CN115251064B - 一种杀菌杀虫组合物及其应用 - Google Patents
一种杀菌杀虫组合物及其应用 Download PDFInfo
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- CN115251064B CN115251064B CN202110474958.4A CN202110474958A CN115251064B CN 115251064 B CN115251064 B CN 115251064B CN 202110474958 A CN202110474958 A CN 202110474958A CN 115251064 B CN115251064 B CN 115251064B
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Classifications
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
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- A—HUMAN NECESSITIES
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- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
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- A—HUMAN NECESSITIES
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- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
- A01N37/24—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides containing at least one oxygen or sulfur atom being directly attached to the same aromatic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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- A—HUMAN NECESSITIES
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- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/50—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids the nitrogen atom being doubly bound to the carbon skeleton
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
- A01N43/42—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
本发明属于农药复配的技术领域,公开了一种杀菌杀虫组合物及其应用。所述组合物包括有效活性成分,所述有效活性成分包括化合物I和化合物II,所述化合物I为7‑氯‑1‑环丙基‑6‑氟‑4‑氧代‑1,4‑二氢喹啉‑3‑羧酸‑2‑甲氧基乙酯,所述化合物II为杀菌剂或杀虫剂。本发明的增效组合物,具有以下优点:1)具有协同增效作用,可提高防治效果;2)扩大杀菌谱,田间病害多混合发生,对细菌病害作用更强;3)两种有效成分作用机理不同,混配使用可延缓病原菌抗药性的产生;4)降低施药量,减少使用次数,降低使用成本。
Description
技术领域
本发明属于农药复配的技术领域,特别是涉及一种含喹诺酮类化合物的增效组合物及其应用。
背景技术
近年来,各种作物细菌性病害的发生呈现逐年加重的趋势,发生面积逐年增长,给农业生产带来巨大危害,例如粮食作物中的水稻细菌性条斑病、水稻白叶枯病、水稻细菌性褐条病,果树中的猕猴桃溃疡病、柑橘溃疡病、桃细菌性穿孔病,茄科蔬菜青枯病,马铃薯黑胫病、环腐病,黄瓜细菌性角斑病,烟草野火病,十字花科蔬菜软腐病等细菌性病害都给作物造成了严重的损失。
目前市场上欠缺用于防治细菌性病害的高效药剂,农民为了提高防治效果加大用药量或者随意混配药剂,这种不科学用药,不仅达不到增效作用,反而导致农药的浪费、残留超标、污染环境、导致病菌对农药产生抗性等问题。因此,亟需研制一种针对细菌病害的增效组合物,能达到扩大防治对象范围、降低用药量、延缓抗性产生的效果。
在农业生产的实际过程中,长期连续单一的使用同一种药剂,病原菌很快就会产生抗药性,导致防效降低,农药使用量增加,加剧农产品农药残留和生态环境的破坏。通过与作用机理完全不同的杀菌剂品种进行复配,是延缓病原菌产生抗药性、扩大杀菌谱、延长使用寿命、降低农药使用量的有效途径。但如何进行复配,使得各药物之间产生协同而非拮抗作用是一大难点。
喹诺酮类化合物的化学名称为:7-氯-1-环丙基-6-氟-4-氧代-1,4-二氢喹啉-3-羧酸-2-甲氧基乙酯,其具有广谱的杀菌活性,尤其对细菌活性更高,对革兰氏阳性菌、革兰氏阴性菌均表现出优异的活性。对多种作物细菌性病害例如水稻细菌性条斑病、水稻白叶枯病、水稻细菌性褐条病、猕猴桃溃疡病、柑橘溃疡病、桃细菌性穿孔病、茄科蔬菜青枯病、马铃薯黑胫病、环腐病,黄瓜细菌性角斑病、烟草野火病和十字花科蔬菜软腐病等均具有优异活性。
发明内容
为了改善现有技术的不足,本发明的目的在于提供一种含有喹诺酮类化合物的增效组合物及其应用,所述组合物包括有效活性成分,所述有效活性成分包括化合物I和化合物II,其中,所述化合物I为7-氯-1-环丙基-6-氟-4-氧代-1,4-二氢喹啉-3-羧酸-2-甲氧基乙酯,所述化合物II为杀菌剂类(氯溴异氰尿酸、辛菌胺醋酸盐、三氯异氰尿酸、铜制剂、多粘类芽孢杆菌、枯草芽孢杆菌、菌毒清、苯霜灵、恶霜灵、嘧酚磺酸酯、聚二甲基硅氧烷醇、辛菌胺、乙基咪唑、辛噻酮、恶喹酸、麦穗灵、噻菌灵、甲基托布津、噻唑菌胺、氟吡菌胺、氰烯菌酯、二氟林、唑虫酰胺、异佛尔胺、苯并烯氟菌唑、呋吡菌胺、氟唑菌苯胺、氟唑环菌胺、唑菌酯、唑胺菌酯、氯啶菌酯、甲霜灵、肟醚菌胺、恶唑菌酮、吡菌苯威、吲哚磺菌胺、芬太芬醋酸盐、氯化芬汀、喹氧灵、丙氧喹啉、异菌脲、乙烯利、菌核净、克瘟散、啶菌磷、氯甲氧苯、二甲苯基丙烯酯、胺丙威、微生物、植物提取物、十三吗啉、丁苯吗啉、十二环吗琳、4-十二烷基-2,6-二甲基吗啉、苯锈啶、哌丙灵、螺环菌胺、环酰菌胺、胺苯吡菌酮、萘替芳、特比萘芳、吡吗啉、赛菌胺酯、缬霉威、缬菌胺、咯喹酮、苯并噻二唑、海带多糖、三乙膦酸铝、亚磷酸和盐、叶枯酞、咪唑嗪、哒菌清、磺菌威、环氟菌胺、多果定、嘧菌腙、flutianil、tebufloquin、picarbutrazox、抑菌灵、对甲抑菌灵、双辛胍胺、双胍辛胺、二氰蒽醌、啶菌噁唑、毒氟磷、氟唑活化酯、丁吡吗啉、环己磺菌胺、甲噻诱胺、苯噻菌酯、苯丙烯菌酮、酚菌酮、氯苯醚酰胺、氟苯醚酰胺、唑醚磺胺酯、苯噻菌胺、四唑吡氨酯、烯丙苯噻唑、isofetamid、pyraziflumid、Inpyrfluxam、Pyrapropoyne、Pyribencarb、Mandestrobin、Metyltetraprole、Fenpicoxamid、Florylpicoxamid、Flutianil、Tebufloquin、Pyriofenone、Tolprocarb、Quinofumelin、Dichlobentiazox、Aminopyrifen、Dipymetitrone、Buoxapiprolin、苯氧喹啉、螺嘧环胺、Bixafen、氟啶菌酰胺、咪唑菌酮)和杀虫剂中的至少一种。所述化合物I和所述化合物II的混合使用可以形成增效组合物,有效活性成分包括化合物I和化合物II,二者的混合使用具有明显的增效互补作用,利用病菌作用位点的不同,作用机理的不同,复配可对病原菌多位点作用,扩大杀菌谱、提高防效、降低农药使用量、延缓抗药性的产生,还可以降低成本。
本发明采取以下方案:
一种杀虫杀菌组合物,该组合物包括有效活性成分,所述有效活性成分包括化合物I和化合物II,所述化合物I为7-氯-1-环丙基-6-氟-4-氧代-1,4-二氢喹啉-3-羧酸-2-甲氧基乙酯,所述化合物II选自以下杀菌剂或杀虫剂;杀菌剂选自酰基丙氨酸类、恶唑烷酮类、丁内酯类、羟基嘧啶类、异恶唑类、异噻唑啉酮类、羧酸类、苯并咪唑类、托布津类、N-苯基氨基甲酸酯类、甲苯酰胺类、乙基氨基-噻唑-甲酰胺类、苯基脲类、吡啶基甲基-苯甲酰胺、氨基氰基丙烯酸酯、嘧啶胺类、吡唑-5-甲酰胺类、苯基-苯甲酰胺、苯基-氧代-乙基噻吩酰胺类、吡啶基-乙基-苯甲酰胺类、呋喃甲酰胺类、氧硫辛酸-甲酰胺类、噻唑甲酰胺类、吡唑-4-甲酰胺类、N-甲氧基-(苯基-乙基)-吡唑-甲酰胺类、吡啶甲酰胺类、吡嗪-甲酰胺类、甲氧基丙烯酸酯类、甲氧基乙酰胺类、甲氧基氨基甲酸酯类、肟基乙酸酯类、肟基乙酰胺类、恶唑烷二噁英类、二氰二恶嗪类、咪唑啉酮类、苄基-氨基甲酸酯类、氰基吡唑类、氨磺酰基-***类、巴豆酸二硝基苯酯类、2,6-二硝基苯胺、哒嗪酮、三苯基锡化合物、噻吩-甲酰胺类、***并嘧啶胺类、苯胺基嘧啶类、芳氧基喹啉类、喹唑啉酮类、苯基吡咯类、二甲酰亚胺类、磷硫醇盐类、二硫戊环类、芳烃类、1,2,4-噻二唑类、氨基甲酸酯类、微生物类、香菇多糖等植物提取物、哌啶基-噻唑-异恶唑啉类、***类、***硫酮类、吗啉类、哌啶类、螺缩酮胺类、羟基苯胺类、氨基吡唑啉酮类、硫代氨基甲酸盐类、烯丙胺类、肽基嘧啶核苷类、肉桂酸酰胺类、缬氨酰胺氨基甲酸酯类、扁桃酸酰胺类、异苯并呋喃酮类、吡咯并喹啉酮类、***并苯并噻唑类、环丙烷甲酰胺类、甲酰胺类、丙酰胺类、三氟乙基-氨基甲酸酯类、苯并噻二唑类、苯并异噻唑类、噻二唑-甲酰胺类、多糖类、氰乙酰胺类、乙基膦酸酯类、邻苯二甲酰酪氨酸类、苯并三嗪类、苯磺酰胺类、哒嗪酮类、硫代氨基甲酸盐类、苯基乙酰胺类、二苯甲酮类、苯甲酰基吡啶类、胍类、氰基亚甲基-噻唑烷类、嘧啶酮腙类、4-喹啉基乙酸酯类、四唑基肟类、二硫代氨基甲酸盐和类似物、邻苯二甲酰亚胺类、氯腈类、磺酰胺类、双胍类、三嗪类、醌类、喹喔啉类、马来酰亚胺类、多肽类、木霉属和产生的杀真菌代谢物,主要包括以下主要成分:氯溴异氰尿酸、辛菌胺醋酸盐、三氯异氰尿酸、铜制剂、多粘类芽孢杆菌、枯草芽孢杆菌、嘧酚磺酸酯、聚二甲基硅氧烷醇、菌毒清(辛菌胺)、噻唑菌胺、氟吡菌胺、氰烯菌酯、二氟林、唑虫酰胺、苯并烯氟菌唑、呋吡菌胺、氟唑菌苯胺、氟唑环菌胺、唑菌酯、唑胺菌酯、氯啶菌酯、甲霜灵、肟醚菌胺、恶唑菌酮、吡菌苯威、吲哚磺菌胺、芬太芬醋酸盐、氯化芬汀、喹氧灵、丙氧喹啉、异菌脲、乙烯利、菌核净、克瘟散、啶菌磷、氯甲氧苯、二甲苯基丙烯酯、胺丙威、钙制剂、盐酸吗啉胍、葡聚烯糖、几丁聚糖、苦参碱、硫磺、十三吗啉、丁苯吗啉、十二环吗琳、4-十二烷基-2,6-二甲基吗啉、苯锈啶、哌丙灵、螺环菌胺、环酰菌胺、胺苯吡菌酮、萘替芳、特比萘芳、吡吗啉、赛菌胺酯、缬霉威、缬菌胺、咯喹酮、苯并噻二唑、烯腺嘌呤、三十烷醇、海带多糖、三乙膦酸铝、亚磷酸和盐、叶枯酞、咪唑嗪、哒菌清、磺菌威、环氟菌胺、多果定、嘧菌腙、flutianil、tebufloquin、picarbutrazox、抑菌灵、对甲抑菌灵、双辛胍胺、双胍辛胺、二氰蒽醌、啶菌噁唑、毒氟磷、氟唑活化酯、丁吡吗啉、环己磺菌胺、甲噻诱胺、苯噻菌酯、苯丙烯菌酮、酚菌酮、氯苯醚酰胺、氟苯醚酰胺、唑醚磺胺酯、苯噻菌胺、嘧螨胺、四唑吡氨酯、烯丙苯噻唑、Isofetamid、Pyraziflumid、Inpyrfluxam、Pyrapropoyne、Pyribencarb、Mandestrobin、Metyltetraprole、Fenpicoxamid、Florylpicoxamid、Flutianil、Tebuboquin、Pyriofenone、Tolprocarb、Quinofumelin、Dichlobentiazox、Aminopyrifen、Dipymetitrone、Buoxapiprolin、苯氧喹啉、螺嘧环胺、Bixafen、氟啶菌酰胺和咪唑菌酮中的至少一种;
杀虫剂选自Ⅱ-M.1烟碱乙酰胆碱受体激动剂:
Ⅱ-M.1A新烟碱类:氯噻啉、可尼丁、吡虫清、硝胺烯啶、环氧虫啶、氟吡呋喃酮;或:
Ⅱ-M.1A.1:1-[(6-氯-3-吡啶基)甲基]-2,3,5,6,7,8-六氢-9-硝基-(5S,8R)-5,8-环氧基-1H-咪唑并[1,2-a]氮杂或
Ⅱ-M.1A.2:(2E-)-1-[(6-氯吡啶-3-基)甲基]-N’-硝基-2-亚戊基氨基胍;或
Ⅱ-M.1A.3:1-[(6-氯吡啶-3-基)甲基]-7-甲基-8-硝基-5-丙氧基-1,2,3,5,6,7-六氢咪唑并[1,2-a]吡啶;或
Ⅱ-M.1B或
Ⅱ-M.1C烟碱;或
Ⅱ-M.1D三氟苯嘧啶、二氯噻吡嘧啶;
Ⅱ-M.2烟碱乙酰胆碱受体变构活化剂:多杀菌素类;
Ⅱ-M.3钠通道调节剂:
Ⅱ-M.3A拟除虫菊酯类:右旋反式氯丙炔菊酯、高效氯氰菊酯、氟丙菊酯、丙烯除虫菊、右旋丙烯菊酯、右旋反式丙烯菊酯、氟氯菊酯、生物烯丙菊酯、2-环戊烯基生物烯丙菊酯、生物苄呋菊酯、高效氟氯氰菊酯、(RS)氯氟氰菊酯、氯氟氰菊酯、精高效氯氟氰菊酯、甲体氯氰菊酯、乙体氯氰菊酯、高效反式氯氰菊酯、苯醚氰菊酯、烯炔菊酯、高氰戊菊酯、杀灭菊酯、氟氯苯菊酯、右旋七氟甲醚菊酯、咪炔菊酯、氯氟醚菊酯、momfluorothrin、苯醚菊酯、炔酮菊酯、除虫菊酯(除虫菊)、灭虫菊、灭虫硅醚、胺菊酯、乙氰菊酯、苄螨醚、右旋炔丙菊酯、氟硅菊酯、右旋胺菊酯、四氟菊酯;或
Ⅱ-M.3B钠通道调节剂:滴滴涕和甲氧滴滴涕;或
Ⅱ-M.3C藜芦碱;
Ⅱ-M.4双酰胺类的鱼尼汀受体调节剂:氟苯虫酰胺、氯氟氰虫酰胺、溴氰虫酰胺、四氯虫酰胺、环丙虫酰胺、四唑虫酰胺、环溴虫酰胺、氟氰虫酰胺、氟氧虫酰胺、噻虫酰胺、硫虫酰胺、氟苯醚酰胺、氟虫双酰胺,或邻苯二甲酰胺类化合物:
Ⅱ-M.4.1:(R)-3-氯-N1-{2-甲基-4-[1,2,2,2-四氟-1-(三氟甲基)乙基]苯基}-N2-(1-甲基-2-甲基磺酰基乙基)邻苯二甲酰胺;和
Ⅱ-M.4.2:(S)-3-氯-N1-{2-甲基-4-[1,2,2,2-四氟-1-(三氟甲基)乙基]苯基}-N2-(1-甲基-2-甲基磺酰基乙基)邻苯二甲酰胺;或化合物
Ⅱ-M.4.3:2-[3,5-二溴-2-({[3-溴-1-(3-氯吡啶-2-基)-1H-吡唑-5-基])基}氨基)苯甲酰基]-1,2-二甲基肼羧酸甲酯;或选自M.4.5a)至M.4.5l)的化合物
Ⅱ-M.4.4a)N-[4,6-二氯-2-[(二乙基-λ-4-亚硫烷基(sulfanylidene))氨基甲酰基]苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4b)N-[4-氯-2-[(二乙基-λ-4-亚硫烷基)氨基甲酰基]-6-甲基苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4c)N-[4-氯-2-[(二-2-丙基-λ-4-亚硫烷基)氨基甲绊基]-6-甲基苯基]-2-(3-氛-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4d)N-[4,6-二氯-2-[(二-2-丙基-λ-4-亚硫烷基)氨基甲酰基]苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4e)N-[4,6-二氯-2-[(二乙基-λ-4-亚硫烷基)氨基甲酰基]-苯基]-2-(3-氯-2-吡啶基)-5-二氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4f)N-[4,6-二溴-2-[(二-2-丙基-λ-4-亚硫烷基)氨基甲酰基]-苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4g)N-[4-氯-2-[(二-2-丙基-λ-4-亚硫烷基)氨基甲酰基]-6-氰基苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4h)N-[4,6-二溴-2-[(二乙基-λ-4-亚硫烷基)氨基甲酰基]-苯基]-2-(3-氯-2-吡啶基)-5-三氟甲基吡唑-3-甲酰胺;
Ⅱ-M.4.4i)N-[2-(5-氨基-1,3,4-噻二唑-2-基)-4-氯-6-甲基苯基]-3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-甲酰胺;
Ⅱ-M.4.4j)3-氯-1-(3-氯-2-吡啶基)-N-[2,4-二氯-6-[[(1-氰基-1-甲基乙基)氨基]羧基]苯基]-1H-吡唑-5-甲酰胺;
Ⅱ-M.4.4k)3-溴-N-[2,4-二氯-6-(甲基氨基甲酰基)苯基]-1-(3,5-二氯-2-吡啶基)-1H-吡唑-5-甲酰胺;
Ⅱ-M.4.41)N-[4-氯-2-[[(1,1-二甲基乙基)氨基]羧基]]-6-甲基苯基]-1-(3-氯-2-吡啶基)-3-(氟甲氧基)-1H-吡唑-5-甲酰胺;
或选自如下的化合物:
Ⅱ-M.4.5:N-(2-氰基丙-2-基)-N-(2,4-二甲基苯基)-3-碘苯-1,2-二甲酰胺;或
Ⅱ-M.4.6:3-氯-N-(2-氰基丙-2-基)-N-(2,4-二甲基苯基)-苯-1,2-二甲酰胺;
Ⅱ-M.4.7a)1-(3-氯-2-吡啶基)-N-[4-氰基-2-甲基-6-[(甲基氨基)羧基]苯基]-3-[[5-(三氟甲基)-2H-四唑-2-基]甲基]-1H-吡唑-5-甲酰胺;或者
Ⅱ-M.4.7b)1-(3-氯-2-吡啶基)-N-[4-氰基-2-甲基-6-[(甲基氨基))基]苯基]-3-[[5-(三氟甲基)-1H-四唑-1-基]甲基]-1H-吡唑-5-甲酰胺;
Ⅱ-M.5GABA门控氯离子通道拮抗剂:
Ⅱ-M.5A有机氯化合物:毒杀芬、狄氏剂、七氯、灭蚁灵、艾氏剂、氯丹;或
Ⅱ-M.5B苯基吡唑类:乙虫腈、丁虫腈、吡嗪氟虫腈、吡啶氟虫腈、乙酰虫腈、丁烯氟虫腈、pyrafluprole和pyriprole;
Ⅱ-M.5C异噁唑类:氟噁唑酰胺、氟雷拉纳、阿福拉纳、沙罗拉纳、洛替拉纳、异噁唑虫酰胺;
Ⅱ-M.5D:间双酰胺类:溴虫氟苯双酰胺、环丙氟虫胺
Ⅱ-M.6选择性同翅目昆虫进食阻断剂:拒嗪酮、pyrifluquinazon;
Ⅱ-M.7乙酰胆碱酯酶抑制剂
