JP4644165B2 - Water-dispersible microbial pesticide solid preparation - Google Patents
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本明細書記載の発明は、微生物を活性成分として含有する水分散性の農薬固形製剤に関する。 The invention described in the present specification relates to a water-dispersible agricultural chemical solid preparation containing a microorganism as an active ingredient.
従来より水に希釈して散布するタイプの固体製剤としては、粉状の水和剤および粒状の顆粒水和剤がある。これらの製剤は、通常、活性成分、固体担体および補助剤から構成されている。固体担体は、活性成分を適当な濃度に希釈するために用いられ、具体的には、クレー、タルク、炭酸カルシウム、珪藻土、ホワイトカーボン等の微粉末が挙げられる。補助剤は、活性成分の安定性向上や活性成分および固体担体の湿潤性、分散性、懸垂性を向上させるために添加されるものであり、具体的には安定剤、界面活性剤などが挙げられる。 Conventional solid preparations that are dispersed in water and sprayed include powdered wettable powder and granular granular wettable powder. These preparations are usually composed of an active ingredient, a solid carrier and an adjuvant. The solid carrier is used for diluting the active ingredient to an appropriate concentration, and specific examples thereof include fine powders such as clay, talc, calcium carbonate, diatomaceous earth, and white carbon. Adjuvants are added to improve the stability of the active ingredient and to improve the wettability, dispersibility, and suspension of the active ingredient and the solid carrier. Specific examples include stabilizers and surfactants. It is done.
しかし、微生物農薬は、生菌体、死菌体、包埋体、宿主昆虫由来の蛋白質や脂質などが製剤中に含有するため、従来の一般的な農薬を水分散性の固体製剤にするための製剤構成で製剤化し、水に希釈して散布しようとすると、固体製剤が水に湿潤し難かったり、水中に分散し難く、均一な散布ができず結果的に農薬の効力に悪影響を与えるといった問題が生じる。これらの問題を解決するため、例えば特許文献１では、微生物と水溶性高分子化合物を含有する微生物農薬が提案されている。 However, since microbial pesticides contain live cells, dead cells, embedded bodies, proteins and lipids derived from host insects, etc., in order to make conventional general pesticides into water-dispersible solid formulations If it is formulated with the formulation composition of the above, diluted in water and sprayed, the solid formulation is difficult to wet in water or difficult to disperse in water, and cannot be uniformly sprayed, resulting in adverse effects on the efficacy of the agricultural chemicals. Problems arise. In order to solve these problems, for example, Patent Document 1 proposes a microbial pesticide containing a microorganism and a water-soluble polymer compound.
しかし、微生物、水溶性高分子化合物および珪藻土等の水不溶性の固体担体で構成された混合物を水和剤に製剤化しても水への希釈時の湿潤性、分散性および懸垂性は不十分で、均一な散布をするのには問題があった。 However, even when a mixture composed of a water-insoluble solid carrier such as a microorganism, a water-soluble polymer compound, and diatomaceous earth is formulated into a wettable powder, the wettability, dispersibility, and suspension are not sufficient when diluted in water. There was a problem with uniform spraying.
上述した課題を解決するため、本発明者が鋭意検討した結果、（１）微生物、（２）水溶性固体担体及び（３）水溶性高分子化合物及び／または界面活性剤を組み合わせ、（３）成分が界面活性剤の場合には、更に水不溶性固体担体を組み合わせて、水分散性農薬固形製剤に製剤化することにより水への希釈時の湿潤性、分散性および懸垂性が著しく向上することを見出し、本明細書記載の発明を完成した。
即ち、本発明は、
In order to solve the above-mentioned problems, the present inventors have intensively studied. As a result, (1) a microorganism, (2) a water-soluble solid carrier, and (3) a water-soluble polymer compound and / or a surfactant are combined. In the case where the component is a surfactant, the wettability, dispersibility and suspension properties when diluted in water are significantly improved by combining a water-insoluble solid carrier and formulating into a water-dispersible agricultural chemical solid formulation. The present invention described in this specification has been completed.
That is, the present invention
（１）（１）微生物として、核多角体病ウイルス罹患ハスモンヨトウから得られた、夾雑物を含む核多角体病ウイルス、（２）水溶性固体担体として硫酸アンモニウム及び硫酸アルカリ金属塩からなる群から選ばれる少なくとも１種、及び（３）水溶性高分子化合物を含有することを特徴とする水分散性農薬固形製剤、
（２）更に水不溶性固体担体を含有することを特徴とする前項（１）に記載の水分散性農薬固形製剤、
（３）核多角体病ウイルスがハスモンヨトウによって増殖されたものである前項（１）又は（２）に記載の水分散性農薬固形製剤、
（４）水溶性硫酸塩が硫酸アンモニウムである前項（１）〜（３）のいずれか一項に記載の水分散性農薬固形製剤、
（５）水溶性高分子化合物がポリエチレングリコールである前項（１）〜（４）のいずれか一項に記載の水分散性農薬固形製剤、
（６）（１）核多角体病ウイルスをウイルスの包埋体として１×１０ ７ 個／ｇ以上、（２）水溶性固体担体を、製剤中１０〜９５％（ｗ／ｗ）、（３）水溶性高分子化合物を製剤中、０．１〜４０％（ｗ／ｗ）を含有する前項（１）〜（５）のいずれか一項に記載の水分散性農薬固形製剤、
に関する。
また、本明細書には、参考のため、下記の発明、
（１）（１）微生物、（２）水溶性固体担体、及び（３）水溶性高分子化合物及び／または界面活性剤を含有し、（３）の成分が界面活性剤であるときには更に水不溶性固体担体を含有することを特徴とする水分散性農薬固形製剤（但し、上記本発明は除く）。
（２）水溶性固体担体が、水溶性硫酸塩、水溶性塩化物、水溶性糖類及び尿素からなる群から選択される少なくとも１種であることを特徴とする前項（１）に記載の水分散性農薬固形製剤、
（３）微生物が宿主昆虫及び／または代替え宿主昆虫によって増殖されたものである前項（１）又は（２）に記載の水分散性農薬固形製剤、
（４）微生物が核多角体病ウイルスである前項（１）〜（３）のいずれか一項に記載の水分散性農薬固形製剤、
（５）水溶性高分子化合物がポリエチレングリコールである前項（１）〜（４） のいずれか一項に記載の水分散性農薬固形製剤、
（６）界面活性剤がラウリル硫酸ナトリウムである前項（１）〜（５）のいずれか一項に記載の水分散性農薬固形製剤、
も開示されている。
(1) (1) As a microorganism , a nuclear polyhedrosis virus containing foreign substances obtained from a pods affected with nuclear polyhedrosis virus, (2) selected from the group consisting of ammonium sulfate and alkali metal sulfate as a water-soluble solid carrier at least one, and (3) water-dispersible agrochemical solid preparation characterized by containing a water-soluble polymer compound,
(2) further water-dispersible agrochemical solid formulation according to the above (1), characterized in that it contains a water-insoluble solid carrier,
( 3 ) The water-dispersible agrochemical solid preparation according to (1) or (2) above, wherein the nuclear polyhedrosis virus is propagated by Spodoptera litura
( 4 ) The water-dispersible agricultural chemical solid preparation according to any one of ( 1) to (3), wherein the water-soluble sulfate is ammonium sulfate,
( 5 ) The water-dispersible agricultural chemical solid preparation according to any one of (1) to ( 4) , wherein the water-soluble polymer compound is polyethylene glycol,
( 6 ) (1) 1 × 10 7 cells / g or more with a nuclear polyhedrosis virus as an embedded body of virus , (2) 10 to 95% (w / w), (3) ) The water-dispersible agricultural chemical solid preparation according to any one of (1) to (5) above, which contains 0.1 to 40% (w / w) of the water-soluble polymer compound in the preparation,
About.
