KR20150135865A - Composition for Repelling Ant Comprising Supercritical Fluid Extract Oils from Plant as Active Ingredient - Google Patents

Abstract

The present invention relates to a composition for repelling an ant including a mixture of a Cinnamomum verum supercritical extract (i) and an Acorus gramineus supercritical extract or a Zanthoxylum schinifolium supercritical extract (ii) as an active ingredient, and to a manufacturing method of the composition for repelling an ant. The supercritical extract of the present invention can be manufactured at low costs and is economical, has excellent durability of an ant repelling activity, and has a safer property as a repellent agent derived from a natural product in comparison with an existing compound repellent agent. Accordingly, the composition of the present invention can be developed as an active ingredient of an ant repellent agent.

Description

TECHNICAL FIELD The present invention relates to a composition for avoiding ants containing supercritical extract of a natural product as an active ingredient,

The present invention relates to a composition for avoiding ants containing a supercritical extract of a natural product as an active ingredient. More specifically, (i) Cinnamomum verum supercritical extract; And (ii) a supercritical extract of Acorus gramineus or a mixture of supercritical extract of Zanthoxylum schinifolium as an active ingredient.

Essential oil is a non-polar material that is volatilized as a secretion from the stem or leaf of food. Essential oils extracted from plants are a mixture of mono-component, monoterpene-based, and phenylpropene-based compounds. There are differences in the essential oil components depending on the genetic characteristics and cultivation environment of the extracted plant species. The form of essential oil is cavity, ducts, grandular, trichome, and cell. Antioxidant, antibacterial, anticancer, immunological and anti-inflammatory effects, oral bacteria killing effect and antihypertensive effect on natural essential oils have been reported.

Extracting a specific useful substance from a nonpolar natural essential oil is a very difficult process. Generally, a method of extracting a natural product with an organic solvent is widely used. A typical method is extraction of soxhlet, which is deteriorated by loss of active ingredient because it is used at high temperature for a long time. The plant-derived essential oil component is a representative natural nonpolar material containing a variety of compounds. Since most of the components are structurally very complicated and elaborate as well as highly unstable, efficient methods of extracting organic solvents and high temperatures are effective It is not.

Supercritical fluid extraction (SFE) is an extraction method using a supercritical fluid. Since it extracts fragile essential oil components without using heat, the solvent extraction method using the difference in solubility in a specific solvent In comparison, the supercritical fluid has a high diffusion coefficient and low viscosity, so it can be rapidly extracted and phase separated and the solvent can be easily recovered through changes in temperature and pressure. Recently, supercritical fluid extraction technology has been widely used for carbon dioxide extraction under mild conditions with low critical temperature and critical pressure, and it has less toxicity, flammability, corrosion and environmental problems than conventional organic solvents.

Acorus gramineus AG, Zanthoxylum schinifolium (ZS) and cinnamomum verum (CV) are natural fragrant plants that have been used for various purposes as well as foods. Studies on the processing methods for effectively extracting and commercializing soluble substances and active ingredients of cinnamon (CV) have been carried out. However, studies on processing methods for efficiently extracting and commercializing the soluble substances and active ingredients of cinnamon have revealed that, There is a report that facilitates the separation of the filtration by reducing the production of the constituent substances. However, there are reports that the contents of the research can not be published because of industrial and mechanical limitations.

