Abstract: A synergistic insecticidal and fungicidal composition comprising of (A) Etofenoprox (B) tebuconazole and; (c) Azoxystrobin. The invention further relates to formulations comprising the composition of the present invention and method of controlling insect and fungal pests infesting plants especially crops.
Description:FIELD OF THE INVENTION:
The present invention relates to a combination of Etofenprox, Tebuconazole and Azoxystrobin and its composition and methods of preparation thereof. Particularly, the present invention relates to a synergistic composition comprising Etofenprox, Tebuconazole and Azoxystrobin, methods of preparation of the composition and use thereof for the control of a wide variety of undesired phytopathogenic microorganisms, insect and fungi pest.
BACKGROUND OF THE INVENTION:
In many economically important crops, such as rice, peppers, tomatoes, grapes, peas, cotton and other agricultural and horticultural crops, fungal infection and insect infestation may occur simultaneously for which growers are applying control measures either separately or by simply tank mixing various insecticides and fungicides together. This practice of mixing various pesticides might lead to poor efficacy and crop damage due to compatibility issues hence a premix of the best possible formulation for a combination of an insecticide and a fungicide would help growers to combat these important diseases and insects/mites in those crop stages.
Typical problems arising in the field of pest control is to reduce the dose rates of the active ingredients in order to reduce or avoid unfavorable environmental or toxicological effects whilst still allowing effective disease/pest control. Therefore, a combined application of an effective amount of fungicide and insecticide as a uniform composition is a practical necessity.
Rice (Oryza sativa) crop is of paramount importance for global food security, nutrition, and livelihoods, playing a vital role in the agricultural economies and cultural heritage of many countries. It occupies about 23.3% of gross cropped area of the country and plays vital role in the national food grain supply. Rice contributes 43% of total food grain production and 46% of the total cereal production of the country. It is the staple food of more than 60% of the world's population especially for most of the people of South-East Asia. Among the rice growing countries in the world, India has the largest area under rice crop and ranks second in production next to China. In India, rice is grown under widely varying conditions of altitude and climate. Therefore, the rice growing seasons vary in different parts of the country, depending upon temperature, rainfall, soil types, water availability and other climatic conditions.
Blast disease caused by Pyriculariaoryzae & Sheath blight disease caused by Rhizoctoniasolani the serious fungal diseases affecting rice crop and have gained the status of most significant diseases on all the major high yielding varieties of rice. Blast & Sheath blight are a very destructive diseases of rice under favorable weather conditions causing high yield loss. The diseases are particularly important in intensive rice production systems due to high plant density and high rate of application of nitrogenous fertilizers, which favor the disease development.
Etofenprox with CAS registration number 80844-07-1 is a derivative of an aromatic ether that is 3-phenoxybenzyl ether of 2-(4-ethoxyphenyl)-2-methylpropan-1-ol. It has the role as a pyrethroid ether insecticide. It is functionally related to a 2-(4-ethoxyphenyl)-2-methylpropan-1-ol.
It has an IUPAC name 1-ethoxy-4-[2-methyl-1-[(3-phenoxyphenyl)methoxy]propan-2-yl]benzene having chemical structure as:
ETOFENPROX
Azoxystrobin with CAS registration no 131860-33-8is an aryloxy pyrimidine having a 4,6-diphenoxypyrimidine skeleton An inhibitor of mitochondrial respiration by blocking electron transfer between cytochromes b and c1, it is used widely as a fungicide in agriculture. It has a role as a mitochondrial cytochrome-bc1 complex inhibitor, a xenobiotic, an environmental contaminant, an antifungal agrochemical and a quinone outside inhibitor. It is a nitrile, an aryloxy pyrimidine, an enol ether, a methyl ester and a methoxy acrylate strobilurin antifungal agent.
It has an IUPAC namemethyl-(E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-yl]oxyphenyl]-3-methoxyprop2-enoatehaving chemical structure as:
AZOXYSTROBIN
Tebuconazole with CAS registration number 107534-96-3. it belongs to triazole bactericides, is a sterol demethylation inhibitor, is a high-efficiency bactericide for seed treatment or leaf surface spraying of important economic crops, and can effectively prevent and treat various rust diseases, powdery mildew, net blotch, root rot, gibberellic disease, smut, seed-borne wheel spot and the like of cereal crops.
It has an IUPAC name IUPAC name is 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-ylmethyl)pentan-3-olhaving chemical structure as below:
TEBUCONAZOLE
OBJECT OF THE INVENTION
The main objective of the disclosure is to provide a synergistic insecticidal and fungicidal composition combining Etofenprox, Tebuconazole and Azoxystrobin that enhances pest control efficacy beyond the sum of individual effects.
Another objective of the present invention is to provide a novel and effective synergistic insecticidal and fungicidal composition for controlling the harmful broad spectrum of pests in plants.
Another important object of the present disclosure is to deliver broad-spectrum pest control that effectively targets a variety of insect and fungi pests, including Blast and Sheath blight, across different crops like Rice.
Another object of the present disclosure is to reduce the likelihood of pest resistance by utilizing a multi-component approach, thereby decreasing the dependence on single-action insecticides and fungicides.
Yet another object of the present disclosure is to ensure stability of the formulation under various environmental conditions, minimizing separation or degradation of active ingredients for consistent performance.
Yet another object of the present disclosure is to lower the required dosage levels while maintaining effective pest control, reducing potential phytotoxicity to crops and minimizing environmental impact.
Yet another object of the present disclosure is to provide an easy-to-mix and apply formulation that ensures uniform distribution on crops, improving application efficiency and overall pest control results.
Yet another object of the present disclosure is to create an environmentally safer alternative by minimizing harmful residues, thus reducing health risks for farmers, consumers, and non-target organisms.
SUMMARY OF THE INVENTION
In one aspect, the present invention provides a composition comprising of:
a) an effective amount of Etofenprox or salt(s) thereof,
b) an effective amount of Tebuconazole or salt(s) thereof,
c) an effective amount of Azoxystrobin or salt(s) thereof,
d) agriculturally acceptable additives.
In a particular aspect, the present invention provides a synergistic combination of Etofenprox, Tebuconazole and Azoxystrobin to control a wide variety of undesired phytopathogenic microorganisms, insect and fungi pest.
In another aspect, the present invention provides a synergistic fungicidal and insecticidal combination of Etofenprox, Tebuconazole and Azoxystrobin.
In yet another aspect, the present invention provides a synergistic fungicidal combination of Etofenprox, Tebuconazole and Azoxystrobin.
In a further aspect, the present invention provides a synergistic insecticidal combination of Etofenprox, Tebuconazole and Azoxystrobin.