In addition, in this specification, for reference, the following invention,
(1) (1) a microorganism, (2) a water-soluble solid carrier, and (3) a water-soluble polymer compound and / or a surfactant, and when the component (3) is a surfactant, further water-insoluble A water-dispersible agrochemical solid preparation characterized by containing a solid carrier (however, the present invention is excluded).
(2) water-soluble solid carrier, water-soluble sulfate, water-soluble chlorides, water dispersible according to the above (1), wherein the at least one selected from the group consisting of water-soluble sugars and urea Agrochemical solid formulation,
( 3 ) The water-dispersible agrochemical solid preparation according to (1) or (2) above, wherein the microorganism is grown by a host insect and / or an alternative host insect,
( 4 ) The water-dispersible agricultural chemical solid preparation according to any one of (1) to ( 3 ), wherein the microorganism is a nuclear polyhedrosis virus,
( 5 ) The water-dispersible agricultural chemical solid preparation according to any one of (1) to ( 4 ), wherein the water-soluble polymer compound is polyethylene glycol,
( 6 ) The water dispersible agricultural chemical solid preparation according to any one of (1) to ( 5 ), wherein the surfactant is sodium lauryl sulfate,
Is also disclosed.
本発明によれば、（１）活性成分である微生物として、核多角体病ウイルス罹患ハスモンヨトウから得られた、夾雑物を含む核多角体病ウイルス、（２）水溶性固体担体として硫酸アンモニウム及び硫酸アルカリ金属塩からなる群から選ばれる少なくとも１種、及び（３）水溶性高分子化合物を組み合わせ、水分散性農薬固形製剤に製剤化することにより、水への希釈時の湿潤性、分散性および懸垂性が著しく向上し、均一な散布ができ、結果的に効力が向上した微生物農薬を提供することができる。
なお、参考のために開示される発明においても効果の大きさに差はあっても同様な効果がある。
According to the present invention, (1) as the microorganism which is an active ingredient, obtained from nuclear polyhedrosis virus suffering litura nuclear polyhedrosis virus containing contaminants, (2) ammonium sulfate as a water-soluble solid carrier and an alkali sulfate By combining at least one selected from the group consisting of metal salts and (3) a water-soluble polymer compound into a water-dispersible agricultural chemical solid preparation, the wettability upon water dilution, dispersibility and It is possible to provide a microbial pesticide that has significantly improved suspension and can be uniformly sprayed, resulting in improved efficacy.
Note that the invention disclosed for reference has the same effect even if there is a difference in effect.
本明細書記載の発明は、（１）微生物（２）水溶性固体担体、（３）水溶性高分子化合物及び／または界面活性剤を含有し、（３）の成分が界面活性剤であるときには更に水不溶性固体担体を含有する水分散性農薬固形製剤であり、更に、必要に応じて、上記成分以外の補助剤（（３）の成分が水溶性高分子化合物であるときは、水不溶性固体担体等の水不溶性増量剤も含む）を使用することが出来る。 The invention described in the present specification includes (1) a microorganism, (2) a water-soluble solid carrier, (3) a water-soluble polymer compound and / or a surfactant, and the component (3) is a surfactant. Furthermore, it is a water-dispersible agricultural chemical solid preparation containing a water-insoluble solid carrier, and if necessary, when the auxiliary agent other than the above-mentioned components ((3) is a water-soluble polymer compound, a water-insoluble solid A water-insoluble extender such as a carrier) can also be used.
本発明の水分散性農薬固形製剤において使用される微生物は、核多角体病ウイルスであり、参考のために開示される発明（以下参考発明という）においては、更に、顆粒病ウイルス、細菌類、放線菌類、真菌類などを挙げることができる。また、これらの微生物を２種類以上組み合わせて使用することも可能である。これらの微生物は、宿主昆虫及び／又は代替え宿主昆虫を飼育して増殖させたものや、培養細胞によって増殖させたものなど、通常の方法により生産されたものを用いることが出来る。本明細書記載の発明の水分散性農薬固形製剤において使用される微生物は、精製したものでも構わないが、生産に用いた宿主昆虫あるいは代替え宿主昆虫や培養細胞から遊離させる際、分離されずに残った蛋白質、脂質などの不純物、あるいは虫体残渣が夾雑しているものが適している。これら微生物のうち、好ましい微生物としては、宿主昆虫および／または代替え宿主昆虫によって増殖されたものであり、更に好ましいのは、核多角体病ウイルスであり、より好ましくはハスモンヨトウより採取された核多角体病ウイルスである。該核多角体病ウイルスは独立行政法人農業生物資源研究所ジーンバンクから、ハスモンヨトウ核多角体病ウイルス（MAFF番号１０７００１）として入手することができる。
製剤中の微生物濃度は、微生物が核多角体病ウイルス等のウイルスの場合は、包埋体として通常１×１０７個／ｇ以上、好ましくは１×１０８個／ｇ以上、より好ましくは１×１０9個／ｇ以上、最も好ましくは１×１０9個／ｇ〜１×１０12個／ｇである。
The microorganism used in the water-dispersible agricultural chemical solid preparation of the present invention is a nuclear polyhedrosis virus. In the invention disclosed for reference (hereinafter referred to as reference invention) , granule disease virus, bacteria, Examples include actinomycetes and fungi . It is also possible to use a combination of two or more of these microorganisms. As these microorganisms, those produced by ordinary methods such as those obtained by breeding and growing host insects and / or alternative host insects, and those grown by cultured cells can be used. The microorganism used in the water-dispersible agricultural chemical solid preparation of the invention described in the present specification may be purified, but it is not separated when it is released from the host insect used for production or the alternative host insect or cultured cell. The remaining proteins, impurities such as lipids, or those containing insect residue are suitable. Among these microorganisms, preferable microorganisms are those grown by host insects and / or alternative host insects, more preferably nuclear polyhedrosis virus, more preferably nuclear polyhedra collected from Spodoptera litura. It is a disease virus. The nuclear polyhedrosis virus can be obtained from the National Institute of Agrobiological Sciences, Genebank, as the Japanese scorpion nucleopolyhedrovirus (MAFF No. 107001).
When the microorganism is a virus such as a nuclear polyhedrosis virus, the concentration of the microorganism in the preparation is usually 1 × 10 7 / g or more, preferably 1 × 10 8 / g or more, more preferably 1 as an embedded body. × 10 9 cells / g or more, and most preferably 1 × 10 9 cells / g to 1 × 10 12 cells / g.