Although human technology is developing at an extremely high level, global warming and climatic changes such as El Niño are associated with environmental problems and threats to human life. Particularly, harmful insect pests are frequent, and the area of occurrence is increased and the density is increased, so that the damage caused by the mosquito is getting worse. Such insect pests indirectly, directly mediate various diseases or spread infectious diseases to human beings for survival, and it has done much damage to the past mankind. Typical insect pests include mosquitoes, ants and mites, and they have mediated or spread various diseases such as dengue fever, malaria, and allergic diseases. These diseases carry more than 700 million people each year, with more than a million deaths annually, and more than 3,000 people die per day from malaria. In particular, ants are the most common pest insects, causing considerable damage to households and industries, and can cause food allergy, food poisoning, economic loss and allergic reactions by injecting allergic pathogens into the body. The ants are widely alive worldwide, including domestically, and about 100 million years ago, more than 9,000 species are distributed throughout the world and are widely known as plague mediators from ancient times. Recently, it has been reported that ants can act as inhalation allergens and cause bronchial asthma. In addition to this, attention should be paid to headache, boredom, fever, convulsions, palpitations and general allergic reactions caused by Formic Acid when it is bothered by ants. In order to combat the ants mediating these infectious diseases, human beings are exploring various ways of controlling pests in various environments and development is actively under way. DEET is the most widely used general-purpose repellent ingredient, but it has problems of safety and unpleasant odor due to its high skin permeability. To overcome this problem, many DEET derivatives have been developed and attempted with microencapsulation, such as KBR 3023 (1-methyl-propyl 2- (2-hydroxyethyl) -1-piperidinecarboxylate), CIC-4 (hydroxymethylcyclohexyl acetic acid lactone) Have been developed, but they have not shown a remarkable effect in the avoidance effect. Therefore, it is necessary to develop a repellent to replace DEET.

Numerous papers and patent documents are referenced and cited throughout this specification. The disclosures of the cited papers and patent documents are incorporated herein by reference in their entirety to better understand the state of the art to which the present invention pertains and the content of the present invention.

Korea Patent Publication No. 10-2009-0103280 Korean Patent Publication No. 10-2007-0011590

The present inventors have made efforts to develop an active ingredient which can be used as an antidemic agent from a strong natural product. As a result, the present inventors have completed the present invention by experimentally proving that the oil component obtained by supercritical extraction of Seokchonpo, Sancho and Cinnamon is superior to ants repelling agents conventionally used.

Accordingly, it is an object of the present invention to provide a composition for avoiding ants which comprises a supercritical extract of Seokchonpo, sancho, or cinnamon as an active ingredient.

Another object of the present invention is to provide a method for combating ants comprising the step of spraying the composition for avoiding ants.

It is still another object of the present invention to provide a method for producing the composition for avoiding ants.

The objects and advantages of the present invention will become more apparent from the following detailed description of the invention, claims and drawings.

According to one aspect of the present invention, the present invention provides a composition comprising (i) cinnamomum verum supercritical extract; And (ii) a supercritical extract of Acorus gramineus or a mixture of supercritical extract of Zanthoxylum schinifolium as an active ingredient.

As used herein, the term " composition for avoiding ants " means the same composition as ant anticipatory agent, and is used for the purpose of chasing ants using the property that ants avoid odor and taste.

According to a preferred embodiment of the present invention, (i) cinnamon supercritical extract; And (ii) the mixing ratio of the supercritical extract of Seokchangpo or the supercritical water extract of Chojang supernatant is 1: 1 by weight.

According to another preferred embodiment of the present invention, the supercritical extract as the active ingredient is contained in an amount of 0.1 to 30% by weight based on the total composition.

According to another preferred embodiment of the present invention, the supercritical extract as an active ingredient is used in an amount of 0.1 to 20% by weight, more preferably 1 to 10% by weight, and still more preferably 1 to 5% by weight, .

As used herein, the term " supercritical extraction "refers to a method of extraction using supercritical fluid, which is a fluid at a critical temperature and pressure above the boundary pressure. When the gas is below the critical temperature, it liquefies when it exceeds a certain pressure, but when it is above the critical temperature, it shows a continuous phase from low pressure to high pressure and it can not distinguish gas and liquid properties. Therefore, supercritical fluids have high density, low viscosity, and about one hundred times as much liquid as liquids. Therefore, supercritical extraction using supercritical fluid is an efficient extraction method compared to liquid extraction.

According to a preferred embodiment of the present invention, the supercritical extraction method uses carbon dioxide as a supercritical fluid.

The co-solvent used in conjunction with the supercritical fluid includes polar solvents commonly used in the art, preferably alcohols, water, ethylene glycol, polyethylene glycol, propylene carbonate, formic acid , Acetic acid, acetonitrile, chlorodifluoromethane or mixtures thereof, more preferably selected from the group consisting of methanol, ethanol, propanol, 1-hexanol, 2-methoxyethanol and combinations thereof Alcohol, more preferably methanol or ethanol, and most preferably ethanol.

