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CN115918661B - Cyclobutrifluram-containing nematicidal composition and application thereof - Google Patents

Cyclobutrifluram-containing nematicidal composition and application thereof Download PDF

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CN115918661B
CN115918661B CN202310022535.8A CN202310022535A CN115918661B CN 115918661 B CN115918661 B CN 115918661B CN 202310022535 A CN202310022535 A CN 202310022535A CN 115918661 B CN115918661 B CN 115918661B
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active ingredient
cyclobutrifluram
nematodes
mass ratio
test
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CN115918661A (en
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葛尧伦
刘桂娟
杨志鹏
刘金玲
隋书婷
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Qingdao Hailier Biotechnology Co ltd
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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
    • 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
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P5/00—Nematocides
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Life Sciences & Earth Sciences (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Plant Pathology (AREA)
  • Environmental Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a nematicidal composition containing Cyclobutrifluram and application thereof, wherein the composition comprises an active ingredient A and an active ingredient B, the active ingredient A is Cyclobutrifluram, the active ingredient B is any one of trifloxystrobin, isoflucypram or Phosphocarb, and the mass ratio of the active ingredient A to the active ingredient B is 1:36-36:1. The nematicide composition can improve the actual control effect, effectively slow down the generation of drug resistance of target pests and reduce the occurrence of soil-borne diseases.

Description

Cyclobutrifluram-containing nematicidal composition and application thereof
The invention relates to a nematicidal composition containing Cyclobutrifluram and application thereof, which are respectively applied for the application number CN202210081714.4, the application date 2022, the month 01 and the day 24.
Technical Field
The invention belongs to the technical field of pesticide compounding, and particularly relates to a nematicide composition containing Cyclobutrifluram and application thereof.
Background
Nematode disease is a plant disease caused by plant parasitic nematode attack and parasitism. The victim plant can influence normal growth and development due to the invasion of the nematode to absorb nutrition in the body; secretions from the metabolic processes of nematodes also stimulate cells and tissues of the host plant, resulting in plant malformations, reduced yields and quality of agricultural products. The plant nematode diseases which are serious in China are root knot nematode diseases, soybean cyst nematode diseases, wheat kernel nematode diseases, sweet potato stem nematode diseases, rice stem nematode diseases, maize nematode diseases, pine wood nematode diseases, citrus half-penetration nematode diseases and the like of various crops such as peanuts.
Cyclobutrifluram is a novel nicotinamide class of bactericidal nematicide developed by zhengda corporation. Chemical name: n- [2- (2, 4-dichlorophenyl) cyclobutyl ] -2- (trifluoromethyl) nicotinamide comprising 80% to 100% of the (1 s,2 s) -enantiomer and 0% to 20% of the (1 r,2 r) -enantiomer; CAS accession number: 1460292-16-3; the molecular formula: c 17H13CI2F3N2 O. Cyclobutrifluram has broad control spectrum, high efficiency, small dosage and easy use, can effectively control various nematodes and main fungal diseases, has high efficiency on root knot nematodes, beet cyst nematodes, corn short body nematodes and the like on crops such as cucumber, tomato, corn, beet, and the like, can treat soil or seeds, and can control the nematodes and diseases in main crops and various environments for a long time.
Trifloxystrobin, international generic name: trifluenfuronate, chemical name: 3, 4-trifluoro-but-3-en-1-yl 2- (2-methoxyphenyl) -5-oxoy-lidene tetrahydrofuran-3-carboxylate; CAS number: 2074661-82-6; the molecular formula: c 16H15F3O5; the trifloxystrobin has the advantages of low toxicity, high safety, long lasting period and good application and development prospect.
Isoflucypram, a pyrazole carboxamide fungicide developed by bayer crop science, inc., chemical name: n- [ [ 5-chloro-2- (1-methylethyl) phenyl ] methyl ] -N-cyclopropyl-3- (difluoromethyl) -5-fluoro-1-methyl-1H-pyrazole-4-carboxamide, CAS accession No.: 1255734-28-1.
Isoflucypram belongs to SDHI bactericides and has excellent efficacy on main leaf diseases such as leaf spot, net blotch, stripe rust, leaf rust and the like.
Phosphocarb CAS accession number 126069-54-3, belonging to the class of organophosphorus nematicides, chemical name: [2- [ ethoxy (propylthio) phosphoryl ] oxyphenyl ] N-methylcarbamate.
The pesticide containing single active component has the defects of different degrees in preventing and controlling crop diseases and insect pests, and is easy to generate drug resistance after continuous use, and the problems of narrow insecticidal spectrum, environmental pollution and the like occur. The applicant experiment shows that Isoflucypram has a certain control effect on nematodes, and Cyclobutrifluram with different action mechanisms is mixed with trifloxystrobin, isoflucypram or Phosphocarb, so that the pesticide composition has a good control effect on crop nematode diseases, is environment-friendly and has low toxicity to people and livestock.
