RU2395201C1 - Insecticide composition and method of cultivated plants insect pest control - Google Patents

Abstract

FIELD: agriculture. ^ SUBSTANCE: described insecticide composition in the form of suspension concentrate containing as an active substance a combination of imidacloprid and lambda-Cyhalothrin in synergistically effective amounts. Amount of active ingredient is 6-45 wt %, the ratio of components in it is from 1:5 to 5:1. To increase the effectiveness of the composition additional mineral or vegetable oil and as adhesive aqueous emulsion of acrylic copolymer are included. A method of cultivated plants insect pest control is also described. ^ EFFECT: preparation is an effective mean for cereals, potatoes and soybeans insect pest control. ^ 8 cl, 6 tbl, 5 ex

Description

The present invention relates to means for protecting agricultural crops from pests, in particular to a new insecticidal composition in the form of a water-based suspension concentrate containing, as an active active ingredient, a synergistically effective combination of imidacloprid and lambda-cygalotrin.

The creation of new combinations of already known biologically active substances, the combined use of which leads to a mutual enhancement of biological activity, and preparative forms that contribute to the manifestation of this increased biological activity is still an urgent task, since its solution allows the most affordable way to reduce the rate of application of drugs and, thus reducing the environmental burden on the environment while expanding the spectrum of action used to control pests the drug, as well as overcoming or preventing the development of resistance to individual components of a synergistically effective combination of active active substances.

At present, quite a lot of synergistically effective mixtures of compounds from the group of neonicotinoids, including imidacloprid, with synthetic pyrethroids, recommended for controlling various pests of crops, are already known.

Japanese patent JP 63126805 describes insecticidal compositions for use in agriculture and horticulture containing mixtures of imino-substituted heterocyclic compounds, including imidacloprid, with synthetic pyrethroids such as deltamethrin, cygalotrin, phenpropatrin, phenvalerate, tsiflutrin, permethrin, tsiperperrin, cypermethrin, cypermitrin. A synergistic effect is shown for mixtures whose components are taken in amounts of 40 + 8 ppm respectively. Information about the preparative forms and comparative data on biological activity in the description of the invention are absent.

In the application for invention No. 2784011 (France), insecticidal compositions are described, including pyrethroids, preferably cypermethrin, and one insecticide from the group of neonicotinoids, including imidacloprid, having therapeutic and protective effects. The description provides an example of a composition in the form of a suspension concentrate without specifying specific components of the active substance.

In the description of International Application WO 02/28186, a long list of (over 800) 2-component synergistic mixtures of various pyrethroids with other insecticides, including a mixture of lambda-cygalotrin and imidacloprid, is given. There is no specific information disclosing the properties of this composition.

International application WO 2006/008614 provides a synergistic insecticidal composition containing one compound from the group of neonicotinoids in an amount of 0.1-5.0% by weight. Only one composition is fully disclosed: imidacloprid + cypermethrin, in the form of an emulsifiable concentrate, wettable powder or dispersible granules.

WO 03063592 describes a synergistic insecticidal mixture of lambda-cygalotrin with clothianidin.

Non-aqueous suspension concentrates are known based on neonicotinoids or mixtures thereof with pyrethroids, in which, along with the active active ingredient and surfactants, contain vegetable oil and high molecular weight alkoxylates of fatty alcohols, in quantities significantly exceeding the amount of active active substance; sometimes an organic solvent is added. See, for example, WO 2006/111279 and EAPO application 2008 01 020. An analysis of the compositions given in these publications indicates a very high viscosity of the resulting systems and raises doubts about their stability (according to international standards, the fraction of particles less than 5 microns should be at least 85%). To make such compositions in a production environment and ensure their safety is extremely difficult. To date, not a single commercial preparation in the form of an oil-based suspension suspension concentrate is known, that is, these formulations have no practical significance.

