Description:FIELD OF THE INVENTION:
The present invention relates to synergistic insecticidal compositions comprising bioactive amounts of (A) Etofenprox; (B) Diafenthiuron (C) Pyriproxyfen. The present invention further relates to process of preparing said composition along with at least one inactive excipients and formulation thereof..
BACKGROUND OF THE INVENTION:
Combination of insecticides are used to broaden the spectrum of control of insect, to improve the pest control with synergistic effect, reduce dosage, thereby reducing environmental impact, to broaden the spectrum of control, i.e. chewing and sucking insects at a time, decrease chances of development and management of resistance and to enhance residual control so lesser the number of sprays for crop protections and minimizing the pesticidal load in ecosystem. The combination of insecticides at times demonstrate an additive or synergistic effect that results in an improved control on the pests.
Insecticide or pesticides are used widely and very frequently in commercial agriculture and have enabled an enormous increase in crop yields and product quality which ultimately increased the ease to farmers in term of economic advantage as well as ease of farming activities.
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 name1-ethoxy-4-[2-methyl-1-[(3-phenoxyphenyl)methoxy]propan-2-yl]benzenehaving chemical structure as:

ETOFENPROX
Diafenthiuron with CAS registration number 80060-09-9, is an aromatic ether that is 1,3-diisopropyl-5-phenoxybenzene in which the hydrogen atom at position 2 is substituted by a (tert-butylcarbamothioyl) nitrilo group. An agricultural insecticide which is used to control mites, aphids and whitefly in cotton. It has a role as an oxidative phosphorylation inhibitor and an insecticide. It is a thiourea acaricide, a thiourea insecticide and an aromatic ether. It is functionally related to a diphenyl ether.
It has an IUPAC name 1-tert-butyl-3-[4-phenoxy-2,6-di(propan-2-yl)phenyl]thiourea having chemical structure as:

DIAFENTHIURON
PyriproxyfenwithCAS registration number 95737-68-1. It is an aromatic ether and a member of pyridines. It is functionally related to a4-phenoxyphenol. It is a pyridine-based pesticide which is found to be effective against a variety of arthropoda. It was introduced to the US in 1996, to protect cotton crops against whitefly. It has also been found useful for protecting other crops. It is also used as a prevention for fleas on household pets.
It has an IUPAC name IUPAC name 2-[1-(4-phenoxyphenoxy)propan-2-yloxy]pyridine having chemical structure as below:

PYRIPROXYFEN
OBJECT OF THE INVENTION
The main objective of the disclosure is to provide a synergistic insecticidal composition combining Etofenprox, Diafenthiuron, and Pyriproxyfen 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 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 pests, including whiteflies, Jassids, across different crops like cotton and chili.
Another object of the present disclosure is toreduce the likelihood of pest resistance by utilizing a multi-component approach, thereby decreasing the dependence on single-action insecticides.
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
Accordingly, in one aspect, the present invention provides an insecticide composition comprising Etofenprox, Diafenthiuron, and Pyriproxyfen.
In one aspect, the present invention provides a synergistic composition of Etofenprox, Diafenthiuron, and Pyriproxyfen and agrochemically acceptable additives.
In yet another aspect, the present invention provides a synergistic composition comprising Etofenprox, Diafenthiuron, and Pyriproxyfen, the composition possesses Insecticidal activity.
In a further aspect, the present invention provides a method for effective control of various pest in plants.
In one aspect of the present invention, the Insecticidal composition of the present invention further comprises an agrochemically acceptable excipients selected from the group consisting of anti-freezing agent, dispersing agents, wetting agents, antifoaming agents, biocides, thickeners, Super-Wetting-spreading-penetrating agent, surfactants, preservatives, colorants, pigments, buffers, solvents, and the like. Additional components may also be included, e.g., protective colloids, adhesives, thickeners, thixotropic agents, penetration agents, stabilisers, sequestering agents.
In another aspect of the present invention, the Insecticidal composition is formulated as capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG) Emulsifiable water-in-oil (EO), Emulsifiable powder (EP), Emulsifiable for seed treatment (ES), Emulsifiable oil-in-water (EW), flowable concentrate for seed treatment (FS), Suspension Concentrate (SC), Suspo-emulsion (SE), Oil Dispersion (OD).Water dispersible powder for slurry seed treatment (WS), Water dispersible granules (WDG) and Wettable powders (WP), a mixed formulation of CS and SC (ZC), soluble liquid (SL).
In another further aspect the insecticidal composition of the present invention is preferably formulated as a Suspo-emulsion (SE) and Oil Dispersion (OD).
In yet 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 capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG) Emulsifiable water-in-oil (EO), Emulsifiable powder (EP), Emulsifiable for seed treatment (ES), Emulsifiable oil-in-water (EW), flowable concentrate for seed treatment (FS), Suspension Concentrate (SC), Suspo-emulsion (SE), Water dispersible powder for slurry seed treatment (WS), Water dispersible granules (WDG) and Wettable powders (WP), a mixed formulation of CS and SC (ZC), soluble liquid (SL).
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 “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, Diafenthiuron, and Pyriproxyfen.
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 Insecticidal composition wherein the Diafenthiuron ranging from 0.1% to 30.0% by weight of the Insecticidal composition.
In an embodiment, the Insecticidal composition wherein the Pyriproxyfen ranging from 0.1% to 30.0% by weight of the Insecticidal 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 Suspension Concentrate (SC), Suspo-emulsion (SE), oil dispersion (OD), Water dispersible granules (WDG), Granules (GR) and Wettable powders (WP).
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, Super-Wetting-spreading-penetrating agent, Rheology modifiers, solvents, biocides, pH stabilizers, Stabilizing agents and anti-freezing agents .
Emulsifiers is selected from the group comprising of, but not limited to ethoxylated propoxylated alcohols, alkylphenol ethoxylates, alkoxylatedtristyrylphenols, calcium dodecyl benzenesulfonate, 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, alkoxylated phosphate ester or mixtures thereof; These binders or adhesive imparting agents may be used alone or in combination 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.
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, Acrylic copolymer, polycarboxylates, calcium dodecylbenzene sulfonate, aryl sulphonate condensate,sodium lignosulphonate, dispertox BS SPL, Polymeric ester dispersant, Ethoxylated polyarylphenol phosphate ester polystyrenated acrylated co-polymer, modified styrene acrylic copolymer, salts of phenol sulfonic acids, Terwet 2700,butyl polyalkylene oxide block co-polymer, Polymeric ester dispersant, 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, organic derivative of hectorite clay, hydrophobic fumed silica, Rhodopol 23, Precipitated 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.
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, Polyalkyleneoxide modified heptamethyltrisiloxane 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.
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.
pH stabilizers 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% to 10% by weight based on a total weight of the composition.
The composition of the present invention is effective for management of insect 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 combination or composition comprising of Etofenprox, Diafenthiuron, and Pyriproxyfen 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 composition as Suspo-emulsion (SE) formulation:
In an embodiment, the chemical composition of the present insecticidal is depicted below in Table 1 below:

Table 1: Insecticidal Composition for Suspo-emulsion (SE) Formulation.
Component Composition (%w/w) Remark
Etofenprox 7.50 Active Ingredient
Diafenthiuron 31.0 Active Ingredient
Pyriproxyfen 7.00 Active Ingredient
Polyalkoxylated butyl ether block co-polymer 2.00 Emulsifier
Ethoxylated tristyrylphenol 2.00 Emulsifier
Nonionic proprietary surfactant blend 2.00 Dispersing agent
Acrylic copolymer 2.00 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 1.00 Stabilizing agent
Precipitated silica 1.00 Rheology modifier
Rhodopol 23 0.10 Rheology modifier
Demineralizedwater Balance to 100 Solvent

