FIELD OF THE INVENTION

The present invention relates to a synergistic insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen. The present invention also includes process of preparation of the composition and uses thereof.
BACKGROUND OF THE INVENTION
In economically important crops, higher crop efficiency is achieved by controlling the invertebrate pests. Invertebrate pest causes damage to growing agronomic crops and thereby result in significant reduction in the crop productivity. Therefore, the control of invertebrate pests is economically important for the crop productivity. Many products are available as single or in combinations of two or more active ingredients. However, more economically efficient and ecologically safe pesticidal composition and methods are still being sought.
Chinese patent application No. 103271035 discloses the insecticidal composition containing flonicamid and pyriproxyfen, wherein the mass ratio of flonicamid and pyriproxyfen is 1:40-40:1.
Chinese patent application No. 103004842 discloses the insecticidal composition containing flonicamid and acetamiprid, wherein the mass ratio of acetamiprid and flonicamid is 10:1 to 1:40.
PCT publication no. WO/2002/037964 discloses a composition comprising a compound of Formula A (Flonicamid) and one or more of the compounds such as: abamectin; azamethiphos; bromopropylate; chlorfenvinphos; cypermethrin, cypermethrin high-cis; cyromazin; diafenthiuron; diazinon; dicrotophos; dicyclanil; emamectin; fenoxycarb; lufenuron; methidathion; monocrotophos; profenofos; pymetrozine; tau-fluvalinate; thiamethoxam; azoxystrobin; bensultap; chlorothalonil; fenpyroximate; fluazinam; flufenprox; flutriafol; lambda-cyhalothrin; phosmet; picoxystrobin; primicarb; pyridaben; or tefluthrin.
Further it provides that the composition may comprise a compound of Formula A and one of more of compounds I to CCLIX. All the examples in the patent application provide only binary combination, that is, compound of Formula A along with any one of compounds I to CCLIX.

Also, the examples only suggest synergistic effect of binary combination. Moreover, the patent application fails to provide any examples of ternary combination.
In order to reduce the risk from increased number of resistant insect pest strains, mixtures of different active compounds are nowadays employed for controlling harmful pests. By combining different active compounds having different mechanisms of action, it is possible to ensure successful control of pests of different groups over a relatively longer period of time and preventing development of resistance.
Therefore, there still exists a need to develop insecticidal composition, which is stable, synergistic, more effective in control of a wide spectrum of insect pests in crops and environmentally safe. The insecticidal compositions must show a broader scope of activity to avoid or to prevent the development of resistant strains or to the mixtures of known active ingredients used by farmer while minimising the doses of chemical products sprayed in the agriculture fields.
As a solution to the above mentioned problems, the inventors of the present invention surprisingly found that insecticidal composition comprising Acetamiprid, Flonicamid, and Pyriproxyfen provides effective control of a wide spectrum of insect pests.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides a combination comprising of Acetamiprid, Flonicamid and Pyriproxyfen.
In one aspect, the present invention provides a synergistic insecticidal composition comprising of Acetamiprid, Flonicamid and Pyriproxyfen with at least one excipient, wherein Acetamiprid is present in an amount in the range from 1% to 10%, Flonicamid is present in an amount in the range from 7% to 40% and Pyriproxyfen is present in an amount in the range from 6%> to 50%.
In another aspect the composition of the present invention is one of:
a) Acetamiprid is present in an amount of 1% w/w; Flonicamid is present in an amount of 7.5%) w/w; and Pyriproxyfen is present in an amount of 6%> w/w and at least one excipient.

b) Acetamiprid is present in an amount of 2% w/w; Flonicamid is present in an amount of 15% w/w; and Pyriproxyfen is present in an amount of 12% w/w and at least one excipient.
c) Acetamiprid is present in an amount of 5% w/w; Flonicamid is present in an amount of 40%) w/w; and Pyriproxyfen is present in an amount of 20% w/w and at least one excipient.
d) Acetamiprid is present in an amount of 10%> w/w; Flonicamid is present in an amount of 20%) w/w; and Pyriproxyfen is present in an amount of 50% w/w and at least one excipient.
In an aspect, the composition of the present invention is formulated as Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG), Emulsion water-in-oil (EO), Emulsifiable powder (EP), Emulsion for seed treatment (ES), Emulsion oil-in-water (EW), Flowable concentrate for seed treatment (FS), Granules (GR), Micro-emulsion (ME), Oil-dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Oil dispersible powder (OP), Suspension concentrate (SC), Suspension concentrate for direct application (SD), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC) or A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).
In a preferred aspect, the composition of the present invention is formulated as micro-emulsion (ME), oil-dispersion (OD), suspension concentrate (SC) or water dispersible granule (WG).
In another aspect, the composition of the present invention comprises at least one excipient selected from the group comprising solvent, emulsifier, wetting agent, dispersing agent, defoamer, thickener, anti-freezing agent, biocide, disintegrating agent, filler or a combination thereof.
The above aspects will become more apparent in view of the description given below.

DETAILED DESCRIPTION OF THE INVENTION
The definitions provided herein for the terminologies used in the present disclosure are for illustrative purpose only and in no manner limit, the scope of the present invention disclosed in the present disclosure.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention pertains. Although other methods and materials similar, or equivalent, to those described herein can be used in the practice of the present invention, the preferred materials and methods are described herein.
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.
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.
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 Acetamiprid, Flonicamid and Pyriproxyfen.
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 insect pests.
As used herein, the term "insecticide", refers to any chemical substance used to destroy/kill, inhibit or otherwise adversely affect the insect pests.

As used herein, the term "Acetamiprid" encompasses Acetamiprid or its agrochemically acceptable salt(s), derivative(s) or any other modified form of Acetamiprid.
Acetamiprid acts as nicotinic acetylcholine receptor agonist with translaminar activity and with contact and stomach action. It is a neonicotinoid insecticide. It is used to control Hemiptera (especially aphids), Thysanoptera and Lepidoptera in a wide variety of crops, especially vegetables, fruit and tea by soil or foliar application.
As used herein, the term "Flonicamid" encompasses Flonicamid or its agrochemically acceptable salt(s), derivative(s) or any other modified form of Flonicamid.
Flonicamid acts by inhibiting feeding and has systemic and translaminar activity. It is a pyridine carboxamide derivative compound. It is used to control aphids and some other sucking insects in fruit, cereals, potatoes, cotton, tea and vegetables.
As used herein, the term "Pyriproxyfen" encompasses Pyriproxyfen or its agrochemically acceptable salt(s), derivative(s) or any other modified form of Pyriproxyfen.
Pyriproxyfen acts as an insect growth regulator, suppressor of embryogenesis, inhibitor of metamorphosis and inhibitor of reproduction. It is used to control whiteflies and thrips.
The present invention provides a synergistic insecticidal combination of Acetamiprid, Flonicamid and Pyriproxyfen.
In one embodiment, the present invention provides a synergistic insecticidal composition comprising of Acetamiprid, Flonicamid and Pyriproxyfen and at least one excipient.
In another embodiment, the composition according to the present invention comprises Acetamiprid in an amount in the range from 1% to 20% w/w, Flonicamid in an amount in the range from 1% to 40% w/w and Pyriproxyfen in an amount in the range from 1% to 50% w/w and at least one excipient.
In yet another embodiment, the composition according to the present invention comprises Acetamiprid in an amount in the range from 1% to 10% w/w, Flonicamid in an amount in the range from 7% to 40% w/w and Pyriproxyfen in an amount in the range from 6% to 50% w/w and at least one excipient.