In another aspect, the present invention is to provide longer residual control of the undesired phytopathogenic microorganisms, insect and fungi pest treated with the combination of Etofenprox, Tebuconazole and Azoxystrobin.
In a further aspect, the present invention provides a synergistic composition comprising of:
a) an effective amount of Etofenprox or salt(s) thereof,
b) an effective amount of Tebuconazole or salt(s) thereof,
c) an effective amount of Azoxystrobin or salt(s) thereof
d) agriculturally acceptable additives.
In one aspect, the present invention provides a synergistic composition of Etofenprox, Tebuconazole and Azoxystrobin to control a wide variety of undesired phytopathogenic microorganisms, insect and fungi pest .
In a further aspect, the present invention provides a synergistic composition comprising Etofenprox, Tebuconazole and Azoxystrobin; the composition possesses fungicidal and/or insecticidal activity.
In another aspect, the present invention provides a method for the preparation of the composition comprising of Etofenprox, Tebuconazole and Azoxystrobin.
In a further aspect, the present invention provides a method for improving crop health (phyto tonic effect), comprising treating a plant with an effective amount of the composition of Etofenprox, Tebuconazole and Azoxystrobin.
DETAILED DESCRIPTION OF THE INVENTION
Discussed below are some representative embodiments of the present invention. The invention in its broader aspects is not limited to the specific details and representative methods. The illustrative examples are described in this section in connection with the embodiments and methods provided. The invention according to its various aspects is particularly pointed out and distinctly claimed in the appended claims read in view of this specification and appropriate equivalents.
It is to be noted that, as used in the specification and the appended claims, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to a composition containing “a compound” includes a mixture of two or more compounds. It should also be noted that the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise.
The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total solution or composition unless otherwise specified.
The term “active ingredient” (a.i.) or “active agent” used herein refers to that component of the composition responsible for control of Fungal-pests or disease.
As used herein, the terms "comprises", "comprising", "includes", "including", or any other variation thereof, are intended to cover a non-exclusive inclusion, subject to any limitation explicitly indicated. For example, a composition or a method that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, or method.
The term "synergistic", as used herein, refers the combined action of two or more active agents blended together and administered conjointly that is greater than the sum of their individual effects.
As used herein, the term “insecticidal” refers to the ability of a composition or substance to improve the ability of insect mortality or inhibit the growth rate.
As used herein the term “fungicidal” refers to the ability of a composition or substance to reduce the rate of fungal growth or increase fungal mortality.
As used herein, the term “composition” or "formulation" can be used interchangeably, unless stated otherwise, is meant to encompass, and are not limited to, compositions or formulations containing the combination of Etofenprox, Tebuconazole and Azoxystrobin.
As used herein, the term “additive(s)” or "auxiliary agent(s)" or “agrochemically acceptable carrier(s)” can be used interchangeably and refers to inert substances which are commonly used as diluent, to provide stability or to increase the activity profile of the composition or formulation with or without having agrochemical activity or direct effect on the undesired phytopathogenic insects and/or microorganisms.
As used herein, the term "agrochemically acceptable salts" are typically acid addition salts of inorganic or organic acids, preferably of hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, perchloric acid, phosphoric acid, formic acid, acetic acid, trifluoroacetic acid, oxalic acid, malonic acid, toluenesulfonic acid or benzoic acid.
As used herein, the term "effective amount" means the amount of the active substances in the compositions to achieve an observable effect on growth, including the effects of necrosis, death, retardation, prevention, and removal, destruction, or otherwise diminishing the occurrence and activity of the target organism. The effective amount can vary for the various compositions used in the present invention. An effective amount of the compositions will also vary according to the prevailing conditions such as desired pesticidal effect and duration, weather, target species, locus, mode of application, and the like.
In an embodiment, the Insecticidal composition wherein the Etofenprox ranging from 0.1% to 30.0% by weight of the Insecticidal composition.
In an embodiment, the fungicidal composition wherein the Tebuconazole ranging from 0.1% to 40.0% by weight of the fungicidal composition.
In an embodiment, the fungicidal composition wherein the Azoxystrobin ranging from 0.1% to 30.0% by weight of the fungicidal composition.
In another embodiment of the present invention, the invention further provides the process for preparation of the said formulation wherein, the said formulation can be one or more of as suspension concentrate (SC), wettable granules (WG), wettable powder (WP), a water dispersible granule (WDG), a water dispersible tablet (WT), an ultra-low volu (ULV) liquid (UL), an ultra-low volume (ULV) suspension (SU), a water soluble powder (SP), a suspo-emulsion (SE), granule (GR), an emulsifiable granule (EG), an oil-in-water or water in oil emulsion (EW), an emulsifiable concentrate (EC), a micro-emulsion (ME), an oil dispersion (OD), a capsule suspension (CS), a dustable powder (DP) or an aerosol (AE).
In preferred embodiment of the present invention, the formulation is Suspo-emulsion (SE), oil dispersion (OD).
In yet another embodiment of the present invention, the agrochemically acceptable excipients of the formulation are selected from the group consisting of Emulsifiers dispersing agents, antifoaming agents, Rheology modifiers, solvents, biocides, pH Modifiers, Super-Wetting-spreading-penetrating agent, Stabilizing agents and anti-freezing agent.
Dispersing agent is selected from the group comprising of, but not limited to polymeric ester dispersant, ethoxylated polyarylphenol phosphate ester, sodium salt of naphthalene sulfonate condensate/naphthalene sulphonic acid condensate, acrylic copolymer,nonionic proprietary surfactant blend, polycarboxylates, calcium dodecylbenzene sulfonate, aryl sulphonate condensate,sodium lignosulphonate, dispertox BS SPL, polystyrenated acrylated co-polymer, modified styrene acrylic copolymer, salts of phenol sulfonic acids, Terwet 2700,butyl polyalkylene oxide block co-polymer, mixture of tristyrylphenolethoxylates and polyalkylene oxide derivative of a synthetic alcohol, random co-polymer of alcoxylated polyethylene glycol or mixtures thereof; The Dispersing agent is present in an amount of from 0.1% to 20.0% by weight based on a total weight of the composition.
Antifoaming agent is selected from the group comprising of, but not limited to polydimethyl siloxane, polydimethyl siloxane emulsion or mixtures thereof; The Antifoaming agent is present in an amount of from 0.01% to 5.0% by weight based on a total weight of the composition.
Rheology modifier is selected from the group comprising of, but not limited to precipitated silica, fumed silica, modified fumed silica, bentonite, hydroxymethyl cellulose, carboxymethyl cellulose, xanthan gum, thickening silica, hydrated clay minerals, magnesium aluminium silicates, Rhodopol 23, organic derivative of hectorite clay, hydrophobic fumed silica, polyvinylpyrrolidone (PVP) or mixture thereof; The Rheology modifier is present in an amount of from 0.1% to 20.0% by weight based on a total weight of the composition.
