WO2019117164A1 - Metered-spray aerosol, method for spraying metered-spray aerosol, and method for improving effect of chemical agent - Google Patents

Metered-spray aerosol, method for spraying metered-spray aerosol, and method for improving effect of chemical agent Download PDF

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Publication number
WO2019117164A1
WO2019117164A1 PCT/JP2018/045553 JP2018045553W WO2019117164A1 WO 2019117164 A1 WO2019117164 A1 WO 2019117164A1 JP 2018045553 W JP2018045553 W JP 2018045553W WO 2019117164 A1 WO2019117164 A1 WO 2019117164A1
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WIPO (PCT)
Prior art keywords
injection
aerosol
fixed
amount
stock solution
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PCT/JP2018/045553
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French (fr)
Japanese (ja)
Inventor
優八 鈴木
練 阿部
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アース製薬株式会社
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Application filed by アース製薬株式会社 filed Critical アース製薬株式会社
Priority to JP2019559670A priority Critical patent/JP7548698B2/en
Priority to CN201880080331.7A priority patent/CN111465564A/en
Publication of WO2019117164A1 publication Critical patent/WO2019117164A1/en
Priority to PH12020550851A priority patent/PH12020550851A1/en
Priority to JP2021213170A priority patent/JP7518058B2/en
Priority to JP2022115746A priority patent/JP2022140536A/en
Priority to JP2024051966A priority patent/JP2024071611A/en

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01M—CATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
    • A01M7/00—Special adaptations or arrangements of liquid-spraying apparatus for purposes covered by this subclass
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06—Aerosols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B9/00—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
    • B05B9/03—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material
    • B05B9/04—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D83/00—Containers or packages with special means for dispensing contents
    • B65D83/14—Containers or packages with special means for dispensing contents for delivery of liquid or semi-liquid contents by internal gaseous pressure, i.e. aerosol containers comprising propellant for a product delivered by a propellant
    • B65D83/44—Valves specially adapted therefor; Regulating devices
    • B65D83/52—Valves specially adapted therefor; Regulating devices for metering
    • B65D83/54—Metering valves ; Metering valve assemblies

Definitions

  • the present invention relates to a metered-dose aerosol, a jetting method using the same, and a method for improving the efficacy of a drug that is discharged when a metered-dose aerosol is jetted.
  • a fixed quantity injection type aerosol which injects a fixed amount of an aerosol composition consisting of a stock solution containing a drug as an active ingredient and a propellant in a single injection operation.
  • the fixed injection type aerosol discharges a predetermined amount of medicine in a single injection operation, so it is difficult for the user to make a difference in the operation method (difference between the depression method of the injection button and the injection amount due to the depression time).
  • the variation is small.
  • Patent Document 1 discloses a pest control aerosol provided with an aerosol valve for fixed amount spraying having a spray volume of 0.35 to 0.9 mL per time. There is.
  • fixed injection aerosols for use in spaces such as insecticide aerosols and fragrance aerosols have the advantage of less variation in their effects, but when the injection amount per shot is small, the feeling of use is sufficient Although it could not be obtained, although the effective amount of the medicine was discharged by one injection, it could be injected several times and consumed excessively.
  • the conventional fixed injection aerosol there is a limit to the duration of the effect of the drug, and in order to continue this effect, the injection operation has to be repeated after a predetermined time has elapsed from the injection, and the frequency is high. Then, this invention aims at providing the fixed quantity jet type aerosol which improves the efficacy of a medicine, improves the persistence of the effect, and can obtain feeling of use.
  • the present invention is characterized by the following (1) to (8).
  • a quantitative injection type aerosol that injects a fixed amount of aerosol composition in a single injection operation, wherein the aerosol composition comprises an undiluted solution containing a drug and a propellant, and is filled in a pressure resistant container,
  • the fixed jet aerosol is a fixed jet aerosol having an injection volume of 1.0 to 3.0 mL and an injection time of 0.8 seconds or less.
  • the quantitative spray aerosol according to any one of the above (1) to (3) wherein the content of the drug is 0.01 to 70% by mass / volume in the stock solution.
  • the drug is at least one selected from the group consisting of a pest control component, an aroma component, a deodorizing component, and a disinfecting / disinfecting component. Metered jet aerosol as described.
  • the injection amount is 1.0 to 3.0 mL and the injection time per one injection operation using a fixed amount injection type aerosol filled with an aerosol composition consisting of a stock solution containing a drug and a propellant in a pressure resistant container
  • the injection method of the fixed injection type aerosol which jets so that it becomes within 0.8 seconds.
  • the aerosol composition can be mass-sprayed in a predetermined amount in the range of 1.0 to 3.0 mL in one injection operation, and furthermore, the drug in the aerosol composition Sustainability of the effects of Therefore, since the difference in the operation method by a user does not arise, there is no dispersion
  • FIG. 1 is a plan view for explaining a test chamber used in Test Example 1.
  • FIG. 2 is a perspective view for explaining the test method of Test Example 2.
  • FIG. 3 is a plan view for explaining the test chamber used in Test Example 4.
  • weight is synonymous with “weight”.
  • the fixed jet aerosol according to the present invention is formed by filling an aerosol composition containing a drug-containing stock solution and a propellant in a pressure container.
  • an aerosol composition containing a drug-containing stock solution and a propellant in a pressure container.
  • stock solution which comprises the aerosol composition of this invention contains the chemical
  • the active ingredient refers to one that exerts some action when using a quantitative injection type aerosol, and is not particularly limited, and examples thereof include pest control ingredients, aroma ingredients, deodorant ingredients, disinfecting and disinfecting ingredients, etc. .
  • the pest control component is a component capable of killing, repelling, knocking down, etc. the target pest.
  • the type of pest control component is not particularly limited, and known compounds can be used.
  • Pest controlling ingredients include, for example, permethrin, pyrethrin, allethrin, phthalthrin, resmethrin, flamothrin, phenothrin, empentrin, Mostethrin, cifenothrin, imiprothrin, transfluthrin, metfluthrin, dimefluthrin, mepafluthrin, pyrethroid compounds such as fenitrothion, dichlorvos, Organophosphorus compounds such as chlorpyrifos methyl, diazinone and fenthion; Carbamate compounds such as carbaryl and propoxur; Compounds such as methoprene, pyriproxyfen, methoxadiazon, fipronil, amidoflumetho, brofuran
  • the pest control component may be appropriately selected according to the type of the target pest.
  • the target pests include, for example, mosquitoes, flies, moths, bees, bugs, roaches, cockroaches, ants, spiders, snails, ticks, lice, centipedes, caterpillars, worms, spiders, spiders, flies, blowfish, butterfly flies, termites, insects, stick beetles, beetles , Beetles, earwigs, stains, longhorn beetles, cutworms, spinybees, liga, koiga and the like.
  • Transfluthrin, methofluthrin, profluthrin, phthalthrin, prarethrin, monfluorothrin, etc. are suitable for flying pests such as mosquitoes, flies, moths, bees, flies, bush flies, leafhoppers, butterfly flies, iga and koiga .
  • phthalthrin, praretrin imiprothrin, permethrin, Phenothrin is preferred.
  • the aroma component is a component that emits an aroma.
  • the fragrant component for example, natural perfumes such as anise oil, lavender oil, rose oil, rosemary oil, grapefruit oil and the like in addition to the above-mentioned essential oil components; camphene, p-cymene, citronellol, nerol, benzyl alcohol, n- Synthetic perfumes such as butyraldehyde, isobutyraldehyde, coumarin, cineole, etc. may be mentioned. One of these may be used alone, or two or more may be used in combination.
  • the deodorizing component is a component capable of eliminating the odor.
  • a deodorant component for example, a component which adsorbs an odor component such as green tea extract, tannin, lauryl methacrylate, methyl benzoate, methyl phenylacetate, geranyl crolate, acetophenone myristate, benzyl acetate, benzyl propionate, silver and the like And components which mask off odorous components such as the above-mentioned aroma components.
  • an odor component such as green tea extract, tannin, lauryl methacrylate, methyl benzoate, methyl phenylacetate, geranyl crolate, acetophenone myristate, benzyl acetate, benzyl propionate, silver and the like
  • components which mask off odorous components such as the above-mentioned aroma components.
  • One of these may be used alone, or two or more may be used in combination.
  • the germicidal and bactericidal component is a component that removes or kills microorganisms, molds and bacteria.
  • Examples of the germicidal and bactericidal components include ethanol, hinokitiol, 2-mercaptobenzothiazole, 2- (4-thiazolyl) benzimidazole, 5-chloro-2-methyl-4-isothiazolin-3-one, trifolin, p- Chlorometaxylenol, 3-methyl-4-isopropylphenol, ortho-phenylphenol, chlorhexidine gluconate, polylysine, chitosan, tetrahydrolinalol, dialkyldimethyl ammonium chloride and the like can be mentioned. One of these may be used alone, or two or more may be used in combination.
  • the agents described above can be used in combination with components having different effects.
  • the pest control component and the aroma component can be used in combination, or the aroma component and the deodorizing component other than the aroma component can be used in combination.
  • the stock solution may contain a solvent for the purpose of adjusting the viscosity of the stock solution, improving the production suitability, and increasing the permeability of the drug to pests.
  • solvents include the above-described glycol ethers, hydrocarbon solvents, alcohol solvents, aromatic solvents, ester solvents and the like.
  • water and surfactants can be used.
  • hydrocarbon solvents include aliphatic hydrocarbons such as paraffinic hydrocarbons and naphthenic hydrocarbons, and alicyclic hydrocarbons. Kerosenes such as JIS No. 1 kerosene are preferable. Specific examples include normal paraffin, isoparaffin and the like.
  • the normal paraffin is typically one having 8 to 16 carbon atoms, and examples thereof include neothiozole manufactured by Chuo Kasei Co., Ltd., normal paraffin MA manufactured by JXTG Energy Co., Ltd., and the like.
  • isoparaffins those having 8 to 16 carbon atoms are representative, and examples thereof include IP Clean LX and Super Sol FP 25 manufactured by Idemitsu Kosan Co., Ltd.
  • the alcohol solvents include lower alcohols such as ethanol and propanol (normal and iso), polyhydric alcohols such as glycerin and ethylene glycol, and the like.
  • the aromatic solvents include toluene and xylene.
  • ester solvents include isopropyl myristate, hexyl laurate, isopropyl palmitate and the like.
  • the content of the solvent is preferably 30 to 99.99% by mass / volume in the stock solution.
  • the lower limit of the content of the solvent is preferably 35% by mass or more, more preferably 50% by mass or more, and the upper limit is preferably 99.9% by mass or less, and 99.5% by mass. It is further preferable that the ratio is not more than volume%.
  • stock solution can be made to contain other components in the range which does not impair the effect of this invention.
  • other components for example, preservatives, pH adjusters, ultraviolet absorbers, inorganic substances, surfactants, solubilizers and the like can be mentioned.
  • the content of the undiluted solution in the aerosol composition can be appropriately changed depending on the purpose of the fixed jet aerosol and the combination with the propellant, and is not particularly limited. For example, 1 to 50% by volume in the aerosol composition It can be done. If the stock solution in the aerosol composition is 1% by volume or more, sufficient drug effects can be obtained, and if it is 50% by volume or less, the stock solution can be sprayed as spray particles, for example, used indoors In this case, it is possible to reduce the contamination of furniture, floors, walls, etc. by the undiluted solution.
  • the lower limit of the undiluted solution content is preferably 3% by volume or more, more preferably 5% by volume or more, and the upper limit is more preferably 40% by volume or less, and 30% by volume The following are more preferable.
  • the propellant is a medium for injecting the above-mentioned stock solution, and is pressure-filled in the pressure container together with the stock solution.
  • the propellant for example, liquefied petroleum gas (LPG) such as propane, propylene, n-butane, isobutane or the like, liquefied gas such as dimethyl ether (DME), carbon dioxide gas, nitrogen gas, compressed gas such as compressed air, HFC-152a
  • LPG liquefied petroleum gas
  • DME dimethyl ether
  • carbon dioxide gas such as dimethyl ether
  • nitrogen gas such as compressed air
  • HFC-152a One or more kinds of halogenated carbon gases such as HFC-134a, HFO-1234yf and HFO-1234ze can be used.
  • the propellant to be used may be appropriately selected in accordance with the compatibility with the stock solution and the container member such as the aerosol valve.
  • the content of the propellant in the aerosol composition can be appropriately changed according to the purpose of use of the quantitative injection aerosol and the combination with the stock solution, and is not particularly limited. For example, 50 to 99% by volume in the aerosol composition It can be done. If the amount of the propellant in the aerosol composition is 50% by volume or more, the stock solution can be jetted as spray particles, whereby the drug is more easily diffused, and the effect of the drug is easily sustained. In addition, when the amount of the propellant is 99% by volume or less, a sufficient drug effect can be obtained.
  • the lower limit of the content of the propellant in the aerosol composition is preferably 60% by volume or more, more preferably 70% by volume or more, and the upper limit is more preferably 97% by volume or less, and 95% by volume or less More preferable.
  • the volume ratio of the undiluted solution to the propellant in the aerosol composition is preferably 1:99 to 50:50, more preferably 3:97 to 40:60, and still more preferably 5:95 to 30:70. . With such a volume ratio, a sufficient drug effect can be obtained.
