A synergistic insecticidal composition

WO2026181113A1PCT designated stage Publication Date: 2026-09-03LEEDS LIFE SCIENCES PTE LTD
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Patent Information

Application Number
PCT/IN2026/050365
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2025-02-28
Filing Date
2026-02-27
Publication Date
2026-09-03

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Abstract

The present invention provides a novel synergistic insecticidal composition comprising of N- (Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, Indoxacarb, a stabilizer, and a pH modifying agent, along with at least one agriculturally acceptable excipient. The invention also 5 provides a process for preparation of the said insecticidal composition.
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Description

[0001] A SYNERGISTIC INSECTICIDAL COMPOSITION

[0002] FIELD OF INVENTION

[0003] The present invention relates to a synergistic insecticidal composition comprising a synergistically effective amount of at least two actives. More particularly, the present invention relates to a pesticidal composition comprising N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide, and at least one oxadiazine insecticide, and a process of preparation thereof.

[0004] BACKGROUND OF THE INVENTION

[0005] Controlling invertebrate pests’ results in improved crop efficiency in economically important crops. Invertebrate pests cause damage to growing and stored agronomic crops, resulting in a considerable decrease in crop yield. As a result, controlling invertebrate pests is economically important for crop productivity. To manage invertebrate pests, many treatments are available as single active components or in mixtures of two or more active compounds. However, more cost-effective and environmentally safe insecticidal compositions and process are continuously sought.

[0006] Furthermore, repeated and prolonged application of single compounds often leads to the development of resistance against the active compounds. Normally, such pests develop crossresistance against other actives having the same mode of action. Hence, there is a need for combinations of actives belonging to different classes and groups to allow for a broader disease control spectrum that combines curative and preventive actives and is stable.

[0007] In addition to biological efficacy and resistance management, formulation performance and storage stability is one of the major technical hurdles in developing commercially viable insecticidal composition. In practice, mixtures of actives particularly when formulated as concentrated dispersion-based products may suffer from instability during storage and transport. Such issues include physical instability (e.g., sedimentation, caking, poor redispersibility, viscosity drift, phase separation, particle-size growth, and loss of flowability), as well as chemical instability (e.g., degradation pathways sensitive to temperature, moisture, and pH). Under accelerated storage conditions, most of the formulations exhibit rapid deterioration, including crystallisation of one or more active ingredients, formation of hard cakes that are difficult to redispers, gradual increases in particle size leading to reduced suspension stability, and inconsistent sprayability and field deposition. These formulation-related problems are notcosmetic; they can translate into reduced bioavailability of the active ingredients on crop surfaces, diminished knockdown and residual performance, and variable pest control outcomes across crops and environmental conditions.

[0008] There is a need in the art to develop an insecticidal composition that is stable, synergistic, broad spectrum, environmentally safe, and effective in controlling a broad range of insect pests in crops. Insecticidal compositions with a broad range of activity are needed in order to avoid or delay the development of resistant strains to the active ingredients or mixtures of known active ingredients used by farmers while reducing chemical doses sprayed in agriculture fields.

[0009] OBJECT OF THE INVENTION

[0010] A primary objective of the present invention is to provide an insecticidal composition having an improved spectrum of insecticidal activity.

[0011] Another objective of the present invention is to provide an insecticidal composition having improved formulation stability, including improved physical and / or chemical stability.

[0012] Another objective of the present invention is to provide an insecticidal composition having extended shelflife, reduced crystallisation risk, improved dispersibility, and reduced caking.

[0013] Another objective of the present invention is to provide an insecticidal composition having a synergistic effect.

[0014] Another objective of the present invention is to provide a process for preparing the insecticidal composition.

[0015] Another objective of the present invention is to provide a method for controlling pests and diseases in the agriculture field.

[0016] Some or all these and other objectives of the invention may be achieved by way of the invention described hereinafter.

[0017] SUMMARY OF THE INVENTION

[0018] In an aspect, the present invention provides an insecticidal composition, comprising:a. N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount ranging from 1-60% w / w;

[0019] b. Indoxacarb in an amount ranging from 1-15% w / w; and

[0020] c . a stabilizer in an amount ranging from 0.01-15% w / w.

[0021] In another aspect, the stabilizer is poly (ethylene glycol-ran-propylene glycol) monobutyl ether.

[0022] In further aspect of the present invention, the composition comprises a pH modifying system, wherein said pH modifying system is present in an amount ranging from 0.01-8% w / w.

[0023] In yet another aspect, the pH modifying system comprises a mixture of Sodium hydroxide and Potassium Dihydrogen Phosphate.

[0024] In further aspect, the composition comprises at least one agriculturally acceptable excipient, wherein the agriculturally acceptable excipient are selected from dispersing agent, antifreezing agent, anti-foaming agent, a thickener, rheological modifier, a biocide, a wetting agent, a binder, an emulsifier, a carrier, a solvent, a co-solvent, or a mixture thereof.

[0025] In another aspect of the present invention, the composition comprises of:

[0026] the dispersing agent is present in an amount ranging from 0.1-20% w / w,

[0027] the anti -freezing agent is present in an amount ranging from 0.1-15% w / w, the wetting agent is present in an amount ranging from 0.1-15% w / w

[0028] the anti -foaming agent is present in an amount ranging from 0.1-2% w / w, the thickener is present in an amount ranging from 0.1-20% w / w,

[0029] the biocide is present in an amount ranging from 0.1-5% w / w,

[0030] the wetting agent is present in an amount from 0.1-10% w / w,

[0031] the binder is present in an amount ranging from 0.1-20% w / w,

[0032] the emulsifier is present in an amount ranging from 0.1-25% w / w.

[0033] In another aspect, the composition of the present invention may be formulated as into 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).

[0034] In an aspect, the present invention provides a process for preparing an insecticidal composition comprising N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and indoxacarb, the process comprising:

[0035] a. providing N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and indoxacarb;

[0036] b. providing an additive system comprising (i) a stabilizer and (ii) a pH-modifying system; c. mixing the N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and the indoxacarb with the additive system and at least one agriculturally acceptable excipient to form a process mixture; and

[0037] d. subjecting the process mixture to homogenisation to obtain a formulated composition.

[0038] In another aspect, the composition comprises stabilizer comprises poly (ethylene glycol-ran-propylene glycol) monobutyl ether and the pH-modifying system comprises a mixture of sodium hydroxide and potassium dihydrogen phosphate.

[0039] In another aspect, the composition comprises comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount of 1-60 wt.%, indoxacarb in an amount of 1-15 wt.%, the stabilizer in an amount of 0.01-15 wt.%, and the pH-modifying system in an amount of 0.1-5 wt.%.

[0040] In another aspect, the formulated composition is a suspension concentrate (SC), and wherein step (d) comprises:

[0041] forming the process mixture as an aqueous suspension comprising water;

[0042] wet-milling the aqueous suspension to obtain a particle size of below 10 pm; andincorporating a rheology modifier and a biocide to obtain the SC,

[0043] wherein, the SC comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.1-5 wt.%, stabilizer 0.01-15 wt.%, dispersing agent 1-5 wt.%, rheology modifier 0.1-2 wt.%, and preservative 0.1-2 wt.%.

[0044] In another aspect, the formulated composition is water dispersible granules (WDG), and wherein step (d) comprises:

[0045] dry-blending the process mixture with a carrier, a wetting agent and a dispersing agent to obtain a dry blend;

[0046] dry-milling the dry blend; and

[0047] granulating and drying the milled material to obtain the WDG,

[0048] wherein the WDG comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.1-5 wt.%, stabilizer 0.01-15 wt.%, dispersing agent 1-15 wt.%, stabilizer 0.01-15 wt.%, and pH-modifying system 0.1-2 wt.%.

