JP4330718B2

JP4330718B2 - Agricultural and horticultural insecticide composition

Info

Publication number: JP4330718B2
Application number: JP23925499A
Authority: JP
Inventors: 耕一西牟田; 正明猪野; 智明本郷; 健吉濱; 俊明山中
Original assignee: サンケイ化学株式会社
Priority date: 1999-08-26
Filing date: 1999-08-26
Publication date: 2009-09-16
Anticipated expiration: 2019-08-26
Also published as: JP2001064103A

Description

【０００１】
【発明の属する技術分野】
本発明は中鎖脂肪酸グリセライドとバチルスチューリンゲンシス菌の産生毒素を有効成分として含有する野菜、果樹、花き類等の殺虫剤に関するものである。より具体的には野菜、果樹、花き類を加害するコナガ類、ヨトウ類、ハマキ類、ガ類等の害虫防除剤に関するものである。
【０００２】
【従来の技術とその問題点】
農作物の品質の向上、増収にかかわる農薬の果たす役割は非常に重要で、近年、農業生産を行う上で、欠かすことのできない資材である。毎年多数の有機化合物が国内外で農薬として使用されている。現在の代表的な殺虫剤として有機リン系、カーバメイト系、合成ピレスロイド系、昆虫成長制御剤（ＩＧＲ）など各種有機化合物を成分とする殺虫剤が多数ある。これらは安全性が高く、低薬量で、広い殺虫スペクトルを有し、防除法が手軽なことより、広く農業生産活動に使用され、品質の向上、増収に貢献している。
【０００３】
近年、消費者のニーズの多様化により、農業生産もそれに対応し、農作物の種類の増加、栽培体系が多様化してきている。この弊害として病害虫の発生状況も変化し、農薬の使用回数も増加し、同一系統の農薬の連続散布による病害虫の薬剤抵抗性の出現が深刻な問題になり、薬剤の種類、使用方法に様々な制約が設けられている。また消費者の安全性への意識の高まりにより、有機化合物を成分とする農薬を取り巻く環境は年々厳しくなり、使用回数の増加による環境への負荷等が問題視されてきている。
後述の本発明にかかる中鎖脂肪酸グリセライドとバチルスチューリンゲンシス菌の産生毒素を有効成分とする殺虫剤組成物に関する先行技術としては、中鎖脂肪酸グリセライド、バチルスチューリンゲンシス菌の産生毒素単独での先行技術は数多く報告されているが、両者の混合における殺虫活性、製剤化に関するものはない。また、該毒素との混合物に関しては、特開昭６２−２９５０５号公報、特公昭５５−４７００７号公報がある。しかしそれらは合成ピレスロイド、カルタップ塩などのそれ自体に同様の殺虫活性を有する殺虫成分との混合に関する先行技術であり、中鎖脂肪酸グリセライドとバチルスチューリンゲンシス菌の産生毒素との殺虫効果について言及したものではない。
【０００４】
【発明が解決しようとする課題】
現在の代表的な殺虫剤として有機リン系、カーバメイト系、合成ピレスロイド系、昆虫成長制御剤（ＩＧＲ）など各種有機化合物を成分とする殺虫剤が多数ある。しかし害虫の薬剤抵抗性の発現、環境への負荷等の問題で、近年、有用微生物、天敵、フェロモン等の農業生産への利用法の研究が進み、実用化されている。これらはいずれも人畜への影響は少なく、環境への影響が少ないクリーンな防除法として注目を浴びている。
しかしこれらは製剤、散布等の処理に手間がかかり、殺虫スペクトルが狭く、雨、光等による効力低下、高価であるなど問題があり、農業生産への普及すなわち、効果的な適用方法の発見に苦慮しているのが現状である。それらの中で有用微生物であるバチルスチューリンゲンシス菌の産生毒素は、有機化合物を有効成分とする殺虫剤で薬剤抵抗性が発現した難防除害虫のコナガに対して有効である。
また比較的殺虫スペクトルも広く、タマナキンウワバ、ハスモンヨトウ、シロイチモジヨトウ、チャハマキ、チャノコカクモンハマキ、チャノホソガ、スジキリヨトウ、シバツトガ、タマナヤガなどの害虫に対して有効で、以前から注目され、殺虫剤として商品化されてきた。しかしバチルスチューリンゲンシス菌の産生毒素は紫外線による効力低下が激しく、また植物体に付着した毒素を害虫が摂取することにより、効力が発現するタイプの殺虫活性のため、十分に植物体に毒素が付着していないと効果が不安定になるなどの問題がある。
上述のように農園芸作物の害虫防除剤として様々な問題点が浮き彫りになるなか、それに代わる防除剤が強く要望されてきている。本発明者等は、かかる観点から鋭意検討した結果、植物体、特にヤシ油等から抽出された中鎖脂肪酸グリセライドと有用微生物であるバチルスチューリンゲンシス菌の産生毒素を有効成分とする殺虫剤組成物が薬剤抵抗性の発現した害虫に有効で、耐雨性、残効性が優れ、農作物に安全でかつ無毒ないしは低毒性で、環境に負担の少ない殺虫剤組成物であることを知見し、この知見に基づいて本発明を完成した。以上の記述から明らかなように、本発明の目的は上述のような問題点のない農園芸用殺虫剤を提供することである。
【０００５】
【課題を解決するための手段】
本発明は、下記（１）、（２）、（３）および（４）の構成を有する。
【０００６】
（１）カプリル酸トリグリセライドおよびカプリン酸トリグリセライドの混合物と、バチルスチューリンゲンシス菌の産生毒素とを含有することを特徴とする農園芸用殺虫剤組成物。
【０００７】
（２）前記混合物は、前記カプリル酸トリグリセライド７５％、および、前記カプリン酸トリグリセライド２５％の混合物である前記（１）に記載の農園芸用殺虫剤組成物。
【０００８】
（３）前記混合物５０〜９０質量部、前記産生毒素０．１〜４０質量部および界面活性剤１〜９．９質量部を含有する油系フロアブル剤型であることを特徴とする前記（１）または前記（２）に記載の農園芸用殺虫剤組成物。
【０００９】
（４）前記界面活性剤は、アニオン系界面活性剤、カチオン系界面活性剤、ノニオン系界面活性剤および両性界面活性剤よりなる群から選択される１種以上の界面活性剤であることを特徴とする前記（３）に記載の農園芸用殺虫剤組成物。
【００１１】
本発明の構成と効果につき以下に詳述する。本発明に使用されている中鎖脂肪酸グリセライドは、天然に存在する物質であり、無味無臭の特性を有することから、食用油脂、食品製造機器の潤滑油、医薬品用製品、化粧品の添加剤として広く使われているものである。またその化学構造中に二重結合を有さないため、一般の食用油にくらべ、酸化作用を受け難い特徴を有している。
一般的に広く使用されている中鎖脂肪酸グリセライドは、グリセリン１分子に炭素数７〜１１の中鎖脂肪酸３分子とが結合したものが大部分であるが、部分的に加水分解されてグリセリンに１〜２つの中鎖脂肪酸が付加したものも存在する。これらは単独でのダニ、アブラムシ類への殺虫活性およびうどんこ病等の殺菌活性が報告されているが、バチルスチューリンゲンシス菌の産生毒素との混合による殺虫活性についての報告は皆無であり、本発明が最初のものである。
また炭素数６以下の低級脂肪酸グリセライドおよび炭素数１２以上の長級脂肪酸グリセライドとバチルスチューリンゲンシス菌の産生毒素との混合物による殺虫活性は、ある程度の殺虫活性は認められるものの十分ではない。この原因としては不明であるが、中鎖脂肪酸グリセライドは植物体への産生毒素の付着能力が高く、害虫の皮膚に対して格別な浸透力を有するため殺虫活性が高いと推察される。しかし低級、長級脂肪酸グリセライドは、水希釈後、散布を行う際、水中および葉面上で固化する性質があり、本来同じような性質を持ち合わせているが、現在公知の散布方法では性質を発揮できないのではないかと推察される。
【００１２】
本発明に使用されているバチルスチューリンゲンシス菌の産生毒素は、バチルスチューリンゲンシス菌の亜種クルスタキー、アイザワイ、ケニアーエなどの体内に生成する結晶毒素タンパクで、人畜に対しては結晶毒素タンパクが酸性の胃液によって分解され毒性を示さないため非常に安全性の高い殺虫成分である。現在製品化の際、芽胞の殺滅処理を行っているものと、行っていないものが商品として数多く発売されている。
バチルスチューリンゲンシス菌の産生毒素の殺虫活性は、産生された結晶毒素タンパクがリン翅目害虫の中腸のアルカリ条件下で可溶化された後、タンパク分解酵素の作用を受け殺虫活性を示すタンパクが生成する。その活性トキシンタンパクが中腸の上皮細胞膜に結合して、上皮細胞を破壊する。その結果、害虫は食物の摂取、消化吸収ができなくなり、餓死したり、弱化した生体に他の微生物、ウイルスが侵入して、病死し、あるいは全身麻痺により死亡する殺虫活性であると報告されている。これらバチルスチューリンゲンシス菌の産生毒素と中鎖脂肪酸グリセライドを混合製剤化を行った際の殺虫活性の報告については皆無であり、本発明が最初のものである。
【００１３】
本発明の中鎖脂肪酸グリセライドとバチルスチューリンゲンシス菌の産生毒素からなる組成物を害虫防除剤として適用する場合は、適切に選択された界面活性剤、担体、水等と混合することによって、水和剤、サスポエマルション剤等の剤型にすることができるが、好ましくは油系フロアブルにすることが望ましい。活性成分の製剤中の配合比は中鎖脂肪酸グリセライドが５０〜９０重量部、バチルスチューリンゲンシス菌の産生毒素が０．１〜４０重量部程度が必要であり、好ましくは合計１００重量部に達するまでの残りは後述の各種界面活性剤からなる。そして使用目的によってはこれらの濃度を適宜増減して良い。