Solvents is selected from the group comprising of, but not limited to Demineralized (DM) water, N-alkyl-pyrrolidone, oil medium selected from the group comprising, esterified fatty acids selected from methyl and/or ethyl ester of vegetable oil such as methyl soyate, ethyl soyate, rapeseed methyl ester, rapeseed ethyl ester or mixtures thereof. The Solvents is present in an amount of from 0% to 95% by weight based on a total weight of the composition.
Biocides is selected from the group comprising of, but not limited to biocide by weight of the formulation selected from the group comprising of 1,2-benzisothiazolin-3-one, formaldehyde, dipropyl glycol solution of 1,2-benzisothiazolin-3-one or mixtures thereof. The Biocides is present in an amount of from 0% to 3% by weight based on a total weight of the composition.
Anti freezing agents is selected from the group comprising of, but not limited to selected from the group comprising of ethylene glycol, propane-1,2-diol, propane-1,2,3-triol, urea or mixtures thereof. The Anti freezing agents is present in an amount of from 0% to 15% by weight based on a total weight of the composition.
Stabilizing agents is selected from the group comprising of, but not limited to selected from the group comprising of epoxidized soyabean oil, butylated hydroxy toluene, ethylenediaminetetraacetic acid, sodium benzoate, etc. or mixtures thereof. The Stabilizing agents is present in an amount of from 0% to 5% by weight based on a total weight of the composition.
Super-Wetting-spreading-penetrating agent is blend of methylated seed oil-organic silicone compound may be selected from methylated seed oil-polyalkyleneoxide modified trisiloxane, methylated seed oil-polyalkyleneoxide modified polydimethylsiloxane, methylated seed oil-20 trisiloxane ethoxylate, methylated seed oil-polyoxyethylene methyl polysiloxane, methylated seed oil-polyether polymethyl siloxane copolymer, methylated seed oil-polyether modified polysiloxane. The Super-Wetting-spreading-penetrating agent is present in an amount of from 0.1% to 5.0% by weight based on a total weight of the composition.
pH stabilizer is selected from the group comprising of, but not limited to selected from the group comprising of sodium pyrophosphate, sodium acetate, sodium oxalate, sodium carbonate, sodium bicarbonate, trisodium phosphate, citric acid, trisodium citrate, monoethanol amine, triethanol amine, triethylamine, dibasic esters selected from dimethyl succinate, dimethyl glutarate, dimethyl adipate, ortho phosphoric acid, oxalic acid, citric acid, hydrochloric acid.The pH Stabilizers is present in an amount of from 0.01% to 10% by weight based on a total weight of the composition.
Emulsifiers is selected from the group comprising of, but not limited to formulation selected from the group comprising of ethoxylated propoxylated alcohols, alkylphenolethoxylates, alkoxylated tristyrylphenols, calcium dodecylbenzenesulfonate, mixture of fatty acid polyethylene glycol ester, ethoxylated propoxylated polyaryl phenol, ethoxylated fatty acids, fatty alcohol ethoxylates, ethoxylated ricinoleic acid triglycerides, sorbitan trioleate, tridecyl alcohol ethoxylate, castor oil ethoxylate, Calcium dodecylbenzenesulfonate, Dioctyl sulfosuccinate sodium salt, Mixture of fatty acid polyethylene glycol ester, Polyalkoxylated butyl ether block co-polymer, alkoxylated phosphate ester or mixtures thereof; The Emulsifiers is present in an amount of from 0.1% to 20.0% by weight based on a total weight of the composition.
The composition of the present invention is effective for management of insect and fungi or pests selected from one or more of Cotton (Gossypium spp.), Paddy (Oryza sativa), Wheat (Triticumaestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Sugarbeet (Beta vulgaris), Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Castor (Ricinus communis), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Ciceraritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus), Onion (Allium cepa L.), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Sweet potato (Ipomoea batatas), Chilly (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus), Muskmelons (Cucumis melo), Watermelon (Citrullus lanatus), Bottle gourd (Lagenaria siceraria), Bitter gourd (Momordica charantia), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica rapasubsprapa), Apple (Melus domestica), Banana (Musa 25 spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punica granatum) , Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Fenugreek (Trigonella foenum-30 graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermumammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safedmusli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), Mentha ( Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold (Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis), Gerbera (Gerbera jamesonii), Carnation (Dianthus caryophyllus) or GMO form thereof.
In yet another preferred embodiment, the present invention provides a insecticidal and fungicidal combination or composition comprising of Etofenprox, Tebuconazole and Azoxystrobin. to control the pathogenic microorganism on economically important crops such as rice, chilli, apple, peppers, soybean, cotton, chick pea, pigeon pea, Grapes, Apple and pomegranate, tea, potato, and tomato.
The invention is illustrated by the experiments as exemplified below.
Examples:
The examples below are given solely for the purpose of illustration and are not to be construed as limitations of the present invention, as many variations thereof are possible without departing from the spirit and scope of the invention.
Example 1: Preparation of insecticidal and fungicidal composition as Suspo-emulsion (SE) formulation:
In an embodiment, the chemical composition of the present insecticidal and fungicidal is depicted below in Table 1 below:
Table 1: Insecticidal and fungicidal Composition for Suspo-emulsion (SE) Formulation.
Component Composition (%w/w) Remark
Etofenprox Active Ingredient
Tebuconazole Active Ingredient
Azoxystrobin Active Ingredient
Polyalkoxylated butyl ether block co-polymer 3.00 Emulsifier
Ethoxylatedtristyrylphenol 2.00 Emulsifier
Nonionic proprietary surfactant blend 2.00 Dispersing agent
Acrylic copolymer 1.50 Dispersing agent
Propane-1,2,3-triol 6.50 Antifreezing Agent
Dipropylene glycol solution of 1,2-benzisothiazolin-3-one 0.10 Biocide
Polydimethylsiloxane emulsion 0.30 Antifoaming agent
Citric acid 0.20 pH stabilizer
Sodium Benzoate 1.50 Stabilizing agent
Precipitated Silica 1.00 Rheology modifier
Rhodopol 23 0.10 Rheology modifier
Aromatic solvent naphtha 10.0 Solvent
Demineralizedwater Balance to 100 Solvent
Process for preparing Suspo-emulsion (SE)formulation:
Preparation of Etofenprox oil phase
The active ingredient Etofenprox was dissolved in aromatic solvent naphtha at room temperature. To this solution polyalkoxylated butyl ether block co-polymer and ethoxylated tristyrylphenol under stirring to form Etofenprox oil phase.
