JP2014028779A - Grape insect pest extermination formulation and grape insect pest extermination method - Google Patents

Grape insect pest extermination formulation and grape insect pest extermination method Download PDF

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JP2014028779A
JP2014028779A JP2012170311A JP2012170311A JP2014028779A JP 2014028779 A JP2014028779 A JP 2014028779A JP 2012170311 A JP2012170311 A JP 2012170311A JP 2012170311 A JP2012170311 A JP 2012170311A JP 2014028779 A JP2014028779 A JP 2014028779A
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insecticidal component
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JP6001947B2 (en
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Mikihiko Shin
幹彦 新
Kazuya Onishi
和也 大西
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Earth Corp
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Abstract

PROBLEM TO BE SOLVED: To provide an insect pest extermination formulation that is excellent in safety and can obtain a high insect pest extermination effect.SOLUTION: A solid grape insect pest extermination formulation includes: an insecticidal component having a hard volatilization property at an atmospheric temperature; and a sublimable substance that has an easier volatilization property than that of the insecticidal component at an atmospheric temperature, and in the grape insect pest extermination formulation, a volume reduces with time or a form is broken with time by sublimation of the sublimable substance, a content of the insecticidal component in the formulation does not substantially reduce with time, and a concentration of the insecticidal component in the formulation increases with a balance change of a volume of the formulation and a content of the insecticidal component.

Description

本発明は、匍匐害虫駆除製剤および匍匐害虫を駆除する方法に関し、詳細には、安全性に優れ、高い害虫駆除効果を発揮する匍匐害虫駆除製剤、および該製剤を用いた匍匐害虫の駆除方法に関する。   The present invention relates to a moth pest control formulation and a method for controlling moth pests, and in particular, to a moth pest control formulation that exhibits excellent safety and a high pest control effect, and a method for controlling worm pests using the preparation .

従来の害虫駆除製剤(スプレー等)では、隙間や冷蔵庫の裏に潜んでいる害虫など、直接薬剤を処理することのできない害虫に対して、有効な量の殺虫成分を処理することが難しく、長いノズルを設けることや、噴射剤を増やし遠くまで薬液が届くようにし、大量に噴射することで隙間の奥まで薬剤を処理していた(特許文献1〜3参照)。しかし、大量のエアゾールを噴射すると、可燃性ガスが含まれるため、大量に処理すると引火するなどの危険があった。さらに、舞い散った薬を吸い込むなど安全性に問題がある場合もあった。
また、一度の接触で確実に駆除できるだけの致死量の殺虫成分を、予め害虫の通りそうな箇所に塗布等する方法も考えられるが、そのためには大量の薬剤が必要であり、さらには子供がその薬剤に直接触れるおそれがあるなどの、安全上の問題もあった。また、溶剤を含む薬液を多量に処理することで室内が汚れるなどの問題もあった。
In conventional pest control formulations (sprays, etc.), it is difficult to process an effective amount of an insecticidal component against pests that cannot be directly treated with chemicals, such as pests lurking in the gaps and refrigerators. The chemical | medical agent was processed to the back of the clearance gap by providing a nozzle, increasing a propellant so that a chemical | medical solution may reach far, and injecting in large quantities (refer patent documents 1-3). However, when a large amount of aerosol is injected, flammable gas is contained, and there is a danger of igniting if treated in large quantities. In some cases, there were safety issues such as inhaling scattered medicine.
In addition, a method of applying a lethal amount of an insecticidal component that can be surely controlled with a single contact to a place where a pest is likely to pass is considered. There were also safety issues such as the possibility of direct contact with the drug. In addition, there is a problem that the interior of the room becomes dirty by treating a large amount of a chemical solution containing a solvent.

特開2004−26278号公報JP 2004-26278 A 特開平8−259404号公報JP-A-8-259404 国際公開第2005/013685号International Publication No. 2005/013685

本発明は上記従来の問題に鑑み、安全性に優れ、かつ高い害虫駆除効果が得られる匍匐害虫駆除製剤を提供することを目的とする。   In view of the above-described conventional problems, an object of the present invention is to provide a moth pest control preparation which is excellent in safety and has a high pest control effect.

本発明者らは、鋭意研鑽を積んだ結果、下記構成により、上記目的を達成し得ることを見出し、本発明を完成するに至った。   As a result of earnest study, the present inventors have found that the above object can be achieved by the following constitution, and have completed the present invention.

すなわち、本発明は、以下の(1)から(4)に関するものである。
(1)常温で難揮散性の殺虫成分と、常温で前記殺虫成分よりも揮散しやすい昇華性物質とを含有する固形の匍匐害虫駆除製剤であって、
前記製剤は、前記昇華性物質の昇華によって、体積が経時的に減少するものか、または形状が経時的に崩壊するものであり、
前記製剤中の殺虫成分の含有量は、実質的に、経時的に減少しないものであり、
製剤の体積と、殺虫成分の含有量とのバランス変化にともない、製剤中における殺虫成分の濃度が増加する匍匐害虫駆除製剤。
(2)前記昇華性物質がイソプロピルトリオキサン、アダマンタン、メントール、ナフタレン、樟脳、及びパラジクロロベンゼンから選ばれる少なくとも1種である上記(1)に記載の匍匐害虫駆除剤。
(3)滑沢剤としてステアリン酸塩、タルク、酸化チタン、パラフィン、及び多価アルコールから選ばれる少なくとも1種を含む上記(1)または(2)に記載の匍匐害虫駆除剤。
(4)常温で難揮散性の殺虫成分と、常温で前記殺虫成分よりも揮散しやすい昇華性物質とを含有する固形の匍匐害虫駆除製剤であって、前記昇華性物質の昇華によって、体積が経時的に減少または形状が経時的に崩壊し、製剤の体積と、殺虫成分の含有量とのバランス変化にともない、殺虫成分の濃度が増加する固形の匍匐害虫駆除製剤を、害虫の生息しうる場所に設置する、匍匐害虫駆除方法。
That is, the present invention relates to the following (1) to (4).
(1) A solid insect pest control formulation comprising a non-volatile insecticidal component at room temperature and a sublimable substance that is more easily volatilized than the insecticidal component at room temperature,
The preparation is one whose volume decreases with time due to sublimation of the sublimable substance or whose shape collapses with time.
The content of the insecticidal component in the preparation is substantially not reduced over time,
A pest control formulation in which the concentration of the insecticidal component in the formulation increases as the balance between the volume of the formulation and the content of the insecticidal component changes.
(2) The pest control agent according to (1), wherein the sublimable substance is at least one selected from isopropyltrioxane, adamantane, menthol, naphthalene, camphor, and paradichlorobenzene.
(3) The pest control agent according to (1) or (2) above, which contains at least one selected from stearates, talc, titanium oxide, paraffin, and polyhydric alcohols as a lubricant.
(4) A solid insect pest control formulation comprising a non-volatile insecticidal component that is difficult to volatilize at room temperature and a sublimable substance that is more easily volatilized than the insecticidal component at room temperature, and the volume is reduced by sublimation of the sublimable substance. Insect pest control, a solid moth pest control formulation that increases in concentration as the amount of the insecticidal component increases and the balance of the volume of the formulation and the content of the insecticidal component changes as the volume decreases over time or the shape collapses over time A pest control method to be installed at the site.

