JP2014034526A - Repellant - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a repellant that can obtain high repellent effect and has a long-lasting property.SOLUTION: A repellant is for at least one of myriapod and mite, and the repellant includes an extract of rosemary oil in which elution is performed from a column in which the rosemary oil is adsorbed to an adsorption agent using chromatography by using hexane or a hexane/diethyl ether mixed solvent in which hexane is included by at least the same amount to diethyl ether by a capacitance ratio as an expansion solvent, then elution is performed from a residual by using a mixed solvent of hexane/diethyl ether in which diethyl ether is included more than hexane as an expansion solvent by a capacitance ratio, as an active ingredient.

Description

  The present invention relates to repellents.

  Multipods that inhabit the field such as centipedes are harmful to the human body, such as discomfort in appearance and swelling when bitten because they are poisonous. Therefore, various control agents such as application of various essential oils as a repellent for these unpleasant insects have been studied.

  For example, a pest control composition containing, for example, perilla oil, lavender oil, thymol and the like as an active ingredient (for example, see Patent Document 1), and a powder for controlling multipods containing cinnamon powder as an active ingredient (for example, Patent Document) 2) is proposed.

JP-A-11-60421 JP 2007-112773 A

  When powder is sprayed on the ground to control pests, polypods have many body segments and bend and lift the body, so the insect body does not touch the drug sufficiently and the tactile head You can get over the drug without touching it directly. In addition, polypods such as centipedes live in the ground where dead leaves and dead trees are deposited, and because they have short antennae and weak visual perception, they are insensitive to external stimuli, such as mosquitoes, flies, cockroaches, etc. Unlike hygiene pests, it is difficult to obtain repellent effects.

  Although the above-mentioned patent documents 1 and patent documents 2 can obtain a control effect by applying directly to multipods, they are not satisfactory in terms of sustaining the control effect over a long period of time.

  Then, this invention makes it a subject to provide the high repellent effect with respect to an unpleasant pest, and to provide the persistent repellent.

As a result of intensive research to solve the above problems, the present inventors have found that a specific fraction component among rosemary oil components has an excellent repellent effect against unpleasant pests such as polypods. The present invention has been completed.
That is, the subject of this invention is achieved by following (1)-(3).
(1) A repellent of at least one of polypods and ticks, and from a column in which rosemary oil is adsorbed to an adsorbent using chromatography, hexane or hexane is converted into diethyl ether by volume ratio. After elution using a mixed solvent of hexane / diethyl ether contained in the same amount or more as a developing solvent, the residue was mixed with a mixed solvent of hexane / diethyl ether containing more diethyl ether than hexane in a volume ratio. A repellent comprising a rosemary oil extract eluted as a developing solvent as an active ingredient.
(2) From a column in which the rosemary oil is adsorbed on an adsorbent,
(A) a step of eluting the first fraction component using hexane as a developing solvent;
(B) From the residue obtained by collecting the first fraction component, the second fraction component using a mixed solvent of hexane: hexane / diethyl ether mixed solvent (hexane: diethyl ether (4: 1)) = 1: 1 as a developing solvent. Elution step,
(C) a step of eluting the third fraction component from the residue obtained by collecting the second fraction component using a mixed solvent of hexane: diethyl ether = 1: 1 as a developing solvent;
(D) Rose of the fourth fraction component obtained by the step of eluting the fourth fraction component from the residue obtained by collecting the third fraction component using a mixed solvent of hexane: diethyl ether = 1: 4 as a developing solvent. The repellent according to (1) above, which contains a mary oil extract as an active ingredient.
(3) The repellent as described in (1) or (2) above, wherein the polypod is at least one selected from centipedes, millipedes, geese, brackish beetles, and gumworms.

By using the repellent of the present invention, a rapid repellent action can be exhibited over a long period of time against multipods such as centipedes, millipedes, and rotifers, which are unpleasant pests, and a high repellent effect can be exhibited. Furthermore, a high repellent effect can be exhibited against mites.
The active ingredient of the present invention exhibits a high repellent effect even when it is in direct contact with pests or volatilized.

It is a schematic diagram explaining the repelling test method. It is a schematic diagram explaining the repelling test method.

  Hereinafter, the repellent of the present invention will be described in detail.