  • the fixed jet aerosol according to the present invention is constituted by filling the above-mentioned stock solution and propellant in a pressure container for aerosol, and closing the opening of the pressure container by the aerosol valve.
  • fixed injection type aerosol is aerosol which injects a certain amount of aerosol composition by one injection operation.
  • an aerosol composition (undiluted solution and propellant in the pressure resistant container) passes through the aerosol valve by the user operating the injection member attached to the aerosol valve (hereinafter also referred to as the injection button).
  • a certain amount is injected, and the stock solution is made into particles by a propellant and injected as spray particles.
  • the aerosol valve has an opening and closing member for switching communication between the inside and the outside of the pressure resistant container and the outside when the injection member is operated by the user, a housing to which the opening and closing member is attached, and the housing at a predetermined position of the pressure resistant container. It has a mounting member for holding.
  • the opening and closing member includes a stem that slides up and down in conjunction with the injection member. The sliding of the stem switches the communication (injection state) and shutoff (non-injection state) of the aerosol composition.
  • the aerosol valve is formed with a housing hole for taking in the aerosol composition from the pressure container and a stem hole for sending the taken-in aerosol composition to the injection member.
  • the housing is formed with a housing hole for taking in the aerosol composition from the pressure container.
  • the stem is formed with a stem hole for delivering the aerosol composition taken into the housing to the spray member.
  • the path from the housing bore to the stem bore constitutes an internal passage through which the aerosol composition passes.
  • the aerosol valve is an aerosol valve of a metering type, which is jetted quantitatively by operating the jetting member once.
  • the injection amount of the aerosol valve is a predetermined constant amount in the range of 1.0 to 3.0 mL in one injection operation.
  • the injection member is a member attached to the pressure resistant container via the aerosol valve.
  • the injection button is formed with a passage in the operation portion through which the aerosol composition taken in from the pressure resistant container passes through the stem hole of the aerosol valve and a nozzle hole from which the aerosol composition is injected.
  • the inner diameter (injection hole diameter) of the injection port of the injection button is preferably ⁇ 0.45 to 3.0 mm, more preferably ⁇ 0.5 to 2.0 mm, and ⁇ 0. 6 to 1.6 mm is more preferable. Moreover, there is no problem even if it has a plurality of injection ports having the same area as these.
  • the metered-dose aerosol of the present invention is filled with the undiluted solution and the propellant, ie, the aerosol composition, in the pressure container for aerosol as described above, and the aerosol button is pressed to press the injection button. Is injected.
  • the injection pressure of the aerosol composition at a position 20 cm away from the injection port is preferably 5 to 40 gf, more preferably 8 to 30 gf.
  • the injection time can be made into a desired range because injection pressure is the said range.
  • the injection pressure is a digital force gauge (for example, manufactured by Imada Co., Ltd., model number: DS2-2N), which is placed sideways at a distance of 20 cm from the injection port of the fixed injection type aerosol under room temperature conditions of 25 ° C.
  • the maximum value when the aerosol composition is jetted toward the center of the circular flat plate with a diameter of 60 mm mounted on the surface of the disc can be used as the jet load, and the average can be calculated.
  • the injection time per one injection operation is within 0.8 seconds.
  • the reason why the effects of the present invention can be obtained is not clear, but by injecting an aerosol composition having a predetermined injection amount in a range of 1.0 to 3.0 mL per injection within 0.8 seconds, Since the volatilization of the drug can be efficiently enhanced, the efficacy of the drug can be enhanced, and the sustainability of the effect is considered to be enhanced.
  • the injection time per injection operation is preferably within 0.75 seconds, more preferably 0.10 to 0.75 seconds, further preferably 0.20 to 0.75 seconds, and 0.25 to 0. Particularly preferred is .75 seconds.
  • a method of adjusting the injection time by one injection operation for example, a method of adjusting the size of the injection port of the injection button, a method of adjusting the injection pressure of fixed injection type aerosol, stem hole diameter of an aerosol valve , A method of adjusting the pressure of the propellant, and a combination thereof.
  • the metered dose aerosol of the present invention by injecting a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds, Efficacy can be improved, thus enhancing the persistence of the effect of the drug.
  • Example 1 Insecticidal Efficacy Test on Culex pipiens> 1. Preparation of stock solution According to the formulation shown in Table 1, transfluthrin was measured, and isopropanol (specific gravity 0.785 (20 ° C.)) was added to make up to 100 mL, to prepare stock solutions 1 to 3.
  • Example 1 12.8 mL of undiluted solution 1 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem hole area 1.4 mm 2 ). Subsequently, 187.2 mL of pressurized liquefied petroleum gas (0.49 MPa (25 ° C.)) was loaded as a propellant. The injection button (injection hole diameter ⁇ 1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of transfluthrin was 16 mg of a fixed injection aerosol.
  • Example 2 In the same manner as in Example 1 except that the injection button was changed to the injection hole diameter ⁇ 0.6 mm, a fixed amount injection aerosol having an injection amount of 1.0 mL per push and a discharge amount of transfluthrin of 16 mg was obtained .
  • Example 3 In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.5 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
  • Example 4 In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.28 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
  • Example 2 In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.13 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
  • Example 5 12.8 mL of undiluted solution 2 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (one injection amount: 2.2 mL, stem hole area: 1.4 mm 2 ). Subsequently, 187.2 mL of pressurized liquefied petroleum gas (0.49 MPa (25 ° C.)) was loaded as a propellant. A jet button (injection hole diameter: ⁇ 1.6 mm) was attached to the aerosol valve, and a jet volume of 2.2 mL per push and a discharge volume of transfluthrin of 16 mg was obtained.
  • a laser light diffraction type particle size measurement device (Microtrac Bell Co., Ltd. “LDSA-1400A”) is installed at a position 5 cm away in a straight line in the injection direction (horizontal direction) from the injection port of the fixed injection type aerosol. And the laser light is made to strike from the direction perpendicular to the direction of ejection.
  • the jet button was operated once (1 push) to jet the video. The moving image was reproduced, and the longest continuous time at which the laser beam was turned on by the spray particles was measured in 0.01 second units.
  • the injection button of the fixed injection type aerosol was operated once (1 push) toward the central area A at an angle of 45 degrees diagonally higher than the height of 1 m from the floor of the corner B.
  • the time until knockdown of Culex pipiens (falling down and immobilizing) was measured, and KT50 (minute) (the time required for knocking down 50% of Culex pipiens) was determined by the Probit method.
  • the test was performed three times and the average was determined. The results are shown in Table 3.
  • a cage (a 25-cm ⁇ 25-cm 16 mesh gauge folded in half and stapled around by a stapler to prepare a tubular shape) containing 10 red house mosquitoes was prepared.
  • the fixed injection aerosol is directed toward the central part A at an angle of 45 degrees above the floor of the corner B of the test room 10 of 8 tatami spaces (volume 31.1 m 3 ) and 1 m from the height was operated once (1 push).
  • Examples 1 to 4 and Comparative Examples 1 to 2 are examples in which the injection amount per push is 1 mL and the hole diameter of the injection hole of the injection button or the area of the stem hole is changed. In comparison, the average of KT50 was remarkably short, and in Examples 3 and 4, the average of KT50 was significantly shorter than that of Comparative Example 2.
  • Example 5 and Comparative Example 3 are examples in which the injection hole diameter of the injection button is changed with the injection amount per push set to 2.2 mL, but Example 5 has a significantly shorter average of KT 50 compared to Comparative Example 3.
  • Comparative Examples 4 and 5 are examples in which the injection amount per push is 0.2 mL, in Comparative Examples 4 and 5, even after 3 hours of injection, the average of KT 50 is the same regardless of the injection time. Met. From these results, it was found that the drug durability changes depending on the injection time in the case of a large-scale jettable fixed injection aerosol of 1.0 mL or more.
  • ⁇ Test Example 2 Insecticidal efficacy confirmation test against cockroach> 1.
  • Preparation of stock solution Measure 0.5 g of imiprotoline and 10 g of isopropyl myristate and add kerosene No. 1 (normal paraffin, "Neothiozole” manufactured by Chuo Kasei Co., Ltd., carbon number 11-15, specific gravity 0.761 (15 ° C))
  • the stock solution 4 was prepared by measuring up to 100 mL.
  • Example 6 46 mL of the stock solution 4 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem area: 1.4 mm 2 ). Subsequently, 154 mL of dimethyl ether (DME) as a propellant was pressure-filled. An injection button (injection hole diameter ⁇ 1.6 mm) was attached to the aerosol valve, and a fixed amount injection aerosol with an injection amount of 1.0 mL per push and a discharge amount of imiprotorin of 1.2 mg was obtained.
  • DME dimethyl ether
  • Example 7 In the same manner as in Example 6 except that the injection button was changed to one having an injection hole diameter of 0.6 mm, a fixed injection aerosol with an injection amount of 1.0 mL per push and an ejection amount of imiprotorin of 1.2 mg was obtained .
  • Example 6 In the same manner as in Example 6 except that the injection button was changed to one having an injection hole diameter of 0.4 mm, a fixed injection aerosol having an injection amount of 1.0 mL per push and an ejection amount of imiprotorin of 1.2 mg was obtained. .
  • Example 8 In the same manner as in Example 6 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.5 mm 2 , the injection amount per push was 1.0 mL and the discharge amount of imiprotorin was A fixed dose aerosol of 1.2 mg was obtained.
  • Example 9 In the same manner as in Example 6 except that the aerosol valve was changed to an injection amount of 1.0 mL once and a stem hole area of 0.28 mm 2 , the injection amount per push was 1.0 mL and the discharge amount of imiproline was A fixed dose aerosol of 1.2 mg was obtained.
  • Example 7 In the same manner as in Example 6 except that the aerosol valve was changed to an injection amount of 1.0 mL once and a stem hole area of 0.13 mm 2 , the injection amount per push was 1.0 mL, and the discharge amount of imiproline was A fixed dose aerosol of 1.2 mg was obtained.
  • a cylinder 2 (diameter ⁇ 50 cm, height 15 cm) made of vinyl chloride was placed on the floor on which the filter paper 1 was laid, and the inside was used as a test zone. Calcium carbonate was applied to the inner side wall of the cylinder 2 so that the test insect could not crawl up. A position on the filter paper 1 in the test area, close to the inner sidewall of the cylinder 2, was marked as the target point 3 of the jet.
  • Examples 6 to 7 and Comparative Example 6 are examples in which the injection hole diameter of the injection button is changed in a fixed injection type aerosol having an injection amount of 1 mL per push, and Examples 8 to 9 and Comparative Example 7 are stem holes. This is an example in which the area is changed. From the results of Table 6, in Examples 6 and 7 in which the injection time is 0.3 seconds and 0.73 seconds, the knock-down time of the black-necked roach is noticeably compared to Comparative Example 6 in which the injection time is 1.36 seconds. In Examples 8 and 9, which are short and the injection time is 0.58 seconds and 0.73 seconds, it is found that the knock-down time of the black-necked roach is remarkably short as compared with Comparative Example 7 whose injection time is 1.2 seconds. The
  • Example 3 Insecticidal efficacy confirmation test on house fly> 1. Preparation of undiluted solution Measure 1.4 g of phthalthrin, add No. 1 kerosene (normal paraffin, "Neothiosol” manufactured by Chuo Kasei Co., Ltd., carbon number 11-15, specific gravity 0.761 (15 ° C)), and measure up to 100 mL. The stock solution 5 was prepared by
  • Example 10 40 mL of the stock solution 5 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem area: 1.4 mm 2 ). Subsequently, 160 mL of pressurized liquefied petroleum gas (0.29 MPa (25 ° C.)) was injected as a propellant. The injection button (injection hole diameter ⁇ 1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of phthalthrin was 2.8 mg.
  • Example 11 In the same manner as in Example 10 except that the injection button was changed to the injection hole diameter ⁇ 0.6 mm, a fixed amount injection aerosol with an injection amount per push of 1.0 mL and a phthalthrin discharge amount of 2.8 mg was obtained .
  • Test Example 4 Aroma efficacy check test 1. Preparation of stock solution 0.5 g of linalool was measured, and absolute ethanol (specific gravity 0.785 (25 ° C.)) was added to make up to 100 mL, to prepare stock solution 6.
  • Example 12 40 mL of undiluted solution 6 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem hole area 1.4 mm 2 ). Subsequently, 160 mL of pressurized liquefied petroleum gas (0.29 MPa (25 ° C.)) was injected as a propellant. The injection button (injection hole diameter ⁇ 1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of Lina Roll was 1.0 mg.
  • Aroma sensory test (sensory evaluation after 10 seconds of spraying) As shown in FIG. 3, it faces the first wall 21 substantially horizontally to the floor surface from a height of 100 cm from the floor of the central position F of the first wall 21 of the test room 20 of six tatami mat space (volume 25 m 3 )
  • the injection button of the constant injection aerosol was operated once (one push) toward the third wall 23. 10 seconds after the injection, the central position F of the first wall 21 which is the injection position, the central position G of the second wall 22 orthogonal to the first wall 21, and the third wall facing the first wall 21 Standing at the central position H of 23 and the odor intensity was evaluated according to the evaluation criteria of the 6-step odor intensity display method.