本発明によれば、害虫、とりわけ匍匐害虫に対して優れた駆除効果を発揮し、さらには、製剤作製時には殺虫成分を低濃度で仕込んでも、製剤の外層の殺虫成分の経時的な濃縮により、害虫に対して致死量の薬剤を暴露させることが可能な、安全性や取扱性に優れた害虫駆除剤を提供することができる。   According to the present invention, it exerts an excellent controlling effect against pests, particularly moth pests, and further, even when charged with a low concentration of the insecticidal component at the time of preparation, the concentration of the insecticidal component in the outer layer of the formulation over time, It is possible to provide a pest control agent that is capable of exposing a lethal dose of a pest to a pest and is excellent in safety and handling.

本発明の匍匐害虫駆除製剤(以下「本発明の製剤」とも称する。)は、常温で難揮散性の殺虫成分と、殺虫成分よりも常温で揮散しやすい昇華性物質とを含有する。該製剤による害虫駆除機構は定かではないが、該昇華性物質が昇華することで経時的に製剤の殺虫成分が濃縮されることにより、虫体に付着する際、または、付着した後の虫体表面における殺虫成分濃度が、薬剤そのものと同程度になり、薬剤が体表に直接接触する作用の他、グルーミング行動による経口摂取を通じて害虫を死に至らしめるものと推測される。
したがって、本発明の製剤は、製剤調製時の殺虫成分の仕込み濃度が低くても、高い害虫駆除効果が得られるため、安全性が高く、取扱いも容易である。
The pest control formulation of the present invention (hereinafter also referred to as “the formulation of the present invention”) contains a non-volatile insecticidal component at room temperature and a sublimable substance that is easier to evaporate at room temperature than the insecticidal component. The pest control mechanism by the preparation is not clear, but when the sublimable substance is sublimated, the insecticidal component of the preparation is concentrated over time, so that the insect body adheres to the insect body or after the attachment. The concentration of the insecticidal component on the surface becomes the same as that of the drug itself, and it is presumed that the pest is killed through ingestion by grooming behavior in addition to the action of the drug directly contacting the body surface.
Therefore, the preparation of the present invention is highly safe and easy to handle because a high pest control effect can be obtained even if the concentration of the insecticidal component used at the preparation of the preparation is low.

本発明の製剤に含まれる殺虫成分としては、常温で難揮散性の殺虫成分であればよい。ここで難揮散性とは、25℃における蒸気圧が1.0×10−4Pa未満であることを意味する。25℃における蒸気圧が1.0×10−Pa未満であれば、製剤中の殺虫成分の含有量は実質的に減少しない。ここで実質的に減少しないとは、常温2週間における減少量が5%以下のことを示す。殺虫成分が難揮散性であれば、担体の役割を担う昇華性物質が先に昇華することにより製剤中の殺虫成分濃度が上昇する。具体的には、例えば、ジノテフラン、ペルメトリン、イミプロトリン、ビフェントリン等の殺虫成分が挙げられる。殺虫成分は1種を単独で用いても、2種以上を併用してもよい。また、殺虫成分は、製剤全体の質量に対して0.001質量%〜20質量%であることが好ましく、0.001質量%〜10質量%であることがより好ましい。 The insecticidal component contained in the preparation of the present invention may be any insecticidal component that is hardly volatile at room temperature. Here, “non-volatile” means that the vapor pressure at 25 ° C. is less than 1.0 × 10 −4 Pa. If it is less than 1.0 × 10- 4 Pa vapor pressure at 25 ° C., the content of the insecticidal ingredient in the formulation does not substantially decrease. Here, “substantially not reduced” means that the amount of reduction at room temperature for 2 weeks is 5% or less. If the insecticidal component is non-volatile, the concentration of the insecticidal component in the preparation is increased by sublimating the sublimable substance that plays the role of the carrier first. Specific examples include insecticidal components such as dinotefuran, permethrin, imiprothrin, bifenthrin and the like. One insecticide component may be used alone, or two or more insecticide components may be used in combination. Moreover, it is preferable that an insecticidal component is 0.001 mass%-20 mass% with respect to the mass of the whole preparation, and it is more preferable that it is 0.001 mass%-10 mass%.