本明細書記載の発明における水溶性固体担体は、（３）の水溶性高分子化合物及び／または界面活性剤と重複しない意味で使用される。例えば（３）の成分が水溶性高分子化合物であるときは、（２）の水溶性固体担体は水溶性高分子化合物を含まないものである。従って、本明細書記載の発明の製剤においては、（２）の成分と（３）の成分の両者が共存する。そして、（３）の成分が界面活性剤であるときは、更に水不溶性固体担体が共存する。
本明細書記載の発明の水分散性農薬固形製剤において使用される水溶性固体担体としては、２０℃において、０．１ｇ／ｍｌ以上の水溶性を有するものが好ましく、より好ましくは０．４ｇ／ｍｌ以上の水溶性を有するものである。例えば、硫酸アンモニウム、硫酸ナトリウム等の水溶性硫酸塩（好ましくは水溶性無機硫酸塩、より好ましくは硫酸アンモニウム及び硫酸アルカリ金属塩からなる群から選ばれる少なくとも１種）、塩化アンモニウム、塩化ナトリウム、塩化カリウム等の水溶性ハロゲン化物（好ましくは水溶性無機塩化物、より好ましくは塩化アンモニウム及び塩化アルカリ金属塩からなる群から選ばれる少なくとも１種）、ブドウ糖、ショ糖、果糖、乳糖等の水溶性糖類（好ましくは単糖類又は／及びオリゴ糖類、オリゴ糖類としては２糖類が好ましい）、尿素などを挙げることができる。これらは１種類又は２種類以上を組み合わせて用いることができる。これらの水溶性固体担体で、好ましいのは、水溶性硫酸塩であり、より好ましくは硫酸アンモニウム及び硫酸アルカリ金属塩からなる群から選ばれる少なくとも１種であり、最も好ましくは硫酸アンモニウムである。これらの水溶性固体担体の使用量は、通常、製剤中、１０〜９５％（ｗ／ｗ）（以下特に断らない限り、同じ）で、好ましくは４０〜９０％、更に好ましくは６０〜９０％程度である。
The water-soluble solid carrier in the invention described in the present specification is used in the sense that it does not overlap with the water-soluble polymer compound (3) and / or surfactant. For example, when the component (3) is a water-soluble polymer compound, the water-soluble solid carrier (2) does not contain a water-soluble polymer compound. Therefore, in the formulation of the invention described in the present specification , both the component (2) and the component (3) coexist. When the component (3) is a surfactant, a water-insoluble solid carrier is further present.
The water-soluble solid carrier used in the water-dispersible agricultural chemical solid preparation of the invention described in the present specification preferably has a water solubility of 0.1 g / ml or more at 20 ° C., more preferably 0.4 g / ml. It has water solubility of more than ml. For example, water-soluble sulfates such as ammonium sulfate and sodium sulfate (preferably water-soluble inorganic sulfate, more preferably at least one selected from the group consisting of ammonium sulfate and alkali metal sulfate), ammonium chloride, sodium chloride, potassium chloride, etc. Water-soluble halides (preferably water-soluble inorganic chlorides, more preferably at least one selected from the group consisting of ammonium chloride and alkali metal chloride salts), water-soluble saccharides such as glucose, sucrose, fructose and lactose (preferably Monosaccharides and / or oligosaccharides, and disaccharides are preferred as oligosaccharides) and urea. These can be used alone or in combination of two or more. Among these water-soluble solid carriers, preferred are water-soluble sulfates, more preferably at least one selected from the group consisting of ammonium sulfate and alkali metal sulfate, and most preferably ammonium sulfate. The use amount of these water-soluble solid carriers is usually 10 to 95% (w / w) in the preparation (the same unless otherwise specified), preferably 40 to 90%, more preferably 60 to 90%. Degree.
また、本明細書記載の発明の水分散性農薬固形製剤において使用しうる水溶性高分子化合物としては、ポリエチレングリコール、ポリビニルアルコール、ポリビニルピロリドン、ポリアクリル酸ナトリウム、カルボキシメチルセルロースナトリウム、アルギン酸ナトリウム、デキストリン、可溶性デンプンなどを挙げることができ、これらを１種類又は２種類以上を組み合わせて用いることができる。本発明の製剤において、水溶性高分子化合物として好ましいのは、ポリエチレングリコール、ポリビニルアルコール又はカルボキシメチルセルロースナトリウム等が挙げられ、より好ましくはポリエチレングリコールである。ポリエチレングリコールの分子量は本発明の目的が達成される限り特に制限は無いが、通常１００〜２００００程度のものが挙げられ、好ましくは１００〜６０００、より好ましくは１００〜１０００程度である。これらの水溶性高分子化合物の使用量は、通常、製剤中、０．１〜４０％（ｗ／ｗ）、０．１〜２０％（ｗ／ｗ）、好ましくは０．５〜１０％（ｗ／ｗ）である。 Examples of the water-soluble polymer compound that can be used in the water-dispersible agricultural chemical solid preparation of the invention described herein include polyethylene glycol, polyvinyl alcohol, polyvinyl pyrrolidone, sodium polyacrylate, sodium carboxymethyl cellulose, sodium alginate, dextrin, Soluble starch etc. can be mentioned, These can be used 1 type or in combination of 2 or more types. In the preparation of the present invention, preferable examples of the water-soluble polymer compound include polyethylene glycol, polyvinyl alcohol, sodium carboxymethyl cellulose and the like, and more preferably polyethylene glycol. The molecular weight of polyethylene glycol is not particularly limited as long as the object of the present invention is achieved, but usually about 100 to 20000, preferably about 100 to 6000, more preferably about 100 to 1000. The amount of these water-soluble polymer compounds used is usually 0.1 to 40% (w / w), 0.1 to 20% (w / w), preferably 0.5 to 10% in the preparation. w / w).