Disclosure of Invention
The invention aims to provide a nematicide composition with higher activity on plant parasitic nematodes, which can improve the actual control effect, effectively slow down the generation of drug resistance of target pests and reduce the occurrence of soil-borne diseases.
In order to achieve the above purpose, the present invention is realized by the following technical scheme: a nematicidal composition containing Cyclobutrifluram comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is Cyclobutrifluram, the active ingredient B is any one of trifloxystrobin and Isoflucypram, phosphocarb, and the mass ratio of the active ingredient A to the active ingredient B is 1:36-36:1.
Further, the active ingredient B is trifloxystrobin, and the mass ratio of the active ingredient A to the active ingredient B is 1:19-19:1;
further, the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:12-12:1;
Further, the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:12, 1:6, 1:2, 1:1, 2:1, 3:1, 4:1, 6:1, 7:1, 12:1;
Further, the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:6-4:1;
Further, the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:6, 1:2, 1:1, 2:1, 3:1, 4:1;
further, the active component B is Isoflucypram, and the mass ratio of the active component A to the active component B is 1:30-30:1;
Further, the mass ratio of Cyclobutrifluram to Isoflucypram is 1:5-5:1;
further, the mass ratio of Cyclobutrifluram to Isoflucypram is 1:5, 2:3, 1:2, 1:1, 2:1, 3:2, 5:1;
further, the active component B is Phosphocarb, and the mass ratio of the active component A to the active component B is 1:12-20:1;
further, the mass ratio of Cyclobutrifluram to Phosphocarb is 1:9-6:1;
Further, the mass ratio of Cyclobutrifluram to Phosphocarb is 1:9, 1:6, 1:4, 1:1, 4:1, 6:1;
Further, the total weight of the active ingredient A and the active ingredient B accounts for 0.1% -80% of the composition;
further, the total weight of the active ingredient A and the active ingredient B accounts for 0.1% -60% of the composition;
Further, the nematicidal composition comprises an agriculturally acceptable auxiliary ingredient in addition to the active ingredient, wherein the auxiliary ingredient is selected from one or more of wetting agents, dispersing agents, thickening agents, disintegrating agents, emulsifying agents, antifoaming agents, preservatives, stabilizers, synergists and carriers;
Further, the wetting agent is selected from one or more of sodium dodecyl benzene sulfate, sodium dodecyl benzene sulfonate, spina gleditsiae powder, alkyl sulfate, nekal BX, silkworm excrement, alkylphenol ethoxylates, fatty alcohol ethoxylates, alkanolamide ethoxylates and phosphate or sulfate salt thereof, and alkyl polyoxyethylene ether succinate sulfonate;
The dispersing agent is selected from one or more of polycarboxylate, lignosulfonate, naphthalene or alkyl naphthalene formaldehyde condensate sulfonate, calcium alkyl benzene sulfonate, alkylphenol polyoxyethylene phosphate, fatty alcohol polyoxyethylene polyoxypropylene ether, fatty alcohol polyoxypropylene ether and polymeric alkylaryl sulfonate;
The emulsifier is selected from one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester;
The thickener is selected from one or more of xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate and carboxymethyl cellulose;
the disintegrating agent is selected from one or more of aluminum chloride, bentonite, sucrose, modified starch, cellulose, urea, sodium carbonate, sodium bicarbonate, sodium chloride, sodium sulfate, citric acid and tartaric acid;
the antifreezing agent is selected from one or a mixture of more of alcohols, alcohol ethers and inorganic salts;
The defoaming agent is selected from one or a mixture of more of silicone oil, C 10～C20 saturated fatty acid compounds, C 8～C10 fatty alcohol compounds or silicone compounds;
The solvent is selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, N-butanol, diesel oil, N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, solvent oil, vegetable oil derivatives and deionized water;
The preservative is selected from one or a mixture of more of sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium parahydroxybenzoate and methyl parahydroxybenzoate;
The stabilizer is selected from one or a mixture of more of oxalic acid, succinic acid, adipic acid, borax and epoxidized vegetable oil;
the warning color is selected from any one or more of red, yellow, blue, green and purple regulating colors;
The film forming agent is one or more selected from sodium carboxymethyl starch, cellulose derivatives (sodium carboxymethyl cellulose, sodium alginate and polyvinyl alcohol) and polyacrylic acid;
the carrier is selected from one or a mixture of more of kaolin, bentonite, attapulgite, light calcium carbonate, diatomite and white carbon black;
Further, the composition can be prepared into any agriculturally acceptable preparation formulation, including any one of powder, wettable powder, microcapsule suspending agent, water dispersible granule, soluble tablet, soluble powder, dispersible oil suspending agent, emulsifiable concentrate, aqueous emulsion, suspending agent, suspoemulsion, soluble solution, microemulsion and seed treatment suspending agent;
further, the preparation formulation is any one of granules, aqueous emulsion and seed treatment suspending agent.
