Dose-Counted Disinfectant Spray Sol, Disinfectant Spray Sol Application Methods, and Methods for Improving the Durability and Effectiveness of Disinfectant / Sterilizing Components

VN126273APending Publication Date: 2026-06-15EARTH CORP
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Patent Information

Authority / Receiving Office
VN · VN
Patent Type
Applications
Current Assignee / Owner
EARTH CORP
Filing Date
2018-12-11
Publication Date
2026-06-15

AI Technical Summary

Technical Problem

Conventional metered-dose aerosols have limitations in drug efficacy and durability due to small spray volumes, leading to excessive consumption and frequent reapplication, with user experience and effectiveness varying based on injection method.

Method used

A metered-dose aerosol system that injects a fixed amount of 1.0 to 3.0 mL of aerosol composition within 0.8 seconds, optimizing the balance between injection volume and time to enhance drug efficacy and durability, using a pressure-resistant container filled with a stock solution containing a drug and propellant.

Benefits of technology

The system ensures consistent drug delivery with reduced variation, increased user satisfaction, and prolonged drug effect sustainability, minimizing wasteful overuse while maintaining effectiveness with a single injection operation.

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Abstract

The invention relates to a metered aerosol in which the stability of the chemical agent is increased and its efficacy is improved. The metered aerosol in the invention is a metered aerosol for the spraying of a fixed amount of aerosol preparation by a single spraying operation, in which the aerosol preparation consists of a base solution containing the chemical agent and a propellant and is loaded into a pressurized container, and in which the amount sprayed per operation is 1.0 to 3.0 mL and the spraying time per operation is 0.8 seconds or less.
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Description

Metered dose aerosol, method for spraying metered dose aerosol, and method for improving the efficacy of medicine

[0001] The present invention relates to a metered dose aerosol, a spraying method using the same, and a method for improving the efficacy of a drug ejected when the metered dose aerosol is sprayed.

[0002] Metered-dose aerosols are known that spray a fixed amount of an aerosol composition consisting of a concentrate containing a drug as an active ingredient and a propellant in a single spray operation. Because metered-dose aerosols eject a predetermined amount of drug in a single spray operation, there is little variation in the operation method between users (such as differences in the amount sprayed due to the method of pressing the spray button or the duration of pressing the button), and this has the advantage of less variation in effectiveness.

[0003] As an example of such a metered dose aerosol, Patent Document 1 discloses an aerosol for pest control equipped with a metered dose aerosol valve that sprays 0.35 to 0.9 mL per spray.

[0004] Japanese Patent Application Publication No. 2010-280633

[0005] As mentioned above, metered-dose aerosols for use in the air, such as insecticide aerosols and fragrance aerosols, have the advantage of little variation in effectiveness. However, if the amount sprayed per spray is small, the user may not feel a sense of use, and even though an effective amount of the agent is ejected in one spray, multiple sprays may result in excessive consumption. Furthermore, conventional metered-dose aerosols have a limited duration of the agent's effectiveness, and in order to maintain this effect, the spray operation must be repeated after a certain period of time has elapsed since the spray, which requires frequent re-spraying. Therefore, the object of the present invention is to provide a metered-dose aerosol that improves the efficacy of the agent, increases the duration of its effect, and provides a sense of use.

[0006] As a result of extensive research, the inventors have found that if a metered dose aerosol capable of spraying large volumes of 1.0 mL or more is developed, the amount sprayed per spray operation will be large, thereby improving the feel of use while also increasing the amount of medicine ejected; further, with a metered dose aerosol that sprays large volumes, the duration of the medicine's effect will vary depending on the spray duration per spray operation, and that there is an optimal balance between the amount of aerosol composition sprayed per spray operation and the spray duration for sustaining the medicine's effect.

[0007] That is, the present invention is characterized by the following (1) to (8). (1) A metered dose aerosol that sprays a fixed amount of an aerosol composition with a single spray operation, the aerosol composition comprising a drug-containing concentrate and a propellant, and filled in a pressure-resistant container, the metered dose aerosol having a single spray volume of 1.0 to 3.0 mL and a single spray time of 0.8 seconds or less. (2) The metered dose aerosol according to (1) above, wherein the single spray time is 0.20 to 0.75 seconds. (3) The metered dose aerosol according to (1) or (2) above, wherein the concentrate further contains a solvent. (4) The metered dose aerosol according to any one of (1) to (3) above, wherein the drug content in the concentrate is 0.01 to 70% by mass / volume. (5) The metered-dose aerosol according to any one of (1) to (4), wherein the volume ratio of the concentrate to the propellant in the aerosol composition is 1:99 to 50:50. (6) The metered-dose aerosol according to any one of (1) to (5), wherein the chemical agent is at least one selected from the group consisting of pest control ingredients, fragrance ingredients, deodorizing ingredients, and disinfecting / sterilizing ingredients. (7) A method for spraying a metered-dose aerosol, comprising using a pressure-resistant container filled with an aerosol composition comprising a concentrate containing a chemical agent and a propellant, spraying the amount sprayed in one spray operation to be 1.0 to 3.0 mL and the spray time to be within 0.8 seconds. (8) A method for improving the efficacy of a chemical agent in an aerosol composition sprayed using a metered-dose aerosol, comprising spraying a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds.