Process for preparing Suspo-emulsion (SE)formulation:
Preparation of Etofenprox oil phase
The active ingredient Etofenprox was mixed with polyalkoxylated butyl ether block co-polymer and ethoxylated tristyrylphenol under stirring to form Etofenprox oil phase.
Preparation of aqueous phase of Diafenthiuron and Pyriproxyfen
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 copolymeras 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, Pyriproxyfen, Diafenthiuron 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 Diafenthiuron and Pyriproxyfen of desirable particle size of d(90)<20 micron. The aqueous phase of Diafenthiuron and Pyriproxyfen 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 Diafenthiuron and Pyriproxyfen 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 insecticidal suspo-emulsion (SE) formulation.
Example 2: Preparation of insecticidal composition as Oil Dispersion (OD) formulation:
Table-1 (b): Insecticidal Composition of the Oil Dispersion (OD) formulation
Component Composition (%w/w) Remark
Etofenprox 3.75 Active Ingredient
Diafenthiuron 15.5 Active Ingredient
Pyriproxyfen 3.5 Active Ingredient
Castor oil ethoxylate (10 mole) 6.00 Emulsifier
Calcium dodecylbenzenesulfonate 2.00 Emulsifier
Mixture of fatty acid polyethylene glycol ester 4.00 Emulsifier
Polymeric ester dispersant 0.50 Dispersing agent
Ethoxylated polyarylphenol phosphate ester 0.50 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 dodecylbenzene sulfonate, ethoxylated polyarylphenol phosphate ester, mixture of fatty acid polyethylene glycol ester and polymeric ester dispersant as mentioned in Table 2were 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, Diafenthiuron and Pyriproxyfen were added to the obtained mixture and continued to mix for sufficient time with the homogenizer to obtain 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 insecticidal Oil Dispersion (OD) formulation.
Example 3: Preparation of insecticidal composition as Water Dispersible Granules (WDG)formulation:

Table-1 (c): Insecticidal Composition for Water dispersible granule (WDG).
Component Quantity
(% w/w) Function
Etofenprox 7.50 Active Ingredient
Diafenthiuron 31.0 Active Ingredient
Pyriproxyfen 7.00 Active Ingredient
Sodium lauryl sulphate 3.00 Wetting agent
Sodium salt of naphthalene sulfonate condensate 3.00 Dispersing agent
Sodium ligno sulfonate 3.00 Dispersing agent
Polyoxyethylene sorbitan monooleate 1.00 Wetting agent
Polyoxyethylene Ether 1.00 Wetting agent
Polyalkoxylated butyl ether block co-polymer 1.50 Emulsifier
Ethoxylated tristyrylphenol 1.50 Emulsifier
Polydimethylsiloxane emulsion 0.50 Antifoaming agent
Citric acid 0.50 pH modifier
Ammonium sulphate 1.00 Inert carrier
Precipitated silica 2.00 Inert carrier
Kaolin QS Inert carrier

Process for preparing Water dispersible granule (WDG)formulation:
The required amounts of Diafenthiuron and Pyriproxyfen technical, sodium lauryl sulphate, sodium salt of naphthalene sulfonate condensate, Sodium ligno sulfonate, citric acid, polyvinylpyrrolidone, ammonium sulphate, precipitated silica and kaolin were blended with suitable equipment. The mixture was milled with appropriate equipment to form Diafenthiuron and Pyriproxyfen milled pre-mix. To this milled pre-mix required amount of Etofenprox technical, polyoxyethylene sorbitan monooleate, polyoxyethylene ether, polyalkoxylated butyl ether block co-polymer, ethoxylated tristyrylphenol and polydimethylsiloxane emulsion were blended. Then dough was prepared by adding appropriate amount of water. The dough was extruded with the help of a suitable extruder. The extrudes were dried with appropriate equipment. The dried extrude was sieved to form insecticidal composition of Etofenprox, Diafenthiuron and Pyriproxyfen water dispersible granules.
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 insecticidal formulation composition of examples 1 - 2 were found stable during accelerated stability study at 54±2° C for 14 days and low temperature at 0 ± 2°C for 7 days.The insecticidal formulation composition of example 3 was found stable during accelerated stability study at 54±2° C for 14 days.
Synergistic effect of the different Insecticidal Composition:
Synergisticeffect 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 10000
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 analysed by one-way Analysis of variance (ANOVA), with the level of significance set at p < 0.01.
Example 4: Evaluation of Bio-efficacy of insecticidal Composition and thereof (Etofenprox + Diafenthiuron + Pyriproxyfen) against whitefly on Chilli crop.
For the evaluation of Phytotoxicity on cotton crop observations were made by observing the temporary or long lasting damage to the leaves if any viz., yellowing, wilting, necrosis, epinasty and hyponasty at 5, 10 and 15DAT of the synergistic insecticidal composition of the present invention. Crop injury was observed on visual rating from 0-10 scale .

