CN112493245A - Synergistic bactericidal composition - Google Patents

Synergistic bactericidal composition Download PDF

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Publication number
CN112493245A
CN112493245A CN202011482015.8A CN202011482015A CN112493245A CN 112493245 A CN112493245 A CN 112493245A CN 202011482015 A CN202011482015 A CN 202011482015A CN 112493245 A CN112493245 A CN 112493245A
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active ingredient
bactericidal composition
pyraclostrobin
iflufenoquin
test
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葛家成
巨翠红
杨志鹏
吕文东
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Qingdao Hailier Biotechnology Co ltd
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Qingdao Hailier Biotechnology Co ltd
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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
    • 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
    • A01N43/42Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
    • 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
    • A01N47/08Biocides, 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 one or more single bonds to nitrogen atoms
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof

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

Abstract

The bactericidal composition contains an active ingredient A of Iflufenoquin and an active ingredient B of pyraclostrobin. The weight ratio of the active ingredient A to the active ingredient B is 1: 50-50: 1. The total weight of the active component A and the active component B is 1 to 90 percent, preferably 5 to 80 percent, and the composition can be prepared into agriculturally allowable dosage forms. The invention has reasonable components and good bactericidal effect, and the activity and the bactericidal effect of the invention are not simple superposition of single components, compared with single agent, the invention has obvious bactericidal effect and good safety to crops.

