CN110800750A - Pesticide bactericidal composition and preparation thereof - Google Patents
Pesticide bactericidal composition and preparation thereof Download PDFInfo
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- CN110800750A CN110800750A CN201911131548.9A CN201911131548A CN110800750A CN 110800750 A CN110800750 A CN 110800750A CN 201911131548 A CN201911131548 A CN 201911131548A CN 110800750 A CN110800750 A CN 110800750A
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Classifications
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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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- 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
- A01N43/42—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
Abstract
The invention discloses a pesticide sterilization composition and a preparation thereof, wherein the pesticide sterilization composition comprises 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thioketone and 2-cyclopentyl-4-p-toluidine quinoline according to the mass ratio of (1-5) to (1-5).
Description
Technical Field
The invention relates to the technical field of pesticide compound sterilization, in particular to a pesticide sterilization composition and a preparation thereof.
Background
Among the crop infectious diseases, there are two main fungal diseases and bacterial diseases, wherein the fungal diseases account for about 80% of the diseases. Because the fungal diseases and the bacterial diseases have different origins, the control method and the medicament use are also different.
Bacterial wilt is a devastating soil-borne disease widely distributed around the world, pseudomonas solanacearum (Ralstonia solanacearum) is the root cause of the disease, pseudomonas solanacearum invades a xylem duct from the root of a host plant, and rapidly expands to the overground part of the plant through a vascular bundle system, and a large amount of colonization of the pathogen causes duct function loss, so that plant wilting is caused, and plant death is caused. The bacterial wilt is likely to occur in the whole growth period of crops, the symptoms of bud initiation are most obvious, particularly after the plum rain season, the disease is serious, the plants die in a row and the yield is greatly reduced.
At present, how to safely and efficiently prevent and treat the disease is still a problem. The control of the bacterial wilt is mainly characterized by taking a single chemical agent as an active ingredient, and applying the single chemical fungicide continuously and efficiently for a long time easily causes the residue of the agent, causes the problems of drug resistance of plants, soil deterioration, ecological balance damage, pesticide residue and the like, harms the health of human bodies and causes great economic loss. The chemical bactericides of different types are used in a compounding way, and the composition has the positive characteristics of improving the control effect, prolonging the application of proper amount, reducing the dosage, reducing the key, reducing the residue, delaying the occurrence and the development of the drug resistance and the like of fungi.
In order to solve the technical problems, the inventor screens out 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline by a large amount of biological tests to compound, the bactericidal composition compounded by 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thioketone and 2-cyclopentyl-4-p-toluidine quinoline is not found to be applied to the prevention and treatment research or report of the crop bacterial wilt.
Disclosure of Invention
Based on the defects of the prior art, the invention provides a pesticide sterilization composition and a preparation thereof, and the 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thioketone and 2-cyclopentyl-4-p-toluidine quinoline are compounded, so that the pesticide sterilization composition has obvious synergistic effect, reduces the dosage and has good control effect on crop bacterial wilt.
In order to achieve the purpose, the invention provides the following technical scheme:
a pesticide bactericide composition is composed of 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline.
Preferably, the pesticide sterilization composition comprises 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline according to the mass ratio of (1-5) to (1-5).
More preferably, the pesticide sterilization composition comprises 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline according to the mass ratio of (1-3) to (1-5), and optimally 2: 5.
The invention also provides a pesticide sterilization preparation, which is prepared into any agriculturally allowable dosage form by using the pesticide sterilization composition as an active ingredient and a pesticide auxiliary agent or auxiliary material.
The auxiliary ingredients comprise one or more of an emulsifier, a solvent, a dispersing agent, a wetting agent, a disintegrating agent, a thickening agent, a stabilizing agent, a defoaming agent or a filler.
The auxiliary components are various components which are commonly used or allowed to be used in the pesticide preparation, and are not particularly limited. The specific components and the dosage are determined by simple experiments according to the formula requirements.
The pesticide sterilization preparation can be prepared into any one preparation suitable for agriculture by using a known method, such as self-wetting powder, suspoemulsion, missible oil, microemulsion, emulsion in water and water dispersible granules.
Preferably, in the self-wetting powder, the weight percentage of the bactericidal composition is 20-80%.
Preferably, in the suspoemulsion, the content of the bactericidal composition is 20-40% by weight.
Preferably, in the emulsifiable solution, the weight percentage of the bactericidal composition is 10-20%.