[0049] In another aspect, the formulated composition is an oil dispersion (OD), and wherein step (d) comprises:

[0050] dispersing the process mixture in an oil phase comprising an oil and a solvent to obtain a dispersion; and

[0051] wet-milling the dispersion to obtain the OD,

[0052] wherein the OD comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.1-5 wt.%, stabilizer 0.01-15 wt.%, wetting agent 0.5-10 wt.%, and dispersing agent 0.5-10 wt.%.

[0053] In another aspect, the formulated composition is a dispersible concentrate (DC) or an emulsifiable concentrate (EC), and wherein step (d) comprises:

[0054] dissolving N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in a solvent system comprising a solvent and optionally a co-solvent to obtain a solution;

[0055] adding indoxacarb to obtain a homogeneous composition; and

[0056] incorporating an emulsifier system together with the stabilizer and the pH-modifying system to obtain the DC or the EC,

[0057] wherein, when the formulation is an EC, the obtained composition is filtered, andwherein the DC and EC comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.1-5 wt.%, stabilizer 0.01-15 wt.%, emulsifier 5-15 wt.%, and optionally co-solvent 1-30 wt.%.

[0058] In another aspect, the formulated composition is a wettable powder (WP), and wherein step (d) comprises:

[0059] dry-blending the process mixture with a dispersing agent to obtain a blend; and

[0060] grinding the blend to obtain particles having a size of below 20 pm, thereby obtaining the WP, wherein the WP comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.1-5 wt.%, stabilizer 0.01-15 wt.%, and dispersing agent 1-20 wt.%.

[0061] DETAILED DESCRIPTION OF THE INVENTION

[0062] Those skilled in the art will be aware that the invention described herein is subject to variations and modifications other than those specifically described. It is to be understood that the invention described herein includes all such variations and modifications. The invention also includes all such steps, features, compositions and compounds referred to or indicated in this specification, individually or collectively, and all combinations of any two or more of said steps or features.

[0063] Unless otherwise specified, all terms used in disclosing the invention, including technical and scientific terms, have the meaning as commonly understood by a person skilled in the art to which the invention belongs. For further guidance, term definitions may be included to better appreciate the teaching of the present invention. It is to be understood that the singular forms “a,” “an,” and “the” include plural referents unless the context clearly dictates otherwise.

[0064] It should be emphasized that the term “comprises / comprising” when used in this specification is taken to specify the presence of stated features, steps or components but does not preclude the presence or addition of one or more other features, steps, components or groups thereof.

[0065] As used herein, the term "insects" as used herein, includes all organisms in the class "Insecta."

[0066] The term “crop” shall include a multitude of desired crop plants or an individual crop plant. The term “control” means to inhibit the ability of pests to survive, grow, feed and / or reproduce,or to limit the pests related damage or loss in crop plants. To “control” pests may or may not mean killing the insects although, it may mean killing the pests.

[0067] The term “insecticide” or “pesticide” as used herein refers to any chemical substance used to destroy / kill, inhibit or otherwise adversely affect the insect pests.

[0068] The term “synergistic” as used herein, refers to the combined action of two or more active agents blended together and administered conjointly that is greater than the sum of their individual effects.

[0069] The terms “weight percent”, “wt-%”, “percent by weight”, “% by weight” and variations thereof, as used herein, refer to the concentration of a substance as the weight of that substance divided by the total weight of the composition and multiplied by 100. It is understood that, as used here, “percent “, “%” and the like are intended to be synonymous with “weight percent”, “wt. %”, etc.

[0070] Features that are described and / or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more embodiments and / or in combination with or instead of the features of the other embodiments.

[0071] Accordingly, the present invention aims to provide a synergistic insecticidal composition comprising at least one active compound selected from N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide, and oxadiazine insecticide.

[0072] As used herein, the active ingredient encompasses its agrochemically acceptable salt(s), derivative(s), or any other modified form.

[0073] In an embodiment, the insecticidal composition comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in the range of 1 to 60% w / w of the composition and oxadiazine compound in the range of 1 to 15% w / w of the composition.

[0074] In an embodiment, the insecticidal composition comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in the range of 1 to 60% w / w of the composition and indoxacarb in the range of 1 to 15% w / w of the composition.During composition development, significant technical problems such as instability under accelerated storage conditions, formation of hard cakes during grinding and storage, an increase in particle size over time leading to reduced flowability and poor dispersion, adverse effects on viscosity and suspension stability, and rapid crystallisation of one or both active ingredients were encountered. In addition to storage -related defects, early field evaluations showed reduced bio-efficacy and variability in pest control performance across crops, which was attributed to inconsistent dispersion, particle growth, and loss of chemical integrity during storage.

[0075] Accordingly, the composition was formulated with a polymeric stabiliser, namely oxirane, methyl-, polymer with oxirane, monobutyl ether (also referred to herein as “poly (ethylene glycol-ran-propylene glycol) monobutyl ether”.

[0076] In an embodiment, the composition of the present invention comprises of a stabilizer in combination with N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and indoxacarb. The stabilizer is in the range of 0.01 to 15% w / w of the composition.

[0077] In a further embodiment, the composition of the present invention further comprises a pH-modifying system, a mixture of sodium hydroxide and potassium dihydrogen phosphate in the range of 0.1 to 5% w / w of the composition.

[0078] In another embodiment, the stabilizer and the pH-modifying system act together to provide a synergistic stabilisation effect, producing an insecticidal composition that is stable, effective, and commercially viable.

[0079] In an embodiment, the insecticidal composition comprises:

[0080] a. N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide;

[0081] b. indoxacarb; and

[0082] c. a stabiliser.

[0083] In an embodiment, the insecticidal composition comprises:

[0084] a. N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide;

[0085] b. indoxacarb;

[0086] c. a stabiliser;d. a pH-modifying system; and

[0087] e. at least one agriculturally acceptable excipient.

[0088] In an embodiment aspect, the insecticidal composition, comprises:

[0089] a. N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount ranging from 1-60% w / w;

[0090] b. Indoxacarb in an amount ranging from 1-15% w / w; and

[0091] c . a stabilizer in an amount ranging from 0.01-15% w / w.

[0092] In another embodiment, the insecticidal composition comprises:

[0093] a. N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount ranging from 1-60% w / w;

[0094] b. Indoxacarb in an amount ranging from 1-15% w / w; and

[0095] c . a stabilizer in an amount ranging from 0.01-15% w / w.

[0096] d. a pH modifying system in an amount ranging from 0.01-8% w / w; and

[0097] e. at least one agriculturally acceptable excipient.

[0098] The stabilizer is poly (ethylene glycol-ran-propylene glycol) monobutyl ether. Commonly poly (ethylene glycol-ran-propylene glycol) monobutyl ether is also known as oxirane, methyl-, polymer with oxirane, monobutyl ether.

[0099] The pH modifying system is a mixture of sodium hydroxide and potassium dihydrogen phosphate.

