CN114931142B - Mite-killing composition and preparation method and application thereof - Google Patents
Mite-killing composition and preparation method and application thereof Download PDFInfo
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- CN114931142B CN114931142B CN202210605306.4A CN202210605306A CN114931142B CN 114931142 B CN114931142 B CN 114931142B CN 202210605306 A CN202210605306 A CN 202210605306A CN 114931142 B CN114931142 B CN 114931142B
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
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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
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- 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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Abstract
The invention discloses a mite-killing composition which is characterized by comprising active components A and B, wherein the component A has the structural formula:
Description
Technical Field
The invention relates to the field of agrochemistry, in particular to a mite-killing composition, a preparation method and application thereof.
Background
Spidoxamat IUPAC name: 11- (4-chloro-2, 6-dimethylphenyl) -12-hydroxy-1, 4-dioxa-9-azadispiro [4.2.4 8.25 ] tetradec-11-en-10-one CAS:907187-07-9 is used for controlling aphids, white flies, mealybugs, spider mites, psyllids, thrips and the like of crops such as soybeans, cotton, fruits, vegetables and the like, and has the following chemical structural formula:
Etoxazole (Etoxazole), the chemical name of which is (RS) -2- (2, 6-difluorophenyl) -4- (2-ethoxy-4-tert-butylphenyl) -4, 5-dihydro-1, 3-oxazoline, belongs to 2, 4-diphenyl-1, 3-oxazoline insecticidal acaricides. The etoxazole has excellent control effects on spider mites, tetranychus, panonychus, tetranychus urticae, tetranychus cinnabarinus and other mites of crops such as citrus. The method has the effects of inhibiting embryo formation of mite eggs and the process of molting from young mites to adult mites, and is effective on eggs and young mites, so that the optimal control time is the early stage of mite damage. The etoxazole has good control effect on red spiders of citrus trees.
Mites are a common type of pest which damages crops such as vegetables, fruit trees, cotton and the like, and often causes destructive disasters to the crops. Because of the large number of generations of mites, rapid propagation, serious generation overlapping phenomenon and easy generation of drug resistance to acaricides, the development of a compound composition with high efficiency, low toxicity, low residue and different action mechanisms and synergistic action is needed.
Disclosure of Invention
In order to overcome the defects of the existing single preparation, the first aim of the invention is to provide a compound drug cost-effective acaricidal composition with good synergistic effect and good acaricidal effect.
The composition comprises active components A and B, wherein the component A has the structural formula
The component B is etoxazole.
The weight ratio of the components A to the B is 1:30-30:1, preferably 1:15-150:1, more preferably 1:5 or 15:1..
The sum of the contents of component A and component B is 1% to 80%, preferably 15% to 60%, more preferably 15% to 50% of the total weight of the composition.
The composition may include adjuvants and/or carriers.
For emulsifiable concentrates, the auxiliary agents of the composition comprise one or more of auxiliary agents such as emulsifying agents, dispersing agents, thickening agents, anti-freezing agents, preservatives, defoamers, deflocculants, colorants and the like;
the emulsifier includes ionic and/or nonionic emulsifiers such as one or more of alkylbenzene sulfonate, alkylbenzenesulfonate, alkyl sulfonate, carboxylate, alcohol alkoxylate, alkylphenol ethoxylate, castor oil ethoxylate, amine ethoxylate, sorbitan ester, alkyl glycoside, ethylene oxide-propylene oxide copolymer, ethoxylated phenol phosphate, tristyrylphenol phosphate, fatty alcohol polyoxyethylene ether, and fatty acid polyoxyethylene ester.
For dispersion stabilization, attachment and/or incorporation of the active ingredient, thickeners such as xanthan gum, magnesium aluminum silicate, gelatin, starch, cellulose methyl ether, polyvinyl alcohol, polyvinyl acetate and natural phospholipids (e.g., cephalins and lecithins), synthetic phospholipids, bentonite, sodium lignin sulfonate and the like may be used as adjuvants.
Wherein the antifreezing agent can be selected from ethylene glycol, propylene glycol, glycerol, and sorbitol.
As the defoaming agent, a silicone defoaming agent can be used.