【００１４】
本発明に使用する界面活性剤は限定されない。すなわち、アニオン系、カチオン系、ノニオン系、両性のいずれの界面活性剤も使用でき、それらは単独、若しくは２種類以上混合して使用できる。中鎖脂肪酸グリセライド及びバチルスチューリンゲンシス菌の産生毒素と界面活性剤との混合方法ならびに混合順序は限定されないが、界面活性剤の使用量は、通常前二者に比べて、比較的少量であること並びに、界面活性剤の共存が前二者の混合を容易にすることから、３者をほぼ同時期に混合器中に投入し、機械的に混合することが望ましい。
【００１５】
本発明の組成物の製造に使用する製造機器は、バチルスチューリンゲンシス菌の産生毒素は液体又は固体、中鎖脂肪酸グリセライドは室温で液体であることより、両者を必要な界面活性剤と共に均一混合するには、適切な形態、容量および混合能力を有する混合器もしくは湿式粉砕器を使用する必要がある。それらの具体例としてはホモミキサー、サンドグラインダー、ペイントシェイカー等を挙げることができる。混合条件は限定されないが、５０００ｒｐｍ以上の高速攪拌で１分〜１時間、０．５〜１．０ｍｍのメディアを試作量と同等〜三倍程度加えた後、１分〜５時間、１０００ｒｐｍ程度で攪拌、もしくはシェイクすることが望ましい。
【００１６】
かくして本発明の農園芸用殺虫剤組成物が得られる。該組成物がフロアブル若しくは油系フロアブルである場合、公知方法で対象作物に散布される。後述の試験例３〜５にも示されているように本発明品は、既存の同等の目的の殺虫剤製品より殺虫活性が顕著に優れているだけでなく耐雨性、残効性に優れ、しかも製剤として好ましくは０〜４０℃の条件下で長期保存が可能である。
したがって、本発明は、対象とする農園芸作物用の殺虫剤の分野で既存製品に大きく取って換るべきものである。
【００１７】
【実施例】
次に、実施例、比較例および試験例によって本発明を説明するが、本発明はその要旨を超えない限り、以下の実施例に制約されるものではない。各実施例、比較例において部は重量部をあらわす。
【００１８】
実施例−１
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名トアローＣＴ水和剤産生毒素７％芽胞死滅菌処理東亜合成（株）製）３６部、中鎖脂肪酸グリセライド（商品名Ｏ．Ｄ．Ｏカプリル酸トリグリセライド７５％＋カプリン酸トリグリセライド２５％混合品日清製油（株）製）５５部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００１９】
実施例−２
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名ダイポール水和剤産生毒素１０％芽胞非死滅菌処理サンケイ化学（株）製）２５部、中鎖脂肪酸グリセライド（商品名Ｏ．Ｄ．Ｏカプリル酸トリグリセライド７５％＋カプリン酸トリグリセライド２５％混合品日清製油（株）製）６６部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２０】
実施例−３
バチルスチューリンゲンシス菌（アイザワイ菌）の産生毒素（商品名ゼンターリ−水和剤産生毒素１０％芽胞非死滅菌処理武田薬品工業（株）製）２５部、中鎖脂肪酸グリセライド（商品名Ｏ．Ｄ．Ｏカプリル酸トリグリセライド７５％＋カプリン酸トリグリセライド２５％混合品日清製油（株）製）６６部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２１】
実施例−４
バチルスチューリンゲンシス菌（クルスタキー菌＋アイザワイ菌）の産生毒素（商品名バシレックス水和剤産生毒素１０％芽胞非死滅菌処理塩野義製薬（株）製）２５部、中鎖脂肪酸グリセライド（商品名Ｏ．Ｄ．Ｏカプリル酸トリグリセライド７５％＋カプリン酸トリグリセライド２５％混合品日清製油（株）製）６６部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２２】
比較例−１
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名トアローＣＴ水和剤産生毒素７％芽胞死滅菌処理東亜合成（株）製）３６部、ヤシ油５５部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２３】
比較例−２
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名トアローＣＴ水和剤産生毒素７％芽胞死滅菌処理東亜合成（株）製）３６部、なたね油５５部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２４】
比較例−３
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名ダイポール水和剤産生毒素１０％芽胞非死滅菌処理サンケイ化学（株）製）２５部、ヤシ油６６部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２５】
比較例−４
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名ダイポール水和剤産生毒素１０％芽胞非死滅菌処理サンケイ化学（株）製）２５部、なたね油６６部、界面活性剤（商品名エキセル３００花王（株）製）１部、界面活性剤（商品名エマルゲン９０５花王（株）製）８部を混合後、試作量の同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部の油系フロアブルを得た。
【００２６】
比較例−５
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名トアローＣＴ水和剤産生毒素７％芽胞死滅菌処理東亜合成（株）製）３６部、界面活性剤（商品名ニューカルゲンＦＳ−３ＰＧ竹本油脂（株）製）１０部、消泡剤（商品名アンチホームＥ−２０花王（株）製）０．５部、増粘剤（商品名アグリゾールＦＬ−１０４Ａ花王（株）製）２部、防腐剤（商品名ＰｒｏｘｅｌＧＸＬ（株）ゼネカ製）０．５部、蒸留水５１部を混合後、試作量と同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部のフロアブルを得た。
【００２７】
比較例−６
バチルスチューリンゲンシス菌（クルスタキー菌）の産生毒素（商品名ダイポール水和剤産生毒素１０％芽胞非死滅菌処理サンケイ化学（株）製）２５部、界面活性剤（商品名ニューカルゲンＦＳ−３ＰＧ竹本油脂（株）製）１０部、消泡剤（商品名アンチホームＥ−２０花王（株）製）０．５部、増粘剤（商品名アグリゾールＦＬ−１０４Ａ花王（株）製）２部、防腐剤（商品名ＰｒｏｘｅｌＧＸＬ（株）ゼネカ製）０．５部、蒸留水６２部を混合後、試作量と同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部のフロアブルを得た。
【００２８】
比較例−７
バチルスチューリンゲンシス菌（アイザワイ菌）の産生毒素（商品名ゼンターリ水和剤産生毒素１０％芽胞非死滅菌処理武田薬品工業（株）製）２５部、界面活性剤（商品名ニューカルゲンＦＳ−３ＰＧ竹本油脂（株）製）１０部、消泡剤（商品名アンチホームＥ−２０花王（株）製）０．５部、増粘剤（商品名アグリゾールＦＬ−１０４Ａ花王（株）製）２部、防腐剤（商品名ＰｒｏｘｅｌＧＸＬ（株）ゼネカ製）０．５部、蒸留水６２部を混合後、試作量と同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部のフロアブルを得た。
【００２９】
比較例−８
バチルスチューリンゲンシス菌（クルスタキー菌＋アイザワイ菌）の産生毒素（商品名バシレックス水和剤産生毒素１０％芽胞非死滅菌処理塩野義製薬（株）製）２５部、界面活性剤（商品名ニューカルゲンＦＳ−３ＰＧ竹本油脂（株）製）１０部、消泡剤（商品名アンチホームＥ−２０花王（株）製）０．５部、増粘剤（商品名アグリゾールＦＬ−１０４Ａ花王（株）製）２部、防腐剤（商品名ＰｒｏｘｅｌＧＸＬ（株）ゼネカ製）０．５部、蒸留水６２部を混合後、試作量と同量の１ｍｍ径ガラスビーズを加え、サンドグラインダーで２時間粉砕し、１００部のフロアブルを得た。
【００３０】
比較例−９
トアローＣＴ水和剤産生毒素７％芽胞死滅菌処理東亜合成（株）製
【００３１】
比較例−１０
ダイポール水和剤産生毒素１０％芽胞非死滅菌処理サンケイ化学（株）製
【００３２】
比較例−１１
ゼンターリー水和剤産生毒素１０％芽胞非死滅菌処理武田薬品工業（株）製
【００３３】
比較例−１２
バシレックス水和剤産生毒素１０％芽胞非死滅菌処理塩野義製薬（株）製
【００３４】
本発明の効果を試験例にて説明する。但し、試験例に用いた製剤は実施例−１〜４、比較例−１〜８にしたがって製剤化したもの若しくは比較例−９〜１２に係る市販品である。
【００３５】
試験例−１
実施例−１〜４および比較例−５〜８の製剤をサンプル管瓶に入れ、室温および４０℃虐待条件下に保存し、外観、懸濁安定性、懸垂性を観察した。その結果を表１、２に示した。
【００３６】
【表１】

