JP2001348307A - Method for producing extract from eucalyptus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing an extract from a plant of the genus Eucalyptus not reducing activity of the active ingredient component when removing a color or a smell, and usable as an antimicrobial agent, quasi medicine, cosmetic, etc. SOLUTION: A color and/or a smell is removed from a solution of an extract prepared by extracting a plant of the genus Eucalyptus with a polar solvent by using at least one kind selected from an adsorbent and an inclusion agent. Activated carbon, celite, silica gel, diatomaceous earth, zeolite, etc., are preferable as the adsorbent. A cyclodextrin is preferable as the inclusion agent.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a method for producing an Eucalyptus plant extract which can be used as an antibacterial agent, a quasi-drug, a cosmetic or the like.

[0002]

2. Description of the Related Art It has been reported that essential oils and organic solvent extracts of eucalyptus plants contain various physiologically active substances such as anti-inflammatory, antioxidant, and antibacterial substances. Biological Resource Eucalyptus ”published in 1987). When an extract of a eucalyptus plant is used for cosmetics, pharmaceuticals, quasi-drugs, antibacterial agents, foods, and the like, the odor and color of the extract may be problematic depending on the use.

[0003] By the way, various adsorbents are generally studied for the removal of offensive odors. In particular, activated carbon has a high adsorption characteristic to the offensive odor (especially neutral gas) in the gas phase, and toilets, refrigerators, etc. Widely used for deodorizing. As an example in which activated carbon is used for producing an extract, a method for producing an antioxidant spice extract (Japanese Patent Application Laid-Open No. 5-139332) has been reported.

On the other hand, it has been reported that clathrates have an effect of masking and reducing odor. For example, it has been reported that cyclodextrin is effective in suppressing the smell of pets (Japanese Patent Application Laid-Open No. 9-299664).
Also, it has been reported that the release of the scent of a fragrance (essential oil) is regulated by cyclodextrin (Japanese Patent Laid-Open No. 6-2).
05823).

[0005]

With respect to the eucalyptus extract, no method has been reported for removing odor or color with an adsorbent or clathrate. Also, changes in the activity of the eucalyptus extract due to them are not known. The present invention
An object of the present invention is to propose a method for producing a eucalyptus extract which does not reduce the activity of a target component even if the color and odor are removed.

[0006]

In order to solve the above problems, the present invention employs the following constitution. That is, a first aspect of the present invention is to remove a color and / or odor of an extract solution obtained by extracting a eucalyptus plant with a polar solvent using at least one material selected from an adsorbent and an clathrate. A method for producing a eucalyptus extract. "

A second aspect of the present invention is the method according to the first aspect, wherein the extract solution contains activated carbon, celite, silica gel,
Production of a eucalyptus extract, characterized by adding at least one adsorbent selected from diatomaceous earth and zeolite, adsorbing color and odor to the adsorbent, and then separating the extract solution and the adsorbent Is the way. Third of the present invention
Is characterized in that, in the second invention, the adsorbent is added in an amount of 0.01 part by weight or more based on 1 part by weight of the extract component.

A fourth aspect of the present invention is the method for producing a eucalyptus extract according to the first aspect, wherein the odor is removed by adding a clathrate to the extract solution. According to a fifth aspect, in the fourth aspect, the clathrate is added in an amount of 0.01 to 100 parts by weight based on 1 part by weight of the extract component.

A sixth invention is characterized in that, in the fourth or fifth invention, the clathrate is cyclodextrin.

A seventh invention is characterized in that in the first to sixth inventions, the eucalyptus extract is used by being added to a beverage.

[0011]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The configuration of the present invention will be described below in detail. The raw material of the Eucalyptus plant used in the present invention is not particularly limited as long as it is a Eucalyptus plant of the family Myrtaceae, and may be used alone or in combination of two or more.
Eucalyptus plants are evergreen broad-leaved trees distributed in temperate regions around the world. In recent years, they have been actively planted in Australia, New Zealand, Vietnam, and the like for use as pulp materials. In addition to being used as pulp and medicinal materials, it has a wide range of uses such as park trees, garden trees, construction materials, equipment materials, civil engineering materials, and marine materials. The site of the plant to be extracted is not particularly limited, but is preferably a branch or leaf that is easy to collect, and particularly preferably a leaf.

