CN112155016B - Isothiocyanate and fluopyram composition, preparation and application - Google Patents

Isothiocyanate and fluopyram composition, preparation and application Download PDF

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CN112155016B
CN112155016B CN202010928366.0A CN202010928366A CN112155016B CN 112155016 B CN112155016 B CN 112155016B CN 202010928366 A CN202010928366 A CN 202010928366A CN 112155016 B CN112155016 B CN 112155016B
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isothiocyanate
fluopyram
percent
soil
composition
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CN112155016A (en
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吴华
任晶晶
冯俊涛
马志卿
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Northwest A&F University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
    • A01N47/46Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=C=S groups
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/18Vapour or smoke emitting compositions with delayed or sustained release
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention discloses a composition of isothiocyanate and fluopyram, a preparation and an application, wherein the composition comprises the following components in parts by weight: the weight ratio of the isothiocyanate to the fluopyram is 1:9-9:1. The compound agent can be prepared into soluble liquid, aqueous emulsion, oil agent and microemulsion, and is applied to the prevention and treatment of soil nematodes, soil pests and soil-borne pathogenic bacteria. The compound agent has obvious synergy, high bacteriostatic and nematicidal activity and small relative dosage, and particularly has obvious fumigation effect on pests such as soil-borne pathogenic fungi, soil nematodes and the like.

Description

Isothiocyanate and fluopyram composition, preparation and application
Technical Field
The invention belongs to the technical field of pesticide compounding, in particular relates to a pesticide composition for preventing and treating pests (nematodes, soil-borne pathogenic fungi, soil-borne pathogenic bacteria and soil pests) in soil, and particularly relates to a compound agent of isothiocyanate and fluopyram and application thereof in preparation of a pesticide fumigant, such as: a composition of isothiocyanate and fluopyram, a preparation and an application thereof.
Background
Isothiocyanates (ITCs) are widely present in cruciferous plants, and particularly in Brassica and Armoracia plants, in appreciable amounts. Isothiocyanate-type compounds contained in various plants vary in kind, and most plants contain Allyl Isothiocyanate (AITC), aryl isothiocyanate, propyl isothiocyanate, 4-isopentenyl isothiocyanate, phenyl isothiocyanate, benzyl isothiocyanate, 5-methylthiopentoisothiocyanate, 6-methylthiohexyl isothiocyanate, 7-methylthioheptyl isothiocyanate, and the like. In plant tissues, various types of ITCs coexist, fat ITCs possibly play a role in biological fumigation firstly, and aromatic ITCs are slowly released to play a role in synergism and prolonging the effective period. Besides the flavoring effect, various biological activities of isothiocyanate compounds are widely researched, and the isothiocyanate compounds are proved to have the capability of killing or inhibiting bacteria, such as stronger inhibitory activity on vibrio cholerae, typhoid bacillus, staphylococcus aureus, tubercle bacillus, salmonella, bai Houjun, escherichia coli, bacillus subtilis and the like. Has high antibacterial rate to fungi such as Paecilomyces variotii and cerevisiae Fermentum.
Fluopyram (fluopyram) is a succinate dehydrogenase inhibitor type bactericide and nematicide developed by Bayer, and has a chemical name of N- {2- [ 3-chloro-5- (trifluoromethyl) -2-pyridyl]Ethyl } -alpha, alpha-ortho-trifluoromethyl-benzamideCAS number 658066-35-4. It is not only a new generation of excellent nematocide, but also a broad-spectrum bactericide, a seed treatment agent, an agricultural product storage preservative and the like, and has multiple functions. The nematicide is mainly used for preventing and controlling alternaria leaf spot, gray mold, powdery mildew, sclerotinia, early blight and the like on vegetables such as grapes, pear trees, bananas, apples, cucumbers, tomatoes and the like and field crops and the like, can be registered on various crops for preventing and controlling various nematodes, and is an efficient, green and low-toxicity nematicide.
CN1124075C discloses a composition containing isothiocyanate and its use, which contains AITC and an antibacterial composition of polyhydric alcohol with aldehyde group or ketone group, and is mainly used for the purpose of treating microorganisms, vegetable fresh-keeping and treating perishable goods. CN101133739 has proposed several formulations of products containing allyl isothiocyanate as the main active ingredient for soil, foodstuff, textile and tobacco warehouses, respectively, and provides a fumigating method very convenient for users, and also indicates the specific application and dosage of AITC as a pesticide product.
Bayer corporation owns the core compound patent ZL03819471.6, filed 8/2003, granted 6/2007, and the protective period will last 8/2023. The protection scope of the patent is subject to the content of the claims. The compounds claimed in this patent correspond to, but are not limited to, fluopyram, and in addition to the core compound patent, bayer corporation has multiple patents on fluopyram compounds that expire during 2025-2031, including, but not limited to, the following patents: the patent No ZL200580004215.X is characterized in that the mixed components comprise fluopyram, trifloxystrobin, azoxystrobin, fluoxastrobin, dimoxystrobin and picoxystrobinPyraclostrobin, 2- {2- [6- (3-chloro-2-methylphenoxy) -5-fluoro-pyrimidin-4-yloxy ] -ethyl]-phenyl } 2-methoxyimino-N-methylacetamide, dimoxystrobin,N- [2- (1,3-dimethylbutyl) phenyl ] methyl ester]-5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxamides, boscalid,N- (3 ',4' -dichloro-5-fluorobiphenyl-2-yl) -3- (difluoromethyl) -1-methyl-1H-pyrazole-4-carboxamides, fenamidone orN- [2- (1,3-dimethylbutyl) thiophen-3-yl]-1-dimethyl-3- (trifluoromethyl) -1H-pyrazole-4-hydroxyamide; patent No. ZL200580004216.4, the mixed components are fluopyram, bi-benzene diazolol, cyproconazole, difenoconazole, epoxiconazole, hexaconazole, metconazole, myclobutanil, propiconazole, prothioconazole, tebuconazole or triadimenol; the patent No. ZL200580004217.9 is prepared from fluopyram and cyprodinil, mepanipyrim or pyrimethanil. Currently, the registered fluopyram products of Bayer company are specifically as follows: the registration certificate number PD20200234, 500 g/l fluopyram-pyrimethanil suspending agent; the registration certificate number PD20172927, 35% fluorine bacteria tebuconazole suspending agent; registration certificate number PD20172803, 43% fluobacteria trifloxystrobin suspending agent; registration certificate number PD20121673, 96% fluopyram original drug; registration number PD20121664, 41.7% fluopyram suspension. CN103766353B discloses a fluopyram-containing bactericidal composition, the effective components of which are fluopyram and amino-oligosaccharin, the mass ratio of which is 20:1-1:20, is used for preventing and treating fungal diseases of flowers, wheat, fruit trees, cotton and vegetables.