【００３７】
【表２】

【００３８】
懸濁安定性の判定方法
【数１】

懸垂性の判定方法
１００ｍｌ懸垂管に水道水を入れ、製剤を５００倍相当量に希釈し、１分間に３０回倒立混合を行い、静置５、３０分後の泡立ち、沈殿量、凝集の程度、６０分後の沈殿量、凝集の程度の観察を行った。
懸垂性観察時の凝集の程度判定基準
−；よく分散している
±；若干の凝集が認められる
＋；凝集が認められる
＋＋；激しい凝集が認められる
以上、製剤の保存性に関する検討を行った結果、実施例−１〜４の油系フロアブルの各製剤は、室温、４０℃虐待条件下に保存しても、外観、懸垂性に影響は認められず、懸濁安定性については、保存期間経過にともない、悪化する傾向は認められるが、実用上問題のない数値で推移した。しかし比較例−５〜８の水系フロアブルの各製剤は、外観については、バチルスチューリンゲンシス菌の芽胞を死滅処理したものを使用した比較例−５は変化はみられないものの、死滅処理をしていないものを使用した比較例−６〜８は赤色〜茶色に変色し、処方中に防腐剤を添加しているのにも係わらず、激しい腐敗臭が発生した。
懸濁安定性についてはスケ等は認められないが製剤自体が高粘度となり、最終的には固化し、流動性が失われた。懸垂性は保存期間の経過とともに悪化する傾向が認められ、比較例−５〜８の各製剤は、実用上、長期保存は不可能と考えられた。
【００３９】
試験例−２
実施例−１、２および比較例−１〜４の製剤をサンプル管瓶に入れ、４０℃虐待条件下に保存し、外観、懸濁安定性、懸垂性を観察した。その結果を表３に示した。
【００４０】
【表３】