Ⅱ-M.7A氨基甲酸酯类:甲萘威、虫螨威、灭虫威、灭多虫、甲氨叉威、灭害威、噁虫威、丁叉威、氧丁叉威、虫螨威、丁酮砜威、西维因、乙硫甲威、速灭威、敌克威、混灭威、唑蚜威、灭除威、苯虫威、丁苯威、特氨叉威、混杀威、二甲威;或
Ⅱ-M.7B有机磷酸酯类:硝虫硫磷、氯唑磷、高灭磷、乙基谷硫磷、辛硫磷、谷硫磷、苯硫磷、灭克磷、氨磺磷、毒虫畏、甲基毒死蜱、庚虫磷、imicyafos、甲基内吸磷、二嗪农、二溴磷、百治磷、甲基乙拌磷、克线磷、倍硫磷、异噁唑磷、灭蚜磷、速灭磷、砜吸磷、一六零五、甲基一六零五、稻丰散、伏杀磷、磷胺、虫螨磷、烯虫磷、丙硫磷、甲基吡噁磷、益棉磷、保棉磷、吡唑硫磷、喹恶磷、打杀磷、硫特普、硫甲双磷、嘧丙磷、氯氧磷、氯甲硫磷、蝇毒磷、杀螟腈、杀螟松、特丁硫磷、沙虫畏、香芹油、香茅油、丙胺磷、0-(甲氧基氨硫代磷酰基)水杨酸异丙酯、敌百虫、唑啶磷、壤虫氯磷、氯甲磷、甲基毒虫畏、噻唑酮磷、蚜灭多;
Ⅱ-M.8氯离子通道激动剂:米尔贝霉素:伊维菌素、齐墩螨素、雷皮菌素和米尔螨素;
Ⅱ-M.9保幼激素模拟物:蒙五一二、蒙七七七、烯虫炔酯、蒙五一五、双氧威、蚊蝇醚、烯虫乙酯、烯虫酯;
Ⅱ-M.10螨生长抑制剂:噻螨酮、特苯噁唑、氟螨嗪;
Ⅱ-M.11线粒体ATP合成酶抑制剂:杀螨硫隆、杀螨锡、唑环锡、三环锡、克螨特、三氯杀螨砜、***锡、苯丁锡、丁醚脲、二环己基碳二亚胺、4,6-二硝基邻甲酚(DNOC);
Ⅱ-M.12经由质子梯度干扰的氧化磷酸化去偶剂:氟唑虫清、二硝甲酚、氟虫胺;
Ⅱ-M.13烟碱乙酰胆碱受体通道阻断剂:巴丹、硫环杀;
Ⅱ-M.14苯甲酰脲类的几丁质生物合成类型0抑制剂,包含双三氟虫脲、氟脲杀、氟螨脲、氟丙氧脲、双苯氟脲、多氟脲、氟环脲;
Ⅱ-M.15几丁质生物合成类型1抑制剂:噻嗪酮;
Ⅱ-M.16蜕皮干扰剂:KK-42;
Ⅱ-M.17蜕皮激素受体激动剂:甲氧苯酰肼、双苯酰肼、特丁苯酰肼、呋喃虫酰肼、环虫酰肼、环氧酰肼、虫酰肼、印楝素;
Ⅱ-M.18章鱼胺受体激动剂:双甲脒(虫螨脒);
Ⅱ-M.19线粒体配合物电子传输抑制剂:
Ⅱ-M.19.A线粒体配合物I电子传输抑制剂类:喹螨醚、嘧胺苯醚、哒螨酮、吡螨胺、嘧螨醚、唑虫酰胺、嘧虫胺、鱼藤酮;
Ⅱ-M.19.B线粒体配合物III电子传输抑制剂类:flometoquin、灭蚁腙、灭螨醌、嘧螨酯、抗霉素;
Ⅱ-M.20电压依赖性钠通道阻断剂:噁二唑虫、氰氟虫胺、2-[2-(4-氰基苯基)-1-[3-(三氟甲基)苯基]亚乙基]-N-[4-(二氟甲氧基)苯基]氨基脲、N-(3-氯-2-甲基苯基)-2-[(4-氯苯基)[4-[甲基(甲基磺酰基)氨基]苯基]亚甲基]氨基脲;
Ⅱ-M.21乙酰CoA羧化酶抑制剂:包括特窗酸和特拉姆酸衍生物,包括螺甲螨酯、甲氧哌啶乙酯;
Ⅱ-M.22线粒体复合体IV电子传输抑制剂:
Ⅱ-M.22.A含磷化合物:磷化铝、磷化氢、磷化钙、膦和磷化锌;
Ⅱ-M.22.B氰化物;
Ⅱ-M.23β-酮腈衍生物类别的线粒体复合体II电子传输抑制剂;
Ⅱ-M.24混杂非特异性(多位点)抑制剂:
Ⅱ-M.24.A烷基卤:甲基溴、其他烷基卤;
Ⅱ-M.24.B氯化苦、硫酰氟、硼砂、吐酒石;
Ⅱ-M.24.C释放异硫氰酸甲酯:棉隆、威百亩;
Ⅱ-M.25生物胺受体竞争剂类化合物:双甲脲、苯甲醛腙、苯甲醛半卡巴腙;
Ⅱ-M.26神经细胞抑制剂:联苯肼酯;
Ⅱ-M.27顺乌头酸抑制剂:氟乙酸;
Ⅱ-M.28昆虫中肠膜微生物紊乱剂:枯草芽孢杆菌、球形芽孢杆菌及其产生的杀虫蛋白,如苏云金杆菌Israelensis亚种、苏云金杆菌Aizawai亚种、苏云金杆菌Kurstaki亚种、苏云金杆菌Tenebrionis亚种,或Bt作物蛋白:Cry1Ab、Cry1Ac、Cry1Fa、Cry2Ab、mCry3A、Cry3Ab、Cry3Bb和Cry34/35Ab1;
Ⅱ-M.29未知或不确定作用模式的杀虫活性化合物:氟烯酰砜、磺胺螨酯、苯螨特、溴螨酯、喹菌酮、冰晶石、苦参碱、藜芦碱、松螨鲨、橄榄鲨、螺螨双酯、嘧虫胺、氟噻虫砜、fluhexafon、氟吡菌酰胺、噁虫酮、硫酰氟、氟螨嗪、灭螨猛、啶虫丙醚、代森锰锌、pyflubumide和pyrifluquinazon。
根据本发明的实施方案,所述化合物I和化合物II的质量比为80~1:1~80。
根据本发明的实施方案,所述化合物I和化合物II的质量比为50~1:1~50。
根据本发明的实施方案,所述化合物I和化合物II的质量比为30~1:1~30。
根据本发明的实施方案,所述化合物I和化合物II的质量比为80:1、75:1、70:1、65:1、60:1、55:1、50:1、45:1、40:1、35:1、30:1、25:1、20:1、15:1、10:1、5:1、1:1、1:5、1:10、15:1、1:20、25:1、1:30、35:1、1:40、45:1、1:50、55:1、1:60、65:1、1:70、75:1、1:80。
根据本发明的实施方案,以所述组合物的总重量为100%计,所述化合物I与化合物II在组合物中的质量之和为1~80%,优选为20~60%,例如1%、5%、8%、10%、13%、15%、18%、20%、24%、30%、35%、38%、42%、45%、50%、55%、60%、65%、68%、75%、80%、85%、90%。
根据本发明的实施方案,所述组合物可制备成液体制剂或固体制剂。
根据本发明的实施方案,根据不同的制剂类型,制剂中有效活性成分含量范围有所不同,通常,液体制剂中含有按重量计1%~60%的有效活性成分,优选为5%~50%;固体制剂中含有按重量计5%~80%的有效活性成分,优选为10%~70%。
根据本发明的实施方案,所述组合物中还包括去离子水、有机溶剂、乳化剂、分散剂、润湿剂、增稠剂、消泡剂、稳定剂、粘结剂、崩解剂、抗冻剂、抗结剂、助悬剂、成膜剂、防腐剂、着色剂、高分子囊壁材料、pH调节剂或填料等。
根据本发明的实施方案,所述组合物可以由使用者在使用前经稀释或直接使用。其配制可由本领域技术人员所公知的加工方法制备,即将有效活性成分与去离子水、有机溶剂、乳化剂、分散剂、润湿剂、增稠剂、消泡剂、稳定剂、粘结剂、崩解剂、抗冻剂、抗结剂、助悬剂、成膜剂、防腐剂、着色剂、高分子囊壁材料、pH调节剂或填料等中的一种或几种混合,制备得到所述组合物。
根据本发明提供的制剂,所述组合物可以制作成各种剂型,优选地,所述剂型包括水分散粒剂、可分散液剂、可湿性粉剂、悬浮剂、水乳剂、微乳剂、悬乳剂、微囊悬浮剂、微囊悬浮-悬浮剂、悬浮种衣剂、乳油或颗粒剂。
根据本发明的实施方案,所述组合物制成可湿性粉剂时包含如下组分及含量:化合物I 1%~80%,化合物II 1%~80%,分散剂1%~12%,润湿剂1%~8%,余量为填料。
根据本发明的实施方案,所述组合物制成水分散粒剂时包括如下组分及含量:化合物I 1%~80%,化合物II 1%~80%,分散剂1%~12%,润湿剂1%~8%,崩解剂1%~10%,余量为填料。
根据本发明的实施方案,所述组合物制成悬浮剂时包括如下组分及含量:化合物I1%~50%,化合物II 1%~50%,分散剂1%~12%,润湿剂1%~10%,增稠剂0.1%~8%,抗冻剂0.1%~8%,余量为去离子水。
根据本发明的实施方案,所述组合物制成水乳剂时包括如下组分及含量:化合物I1%~50%,化合物II 1%~50%,有机溶剂1%~60%,乳化剂1%~12%,抗冻剂0.1%~8%,消泡剂0.01%~2%,增稠剂0.1%~2%,余量为去离子水。
根据本发明的实施方案,所述组合物制成悬浮种衣剂时包括如下组分及含量:化合物I 1%~50%,化合物II 1%~50%,分散剂1%~12%,润湿剂1%~10%,抗冻剂1-10%,抗结剂0.1-10%,助悬剂0.1-5%,成膜剂1-10%,防腐剂0.1-5%,着色剂1-30%,pH调节剂0.1%~5%,增稠剂0.1%~8%,余量为去离子水。
根据本发明的实施方案,所述组合物制成微囊悬浮剂时包括如下组分及含量:化合物I 1%~50%,化合物II 1%~50%,高分子囊壁材料1-30%,分散剂2%~10%,有机溶剂1-50%,乳化剂1%~7%,pH调节剂0.1%~5%,消泡剂0.01%~2%,增稠剂0.1%~8%,抗冻剂0.1%~8%,余量为去离子水。
根据本发明的实施方案,所述组合物制成微囊悬浮-悬浮剂时包括如下组分及含量:化合物I 1%~50%,化合物II 1%~50%,高分子囊壁材料1%~12%,分散剂1%~12%,润湿剂1%~8%,有机溶剂1-50%,乳化剂1%~8%,消泡剂0.01%~2%,增稠剂0.1%~8%,pH调节剂0.1%~5%,抗冻剂0.1%~8%,余量为去离子水。
根据本发明的实施方案,所述组合物制成乳油时包括如下组分及含量:化合物I1%~50%,化合物II 1%~50%,有机溶剂1-50%,乳化剂1-30%,抗冻剂1%~10%,稳定剂0.1%~5%,余量为有机溶剂。
根据本发明的实施方案,所述组合物制成微乳剂时包括如下组分及含量:化合物I1%~50%,化合物II 1%~50%,有机溶剂1-50%,乳化剂1-30%,抗冻剂1%~10%,稳定剂0.1%~5%,余量为去离子水。
根据本发明的实施方案,所述组合物制成可分散液剂时包括如下组分及含量:化合物I 1%~50%,化合物II 1%~50%,乳化剂1-30%,抗冻剂1%~10%,稳定剂0.1%~5%,余量为有机溶剂。