  • Example 12 in which the injection time is 0.31 seconds is excellent in spread and intensity of the aroma after 30 minutes as compared with Comparative Example 9 in which the injection time is 1.35 seconds, and 30 minutes. It turned out that the persistence of the aroma is excellent even after the lapse.
  • ⁇ Test Example 5 Bactericidal efficacy confirmation test> 1. Preparation of stock solution 20 g of isopropylmethylphenol (IPMP) was measured, and 99.5% ethanol (specific gravity 0.785 (25 ° C.)) was added to make up to 100 mL to prepare stock solution 7.
  • IPMP isopropylmethylphenol

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Abstract

The present invention addresses the problem of providing a metered-spray aerosol in which the durability of a chemical agent is increased and the effect thereof is improved. This metered-spray aerosol sprays a fixed amount of an aerosol composition in one use of a spray operation, wherein the aerosol composition comprises a chemical-agent-containing raw liquid and a spraying agent, the aerosol composition fills a pressure-resistant container, and the metered-spray aerosol has a spray amount of 1.0-3.0 mL per use and a spray time of 0.8 seconds or less per use.

Description

定量噴射型エアゾール、定量噴射型エアゾールの噴射方法及び薬剤の効力向上方法Metered spray type aerosol, jet type of metered spray type aerosol and method of improving efficacy of medicine
　本発明は、定量噴射型エアゾール、及びこれを用いた噴射方法、並びに定量噴射型エアゾールを噴射した際に吐出される薬剤の効力を向上させる方法に関する。 TECHNICAL FIELD The present invention relates to a metered-dose aerosol, a jetting method using the same, and a method for improving the efficacy of a drug that is discharged when a metered-dose aerosol is jetted.
　有効成分となる薬剤が含有された原液と噴射剤とからなるエアゾール組成物を１回の噴射操作で一定量噴射する定量噴射型エアゾールが知られている。定量噴射型エアゾールは１回の噴射操作で所定量の薬剤が吐出されるので、使用者による操作方法の差（噴射ボタンの押し下げ方法や押し下げ時間による噴射量等の差）が生じにくく、効果のバラツキが少ないという利点がある。 A fixed quantity injection type aerosol is known which injects a fixed amount of an aerosol composition consisting of a stock solution containing a drug as an active ingredient and a propellant in a single injection operation. The fixed injection type aerosol discharges a predetermined amount of medicine in a single injection operation, so it is difficult for the user to make a difference in the operation method (difference between the depression method of the injection button and the injection amount due to the depression time). There is an advantage that the variation is small.
　このような定量噴射型エアゾールとしては、例えば、特許文献１には、１回当たりの噴霧容量が０．３５～０．９ｍＬである定量噴霧用エアゾールバルブを備えた害虫防除用エアゾールが開示されている。 As such a quantitative injection type aerosol, for example, Patent Document 1 discloses a pest control aerosol provided with an aerosol valve for fixed amount spraying having a spray volume of 0.35 to 0.9 mL per time. There is.
日本国特開２０１０－２８０６３３号公報Japanese Unexamined Patent Publication No. 2010-280633
　殺虫剤エアゾールや芳香剤エアゾール等の空間に使用するための定量噴射型エアゾールは、上記したように効果のバラツキが少ないという利点があるが、１回当たりの噴射量が少ないと使用実感が十分に得られず、１回噴射により有効量の薬剤が吐出されているにもかかわらず複数回噴射してしまい過剰に消費してしまうことがあった。また、従来の定量噴射型エアゾールでは薬剤の効果の持続に限度があり、この効果を継続させるために噴射から一定時間経過後に噴射操作を繰り返さなければならず、その頻度が高かった。
　そこで、本発明は、薬剤の効力を向上させてその効果の持続性を高め、使用実感が得られる定量噴射型エアゾールを提供することを目的とする。 As described above, fixed injection aerosols for use in spaces such as insecticide aerosols and fragrance aerosols have the advantage of less variation in their effects, but when the injection amount per shot is small, the feeling of use is sufficient Although it could not be obtained, although the effective amount of the medicine was discharged by one injection, it could be injected several times and consumed excessively. In addition, in the conventional fixed injection aerosol, there is a limit to the duration of the effect of the drug, and in order to continue this effect, the injection operation has to be repeated after a predetermined time has elapsed from the injection, and the frequency is high.
Then, this invention aims at providing the fixed quantity jet type aerosol which improves the efficacy of a medicine, improves the persistence of the effect, and can obtain feeling of use.
　本発明者らは鋭意検討を重ねた結果、１．０ｍＬ以上の大量噴射が可能な定量噴射型エアゾールとすれば１回の噴射操作による噴射量が多くなるため使用実感を高めつつ薬剤の吐出量も多くすることができ、さらに、大量噴射する定量噴射型エアゾールでは１回の噴射操作による噴射時間により薬剤の効果の持続性が変化すること、そして１回の噴射操作当たりのエアゾール組成物の噴射量と噴射時間には薬剤の効果を持続させる最適なバランスがあることを見出した。 As a result of intensive investigations by the present inventors, if a quantitative injection type aerosol capable of large-scale injection of 1.0 mL or more is used, the injection amount per injection operation increases, and therefore the discharge amount of the drug while enhancing the feeling of use In the case of a large amount of injected fixed injection aerosol, the duration of the effect of the drug changes with the injection time per injection operation, and the injection of aerosol composition per injection operation is also possible. We found that the amount and the injection time had the best balance to sustain the effect of the drug.
　すなわち、本発明は以下の（１）～（８）を特徴とする。
（１）１回の噴射操作で一定量のエアゾール組成物を噴射する定量噴射型エアゾールであって、前記エアゾール組成物は薬剤を含む原液と噴射剤とからなり、耐圧容器に充填されており、前記定量噴射型エアゾールは、１回の噴射量が１．０～３．０ｍＬであり、且つ１回の噴射時間が０．８秒以内である定量噴射型エアゾール。
（２）前記１回の噴射時間が、０．２０～０．７５秒である、前記（１）に記載の定量噴射型エアゾール。
（３）前記原液がさらに溶剤を含む、前記（１）又は（２）に記載の定量噴射型エアゾール。
（４）前記薬剤の含有量が、前記原液中０．０１～７０質量／容量％である、前記（１）～（３）のいずれか１つに記載の定量噴射型エアゾール。
（５）前記エアゾール組成物中の前記原液と前記噴射剤の体積比が、１：９９～５０：５０である、前記（１）～（４）のいずれか１つに記載の定量噴射型エアゾール。
（６）前記薬剤が、害虫防除成分、芳香成分、消臭成分及び除菌・殺菌成分からなる群から選択される少なくとも１種である、前記（１）～（５）のいずれか１つに記載の定量噴射型エアゾール。
（７）耐圧容器に薬剤を含む原液と噴射剤とからなるエアゾール組成物が充填された定量噴射型エアゾールを用いて、１回の噴射操作で噴射量が１．０～３．０ｍＬ且つ噴射時間が０．８秒以内となるように噴射する定量噴射型エアゾールの噴射方法。
（８）定量噴射型エアゾールを用いて噴射されるエアゾール組成物中の薬剤の効力を向上させる方法であって、１．０～３．０ｍＬの範囲にある前記エアゾール組成物の一定量を、０．８秒以内に噴射する薬剤の効力向上方法。 That is, the present invention is characterized by the following (1) to (8).
(1) A quantitative injection type aerosol that injects a fixed amount of aerosol composition in a single injection operation, wherein the aerosol composition comprises an undiluted solution containing a drug and a propellant, and is filled in a pressure resistant container, The fixed jet aerosol is a fixed jet aerosol having an injection volume of 1.0 to 3.0 mL and an injection time of 0.8 seconds or less.
(2) The fixed jet aerosol according to (1), wherein the one injection time is 0.20 to 0.75 second.
(3) The fixed jet according to (1) or (2), wherein the stock solution further contains a solvent.
(4) The quantitative spray aerosol according to any one of the above (1) to (3), wherein the content of the drug is 0.01 to 70% by mass / volume in the stock solution.
(5) The quantitative spray aerosol according to any one of (1) to (4), wherein the volume ratio of the undiluted solution to the propellant in the aerosol composition is 1:99 to 50:50. .
(6) In any one of the above (1) to (5), the drug is at least one selected from the group consisting of a pest control component, an aroma component, a deodorizing component, and a disinfecting / disinfecting component. Metered jet aerosol as described.
(7) The injection amount is 1.0 to 3.0 mL and the injection time per one injection operation using a fixed amount injection type aerosol filled with an aerosol composition consisting of a stock solution containing a drug and a propellant in a pressure resistant container The injection method of the fixed injection type aerosol which jets so that it becomes within 0.8 seconds.
(8) A method for improving the efficacy of a drug in an aerosol composition to be jetted using a metered jet aerosol, wherein the fixed quantity of the aerosol composition in the range of 1.0 to 3.0 mL is . A method to improve the efficacy of drugs injected within 8 seconds.
　本発明の定量噴射型エアゾールによれば、エアゾール組成物を、１回の噴射操作により１．０～３．０ｍＬの範囲にある所定量で大量噴射することができ、さらにエアゾール組成物中の薬剤の効果の持続性を高めることができる。よって、使用者による操作方法の差が生じないため効果のバラツキがなく、無駄な過剰使用を回避できるとともに、１回の噴射操作で薬剤の効果を持続させることができる。 According to the metered-dose aerosol of the present invention, the aerosol composition can be mass-sprayed in a predetermined amount in the range of 1.0 to 3.0 mL in one injection operation, and furthermore, the drug in the aerosol composition Sustainability of the effects of Therefore, since the difference in the operation method by a user does not arise, there is no dispersion | variation of an effect, and while being able to avoid useless excessive use, the effect of a chemical | medical agent can be maintained by one injection operation.
図１は、試験例１で使用した試験室を説明するための平面図である。FIG. 1 is a plan view for explaining a test chamber used in Test Example 1. 図２は、試験例２の試験方法を説明するための斜視図である。FIG. 2 is a perspective view for explaining the test method of Test Example 2. 図３は、試験例４で使用した試験室を説明するための平面図である。FIG. 3 is a plan view for explaining the test chamber used in Test Example 4.
　以下、本発明の実施形態についてさらに詳しく説明する。
　なお、本明細書において、「質量」は「重量」と同義である。 Hereinafter, embodiments of the present invention will be described in more detail.
In the present specification, “mass” is synonymous with “weight”.
　本発明の定量噴射型エアゾールは、薬剤を含む原液と噴射剤とを含むエアゾール組成物が耐圧容器に充填されてなる。以下、各成分について説明する。 The fixed jet aerosol according to the present invention is formed by filling an aerosol composition containing a drug-containing stock solution and a propellant in a pressure container. Each component will be described below.
（原液）
　本発明のエアゾール組成物を構成する原液は、少なくとも有効成分である薬剤を含有する。有効成分とは、定量噴射型エアゾールを使用した時に、何らかの作用を発揮するものを言い、特に限定されないが、例えば、害虫防除成分、芳香成分、消臭成分、除菌・殺菌成分等が挙げられる。 (Stock solution)
The undiluted | stock solution which comprises the aerosol composition of this invention contains the chemical | medical agent which is an active ingredient at least. The active ingredient refers to one that exerts some action when using a quantitative injection type aerosol, and is not particularly limited, and examples thereof include pest control ingredients, aroma ingredients, deodorant ingredients, disinfecting and disinfecting ingredients, etc. .
　害虫防除成分は、対象害虫を殺虫、忌避、ノックダウン等することができる成分である。害虫防除成分の種類は、特に限定されず、公知の化合物を使用できる。
　害虫防除成分としては、例えば、ペルメトリン、ピレトリン、アレスリン、フタルスリン、レスメトリン、フラメトリン、フェノトリン、エムペントリン、プラレトリン、シフェノトリン、イミプロトリン、トランスフルトリン、メトフルトリン、ジメフルトリン、メパフルトリン等のピレスロイド系化合物；フェニトロチオン、ジクロルボス、クロルピリホスメチル、ダイアジノン、フェンチオン等の有機リン系化合物；カルバリル、プロポクスル等のカーバメイト系化合物；メトプレン、ピリプロキシフェン、メトキサジアゾン、フィプロニル、アミドフルメト、ブロフラニリド等の化合物；ハッカ油、オレンジ油、ウイキョウ油、ケイヒ油、チョウジ油、テレビン油、ユーカリ油、ヒバ油、ジャスミン油、ネロリ油、ペパーミント油、ベルガモット油、ブチグレン油、レモン油、レモングラス油、シナモン油、シトロネラ油、ゼラニウム油、シトラール、ｌ－メントール、酢酸シトロネリル、シンナミックアルデヒド、テルピネオール、ノニルアルコール、ｃｉｓ－ジャスモン、リモネン、リナロール、１，８－シネオール、ゲラニオール、α－ピネン、ｐ－メンタン－３，８－ジオール、オイゲノール、酢酸メンチル、チモール、安息香酸ベンジル、サリチル酸ベンジル等の各種精油成分；プロピレングリコールモノプロピルエーテル、プロピレングリコールモノブチルエーテル、ジプロピレングリコールモノプロピルエーテル、ジプロピレングリコールモノブチルエーテル、ジプロピレングリコールジメチルエーテル、エチレングリコールモノイソブチルエーテル、ジエチレングリコールモノイソブチルエーテル、ジエチレングリコールジブチルエーテル、ジエチレングリコールジメチルエーテル、トリエチレングリコールジメチルエーテル等のグリコールエーテル類；アジピン酸ジブチル等の二塩基酸エステル類等が挙げられる。これらは、１種を単独で使用してもよく、２種以上を組み合わせて使用してもよい。 The pest control component is a component capable of killing, repelling, knocking down, etc. the target pest. The type of pest control component is not particularly limited, and known compounds can be used.