【００４１】
懸濁安定性の判定方法
【数２】

懸垂性の判定方法
１００ｍｌ懸垂管に水道水を入れ、製剤を５００倍相当量に希釈し、１分間に３０回倒立混合を行い、静置５、３０分後の泡立ち、沈殿量、凝集の程度、６０分後の沈殿量、凝集の程度の観察を行った。
懸垂性観察時の凝集の程度判定基準
−；よく分散している
±；若干の凝集が認められる
＋；凝集が認められる
＋＋；激しい凝集が認められる
以上、油系フロアブルに使用する油の違いによる製剤の保存性の比較を行った結果、実施例−１〜４の中鎖脂肪酸グリセライドを使用する油系フロアブルの各製剤は、４０℃虐待条件下に保存しても、外観、懸垂性に影響は認められず、懸濁安定性も、保存期間の経過とともに悪化する傾向は認められるが、実用上問題はなかった。しかし比較例−１〜４については、保存期間の経過（保存３０日後）とともに黄色に変色し、脂肪酸臭が強くなった。また懸垂性は沈殿量への影響はみられないものの、泡立ちがなくなり、希釈液面上に油状物が浮遊してきた。
【００４２】
試験例−３
４０℃虐待条件下に３ヶ月間保存した実施例−１〜４および比較例−５〜８の製剤を所定濃度に希釈し、また対照として比較例−９〜１２を所定濃度に希釈し、キャベツ（品種おきな３〜４葉期）に噴霧器にて散布し、散布１日後キャベツ葉を採取し、ポリカップに入れ、コナガ４齢幼虫を５頭放虫し、２５℃の暗室に保存した。調査は放虫１日後、３日後の生死状況、食害程度を観察した。その結果を表４に示した。尚、試験は３反復で行った。
【００４３】
【表４】

【００４４】
コナガのキャベツ葉の食害程度
−；食害なし
±；食害がキャベツ葉の面積の５％未満
＋；食害がキャベツ葉の面積の５％〜１０％
＋＋；食害がキャベツ葉の面積の１０％〜２５％
＋＋＋；食害がキャベツ葉の面積の２５％〜５０％
＋＋＋＋；食害がキャベツ葉の面積の５０％以上
以上、各製剤を長期保存した場合のコナガに対する殺虫活性への影響を検討した結果、実施例−１〜４の油系フロアブルの各製剤は、４０℃９０日間虐待条件下に保存しても、コナガに対する殺虫活性の減退は認められなかった。それに対して比較例−５〜８の水系フロアブルの各製剤は、虐待条件下で保存すると、コナガに対する殺虫活性の減退が顕著に認められ、製剤の物理性と同様、殺虫活性の面からも長期保存は不可能と考えられた。
また、既存薬剤の比較例−９〜１２と実施例−１〜４のコナガに対する殺虫活性を比較すると、実施例−１〜４の未保存品、９０日間保存品ともに、比較例−９〜１２と同濃度でありながら、コナガに対する殺虫活性（速効性）が向上する傾向が認められた。
【００４５】
試験例−４
実施例−１〜４および比較例−５〜１２の製剤を所定濃度に希釈し、圃場に定植済みキャベツ（品種おきな７〜８葉期）に散布し、散布１日後、６日後、１０日後キャベツ葉を採取し、ポリカップに入れ、コナガ４齢幼虫を５頭放虫し、２５℃の暗室に保存した。調査は放虫１日後、３日後の生死状況、食害程度を観察した。その結果を表５、表６、表７に示した。尚、試験は３反復で行った。
【００４６】
【表５】

【００４７】
【表６】

【００４８】
【表７】

【００４９】
コナガのキャベツ葉の食害程度
−；食害なし
±；食害がキャベツ葉の面積の５％未満
＋；食害がキャベツ葉の面積の５％〜１０％
＋＋；食害がキャベツ葉の面積の１０％〜２５％
＋＋＋；食害がキャベツ葉の面積の２５％〜５０％
＋＋＋＋；食害がキャベツ葉の面積の５０％以上
以上、各製剤のコナガに対する殺虫活性の残効性について、自然条件下の圃場にて検討した結果、既存薬剤の比較例−９〜１２では、散布６日後でコナガに対する殺虫活性の減退が認められた。これは既存薬剤が耐雨性、残効性がおとる、本来の通説通りの結果であった。これに対して実施例−１〜４の油系フロアブルの各製剤は、散布後日数が経過しても、コナガに対する殺虫活性の減退が僅かで、残効性が既存薬剤と比較し向上していることが認められた。
また比較例−５〜８の水系フロアブルの各製剤は、既存薬剤と同様に、散布６日後でコナガに対する殺虫活性が大きく減退し、残効性の改善は認められなかった。
【００５０】
試験例−５
実施例−３および比較例−７、−１１の製剤を所定濃度に希釈し、圃場に定植済みキャベツ（品種おきな７〜８葉期）に散布し、散布１日後、６日後、１０日後キャベツ葉を採取し、ポリカップに入れ、ハスモンヨトウ３齢幼虫を１０頭放虫し、２５℃の暗室に保存した。調査は放虫２日後、４日後の生死状況、食害程度を観察した。その結果を表８、表９、表１０に示した。尚、試験は３反復で行った。
【００５１】
【表８】