[0008] The metered dose aerosol of the present invention allows a large amount of the aerosol composition to be sprayed in a predetermined amount in the range of 1.0 to 3.0 mL in a single spray operation, and furthermore, the duration of the effect of the drug in the aerosol composition can be increased. Therefore, there is no difference in the operation method depending on the user, so there is no variation in the effect, wasteful overuse can be avoided, and the effect of the drug can be sustained with a single spray operation.

[0009] Fig. 1 is a plan view illustrating the test chamber used in Test Example 1. Fig. 2 is a perspective view illustrating the test method of Test Example 2. Fig. 3 is a plan view illustrating the test chamber used in Test Example 4.

[0010] Hereinafter, embodiments of the present invention will be described in more detail. In this specification, "mass" is synonymous with "weight."

[0011] The metered dose aerosol of the present invention is prepared by filling a pressure-resistant container with an aerosol composition containing a drug concentrate and a propellant. Each component will be described below.

[0012] The concentrate constituting the aerosol composition of the present invention contains at least a chemical agent as an active ingredient. The active ingredient refers to a substance that exerts some kind of effect when a metered-dose aerosol is used, and includes, but is not limited to, pest control ingredients, fragrance ingredients, deodorizing ingredients, disinfecting / sterilizing ingredients, etc.

[0013] The pest control component is a component that can kill, repel, knock down, etc., target pests. The type of pest control component is not particularly limited, and known compounds can be used. Examples of pest control components include pyrethroid compounds such as permethrin, pyrethrins, allethrin, phthalthrin, resmethrin, furamethrin, fenothrin, empenthrin, prallethrin, cyphenothrin, imiprothrin, transfluthrin, metofluthrin, dimefluthrin, and mepafluthrin; organophosphorus compounds such as fenitrothion, dichlorvos, chlorpyrifos-methyl, diazinon, and fenthion; carbaryl, Carbamate compounds such as propoxur; compounds such as methoprene, pyriproxyfen, methoxadiazone, fipronil, amidoflumet, and broflanilide; peppermint oil, orange oil, fennel oil, cinnamon oil, clove oil, turpentine oil, eucalyptus oil, hiba oil, jasmine oil, neroli oil, peppermint oil, bergamot oil, butygrain oil, lemon oil, lemongrass oil, cinnamon oil, citronella oil, geranium oil, citral, and l-menthol. essential oil components such as ethanol, citronellyl acetate, cinnamic aldehyde, terpineol, nonyl alcohol, cis-jasmone, limonene, linalool, 1,8-cineole, geraniol, α-pinene, p-menthane-3,8-diol, eugenol, menthyl acetate, thymol, benzyl benzoate, and benzyl salicylate; glycol ethers such as propylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, dipropylene glycol dimethyl ether, ethylene glycol monoisobutyl ether, diethylene glycol monoisobutyl ether, diethylene glycol dibutyl ether, diethylene glycol dimethyl ether, and triethylene glycol dimethyl ether; and dibasic acid esters such as dibutyl adipate. These may be used alone or in combination of two or more.

[0014] The pest control component may be appropriately selected according to the type of target pest. Examples of target pests include mosquitoes, flies, moths, bees, stink bugs, cockroaches, ants, spiders, pill bugs, mites, lice, centipedes, caterpillars, millipedes, spiders, horseflies, black flies, moth flies, termites, midges, leafhoppers, bark beetles, ground beetles, earwigs, silverfish, longhorn beetles, dermestid beetles, booklice, bur moths, and the like. Transfluthrin, metofluthrin, profluthrin, phthalthrin, prallethrin, momfluorothrin, and the like are suitable for use against flying pests such as mosquitoes, flies, moths, bees, horseflies, black flies, moth flies, midges, leafhoppers, moth flies, moth flies, and the like. Furthermore, for crawling pests such as cockroaches, stink bugs, ants, spiders, pill bugs, mites, lice, centipedes, caterpillars, millipedes, spiders, termites, wood beetles, ground beetles, earwigs, silverfish, and the like, phthalthrin, prallethrin, imiprothrin, permethrin, fenothrin, and the like are suitable.

[0015] Aromatic components are components that emit fragrance. Examples of aromatic components include the essential oil components described above, as well as natural fragrances such as anise oil, lavender oil, rose oil, rosemary oil, and grapefruit oil; and synthetic fragrances such as camphene, p-cymene, citronellol, nerol, benzyl alcohol, n-butyraldehyde, isobutyraldehyde, coumarin, and cineole. These may be used alone or in combination of two or more.

[0016] The deodorizing component is a component that can eliminate odors. Examples of deodorizing components include components that adsorb odorous components such as green tea extract, persimmon tannin, lauric acid methacrylate, methyl benzoate, methyl phenylacetate, geranyl crotrate, acetophenone myristate, benzyl acetate, benzyl propionate, and silver, as well as components that mask odorous components such as the above-mentioned aromatic components. These may be used alone or in combination of two or more.

[0017] The disinfecting / sterilizing component is a component that removes or kills microorganisms, molds, and bacteria. Examples of the disinfecting / sterilizing component include ethanol, hinokitiol, 2-mercaptobenzothiazole, 2-(4-thiazolyl)benzimidazole, 5-chloro-2-methyl-4-isothiazolin-3-one, triforine, p-chlorometaxylenol, 3-methyl-4-isopropylphenol, ortho-phenylphenol, chlorhexidine gluconate, polylysine, chitosan, tetrahydrolinalool, and dialkyldimethylammonium chloride. These may be used alone or in combination of two or more.