In the longitudinal view of the above patents, fluopyram or isothiocyanate is mostly used as the main active ingredient for agricultural application, and is used for preventing and treating common agricultural diseases and pests, and the application of fluopyram and isothiocyanate as a compound preparation for preventing and treating stubborn soil-borne pathogenic fungi, soil-borne pathogenic bacteria and soil nematodes has not been disclosed and reported so far.
Disclosure of Invention
The invention aims to provide a composition and a compound agent of isothiocyanate and fluopyram with obvious synergistic effect.
The invention also aims to provide the application of the compound agent of the isothiocyanate and the fluopyram in preparing the pesticide fumigant for preventing and treating soil-borne pathogens and soil nematodes.
In order to achieve the purpose, the invention adopts the technical scheme that:
an isothiocyanate and fluopyram composition comprising, in combination: the weight ratio of the isothiocyanate to the fluopyram is 1:9-9:1.
Optionally, the weight ratio of the isothiocyanate to the fluopyram is 1:1-6:1.
Optionally, the isothiocyanate is selected from the group consisting of allyl isothiocyanate, benzyl isothiocyanate, 1-phenylethyl isothiocyanate, 2-phenylethyl isothiocyanate and p-trifluoromethylphenyl isothiocyanate.
An isothiocyanate and fluopyram preparation, which contains the isothiocyanate and fluopyram composition.
Optionally, the preparation is an oil agent;
the oil agent comprises the following components in percentage by weight:
1 to 30 percent of isothiocyanate,
1 to 20 percent of fluopyram,
0.1 to 2 percent of antioxidant,
10 to 85 percent of solvent,
the vegetable oil is supplemented to 100%;
wherein the antioxidant is ascorbic acid substances or amyl gallate; the solvent is ethyl acetate or sec-butyl acetate; the vegetable oil is turpentine oil or ligusticum chuanxiong hort oil.
Optionally, the preparation is an aqueous emulsion;
the aqueous emulsion comprises the following components in percentage by weight:
1 to 40 percent of isothiocyanate,
0.25 to 10 percent of fluopyram,
12 to 28 percent of emulsifier,
0.1 to 2 percent of ascorbic acid,
10 to 30 percent of solvent,
supplementing water to 100%;
wherein the emulsifier is No. 500, 602, OP-10, well201, TX-10, well205 or M30; the solvent is ethyl acetate, sec-butyl acetate or vegetable oil.
Optionally, the preparation is a soluble liquid;
the soluble liquid comprises the following components in percentage by weight:
1 to 60 percent of isothiocyanate,
0.2 to 20 percent of fluopyram,
12 to 60 percent of emulsifier,
1 to 8 percent of ascorbic acid,
the solvent is replenished to 100 percent;
wherein the emulsifier is No. 500, 602, OP-10, well201, well205 or M30; the solvent is ethyl acetate, sec-butyl acetate or turpentine.
Optionally, the preparation is a microemulsion;
the microemulsion comprises the following components in percentage by weight:
1 to 10 percent of fluopyram,
1 to 60 percent of isothiocyanate,
10 to 40 percent of solvent,
5 to 20 percent of emulsifier,
0.1 to 2 percent of ascorbic acid;
wherein the emulsifier is 500, 602, OP-10, well201, well205, M30; the solvent is ethyl acetate, sec-butyl acetate or turpentine.
The composition of the isothiocyanate and the fluopyram is applied to preparing a fumigant for preventing and treating soil-borne pathogens and/or soil nematodes.
The isothiocyanate and fluopyram preparation disclosed by the invention is applied to preparation of a fumigant for preventing and treating soil-borne pathogens and/or soil nematodes.
The invention has the beneficial effects that:
the invention takes isothiocyanate as a main active ingredient and takes fluopyram as a synergistic ingredient; the fumigation agent is suitable for fumigation of different occasions such as greenhouse soil, protected land and the like; has biological activities of killing bacteria, nematodes and the like; it can kill plant root-knot nematode by fumigation; meanwhile, the composite can fumigate and kill various harmful soil-borne pathogenic fungi and bacteria, has obvious synergistic effect, reduces the consumption of isothiocyanate, reduces toxicity and is beneficial to environmental protection.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the existing nematicide registered products taking allyl isothiocyanate as an active ingredient, the contents of the products are respectively 20% of allyl isothiocyanate aqueous emulsion and 20% of soluble liquid, but the high-content allyl isothiocyanate is fumigated by soil or soil coated with a film, so that the use is very inconvenient for operators, the fumigation is dazzling, and in order to effectively assist the use of the new product, a fumigation synergistic combination is needed to reduce the content of the preparation. Fluopyram is an excellent bactericide and nematicide developed by Bayer companies, but the prevention and control of nematodes in soil are extremely difficult, on one hand, the nematodes are hidden in plant roots, on the other hand, the nematodes are hidden in the soil, and the pesticide is required to have strong contact activity and fumigation activity or good penetrability. The allyl isothiocyanate has good fumigating activity on nematodes and soil-borne pathogens, the fluopyram has good contact killing activity on the nematodes and the soil-borne pathogens, and the combination of the allyl isothiocyanate and the fluopyram effectively controls soil-borne pests in different action modes and action mechanisms.
The inventor finds that the isothiocyanate single agent has the defects of limited penetrating capacity, short acting time, easy influence of soil moisture, easy hydrolysis under an acidic condition and the like in use when carrying out an isothiocyanate soil fumigation test, has abnormal pungent odor, is easy to hurt operators when in application, needs to be compounded to find the purpose of remarkable synergism, increase the acting time and the acting effect, improve the prevention and treatment effect, reduce the dosage of the medicament and reduce the environmental pollution.
Therefore, through a large number of experiments, the inventor prepares five isothiocyanate single agents of allyl isothiocyanate, benzyl isothiocyanate, 1-phenylethyl isothiocyanate, 2-phenylethyl isothiocyanate and p-trifluoromethylphenyl isothiocyanate, and performs fumigation activity screening on pathogenic fungi and root-knot nematodes.