The invention also discloses the use of the Cyclobutrifluram-containing nematicidal composition and/or formulations thereof as described above for controlling plant parasitic pests;
further, the plant parasitic pest is a plant parasitic nematode;
further, the plant parasitic nematodes are any one or more of root-knot nematodes (Meloidogyne), cyst nematodes (Heterodera), aphelenchus xylophilus (APHELENCHINA), stem nematodes (Ditylenchus), root-knot nematodes (Nacobbus), root-rot nematodes (Pratylenchus) and pine nematodes (Bursa phelenchus xylophilus);
further, the plant parasitism is root knot nematode (Meloidogyne), cyst nematode (Heterodera);
Further, the root-knot nematode is southern root-knot nematode [ Meloidogyne incongnita (Kofold & White) Chitwood ]; the cyst nematode is soybean cyst nematode (Heterodera glycinea).
Compared with the prior art, the invention has the following advantages:
1) The composition selects medicaments with different mechanisms for compound use, improves the control effect, reduces the application cost and delays the generation of drug resistance of pests, and provides a new solution for the efficient control of nematodes.
2) The composition has lower toxicity, less residue in crops and soil, and effectively reduces environmental pollution and medicament residue.
Detailed Description
In order to better illustrate the effective control effect of the present invention, the technical solution, purpose and advantages of the present invention are more clearly understood by using the above-described agent of examples, but the present invention is not limited to these examples. The effect experiment of the invention adopts a mode of combining in-house biological measurement and field test.
Formulation preparation examples:
Preparation example preparation process:
1. The preparation process of the seed treatment suspending agent comprises the following steps: and (3) cutting, shearing, mixing and stirring the raw materials, the auxiliary agent and the water according to the proportion, and sanding for 2.5 hours by a sanding machine to ensure that the average particle size reaches 1-5 microns, thus obtaining the seed coating suspending agent.
2. The preparation process of the granule comprises the following steps: the preparation method comprises the steps of adopting a coating granulation method, crushing and mixing raw materials, dispersing agents and auxiliary agents uniformly to prepare mother powder, adding the mother powder and a carrier into a coating granulator together, stirring, adding a prepared aqueous solution of a binder while stirring, fully and uniformly mixing, discharging, drying and sieving to obtain the granule.
3. The preparation process of the aqueous emulsion comprises the following steps: mixing surfactant, antifreezing agent, density regulator and water into water phase, dissolving the original medicinal solvent, adding into the water phase under stirring, adding thickener and antiseptic, shearing for 10min, adding defoamer, and stirring to obtain O/W type water emulsion.
Preparation example 1:15% Cyclobutrifluram. Trifloxalate seed treatment suspension (1:2)
Preparation example 2:12% Cyclokutrifluram Isoflucypram seed treatment suspension (1:1)
Preparation example 3:8% Cyclobutrifluram trifloxystrobin granules (1:1)
Component (A) Content of
Cyclobutrifluram 4％
Trifloxystrobin 4％
Polycarboxylic acid sodium salt 3％
Potassium humate 5％
White carbon black 10％
Carboxymethyl cellulose 3％
Diatomite particles Make up for the allowance
Preparation example 4:6% Cyclokutrifluram Isoflucypram granules (1:2)
Preparation example 5:12% Cyclokutrifluram Phosphocarb granules (1:1)
Component (A) Content of
Cyclobutrifluram 6％
Phosphocarb 6％
Sodium lignin sulfonate 5％
Sodium alginate 3％
Attapulgite particles Make up for the allowance
Preparation example 6:10% Cyclokutrifluram Phosphocarb aqueous emulsion (4:1)
Component (A) Content of
Cyclobutrifluram 8％
Phosphocarb 2％
EO-PO block copolymers 6％
Cyclohexanone 20％
Xanthan gum 0.2％
Propylene glycol 3％
Urea 3％
Sodium benzoate 0.5％
Organosilicon defoamer 0.2％
Deionized water Make up for the allowance
Preparation example 7:15% Cyclokutrifluram Isoflucypram aqueous emulsion (2:1)
Component (A) Content of
Cyclobutrifluram 10％
Isoflucypram 5％
Alkylphenol polyoxyethylene 3％
Polyoxyethylene sorbitan monooleate 3％
Cyclohexanone 25％
Xanthan gum 0.2％
Ethylene glycol 3％
Urea 3％
Sorbic acid sodium salt 0.5％
Organosilicon defoamer 0.5％
Deionized water Make up for the allowance
Preparation example 8:12% Cyclobutrifluram trifloxystrobin aqueous emulsion (3:1)
Component (A) Content of
Cyclobutrifluram 9％
Trifloxystrobin 3％
Styrylphenol polyoxyethylene ether phosphate 1％
EO-PO block copolymers 6％
Cyclohexanone 22％
Xanthan gum 0.2％
Glycerol 5％
Urea 3％
Sorbic acid sodium salt 0.5％
Organosilicon defoamer 0.5％
Deionized water Make up for the allowance
Indoor bioassay test
Example 1: combined toxicity test of Cyclobutrifluram and trifloxystrobin or Isoflucypram on soybean cyst nematode
Test subject: soybean cyst nematode (Heterodera glycinea) is collected from soybean test fields with serious group morbidity, the collected disease soil is used for separating cysts by a floating method, fresh and mature cysts are picked up under a dissecting mirror, and the cysts are stored at the temperature of 4 ℃ for standby.