Phytotoxicity rating scale
Rating Crop Injury (%) Verbal Description
0 - No symptoms
1 1-10 Verbal slight discoloration
2 11-20 More severe, but not lasting
3 21-30 Moderate and more lasting
4 31-40 Medium and lasting
5 41-50 Moderately heavy
6 51-60 Heavy
7 61-70 Very heavy
8 71-80 Nearly destroyed
9 81-90 Destroyed
10 91-100 Completely destroyed

Table 2: Effect of different treatments on population of whitefly in chillicrop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of whitefly per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 7.55
(2.92) 7.67
(2.94) 41.07 8.69
(3.11) 10.80
(3.43) 44.43
2 Diafenthiuron 50% WP 300 600 6.67
(2.76) 6.03
(2.65) 53.63 6.47
(2.73) 9.08
(3.17) 53.26
3 Pyriproxyfen 10% EC 100 1000 6.76
(2.78) 6.77
(2.78) 47.99 6.85
(2.80) 8.26
(3.04) 57.48
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 2.60
(1.92) 1.40
(1.54) 89.24 1.003 2.00
(1.72) 1.97
(1.72) 89.88 1.010
5 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 42.25 + 175.50 + 42.25 650 3.40
(2.09) 2.67
(1.91) 79.50 0.894 2.73
(1.93) 3.00
(1.99) 84.56 0.951
6 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 48.75 + 202.50 + 48.75 750 2.93
(1.97) 2.03
(1.73) 84.37 0.948 2.27
(1.80) 2.60
(1.89) 86.62 0.974
7 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 55.25 + 229.50 + 55.25 850 2.73
(1.93) 1.73
(1.65) 86.68 0.974 2.20
(1.78) 2.50
(1.87) 87.14 0.980
8 Untreated Check - - 11.00
(3.46) 13.01
(3.74) 15.80
(4.09) 19.43
(4.51)
CD at 5% 0.174 0.176 0.146 0.147
SE (m) 0.057 0.058 0.048 0.048
Figure in parenthesis represents square root transformed value

Results:
a) Whitefly :Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 6.5 % + Diafenthiuron 27 % + Pyriproxyfen 6.5 % @ 55.25 + 229.50 + 55.25 gm a.i./ha and @ 48.75 + 202.50 + 48.75 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent whitefly per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.88 %, 87.14 % and 86.62 % reduction over control at 10th DAT, respectively.
All the doses of Etofenprox 6.5% + Diafenthiuron 27 % + Pyriproxyfen 6.5 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (44.43%), Diafenthiuron 50% @ 300 gm a.i /ha (53.26 %) andPyriproxyfen10 % @ 100 gm a.i /ha (57.48 %) against whitefly in Chilli at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@75 + 300 + 100 gm a.i./ha showed synergistic effect with the synergistic ratio 1.010 (>1) at 10 DAT (Table 2)

Table 3: Effect of different treatments on population of whitefly in Chilli crop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of whitefly per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 7.45
(2.90) 8.63
(3.10) 42.50 9.08
(3.17) 11.23
(3.49) 44.84
2 Diafenthiuron 50% WP 300 600 7.07
(2.83) 6.46
(2.73) 56.98 6.47
(2.73) 9.13
(3.18) 55.19
3 Pyriproxyfen 10% EC 100 1000 6.50
(2.73) 5.88
(2.62) 60.83 6.87
(2.80) 8.74
(3.12) 57.07
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 2.8
(1.95) 1.60
(1.60) 89.34 0.999 2.10
(1.75) 2.13
(1.76) 89.53 1.002
5 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 48.75 + 201.50 + 45.50 650 3.23
(2.05) 2.17
(1.77) 85.57 0.957 2.50
(1.86) 2.77
(1.94) 86.42 0.967
6 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 56.25 + 232.50 + 52.50 750 2.86
(1.96) 1.63
(1.61) 89.12 0.997 1.97
(1.72) 2.07
(1.75) 89.85 1.005
7 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 63.75 + 263.50 + 59.50 850 2.87
(1.96) 1.57
(1.59) 89.56 1.002 1.80
(1.67) 1.97
(1.72) 90.34 1.011
8 Untreated Check - - 12.34
(3.65) 15.01
(4.00) 17.46
(4.29) 20.37
(4.62)
CD at 5% 0.189 0.190 0.164 0.152
SE (m) 0.062 0.062 0.054 0.050
Figure in parenthesis represents square root transformed value

Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 % @ 63.75 + 263.50 + 59.50 gm a.i./ha and @ 56.25 + 232.50 + 52.50 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent whitefly per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.53 %, 90.34 % and 89.85 % reduction over control at 10th DAT, respectively.

All the doses of Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (44.84%), Diafenthiuron 50% @ 300 gm a.i /ha (55.19 %) andPyriproxyfen10 % @ 100 gm a.i /ha (57.07 %) against whitefly in Chilli at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@75 + 300 + 100 gm a.i./ha showed synergistic effect with the synergistic ratio 1.002, 1.011 and 1.005 (>1) at 10 DAT (Table 3)


Table 4: Effect of different treatments on population of whitefly in chilli crop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of whitefly per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 8.23
(3.03) 8.77
(3.12) 38.88 9.10
(3.17) 11.50
(3.53) 45.41
2 Diafenthiuron 50% WP 300 600 6.63
(2.75) 6.73
(2.78) 53.06 6.47
(2.73) 9.46
(3.23) 55.08
3 Pyriproxyfen 10% EC 100 1000 6.76
(2.78) 6.15
(2.67) 57.12 6.87
(2.80) 8.99
(3.16) 57.33
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 4.2
(2.28) 1.47
(1.56) 89.77 1.003 1.97
(1.71) 2.17
(1.77) 89.72 1.002
5 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9 55.25 + 224.25 + 58.50 650 4.56
(2.35) 2.13
(1.76) 85.13 0.951 2.23
(1.79) 2.77
(1.93) 86.87 0.970
6 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9% 63.75 + 258.75 + 67.50 750 3.13
(2.02) 1.80
(1.67) 87.45 0.977 2.00
(1.72) 1.80
(1.66) 91.46 1.021
7 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9% 72.25 + 293.25 + 76.50 850 2.93
(1.98) 1.43
(1.55) 90.01 1.005 1.90
(1.70) 1.67
(1.62) 92.09 1.029
8 Untreated Check - - 12.07
(3.61) 14.34
(3.91) 17.80
(4.33) 21.07
(4.69)
CD at 5% 0.192 0.176 0.187 0.205
SE (m) 0.063 0.057 0.061 0.067
Figure in parenthesis represents square root transformed value

Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 8.5 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % @ 72.25+ 293.25 + 76.50 gm a.i./ha and @ 72.25 + 293.25 + 76.50 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent whitefly per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.72 %, 92.09 % and 91.46 % reduction over control at 10th DAT, respectively.
All the doses of Etofenprox 8.5 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (45.41%), Diafenthiuron 50% @ 300 gm a.i /ha (55.08 %) andPyriproxyfen10 % @ 100 gm a.i /ha (57.33 %) against whitefly in Chilli at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@ 75 + 300 + 100 gm a.i./ha showed synergistic effect with the synergistic ratio 1.002, 1.029 and 1.021 (>1) at 10 DAT (Table 4)
Conclusion
After evaluation of three formulations i.e., Etofenprox 6.5 % + Diafenthiuron 27 % + Pyriproxyfen 6.5 %Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 and Etofenprox 8.4 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % EC at three different doses (650 ml/ ha, 750 ml/ha & 850 ml/ha)., Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 EC @ 750 ml/ha
found to be effective against whitefly in chillicrop in comparison to tank mix formulation Tank mix formulation (Etofenprox 10% EC + Diafenthiuron 50% WP +Pyriproxyfen 10 % EC) as well as solo treatments (Etofenprox 10 % EC, Diafenthiuron 50 % WP and Pyriproxyfen 10% EC) Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 % EC @ 750 ml/ha. was found at par with higher formulation, higher dose and higher active ingredient.