In a preferred embodiment, the synergistic insecticidal composition comprises of Acetamiprid is present in an amount of 1% w/w; Flonicamid is present in an amount of 7.5% w/w; and Pyriproxyfen is present in an amount of 6% w/w and at least one excipient.
In another preferred embodiment, the synergistic insecticidal composition comprises of Acetamiprid is present in an amount of 2% w/w; Flonicamid is present in an amount of 15% w/w; and Pyriproxyfen is present in an amount of 12% w/w and at least one excipient.
In a further preferred embodiment, the synergistic insecticidal composition comprises of Acetamiprid is present in an amount of 5% w/w; Flonicamid is present in an amount of 40% w/w; and Pyriproxyfen is present in an amount of 20% w/w and at least one excipient.
In yet another preferred embodiment, the synergistic insecticidal composition comprises of Acetamiprid is present in an amount of 10% w/w; Flonicamid is present in an amount of 20% w/w; and Pyriproxyfen is present in an amount of 50% w/w and at least one excipient.
The inventors have surprisingly found that the insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen of the present invention provides synergistic effect to control of wide variety of insect pests.
In yet another embodiment, the composition of the present invention is formulated as Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG), Emulsion water-in-oil (EO), Emulsifiable powder (EP), Emulsion for seed treatment (ES), Emulsion oil-in-water (EW), Flowable concentrate for seed treatment (FS), Granules (GR), Micro-emulsion (ME), Oil-dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Oil dispersible powder (OP), Suspension concentrate (SC), Suspension concentrate for direct application (SD), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC) or A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).
In a preferred embodiment, the composition of the present invention is formulated as Micro-emulsion (ME).

In another preferred embodiment, the composition of the present invention is formulated as Oil-dispersion (OD).
In yet another preferred embodiment, the composition of the present invention is formulated as suspension concentrate (SC).
In a further preferred embodiment, the composition of the present invention is formulated as water dispersible granule (WG).
As used herein, the term "excipient" refers to inert substances which are commonly used as diluent, to provide stability or to increase the activity profile of the composition or formulation without having any insecticidal activity or direct effect on the insect pests.
The composition of the present invention comprises excipients selected from the group comprising of solvent, emulsifier, wetting agent, dispersing agent, defoamer, thickener, anti-freezing agent, biocide, disintegrating agent, filler and/or a combination thereof. The composition may also contain if desired, one or more auxiliaries customary for crop protection compositions.
As used herein, the term "solvent" refers to liquid chemicals that are added to a pesticide product to aid in the delivery of the active ingredient.
Solvent is selected from the group comprising of, but not limited to, water; alcohols such as ethanol, propanol, butanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, glycerin; polyol ethers such as ethylene glycol monopropyl ether, diethylene glycol monomethyl ether, dipropylene glycol dimethyl ether; ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone; ethers such as dipropyl ether, dioxane, tetrahydrofuran; aliphatic hydrocarbons such as normal paraffin, isoparaffin, kerosene, mineral oil; aromatic hydrocarbons such as xylene, toluene, naphthalene, solvent naphtha, solvent CIX, solvent CX, solvent CXII, solvent N,N-decanamide (Armid 10), solvesso 100, solvesso 150, solvesso 200; chlorinated aliphatic or aromatic hydrocarbons such as chlorobenzene, chloroethylene, methylene chloride; esters such as ethyl acetate, diisopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; amides such as dimethylformamide, N-methyl-2-pyrrolidone, N-octylpyrolidone, N,N-dimethyldecanamide; nitriles such as acetonitrile; organosulfur

compound such as dimethyl sulfoxide. These solvents may be used alone or in combination thereof.
Preferably, the solvent is selected from the group comprising solvent CIX, solvent N,N-decanamide (Armid 10), water, mineral oil, or a combination thereof and present in an amount in the range from 5 to 80% w/w.
As used herein, the term "surfactant" means a compound that, when dissolved in a liquid, reduces the surface tension of the liquid, which reduces the interfacial tension between two liquids or which reduces surface tension between a liquid and a solid. Surfactant are non-ionic or anionic surfactants or a combination of these surfactants. It is preferred to use one or more than one kind of surfactants. Depending on the nature of the hydrophilic and lipophilic groups in a surfactant molecule, surfactants can be useful as emulsifier, wetting agent or dispersing agent.
Surfactant is selected from the group comprising of, but not limited to, sugar esters such as sorbitan monolaurate, polyoxyethylene sorbitan monolaurate; alkyl polyglucoside such as decyl glucoside; polyoxyethylene alkyl ethers such as polyoxyethylene lauryl ether or polyoxyethylene coconut fatty alcohol ether; polyoxyethylene alkynyl ether such as 2,4,7,9-tetramethyl-5-decyn-4,7-diol ether; polyoxyethylene aryl ethers such as polyoxyethylene nonylphenyl ether or polyoxyethylene tristyrylphenyl ether; polyoxyethylene vegetable oil ethers such as polyoxyethylene castor oil or polyoxyethylene hydrogenated castor oil; polyoxyethylene fatty acid esters such as polyoxyethylene monolaurate, polyoxyethylene distearate or polyoxyethylene resin acid ester; polyalkylene oxide block copolymer such as polyoxyethylene polyoxypropylene block copolymers (such as Pluronic®); polyoxyethylene polyoxypropylene alkyl ether such as polyoxyethylene polyoxypropylene lauryl ether; polyoxyethylene polyoxypropylene aryl ether such as polyoxyethylene polyoxypropylene styrylphenyl ether; polyoxyethylene alkyl amines such as polyoxyethylene stearyl amine; polyoxyethylene fatty acid amide such as lauric acid diethanolamid; fluorinated surfactant; alkyl sulfates such as sodium lauryl sulfate, sodium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates such as sodium polyoxyethylene lauryl ether sulfate; polyoxyethylene aryl ether sulfates such as sodium polyoxyethylene nonylphenyl ether sulfate or ammonium polyoxyethylene tristyrylphenyl ether sulfate; tristyryl phenol ethoxylated, amine salt of phosphate tristyryl phenol ethoxylated; aryl sulfonate such as calcium dodecyl benzene sulfonate, naphthalene sulphonate derivative like salt of naphthalene sulfonate such as sodium