また、本発明の製剤に含まれる昇華性物質としては、殺虫成分よりも常温で揮散しやすいもの、好ましくは殺虫成分よりも蒸気圧が高いものであれば限定されず、例えば、イソプロピルトリオキサン(商品名「サンサブリB」、小川香料(株)製)、アダマンタン、ネオペンチルグリコール、パラジクロロベンゼン、ナフタレン、樟脳、メントール、ヒドロキノン等が挙げられる。この中でも、刺激が少なく、身体への安全性が高いという観点から、プロピルトリオキサン、アダマンタン、メントールが好ましい。さらに、打錠として用いる場合には、賦形性が高いという点でイソプロピルトリオキサン、アダマンタンが特に好ましい。また、昇華性物質の蒸気圧が殺虫成分の蒸気圧に対して10Pa以上高いことが好ましい。   In addition, the sublimable substance contained in the preparation of the present invention is not limited as long as it is more easily vaporized at room temperature than the insecticidal component, and preferably has a higher vapor pressure than the insecticidal component. Name “Sunsaburi B” (manufactured by Ogawa Fragrance Co., Ltd.), adamantane, neopentyl glycol, paradichlorobenzene, naphthalene, camphor, menthol, hydroquinone and the like. Among these, propyltrioxane, adamantane, and menthol are preferable from the viewpoint of low irritation and high safety to the body. Furthermore, when used as a tablet, isopropyltrioxane and adamantane are particularly preferable in terms of high formability. Moreover, it is preferable that the vapor pressure of the sublimable substance is 10 Pa or more higher than the vapor pressure of the insecticidal component.

昇華性物質の含有量は、製剤全体の質量に対して50質量%〜99.999質量%であることが好ましく、70質量%〜99.99質量%であることがより好ましい。
なお、これら昇華性物質には、製剤の害虫の虫体表面への付着性を向上させる働きもある。
The content of the sublimable substance is preferably 50% by mass to 99.999% by mass and more preferably 70% by mass to 99.99% by mass with respect to the mass of the entire preparation.
These sublimable substances also have a function of improving the adherence of the preparation to the insect pest surface.

本発明の製剤により駆除する対象害虫としては、例えば、農業害虫、貯穀害虫、衛生害虫、不快害虫等が挙げられる。より具体的には、ゴキブリ、トコジラミ、ムカデ、ヤスデ、ダンゴムシ等が挙げられる。中でも、ゴキブリ等の匍匐害虫に対して、特に高い駆除効果を発揮する。   Examples of the target pests to be controlled by the preparation of the present invention include agricultural pests, stored grain pests, hygiene pests, and unpleasant pests. More specifically, cockroaches, bed bugs, centipedes, millipedes, dandelions and the like can be mentioned. Above all, it exhibits a particularly high control effect against worms such as cockroaches.

本発明の製剤は固形の製剤である。剤形が固形であることにより、製造時と取り扱い時の利便性が高く好ましい。具体的には、一定の形状に整えた打錠剤、丸剤、散剤、顆粒剤、等が挙げられる。中でも、打錠剤、顆粒剤が好ましく、害虫の生息し得る場所に設置する定置型の打錠剤であることがより好ましい。   The preparation of the present invention is a solid preparation. The solid dosage form is preferable because it is highly convenient during production and handling. Specific examples include tableting tablets, pills, powders, granules, and the like arranged in a certain shape. Among these, tableting tablets and granules are preferable, and stationary tableting installed in a place where pests can live is more preferable.

本製剤は、昇華性物質の昇華に伴い、製剤の体積は経時的に減少するか、製剤の形状が経時的に崩壊する。これに対し、殺虫成分は常温で難揮散性であるため、製剤中における含有量は実質的に、経時的に減少しない。その結果、製剤の体積と、殺虫成分の含有量とのバランス変化にともない、製剤における殺虫成分濃度が経時的に上昇する。そのために、製剤作製時の殺虫成分濃度が本来は害虫が死に至らない程度の低い濃度であっても、害虫の虫体表面に付着して、殺虫成分原体の濃度と同程度まで高くなる。そして、該製剤は害虫の体表に直接接触する作用の他、グルーミング行動により、径口摂取されることで、害虫駆除効果が十分に得られる。製剤中の殺虫成分の濃縮は少なくとも製剤外層で発現し、製剤内部でも徐々に進行すると考えられる。   In the present preparation, as the sublimable substance is sublimated, the volume of the preparation decreases with time or the shape of the preparation collapses with time. On the other hand, since the insecticidal component is hardly volatile at room temperature, the content in the preparation does not substantially decrease with time. As a result, the concentration of the insecticidal component in the preparation increases with time as the balance between the volume of the preparation and the content of the insecticidal component changes. Therefore, even if the concentration of the insecticidal component at the time of preparation is low enough not to cause the pest to die, it adheres to the surface of the insect pest and increases to the same level as the concentration of the insecticidal component drug substance. In addition to the effect of directly contacting the body surface of the pest, the preparation can be sufficiently ingested by a grooming action to sufficiently obtain a pest control effect. It is considered that the concentration of the insecticidal component in the preparation is expressed at least in the outer layer of the preparation and gradually proceeds inside the preparation.

また、昇華性物質の昇華に伴い、製剤の体積は経時的に減少するか、製剤の形状が経時的に崩壊するため、製剤が微細化しやすい。微細化した製剤に対して、まだ昇華せずに残存している昇華性物質が展着剤の役割を果たし、虫体表面に殺虫成分が付着しやくなると考えられる。
虫体表面に付着した製剤は、昇華性物質の昇華によって殺虫成分濃度上昇がさらに進み、虫体自身のグルーミングや他虫体との接触により、害虫自らが殺虫成分を伝播する。
虫体に付着した殺虫成分は、定かではないが、直接の接触の他、経口摂取され、害虫を死に至らしめるという経路が考えられる。
In addition, as the sublimable substance sublimates, the volume of the preparation decreases with time, or the shape of the preparation collapses with time, and thus the preparation is easily miniaturized. It is considered that the sublimable substance that has not yet sublimated yet acts as a spreading agent on the micronized preparation, and the insecticidal component easily adheres to the surface of the worm body.
In the preparation adhered to the surface of the insect body, the concentration of the insecticidal component is further increased by sublimation of the sublimable substance, and the insect body itself propagates the insecticidal component by the grooming of the insect body itself or contact with other insect bodies.
Although the insecticidal component adhering to the worm body is not certain, there is a route through which it can be taken orally and lead to the death of the pest in addition to direct contact.