  The repellent of this invention contains the specific fraction component fractionated from rosemary oil as an active ingredient. This active ingredient can be obtained from a column in which rosemary oil is adsorbed on an adsorbent using chromatography, or hexane or a mixture of hexane and diethyl ether containing hexane in a volume ratio equal to or greater than diethyl ether. After elution using a solvent as a developing solvent, the residue was eluted using a mixed solvent of hexane / diethyl ether containing a larger volume of diethyl ether than hexane in a volume ratio (hereinafter referred to as “the present invention”). May be referred to as "rosemary oil extract").

  Rosemary (scientific name: Rosmarinus officinalis) is an evergreen shrub belonging to the family Lamiaceae widely distributed in the countries of the Mediterranean coast. Rosemary oil is an essential oil collected by distilling leaves and flowers of rosemary. It is liquid. Examples of the rosemary oil that can be used in the present invention include rosemary cineole, rosemary berbenone, rosemary camphor and the like.

  Rosemary oil is fractionated by adsorption column chromatography, liquid chromatography, or gas chromatography using an adsorbent such as silica gel, alumina, glass beads, polymer resin, or diatomaceous earth. In the present invention, it is preferable to use adsorption column chromatography using silica gel because the operation is simple and a large amount of sample can be processed.

  When using adsorption column chromatography, it is preferable to use a developing solvent in order from a low polarity and to elute in multiple steps. This is because, by gradually increasing the polarity of the solvent, it is possible to sequentially elute high polar substances from low polar substances. Examples of the developing solvent include hexane, diethyl ether, ethyl acetate, and the like. These solvents can be mixed, and the polarity of the developing solvent can be changed depending on the mixing ratio.

  In the present invention, from a column in which rosemary oil is adsorbed on an adsorbent, hexane or a hexane / diethyl ether mixed solvent containing hexane in a volume ratio equal to or more than diethyl ether is used as a developing solvent. After elution and separation of components other than repellent components, the residue is eluted with a hexane / diethyl ether mixed solution containing more diethyl ether than hexane in a volume ratio to purify and concentrate the repellent components To do.

  Specifically, first, the first fraction component is eluted from the rosemary oil adsorbed on an adsorbent such as silica gel using hexane as a developing solvent using chromatography. Next, the residue obtained by collecting the first fraction component is chromatographed using a mixed solvent of hexane: hexane / diethyl ether (hexane: diethyl ether (4: 1)) = 1: 1 as a developing solvent. Elute the second fraction component. Subsequently, the residue obtained by collecting the second fraction component is subjected to chromatography using a mixed solvent of hexane: diethyl ether = 1: 1 as a developing solvent to elute the third fraction component. Then, the residue obtained by collecting the third fraction component is subjected to chromatography using a mixed solvent of hexane: diethyl ether = 1: 4 as a developing solvent to elute the fourth fraction component. It is considered that the aromatic component, antioxidant component, and deodorizing component of rosemary oil are purified, concentrated and eluted from these first to third fraction components.

  In this way, an eluent using a mixed solvent of hexane / diethyl ether containing more diethyl ether than hexane in a volume ratio by eluting sequentially from aromatic components and antioxidant components that are easily soluble in a low polarity solvent , The repellent component for polypods is purified, concentrated and eluted. In addition, although the rosemary extract of this invention can be obtained by four processes using the above-mentioned four kinds of developing solvents, it is not limited to the method of separating into the above four processes, and any number of processes can be performed. good.

  The obtained rosemary oil extract of the present invention may be used as an elution stock solution as it is, but may be used after being concentrated and dried by an appropriate method, or may be used after being dissolved in an appropriate solvent. Examples of the solvent include acetone, ethanol, methanol, paraffin, and the like.

  The repellent of the present invention can be used as various preparations, and may be only an active ingredient (rosemary oil extract of the present invention), or a carrier such as a liquid or a solid. For example, it can be formulated as a liquid, gel, sol, granule, granule, microcapsule, tablet, aerosol, sheet or the like.

Examples of the method for formulating using a carrier or the like include the following methods.
(1) A method of mixing the rosemary oil extract of the present invention with a solid carrier, a liquid carrier, a gaseous carrier or the like.
(2) A method of impregnating a solid support with the rosemary oil extract of the present invention.
(3) A method of molding after mixing the rosemary oil extract of the present invention and a solid carrier.