naphthalene sulfonate; naphthalene sulfonate of formaldehyde condensate or sodium naphthalene sulfonate formaldehyde condensate, naphthalene alkyl aryl sulphonate; ' alpha'-olefin sulfonate; alkyl sulfosuccinate such as sodium dioctyl sulfosuccinate; lignin based sulfonate such as sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; alkoxylated phosphate ester such as high molecular weight polymer PEG-10 PPG-5-cetyl phosphate; ethoxylated polyarylphenol phosphate ester, polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates such as polyoxyethylene phenyl ether phosphate or polyoxyethylene nonylphenyl ether phosphate; polyoxyethylene polyoxypropylene block copolymer phosphate; graft copolymer such as polymethyl methacrylate-polyethylene glycol graft copolymer; acrylic copolymer; alcohol block copolymer; ethylene oxide (EO)-polyethylene oxide (PO) block copolymer, non-ionic ethoxylated, polyoxyethylene ether of triglyceride ester, Poly(oxy-l,2-ethanediyl) alpha-(tris(l-phenylethyl)phenyl)-omega-hydroxy. The surfactant is present in an amount in the range from 1 to 20%w/w.
An emulsifier is a kind of surfactant. It helps to prevent the droplets of the dispersed phase of an emulsion from flocculating or coalescing in the emulsion. The emulsifier is selected from the group comprising of mixture of non-ionic surfactants and amine salt of phosphate tristyryl phenol ethoxylated, acrylic copolymer, ethoxylated polyarylphenol phosphate ester, polyoxyethylene ether of triglyceride ester, Poly(oxy-l,2-ethanediyl) alpha-(tris(l-phenylethyl)phenyl)-omega-hydroxy or a combination thereof, and present in an amount in the range from 5 to 20% w/w.
In an embodiment, the emulsifier is a blend of anionic and non-ionic surfactant.
It is generally observed that solid particles in a liquid undergo spontaneous aggregation to form lumps. Hence, it is recommended to add a dispersing agent which prevents agglomeration of solid particles and keep them suspended in fluid. The dispersing agent is selected from the group comprising of naphthalene sulphonate derivative, naphthalene sulfonate of formaldehyde condensate, acrylic copolymer, graft copolymer, lignin based sulfonate, amine salt of phosphate tristyryl phenol ethoxylated or a combination thereof, and present in an amount in the range from 1 to 10% w/w.
Wetting is the first stage of dispersion, in which air surrounding the granular composition is substituted with water. Wetting of the composition with water cannot occur if the surface

tension of the liquid is very high. Hence, it is recommended to add a wetting agent to the composition to facilitate the process of dispersion of the granules in the liquid. The wetting agent is selected from the group comprising of naphthalene alkyl aryl sulphonate, dioctyl sulfosuccinate, sodium lauryl sulfate, non-ionic ethoxylated, ethoxylated polyarylphenol phosphate ester, sodium alkyl naphthalene sulfonate or a combination thereof, and present in an amount in the range from 1 to 15% w/w.
As used herein, the term "defoaming agent" or "defoamer" or "anti-foaming agent" refers to an excipient that reduces and hinders the formation of foam in the liquid, semi-solid, or solid formulations.
Defoamer is selected from the group comprising of, but not limited to, silicone compounds such as dimethyl polysiloxane emulsion and organic fluorine compounds. These defoaming agents may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises dimethyl polysiloxane emulsion as defoamer. The defoamer is present in an amount in the range from 0.01 to 2.0% w/w.
As used herein, the term "thickener" or "rheology modifier" refers to a polymeric material, which at a low concentration increases the viscosity of an aqueous solution and helps to stabilize the composition.
Thickener is selected from the group comprising of, but not limited to, water-soluble polymer and inorganic fine powder, wherein water-soluble polymer such as xanthan gum, welan gum, guar gum, polyvinyl alcohol, carboxymethylcellulose, polyvinylpyrrolidone, carboxyvinyl polymer, acrylic polymer, starch derivative or polysaccharide; or an inorganic fine powder selected from high purity silica, bentonite, white carbon. These thickeners may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises xanthan gum as thickener. The thickener is present in an amount in the range from 0.01 to 3.0% w/w.
As used herein, the term "anti-freezing agent" refers to a compound used to prevent deleterious effects due to freezing and lyophilization (lyophilisation).
Anti-freezing agent is selected from the group comprising of, but not limited to, polyhydric alcohol such as ethylene glycol, polyethylene glycol, diethylene glycol, propylene glycol, and

glycerine. These anti-freezing agents may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises ethylene glycol, diethylene glycol or propylene glycol as anti-freezing agent. The anti-freezing agent is present in an amount in the range from 2 to 10% w/w.
As used herein, the term "biocide" refers to an agent that prevents spoilage from bacteria, yeasts and fungi.
Biocide is selected from the group comprising of, but not limited to, 20% aqueous dipropylene glycol solution of l,2-benzisothiazolin-3-one (Proxel GXL), formaldehyde, isothiazolinone or a combination thereof. The biocide is added to the composition of the present invention for its preservation against spoilage from bacteria, yeasts and fungi. The biocide is present in an amount in the range from 0.01 to 0.50% w/w.
As used herein, the term "disintegrating agent" refers to an excipient that can swell or disintegrate the composition.
Disintegrating agent is selected from the group comprising of, but not limited to, citric acid, sodium bicarbonate, sodium tripolyphosphate, stearic acid metal salt, cellulose powder, dextrin, methacrylate copolymer, cross-linked polyvinylpyrrolidone, polyaminocarboxylic acid chelate compound, styrene sulfonate/isobutylene/maleic anhydride copolymer, starch/polyacrylonitrile graft copolymer, sodium hexametaphosphate, microcrystalline cellulose, carboxymethyl cellulose, sodium starch glycolate, sodium polycarbonate, bentonite. These disintegrating agents may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises of citric acid or sodium bicarbonate as disintegrating agent. The disintegrating agent is present in an amount in the range from 1 to 5% w/w.
As used herein, the term "filler" refers to solid chemicals that are added to a pesticide formulation to aid in the delivery of the active ingredient.
Filler is selected from the group comprising of, but not limited to, natural minerals such as quartz, talc, kaolin, pyrophyllite, montmorillonite, attapulgite, bentonite clay, china clay, kieselguhr, chalk, zeolite, calcite, sericite, acid clay, diatomaceous earth, natural rock, Fuller's earth, meerschaum, gibbsite, dolomite or pumice; synthetic minerals such as precipitated silica,