根据本发明的实施方案,所述组合物制成颗粒剂时包括如下组分及含量:化合物I0.5%~10%,化合物II 0.5%~10%,分散剂1%~12%,润湿剂1%~10%,粘结剂0.1%~8%,余量为填料。
根据本发明的实施方案,所述乳化剂可以选用如下中的一种:木质素磺酸钠、农乳、苯基酚聚氧乙基醚磷酸酯、三苯乙烯基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐、苄基二甲基酚聚氧乙基醚、失水山梨醇脂肪酸酯聚氧乙烯醚、山梨醇酐油酸酯(斯盘-80)、脂肪醇聚氧乙烯醚、烷基萘磺酸钠、异辛醇琥珀酸酯磺酸钠、壬基酚聚氧乙烯醚磷酸酯、蓖麻油聚氧乙烯醚磷酸酯中的一种或多种。
根据本发明的实施方案,所述分散剂可以选用:甘油脂肪酸聚氧乙烯醚、聚氧乙烯烷基芳基醚、木质素磺酸钠、萘磺酸盐甲醛缩合物、脂肪醇聚氧乙烯醚硫酸盐、萘磺酸盐甲醛缩合物、萘磺酸甲醛缩合物钠盐、壬基酚聚氧乙烯醚、聚氧乙烯羊毛脂醇、烷基酚聚氧乙烯醚甲醛缩合物、脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯醚磷酸酯、聚氧乙烯山梨聚糖脂肪酸酯、磷酸酯中的一种或多种。
根据本发明的实施方案,所述润湿剂可以选用:三硅氧烷聚氧乙烯醚,N-月桂酰基谷氨酸钠、十二烷基硫酸钠、月桂酰基肌氨酸钠、甲基萘磺酸钠甲醛缩合物、蓖麻油聚氧乙烯醚、三苯乙基苯酚聚氧乙烯醚、十二烷基苯磺酸钠、烷基萘磺酸钠、异辛醇琥珀酸酯磺酸钠、聚氧乙烯烷基芳基醚、脂肪醇聚醚甘油脂肪酸聚氧乙烯醚、脂肪醇聚氧乙烯醚中的一种或多种。
根据本发明的实施方案,所述粘结剂可以选用:黄原胶、淀粉、脲醛树脂、明胶、***胶、羧甲基纤维素、羧乙基纤维素、聚乙烯醇中的一种或多种。
根据本发明的实施方案,所述崩解剂可以选用:碳酸氢钠、硫酸铵、硫酸钠、硫酸钙、氯化镁中的一种或多种。
根据本发明的实施方案,所述增稠剂可以选用:硅酸镁铝、聚乙酸乙烯酯、黄原胶、明胶、***胶、聚乙烯醇中的一种或多种。
根据本发明的实施方案,所述消泡剂可以选用:硅油、正-辛醇、硅酮、磷酸丁酯、磷酸异丁酯等中的一种或多种。
根据本发明的实施方案,所述抗冻剂可以选用:丙二醇、乙二醇、丙三醇等中的一种或多种。
根据本发明的实施方案,所述稳定剂可以选用:三乙醇胺、环氧氯丙烷、丁基缩水甘油醚、亚磷酸三苯酯、N-大豆油基三亚甲基二胺、二烷基丁二酸醋磺酸盐等中的一种或多种。
根据本发明的实施方案,所述填料包括固体填料和液体填料,其中,所述固体填料可以选用:高岭土、凹凸棒土、硅藻土、白炭黑、膨润土、蒙脱石、碳酸钙、滑石粉中的一种或多种。所述液体填料可以选用大豆油、蓖麻油、矿物油中的一种或多种。
根据本发明的实施方案,所述有机溶剂可以选用:乙酸乙酯、丙酮、异丙醇、2,2,2-三氟乙醇、碳酸丙烯酯、苯、甲苯、二甲苯、二甲基甲酰胺、二甲基亚砜、二氯甲烷、环己烷、环己酮、N-甲基吡咯烷酮、溶剂油(如150#溶剂油)中的一种或多种。
本发明还提供上述组合物用于防治农业病害和虫害的用途。
本发明提供上述组合物在防治农业病害和虫害,尤其防治细菌及细菌引起的植物细菌性病害中的应用。
根据本发明的实施方案,所述组合物在防治瓜类细菌性角斑病、水稻白叶枯、水稻细菌性条斑病、柑橘溃疡病、芒果角斑病、烟草野火病、水稻细菌性褐条病、猕猴桃溃疡病、马铃薯黑胫病、环腐病、瓜类霜霉病、黄瓜靶斑病、黄瓜灰霉病、棉花立枯病、黄瓜白粉病、黄瓜炭疽病、瓜类黑星病、水稻稻瘟病、柑橘疮痂病等病害以及防治蓟马、蚜虫、红蜘蛛、棉铃虫、跳甲、菜青虫、介壳虫、粉虱、欧洲玉米螟、春尺蠖、柳春蛾、小菜蛾、绿盲蝽、稻纵卷叶螟、稻飞虱、豆荚螟、甜菜夜蛾、斜纹夜蛾、苹果蠹蛾与地下害虫蝼蛄、蛴螬、金针虫、地老虎、根蛆、根蝽、根蚜、拟地甲、蟋蟀、根蚧、根叶甲、根天牛、桃小食心虫、根象甲和白蚁中的应用。
根据本发明的实施方案,所述组合物在防治大白菜软腐病、黄瓜细菌性角斑病、西瓜果斑病、水稻白叶枯病、水稻细菌性条斑病、番茄青枯病、马铃薯黑胫病、芒果角斑病、柑橘溃疡病、桃树细菌性穿孔病和马铃薯疮痂病中的应用。
其中,上述组合物对细菌性病害方面效果卓越,对于黄瓜霜霉病、黄瓜靶斑病、水稻稻瘟病、水稻纹枯病等病害有一定防效。
本发明还提供一种防治病原菌及其引起的农业病害,尤其是细菌及细菌引起的植物细菌性病害的方法,该方法包括将上述组合物施用于存在病害的植物上。
本发明还提供一种防治农业病害和虫害的方法,包括将如上组合物施用于存在病害和虫害的植物上。
本发明的组合物可以以成品制剂形式提供,也可以以单剂形式提供,使用前直接混合,然后兑水混匀配成所需浓度,可以以任何方式施用于作物上,例如喷施、植株根部灌施、涂抹等。具体应用时,也可以与其它药剂如生长调节剂、土壤调节剂、除草剂、杀线虫剂等混合使用。
本发明的有益效果:
本发明提供的杀菌杀虫(增效)组合物,具有以下优点:
1)具有协同增效作用,可提高防治效果;2)扩大杀菌谱,田间病害多混合发生,对细菌病害作用更强;3)两种有效成分作用机理不同,混配使用可延缓病原菌抗药性的产生;4)降低施药量,减少使用次数,降低使用成本。
具体实施方式
下文将结合具体实施例对本发明做更进一步的详细说明。应当理解,下列实施例仅为示例性地说明和解释本发明,而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
下述实施例中所使用的实验方法如无特殊说明,均为常规方法;下述实施例中所用的试剂、材料等,如无特殊说明,均可从商业途径得到。
本发明采用室内生物测定和田间试验相结合的方法对所述组合物的杀菌效果进行性能测试。应当指出的是,凡在本发明的精神和原则之内所做的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
一、制剂制备例:
制备例1:可湿性粉剂
将上述材料按比例粗粉碎后进入混合器中混合均匀,再经气流粉碎后即制得成品。
制备例2:水分散粒剂
将有效活性成分及各种助剂等按配方的比例混合均匀,经气流粉碎后得到粉料,再加入一定量的水混合挤压造粒,经干燥筛分后得到成品。
制备例3:悬浮剂
将有效活性成分及各种助剂按配方的比例混合均匀,经高速剪切后并砂磨得到成品。
制备例4:乳油
将上述原料按比例混合,使其溶解为均匀油相;经检验合格后,进行计量分装即成品。
制备例5:水乳剂
按配方要求,将以上原料加入到配料釜中,经高速剪切机混合均匀制成水乳剂,经检验合格后,进行计量分装即成品。
制备例6:乳油
将上述原料按比例混合,使其溶解为均匀油相;经检验合格后,进行计量分装即成品。
制备例7:乳油
将上述原料按比例混合,使其溶解为均匀油相;经检验合格后,进行计量分装即成品。
制备例8:颗粒剂
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按配方比例将各组分充分混合,粉碎,加水润湿后再充分搅拌均匀,再用螺杆挤压造粒机造粒,干燥后过筛,即得成品。
二、室内毒力测定实施例
(1)供试病原菌:大白菜软腐病、黄瓜细菌性角斑病、西瓜果斑病、水稻白叶枯病、水稻细菌性条斑病、马铃薯晚疫病和辣椒炭疽病。
(2)测定方法:
细菌毒力测定方法
病原细菌毒力测定以大白菜软腐病、黄瓜细菌性角斑病、西瓜果斑病、水稻白叶枯病、水稻细菌性条斑病等细菌性病害为试验材料,采用离体浑浊度法对化合物I、化合物II及其混配制剂进行毒力测定。
参照中华人民共和国农业行业标准NY/T 1156.16-2008,先将供试药剂(包括化合物I、化合物II)用合适的溶剂(溶剂的种类如丙酮、甲醇、N,N二甲基甲酰胺和二甲基亚砜等,并且依据其对样品的溶解能力而选择)配制成7个浓度梯度(化合物I:0.5,1.0,2.0,4.0,8.0,16.0,32.0mg/L等7个浓度梯度;化合物II:0.5,1.0,2.0,4.0,8.0,16.0,32.0mg/L等7个浓度梯度),将供混配的化合物I、化合物II分别按其EC50值按质量比例设置一系列比例,按不同配比配制成最终质量浓度(指化合物I、化合物II的总质量)为0.5,1.0,2.0,4.0,8.0,16.0,32.0mg/L7个系列浓度。
在无菌操作条件下,将NB(营养肉汤,每升中含有10g蛋白胨、3g牛肉浸粉、5g氯化钠)培养液等量分装至试管中,从低浓度到高浓度依次定量吸取药液,分别加入上述试管中,充分摇匀,然后分别等量加入处于对数生长期的菌悬液,每处理重复4次。混匀后,放于25℃振荡培养箱黑暗培养,待对数生长期测量OD值。取有效的4个重复的平均值为测定结果,计算相对抑制率,将抑制率换算成机率值(y),药液浓度(μg/mL)转换成对数值(x),以最小二乘法求得毒力回归方程(y=a+bx),并由此计算出每种药剂的EC50值。
同时根据Wadley法计算两药剂不同配比联合增效比值(SR),SR<0.5为拮抗作用,0.5≤SR≤1.5为相加作用,SR>1.5为增效作用。计算公式如下:
SR=EC50(理论值)/EC50(实测值)
EC50(理论值)=(a+b)/[(a/A的EC50)+(b/B的EC50)
式中:A为化合物I,B为化合物II;a、b分别为化合物I与化合物II在组合物中所占的比例;
不同品种的农药混合后,通常表现出三种作用类型,即相加作用、增效作用和拮抗作用,但具体为何种作用,无法预测。本发明所述的组合物以化合物I与化合物II为有效活性成分,采用生物测定实例加以说明。