[0018] The above-mentioned chemicals can be used in combination with components having different effects, for example, a pest control component and a fragrance component can be used in combination, or a fragrance component can be used in combination with a deodorizing component other than a fragrance component.

[0019] The content of the chemical agent in the concentrate is preferably 0.01 to 70% by mass / volume. A chemical agent content of 0.01% by mass / volume or more in the concentrate can provide sufficient chemical effects, while a content of 70% by mass / volume or less improves productivity. The lower limit of the chemical agent content is more preferably 0.1% by mass / volume or more, even more preferably 0.3% by mass / volume or more, and particularly preferably 0.5% by mass / volume or more, while the upper limit is more preferably 65% ​​by mass / volume or less, even more preferably 50% by mass / volume or less, and particularly preferably 25% by mass / volume or less.

[0020] The stock solution may contain a solvent for purposes such as adjusting the viscosity of the stock solution, improving production suitability, and increasing the penetration of the pesticide against pests. Examples of such solvents include the glycol ethers mentioned above, hydrocarbon solvents, alcohol solvents, aromatic solvents, and ester solvents. Water and surfactants may also be used. Examples of hydrocarbon solvents include aliphatic and alicyclic hydrocarbons such as paraffinic hydrocarbons and naphthenic hydrocarbons, with kerosene such as JIS No. 1 kerosene being preferred. Specific examples include normal paraffins and isoparaffins. Typical normal paraffins have 8 to 16 carbon atoms, such as Neothiosol manufactured by Chuo Kasei Co., Ltd. and Normal Paraffin MA manufactured by JXTG Nippon Oil & Energy Corporation. Typical isoparaffins have 8 to 16 carbon atoms, such as IP Clean LX and Supersol FP25 manufactured by Idemitsu Kosan Co., Ltd. Examples of alcohol-based solvents include lower alcohols such as ethanol and propanol (normal and iso), and polyhydric alcohols such as glycerin and ethylene glycol. Examples of aromatic solvents include toluene and xylene. Examples of ester-based solvents include isopropyl myristate, hexyl laurate, and isopropyl palmitate.

[0021] The solvent content in the concentrate is preferably 30 to 99.99% by mass / volume. Having the solvent content in the concentrate at 30% by mass / volume or more can improve productivity, while a content of 99.99% by mass / volume or less is preferred because sufficient drug efficacy can be ensured. The solvent content is more preferably 35% by mass / volume or more in lower limit, more preferably 50% by mass / volume or more in upper limit, more preferably 99.9% by mass / volume or less in upper limit, more preferably 99.5% by mass / volume or less in upper limit.

[0022] The concentrate may contain other ingredients, such as preservatives, pH adjusters, UV absorbers, inorganic substances, surfactants, and solubilizing agents, as long as the ingredients do not impair the effects of the present invention.

[0023] The content of the concentrate in the aerosol composition can be varied as appropriate depending on the intended use of the metered dose aerosol and the combination with the propellant, and is not particularly limited, but can be, for example, 1 to 50% by volume in the aerosol composition. When the concentrate is 1% by volume or more in the aerosol composition, sufficient drug efficacy can be obtained, and when the concentrate is 50% by volume or less, the concentrate can be sprayed as atomized particles, thereby reducing contamination of furniture, floors, walls, etc., when used indoors, for example. The lower limit of the concentrate content in the aerosol composition is more preferably 3% by volume or more, and even more preferably 5% by volume or more, and the upper limit is more preferably 40% by volume or less, and even more preferably 30% by volume or less.

[0024] (Propellant) The propellant is a medium for spraying the concentrate, and is filled under pressure together with the concentrate into a pressure-resistant container. Examples of propellants that can be used include liquefied gases such as liquefied petroleum gases (LPG) (e.g., propane, propylene, n-butane, isobutane) and dimethyl ether (DME), compressed gases (e.g., carbon dioxide, nitrogen gas, compressed air), and halogenated carbon gases (e.g., HFC-152a, HFC-134a, HFO-1234yf, HFO-1234ze). The propellant used may be selected appropriately depending on its compatibility with the concentrate and the container components, such as an aerosol valve.

[0025] The propellant content in the aerosol composition can be varied as appropriate depending on the intended use of the metered-dose aerosol and the combination with the concentrate, and is not particularly limited. For example, it can be 50 to 99% by volume in the aerosol composition. When the propellant content in the aerosol composition is 50% by volume or more, the concentrate can be sprayed as spray particles, making the drug more easily diffused and the drug's effect more likely to last. Furthermore, when the propellant content is 99% by volume or less, sufficient drug effect can be obtained. The propellant content in the aerosol composition is preferably 60% by volume or more at its lower limit, more preferably 70% by volume or more, and more preferably 97% by volume or less at its upper limit, more preferably 95% by volume or less.

[0026] The volume ratio of the concentrate to the propellant in the aerosol composition is preferably 1:99 to 50:50, more preferably 3:97 to 40:60, and even more preferably 5:95 to 30:70. By setting such a volume ratio, sufficient drug effects can be obtained.