Fluopyram is a new generation of excellent nematicides, acting on complex II [ Succinate Dehydrogenase (SDH) or succinate-coenzyme Q reductase (SQR) ] on the mitochondrial respiratory electron transport chain. The nematicide can be used for alternaria leaf spot, gray mold, powdery mildew, sclerotinia, early blight and the like on vegetables such as grapes, pear trees, bananas, apples, cucumbers, tomatoes and the like and field crops and the like, can be registered on various crops for preventing and controlling various nematodes, is an efficient, green and low-toxicity nematicide, and after the nematodes are treated by fluopyram, the bodies of the nematodes become needle-shaped and the activity is rapidly reduced. It has broad spectrum and long residual effect, can protect and promote early plant growth, and can be produced by Bayer AG.
The fumigation activity of the isothiocyanate is obvious, but the duration is short, the screening of the isothiocyanate synergist shows that the fluopyram and the isothiocyanate composition have obvious synergistic effect compared with a single agent, the using amount of the isothiocyanate is reduced, the quick effect is obvious, the duration is long, the environment is friendly, the composition is safe to people and livestock, a more ideal fumigation medicament can be formed, and the isothiocyanate and the fluopyram are mixed to form a novel nematicide (bactericide).
The mechanism of the fumigating action of the athomin (isothiocyanate) on the pests is as follows: the horseradish peroxidase binds to the mitochondrial complexes I and IV and inhibits the activity thereof, resulting in incomplete oxygen reduction, and active oxygen radicals are generated in vivo, and in the case where the CAT and POD activities are inhibited and the SOD activity is increased, it further results in excessive accumulation of oxygen radicals, thereby causing lipid peroxidation of the mitochondrial membrane, and ultimately death.
In order to realize the purpose of the invention, the ratio screening of two compounds is further carried out to find the effective component of isothiocyanate and the synergistic component of fluopyram, wherein the isothiocyanate is preferably selected from the following components: allyl isothiocyanate, benzyl isothiocyanate, 1-phenylethyl isothiocyanate, 2-phenylethyl isothiocyanate, p-trifluoromethylphenyl isothiocyanate. The weight ratio of the isothiocyanate to the fluopyram is 1:9-9:1, and the preferable weight ratio is 1:1-6:1.
The compound preparation of isothiocyanate and fluopyram can be prepared into pesticide preparations which are well known in the field, such as soluble liquid, aqueous emulsion, oil solution, microemulsion and the like. Can be made into different dosage forms according to different application occasions.
The oil agent comprises the following components in percentage by weight:
1 to 30 percent of isothiocyanate,
1 to 20 percent of fluopyram,
0.1 to 2 percent of antioxidant,
10 to 85 percent of solvent,
the vegetable oil is supplemented to 100 percent,
wherein the antioxidant is ascorbic acid or amyl gallate, the solvent is ethyl acetate or sec-butyl alcohol acetate, and the vegetable oil is oleum Terebinthinae or rhizoma Ligustici Chuanxiong oil.
The preparation process comprises the following steps: firstly, the antioxidant is added into the mixed mother liquor of the fluopyram and the isothiocyanate which are weighed quantitatively and fully and evenly stirred. And fully and uniformly mixing the vegetable oil and the solvent which are weighed accurately and quantitatively. And finally, mixing the two solutions in a preparation tank and continuously stirring for 1-3 hours. The product is subpackaged in a double-barrier plastic bottle or an aluminum bottle internally coated with a barrier layer and is stored in a sealed way.
The aqueous emulsion comprises the following components in percentage by weight:
1 to 40 percent of isothiocyanate,
0.25 to 10 percent of fluopyram,
12 to 28 percent of emulsifier,
0.1 to 2 percent of ascorbic acid,
10 to 30 percent of solvent,
the water is used for supplementing the mixture to 100 percent,
wherein the emulsifier is No. 500, no. 602 (the two emulsifiers are produced by Stadium petrochemical industry), OP-10, well201, well205 or M30 (the four emulsifiers are produced by Fujianwell chemical industry); the solvent is ethyl acetate or sec-butyl alcohol acetate.
The preparation process comprises the following steps: firstly, ascorbic acid is put into the mixed mother liquor of fluopyram and isothiocyanate which are quantitatively weighed and fully and evenly stirred. And fully and uniformly mixing the emulsifier and the solvent which are weighed accurately and quantitatively. And finally, continuously stirring the two solutions in a preparation tank for 1-3 hours. The product is subpackaged in a double-barrier plastic bottle, a glass bottle or an aluminum bottle internally coated with a barrier layer, and is stored in a sealed way.
The soluble liquid comprises the following components in percentage by weight:
1 to 60 percent of isothiocyanate,
0.2 to 20 percent of fluopyram,
12 to 60 percent of emulsifier,
1 to 8 percent of ascorbic acid,
the solvent is filled to 100 percent.
Wherein the emulsifier is No. 500, 602 (the two are Zhong Shandan for production), OP-10, well201, well205 or M30 (the four are Fujianwell chemical production); the solvent is ethyl acetate or sec-butyl acetate, wherein a mixed solvent is preferred, and the ratio of ethyl acetate to sec-butyl acetate is 1:1 (V/V).
The preparation process comprises the following steps: firstly, adding ascorbic acid into a mixed mother solution of fluopyram and isothiocyanate which are quantitatively weighed, and fully and uniformly stirring. And fully and uniformly mixing the agricultural emulsifier and the solvent which are weighed accurately and quantitatively. And finally, continuously stirring the two solutions in a preparation tank for 1-3 hours. The product is subpackaged in double-barrier plastic bottles and is stored in a sealed way.
The microemulsion comprises the following components in percentage by weight:
1 to 10 percent of fluopyram,
1 to 60 percent of isothiocyanate,
10 to 40 percent of solvent,
5 to 20 percent of emulsifier,
0.1 to 2 percent of ascorbic acid,
wherein, the emulsifier is 500 # and 602 (the two are Zhong Shandan for production), OP-10, well201, well205 and M30 (the four are in Fujianwell chemical production); the solvent is ethyl acetate or sec-butyl acetate.