Preferably, in the microemulsion, the weight percentage of the bactericidal composition is 3% -10%.
Preferably, in the aqueous emulsion, the weight percentage of the bactericidal composition is 5-10%.
Preferably, in the water dispersible granule, the weight percentage of the bactericidal composition is 50-80%.
The bactericidal composition is mainly used for controlling bacterial wilt of crops such as hot pepper, tomato, eggplant and the like.
The invention has the beneficial effects that:
2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione has different action mechanisms with other systemic bactericides, influences the formation of fungal cell walls by hindering and inhibiting the biosynthesis of ergosterol in fungi, has protection, treatment and eradication effects, but has relatively poor safety to crops, and needs to reduce the dosage of the 2-cyclopentyl-4-p-toluidine quinoline, and the bactericides can be absorbed by leaves, stems, fruits, roots and other parts of plants, are conducted up and down, are systemic bactericides, are particularly suitable for growing plants, are generally used for starting to be used before the onset of diseases, and prevent the occurrence of diseases.
The 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline in the pesticide bactericidal composition have different action mechanisms, and are favorable for delaying the generation of drug resistance.
Compared with 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione or 2-cyclopentyl-4-p-toluidine quinoline single agent, the compound bactericidal composition has obvious synergistic effect on crop bacterial wilt diseases, improves the prevention and treatment effect, and can reduce the usage amount of pesticide active ingredients, thereby reducing the cost and lightening the environmental pollution.
Detailed Description
The invention discloses a bactericidal composition and a preparation thereof. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
In order to achieve the above object, the present invention provides the following technical solutions:
the active ingredients in the bactericidal composition consist of 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline.
Reagent to be tested:
2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione, synthesized by the method of example 3 in patent CN 110183389A.
2-cyclopentyl-4-p-toluidine quinoline, which is synthesized by referring to the method of example 1 in patent CN 110372588A.
Example 1: preparation of the bactericidal composition and indoor toxicity determination:
1. reagent for testing
2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione.
2-cyclopentyl-4-p-toluidine quinoline.
2. Test pathogen
Tomato ralstonia solanacearum (bacterial wilt pathogen provided by the molecular interaction laboratory of plants and microorganisms of the university of Hunan agriculture).
3. Test processing method
Preparation of medicinal liquid
2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione: 2-cyclopentyl-4-p-toluidine quinoline was prepared into 200mL portions of 5mg/mL liquid medicines using acetone as a solvent in mass ratios of (1: 0), (1: 1), (1: 2), (1: 3), (1: 4), (1: 5), (0: 1), (2: 1), (3: 1), (4: 1) and (5: 1).
4. Spraying liquid medicine for seedling culture and inoculating ralstonia solanacearum
The tomato seedlings are cultivated in seedling pots and are placed at room temperature for cultivation, after the plants grow to the stage of three to four leaves, 10mL of liquid medicine prepared according to the mass ratio is uniformly sprayed on the leaves until the leaves are completely wetted, 5 pots of liquid medicine are processed each time, the experiment is repeated for three times, and the liquid medicine is naturally dried for later use. And a blank control was set for treatment containing only solvent and no active ingredient. After 24h of medicament treatment, adopting a seedling-stage root-damaging-root-soaking inoculation method to artificially inoculate ralstonia solanacearum (the concentration is 5 multiplied by 10)8cfu·mL-1). After inoculation, placing the mixture in an artificial climate box for culturing for 5d, wherein the culture condition is that the light period is 14h every day, the temperature is 30 ℃, and the illumination intensity is 7000 lx; dark period of 10h and temperature of 25 ℃; the relative humidity of air is 70%, and the water and fertilizer management is unified during the culture period. 8d rear view blankAnd (5) carrying out graded investigation according to the disease condition, and calculating the control effect% according to the disease index.
5. Virulence determination method
Grading standard of individual disease condition: level 0: no obvious disease symptoms; level 1: 1 leaf wilting; and 2, stage: 2-3 leaves withering; and 3, level: wilting over 4 leaves; 4, level: the whole plant will wilt or die. Disease index: DI ═ Z (disease grade × number of disease-grade plants)/(highest disease grade × number of investigational plants) × 100
The prevention and treatment effect (%) is [1- (pre-drug control disease index x post-drug treatment disease index)/(post-drug control disease index x pre-drug treatment disease index) ] × 100
The preventing and treating effect is converted into a probability value (y), the concentration of the liquid medicine (ug/mL) is converted into a logarithmic value (x), and a virulence equation and an inhibition medium concentration LC are calculated by minimum multiplication50The virulence index and the cotoxicity coefficient (CTC) of the medicament are calculated according to the Sun Yunpei method.