Pest controlling ingredients include, for example, permethrin, pyrethrin, allethrin, phthalthrin, resmethrin, flamothrin, phenothrin, empentrin, praguethrin, cifenothrin, imiprothrin, transfluthrin, metfluthrin, dimefluthrin, mepafluthrin, pyrethroid compounds such as fenitrothion, dichlorvos, Organophosphorus compounds such as chlorpyrifos methyl, diazinone and fenthion; Carbamate compounds such as carbaryl and propoxur; Compounds such as methoprene, pyriproxyfen, methoxadiazon, fipronil, amidoflumetho, brofuranilide and the like; peppermint oil, orange oil, fennel oil, caffeine oil , Clove oil, turpentine oil, eucalyptus oil, hiba oil, jasmine oil, neroli oil, peppermint oil, Rugamotto oil, Butyglen oil, Lemon oil, Lemongrass oil, Cinnamon oil, Citronella oil, Geranium oil, Citral, l-menthol, Citronellol acetate, Cinnamic aldehyde, Terpineol, Nonyl alcohol, cis-Jasmone, limonene, linalool, 1, Various essential oil components such as 8-cineole, geraniol, α-pinene, p-menthane-3,8-diol, eugenol, menthyl acetate, thymol, benzyl benzoate, benzyl salicylate, etc .; propylene glycol monopropyl ether, propylene glycol monobutyl ether, Dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, dipropylene glycol dimethyl ether, ethylene glycol monoisobutyl ether, diethyl Glycol ethers such as glycol monoisobutyl ether, diethylene glycol dibutyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether; dibasic acid esters such as dibutyl adipate and the like. One of these may be used alone, or two or more may be used in combination.
　なお、害虫防除成分は、対象害虫の種類に合わせて適宜選択すればよい。対象害虫としては、例えば、蚊、ハエ、ガ、ハチ、カメムシ、ゴキブリ、アリ、クモ、ダンゴムシ、ダニ、シラミ、ムカデ、ケムシ、ヤスデ、クモ、アブ、ブユ、チョウバエ、シロアリ、ユスリカ、ヨコバイ、キクイムシ、ゴミムシ、ハサミムシ、シミ、カミキリムシ、カツオブシムシ、チャタテムシ、イガ、コイガ等が挙げられる。
　蚊、ハエ、ガ、ハチ、アブ、ブユ、ユスリカ、ヨコバイ、チョウバエ、イガ、コイガ等の飛翔害虫に対しては、トランスフルトリン、メトフルトリン、プロフルトリン、フタルスリン、プラレトリン、モンフルオロトリン等が好適である。また、ゴキブリ、カメムシ、アリ、クモ、ダンゴムシ、ダニ、シラミ、ムカデ、ケムシ、ヤスデ、クモ、シロアリ、キクイムシ、ゴミムシ、ハサミムシ、シミ等の匍匐害虫に対しては、フタルスリン、プラレトリン、イミプロトリン、ペルメトリン、フェノトリン等が好適である。 The pest control component may be appropriately selected according to the type of the target pest. The target pests include, for example, mosquitoes, flies, moths, bees, bugs, roaches, cockroaches, ants, spiders, snails, ticks, lice, centipedes, caterpillars, worms, spiders, spiders, flies, blowfish, butterfly flies, termites, insects, stick beetles, beetles , Beetles, earwigs, stains, longhorn beetles, cutworms, spinybees, liga, koiga and the like.
Transfluthrin, methofluthrin, profluthrin, phthalthrin, prarethrin, monfluorothrin, etc. are suitable for flying pests such as mosquitoes, flies, moths, bees, flies, bush flies, leafhoppers, butterfly flies, iga and koiga . In addition, against insect pests such as cockroaches, bugs, ants, spiders, spider gums, mites, lice, centipedes, worms, stamens, spiders, termites, bark beetles, caterpillars, earwigs, stains, etc., phthalthrin, praretrin, imiprothrin, permethrin, Phenothrin is preferred.
　芳香成分は、香気を発する成分である。芳香成分としては、例えば、上記した精油成分の他に、アニス油、ラベンダー油、ローズ油、ローズマリー油、グレープフルーツ油等の天然香料；カンフェン、ｐ－シメン、シトロネロール、ネロール、ベンジルアルコール、ｎ－ブチルアルデヒド、イソブチルアルデヒド、クマリン、シネオール等の合成香料等が挙げられる。これらは、１種を単独で使用してもよく、２種以上を組み合わせて使用してもよい。 The aroma component is a component that emits an aroma. As the fragrant component, for example, natural perfumes such as anise oil, lavender oil, rose oil, rosemary oil, grapefruit oil and the like in addition to the above-mentioned essential oil components; camphene, p-cymene, citronellol, nerol, benzyl alcohol, n- Synthetic perfumes such as butyraldehyde, isobutyraldehyde, coumarin, cineole, etc. may be mentioned. One of these may be used alone, or two or more may be used in combination.
　消臭成分は、臭気を消すことができる成分である。消臭成分としては、例えば、緑茶エキス、柿タンニン、ラウリル酸メタクリレート、安息香酸メチル、フェニル酢酸メチル、ゲラニルクロトレート、ミリスチン酸アセトフェノン、酢酸ベンジル、プロピオン酸ベンジル、銀等の臭気成分を吸着する成分や、上記した芳香成分のような臭気成分をマスキングする成分等が挙げられる。これらは、１種を単独で使用してもよく、２種以上を組み合わせて使用してもよい。 The deodorizing component is a component capable of eliminating the odor. As a deodorant component, for example, a component which adsorbs an odor component such as green tea extract, tannin, lauryl methacrylate, methyl benzoate, methyl phenylacetate, geranyl crolate, acetophenone myristate, benzyl acetate, benzyl propionate, silver and the like And components which mask off odorous components such as the above-mentioned aroma components. One of these may be used alone, or two or more may be used in combination.
　除菌・殺菌成分は、微生物、カビ、細菌を除去又は死滅させる成分である。除菌・殺菌成分としては、例えば、エタノール、ヒノキチオール、２－メルカプトベンゾチアゾール、２－（４－チアゾリル）ベンゾイミダゾール、５－クロロ－２－メチル－４－イソチアゾリン－３－オン、トリホリン、ｐ－クロロメタキシレノール、３－メチル－４－イソプロピルフェノール、オルト－フェニルフェノール、グルコン酸クロルヘキシジン、ポリリジンやキトサン、テトラヒドロリナロール、ジアルキルジメチルアンモニウムクロライド等が挙げられる。これらは、１種を単独で使用してもよく、２種以上を組み合わせて使用してもよい。 The germicidal and bactericidal component is a component that removes or kills microorganisms, molds and bacteria. Examples of the germicidal and bactericidal components include ethanol, hinokitiol, 2-mercaptobenzothiazole, 2- (4-thiazolyl) benzimidazole, 5-chloro-2-methyl-4-isothiazolin-3-one, trifolin, p- Chlorometaxylenol, 3-methyl-4-isopropylphenol, ortho-phenylphenol, chlorhexidine gluconate, polylysine, chitosan, tetrahydrolinalol, dialkyldimethyl ammonium chloride and the like can be mentioned. One of these may be used alone, or two or more may be used in combination.
　上記した薬剤は、効果の異なる成分同士を組み合わせて使用することができる。例えば、害虫防除成分と芳香成分を組み合わせて使用することや、芳香成分と芳香成分以外の消臭成分を組み合せて使用することができる。 The agents described above can be used in combination with components having different effects. For example, the pest control component and the aroma component can be used in combination, or the aroma component and the deodorizing component other than the aroma component can be used in combination.
　薬剤の含有量は、原液中０．０１～７０質量／容量％であることが好ましい。薬剤が原液中に０．０１質量／容量％以上であることで、十分な薬剤の効果を得ることができ、７０質量／容量％以下であると生産適性が向上される。薬剤の含有量は、下限は０．１質量／容量％以上であることがより好ましく、０．３質量／容量％以上がさらに好ましく、０．５質量／容量％以上が特に好ましく、また上限は６５質量／容量％以下がより好ましく、５０質量／容量％以下がさらに好ましく、２５質量／容量％以下が特に好ましい。 The content of the drug is preferably 0.01 to 70% by mass / volume in the stock solution. When the amount of the drug in the stock solution is 0.01% by mass / volume or more, a sufficient effect of the agent can be obtained, and when it is 70% by mass or less, the production suitability is improved. The lower limit of the content of the drug is more preferably 0.1% by mass or more, still more preferably 0.3% by mass or more, and particularly preferably 0.5% by mass or more, and the upper limit is more preferably 65 mass / vol% or less is more preferable, 50 mass / vol% or less is more preferable, and 25 mass / vol% or less is particularly preferable.
　原液には、原液の粘度を調整するためや、生産適性を向上させるため、害虫に対する薬剤の浸透性を上げるため等の目的のために溶剤を含有することができる。このような溶剤としては、例えば、上記したグリコールエーテル類や、炭化水素系溶剤、アルコール系溶剤、芳香族系溶剤、エステル系溶剤等が挙げられる。また、水や界面活性剤の使用もできる。
　炭化水素系溶剤としては、例えば、パラフィン系炭化水素やナフテン系炭化水素等の脂肪族炭化水素及び脂環式炭化水素が挙げられ、ＪＩＳ　１号灯油等の灯油が好ましい。具体的にはノルマルパラフィン、イソパラフィン等が挙げられる。ノルマルパラフィンとしては、炭素数が８～１６のものが代表的で、例えば、中央化成株式会社製のネオチオゾール、ＪＸＴＧエネルギー株式会社製のノルマルパラフィンＭＡ等が挙げられる。イソパラフィンとしては、炭素数が８～１６のものが代表的で、例えば、出光興産株式会社製のＩＰクリーンＬＸ、スーパーゾルＦＰ２５等が挙げられる。
　アルコール系溶剤としては、例えば、エタノール、プロパノール（ノルマル、イソ）等の低級アルコール、グリセリン、エチレングリコール等の多価アルコール等が挙げられる。
　芳香族系溶剤としては、例えば、トルエン、キシレン等が挙げられる。
　エステル系溶剤としては、例えば、ミリスチン酸イソプロピル、ラウリン酸ヘキシル、パルミチン酸イソプロピル等が挙げられる。 The stock solution may contain a solvent for the purpose of adjusting the viscosity of the stock solution, improving the production suitability, and increasing the permeability of the drug to pests. Examples of such solvents include the above-described glycol ethers, hydrocarbon solvents, alcohol solvents, aromatic solvents, ester solvents and the like. Also, water and surfactants can be used.
Examples of hydrocarbon solvents include aliphatic hydrocarbons such as paraffinic hydrocarbons and naphthenic hydrocarbons, and alicyclic hydrocarbons. Kerosenes such as JIS No. 1 kerosene are preferable. Specific examples include normal paraffin, isoparaffin and the like. The normal paraffin is typically one having 8 to 16 carbon atoms, and examples thereof include neothiozole manufactured by Chuo Kasei Co., Ltd., normal paraffin MA manufactured by JXTG Energy Co., Ltd., and the like. As isoparaffins, those having 8 to 16 carbon atoms are representative, and examples thereof include IP Clean LX and Super Sol FP 25 manufactured by Idemitsu Kosan Co., Ltd.
Examples of the alcohol solvents include lower alcohols such as ethanol and propanol (normal and iso), polyhydric alcohols such as glycerin and ethylene glycol, and the like.
Examples of the aromatic solvents include toluene and xylene.
Examples of ester solvents include isopropyl myristate, hexyl laurate, isopropyl palmitate and the like.
　溶剤の含有量は、原液中３０～９９．９９質量／容量％であることが好ましい。溶剤が原液中に３０質量／容量％以上であることで、生産適性を向上させることができ、９９．９９質量／容量％以下であると、十分な薬剤の効果を担保できるため好ましい。溶剤の含有量は、下限は３５質量／容量％以上であることがより好ましく、５０質量／容量％以上がさらに好ましく、また上限は９９．９質量／容量％以下がより好ましく、９９．５質量／容量％以下がさらに好ましい。 The content of the solvent is preferably 30 to 99.99% by mass / volume in the stock solution. When the solvent is 30% by mass or more in the stock solution, the production suitability can be improved, and when it is 99.99% by mass or less, a sufficient effect of the drug can be secured, which is preferable. The lower limit of the content of the solvent is preferably 35% by mass or more, more preferably 50% by mass or more, and the upper limit is preferably 99.9% by mass or less, and 99.5% by mass. It is further preferable that the ratio is not more than volume%.
　原液には、本発明の効果を損なわない範囲で、その他の成分を含有させることができる。その他の成分としては、例えば、防腐剤、ｐＨ調整剤、紫外線吸収剤、無機物、界面活性剤、溶解助剤等が挙げられる。 The undiluted | stock solution can be made to contain other components in the range which does not impair the effect of this invention. As other components, for example, preservatives, pH adjusters, ultraviolet absorbers, inorganic substances, surfactants, solubilizers and the like can be mentioned.
