, methyl ethyl ketone, hexane, pentane or these It is a mixture of these, More preferably, it is acetone, methyl ethyl ketone, or a mixture thereof.

According to another aspect of the present invention, the present invention comprises the steps of (a) adding a mastic to an organic solvent having a boiling point of 30 to 90 ℃ at normal pressure and room temperature to obtain a mastic organic solution; (b) adding water to the mastic organic solution to obtain a mastic mixed solution; And (c) distilling the organic solvent contained in the mastic mixed solution by heating the mastic mixed solution at 50 to 95 ° C., wherein the organic solvent is contained in less than 0.03%, and the mastic is dispersed in water. It provides a method for producing a mastic aqueous dispersion comprising the step of obtaining a mastic aqueous dispersion.

According to another preferred embodiment of the present invention, the method further comprises the step of (d) recycling the organic solvent distilled in step (c) and then recycling to step (a).

According to another aspect of the invention, there is provided a food supplement, animal feed, food, pharmaceutical or cosmetic preparation comprising a mastic aqueous dispersion.

The mastic aqueous dispersion of the present invention is uniformly dispersed in water, so that the mastic can be easily used in a product for preventing or treating diseases such as gastrointestinal oral cavity as compared to the case where the mastic is dissolved in a solid state or oil. have. In addition, the nano-size mastic is effective even when using a small amount of the large surface area of the particle, the manufacturing cost can be significantly reduced.

1 is a process chart for preparing a mastic aqueous dispersion from mastic according to the present invention.
Figure 2 is a photograph showing the degree of precipitation of the mastic aqueous dispersion prepared by using acetone and the mastic aqueous dispersion prepared by dissolving the integrated mastic in water.

Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings.

The mastic aqueous dispersion of the present invention can be obtained by adding mastic to an organic solvent, adding water thereto, and then selectively distilling and removing only the organic solution.

Mastic used in addition to the organic solvent in the present invention is a substance having a function of inhibiting the development of Helicobacter bacteria and periodontal pathogens, and has an insoluble or poorly soluble property in water. The mastic of the present invention includes a mastic oil, a masticadieneic acid, an isosticadienoic acid, a triterthenic acid, polybetamycin, preferably 0.5 to 5% by weight of a mastic oil, a mastica 5 to 20% by weight of dienoic acid, 5 to 25% by weight of isomisticadienoic acid, 35 to 55% by weight of triterpenic acid, and 15 to 30% by weight of polybetamycin.

The mastic of the present invention added to the organic solvent is in the form of a natural sap, in the form of a solid mass dried natural sap, or in the form of a solid powder pulverized a solid mass, and due to the ease of storage and handling, and ease of quantitative measurement Preference is given to using mastic in the form of a solid powder.

Referring to step (a) of FIG. 1, in order to uniformly disperse a mastic in water in the present invention, the mastic is dissolved in an organic solvent before adding water to the mastic. The organic solvent is a material having a boiling point of 30 to 90 ° C., preferably 50 to 80 ° C. at normal pressure and room temperature, and may be distilled before water when heated to 50 to 95 ° C. The organic solvent used in the present invention is diethyl ether, methyl propyl ether, diisopropyl ether, methyl t-butyl ether, divinyl ether acetone, methyl ethyl ketone, hexane, pentane or a mixture thereof, more preferably Acetone, methyl ethyl ketone or mixtures thereof, most preferably acetone.

In step (b), the mastic is added to the organic solvent and stirred to prepare a mastic organic solution, and then the process water (water) is added to the mastic organic solution to obtain a mastic mixed solution. At this time, the organic solvent is stirred using a stirrer to be uniformly mixed with the process water (water), preferably for about 10 minutes to 1 hour.

In step (c), the mastic mixed solution mixed with mastic, organic solvent and water is heated at 50 to 95 ° C. to distill off the organic solvent added to the mastic mixed solution. As shown in step (d), the distilled gaseous organic solvent is preferably cooled and reduced to a liquid state, and then mixed with the organic solvent used to dissolve the mastic and reused.

The mastic aqueous dispersion obtained by removing the organic solvent is formed by uniformly dispersing mastic having an average particle diameter (D ₅₀ ) of 0.1 to 50 nm, preferably 0.1 to 25 nm, by dynamic light scattering. When the average particle diameter of the mastic exceeds 50 nm, aggregation occurs between the mastic particles over time, and precipitation occurs. When the average particle diameter of the mastic is less than 0.1 nm, the organic solvent evaporates together. And the amount of mastic removed is large.