Preparation of aqueous phase of Tebuconazole and Azoxystrobin:
In demineralized water constituents namely dipropylene glycol solution of 1,2-benzisothiazolin-3-one, polydimethylsiloxane emulsion, propane-1,2,3-triol, nonionic proprietary surfactant blend and acrylic copolymer as mentioned in Table 1 were added into the clean pre-mixing vessel fitted with the homogenizer and all the ingredients were mixed for sufficient time with the homogenizer to obtain a mixture. The active ingredients, Tebuconazole, Azoxystrobin and precipitated silica were added to the above mixture and continued to mix for sufficient time with the homogenizer to obtain a slurry. The slurry was passed through jacketed bead mill with chilled water circulation for particle size reduction to obtain a aqueous phase of Tebuconazole and Azoxystrobin of desirable particle size of d(90)<20 micron. The aqueous phase of Tebuconazole and Azoxystrobin was collected into mixing vessel fitted with the stirrer.
Preparation of Suspo-emulsion (SE) formulation:
The Etofenprox oil phase was added to the aqueous phase of Tebuconazole and Azoxystrobin under a continuous agitation for an optimum amount of time at room temperature. Then a suitable quantity of pH adjuster, stabilizer and rhodopol 23 was added to the mixture. The mixture was continuously agitated until the appropriate time to form pesticidal suspo-emulsion (SE) formulation.
Example 2: Preparation of insecticidal and fungicidal composition as Oil Dispersion (OD) formulation:
Table-1 (b):Insecticidal and fungicidal composition of the Oil Dispersion (OD) formulation
Component Composition (%w/w) Remark
Etofenprox Active Ingredient
Tebuconazole Active Ingredient
Azoxystrobin Active Ingredient
Castor oil ethoxylate(10 mole) 6.00 Emulsifier
Calcium dodecylbenzenesulfonate 1.00 Emulsifier
Dioctyl sulfosuccinate sodium salt 1.00 Emulsifier
Mixture of fatty acid polyethylene glycol ester 4.00 Emulsifier
Polymeric ester dispersant 0.5 Dispersing agent
Ethoxylated polyarylphenolphosphate ester 0.5 Dispersing agent
Propane-1,2,3-triol 2.00 Antifreezing Agent
Polyalkyleneoxide modified heptamethyltrisiloxane 1.00 Super-Wetting-spreading-penetrating agent
Polydimethylsiloxane 0.30 Antifoaming agent
Fumed silica 1.50 Rheology modifier
Citric acid 0.10 pH stabilizer
Bentonite clay 1.50 Rheology modifier
Methyl ester of vegetable oil Balance to 100 Solvent
Process for preparing Oil Dispersion (OD)formulation:
In methyl ester of vegetable oil constituents namely, polyalkyleneoxide modified heptamethyltrisiloxane, polydimethylsiloxane, propane-1,2,3-triol, castor oil ethoxylate(10 mole), calcium dodecylbenzenesulfonate, dioctyl sulfosuccinate sodium salt, ethoxylated polyarylphenol phosphate ester, mixture of fatty acid polyethylene glycol ester and polymeric ester dispersant added into the clean pre-mixing vessel fitted with the homogenizer and all the ingredients were mixed for sufficient time with the homogenizer to obtain a mixture. The active ingredients, Etofenprox, Tebuconazole and Azoxystrobin were added to the obtained mixture and continued to mix for sufficient time with the homogenizer to obtain a slurry. The slurry was passed through jacketed bead mill with chilled water circulation for particle size reduction to obtain a milled slurry of desirable particle size of d(90)<20 micron. The milled slurry was collected into post mixing vessel fitted with the stirrer. To milled slurry pH stabilizer, bentonite clay and fumed silica was added under stirring into the post mixing vessel and continued to mix for sufficient time up to proper mixing to form pesticidal Oil Dispersion (OD) formulation.
Stability Data
Stability Study (Accelerated Storage test and low-temperature storage test)
According to the FAO/WHO manual, the “accelerated storage test” is considered as an indicative of product stability. That is, accelerated storage test data provides an indication that the product is stable for at least two years at ambient temperature. Further, the FAO/WHO manual indicates storage at 54 ± 2°C for 14 days as the default test conditions. Further, the FAO/WHO manual indicates low-temperature storage at 0 ± 2°C for 7 days.
The “accelerated storage” is the sample after subjecting the sample to accelerated storage tests at 54±2°C for 14 days.
The pesticidal formulation composition of examples 1 - 3 were found stable during accelerated stability study at 54±2° C for 14 days and low temperaturestudy at 0 ± 2°C for 7 days.
Example 3: Evaluation of Bio-efficacy & Phytotoxicity of Fungicidal Composition and thereof (Etofenprox + Tebuconazole + Azoxystrobin) against Blast (Pyriculariaoryzae)& Sheath blight (Rhizoctonia solani) disease on Rice crop.
Field evaluation of the bio-efficacy of present fungicidal composition:
The presently disclosed fungicidal (Etofenprox + Tebuconazole + Azoxystrobin) composition was tested for its bio efficacy against Blast (Pyriculariaoryzae)&Sheath blight (Rhizoctonia solani)diseases of rice crop, trial was laid out in a randomized block design consisting of eight treatments including control in three replications.
Measured quantity of the chemical was added to required volume of water @ 500 lit. /ha for foliar spraying. The spray tank was filled with ½ the quantity of clean required volume of water and then the measured chemical (according to the dose) was added followed by the rest half quantity of water added. Knapsack sprayer fitted with boom along with flood jet nozzle was used to apply the fungicidal composition.
Synergistic effect of the different Fungicidal compositions:
Synergistic effect was checked using Colby’s method for ternary mixes. In the Colby’s method, for a given combination of three active components, E (expected efficacy) can be expressed as:
E = A+B+C – (AB+AC+BC) + (ABC)
100 1000
Where, E = expected efficacy,
A, B and C = the efficacy of three active ingredients A, B and C at a given dose.
Synergy ratio (R) = experimentally observed efficacy (O)
Expected efficacy (E)
If the synergism ratio (R) between observed and expected is > 1 then synergy is exhibited, if R = 1 then the effect is additive and if R<1 then the mix is antagonistic.
The experimental data was statistically analysed by Randomized Block Design (RBD) (One factor analysis) using OPSTAT HAU statistical software. The results are expressed as Mean +SE (standard error) and data was statistically analyses by one-way analysis of variance (ANOVA), with the level of significance set at p < 0.01.
Evaluation of Bio-efficacy against Blast & Sheath blight disease of Rice-
Disease rating scale for Blast (Pyriculariaoryzae) disease of Rice:
0-9 Scale Lesion area (% infected leaf area)
0 No visible lesions
1 Small brown specs of pin point size or larger brown specks without sporulating center.
3 Small, roundish to slightly elongated necrotic sporulating spots, about 1-2 mm in diameter with a distinct brown margin or yellow.