本明細書記載の発明の水分散性農薬固形製剤において使用しうる界面活性剤としては、特に限定されないが、例えばポリオキシエチレンラウリルエーテル等のポリオキシエチレンアルキルエーテル、ポリオキシエチレンノニルフェニルエーテル等のポリオキシエチレンアルキルアリールエーテル、ポリオキシエチレンモノラレート等のポリオキシエチレンアルキルエステル、ポリオキシエチレンスチリルフェニルエーテル、ポリオキシエチレン・ポリオキシプロピレンブロックポリマー、リグニンスルホン酸カルシウム等のリグニンスルホン酸塩、アルキルナフタレンスルホン酸ナトリウム塩等のアルキルナフタレンスルホン酸塩、ラウリル硫酸ナトリウム等のアルキル硫酸ナトリウム、アルキルベンゼンスルホン酸ナトリウムなどが挙げられる。これらは１種又は２種以上を併用しても構わない。これらの中で、アルキル硫酸ナトリウムが好ましく、アルキルとしてはＣ８〜Ｃ２０程度、好ましくはＣ１０〜Ｃ１８、より好ましくはＣ１０〜Ｃ１６程度のものが好ましい。最も好ましくはラウリル硫酸ナトリウムである。これら界面活性剤の使用量は、製剤中、通常、０．１〜８０％（ｗ／ｗ）、好ましくは、０．１〜６０％（ｗ／ｗ）、より好ましくは０．５〜４０％（ｗ／ｗ）である。場合により、０．５〜２０％（ｗ／ｗ）、更には１〜１０％程度が最も好ましい。
（３）の成分（水溶性高分子化合物または界面活性剤）の内では、水溶性高分子化合物が好ましい。
The surfactant that can be used in the water-dispersible agricultural chemical solid preparation of the invention described in the present specification is not particularly limited. For example, polyoxyethylene alkyl ether such as polyoxyethylene lauryl ether, polyoxyethylene nonylphenyl ether, and the like. Polyoxyethylene alkyl aryl ether, polyoxyethylene alkyl ester such as polyoxyethylene monolarate, polyoxyethylene styryl phenyl ether, polyoxyethylene / polyoxypropylene block polymer, lignin sulfonate such as calcium lignin sulfonate, alkylnaphthalene Alkylnaphthalene sulfonates such as sodium sulfonate, sodium alkyl sulfates such as sodium lauryl sulfate, sodium alkylbenzene sulfonate, etc. That. These may be used alone or in combination of two or more. Among these, sodium alkyl sulfate is preferable, and the alkyl is preferably about C8 to C20, preferably C10 to C18, more preferably about C10 to C16. Most preferred is sodium lauryl sulfate. The amount of these surfactants used is usually 0.1 to 80% (w / w), preferably 0.1 to 60% (w / w), more preferably 0.5 to 40% in the preparation. (W / w). In some cases, 0.5 to 20% (w / w), more preferably about 1 to 10% is most preferable.
Among the components (3) (water-soluble polymer compound or surfactant), a water-soluble polymer compound is preferable.
本明細書記載の発明の水分散性農薬固形製剤は上記の微生物、水溶性固体担体、水溶性高分子化合物、界面活性剤以外に、必要に応じて、水不溶性固体担体、その他の補助剤として結合剤、酸化防止剤、紫外線防止剤などを含有することができる。 The water-dispersible agricultural chemical solid preparation of the invention described in the present specification can be used as a water-insoluble solid carrier or other auxiliary agent, if necessary, in addition to the above-mentioned microorganism, water-soluble solid carrier, water-soluble polymer compound and surfactant. A binder, an antioxidant, an ultraviolet ray inhibitor and the like can be contained.
本明細書記載の発明の水分散性農薬固形製剤に使用しうる水不溶性固体担体としては、タルク、クレー、カオリン、炭酸カルシウム、珪藻土、ゼオライト、ベントナイト、ジークライト、パーライト、ホワイトカーボンなどが挙げられるが、特にこれらに限定されず、１種または２種以上を併用しても構わない。これら水不溶性固体担体の使用量は、使用する場合、通常、製剤中、０．１〜８０％（ｗ／ｗ）、好ましくは、０．１〜６０％（ｗ／ｗ）、より好ましくは０．５〜４０％（ｗ／ｗ）である。該水不溶性固体担体は、場合により無くてもよいが、使用する方が好ましい。従って、場合により、０〜３０％程度、使用する場合のみのときは、０．１〜３０％程度、さらには、０．５〜２５％程度が最も好ましい。
水不溶性固体担体の粒度は本発明の効果を達成する限り、特に限定は無いが、通常１〜１００μｍ程度、より好ましくは１〜５０μｍ程度である。
Examples of the water-insoluble solid carrier that can be used in the water-dispersible agricultural chemical solid preparation of the invention described in the present specification include talc, clay, kaolin, calcium carbonate, diatomaceous earth, zeolite, bentonite, dikelite, perlite, and white carbon. However, it is not particularly limited to these, and one kind or two or more kinds may be used in combination. When used, the amount of these water-insoluble solid carriers is usually 0.1 to 80% (w / w), preferably 0.1 to 60% (w / w), more preferably 0 in the preparation. 5 to 40% (w / w). The water-insoluble solid carrier may be omitted depending on circumstances, but it is preferable to use it. Accordingly, in some cases, about 0 to 30%, and when used only, about 0.1 to 30%, and more preferably about 0.5 to 25% are most preferable.
The particle size of the water-insoluble solid carrier is not particularly limited as long as the effect of the present invention is achieved, but is usually about 1 to 100 μm, more preferably about 1 to 50 μm.
本明細書記載の発明の水分散性農薬固形製剤に使用しうる結合剤としては、結合剤としての作用を有するものであれば特に限定されないが、例えば、アラビアガム、トラガントガム、グアーガム、マンナン、キサンタンガム、エチルセルロース、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロースなどが挙げられる。これらは１種または２種以上を併用しても構わない。これら結合剤の使用量は、通常０〜８０％程度の範囲である。使用する場合、通常、製剤中、０．１〜８０％（ｗ／ｗ）、好ましくは、０．１〜６０％（ｗ／ｗ）、より好ましくは０．５〜４０％（ｗ／ｗ）である。但し、これらの結合剤が本発明で使用する（３）の水溶性高分子化合物の範疇に入るものであるときは、（３）の成分として使用されたものと見なす。 The binder that can be used in the water-dispersible agricultural chemical solid preparation of the invention described in the present specification is not particularly limited as long as it has an action as a binder. For example, gum arabic, gum tragacanth, guar gum, mannan, xanthan gum , Ethyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose and the like. These may be used alone or in combination of two or more. The amount of these binders used is usually in the range of about 0 to 80%. When used, it is usually 0.1 to 80% (w / w), preferably 0.1 to 60% (w / w), more preferably 0.5 to 40% (w / w) in the preparation. It is. However, when these binders fall within the category of the water-soluble polymer compound (3) used in the present invention, they are regarded as being used as the component (3).
本明細書記載の発明の好ましい製剤組成としては、例えば下記の組成が挙げられる。
（１）微生物：微生物菌体を前記範囲で含む固形分０．５〜２０％、好ましくは１〜１０％、
（２）水溶性固体担体：１０〜９５％、好ましくは４０〜９５％、更に好ましくは６０〜９５％、
（３）の水溶性高分子化合物及び／または界面活性剤：０．１〜４０％、好ましくは、水溶性高分子化合物の場合は０．１〜２０％（ｗ／ｗ）、より好ましくは０．５〜１０％（ｗ／ｗ）、界面活性剤の場合は０．５〜２０％（ｗ／ｗ）、より好ましくは１〜１０％、
（４）水不溶性固体担体：上記（３）成分が水溶性高分子化合物の場合、０〜３０％程度、好ましくは、０．１〜３０％程度、より好ましくは０．５〜２５％程度、上記（３）成分が界面活性剤の場合、好ましくは０．５〜２０％（ｗ／ｗ）、より好ましくは１〜１０％程度、
であり、これらの成分含量の合計が１００％になるように各成分を適宜配合することにより本明細書記載の発明の製剤とすることができる。
本明細書記載の発明のより好ましい製剤の一つは、（１）微生物、（２）の水溶性固体担体としての水溶性硫酸塩、及び（３）水溶性高分子化合物を含む製剤であり、更に好ましい製剤は、（４）として水不溶性固体担体を含む製剤である。そして、これらの各成分は、それぞれ好ましい範囲で含まれるとき、より好ましい。
本明細書記載の発明の水分散性農薬固形製剤は、例えば以下の製造法によって得ることができる。
Examples of the preferable pharmaceutical composition of the invention described in the present specification include the following compositions.