实施例1:为验证化合物I和辛菌胺醋酸盐不同配比用量对黄瓜细菌性角斑病抑菌效果,进行了化合物I和辛菌胺醋酸盐不同配比对黄瓜细菌性角斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表1化合物I和辛菌胺醋酸盐单剂及其混剂对黄瓜细菌性角斑病菌毒力测定结果
由表1结果可知,化合物I和辛菌胺醋酸盐不同配比用量混配对黄瓜细菌性角斑病菌的抑制均具有明显增效作用。
实施例2:为验证化合物I和氯溴异氰尿酸不同配比用量对西瓜细菌性果斑病抑菌效果,进行了化合物I和氯溴异氰尿酸不同配比对西瓜细菌性果斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表2化合物I和氯溴异氰尿酸单剂及其混剂对西瓜细菌性果斑病菌毒力测定结果
由上表可知,化合物I、氯溴异氰尿酸及其混配制剂对西瓜细菌性果斑病菌的抑制均具有明显增效作用。
实施例3:为验证化合物I和三氯异氰尿酸不同配比用量对大白菜软腐病抑菌效果,进行了化合物I和三氯异氰尿酸不同配比对大白菜软腐病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表3化合物I和三氯异氰尿酸单剂及其混剂对大白菜软腐病菌毒力测定结果
由上表可知,化合物I、三氯异氰尿酸及其混配制剂对大白菜软腐病菌的抑制均具有明显增效作用。
实施例4:为验证化合物I和菌毒清不同配比用量对水稻细菌性条斑病抑菌效果,进行了化合物I和菌毒清不同配比对水稻细菌性条斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表4化合物I和菌毒清单剂及其混剂对水稻细菌性条斑病菌毒力测定结果
由上表可知,化合物I、菌毒清及其混配制剂对水稻细菌性条斑病菌的抑制均具有明显增效作用。
实施例5:为验证化合物I和多粘类芽孢杆菌不同配比用量对水稻白叶枯抑菌效果,进行了化合物I和多粘类芽孢杆菌不同配比对水稻白叶枯的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表5化合物I和多粘类芽孢杆菌单剂及其混剂对水稻白叶枯病菌毒力测定结果
由上表可知,化合物I、多粘类芽孢杆菌及其混配制剂对水稻白叶枯病菌的抑制均具有明显增效作用。
实施例6:为验证化合物I和苯霜灵不同配比用量对黄瓜细菌性角斑病抑菌效果,进行了化合物I和苯霜灵不同配比对黄瓜细菌性角斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表6化合物I和苯霜灵单剂及其混剂对黄瓜细菌性角斑病菌毒力测定结果
由表6结果可知,化合物I和苯霜灵不同配比用量混配对黄瓜细菌性角斑病菌的抑制均具有明显增效作用。
实施例7:为验证化合物I和苯氧喹啉不同配比用量对西瓜细菌性果斑病抑菌效果,进行了化合物I和苯氧喹啉不同配比对西瓜细菌性果斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表7化合物I和苯氧喹啉单剂及其混剂对西瓜细菌性果斑病菌毒力测定结果
由上表可知,化合物I、苯氧喹啉及其混配制剂对西瓜细菌性果斑病菌的抑制均具有明显增效作用。
实施例8:为验证化合物I和辛噻酮不同配比用量对大白菜软腐病抑菌效果,进行了化合物I和辛噻酮不同配比对大白菜软腐病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表8化合物I和辛噻酮单剂及其混剂对大白菜软腐病菌毒力测定结果
由上表可知,化合物I、辛噻酮及其混配制剂对大白菜软腐病菌的抑制均具有明显增效作用。
实施例9:为验证化合物I和氟吡菌胺不同配比用量对水稻细菌性条斑病抑菌效果,进行了化合物I和氟吡菌胺不同配比对水稻细菌性条斑病的室内毒力测定,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表9化合物I和氟吡菌胺单剂及其混剂对水稻细菌性条斑病菌毒力测定结果
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由上表可知,化合物I、氟吡菌胺及其混配制剂对水稻细菌性条斑病菌的抑制均具有明显增效作用。
实施例10:为验证化合物I和异菌脲不同配比用量对水稻白叶枯抑菌效果,进行了化合物I和异菌脲不同配比对水稻白叶枯的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表10化合物I和异菌脲单剂及其混剂对水稻白叶枯病菌毒力测定结果
由上表可知,化合物I、异菌脲及其混配制剂对水稻白叶枯病菌的抑制均具有明显增效作用。
真菌毒力测定方法
选择马铃薯晚疫、辣椒炭疽为供试病原菌,采用菌丝生长速率法对化合物I、化合物II及其混配制剂进行毒力测定。
参照中华人民共和国农业行业标准NY/T 1156.2-2006,先将供试药剂(包括化合物I、化合物II)用合适的溶剂(溶剂的种类如丙酮、甲醇、N,N二甲基甲酰胺和二甲基亚砜等,并且依据其对样品的溶解能力而选择)配制成7个浓度梯度(化合物I:1.0、2.0、4.0、8.0、16.0、32.0、64.0μg/mL等7个浓度梯度;化合物II:1.0、2.0、4.0、8.0、16.0、32.0、64.0μg/mL等7个浓度梯度),将供混配的化合物I、化合物II分别按其EC50值剂量按质量比例设置一系列个配比,按不同配比配制成最终质量浓度(指化合物I、化合物II的总质量)为1.0、2.0、4.0、8.0、16.0、32.0、64.0μg/mL 7个系列浓度,在无菌操作条件下,根据试验处理将预先融化的灭菌PDA培养基(每升中含有6g马铃薯浸粉、20g葡萄糖和20g琼脂)定量加入无菌锥形瓶中,从低浓度到高浓度依次定量吸取药液,分别加入上述锥形瓶中,充分摇匀。然后等量倒入3个以上直径为9cm的培养皿中,制成相应浓度的含药平板。试验设不含药剂的处理作空白对照,每处理不少于3个重复。将培养好的病原菌,在无菌条件下用直径5mm的灭菌打孔器,自菌落边缘切取菌饼,用接种器将菌饼接种于含药平板中央,菌丝面朝上,盖上皿盖,置适宜温度的培养箱中培养。观察并用卡尺量菌落直径(须十字交叉量取两次,用其平均数)并做记录统计。如果发现有污染必须进行重复试验。最后进行活性初筛结果计算。结果以抑制率表示,具体公式如下:根据调查结果,按公式(1)、(2)计算各处理浓度对供试靶标菌的菌丝生长抑制率,单位为百分率(%),计算结果保留小数点后两位。
公式(1):D=D1-D2
式中:D——菌落增长直径;D1——菌落直径;D2——菌饼直径。
公式(2):I=(D0-Dt)/D0×100
式中:I——菌丝生长抑制率;D0——空白对照菌落增长直径;Dt——药剂处理菌落增长直径。接入菌饼后,放于25℃振荡培养箱黑暗培养,待对照菌丝长满2/3平皿时,用卡尺量菌落直径(须十字交叉量取两次,用其平均数),取有效的3个重复的平均值为测定结果,计算相对抑制率。将抑制率换算成机率值(y),药液浓度(μg/mL)转换成对数值(x),以最小二乘法求得毒力回归方程(y=a+bx),并由此计算出每种药剂的EC50值。
同时根据Wadley法计算两药剂不同配比联合增效比值(SR),SR<0.5为拮抗作用,0.5≤SR≤1.5为相加作用,SR>1.5为增效作用。计算公式如下:
SR=EC50(理论值)/EC50(实测值)
EC50(理论值)=(a+b)/[(a/A的EC50)+(b/B的EC50)
式中:A为化合物I,B为化合物II;a、b分别为化合物I与化合物II在组合物中所占的比例;
不同品种的农药混合后,通常表现出三种作用类型,即相加作用、增效作用和拮抗作用,但具体为何种作用,无法预测。本发明所述的组合物以化合物I与化合物II为有效活性成分,采用生物测定实例加以说明。
实施例11:为验证化合物I和甲霜灵不同配比用量对马铃薯晚疫病菌抑菌效果,进行了化合物I和甲霜灵不同配比对马铃薯晚疫病菌的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表11化合物I和甲霜灵单剂及其混剂对马铃薯晚疫病菌毒力测定结果
由上表可知,化合物I、甲霜灵及其混配制剂对马铃薯晚疫病菌的抑制均具有明显增效作用。
实施例12:为验证化合物I和多粘类芽孢杆菌不同配比用量对辣椒炭疽抑菌效果,进行了化合物I和多粘类芽孢杆菌不同配比对辣椒炭疽的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表12化合物I和多粘类芽孢杆菌单剂及其混剂对辣椒炭疽毒力测定结果
由上表可知,化合物I、多粘类芽孢杆菌及其混配制剂对辣椒炭疽病菌的抑制均具有明显增效作用。
实施例13:为验证化合物I和枯草芽孢杆菌不同配比用量对马铃薯晚疫病菌抑菌效果,进行了化合物I和枯草芽孢杆菌不同配比对马铃薯晚疫病菌的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表13化合物I和枯草芽孢杆菌单剂及其混剂对马铃薯晚疫病菌毒力测定结果
由上表可知,化合物I、枯草芽孢杆菌及其混配制剂对马铃薯晚疫病菌的抑制均具有明显增效作用。
实施例14:为验证化合物I和甲基托布津不同配比用量对辣椒炭疽抑菌效果,进行了化合物I和甲基托布津不同配比对辣椒炭疽的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表14化合物I和甲基托布津单剂及其混剂对辣椒炭疽毒力测定结果