5 Narrow or slightly elliptical lesions, 1-2 mm in breadth, more than 3 mm long with a brown margin.
7 Broad spindle shaped lesion with yellow, brown or purple margin.
9 Rapidly coalescing small, whitish, grayish or bluish lesions without distinct margins.
Disease rating scale for Sheath blight (Rhizoctonia Solani)disease of Rice:
0-9 Scale Lesion area (% infected leaf area)
0 No lesions
1 Small, brown, specks of pinhead size
3 S small, roundish to slightly elongated, necrotic, grey spots about 1-2 mm in diameter
5 Typically blast lesion, infecting <10% of the leaf area
7 Typically blast lesion, infecting 26-50% of the leaf area
9 All leaves dead
The per cent disease index (PDI) for above mentioned diseases was calculated according to the following formula:
Sum of all numerical rating
Per cent disease index = ×100
Total No. of leaves × Maximum Rating Grade
Table 2: Evaluation of bio-efficacy of Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% against Blast (Pyriculariaoryzae) disease of Rice
T.no. Treatments Dose/ha
a.i.(g/ml)
Formulation
(g/ml)/ha
5 DAT Colby,sValue
10 DAT Colby,sValue
PDI %Control PDI %Control
1 Etofenprox 10% EC 75 750 36.00
(36.85) 12.20
-
47.33
(43.45) 13.94
-
2 Tebuconazole 38.39% SC 191.95 500 22.67
(28.41) 44.72 28.33
(32.14) 48.48
3 Azoxystrobin 23%SC 125 500 23.67
(29.09) 42.28 29.67
(32.98) 46.06
4 Etofenprox 10% EC +Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+125 750+500+500 7.67
(16.06) 81.30 1.13 9.33
(17.77) 83.03 1.09
5 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 24.5+52.5+37.5 500 15.00
(22.77) 63.41 0.88 17.67
(24.83) 67.88 0.89
6 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 36.75+78.75+56.5 750 13.33
(21.40) 67.48 0.94 15.33
(23.02) 72.12 0.95
7 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 49+105+75 1000 12.00
(20.21) 70.73 0.98 13.77
(21.74) 74.97 0.98
8 Untreated Control - - 41.00
(39.79) - - 55.00
(47.85) - -
CD (5%) - - 1.67 - - 1.72 - -
SE(m) - - 0.54 - - 0.56 - -
Figures in parenthesis are angular transformed values
Results:
Results presented in Table 2 showed that incidence of Blast disease reduced in all the treatments. At 5th and 10th DAT, Tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha was found as the best treatment in reducing the incidence to 81.30% and 83.03% control respectively followed by Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @1000 ml/ha with 70.30% and 74.97% control, respectively. Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @750 ml/ha resulted in 67.48% and 72.12% control, whereas, Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @500 ml/ha provided 63.41% and 67.88% control, respectively after 5th and 10th DAT, which were significantly superior in comparison to the solo application of Etofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Blast (Pyricularia oryzae) disease of Rice. Among the treatments mentioned in Table 3, only tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha showed synergistic effect with Colby’s synergistic value of 1.13 and 1.09 on 5th and 10th DAT, respectively.
Table 3. Evaluation of bio-efficacy of Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% against Blast (Pyricularia oryzae) disease of Rice
T. no. Treatments Dose/ha
a.i.(g/ml)
Formulation
(g/ml)/ha
5 DAT Colby,s
Value
10 DAT Colby,s
Value
PDI %Control PDI %Control
1 Etofenprox 10% EC 75 750 35.67
(36.65) 13.01 -
47.00
(43.26) 14.55
-
2 Tebuconazole 38.39% SC 191.95 500 23.00
(28.64) 43.90 28.67
(32.35) 47.88
3 Azoxystrobin 23%SC 125 500 23.83
(29.20) 41.87 30.00
(33.19) 45.45
4 Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+125 750+500+500 7.50
(15.88) 81.71 1.14 9.17
(17.60) 83.33 1.10
5 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 30+70+46 500 12.00
(20.24) 70.73 0.98 14.33
(22.21) 73.94 0.97
6 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 45+105+69 750 7.33
(15.69) 82.11 1.14 8.67
(16.99) 84.24 1.11
7 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 60+140+92 1000 6.83
(15.140 83.33 1.16 8.00
(16.40) 85.45 1.12
8 Untreated Control - - 41.00
(39.79) - - 55.00
(47.85) - -
CD (5%) - - 1.19 - - 1.71 - -
SE(m) - - 0.39 - - 0.56 - -
Figures in parenthesis are angular transformed values
Results presented in Table 3 showed that Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 1000 ml/ha was found most effective with 85.45% control followed by Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@750 ml/ha with 84.24% control, both of the treatments were found at par with tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha with 83.33% control and Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 500 ml/ha resulted in 73.94% control after 10th DAT, which were significantly superior in comparison to the solo application of of Etofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Blast (Pyricularia oryzae) disease of Rice. Among the treatments mentioned in Table 4, Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 1000 ml/ha, Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@750 ml/ha and Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha showed synergistic effect. On 5th and 10th DAT, Colby’s synergistic value of 1.14 and 1.11 was calculated for Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 750 ml/ha.
Table 4. Evaluation of bio-efficacy of Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% against Blast (Pyricularia oryzae) disease of Rice
T. no. Treatments Dose/ha
a.i.(g/ml) Formulation
(g/ml)/ha 5 DAT Colby,sValue 10 DAT Colby,sValue
PDI %Control
-
PDI %Control
-
1 Etofenprox 10% EC 75 750 35.83
(36.71) 12.60 47.17
(43.35) 14.24
2 Tebuconazole 38.39% SC 191.95 500 23.17
(28.75) 43.50 29.00
(32.56) 47.27
3 Azoxystrobin 23%SC 125 500 23.67
(29.07) 42.28 29.67
(32.95) 46.06
4 Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+125 750+500+500 8.00
(16.07) 80.49 1.13 9.70
(17.60) 82.36 1.09
5 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 36.5+88+57 500 11.33
(19.52) 72.36 1.01 13.67
(21.67) 75.15 0.99
6 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 54.75+132+85.5 750 6.33
(14.43) 84.55 1.18 8.00
(16.40) 85.45 1.13
7 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 73+176+114 1000 6.00
(14.04) 85.37 1.19 7.67
(16.06) 86.06 1.14
8 Untreated Control - - 41.00
(39.78) - - 55.00
(47.85) - -
CD (5%) - - 2.84 - - 2.08 - -
SE(m) - - 0.93 - - 0.68 - -
Figures in parenthesis are angular transformed values
Results presented in Table 4 showed that Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 1000 ml/ha was found most effective with 86.06% control followed by Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 750 ml/ha found effective with 85.45% control, both of the treatments were found at par with tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha with 82.36% control and Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 500 ml/ha resulted in 75.15% control after 10th DAT, which were significantly superior in comparison to the solo application of Etofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Blast (Pyriculariaoryzae) disease of Rice. Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 750 ml/ha also showed synergistic effect with Colby’s synergistic value of 1.18 and 1.13 at 5th and 10th DAT, respectively.