A well-known commercial preparation is the company Syngenta "Endigo", in the form of a water-based suspension concentrate. As an active active substance, the preparation contains a mixture of lambda-cygalothine (9.48%) and thiamethoxam (12.60%). Information on other components of the formulation, except for water, titanium dioxide, glycerin and oil solvent, without indicating their quantitative content, is not available. The drug is recommended for controlling pests on cotton, cereals, potatoes and soy (See www.syngenta.com; Syngenta promotional materials).

The object of the present invention is an insecticidal composition in the form of a water-oil-based suspension suspension concentrate containing, as an active active ingredient, a mixture of imidacloprid and lambda-cygalotrin in synergistically effective amounts.

Imidacloprid is the common name for the compound 1- (6-chloro-3-pyridylmethyl) -N-nitro-imidazolidin-2-ylideneamine.

Systemic insecticide for controlling sucking insects. See European Patent No. 0192060 and US Patent No. 4742060 (Nihon Bayer Agrochem K.K.). Imidacloprid - the active substance of the Tanrek preparation (Handbook of pesticides and agrochemicals approved for use in the Russian Federation. 2008, p. 41).

-циано-3-феноксибензилового эфира (IR, цис) -3-(Z-2-хлор-3,3,3-трифторпроп-1-ен-1-ил)-2,2-диметилциклопропановой кислоты и (R)-

-циано-3-феноксибензилового эфира (IS, цис) -3-(Z-2-хлор-3,3,3-трифтор-1-ен-1-ил)-2,2-диметилциклопропановой кислоты в рацемической пропорции, то есть 1:1.Lambda-cygalotrin is the common name for the crystalline enantiomeric pair of S- isomers

-cyano-3-phenoxybenzyl ester (IR, cis) -3- (Z-2-chloro-3,3,3-trifluoroprop-1-en-1-yl) -2,2-dimethylcyclopropanoic acid and (R) -

of cyano-3-phenoxybenzyl ester (IS, cis) -3- (Z-2-chloro-3,3,3-trifluoro-1-en-1-yl) -2,2-dimethylcyclopropanoic acid in a racemic proportion, then there is 1: 1.

See UK patents No. 2128607 and No. 2130199, US Pat. USSR No. 1225483.

Lambda-cygalotrin is the active ingredient of the Karate preparation registered in the Russian Federation (Handbook of pesticides and agrochemicals approved for use on the territory of the Russian Federation. 2006, p. 49).

In all the sources cited above and other sources known to the applicant, characterizing the previous technical level, there is no information on specific insecticidal compositions containing, as active substance, a mixture of lambda-cygalotrin with imidacloprid, characterizing their composition, level of synergistic action, components and biological activity compared to other known drugs.

The composition in accordance with the present invention contains an active substance, i.e. a combination of imidacloprid (I) with lambda-cygalotrin (II) in an amount of 6-45% by weight, with a ratio of components I: II from 1: 5 to 5: 1, preferably from 1: 1 to 5: 1.

The composition is in the form of a suspension concentrate, therefore, in addition to the active active substance and water, it also includes surfactants, both anionic and nonionic, antifreeze, thickener or stabilizer suspension, antifoam (anti-foaming agent), as well as additives such as biocide, light stabilizer , acidity regulator and dye. As surface-active substances can be used ethoxylated tristyrylphenol phosphate, ethoxylated alkyl phenol, polycarboxylate salt, ethoxy (propoxylated) polyaryl phenol, condensed alkynaphthalene sulfonate, block copolymers of ethylene (propylene) oxide, ethoxy (propoxylated) fatty ethers, polyethylene ethers acids and polyols.

Ethylene or propylene or di (tetra) ethylene glycol or glycerin is used as antifreeze.