Example 5: Evaluation of Bio-efficacy of insecticidal Composition and thereof (Etofenprox + Diafenthiuron + Pyriproxyfen) against Jassids on Cotton crop.
Table 5: Effect of different treatments on population of Jassids in cotton crop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Jassids per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 6.27
(2.69) 6.60
(2.75) 52.17 7.23
(2.86) 8.23
(3.03) 52.95
2 Diafenthiuron 50% WP 300 600 5.30
(2.50) 6.10
(2.66) 55.80 6.73
(2.78) 7.60
(2.93) 56.57
3 Pyriproxyfen 10% EC 100 1000 4.97
(2.44) 5.80
(2.60) 57.97 6.00
(2.64) 7.10
(2.84) 59.43
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 3.13
(2.03) 1.4
(1.55) 89.61 1.007 2.27
(1.80) 1.80
(1.67) 89.71 1.009
5 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 42.25 + 175.50 + 42.25 650 3.40
(2.09) 2.30
(1.81) 83.33 0.937 2.53
(1.87) 2.70
(1.92) 84.57 0.951
6 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 48.75 + 202.50 + 48.75 750 3.20
(2.04) 2.00
(1.72) 85.51 0.961 1.90
(1.70) 2.47
(1.85) 85.90 0.966
7 Etofenprox 6.5% +Diafenthiuron 27% + Pyriproxyfen 6.5% 55.25 + 229.50 + 55.25 850 3.03
(2.00) 1.87
(1.69) 86.47 0.972 1.70
(1.64) 2.17
(1.77) 87.62 0.985
8 Untreated Check - - 10.63
(3.41) 13.80
(3.84) 15.07
(4.00) 17.50
(4.30)
CD at 5% 0.167 0.195 0.169 0.197
SE (m) 0.055 0.064 0.055 0.064
Figure in parenthesis represents square root transformed value

Results :
(a) Jassids
Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 6.5 % + Diafenthiuron 27 % + Pyriproxyfen 6.5 % @ 55.25 + 229.50 + 55.25 gm a.i./ha and @ 48.75 + 202.50 + 48.75 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent Jassids per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.88 %, 87.14 % and 86.62 % reduction over control at 10th DAT, respectively.
All the doses of Etofenprox 6.5% + Diafenthiuron 27 % + Pyriproxyfen 6.5 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (44.43%), Diafenthiuron 50% @ 300 gm a.i /ha (53.26 %) andPyriproxyfen10 % @ 100 gm a.i /ha (57.48 %) against Jassids in cotton at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@75 + 300 + 100gm a.i./ha showed synergistic effect with the synergistic ratio 1.010 (>1) at 10 DAT (Table 5).

Table 6: Effect of different treatments on population of Jassids in cotton crop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Jassids per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 5.60
(2.56) 6.73
(2.78) 52.02 7.27
(2.87) 8.10
(3.01) 54.41
2 Diafenthiuron 50% WP 300 600 5.20
(2.48) 6.30
(2.70) 55.11 6.63
(2.76) 7.20
(2.86) 59.47
3 Pyriproxyfen 10% EC 100 1000 4.97
(2.44) 5.83
(2.61) 58.43 6.23
(2.68) 7.07
(2.84) 60.23
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 3.37
(2.08) 1.40
(1.54) 90.02 1.007 2.00
(1.72) 1.83
(1.68) 89.68 1.003
5 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 48.75 + 201.50 + 45.50 650 3.47
(2.11) 2.07
(1.75) 85.27 0.954 2.33
(1.82) 2.40
(1.84) 86.49 0.968
6 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 56.25 + 232.50 + 52.50 750 2.40
(1.84) 1.40
(1.54) 90.02 1.007 2.03
(1.73) 1.70
(1.64) 90.43 1.012
7 Etofenprox 7.5 % +Diafenthiuron 31 % + Pyriproxyfen 7.0% 63.75 + 263.50 + 59.50 850 2.23
(1.79) 1.37
(1.53) 90.26 1.010 1.80
(1.67) 1.53
(1.58) 91.37 1.022
8 Untreated Check - - 11.37
(3.51) 14.03
(3.87) 15.50
(4.06) 17.77
(4.33)
CD at 5% 0.176 0.182 0.201 0.158
SE (m) 0.061 0.060 0.066 0.052
Figure in parenthesis represents square root transformed value

Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 % @ 63.75 + 263.50 + 59.50 gm a.i./ha and @ 56.25 + 232.50 + 52.50 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent Jassids per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.68 %, 91.37 % and 90.43 % reduction over control at 10th DAT, respectively.
All the doses of Etofenprox 7.5% + Diafenthiuron 31 % + Pyriproxyfen 7.0 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (54.41%), Diafenthiuron 50% @ 300 gm a.i /ha (59.47 %) andPyriproxyfen10 % @ 100 gm a.i /ha (60.23 %) against Jassids in cotton at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@75 + 300 + 100 gm a.i./ha showed synergistic effect with the synergistic ratio 1.003,1.022 and 1.012 (>1) at 10 DAT (Table 6)

Table 7: Effect of different treatments on population of Jassids in cotton crop.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Jassids per leaf
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS % Control
5 DAS Colby Value 5 DAS 7 DAS 10 DAS % Control
10 DAS Colby Value 10 DAS
1 Etofenprox 10% EC 75 750 5.27
(2.50) 5.97
(2.63) 57.88 6.90
(2.81) 7.87
(2.97) 57.32
2 Diafenthiuron 50% WP 300 600 4.90
(2.42) 6.40
(2.72) 54.82 6.53
(2.74) 7.53
(2.92) 59.13
3 Pyriproxyfen 10% EC 100 1000 5.30
(2.51) 5.83
(2.61) 58.82 6.00
(2.64) 6.93
(2.81) 62.39
4 Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC 75 + 300 + 100 750+600+1000 3.37
(2.08) 1.4
(1.54) 90.12 1.007 1.90
(1.70) 1.90
(1.70) 89.69 1.002
5 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9 55.25 + 224.25 + 58.50 650 3.90
(2.21) 2.27
(1.80) 84.00 0.938 2.50
(1.87) 2.30
(1.81) 87.52 0.978
6 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9% 63.75 + 258.75 + 67.50 750 3.07
(2.01) 1.43
(1.55) 89.88 1.004 1.93
(1.71) 1.73
(1.65) 90.60 1.012
7 Etofenprox 8.5 % +Diafenthiuron 34.50 % + Pyriproxyfen 9% 72.25 + 293.25 + 76.50 850 2.80
(1.94) 1.33
(1.52) 90.59 1.012 1.60
(1.61) 1.50
(1.58) 91.86 1.026
8 Untreated Check - - 12.10
(3.61) 14.17
(3.89) 16.10
(4.13) 18.43
(4.40)
CD at 5% 0.153 0.127 0.168 0.160
SE (m) 0.050 0.041 0.055 0.052
Figure in parenthesis represents square root transformed value