Even if the mastic aqueous dispersion of the present invention is removed by evaporating the organic solvent, some of the organic solvent may remain in the aqueous dispersion due to the action of water and attraction. In the case of the present invention, the organic solvent contained in the mastic aqueous dispersion is 0.03% by weight or less, preferably 0.01% by weight or less. When the organic solvent exceeds 0.03% by weight, it does not meet the usage criteria taught by the Korea Food and Drug Administration (use standards of acetone and preparations containing food additives), and thus improves the oral and gastrointestinal diseases of the mastic aqueous dispersion of the present invention. It cannot be mixed with a product.

Meanwhile, the mastic aqueous dispersion of the present invention contains 0.1 to 5% by weight, preferably 0.5 to 3% by weight, based on the total mastic aqueous dispersion. When the amount of mastic is less than 0.1% by weight, the effect of improving oral and gastrointestinal diseases is poor. When the amount of mastic is more than 5% by weight, there is no difference between the content and the cost of the mastic, considering that the mastic is expensive. There is a problem that raises the difficulty in using realistically.

The mastic particles of the present invention can take a stable dispersion state in water (dispersion medium). The dispersion state of mastic particle | grains in water can be evaluated by the dynamic scattering method, The principle is as follows. In general, particles whose particle diameters are in the range of about 1 nm to 5 μm change their position and direction at different times by brown motion such as translation and rotation in a liquid. However, when such particles detect scattered light emitted by laser light, The fluctuations of the scattered light intensity depend on the Brownian motion. By observing the fluctuations of the scattered light intensity over time, the velocity (diffusion coefficient) of the Brownian motion of the particles is obtained, and the size of the particles can be known. Using this principle, when the average particle diameter in a dispersion medium is measured, and when the measured value is close to the average particle diameter (D _TEM ) obtained by TEM observation, the particle | grains in liquid are monodisperse individually (particles To not bond or agglomerate). That is, in the dispersion medium, the particles are dispersed at intervals from each other, and each particle is in a state capable of moving independently. Therefore, the average particle diameter (D ₅₀₎ and TEM (transmission electron microscope), the ratio (polydispersity _{= (D 50) / (D} TEM)) of the mean particle diameter (D _TEM), as measured by observation of 5.0 or less by the dynamic light scattering method If it is preferably 3.0 or less, it may be considered that good dispersion is maintained, and the mastic aqueous dispersion according to the present invention satisfies the above dispersion degree conditions.

The mastic aqueous dispersion of the present invention can be used by easily adding it to a food supplement, an animal feed, a food, a pharmaceutical or a cosmetic preparation. For example, the mastic aqueous dispersion of the present invention may be mixed or applied to tofu, rice, or the like to be sold as mastic tofu, mastic rice, or the like. In addition, the drink may be prepared by improving the oral and gastrointestinal diseases by mixing the mastic aqueous dispersion with alcohol, beverages and the like. In particular, ingesting liquor with a mastic aqueous dispersion may have a less drunk effect than a mastic aqueous dispersion.

The mastic aqueous dispersion of the present invention is uniformly dispersed in water, so that the mastic can be easily used in a product for preventing or treating diseases such as gastrointestinal oral cavity as compared to the case where the mastic is dissolved in a solid state or oil. have.

Example

Hereinafter, the present invention will be described in more detail with reference to the following Examples, but the scope of the present invention is not limited to the following Examples.

Example  1: using acetone Mastic Aqueous dispersion  Produce

10 g of powdered solid mastic was added to a dissolution bath containing 50 mL of acetone, and then uniformly dissolved at room temperature for 60 minutes to prepare a mastic acetone solution. Thereafter, the mastic acetone solution was stirred for 10 minutes while injecting 500 g of water into the mixing bath to obtain a mastic mixed solution.

The mastic mixture solution was placed in an evaporation tank and gradually heated up under atmospheric pressure to be heated to 97 ° C. for 1 hour to remove the organic solvent contained in the mastic mixture solution. An aqueous dispersion dispersed in was obtained. The content of acetone in the mastic aqueous dispersion was analyzed using an organic compound analyzer (Wasson-ECE), which was 0.0031 wt% based on the aqueous dispersion.

Example  2-3: methyl ethyl ketone and Diethyl ether  Used Mastic Aqueous dispersion  Produce

An aqueous dispersion containing mastic was prepared in the same manner as in Example 1, except that methyl ethyl ketone (Example 2) and diethyl ether (Example 3) were used instead of acetone as the organic solvent. The organic compound analyzer (Wasson-ECE) was used to measure the content of diethyl ether in the aqueous dispersion, which was 0.007 and 0.009% by weight, respectively.