[0027] (Metered-Dose Aerosol) The metered-dose aerosol of the present invention is constructed by filling the concentrate and propellant described above into a pressure-resistant aerosol container, and closing the opening of the pressure-resistant container with an aerosol valve.

[0028] A metered dose aerosol is an aerosol that sprays a fixed amount of aerosol composition with one spray operation. When a user operates a spray member (hereinafter also referred to as a spray button) attached to an aerosol valve, a fixed amount of the aerosol composition (concentrate and propellant) in a pressure-resistant container is sprayed through the aerosol valve, and the concentrate is converted into particles by the propellant and sprayed as spray particles.

[0029] (Aerosol Valve) The aerosol valve comprises an opening / closing member for switching communication between the inside and outside of the pressure-resistant container on and off by operating the spray member by the user, a housing to which the opening / closing member is attached, and a mounting member for holding the housing in a predetermined position on the pressure-resistant container. The opening / closing member also includes a stem that slides up and down in conjunction with the spray member. The sliding of the stem switches between communication (spraying state) and blocking (non-spraying state) of the aerosol composition. The aerosol valve is formed with a housing hole for taking in the aerosol composition from the pressure-resistant container and a stem hole for delivering the taken-in aerosol composition to the spray member. The housing is formed with a housing hole for taking in the aerosol composition from the pressure-resistant container. The stem is formed with a stem hole for delivering the aerosol composition taken in the housing to the spray member. The path from the housing hole to the stem hole constitutes an internal passage through which the aerosol composition passes.

[0030] In the present invention, the aerosol valve is a metered-volume aerosol valve that sprays a fixed amount with a single operation of the spray member. The spray volume of the aerosol valve is a predetermined fixed amount in the range of 1.0 to 3.0 mL per spray operation. By using an aerosol valve having a housing that can store a predetermined amount of aerosol composition in the range of 1.0 to 3.0 mL per spray operation, a predetermined fixed amount in the range of 1.0 to 3.0 mL can be sprayed with a single spray operation, making it possible to spray a large amount of medicine. The spray volume of the aerosol valve can be appropriately set within the above range.

[0031] The spray member (spray button) is a component attached to the pressure-resistant container via the aerosol valve. The spray button is formed with a passage in the operating portion through which the aerosol composition taken in from the pressure-resistant container via the stem hole of the aerosol valve passes, and with a nozzle through which the aerosol composition is sprayed.

[0032] From the viewpoint of setting the injection time within the desired range, the inner diameter of the injection nozzle of the injection button (injection nozzle hole diameter) is preferably 0.45 to 3.0 mm, more preferably 0.5 to 2.0 mm, and even more preferably 0.6 to 1.6 mm. It is also acceptable to have multiple injection nozzles with the same area.

[0033] (Spray Pressure) As described above, the metered dose aerosol of the present invention is prepared by filling a pressure-resistant aerosol container with the concentrate and propellant, i.e., the aerosol composition, and then pressing the spray button once to spray a fixed amount of the aerosol composition. The spray pressure of the aerosol composition at a position 20 cm away from the nozzle is preferably 5 to 40 gf, more preferably 8 to 30 gf. By maintaining the spray pressure within this range, the spray time can be adjusted to the desired range. The spray pressure can be measured at room temperature of 25°C by spraying the aerosol composition toward the center of a circular plate with a diameter of 60 mm attached to a digital force gauge (e.g., Imada Co., Ltd., model number: DS2-2N) placed on its side 20 cm from the nozzle of the metered dose aerosol, and calculating the average of the maximum spray load.

[0034] (Ejection Time) The metered dose aerosol of the present invention has an ejection time of 0.8 seconds or less per ejection operation. Although the reason why the effects of the present invention are achieved is unclear, it is believed that by ejecting a predetermined amount of aerosol composition in the range of 1.0 to 3.0 mL per ejection within 0.8 seconds, the volatility of the drug can be efficiently increased, thereby improving the efficacy of the drug and increasing the duration of its effect. The ejection time per ejection operation is preferably 0.75 seconds or less, more preferably 0.10 to 0.75 seconds, even more preferably 0.20 to 0.75 seconds, and particularly preferably 0.25 to 0.75 seconds.

[0035] In the present invention, examples of methods for adjusting the spray time for one spray operation include adjusting the size of the nozzle of the spray button, adjusting the spray pressure of a metered dose aerosol, adjusting the stem hole diameter of an aerosol valve, adjusting the pressure of the propellant, and combinations of these.

[0036] By using the metered dose aerosol of the present invention to spray a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds, the efficacy of the drug in the sprayed aerosol composition can be improved, thereby increasing the duration of the drug's effectiveness.

[0037] The present invention will be further explained below with reference to examples and comparative examples, but the present invention is not limited to the following examples.

[0038] <Test Example 1: Insecticidal efficacy confirmation test against Culex pipiens mosquito> 1. Preparation of stock solutions According to the formulation shown in Table 1, transfluthrin was measured out and isopropanol (specific gravity 0.785 (20°C)) was added to make up to 100 mL, to prepare stock solutions 1 to 3.

[0039]

[0040] 2. Preparation of Metered-Dose Aerosols According to Table 2, metered-dose aerosols of Examples 1 to 5 and Comparative Examples 1 to 5 were prepared.