本発明の製剤は、さらに、ステアリン酸マグネシウム、ステアリン酸カルシウム、タルク、フマル酸ステアリルナトリウム、ステアリン酸、パラフィン、カルナウバロウ、多価アルコール、軽質無水ケイ酸、含水二酸化ケイ素等の添加剤、滑沢剤を1種以上配合してもよい。これらを含有することにより製剤の賦型性、安定性、加工性や害虫への付着性が向上する。これらの製剤における含有量は0.1〜2.0質量%であることが好ましい。   The preparation of the present invention further includes additives such as magnesium stearate, calcium stearate, talc, sodium stearyl fumarate, stearic acid, paraffin, carnauba wax, polyhydric alcohol, light anhydrous silicic acid, hydrous silicon dioxide, and a lubricant. You may mix | blend 1 or more types. By containing these, the formability, stability, processability and adhesion to pests of the preparation are improved. The content in these preparations is preferably 0.1 to 2.0% by mass.

特にステアリン酸マグネシウムは、製剤の保形剤的役割を果たして、昇華性物質の昇華による製剤の早すぎる崩壊を防ぐ効果が期待できる。これにより、製剤外層の殺虫成分濃度が、害虫駆除に充分な程高くなると共に、必要に応じた効果維持期間を持たせることが可能となり、一定期間は害虫の駆除効果を発揮するので、より好ましい。   In particular, magnesium stearate plays a role as a shape-retaining agent of the preparation, and can be expected to prevent premature disintegration of the preparation due to sublimation of the sublimable substance. As a result, the concentration of the insecticidal component in the outer layer of the preparation is sufficiently high for pest control, and it is possible to have an effect maintenance period as necessary, and it is more preferable because it exerts a pest control effect for a certain period of time. .

本発明の製剤には、上記の成分のほかに、例えば保形剤、展着剤、コーティング剤、賦形剤、結合剤、誤食防止剤、安定化剤、吸着剤、香料、着色剤等の各種添加剤を適宜配合してもよい。   In the preparation of the present invention, in addition to the above-mentioned components, for example, a shape-retaining agent, a spreading agent, a coating agent, an excipient, a binder, an anticorrosive agent, a stabilizer, an adsorbent, a fragrance, a coloring agent, etc. These various additives may be appropriately blended.

以下に実施例を挙げ、本発明を詳細に説明するが、本発明はこれらの実施例によって限定されるものではない。   EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples.

<実施例1−1〜1−12>
下記条件に基づき、方法1〜4によって昇華性物質の種類を変化させて害虫駆除効果を確認した。
製剤処方(10g);
ジノテフラン(殺虫成分) 1.0質量%
ステアリン酸マグネシウム 0.5質量%
昇華性物質 98.5質量%
昇華性物質としては、イソプロピルトリオキサン、アダマンタン、メントール、ナフタレン、樟脳、及びパラジクロロベンゼンを使用した。
<Examples 1-1 to 1-12>
Based on the following conditions, the type of the sublimable substance was changed by methods 1 to 4, and the pest control effect was confirmed.
Formulation formulation (10 g);
Dinotefuran (insecticidal component) 1.0% by mass
Magnesium stearate 0.5% by mass
98.5% by mass of sublimable substances
As the sublimable substance, isopropyltrioxane, adamantane, menthol, naphthalene, camphor, and paradichlorobenzene were used.

(方法1)
ジノテフラン、ステアリン酸マグネシウムおよび各昇華性物質を混合し、油圧式ポンプと金型を用いて300kg・f/mの圧力で厚さ6mm、直径9mmの打錠剤(0.3g)を成形した。
(方法2)
試験空間となるプラスチックケース(縦18cm×横25cm×高さ10cm)に、ゴキブリ用シェルター、固形飼料、および水を設置した。
(方法3)
供試虫として感受性チャバネゴキブリ雌雄各10頭の計20頭と、クロゴキブリ雌雄各5頭の計10頭をそれぞれの試験空間に放ち、試験空間温度25℃、湿度60%の条件で1日馴化後、検体である打錠剤を固形飼料と水の間に設置して試験を開始した。対照試験区として、固形飼料と水のみを設置した試験区を感受性チャバネゴキブリ、クロゴキブリそれぞれに設けた。
(方法4)
経時的にノックダウン頭数と致死頭数をカウントし、下記式(1)により致死率(%)(ノックダウン含む)を算出した。
検体致死率
=(致死数/供試虫全数)×100 (1)
使用した昇華性物質ごとの効力試験の結果を表1に示す。
(Method 1)
Dinotefuran, magnesium stearate and each sublimable substance were mixed, and a tablet (0.3 g) having a thickness of 6 mm and a diameter of 9 mm was formed using a hydraulic pump and a mold at a pressure of 300 kg · f / m 2 .
(Method 2)
A cockroach shelter, solid feed, and water were installed in a plastic case (18 cm long × 25 cm wide × 10 cm high) serving as a test space.
(Method 3)
A total of 20 susceptible German cockroaches, 10 males and 10 males, and 5 black and white cockroaches, males and females, were released into each test space as test worms, and acclimated for 1 day under conditions of a test space temperature of 25 ° C and humidity of 60%. The test was started by placing a tablet as a specimen between solid feed and water. As control test plots, test plots with only solid feed and water were provided for each sensitive German cockroach and black cockroach.
(Method 4)
The number of knockdowns and the number of lethals were counted over time, and the lethality (%) (including knockdown) was calculated by the following formula (1).
Specimen mortality rate = (lethal number / total number of test insects) x 100 (1)
Table 1 shows the results of the efficacy test for each sublimable substance used.