As the eucalyptus extract solution in the present invention, an extract obtained by extracting eucalyptus leaves, branches, etc. with a polar solvent may be used as it is. Alternatively, the extract may be a solution obtained by concentrating, diluting, or replacing the solvent.
Examples of the polar solvent used for the extraction include alcohols, glycols, ketones, esters, ethers, and halogenated carbons. Examples of lower alcohols include ethanol, methanol and propanol. Examples of the glycols include ethylene glycol, diethylene glycol, butylene glycol, propylene glycol and the like. Examples of ketones include acetone and methyl ethyl ketone, and examples of esters include ethyl acetate, propyl acetate, and ethyl formate. These solvents may be used singly or as an aqueous solution, or may be used as a mixture of two or more optional solvents. Among the above solvents, ethanol, acetone and ethyl acetate are preferred from the viewpoint of antibacterial properties. From the viewpoint of hair growth promoting activity, acetone, ethanol, butylene glycol and propylene glycol are preferred.

The extract is obtained, for example, as follows. The dry matter of Eucalyptus leaves is crudely extracted with acetone, lower alcohol or glycols. Prior to the crude extraction, the dried leaves are pre-treated, for example, by pulverizing the dried leaves into a suitable size or pulverizing the dried leaves to facilitate solvent extraction.

The extraction method may be a commonly used method, for example, a method in which eucalyptus leaves are immersed in an organic solvent for a long time, an extraction is carried out while heating and stirring at a temperature lower than the boiling point of the organic solvent, and filtration is performed. To obtain an extract.

In order to obtain a eucalyptus extract having higher antibacterial activity and hair growth promoting activity during the above-mentioned extraction operation, the eucalyptus leaves are dried more than directly extracted with acetone, lower alcohol or glycols. It is preferable to degrease with a non-polar organic solvent, remove essential oils, and then extract with lower alcohols or glycols. This operation can also be performed by removing essential oils by steam distillation, and then extracting by adding a lower alcohol or glycol to the residue. Examples of the non-polar solvent include alkanes such as hexane, pentane and heptane.

Hereinafter, a method for removing the color and odor of the extract solution will be described. As a treatment method using an adsorbent, for example, a method of mixing the extract solution and the adsorbent in a container, stirring or standing, and then allowing the mixture to stand for a certain period of time, followed by filtration, or a column filled with the adsorbent, A method of passing the extract is exemplified. The ratio of the adsorbent mixed with the extract solution is preferably at least 0.01 part by weight, more preferably 0.25 to 10 parts by weight, per 1 part by weight of the extract. Above this range, physiologically active substances other than the color and odor components, such as antibacterial active components and hair growth active components, are also undesirably adsorbed on the activated carbon. The concentration of the extract component in the extract solution when the adsorbent is added is preferably 0.1 to 50% by weight, and more preferably 0.5 to 5% by weight.

As the adsorbent, activated carbon, celite, silica gel, diatomaceous earth, clay, activated clay, zeolite, alumina, kaolin, styrene, divinylbenzene, silicic acid, zinc oxide, montmorillonite, bentonite, titania, zirconia, styrene divinyl Synthetic resins such as benzene-based copolymer resins, acrylic ester resins, and polystyrene-based resins, and ion-exchange resins are exemplified. In order to efficiently remove the color and odor of the extract, it is preferable to use activated carbon, celite, silica gel, and diatomaceous earth, and it is more preferable to use activated carbon.

As the raw material of the activated carbon to be used, for example, plant raw materials such as wood flour, charcoal and coconut shell, peat, lignite, anthracite,
Fossil raw materials such as petroleum pitch, coke, and coal tar; synthetic resin raw materials such as phenolic resin, vinyl acetate resin and polyester resin; and synthetic rubber raw materials such as polybutyl, polybutadiene, and polychloroprene. These activated carbon raw materials are, for example, carbonized and activated in a fixed bed, a moving bed, a fluidized bed, and the like.For activation, for example, gas activation using steam, hydrogen chloride, carbon monoxide, carbon dioxide, oxygen, or the like, Chemical activation using an alkali, an acid, or a salt may be mentioned. In the present invention, any activated by any of them can be used. The activated carbon used in the present invention may have any shape such as powdered carbon, granular coal, crushed carbon, and the like. The type of activated carbon to be used may be one type, or two or more types of activated carbons of different types may be mixed and used.

Next, the case of adding a clathrate to the extract solution will be described. The amount of addition is 0.001 part by weight or more, preferably 0.05 to 10 parts by weight per 1 part by weight of the eucalyptus plant extract.
It is desirable to add 0 parts by weight. When an inclusion agent is added, the concentration of the extract in the extract solution may be arbitrary.