[0041] (Example 1) 12.8 mL of concentrate 1 was filled into an aerosol pressure can (volume 294 mL), and an aerosol valve (amount per injection: 1.0 mL, stem hole area: 1.4 mm 2 The pressure-resistant aerosol can was closed with a cap. Subsequently, 187.2 mL of liquefied petroleum gas (0.49 MPa (25°C)) was pressurized and filled as a propellant. A spray button (nozzle hole diameter φ1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 1.0 mL per push and an ejection volume of 16 mg of transfluthrin.

[0042] Example 2 A metered-dose aerosol with a spray amount of 1.0 mL per push and a transfluthrin ejection amount of 16 mg was obtained in the same manner as in Example 1, except that the spray button was changed to one with a nozzle hole diameter of 0.6 mm.

[0043] Comparative Example 1 A metered-dose aerosol with a spray amount of 1.0 mL per push and a transfluthrin ejection amount of 16 mg was obtained in the same manner as in Example 1, except that the spray button was changed to one with a nozzle hole diameter of 0.4 mm.

[0044] (Example 3) The aerosol valve was set to a single injection volume of 1.0 mL and a stem hole area of ​​0.5 mm 2 A metered dose aerosol spray with a spray amount of 1.0 mL per push and a discharge amount of transfluthrin of 16 mg was obtained in the same manner as in Example 1, except that the above was changed to

[0045] (Example 4) The aerosol valve was set to a single injection volume of 1.0 mL and a stem hole area of ​​0.28 mm 2 A metered dose aerosol spray with a spray amount of 1.0 mL per push and a discharge amount of transfluthrin of 16 mg was obtained in the same manner as in Example 1, except that the above was changed to

[0046] (Comparative Example 2) The aerosol valve had a single injection volume of 1.0 mL and a stem hole area of ​​0.13 mm 2 A metered dose aerosol spray with a spray amount of 1.0 mL per push and a discharge amount of transfluthrin of 16 mg was obtained in the same manner as in Example 1, except that the above was changed to

[0047] (Example 5) 12.8 mL of concentrate 2 was filled into an aerosol pressure can (volume 294 mL), and an aerosol valve (amount per injection: 2.2 mL, stem hole area: 1.4 mm 2 The pressure-resistant aerosol can was then closed with a cap. Subsequently, 187.2 mL of liquefied petroleum gas (0.49 MPa (25°C)) was pressurized and filled as a propellant. A spray button (nozzle hole diameter φ1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 2.2 mL per push and an ejection volume of 16 mg of transfluthrin.

[0048] Comparative Example 3 A metered-dose aerosol with a spray amount of 2.2 mL per push and a transfluthrin ejection amount of 16 mg was obtained in the same manner as in Example 5, except that the spray button was changed to one with a nozzle hole diameter of 0.6 mm.

[0049] Comparative Example 4: 3.2 mL of concentrate 3 was filled into an aerosol pressure can (volume 59 mL), and an aerosol valve (amount per injection: 0.2 mL, stem hole area: 0.4 mm 2 The pressure-resistant aerosol can was then closed with a cap. Subsequently, 16.8 mL of liquefied petroleum gas (0.49 MPa (25°C)) was pressurized and filled as a propellant. A spray button (nozzle hole diameter φ0.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 0.2 mL per push and an ejection volume of 16 mg of transfluthrin.

[0050] Comparative Example 5 A metered-dose aerosol with a spray amount of 0.2 mL per push and an ejection amount of transfluthrin of 16 mg was obtained in the same manner as in Comparative Example 4, except that the spray button was changed to one with an orifice diameter of 0.23 mm.

[0051]

[0052] 3. Measurement of spray time A laser diffraction particle size analyzer (Microtrac Bell Corporation, "LDSA-1400A") was placed 5 cm in a straight line in the spray direction (horizontal direction) from the nozzle of the constant-volume aerosol, so that the laser light was directed perpendicular to the spray direction. The spray button was pressed once (one push) to spray, and a video of the spray was taken. The video was played back, and the longest continuous time during which the laser light could be confirmed to be lit by the spray particles was measured in 0.01-second increments. Note that interruptions in the laser light illumination of 0.05 seconds or less were considered continuous, and the measurement was terminated when the laser light did not illuminate for 0.06 seconds or more, and the final time the laser light was lit was taken as the measurement time. The results are shown in Tables 3 and 4, respectively.

[0053] 4. Insecticidal efficacy test against Culex pipiens pallens (verification of insecticidal efficacy immediately after spraying) A cage (a 16-mesh cage measuring 25 cm long x 25 cm wide, folded in half and stapled around the edges to form a cylindrical shape) containing 10 Culex pipiens pallens was prepared as test insects. As shown in Figure 1, an 8-tatami room (volume 31.1 m) was sprayed. 3 Cages containing Culex pipiens mosquitoes were placed at the four corners (corners B to E) of test chamber 10 (Fig. 1B) on the floor (height 0 cm) and at a height of 75 cm from the floor. The spray button of a metered-dose aerosol was operated once (one push) at a height of 1 m from the floor at corner B, at a 45-degree angle diagonally upward, toward center A. The time until the Culex pipiens mosquitoes were knocked down (they fell over and became immobile) was measured, and KT50 (minutes) (the time required for 50% of the Culex pipiens mosquitoes to be knocked down) was calculated using the probit method. The test was performed three times, and the average was calculated. The results are shown in Table 3.