(1) Microorganism: 0.5 to 20%, preferably 1 to 10% solid content containing microbial cells in the above range,
(2) Water-soluble solid carrier: 10 to 95%, preferably 40 to 95%, more preferably 60 to 95%,
(3) Water-soluble polymer compound and / or surfactant: 0.1 to 40%, preferably 0.1 to 20% (w / w) in the case of water-soluble polymer compound, more preferably 0 5-10% (w / w), 0.5-20% (w / w) in the case of surfactants, more preferably 1-10%,
(4) Water-insoluble solid carrier: When the component (3) is a water-soluble polymer compound, about 0 to 30%, preferably about 0.1 to 30%, more preferably about 0.5 to 25%, When the above component (3) is a surfactant, preferably 0.5 to 20% (w / w), more preferably about 1 to 10%,
It is possible to obtain the preparation of the invention described in the present specification by appropriately blending each component so that the total content of these components is 100%.
One of the more preferable preparations of the invention described in the present specification is a preparation comprising (1) a microorganism, (2) a water-soluble sulfate as a water-soluble solid carrier, and (3) a water-soluble polymer compound. A more preferred preparation is a preparation containing a water-insoluble solid carrier as (4). And each of these components is more preferable when each is contained in a preferable range.
The water-dispersible agricultural chemical solid preparation of the invention described in the present specification can be obtained, for example, by the following production method.
精製した微生物と、水溶性固体担体、水溶性高分子化合物及び／又は界面活性剤、水不溶性固体担体などを、リボンミキサー、ナウターミキサー、双腕ニーダ−などで混合後、ハンマーミル、ピンミル、ジェットミルなどで粉砕して得ることができる。また、ウイルスに罹病させた罹病虫体を磨砕し濾過した虫体液と水溶性固体担体、水溶性高分子化合物、界面活性剤、結合剤および水不溶性の固体担体などをナウターミキサー、双腕ニーダ−などで混練し、虫体液中の水分を乾燥後、ハンマーミル、ピンミル、ジェットミルなどで粉砕して得ることもできる。このようにして得られた本発明の水分散性農薬固形製剤の平均粒径は１〜１００μｍ、好ましくは１〜５０μｍ程度である。
本明細書記載の発明の水分散性農薬固形製剤は、通常、水に希釈して使用される。例えば、本剤１００ｇを１００Ｌの水に加え、攪拌分散させ散布液を調製し、散布液を手動式スプレイヤー、動力式スプレイヤー等で対象となる作物に１０アールあたり２００Ｌを噴霧散布する。
After mixing the purified microorganism with a water-soluble solid carrier, a water-soluble polymer compound and / or a surfactant, a water-insoluble solid carrier, etc. with a ribbon mixer, a nauter mixer, a double arm kneader, etc., a hammer mill, a pin mill, It can be obtained by pulverizing with a jet mill or the like. In addition, the worm body affected by the virus is ground and filtered, and the body fluid and water-soluble solid carrier, water-soluble polymer compound, surfactant, binder, water-insoluble solid carrier, etc. It can also be obtained by kneading with a kneader or the like, drying the moisture in the insect body fluid, and then pulverizing with a hammer mill, pin mill, jet mill or the like. The average particle size of the water-dispersible agricultural chemical solid preparation of the present invention thus obtained is 1 to 100 μm, preferably about 1 to 50 μm.
The water-dispersible agricultural chemical solid preparation of the invention described in the present specification is usually used after diluted in water. For example, 100 g of this agent is added to 100 L of water, and dispersed by stirring to prepare a spray liquid, and sprayed with 200 L per 10 ares on the target crop with a manual sprayer, a power sprayer or the like.
実施例
以下、実施例により本発明を詳細に説明するが、これらに限定されるものではない。尚、実施例及び参考例中、部とはすべて重量部を示す。
また、実施例、参考例及び比較例で使用した核多角体病ウイルスを混練した人工飼料は次のようにして調製した。
人工飼料の調製方法
ふすま２５０ｇ、ウズラ豆１００ｇ、小麦粉１００ｇ、Ｌアスコルビン酸（防腐剤）１３ｇ、ヒドロキシ安息香酸メチル（防腐剤）１０ｇ、ソルビン酸（防腐剤）５ｇ、蒸留水５５０ｍｌ、ハスモンヨトウ核多角体病ウイルス（３〜５×１０９個／ｍｌ）１５ｍｌを混練し、ハスモンヨトウ核多角体病ウイルスを混練した人工飼料を得た。
EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples, but is not limited thereto. In the examples and reference examples , all parts are parts by weight.
Moreover, the artificial feed which knead | mixed the nuclear polyhedrosis virus used by the Example , the reference example, and the comparative example was prepared as follows.
Artificial feed preparation method 250g bran, 100g quail beans, 100g wheat flour, 13g L ascorbic acid (preservative), 10g methyl hydroxybenzoate (preservative), 5g sorbic acid (preservative), 550ml distilled water, pods 15 ml of disease virus (3-5 × 10 9 cells / ml) was kneaded to obtain an artificial feed kneaded with Spodoptera litura nuclear polyhedrosis virus.
参考例１
１ｇ当たり、４．５×１０７〜７．５×１０７個の核多角体病ウイルスを混練した人工飼料をプラスチック容器に１ｇずつ入れ、さらに、５齢初期のハスモンヨトウ幼虫を１頭ずつ入れて摂食させ、感染させた。これを６日間飼育し、核多角体病ウイルスを増殖させる。このウイルスに罹病させた致死直前のハスモンヨトウ罹病虫をジューサーミキサーで磨砕し、磨砕液を目開き０．２１０ｍｍの篩で濾過して虫体液を得た。得た虫体液１ｇ中に１×１０１０個の核多角体病ウイルスを含有するように調整した。本調整虫体液２０部（固形分として３．２部）、水不溶性の固体担体としてカープレックス８０Ｄ（ホワイトカーボン、ＤＳＬ．ジャパン株式会社製）１０部、界面活性剤としてラウリル硫酸ナトリウム５部、および水溶性固体担体として硫酸アンモニウム８１．８部を双腕ニーダ− で混練後、４０℃±１℃の恒温槽で乾燥する。乾燥品をハンマーミルで粉砕し、参考例の水分散性農薬固形製剤を得た。本製剤１ｇ中に２×１０９個の核多角体病ウイルスを含有する。
Reference example 1
1 g of artificial feed kneaded with 4.5 × 10 7 to 7.5 × 10 7 nuclear polyhedrosis virus per 1 g is put into a plastic container, and further, one 5 year-old early-spotted beetle larva is added. Feeded and infected. This is bred for 6 days to propagate the nuclear polyhedrosis virus. The insects that were infected with this virus and were killed immediately before death were ground with a juicer mixer, and the ground solution was filtered through a sieve having an opening of 0.210 mm to obtain a body fluid. Insect body fluid 1g obtained was adjusted to contain 1 × 10 10 pieces of nuclear polyhedrosis virus. 20 parts of this worm body fluid (3.2 parts as solid content), 10 parts of Carplex 80D (white carbon, manufactured by DSL Japan Co., Ltd.) as a water-insoluble solid carrier, 5 parts of sodium lauryl sulfate as a surfactant, and 81.8 parts of ammonium sulfate as a water-soluble solid carrier is kneaded with a double-arm kneader and then dried in a constant temperature bath at 40 ° C. ± 1 ° C. The dried product was pulverized with a hammer mill to obtain a water-dispersible agricultural chemical solid preparation of Reference Example . 2 × 10 9 nuclear polyhedrosis virus is contained in 1 g of this preparation.