Xanthan gum is used as a thickening agent (suspension stabilizer), polydimethylsiloxane is used as a defoamer, limonic acid is used as an acidity regulator, 5-chloro-2-methyl-3 (2H) -isothiazolone or hexahydro-1,3 is used as a biocide, 5-tris- (2-hydroxy-ethyl) sym.-triazine, as a dye - cationic dyes or varnishes (such as Cationic red 2C, Lac Rubin 2SK), as a UV stabilizer (UV absorber) - benzotriazole or benzophenone.

For comparison with the prototype according to the recipe given in patent application No. 2784011 (France), a preparation was prepared containing 37.5% imidacloprid (I) and 12.5% cypermethrin (III) as the active substance. An I: III ratio of 3: 1 is best for the composition of the present invention.

Unlike the prototype, the composition in accordance with the present invention additionally contains mineral or vegetable oil in an amount of from 1 to 20 wt.%. The introduction of a small amount of oil into the formulation makes it easier, as experiments have shown, to transport the active substance into the object by forming an oil emulsion in water, in which the smallest particles of the active substance are distributed.

It was also unexpected that the addition to the composition of small amounts (from 0.1 to 0.4% by weight) of an aqueous emulsion of an acrylic copolymer Plastitex SD (TU 6-38-05800142-302-99), known as a thickener, improves the uniform distribution and retention of the worker solution on the surface of the treated object, thus providing prolonged contact with the insect, increasing the exposure time to the harmful object and resistance to weather conditions, i.e. this emulsion works as an adhesive or adhesive.

The composition in accordance with the present invention has high storage stability, including high and low temperature conditions. In biological activity, it significantly exceeds the composition of the prototype and is not inferior to the “Endigo” drug taken as a reference, and in some cases surpasses it.

Example 1

Obtaining samples 1-9 in the form of suspension concentrates

The required amount of water, antifreeze, dispersant, wetting agent, antifoam, if necessary dye, technical lambda-cygalotrin and imidacloprid are placed in the reactor, thoroughly mixed until a uniform suspension is formed at a temperature of 25-30 ° C, the required amount of oil and UV stabilizer are added and milled in a Dyno-Mill bead mill until a particle size of at least 85% of the particles is not more than 5 microns. An aqueous solution is added to the resulting product, containing a thickener-stabilizer and a bactericide, an adhesive, an acid stabilizer is added to the desired pH value and the physicochemical characteristics of the resulting suspension concentrate are determined.

All amounts of each of the components of the sample preparations 1 to 9 and the prototype are presented in table 1.

Physico-chemical properties of the obtained samples of the drugs are presented in table 2.

Example 2

Assessment of the stability of various types of formulations during storage

To assess the possibility of storing drugs for 2 years at a temperature of minus 10 to plus 35 ° C, the following tests were carried out:

1. Test for accelerated storage: the preparations were kept in a thermostat at plus 54 ° C for 2 weeks (CIPAC MT 46 technique);

2. Test for frost resistance: the preparations were kept in a thermostat at a temperature of minus 15 ° С for 10 days (GOST 9.707-81 and Surfactants and Specialites for Plant Protection, Rhodia);

3. Heat aging test: the preparations were kept in a thermostat at a temperature of plus 45 ° С for 60 days (GOST 9.707-81 and Surfactants and Specialites for Plant Protection, Rhodia).

Repeatability of tests is 3 times.

The viscosity of the preparations both before and after storage was determined on a Brookfield viscometer, stability was determined according to GOST 16484-79 and the CIPAC MT161 Method, dispersion was determined on a Fritsch-Analysette 22 laser particle analyzer. The results are presented in table 3.

As can be seen from table 3, all formulations, except the composition of the prototype, are stable and can be stored for two years in unheated warehouses.

Example 3

Evaluation of the synergistic activity of mixtures of imidacloprid and lambda-cygalotrin

The synergistic activity of a mixture of imidacloprid with lambda-cygalotrin was evaluated by intestinal exposure to a biological object, which is most pronounced for both active substances.

Liquid lures were prepared on the basis of 10% sugar syrup with the addition of various concentrations of the studied active substances.