Colorants that may be used, for example, inorganic pigments such as iron oxide, titanium oxide, and Prussian blue; organic pigments/dyes: alizarin dyes, azo dyes and metal phthalocyanine dyes; and trace elements such as iron, manganese, boron, copper, cobalt, molybdenum and zinc salts.
Optionally, the pesticidal liquid compositions of the present invention may also comprise other additional adjuvants, such as protective colloids, binders, thixotropic agents, penetrants, stabilizers, masking agents.
The liquid carrier of the composition of the present invention comprises an organic diluent or solvent. The liquid carrier may be polar or nonpolar, such as one or more of aromatic hydrocarbons (e.g., benzene, toluene, xylene, solvent oils, alkyl naphthalenes, chlorinated aromatic hydrocarbons, chlorinated aliphatic hydrocarbons, chlorobenzene, etc.), alcohols (e.g., methanol, ethanol, isopropanol, butanol, ethylene glycol, etc.), ketones (e.g., acetone, methyl ethyl ketone, diisobutyl ketone, cyclohexanone, etc.), ethers (e.g., diethyl ether, methyl cellulose, tetrahydrofuran, etc.), aliphatic hydrocarbons (e.g., kerosene, mineral oil, etc.), halogenated hydrocarbons, amides, sulfones (e.g., dimethyl sulfoxide), mineral and vegetable oils, animal oils, etc.
For suspending agents, adjuvants which may be used are: dispersants such as one or more of polycarboxylates, lignosulfonates, alkyl naphthalene sulfonates, TERSPERSE 2020 (available from HUNTSMAN corporation, alkyl naphthalene sulfonates, U.S.A.); emulsifying agents such as one or more of Nongru No. 700 (common name: alkylphenol formaldehyde polyoxyethylene ether), st.pan-60 No. (common name: sorbitan monostearate), tween-60 No. (common name: sorbitan monostearate polyoxyethylene ether), nongru No. 1601 (common name: phenethylphenol polyoxyethylene polyoxypropylene ether), TERSPERSE 4894 (manufactured by Hensmei corporation, U.S.A.); wetting agents such as one or more of alkylphenol ethoxylate formaldehyde condensate sulfate, alkylphenol ethoxylate phosphate, phenethyl phenol ethoxylate phosphate, alkyl sulfate, alkyl sulfonate, naphthalene sulfonate, TERSPERSE 2500 (manufactured by hounsfield corporation, usa); thickeners such as one or more of xanthan gum, polyvinyl alcohol, bentonite, magnesium aluminum silicate; preservatives such as one or more of formaldehyde, benzoic acid, sodium benzoate; defoaming agents such as silicone-based defoaming agents; antifreezing agents such as one or more of ethylene glycol, propylene glycol, glycerol, urea, and inorganic salts such as sodium chloride.
The acaricidal composition is an emulsifiable concentrate preparation, and comprises the following components in parts by mass:
Spidoxamat 1-80％；
1-80% of etoxazole;
1-20% of an emulsifying agent;
The solvent makes up 100%.
The effective components, the emulsifying agent and the solvent are stirred, mixed and dissolved to obtain the emulsifiable concentrate preparation.
The acaricidal composition is a suspending agent and comprises the following components in parts by mass:
Spidoxamat 1～80％；
1-80% of etoxazole;
0.3-10% of dispersing agent;
0.2-10% of wetting agent;
0.1 to 2 percent of thickening agent;
0.1-2% of preservative;
the water is filled up to 100%.
The suspending agent is prepared by mixing the active ingredients, the dispersing agent, the wetting agent, the thickening agent and deionized water, performing high-speed shearing dispersion and sanding in a sand mill, and forming a high-dispersion and stable suspension system in an aqueous medium.
A second object of the present invention is to provide the use of the above acaricidal composition for controlling mites of crops, which are one or more of citrus, cotton, flowers, apples, medlar or vegetables;
the pest mites are red spider, rust ticks, tarsonemus, tea yellow mite, tetranychus cinnabarinus and Tetranychus urticae.
A third object of the present invention is to provide a method for controlling crop mites, by applying the above composition to the mites and/or their growing environment.
The acaricidal composition provided by the invention has the following technical effects:
1. The mixed preparation has obvious synergistic effect, and compared with single dosage, the single dosage has improved effect of preventing and treating mites.