Test agent: 90% of the cyclob (r) fluram crude drug, 94.2% of the isof (r) fluroxypram crude drug and 98% of the trifloxystrobin crude drug are all provided by the group development center.
And (3) preparation of a medicament: the raw materials are dissolved by acetone and then diluted by 0.1% Tween-80 aqueous solution. Each agent was set up with 5 series of concentration gradients, with the same solvent content in aqueous solution without agent as a control.
Preparation of nematode suspension: the sterilized cysts are placed in a sterilized hatching pond for hatching, sterilized water is used as hatching liquid, and the sterilized water is suitable for slightly overflowing the cysts. Hatching is carried out under the dark condition of a 25 ℃ incubator, and two-instar larvae with consistent instar are obtained to prepare nematode suspension, wherein each 1mL of suspension contains at least 100 nematodes for standby.
The test method comprises the following steps: sequentially sucking 3mL of liquid medicine from low concentration to high concentration by a pipette, respectively adding the liquid medicine into a test tube, and then sucking 3mL of prepared equivalent nematode suspension into the test tube, so that the liquid medicine and the nematode suspension are uniformly mixed in equivalent. And (3) transferring a certain volume of the mixed solution into the small holes of the porous biochemical test plate by using a pipetting gun, capping, repeating the treatment for 4 times, and taking an aqueous solution which does not contain a medicament and has the same solvent content as a control. Culturing at 25 ℃ for 24 hours, checking the activity condition of nematodes, and calculating the relative mortality rate of each medicament treatment to the nematodes.
Experimental investigation: 1mL of the mixed solution is taken from each treatment, the death condition of the nematodes is observed under a dissecting mirror, and the number of the nematodes observed repeatedly is not less than 100. The total number of nematodes investigated and the number of dead nematodes were recorded. Dead nematodes are often stiff and cannot flex by touching with hairpins or bamboo pins.
The calculation method comprises the following steps:
According to the investigation data, the mortality of each treatment is calculated, the calculation is carried out according to the following formula, and the calculation results are reserved to two positions after decimal points:
if the control mortality is less than 5%, correction is not needed; if the control mortality is between 5% and 15%, correcting according to a correction mortality formula; control mortality was greater than 15% and the test required reworking.
Statistical analysis: and (3) according to the concentration log values of each medicament and the corresponding mortality, analyzing by using an IBM SPSS STATISTICS statistical analysis system, obtaining a virulence regression line, an LC 50 value and a correlation coefficient R 2, and evaluating the activity of the test medicament on the biological test material.
Co-toxicity coefficient (CTC) of the blends was calculated according to the grand cloud Pei method and the type of combined effect was evaluated.
CTC.gtoreq.120 shows synergistic effect, CTC.gtoreq.80 shows antagonistic effect, CTC between 80 and 120 shows additive effect.
The co-toxicity coefficient (CTC value) of the blend was calculated as follows:
Wherein:
ati—actual measured virulence index of the mixture;
S-LC 50 of standard insecticide in milligrams per liter (mg/L);
M-LC 50 of the mix in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A A agent toxicity index;
The percentage content of the P A -A medicament in the mixture is expressed as percentage (%);
TI B -agent toxicity index;
the percentage of the P B -B medicament in the mixture is expressed as percentage (%).
Wherein:
Ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The test results are shown in the following table.