Figure 2014028779
Figure 2014028779

表1より、検体設置1日後は昇華性物質の違いにより、致死効果に差が見られたものの、検体設置2日後には、害虫の種類や昇華性物質の種類に因ることなく、全検体で90%以上の高い致死率を示した。   According to Table 1, although the difference in lethal effect was observed one day after the specimen was installed due to the difference in sublimable substances, all specimens were observed two days after the specimen was installed, regardless of the type of pest or the sublimable substance. Showed a high mortality rate of over 90%.

以上のことから、本発明の製剤は、昇華性物質の種類によって、薬剤としての効果発現までに要する時間に差があるものの、いずれも害虫の駆除に有効であることが確認された。   From the above, it was confirmed that all of the preparations of the present invention are effective in controlling pests, although there are differences in the time required to develop the effect as a drug depending on the type of sublimable substance.

<実施例2−1〜2−6および比較例2−1〜2−2>
下記条件に基づき、方法1〜4によって昇華性物質または非昇華性物質を基剤に用いた場合の害虫駆除効果を確認した。
製剤処方(0.7g):
ジノテフラン(殺虫成分) 表2に示す含有量(質量ppm)
基剤 残部
基剤としては、昇華性物質であるイソプロピルトリオキサン、または非昇華性物質であるケイ酸カルシウム(商品名:フローライトRN)を用いた。
<Examples 2-1 to 2-6 and Comparative Examples 2-1 to 2-2>
Based on the following conditions, the insect pest control effect when using a sublimable substance or a non-sublimable substance as a base was confirmed by methods 1 to 4.
Formulation formulation (0.7 g):
Dinotefuran (insecticidal component) Content shown in Table 2 (mass ppm)
Base Remaining As the base, isopropyltrioxane, which is a sublimation substance, or calcium silicate (trade name: Florite RN), which is a non-sublimation substance, was used.

(方法1)
ジノテフランと各基剤を混合し、油圧式ポンプと金型を用いて300kg・f/mの圧力で厚さ3mm、直径20mmの打錠剤(0.7g)を成形した。
(方法2)
試験空間となるプラスチックケース(縦18cm×横25cm×高さ10cm)に紙製のシェルター、固形飼料、および水を設置した。
(方法3)
供試虫として感受性チャバネゴキブリ雌雄各5頭の計10頭とクロゴキブリ雌雄各5頭の計10頭をそれぞれの試験空間に放ち、試験空間温度25℃、湿度60%の条件で1日間馴化後、検体である打錠剤を固形飼料と水の間に設置して試験を開始した。対照試験区として、固形飼料と水のみを設置した試験区を、感受性チャバネゴキブリ、クロゴキブリそれぞれに設けた。
(方法4)
経時的にノックダウン頭数と致死頭数をカウントし、実施例1−1と同様の式(1)により致死率(%)を算出した。
結果を表2に示す。
(Method 1)
Dinotefuran and each base were mixed, and a tablet (0.7 g) having a thickness of 3 mm and a diameter of 20 mm was formed using a hydraulic pump and a mold at a pressure of 300 kg · f / m 2 .
(Method 2)
A paper shelter, solid feed, and water were placed in a plastic case (vertical 18 cm × width 25 cm × height 10 cm) serving as a test space.
(Method 3)
A total of 10 susceptible cockroach males and 5 males and 5 male and female black cockroaches were released as test insects in each test space, and acclimated for 1 day under conditions of a test space temperature of 25 ° C. and a humidity of 60%. The test was started by placing a tablet tablet as a specimen between solid feed and water. As control test plots, test plots with only solid feed and water were provided in each of the sensitive German cockroaches and black cockroaches.
(Method 4)
The number of knockdowns and the number of lethals were counted over time, and the lethality (%) was calculated by the same formula (1) as in Example 1-1.
The results are shown in Table 2.

Figure 2014028779
Figure 2014028779

以上のことから、非昇華性物質を基剤とした場合には、全く害虫防除効果が得られない殺虫成分濃度であっても、本発明の製剤では昇華性物質を基剤とすることにより高い駆除効果が得られることが確認された。   From the above, when a non-sublimable substance is used as a base, the concentration of the insecticidal component at which no pest control effect can be obtained is high by using the sublimable substance as a base in the preparation of the present invention. It was confirmed that the extermination effect was obtained.

<実施例3−1〜3−4および比較例3−1〜3−2>
下記条件に基づき、方法1〜3によって製剤中の製剤の崩壊性について確認した。
製剤処方(100g):
ジノテフラン(殺虫成分) 1.0質量%
ステアリン酸マグネシウム 0.5質量% または なし
イソプロピルトリオキサン(昇華性物質) 98.5質量% または 99.0質量%
<Examples 3-1 to 3-4 and Comparative Examples 3-1 to 3-2>
Based on the following conditions, the disintegration property of the preparation in the preparation was confirmed by methods 1 to 3.
Formulation formulation (100 g):
Dinotefuran (insecticidal component) 1.0% by mass
Magnesium stearate 0.5% by mass or none Isopropyltrioxane (sublimable substance) 98.5% by mass or 99.0% by mass