In the laboratory experiment, hungry house flies (Musca domestica) of the sensitive race (Cooper) of 3-6 days of age were used as biological material.

The experiment was carried out in 3-fold repetition, 10 individuals in each repetition. Accounting for death was carried out after 24 hours.

The degree of toxicity of the samples for the test object was evaluated by the value of the effective dose that causes the death of 50% of the experimental individuals (ED ₅₀ , mg a.v. / l). To determine the ED ₅₀ , a series of logarithmically decreasing concentrations was prepared in the range causing 10-95% insect death. The data obtained were subjected to a Bliss regression probit analysis with the ED _{50 being} in the modification of P.V. Popova (see. Chemistry in Agriculture. / 1965, No. 10, pp. 72-74).

Assessment of the toxic effect of mixtures of imidacloprid and lambda-cygalotrin was carried out according to the formula of P.V. Popov (see Chemistry in Agriculture. 1976, No. 11, p. 54):

,

,

Where

T - additive toxicity, expressed in the same units as the toxicity indicators of the components of the mixture;

A and B - the proportion of pesticides in the mixture;

a and b are indicators of the toxicity of the components of the mixture.

The nature of the action of pesticides in the mixture is expressed using the coefficient of joint action (KSD), which is a quotient from dividing the calculated value of the ED ₅₀ (T value) by the corresponding value of the ED ₅₀ obtained experimentally. With KSD equal to unity, the mixture is additive, that is, its components show neither synergism nor antagonism. A value of KSD greater than unity indicates the presence of synergism of the components in the mixture. The higher the CSD value, the more toxic the mixture compared to the mixture exhibiting an additive effect.

The results of evaluating the toxic effects of mixtures of imidacloprid and lambda-cygalotrin are presented in the table, which shows that the combined use of imidacloprid with lambda-cygalotrin gives a synergistic effect. The greatest degree of synergism is observed in sample No. 3, consisting of 3 parts of imidacloprid and 1 part of lambda-cygalotrin.

Indicators of toxicity and coefficients of the joint action of imidacloprid and lambda-cygalotrin

Example 4

Assessment of the biological activity of the insecticidal composition

Comparative tests of drugs were carried out according to the "Guidelines for the registration tests of insecticides, acaricides, molluscicides and rodenticides in agriculture." St. Petersburg, 2004. The tests were carried out under conditions of small-plot experiments. The following are the experimental conditions for each object separately.

Bed bug bug:

1. Pest phase at the time of treatment: larvae of II-III ages.

2. Culture: winter wheat.

3. Variety: "Stanichnaya".

4. The phase of plant development at the time of processing: milk-wax ripeness.

5. Type of experience: small-scale.

6. The size of the plots and their distribution: 100 m ² , randomized.

7. The number of repetitions: 4.

8. Method of application: spraying.

9. Flow rate: 250 l / ha.

10. Records of harmful objects: before processing, 3 days after processing, 7 days after processing and 14 days after processing.

Cereal aphids:

1. The phase of the pest at the time of processing: imago and larvae.

2. Culture: barley.

3. Variety: "Prairie".

4. The phase of plant development at the time of processing: milk ripeness.

5. Type of experience: small-scale.

6. The size of the plots and their distribution: 100 m ² , randomized.

7. The number of repetitions: 4.

8. Method of application: spraying.

9. Flow rate: 300 l / ha.

10. Records of harmful objects: before processing, 3 days after processing, 7 days after processing and 14 days after processing.

Colorado beetle:

1. The phase of the pest at the time of processing: imago and larvae of I-III ages.

2. Culture: potatoes.

3. Variety: "Nevsky".

4. The phase of plant development at the time of processing: the end of budding.

5. Type of experience: small-scale.

6. The size of the plots and their distribution: 100 m ² , randomized.

7. The number of repetitions: 4.

8. Method of application: spraying.

9. Flow rate: 300 l / ha.

10. Records of harmful objects: before processing, 3 days after processing, 7 days after processing and 14 days after processing.