[0100] The insecticidal composition comprises of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide in an amount ranging from 1-60% w / w, Indoxacarb in an amount ranging from 1-15% w / w, a stabilizer in an amount ranging from 0.01-15% w / w, a pH modifying system in an amount ranging from 0.01-8% w / w and at least one agriculturally acceptable excipient. In a preferred embodiment, the composition comprises of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount ranging from 1-50% w / w, Indoxacarb in an amount ranging from 1-15% w / w, a stabilizer in an amount ranging from 0.01-14% w / w, a pH modifying system in an amount ranging from 0.01-8% w / w and at least one agriculturally acceptable excipient.The composition of the present invention comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide, Indoxacarb, stabilizer and or pH modifying system and at least one at least one agriculturally acceptable excipient has synergistic action towards the pest control and are effective in terms of prolonged pest control in crops. In addition, the compositions of the present invention are also stable over a long period of time.

[0101] In another embodiment of the present invention, the synergistic composition may comprise one or more inactive excipients selected from, but not limited to, the group comprising carrier(s), surfactant(s), binder(s), disintegrating agent(s), dispersants or dispersing agent(s), wetting agent(s), stabilizer, pH modifier(s), emulsifier(s), plant growth enhancer(s), thickener(s), biocide(s), emulsifier(s), preservative(s), anti-freezing agent(s), antifoaming agent(s), defoamers colorant(s), inert filler(s), light absorber(s), mixing aid(s), solvent(s), pH-modifying substance(s) and buffer(s), pH modifying system, corrosion-inhibitor(s), fragrance(s), protective colloid(s), liquid and solid fertilizers), wetting agent(s), co-solvent(s), biocide(s), carrier(s), rheological modifier(s), or a combination thereof.

[0102] Exemplary emulsifiers that may be used in the compositions and formulations of the present invention include, but not limited to, salts of alkyl sulfates, such as di -ethanol ammonium lauryl sulfate; salts of aryl sulfonates, such as calcium dodecyl benzene sulfonate; alkyl phenolalkylene oxide addition products, such as nonyl phenol ethoxylate; alcohol-alkylene oxide addition products, such as tri-decyl alcohol ethoxylate; soaps, such as sodium stearate; dialkyl esters of sulfosuccinate salts, such as sodium di-(2 -ethylhexyl) sulfosuccinate; sorbitol esters, such as sorbitol oleate; quaternary amines, such as lauryl trimethyl ammonium chloride; polyethylene glycol esters of fatty acids, such as polyethylene glycol stearate; poly ethanoxy ether derivatives in organic solvent; block copolymers of ethylene oxide and propylene oxide; and salts of mono- and di-alkyl phosphate esters, or Ethoxylated castor oil or similar. It is also possible to use a mixture of one or more of these emulsifiers. The emulsifiers may be present in an amount of about 0-80% w / w of the composition.

[0103] Antioxidants that may be used in the compositions and formulations of the present invention include, but are not limited to, ascorbyl palmitate and ascorbyl tetra isopalmitate, Mg-ascorbyl phosphate, Na-ascorbyl phosphate, ascorbyl-acetate, tocopherol and derivates (such as vitamin E-acetate), mixtures of vitamin E, vitamin A and derivatives (vitamin-A -palmitate and acetate), as well as coniferyl benzoate, retinoic acid and derivatives, alpha-glucosyl rutin, ferulic acid,citric acid, furfurylidene glucitol, carnosine, butyl hydroxyl toluene, butyl hydroxyl anisole, and tri hydroxyl butyrophenone. It is also possible to use a mixture of one or more of these antioxidants. The antioxidants may be present in an amount of about 0-10% w / w of the composition.

[0104] Thickening agents or binder that may be used in the compositions and formulations of the present disclosure include, but not limited to, xanthan gum, modified xanthan gum, agar, succinoglycan gum (Rheozan), alginic acid, lactose, lactose monohydrate, alginate, a hydrated magnesium-aluminum silicate, for example attapulgite, calcium lactobionate, carrageenan, gellan gum, and guar gum. The thickening agent may be present in an amount of about 0-10% w / w of the composition.

[0105] The non-ionic surfactants or dispersants suitable that may be used in the compositions or formulations according to the present disclosure includes, but not limited to, polyethylene oxide-polypropylene oxide block copolymers, polyethylene glycol ethers of linear alcohols, reaction products of fatty acids with ethylene oxide and / or propylene oxide, furthermore polyvinyl alcohol, polyvinyl pyrrolidone, copolymers of polyvinyl alcohol and polyvinyl pyrrolidone and copolymers of (meth) acrylic acid and (meth) acrylic acid esters, furthermore Alkyl ethoxylates and alkylaryl ethoxylates, which may optionally be phosphated and optionally neutralized with bases, wherein sorbitol ethoxylates may be mentioned by way of example, as well as polyoxy alkylene amine derivatives.

[0106] The anionic surfactants or dispersants suitable for realizing the compositions or formulations according to the present disclosure include, but are not limited to, alkali metal and alkaline earth metal salts of alkylsulfonic acids or alkylaryl sulfonic acids. More preferably, the anionic surfactant may be a sodium salt of linear alkyl benzene sulphonate.

[0107] In exemplary embodiments, the surfactant / dispersant comprises an anionic surfactant / dispersant.

[0108] Antifoaming agents or defoamers suitable for realizing the compositions or formulations according to the present disclosure includes, but not limited to, silicone oils, polymethylsiloxane, simethicone octanol, magnesium stearate and combinations thereof. It is also possible to use a mixture of one or more of these antifoaming agents.Inert fillers suitable for realizing the compositions or formulations according to the present disclosure include, but are not limited to, inorganic particles such as carbonates, silicates, and oxides, organic substances, such as urea formaldehyde condensates, kaolin, rutile, silicon dioxide, silicon, highly disperse silica, silica gels, precipitated silica, colloidal silica, attapulgite china clay, and natural and synthetic silicates, talc and the likes or any combination thereof. The solvents that may be used for realizing the compositions and formulations of the present disclosure include, but are not limited to, water, water soluble solvents, alcohols, water insoluble solvents, organic solvents, and the like or combinations thereof. The solvent may be present in an amount of about 0-80% w / w of the composition.

[0109] Solvent(s) may be selected from the group comprising of, but not limited to, water, demineralized water (DM); alcohols such as ethanol, propanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, glycerine; 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 C9, solvent CIO, solvent C12, solvesso 100, solvesso 150, solvesso 200; chlorinated aliphatic or aromatic hydrocarbons such as chloro benzene, chloro ethylene, methylene chloride; esters such as ethyl acetate, di-isopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gammabutyrolactone; amides such as dimethyl formamide, N-methyl-2-pyrrolidone (NMP), N-octyl pyrolidone, N, N dimethyl decanamide; nitriles such as acetonitrile; cyclohexane, dimethyl formamide, isophoron and N-methyl pyrrolidon; organo sulfur compounds.

[0110] A dispersant, also known as a dispersing agent, is a substance that adsorbs onto the surface of particles, preserving their dispersion and preventing them from reaggregating. Dispersants are added to agrochemical formulations to aid in particle dispersion and suspension during manufacturing, as well as to ensure particles re-disperse in water in a spray tank. They're a common ingredient in wettable powders, suspension concentrates, and water-dispersible granules. Surfactants used as dispersants have the ability to strongly adsorb onto a particle surface and offer a charged or steric barrier to particle re -aggregation. Surfactants that are oftenemployed are anionic, non-ionic, or mixes of the two. Sodium lingo sulphonates are the most often used dispersants in wettable powder compositions.

[0111] Dispersing agent(s) may be selected from the group comprising, but not limited to, acrylic copolymer solution, alcohols, C9-ll-iso-, CIO-rich, and ethoxylated, acrylic graft copolymer.