The pressure and temperature in the supercritical extraction can be selected by a person skilled in the art within a suitable range.

According to a preferred embodiment of the present invention, the supercritical extraction is performed at a pressure of 100-500 bar and a temperature of 30 ° C-50 ° C.

In the present invention, the supercritical extract of cinnamon extracted under supercritical conditions includes trans-cinnamaldehyde, coumarin and 4-methoxycinnamaldehyde, Critical extracts include cis-asarone, linoleic acid, and benzene, and supercritical extracts of sancho include oleic acid, acetate, citronella, palmitic acid, 2 , 2,6-octadiene, and cryptone.

According to another aspect of the present invention, the present invention provides a method for combating ants comprising the step of spraying the composition for avoiding ants described above.

According to another aspect of the present invention, the present invention provides a method for preparing ant antiperspirant composition comprising the steps of:

(a) Cinnamomum verum was heated at a pressure of 150-250 bar, at a temperature of 25-35 ° C, and as supercritical fluid and co-solvent with carbon dioxide: ethanol at a flow rate of 47.5 g / min: 2.5 g / min ) To obtain a supercritical extract of cinnamon;

(b) Acorus gramineus was treated with a pressure of 130-230 bar, a temperature of 40-50 ° C, and a supercritical fluid and a co-solvent of carbon dioxide: ethanol at a flow rate of 120 g / min: 3.6 g / min ) Under supercritical condition to obtain a supercritical extract of Seokchangpo;

(c) dissolving Zanthoxylum schinifolium at a pressure of 400-500 bar, a temperature of 40-50 ° C, and a supercritical fluid and an auxiliary solvent such as carbon dioxide: ethanol at a flow rate of 120 g / min: 3.6 g / min ) Under supercritical condition to obtain a supercritical extract of Sanchos; And

(d) mixing supercritical extract of cinnamon and supercritical extract of licorice root or supercritical extract of acacia var. chow at a weight ratio of 1: 1 to prepare a mixture.

According to still another aspect of the present invention, there is provided an antidumping composition comprising a supercritical extract of cinnamon and a supercritical extract of cinnamon or sancho as an active ingredient.

(I) Cinnamomum verum supercritical extract; And (ii) a supercritical extract of Acorus gramineus or a mixture of supercritical extract of Zanthoxylum schinifolium as an active ingredient, and a method for preparing the composition for avoiding ants. The supercritical extract of the present invention can be manufactured at low cost, is economical, has excellent persistence of antiproliferative activity, and is a safener derived from a natural product, so that it has safety characteristics as compared with a conventional compound repellent. Thus, the composition of the present invention can be developed as an active ingredient of antiprotting agents.

Figure 1 is a photograph of a cage (15 x 15 x 7 cm) for an ant escape experiment.
Figure 2 is a cage photograph for an antidisruption persistence experiment.
Figure 3 shows the antifrontal activity of a supercritical extract alone (A panel) or a mixture of its extracts (B panel) of Acorus gramineus (AG), Zanthoxylum schinifolium (ZS) or Cinnamomum verum (C panel) in the dark environment, as shown in FIG.

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for describing the present invention in more detail and that the scope of the present invention is not limited by these embodiments in accordance with the gist of the present invention .

Example

Materials and methods

1. Manufacture of Supercritical Oil of Seocheongpo (AG), Sancho (ZS), and Cinnamon (CV)

The seokchangpo used in the experiment (Acorus gramineus, AG), Japanese pepper (Zanthoxylum schinifolium, ZS), cinnamon (Cinnamomum verum, CV) was used to purchase the powdered dry state in the cod yakryeong market. Supercritical extraction system for supercritical extraction was a Waters AD-RC 08 (Waters Co., Miford, MA, USA). 300 g of each sample was added to the extraction container. Seokchangpo was extracted with 150g / min of CO ₂ flow rate: 120 g / min: 3.6 g / min at 180 bar and 45 ℃. Sancho was extracted at 450 bar and 45 ℃ for 120 min at a CO ₂ flow rate of 120 g / min: 3.6 g / min. Cinnamon was extracted at 200 bar and 30 ℃ for 120 min at a CO ₂ flow rate of 47.5 g / min: 2.5 g / min. An essential oil component was obtained for each sample by the above method. HPLC-grade ethyl alcohol (JT Baker Co., Phillipsburg, NJ, USA) was used as a co-solvent.