The preparation process comprises the following steps: the isothiocyanate and the fluopyram are fully and uniformly mixed in a blending tank (1). Adding ascorbic acid into the blending tank (1) and fully mixing. Adding an emulsifier into the blending tank (2), mixing, adding a solvent, and fully and uniformly mixing. And (3) completely moving the materials in the blending tank (2) into the blending tank (1) through a pipeline, sealing the opening of the tank, and then starting a stirrer for stirring. And subpackaging the product into double-barrier plastic bottles, wherein each bottle contains 500mL of medicine.
The production process is completed by a machine under a closed condition, and personnel are prevented from directly contacting the liquid medicine.
The composition of isothiocyanate and fluopyram is used for preparing pesticide fumigants for preventing and treating soil nematodes and harmful fungi and bacteria.
Watermelon wilt bacterium used in the following experiment (Fusarium oxysporum) And Agrobacterium tumefaciens(Agrobacterium tumefaciens)The virus is a conventional pathogen which can be obtained by self separation and identification in a laboratory or purchased in the market.
Experimental example 1: the five compounds and the compound agent thereof are used for measuring the research on the biological activity fumigation activity of pathogenic bacteria, and 10 treatments are set in the test;
(1) 30 μ g/mL allyl isothiocyanate;
(2) 30 μ g/mL benzyl isothiocyanate;
(3) 30 μ g/mL 1-phenylethyl isothiocyanate;
(4) 2-phenylethyl isothiocyanate at 30 μ g/mL;
(5) 30 μ g/mL of p-trifluoromethylphenyl isothiocyanate;
(6) 30 μ g/mL allyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(7) 30 μ g/mL benzyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(8) 30 μ g/mL 1-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(9) 30 μ g/mL 2-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(10) 30 μ g/mL p-trifluoromethylphenyl isothiocyanate +5 μ g/mL fluopyram (6:1);
TABLE 1 Fumigation Activity of different isothiocyanates single and complex formulations against biological Activity of pathogenic bacteria
Treatment of Inhibition ratio (%) of watermelon wilt bacteria Agrobacterium tumefaciens inhibitory rate (%)
1 92.8 94.1
2 66.3 39.3
3 63.9 41.7
4 72.3 34.5
5 57.8 35.7
6 100 100
7 90.4 79.8
8 94 73.8
9 91.6 66.7
10 90.4 75
Allyl isothiocyanate, benzyl isothiocyanate, 1-phenylethyl isothiocyanate, 2-phenylethyl isothiocyanate and p-trifluoromethylphenyl isothiocyanate all have strong fumigating activity against Fusarium oxysporum and Agrobacterium tumefaciens at a concentration of 30. Mu.g/mL. Allyl isothiocyanate showed the highest biological activity for fumigating hyphae. The effect of the compound preparation is higher than that of a single preparation, wherein the allyl compound preparation shows the highest biological activity.
Experimental example 2, research on indoor biological activity of pathogenic bacteria by isothiocyanate, fluopyram and a compound agent thereof respectively, wherein 11 treatments are set in the experiment;
(1) 20 μ g/mL allyl isothiocyanate;
(2) Benzyl isothiocyanate, 20. Mu.g/mL;
(3) 20 μ g/mL 1-phenylethyl isothiocyanate;
(4) 20 μ g/mL 2-phenylethyl isothiocyanate;
(5) 20 μ g/mL of p-trifluoromethylphenyl isothiocyanate;
(6) 20 mu g/mL fluopyram;
(7) 20 μ g/mL allyl isothiocyanate +20g/mL fluopyram (1:1);
(8) 20 μ g/mL benzyl isothiocyanate +20 μ g/mL fluopyram (1:1);
(9) 20 μ g/mL 1-phenylethyl isothiocyanate +20 μ g/mL fluopyram (1:1);
(10) 20 μ g/mL 2-phenylethyl isothiocyanate +20 μ g/mL fluopyram (1:1);
(11) 20 μ g/mL p-trifluoromethylphenyl isothiocyanate +20 μ g/mL fluopyram (1:1);
TABLE 2 indoor biological activity of different isothiocyanates single and compound preparations against pathogenic bacteria
Figure 763601DEST_PATH_IMAGE001
The inhibition effect of the five isothiocyanate compounds on soil-borne pathogen fungi watermelon wilt pathogenic bacteria and soil-borne pathogen bacteria Agrobacterium tumefaciens is determined by a bacteriostatic circle method, and the result shows that the bacteriostatic activity of aryl ITCs such as benzyl and 2-phenylethyl isothiocyanate on a culture medium is superior to that of aliphatic isothiocyanate, and the activity of the benzyl and 2-phenylethyl isothiocyanate is higher. The inhibition rates of 20 mu g/mL fluopyram on Fusarium oxysporum and Agrobacterium tumefaciens are 57.8% and 46.4%, respectively. The effect of the compound agent is higher than that of a single agent, the compound effect of the benzyl isothiocyanate, the 2-phenylethyl isothiocyanate and the fluopyram is better, and the inhibition rate reaches 100 percent.
Experimental example 3: measurement result of biological activity of 2-phenylethyl isothiocyanate and fluopyram composition oil agent on pathogenic bacteria
The fluopyram and aryl isothiocyanate obtained in the above way are respectively combined according to different proportions, and are prepared into different concentrations by acetone, and the biological activity of pathogenic bacteria is compounded and screened. The indoor biological activity determination of the compound agents with different proportions on the fungi in the soil is researched by adopting a direct fumigation method (the fungi in the soil are mainly Fusarium oxysporum f.sp.citrulli of Deuteromycotina). Checking the result after 3d fumigation, taking the average colony number to calculate the inhibition rateAnd EC thereof 50 And the synergy index was calculated using the following formula.
Figure 499476DEST_PATH_IMAGE002
EC 50F Represents the inhibitory median concentration, EC, of fluopyram against certain pathogenic bacteria 50X Represents the inhibitory median concentration, EC, of the isothiocyanate against a certain pathogen 50FX Represents the inhibiting medium concentration of the mixture of fluopyram and isothiocyanate on certain pathogenic bacteria,P F represents the proportion of fluopyram in the mixture,P X representing the proportion of isothiocyanate in the mixture.
CTC < 80 for antagonism, 80< CTC < 120 for additivity, CTC >120 for synergy.
TABLE 3 indoor bioactivity of the compounded preparation on fungi in soil
Figure 963955DEST_PATH_IMAGE003
Note: in the table, "F" represents fluopyram and "P" represents 2-Phenylethyl ITC (2-Phenylethyl isothiocyanate).