Among all the doses rates of combination and individual treatment, Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10% EC @ 75 + 300 + 100 gm a.i./ha and Etofenprox 8.5 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % @ 72.25 + 293.25 + 76.50 gm a.i./ha and @ 63.75 + 258.75 + 67.50 gm a.i./ha, treated plots were observed with highest per cent reduction over control, along with lowest per cent whitefly per leaf at 3rd, 5th, 7th and 10th days after treatment (DAT) in comparison with other treatments. All the three doses showed 89.69 %, 91.86 % and 90.60 % reduction over control at 10th DAT, respectively.
All the doses of Etofenprox 8.5 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % showed better result compared to individual application of Etofenprox 10% EC @ 75 gm a.i./ha (57.32%), Diafenthiuron 50% @ 300 gm a.i /ha (59.13 %) andPyriproxyfen10 % @ 100 gm a.i /ha (62.39 %) against whitefly in cotton at 10 DAT. The application of Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC@75 + 300 + 100 gm a.i./ha showed synergistic effect with the synergistic ratio 1.002, 1.026 and 1.012 (>1) at 10 DAT (Table 7)
Conclusion
After evaluation of three formulations i.e., Etofenprox 6.5 % + Diafenthiuron 27 % + Pyriproxyfen 6.5%,Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 and Etofenprox 8.5 % + Diafenthiuron 34.50 % + Pyriproxyfen 9.0 % EC at three different doses (650 ml/ ha, 750 ml/ha & 850 ml/ha)., Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 EC @ 750 ml/ha found to be effective against Jassids in cotton crop in comparison to tank mix formulation Tank mix formulation (Etofenprox 10% EC + Diafenthiuron 50% WP + Pyriproxyfen 10 % EC) as well as solo treatments (Etofenprox 10 % EC, Diafenthiuron 50 % WP and Pyriproxyfen 10% EC) Etofenprox 7.5 % + Diafenthiuron 31 % + Pyriproxyfen 7.0 % EC @ 750 ml/ha. was found at par with higher formulation, higher dose and higher active ingredient.
, 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. Diafenthiuron is present in an amount ranging from 0.1% to 50.0% by weight;
c. Pyriproxyfen is present in an amount ranging from 0.1% to 30.0% 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, Anti freezing Agent, Anti foaming agent, Rheology modifier, pH stabilizer, Super-Wetting-spreading-penetrating agent, Stabilizing agent, 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, alkoxylatedtristyrylphenols, calcium dodecylbenzenesulfonate,Polyalkoxylated butyl ether block co-polymer,ethoxylated propoxylated polyaryl phenol, ethoxylated fatty acids, Ethoxylated tristyrylphenol, fatty alcohol ethoxylates, ethoxylatedricinoleic acid triglycerides, sorbitan trioleate, tridecyl alcohol ethoxylate, castor oil ethoxylate, 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 dispersant, ethoxylated polyarylphenol phosphate ester, sodium salt of naphthalene sulfonate condensate/naphthalene sulphonic acid condensate, acrylic copolymer,nonionic proprietary surfactant blend, Acrylic copolymer, polycarboxylates, calcium dodecylbenzene sulfonate, aryl sulphonate condensate,sodium lignosulphonate, dispertox BS SPL, Polymeric ester dispersant, Ethoxylated polyarylphenol phosphate ester polystyrenated acrylated co-polymer, modified styrene acrylic copolymer, salts of phenol sulfonic acids, Terwet 2700,butyl polyalkylene oxide block co-polymer, Polymeric ester dispersant, 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 topolydimethylsiloxane 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, Rhodopol 23, Precipitated silica, 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 from 0 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 ofvegetable oil triglycerides containing C12–C22 saturated and unsaturated fatty acid.
9. The insecticidal composition as claimed in claim 1, wherein the antifreezing agent is in an amount ranging from 0 to 15% by weight, selected from but not limited to ethylene glycol or propane-1,2-diol or propane-1,2,3-triol, urea.

10. The insecticidal composition as claimed in claim 1, wherein the stabilizing agent is in an amount ranging from 0 to 5% by weight, selected from but not limited to epoxidized soyabean oil, butylated hydroxy toluene, ethylenediaminetetraacetic acid.

11. The insecticidal composition as claimed in claim 1, wherein the pH Stabilizers is in an amount ranging from 0 to 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.

12. The insecticidal composition as claimed in claim 1, wherein the Biocide is in an amount ranging from 0 to 3.0% by weight, selected from the group comprising of 1,2-benzisothiazolin-3-one, formaldehyde, dipropyl glycol solution of 1,2-benzisothiazolin-3-one.
13. The insecticidal composition as claimed in claim 1, wherein the Super-Wetting-spreading-penetrating agent is in an amount ranging from 0.1% to 5.0% by weight is a 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, Polyalkyleneoxide modified heptamethyltrisiloxane methylated seed oil-polyoxyethylene methyl polysiloxane, methylated seed oil-polyether polymethyl siloxane copolymer, methylated seed oil-polyether modified polysiloxane.

14. The process of preparation of an insecticidal composition as claimed in claim 1, the process comprising: preparation of the said composition with agriculturally acceptable excipients