Table 1 Cyclobutrifluram results of combined toxicity test of the combination of trifloxystrobin and the soybean cyst nematode
Test agent and ratio Regression equation Correlation coefficient R 2 LC50(mg/L) Co-toxicity coefficient
Clclobutrifluram(A) y＝1.166x-0.703 0.996 4.007 -
Trifluoro line killing ester (B) y＝1.816x-2.618 0.996 27.634 -
A:B＝1:36 y＝1.594x-2.028 0.989 18.731 127.252
A:B＝1:19 y＝1.629x-1.964 0.989 16.052 132.955
A:B＝1:12 y＝1.799x-1.934 0.989 11.878 160.053
A:B＝1:6 y＝1.904x-1.746 0.982 8.265 181.480
A:B＝1:2 y＝1.381x-0.921 0.997 4.644 200.658
A:B＝1:1 y＝1.337x-0.745 0.994 3.606 194.096
A:B＝2:1 y＝1.525x-0.741 0.994 3.061 183.084
A:B＝6:1 y＝1.836x-0.821 0.995 2.800 163.019
A:B＝12:1 y＝1.576x-0.763 0.995 3.049 140.672
A:B＝19:1 y＝1.136x-0.575 0.994 3.206 130.566
A:B＝36:1 y＝1.593x-0.825 0.999 3.296 124.447
As can be seen from Table 1, cyclobutrifluram and triflumuron are mixed in a mass ratio of 1:36-36:1, the soybean cyst nematode is well controlled, and the combined effect is synergistic; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:12-6:1, the co-toxicity coefficient is more than 160, and the synergistic effect is outstanding; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:6-2:1, the co-toxicity coefficient is more than 180, and the synergistic effect is obvious; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:2, the co-toxicity coefficient is 200.658 at maximum, which shows that the compound of Cyclobutrifluram and trifloxystrobin has the best activity on soybean cyst nematodes.
Tables 2 Cyclobutrifluram and Isoflucypram combined toxicity test results for soybean cyst nematode
Test agent and ratio Regression equation Correlation coefficient R 2 LC50(mg/L) Co-toxicity coefficient
Clclobutrifluram(A) y＝1.509x-0.920 0.993 4.071 -
Isoflucypram(B) y＝1.729x-1.615 0.990 8.592 -
A:B＝1:16 y＝1.673x-1.313 0.993 6.094 132.346
A:B＝1:9 y＝1.563x-1.128 0.997 5.267 146.824
A:B＝1:5 y＝1.797x-1.105 0.998 4.121 175.930
A:B＝2:3 y＝1.784x-0.868 0.994 3.066 194.040
A:B＝1:1 y＝1.762x-0.849 0.981 3.032 182.205
A:B＝3:2 y＝1.604x-0.740 0.985 2.893 178.232
A:B＝5:1 y＝1.639x-0.822 0.980 3.174 140.590
A:B＝9:1 y＝1.254x-0.645 0.990 3.269 131.450
A:B＝16:1 y＝1.384x-0.720 0.996 3.313 126.804
As can be seen from Table 2, cyclobutrifluram and Isoflucypram have better control effect on soybean cyst nematode at a mass ratio of 1:16-16:1, and the combined effect is shown as synergy; when the mass ratio of Cyclobutrifluram to Isoflucypram is 1:9-5:1, the co-toxicity coefficient is greater than 140, and the synergy is remarkable; when the mass ratio of Cyclobutrifluram to Isoflucypram is 1:5-3:2, the co-toxicity coefficient is more than 170, and the synergistic effect is outstanding; when the mass ratio of Cyclobutrifluram to Isoflucypram is 2:3, the co-toxicity coefficient is 194.040 at maximum, which indicates that the compound of Cyclobutrifluram and Isoflucypram has the best activity on the soybean cyst nematode at the mass ratio.
Example 2: combined toxicity test of Cyclobutrifluram and trifloxystrobin or Isoflucypram or phosphocarb on meloidogyne incognita
The test is based on: test reference NY/T1833.1-2009 section 1 of standard nematicide for in-house bioassay tests for pesticides: test of insect dipping method for inhibiting plant pathogenic nematodes.
Test subject: southern root knot nematode [ Meloidogyne incongnita (Kofold & White) Chitwood ] was isolated from tomato root knot samples from the greenhouse of the Qingdao city, i.e., the Shimadzu, and grown and propagated on living tomato plants in the laboratory.
Test agent: 90% of cyclob technical, 94.2% of Isoflucypram technical, 98% of trifloxystrobin technical and 92% of phosphocarb technical, all of which are provided by the group development center.
And (3) preparation of a medicament: the raw materials are dissolved by acetone and then diluted by 0.1% Tween-80 aqueous solution. Each agent was set up with 5 series of concentration gradients, with the same amount of solvent in water without agent being used as a control.
Preparation of nematode suspension: the method comprises the steps of picking root knot nematode egg masses from tomato root knots with serious root knot nematode disease, cleaning with clear water, placing the root knot nematode egg masses on filter paper in a culture dish, adding a proper amount of distilled water, placing the filter paper in a culture box at 25+/-1 ℃ for incubation and culture, collecting second-instar larvae with consistent instar after 24 hours, and preparing root knot nematode suspension, wherein each 1mL of suspension contains at least 100 nematodes for standby.