由上表可知,化合物I、甲基托布津及其混配制剂对辣椒炭疽病菌的抑制均具有明显增效作用。
实施例15:为验证化合物I和氟唑菌苯胺不同配比用量对马铃薯晚疫病菌抑菌效果,进行了化合物I和氟唑菌苯胺不同配比对马铃薯晚疫病菌的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表15化合物I和氟唑菌苯胺单剂及其混剂对马铃薯晚疫病菌毒力测定结果
由上表可知,化合物I、氟唑菌苯胺及其混配制剂对马铃薯晚疫病菌的抑制均具有明显增效作用。
实施例16:为验证化合物I和唑菌酯不同配比用量对辣椒炭疽抑菌效果,进行了化合物I和唑菌酯不同配比对辣椒炭疽的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表16化合物I和唑菌酯单剂及其混剂对辣椒炭疽毒力测定结果
由上表可知,化合物I、唑菌酯及其混配制剂对辣椒炭疽病菌的抑制均具有明显增效作用。
实施例17:为验证化合物I和肟醚菌胺不同配比用量对马铃薯晚疫病菌抑菌效果,进行了化合物I和肟醚菌胺不同配比对马铃薯晚疫病菌的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表17化合物I和肟醚菌胺单剂及其混剂对马铃薯晚疫病菌毒力测定结果
由上表可知,化合物I、肟醚菌胺及其混配制剂对马铃薯晚疫病菌的抑制均具有明显增效作用。
实施例18:为验证化合物I和环酰菌胺不同配比用量对辣椒炭疽抑菌效果,进行了化合物I和环酰菌胺不同配比对辣椒炭疽的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表18化合物I和环酰菌胺单剂及其混剂对辣椒炭疽毒力测定结果
由上表可知,化合物I、环酰菌胺及混配制剂对辣椒炭疽病菌的抑制均具有明显增效作用。
实施例19:为验证化合物I和噻菌灵不同配比用量对马铃薯晚疫病菌抑菌效果,进行了化合物I和噻菌灵不同配比对马铃薯晚疫病菌的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表19化合物I和噻菌灵单剂及其混剂对马铃薯晚疫病菌毒力测定结果
由上表可知,化合物I、噻菌灵及其混配制剂对马铃薯晚疫病菌的抑制均具有明显增效作用。
实施例20:为验证化合物I和咪唑菌酮不同配比用量对辣椒炭疽抑菌效果,进行了化合物I和咪唑菌酮不同配比对辣椒炭疽的室内毒力测定试验,按照表内重量百分比配成相应浓度,进行室内抑菌试验,试验结果如下:
表20化合物I和咪唑菌酮单剂及其混剂对辣椒炭疽毒力测定结果
由上表可知,化合物I、咪唑菌酮及混配制剂对辣椒炭疽病菌的抑制均具有明显增效作用。
三、大田药效实施例
为了明确化合物I和化合物II单剂和混剂对黄瓜细菌性角斑病、柑橘溃疡病、水稻白叶枯、马铃薯晚疫病和辣椒炭疽病防治效果,在国内不同地区开展了多次药效试验。
黄瓜细菌性角斑病大田药效试验(于山东聊城冠县开展):
试验方法:根据《中华人民共和国国家标准GB/T 17980.110-2004》规定施药方法,在初见病斑时施药,7天后第2次施药,共施药两次,重复次数4次。
调查方法:根据《中华人民共和国国家标准GB/T 17980.110-2004》规定的调查方法,第2次施药后7天和14天调查防治效果。每小区对角线3点取样,每点5株,调查全部叶片,以每叶片病斑面积占整个叶片面积百分率分级。
分级方法:
0级:无病斑;1级:病斑面积占整个叶面积的5%以下;3级:病斑面积占整个叶面积的6%~10%;5级:病斑面积占整个叶面积的11%~20%;7级:病斑面积占整个叶面积的21%~50%;9级:病斑面积占整个叶面积的51%以上。
下述各实施例中的试剂的制备方法如上述制备例1-8所示,示例性地,实施例1的10%化合物I·辛菌胺醋酸盐可湿性粉剂的制备方法同制备例1,其中化合物II选自辛菌胺醋酸盐,实施例8的10%化合物I·三氯异氰尿酸可湿性粉剂的制备方法同制备例1,其中化合物II选自三氯异氰尿酸,同理,其他的实施例的制备参考上述制备例1-8。
下述各对比例中的制剂的制备方法同样如上述制备例1-8所示,只是其中的活性组分的含量可能会有所不同,相应的,制剂中的填料或水将组分补齐至100%。例如,对比例1的10%化合物I水分散粒剂的制备方法参照制备例2,其中10%化合物I替换制备例2中的20%化合物I和10%化合物II,含量的差异通过填料来填补。又例如,对比例2的3%辛菌胺醋酸盐可湿性粉剂的制备方法参照制备例1,其中3%辛菌胺醋酸盐可湿性粉剂替换制备例1中的5%化合物I和5%化合物II,含量的差异通过填料来填补。
表21化合物I与辛菌胺醋酸盐复配对黄瓜细菌性角斑病大田药效试验
注:同列数据后不同字母(a或b)表示经Duncan氏新复极差法检验在P<0.05水平差异显著,表22-表60具有相同的含义。
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与辛菌胺醋酸盐复配和单剂相比,在同等有效成分用量下,化合物I与辛菌胺醋酸盐复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.3%以上,持效期较长。
表22化合物I与三氯异氰尿酸复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与三氯异氰尿酸复配和单剂相比,在同等有效成分用量下,化合物I与三氯异氰尿酸复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到81.3%以上,持效期较长。
表23化合物I与氯溴异氰尿酸复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与氯溴异氰尿酸复配与单剂相比,在同等有效成分用量下,化合物I与氯溴异氰尿酸复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.2%以上,持效期较长。
表24化合物I与菌毒清复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与氯溴异氰尿酸复配与单剂相比,在同等有效成分用量下,化合物I与氯溴异氰尿酸复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到80.1%以上,持效期较长。
水稻白叶枯病大田药效试验(于江苏南京开展):
试验方法:根据《中华人民共和国国家标准GB/T 17980.19-2000》规定施药方法,在初见病斑时施药,7天后第2次施药,共施药两次,重复次数4次。
调查方法:根据《中华人民共和国国家标准GB/T 17980.19-2000》规定的调查方法,第2次施药后7天和14天调查防治效果。
白叶枯病病情普遍率(以目测分级):
0级:无病;1级:零星发病或有中心病团;3级:发病面积占总面积四分之一左右;5级:发病面积占总面积三分之一左右;7级:发病面积占总面积二分之一左右;9级:发病面积占总面积四分之三以上。
表25化合物I与辛菌胺醋酸盐复配对水稻白叶枯病大田药效试验
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由测定结果可知,在防治水稻白叶枯病时,化合物I与辛菌胺醋酸盐复配和单剂相比,在同等有效成分用量下,化合物I与辛菌胺醋酸盐对水稻白叶枯病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到81.2%以上,持效期较长。
表26化合物I与菌毒清复配对水稻白叶枯病大田药效试验
由测定结果可知,在防治水稻白叶枯病时,化合物I与菌毒清复配和单剂相比,在同等有效成分用量下,化合物I+菌毒清复配对对水稻白叶枯病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.4%以上,持效期较长。
柑橘溃疡病大田药效试验(于广西武鸣开展):
根据《农药田间药效试验准则(GB/T17980.103-2004)》规定施药方法,在始见开花之前第一次喷雾施药,出现病害后第二次喷雾施药。共施药两次,每个处理小区面积为成龄果树3株,重复次数4次。记录施药次数和每次施药日期及果树生育期。
调查方法:根据《农药田间药效试验准则(GB/T17980.103-2004)》规定调查方法,第二次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上的全部叶片,计算防治防效。
叶分级方法:
0级:每叶有病斑1~5个;3级:每叶有病斑6~10个;5级:每叶有病斑11~15个;7级:每叶有病斑15~20个;9级:每叶有病斑21个以上;
表27化合物I与辛菌胺醋酸盐复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与辛菌胺醋酸盐复配和单剂相比,在同等有效成分用量下,化合物I与辛菌胺醋酸盐复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到80.2%以上,持效期较长。
表28化合物I与氯溴异氰尿酸复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与氯溴异氰尿酸复配和单剂相比,在同等有效成分用量下,化合物I与氯溴异氰尿酸复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.5%以上,持效期较长。