　エアゾール組成物中の原液の含有量は、定量噴射型エアゾールの使用目的や噴射剤との組み合わせに応じて適宜変更可能であり、特に限定されないが、例えば、エアゾール組成物中に１～５０容量％とすることができる。エアゾール組成物中に原液が１容量％以上であると、十分な薬剤の効果を得ることができ、５０容量％以下であると、原液を噴霧粒子として噴射することができるので、例えば室内で使用した場合に、原液による家具、床、壁等の汚染を少なくできる。原液の含有量は、エアゾール組成物中、下限は３容量％以上であることがより好ましく、５容量％以上がさらに好ましく、また、上限は４０容量％以下であることがより好ましく、３０容量％以下がさらに好ましい。 The content of the undiluted solution in the aerosol composition can be appropriately changed depending on the purpose of the fixed jet aerosol and the combination with the propellant, and is not particularly limited. For example, 1 to 50% by volume in the aerosol composition It can be done. If the stock solution in the aerosol composition is 1% by volume or more, sufficient drug effects can be obtained, and if it is 50% by volume or less, the stock solution can be sprayed as spray particles, for example, used indoors In this case, it is possible to reduce the contamination of furniture, floors, walls, etc. by the undiluted solution. In the aerosol composition, the lower limit of the undiluted solution content is preferably 3% by volume or more, more preferably 5% by volume or more, and the upper limit is more preferably 40% by volume or less, and 30% by volume The following are more preferable.
（噴射剤）
　噴射剤は、上記原液を噴射するための媒体であり、原液とともに耐圧容器に加圧充填される。
　噴射剤としては、例えば、プロパン、プロピレン、ｎ－ブタン、イソブタン等の液化石油ガス（ＬＰＧ）やジメチルエーテル（ＤＭＥ）等の液化ガス、炭酸ガス、窒素ガス、圧縮空気等の圧縮ガス、ＨＦＣ－１５２ａ、ＨＦＣ－１３４ａ、ＨＦＯ－１２３４ｙｆ、ＨＦＯ－１２３４ｚｅ等のハロゲン化炭素ガス等の１種又は２種以上を用いることができる。使用する噴射剤は、原液との相溶性やエアゾールバルブ等の容器部材に合わせて適宜選択すればよい。 (Propellant)
The propellant is a medium for injecting the above-mentioned stock solution, and is pressure-filled in the pressure container together with the stock solution.
As the propellant, for example, liquefied petroleum gas (LPG) such as propane, propylene, n-butane, isobutane or the like, liquefied gas such as dimethyl ether (DME), carbon dioxide gas, nitrogen gas, compressed gas such as compressed air, HFC-152a One or more kinds of halogenated carbon gases such as HFC-134a, HFO-1234yf and HFO-1234ze can be used. The propellant to be used may be appropriately selected in accordance with the compatibility with the stock solution and the container member such as the aerosol valve.
　エアゾール組成物中の噴射剤の含有量は、定量噴射型エアゾールの使用目的や原液との組み合わせに応じて適宜変更可能であり、特に限定されないが、例えば、エアゾール組成物中に５０～９９容量％とすることができる。エアゾール組成物中に噴射剤が５０容量％以上であると、原液を噴霧粒子として噴射することができるため薬剤がより拡散しやすくなり、薬剤の効果が持続しやすくなる。また、噴射剤が９９容量％以下であると、十分な薬剤の効果を得ることができる。噴射剤の含有量は、エアゾール組成物中、下限は６０容量％以上であることがより好ましく、７０容量％以上がさらに好ましく、また、上限は９７容量％以下がより好ましく、９５容量％以下がさらに好ましい。 The content of the propellant in the aerosol composition can be appropriately changed according to the purpose of use of the quantitative injection aerosol and the combination with the stock solution, and is not particularly limited. For example, 50 to 99% by volume in the aerosol composition It can be done. If the amount of the propellant in the aerosol composition is 50% by volume or more, the stock solution can be jetted as spray particles, whereby the drug is more easily diffused, and the effect of the drug is easily sustained. In addition, when the amount of the propellant is 99% by volume or less, a sufficient drug effect can be obtained. The lower limit of the content of the propellant in the aerosol composition is preferably 60% by volume or more, more preferably 70% by volume or more, and the upper limit is more preferably 97% by volume or less, and 95% by volume or less More preferable.
　なお、エアゾール組成物中の原液と噴射剤の体積比は、１：９９～５０：５０であることが好ましく、３：９７～４０：６０がより好ましく、５：９５～３０：７０がさらに好ましい。このような体積比とすることで、十分な薬剤の効果を得ることができる。 The volume ratio of the undiluted solution to the propellant in the aerosol composition is preferably 1:99 to 50:50, more preferably 3:97 to 40:60, and still more preferably 5:95 to 30:70. . With such a volume ratio, a sufficient drug effect can be obtained.
（定量噴射型エアゾール）
　本発明の定量噴射型エアゾールは、上記した原液と噴射剤がエアゾール用の耐圧容器に充填され、該耐圧容器がエアゾールバルブによりその開口を閉止されることにより構成される。 (Quantitative injection type aerosol)
The fixed jet aerosol according to the present invention is constituted by filling the above-mentioned stock solution and propellant in a pressure container for aerosol, and closing the opening of the pressure container by the aerosol valve.
　なお、定量噴射型エアゾールとは、１回の噴射操作で一定量のエアゾール組成物を噴射するエアゾールである。定量噴射型エアゾールは、エアゾールバルブに取り付けられた噴射部材（以下、噴射ボタンともいう。）が使用者に操作されることにより、エアゾールバルブを通って耐圧容器内のエアゾール組成物（原液と噴射剤）の一定量が噴射され、原液は噴射剤によって粒子状とされて噴霧粒子として噴射される。 In addition, fixed injection type aerosol is aerosol which injects a certain amount of aerosol composition by one injection operation. In the fixed injection type aerosol, an aerosol composition (undiluted solution and propellant in the pressure resistant container) passes through the aerosol valve by the user operating the injection member attached to the aerosol valve (hereinafter also referred to as the injection button). A certain amount is injected, and the stock solution is made into particles by a propellant and injected as spray particles.
（エアゾールバルブ）
　エアゾールバルブは、噴射部材が使用者に操作されることにより耐圧容器内と外部との連通および遮断を切り替えるための開閉部材と、開閉部材が取り付けられるハウジングと、ハウジングを耐圧容器の所定の位置に保持するためのマウント部材を備える。また、開閉部材は、噴射部材と連動して上下に摺動するステムを含む。ステムの摺動によりエアゾール組成物の連通（噴射状態）および遮断（非噴射状態）が切り替えられる。エアゾールバルブには、耐圧容器からエアゾール組成物を取り込むためのハウジング孔と、取り込まれたエアゾール組成物を噴射部材に送るためのステム孔とが形成されている。ハウジングには、耐圧容器からエアゾール組成物を取り込むためのハウジング孔が形成されている。ステムには、ハウジング内に取り込まれたエアゾール組成物を噴射部材に送るためのステム孔が形成されている。ハウジング孔からステム孔までの経路は、エアゾール組成物が通過する内部通路を構成する。 (Aerosol valve)
The aerosol valve has an opening and closing member for switching communication between the inside and the outside of the pressure resistant container and the outside when the injection member is operated by the user, a housing to which the opening and closing member is attached, and the housing at a predetermined position of the pressure resistant container. It has a mounting member for holding. In addition, the opening and closing member includes a stem that slides up and down in conjunction with the injection member. The sliding of the stem switches the communication (injection state) and shutoff (non-injection state) of the aerosol composition. The aerosol valve is formed with a housing hole for taking in the aerosol composition from the pressure container and a stem hole for sending the taken-in aerosol composition to the injection member. The housing is formed with a housing hole for taking in the aerosol composition from the pressure container. The stem is formed with a stem hole for delivering the aerosol composition taken into the housing to the spray member. The path from the housing bore to the stem bore constitutes an internal passage through which the aerosol composition passes.
　本発明において、エアゾールバルブは、噴射部材を１回操作することで定量噴射される定量型のエアゾールバルブである。エアゾールバルブの噴射量は、１回の噴射操作で１．０～３．０ｍＬの範囲の所定の一定量とされている。１回当たりの噴射量が１．０～３．０ｍＬの範囲の所定量となるエアゾール組成物を貯留できるハウジングを有するエアゾールバルブを用いることで、１回の噴射操作により１．０～３．０ｍＬの範囲の所定の一定量を噴射することができ、薬剤の大量噴射が可能となる。エアゾールバルブの噴射量は、前記範囲であれば所定の噴射量を適宜設定することができる。 In the present invention, the aerosol valve is an aerosol valve of a metering type, which is jetted quantitatively by operating the jetting member once. The injection amount of the aerosol valve is a predetermined constant amount in the range of 1.0 to 3.0 mL in one injection operation. By using an aerosol valve having a housing capable of storing an aerosol composition having a predetermined injection amount in the range of 1.0 to 3.0 mL per injection, 1.0 to 3.0 mL in one injection operation It is possible to inject a predetermined constant amount in the range of (1), allowing mass injection of medicine. If the injection amount of the aerosol valve is in the above range, a predetermined injection amount can be set appropriately.
（噴射部材）
　噴射部材（噴射ボタン）は、エアゾールバルブを介して耐圧容器に取り付けられる部材である。噴射ボタンには、エアゾールバルブのステム孔を介して耐圧容器から取り込まれるエアゾール組成物が通過する操作部内通路とエアゾール組成物が噴射される噴口が形成されている。 (Jecting member)
The injection member (injection button) is a member attached to the pressure resistant container via the aerosol valve. The injection button is formed with a passage in the operation portion through which the aerosol composition taken in from the pressure resistant container passes through the stem hole of the aerosol valve and a nozzle hole from which the aerosol composition is injected.
　噴射ボタンの噴口の内径（噴口孔径）は、噴射時間を所望の範囲とするという観点から、φ０．４５～３．０ｍｍであることが好ましく、φ０．５～２．０ｍｍがより好ましく、φ０．６～１．６ｍｍがさらに好ましい。また、これらと等しい面積を有する複数の噴口を有していても問題ない。 The inner diameter (injection hole diameter) of the injection port of the injection button is preferably φ0.45 to 3.0 mm, more preferably φ0.5 to 2.0 mm, and φ0. 6 to 1.6 mm is more preferable. Moreover, there is no problem even if it has a plurality of injection ports having the same area as these.
（噴射圧）
　本発明の定量噴射型エアゾールは、上記したようにエアゾール用耐圧容器に原液と噴射剤、すなわちエアゾール組成物が充填され、噴射ボタンを押圧することにより、１回の押圧によって一定量のエアゾール組成物が噴射される。噴口から２０ｃｍ離れた位置におけるエアゾール組成物の噴射圧は、５～４０ｇｆであることが好ましく、８～３０ｇｆがより好ましい。噴射圧が前記範囲であることで、噴射時間を所望の範囲とすることができる。
　なお、前記噴射圧は、２５℃の室温条件下で、定量噴射型エアゾールの噴口から２０ｃｍの距離を置いたところに横倒しにしたデジタルフォースゲージ（例えば、株式会社イマダ製、型番：ＤＳ２－２Ｎ）に装着した直径φ６０ｍｍの円状の平板の中心に向かってエアゾール組成物を噴射した際の最大値を噴射荷重とし、平均を算出することにより測定できる。 (Injection pressure)
As described above, the metered-dose aerosol of the present invention is filled with the undiluted solution and the propellant, ie, the aerosol composition, in the pressure container for aerosol as described above, and the aerosol button is pressed to press the injection button. Is injected. The injection pressure of the aerosol composition at a position 20 cm away from the injection port is preferably 5 to 40 gf, more preferably 8 to 30 gf. The injection time can be made into a desired range because injection pressure is the said range.
The injection pressure is a digital force gauge (for example, manufactured by Imada Co., Ltd., model number: DS2-2N), which is placed sideways at a distance of 20 cm from the injection port of the fixed injection type aerosol under room temperature conditions of 25 ° C. The maximum value when the aerosol composition is jetted toward the center of the circular flat plate with a diameter of 60 mm mounted on the surface of the disc can be used as the jet load, and the average can be calculated.
（噴射時間）
　本発明の定量噴射型エアゾールは、１回の噴射操作による噴射時間が０．８秒以内である。本発明の効果が得られる理由は定かではないが、１回当たりの噴射量が１．０～３．０ｍＬの範囲の所定量であるエアゾール組成物を０．８秒以内で噴射させることにより、薬剤の揮散性を効率良く高めることができるため、薬剤の効力を向上させることができ、その効果の持続性が高まると考えられる。
　１回の噴射操作による噴射時間は、０．７５秒以内であることが好ましく、０．１０～０．７５秒がより好ましく、０．２０～０．７５秒がさらに好ましく、０．２５～０．７５秒が特に好ましい。 (Injection time)
In the fixed injection aerosol of the present invention, the injection time per one injection operation is within 0.8 seconds. The reason why the effects of the present invention can be obtained is not clear, but by injecting an aerosol composition having a predetermined injection amount in a range of 1.0 to 3.0 mL per injection within 0.8 seconds, Since the volatilization of the drug can be efficiently enhanced, the efficacy of the drug can be enhanced, and the sustainability of the effect is considered to be enhanced.