【００５２】
【表９】

【００５３】
【表１０】

【００５４】
ハスモンヨトウのキャベツ葉の食害程度
−；食害なし
±；食害がキャベツ葉の面積の５％未満
＋；食害がキャベツ葉の面積の５％〜１０％
＋＋；食害がキャベツ葉の面積の１０％〜２５％
＋＋＋；食害がキャベツ葉の面積の２５％〜５０％
＋＋＋＋；食害がキャベツ葉の面積の５０％以上
以上、各製剤のハスモンヨトウに対する殺虫活性の残効性について、自然条件下の圃場にて検討した結果、実施例−３の油系フロアブルの製剤は、コナガに対する殺虫活性（残効性）と同様に、散布後日数が経過してもハスモンヨトウに対する殺虫活性の減退が僅かで、残効性が既存薬剤と比較し向上していることが認められた。
また比較例−７の水系フロアブルの各製剤は、既存薬剤の比較例−１１と同様に、散布６日後でハスモンヨトウに対する殺虫活性が大きく減退し、残効性の改善は認められなかった。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to insecticides such as vegetables, fruit trees, and flowering plants containing medium chain fatty acid glyceride and toxin produced by Bacillus thuringiensis as active ingredients. More specifically, the present invention relates to insect pest control agents such as diamondback moths, sweet potatoes, oysters, moths and the like that harm vegetables, fruit trees and flowers.
[0002]
[Prior art and its problems]
The role of agricultural chemicals for improving the quality of crops and increasing sales is very important, and is an indispensable material for agricultural production in recent years. A large number of organic compounds are used as agricultural chemicals at home and abroad every year. There are many insecticides containing various organic compounds such as organophosphorus, carbamate, synthetic pyrethroid, and insect growth regulator (IGR) as typical insecticides. These are highly safe, have low dosage, have a broad insecticidal spectrum, and are easy to control, so they are widely used in agricultural production activities, contributing to quality improvement and increased sales.
[0003]
In recent years, due to diversification of consumer needs, agricultural production has also responded to this, and the types of crops have increased and the cultivation system has diversified. As a result of this adverse effect, the occurrence of pests has changed, the use of pesticides has increased, and the emergence of pesticide resistance due to continuous spraying of pesticides of the same system has become a serious problem. There are restrictions. In addition, with increasing consumer awareness of safety, the environment surrounding pesticides composed of organic compounds has become harsher year by year, and the burden on the environment due to the increased number of uses has been regarded as a problem.
As the prior art relating to the insecticidal composition comprising the medium-chain fatty acid glyceride and Bacillus thuringiensis-producing toxin according to the present invention described later as the active ingredients, the medium-chain fatty acid glyceride and the prior art of Bacillus thuringiensis-producing toxin alone Have been reported, but there is nothing related to insecticidal activity and formulation in the mixture of both. Japanese Patent Application Laid-Open No. 62-29505 and Japanese Patent Publication No. 55-47007 are available for the mixture with the toxin. However, they are prior arts related to the mixing of synthetic pyrethroids, cartap salts, etc. with insecticidal ingredients having similar insecticidal activity, and mention the insecticidal effect of medium-chain fatty acid glycerides and toxins produced by Bacillus thuringiensis. is not.
[0004]
[Problems to be solved by the invention]
There are many insecticides containing various organic compounds such as organophosphorus, carbamate, synthetic pyrethroid, and insect growth regulator (IGR) as typical insecticides. However, in recent years, research on the use of useful microorganisms, natural enemies, pheromones and the like for agricultural production has been advanced and put into practical use due to problems such as the development of drug resistance of pests and the burden on the environment. All of these are attracting attention as clean control methods with little impact on human livestock and less impact on the environment.
However, these are troublesome in the treatment of preparations, spraying, etc., have a narrow insecticidal spectrum, decrease in efficacy due to rain, light, etc., are expensive, and spread to agricultural production, that is, to find effective application methods. The current situation is struggling. Among them, the toxin produced by Bacillus thuringiensis, which is a useful microorganism, is effective against the hard-to-control insect pest that has developed drug resistance with an insecticide containing an organic compound as an active ingredient.
In addition, it has a relatively broad insecticidal spectrum and is effective against insects such as Tamanakinawaba, Hasmonyotou, Shirouchimojiyotou, Chahamaki, Chanokokukakumonhamaki, Chanohosoga, Sugikirayotou, Shibatatsuga, Tamanayaga, and has been commercialized as an insecticide. . However, the toxin produced by Bacillus thuringiensis is drastically reduced by ultraviolet rays, and when the insects ingest the toxin attached to the plant, the toxin is sufficiently attached to the plant because of the insecticidal activity that manifests its efficacy. If not, there are problems such as unstable effects.
As described above, various problems have been highlighted as pest control agents for agricultural and horticultural crops, and there has been a strong demand for control agents that can replace them. As a result of intensive investigations from such a viewpoint, the present inventors have found that an insecticide composition comprising a medium-chain fatty acid glyceride extracted from a plant body, particularly coconut oil and the like, and a toxin produced by Bacillus thuringiensis, which is a useful microorganism, as active ingredients Has been found to be an insecticide composition that is effective against insect pests that exhibit drug resistance, has excellent rain resistance and residual effect, is safe and non-toxic or low toxic for agricultural crops, and has a low environmental burden. The present invention has been completed based on the above. As is clear from the above description, an object of the present invention is to provide an agricultural and horticultural insecticide which does not have the above-mentioned problems.
[0005]
[Means for Solving the Problems]
The present invention provides the following (1), (2), (3) And (4) It has the composition of.
[0006]
(1) A mixture of caprylic acid triglyceride and capric acid triglyceride and a toxin produced by Bacillus thuringiensis The It is characterized by containing Agricultural and horticultural insecticide composition.
[0007]
(2) The mixture is A mixture of 75% caprylic acid triglyceride and 25% capric acid triglyceride The agricultural and horticultural insecticide composition according to (1) above.
[0008]
(3) Said mixture 50-90 Parts by mass, Above Toxin produced 0.1-40 Contains 1 part by weight and 1 to 9.9 parts by weight of surfactant It is an oil-based flowable agent type In (1) or (2) above The agricultural and horticultural insecticide composition described.
[0009]
(4) The surfactant is , Anion Surfactants , Cation Surfactants , Nonion Surfactants and Amphoteric surfactant One selected from the group consisting of The above surfactants (3) characterized in that The agricultural and horticultural insecticide composition described.
[0011]
The configuration and effects of the present invention will be described in detail below. The medium chain fatty acid glyceride used in the present invention is a naturally occurring substance and has tasteless and odorless characteristics, so it is widely used as an additive in edible oils and fats, food manufacturing equipment lubricants, pharmaceutical products, and cosmetics. It is what is used. Moreover, since it does not have a double bond in its chemical structure, it has a feature that it is less susceptible to oxidation than ordinary edible oils.
Most of the medium chain fatty acid glycerides that are widely used are those in which one molecule of glycerin and three molecules of medium chain fatty acid having 7 to 11 carbon atoms are combined, but are partially hydrolyzed into glycerin. There are also those with one or two medium chain fatty acids added. These have reported insecticidal activity against mites and aphids alone, and bactericidal activity such as powdery mildew, but there are no reports of insecticidal activity by mixing with toxins produced by Bacillus thuringiensis. The invention is the first.
In addition, the insecticidal activity of the mixture of lower fatty acid glycerides having 6 or less carbon atoms and long fatty acid glycerides having 12 or more carbon atoms and toxin produced by Bacillus thuringiensis is not sufficient, although some insecticidal activity is observed. Although the cause of this is unknown, it is presumed that medium-chain fatty acid glyceride has a high ability to adhere the produced toxin to the plant body and has a particularly high osmotic activity on the skin of pests, so that it has a high insecticidal activity. However, lower and long fatty acid glycerides have the property of solidifying in water and on the leaf surface when sprayed after dilution with water. I guess it is impossible.
[0012]
The toxin produced by Bacillus thuringiensis used in the present invention is a crystalline toxin protein produced in the body of subtypes of Bacillus thuringiensis, such as Kurstakey, Aizawai, Kenyae, etc. It is a very safe insecticidal component because it is decomposed by gastric juice and does not show toxicity. At the time of commercialization, there are many products that have been spore-killed and those that have not.
The insecticidal activity of the toxin produced by Bacillus thuringiensis is that the produced crystal toxin protein is solubilized under alkaline conditions in the midgut of the moss, and then the protein that exhibits insecticidal activity is affected by the action of proteolytic enzymes. Generate. The active toxin protein binds to the epithelial membrane of the midgut and destroys epithelial cells. As a result, pests are reported to have insecticidal activity that prevents food intake, digestion and absorption, starvation, or death of other microorganisms or viruses by invading weakened organisms, or death due to general paralysis. Yes. There are no reports of insecticidal activity when a mixed preparation of the toxin produced by Bacillus thuringiensis and medium-chain fatty acid glyceride is prepared, and the present invention is the first.
[0013]
When applying the composition comprising the medium chain fatty acid glyceride of the present invention and the toxin produced by Bacillus thuringiensis as a pest control agent, it is hydrated by mixing with a suitably selected surfactant, carrier, water, etc. However, it is desirable to make it oil-based flowable. The mixing ratio of the active ingredient in the preparation requires 50 to 90 parts by weight of medium-chain fatty acid glyceride and 0.1 to 40 parts by weight of the toxin produced by Bacillus thuringiensis, preferably until the total reaches 100 parts by weight. The remainder consists of various surfactants described below. Depending on the purpose of use, these concentrations may be increased or decreased as appropriate.
[0014]