fumed silica, sodium silicate, alumina, aluminium hydroxide; inorganic salts such as calcium carbonate, ammonium sulfate or other ammonium salts, sodium sulfate, potassium chloride. The filler may be used alone or in combination thereof. Preferably, the filler is selected from the group comprising bentonite clay, china clay, silica, kaolin, diatomaceous earth or a combination thereof, and present in an amount in the range from 4 to 25% w/w.
In an embodiment, the present invention provides a process of preparing a micro-emulsion (ME) formulation comprising the steps of:
a) mixing solvent, acetamiprid, flonicamid, pyriproxyfen, and emulsifier to obtain a clear solution;
b) filtering the solution through a filtration apparatus to obtain a micro-emulsion formulation.
In another embodiment, the present invention provides a process of preparing an oil-dispersion (OD) formulation comprising the steps of:
a) mixing wetting agent, emulsifier and oil by high shear mixing;
b) adding acetamiprid, flonicamid, pyriproxyfen, defoamer to step a) mixture to form a homogenous mass;
c) grinding the homogenous mass to obtain a mean particle size of 3 to 5 (D-90) microns;
d) adding thickener under low stirring to obtain an oil-dispersion formulation.
In a further embodiment, the present invention provides a process of preparing a suspension concentrate (SC) formulation comprising the steps of:
a) mixing wetting agent, dispersing agent and de-mineralized water by high shear mixing;
b) adding acetamiprid, flonicamid, pyriproxyfen, anti-freezing, defoamer to step a) mixture to form a homogenous mass;
c) grinding the homogenous mass to obtain a mean particle size of 3 to 5 (D-90) microns;
d) adding a solution containing thickener and water under low stirring to obtain a suspension concentrate formulation.

In another embodiment, the present invention provides a process of preparing of a water dispersible granule (WG) formulation comprising the steps of:
a) mixing acetamiprid, flonicamid, pyriproxyfen, dispersing agent, wetting agent, disintegrating agent, defoamer and filler in a blender to form a homogenous mass;
b) milling the homogenous mass to obtain particle size below 10 microns;
c) preparing a dough using the above milled material by using 10 to 20% water;
d) extruding the dough using a extruder having a suitable screen by maintaining the temperature of the screen below 50°C to obtain extruded granules;
e) drying the extruded granules using a fluid bed dryer by keeping air flow at 75% to 80% and maintaining the temperature of the air at 50°C to obtain free flowing WG formulation.
The composition of the present invention can be applied by any one of the methods selected from atomization, spreading, dusting, spraying, diffusion, immersion, irrigation, injection, mixing, sprinkling (water immersion), foaming, dressing, coating, blasting, fumigation, smoking, smog and painting.
In another embodiment, the present invention further provides a composition of Acetamiprid, Flonicamid and Pyriproxyfen for the control of a wide variety of undesired insect pests.
In an embodiment the synergistic insecticidal composition of the present invention is found to be effective to control wide variety of insect pests. More particularly, the composition of the present invention is used to control the insect pests from the orders of moths and butterflies (Lepidoptera), beetles (Coleoptera), flies, whiteflies (Bemisia tabaci Gennadius), mosquitoes (Diptera), sucking pests, jassids (Amrasca biguttula biguttula Ishida), aphids {Aphis gossypii Glover), thrips {Thrips tabaci Lindeman -Ihysanoptera), cockroaches (Blattaria - Blattodea), true bugs (Hemiptera), crickets, grasshoppers, locusts (Orthoptera), arachnids (Acarina), fleas (Siphonaptera), silverfish, firebrat (Thysanura), millipedes (Diplopoda), earwigs (Dermaptera), lice (Phthiraptera), or plant parasitic nematodes.
The inventors of the present invention have surprisingly found that the composition of the present invention is synergetic in nature. The synergetic insecticidal composition of the present invention is more effective than their individual counterparts or when two actives are taken together. The synergetic insecticidal composition of the present invention also makes it

possible to use markedly smaller quantities of the active ingredients as compared to their individual counterparts. This allows a substantial reduction in the application rates of each of these active ingredients, while maintaining good efficacy. The decrease in application rates reduces treatment cost to the farmer and also eases the burden on the environment from crop protection chemical residues.
The synergistic insecticidal composition of the present invention provides a number of other advantages:
• Increased efficacy in comparison to the other formulations tested during the trial.
• Economically beneficial to the farmers as it provides better yield of the crop with reduction in the number of sprays.
• Reduced possibility of hazards to the farmers due to occupational exposure because of reduction in the number of sprays.
• Is storage-stable.
• Is non-phytotoxic.
• Number of sprays will reduce which in turn reduce the quantity of water required for spray.
• Lower consumption of the chemicals will reduce the generation of number of empty containers there by reducing the concern for disposal.
The embodiments of the present invention are more particularly described in the following examples that are intended as illustrations only, since numerous modifications and variations within the scope of the present invention will be apparent to those of skill in the art. Unless otherwise noted, all parts, percentages and ratios reported in the following examples are on a weight basis and all reagents used in the examples were obtained or are available from the chemical suppliers.
EXAMPLES
The synergistic insecticidal composition of the present invention comprising of Acetamiprid, Flonicamid and Pyriproxyfen in the form of micro-emulsion (ME) is provided in table 1 and 2, in the form of oil-dispersion (OD) is provided in table 3 and table 4, in the form of suspension concentrate (SC) is provided in table 5 and table 6 and in the form of water dispersible granules (WG) is provided in table 7 and table 8. The unit of each component of the composition are

expressed in "% w/w" i.e. the percentage by weight, relative to the weight of the total solution or composition.
Table 1: Synergistic insecticidal composition of the present invention comprising Acetamiprid, Flonicamid and Pyriproxyfen in ME form

S.No. Ingredients Quantity (% w/w)

Eg:l Eg: 2
1 Acetamiprid Technical (Basis of 100.0%) 1 2
2 Flonicamid Technical (Basis of 100.0%) 7.5 15
3 Pyriproxyfen Technical (Basis of 100.0%) 6 12
4 Emulsifiers (blend of anionic and non-ionic surfactant) 6-7 5-10
5 Solvent -N, N-Decanamide (Armid 10) 8-12 8-10
6 Solvent - CIX Q.S. to make 100% Q.S. to make 100%
QS: quantity sufficient required to make 100%) w/w formulation
Example I: Process of preparing synergistic insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen in ME form
All the ingredients were weighed as per table 2. Table 2 provides quantities of active ingredients and raw material charged to prepare the synergistic insecticidal composition of the present invention in ME form. In table 2 the active ingredients are in technical grade with 98%> purity (acetamiprid) and 97% purity (flonicamid and acetamiprid) whereas entries for active ingredients in table 1 for 100%) pure compounds. Particularly, the examples 1 and 2 as given in Table 1 above corresponds to column A and B in table 2.
Table 2: Quantities of active ingredients and raw material charged

S.No. Ingredients Function Quantity (g)