Comparative example  1: without organic solvent Mastic Aqueous dispersion  Produce

10 g of the solid mastic in the form of powder was frozen at -10 ° C., and then converted into frozen powder and then in a powder state. The mixture was added to 500 g of water at room temperature, followed by stirring to prepare an aqueous solution containing mastic.

Experimental Example  One

The average particle diameter of the mastic particles contained in the mastic aqueous dispersions of Examples 1-3 and Comparative Example 1 was measured. Using a Zetasizer 3000 HSa instrument (Malvern Instruments, UK), the average particle diameter (D ₅₀ ) of mastic particles present in the dispersion was measured by dynamic light scattering, and TEM was measured. The average particle diameter (D _TEM ) of the mastic particles was measured. In addition, the dispersion degree was measured using the ratio of D ₅₀ and D _TEM . The results are shown in Table 1 below.

[Table 1]

As can be seen from Table 1, in Example 1-3, the average particle diameters of the dynamic light scattering method were 1 nm, 3.5 nm, and 46 nm, respectively, and the dispersion degree was 3.0 or less. It can be seen that this is uniformly dispersed. This means that by using the present invention, an aqueous dispersion in which mastic insoluble in water is uniformly dispersed can be obtained.

Experimental Example  2

In order to measure the dispersion stability of the mastic aqueous dispersion of Example 1 and Comparative Example 1, the mastic aqueous dispersion was stored at room temperature, and the precipitation state of the solid was visually measured with time. The results are shown in Table 2, and the photographs comparing Example 1 and Comparative Example 1 are shown in FIG.

[Table 2]

As can be seen from Table 2 and FIG. 2, when the mastic is directly dissolved in water, the mastic is not easily dissolved, and it can be seen that a large amount of precipitate is settled over time. In contrast, when a mastic aqueous dispersion was prepared using acetone, methyl ethyl ketone, or diethyl ether as an organic solvent, solids did not precipitate over time.

On the other hand, the smaller the size of the mastic particles contained in the mastic aqueous dispersion and the higher the degree of dispersion, it can be determined that the more effective in oral and gastrointestinal diseases. This is because the smaller the size of the mastic particles can exhibit an excellent effect as the surface area is wider. As a result, the mastic aqueous dispersion of the present invention in which the mastic having an average particle diameter of 0.1 to 50 nm of the present invention is uniformly dispersed is more easily used as a product for preventing or treating diseases such as gastrointestinal oral cavity than conventionally used products. Can be.

The specific parts of the present invention have been described in detail above, and for those skilled in the art, these specific descriptions are merely preferred embodiments, and the scope of the present invention is not limited thereto. Thus, the substantial scope of the present invention will be defined by the appended claims and equivalents thereof.

Claims (8)

As a method of producing a mastic aqueous dispersion,
(a) adding mastic to an organic solvent at normal pressure and room temperature to obtain a mastic organic solution;
(b) adding water to the mastic organic solution to obtain a mastic mixed solution; And
(c) heating the mastic mixture solution to 50-95 ° C. to distill the organic solvent contained in the mastic mixture solution, wherein the mastic is dispersed in water, containing less than 0.03% of the organic solvent. Obtaining a stick aqueous dispersion,
The manufacturing method of the mastic aqueous dispersion is characterized in that no emulsifier or oil is used.
The method of claim 1, wherein the method further comprises the step of (d) cooling the organic solvent distilled in the step (c) and recycling to the step (a).
The method of claim 1, wherein the organic solvent is diethyl ether, methyl propyl ether, diisopropyl ether, methyl t-butyl ether, divinyl ether acetone, methyl ethyl ketone, hexane, pentane or a mixture thereof Method of producing a mastic aqueous dispersion.
The method of claim 1, wherein the organic solvent is acetone, methyl ethyl ketone, diethyl ether or a mixture thereof.
The mastic aqueous dispersion prepared according to claim 1 or 2, wherein the mastic is dispersed in water, and the average particle diameter by dynamic light scattering method of mastic dispersed in the mastic aqueous dispersion ( D ₅₀ ) is 0.1 to 50 nm, and the mastic aqueous dispersion contains less than 0.03% by weight of an organic solvent and contains no oil or emulsifier.
The mastic aqueous dispersion according to claim 5, wherein the mastic content is 0.1 to 5% by weight based on the total mastic aqueous dispersion.
The mastic aqueous dispersion according to claim 5, wherein the dispersion degree of the mastic aqueous dispersion [(D ₅₀ ) / (D _TEM )] is 5.0 or less.
A food supplement, animal feed or food preparation comprising the mastic aqueous dispersion of claim 5.

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