Inclusion agent (including intercalation agent)
Cyclodextrin, crown ether,
Examples include cellulose, carboxymethylcellulose, sepiolite, xanthothine, urea, aromatic carboxylic acid, dicarboxylic acid, cholic acid, deoxycholic acid, butylhydroquinone, corn starch and the like.

The types of cyclodextrins include, for example, α-type, β-type, γ-type and mixtures thereof, sugars,
For example, various types to which a derivative such as an alkyl group is added may be mentioned.

By the above adsorbent treatment, the color and odor of the eucalyptus extract are removed, and the antibacterial activity and hair growth activity of the extract are increased. In addition, the odor of the eucalyptus extract can be removed by the clathrate treatment. Above, adsorbent treatment,
Extracts obtained by clathrate treatment, for example, pharmaceuticals,
It can be used for quasi-drugs, cosmetics, antibacterial agents, freshness preservatives, food preservatives, anti-fading agents and the like. The freshness preserving agent, food preservative, and anti-fading agent can be preferably used for applications such as preserving freshness, preserving, and preventing fading of foods such as vegetables, fruits, meats, and fish. In addition, deodorant, antioxidant, insect repellent, anti-mite agent, pest repellent, bath agent, herbicide, agricultural chemical, plant growth agent, cut flower activator, diet food, feed, paper, ink, inkjet It can be blended with products that can use eucalyptus extracts, such as recording materials.

Examples of the antibacterial agent include household goods such as tables, tableware, cutting boards, countertops, toilet seats, etc., livestock houses, poultry houses, buildings for animal breeding, utensils, meat processing in general households and restaurants. Facilities and machinery, kitchens of restaurants and households, skin of humans and animals, eggshells of chicken eggs and quail,
In hospitals and nursing homes, doors, door handles,
Floor, bed railing, medical equipment such as surgical instruments, medical equipment, food such as meat, fish, vegetables, etc., as a disinfectant for plant seeds, wet tissues, diapers, sheets, clothing, sanitary cotton, Wipes, non-woven fabric, oil-absorbing paper, paper (sheets) for food packaging, cardboards, papers (sheets) laid under food, paper slippers, towels, towels, covers, animal and fish feed, gum, Candied products such as candies, kamaboko and chikuwa, livestock products such as sausage and ham, western confectionery, Japanese confectionery, raw noodles, buckwheat noodles,
It can be used as an antibacterial agent to add antibacterial activity to sauces, seasonings such as soy sauce, pickles, prepared dishes, processed eggs, sandwiches, mayonnaise, cream puffs and the like. It can also be added to soaps, detergents, creams, etc., or added to beverages (juices, milk, etc.), mouthwashes, toothpastes, oral drugs and the like. It can also be used as a bactericide in the production process of beverages.

[0024]

EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples. However, these examples are illustrative, and the scope of the present invention is defined by the appended claims.

<Production Example 1> Eucalyptus globu
lus ) (Lot. 1) (100 g, dry weight) was immersed in 1 L of ethanol for 3 days to obtain 950 ml of an extract solution.
In the present embodiment, the extract component excluding the solvent is referred to as an extract. In addition, liter is indicated by L, and milliliter is m
Indicated by 1 and microliter by μl.

<Production Example 2> Eucalyptus globu
lus ) (Lot.2) (250 g, dry weight) was steam distilled, the leaves were dried, immersed in ethanol for 3 days, and the extract 9
30 ml were obtained.

<Production Example 3> 100 g (dry weight) of eucalyptus (E. globulus) leaves (Lot. 3) was immersed in 1 L of ethanol (at room temperature for 2 days) to obtain 940 ml of an extract solution (extract) Concentration: 2.0% by weight). 23.5 g of activated carbon was added to the extract and stirred at room temperature for 1 hour. Next, the mixture was filtered under pressure to obtain a filtrate (extract) (concentration of extract: 1.
0% by weight). Glycerin fatty acid ester was added to this extract so that the final concentration was 0.6% by weight.