[0054] (Verification of insecticidal efficacy 3 hours after spraying) A cage (a 16-mesh cage measuring 25 cm long x 25 cm wide, folded in half and stapled around the edges to form a cylindrical shape) containing 10 Culex pipiens mosquitoes was prepared as test insects. As shown in Figure 1, an 8-tatami room (volume 31.1 m) was sprayed. 3The spray button of the metered-dose aerosol was operated once (one push) at a height of 1 m from the floor at corner B of test chamber 10, at a 45-degree angle diagonally upwards, toward center A. Test chamber 10 was left sealed, and after 3 hours had passed, cages containing Culex pipiens mosquitoes were placed on the floor (height 0 cm) and at a height of 75 cm from the floor at the four corners (corners B to E) of test chamber 10. The time until the Culex pipiens mosquitoes were knocked down was measured, and KT50 (minutes) was calculated using the probit method. The test was performed three times, and the average was calculated. The results are shown in Table 4.

[0055]

[0056]

[0057] As shown in Table 3, the average KT50 for all metered dose aerosols immediately after spraying was approximately 3 minutes. In contrast, as shown in Table 4, differences were observed in the average KT50 three hours after spraying. Examples 1 to 4 and Comparative Examples 1 and 2 are examples in which the spray volume per push was 1 mL and the nozzle hole diameter of the spray button or the area of ​​the stem hole was changed. Examples 1 and 2 had significantly shorter average KT50 than Comparative Example 1, and Examples 3 and 4 had significantly shorter average KT50 than Comparative Example 2. Example 5 and Comparative Example 3 are examples in which the spray volume per push was 2.2 mL and the nozzle hole diameter of the spray button was changed. Example 5 had a significantly shorter average KT50 than Comparative Example 3. Comparative Examples 4 and 5 were examples in which the spray volume per push was 0.2 mL, but for Comparative Examples 4 and 5, the average KT50 was similar even three hours after spraying, regardless of the spray time. These results demonstrate that the persistence of the drug varies depending on the spray time when using a metered-dose aerosol that can spray large amounts of 1.0 mL or more.

[0058] Test Example 2: Insecticidal efficacy test against cockroaches 1. Preparation of stock solution 0.5 g of imiprothrin and 10 g of isopropyl myristate were measured out, and No. 1 kerosene (normal paraffin, "Neothiosol" manufactured by Chuo Kasei Co., Ltd., carbon number 11 to 15, specific gravity 0.761 (15°C)) was added and made up to 100 mL to prepare stock solution 4.

[0059] 2. Preparation of Metered-Dose Aerosols According to Table 5, metered-dose aerosols of Examples 6 to 9 and Comparative Examples 6 and 7 were prepared.

[0060] (Example 6) 46 mL of concentrate 4 was filled into an aerosol pressure can (volume 294 mL), and an aerosol valve (amount per injection: 1.0 mL, stem hole area: 1.4 mm 2 The pressure-resistant aerosol can was closed with a cap. Subsequently, 154 mL of dimethyl ether (DME) was filled under pressure as a propellant. A spray button (nozzle hole diameter: 1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin.

[0061] Example 7 A metered dose aerosol with a spray amount of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin was obtained in the same manner as in Example 6, except that the spray button was changed to one with an orifice diameter of 0.6 mm.

[0062] Comparative Example 6 A metered-dose aerosol spray with a spray amount of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin was obtained in the same manner as in Example 6, except that the spray button was changed to one with an orifice diameter of 0.4 mm.

[0063] (Example 8) The aerosol valve was set to a single injection volume of 1.0 mL and a stem hole area of ​​0.5 mm 2 A metered dose aerosol spray with a spray amount of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin was obtained in the same manner as in Example 6, except that the spray amount was changed to

[0064] (Example 9) The aerosol valve was set to a single injection volume of 1.0 mL and a stem hole area of ​​0.28 mm 2 A metered dose aerosol spray with a spray amount of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin was obtained in the same manner as in Example 6, except that the spray amount was changed to

[0065] (Comparative Example 7) The aerosol valve was set to a single injection amount of 1.0 mL and a stem hole area of ​​0.13 mm 2A metered dose aerosol spray with a spray amount of 1.0 mL per push and an ejection amount of 1.2 mg of imiprothrin was obtained in the same manner as in Example 6, except that the spray amount was changed to

[0066]

[0067] 3. Measurement of spray time The spray time of the metered dose aerosol was measured in the same manner as in Test Example 1. The results are shown in Table 6.

[0068] 4. Insecticidal Efficacy Test Against Smoky Brown Cockroaches As shown in Figure 2, a vinyl chloride cylinder 2 (diameter φ50 cm, height 15 cm) was placed on a floor covered with filter paper 1, and the interior of the cylinder served as the test area. Calcium carbonate was applied to the inner sidewall of cylinder 2 to prevent test insects from climbing up. A mark was made on filter paper 1 in the test area, close to the inner sidewall of cylinder 2, as target point 3 for spraying. A female Smoky Brown cockroach 5 was released into the test area as the test insect and allowed to acclimate for a while. When Smoky Brown Cockroach 5 reached target point 3, the spray button of a metered-volume aerosol sprayer was operated once (one push) from a distance of 50 cm, directed at Smoky Brown Cockroach 5. The time until the Smoky Brown Cockroach was knocked down (turned over and immobilized) was measured. The test was performed three times, and the average was calculated. The results are shown in Table 6.