[0112] Anti-freezing agent(s) may be selected from the group comprising, but not limited to, glycols, mono-ethylene glycol, di-ethylene glycol, propylene glycol, polyethylene glycols, methoxy polyethylene glycols, polypropylene glycols, poly-butylene glycols, glycerine, and ethylene glycol. Water-based formulations often cause foam during mixing operations in production. In order to reduce the tendency for foaming, anti -foaming agents are often added either during the production stage or before filling bottles. Generally, there are two types of anti -foaming agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane, while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.

[0113] Antifoaming agent(s) may be selected from the group comprising, but not limited to, silicon emulsion based anti-foam agents, Siloxane poly alkylene oxide, Poly dimethyl Siloxane, tri siloxane ethoxylates, and mixtures thereof.

[0114] Wetting agent(s) may be selected from the group comprising, but not limited to, alcohols, C9-II -iso-, CIO-rich, and ethoxylated, Oxirane, methyl-, polymer with oxirane, monobutyl ether.

[0115] Thickener(s) may be selected from the group comprising, 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, carboxy methylcellulose, polyvinyl pyrrolidone, carboxyvinyl polymer, acrylic polymer, starch derivative, or polysaccharide; or an inorganic fine powder selected from high purity silica, bentonite, or white carbon. These thickeners may be used alone or in combination.

[0116] Buffering agent(s) may be selected from the group comprising, but not limited to, potassium dihydrogen phosphate, and sodium hydroxide or a combination thereof.Preservatives or biocide may be selected from the group comprising, but not limited to, 20% aqueous dipropylene glycol solution of 1, 2-benzisothiazolin-3-one, 1, 2-benzisothiazolin-3-one, formaldehyde potassium sorbate, 4-hydroxybenzoic acid esters, 2-methyl-4-isothiazolin-3 -one, and 5-chloro-2-methyl-4-isothiazolin-3-one.

[0117] In an embodiment of the present invention, the insecticide is formulated into 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).