The injection time per injection operation is preferably within 0.75 seconds, more preferably 0.10 to 0.75 seconds, further preferably 0.20 to 0.75 seconds, and 0.25 to 0. Particularly preferred is .75 seconds.
　本発明において、１回の噴射操作による噴射時間を調整する方法としては、例えば、噴射ボタンの噴口の大きさを調整する方法、定量噴射型エアゾールの噴射圧を調整する方法、エアゾールバルブのステム孔径を調整する方法、噴射剤の圧力を調整する方法、及びこれらの組み合せ等が挙げられる。 In the present invention, as a method of adjusting the injection time by one injection operation, for example, a method of adjusting the size of the injection port of the injection button, a method of adjusting the injection pressure of fixed injection type aerosol, stem hole diameter of an aerosol valve , A method of adjusting the pressure of the propellant, and a combination thereof.
　本発明の定量噴射型エアゾールを用いて、１．０～３．０ｍＬの範囲にあるエアゾール組成物の一定量を、０．８秒以内に噴射することで、噴射されたエアゾール組成物の薬剤の効力を向上させることができ、よって薬剤の効果の持続性を高めることができる。 Using the metered dose aerosol of the present invention, by injecting a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds, Efficacy can be improved, thus enhancing the persistence of the effect of the drug.
　以下、本発明を実施例及び比較例によりさらに説明するが、本発明は下記例に制限されるものではない。 Hereinafter, the present invention will be further described by way of examples and comparative examples, but the present invention is not limited to the following examples.
＜試験例１：アカイエカに対する殺虫効力確認試験＞
１．原液の調製
　表１に示す配合処方に従い、トランスフルトリンを測り取り、イソプロパノール（比重０．７８５（２０℃））を加えて１００ｍＬにまでメスアップすることにより、原液１～３を調製した。 <Test Example 1: Insecticidal Efficacy Test on Culex pipiens>
1. Preparation of stock solution According to the formulation shown in Table 1, transfluthrin was measured, and isopropanol (specific gravity 0.785 (20 ° C.)) was added to make up to 100 mL, to prepare stock solutions 1 to 3.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
２．定量噴射型エアゾールの作製
　表２に従い、実施例１～５、比較例１～５の定量噴射型エアゾールを作製した。 2. Preparation of fixed injection aerosol According to Table 2, fixed injection aerosols of Examples 1 to 5 and Comparative Examples 1 to 5 were manufactured.
（実施例１）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液１を１２．８ｍＬ充填し、エアゾールバルブ（１回噴射量１．０ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．４９ＭＰａ（２５℃））を１８７．２ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 Example 1
12.8 mL of undiluted solution 1 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem hole area 1.4 mm 2 ). Subsequently, 187.2 mL of pressurized liquefied petroleum gas (0.49 MPa (25 ° C.)) was loaded as a propellant.
The injection button (injection hole diameter φ1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of transfluthrin was 16 mg of a fixed injection aerosol.
（実施例２）
　噴射ボタンを噴口孔径φ０．６ｍｍのものに変更した以外は実施例１と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Example 2)
In the same manner as in Example 1 except that the injection button was changed to the injection hole diameter φ 0.6 mm, a fixed amount injection aerosol having an injection amount of 1.0 mL per push and a discharge amount of transfluthrin of 16 mg was obtained .
（比較例１）
　噴射ボタンを噴口孔径φ０．４ｍｍのものに変更した以外は実施例１と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Comparative example 1)
In the same manner as in Example 1 except that the injection button was changed to an injection hole diameter of φ 0.4 mm, an injection amount per push was 1.0 mL, and a discharge amount of transfluthrin was 16 mg. .
（実施例３）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．５ｍｍ２のものに変更した以外は実施例１と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Example 3)
In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.5 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
（実施例４）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．２８ｍｍ２のものに変更した以外は実施例１と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Example 4)
In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.28 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
（比較例２）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．１３ｍｍ２のものに変更した以外は実施例１と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Comparative example 2)
In the same manner as in Example 1 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.13 mm 2 , the injection amount per push was 1.0 mL and discharge of transfluthrin A dose of 16 mg was obtained.
（実施例５）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液２を１２．８ｍＬ充填し、エアゾールバルブ（１回噴射量２．２ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．４９ＭＰａ（２５℃））を１８７．２ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が２．２ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Example 5)
12.8 mL of undiluted solution 2 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (one injection amount: 2.2 mL, stem hole area: 1.4 mm 2 ). Subsequently, 187.2 mL of pressurized liquefied petroleum gas (0.49 MPa (25 ° C.)) was loaded as a propellant.
A jet button (injection hole diameter: φ1.6 mm) was attached to the aerosol valve, and a jet volume of 2.2 mL per push and a discharge volume of transfluthrin of 16 mg was obtained.
（比較例３）
　噴射ボタンを噴口孔径φ０．６ｍｍのものに変更した以外は実施例５と同様にして、１プッシュ当たりの噴射量が２．２ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Comparative example 3)
In the same manner as in Example 5 except that the injection button was changed to the injection hole diameter φ 0.6 mm, a quantitative injection aerosol having an injection amount of 2.2 mL per push and a discharge amount of transfluthrin of 16 mg was obtained .
（比較例４）
　エアゾール用耐圧缶（容量５９ｍＬ）に、原液３を３．２ｍＬ充填し、エアゾールバルブ（１回噴射量０．２ｍＬ、ステム孔面積０．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．４９ＭＰａ（２５℃））を１６．８ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ０．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が０．２ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Comparative example 4)
3.2 mL of undiluted solution 3 was filled in a pressure resistant can for aerosol (volume 59 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (injection volume 0.2 mL, stem hole area 0.4 mm 2 ). Subsequently, 16.8 mL of pressurized liquefied petroleum gas (0.49 MPa (25 ° C.)) was loaded as a propellant.
A jet button (injection hole diameter φ 0.6 mm) was attached to the aerosol valve, and a jet amount of 0.2 ml per push and a discharge amount of transfluthrin of 16 mg were obtained.
（比較例５）
　噴射ボタンを噴口孔径φ０．２３ｍｍのものに変更した以外は比較例４と同様にして、１プッシュ当たりの噴射量が０．２ｍＬ、トランスフルトリンの吐出量が１６ｍｇの定量噴射型エアゾールを得た。 (Comparative example 5)
In the same manner as in Comparative Example 4 except that the injection button was changed to the injection hole diameter φ 0.23 mm, the injection amount per push was 0.2 mL, and the discharge amount of transfluthrin was 16 mg. .
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
３．噴射時間の測定
　定量噴射型エアゾールの噴口から噴射方向（水平方向）に直線で５ｃｍ離れた位置に、レーザー光回析式粒度測定装置（マイクロトラック・ベル株式会社製「ＬＤＳＡ－１４００Ａ」）を設置し、噴射方向に対して垂直方向からレーザー光が当たるようにした。噴射ボタンを１回操作（１プッシュ）して噴射し、その動画を撮影した。動画を再生し、０．０１秒単位で、噴霧粒子によるレーザー光の点灯が確認できる最長の連続時間を測定した。なお、０．０５秒以内のレーザー光の点灯の途切れについては連続と判断し、０．０６秒以上のレーザー光が点灯しなかった時に測定を終了し、レーザー光が点灯していた最終の時間を測定時間とした。結果を表３、４それぞれに示す。 3. Measurement of injection time A laser light diffraction type particle size measurement device (Microtrac Bell Co., Ltd. “LDSA-1400A”) is installed at a position 5 cm away in a straight line in the injection direction (horizontal direction) from the injection port of the fixed injection type aerosol. And the laser light is made to strike from the direction perpendicular to the direction of ejection. The jet button was operated once (1 push) to jet the video. The moving image was reproduced, and the longest continuous time at which the laser beam was turned on by the spray particles was measured in 0.01 second units. In addition, it is judged as continuous about the interruption of lighting of the laser light within 0.05 seconds, and measurement is ended when the laser light of 0.06 seconds or more is not lighting, and the last time the laser light was on Was taken as the measurement time. The results are shown in Tables 3 and 4 respectively.
４．アカイエカに対する殺虫効力確認試験
（噴射直後の殺虫効力の確認）
　供試虫としてアカイエカ１０匹を入れたケージ（縦２５ｃｍ×横２５ｃｍの１６メッシュゲージを二つ折りにし、まわりをホッチキスで止めて筒状に作製したもの）を用意した。
　図１に示すように、８畳空間（容積３１．１ｍ３）の試験室１０の四隅（隅部Ｂ～Ｅ）の床（高さ０ｃｍ）と床から７５ｃｍの高さに、アカイエカを入れたケージを設置した。隅部Ｂの床から１ｍの高さより斜め上４５度の角度で中央部Ａに向けて、定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）した。アカイエカがノックダウンする（転倒して動けなくなる）までの時間を計測し、プロビット法によりＫＴ５０（分）（アカイエカの５割がノックダウンするのに要する時間）を求めた。試験は３回行い、平均を求めた。結果を表３に示す。 4. Insecticidal efficacy confirmation test against Culex pipiens (confirmation of insecticidal efficacy immediately after spraying)
As a test insect, a cage (a 25-cm × 25-cm 16 mesh gauge folded in half and stapled around by a stapler to prepare a tubular shape) containing 10 red house mosquitoes was prepared.
As shown in FIG. 1, Culex pipiens was placed on the floor (0 cm in height) of the four corners (corners B to E) of the test room 10 of 8 tatami spaces (volume 31.1 m 3 ) and at a height of 75 cm from the floor. I installed a cage. The injection button of the fixed injection type aerosol was operated once (1 push) toward the central area A at an angle of 45 degrees diagonally higher than the height of 1 m from the floor of the corner B. The time until knockdown of Culex pipiens (falling down and immobilizing) was measured, and KT50 (minute) (the time required for knocking down 50% of Culex pipiens) was determined by the Probit method. The test was performed three times and the average was determined. The results are shown in Table 3.
（噴射３時間後の殺虫効力の確認）
　供試虫としてアカイエカ１０匹を入れたケージ（縦２５ｃｍ×横２５ｃｍの１６メッシュゲージを二つ折りにし、まわりをホッチキスで止めて筒状に作製したもの）を用意した。
　図１に示すように、８畳空間（容積３１．１ｍ３）の試験室１０の隅部Ｂの床から１ｍの高さより斜め上４５度の角度で中央部Ａに向けて、定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）した。試験室１０を密閉状態にして放置し、３時間経過後にアカイエカを入れたケージを、試験室１０の四隅（隅部Ｂ～Ｅ）の床（高さ０ｃｍ）と床から７５ｃｍの高さに設置した。アカイエカがノックダウンするまでの時間を計測し、プロビット法によりＫＴ５０（分）を求めた。試験は３回行い、平均を求めた。結果を表４に示す。 (Confirmation of insecticidal efficacy 3 hours after injection)
As a test insect, a cage (a 25-cm × 25-cm 16 mesh gauge folded in half and stapled around by a stapler to prepare a tubular shape) containing 10 red house mosquitoes was prepared.
As shown in FIG. 1, the fixed injection aerosol is directed toward the central part A at an angle of 45 degrees above the floor of the corner B of the test room 10 of 8 tatami spaces (volume 31.1 m 3 ) and 1 m from the height Was operated once (1 push). Leave the test room 10 in a closed state, and after 3 hours, install a cage containing the green house mosquitoes at the four corners (corners B to E) of the test room 10 (height 0 cm) and 75 cm from the floor did. The time until knockdown of Culex pipiens was counted, and KT50 (minutes) was determined by the probit method. The test was performed three times and the average was determined. The results are shown in Table 4.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
　表３に示したように、噴射直後はいずれの定量噴射型エアゾールにおいてもＫＴ５０の平均が３分程度であった。これに対し、表４に示したように、噴射３時間後ではＫＴ５０の平均に差がみられた。実施例１～４及び比較例１～２は１プッシュあたりの噴射量を１ｍＬとして噴射ボタンの噴口孔径又はステム孔の面積を変化させた例であるが、実施例１、２は比較例１に比べてＫＴ５０の平均が顕著に短く、実施例３、４は比較例２に比べてＫＴ５０の平均が顕著に短かった。実施例５及び比較例３は１プッシュあたりの噴射量を２．２ｍＬとして噴射ボタンの噴口孔径を変化させた例であるが、実施例５は比較例３に比べてＫＴ５０の平均が顕著に短かった。なお、比較例４～５は１プッシュあたりの噴射量を０．２ｍＬとした例であるが、比較例４、５については、噴射３時間後においても噴射時間に関わらずＫＴ５０の平均は同程度であった。これらの結果から、１．０ｍＬ以上の大量噴射可能な定量噴射型エアゾールでは、噴射時間により薬剤の持続性が変化することが分かった。 As shown in Table 3, the average of KT50 was about 3 minutes in any of the fixed injection aerosols immediately after the injection. On the other hand, as shown in Table 4, a difference was found in the average of KT50 three hours after the injection. Examples 1 to 4 and Comparative Examples 1 to 2 are examples in which the injection amount per push is 1 mL and the hole diameter of the injection hole of the injection button or the area of the stem hole is changed. In comparison, the average of KT50 was remarkably short, and in Examples 3 and 4, the average of KT50 was significantly shorter than that of Comparative Example 2. Example 5 and Comparative Example 3 are examples in which the injection hole diameter of the injection button is changed with the injection amount per push set to 2.2 mL, but Example 5 has a significantly shorter average of KT 50 compared to Comparative Example 3. The Although Comparative Examples 4 and 5 are examples in which the injection amount per push is 0.2 mL, in Comparative Examples 4 and 5, even after 3 hours of injection, the average of KT 50 is the same regardless of the injection time. Met. From these results, it was found that the drug durability changes depending on the injection time in the case of a large-scale jettable fixed injection aerosol of 1.0 mL or more.