１ｇ当たり、４．５×１０ ７ 〜７．５×１０ ７ 個の核多角体病ウイルスを混練した人工飼料をプラスチック容器に１ｇずつ入れ、さらに、５齢初期のハスモンヨトウ幼虫を１頭ずつ入れて摂食させ、感染させた。これを６日間飼育し、核多角体病ウイルスを増殖させる。このウイルスに罹病させた致死直前のハスモンヨトウ罹病虫をジューサーミキサーで磨砕し、磨砕液を目開き０．２１０ｍｍの篩で濾過して虫体液を得た。得た虫体液１ｇ中に１×１０ １０ 個の核多角体病ウイルスを含有するように調整した。本調整虫体液２０部（固形分として３．２部）、水不溶性の固体担体としてカープレックス８０Ｄ（ホワイトカーボン、ＤＳＬ．ジャパン株式会社製）１０部、水溶性高分子化合物であるポリエチレングリコール４００（以下ＰＥＧ−４００という）５部、および水溶性固体担体として硫酸アンモニウム８１．８部を双腕ニーダ− で混練後、４０℃±１℃の恒温槽で乾燥する。乾燥品をハンマーミルで粉砕し、本発明の水分散性農薬固形製剤を得た。本製剤１ｇ中に２×１０ ９ 個の核多角体病ウイルスを含有する。 1 g of artificial feed kneaded with 4.5 × 10 7 to 7.5 × 10 7 nuclear polyhedrosis virus per 1 g is put into a plastic container, and further, one 5 year-old early- spotted beetle larva is added. Feeded and infected. This is bred for 6 days to propagate the nuclear polyhedrosis virus. The insects that were infected with this virus and were killed immediately before death were ground with a juicer mixer, and the ground solution was filtered through a sieve having an opening of 0.210 mm to obtain a body fluid. Insect body fluid 1g obtained was adjusted to contain 1 × 10 10 pieces of nuclear polyhedrosis virus. 20 parts of this worm body fluid (3.2 parts as solid content), 10 parts of Carplex 80D (white carbon, manufactured by DSL Japan Co., Ltd.) as a water-insoluble solid carrier, polyethylene glycol 400 (water-soluble polymer compound) (Hereinafter referred to as PEG-400) 5 parts, and 81.8 parts of ammonium sulfate as a water-soluble solid support are kneaded in a double arm kneader and dried in a constant temperature bath at 40 ° C. ± 1 ° C. The dried product was pulverized with a hammer mill to obtain the water-dispersible agricultural chemical solid preparation of the present invention. 2 × 10 9 nuclear polyhedrosis virus is contained in 1 g of this preparation .
実施例１における水溶性高分子化合物をゴーセノールＧＬ−０５Ｓ（商品名、ポリビニルアルコール、日本合成化学工業株式会社製）に変える以外は、実施例１と同様の方法で本発明の水分散性農薬固形製剤を得た。 The water-soluble polymer compound in Example 1 Gohsenol GL-05S (trade name, polyvinyl alcohol, Nippon Synthetic Chemical Industry Co., Ltd.), except for changing the water dispersible pesticide of the present invention in the same manner as in Example 1 A solid formulation was obtained.
実施例１における水溶性高分子化合物をセロゲン７Ａ（商品名、カルボキシメチルセルロースナトリウム、第一工業製薬株式会社製）に変える以外は、実施例１と同様の方法で本発明の水分散性農薬固形製剤を得た。 Serogen 7A the definitive water-soluble polymer in Example 1 (trade name, sodium carboxymethyl cellulose, manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.), except for changing the water dispersible agrochemical solid present invention in the same manner as in Example 1 A formulation was obtained.
参考例２
参考例１において、水溶性固体担体として用いた硫酸アンモニウムを硫酸ナトリウム（１０水塩）に変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference example 2
In Reference Example 1, a water-dispersible agricultural chemical solid preparation of Reference Example was obtained in the same manner as in Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to sodium sulfate (decahydrate).
実施例１において、水溶性固体担体として用いた硫酸アンモニウムを硫酸ナトリウム（１０水塩）に変える以外は、実施例１と同様の方法で本発明の水分散性農薬固形製剤を得た。 A water-dispersible agricultural chemical solid preparation of the present invention was obtained in the same manner as in Example 1 except that ammonium sulfate used as a water-soluble solid carrier in Example 1 was changed to sodium sulfate (10 hydrate).
参考例３
実施例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化アンモニウムに変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference example 3
In Example 1 , a water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to ammonium chloride.
参考例４
実施例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化ナトリウムに変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference example 4
In Example 1 , a water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to sodium chloride.
参考例５
実施例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化カリウムに変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 5
A water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier in Example 1 was changed to potassium chloride.
参考例６
実施例１において、水溶性固体担体として用いた硫酸アンモニウムを尿素に変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 6
A water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier in Example 1 was changed to urea.
参考例７
実施例１において、水溶性固体担体として用いた硫酸アンモニウムをブドウ糖に変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 7
In Example 1 , a water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to glucose.
参考例８
実施例１において、水溶性固体担体として用いた硫酸アンモニウムをショ糖に変える以外は、実施例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 8
A water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as in Example 1 except that ammonium sulfate used as the water-soluble solid carrier in Example 1 was changed to sucrose.
参考例９
参考例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化アンモニウムに変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 9
In Reference Example 1, a water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to ammonium chloride.
参考例１０
参考例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化ナトリウムに変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 10
In Reference Example 1, a water-dispersible agricultural chemical solid preparation of Reference Example was obtained in the same manner as Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to sodium chloride.
参考例１１
参考例１において、水溶性固体担体として用いた硫酸アンモニウムを塩化カリウムに変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 11
In Reference Example 1, a water-dispersible agricultural chemical solid preparation of Reference Example was obtained in the same manner as in Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to potassium chloride.
参考例１２
参考例１において、水溶性固体担体として用いた硫酸アンモニウムを尿素に変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 12
In Reference Example 1, a water-dispersible agricultural chemical solid preparation of Reference Example was obtained in the same manner as Reference Example 1, except that ammonium sulfate used as the water-soluble solid carrier was changed to urea.
参考例１３
参考例１において、水溶性固体担体として用いた硫酸アンモニウムをブドウ糖に変える以外は、参考例１と同様の方法で参考例の水分散性農薬固形製剤を得た。
Reference Example 13
In Reference Example 1, a water-dispersible agrochemical solid preparation of Reference Example was obtained in the same manner as Reference Example 1, except that ammonium sulfate used as the water-soluble solid carrier was changed to glucose.