[0118] The composition of the present invention can be used to control the nsects from the order of the Lepidoptera, for example Agrotis ypsilon, Alabama argillacea, Anticarsia gemmatalis, Cacoecia murinana, Capua reticulana, Chilo partellus, Chilo suppressalis, Choristoneura fumiferana, Choristoneura occidentalis, Cirphis unipuncta, Cnaphalocrocis medinalis, Cydia pomonella, Diatraea saccharalis, Dendrolimus pini, Diaphania nitidalis, Earias vittella, Earias insulana, Elasmopalpus lignosellus, Eupoecilia ambiguella, Evetria bou-liana, Exelastis atomosa, Feltia subterranea, Galleria mellonella, Grapholitha fimebrana, Helicoverpa armigera, Helicoverpa virescens, Helicoverpa zea, Hellula undalis, Hibernia defoliaria, Hyphantria cunea, Hyponomeuta malinellus, Keiferia lycopersicella, Laphygma exigua, Leucinodes orbonalis, Leucoptera coffeella, Leucoptera scitella, Lithocol-letis blancardella, Lobesia botrana, Loxostege sticticalis, Lymantria dispar, Lyonetia clerkella, Malacosoma neustria, Mamestra brassicae, Marasmia pantalis, Maruca vitrata, Maruca testulalis, Mythimna separata, Orgyia pseu-dotsugata, Ostrinia nubilalis, Panolis flammea, Pectinophora gossypiella, Peridroma saucia, Phalera bucephala, Phthorimaea operculella, Phyllocnistis citrella, Pieris bras-sicae, Plathypena scabra, Plutella xylostella, Pseudoplusia includens,Rhyacionia frus-trana, Scirpophaga incertulas, Scirpophaga innotata, Scrobipalpula absoluta, Sesamia inferens, Sitotroga cerealella, Sparganothis pilleriana, Spilosoma obliqua, Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Thaumatopoea pityocampa, Tortrix viridana, Trichoplusia ni, Tuta absoluta and Zeiraphera Canadensis; beetles (Coleoptera), for example Adoretus bicolor, Agrilus sinuatus, Agriotes lineatus, Agriotes obscu-rus, Amphimallus solstitialis, Anisandrus dispar, Anthonomus grandis, Anthonomus pomorum, Anomala benghalensis, Aphthona euphoridae, Apogonia aerea, Athens haemorrhoidalis, Atomaria linearis, Blasto-phagus piniperda, Blitophaga undata, Bruchus rufimanus, Bruchus pisorum, Bruchus lentis, Byctiscus betulae, Cassida nebulosa, Cerotoma trifurcata, Cetonia aurata, Ceuthorrhynchus assimilis, Ceuthorrhynchus napi, Chaetocnema tibialis, Chiloloba acuta, Conoderus vespertinus, Crioceris asparagi, Ctenicera ssp., Diabrotica longicomis, Diabrotica semipunctata, Diabrotica punctata, Diabrotica speciosa, Diabrotica virgifera, Dicladispa armigera, Epila-chna varivestis, Epitrix hirtipennis, Eutinobothrus brasiliensis, Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Hylobius abietis, Hypera brunneipennis, Hypera postica, Ips typographus, Lema bilineata, Lema melanopus, Leptinotarsa decemlineata, Lepidiota stigma, Limonius califomicus, Lissorhoptrus oryzophilus, Maladera indica, Melanotus communis, Meligethes aeneus, Melolontha hippocastani, Melolontha melolontha, Oberea brevis, Oulema oryzae, Ortiorrhynchus sulcatus, Otiorrhynchus ovatus, Phaedon cochleariae, Phyllobius pyri, Phyllotreta chrysocephala, Phyllophaga sp., Phyllopertha horticola, Phyllotreta nemorum, Phyllotreta striolata, Popillia japonica, Sitona lineatus and Sito-philus granaria; flies, mosquitoes (Diptera), e.g. Atherigona orientalis, Calliphora vicina, Ceratitis capitata, Chrysomya bezziana, Chrysomya hominivorax, Chrysomya macellaria, Chrysops discalis, Chrysops silacea, Chrysops atlanticus, Cochliomyia hominivorax, Contarinia sorghicola Cordylobia anthropophaga, Culicoides furens, Culiseta inomata, Culiseta melanura, Dacus cucurbi-tae, Dacus oleae, Dasineura brassicae, Delia antique, Delia coarctata, Delia platura, Delia radicum, Dermatobia hominis, Fanniacanicularis, Geomyza Tripunctata, Gaster-ophilus intestinalis, Glossina morsitans, Glossina palpalis, Glossina fuscipes, Glossina tachinoides, Haematobia irritans, Haplodiplosis equestris, Hippelates spp., Hylemyia platura, Hypoderma lineata, Leptoconops torrens, Liriomyza sativae, Liriomyza trifolii, Lucilia caprina, Lucilia cuprina, Lucilia sericata, Lycoria pectoralis, Mansonia titillanus, Mayetiola destructor, Melanagromyza obtuse, Muscina stabulans, Oestrus ovis, Ophiomyia phaseli, Opomyza florum, Orseolia oryzae, Oscinella frit, Pegomya hysocyami, Phorbia antiqua, Phorbia brassicae, Phor-bia coarctata, Phlebotomus argentipes, Psorophora columbiae, Psila rosae, Psoro-phora discolor, Prosimulium mixtum, Rhagoletiscerasi, Rhagoletis pomonella, Sar-cophaga haemorrhoidalis, Sarcophaga sp., Simulium vittatum, Stomoxys calcitrans, Tabanus bovinus, Tabanus atratus, Tabanus lineola, and Tabanus similis, Tipula ol-eracea, and Tipula paludosa; thrips (Thysanoptera), e.g. Dichromothrips corbetti, Dichromothrips ssp , Frankliniella fusca, Frankliniella occidentalis, Frankliniella tritici, Scirtothrips citri, Scirtothrips dorsalis, Thrips oryzae, Thrips palmi and Thrips tabaci; termites (Isoptera), e.g. Calotermes flavicollis, Coptotermes formosanus, Heterotermes aureus, Leucotermes flavipes, Microtermes obesi, Odontotermes obesus, Reticulitermes flavipes, Termes natalensis; cockroaches (Blattaria - Blattodea), e.g. Blattella germanica, Penplaneta americana, Periplaneta japonica and Blatta orientalis; true bugs (Hemiptera), e.g. Acrostemum hilare, Acyrtho-siphon pisum, Acyrthosiphon onobrychis, Adelges laricis, Amrasca biguttula biguttula, Amrasca devastans, Amritodus atkinsoni, Aphidula nasturtii, Aphis fabae, Aphis forbesi, Aphis pomi, Aphis gossypii, Aphis crassivora, Aphis grossulariae, Aphis schneideri, Aphis spiraecola, Aphis sambuci, Aulacorthum solani, Bemisia argentifolii, Bemisia tabaci, Brachycaudus cardui, Brachy-caudus helichrysi, Brachycaudus persicae, Brachycaudus prunicola, Brevicoryne brassicae, Capitophorus homi, Cerosipha gossypii, Chaetosiphon fragaefolii, Cicadulina spp., Clavigralla gibbosa, Cryptomyzus ribis, Dreyfusia nordmannianae, Dreyfusia piceae, Dysdercus cingulatus, Dysaphis radicola, Dysaulacorthum pseudosolani, Dysaphis plantaginea, Dysaphis pyri, Empoasca fabae, Hyalopterus pruni, Hyperomyzus lactucae, Idioscopus spp. Leptoglossus phyllopus, Leptocorisa acuta, Lygus lineolaris, Lygus pratensis, Macrosiphum avenae, Macrosiphum euphorbiae, Ma-crosiphon rosae, Megoura viciae, Melanaphis pyrarius, Metopolophium dirhodum, My-zus persicae, Myzus ascalonicus, Myzus cerasi, Myzus varians, Nezara viridula, Nasonovia ribis-nigri, Nilaparvata lugens, Nephotettix virescens, Nephotettix nigropictus, Pemphigus bursarius, Perkinsiella saccharicida, Peregrinus maidis, Phorodon humuli, Pianococcus spp., Pseudococcus spp., Pyrilla perpusilla, Psylla mali, Psylla piri, Rhopalomyzus ascalonicus, Rhopalosiphum maidis, Rhopalosi-phum padi, Rhopalosiphum insertum, Sappaphis mala, Sappaphis mail, Schizaphis graminum, Schizoneura lanuginosa, Sitobion avenae, Sogatella furcifera, Trialeurodes vaporariorum, Toxoptera aurantiia, Psylla spp., Rhopalosiphum spp., Sitobion spp., Aonidiella aurantii, Lepidosaphes beckii, Saissetia oleae, Coccus hesperidum, Parthenolecanium comi; ants, bees, wasps, sawflies (Hymenoptera), e.g. Athalia rosae, Atta cephalotes, Atta capiguara, Atta cephalotes, Atta laevigata, Atta robusta, Atta sexdens, Atta texana, Crematogaster spp., Hoplocampa minuta, Hoplocampa testudinea, Monomorium pha-raonis, Solenopsis geminata, Solenopsis invicta, Solenopsis richteri, Solenopsis xyloni, Pogonomyrmex barbatus, Pogonomyrmex califomicus, Pheidole megacephala, Dasy-mutillaoccidentalis, Bombus spp. Vespula squamosa, Paravespula vulgaris, Paraves-pula pennsylvanica, Paravespula germanica, Dolichovespula maculata, Vespa crabro, Polistes rubiginosa, Camponotus floridanus, and Linepithema humile; crickets, grasshoppers, locusts (Orthoptera), e.g. Acheta domestica, Gryllotalpa gryllo-talpa, Locusta migratoria, Melanoplus bivittatus, Melanoplus femurrubrum, Melanoplus mexicanus, Melanoplus sanguinipes, Melanoplus spretus, Nomadacris septemfasciata, Schistocerca americana, Schistocerca gregaria, Dociostaurus maroccanus, Tachycines asynamorus, Oedaleus senegalensis, Zonozerus variegatus, Hieroglyphus daganensis, Kraussaria angulifera, Calliptamus italicus, Chortoicetes terminifera, and Locustana pardalina; Arachnoidea, such as arachnids (Acarina), e.g. of the families Argasidae, Ixodidae and Sarcoptidae, such as Amblyomma americanum, Amblyomma variegatum, Ambryomma maculatum, Argas persicus, Boophilus annulatus, Boophilus decoloratus, Boophilus microplus, Dermacentor silvarum, Dermacentor andersoni, Dermacentor variabilis, Hyalomma truncatum, Ixodes ricinus, Ixodes rubicundus, Ixodes scapularis, Ixodes holocyclus, Ixodes pacificus, Omithodorus moubata, Omithodorus hermsi, Omithodo-rus turicata, Omithonyssus bacoti, Otobius megnini, Dermanyssus gallinae, Psoroptes ovis, Rhipicephalus sanguineus, Rhipicephalus appendiculatus, Rhipicephalus evertsi, Sarcoptes scabiei, and Eriophyidae spp. such as Aculus schlechtendali, Phyllocoptrata oleivora and Eriophyes sheldoni; Tarsonemidae spp. such as Phytonemus pallidus and Polyphagotarsonemus latus; Tenuipalpidae spp. such as Brevipalpus phoenicis; Tetra-nychidae spp. such as Tetranychus cinnabarinus, Tetranychus kanzawai, Tetranychus pacificus, Tetranychus telarius and Tetranychus urticae, Panonychus ulmi, Panony-chus citri, and Oligonychus pratensis; Araneida, e.g. Latrodectus mactans, and Loxos-celes recluse; fleas (Siphonaptera), e.g. Ctenocephalides felis, Ctenocephalides canis, Xenopsylla cheopis, Pulex irritans, Tunga penetrans, and Nosopsyllus fasciatus; silverfish, firebrat (Thysanura), e.g. Lepisma saccharina and Thermobia domestica; centipedes (Chilopoda), e.g. Scutigera coleoptrata; millipedes (Diplopoda), e.g. Narceus spp.; Earwigs (DermapteraJ, e.g. forficula auricularia. Preferbaly the composition is useful against Plutella xylostella, Liriomyza trifolii, Frankliniella occidentalis, Scirtothrips dorsalis, Thrips tabaci, Amrasca biguttula biguttula, Amrasca devastans, Amritodus atkinsoni, Aphis gossypii, Aphis crassivora, Bemisia argentifolii, Bemisia tabaci, Empoasca fabae, Nilaparvata lugens, Nephotettix virescens, Nephotettix nigropictus, Pianococcus spp., Pseudococcus spp., Pyrilla perpusilla, Trialeurodes vaporariorum, Tetranychus cinnabarinus, Tetranychus telarius and Tetranychus urticae, Panonychus ulmi, Oligonychus pratensis, Polyphagotarsonemus latus.The list of crops which can be suitable for protection by the present composition are Cotton (Gossypium spp.), Jute (Corchorus oliotorus), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Ragi (Eleusine coracana), Pearl millet (Pennisetum glaucum), 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 (Cicer aritinum), 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 rapa subsp rapa), Apple (Melus domestica), Banana (Musa 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-graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (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) and GMO derivatives thereof.