2. The dual action mechanism delays the generation of drug resistance of mites.
3. The synergistic effect produced by mixing the two active ingredients is utilized, the pesticide usage amount is reduced, and the use cost and the environmental pollution are reduced.
Detailed Description
The following examples further illustrate some of the features of the present invention, but the scope and content of the invention is not limited by the examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Formulation examples
The percentages of the components in the examples are all weight percentages.
EXAMPLE 1-1 24% spidoxamat, etoxazole emulsifiable concentrate
| Component (A) | Composition% | Remarks |
| Spidoxamat | 4 | Active ingredient |
| Etoxazole | 20 | Active ingredient |
| Tween 80 | 5 | Emulsifying agent |
| Pesticide emulsion 600 #) | 8 | Emulsifying agent |
| Vegetable oil | Complement 100 | Solvent(s) |
Examples 1-2% spidoxamat, etoxazole emulsifiable concentrate
| Component (A) | Composition% | Remarks |
| Spidoxamat | 3 | Active ingredient |
| Etoxazole | 15 | Active ingredient |
| Tween 80 | 5 | Emulsifying agent |
| Pesticide emulsion 600 #) | 8 | Emulsifying agent |
| Vegetable oil | Complement 100 | Solvent(s) |
Examples 1-3 16% Spidoxamat, etoxazole suspension
| Component (A) | Composition% | Remarks |
| Spidoxamat | 15 | Active ingredient |
| Etoxazole | 1 | Active ingredient |
| Dodecyl benzene sulfonic acid calcium salt | 6 | Wetting agent |
| Sodium lignin sulfonate | 5 | Dispersing agent |
| Xanthan gum | 2 | Thickening agent |
| Magnesium aluminum silicate | 1 | Thickening agent |
| Sodium benzoate | 0.5 | Preservative agent |
| Deionized water | Complement 100 | Solvent(s) |
Examples 1-4% Spidoxamat, etoxazole suspension
| Component (A) | Composition% | Remarks |
| Spidoxamat | 10 | Active ingredient |
| Etoxazole | 10 | Active ingredient |
| Dodecyl benzene sulfonic acid calcium salt | 7 | Wetting agent |
| Sodium lignin sulfonate | 4 | Dispersing agent |
| Xanthan gum | 1 | Thickening agent |
| Magnesium aluminum silicate | 1 | Thickening agent |
| Sodium benzoate | 0.5 | Preservative agent |
| Deionized water | Complement 100 | Solvent(s) |
The preparation method comprises the following steps: and (3) preparing emulsifiable concentrate: mixing the above effective components, emulsifying agent and solvent, stirring, and dissolving to obtain emulsifiable concentrate preparation. Preparing a suspending agent: the suspending agent can be prepared by mixing the active ingredients, the dispersing agent, the wetting agent, the thickening agent, the antifreezing agent, the defoaming agent and deionized water, performing high-speed shearing dispersion and sanding in a sand mill, and forming a high-dispersion and stable suspension system in an aqueous medium.
2. Examples of efficacy verification
(One) indoor biological Activity assay
Test agent: spidomaxmat raw medicines; etoxazole original drug;
test insects: citrus red spider (Panonychus citriMcGregor) collected in the field, and raising indoors.
The test method adopts a leaf butterfly spray method (refer to NY/T1154.13-2008 pesticide laboratory biological assay test criterion pesticide. Part 13: she Die spray method).
The specific operation method is as follows: each single dose and the mixed medicament are provided with 5 different concentration gradients (based on the preliminary test result, the death rate of the citrus red spider is set according to the geometric progression within the range of 5% -90%).
Selecting healthy citrus leaves, making She Die by using a puncher, placing a wet sponge block in a culture dish, placing filter paper on the wet sponge block, placing leaf butterflies on the filter paper, placing 2 leaf butterflies on each dish, selecting healthy red spiders with consistent age, inoculating the red spiders on the leaf butterflies, and inoculating 20 red spiders on each leaf butterflies.
Placing the petri dish connected with the leaf butterfly under a potter spray tower, spraying under 50PSI pressure, settling for 1min, taking out the petri dish, placing the treated petri dish into a 25 ℃ 12H/12H illumination incubator for culturing, checking the death number for 48H, and calculating the death rate. Each treatment was repeated 4 times and a clear water placebo treatment was set.