参考例１４
参考例１において、水溶性固体担体として用いた硫酸アンモニウムをショ糖に変える以外は、参考例１と同様の方法で本参考例の水分散性農薬固形製剤を得た。
Reference Example 14
In Reference Example 1, a water-dispersible agricultural chemical solid preparation of this Reference Example was obtained in the same manner as Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to sucrose.
１ｇ当たり、４．５×１０ ７ 〜７．５×１０ ７ 個の核多角体病ウイルスを混練した人工飼料をプラスチック容器に１ｇずつ入れ、さらに、５齢初期のハスモンヨトウ幼虫を１頭ずつ入れて摂食させ、感染させた。これを６日間飼育し、核多角体病ウイルスを増殖させる。このウイルスに罹病させた致死直前のハスモンヨトウ罹病虫をジューサーミキサーで磨砕し、磨砕液を目開き０．２１０ｍｍの篩で濾過して虫体液を得た。得た虫体液１ｇ中に１×１０ １０ 個の核多角体病ウイルスを含有するように調整した。本調整虫体液２０部（固形分として３．２部）、水不溶性の固体担体としてカープレックス８０Ｄ（ホワイトカーボン、ＤＳＬ．ジャパン株式会社製）１０部、界面活性剤として用いたラウリル硫酸ナトリウムを２．５部、水溶性高分子化合物であるＰＥＧ−４００を２．５部および水溶性固体担体として硫酸アンモニウム８１．８部を双腕ニーダ− で混練後、４０℃±１℃の恒温槽で乾燥する。乾燥品をハンマーミルで粉砕し、本発明の水分散性農薬固形製剤を得た。本製剤１ｇ中に２×１０ ９ 個の核多角体病ウイルスを含有する。 1 g of artificial feed kneaded with 4.5 × 10 7 to 7.5 × 10 7 nuclear polyhedrosis virus per 1 g is put into a plastic container, and further, one 5 year-old early- spotted beetle larva is added. Feeded and infected. This is bred for 6 days to propagate the nuclear polyhedrosis virus. The insects that were infected with this virus and were killed immediately before death were ground with a juicer mixer, and the ground solution was filtered through a sieve having an opening of 0.210 mm to obtain a body fluid. Insect body fluid 1g obtained was adjusted to contain 1 × 10 10 pieces of nuclear polyhedrosis virus. 20 parts of this worm body fluid (3.2 parts as solid content), 10 parts of Carplex 80D (white carbon, manufactured by DSL Japan Co., Ltd.) as a water-insoluble solid carrier , 2 sodium lauryl sulfate used as a surfactant .5 parts , 2.5 parts of PEG-400, which is a water-soluble polymer compound, and 81.8 parts of ammonium sulfate as a water-soluble solid carrier were kneaded with a double arm kneader and then dried in a constant temperature bath at 40 ° C. ± 1 ° C. . The dried product was pulverized with a hammer mill to obtain the water-dispersible agricultural chemical solid preparation of the present invention. 2 × 10 9 nuclear polyhedrosis virus is contained in 1 g of this preparation .
１ｇ当たり、３×１０７〜５×１０７個の核多角体病ウイルスを混練した人工飼料をプラスチック容器に１ｇずつ入れ、さらに、５齢初期のハスモンヨトウ幼虫を１頭ずつ入れて摂食させ、感染させた。これを６日間飼育し、核多角体病ウイルスを増殖させる。このウイルスに罹病させた致死直前のハスモンヨトウ罹病虫をジューサーミキサーで磨砕し、磨砕液を目開き０．２１０ｍｍの篩で濾過して虫体液を得た。得た虫体液１ｇ中に１×１０１０個の核多角体病ウイルスを含有するように調整した。本調整虫体液をシャーレ上で４０℃±１℃の恒温槽で乾燥した。この乾燥物３．２部、水溶性高分子化合物としてＰＥＧ-４００を５部、および水溶性固体担体として硫酸アンモニウム９１．８部を双腕ニーダ− で混合後、ハンマーミルで粉砕し、本発明の水分散性農薬固形製剤を得た。本製剤１ｇ中に２×１０９個の核多角体病ウイルスを含有する。 1 g of artificial feed kneaded with 3 × 10 7 to 5 × 10 7 nuclear polyhedrosis virus per 1 g is put in a plastic container, and further, one of the five-year-old early-season moth larvae is added and fed. Infected. This is bred for 6 days to propagate the nuclear polyhedrosis virus. The insects that were infected with this virus and were killed immediately before death were ground with a juicer mixer, and the ground solution was filtered through a sieve having an opening of 0.210 mm to obtain a body fluid. Insect body fluid 1g obtained was adjusted to contain 1 × 10 10 pieces of nuclear polyhedrosis virus. This adjusted insect body fluid was dried on a petri dish in a constant temperature bath of 40 ° C. ± 1 ° C. After mixing 3.2 parts of this dried product, 5 parts of PEG-400 as a water-soluble polymer compound, and 91.8 parts of ammonium sulfate as a water-soluble solid carrier with a double arm kneader, the mixture was pulverized with a hammer mill. A water-dispersible agricultural chemical solid preparation was obtained. 2 × 10 9 nuclear polyhedrosis virus is contained in 1 g of this preparation.
比較例１
参考例１において、水溶性個体担体として用いた硫酸アンモニウムを水不溶性固体担体であるクレーに変える以外は、参考例１と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 1
In Reference Example 1, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Reference Example 1 except that ammonium sulfate used as the water-soluble solid carrier was changed to clay which was a water-insoluble solid carrier.
比較例２
比較例１において、水不溶性固体担体として用いたクレーをタルクに変える以外は、比較例１と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 2
In Comparative Example 1, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Comparative Example 1, except that the clay used as the water-insoluble solid carrier was changed to talc.
比較例３
比較例１において、水不溶性固体担体として用いたクレーを珪藻土に変える以外は、比較例１と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 3
In Comparative Example 1, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Comparative Example 1, except that the clay used as the water-insoluble solid carrier was changed to diatomaceous earth.
比較例４
比較例１において、界面活性剤として用いたラウリル硫酸ナトリウムを水溶性高分子化合物であるＰＥＧ−４００に変える以外は、比較例１と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 4
In Comparative Example 1, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Comparative Example 1, except that sodium lauryl sulfate used as the surfactant was changed to PEG-400, which is a water-soluble polymer compound. .
比較例５
比較例４において、水不溶性固体担体として用いたクレーをタルクに変える以外は、比較例４と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 5
In Comparative Example 4, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Comparative Example 4 except that the clay used as the water-insoluble solid carrier was changed to talc.
比較例６
比較例４において、水不溶性固体担体として用いたクレーを珪藻土に変える以外は、比較例４と同様の方法で比較用の水分散性農薬固形製剤を得た。
Comparative Example 6
In Comparative Example 4, a comparative water-dispersible agricultural chemical solid preparation was obtained in the same manner as in Comparative Example 4 except that the clay used as the water-insoluble solid carrier was changed to diatomaceous earth.
試験例１
実施例１〜６、参考例１〜１４および比較例１〜６で製造した水分散性農薬固形製剤を、下記の試験方法で評価した。この結果を表１に示した。
Test example 1
The water-dispersible agricultural chemical solid preparations produced in Examples 1 to 6, Reference Examples 1 to 14 and Comparative Examples 1 to 6 were evaluated by the following test methods. The results are shown in Table 1.