Measured toxicity index (ATI) ═ standard medicament LC50Test agent LC50)×100
Theoretical virulence index (TTI) ═ A agent virulence index x percent of A in the mixture + B agent virulence index x percent of B in the mixture
Co-toxicity coefficient (CTC) ═ measured toxicity index (ATI) of the mixture/Theoretical Toxicity Index (TTI) of the mixture x 100
When the co-toxicity coefficient is obviously more than 100, the synergistic effect is shown; approaching 100, indicating an additive effect; obviously less than 100, indicating antagonism.
6. Results and analysis
Table 1: 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline in a mass ratio of (1-5) analysis of indoor toxicity measurement for tomato bacterial wilt disease after compounding (1-5) 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione is represented by A, and 2-cyclopentyl-4-p-toluidine quinoline is represented by B.
Table 1A: b is (1-5) by mass: (1-5) analysis of virulence determination result of tomato bacterial wilt by compounding
The measurement results in table 1 show that when the mass ratio of 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione to 2-cyclopentyl-4-p-toluidine quinoline is (1) - (5), the co-toxicity coefficients are all higher than 100, and the synergistic effect is achieved, and particularly, when the mass ratio is 1- (1) - (5), the co-toxicity coefficients are higher than 150, and the synergistic effect is more prominent.
Example 2: preparation of fungicidal preparations
The preparation is prepared into water dispersible granules.
The preparation method of the water dispersible granule comprises the following steps:
uniformly mixing the active ingredient A, the active ingredient B, the dispersing agent, the water, the disintegrating agent and the filler, crushing by using an ultramicro jet mill, kneading, adding into a fluidized bed granulation dryer for granulation, drying, screening, and then sampling and analyzing to obtain the water dispersible granules of the bactericidal composition.
According to the indoor toxicity test determination results in table 1, the mass ratio of 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione to 2-cyclopentyl-4-p-toluidine quinoline is (1-5): (1-5) all have synergistic effect, wherein 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline have the highest co-toxicity coefficient of 183.45 and the best synergistic effect when the mass ratio is 1: 2, so that the water dispersible granule preparation is prepared within the mass ratio of about 1: 2.
Table 2 water dispersible granule formulations 1-6 examples are as follows
Example 3: test of field drug effect
In order to further verify the practical application effect of the invention, the field efficacy test for preventing and treating tomato bacterial wilt is carried out by adopting the water dispersible granule of the bactericidal composition prepared by the invention.
And (3) performing test treatment, namely performing a field pesticide effect test for preventing and treating the tomato bacterial wilt according to the water dispersible granule formula 1-6 prepared in the example 2 in the test.
The test method comprises the following steps: each cell area is 10m2Repeating the steps for 3 times; the method for investigating before pesticide application and after prevention and treatment comprises randomly sampling 5 points in the treatment area, selecting 4 plants at fixed points, grading the disease conditions according to the relevant standards of national field test, recording the disease conditions of the individual plants, and calculating the prevention and treatment effects.
Grading standard of individual disease condition: level 0: no obvious disease symptoms; level 1: 1 leaf wilting; and 2, stage: 2-3 leaves withering; and 3, level: wilting over 4 leaves; 4, level: the whole plant will wilt or die. Disease index: DI ═ Z (disease grade × number of disease-grade plants)/(highest disease grade × number of investigational plants) × 100
The prevention and treatment effect (%) is [1- (pre-drug control disease index x post-drug treatment disease index)/(post-drug control disease index x pre-drug treatment disease index) ] × 100
The results of the field efficacy test are shown in Table 3
The field pesticide effect results show that the sterilization composition has obvious synergistic effect, the control effect of the sterilization composition is excellent, the pesticide effect duration is long, the control effect of the pesticide sterilization compositions in the formulas 2 to 5 on the tomato bacterial wilt is better than that of a single pesticide, and particularly the control effect of the pesticide sterilization composition in the formula 4 is as high as 95.75 percent 30 days after the pesticide is applied. In addition, in the application range, no harmful effect of the pesticide sterilization composition on tomatoes is found, and the pesticide sterilization composition has better safety.