From the above table, 2-phenylethyl isothiocyanate: fluopyram 6:1 has the strongest inhibiting effect on soil fungi mainly including Fusarium oxysporum f.sp.citrulli of Fusarium of fungi imperfecti, and EC thereof 50 6.3 mL/kg, coefficient of synergy 186.81, remarkable synergy and EC 50 The value is lower, and the practical possibility of application to production is provided.
According to the method, the soft rot in the soil is treated by compounding the medicaments in different proportions(Erwinia aroideae)Indoor biological activity assay of (1). Checking the result after 3d fumigation, taking the average colony number to calculate the inhibition rate and EC thereof 50 And the synergy coefficient was calculated using the Sun Yun Peterson equation (the calculation equation is as above).
TABLE 4 indoor bioactivity of the compounded preparation on bacteria in soil
Figure 960730DEST_PATH_IMAGE004
Note: in the table, "F" represents fluopyram and "P" represents 2-Phenylethyl ITC (2-Phenylethyl isothiocyanate).
As shown in the results of Table 4, the combination of 2-phenylethyl isothiocyanate has certain synergistic effect on the tested germs in the weight ratio of 9/1 to 4/1, especially when the weight ratio of 2-phenylethyl isothiocyanate is 6:1, the CTC value of soil bacteria is 233.06, and the synergistic effect is certain, and the EC is 50 The value decreases significantly.
Experimental example 4: indoor joint toxicity determination of fluopyram on pathogenic bacteria by respectively using fluopyram and allyl isothiocyanate, benzyl isothiocyanate and composition
The allyl isothiocyanate and the benzyl isothiocyanate which are separated and prepared as above are combined with the fluopyram according to the proportion shown in the table, acetone is used for preparing different concentrations, and the results of the compound screening of the biological activity of the second-instar larvae of the meloidogyne incognita are shown in the table 5.
TABLE 5 indoor toxicity determination of two isothiocyanates and fluopyram compounded preparations on pathogenic bacteria
Figure 219673DEST_PATH_IMAGE005
The results in Table 5 show that the combination of two different isothiocyanates and fluopyram has a synergistic effect on both the wilt bacteria of watermelon and the A.tumefaciens to be tested, especially on the wilt bacteria of watermelon EC when the weight ratio of allyl isothiocyanates to fluopyram is 6:1 50 The lowest value, only 1.98 μ g/mL, whereas benzyl isothiocyanate: fluopyram =6:1 against A. Tumefaciens EC 50 The value is lowest, and is only 6.17 mug/mL.
Experimental example 5: fumigation activity of different isothiocyanate preparations and compound agents thereof on root-knot nematodes
And (3) carrying out indoor biological activity determination on the root-knot nematode by using different isothiocyanate single agents by using a dryer in-vitro fumigation method. Taking out twenty-four hole plates under microscope with bottom light source after fumigating at 24h,48h and 72h respectively, wherein the number of nematode in each visual field is about 200, observing and recording the death condition of nematode.
Different isothiocyanates are prepared by separation as above, acetone is used for preparing different concentrations, the primary screening of the biological activity of the root-knot nematode is carried out, and 10 treatments are arranged in the test:
(1) 30 μ g/mL allyl isothiocyanate;
(2) 30 μ g/mL benzyl isothiocyanate;
(3) 1-phenylethyl isothiocyanate at 30 μ g/mL;
(4) 2-phenylethyl isothiocyanate at 30 μ g/mL;
(5) 30 μ g/mL of p-trifluoromethylphenyl isothiocyanate;
(6) 30 μ g/mL allyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(7) 30 μ g/mL benzyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(8) 30 μ g/mL 1-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(9) 30 μ g/mL 2-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(10) 30 μ g/mL p-trifluoromethylphenyl isothiocyanate +5 μ g/mL fluopyram (6:1);
TABLE 6 Fumigation Activity of different isothiocyanate mono-and combinations on Meloidogyne incognita
Treatment of 24h mortality (%) 48h mortality (%) Mortality rate (%) at 72h
1 97.5 98.9 99.1
2 24.99 31.27 57.48
3 22.28 30.18 50.5
4 35.46 42.14 48.12
5 32.13 43.55 49.33
6 98.6 99.4 100
7 43.26 65.43 87.37
8 46.57 61.05 84.23
9 66.65 75.63 85.16
10 62.78 74.56 84.44
As shown in the results of the above Table 6, the fumigation effect of allyl isothiocyanate for 72h reached 99.1% at 30. Mu.g/mL in the same concentration treatment. Most aromatic isothiocyanates have a lower fumigant activity than aliphatic isothiocyanates. The biological activity of the compound preparation is obviously higher than that of a single preparation, and the using amount of the isothiocyanic acid can be obviously reduced.
Experimental example 6: respectively testing the indoor biological activity of the isothiocyanate preparation, the fluopyram preparation and the compound agent thereof on the meloidogyne, and setting 11 treatment groups in total in the test;
(1) 30 μ g/mL allyl isothiocyanate;
(2) 30 μ g/mL benzyl isothiocyanate;
(3) 30 μ g/mL 1-phenylethyl isothiocyanate;
(4) 2-phenylethyl isothiocyanate at 30 μ g/mL;
(5) 30 μ g/mL of p-trifluoromethylphenyl isothiocyanate;
(6) 5 mug/mL fluopyram;
(7) 30 μ g/mL allyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(8) 30 μ g/mL benzyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(9) 30 μ g/mL 1-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(10) 30 μ g/mL 2-phenylethyl isothiocyanate +5 μ g/mL fluopyram (6:1);
(11) 30 μ g/mL p-trifluoromethylphenyl isothiocyanate +5 μ g/mL fluopyram (6:1);
TABLE 7 indoor bioactivity of different isothiocyanate single and compound preparations on Meloidogyne incognita
Treatment of 24h corrected mortality (%) 48h corrected mortality (%)
1 11.27 15.54
2 37.75 44.38
3 17.56 28.24
4 33.64 43.36
5 25.13 32.23
6 38.77 59.6
7 41.55 61.73
8 64.41 88.84
9 53.19 73.36
10 62.28 84.55
11 52.78 69.65
A24-hole disc method is used for preparing a drug-containing suspension with a certain concentration, prepared second-instar larvae are added, the mortality of the nematodes is observed and counted after 24 hours and 48 hours, and preliminary screening results show that the activity is improved along with the extension of carbon chains. And on the whole, the activity of the aromatic isothiocyanate contact killing activity is higher than that of aliphatic isothiocyanate, especially the activity of benzyl and 2-phenylethyl isothiocyanate is higher than that of allyl isothiocyanate by more than 25%, fluopyram also has certain contact killing activity, when the concentration of fluopyram is 5 mu g/mL, the control effects of 24h and 48h on meloidogyne incognita are respectively 38.77% and 59.6%, the biological activity of the compound agent is obviously higher than that of a single agent, and the using amount of the isothiocyanate can be obviously reduced.