[0119] EXAMPLES

[0120] 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 a suspension concentrate (20% N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide + 12% Indoxacarb)

[0121] Table 1

[0122] &

[0123]

[0124] Preparation method is as follows:

[0125] Step 1 : The required amount of demineralised water was taken into a prefeed mixing vessel, followed by the addition of a pH-modifying agent (mixture of Potassium Dihydrogen Phosphate and Sodium Hydroxide) and an antifoaming agent (Silicon defoamer). The constituents were mixed thoroughly to obtain a homogeneous solution. This is followed by adding an antifreeze agent (propylene glycol) under constant stirring to obtain a uniform homogeneous solution.

[0126] Step 2: The dispersing agent (acrylic graft polymer) and the stabilizer (poly (ethylene gly col-ran-propylene glycol) monobutyl ether) were added to the pre-mixed solution. The resulting mixture was stirred continuously for 15-20 minutes to ensure a uniformly dispersed solution.

[0127] Step 3: N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (Technical) and Indoxacarb (Technical) were added to the above mixture. The mixture was homogenised for20-40 minutes to achieve a uniform dispersion of the active components. More particularly, the mixture was homogenised for 30 minutes to achieve a uniform dispersion.

[0128] Step 4: The homogeneous dispersion was transferred to a ball mill and ground under wet conditions to reduce particle size. The mean particle size targeted was less than 10 microns.

[0129] Step 5: A solution of the thickener (xanthan gum), the biocide (l,2-Benzisothiazolin-3-one), and the remaining quantity of demineralised water was added to the milled material, thoroughly mixed to achieve a uniform composition. The entire mass was homogenised using a high-shear homogeniser for 20 minutes to obtain a uniform, stable formulation.

[0130] Step 6: The homogeneous formulation is subjected to analytical testing by the quality control department to check for the quality parameters. The formulation upon meeting the parameters was packed for final handling upon receiving approval from Quality Check.

[0131] Storage stability of the Suspension concentrate

[0132] The chemical and physical stability of the composition was evaluated by Accelerated Heat Storage (AHS) study. The AHS is a type of testing in agrochemical development that subjects products to elevated temperature and humidity conditions to predict their shelf-life and stability.

[0133] Table 2 summarizes the stability of the active ingredient(s) and critical physical-chemical properties (such as suspensibility, pH, viscosity, and density) at 25°C and 54°C at a time-period of 14 days.

[0134] Table 2: Storage stability data

[0135]

[0136] >

[0137]

[0138] As shown in Table 2, both active ingredients (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and Indoxacarb) undergo minimal degradation, indicating greater stability of the formulation. The suspensibility of both active ingredients is very high, indicating uniform dispersion. Other physical parameters, such as pH, viscosity, density, and particle size, show minimal to negligible changes even after 14 days at 54 °C. Thus, the above data indicate that the formulation is highly stable.

[0139] The long-term stability of the formulation was evaluated to determine its shelf-life stability and performance overtime. Table 3 shows shelf-life stability data at 3 -month, 6-month, and 1-year intervals. This data shows the physical attributes such as suspensibility, pH, viscosity and density of the formulation over the time period of 3 months, 6 months and 1 year.

[0140] Table 3: Shelf-life stability data

[0141]

[0142]

[0143] Table 3 shows the stability data for the suspension concentrate over 3 months, 6 months, and 1 year. The experimental data show that the physical properties of the suspension, such as pH, viscosity, density, and particle size, change minimally to negligibly, reflecting the high stability of the formulation.

[0144] Example 2: Suspension concentrate (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 25%+ Indoxacarb 8%)

[0145] Table 4: Preferred composition

[0146] &

[0147]

[0148] The storage stability data of the above composition is shown in Table 5.

[0149] Table 5

[0150]

[0151] >

[0152]

[0153] As shown in Table 5, the active ingredients exhibit minimal degradation over 14 days, even at 54 °C. Furthermore, the formulation's physical parameters, such as suspensibility, pH, viscosity, density, and particle size, show minimal to negligible degradation over 14 days. Therefore, it is evident that the formulation is highly stable.

[0154] The shelf-life stability data are shown in Table 6.

[0155] Table 6

[0156]

[0157]

[0158] Table 6 shows the stability data for the suspension concentrate over 3 months, 6 months, and 1 year. The table shows that the suspension concentrate parameters exhibit minimal to negligible degradation over 1 year. Thus, the formulation is highly stable and can be stored for at least a period of 1 year without losing its efficacy.

[0159] Example 3: Suspension concentrate (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 19% + Indoxacarb 8.5%)

[0160] Table 7

[0161] &

[0162]

[0163] Preparation Method

[0164] Step 1 : The required amount of demineralised water was taken into a prefeed mixing vessel, followed by the addition of a pH-modifying agent (a mixture of Potassium Dihydrogen Phosphate and Sodium Hydroxide) and an antifoaming agent (Silicon defoamer). The constituents were mixed thoroughly to obtain a homogeneous solution. This is followed byadding an antifreeze agent (propylene glycol) under constant stirring to obtain a uniform homogeneous solution.

[0165] Step 2: The dispersing agent (acrylic graft polymer) and the stabilizer (poly (ethylene glycol-ran-propylene glycol) monobutyl ether) were added to the pre-mixed solution. The resulting mixture was stirred continuously for 15-20 minutes to ensure a uniformly dispersed solution.

[0166] Step 3: N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (Technical) and Indoxacarb (Technical) were added to the above mixture. The mixture was homogenised for 20-40 minutes to achieve a uniform dispersion of the active components. More particularly, the mixture was homogenised for 30 minutes to achieve a uniform dispersion.

[0167] Step 4: The homogeneous dispersion was transferred to a ball mill and ground under wet conditions to reduce particle size. The mean particle size targeted was less than 10 microns.

[0168] Step 5: A solution of the thickener (xanthan gum), the biocide (l,2-Benzisothiazolin-3-one), and the remaining quantity of demineralised water was added to the milled material, thoroughly mixed to achieve a uniform composition. The entire mass was homogenised using a high-shear homogeniser for 20 minutes to obtain a uniform, stable formulation.

[0169] Step 6: The homogeneous formulation is subjected to analytical testing by the quality control department to check for the quality parameters. The formulation upon meeting the parameters was packed for final handling upon receiving approval from Quality Check.

[0170] The storage stability data of the above composition is shown below in Table 8.

[0171] Table 8

[0172]

[0173]

[0174] As shown in Table 8, both active ingredients (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and Indoxacarb) undergo minimal degradation, indicating greater stability of the formulation. The suspensibility of both active ingredients is very high, indicating uniform dispersion. Other physical parameters, such as pH, viscosity, density, and particle size, show minimal to negligible changes even after 14 days at 54 °C. Thus, the above data indicate that the formulation is highly stable.

[0175] The shelf-life stability data of the above composition is shown below in Table 9.

[0176] Table 9

[0177]

[0178] Table 9 shows the stability data for the suspension concentrate over 3 months, 6 months, and 1 year. The table shows that the suspension concentrate parameters exhibit minimal to negligible degradation over 1 year. Thus, the formulation is highly stable and can be stored for at least 1 year without losing efficacy.

[0179] Example 4: Preparation of insecticidal composition as a water dispersible granule (WDG) (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10%).

[0180] Table 11: WDG) (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10%).