A B
1 Acetamiprid Technical (Basis of 98.0%>) Active Ingredient 1.02 2.04
2 Flonicamid Technical (Basis of 97.0%) Active Ingredient 7.73 15.46
3 Pyriproxyfen Technical (Basis of 97.0%) Active Ingredient 6.19 12.37
4 Polyoxyethylene ether of triglyceride ester Emulsifier 4.00 4.00
5 Poly(oxy-1,2-ethanediyl) alpha-(tris( 1 -phenylethyl)phenyl)-omega-hydroxy Emulsifier 3.00 4.00
6 Solvent - N, N- Decanamide (Armid 10) Solvent 10 10
7 Solvent - CIX Solvent 68.06 52.13
Total Quantity 100 100

The acetamiprid (1.02 g/ 2.04 g), flonicamid (7.73 g/ 15.46 g), pyriproxyfen (6.18 g/ 12.37 g), solvent and emulsifier were weighed as per table 2 and mixed to obtain a clear solution. The solution was then filtered through a filtration apparatus to obtain the insecticidal composition in ME form.
Table 3: Synergistic insecticidal composition of the present invention comprising Acetamiprid, Flonicamid and Pyriproxyfen in OD form

S.No. Ingredients Quantity (% w/w)

Eg: 3 Eg: 4
1 Acetamiprid Technical (Basis of 100.0%) 1 2
2 Flonicamid Technical (Basis of 100.0%) 7.5 15
3 Pyriproxyfen Technical (Basis of 100.0%) 6 12
4 Emulsifiers (Mixture of nonionic surfactants and amine salt of phosphate tristyryl phenol ethoxylated / Acrylic copolymer/ Ethoxylated polyarylphenol phosphate ester) 5-20 5-20
5 Wetting agent (sodium alkyl naphthalene sulfonate blend/ sodium alkyl naphthalene sulfonate) 5-15 5-15
6 Defoamer (Dimethyl Polysiloxane emulsion) 0.1-2 0.5-2
7 Thickener 0.1-3 0.1-3
8 Mineral oil Q.S. to make 100% Q.S. to make 100%
QS: quantity sufficient required to make 100%) w/w formulation
Example II: Process of preparing synergistic insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen in OD form
All the ingredients were weighed as per table 4. Table 4 provides quantities of active ingredients and raw material charged to prepare the synergistic insecticidal composition of the present invention in OD form. In table 4 the active ingredients are in technical grade with 98%> purity (acetamiprid) and 97%> purity (flonicamid and acetamiprid) whereas entries for active ingredients in table 3 for 100%) pure compounds. Particularly, the examples as given in Table 3 above corresponds to column C and D in table 4.
Table 4: Quantities of active ingredients and raw material charged

S.No. Ingredients Function Quantity (g)

C D
1 Acetamiprid Technical (Basis of 98.0%>) Active ingredient 1.02 2.04

2 Flonicamid Technical (Basis of 97.0%) Active ingredient 7.73 15.46
3 Pyriproxyfen Technical (Basis of 97.0%) Active ingredient 6.19 12.37
4 Mixture of Nonionic surfactants and Amine salt of phosphate tristyryl phenol ethoxylated Emulsifier 12.00 12.00
5 Sodium alkyl naphthalene sulfonate blend Wetting agent 12.00 10.00
6 Dimethyl Polysiloxane emulsion Defoamer 1.00 1.00
7 Xanthan gum Thickener 0.30 0.30
8 Mineral oil Solvent 59.76 46.83
Total Quantity 100 100
The wetting agent and emulsifier and oil were weighed as per table 4 and solubihzed by high shear mixing. Then acetamiprid (1.02 g/ 2.04 g), flonicamid (7.73 g/ 15.46 g), pyriproxyfen (6.18 g/12.37 g), defoamer were added to obtain a homogenous mass. The homogenous mass was grinded in bead mill. The grinding was carried out until a mean particle size of 3 to 5 (D-90) microns was obtained. After grinding, thickener was added under low stirring to obtain the title insecticidal composition in OD form.
Table 5: Synergistic insecticidal composition of the present invention comprising Acetamiprid, Flonicamid and Pyriproxyfen in SC form

S.No. Ingredients Quantity (% w/w)

Eg: 5 Eg: 6
1 Acetamiprid Technical (Basis of 100.0%) 1 2
2 Flonicamid Technical (Basis of 100.0%) 7.5 15
3 Pyriproxyfen Technical (Basis of 100.0%) 6 12
4 Anti-freezing agent (propylene glycol/ diethylene glycol/ ethylene glycol) 2-10 2-10
5 Dispersing agent (Amine salt of phosphate tristyryl phenol ethoxylated/ Acrylic copolymer/ Graft copolymer) 2-10 2-10
6 Wetting agent (Ethoxylated polyarylphenol phosphate ester/ Dioctyl sulphosuccinate/ Non-ionic ethoxylate) 1-5 1-5
7 Defoamer (Dimethyl Polysiloxane emulsion) 0.01-0.5 0.01-0.5
8 Biocide (Proxel GXL/ Formaldehyde) 0.01-0.5 0.01-0.5
8 Thickener (Xanthan gum) 0.01-0.5 0.01-0.5
9 Demineralized water Q.S. to make 100% Q.S. to make 100%
QS: quantity sufficient required to make 100%) w/w formulation

Example III: Process of preparing synergistic insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen in SC form
All the ingredients were weighed as per table 6. Table 6 provides quantities of active ingredients and raw material charged to prepare the synergistic insecticidal composition of the present invention in SC form. In table 6 the active ingredients are in technical grade with 98% purity (acetamiprid) and 97% purity (flonicamid and acetamiprid) whereas entries for active ingredients in table 5 for 100%) pure compounds. Particularly, the examples as given in Table 5 above corresponds to column E and F in table 6.
Table 6: Quantities of active ingredients and raw material charged

s.
No. Ingredients Function Quantity (g)

E F
1 Acetamiprid Technical (Basis of 98.0%) Active Ingredient 1.02 2.04
2 Flonicamid Technical (Basis of 97.0%) Active Ingredient 7.73 15.46
3 Pyriproxyfen Technical (Basis of 97.0%) Active Ingredient 6.19 12.37
4 Propylene glycol Anti-freezing agent 5.00 5.00
5 Graft copolymer Dispersing agent 5.00 5.00
6 Non-ionic ethoxylated Wetting agent 3.00 3.00
7 Dimethyl Polysiloxane emulsion Defoamer 0.10 0.10
8 Proxel GXL Biocide 0.10 0.10
8 Xanthan gum Thickener 0.10 0.10
9 Demineralized water Solvent 71.76 56.83
Total 100 100
The dispersing agent, and wetting agent were weighed as per table 6 and diluted in demineralised water and solubilized by high shear mixing. Then anti-freezing agent (5g), acetamiprid (1.02 g/ 2.04 g), flonicamid (7.73 g/ 15.46 g), pyriproxyfen (6.18 g/ 12.37 g), defoamer and biocide were added and mixed to obtain a homogeneous mass. The homogeneous mass was grinded in bead mill. The grinding was carried out until a mean particle size below 5(D-90) microns was obtained. After grinding, thickener was added under low stirring to obtain the title insecticidal composition in SC form.
Table 7: Synergistic insecticidal composition of the present invention comprising Acetamiprid, Flonicamid and Pyriproxyfen in WG form

s.
No. Ingredients Quantity (% w/w)