The test method comprises the following steps: sequentially sucking 3mL of liquid medicine from low concentration to high concentration by a pipette, respectively adding the liquid medicine into a test tube, and then sucking 3mL of prepared equivalent nematode suspension into the test tube, so that the liquid medicine and the nematode suspension are uniformly mixed in equivalent. And (3) transferring a certain volume of the mixed solution into the small holes of the porous biochemical test plate by using a liquid transferring gun, covering, repeating the treatment for 4 times, and taking the solvent aqueous solution which does not contain the same content of the medicament as a control. Culturing at 25 ℃ for 24 hours, checking the activity condition of nematodes, and calculating the relative mortality rate of each medicament treatment to the nematodes.
Experimental investigation: 1mL of the mixed solution is taken from each treatment, the death condition of the nematodes is observed under a dissecting mirror, and the number of the nematodes observed repeatedly is not less than 100. The total number of nematodes investigated and the number of dead nematodes were recorded. Dead nematodes are often stiff and cannot flex by touching with hairpins or bamboo pins.
The calculation method comprises the following steps:
According to the investigation data, the mortality of each treatment is calculated, the calculation is carried out according to the following formula, and the calculation results are reserved to two positions after decimal points:
if the control mortality is less than 5%, correction is not needed; if the control mortality is between 5% and 15%, correcting according to a correction mortality formula; control mortality was greater than 15% and the test required reworking.
Statistical analysis: and (3) according to the concentration log values of each medicament and the corresponding mortality, analyzing by using an IBM SPSS STATISTICS statistical analysis system, obtaining a virulence regression line, an LC 50 value and a correlation coefficient R 2, and evaluating the activity of the test medicament on the biological test material.
Co-toxicity coefficient (CTC) of the blends was calculated according to the grand cloud Pei method and the type of combined effect was evaluated.
CTC.gtoreq.120 shows synergistic effect, CTC.gtoreq.80 shows antagonistic effect, CTC between 80 and 120 shows additive effect.
The co-toxicity coefficient (CTC value) of the blend was calculated as follows:
Wherein:
ati—actual measured virulence index of the mixture;
S-LC 50 of standard insecticide in milligrams per liter (mg/L);
M-LC 50 of the mix in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A A agent toxicity index;
The percentage content of the P A -A medicament in the mixture is expressed as percentage (%);
TI B -agent toxicity index;
the percentage of the P B -B medicament in the mixture is expressed as percentage (%).
Wherein:
Ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The test results are shown in the following table.
TABLE 3 determination of combined toxicity test results of the combination of Cyclobutrifluram and trifloxystrobin on Meloidogyne incorporable to Meloidogyne incorporable article
As can be seen from the table 3, cyclobutrifluram and triflumuron are used for controlling the meloidogyne incognita when the mass ratio of the triflumuron to the nematicide is 1:19-12:1, and the combined effect is shown as synergy; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:12-7:1, the co-toxicity coefficient is more than 140, and the synergy is obvious; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:6-4:1, the co-toxicity coefficient is more than 170, and the synergistic effect is outstanding; when the mass ratio of Cyclobutrifluram to trifloxystrobin is 3:1, the co-toxicity coefficient is 208.881 at maximum, which shows that the compound of Cyclobutrifluram and trifloxystrobin has the best activity on the meloidogyne incognita at the mass ratio.
Tables 4 Cyclobutrifluram and Isoflucypram were combined to determine the results of the combined toxicity test for meloidogyne incognita
Test agent and ratio Regression equation Correlation coefficient R 2 LC50(mg/L) Co-toxicity coefficient
Clclobutrifluram(A) y＝1.507x-0.621 0.992 2.583 -
Isoflucypram(B) y＝1.402x-0.982 0.993 5.019 -
A:B＝1:30 y＝1.782x-1.082 0.987 4.047 120.356
A:B＝1:20 y＝1.67x-0.873 0.999 3.333 144.113
A:B＝1:10 y＝1.704x-0.811 0.997 2.992 154.501
A:B＝1:5 y＝1.980x-0.831 0.995 2.629 164.978
A:B＝1:2 y＝2.027x-0.659 0.998 2.114 180.633
A:B＝1:1 y＝1.957x-0.438 0.986 1.674 203.746
A:B＝2:1 y＝1.857x-0.394 0.998 1.630 189.052
A:B＝5:1 y＝1.829x-0.433 0.990 1.725 162.918
A:B＝10:1 y＝1.797x-0.499 0.985 1.895 142.598
A:B＝20:1 y＝1.717x-0.507 0.990 1.974 133.947
A:B＝30:1 y＝1.683x-0.534 0.988 2.076 126.401
As can be seen from the table 4, cyclobutrifluram and Isoflucypram have better control effect on the meloidogyne incognita when the mass ratio is 1:30-30:1, and the combined effect is shown as synergy; when the mass ratio of Cyclobutrifluram to Isoflucypram is 1:20-10:1, the co-toxicity coefficient is greater than 140, and the synergy is remarkable; when the mass ratio of Cyclobutrifluram to Isoflucypram is 1:5-5:1, the co-toxicity coefficient is more than 160, and the synergistic effect is outstanding; when the mass ratio of Cyclobutrifluram to Isoflucypram is 1:1, the co-toxicity coefficient is 203.746 at maximum, which indicates that the compound of Cyclobutrifluram and Isoflucypram has the best activity on the meloidogyne incognita at the mass ratio.