<Examples 1 to 5> The extract of Preparation Example 1 was prepared with ethanol so that the extract had a concentration of 2.0% by weight. 50 ml of this extract solution was put in a container, and mixed with an adsorbent (activated carbon: Sigma, Celite: Wako, silica gel: Merck, diatomaceous earth: Wako, zeolite A-3: Wako).
As for activated carbon, 0.01 part by weight of the extract was used.
~ 2.5 parts by weight of the extract mixed with
Also, Celite, silica gel, diatomaceous earth, zeolite A-
About 3, with respect to 1 part by weight of the extract, 0.05 to
It mixed with the extract so that it might become 2.5 weight part addition amount, and stirred at room temperature for 1 hour. Next, the mixture was filtered through filter paper, and the filtrate was concentrated under reduced pressure to obtain an extract (solid content). The degree of decolorization of the extract was evaluated by visual observation and measuring the rate of decrease in absorbance. For the absorbance measurement, the extract was dissolved in ethanol so that the final concentration was 0.02% by weight, and the absorbance at 393 nm and 664 nm was measured. Further, the degree of the odor was evaluated according to the following five grades.

Strongest smell 5 Strong smell 4 Smell 3 Smell slightly 2 No smell 1

With respect to the antibacterial activity of the extract, Staphylococcus aureus IFO12732 and Alicyclobacillus acidoterrestris A
TCC49025), dental caries ( Streptococcus mutans GS-5),
Periodontal disease bacteria ( Porphyromonas gingivalis 381), halitosis bacteria ( Fusobacterium nucleatum ATCC49256), H. pylori ( H
elicobacter pylori ATCC43504) was measured. The minimum growth inhibitory concentration was measured as follows. After pre-culturing the bacteria, the cells were diluted with physiological saline to adjust the number of bacteria to about 5 × 10 ⁸ cells / ml. S.aure
ua , A. acidoterrestris , S. mutans , P. gingivalis , F.
For nucleatum , the eucalyptus plant extract is dissolved in DMSO and the final concentration of the extract is 250-0.2 μg / ml
Was added to 950 μl of the liquid medium. 10 μl of the above bacterial suspension was added to this mixture, and the mixture was incubated at 37 ° C. for 24 hours, and the presence or absence of bacterial growth was visually observed.
In addition, about F.nucleatum , it culture | cultivated on anaerobic conditions. For H.pylori , extract of Eucalyptus plant
Dissolve in DMSO and bring this solution to a final extract concentration of 250-0.2
Add 500 μl to 9.5 ml of agar medium to be μg / ml,
Solidified. The bacterial suspension (1.0 × 10 ⁸
/ ml) was inoculated with one streak ear streak and anaerobic conditions (5% CO ₂ ) 37
After incubation at 48 ° C for 48 hours, the presence or absence of bacterial growth was visually observed. Table 1 shows the results of the adsorbent treatment (Examples 1 to 5) and the untreated treatment (Comparative Example 1). When the extract solution was treated with the adsorbent, the color and odor of the extract were reduced as compared with the case where the extract solution was not treated. As a result of the absorbance measurement, the absorbance at 393 nm and 664 nm decreased when the adsorbent was treated. Among the various adsorbents, activated carbon had the highest degree of decolorization (visual observation, degree of decrease in absorbance) and degree of decrease in odor. or,
Sorbent (activated carbon, celite, silica gel, diatomaceous earth,
When 2.5 parts by weight of (zeolite) was added, the antibacterial activity increased as compared with the untreated (blank). Extract 1 in FIG.
The spectra of the extract treated with 2.5 parts by weight of activated carbon per part by weight and the untreated (blank) extract are shown. The extract treated with activated carbon was 393 compared to the untreated extract.
nm and 664 nm peaks decreased.

[0031]

[Table 1]

In Table 1, the addition amount "^a" indicates the addition amount relative to 1 part by weight of the eucalyptus extract. Sa is Staphylococcu
s aureus , Aa is Alicyclobacillus acidoterrestris ,
Sm is Streptococcus mutans , Pg is Porphyromonas ging
ivalis , Fn is Fusobacterium nucleatum , Hp is Helicob
Acter pylori is shown respectively.

Example 6 The extract of Preparation Example 2 was prepared with ethanol so that the extract had a concentration of 2.0% by weight.
This extract solution was mixed with activated carbon in the same manner as in Example 1, and the degree of decolorization and the odor of the extract after the activated carbon treatment were evaluated. The antibacterial activity was also measured. Table 2 shows the results of the activated carbon treatment (Example 6) and the untreated (Comparative Example 2). As the amount of activated carbon added increased, the color and odor of the extract decreased. As a result of absorbance measurement, when activated carbon treatment,
The absorbance at 393 nm and 664 nm decreased. That is, there was an effect of removing the odor remaining in the extract that was not removed by the steam distillation. When 2.5 parts by weight of activated carbon was added, the antibacterial activity increased. In Table 2, the addition amount and the microorganism name have the same meanings as in Table 1.