Description

Synergistic bactericidal composition
Technical Field
The invention relates to an active compound composition, in particular to a binary bactericidal composition which comprises active compounds Iflufenoquin and pyraclostrobin. The present invention relates to a method for the therapeutic or prophylactic or eradicative control of plant diseases.
Background
Iflufenoquin is a quinoline bactericide developed by Nippon Caoda company, has a development code NF-180 and a structural formula as follows:
Figure BDA0002838420260000011
chemical name: 2- [ (7, 8-difluoro-2-methyl-3-quinolinyl) oxy ] -6-fluoro- α, α -dimethylbenzyl alcohol, CAS registry number 1314008-27-9. The compound is a broad-spectrum bactericide, is effective to various diseases, has a novel action mechanism, and can be used for preventing and treating pathogenic bacteria generating resistance to the existing medicaments.
Pyraclostrobin is strobilurin bactericide developed by BASF, belongs to mitochondrial respiration inhibitor, and can prevent mitochondria from generating and providing energy required by normal metabolism of cells by preventing electron transfer of cytochrome bcl complex, thereby finally causing cell death. Pyraclostrobin has strong capability of inhibiting germ spore germination, has good inhibition effect on hypha growth in leaves, has long lasting period, and has potential therapeutic activity. Pyraclostrobin has the advantages of protective effect, therapeutic effect, systemic conductivity and rain erosion resistance, has a wide application range, and is widely used for preventing and controlling various diseases of more than 100 crops at present. Pyraclostrobin can induce physiological change of many crops, especially grains, besides direct action on pathogenic bacteria, and can enhance activity of nitrate (nitrification) reductase, thereby improving nitrogen absorption of crops in a rapid growth stage; meanwhile, the compound can reduce the biosynthesis of ethylene, thereby delaying the crop senescence; when the plant is attacked by virus, it can accelerate the formation of resistin, and the synthesis of resistin is the same as that of salicylic acid compound in plant. Pyraclostrobin can improve crop yield by controlling secondary disease and relieving stress from abiotic factors even in the absence of disease in plants.
A method for preparing Ipflufenoquin from commercially available materials and its use as a bactericide is disclosed in WO 2011081174. Mixtures of Ipflufenoquin and a bactericide are disclosed in WO2013047441, and although the patent discloses that Ipflufenoquin can be compounded with QoI bactericides, no disclosure is made as to the biological activity of the compositions of the present invention.
Disclosure of Invention
The invention aims to provide a bactericidal composition which has reasonable components, obvious synergistic effect, good bactericidal effect, low medication cost, difficult generation of drug resistance and safety to crops and a preparation formulation thereof.
The invention also aims to provide application of the composition in preventing and treating apple ring spot and potato early blight.
In order to overcome the defects of the existing single preparation, the technical scheme of the invention is as follows: a synergistic bactericidal composition comprises an active ingredient A, an active ingredient B and an auxiliary ingredient of a pesticide preparation, wherein the active ingredient A is Iflufenoquin, and the active ingredient B is pyraclostrobin.
Further, the weight ratio of the active ingredient A to the active ingredient B is 1: 50-50: 1;
further, the weight ratio of the active ingredient A to the active ingredient B is 1: 5-5: 1;
further, the weight ratio of the active ingredient A to the active ingredient B is 1: 5-3: 1;
further, the weight ratio of the active ingredient A to the active ingredient B is 1: 5-2: 1.
Further, the pesticide preparation auxiliary component comprises one or more of fillers, carriers, emulsifiers, dispersing agents, wetting agents, spreading agents, solvents, sticking agents, stabilizing agents, synergists and defoaming agents.
The total content of the active component A and the active component B is 1 to 90 percent of the total weight of the composition, and preferably 5 to 80 percent.
The components of the synergistic fungicidal compositions of the present invention may be applied separately or as part of other pesticidal compositions.
The synergistic bactericidal composition can be prepared into agriculturally acceptable dosage forms according to a method known by persons in the technical field, and the preferred dosage forms are water dispersible granules, wettable powder and suspending agents.
Further, the water dispersible granule comprises one or more of a synergistic bactericidal composition, a wetting agent, a dispersing agent, a stabilizing agent, a synergist or a carrier. Wherein, the content of the synergistic bactericidal composition accounts for 5 to 90 percent of the total mixture, and more preferably 10 to 75 percent;
further, the wettable powder comprises a synergistic bactericidal composition, a filler, a dispersing agent and a wetting agent. Wherein, the content of the synergistic bactericidal composition accounts for 5 to 90 percent of the total mixture, and more preferably 10 to 75 percent;
further, the suspending agent comprises a synergistic bactericidal composition, a carrier, a dispersing agent, a wetting agent, a thickening agent and an antifoaming agent. Wherein the content of the synergistic bactericidal composition accounts for 5-70 percent of the total mixture, and more preferably 10-60 percent.
The active ingredient A is prepared by the inventor according to the preparation method of example 25 in the specification of the patent WO 2011081174; the active ingredient B and other pesticide auxiliary ingredients are commercially available products.
The invention has reasonable combination and good sterilization effect, can reduce the times of drug administration, slow down the occurrence of drug resistance of diseases, has treatment and protection effects on crops, has obvious synergistic effect instead of simple superposition of all components in the activity and the sterilization effect, has good safety on crops and meets the safety requirement of pesticide preparations. The invention has better control effect on apple ring spot and potato early blight.