Phytotoxicity observations
Various Fungicidal compositions of the present invention provided good control of Blast &Sheath blight disease of Rice as compared to the reference products. Further, the use of these Fungicidal compositions resulted in better crop condition i.e. fresh green leaves and didn’t produce any phytotoxic symptoms on the plants. Table 10-12 depicts the phytotoxic effects of the various fungicidal compositions of the present invention on Rice at 3rd, 5th, 7th and 10th DAT.
Table 5. Evaluation of bio-efficacy of Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% against Sheath blight (Rhizoctoniasolani) disease of Rice
T. no. Treatments Dose/ha
a.i.(g/ml)
Formulation
(g/ml)/ha
5 DAT Colby,s Value
10 DAT Colby,s Value
PDI % Control PDI % Control
1 Etofenprox 10% EC 75 750 37.00
(37.44) 15.27
-
50.67
(45.36) 16.02
-
2 Tebuconazole 38.39% SC 191.95 500 23.33
(28.87) 46.56 30.00
(33.19) 50.28
3 Azoxystrobin 23%SC 125 500 24.33
(29.54) 44.27 31.00
(33.80) 48.62
4 Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+ 125 750+500+ 500 7.83
(16.23) 82.06 1.09 9.67
(18.10) 83.98 1.06
5 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 24.5+52.5+ 37.5 500 14.33
(22.21) 67.18 0.89 17.33
(24.59) 71.27 0.90
6 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 36.75+78.75+ 56.5 750 13.00
(21.11) 70.23 0.93 16.00
(23.56) 73.48 0.93
7 Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% 49+105+75 1000 11.33
(19.64) 74.05 0.99 13.77
(21.74) 77.18 0.98
8 Untreated Control - - 43.67
(41.34) - - 60.33
(50.94) - -
CD (5%) - - 1.62 - - 1.48 - -
SE(m) - - 0.52 - - 0.48 - -
Figures in parenthesis are angular transformed values
Results presented in Table 5 showed that incidence of Sheath blight disease reduced in all the treatments. At 5th and 10th DAT, Tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha was found as the best treatment in reducing the incidence to 82.06% and 83.98% control respectively followed by Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @1000 ml/ha with 74.05% and 77.18% control, respectively. Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @750 ml/ha resulted in 70.23% and 73.48% control, whereas, Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% @500 ml/ha provided 67.18% and 71.27% control, respectively after 5th and 10th DAT, which were significantly superior in comparison to the solo application of Etofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Sheath blight (Rhizoctoniasolani) disease of Rice. Among the treatments mentioned in Table 3, only tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha showed synergistic effect with Colby’s synergistic value of 1.09 and 1.06 on 5th and 10th DAT, respectively.
Table 6. Evaluation of bio-efficacy of Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% against Sheath blight (Rhizoctonia solani) disease of Rice
T. No. Treatments Dose/ha
a.i.(g/ml) Formulation
(g/ml)/ha 5 DAT Colby,s Value
10 DAT Colby,s Value
PDI % Control PDI % Control
1 Etofenprox 10% EC 75 750 37.33
(37.64) 14.50
51.00
(45.55) 15.47
2 Tebuconazole 38.39% SC 191.95 500 23.00
(28.63) 47.33 29.33
(32.77) 51.38
3 Azoxystrobin 23%SC 125 500 24.00
(29.31) 45.04 30.67
(33.60) 49.17
4 Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+ 125 750+500+ 500 7.85
(16.25) 82.02 1.09 9.50
(17.94) 84.25 1.07
5 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 30+70+46 500 12.33
(20.53) 71.76 0.95 15.00
(22.74) 75.14 0.95
6 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 45+105+69 750 6.83
(15.14) 84.35 1.12 8.00
(16.26) 86.74 1.09
7 Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% 60+140+92 1000 6.33
(14.43) 85.50 1.14 7.33
(15.56) 87.85 1.11
8 Untreated Control - - 43.67
(41.34) - - 60.33
(50.94) - -
CD (5%) - - 2.18 - - 3.00 - -
SE(m) - - 0.71 - - 0.98 - -
Figures in parenthesis are angular transformed values
Results presented in Table 6 showed that Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 1000 ml/ha was found most effective with 87.85% control followed by Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@750 ml/ha with 86.74% control, both of the treatments were found at par with tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha with 84.25% control and Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 500 ml/ha resulted in 75.14% control after 10th DAT, which were significantly superior in comparison to the solo application of ofEtofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Sheath blight (Rhizoctoniasolani) disease of Rice. Among the treatments mentioned in Table 4, Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 1000 ml/ha, Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@750 ml/ha and Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha showed synergistic effect. On 5th and 10th DAT, Colby’s synergistic value of 1.12 and 1.09 was calculated for Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2%@ 750 ml/ha.
Table 7. Evaluation of bio-efficacy of Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% against Sheath blight (Rhizoctonia solani) disease of Rice.
T. no. Treatments Dose/ha
a.i.(g/ml) Formulation
(g/ml)/ha 5 DAT Colby,s Value 10 DAT Colby,s Value
PDI % Control PDI % Control
1 Etofenprox 10% EC 75 750 37.50
(37.74) 14.12
51.17
(45.65) 15.19
2 Tebuconazole 38.39% SC 191.95 500 23.17
(28.74) 46.95 29.17
(32.67) 51.66
3 Azoxystrobin 23%SC 125 500 24.17
(29.43) 44.66 30.83
(33.70) 48.90
4 Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC 75+191.95+ 125 750+500+ 500 8.00
(16.40) 81.68 1.09 9.43
(17.87) 84.36 1.06
5 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 36.5+88+57 500 11.67
(19.90) 73.28 0.98 14.00
(21.95) 76.80 0.97
6 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 54.75+132+ 85.5 750 6.33
(14.56) 85.50 1.14 7.67
(15.92) 87.29 1.10
7 Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% 73+176+114 1000 6.00
(14.04) 86.26 1.15 7.00
(15.23) 88.40 1.11
8 Untreated Control - - 43.67
(41.34) - - 60.33
(50.94) - -
CD (5%) - - 2.457 - - 2.636 - -
SE(m) - - 0.802 - - 0.861 - -
Figures in parenthesis are angular transformed values
Results presented in Table 7 showed that Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 1000 ml/ha was found most effective with 88.40% control followed by Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 750 ml/ha found effective with 87.29% control, both of the treatments were found at par with tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23% SC @ 750+500+500 ml/ha with 84.36% control and Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 500 ml/ha resulted in 76.80% control after 10th DAT, which were significantly superior in comparison to the solo application of Etofenprox 10% EC @ 750 ml/ha, Tebuconazole 38.39% SC @ 500 ml/ha and Azoxystrobin 23% SC @ 500 ml/ha against Sheath blight (Rhizoctoniasolani) disease of Rice. Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% @ 750 ml/ha also showed synergistic effect with Colby’s synergistic value of 1.14 and 1.10 at 5th and 10th DAT, respectively.