Comparative example 1:
substitution of 2-cyclopentyl-4-p-toluidine quinoline for the analogous derivative 6, 8-difluoro-2, 3-dimethyl-4-quinolinol, represented by B1, as a: b1 preparation of the combined sterilizing water dispersible granule according to the method of example 2, wherein the ratio of the effective ingredients is 2:5, and the field efficacy test is carried out.
The 6, 8-difluoro-2, 3-dimethyl-4-quininol is synthesized according to the method in the specification of 2, 3-dimethyl quinoline compounds such as Fangwenyu, Jiangxianru, Tianjunfeng and the like and the biological activity [ J ] pesticide, 2013,52(3): 171-.
Table 4 water dispersible granule formulations 7-8 examples are as follows
The results of the field efficacy test are shown in Table 5
As shown by the field efficacy results, as shown in table 5, a: the proportion of the effective components of B2 is 2:5, the prevention and treatment effect is not good, and is lower than that of the single agent A.
The foregoing embodiments illustrate some exemplary embodiments of the present invention, but it will be apparent to those skilled in the art that various modifications can be made in the exemplary embodiments without departing from the principles and spirit of the invention, and the scope of the invention is defined by the appended claims.
Claims (10)
1. The pesticide sterilization composition is characterized by comprising 2- [2- (2, 4-dichlorophenyl-2-hydroxy-hexyl ] -2, 4-dihydro- [1,2,4] triazole-3-thione and 2-cyclopentyl-4-p-toluidine quinoline in a mass ratio of (1-5) to (1-5).
2. A pesticide sterilization preparation, which is characterized in that the pesticide sterilization composition as described in claim 1 and pesticide adjuvant or auxiliary materials are prepared into any agriculturally acceptable dosage form.
3. The pesticidal bactericidal formulation according to claim 2, wherein the formulation of the pesticidal bactericide is a self-wetting powder, a suspoemulsion, an emulsifiable concentrate, a microemulsion, an aqueous emulsion, a water dispersible granule.
4. The pesticide sterilization preparation as claimed in claim 3, wherein the pesticide sterilization preparation is in the form of self-wetting powder, and the weight percentage of the pesticide sterilization composition is 20-80%.
5. The pesticide sterilization preparation as claimed in claim 3, wherein the pesticide sterilization preparation is in the form of a suspoemulsion, and the weight percentage of the pesticide sterilization composition is 20-40%.
6. The pesticide sterilization preparation as claimed in claim 3, wherein the pesticide sterilization preparation is in the form of emulsifiable concentrate, and the weight percentage of the pesticide sterilization composition is 10-20%.
7. The pesticide sterilization preparation according to claim 3, wherein the pesticide sterilization preparation is in the form of microemulsion, and the weight percentage of the pesticide sterilization composition is 3-10%.
8. The pesticide sterilization preparation as claimed in claim 3, wherein the pesticide sterilization preparation is in the form of an aqueous emulsion, and the weight percentage of the pesticide sterilization composition is 5-10%.
9. The pesticide sterilization preparation as claimed in claim 3, wherein the pesticide sterilization preparation is in the form of water dispersible granules, and the pesticide sterilization composition is 50-80% by weight.
10. The use of the pesticidal bactericidal formulation of any one of claims 2-9 in the control of bacterial wilt in crops.
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| CN113125643A (en) * | 2021-04-02 | 2021-07-16 | 宁波市农业科学研究院 | Method for rapidly identifying tomato bacterial wilt seedling stage resistance by injection inoculation method |
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| CN110183389A (en) * | 2019-06-25 | 2019-08-30 | 芮城县斯普伦迪生物工程有限公司 | A kind of triazole thioketone derivative compound and preparation method |
| CN110372588A (en) * | 2019-08-29 | 2019-10-25 | 成都理工大学 | A kind of 4- amido quinoline compound and its preparation method and application |
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| CN110183389A (en) * | 2019-06-25 | 2019-08-30 | 芮城县斯普伦迪生物工程有限公司 | A kind of triazole thioketone derivative compound and preparation method |
| CN110372588A (en) * | 2019-08-29 | 2019-10-25 | 成都理工大学 | A kind of 4- amido quinoline compound and its preparation method and application |
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| CN113125643A (en) * | 2021-04-02 | 2021-07-16 | 宁波市农业科学研究院 | Method for rapidly identifying tomato bacterial wilt seedling stage resistance by injection inoculation method |
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Application publication date: 20200218 |