2. Component analysis by gas chromatography mass spectrometer (GC / MS, Gas chromatograph)

The oil obtained by supercritical extraction was analyzed by gas chromatograph mass spectrometer (GC / MS). The GC / MS system used in the experiment was HP 190914-433 model (Paloalto, California, USA) and HP-5MS (30 mx 0.255 mm, 0.25 μM) was used for the column. A mass spectrometer was used as the detector, and ionization was performed at energy of 70 eV in the ESI mode, and the mass was confirmed by setting the ion mass range to 10-800 in the SCAN model of TIC. The injector temperature was set at 260 ° C, the detector temperature was set at 280 ° C, the carrier gas was helium, and the oven temperature was initially set at 50 ° C for 5 minutes And the temperature was raised to 200 ° C at a rate of 4 ° C / min. Thereafter, the temperature was increased from 200 ° C to 280 ° C at a rate of 20 ° C / min and then maintained for 20 minutes. Each supercritical extraction oil was filtered through a 0.45 μM membrane filter and diluted in HPLC grade ethyl alcohol (JT Baker Co., Phillipsburg, NJ, USA).

3. Test insect

The ants used in the evaluation of repellency against ants were Camponotus japonicus (Bibobibaant kingdom Co., Deagu, Korea). Feeding conditions were kept at 25-30 ℃ and humidity was 40-60%, and feed jelly was fed for feeding and watering. The most active time was selected in consideration of the state of ants and used in the ant escape experiments.

4. ant avoidance experiment

For the ant avoidance experiment, a cage 15 x 15 x 7 cm in size was prepared and 30 ants were put into the experiment (see Fig. 1). The cage was divided into two spaces to distinguish the untreated side from the untreated side, and ventilation holes were made so that the sample was ventilated. For the treatment of the sample, dilute each supercritical extract oil to 10% concentration in ethanol with a size of 8 x 8 cm, dispense 1 mL of the supernatant into the filter paper, dry it thoroughly, place the filter paper on the bottom, Respectively. On top of that, jelly for feed was installed in a size of 2 x 2 x 2 cm. The animals were fasted 12 hours before the experiment, and the ants were replaced with new colonies each time according to the sample, and the experiment was repeated 3 times. As a control, 1 mL of ethanol was added to the filter paper, and DEET was dispensed in the same manner as the material control. The eruption power was calculated by counting the number of ants that were brought on the glass plate at intervals of 10 minutes for 1 hour.

5. Ant survival experiment

The ants were able to survive by constructing habitats in the dark by forming communities. Therefore, the effect of supercritical oil was investigated in dark conditions. Prepare two moving passages in a 15 x 15 x 8 cm acrylic cage and attach a 50 mL tube to the inside of the tube. Dilute the sample to the outside with 10% concentration, apply 2 mL, dry, and then use foil And the tube was wrapped to block light (see FIG. 2). The ants were fasted for 24 hours in an acrylic cage. After 24 hours, the number of ants in the 50 mL tube was observed. 70% ethanol was used as a control and DEET was used as a substance control.

Results and discussion

1. Analysis of GC / MS components of petroleum jelly, Sancho and cinnamon supercritical oils

The results of analysis of three natural supercritical extraction oils, GC / MS, are shown in Table 2 below. Table 1 shows only peaks having a quality of at least 90% and an area of 1.0 or more at the entire peak. Generally, extraction of soluble organic compounds from an insoluble material is carried out by shaking or filtering the sample with a solvent, and a representative method is soxhlet extraction. The greatest vulnerability of soxhlet extraction is that it is not ideal because it can destroy useful materials in natural products because it requires constant heating and uses a large amount of solvent. In the experimental results of the present invention, three kinds of fragrant plants were subjected to extraction using a supercritical process. As a result, the contents of cis-asarone, oleic acid and acetate were the highest in Seokchangpo, and cinnamaldehyde was the highest in cinnamon.