The surfactant used in the present invention is not limited. That is, any of anionic, cationic, nonionic and amphoteric surfactants can be used, and these can be used alone or in admixture of two or more. The mixing method and mixing order of medium chain fatty acid glyceride and Bacillus thuringiensis toxin and surfactant are not limited, but the amount of surfactant used is usually relatively small compared to the former two. In addition, since the coexistence of the surfactant facilitates the mixing of the former two, it is desirable that the three are put into the mixer almost simultaneously and mixed mechanically.
[0015]
The production equipment used for the production of the composition of the present invention is that the toxin produced by Bacillus thuringiensis is liquid or solid, and the medium-chain fatty acid glyceride is liquid at room temperature, so both are uniformly mixed with the necessary surfactant. It is necessary to use a mixer or wet grinder having an appropriate form, capacity and mixing capacity. Specific examples thereof include a homomixer, a sand grinder, and a paint shaker. The mixing conditions are not limited, but after adding a medium of 0.5 to 1.0 mm, which is equivalent to about 3 times as much as the prototype amount, at a high speed stirring of 5000 rpm or more, about 1 minute to 5 hours and about 1000 rpm. It is desirable to stir or shake.
[0016]
Thus, the agricultural and horticultural insecticide composition of the present invention is obtained. When the composition is flowable or oil-based flowable, it is applied to the target crop by a known method. As shown in Test Examples 3 to 5 described later, the present invention product is not only excellent in insecticidal activity but also excellent in rain resistance and residual effect than existing insecticide products for the same purpose, Moreover, the preparation can be stored for a long period of time preferably at 0 to 40 ° C.
Therefore, the present invention should largely replace existing products in the field of insecticides for targeted agricultural and horticultural crops.
[0017]
【Example】
Next, the present invention will be described with reference to examples, comparative examples, and test examples. However, the present invention is not limited to the following examples unless it exceeds the gist. In each example and comparative example, the part represents part by weight.
[0018]
Example-1
Bacillus thuringiensis (Kursta key) produced toxin (trade name Toarro CT wettable powder produced toxin 7% spore death sterilization treatment Toa Gosei Co., Ltd.) 36 parts, medium chain fatty acid glyceride (trade name OD Capryl) Acid triglyceride 75% + capric acid triglyceride 25% mixture Nisshin Oil Co., Ltd. 55 parts, surfactant (trade name EXCEL 300 Kao Co., Ltd.) 1 part, surfactant (trade name Emulgen 905 Kao (trade name) After mixing 8 parts), the same amount of 1 mm diameter glass beads as a prototype was added and pulverized with a sand grinder for 2 hours to obtain 100 parts of an oil-based flowable.
[0019]
Example-2
Bacillus thuringiensis (Kursta key) produced toxin (trade name: Dipole wettable powder, produced toxin 10%, non-spore sterilization treatment Sankei Chemical Co., Ltd.) 25 parts, medium chain fatty acid glyceride (trade name: OD Capryl) Acid triglyceride 75% + capric triglyceride 25% mixture Nisshin Oil Co., Ltd. 66 parts, surfactant (trade name EXCEL 300 manufactured by Kao Corporation) 1 part, surfactant (trade name Emulgen 905 Kao (trade name) After mixing 8 parts), the same amount of 1 mm diameter glass beads as a trial product was added and pulverized with a sand grinder for 2 hours to obtain 100 parts of oil-based flowable.
[0020]
Example-3
Bacillus thuringiensis (Aisawa) produced toxin (trade name: Zentari-wettable powder produced toxin 10% non-spore sterilization treatment Takeda Pharmaceutical Co., Ltd.) 25 parts, medium chain fatty acid glyceride (trade name OD O Caprylic acid triglyceride 75% + Capric acid triglyceride 25% mixture Nisshin Oil Co., Ltd. 66 parts, Surfactant (trade name Excel 300 Kao Co., Ltd.) 1 part, Surfactant (trade name Emulgen 905 After mixing 8 parts (produced by Kao Corporation), the same amount of 1 mm diameter glass beads as the trial product was added and pulverized with a sand grinder for 2 hours to obtain 100 parts of oil-based flowable.
[0021]
Example-4
Bacillus thuringiensis bacterium (Kursta key bacterium + Aizawai bacterium) produced toxin (trade name: Basilex wettable powder produced toxin 10% non-spore sterilization treatment Shionogi & Co., Ltd.) 25 parts, medium chain fatty acid glyceride (trade name O .D.O Caprylic acid triglyceride 75% + capric acid triglyceride 25% mixed product 66 parts Nisshin Oil Co., Ltd., surfactant (trade name EXCEL 300 manufactured by Kao Corporation) 1 part, surfactant (product) After mixing 8 parts of name Emulgen 905 manufactured by Kao Co., Ltd., the same amount of 1 mm diameter glass beads as a trial product was added and pulverized with a sand grinder for 2 hours to obtain 100 parts of oil-based flowable.
[0022]
Comparative Example-1
Bacillus thuringiensis (Kursta key fungus) produced toxin (trade name Toarro CT wettable powder produced toxin 7% spore death sterilization treatment Toa Gosei Co., Ltd.) 36 parts, coconut oil 55 parts, surfactant (trade name Excel 300) After mixing 1 part of Kao Co., Ltd.) and 8 parts of surfactant (trade name: Emulgen 905 Kao Co., Ltd.), add the same amount of 1 mm diameter glass beads as the prototype, and grind it with a sand grinder for 2 hours. 100 parts of an oil-based flowable were obtained.
[0023]
Comparative Example-2
Bacillus thuringiensis (Kursta key) produced toxin (trade name: Toorro CT wettable powder, produced toxin 7% Spore death sterilization treatment Toa Gosei Co., Ltd.) 36 parts, rapeseed oil 55 parts, surfactant (trade name Excel 300 Kao) 1 part of a product (made by Co., Ltd.) and 8 parts of a surfactant (product name: Emulgen 905, made by Kao Co., Ltd.) are mixed, and then the same amount of 1 mm diameter glass beads of a trial quantity is added and crushed with a sand grinder for 2 hours. Part of oil-based flowable was obtained.
[0024]
Comparative Example-3
Toxins produced by Bacillus thuringiensis (Kursta key) (trade name: Dipole wettable powder, 10% produced by non-spore sterilized spore-treated Sankei Chemical Co., Ltd.) 25 parts, palm oil 66 parts, surfactant (trade name Excel 300) After mixing 1 part of Kao Co., Ltd.) and 8 parts of surfactant (trade name: Emulgen 905 Kao Co., Ltd.), add the same amount of 1 mm diameter glass beads as the prototype, and grind it with a sand grinder for 2 hours. 100 parts of an oil-based flowable were obtained.
[0025]
Comparative Example-4
Toxins produced by Bacillus thuringiensis (Kursta key fungus) (trade name: Dipole wettable powder, 10% produced toxin, non-spore sterilization treatment Sankei Chemical Co., Ltd.) 25 parts, rapeseed oil 66 parts, surfactant (trade name Excel 300 Kao) 1 part of a product (made by Co., Ltd.) and 8 parts of a surfactant (product name: Emulgen 905, made by Kao Co., Ltd.) are mixed, and then the same amount of 1 mm diameter glass beads of a trial quantity is added and crushed with a sand grinder for 2 hours. Part of oil-based flowable was obtained.
[0026]
Comparative Example-5
Bacillus thuringiensis (Kursta key) produced toxin (trade name Toarro CT wettable powder produced toxin 7% spore death sterilization treatment Toa Gosei Co., Ltd.) 36 parts, surfactant (trade name New Calgen FS-3PG Takemoto Yushi 10 parts), defoaming agent (trade name: Anti Home E-20, Kao Corporation) 0.5 part, thickener (trade name: Agrisol FL-104A, Kao Corporation) 2 parts, antiseptic After mixing 0.5 parts of the agent (trade name: Proxel GXL Co., Ltd.) and 51 parts of distilled water, add 1 mm diameter glass beads of the same amount as the prototype, pulverize with a sand grinder for 2 hours, and 100 parts of floorable Got.
[0027]
Comparative Example-6
Bacillus thuringiensis (Kursta key) produced toxin (trade name: Dipole wettable powder, produced toxin 10%, non-spore sterilization treatment Sankei Chemical Co., Ltd.) 25 parts, surfactant (trade name: New Calgen FS-3PG Takemoto Yushi 10 parts), defoaming agent (trade name: Anti Home E-20, Kao Corporation) 0.5 part, thickener (trade name: Agrisol FL-104A, Kao Corporation) 2 parts, antiseptic After mixing 0.5 parts of the agent (trade name: Proxel GXL Co., Ltd.) and 62 parts of distilled water, add 1 mm diameter glass beads of the same amount as the prototype, pulverize with a sand grinder for 2 hours, and 100 parts of floorable Got.
[0028]
Comparative Example-7
Bacillus thuringiensis (Aisawai) produced toxin (trade name: Zentari wettable powder, produced toxin 10%, non-spore sterilization treatment Takeda Pharmaceutical Co., Ltd.) 25 parts, surfactant (trade name: New Calgen FS-3PG Takemoto 10 parts by oil and fat Co., Ltd., 0.5 parts by defoaming agent (trade name: Antihome E-20, manufactured by Kao Corporation), 2 parts by thickener (trade name: Agrisol FL-104A, produced by Kao Corporation), After mixing 0.5 parts of preservative (trade name: Proxel GXL Co., Ltd., Zeneca) and 62 parts of distilled water, add 1 mm diameter glass beads of the same amount as the prototype, and grind it with a sand grinder for 2 hours. Got a flowable.
[0029]
Comparative Example-8
Bacillus thuringiensis bacteria (Kurstakey bacteria + Aizawai bacteria) produced toxin (trade name: Basilex wettable powder, produced toxin 10% non-spore sterilization treatment Shionogi Pharmaceutical Co., Ltd.) 25 parts, surfactant (trade name New Calgen) FS-3PG Takemoto Yushi Co., Ltd. 10 parts, antifoaming agent (trade name: Antihome E-20, Kao Corporation) 0.5 part, thickener (trade name: Agrisol FL-104A, Kao Corporation ) After mixing 2 parts, 0.5 part of preservative (trade name: Proxel GXL, manufactured by Zeneca Co., Ltd.) and 62 parts of distilled water, add the same amount of 1 mm diameter glass beads as the prototype, and grind with a sand grinder for 2 hours. 100 parts of flowable were obtained.
[0030]
Comparative Example-9
Toarro CT wettable powder 7% Toxin produced by Toa Gosei Co., Ltd.
[0031]
Comparative Example-10
Dipole wettable powder 10% produced toxin Non-spore sterilization treatment Sankei Chemical Co., Ltd.
[0032]
Comparative Example-11
Zentary wettable powder Produced toxin 10% Non-spore sterilization treatment Takeda Pharmaceutical Co., Ltd.
[0033]
Comparative Example-12
Basilex wettable powder Produced toxin 10% Non-spore sterilization treatment Shionogi & Co., Ltd.
[0034]
The effect of the present invention will be described using test examples. However, the formulations used in the test examples are those formulated according to Examples-1 to 4 and Comparative Examples-1 to 8 or commercial products according to Comparative Examples-9 to 12.
[0035]
Test Example-1
The preparations of Examples-1 to 4 and Comparative Examples-5 to 8 were put into sample tube bottles, stored at room temperature and 40 ° C abuse conditions, and appearance, suspension stability, and suspension were observed. The results are shown in Tables 1 and 2.
[0036]
[Table 1]