試験方法１（湿潤性）
５００ｍｌのビーカーに２０℃の３度硬水２００ｍｌを入れ、これに水分散性農薬固形製剤５ｇを水面上約１０ｃｍの位置より薄く広がるように静かに落とす。水分散性農薬固形製剤が落とし終わってから水面下に没するまでの時間を測定する。
Test Method 1 (Wettability)
200 ml of 3 degree hard water at 20 ° C. is put into a 500 ml beaker, and 5 g of the water dispersible agricultural chemical solid preparation is gently dropped so as to spread thinly from a position of about 10 cm above the water surface. Measure the time from when the water-dispersible pesticide solid preparation is dropped to when it is submerged under the surface of the water.
試験方法２（分散性）
上記１の試験で、水面下に没するまでの時間を測定後、直ちに、ガラス棒で右回りに１０回転、左回りに１０回転かきまぜて懸濁の均一性を観察する。
懸濁の均一性評価：
○・・・均一に細かく懸濁している。
△・・・粗い懸濁物が散見される。
×・・・粗い懸濁物が多く見られる。
Test method 2 (dispersibility)
In the test of 1 above, after measuring the time until submerged under water, immediately stir with a glass rod 10 clockwise and 10 counterclockwise to observe the uniformity of suspension.
Suspension uniformity assessment:
○ ... Uniformly finely suspended.
Δ: Coarse suspensions are scattered.
X: Many coarse suspensions are observed.
試験方法３（懸垂性）
２５０ｍｌの共栓付きメスシリンダーに３０℃の３度硬水２５０ｍｌを入れ、これに水分散性農薬固形製剤約５ｇを正確に測りこみ、水面上に静かに落とし栓をする。そのまま１０分間静置後、シリンダーを１分間に３０回倒立してふりまぜ（注）、無振動の３０±１℃の恒温水槽に静置する。１０分間経過したら、吸引用ガラス管で上部の２２５ｍｌ（９／１０に相当する）を１０〜１５秒かけて排除する。このときシリンダー中の沈降物をまきあげないようにする。また、吸引管の先を、いつも液面から数ｍｍ下のところに保って吸引する。シリンダーに残った底部の分散液２５ｍｌを、約３０ｍｌの蒸留水を使用して、重量を測定した直径約１０ｃｍのガラスシャーレに移す。シャーレ中の水分を４０±１℃の恒温槽で蒸発させた後、重量を測定してシャーレ上の固形物の重量を計算して、下記の計算式により懸垂率を求める。
懸垂率（％）＝１１１（Ａ−Ｂ）／Ａ
Ａ（ｇ）＝水分散性農薬固形製剤の試料重量
Ｂ（ｇ）＝低部２５ｍｌ中の固形物重量
（注）「倒立」とは、栓をしたシリンダーを、手で１８０°回転し、また、元に戻す操作で、これを約２秒で行う。
Test method 3 (suspension)
Place 250 ml of 3 degree hard water at 30 ° C. into a 250 ml graduated cylinder with a stopper, accurately measure about 5 g of water-dispersible agricultural chemical solid preparation, and gently drop the stopper on the water surface. After leaving still for 10 minutes, invert the cylinder 30 times per minute and shake (Note), and leave it in a non-vibrating 30 ± 1 ° C. constant temperature water bath. After 10 minutes, the upper 225 ml (corresponding to 9/10) is removed over 10-15 seconds with a glass tube for suction. At this time, the sediment in the cylinder should not be sprinkled up. In addition, suction is always performed while the tip of the suction tube is kept several mm below the liquid level. 25 ml of the bottom dispersion remaining in the cylinder is transferred to a glass petri dish having a diameter of about 10 cm using about 30 ml of distilled water. After evaporating the water in the petri dish in a constant temperature bath of 40 ± 1 ° C., the weight is measured to calculate the weight of the solid on the petri dish, and the suspension rate is obtained by the following formula.
Suspension rate (%) = 111 (A−B) / A
A (g) = Sample weight of water-dispersible agricultural chemical solid preparation B (g) = Weight of solid in 25 ml of lower part (Note) “Inverted” means that the stoppered cylinder is rotated 180 ° by hand, This is done in about 2 seconds with the undo operation.
試験例２
実施例１〜４、参考例１、２と比較例１、４の各製剤を１０００倍に水で希釈し、手動散布器でキャベツ葉に十分量散布した。風乾後、キャベツ葉を採取し、カップ内にキャベツ葉を５枚入れ２齢ハスモンヨトウ幼虫を１０頭放飼後２５℃インキュベ−タ−内で３日間飼育した。その後人工飼料の入ったカップ内にハスモンヨトウ幼虫を移し、２５℃インキュベ−タ−内で個体飼育した。飼育１０日後にウイルス感染死虫数を調査し、結果を下表２に示した。
Test example 2
Each formulation of Examples 1 to 4 , Reference Examples 1 and 2 and Comparative Examples 1 and 4 was diluted 1000 times with water, and a sufficient amount was sprayed on cabbage leaves with a manual sprayer. After air-drying, cabbage leaves were collected, 5 pieces of cabbage leaves were put in a cup, and 10 2nd-year-old Spodoptera larvae were released and then kept in a 25 ° C. incubator for 3 days. After that, the scallop larvae were transferred into a cup containing artificial feed, and were bred individually in a 25 ° C. incubator. The number of virus-infected dead insects was investigated 10 days after the breeding, and the results are shown in Table 2 below.
表１及び２の結果から明らかなように、本発明の水分散性農薬固形製剤は、水希釈時の湿潤性、分散性および懸垂性が優れており、均一な散布をすることが可能であり、且つ微生物農薬の効果（殺虫効果）が優れている。 As is apparent from the results of Tables 1 and 2, the water-dispersible agricultural chemical solid preparation of the present invention has excellent wettability, dispersibility and suspension when diluted with water, and can be uniformly sprayed. And the effect (insecticidal effect) of the microbial pesticide is excellent.
Claims (6)
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| JP2006206105A JP4644165B2 (en) | 2006-07-28 | 2006-07-28 | Water-dispersible microbial pesticide solid preparation |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02157204A (en) * | 1988-12-08 | 1990-06-18 | Hokko Chem Ind Co Ltd | Stable insecticidal preparation and stabilizer |
| JPH0656614A (en) * | 1992-07-31 | 1994-03-01 | Central Glass Co Ltd | Agricultural chemical of microorganism |
| JP2004123606A (en) * | 2002-10-02 | 2004-04-22 | Kumiai Chem Ind Co Ltd | Wettable composition for agriculture, method for producing the same, and preservation method for the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02157204A (en) * | 1988-12-08 | 1990-06-18 | Hokko Chem Ind Co Ltd | Stable insecticidal preparation and stabilizer |
| JPH0656614A (en) * | 1992-07-31 | 1994-03-01 | Central Glass Co Ltd | Agricultural chemical of microorganism |
| JP2004123606A (en) * | 2002-10-02 | 2004-04-22 | Kumiai Chem Ind Co Ltd | Wettable composition for agriculture, method for producing the same, and preservation method for the same |
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