  The repellent of the present invention preferably contains 0.05% by mass or more of the rosemary oil extract of the present invention, more preferably 0.05 to 20% by mass, It is more preferable to contain 2% by mass. If the content of the rosemary oil extract is less than 0.05% by mass in the preparation, a repellent effect on polypods may not be sufficiently obtained. When the active ingredient of the present invention is impregnated and mixed in a carrier, a sufficient repellent effect can be obtained if the content of the rosemary oil extract in the preparation is 20% by mass. When the content exceeds 20% by weight, the cost increases, which is not preferable. In addition, when a powder is used, the properties of the carrier may not be maintained.

  Examples of solid carriers used in the formulation include mineral powders such as talc, wax, kaolin, calcium carbonate, bentonite, silica, feldspar, hydrous silicon dioxide, acid clay, diatomaceous earth powder, and pumice powder; Examples include moving substance powders such as corn starch and silk powder; sugars such as glucose, sucrose, and lactose; inorganic salts such as sodium carbonate, sodium sulfate, potassium chloride, ammonium sulfate, ammonium nitrate, and ammonium phosphate. Among these, mineral powders, particularly talc, clay, silica, feldspar, and kaolin are preferred because they are difficult to scatter and do not dissolve in rainwater. These solid carriers can be used alone or in combination of two or more.

  As the liquid carrier, for example, water, alcohol, hydrocarbon or the like can be used, and further a gel-like liquid containing a thickening polymer compound or an emulsion containing a surfactant may be used. Among these, a gel-like liquid containing a thickening polymer compound is preferable because the volatilization amount is controlled and the repelling effect is easily maintained. These liquid carriers can be used alone or in combination of two or more. In addition, after the rosemary oil extract of the present invention is mixed with a liquid carrier, it can be solidified using a gelling agent or impregnated with a water-absorbing polymer.

  Examples of the gaseous carrier include butane gas, chlorofluorocarbon gas, alternative chlorofluorocarbon gas, liquefied petroleum gas (LPG), dimethyl ether, nitrogen gas, and carbon dioxide gas.

  Moreover, you may add arbitrary components to the repellent of this invention in the range which does not prevent the effect.

  Examples of optional components include solvents, surfactants, ultraviolet absorbers, antioxidants, fragrances, colorants, water repellents, preservatives, pH adjusters, oils, thickeners, and spreading agents. It is done.

  Examples of the solvent include water, alcohols, esters, ketones, ethers, hydrocarbons, aromatics and the like.

  Examples of the surfactant include alkyl sulfate ester salts, alkyl sulfonate salts, alkyl aryl sulfonate salts, alkyl aryl ethers, polyoxyethylenates of alkyl aryl ethers, polyethylene glycol ethers, polyhydric alcohol esters, and the like. Is mentioned.

  Examples of the ultraviolet absorber include benzophenone-based compounds such as 2,4-dihydroxybenzophenone and benzotriazole-based compounds such as 2- (2′-hydroxy-5′-methylphenyl) enzotriazole.

  Examples of the antioxidant include butylhydroxyanisole, dibutylhydroxytoluene, tocopherol, γ-oryzanol, ascorbic acid and the like.

  As the fragrance, for example, essential oils such as rose oil, lavender oil, bergamot oil, cinnamon oil, citronella oil, lemon oil, peppermint oil, aromatic substances such as pinene, linalool, menthol, citral, citronellal, vanillin, borneol, These glycosides, natural fragrances, synthetic fragrances, blended fragrances and the like can be mentioned.

  Examples of the colorant include legal dyes such as Blue No. 1, Green No. 202, and Purple No. 201, and natural dyes such as riboflavin and chlorophyll.

  Examples of the water repellent include silicone oil.

  Examples of the preservative include phenoxyethanol, benzyl alcohol, parabens, quaternary ammonium salts and the like.

  Examples of the pH adjuster include citric acid, phosphoric acid, sodium carbonate, sodium hydrogen carbonate, succinic acid and the like.

  Examples of oils include silicone oils, vegetable oils, animal oils, synthetic oils, and petroleums.

  Examples of the thickener include water-soluble polymer compounds such as xanthan gum and carboxymethyl cellulose, and clay minerals such as bentonite.

  Examples of the spreading agent include polyoxyethylene nonyl phenyl ether and polyoxyethylene lauryl ether.