Eg: 7 Eg: 8
1 Acetamiprid Technical (Basis of 100.0%) 5 10
2 Flonicamid Technical (Basis of 100.0%) 40 20
3 Pyriproxyfen Technical (Basis of 100.0%) 20 50
4 Dispersing Agent (Naphthalene sulphonate of formaldehyde condensate/Acrylic copolymer/Lignin based sulfonate) 1-10 1-10
5 Wetting agent (Naphthalene alkyl aryl sulphonate/ Dioctyl sulfosuccinate/Sodium lauryl sulfate) 1-5 1-5
6 Disintegration Agent (Citric acid/ Sodium bicarbonate) 1-5 1-5
7 Anti-foaming agent (Dimethyl Polysiloxane emulsion) 0.1-1 0.1-1
8 Filler (Bentonite clay/ China clay/ Silica/ Kaolin/ Diatomaceous earth) Q.S.to make 100% Q.S.to make 100%
Example IV: Process of preparing synergistic insecticidal composition comprising Acetamiprid, Flonicamid and Pyriproxyfen in WG form
All the ingredients were weighed as per table 8. Table 8 provides quantities of active ingredients and raw material charged to prepare the synergistic insecticidal composition of the present invention in WG form. In table 8 the active ingredients are in technical grade with 98% purity (acetamiprid) and 97% purity (flonicamid and acetamiprid) whereas entries for active ingredients in table 7 for 100%) pure compounds. Particularly, the examples as given in Table 7 above corresponds to column E and F in table 8.
Table 8: Quantities of active ingredients and raw material charged

s.
No. Ingredients Function Quantity (% w/w)

Eg: 9 Eg: 10
1 Acetamiprid Technical (Basis of 98.0%) Active Ingredient 5.10 10.20
2 Flonicamid Technical (Basis of 97.0%) Active Ingredient 41.24 20.62
3 Pyriproxyfen Technical (Basis of 97.0%) Active Ingredient 20.62 51.54
4 Naphthalene sulphonate derivative Dispersing agent 4.00 5.00
5 Naphthalene alkyl aryl sulphonate Wetting agent 2.00 2.50
6 Citric acid Disintegration agent 5.00 5.00
7 Dimethyl Polysiloxane emulsion Anti-foaming agent 0.5 0.50
8 China clay Filler 21.54 4.64

All the components were weighed as per table 8 and mixed well using proper ribbon blender type mixer to obtain a mixture. The mixture was milled with suitable mill. The mixture was milled to achieve a particle size below 10 microns and then mixed properly in a post blender. A dough was prepared using the milled mixture and 10% to 20% water in suitable dough-mixer. The dough was then extruded using proper extruder having suitable screen while maintaining the temperature of the screen below 50°C to obtain extruded granules. The extruded granules were dried using a fluid bed dryer. The air flow was kept between 75 to 80% and the temperature of the air was maintained at 50°C. The granules were dried till the material becomes free flowing.
Evaluation of bio-efficacy of the synergistic insecticidal composition
Field trials were conducted to evaluate the biological efficacy of different insecticidal compositions of present invention (T1-T4) and reference products (T5-T10) against Whitefly in cotton crop. Table 9 provides treatment details of various insecticidal compositions. T1-T4 represent synergistic insecticidal composition of the present invention and T5-T10 represent: reference products, such as, binary combination products, flonicamid + pyriproxyfen, flonicamid + acetamiprid, and pyriproxyfen + acetamiprid (T5-T7) and solo formulations of flonicamid, pyriproxyfen, acetamiprid (T8-T10).
Table 9: Treatment details for evaluation of bio-efficacy of new insecticide against
Whitefly in Cotton

Treatment Treatment Dose (g/ml /ha) Dose a.i./ha (g) Time of Application
Ti Flonicamid 15%+Pyriproxyfen 12%+ Acetamiprid 2% ME 500 ml 75 + 60 + 10 Insect level
above
Economic
Threshold
Level
T2 Flonicamid 15%+Pyriproxyfen 12%+ Acetamiprid 2% OD 500 ml 75 + 60 + 10

T3 Flonicamid 7.5%+Pyriproxyfen 6%+ Acetamiprid 1% ME 1000 ml 75 + 60 + 10

T4 Flonicamid 7.5%+Pyriproxyfen 6%+ Acetamiprid 1% OD 1000 ml 75 + 60 + 10

T5 Flonicamid 50% WG + Pyriproxyfen 10% EC 150 + 600 75 + 60

T6 Flonicamid 50% WG+ Acetamiprid 20% SP 150 + 50 75 + 10

T7 Pyriproxyfen 10% EC + Acetamiprid 20% SP 600 + 50 60+10

T8 Flonicamid 50% WG 150 75

T9 Pyriproxyfen 10% EC 600 60

Tio Acetamiprid 20% SP 50 10
Tn Control (Water Spray) — —
Details of the experiment:
The experiment was laid out in Randomized Block Design (RBD) with seven replications. The plot size was 100 m2 (10 x 10 m). All the recommended agronomic practices were followed 5 throughout the cropping period. The various insecticidal compositions as per Table 9 were sprayed on cotton crop to evaluate the control of Whitefly (Bemisia tabaci Gennadius). A 5 liter garden pressure hand sprayer fitted with hollow cone nozzle was used for spraying. The spray volume used was 500 liter per hectare. Based on various doses, weighed quantity of test products were dissolved in 5 liter of water/treatment and sprayed uniformly.
Insecticides were applied at the primordial stage of crop with considerable level of pest population above ETL (Economic Threshold Level). Observation on insect population Post treatment count was recorded at 3, 7 and 14 days after application (DAA). Average post treatment population of target insects for each spray was calculated to find out the overall efficacy of insecticides. Ten plants were selected randomly from each plot and no. of white
flies per 3 leaves were counted separately for each plant of every plots before sprays/application as well as on three, seven and fourteen days after each application. The data were statistically analysed as applicable to randomized block design wherever, the results were found significant, the critical differences were computed at 5 per cent level of probability to draw statistical conclusion.
The bio-efficacy effect of different treatment schedules on cotton crop and the treatment wise yield data in cotton crop is summarized in Tables below.
Table 10: Effect of insecticidal composition of present invention against Whitefly population (no./leaf) in Cotton

Treat
-ment
No. Treatment Dose Formulati
on (g/ml/ha) Dose a.i./ha
(g) > fo. of Whitefly/leaf %
Reduction
against
Control