[0037]
[Table 2]

[0038]
Method for judging suspension stability
[Expression 1]

Judgment method of suspension
Tap water is put into a 100 ml suspension tube, the preparation is diluted to a 500-fold equivalent amount, mixed by inversion 30 times per minute, left standing, foaming after 30 minutes, the amount of sediment, the degree of aggregation, after 60 minutes The amount of precipitation and the degree of aggregation were observed.
Criteria for determining the degree of aggregation during suspension observation
-; Well dispersed
±: Some aggregation is observed
+: Aggregation observed
++: Vigorous aggregation is observed
As described above, as a result of the investigation on the preservability of the preparation, each of the oil-based flowable preparations of Examples-1 to 4 has an influence on the appearance and the suspension property even when stored under the abuse condition at room temperature and 40 ° C. First, the suspension stability, although it tended to deteriorate as the storage period progressed, remained unchanged in practical use. However, each of the aqueous flowable preparations of Comparative Examples 5 to 8 was subjected to the killing treatment although Comparative Example-5 using the killed Bacillus thuringiensis spores was not changed. Comparative Examples -6 to 8 which were not used turned red to brown, and despite the addition of a preservative during the formulation, a severe rot odor occurred.
With respect to the suspension stability, no scale was observed, but the formulation itself became highly viscous, eventually solidified, and lost its fluidity. The suspension property tended to deteriorate with the passage of the storage period, and it was considered that the preparations of Comparative Examples-5 to 8 could not be stored for a long time in practical use.
[0039]
Test example-2
The preparations of Examples-1 and 2 and Comparative Examples-1 to 4 were placed in sample tube bottles, stored under 40 ° C abuse conditions, and the appearance, suspension stability and suspension were observed. The results are shown in Table 3.
[0040]
[Table 3]

[0041]
Method for judging suspension stability
[Expression 2]