The repellent of the present invention is treated by placing, applying, spraying, spraying, etc. on the target place and target space, for example, habitats of unpleasant pests such as polypods (plants, soil, indoors, etc.) Used by
The rosemary oil extract, which is an active ingredient of the repellent of the present invention, generally depends on the use scene, method of use, type of preparation, target pest, etc. ^What is necessary is just to apply so that it may become 10-50g per 20 (20-100mg as an active ingredient).

  Examples of the object of the repellent of the present invention include outdoor polypods, such as centipedes such as tobism cadet, aorth cadet, gym cadet, and issun centipede, millipede such as zelkova, red scallop, and baba The present invention can be applied to a rubber leaf, such as a rubber leaf, and a leaf, such as a spring, a white edge. Above all, it is particularly excellent in repellency against centipedes. Furthermore, the present invention can also be applied to mites such as leopard mites, coral mites, claw mites, and house dust mites.

  Hereinafter, although the repellent of this invention is demonstrated in detail from an Example, this invention is not restrict | limited at all by these examples.

<Preparation of rosemary oil extract>
Fractionation of rosemary oil (trade name: ROSEMARY OIL, manufactured by MATIERES PREMIERES ESSENTIELLES) was performed using silica gel chromatography.
Absorbent cotton was packed into the liquid outlet of a glass column for chromatography (inner diameter 50 mm × length 500 mm) for diameter reduction toward the liquid outlet. After pouring an appropriate amount of hexane into the column, sea sand was packed into the reduced diameter portion.
An appropriate amount of hexane was put into a beaker containing 200 g of silica gel (trade name: silica gel 60 (spherical, particle size 63 to 210 μm), manufactured by Kanto Chemical Co., Inc.) and stirred. This was slowly poured into the column, and it was confirmed that silica gel was tightly packed in the column while flowing hexane.
When hexane was dripped from the lower surface position of the silica gel layer, 10 g of rosemary oil was poured to adsorb the rosemary oil onto the silica gel.

After confirming that all of the rosemary oil has soaked into the silica gel, the first to sixth fraction components are eluted and fractionated using the following developing solvent (flow rate: 40 to 50 mL / min). Paint components were obtained.
(Developing solvent)
First fraction: 300 mL of hexane
Second fraction: hexane 300 mL + hexane: diethyl ether = 4: 1 300 mL
Third fraction: hexane: diethyl ether = 1: 1 300 mL
Fourth fraction: hexane: diethyl ether = 1: 4 300 mL
Fifth fraction: diethyl ether 300mL
6th fraction: 300 mL ethyl acetate

  Each of the fraction components was subjected to the following test.

<Preliminary test>
(Preparation of test samples 1 to 6)
0.5 g of absorbent cotton was impregnated with 0.5 mL of a rosemary extract (100% extract) of each fraction component.

(Test method)
Calcium carbonate powder is applied to the upper inner wall (3cm width) of the transparent glass case with a height of 25cm x width 35cm x height 15cm to prevent escape, and one test insect (centipede, 10cm size) is placed inside the case. Put in.
Each of the test samples 1 to 6 was observed to be close to about 1 cm on the head side of the test insect, and the presence or absence of a repellent effect was determined. If the test specimen is brought closer, it will be warped immediately, and if it is not closer, it will be evaluated as `` Yes '' as `` Avoidance '', and if the test specimen is brought closer, it will be warped, and if it is away from the specimen, it will be evaluated as `` △ '' The case where the test specimen did not react even when brought close to the test specimen was evaluated as “x” as “not avoiding”. The results are shown in Table 1. The test was repeated 10 times.

  From the results in Table 1, it was found that the first and fourth to sixth fraction components showed a repellent effect against centipedes, and the fourth fraction component showed a particularly high repellent effect.

<Repellent test 1>
(Production of test specimen: Example 1, Comparative Examples 1 to 3)
The carrier (Kaolin, manufactured by Zhenjiang Ryu Kinka Kogyo Co., Ltd.) was used so that the rosemary oil extract (100% extract), farnesyl acetone, lavender oil, and mint oil of the fourth fraction component prepared above was 0.2% by mass, respectively. 100 g) was impregnated.