3 DAA 7 DAA 14 DAA Mean

Ti Flonicamid
15%+Pyriproxyfen 12%+ Acetamiprid 2% ME 500 ml 75 + 60 + 10 2.33 (1.68) 1.00 (1.22) 1.33 (1.35) 1.55 (1.43) 90.36
T2 Flonicamid
15%+Pyriproxyfen 12%+ Acetamiprid 2% OD 500 ml 75 + 60 + 10 2.00 (1.58) 0.67 (1.08) 1.00 (1.22) 1.22 (1.31) 92.41

T3 Flonicamid
7.5%+Pyriproxyfen 6%+ Acetamiprid 1% ME 1000 ml 75 + 60 + 10 2.67 (1.78) 1.33 (1.35) 1.00 (1.22) 1.67 (1.47) 89.65
T4 Flonicamid
7.5%+Pyriproxyfen 6%+ Acetamiprid 1% OD 1000 ml 75 + 60 + 10 2.33 (1.68) 0.67 (1.08) 1.00 (1.22) 1.33 (1.35) 91.72
T5 Flonicamid 50% WG + Pyriproxyfen 10% EC 150 + 600 75 + 60 4.33 (2.20) 3.67 (2.04) 4.67
(2.27) 4.22 (2.17) 73.78
T6 Flonicamid 50% WG+ Acetamiprid 20% SP 150 + 50 75 + 10 6.33 (2.61) 7.00 (2.74) 8.33 (2.97) 7.22 (2.78) 55.18
T7 Pyriproxyfen 10% EC + Acetamiprid 20% SP 600 + 50 60+10 5.33 (2.41) 5.33 (2.41) 6.67 (2.68) 5.78 (2.51) 64.14
T8 Flonicamid 50% WG 150 75 6.67 (2.68) 7.33 (2.80) 10.00 (3.24) 8.00 (2.92) 50.34
T9 Pyriproxyfen 10% EC 600 60 5.67 (2.48) 6.00
(2.55) 7.33 (2.80) 6.33 (2.61) 60.69
Tio Acetamiprid 20% SP 50 10 8.67 (3.03) 12.33 (3.58) 15.00 (3.94) 12.00 (3.54) 25.51
Tn Control (Water Spray) — — 11.33 15.67 21.33 16.11 -
SE(m) - - 0.225 0.379 0.498 0.368 -
CD. - - 0.670 1.126 1.481 1.092 -
CV - - 7.451 11.90
7 12.22
7 10.722 -
* DAA: Days after application, CD 5%: Critical Difference, CD: Coefficient of Variance, g = Gram; ml = Millilitre, a.i. = active ingredient

Synergistic effect of the composition of the present invention
A synergistic effect exists whenever the action of an active ingredient combination is greater than the sum of the actions of the individual components. Synergism was calculated by using Colby's method, Weeds, vol 15 No. l(Jan 1967), pp 20-2.
The synergistic action expected for a given combination of three active components can be
calculated as follows:
(XY + XZ + YZ) XYZ
E = X + Y + Z- - — - +
100
10000

Wherein,
E = Expected percentage of insecticidal control for the combination of three active ingredients
at defined doses (for example equal to x, y and z respectively),
X = percentage of insecticidal control observed by compound I at a defined dose (equal to x),

Y = percentage of insecticidal control observed by compound II at a defined dose (equal to y),
Z = percentage of insecticidal control observed by compound III at a defined dose (equal to z),
When the percentage of insecticidal control observed for the combination is greater than the expected percentage, there is a synergistic effect.
In the same experiment, to evaluate synergistic impact, mean control of whitefly (% insect control) were taken for insecticidal treatments. Table 11 summarizes the synergistic impact of the composition of the present invention.
Table 11: Synergistic evaluation of insecticidal composition of present invention against
Whitefly in Cotton

Treat-ment No. Treatment Dose
Formulation
(g/ml/ha) Dose
a.i./ha
(g) Mean Control % (Observed) Expected Control Colby Ratio
Ti Flonicamid 15%+Pyriproxyfen 12%+ Acetamiprid 2% ME 500 ml 75 + 60 + 10 90.36 86.88 1.0401
T2 Flonicamid 15%+Pyriproxyfen 12%+ Acetamiprid 2% OD 500 ml 75 + 60 + 10 92.41 86.88 1.0637
T3 Flonicamid
7.5%+Pyriproxyfen
6%+ Acetamiprid
1%ME 1000 ml 75 + 60 + 10 89.65 86.88 1.0319
T4 Flonicamid 7.5%+Pyriproxyfen 6%+ Acetamiprid 1% OD 1000 ml 75 + 60 + 10 91.72 86.88 1.0558
T5 Flonicamid 50% WG +
Pyriproxyfen 10% EC 150 + 600 75 + 60 73.78 82.38 0.8956
T6 Flonicamid 50% WG+ Acetamiprid 20% SP 150 + 50 75 + 10 55.18 66.61 0.7557
T7 Pyriproxyfen 10% EC + Acetamiprid 20% SP 600 + 50 60+10 64.14 70.72 0.9070
T8 Flonicamid 50% WG 150 75 50.34 — —
T9 Pyriproxyfen 10% EC 600 60 60.69 — —

Tio Acetamiprid 20% SP 50 10 25.51 — —
— —
g = Gram; ml = Millilitre, a.i. = active ingredient
It is evident from table 11 that the composition of the present invention is synergistic (treatment no. 1 to 4) as the observed value of mean percentage control of whitefly is greater than the expected mean percentage control of whitefly.
The treatment wise yield data in Cotton crop is summarized in table 12.
Table 12: Treatment Wise Yield Data in Cotton

Treatment No. Lint yield (kgha-1) % increase in lint yield over control
Ti 1128 45.36
T2 1173 51.16
T3 1106 42.53
T4 1132 45.88
T5 988 27.32
T6 810 10.82
T7 912 17.53
T8 860 4.38
T9 898 15.72
Tio 799 2.96
Tn 776 -
SE(m) 11.422 -
CD. 33.933 -
CV 2.057 -
CD 5%: Critical Difference, CD: Coefficient of Variance
The aforementioned trial results indicate that the Treatment TI to T4 result in higher yield. Hence, the composition of the present invention is most effective and affords highest yield as compared to solo formulations (T8 to T10) and binary formulations (T5 to T7).
Phytotoxicity Observations
For phytotoxicity evaluation on cotton, following observations were made by observing temporary or long lasting damage to the leaves if any viz., leaf injury on tips and leaf surface,

wilting, vein clearing, necrosis, epinasty and hyponasty at 1, 3, 7, 14 and 21 days after each application from each and then average was taken. The treatment details were per Table 9. Crop injury was observed on visual rating from 1-10 scale as given in Table 13. Table 14 provides phytotoxic effect of the synergistic composition of the present invention on cotton.
Table 13:

SCORE PHYTOTOXICITY (PERCENT)
0 No phytotoxicity
1 1-10
2 11-20
3 21-30
4 31-40
5 41-50
6 51-60
7 61-70
8 71-80
9& 10 Complete destruction
DAA = Days after application; L = Leaf injury to tip/surface; E/H = Epinasty/Hyponasty; W = Wilting
Table 14: Effect of insecticidal composition of present invention on Phytotoxicity in Cotton

s.
No. Treatments Dose (ml/ha) Phytotoxicity (DAA)

1 DAA 3 DAA 7 DAA 14 DAA 21 DAA
1 Flonicamid 15% + Pyriproxyfen 12% + Acetamiprid 2% ME 500 0 0 0 0 0
2
1000 0 0 0 0 0
3 Flonicamid 15% + Pyriproxyfen 12% + Acetamiprid 2% OD 500 0 0 0 0 0
4
1000 0 0 0 0 0
5 Flonicamid 7.5% + Pyriproxyfen 6% + Acetamiprid 1% ME 1000 0 0 0 0 0
6
2000 0 0 0 0 0

7 Flonicamid 7.5% + Pyriproxyfen 6% + Acetamiprid 1% OD 1000 0 0 0 0 0
8
2000 0 0 0 0 0
9 Control - 0 0 0 0 0
0= No Phytotoxicity
Table 14 above shows that insecticidal composition of the present invention comprising Flonicamid, Pyriproxyfen and Acetamiprid did not show any phytotoxicity when applied at standard as well as higher dose (2x) in cotton crop.
The synergistic insecticidal composition of the present invention gave good control of insect pests along with significant increase in yield and better economics to farmers as compared to the reference products. Further, the use of the synergistic insecticidal composition resulted in better crop condition and did not produce any phytotoxic symptoms on the plants.
Thus, from the foregoing description, it will be apparent to one of the person skilled in the art that many changes and modifications can be made thereto without departing from the spirit or scope of the invention as set forth in the description. Accordingly, it is not intended that the scope of the foregoing description be limited to the description set forth above, but rather that such description be construed as encompassing such features that reside in the present invention, including all the features and embodiments that would be treated as equivalents thereof by those skilled in the relevant art.

We Claim:

[CLAIM 1]. A synergistic insecticidal composition comprising of
a) Acetamiprid;
b) Flonicamid;
c) Pyriproxyfen;
d) and at least one excipient;
wherein acetamiprid is present in an amount in the range from 1% to 10% w/w; flonicamid is present in an amount in the range from 7% to 40% w/w; and pyriproxyfen is present in an amount in the range from 6% to 50% w/w.
[CLAIM 2]. The synergistic insecticidal composition as claimed in claim 1, wherein the composition is one of:
a) acetamiprid is present in an amount of 1% w/w; flonicamid is present in an amount of 7.5% w/w; and pyriproxyfen is present in an amount of 6% w/w and at least one excipient.
b) acetamiprid is present in an amount of 2% w/w; flonicamid is present in an amount of 15% w/w; and pyriproxyfen is present in an amount of 12% w/w and at least one excipient.
c) acetamiprid is present in an amount of 5% w/w; flonicamid is present in an amount of 40% w/w; and pyriproxyfen is present in an amount of 20% w/w and at least one excipient.
d) acetamiprid is present in an amount of 10% w/w; flonicamid is present in an amount of 20% w/w; and pyriproxyfen is present in an amount of 50% w/w and at least one excipient.
[CLAIM 3]. The synergistic insecticidal composition as claimed in claim 1, wherein the composition is formulated as micro-emulsion (ME), oil-dispersion (OD), suspension concentrate (SC) or water dispersible granule (WG).
[CLAIM 4]. The synergistic insecticidal composition as claimed in claim 1 and 2, wherein the excipient is selected from the group comprising solvent, emulsifier, wetting agent, dispersing agent, defoamer, thickener, anti-freezing agent, biocide, disintegrating agent, filler or a combination thereof.

[CLAIM 5]. The synergistic insecticidal composition as claimed in claim 4, wherein the solvent is selected from the group comprising solvent CIX, solvent N,N-decanamide, water, mineral oil, or a combination thereof and present in an amount in the range from 5 to 80% w/w.
[CLAIM 6]. The synergistic insecticidal composition as claimed in claim 4, wherein the emulsifier is selected from the group comprising of a mixture of non-ionic surfactants and amine salt of phosphate tristyryl phenol ethoxylated, acrylic copolymer, ethoxylated polyarylphenol phosphate ester, polyoxyethylene ether of triglyceride ester, poly(oxy-l,2-ethanediyl) alpha-(tris(l-phenylethyl)phenyl)-omega-hydroxy or a combination thereof, and present in an amount in the range from 5 to 20% w/w.
[CLAIM 7]. The synergistic insecticidal composition as claimed in claim 4, wherein the dispersing agent is selected from the group comprising of naphthalene sulphonate derivative, naphthalene sulfonate of formaldehyde condensate, acrylic copolymer, graft copolymer, lignin based sulfonate, amine salt of phosphate tristyryl phenol ethoxylated or a combination thereof, and present in an amount in the range from 1 to 10% w/w.
[CLAIM 8]. The synergistic insecticidal composition as claimed in claim 4, wherein the wetting agent is selected from the group comprising of naphthalene alkyl aryl sulphonate, dioctyl sulfosuccinate, sodium lauryl sulfate, non-ionic ethoxylated, ethoxylated polyarylphenol phosphate ester, sodium alkyl naphthalene sulfonate or a combination thereof, and present in an amount in the range from 1 to 15% w/w.
[CLAIM 9]. The synergistic insecticidal composition as claimed in claim 4, wherein the defoamer is selected from the group comprising dimethyl polysiloxane emulsion, and present in an amount in the range from 0.01 to 2.0%> w/w.

[CLAIM 10]. The synergistic insecticidal composition as claimed in claim 4, wherein the thickener is xanthan gum present in an amount in the range from 0.01 to 3.0%
w/w.
[CLAIM 11]. The synergistic insecticidal composition as claimed in claim 4, wherein the anti-freezing agent is selected from the group comprising ethylene glycol, diethylene glycol, propylene glycol or a combination thereof and present in an amount in the range from 2 to 10% w/w.
[CLAIM 12]. The synergistic insecticidal composition as claimed in claim 4, wherein the biocide is selected from the group comprising 20% aqueous dipropylene glycol solution of 1,2- benzisothiazolin-3-one, formaldehyde or a combination thereof and present in an amount in the range from 0.01 to 0.50% w/w.
[CLAIM 13]. The synergistic insecticidal composition as claimed in claim 4, wherein the disintegrating agent is selected from the group comprising citric acid or sodium bicarbonate, or a combination thereof, and present in an amount in the range from 1 to 5% w/w.
[CLAIM 14]. The synergistic insecticidal composition as claimed in claim 4, wherein the filler is selected from the group comprising bentonite clay, china clay, silica, kaolin, diatomaceous earth or a combination thereof, and present in an amount in the range from 4 to 25% w/w.