表29化合物I与多粘类芽孢杆菌复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与多粘类芽孢杆菌复配和单剂相比,在同等有效成分用量下,化合物I与多粘类芽孢杆菌复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到80.3%以上,持效期较长。
马铃薯晚疫病大田药效试验(于内蒙古赤峰开展):
根据《农药田间药效试验准则(GB/T17980.34-2000)》规定施药方法对马铃薯进行茎叶喷雾。
调查方法:根据《农药田间药效试验准则(GB/T17980.34-2000)》规定调查方法,第二次施药后14d对每个小区调查两株,每株按东西南北中五点取样,每株调查全部叶片,计算防治防效。
分级方法:
0级:无病斑;1级:病斑面积占整个叶面积5%以下;3级:病斑面积占整个叶面积6%~10%;5级:病斑面积占整个叶面积11%~20%;7级:病斑面积占整个叶面积21%~50%;9级:病斑面积占整个叶面积50%以上。
表30化合物I与甲霜灵复配对马铃薯晚疫病大田药效试验
由测定结果可知,在防治马铃薯晚疫病时,化合物I与氟噻唑吡乙酮复配和单剂相比,在同等有效成分用量下,化合物I与氟噻唑吡乙酮复配对马铃薯晚疫病的14天防效明显高于单剂。其中14天防效依然能达到81.7%以上,持效期较长。
辣椒炭疽病大田药效试验(于山东省济南市曲堤镇开展):
根据《农药田间药效试验准则(GB/T17980.33-2000)》规定施药方法对辣椒进行茎叶喷雾。
调查方法:根据《农药田间药效试验准则(GB/T17980.33-2000)》规定调查方法,第二次施药后7d和14d对每个小区进行调查,每小区调查50个果实,计算防治防效。
分级方法:
0级:无病斑;1级:病斑面积占果实面积2%以下;3级:病斑面积占果实面积3%~8%;5级:病斑面积占果实面积9%~15%;7级:病斑面积占果实面积16%~25%;9级:病斑面积占果实面积25%以上。
表31化合物I与多粘类芽孢杆菌复配对辣椒炭疽病大田药效试验
由测定结果可知,在防治辣椒炭疽病时,化合物I与多粘类芽孢杆菌复配和单剂相比,在同等有效成分用量下,化合物I与多粘类芽孢杆菌复配对辣椒炭疽病的14天防效明显高于单剂。其中14天防效依然能达到79.9%以上,持效期较长。
表32化合物I与苯霜灵复配对黄瓜细菌性角斑病大田药效试验
注:同列数据后不同字母表示经Duncan氏新复极差法检验在P<0.05水平差异显著,下同。
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与苯霜灵复配和单剂相比,在同等有效成分用量下,化合物I与苯霜灵复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.8%以上,持效期较长。
表33化合物I与异菌脲复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与异菌脲复配和单剂相比,在同等有效成分用量下,化合物I与异菌脲复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到80.6%以上,持效期较长。
表34化合物I与甲基托布津复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与甲基托布津复配与单剂相比,在同等有效成分用量下,化合物I与甲基托布津复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.4%以上,持效期较长。
表35化合物I与噻菌灵复配对黄瓜细菌性角斑病大田药效试验
由表中测定结果可知,在防治黄瓜细菌性角斑病时,化合物I与噻菌灵复配与单剂相比,在同等有效成分用量下,化合物I与噻菌灵复配对黄瓜细菌性角斑病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.3%以上,持效期较长。
水稻白叶枯病大田药效试验(于江苏南京开展):
试验方法:根据《中华人民共和国国家标准GB/T 17980.19-2000》规定施药方法,在初见病斑时施药,7天后第2次施药,共施药两次,重复次数4次。
调查方法:根据《中华人民共和国国家标准GB/T 17980.19-2000》规定的调查方法,第2次施药后7天和14天调查防治效果。
白叶枯病病情普遍率(以目测分级):
0级:无病;1级:零星发病或有中心病团;3级:发病面积占总面积四分之一左右;5级:发病面积占总面积三分之一左右;7级:发病面积占总面积二分之一左右;9级:发病面积占总面积四分之三以上。
表36化合物I与缬菌胺复配对水稻白叶枯病大田药效试验
由测定结果可知,在防治水稻白叶枯病时,化合物I与缬菌胺复配和单剂相比,在同等有效成分用量下,化合物I与缬菌胺对水稻白叶枯病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.3%以上,持效期较长。
表37化合物I与环酰菌胺复配对水稻白叶枯病大田药效试验
由测定结果可知,在防治水稻白叶枯病时,化合物I与环酰菌胺复配和单剂相比,在同等有效成分用量下,化合物I+环酰菌胺复配对对水稻白叶枯病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.7%以上,持效期较长。
柑橘溃疡病大田药效试验(于广西武鸣开展):
根据《农药田间药效试验准则(GB/T17980.103-2004)》规定施药方法,在始见开花之前第一次喷雾施药,出现病害后第二次喷雾施药。共施药两次,每个处理小区面积为成龄果树3株,重复次数4次。记录施药次数和每次施药日期及果树生育期。
调查方法:根据《农药田间药效试验准则(GB/T17980.103-2004)》规定调查方法,第二次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上的全部叶片,计算防治防效。
叶分级方法:
0级:每叶有病斑1~5个;3级:每叶有病斑6~10个;5级:每叶有病斑11~15个;7级:每叶有病斑15~20个;9级:每叶有病斑21个以上;
表38化合物I与枯草芽孢杆菌复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与枯草芽孢杆菌复配和单剂相比,在同等有效成分用量下,化合物I与枯草芽孢杆菌复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到80.4%以上,持效期较长。
表39化合物I与异菌脲复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与异菌脲复配和单剂相比,在同等有效成分用量下,化合物I与异菌脲复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.5%以上,持效期较长。
表40化合物I与苯氧喹啉复配对柑橘溃疡病大田药效试验
由测定结果可知,在防治柑橘溃疡病时,化合物I与苯氧喹啉复配和单剂相比,在同等有效成分用量下,化合物I与苯氧喹啉复配对柑橘溃疡病的7天防效和14天防效明显高于单剂。其中14天防效依然能达到79.2%以上,持效期较长。
柑橘溃疡病、柑橘蚜虫、红蜘蛛大田药效试验(于广西武鸣开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表41化合物I与氟虫双酰胺复配对柑橘溃疡病大田药效试验
表42化合物I与氟虫双酰胺复配对柑橘蚜虫、红蜘蛛大田药效试验
由表41和表42测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对柑橘溃疡病防效高于化合物I单剂;当组合物中氟虫双酰胺用量与氟虫双酰胺单剂用量相同时,组合物对柑橘树蚜虫和红蜘蛛的防治效果高于氟虫双酰胺单剂。说明化合物I与氟虫双酰胺复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
桃细菌性穿孔病、桃树蚜虫、桃小食心虫大田药效试验(于泰安肥城开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表43化合物I与螺螨双酯复配对桃细菌性穿孔病大田药效试验
表44化合物I与螺螨双酯复配对桃树蚜虫、桃小食心虫大田药效试验
由表43和表44测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对桃细菌性穿孔病防效高于化合物I单剂;当组合物中螺螨双酯用量与螺螨双酯单剂用量相同时,组合物对桃树蚜虫、桃小食心虫的防治效果高于螺螨双酯单剂。说明化合物I与螺螨双酯复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
黄瓜角斑病、黄瓜蓟马、美洲斑潜蝇大田药效试验(于济南市济阳区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表45化合物I与乙虫腈复配对黄瓜角斑病大田药效试验
表46化合物I与乙虫腈复配对黄瓜蓟马、美洲斑潜蝇大田药效试验