＜試験例２：ゴキブリに対する殺虫効力確認試験＞
１．原液の調製
　イミプロトリン０．５ｇ及びミリスチン酸イソプロピル１０ｇを測り取り、１号灯油（ノルマルパラフィン、中央化成株式会社製「ネオチオゾール」、炭素数１１～１５、比重０．７６１（１５℃））を加えて１００ｍＬにまでメスアップすることにより、原液４を調製した。 <Test Example 2: Insecticidal efficacy confirmation test against cockroach>
1. Preparation of stock solution Measure 0.5 g of imiprotoline and 10 g of isopropyl myristate and add kerosene No. 1 (normal paraffin, "Neothiozole" manufactured by Chuo Kasei Co., Ltd., carbon number 11-15, specific gravity 0.761 (15 ° C)) The stock solution 4 was prepared by measuring up to 100 mL.
２．定量噴射型エアゾールの作製
　表５に従い、実施例６～９、比較例６～７の定量噴射型エアゾールを作製した。 2. Preparation of fixed injection aerosol According to Table 5, fixed injection aerosols of Examples 6 to 9 and Comparative Examples 6 to 7 were manufactured.
（実施例６）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液４を４６ｍＬ充填し、エアゾールバルブ（１回噴射量１．０ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤としてジメチルエーテル（ＤＭＥ）を１５４ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Example 6)
46 mL of the stock solution 4 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem area: 1.4 mm 2 ). Subsequently, 154 mL of dimethyl ether (DME) as a propellant was pressure-filled.
An injection button (injection hole diameter φ 1.6 mm) was attached to the aerosol valve, and a fixed amount injection aerosol with an injection amount of 1.0 mL per push and a discharge amount of imiprotorin of 1.2 mg was obtained.
（実施例７）
　噴射ボタンを噴口孔径φ０．６ｍｍのものに変更した以外は実施例６と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Example 7)
In the same manner as in Example 6 except that the injection button was changed to one having an injection hole diameter of 0.6 mm, a fixed injection aerosol with an injection amount of 1.0 mL per push and an ejection amount of imiprotorin of 1.2 mg was obtained .
（比較例６）
　噴射ボタンを噴口孔径φ０．４ｍｍのものに変更した以外は実施例６と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Comparative example 6)
In the same manner as in Example 6 except that the injection button was changed to one having an injection hole diameter of 0.4 mm, a fixed injection aerosol having an injection amount of 1.0 mL per push and an ejection amount of imiprotorin of 1.2 mg was obtained. .
（実施例８）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．５ｍｍ２のものに変更した以外は実施例６と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Example 8)
In the same manner as in Example 6 except that the aerosol valve was changed to one injection amount of 1.0 mL and stem hole area of 0.5 mm 2 , the injection amount per push was 1.0 mL and the discharge amount of imiprotorin was A fixed dose aerosol of 1.2 mg was obtained.
（実施例９）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．２８ｍｍ２のものに変更した以外は実施例６と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Example 9)
In the same manner as in Example 6 except that the aerosol valve was changed to an injection amount of 1.0 mL once and a stem hole area of 0.28 mm 2 , the injection amount per push was 1.0 mL and the discharge amount of imiproline was A fixed dose aerosol of 1.2 mg was obtained.
（比較例７）
　エアゾールバルブを、１回噴射量１．０ｍＬ、ステム孔面積０．１３ｍｍ２のものに変更した以外は実施例６と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、イミプロトリンの吐出量が１．２ｍｇの定量噴射型エアゾールを得た。 (Comparative example 7)
In the same manner as in Example 6 except that the aerosol valve was changed to an injection amount of 1.0 mL once and a stem hole area of 0.13 mm 2 , the injection amount per push was 1.0 mL, and the discharge amount of imiproline was A fixed dose aerosol of 1.2 mg was obtained.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
３．噴射時間の測定
　試験例１と同様の方法により、定量噴射型エアゾールの噴射時間を測定した。結果を表６に示す。 3. Measurement of injection time The injection time of the constant injection aerosol was measured by the same method as in Test Example 1. The results are shown in Table 6.
４．クロゴキブリに対する殺虫効力確認試験
　図２に示すように、ろ紙１を敷いた床に塩化ビニル製の円筒２（直径φ５０ｃｍ、高さ１５ｃｍ）を設置し、その内部を試験区とした。なお、円筒２の内側側壁には供試虫が這い上がれないように炭酸カルシウムを塗布した。試験区内のろ紙１上の、円筒２の内側側壁に近接する位置に、噴射のターゲットポイント３として印をつけた。
　試験区の中に供試虫としてクロゴキブリ５の雌を１頭放ち、暫く放置して馴化させた後、クロゴキブリ５がターゲットポイント３に来た時に、５０ｃｍ離れた距離からクロゴキブリ５に向けて定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）した。クロゴキブリがノックダウンする（ひっくり返って動けなくなる）までの時間を計測した。試験は３回行い、平均を求めた。結果を表６に示す。 4. As shown in FIG. 2, a cylinder 2 (diameter φ 50 cm, height 15 cm) made of vinyl chloride was placed on the floor on which the filter paper 1 was laid, and the inside was used as a test zone. Calcium carbonate was applied to the inner side wall of the cylinder 2 so that the test insect could not crawl up. A position on the filter paper 1 in the test area, close to the inner sidewall of the cylinder 2, was marked as the target point 3 of the jet.
In the test area, release one female Stag beetle 5 as a test insect, leave it for a while, and then acclimate, then head for Stag beetle 5 from a distance of 50 cm when the Stag beetle 5 comes to target point 3 The injection button of the fixed injection type aerosol was operated once (1 push). The time it took for the black flea to knock down (turn over and get stuck) was measured. The test was performed three times and the average was determined. The results are shown in Table 6.
Figure JPOXMLDOC01-appb-T000006
Figure JPOXMLDOC01-appb-T000006
　実施例６～７及び比較例６は１プッシュあたりの噴射量が１ｍＬの定量噴射型エアゾールにおいて噴射ボタンの噴口孔径を変化させた例であり、実施例８～９及び比較例７はステム孔の面積を変化させた例である。表６の結果から、噴射時間が０．３秒、０．７３秒である実施例６、７は、噴射時間が１．３６秒の比較例６に比べて顕著にクロゴキブリのノックダウン時間が短く、噴射時間が０．５８秒、０．７３秒である実施例８、９は、噴射時間が１．２秒の比較例７に比べて顕著にクロゴキブリのノックダウン時間が短いことが分かった。 Examples 6 to 7 and Comparative Example 6 are examples in which the injection hole diameter of the injection button is changed in a fixed injection type aerosol having an injection amount of 1 mL per push, and Examples 8 to 9 and Comparative Example 7 are stem holes. This is an example in which the area is changed. From the results of Table 6, in Examples 6 and 7 in which the injection time is 0.3 seconds and 0.73 seconds, the knock-down time of the black-necked roach is noticeably compared to Comparative Example 6 in which the injection time is 1.36 seconds. In Examples 8 and 9, which are short and the injection time is 0.58 seconds and 0.73 seconds, it is found that the knock-down time of the black-necked roach is remarkably short as compared with Comparative Example 7 whose injection time is 1.2 seconds. The
＜試験例３：イエバエに対する殺虫効力確認試験＞
１．原液の調製
　フタルスリン１．４ｇを測り取り、１号灯油（ノルマルパラフィン、中央化成株式会社製「ネオチオゾール」、炭素数１１～１５、比重０．７６１（１５℃））を加えて１００ｍＬにまでメスアップすることにより、原液５を調製した。 <Test Example 3: Insecticidal efficacy confirmation test on house fly>
1. Preparation of undiluted solution Measure 1.4 g of phthalthrin, add No. 1 kerosene (normal paraffin, "Neothiosol" manufactured by Chuo Kasei Co., Ltd., carbon number 11-15, specific gravity 0.761 (15 ° C)), and measure up to 100 mL. The stock solution 5 was prepared by
２．定量噴射型エアゾールの作製
　表７に従い、実施例１０～１１、比較例８の定量噴射型エアゾールを作製した。 2. Preparation of fixed injection aerosol According to Table 7, fixed injection aerosols of Examples 10 to 11 and Comparative Example 8 were manufactured.
（実施例１０）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液５を４０ｍＬ充填し、エアゾールバルブ（１回噴射量１．０ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．２９ＭＰａ（２５℃））を１６０ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が１．０ｍＬ、フタルスリンの吐出量が２．８ｍｇの定量噴射型エアゾールを得た。 (Example 10)
40 mL of the stock solution 5 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem area: 1.4 mm 2 ). Subsequently, 160 mL of pressurized liquefied petroleum gas (0.29 MPa (25 ° C.)) was injected as a propellant.
The injection button (injection hole diameter φ1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of phthalthrin was 2.8 mg.
（実施例１１）
　噴射ボタンを噴口孔径φ０．６ｍｍのものに変更した以外は実施例１０と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、フタルスリンの吐出量が２．８ｍｇの定量噴射型エアゾールを得た。 (Example 11)
In the same manner as in Example 10 except that the injection button was changed to the injection hole diameter φ 0.6 mm, a fixed amount injection aerosol with an injection amount per push of 1.0 mL and a phthalthrin discharge amount of 2.8 mg was obtained .
（比較例８）
　噴射ボタンを噴口孔径φ０．４ｍｍのものに変更した以外は実施例１０と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、フタルスリンの吐出量が２．８ｍｇの定量噴射型エアゾールを得た。 (Comparative example 8)
In the same manner as in Example 10 except that the injection button was changed to the injection hole diameter φ 0.4 mm, a fixed amount injection aerosol having an injection amount of 1.0 mL per push and a phthalthrin discharge amount of 2.8 mg was obtained .
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
３．噴射時間の測定
　試験例１と同様の方法により、定量噴射型エアゾールの噴射時間を測定した。結果を表８に示す。 3. Measurement of injection time The injection time of the constant injection aerosol was measured by the same method as in Test Example 1. The results are shown in Table 8.
４．イエバエに対する殺虫効力確認試験
　８畳空間（容積３１．１ｍ３）の試験室に供試虫としてイエバエの雌を１頭放った。イエバエが壁に止まったタイミングに合わせ、約５０ｃｍ離れた距離からイエバエに向けて定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）した。イエバエが落下してノックダウンするまでの時間を計測した。試験は３回行い、平均を求めた。結果を表８に示す。 4. Insecticidal efficacy confirmation test on house fly One house fly female was released as a test insect in a test room of 8 tatami mat space (volume 31.1 m 3 ). At the same time as the house fly stopped on the wall, the injection button of the constant injection aerosol was operated once (1 push) toward the house fly from a distance of about 50 cm away. The time until the house fly fell and knocked down was measured. The test was performed three times and the average was determined. The results are shown in Table 8.
Figure JPOXMLDOC01-appb-T000008
Figure JPOXMLDOC01-appb-T000008
　表８の結果から、噴射時間が０．３２秒、０．７４秒である実施例１０、１１は、噴射時間が１．３６秒の比較例８に比べて顕著にイエバエのノックダウン時間が短いことが分かった。 From the results of Table 8, in Examples 10 and 11 in which the injection time is 0.32 seconds and 0.74 seconds, the knockdown time of the house fly is significantly shorter than that in Comparative Example 8 in which the injection time is 1.36 seconds. I found that.
＜試験例４：芳香効力確認試験＞
１．原液の調製
　リナロール０．５ｇを測り取り、無水エタノール（比重０．７８５（２５℃））を加えて１００ｍＬにまでメスアップすることにより、原液６を調製した。 Test Example 4: Aroma efficacy check test
1. Preparation of stock solution 0.5 g of linalool was measured, and absolute ethanol (specific gravity 0.785 (25 ° C.)) was added to make up to 100 mL, to prepare stock solution 6.
２．定量噴射型エアゾールの作製
　表９に従い、実施例１２、比較例９の定量噴射型エアゾールを作製した。 2. Preparation of fixed injection aerosol In accordance with Table 9, fixed injection aerosols of Example 12 and Comparative Example 9 were prepared.
（実施例１２）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液６を４０ｍＬ充填し、エアゾールバルブ（１回噴射量１．０ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．２９ＭＰａ（２５℃））を１６０ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が１．０ｍＬ、リナロールの吐出量が１．０ｍｇの定量噴射型エアゾールを得た。 (Example 12)
40 mL of undiluted solution 6 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, stem hole area 1.4 mm 2 ). Subsequently, 160 mL of pressurized liquefied petroleum gas (0.29 MPa (25 ° C.)) was injected as a propellant.
The injection button (injection hole diameter φ1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of Lina Roll was 1.0 mg.