Example 5: Phytotoxicity observations
Various Fungicidal compositions of the present invention provided good control of Blast &Sheath blight disease of Rice as compared to the reference products. Further, the use of these Fungicidal compositions resulted in better crop condition i.e. fresh green leaves and didn’t produce any phytotoxic symptoms on the plants. Table 8-10 depicts the phytotoxic effects of the various fungicidal compositions of the present invention on Rice at 3rd, 5th, 7th and 10th DAT.
Table 8. Evaluation of Phytotoxicity effect of Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5% against Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctoniasolani) disease of Rice.
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
Table 9. Evaluation of Phytotoxicity effectof Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% against Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctoniasolani) disease of Rice.
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
Table 10. Evaluation of Phytotoxicity effect of Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% against Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctoniasolani) disease of Rice.
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10 3 5 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
Conclusion:
After evaluated of three formulations i.e., (Etofenprox 4.9% + Tebuconazole 10.5% + Azoxystrobin 7.5%, Etofenprox 6% + Tebuconazole 14% Azoxystrobin 9.2% and Etofenprox 7.3% + Tebuconazole 17.6% + Azoxystrobin 11.4% at three different doses @ 500 ml/ha, 750 ml/ha and 1000 ml/ha) Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% @ 750ml/ha was found most effective against Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctonia Solani)diseaseof Rice in comparison to tank mix formulation of Etofenprox 10% EC + Tebuconazole 38.39% SC + Azoxystrobin 23%SC @ 750+500+500 ml/ha. Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% @ 750ml/ha was found at par with higher formulation, higher dose and higher active ingredient and also showed a strong synergistic effect in controlling the Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctonia Solani) disease of Rice.
Therefore, application of Etofenprox 6% + Tebuconazole 14% + Azoxystrobin 9.2% @ 750 ml/h (45+105+69gm a.i/ha) formulation can be recommended for effective control of Blast (Pyriculariaoryzae) & Sheath blight (Rhizoctonia Solani) disease of Rice.
, Claims:
1. An insecticidal composition comprising a synergistic combination of-
a. Etofenprox in an amount ranging from 0.1% to 30.0% by weight;
b. Azoxystrobin is present in an amount ranging from 0.1% to 30.0% by weight;
c. Tebuconazole is present in an amount ranging from 0.1% to 40.0% by weight; and
d. agrochemical acceptable excipient.
2. The insecticidal composition as claimed in claim 1, wherein the agrochemically acceptable excipient is Emulsifier, Dispersing agent, Antifreezing Agent, Adjuvant, Antifoaming agent, Super-Wetting-spreading-penetrating agent, Rheology modifier, pH stabilizer, Solvent and Biocide.
3. The insecticidal composition as claimed in claim 1, wherein the formulation is selected from a suspension concentrate (SC), flowable suspension for seed treatment (FS), oil dispersion (OD), suspo-emulsion (SE), water-dispersible granule (WDG), or wettable powder (WP).
4. The insecticidal composition as claimed in claim 1, wherein the emulsifier is in an amount ranging from 0.1% to 20.0% by weight, selected from selected from but not limited to ethoxylated propoxylated alcohols, alkylphenolethoxylates, alkoxylated tristyrylphenols, calcium dodecylbenzenesulfonate, mixture of fatty acid polyethylene glycol ester, ethoxylated propoxylated polyaryl phenol, ethoxylated fatty acids, fatty alcohol ethoxylates, ethoxylated ricinoleic acid triglycerides, sorbitan trioleate, tridecyl alcohol ethoxylate, castor oil ethoxylate, Calcium dodecylbenzenesulfonate, Dioctyl sulfosuccinate sodium salt, Mixture of fatty acid polyethylene glycol ester, Polyalkoxylated butyl ether block co-polymer, alkoxylated phosphate ester.
5. The insecticidal composition as claimed in claim 1, wherein the dispersing agent is in an amount ranging from 0.1% to 20.0% by weight, selected from selected from but not limited to polymeric ester dispersants, ethoxylated polyarylphenol phosphate esters, or sodium salt of naphthalene sulfonate condensate, acrylic copolymer,nonionic proprietary surfactant blend, polycarboxylates, calcium dodecylbenzene sulfonate, sodium lignosulphonate, polystyrenatedacrylated co-polymer, modified styrene acrylic copolymer, salts of phenol sulfonic acids, butyl polyalkylene oxide block co-polymer, mixture of tristyrylphenolethoxylates and polyalkylene oxide derivative of a synthetic alcohol, random co-polymer of alcoxylated polyethylene glycol.
6. The insecticidal composition as claimed in claim 1, wherein the antifoaming agent is in an amount ranging from 0.01% to 5.0% by weight, selected from selected from but not limited to polydimethylsiloxane or polydimethyl siloxane emulsion.
7. The insecticidal composition as claimed in claim 1, wherein the rheology modifier is in an amount ranging from 0.01% to 20.0% by weight, selected from precipitated silica, fumed silica, modified fumed silica, bentonite clay, Rhodopol 23, hydroxymethyl cellulose, carboxymethyl cellulose, xanthan gum, thickening silica, hydrated clay minerals, magnesium aluminium silicates, organic derivative of hectorite clay, hydrophobic fumed silica, polyvinylpyrrolidone.
8. The insecticidal composition as claimed in claim 1, wherein the solvent component in an amount ranging up to 95.0% of the composition by weight, selected from selected from but not limited to demineralized water or oil media, wherein, oil medium selected from the group comprising, esterified fatty acids selected from methylethyl ester of vegetable oil triglycerides containing C12–C22 saturated and unsaturated fatty acid.
9. The insecticidal composition as claimed in claim 1, wherein the biocide is in an amount ranging up to3.0% by weight, selected from but not limited to 1,2-benzisothiazolin-3-one or formaldehyde-based solutions or dipropylene glycol solution of 1,2-benzisothiazolin-3-one.
10. The insecticidal composition as claimed in claim 1, wherein the antifreezing agent is in an amount ranging up to 15% by weight, selected from but not limited to ethylene glycol or propane-1,2-diol or propane-1,2,3-triol, urea.