由表45和表46测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对黄瓜角斑病防效高于化合物I单剂;当组合物中乙虫腈用量与乙虫腈单剂用量相同时,组合物对黄瓜蓟马、美洲斑潜蝇的防治效果高于乙虫腈单剂。说明化合物I与乙虫腈复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
甘蓝软腐病、甘蓝小菜蛾、菜青虫大田药效试验(于济南市济阳区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表47化合物I与丁虫腈复配对甘蓝软腐病大田药效试验
表48化合物I与丁虫腈复配对甘蓝小菜蛾、菜青虫大田药效试验
由表47和表48测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对甘蓝软腐病防效高于化合物I单剂;在丁虫腈同等用量下,组合物对甘蓝小菜蛾、菜青虫的防治效果高于丁虫腈单剂。说明化合物I与丁虫腈复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
茄子青枯病、茄子蓟马、朱砂叶螨大田药效试验(于济南市济阳区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表49化合物I与喹螨醚复配对茄子青枯病大田药效试验
表50化合物I与喹螨醚复配对茄子蓟马、朱砂叶螨大田药效试验
由表49和表50测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对茄子青枯病防效高于化合物I单剂;当组合物中喹螨醚用量与喹螨醚单剂用量相同时,组合物对茄子蓟马、朱砂叶螨的防治效果高于喹螨醚单剂。说明化合物I与喹螨醚复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。甜瓜角斑病、甜瓜蓟马、烟粉虱大田药效试验(于济南市天桥区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表51化合物I与环氧虫啶复配对甜瓜角斑病大田药效试验
表52化合物I与环氧虫啶复配对甜瓜蓟马、烟粉虱大田药效试验
由表51和表52测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对甜瓜角斑病防效高于化合物I单剂;当组合物中环氧虫啶用量与环氧虫啶单剂用量相同时,组合物对甜瓜蓟马、烟粉虱的防治效果高于环氧虫啶单剂。说明化合物I与环氧虫啶复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。花生青枯病、花生蚜虫、蛴螬大田药效试验(于济南市天桥区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表53化合物I与辛硫磷复配对花生青枯病大田药效试验
表54化合物I与辛硫磷复配对花生蚜虫、蛴螬大田药效试验
由表53和表54测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对花生青枯病防效高于化合物I单剂;当组合物中辛硫磷用量与辛硫磷单剂用量相同时,组合物对花生蚜虫、蛴螬的防治效果高于噻虫胺单剂。说明化合物I与辛硫磷复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
水稻白叶枯病、稻纵卷叶螟、稻飞虱大田药效试验(于江西省吉安县开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表55化合物I与烯虫酯复配对水稻白叶枯病大田药效试验
表56化合物I与烯虫酯复配对稻纵卷叶螟、稻飞虱大田药效试验
由表55和表56测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对水稻白叶枯病防效高于化合物I单剂;当组合物中烯虫酯用量与烯虫酯单剂用量相同时,组合物对稻纵卷叶螟、稻飞虱的防治效果高于烯虫酯单剂。说明化合物I与烯虫酯复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
西瓜果斑病、西瓜烟粉虱、蓟马大田药效试验(于潍坊市昌乐县开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表57化合物I与噻嗪酮复配对西瓜果斑病大田药效试验
表58化合物I与噻嗪酮复配对西瓜烟粉虱、蓟马大田药效试验
由表57和表58测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对西瓜果斑病防效高于化合物I单剂;当组合物中噻嗪酮用量与噻嗪酮单剂用量相同时,组合物对西瓜烟粉虱、蓟马的防治效果高于噻嗪酮单剂。说明化合物I与噻嗪酮复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
番茄青枯病、番茄烟粉虱、蓟马大田药效试验(于济南市天桥区开展):
参照农药田间药效试验准则规定施药方法,病虫害初发期第1次施药,7天后第2次施药。2次施药后7d,14d对每个小区调查两株,每株按东西南北中五点取样,每点调查两个梢上全部叶片的病虫害,计算防治防效。
田间药效试验结果:
表59化合物I与溴氰虫酰胺复配对番茄青枯病大田药效试验
表60化合物I与溴氰虫酰胺复配对番茄烟粉虱、蓟马大田药效试验
由表59和表60测定结果可知,当组合物中化合物I用量与化合物I单剂用量相同时,组合物对番茄青枯病防效高于化合物I单剂;当组合物中溴氰虫酰胺用量与溴氰虫酰胺单剂用量相同时,组合物对番茄烟粉虱、蓟马的防治效果高于溴氰虫酰胺单剂。说明化合物I与溴氰虫酰胺复配能够做到病虫兼防,减少使用次数,降低使用成本。而且在试验用药范围内对靶标作物无不良影响。
以上,对本发明的实施方式进行了说明。但是,本发明不限定于上述实施方式。凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (14)
1.一种杀菌杀虫组合物,所述组合物包括有效活性成分,所述有效活性成分由化合物I和化合物II组成,所述化合物I为7-氯-1-环丙基-6-氟-4-氧代-1,4-二氢喹啉-3-羧酸-2-甲氧基乙酯,所述化合物II为辛菌胺醋酸盐;
其中,所述化合物I和化合物II的质量比为50~1:1~50。
2.根据权利要求1所述的组合物,其中,所述化合物I和化合物II的质量比为30~1:1~30。
3.根据权利要求1或2所述的组合物,其中,以所述组合物的总重量为100%计,所述化合物I与化合物II在组合物中的质量之和为1~80%。
4.根据权利要求1或2所述的组合物,其中,所述组合物制备成液体制剂或固体制剂;其中,液体制剂中含有按重量计1%~60%的有效活性成分;固体制剂中含有按重量计5%~80%的有效活性成分。
5.根据权利要求3所述的组合物,其中,所述组合物制备成液体制剂或固体制剂;
其中,液体制剂中含有按重量计1%~60%的有效活性成分;固体制剂中含有按重量计5%~80%的有效活性成分。
6.根据权利要求1、2和5中任一项所述的组合物,其中,所述组合物中还包括去离子水、有机溶剂、乳化剂、分散剂、润湿剂、增稠剂、消泡剂、稳定剂、粘结剂、崩解剂、抗冻剂、抗结剂、助悬剂、成膜剂、防腐剂、着色剂、高分子囊壁材料、pH调节剂或填料。
7.根据权利要求3所述的组合物,其中,所述组合物中还包括去离子水、有机溶剂、乳化剂、分散剂、润湿剂、增稠剂、消泡剂、稳定剂、粘结剂、崩解剂、抗冻剂、抗结剂、助悬剂、成膜剂、防腐剂、着色剂、高分子囊壁材料、pH调节剂或填料。
8.根据权利要求4所述的组合物,其中,所述组合物中还包括去离子水、有机溶剂、乳化剂、分散剂、润湿剂、增稠剂、消泡剂、稳定剂、粘结剂、崩解剂、抗冻剂、抗结剂、助悬剂、成膜剂、防腐剂、着色剂、高分子囊壁材料、pH调节剂或填料。
9.根据权利要求1、2、5、7和8中任一项所述的组合物,其中,所述组合物的剂型为水分散粒剂、可分散液剂、可湿性粉剂、悬浮剂、水乳剂、微乳剂、悬乳剂、微囊悬浮剂、微囊悬浮-悬浮剂、悬浮种衣剂、乳油或颗粒剂。
10.根据权利要求3所述的组合物,其中,所述组合物的剂型为水分散粒剂、可分散液剂、可湿性粉剂、悬浮剂、水乳剂、微乳剂、悬乳剂、微囊悬浮剂、微囊悬浮-悬浮剂、悬浮种衣剂、乳油或颗粒剂。
11.根据权利要求4所述的组合物,其中,所述组合物的剂型为水分散粒剂、可分散液剂、可湿性粉剂、悬浮剂、水乳剂、微乳剂、悬乳剂、微囊悬浮剂、微囊悬浮-悬浮剂、悬浮种衣剂、乳油或颗粒剂。
12.根据权利要求6所述的组合物,其中,所述组合物的剂型为水分散粒剂、可分散液剂、可湿性粉剂、悬浮剂、水乳剂、微乳剂、悬乳剂、微囊悬浮剂、微囊悬浮-悬浮剂、悬浮种衣剂、乳油或颗粒剂。
13.权利要求1-12中任一项所述的组合物在防治农业病害的应用;
其中,所述应用为在防治黄瓜细菌性角斑病、水稻白叶枯和柑橘溃疡病中的应用。
14.一种防治农业病害的方法,包括将权利要求1-13任一项所述组合物施用于存在农业病害的植物上;其中,所述农业病害为黄瓜细菌性角斑病、水稻白叶枯和柑橘溃疡病中的至少一种。
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