Statistical analysis was performed using DPS statistical analysis software, LC50 was calculated for each agent, and co-toxicity coefficient (CTC value) of the mixture was calculated according to the grand cloud Pei method (s.)
Toxicity Index (ATI) = (standard agent LC 50/test agent LC 50) ×100.
Theoretical Toxicity Index (TTI) =a agent toxicity index x percentage of agent toxicity index in mixture + B agent toxicity index x percentage of agent toxicity in mixture.
Co-toxicity coefficient (CTC) = [ actual drug susceptibility index (ATI)/theoretical drug susceptibility index (TTI) ] x 100.
The classification standard is based on the combination effect of NY/T11547.7-2006 pesticides: the co-toxicity coefficient (CTC) is more than or equal to 120, and the synergistic effect is shown; the cotoxicity coefficient (CTC) is less than or equal to 80 and shows antagonism; a co-toxicity coefficient (CTC) of 80 < 120 shows additive effect.
Indoor toxicity determination of Spidoxamat and etoxazole combination on citrus red mites
The indoor toxicity measurement result shows that: spidoxamat and etoxazole in a weight ratio of 1:30-30:1, the mixed use has better toxicity to citrus red spiders and no antagonism; when the weight ratio of Spidoxamat to etoxazole is 1:5 and 15:1, the synergistic effect is achieved, the dosage of the active ingredients can be reduced, and the generation of drug resistance is slowed down.
(II) field efficacy example
Spidoxamat field efficacy test of the combination of etoxazole on cotton red spiders.
The preparation example medicament is used for preventing and controlling citrus red mites, the number of the insect population is investigated before the medicament is applied, the number of residual live mites is investigated after 7d, 2 plants are investigated per cell during investigation, 5 leaves are respectively investigated per plant according to 4 aspects of east, west, south and north, 40 leaves are investigated per cell, the number of live mites is recorded, and the preventing and controlling effect is calculated.
The control effect calculation method is as follows.
Control effect (%) = (1-CK 1×Pt1/CK2×Pt2) ×100.
Wherein: CK 1 represents the number of pre-drug insect population in the control zone; pt 1 represents the number of insect mouths after the medicine in the treatment area;
CK2 represents the number of insect mouths after the drug in the control area; pt2 represents the number of pre-drug insect population in the treatment area.
From the test results table 4, it can be seen that: the preparation examples 1-1, 1-2, 1-3 and 1-4 of the invention have 4000-6000 times dilution effect on citrus red spider prevention and good persistence, and the medicament is not found to generate phytotoxicity on citrus.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (3)
1. Use of an acaricidal composition for controlling red spiders in crops, the composition comprising active components a and B, the component a having the formula:
The component B is etoxazole;
The mass ratio of the components A and B in the composition is 1:5 and 15:1;
The crop is citrus.
2. Use according to claim 1, characterized in that: the total weight percentage of the components A and B in the composition is 1-80%.
3. The method according to claim 2, wherein the composition is in the form of wettable powder, water dispersible granule, water dispersible tablet, suspension, microemulsion, emulsifiable concentrate or aqueous emulsion.
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| CN101801196A (en) * | 2007-09-21 | 2010-08-11 | 拜尔农作物科学股份公司 | Active ingredient combinations having insecticidal and acaricidal properties |
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| DE102005008021A1 (en) * | 2005-02-22 | 2006-08-24 | Bayer Cropscience Ag | New spiroketal-substituted cyclic ketoenol compounds used for combating animal parasites, undesired plant growth and/or undesired microorganisms |
| CN103704227A (en) * | 2013-12-11 | 2014-04-09 | 北京燕化永乐生物科技股份有限公司 | Composition containing etoxazole |
| CN104115850A (en) * | 2014-06-12 | 2014-10-29 | 广东中迅农科股份有限公司 | Insect and mite killing composition containing etoxazole and spirotetramat |
| WO2020043650A1 (en) * | 2018-08-29 | 2020-03-05 | Bayer Aktiengesellschaft | Active compound combinations having insecticidal/acaricidal properties |
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| CN101801196A (en) * | 2007-09-21 | 2010-08-11 | 拜尔农作物科学股份公司 | Active ingredient combinations having insecticidal and acaricidal properties |
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