[0034]

[Table 2]

Examples 7 and 8 The eucalyptus extract of Production Example 1 was dissolved in ethanol / water (1:19) so that the final concentration of the extract was 0.1%. To this solution was added cyclodextrin (K-100, Isoelite P: saltwater port sugar) in an amount of 0.01 to 1 part by weight of the eucalyptus extract.
It was added so as to be 50 parts by weight, and the odor was evaluated. Table 3
The results of addition of cyclodextrin (Examples 7 and 8) and no addition (Comparative Example 3) show that the odor of the extract decreased as the amount of cyclodextrin added increased.

[0036]

[Table 3]

Example 9 The eucalyptus extract of Production Example 2 was dissolved in ethanol / water (1:19) so that the final concentration of the extract was 0.1%. Cyclodextrin (Iso-Elite P) was added to this solution with Eucalyptus extract 1
It was added in an amount of 0.01 to 50 parts by weight with respect to parts by weight, and the odor was evaluated. Table 4 shows the results of addition of cyclodextrin (Example 9) and no addition (Comparative Example 4). As the amount of cyclodextrin added increased, the odor of the extract decreased. That is, there was an effect of removing the odor remaining in the extract that was not removed by the steam distillation.

[0038]

[Table 4]

<Example 10> The eucalyptus extract used in Example 1 (activated carbon treatment: 2.5 parts by weight of activated carbon added to 1 part by weight of the extract) was added to apple juice at 0.01% by weight, and the mixture was heated at 40 ° C. The mixture was allowed to stand, and it was examined whether or not turbidity and putrefactive odor were formed in the juice. As shown in Table 5, when the eucalyptus extract was added (Example 10), turbidity was observed even after 30 days had passed, and neither putrid smell was observed than when no eucalyptus extract was added (Comparative Example 5).

[0040]

[Table 5]

Example 11 After mixing the extract of Production Example 3 with orange juice at a ratio of 1:99, the mixture was allowed to stand at 40 ° C. to examine whether or not turbidity and putrefactive odor were formed in the juice. As shown in Table 6, when the extract was added (Example 11), turbidity was observed after 30 days as compared with the case where the extract was not added (Comparative Example 6), and neither putrid odor was observed.

[0042]

[Table 6]

[0043]

According to the present invention, an extract having high antibacterial activity from which color and odor have been removed can be obtained.

[Brief description of the drawings]

FIG. 1 shows an absorbance spectrum.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) A61K 7/06 A61K 35/78 C 35/78 A61P 17/14 A61P 17/14 29/00 29/00 31 / 04 31/04 A23L 2/00 NF term (reference) 4B017 LC10 LG15 LL07 4B021 LW06 MC01 MK05 MP01 4C083 AA111 CC37 EE22 FF01 4C088 AB57 AC05 BA10 CA06 CA07 MA01 NA09 ZA92 ZB11 ZB35 4H011 AA02 BA0113

Claims (7)

[Claims] 1. An extract solution obtained by extracting a eucalyptus plant with a polar solvent using at least one material selected from an adsorbent and an clathrate to remove color and / or odor. A method for producing a eucalyptus extract. 2. The extract solution is added with at least one adsorbent selected from activated carbon, celite, silica gel, diatomaceous earth and zeolite, and the color and odor are adsorbed to the adsorbent. The method for producing a eucalyptus extract according to claim 1, wherein the eucalyptus extract is separated from the adsorbent. 3. The method according to claim 2, wherein the adsorbent is added in an amount of 0.01 part by weight or more based on 1 part by weight of the extract component.
3. The method for producing a eucalyptus extract according to item 1. 4. The method for producing a eucalyptus extract according to claim 1, wherein the odor is removed by adding a clathrate to the extract solution. 5. The method for producing a eucalyptus extract according to claim 4, wherein 0.01 to 100 parts by weight of the clathrate is added to 1 part by weight of the extract component. 6. The method for producing a eucalyptus extract according to claim 4, wherein the clathrate is cyclodextrin. 7. The method for producing a eucalyptus extract according to claim 1, which is used by being added to a beverage.