Detailed Description
In order to prevent and treat apple ring rot and potato early blight in agricultural production, the inventor uses an active ingredient A and an active ingredient B to carry out mutual compounding synergistic research, and the specific method comprises the following steps:
example 1: the synergistic bactericidal composition can be used for preventing and treating apple ring spot.
Test targets: apple ring rot pathogen (Botryosphaeria berengiana). The bacteria source is taken from a garden of a water-collecting street, north village and Fucun in the Lai West city of Qingdao. And (4) carrying out separation culture on an indoor PDA culture medium to obtain pure apple ring rot germ hyphae.
The culture conditions are as follows: the test was carried out in a biological incubator at a temperature of 25. + -. 0.5 ℃.
Test agents: 92% Ipfufenoquin technical material
93.5% pyraclostrobin original drug
Preparation and dosage of the medicament:
dissolving Iflufenoquin and pyraclostrobin in DMF to obtain 100mg/L mother solution, and mixing the mother solution with active ingredients at a ratio of 5:1, 3:1, 2:1, 1:2, 1:3 and 1:5 (Iflufenoquin: pyraclostrobin) to obtain a mixed mother solution. The solution was diluted with a 0.1% aqueous solution of Tween 80 to the following concentrations (unit: mg/L). See table 1:
table 1 blending ratios and test concentrations
Figure BDA0002838420260000031
Medicament treatment: under the aseptic operation condition, quantitatively adding the pre-melted sterile culture medium into an aseptic conical flask, quantitatively sucking liquid medicine from low concentration to high concentration in sequence, respectively adding into the conical flasks, and fully shaking up. Then, the mixture was poured into a petri dish having a diameter of 9cm in equal amount to prepare a drug-containing plate having a corresponding concentration. And (5) solidifying for later use. The test was run with no agent treatment as a blank, 4 replicates.
Inoculation and culture: cutting the cultured ring rot of apple with a sterilizing puncher with diameter of 0.6cm under aseptic condition to obtain bacterial cake from the edge of bacterial colony, inoculating the strain with inoculator in the center of the medicated plate with the hypha facing upwards, covering with a dish cover, and culturing in incubator at proper temperature.
Data investigation and statistical analysis:
the investigation method comprises the following steps: at 72 hours after inoculation, the diameter of each colony was measured perpendicularly by the cross method, and the average value was calculated as the percentage inhibition, which is calculated as follows:
percent (%) inhibition was [1- (diameter of colony in treatment area-diameter of cake)/(diameter of colony in control area-diameter of cake) ] × 100
The statistical analysis method comprises the following steps: the effective concentration EC of each drug was determined by using the logarithmic value of the drug concentration (mg/L) as the independent variable (X) and the probability value of the percentage inhibition as the dependent variable (Y)50Co-toxicity coefficient (CTC).
CTC < 80 is antagonistic; 80 or more and 120 or less of CTC is an addition effect; CTC > 120 is synergistic.
The test results are as follows:
TABLE 2 Iflufenoquin and pyraclostrobin for preventing and treating apple ring rot indoor activity
Figure BDA0002838420260000032
Results and analysis: and establishing a regression equation by taking the logarithmic value of the medicament concentration (mg/L) as an independent variable (X) and the probability value of the germ inhibition percentage as a dependent variable (Y), and calculating the co-toxicity coefficient. The measurement result shows that the co-toxicity coefficients of the compound of Iflufenoquin and pyraclostrobin are 102.83, 135.68, 151.94, 259.19, 160.93, 122.58 and 121.57, respectively, the co-toxicity coefficients of the compound of Iflufenoquin and pyraclostrobin are 102.83, 3:1, 2:1, 1:2, 1:3 and 1:5 are higher than 120, wherein the highest co-toxicity coefficient of the compound of 1:1 shows that the compound of Iflufenoquin and pyraclostrobin has good combined action under the above proportion.
Example 2 prevention and treatment of early blight of potato by the synergistic fungicidal composition.
Test targets: early blight of potato (Alternaria solani). The bacterial source is obtained from the water-collecting street of Beizhuang potato field of the Lexi city of Qingdao. Separating, identifying, and storing at 4 deg.C.
The culture conditions are as follows: the test was carried out in a biological incubator at a temperature of 25. + -. 0.5 ℃.
Test agents: 92% Ipfufenoquin technical material
93.5% pyraclostrobin original drug
Setting a medicament: dissolving pyraclostrobin and Iflufenoquin in analytically pure dimethylformamide to prepare 100mg/L mother liquor, and then preparing the mother liquor according to the active ingredients Iflufenoquin: the pyraclostrobin is mixed into mixed mother liquor according to the ratio of 5:1, 3:1, 2:1, 1:2, 1:3 and 1:5, and when the mixed mother liquor is used, the mixed mother liquor is diluted into 0.05, 0.1, 0.2, 0.4 and 0.8mg/L by using a 0.1% Tween 80 aqueous solution. The measured concentrations of Iflufenoquin are 0.0125, 0.025, 0.05, 0.01 and 0.02mg/L, and the measured concentrations of pyraclostrobin are 0.05, 0.1, 0.2, 0.4 and 0.8 mg/L. No drug plate control was set.
The test was repeated: each concentration treatment was repeated 4 times.
The test method comprises the following steps: a hypha growth rate method is adopted. Inoculating the prepared mycelia on culture medium plates with different concentrations of medicinal agents, culturing at 25 deg.C for 8 days, examining colony diameter, and calculating the percentage of each medicinal agent for inhibiting hypha growth. The EC of each drug was determined by linear regression analysis between the probability of inhibition and the logarithm of the drug concentration50And calculating the CTC.
CTC < 80 is antagonistic; 80 or more and 120 or less of CTC is an addition effect; CTC > 120 is synergistic.
Data investigation and statistical analysis
Inhibition rate calculation formula: percent (%) inhibition was [1- (diameter of colony in treatment area-diameter of cake)/(diameter of colony in control area-diameter of cake) ] × 100