（比較例９）
　噴射ボタンを噴口孔径がφ０．４ｍｍのものに変更した以外は実施例１２と同様にして、１プッシュ当たりの噴射量が１．０ｍＬ、リナロールの吐出量が１．０ｍｇの定量噴射型エアゾールを得た。 (Comparative example 9)
In the same manner as in Example 12 except that the injection button was changed to one having an injection hole diameter of φ 0.4 mm, a fixed injection aerosol having an injection amount of 1.0 mL per push and a discharge amount of Linarol of 1.0 mg was obtained. The
Figure JPOXMLDOC01-appb-T000009
Figure JPOXMLDOC01-appb-T000009
３．噴射時間の測定
　試験例１と同様の方法により、定量噴射型エアゾールの噴射時間を測定した。結果を表１０に示す。 3. Measurement of injection time The injection time of the constant injection aerosol was measured by the same method as in Test Example 1. The results are shown in Table 10.
４．芳香官能試験
（噴射１０秒後の官能評価）
　図３に示すように、６畳空間（容積２５ｍ３）の試験室２０の第１の壁２１の中央位置Ｆの床から１００ｃｍの高さより床面とほぼ水平に第１の壁２１に対向する第３の壁２３に向けて、定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）した。噴射１０秒後に、噴射位置である第１の壁２１の中央位置Ｆ、第１の壁２１に直交する第２の壁２２の中央位置Ｇ、及び第１の壁２１に対向する第３の壁２３の中央位置Ｈに立ち、６段階臭気強度表示法の評価基準に従って香りの強度を評価した。試験は３回行い、平均値を四捨五入して６段階の値とした。結果を表１０に示す。
　〔評価基準〕
　０：無臭（平常の嗅覚の持ち主がにおいを感じない状態）
　１：やっと感知できるにおい（検知閾値濃度）
　２：何のにおいであるか分かる弱いにおい（認知閾値濃度）
　３：楽に感知できるにおい
　４：強いにおい
　５：強烈なにおい 4. Aroma sensory test (sensory evaluation after 10 seconds of spraying)
As shown in FIG. 3, it faces the first wall 21 substantially horizontally to the floor surface from a height of 100 cm from the floor of the central position F of the first wall 21 of the test room 20 of six tatami mat space (volume 25 m 3 ) The injection button of the constant injection aerosol was operated once (one push) toward the third wall 23. 10 seconds after the injection, the central position F of the first wall 21 which is the injection position, the central position G of the second wall 22 orthogonal to the first wall 21, and the third wall facing the first wall 21 Standing at the central position H of 23 and the odor intensity was evaluated according to the evaluation criteria of the 6-step odor intensity display method. The test was conducted three times, and the average value was rounded off to obtain six values. The results are shown in Table 10.
〔Evaluation criteria〕
0: Odorless (A state where the owner of ordinary smell does not feel the smell)
1: The odor that can be finally detected (detection threshold concentration)
2: Weak smell (cognitive threshold concentration) to know what smell it is
3: A smell that can be easily detected 4: A strong smell 5: A strong smell
（噴射３０分後の官能評価）
　上記噴射１０秒後の香りの強度を確認した後、試験室２０を密閉状態で放置し、３０分経過後に同様に各壁の中央位置Ｆ～Ｈに立ったときの香りの強度を評価した。試験は３回行い、平均値を四捨五入して６段階の値とした。結果を表１０に示す。 (Sensory evaluation 30 minutes after injection)
After confirming the intensity of the scent 10 seconds after the above injection, the test room 20 was left in a closed state, and after 30 minutes, the intensity of the scent when standing at the central position F to H of each wall was similarly evaluated. The test was conducted three times, and the average value was rounded off to obtain six values. The results are shown in Table 10.
Figure JPOXMLDOC01-appb-T000010
Figure JPOXMLDOC01-appb-T000010
　表１０の結果から、噴射時間が０．３１秒である実施例１２は、噴射時間が１．３５秒の比較例９に比べて３０分後における香りの広がり及び強度に優れており、３０分経過後においても香りの持続性に優れることが分かった。 From the results in Table 10, Example 12 in which the injection time is 0.31 seconds is excellent in spread and intensity of the aroma after 30 minutes as compared with Comparative Example 9 in which the injection time is 1.35 seconds, and 30 minutes. It turned out that the persistence of the aroma is excellent even after the lapse.
＜試験例５：除菌効力確認試験＞
１．原液の調製
　イソプロピルメチルフェノール（ＩＰＭＰ）２０ｇを測り取り、９９．５％エタノール（比重０．７８５（２５℃））を加えて１００ｍＬにまでメスアップすることにより、原液７を調製した。 <Test Example 5: Bactericidal efficacy confirmation test>
1. Preparation of stock solution 20 g of isopropylmethylphenol (IPMP) was measured, and 99.5% ethanol (specific gravity 0.785 (25 ° C.)) was added to make up to 100 mL to prepare stock solution 7.
２．定量噴射型エアゾールの作製
（実施例１３）
　エアゾール用耐圧缶（容量２９４ｍＬ）に、原液７を６０ｍＬ充填し、エアゾールバルブ（１回噴射量１．０ｍＬ、ステム孔面積１．４ｍｍ２）でエアゾール用耐圧缶を閉止した。続いて、噴射剤として液化石油ガス（０．４９ＭＰａ（２５℃））を１４０ｍＬ加圧充填した。
　エアゾールバルブに噴射ボタン（噴口孔径φ１．６ｍｍ）を取り付け、１プッシュ当たりの噴射量が１．０ｍＬ、ＩＰＭＰの吐出量が６０ｍｇの定量噴射型エアゾールを得た。 2. Preparation of quantitative injection type aerosol (Example 13)
60 mL of the stock solution 7 was filled in a pressure resistant can for aerosol (volume 294 mL), and the pressure resistant can for aerosol was closed with an aerosol valve (1.0 mL injection amount, 1.4 mm 2 stem hole area). Subsequently, 140 mL of liquefied petroleum gas (0.49 MPa (25 ° C.)) was pressure-filled as a propellant.
The injection button (injection hole diameter φ 1.6 mm) was attached to the aerosol valve, and the injection amount per push was 1.0 mL, and the discharge amount of IPMP was 60 mg.
３．噴射時間の測定
　試験例１と同様の方法により、定量噴射型エアゾールの噴射時間を測定した。結果を表１１に示す。 3. Measurement of injection time The injection time of the constant injection aerosol was measured by the same method as in Test Example 1. The results are shown in Table 11.
４．効力確認試験
　１０軒の一般家庭の浴室において、浴室掃除を行い、ピンク色のヌメリ（主にRhodotorula（酵母）もしくはMethylobacterium（細菌）によって発生）や黒カビ（主にCladosporium（真菌）によって発生）を取り除いた。その後、ピンク色のヌメリや黒カビが頻繁に発生する場所を２ヶ所選定した。そのうち１ヶ所に向かって、定量噴射型エアゾールの噴射ボタンを１回操作（１プッシュ）し、処理した場所を処理区とした。もう１ヶ所については、薬剤が付着しないようにし、その場所を無処理区とした。浴室掃除及び検体処理を行った日から何日後にピンク色のヌメリもしくは黒カビが発生したかを家庭ごとに確認した。
　試験期間はピンク色のヌメリや黒カビが発生しやすい時期（６～９月、日本）に行った。
　結果を表１１に示す。 4. Efficacy test In 10 common household bathrooms, the bathroom is cleaned to remove pink nello (mainly caused by Rhodotorula (yeast) or Methylobacterium (bacteria)) and black mold (mainly generated by Cladosporium (fungus)) The After that, two locations where pink stains and black mold frequently occur were selected. The injection button of the fixed injection type aerosol was operated once (1 push) toward one of them, and the treated area was defined as the treated area. At the other place, the drug was not attached, and the place was taken as an untreated area. It was confirmed for each household how many days after the day of bathroom cleaning and sample processing that pink slime or black mold had occurred.
The test was conducted at a time when pink slime and black mold were likely to occur (June to September, Japan).
The results are shown in Table 11.
Figure JPOXMLDOC01-appb-T000011
Figure JPOXMLDOC01-appb-T000011
　表１１の結果から、無処理区は１週間以内にピンク色のヌメリ又は黒カビが発生したのに対し、実施例１３の定量噴射型エアゾールを噴射した処理区では、１０日以上の除菌・防カビ効果が得られることがわかった。 According to the results in Table 11, pink rubble or black mold was generated within one week in the non-treated area, whereas in the treated area where the quantitative spray aerosol of Example 13 was sprayed, sterilization and prevention for 10 days or more It turned out that a mold effect can be obtained.
　本発明を詳細にまた特定の実施態様を参照して説明したが、本発明の精神と範囲を逸脱することなく様々な変更や修正を加えることができることは当業者にとって明らかである。本出願は、２０１７年１２月１２日出願の日本特許出願（特願２０１７－２３８１６０）に基づくものであり、その内容はここに参照として取り込まれる。 Although the invention has been described in detail and with reference to specific embodiments, it will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention. This application is based on Japanese Patent Application (Japanese Patent Application No. 2017-238160) filed on Dec. 12, 2017, the contents of which are incorporated herein by reference.
１　　ろ紙
２　　円筒
３　　ターゲットポイント
５　　クロゴキブリ
１０、２０　試験室
２１　第１の壁
２２　第２の壁
２３　第３の壁
Ａ　　中央部
Ｂ～Ｅ　隅部
Ｆ～Ｈ　中央位置 DESCRIPTION OF SYMBOLS 1 filter paper 2 cylinder 3 target point 5 black broom 10, 20 Test room 21 1st wall 22 2nd wall 23 3rd wall A central part B-E corner part F-H central position

Claims (8)

  1. 　１回の噴射操作で一定量のエアゾール組成物を噴射する定量噴射型エアゾールであって、
    　前記エアゾール組成物は薬剤を含む原液と噴射剤とからなり、耐圧容器に充填されており、
    　前記定量噴射型エアゾールは、１回の噴射量が１．０～３．０ｍＬであり、且つ１回の噴射時間が０．８秒以内である定量噴射型エアゾール。     It is a fixed injection type aerosol that injects a fixed amount of aerosol composition in one injection operation,
    The aerosol composition comprises a drug-containing stock solution and a propellant, and is filled in a pressure resistant container,
    The fixed jet aerosol is a fixed jet aerosol having an injection volume of 1.0 to 3.0 mL and an injection time of 0.8 seconds or less.
  2. 　前記１回の噴射時間が、０．２０～０．７５秒である、請求項１に記載の定量噴射型エアゾール。 The metered dose aerosol according to claim 1, wherein the one injection time is 0.20 to 0.75 seconds.
  3. 　前記原液がさらに溶剤を含む、請求項１又は２に記載の定量噴射型エアゾール。 The fixed jet aerosol according to claim 1 or 2, wherein the stock solution further contains a solvent.
  4. 　前記薬剤の含有量が、前記原液中０．０１～７０質量／容量％である、請求項１～３のいずれか１項に記載の定量噴射型エアゾール。 The quantitative injection aerosol according to any one of claims 1 to 3, wherein the content of the drug is 0.01 to 70% by mass / volume in the stock solution.
  5. 　前記エアゾール組成物中の前記原液と前記噴射剤の体積比が、１：９９～５０：５０である、請求項１～４のいずれか１項に記載の定量噴射型エアゾール。 5. The metered dose aerosol according to any one of claims 1 to 4, wherein the volume ratio of the stock solution to the propellant in the aerosol composition is 1:99 to 50:50.
  6. 　前記薬剤が、害虫防除成分、芳香成分、消臭成分及び除菌・殺菌成分からなる群から選択される少なくとも１種である、請求項１～５のいずれか１項に記載の定量噴射型エアゾール。 The quantitative injection type aerosol according to any one of claims 1 to 5, wherein the medicine is at least one selected from the group consisting of pest control components, aroma components, deodorizing components, and microbicidal and bactericidal components. .
  7. 　耐圧容器に薬剤を含む原液と噴射剤とからなるエアゾール組成物が充填された定量噴射型エアゾールを用いて、１回の噴射操作で噴射量が１．０～３．０ｍＬ且つ噴射時間が０．８秒以内となるように噴射する定量噴射型エアゾールの噴射方法。 An injection amount is 1.0 to 3.0 mL and an injection time is 0. 0 in a single injection operation using a fixed amount injection type aerosol filled with an aerosol composition consisting of a stock solution containing a drug and a propellant in a pressure resistant container. Injection method of fixed injection type aerosol to be injected within 8 seconds.
  8. 　定量噴射型エアゾールを用いて噴射されるエアゾール組成物中の薬剤の効力を向上させる方法であって、
    　１．０～３．０ｍＬの範囲にある前記エアゾール組成物の一定量を、０．８秒以内に噴射する薬剤の効力向上方法。     A method of improving the efficacy of a medicament in an aerosol composition to be sprayed using a metered dose aerosol, comprising:
    A method for improving the efficacy of a drug, comprising injecting a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds.
PCT/JP2018/045553 2017-12-12 2018-12-11 Metered-spray aerosol, method for spraying metered-spray aerosol, and method for improving effect of chemical agent WO2019117164A1 (en)

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JP2022115746A JP2022140536A (en) 2017-12-12 2022-07-20 Method for improving durability of isopropyl methylphenol and metered-spray aerosol for disinfection
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