Soya Aphid:

1. Generation and phase of the pest at the time of processing: adults and larvae.

2. Culture: soy.

3. Variety: "Seaside 81".

4. The phase of plant development at the time of processing: the end of budding - the beginning of flowering.

5. Type of experience: small-scale.

6. The size of the plots and their distribution: 100 m ² , randomized.

7. The number of repetitions: 4.

8. Method of application: spraying.

9. Flow rate: 200 l / ha.

10. Records of harmful objects: before processing, 3 days after processing, 7 days after processing and 14 days after processing.

The results are shown in table 5.

Biological effectiveness of drug samples based on a mixture of imidacloprid and lambda-cygalotrin.

Example 5

Assessment of the economic effectiveness of drugs in the field

Evaluation of the economic efficiency of the use of the samples was carried out on wheat of the Enita variety by spraying the crops in the phase of milk-wax ripeness and on the crops of soybean variety Primorskaya 81 in the phase of the beginning of flowering at a flow rate of 300 l / ha. Yield data are presented in table 6.

The impact of drug samples on crop yields, 2008

Claims (8)

1. An insecticidal composition in the form of a suspension concentrate containing, as an active active ingredient, a combination of imidacloprid (I) and synthetic pyrethroid (II) in synergistically effective amounts in combination with components such as surfactants, antifreeze, antifoam, thickener and water characterized in that, as a synthetic pyrethroid, it contains lambda-cygalotrin (II) and additionally includes mineral or vegetable oil and contains an aqueous emulsion as an adhesive iju acrylic copolymer. 2. The insecticidal composition according to claim 1, in which the active active substances are contained in an amount of 6-45 wt.%, And the ratio of the components of the active substance imidacloprid (I) and lambda-cygalotrin (II) is in the range from 1: 5 to 5: one. 3. The insecticidal composition according to claim 1, characterized in that the mineral or vegetable oil is contained in an amount of from 1 to 20 wt.%, And the aqueous emulsion of an acrylic copolymer in an amount of from 0.1 to 0.4 wt.%. 4. The insecticidal composition according to claim 1, characterized in that it contains at least two substances selected from the group consisting of ethoxylated phosphate tristyrylphenol, ethoxy (propoxylated) polyarylphenol, ethoxylated alkylphenol, polycarboxylate salt, as surfactants, condensed alkylnaphthalene sulfonate, ethylene / propylene / oxide block copolymers, ethoxy (propoxylated) fatty alcohols, alkylaryl sulfonate salt, polyethylene glycol esters of fatty acid esters and polyhydric alcohols s in an amount of 1-11 wt.%. 5. The insecticidal composition according to claim 1, characterized in that it contains ethylene or propylene or di (tetra) ethylene glycol or glycerol in the amount of 0.5-10 wt.% As antifoam, polydimethylsiloxane, in as a thickener, xanthan gum in an amount of 0.15-3.7 wt.%. 6. The insecticidal composition according to claim 1, which further comprises a biocide, a UV stabilizer, a dye and an acidity regulator. 7. The insecticidal composition according to claim 1, containing its constituent components in the following proportions, wt.%:
Imidacloprid 3.0-30.0 Lambda cygalothrin 1,0-20,0 Surfactants 1.0-11.0 Mineral or vegetable oil 1,0-20,0 Antifreeze 0.5-10.0 Anti-foaming agent 0.1-2.5 Thickener 0.15-3.7 Adhesive (adhesive) 0.1-0.4 Biocide 0,0-1,5 UV stabilizer 0,0-0,5 Acidity regulator 0,0-0,8 Dye 0,0-0,5 Water up to 100 8. A method of controlling pests of cultivated plants, characterized in that the pests and their habitats are treated with an effective amount of an insecticidal composition according to claims 1-7.