Experimental example 7: determination of indoor combined toxicity of fluopyram and benzyl isothiocyanate composition on meloidogyne incognita
The fluopyram and benzyl isothiocyanate obtained in the above way are respectively combined according to different proportions, acetone is used for preparing different concentrations, the biological activity of the second instar larvae of the meloidogyne incognita is compounded and screened, the formula Sun Yun Pectine is used for calculating the synergistic coefficient (the calculation formula is the same as the above), and the result is shown in table 8.
TABLE 8 indoor bioactivity of benzyl isothiocyanate and fluopyram compounded preparation on Meloidogyne incognita
Treatment of EC50(µg/mL) CTC
BITC 6.35 -
Fluopyram (F) 11.7 -
B:F 1:1 7.7 106.91
B:F 1:2 5.6 163.12
B:F 1:4 7.3 137.16
B:F 1:9 10 107.91
B:F 9:1 5.1 130.48
B:F 4:1 3.1 225.46
B:F 2:1 5.9 126.98
B:F 6:1 2.5 271.75
B:F 1:6 7 149.19
Note: in the table, "B" represents BITC (benzyl isothiocyanate) and "F" represents fluopyram.
The results in Table 8 show that the combination of benzyl isothiocyanate and fluopyram in a weight ratio of 9/1 to 4/1 has a certain synergistic effect on Meloidogyne incognita, especially when the weight ratio of benzyl isothiocyanate to fluopyram is 6:1,the CTC value of the meloidogyne incognita is 271.75, the synergistic effect is obvious, and the EC is 50 The value decreases significantly.
Experimental example 8: determination of indoor combined toxicity of fluopyram, benzyl isothiocyanate and p-trifluoromethylphenyl isothiocyanate composition on meloidogyne incognita
Benzyl isothiocyanate, p-trifluoromethylphenyl isothiocyanate and fluopyram which are prepared by separation according to the method are combined according to the proportion in the table, acetone is used for preparing different concentrations, and the results of the compound screening of the biological activity of the second-instar larvae of the meloidogyne incognita are shown in the table 9.
TABLE 9 indoor bioactivity of two isothiocyanates and fluopyram compounded preparations on Meloidogyne incognita
Treatment of EC50(µg/mL)
Benzyl isothiocyanate: fluopyram =6:1 3.45
Benzyl isothiocyanate: fluopyram =1:6 6.77
P-trifluoromethylphenyl isothiocyanate: fluopyram =6:1 6.25
P-trifluoromethylphenyl isothiocyanate: fluopyram =1:6 6.04
The results in Table 9 show that the combination of two different isothiocyanates and fluopyram in combination has a synergistic effect on the meloidogyne incognita species tested, especially on the meloidogyne incognita EC at a weight ratio of benzylisothiocyanate to fluopyram of 6:1 50 The value is lowest, and is only 3.45 mug/mL.
Experimental example 9: potting test of AITC and fluopyram compounded preparation on Meloidogyne incognita
The soil collected from a cultivated layer (the depth is about 0-15 cm) of a tomato field with serious root knot nematode disease in Shandong Anqiu vegetable planting bases is subjected to heat preservation and moisture preservation, and tomato diseased roots infected with the root knot nematode disease are buried and rotten in the soil. After a period of time, the soil contains a large number of tomato root knot nematode larvae. The soil (absolute water content about 20%) was then mixed well and loaded into pots, 2kg per pot. Then, the following concentration gradient was followed: 10. 50 and 125 mu L/kg (weight ratio of effective components to soil), respectively burying the compound preparation in a position of about 5cm in a basin, and pouring a small amount of clear water. And finally, sealing the pot and the sand which are applied with the pesticide for 7 days by using a polyvinyl chloride plastic film, and transplanting the tomato seedlings and sowing the cucumber seeds which just bud into the flowerpot after opening for 4 days. Meanwhile, 5% of abamectin B2 microcapsule suspending agent with the concentration of 40mg/kg is used as medicament control and treatment without any medicament is used as blank control, each treatment is repeated for 4 times, and the abamectin B2 microcapsule suspending agent is cultivated under the same water and fertilizer management condition. The results were counted two months later and the results are as follows.
TABLE 10 potted plant test results of AITC and Fluopyram formulations for Meloidogyne incognita
Treatment of Concentration (μ L/kg) Average control effect (%)
CK - -
Drug controls 40(mg/kg) 35.88
AITC 10 38.54
50 66.69
125 87.56
Fluopyram (F) 10 31.29
50 53.21
125 75.66
A:F 1:1 10 42.56
50 66.55
125 83.06
A:F 9:1 10 53.65
50 73.49
125 82.13
A:F 6:1 10 59.43
50 78.96
125 95.64
A:F 1:6 10 43.60
50 64.18
125 82.99
A:F 1:9 10 41.29
50 65.22
125 87.33
Note: in the table, "a" represents AITC (allyl isothiocyanate), "F" represents fluopyram, and the control agent is 5% avermectin B2 microcapsule suspension.
From the results, the control effects of the single agents of AITC and the fluopyram respectively reach 66 percent and 53 percent when the single agents of AITC and the fluopyram are treated by 50 mu L/kg, and the control effect can reach 59 percent when the weight ratio of the compound agents of allyl isothiocyanate to the fluopyram is 6:1 and is 10 mu L/kg, so that the control effect of the AITC is obviously improved, and the using amount of the AITC is reduced.
Example 1 production of 15% Allyl Isothiocyanate (AITC) and 5% fluopyram composition oil agent bacitracin a
8 kg of AITC raw drug accounting for 94 percent is weighed accurately and quantitatively, and 2.6 kg of fluopyram raw drug accounting for 96 percent is weighed. Mixing the two active components in 2M 3 Mixing in blending tank. Accurately weighing 1 kg of ascorbic acid, putting the ascorbic acid into the blending tank (1) and fully mixing the ascorbic acid and the ascorbic acid again. Then 19.2 kg of sec-butyl acetate and 19.2 kg of vegetable oil are accurately put into the blending tank and are fully and uniformly mixed in the blending tank. Stirring was continued for 1 hour. Preparing an oil product of the 50KG AITC and fluopyram composition.