(Test method)
As shown in FIG. 1, the test specimen 13 was sprayed in a width of about 3 cm on a substantially central portion in the width direction of a sheet 15 (made of polypropylene) having a length of 25 cm and a width of 35 cm (application amount of the preparation: 20 g / m ² ). This was accommodated in a transparent glass case 17 having an opening of 25 cm in length, 35 cm in width, and 15 cm in height. After placing one test insect 11 (centipede) of each size shown in Table 2 on the sheet 15 and covering it with a plastic cup of 11 cm in diameter and 10 cm in height so as not to move, it was allowed to acclimatize for about 5 minutes. The plastic cup was removed and left in the glass case.
The behavior when the test insect 11 was in contact with the sprayed area of the test sample 13 10 times was observed, and the repelling rate (%) was determined by the following formula (1). In addition, when the test specimen 11 contacted the test specimen 13, it was counted as a repelling action that the test specimen 11 made a U-turn by dragging the half body or did not touch the test specimen 13. The test insects 11 were tested with a body length of 3 cm, 6 cm, and 10 cm.
The results are shown in Table 2.
Repelling rate (%) = number of times of repelling / number of times of contact (10 times) (1)

  From the result of Table 2, Example 1 which used the rosemary oil extract of this invention as an active ingredient was the high repelling rate of 3 times or more compared with Comparative Examples 1-3. Moreover, regardless of the size (size) of the test insect (centipede), Example 1 has a high repellent rate, and the rosemary oil extract of the present invention has an excellent repellent effect against centipede. I found it.

<Repellent test 2>
(Preparation of test sample: Examples 2 to 4)
Carrier (Kaolin, Zhenjiang Long Kinka Kogyo Co., Ltd.) so that the rosemary oil extract (100% extract) of the fourth fraction component prepared above is 0.2% by mass, 0.1% by mass and 0.05% by mass. Manufactured, 100 g).

(Test method)
As shown in FIG. 1, the test specimen 13 was sprayed with a width of about 3 cm on a substantially central portion in the width direction of a sheet 15 (made of polypropylene) having a length of 25 cm and a width of 35 cm (formulation application rate: 20 g / m ² ). . This was accommodated in a transparent glass case 17 having an opening of 25 cm in length, 35 cm in width, and 15 cm in height. Place one test insect 11 (centipede) with a body length of 3cm, 6cm and 10cm on the sheet 15, and at the same time put it on a plastic cup with a diameter of 11cm and a height of 10cm, and leave it for about 5 minutes to acclimatize. After letting go, the plastic cup was removed and left in the glass case.
The behavior when the test insect 11 was in contact with the sprayed area of the test sample 13 10 times was observed, and the repelling rate (%) was obtained by the above formula (1). In addition, when the test specimen 11 contacted the test specimen 13, it was counted as a repelling action that the test specimen 11 made a U-turn by dragging the half body or did not touch the test specimen 13.
The average value of the repellent rate (%) obtained for the test insects 11 of each size was determined, and the results are shown in Table 3.

  From the results of Table 3, the rosemary oil extract (fourth fraction component) of the present invention in Examples 2 to 4 has a high repellent effect even at a low concentration of 0.05 to 0.2% by mass. I understood that.

<Repellent test 3>
(Preparation of test sample: Example 5)
The carrier (kaolin, manufactured by Zhenjiang Ryu Kinka Kogyo Co., Ltd., 100 g) was impregnated so that the rosemary oil extract (100% extract) of the prepared fourth fraction component was 0.2% by mass.

(Test method)
As shown in FIG. 1, the test specimen 13 was sprayed in a width of about 3 cm on a substantially central portion in the width direction of a sheet 5 (made of polypropylene) having a length of 25 cm and a width of 35 cm (application amount of the preparation: 20 g / m ² ). . This was accommodated in a transparent glass case 17 having an opening of 25 cm in length, 35 cm in width, and 15 cm in height to prepare a test box.
After leaving the test box for a day, put one test insect 11 (centipede) of 3 cm, 6 cm and 10 cm in length on the sheet 15 and at the same time put it on a plastic cup with a diameter of 11 cm and a height of 10 cm so as not to move. After being allowed to acclimatize for about 5 minutes, the plastic cup was removed and left in the glass case.
The behavior when the test insect 11 was in contact with the sprayed area of the test sample 13 10 times was observed, and the repelling rate (%) was obtained by the above formula (1). In addition, when the test specimen 11 contacted the test specimen 13, it was counted as a repelling action that the test specimen 11 made a U-turn by dragging the half body or did not touch the test specimen 13.
The average value of the repellent rate (%) obtained for the test insects 11 of each size was determined, and the results are shown in Table 4.
Subsequently, the test box was left for 1 month and the same experiment was conducted after 1 month to obtain the average value of the repelling rate (%). The results are shown in Table 4.