[0181] &

[0182]

[0183] Preparation method

[0184] Step 1: Required amount ofN-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb was taken in a pre-mixing blender along with a carrier (China clay), one or more dispersing agents(Naphthalene and sodium salt of alkyl naphthalene sulphonic acids formaldehyde condensate and Sodium dibutyl naphthalene sulphonate), a wetting agent (linear alcohol derivative), a binder (Lactose), a stabilizer (Oxirane, methyl-, polymer with oxirane, monobutyl ether), and a pH-modifying agent (mix of Sodium hydroxide and Potassium dihydrogen phosphate). The mixture was thoroughly blended for 20-40 minutes (preferably 30) to achieve homogeneity.Step 2: The pre-blended material was passed through a Jet Mill or Air Classifier Mill to achieve the desired particle size (specify target particle size range and operational parameters such as air pressure or mill speed).

[0185] Step 3 : The finely ground particles were transferred to a post-blender and blended for 1 -3 hours (preferably 1.4 hours) to obtain a completely homogeneous mixture. A sample was taken from this homogenous mixture and was sent to the Quality Control (QC) department for analysis. The next steps were carried out after the QC approval.

[0186] Step 4: The required quantity of water was added to the homogeneous mixture to form an extrudable dough. The dough was passed through an extruder to form granules of the required size.

[0187] Step 5 : The obtained wet granules were transferred to a Fluidised Bed Dryer (FBD) for drying while maintaining a required moisture content. The dried granules were passed through vibrating screens to grade them into uniform particle sizes and remove fine and oversized particles.

[0188] Step 6: The granules were sent for Quality check and approval (specify parameters tested and acceptable limits). Upon approval, the granules were packed into appropriate sizes (specify weight or volume per pack), using bags with LDPE liners for moisture protection (specify thickness or LDPE grade).

[0189] Table 12: Physicochemical Properties of the WDG formulation &

[0190]

[0191] Example 5: Water dispersible granules (WDG)Table 13: Composition

[0192] &

[0193]

[0194] The Water Dispersible Granule (WDG) formulation was tested for parameters as shown in Table 14.

[0195] Table 14: Properties of the WDG composition

[0196]

[0197] Example 6: Emulsifiable concentrate (EC) (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 13.5% + Indoxacarb 8%)

[0198] Table 15

[0199]

[0200] & &

[0201]

[0202] Preparation method

[0203] Step 1: A light aromatic solvent (petroleum) was taken in a vessel. To it, the required amount of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and Indoxacarb was added under stirring, followed by the addition of a co-solvent (Dimethylformamide) to the reaction mixture. The mixture was thoroughly stirred until the active ingredients were fully dissolved.

[0204] Step 2: Upon complete dissolution of the active ingredients, an emulsifier (calcium alkyl aryl sulfonate and phenol ethylene oxide), a stabilizer (Oxirane, methyl-, polymer with oxirane, monobutyl ether) and a pH-modifying agent (Mix of Sodium Hydroxide & Potassium dihydrogen phosphate) were added to the solution, followed by continuous stirring for 20 to 40 minutes (preferably 30 minutes) to obtain a reaction mixture.

[0205] Step 3 : The reaction mixture was passed through a sparkler filter to obtain the emulsifiable concentrate (EC) formulation.

[0206] The storage stability data for the EC formulation are shown in Table 16.

[0207] Table 16

[0208]

[0209]

[0210] Example 7: Wettable powder formulation (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 14.50% + Indoxacarb 5.20%)

[0211] Table 17

[0212] &

[0213]

[0214] Preparation method

[0215] Step 1 : The required amounts of the active ingredients were weighed and placed into a preblender. A dispersing agent, a pH-modifying agent, a stabiliser, and citric acid were added to the pre-blender. The entire mass was blended for 20-40 minutes (preferably 30 minutes) to obtain a uniform mixture.

[0216] Step 2: The mixture was passed through an air-classifying mill to obtain a powder comprising fine particles with a particle size below 20 microns. The milled powder mass was collected in a post-blender and homogenised for 20-40 minutes (preferably for 30 minutes) to obtain the wettable powder formulation. The formulation was then sent for quality check.

[0217] Example 8: Oil dispersion (OD) (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 20% + Indoxacarb 4.30%)

[0218] Table 18

[0219] Percentage (w / w)

[0220]

[0221] &

[0222]

[0223] Preparation method

[0224] Step 1 : The required quantity of oil is taken in a manufacturing vessel, followed by the addition of the required amount of solvent, and the mixture is thoroughly mixed using a high-shear homogeniser for 20-40 minutes (preferably 30 minutes) to obtain a homogeneous oil-solvent mixture.

[0225] Step 2: To the homogeneous oil-solvent mixture, required quantities of a wetting agent, a dispersing agent, a stabiliser, a pH-modifying agent and a suspending agent were added. The mixture was homogenised using a high-shear homogeniser for 45-60 minutes to obtain a uniformly dispersed solution.

[0226] Step 3: N-(Cyanomethyl)-4-(trifluorom ethyl) pyridine-3 -carboxamide and Indoxacarb were added to the uniformly dispersed solution and further homogenised for 20-40 minutes (preferably 30 minutes) to obtain a homogeneous mixture.

[0227] Step 4: The homogeneous mixture was passed through a horizontal bead mill to obtain particles with a desired size. The remaining oil, carrier, and carrier solution were added to the milled dispersion, and the mixture was stirred with a homogeniser for 10-30 minutes (preferably 20 minutes) to obtain a homogeneous oil dispersion.

[0228] Step 5 : A sample of the oil dispersion formulation was taken and sent to Quality Control for analysis of various parameters, including active ingredient analysis and particle size analysis.Step 6: Upon QC approval, the final product was transferred to a suitable holding tank for storage under appropriate conditions until packing.

[0229] Example 9: Dispersion concentrate (DC) (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 24.8% + Indoxacarb 3.5%)

[0230] Table 19: Preferred Composition

[0231] &

[0232]

[0233] Preparation method

[0234] Step 1: Required quantities of the solvent (2 -Butoxyethanol) and the co-solvent (N,N-Dimethyl decanamide) were taken in a vessel.

[0235] Step 2: The required quantity ofN-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide (Technical) was added to the solvent mixture under continuous stirring at a controlled speed of 100 RPM, maintaining a temperature between 45 °C and 50 °C. The mixture was stirred for another 20 minutes, then cooled to 25 °C.

[0236] Step 3 : Indoxacarb (Technical) was added to the above mixture under continuous stirring at a controlled temperature range to obtain a homogeneous solution.

[0237] Step 4: An emulsifier (ethoxylated castor oil), a stabiliser, a pH-modifying agent, and a dispersing agent were added to the mixture under continuous stirring. The mixture was homogenised at 1400 RPM for 20-40 minutes (preferably 30 minutes) to obtain a stableemulsion. A sample was obtained and sent for quality analysis to assess various physical and chemical parameters, including physical state, colour, pH, density, dispersion stability, and water solubility. The material was packed after receiving quality control approval.

[0238] The physicochemical properties of the DC formulation are shown in Table 20.

[0239] Table 20

[0240]

[0241] The storage stability data for the DC formulation as shown in Table 21.

[0242] Table 21: Storage stability data

[0243]

[0244] Example 10: Dispersion concentrate (DC).

[0245] Table 22: Preferred Composition

[0246]

[0247] &

[0248]

[0249] Preparation method

[0250] Step 1: Required quantities of the solvent (2 -Butoxyethanol) and the co-solvent (N, N-Dimethyl decanamide) were taken in a vessel.