11. The insecticidal composition as claimed in claim 1, wherein the stabilizing agent is in an amount ranging up to 5% by weight, selected from but not limited to epoxidized soyabean oil, butylated hydroxy toluene, ethylenediaminetetraacetic acid.
12. The insecticidal composition as claimed in claim 1, wherein the pH Stablizer is in an amount ranging up to 0.01 to 0.10% by weight, selected from but not limited to sodium pyrophosphate, sodium acetate, sodium oxalate, sodium carbonate, sodium bicarbonate, trisodium phosphate, citric acid, trisodium citrate, monoethanol amine, triethanol amine, triethylamine, dibasic esters selected from dimethyl succinate, dimethyl glutarate, dimethyl adipate, ortho phosphoric acid, oxalic acid, citric acid, hydrochloric acid.
13. The insecticidal composition as claimed in claim 1, wherein the Super-Wetting-spreading-penetrating agent is in an amount ranging up to 0.1 to 5.0% by weight, Super-Wetting-spreading-penetrating agent is blend of methylated seed oil-organic silicone compound may be selected from methylated seed oil-polyalkyleneoxide modified trisiloxane, methylated seed oil-polyalkyleneoxide modified polydimethylsiloxane, methylated seed oil-20 trisiloxane ethoxylate, methylated seed oil-polyoxyethylene methyl polysiloxane, methylated seed oil-polyether polymethyl siloxane copolymer, methylated seed oil-polyether modified polysiloxane.
14. A process for preparing a Suspo-emulsion composition comprising the steps of-
a. mixing Etofenprox with polyalkoxylated butyl ether and ethoxylated tristyrylphenol to create the Etofenprox oil phase.
b. adding dipropylene glycol solution of 1,2-benzisothiazolin-3-one, polydimethylsiloxane emulsion, propane-1,2,3-triol, a nonionic surfactant blend, and acrylic copolymer to demineralized water in a pre-mixing vessel with a homogenizer.
c. homogenizing the mixture until uniform.
d. introducing Acetamiprid and Diafenthiuron, and mixing to obtain a slurry.
e. reducing the particle size of the slurry using a jacketed bead mill to achieve d(90) less than 20 microns.
f. collecting the aqueous phase into a mixing vessel.
g. adding the Etofenprox oil phase to the aqueous phase under continuous agitation.
h. incorporating a pH adjuster, stabilizer, and Rhodopol 23, then agitating to form the insecticidal suspo-emulsion composition.
15. A process for preparing an Oil-dispersion composition comprising the steps of-
a. adding polyalkylene oxide modified heptamethyltrisiloxane, polydimethylsiloxane, propane-1,2,3-triol, castor oil ethoxylate, calcium dodecylbenzenesulfonate, ethoxylated polyarylphenol phosphate ester, and a fatty acid polyethylene glycol ester mixture to methyl ester of vegetable oil in a pre-mixing vessel with a homogenizer.
b. mixing until uniform.
c. incorporating Etofenprox, Diafenthiuron, and Acetamiprid, and mixing to create a slurry.
d. reducing the particle size of the slurry using a jacketed bead mill to achieve d(90) less than 20 microns.
e. collecting the milled slurry into a post mixing vessel.
f. adding a pH stabilizer, bentonite clay, and fumed silica under stirring.
g. mixing until homogeneous to form the insecticidal Oil-dispersion formulation.
| # | Name | Date |
|---|---|---|
| 1 | 202411104222-STATEMENT OF UNDERTAKING (FORM 3) [29-12-2024(online)].pdf | 2024-12-29 |
| 2 | 202411104222-FORM FOR SMALL ENTITY(FORM-28) [29-12-2024(online)].pdf | 2024-12-29 |
| 3 | 202411104222-FORM FOR SMALL ENTITY [29-12-2024(online)].pdf | 2024-12-29 |
| 4 | 202411104222-FORM 1 [29-12-2024(online)].pdf | 2024-12-29 |
| 5 | 202411104222-FIGURE OF ABSTRACT [29-12-2024(online)].pdf | 2024-12-29 |
| 6 | 202411104222-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [29-12-2024(online)].pdf | 2024-12-29 |
| 7 | 202411104222-EVIDENCE FOR REGISTRATION UNDER SSI [29-12-2024(online)].pdf | 2024-12-29 |
| 8 | 202411104222-DECLARATION OF INVENTORSHIP (FORM 5) [29-12-2024(online)].pdf | 2024-12-29 |
| 9 | 202411104222-COMPLETE SPECIFICATION [29-12-2024(online)].pdf | 2024-12-29 |
| 10 | 202411104222-FORM-26 [10-02-2025(online)].pdf | 2025-02-10 |
| 11 | 202411104222-FORM-9 [13-02-2025(online)].pdf | 2025-02-13 |
| 12 | 202411104222-MSME CERTIFICATE [19-02-2025(online)].pdf | 2025-02-19 |
| 13 | 202411104222-FORM28 [19-02-2025(online)].pdf | 2025-02-19 |
| 14 | 202411104222-FORM 18A [19-02-2025(online)].pdf | 2025-02-19 |
| 15 | 202411104222-Proof of Right [26-03-2025(online)].pdf | 2025-03-26 |
| 16 | 202411104222-FER.pdf | 2025-05-26 |
| 17 | 202411104222-OTHERS [15-07-2025(online)].pdf | 2025-07-15 |
| 18 | 202411104222-FORM 3 [15-07-2025(online)].pdf | 2025-07-15 |
| 19 | 202411104222-FER_SER_REPLY [15-07-2025(online)].pdf | 2025-07-15 |
| 20 | 202411104222-CLAIMS [15-07-2025(online)].pdf | 2025-07-15 |
| 21 | 202411104222-US(14)-HearingNotice-(HearingDate-22-09-2025).pdf | 2025-08-26 |
| 22 | 202411104222-Correspondence to notify the Controller [30-08-2025(online)].pdf | 2025-08-30 |
| 23 | 202411104222-PRE GRANT OPPOSITION FORM [19-09-2025(online)].pdf | 2025-09-19 |
| 24 | 202411104222-PRE GRANT OPPOSITION DOCUMENT [19-09-2025(online)].pdf | 2025-09-19 |
| 25 | 202411104222-FORM-26 [22-09-2025(online)].pdf | 2025-09-22 |
| 26 | 202411104222-Written submissions and relevant documents [24-09-2025(online)].pdf | 2025-09-24 |
| 27 | 202411104222-Response to office action [29-09-2025(online)].pdf | 2025-09-29 |
| 1 | 202411104222_SearchStrategyNew_E_ssE_21-05-2025.pdf |