The sample analysis shows that the content of AITC is 15 percent and the content of fluopyram is 4.99 percent. And (3) subpackaging the product into aluminum cans coated with barrier materials, wherein each can contains 5 kg of the product, and the total amount of the product is 10 cans. Sealing the opening of the tank, and labeling to obtain the composition product, namely the bacterial line athomin A oil solution product with the content of 20%.
Example 2 production of 10% benzyl isothiocyanate and 10% Fluopyram composition soluble liquor bacitracin B
250 kg of 20% benzyl isothiocyanate extraction mother liquor and 52 kg of 96% fluopyram technical are accurately and quantitatively weighed. Mixing the two active medicinal liquids in blending tank (1). Then 18 kg of ascorbic acid is accurately weighed and put into the blending tank (1) to be fully and uniformly mixed again. Adding 10 kg of emulsifier 602 and 10 kg of emulsifier OP-10 kg into the blending tank (2), mixing, adding 120 kg of ethyl acetate, and fully and uniformly mixing. Transferring all the kilogram materials in the blending tank (2) into the blending tank (1) through a pipeline, sealing the opening of the tank, and starting the stirrer to stir for 1 hour. 500 kg of benzyl isothiocyanate soluble liquid product is prepared. The content of benzyl isothiocyanate in the product is analyzed by sampling to be 10 percent, the content of fluopyram is 9.98 percent, and the product is 20 percent of the product of the mycorrhizal horse radish seed B, and the product is subpackaged into double-barrier plastic bottles, wherein each bottle contains 500mL of the medicine.
EXAMPLE 3:2% Fluopyramide and 12% 1-phenylethylisothiocyanate composition in Water emulsion production of mycorrhizal horse radish hormone C
20.8 kg of 96% fluopyram raw material, 133.5 kg of 90% 1-phenylethyl isothiocyanate raw material and 20 kg of ascorbic acid are accurately weighed and fully and uniformly stirred in a blending tank. Then, 100 kg of agricultural emulsifier Well201, 180 kg of ethyl acetate and 180 kg of vegetable oil are quantitatively added into a blending tank, 365.7 kg of water is added while stirring is carried out, and after all the materials are added, the stirring is carried out for 1 hour by a stirrer. The amount of fluopyram in the product for sampling and assay was 1.99%, the content of 1-phenylethyl isothiocyanate was 12%, and 1 ton of the product with the total content of active ingredients of 14% was finally obtained, and the product was sealed with a 500mL glass bottle opening as in example 1.
EXAMPLE 4:3% Fluopyramide and 6% 2-phenylethylisothiocyanate composition soluble liquor line Arthrocidin D production
62.5 kg of 96% fluopyram raw pesticide and 133.5 kg of raw pesticide with the content of 2-phenylethyl isothiocyanate of 90% are accurately and quantitatively weighed. Mixing the two active medicinal liquids in blending tank (1). Then 30 kg of ascorbic acid is accurately weighed and put into the blending tank (1) to be fully and uniformly mixed again. 100 kg of agricultural emulsion No. 500 and 300 kg of emulsifier 602 are added into a blending tank (2), and 1374 kg of ethyl acetate is added after mixing, and the mixture is fully and uniformly mixed. 1774 kg of materials in the blending tank (2) are all transferred into the blending tank (1) through a pipeline, and the stirrer is started to stir for 1 hour after the opening of the tank is sealed. 2000 kg of 2-phenylethyl isothiocyanate and fluopyram soluble liquid product is prepared. And (3) sampling and analyzing the content of fluopyram in the product to be 3 percent and the content of 2-phenylethyl isothiocyanate to be 6 percent to obtain a 9 percent mycorrhizal-killing-horse radish hormone D product, and subpackaging the product into double-barrier plastic bottles, wherein each bottle contains 500mL of medicine.
Example 5:8% Fluopyram and 8% para-trifluoromethylphenyl isothiocyanate composition soluble concentrate Arthrocidin E production
266.7 kg of 15 percent p-trifluoromethyl phenyl isothiocyanate extraction mother liquor and 41.7 kg of raw pesticide with 96 percent fluopyram content are accurately and quantitatively weighed. Mixing the two active medicinal liquids in blending tank (1). Then accurately weighing 15 kg of ascorbic acid, and putting the ascorbic acid into the blending tank (1) to be fully and uniformly mixed again. 10 kg of agricultural emulsion 602 and 50kg of emulsifier OP-10 kg are added into the blending tank (2), and then 116.6 kg of ethyl acetate are added after mixing, and the mixture is fully and uniformly mixed. Transferring all kilogram materials in the blending tank (2) into the blending tank (1) through a pipeline, sealing the opening of the tank, and starting a stirrer to stir for 1 hour. 500 kg of p-trifluoromethylphenyl isothiocyanate soluble liquid product is obtained through preparation. The content of the p-trifluoromethylphenyl isothiocyanate in the product is 8 percent and the content of the fluopyram in the product is 8 percent through sampling analysis, namely the 16 percent of the product of the bacitracin I is killed by the bacteria thread, and the product is subpackaged into double-barrier plastic bottles, wherein each bottle is filled with 500mL of the medicine.
EXAMPLE 6:2% Fluopyram and 10% allyl isothiocyanate composition microemulsion Linesquirolicide F production
200 kg of 25% allyl isothiocyanate extraction mother liquor and 10.5 kg of raw pesticide with 96% fluopyram content are accurately and quantitatively weighed. Mixing the two active medicinal liquids in blending tank (1). Then 5 kg of ascorbic acid is accurately weighed and put into the blending tank (1) to be fully and uniformly mixed again. 20 kg of agricultural emulsion 602 and 80 kg of emulsifier OP-10 kg are added into a blending tank (2), 184.5 kg of ethyl acetate is added after mixing, and the mixture is fully and uniformly mixed. Transferring all the kilogram materials in the blending tank (2) into the blending tank (1) through a pipeline, sealing the opening of the tank, and starting the stirrer to stir for 1 hour. 500 kg of allyl isothiocyanate soluble liquid product is prepared. The content of allyl isothiocyanate in the product is analyzed by sampling to be 10 percent, the content of fluopyram is 2 percent, and the product is the 12 percent of the mycorrhizal horse radish seed F product, and the product is subpackaged into double-barrier plastic bottles, wherein each bottle contains 500mL of the medicine.