Tables 5 Cyclobutrifluram and Phosphocarb Combined toxicity test results for Calodendron
Test agent and ratio Regression equation Correlation coefficient R 2 LC50(mg/L) Co-toxicity coefficient
Clclobutrifluram(A) y＝1.981x-0.794 0.997 2.516 -
Phosphocarb(B) y＝1.759x-2.093 0.997 15.479 -
A:B＝1:15 y＝1.902x-1.938 0.993 10.441 112.141
A:B＝1:12 y＝1.608x-1.518 0.999 8.787 126.158
A:B＝1:9 y＝1.486x-1.188 0.995 6.304 162.050
A:B＝1:6 y＝1.477x-1.069 0.986 5.292 168.487
A:B＝1:4 y＝1.254x-0.788 0.989 4.250 179.375
A:B＝1:1 y＝1.418x-0.519 0.998 2.323 186.330
A:B＝4:1 y＝1.315x-0.272 0.983 1.610 187.714
A:B＝6:1 y＝1.481x-0.378 0.989 1.800 158.773
A:B＝9:1 y＝1.447x-0.427 0.997 1.973 139.177
A:B＝15:1 y＝1.316x-0.404 0.995 2.028 130.915
A:B＝20:1 y＝1.390x-0.453 0.998 2.118 123.725
As can be seen from the table 5, cyclobutrifluram and Phosphocarb have better control effect on the meloidogyne incognita when the mass ratio is 1:12-20:1, and the combined effect is shown as synergy; when the mass ratio of Cyclobutrifluram to Phosphocarb is 1:9-6:1, the co-toxicity coefficient is more than 150, and the synergy is remarkable; when the mass ratio of Cyclobutrifluram to Phosphocarb is 1:4-4:1, the co-toxicity coefficient is more than 170, and the synergistic effect is outstanding; when the mass ratio of Cyclobutrifluram to Phosphocarb is 4:1, the co-toxicity coefficient is 187.714 at maximum, which indicates that the compound of Cyclobutrifluram and Phosphocarb has the best activity on the meloidogyne incognita at the mass ratio.
Field efficacy test
Example 3: cyclobutrifluram field efficacy test of combination with trifloxystrobin or Isoflucypram on soybean cyst nematode
The test is based on: the test refers to GB/T17980.37-2000 "pesticide field efficacy test guidelines (one) nematicide for controlling cyst nematodes".
Test site: the soil property of the test soil is sandy loam, the fertility is good, the soybean is planted for many years continuously, and the soybean cyst nematode disease is serious.
Test crops and varieties: spring soybean, the variety is Mongolian soybean 3. Soybeans were sown 5 months and 9 days in 2019, and harvested 9 months and 30 days.
And (3) medicament treatment: seed dressing treatment is carried out by using a seed treatment suspending agent, and sowing is carried out after drying in the shade. The test agents and the dosage are shown in Table 6.
And (3) test design: the test was set up with a total of 6 treatments, the test cells were arranged in random groups, 15m 2 per cell area, and each treatment was repeated 4 times.
The investigation method comprises the following steps: soil samples are collected by an earth auger before test and after soybean harvesting, 5 points of each district are sampled, 20cm 3 soil is collected at each point, after uniform mixing, the survival number of nematodes is measured by a water bleaching method, and the average value (the number of living nematodes/20 cm 3) of each point is taken. And calculating the control effect according to the nematode population changes before and after treatment.
Investigation of soybean growth and yield: and (3) sampling at random 5 points in each cell in the soybean harvesting period, digging soybean plants 4 plants at each point, keeping the root system intact, respectively measuring the individual plant height and the individual plant root length of the soybean after rinsing the root system with clear water, and recording the average value. And measuring the yield of the soybeans. The test results are shown in Table 7.