[0069]

[0070] Examples 6-7 and Comparative Example 6 are examples in which the nozzle hole diameter of the spray button was changed in a metered-dose aerosol with a spray volume of 1 mL per push, and Examples 8-9 and Comparative Example 7 are examples in which the area of ​​the stem hole was changed. From the results in Table 6, it was found that Examples 6 and 7, with spray times of 0.3 seconds and 0.73 seconds, had significantly shorter knockdown times for Smoky-brown cockroaches than Comparative Example 6, with a spray time of 1.36 seconds, and that Examples 8 and 9, with spray times of 0.58 seconds and 0.73 seconds, had significantly shorter knockdown times for Smoky-brown cockroaches than Comparative Example 7, with a spray time of 1.2 seconds.

[0071] Test Example 3: Insecticidal efficacy test against houseflies 1. Preparation of stock solution 1.4 g of phthalthurin was measured out, and No. 1 kerosene (normal paraffin, "Neothiosol" manufactured by Chuo Kasei Co., Ltd., carbon number 11 to 15, specific gravity 0.761 (15°C)) was added thereto and made up to 100 mL to prepare stock solution 5.

[0072] 2. Preparation of Metered-Dose Aerosols According to Table 7, metered-dose aerosols of Examples 10 and 11 and Comparative Example 8 were prepared.

[0073] (Example 10) 40 mL of concentrate 5 was filled into an aerosol pressure can (volume 294 mL), and an aerosol valve (amount per injection: 1.0 mL, stem hole area: 1.4 mm 2 The pressure-resistant aerosol can was then closed with a cap. Subsequently, 160 mL of liquefied petroleum gas (0.29 MPa (25°C)) was pressurized and filled as a propellant. A spray button (nozzle hole diameter φ1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 1.0 mL per push and an ejection volume of 2.8 mg of phthalthrin.

[0074] (Example 11) A metered dose aerosol with a spray amount of 1.0 mL per push and an ejection amount of 2.8 mg of phthalthrin was obtained in the same manner as in Example 10, except that the spray button was changed to one with an orifice diameter of 0.6 mm.

[0075] (Comparative Example 8) A metered dose aerosol with a spray amount of 1.0 mL per push and an ejection amount of 2.8 mg of phthalthrin was obtained in the same manner as in Example 10, except that the spray button was changed to one with an orifice diameter of 0.4 mm.

[0076]

[0077] 3. Measurement of spray time The spray time of the metered dose aerosol was measured in the same manner as in Test Example 1. The results are shown in Table 8.

[0078] 4. Insecticidal efficacy test against houseflies: 8-tatami room (volume 31.1 m) 3A female housefly was released as a test insect into a test chamber (Fig. 1). When the housefly landed on the wall, the spray button of a metered-volume aerosol sprayer was operated once (one push) at the housefly from a distance of about 50 cm. The time until the housefly fell and was knocked down was measured. The test was performed three times and the average was calculated. The results are shown in Table 8.

[0079]

[0080] From the results in Table 8, it was found that Examples 10 and 11, in which the injection times were 0.32 seconds and 0.74 seconds, respectively, had significantly shorter knockdown times for houseflies than Comparative Example 8, in which the injection time was 1.36 seconds.

[0081] Test Example 4: Fragrance efficacy confirmation test 1. Preparation of stock solution 0.5 g of linalool was measured out, and absolute ethanol (specific gravity 0.785 (25°C)) was added to the solution to make up to 100 mL, to prepare stock solution 6.

[0082] 2. Preparation of Metered-Dose Aerosols According to Table 9, metered-dose aerosols of Example 12 and Comparative Example 9 were prepared.

[0083] (Example 12) 40 mL of concentrate 6 was filled into an aerosol pressure can (volume 294 mL), and an aerosol valve (amount per injection: 1.0 mL, stem hole area: 1.4 mm 2 The aerosol pressure can was closed with a cap. Subsequently, 160 mL of liquefied petroleum gas (0.29 MPa (25°C)) was pressurized and filled as a propellant. A spray button (nozzle hole diameter φ1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained with a spray volume of 1.0 mL per push and a discharge volume of 1.0 mg of linalool.

[0084] (Comparative Example 9) In the same manner as in Example 12, except that the spray button was changed to one with a nozzle hole diameter of φ0.4 mm, a fixed-dose aerosol was obtained with a spray amount of 1.0 mL per push and a discharge amount of linalool of 1.0 mg.

[0085]

[0086] 3. Measurement of spray time The spray time of the metered dose aerosol was measured in the same manner as in Test Example 1. The results are shown in Table 10.