(方法1)
殺虫成分、昇華性物質(イソプロピルトリオキサン)、および、必要に応じてステアリン酸マグネシウムを混合し、油圧式ポンプと金型を用いて300kg・f/mの圧力で厚さ6mm、直径9mmの打錠剤(0.3g)を成形した。
(方法2)
製剤の外観を観察しやすくするためにプラスチックカップの底面に黒色画用紙を敷き、その上に製剤を1錠置いた状態で、25℃で24日間、30℃で30日間の恒温条件下にそれぞれ静置し、経時的に製剤の重量減少を観察した。
(方法3)
得られた製剤の重量変化(同様の試験を3回行った平均減少量)から下記算出式により製剤0.3gにおける推定持続期間を求めた。結果を表3に示す。
0.3gにおける推定持続期間=昇華性物質の重量/日平均減少量
(Method 1)
Insecticidal ingredients, sublimable substance (isopropyltrioxane), and magnesium stearate as necessary are mixed, and using a hydraulic pump and a mold, the pressure is 300 kg · f / m 2 with a thickness of 6 mm and a diameter of 9 mm. Tablets (0.3 g) were formed.
(Method 2)
In order to make it easy to observe the appearance of the preparation, a black drawing paper is placed on the bottom of the plastic cup, and one tablet is placed on the paper, and then statically placed at 25 ° C. for 24 days and 30 ° C. for 30 days. The weight loss of the preparation was observed over time.
(Method 3)
The estimated duration in 0.3 g of the preparation was determined from the change in the weight of the obtained preparation (average reduction amount obtained by conducting the same test three times) according to the following formula. The results are shown in Table 3.
Estimated duration at 0.3 g = weight of sublimable substance / average daily reduction

Figure 2014028779
Figure 2014028779

表3より、実施例3−3と比較例3−1、及び実施例3−4と比較例3−2との結果から、昇華性物質に殺虫成分を混合させた場合でも、昇華性物質単体と製剤の平均減少量は変わらないことが分かる。また、実施例3−1〜3−4の結果から、殺虫成分と昇華性物質とを含む製剤にステアリン酸マグネシウムを混合させても、製剤の減少量および持続期間に顕著な差が見られないことが確認された。   From Table 3, from the results of Example 3-3 and Comparative Example 3-1, and Example 3-4 and Comparative Example 3-2, the sublimable substance alone even when the insecticidal component was mixed with the sublimable substance. It can be seen that the average decrease in the formulation does not change. In addition, from the results of Examples 3-1 to 3-4, even when magnesium stearate is mixed with a preparation containing an insecticidal component and a sublimable substance, there is no significant difference in the amount of reduction and the duration of the preparation. It was confirmed.

<実施例4、比較例4>
下記条件に基づき、製剤について、経時的な殺虫成分濃度変化を確認した。
実施例4:製剤処方(100g);
ジノテフラン(殺虫成分) 10.0重量%
ステアリン酸マグネシウム 0.5重量%
イソプロピルトリオキサン(昇華性物質) 89.5重量%
比較例4:製剤処方(100g);
ジノテフラン(殺虫成分) 10.0重量%
ケイ酸カルシウム(非昇華性物質) 90.0重量%
上記処方を混合し、直径20mm、高さ10mmの打錠剤(7g)を作製した。打錠剤を40℃の恒温室に静置した。一定期間ごとに製剤の重量を測定し、下記所定の条件にて殺虫成分含量を測定した。殺虫成分含有量と製剤重量とから、殺虫成分濃度を算出した。同様の試験を3回行った平均値での結果を表4に示す。
<Example 4, comparative example 4>
Based on the following conditions, the change in insecticidal component concentration over time was confirmed for the preparation.
Example 4: Formulation formulation (100 g);
Dinotefuran (insecticidal component) 10.0% by weight
Magnesium stearate 0.5% by weight
Isopropyltrioxane (sublimable substance) 89.5% by weight
Comparative Example 4: Formulation formulation (100 g);
Dinotefuran (insecticidal component) 10.0% by weight
Calcium silicate (non-sublimable substance) 90.0% by weight
The above formulation was mixed to produce a tablet (7 g) having a diameter of 20 mm and a height of 10 mm. The tablet was placed in a constant temperature room at 40 ° C. The weight of the preparation was measured at regular intervals, and the insecticidal component content was measured under the following predetermined conditions. The insecticidal component concentration was calculated from the insecticidal component content and the formulation weight. Table 4 shows the average results of three similar tests.

<殺虫成分含有量分析方法>
・製剤全量(ジノテフラン約700mg相当)を粉砕し、サンプル瓶に入れた。
・サンプル瓶にメタノール40mlを加え、1時間超音波抽出を行った。
・内標として4−アミノ安息香酸を5ml加え、撹拌した。
(80mg/5mLメタノール溶液)
・一部を採取し、移動相で100倍に希釈した。
・サンプルを孔径0.2μmのメンブレンフィルターでろ過処理し、分析用試料とした。
・移動相として超純水:アセトニトリル=93:7の混合溶媒に10mMリン酸二水素カリウムを加えた溶液を使用し、下記条件にてHPLC分析を行った。
<Insecticide content analysis method>
-The whole preparation (equivalent to about 700 mg of dinotefuran) was pulverized and placed in a sample bottle.
-40 ml of methanol was added to the sample bottle, and ultrasonic extraction was performed for 1 hour.
-As an internal standard, 5 ml of 4-aminobenzoic acid was added and stirred.
(80 mg / 5 mL methanol solution)
A portion was collected and diluted 100 times with mobile phase.
-The sample was filtered through a membrane filter having a pore size of 0.2 µm to obtain a sample for analysis.
-HPLC analysis was performed under the following conditions using a solution obtained by adding 10 mM potassium dihydrogen phosphate to a mixed solvent of ultrapure water: acetonitrile = 93: 7 as a mobile phase.

(HPLC分析条件)
分析機器:Shimadzu HPLC LC−3000
検出器:UV (測定波長:270nm)
流速:1.0mL/min
注入量:1μL
分析カラム:Inertsil ODS φ4.0×250mm(ジーエルサイエンス社製)
(HPLC analysis conditions)
Analytical instrument: Shimadzu HPLC LC-3000
Detector: UV (Measurement wavelength: 270 nm)
Flow rate: 1.0 mL / min
Injection volume: 1 μL
Analysis column: Inertsil ODS φ4.0 × 250 mm (manufactured by GL Sciences Inc.)