2. Evaluation of Antituberculosis and Persistence of Seokchangpo, Sancho, Cinnamon Supercritical Oil

The results of confirming the antipodal force of the ants using three natural oils are shown in the graph (A) of FIG. Cinnamon supercritical extraction oil (CV) showed the highest erectile force among the three oils. Further, two oils or three oils were respectively mixed to evaluate the oil repellency. The evaluation results are shown in the graph (B) of Fig. Compared with mixing all three oils, mixing two oils at a ratio of 1: 1 showed a higher effect than using a single oil. Especially, the most effective effect was obtained by mixing Supercritical Extraction Oil (AG) with Zinc Supercritical Water Extract (ZS).

Since ants live in a community that is invisible to the visible population, blocking them from forming ants migration or communities in dark environments is a fundamental avoidance effect. Therefore, in the experiment of the present invention, each supercritical oil was treated in a dark environment to observe the migration of ants after 24 hours (see graph (C) in Fig. 3). Experimental results showed that all ants migrated to the dark environment after 24 hours. However, when treated with cinnamon supercritical fluid (CV), the number of ants decreased significantly in the dark environment.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the same is by way of illustration and example only and is not to be construed as limiting the scope of the present invention. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (7)

(i) Cinnamomum verum supercritical extract; And (ii) a supercritical extract of Acorus gramineus or a mixture of supercritical extract of Zanthoxylum schinifolium as an active ingredient.
2. The method of claim 1, wherein said (i) cinnamon supercritical extract; And (ii) the mixing ratio of the supercritical extract of Seokchangpo or the supercritical water extract of Chojang supernatant is 1: 1 in weight ratio.
The method of claim 1, wherein the cinnamon supercritical extract comprises trans-cinnamaldehyde, coumarin, and 4-methoxy cinnamaldehyde, wherein the supernatant extract of cucumber iscis-asarone and linoleic acid Characterized in that the supercritical water extract comprises oleic acid, acetate, citronella, palmitic acid, 2,6-octadiene, and krypton. / RTI >
The method according to claim 1, wherein the supercritical extract of Cinnamon, Sejangpo, or Sancho is supercritical extraction using carbon dioxide as a supercritical solvent and ethanol as an auxiliary solvent under a pressure of 100-500 bar and a temperature of 30 ° C-50 ° C Wherein the composition is an anticorrosive composition.
A method for combating ants comprising the step of spraying the composition for avoiding ants according to any one of claims 1 to 4.
A method for preparing an antiperspirant composition comprising the steps of:
(a) Cinnamomum verum under conditions of a pressure of 150-250 bar, a temperature of 25-35 ° C and a flow rate of supercritical carbon dioxide: ethanol of 47.5 g / min: 2.5 g / min Supercritical extraction to obtain a supercritical extract of cinnamon;
(b) Acorus gramineus was treated with a pressure of 130-230 bar, a temperature of 40-50 ° C, and a flow rate of 120 g / min: 3.6 g / min of supercritical carbon dioxide: ethanol Supercritical extraction to obtain a supercritical extract of Seok Changpo;
under conditions as 3.6 g / min: (c) a Japanese pepper (Zanthoxylum schinifolium) 400-500bar pressure, temperature, and the supercritical fluid carbon dioxide of 40-50 ℃: the flow rate ratio of ethanol (flow rate) 120 g / min Supercritical extraction to obtain a supercritical extract of Sanchos; And
(d) mixing supercritical extract of cinnamon and supercritical extract of licorice root or supercritical extract of acacia var. chow at a weight ratio of 1: 1 to prepare a mixture.
A composition for avoiding ants comprising the supercritical extract of cinnamon and the supercritical extract of cinnamon or sancho as an active ingredient, which is produced by the production method according to claim 6.

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