  From the results of Table 4, the preparation loaded with the rosemary oil extract of the present invention of Example 5 (fourth fraction component) showed 100% repellent against centipede even after 1 day and 1 month of treatment, It was found to have a high repellent effect.

<Repellent test 4>
(Production of test sample: Example 6, Comparative Examples 4 to 6)
Using the prepared rosemary oil extract (100% extract), farnesyl acetone, lavender oil, and mint oil as the fourth fraction components, 100 mL of a 0.2% acetone solution was prepared. After impregnating this with a cotton cloth (length 35 mm × width 35 mm × thickness 0.2 mm), acetone was completely vaporized by air drying.

(Test method)
As shown in FIG. 2, a first black paper sheet 25 (90 mm × 90 mm) is placed in the center of a glass petri dish 21 having a diameter of 15 cm and a height of 1 cm. And two cotton cloths 33 (length 35 mm × width 35 mm × thickness 0.2 mm, specimen non-treated section) were installed at two locations diagonally. Then, a second black paper sheet 27 (20 mm × 20 mm) was placed at the center of each of the test specimen 31 and the cotton cloth 33, and 5 mg of a new dry medium 29 prepared as follows was placed at the center. Then, mites cultured in a dry medium prepared as follows were placed together with the medium (tick medium) 23 in the vicinity of the center of each side of the first black paper sheet 25. The amount of the mite medium 23 was adjusted so that there were about 200 to 300 mites moving in the test area.
<Preparation of dry medium>
MF powdered feed for mouse breeding (made by Oriental Yeast Co., Ltd.) was crushed, and a mixture of powdered yeast Ybios (made by Asahi Beer Co., Ltd.) mixed at 1: 1 with a 80-mesh sieve was heat-treated. Thereafter, it was sufficiently dried and cooled to room temperature. Then, it preserve | saved all day and night with 75% RH (saturated salt solution and distilled water use), and adjusted the moisture content to 12 to 13%.

After setting the mite medium 23, the mite was left for 24 hours, the mites on the second black paper sheet 27 gathered in the dry medium 29 were counted, and the repellent rate (%) was obtained by the following formula (2). The test was repeated twice and the average was determined. The results are shown in Table 5.
Repellent rate% = (number of ticks gathered in untreated section−number of ticks gathered in treated section) / number of ticks gathered in untreated section (2)

  From the results of Table 5, it was found that the rosemary oil extract of the present invention of Example 6 exhibited a high repellent effect against mites, and had a significant repellent effect compared to Comparative Examples 4-6. .

11 Test insects (centipede)
13 Test specimen 15 Sheet 17 Glass case 21 Glass petri dish 23 Tick medium 25 First black paper sheet 27 Second black paper sheet 29 Drying medium 31 Test specimen (sample treatment section)
33 Cotton (specimen untreated section)

Claims (3)

A repellent of at least one of multipods and mites,
Using chromatography, a column in which rosemary oil is adsorbed to an adsorbent is used as a developing solvent, hexane or a mixed solvent of hexane / diethyl ether containing hexane or a volume ratio of hexane to diethyl ether in a volume ratio. After elution, the residue contains a rosemary oil extract eluted with a mixed solvent of hexane / diethyl ether containing more diethyl ether than hexane in a volume ratio as an active ingredient. Repellent. From the column in which the rosemary oil is adsorbed on an adsorbent,
(A) a step of eluting the first fraction component using hexane as a developing solvent;
(B) From the residue obtained by collecting the first fraction component, the second fraction component using a mixed solvent of hexane: hexane / diethyl ether mixed solvent (hexane: diethyl ether (4: 1)) = 1: 1 as a developing solvent. Elution step,
(C) a step of eluting the third fraction component from the residue obtained by collecting the second fraction component using a mixed solvent of hexane: diethyl ether = 1: 1 as a developing solvent;
(D) Rose of the fourth fraction component obtained by the step of eluting the fourth fraction component from the residue obtained by collecting the third fraction component using a mixed solvent of hexane: diethyl ether = 1: 4 as a developing solvent. 2. A repellent according to claim 1, comprising a mary oil extract as an active ingredient.   3. The repellent according to claim 1, wherein the polypod is at least one selected from centipedes, millipedes, geese, waraimushi and dandelion. 3.

Images