TABLE 3 Iflufenoquin and pyraclostrobin indoor Activity for controlling Potato early blight
Figure BDA0002838420260000041
Results and analysis: and establishing a regression equation by taking the logarithmic value of the medicament concentration (mg/L) as an independent variable (X) and the probability value of the germ inhibition percentage as a dependent variable (Y), and calculating the co-toxicity coefficient. The determination result shows that the co-toxicity coefficients of the compound of Iflufenoquin and the pyraclostrobin are respectively 80.27, 96.57, 139.40, 166.65, 183.11, 165.52 and 149.77 when the compound of Iflufenoquin and the pyraclostrobin is in a ratio of 5:1, 3:1, 2:1, 1:2, 1:3 and 1:5 are in a ratio of 1:5, wherein the co-toxicity coefficients of the compound of 1:2 are the highest, and the co-toxicity coefficients of 1:1, 1:3, 1:5 and 2:1 are all higher than 120, and the compound of Iflufenoquin and the pyraclostrobin have synergistic combined effects in the ratio.
Example 3: field efficacy test for preventing and treating apple ring rot by synergistic bactericidal composition
Test subjects, crops and varieties: the target of prevention and treatment is apple ring spot, and the pathogen is (Botryosphaeria berengiana). The test tree is a golden crown variety of 10-year-old apples, and the variety is very easy to infect ring rot of apple trees.
The experiment is carried out in the village of the water collection street in the Lai xi city of Qingdao. The experimental garden has good management conditions, moderate tree vigor and 3m multiplied by 5m of plant row spacing.
Test agents: 20% of Iflufenoquin pyraclostrobin suspending agent (1:1), 15% of Iflufenoquin pyraclostrobin suspending agent (1:2), 15% of Iflufenoquin pyraclostrobin water dispersible granule (2:1) and 16% of Iflufenoquin pyraclostrobin wettable powder (3: 1).
Control agents: 250g/L pyraclostrobin missible oil and a blank control.
Dosage and treatment number of medicament:
TABLE 4 test design of test agents
Figure BDA0002838420260000051
Cell area and repetition: each 2 trees was a test cell, each cell had an area of 30 square meters, and each treatment was repeated 4 times.
The application method comprises the following steps: spraying on the whole tree, and applying the medicine for 3 times in the young fruit period of 5 months and 20 days, 6 months and 15 days, and 6 months and 30 days.
Investigation time and number of times: the pre-harvest survey was conducted on day 9, 26, and the post-storage survey was conducted on day 10, 11 and 26, 3 times in total.
The drug effect calculation method comprises the following steps:
disease fruit rate (%) (number of diseased fruits/total number of investigated fruits) × 100
Control effect (%) [ (blank control disease fruit rate-treatment disease fruit rate)/blank control disease fruit rate ] × 100
Results and analysis:
TABLE 5 results of the efficacy test in each treatment field
Figure BDA0002838420260000052
Experiments in 2019 prove that the mixture of Iflufenoquin and pyraclostrobin has a good prevention and treatment effect on apple ring spot when the dosage of the effective ingredients is 500mg/kg, is safe, does not cause phytotoxicity, and has no adverse effect on beneficial organisms. The control effect after each treatment and storage is higher than that of the control medicament.
Example 4: synergistic bactericidal composition field efficacy test for preventing and treating potato early blight
Test targets: potato early blight (Alternaria solani).
Test site: the water collection street in the Lai xi city of Qingdao city is named as Beizhuang Fucun.
Test agent and serial number
TABLE 6 test design of test agents
Figure BDA0002838420260000061
Cell area and repetition: the area of the cell is 20 square meters, and the times of repetition are 4 times.
The application method comprises the following steps: the stem and leaf of the plant are evenly sprayed.
Time and frequency of application: the medicine is applied for 3 times in 6 months, 8 days, 15 days and 22 days in 2019.
The investigation method comprises the following steps: the disease condition base before the first time of medicine application is investigated before the medicine application is carried out for 8 days in 6 months, the control effect investigation is carried out for 7 days after the last time of medicine application, the investigation is carried out for 2 times in total, and the water consumption per mu is 15L.
Sampling 5 points in each cell, investigating 3 plants at each point, investigating all compound leaves by each plant, and dividing disease grades according to the percentage of the lesion area on each compound leaf to the whole compound leaf area:
level 0: no disease;
level 1: the lesion area accounts for less than 5 percent of the whole compound leaf area;
and 3, level: the lesion area accounts for 6 to 10 percent of the whole compound leaf area;
and 5, stage: the lesion area accounts for 11 to 20 percent of the whole compound leaf area;
and 7, stage: the lesion area accounts for 21 to 50 percent of the whole compound leaf area;
and 9, stage: the lesion area accounts for more than 51 percent of the whole compound leaf area.
The drug effect calculation method comprises the following steps:
disease index ∑ (number of diseased leaves at each stage × number of relative stages)/(total number of investigated leaves × 9) × 100
Control effect (%) - (1- (CK)0×PT1)/(CK1×PT0)]×100
In the formula: CK (CK)0、CK1Disease indexes before and after drug application in the blank control area respectively;
PT0、PT1the disease indexes before and after drug application are respectively treated.
Test results and analysis:
TABLE 7 field drug effect of synergistic fungicidal composition for controlling potato early blight
Figure BDA0002838420260000062
Figure BDA0002838420260000071
Test results show that under the condition of the same effective component dosage, the mixture of Iflufenoquin and pyraclostrobin has good control effect on potato early blight, and the control effect is 85.98%, 79.32%, 78.59%, 74.53% and 73.96% after the last dose is taken for 7 days. Control dose was scaled to 70.52%.
Direct impact on crops:
through field irregular observation during the test period, no adverse effect of the test agent on the growth and development of the potatoes in the test dose range is found.