Figure 2014028779
Figure 2014028779

表4に示すように、イソプロピルトリオキサン(昇華性物質)を用いた実施例4に対し、ケイ酸カルシウム(非昇華性物質)を使用した比較例4の製剤では、35日経過しても殺虫成分濃度に経時的変化は確認できなかった。   As shown in Table 4, in contrast to Example 4 using isopropyltrioxane (sublimation substance), the formulation of Comparative Example 4 using calcium silicate (non-sublimation substance) was an insecticidal component even after 35 days. No change in concentration over time could be confirmed.

<実施例5−1>
実施例1−1と同様の処方で作製した打錠剤(殺虫成分濃度1.0質量%)2錠を8.8mの空間に設置し、供試虫であるチャバネゴキブリ雌雄各10頭の計20頭を試験空間に放ち、致死効果の経時変化を確認し、前述の式(1)及び次式(2)を用いて、自然死の値(コントロール致死率)から補正した補正致死率を算出した。
検体致死率
=(致死数/供試虫全数)×100 (1)
補正致死率
=(検体致死率−コントロール致死率)/(1−コントロール致死率) (2)
式(2)の補正致死率とは、検体の自然死による致死率を元にしたコントロール致死率を用いて算出することができる。
<Example 5-1>
Two tablets (pesticide component concentration: 1.0% by mass) prepared in the same manner as in Example 1-1 were placed in a space of 8.8 m 2 and a total of 20 male and female cockroach cockroach males and females were used. The head was released into the test space, the change in lethal effect over time was confirmed, and the corrected lethality corrected from the natural death value (control lethality) was calculated using the above formula (1) and the following formula (2). .
Specimen mortality rate = (lethal number / total number of test insects) x 100 (1)
Corrected lethality = (specimen lethality−control lethality) / (1−control lethality) (2)
The corrected lethality rate in equation (2) can be calculated using a control lethality rate based on the lethality rate due to the natural death of the specimen.

<実施例5−2>
前記実施例5−1に対して、殺虫成分濃度を1/10(0.1質量%)とした打錠剤を、実施例5−1の10倍の錠数(20錠)同空間に設置し、実施例5−1と同様に供試虫であるチャバネゴキブリに対する致死効果の経時変化を確認し、補正致死率を算出した。
<Example 5-2>
A tablet with an insecticidal component concentration of 1/10 (0.1% by mass) with respect to Example 5-1 was placed in the same space as the tablet 10 times as many as Example 5-1 (20 tablets). In the same manner as in Example 5-1, the change over time in the lethal effect on the test insect, German cockroach was confirmed, and the corrected lethality was calculated.

実施例5−1及び5−2の結果を表5に示す。   The results of Examples 5-1 and 5-2 are shown in Table 5.

Figure 2014028779
Figure 2014028779

表5より、製剤中の殺虫成分濃度を1/10に低くし、設置製剤数を10倍とすると、駆除効果が発現するまでの時間は遅くなる。他方、製剤の設置から3日経過後における致死率には差が見られないことから、製剤作製時の殺虫成分が低濃度の製剤であっても、設置する製剤の数を増やすことにより、殺虫成分が高濃度の製剤と同様の駆除効果が得られることが確認された。このことから、本発明における製剤は、殺虫成分の仕込み濃度が低くても、昇華性物質の昇華により製剤外層の殺虫成分が濃縮されるため、害虫駆除に十分な効果を発揮できることが分かる。   From Table 5, when the insecticidal component concentration in the preparation is reduced to 1/10 and the number of installed preparations is 10 times, the time until the extermination effect appears is delayed. On the other hand, since there is no difference in lethality after 3 days from the installation of the preparation, even if the insecticidal ingredient at the time of preparation preparation is a low concentration preparation, by increasing the number of preparations to install, However, it was confirmed that the same disinfecting effect as that of the high concentration preparation was obtained. From this, it can be seen that the preparation according to the present invention can exert a sufficient effect on pest control because the insecticide in the outer layer of the preparation is concentrated by sublimation of the sublimable substance even if the concentration of the insecticide is low.

<実施例6−1、6−2>
下記条件に基づき、方法1〜2によって害虫駆除効果を確認した。
製剤処方(100g);
ジノテフラン(殺虫成分) 1.0質量%
イソプロピルトリオキサン(昇華性物質) 99.0質量%
<Examples 6-1 and 6-2>
Based on the following conditions, the pest control effect was confirmed by methods 1-2.
Formulation formulation (100 g);
Dinotefuran (insecticidal component) 1.0% by mass
Isopropyltrioxane (sublimable substance) 99.0% by mass

(方法1)
ジノテフランと昇華性物質とを混合し、油圧式ポンプと金型を用いて300kg・f/mの圧力で厚さ6mm、直径9mmの打錠剤(0.3g)を成形した。
(方法2)
方法1で得られた打錠剤を1錠または5錠、8.8mの空間に設置し、供試虫であるクロゴキブリに対する致死効果の経時変化を確認し、実施例5−1の前記式(2)を用いて、自然死の値から補正した補正致死率を算出した。結果を表6に示す。
(Method 1)
Dinotefuran and a sublimable substance were mixed, and a tablet (0.3 g) having a thickness of 6 mm and a diameter of 9 mm was formed using a hydraulic pump and a mold at a pressure of 300 kg · f / m 2 .
(Method 2)
One tablet or five tablets obtained by method 1 were placed in a space of 8.8 m 2 , and the change over time of the lethal effect against black wagtails as test insects was confirmed. The above formula of Example 5-1 Using (2), the corrected lethality corrected from the value of natural death was calculated. The results are shown in Table 6.