Example 7:
selecting a field block for planting cucumbers all year round in Shanxi Weinan vegetable base, seriously harming the cucumber root-knot nematodes for a long time, dividing the field block into cells with the same size, wherein the area of each cell is 30m 2 Randomly arranging, opening the same size of holes, irrigating roots in each hole by using the holes, using 5% avermectin B2 microcapsule suspending agent (Hebei Xingbai biological pharmaceutical industry Co., ltd.) as a contrast agent, and using 10% horseradish extract missible oil (10% horseradish extract +10% concentrated milk 500+80% sec-butyl acetate) and 20% bacteria as a treatment group agentAnd diluting the line-killing-athomin A oil agent by 2000 times respectively, performing hole application by 250ml, and counting results after two months, wherein the control group, the 10% athomin (allyl isothiocyanate) missible oil and the 20% line-killing-athomin A oil agent have the control effects of 44%, 67% and 85% respectively.
Example 8:
selecting a field with serious root-knot nematode infection of water spinach in Shandong Shuguang vegetable test base, dividing the field into cells with the same size, and randomly arranging the cells, wherein the area of each cell is 50m 2 Directly pouring water, coating film, fumigating soil for 7 days, and transplanting seedlings at intervals of 14 days. The control agent is 20% fosthiazate water emulsion (Jiangsu Huifeng biological agriculture GmbH), the treatment group agents are 13% athomin (allyl isothiocyanate) missible oil (13% athomin +10% condensed milk 500+3% TX-10+74% sec-butyl acetate) and 20% mycorrhizin B soluble liquid, the treatment agents are respectively diluted by 1200 times, the dosage per square meter of each treatment is 15g, the root knot number per gram of roots is counted after two months, and the control effects are respectively 51%, 79% and 88%.
Example 9:
in the Changyang high mountain vegetable base in Hubei, a field with serious clubroot infection is selected and divided into three districts, and the area of each district is 100m 2 . A ditching and pesticide applying mode is adopted, ditches are arranged at intervals of 0.6m, three processing modes of 14% aqueous emulsion microbial inoculum rodenticide C produced in example 3, 20% horseradish oil (20% horseradish, 50% ethyl acetate, 20% ethyl formate) and clear water are adopted, the agents are 14%, the ditches are filled by diluting the agents by 1200 times, the using amount of each ditch is 10L, soil is covered, then a thick film is paved, the ditches are sealed for seven days, then the ditches are opened for four days, and Chinese cabbages are planted. The treatment and management measures after sowing are the same. And (5) checking the clubroot condition in the harvest season of the Chinese cabbages. The control was 97%, the 14% line-killed-athomin C-treated group had an infection rate of 9% and the single-dose-treated-athomin (1-phenylethyl isothiocyanate) had an infection rate of 25%.
Example 10:
soil is filled with the sagger with serious watermelon blight, and 6 kg of soil is filled in each sagger. 60 sagger bodies are built, wherein the sagger body 30 is filled with clear water 250mL as a blank, and the blank sagger body is tightly wrapped by a double layer of a nylon film bag. Then, the 20% soluble solution prepared in example 2 was diluted 1200 times with bacitracin B, and 250mL of the diluted solution was poured per sagger, followed by soil covering. Tightly and tightly wrapping each sagger with nylon bags according to a wrapping method of wrapping blank as soon as possible, sealing for 7 days, removing the wrapped film, and opening for 7 days. Then transplanting tomato seedlings, two plants per almus bowl. And (5) allowing the melon seedlings to grow for 45 days under the same management condition. The blank control shows that 56 melon seedlings die from 60 melon seedlings, only 2 melon seedlings die from 60 melon seedlings on the soil treated by the pesticide, and the control effect reaches 96%.
Example 11:
the soil blocks infected by the cruciferae soft rot are uniformly mixed and put into flowerpots, and each flowerpot is 2kg. Then, the 9% soluble liquid agent produced in example 4 was diluted 300 times with the colistin D, 300ml of the diluted drug was applied to each pot, the pot was buried in about 5cm, a small amount of clear water was poured, the pot and sand to which the drug was applied were sealed with a polyvinyl chloride plastic film for 7 days, and after 4 days of opening, chinese cabbage seeds were sown in a flowerpot with a blank and a treatment group of 240 seeds. Statistics of the emergence rate after half a month, the control had little survival. The mortality rate of the drug-treated group was only 12.3%.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (6)

1. An isothiocyanate and fluopyram composition, wherein the composition comprises:
the weight ratio of the isothiocyanate to the fluopyram is (1-9): (1-6);
the isothiocyanate is selected from benzyl isothiocyanate and 2-phenylethyl isothiocyanate.
2. An isothiocyanate and fluopyram formulation comprising the isothiocyanate and fluopyram composition of claim 1.
3. The isothiocyanate and fluopyram formulation of claim 2, wherein said formulation is an aqueous emulsion;
the aqueous emulsion comprises the following components in percentage by weight:
1 to 40 percent of isothiocyanate,
0.25 to 10 percent of fluopyram,
12 to 28 percent of emulsifier,
0.1 to 2 percent of ascorbic acid,
10 to 30 percent of solvent,
supplementing water to 100%;
wherein the emulsifier is No. 500, 602, OP-10, well201, TX-10, well205 or M30; the solvent is ethyl acetate, sec-butyl acetate or vegetable oil.
4. The isothiocyanate and fluopyram formulation of claim 2, wherein said formulation is a soluble liquor;
the soluble liquid comprises the following components in percentage by weight:
1 to 60 percent of isothiocyanate,
0.2 to 20 percent of fluopyram,
12 to 60 percent of emulsifier,
1 to 8 percent of ascorbic acid,
the solvent is replenished to 100 percent;
wherein the emulsifier is No. 500, 602, OP-10, well201, well205 or M30; the solvent is ethyl acetate, sec-butyl acetate or turpentine.
5. Use of the isothiocyanate and fluopyram composition of claim 1 in the preparation of a fumigant for the control of soil-borne pathogens and/or soil nematodes.
6. Use of a formulation of isothiocyanate and fluopyram according to any one of claims 2 to 4 for the preparation of a fumigant for the control of soil-borne pathogens and/or soil nematodes.
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