Claims (9)

1. A synergistic bactericidal composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is Iflufenoquin, and the active ingredient B is pyraclostrobin.
2. The bactericidal composition according to claim 1, wherein the weight ratio of the active ingredient A to the active ingredient B is 1: 50-50: 1.
3. The bactericidal composition according to claim 1, wherein the weight ratio of the active ingredient A to the active ingredient B is 1: 5-5: 1.
4. The bactericidal composition according to claim 1, wherein the weight ratio of the active ingredient A to the active ingredient B is 1: 5-2: 1.
5. The bactericidal composition according to claim 1, wherein the total content of the active ingredient a and the active ingredient B is 1% to 90%, preferably 5% to 80% of the total weight of the composition.
6. Use of the fungicidal composition according to any one of claims 1 to 5 for controlling plant diseases.
7. The bactericidal composition of claim 6, wherein the plant is a fruit tree or a vegetable.
8. The bactericidal composition of claim 6, wherein the fruit tree is apple, and the vegetable is potato; the plant diseases comprise ring spot and early blight.
9. The bactericidal composition according to claim 6, wherein the plant diseases are apple ring rot and potato early blight.
CN202011482015.8A 2020-12-16 2020-12-16 Synergistic bactericidal composition Pending CN112493245A (en)

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Application publication date: 20210316