Figure 2014028779
Figure 2014028779

また、表6より、設置する製剤の個数を増やすことにより、害虫に対する即効性が向上することが分かる。一方、製剤の個数が少ない場合であっても、害虫を駆逐するために時間は掛かるが、十分な害虫駆除効果を得られることが確認された。   Moreover, it can be seen from Table 6 that the immediate effect on pests is improved by increasing the number of preparations to be installed. On the other hand, it was confirmed that even if the number of the preparations was small, a sufficient pest control effect could be obtained although it took time to eliminate the pests.

<比較例5>
下記条件に基づき、方法1〜3によって害虫防除効果を確認した。
製剤処方(100mL)
ジノテフラン(殺虫成分) 7.5g
メタノール(溶剤) 適量
<Comparative Example 5>
Based on the following conditions, the pest control effect was confirmed by methods 1-3.
Formulation (100mL)
Dinotefuran (insecticidal component) 7.5g
Methanol (solvent) appropriate amount

(方法1)
縦5cm×横5cm×厚さ2mmの塩化ビニル製の板に製剤1mLを塗布し、メタノールを風乾させ、検体とした。
(方法2)
1mのバット内に紙製シェルター入りの木箱(縦25cm×横35cm×高さ25cm、一部に高さ1cm、幅5cmの開口を設けた)を設置し、同バットに供試虫としてチャバネゴキブリ雌雄各25頭を入れ、25℃の条件で1日馴化後、検体を設置した。
(方法3)
経時的に、供試虫のノックダウン(KD)数および致死数をカウントし、実施例5−1で用いた式(2)を用いて、自然死の値から補正した補正致死率を算出した。
結果を表7に示す。
(Method 1)
1 mL of the preparation was applied to a vinyl chloride plate having a length of 5 cm, a width of 5 cm, and a thickness of 2 mm, and methanol was air-dried to prepare a specimen.
(Method 2)
A wooden box with a paper shelter (length 25 cm x width 35 cm x height 25 cm, with an opening 1 cm in height and 5 cm in width provided in part) in a 1 m 2 bat. Twenty-five German cockroaches were placed and acclimated for one day under the condition of 25 ° C., and then a specimen was placed.
(Method 3)
Over time, the knock-down (KD) number and the lethal number of the test insects were counted, and the corrected lethality corrected from the natural death value was calculated using the formula (2) used in Example 5-1. .
The results are shown in Table 7.

Figure 2014028779
Figure 2014028779

表7の結果より、殺虫成分を含有させる基剤に昇華性物質を用いない場合は、経時的な致死率の向上はみられないことが分かる。昇華性物質を含み、殺虫成分含有量が同条件の上記実施例6−1(1錠設置)では、前述のように致死効果の経時変化が確認できた。   From the results in Table 7, it can be seen that when the sublimable substance is not used as the base containing the insecticidal component, the lethality is not improved over time. In Example 6-1 (one tablet installed) containing a sublimable substance and having the same insecticidal component content, the change over time in the lethal effect was confirmed as described above.

<処方例>
本発明の匍匐害虫駆除製剤の処方例(合計100g)を下記表8に示す。
<Prescription example>
Table 8 below shows formulation examples (total 100 g) of the pest control formulation of the present invention.

Figure 2014028779
Figure 2014028779

Claims (4)

常温で難揮散性の殺虫成分と、常温で前記殺虫成分よりも揮散しやすい昇華性物質とを含有する固形の匍匐害虫駆除製剤であって、
前記製剤は、前記昇華性物質の昇華によって、体積が経時的に減少するものか、または形状が経時的に崩壊するものであり、
前記製剤中の殺虫成分の含有量は、実質的に、経時的に減少しないものであり、
製剤の体積と、殺虫成分の含有量とのバランス変化にともない、製剤中における殺虫成分の濃度が増加する匍匐害虫駆除製剤。
A solid insect pest control formulation comprising a non-volatile insecticidal component at room temperature and a sublimable substance that is easier to evaporate than the insecticidal component at room temperature,
The preparation is one whose volume decreases with time due to sublimation of the sublimable substance or whose shape collapses with time.
The content of the insecticidal component in the preparation is substantially not reduced over time,
A pest control formulation in which the concentration of the insecticidal component in the formulation increases as the balance between the volume of the formulation and the content of the insecticidal component changes.
前記昇華性物質がイソプロピルトリオキサン、アダマンタン、メントール、ナフタレン、樟脳、及びパラジクロロベンゼンから選ばれる少なくとも1種である請求項1に記載の匍匐害虫駆除製剤。   The pesticidal insecticide according to claim 1, wherein the sublimable substance is at least one selected from isopropyltrioxane, adamantane, menthol, naphthalene, camphor, and paradichlorobenzene. 滑沢剤としてステアリン酸塩、タルク、酸化チタン、パラフィン、及び多価アルコールから選ばれる少なくとも1種を含む請求項1または2に記載の匍匐害虫駆除製剤。   The pest control formulation according to claim 1 or 2, comprising at least one selected from stearates, talc, titanium oxide, paraffin, and polyhydric alcohols as a lubricant. 常温で難揮散性の殺虫成分と、常温で前記殺虫成分よりも揮散しやすい昇華性物質とを含有する固形の匍匐害虫駆除製剤であって、前記昇華性物質の昇華によって、体積が経時的に減少または形状が経時的に崩壊し、製剤の体積と、殺虫成分の含有量とのバランス変化にともない、殺虫成分の濃度が増加する固形の匍匐害虫駆除製剤を、害虫の生息しうる場所に設置する、匍匐害虫駆除方法。   A solid pest-control product comprising a non-volatile insecticidal component that is difficult to volatilize at room temperature and a sublimable substance that is more easily volatilized than the insecticidal component at room temperature, and the volume of the insecticide increases by time due to sublimation of the sublimable substance. Decrease or shape collapses over time, and a solid moth pest control formulation that increases the concentration of the insecticidal component as the balance between the volume of the formulation and the content of the insecticidal component increases is installed in a place where pests can live How to control moth pests.
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