Judgment method of suspension
Tap water is put into a 100 ml suspension tube, the preparation is diluted to a 500-fold equivalent amount, mixed by inversion 30 times per minute, left standing, foaming after 30 minutes, the amount of sediment, the degree of aggregation, after 60 minutes The amount of precipitation and the degree of aggregation were observed.
Criteria for determining the degree of aggregation during suspension observation
-; Well dispersed
±: Some aggregation is observed
+: Aggregation observed
++: Vigorous aggregation is observed
As mentioned above, as a result of comparing the preservability of the preparations according to the difference in oil used in the oil-based flowable, each oil-based flowable preparation using the medium chain fatty acid glycerides of Examples 1 to 4 Even when stored, the appearance and suspension were not affected, and the suspension stability tended to deteriorate as the storage period progressed, but there was no practical problem. However, Comparative Examples 1 to 4 turned yellow with the passage of the storage period (30 days after storage), and the fatty acid odor became stronger. In addition, the suspension property did not affect the amount of precipitation, but no foaming occurred, and an oily substance floated on the surface of the diluted solution.
[0042]
Test Example-3
The preparations of Examples 1 to 4 and Comparative Examples 5 to 8 stored for 3 months under 40 ° C. abuse conditions were diluted to a predetermined concentration, and Comparative Examples 9 to 12 were diluted to a predetermined concentration as a control, and cabbage (Spring variety 3-4 leaf stage) was sprayed with a sprayer, one day after spraying, cabbage leaves were collected, put in a plastic cup, 5 4th instar larvae were released, and stored in a dark room at 25 ° C. The survey was to observe the life and death status and the degree of food damage after 1 day of insect release. The results are shown in Table 4. The test was repeated 3 times.
[0043]
[Table 4]

[0044]
Degree of damage to cabbage leaves of konaga
-: No damage
±: Less than 5% of cabbage leaf area
+; 5% to 10% of cabbage leaf area caused by food damage
++; 10% to 25% of cabbage leaf area caused by food damage
++++ 25% to 50% of cabbage leaf area
+++++: More than 50% of cabbage leaf area affected by food damage
As described above, as a result of examining the effect on the insecticidal activity against the diamondback moth when each formulation was stored for a long time, each formulation of the oil-based flowables of Examples-1 to 4 was stored under abuse conditions at 40 ° C. for 90 days. There was no decline in insecticidal activity against the long-tailed moth. On the other hand, each of the aqueous flowable preparations of Comparative Examples-5 to 8 shows a significant decrease in insecticidal activity against the diamondback moth when stored under abused conditions. Preservation was considered impossible.
Moreover, when the insecticidal activity with respect to the diamondback moth of Comparative Examples-9 to 12 and Examples -1 to 4 of the existing drug is compared, both the unstored products of Examples -1 to 4 and the 90-day stored products are Comparative Examples -9 to 12 However, the insecticidal activity (rapid effect) against the diamondback moth tends to be improved.
[0045]
Test Example-4
The preparations of Examples-1 to 4 and Comparative Examples-5 to 12 are diluted to a predetermined concentration and sprayed on the planted cabbage (7-8 leaf stage), 1 day, 6 days and 10 days after spraying Cabbage leaves were collected, placed in a plastic cup, and 5 4th instar larvae were released and stored in a dark room at 25 ° C. The survey was to observe the life and death status and the degree of food damage after 1 day of insect release. The results are shown in Table 5, Table 6, and Table 7. The test was repeated 3 times.
[0046]
[Table 5]

[0047]
[Table 6]

[0048]
[Table 7]

[0049]
Degree of damage to cabbage leaves of konaga
-: No damage
±: Less than 5% of cabbage leaf area
+; 5% to 10% of cabbage leaf area caused by food damage
++; 10% to 25% of cabbage leaf area caused by food damage
++++ 25% to 50% of cabbage leaf area
+++++: More than 50% of cabbage leaf area affected by food damage
As described above, as a result of examining the residual effect of the insecticidal activity against the moths of each preparation in the field under natural conditions, in the comparative examples-9 to 12 of the existing drugs, a decrease in the insecticidal activity against the moths was observed 6 days after spraying. It was. This was the result that the existing drug had rain resistance and residual effect as expected. On the other hand, each of the oil-based flowable preparations of Examples 1 to 4 showed a slight decrease in the insecticidal activity against the diamondback moth even after the number of days after spraying, and the residual effect was improved compared to the existing drugs. It was recognized that
In addition, each of the aqueous flowable preparations of Comparative Examples-5 to 8 showed a significant decrease in the insecticidal activity against the diamondback moth 6 days after spraying, as in the case of the existing drugs, and no improvement in the residual effect was observed.
[0050]
Test Example-5
The preparations of Example-3 and Comparative Examples-7 and -11 were diluted to a predetermined concentration, and sprayed on the planted cabbage (7-8 leaf stages of varieties) on the field, 1 day, 6 days and 10 days after spraying The leaves were collected, placed in a plastic cup, 10 third-instar larvae were released, and stored in a dark room at 25 ° C. In the investigation, the life-and-death situation and the degree of feeding damage were observed after 2 days and 4 days after insect release. The results are shown in Table 8, Table 9, and Table 10. The test was repeated 3 times.
[0051]
[Table 8]

[0052]
[Table 9]

[0053]
[Table 10]

[0054]
Degree of damage to cabbage leaves of Spodoptera litura
-: No damage
±: Less than 5% of cabbage leaf area
+; 5% to 10% of cabbage leaf area caused by food damage
++; 10% to 25% of cabbage leaf area caused by food damage
++++ 25% to 50% of cabbage leaf area
+++++: More than 50% of cabbage leaf area affected by food damage
As mentioned above, as a result of examining the residual effect of the insecticidal activity against Spodoptera litura in each preparation in the field under natural conditions, the oil-based flowable preparation of Example-3 is similar to the insecticidal activity (residual effect) against the diamondback moth. Even after a few days after spraying, the decrease in insecticidal activity against Spodoptera litura was slight, and it was confirmed that the residual efficacy was improved compared to existing drugs.
In addition, each of the aqueous flowable preparations of Comparative Example-7, like Comparative Example-11 of the existing drug, greatly reduced the insecticidal activity against Spodoptera litura 6 days after spraying, and no improvement in residual efficacy was observed.

Claims

A mixture of caprylic acid triglyceride and capric acid triglyceride, Bacillus thuringiensis agricultural or horticultural insecticide composition characterized by containing a production toxin bacteria.

The agricultural and horticultural insecticide composition according to claim 1, wherein the mixture is a mixture of 75% caprylic acid triglyceride and 25% capric acid triglyceride .

50 to 90 parts by weight of the mixture ,
0.1 to 40 parts by weight of the produced toxin , and
The insecticide composition for agricultural and horticultural use according to claim 1 or 2, wherein the composition is an oil-based flowable preparation containing 1 to 9.9 parts by mass of a surfactant .

The surfactant claims, characterized in that the anionic surface active agent, cationic surface active agents, one or more surfactants selected from the group consisting of nonionic surfactants and amphoteric surfactants Item 4. The agricultural and horticultural insecticide composition according to Item 3 .