[0087] 4. Aroma sensory test (sensory evaluation after 10 seconds of spraying) As shown in Figure 3, a 6-tatami room (volume 25 m) was sprayed. 3 The spray button of the metered-dose aerosol was operated once (one push) from a height of 100 cm above the floor at the center position F of the first wall 21 of the test chamber 20, directed toward the third wall 23 opposite the first wall 21 and approximately horizontally to the floor. 10 seconds after spraying, subjects stood at the spray position, center position F of the first wall 21, the center position G of the second wall 22 perpendicular to the first wall 21, and the center position H of the third wall 23 opposite the first wall 21, and evaluated the fragrance intensity according to the evaluation criteria of the 6-level odor intensity rating method. The test was conducted three times, and the average value was rounded to the nearest 1 / 2 orthogonal to the 6-level value. The results are shown in Table 10. [Evaluation criteria] 0: Odorless (a person with a normal sense of smell cannot detect the odor) 1: Odor that can barely be detected (detection threshold concentration) 2: Weak odor that can be identified (recognition threshold concentration) 3: Odor that can be easily detected 4: Strong odor 5: Overpowering odor

[0088] (Sensory evaluation 30 minutes after spraying) After checking the scent intensity 10 seconds after spraying, the test chamber 20 was left sealed, and after 30 minutes, the scent intensity was evaluated while standing at the center positions F to H of each wall. The test was performed three times, and the average value was rounded off to the nearest 1 / 6. The results are shown in Table 10.

[0089]

[0090] The results in Table 10 show that Example 12, which has an injection time of 0.31 seconds, is superior in fragrance spread and intensity after 30 minutes compared to Comparative Example 9, which has an injection time of 1.35 seconds, and is also superior in fragrance durability even after 30 minutes have passed.

[0091] Test Example 5: Sterilization efficacy confirmation test 1. Preparation of stock solution 20 g of isopropylmethylphenol (IPMP) was measured out, and 99.5% ethanol (specific gravity 0.785 (25°C)) was added thereto to make up to 100 mL, thereby preparing stock solution 7.

[0092] 2. Preparation of a metered-dose aerosol (Example 13) A pressure-resistant aerosol can (volume 294 mL) was filled with 60 mL of concentrate 7, and an aerosol valve (amount per injection: 1.0 mL, stem hole area: 1.4 mm 2 The pressure-resistant aerosol can was then sealed with a cap. Subsequently, 140 mL of liquefied petroleum gas (0.49 MPa (25°C)) was pressurized and filled as a propellant. A spray button (with a nozzle hole diameter of φ1.6 mm) was attached to the aerosol valve, and a metered-dose aerosol was obtained, with a spray volume of 1.0 mL per push and a discharge volume of 60 mg of IPMP.

[0093] 3. Measurement of spray time The spray time of the metered dose aerosol was measured in the same manner as in Test Example 1. The results are shown in Table 11.

[0094] 4. Efficacy Confirmation Test Bathrooms in 10 general households were cleaned to remove pink slime (mainly caused by Rhodotorula (yeast) or Methylobacterium (bacteria)) and black mold (mainly caused by Cladosporium (fungi)). Two locations where pink slime or black mold frequently occurs were then selected. One of the locations was targeted and the spray button of a metered-dose aerosol sprayer was pressed once (one push), designating the treated area as the treatment group. The other location was left untreated, and the chemical was not allowed to adhere to it, designating this area as the untreated group. For each household, the number of days after the bathroom cleaning and sample treatment that pink slime or black mold had appeared was determined. The test was conducted during the season when pink slime and black mold are likely to appear (June to September, Japan). The results are shown in Table 11.

[0095]

[0096] The results in Table 11 show that pink slime or black mold developed within one week in the untreated area, whereas the treated area sprayed with the metered dose aerosol of Example 13 achieved a sterilizing and antifungal effect for more than 10 days.

[0097] Although the present 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 present invention. This application is based on a Japanese patent application (Patent Application No. 2017-238160) filed on December 12, 2017, the contents of which are incorporated herein by reference.

[0098] 1 Filter paper 2 Cylinder 3 Target point 5 Smoked cockroach 10, 20 Test chamber 21 First wall 22 Second wall 23 Third wall A Center B to E Corner F to H Center position

Claims

1. A metered dose aerosol that sprays a fixed amount of aerosol composition with one spray operation, wherein the aerosol composition is composed of a concentrate containing a drug and a propellant, and is filled in a pressure-resistant container, and the amount of each spray is 1.0 to 3.0 mL, and the spray time is 0.8 seconds or less.

2. The metered dose aerosol according to claim 1, wherein the duration of each spray is 0.20 to 0.75 seconds.

3. The metered dose aerosol according to claim 1 or 2, wherein the concentrate further comprises a solvent.

4. A metered dose aerosol according to any one of claims 1 to 3, wherein the content of the drug in the concentrate is 0.01 to 70 mass / volume %.

5. A metered dose aerosol according to any one of claims 1 to 4, wherein the volume ratio of said concentrate to said propellant in said aerosol composition is 1:99 to 50:

50.

6. The metered dose aerosol according to any one of claims 1 to 5, wherein the agent is at least one selected from the group consisting of pest control components, fragrance components, deodorizing components, and disinfecting / sterilizing components.

7. A method for spraying a metered-volume aerosol, in which a pressure-resistant container is filled with an aerosol composition consisting of a concentrate containing a drug and a propellant, and the amount sprayed in one spray operation is 1.0 to 3.0 mL and the spray time is 0.8 seconds or less.

8. A method for improving the efficacy of a drug in an aerosol composition sprayed using a metered-dose aerosol, comprising spraying a fixed amount of the aerosol composition in the range of 1.0 to 3.0 mL within 0.8 seconds.