The cyst reduction rate and the control effect were calculated according to the following formula:
Table 6 Cyclobutrifluram results of field efficacy test on soybean cyst nematodes in combination with trifloxystrobin or Isoflucypram
As can be seen from the results of the field test in the table, cyclobutrifluram and the trifloxystrobin or Isoflucypram are compounded to have good control effect on the soybean cyst nematodes.
Table 7 Cyclobutrifluram results of experiments on Soybean growth Effect in combination with trifloxystrobin or Isoflucypram
From the above table, cyclobutrifluram and trifloxystrobin are compounded, and Cyclobutrifluram and Isoflucypram are compounded, so that soybean cyst nematodes can be effectively prevented and treated, the growth of soybean plants is obviously promoted, and the growth and yield of each treated soybean are increased along with the increase of seed dressing dosage.
Example 4: field efficacy test of each nematicidal composition for preventing and controlling tomato root-knot nematode
Field efficacy test
Test object: tomato root knot nematode; the isolation and identification prove that the plant is mainly the southern root-knot nematode [ Meloidogyne incongnita (Kofold & White) Chitwood ].
Test site: in tomato greenhouses in Yuyang county in Jiangsu province, the test areas are cultivated in protected areas, the damage of tomato root knot nematodes is serious in the past, the yield is reduced to a certain extent, the cultivation conditions of each area are uniform and consistent, and the method accords with the local conventional cultivation practice.
Test crops and varieties: tomato (Haovist).
Test agent: the test agents and the dosage of the preparations are shown in Table 8.
And (3) test design: the test cells were arranged in random groups with a cell area of 20m 2 and each treatment was repeated 4 times. When tomato is transplanted, planted and grown, the pesticide is applied for 1 time (10 months and 6 days in 2020), root irrigation and pesticide application are adopted, water is added for root irrigation, and the water consumption of each plant is 200mL.
The investigation method comprises the following steps: the efficacy of the tomato is investigated once before seedling pulling (day 3 and 10 of 2021), 2 plants are taken at each point according to a 5-point sampling method, roots are dug out, the disease grade is investigated, and the morbidity, the disease index and the prevention and treatment effect are calculated.
The disease classification method comprises the following steps:
Level 0: the root system has no insect gall;
stage 1: the root system has a small amount of insect gall;
3 stages: two thirds of the lines are covered with small insect gall;
5 stages: the root system is covered with small insect gall and has secondary insect gall;
7 stages: the root system forms fibrous root clusters.
The drug effect calculation method comprises the following steps:
The test results are shown in Table 8:
table 8 results of field efficacy test of nematicidal compositions against tomato root knot nematodes
As can be seen from Table 8, the nematicidal compositions with different proportions have good control effects on tomato root knot nematodes, wherein the control effects of each preparation example on tomato root knot nematodes are higher than 83%.
In conclusion, through indoor toxicity measurement and field efficacy tests, the nematicidal composition has good control effect on nematodes, is safe to target crops, has remarkable control effect, is superior to a single dose in the aspects of delaying the generation of drug resistance and prolonging the lasting effect, and can effectively reduce the production cost and the use cost.

Claims (8)

1. The application of the Cyclobutrifluram-containing nematicidal composition for preventing and controlling plant parasitic nematodes is characterized in that the nematicidal composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is Cyclobutrifluram, the active ingredient B is trifluoracetate, the mass ratio of the active ingredient A to the active ingredient B is 1:36-36:1, and the nematodes are cyst nematodes (Heterodera).
2. The nematicidal composition of claim 1 wherein the mass ratio of Cyclobutrifluram to trifloxystrobin is from 1:19 to 19:1.
3. The use according to claim 2, wherein the mass ratio of Cyclobutrifluram to trifloxystrobin is 1:12 to 12:1.
4. The use according to claim 1, wherein the total weight of active ingredient a and active ingredient B is between 0.1% and 80% of the composition.
5. The use according to claim 1, wherein the total weight of active ingredient a and active ingredient B is between 0.1% and 60% of the composition.
6. The use according to claim 1, wherein the composition comprises, in addition to the active ingredient, agriculturally acceptable auxiliary ingredients selected from one or more of wetting agents, dispersants, thickeners, disintegrants, emulsifiers, anti-freeze agents, defoamers, preservatives, stabilizers, synergists, warning colors, film formers, carriers.
7. The use of claim 1, wherein the composition is formulated into any agriculturally acceptable formulation, including any of wettable powders, microcapsule suspensions, water dispersible granules, soluble tablets, soluble powders, dispersible oil suspensions, emulsifiable concentrates, aqueous emulsions, suspensions, suspoemulsions, soluble solutions, microemulsions, seed treatment suspensions.
8. The use according to claim 7, wherein the formulation is any one of granules, aqueous emulsion, seed treatment suspension.
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