[0251] Step 2: The required quantity ofN-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide (Technical) was added to the solvent mixture under continuous stirring at a controlled speed of 100 RPM, maintaining a temperature between 45 °C and 50 °C. The mixture was stirred for another 20 minutes, then cooled to 25 °C.

[0252] Step 3 : Indoxacarb (Technical) was added to the above mixture under continuous stirring at a controlled temperature range to obtain a homogeneous solution.

[0253] Step 4: The emulsifier (ethoxylated castor oil), stabiliser, pH-modifying agent, and dispersing agent were added to the mixture under continuous stirring. The mixture was homogenised at 1400 RPM for 20-40 minutes (preferably 30 minutes) to obtain a stable emulsion. A sample was obtained and sent for quality analysis to assess various physical and chemical parameters, including physical state, colour, pH, density, dispersion stability, and water solubility. The material was packed after receiving quality control approval.

[0254] The physicochemical properties and storage stability data of the above DC formulation are shown in Table 23 and 24, respectively.Table 23: Physicochemical properties of the DC formulation

[0255]

[0256] Table 24: Storage stability data

[0257]

[0258] FIELD EVALUATION OF THE BIO EFFICACY OF THE INSECTICIDAL COMPOSITION

[0259] The present invention’s insecticidal combination was tested for its efficacy against Cotton White fly (Bemisiatabaco), Cotton Aphids (Aphis gossypii) and cotton bollworm (Helicoverpa armigera) in cotton crops and okra Jassids (Amrasca biguttula biguttula), Aphids (Aphis gossypii), and Fruit borer (Earias vittella) in okra crops.

[0260] The experiment was laid out in a Randomised Block Design (RBD) with three replications, maintaining a single plot size of 25 m2The test insecticide treatments, as per the treatmentschedule, were applied at pest appearance using 500 litres of water per hectare with a knapsack sprayer, ensuring uniform coverage.

[0261] The treatment details are provided below in Table 25.

[0262] Table 25 : Treatment Details

[0263]

[0264]

[0265] Evaluation of Bio-efficacy:

[0266] The bio-efficacy evaluation was carried out by randomly selecting five plants per replication and observing three leaves per plant (one each from the top, middle, and bottom canopy) for sucking pests in cotton and okra.

[0267] The percent reduction in pest population over untreated control was calculated using the Henderson and Tilton (1955) formula as given below:

[0268]

[0269] Where:

[0270] • Ta = Number of insects in treated plot after application

[0271] • Tb = Number of insects in treated plot before application

[0272] • Ca = Number of insects in untreated control after application

[0273] • Cb = Number of insects in untreated control before application

[0274] Data Collection

[0275] Pre-treatment observations (pre-count) were recorded one day prior to spray application.

[0276] Post-treatment observations were recorded at 3, 7, and 10 days after application (DAA) for sucking pests such as whitefly (Bemisia tabaci) and aphids (Aphis gossypii).

[0277] For bollworm infestation in cotton (Helicoverpa armigerd) and fruit borer in okra (Earias vittella), observations were recorded by counting the number of larvae per plant and percent damaged squares / bolls in cotton and percent damaged fruits in okra from the same selected plants at 3, 7, and 10 DAA.

[0278] Colby’s Method for Synergism / Antagonism

[0279] To determine interaction effects, the observed mortality rates of white fly, cotton bollworm and cotton aphids in two-way combinations were compared with expected mortality rates using Colby’s formula (Colby, 1967).The synergistic action expected for a given combination of two-way active components can be calculated as follows:

[0280]

[0281] Where E is the expected mortality, and A and B are the observed mortalities of the individual components.

[0282] Synergistic effects were indicated if the observed mortality was greater than the expected mortality, while antagonistic effects were noted if the observed mortality was lower.

[0283] Example 11: Field evaluation of the bio efficacy of the present insecticidal composition

[0284] The bio-efficacy of the presently claimed insecticide composition was assessed against Whitefly (Bemisia tabaci). Aphids (Aphis gossypii) and Bollworm (Helicoverpa armigerd) in cotton crops under field conditions. The effectiveness was measured as the percentage reduction of the pests over control at different intervals of 3, 7 and 10 days after application. The studies were carried out in in Rasi (Magic RCH 386 BGII) variety of cotton crops in Kharif season, 2024 in Telengana. The trial was conducted at a temperature range of 26-34°C in a single plot size of 25m2.

[0285] Table 26(a): Effect of insecticide on white fly at 3, 7 and 10 days of application

[0286]

[0287]

[0288] As seen in Table 26(a), the combinations of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb were highly effective against cotton whitefly. The above fielddata also show that the efficacy of the insecticidal combination increases with increasing dosage.

[0289] The highest percentage control was observed with FE3 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 73.69% reduction at 3 DAA, 84.89% reduction at 7 DAA, and 95.32% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine -3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed 74.13% reduction at 3DAA, 88.13% at 7DAA, and 94.77% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 3.5% + Indoxacarb 8% EC) at 750 ml / ha showed 73.24% reduction at 3DAA, 81.16% at 7DAA, and 93.39% at 10DAA. Whereas, the solo application of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and Indoxacarb shows lower reduction rates in cotton plants.

[0290] Table 26(b): Effect of Insecticide on Cotton Aphids at 3, 7 and 10 days of application

[0291]

[0292]

[0293] As seen in Table 26(b), the highest percentage control was observed with FE3 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 78.99% reduction at 3 DAA, 85.02% reduction at 7 DAA, and 92.56% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed reductions of 76.36% at 3DAA, 84.67% at 7DAA, and 90.69% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 13.5% + Indoxacarb 8% EC) at 750 ml / ha showed 72.22% reduction at 3DAA, 83.03% at 7DAA, and 90.41% at 10DAA.

[0294] Table 24(c): Effect of Insecticide on Cotton Bollworm at 3, 7 and 10 days of application

[0295]

[0296]

[0297] As seen in Table 26(c), the highest percentage control was observed with FE3 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 80.35% reduction at 3 DAA, 85.14% reduction at 7 DAA, and 92.89% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed reductions of 78.61% at 3DAA, 83.82% at 7DAA, and 92.27% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 13.5% + Indoxacarb 8% EC) at 750 ml / ha showed 76.27% reduction at 3DAA, 82.05% at 7DAA, and 91.01% at 10DAA. Whereas, the solo application of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb are comparatively less effective against the presently disclosed insecticidal composition.

[0298] Table 27: Synergistic effect of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3- carboxamide + Indoxacarb against cotton aphids, cotton whitefly and cotton bollworm.

[0299]

[0300]

[0301] Example 12: Field evaluation of the bio efficacy of the present insecticidal composition.

[0302] The bio-efficacy of the insecticidal composition was assessed against aphids (Aphis gossypii), jassids (Amrasca bigutella bigutella) and fruit borer (Earias vitelli) in Okra under field conditions. Effectiveness was measured as the percentage reduction in pest numbers relative to the control at 3, 7, and 10 days after application. The studies were conducted on the Namdhari NS862 okra variety during the Kharif season of 2024 in Gujarat. The trial was conducted at a temperature range of 18-30°C in a single plot measuring 25 m2.Table 28(a): Effect of Insecticide on Okra Jassids at 3, 7 and 10 days of application

[0303]

[0304]

[0305] As seen in Table 28(a), the highest percentage control was observed with FE3 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 75.88% reduction at 3 DAA, 85.87% reduction at 7 DAA, and 96.22% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed 73.67% reduction at 3DAA, 85.98% at 7DAA, and 96.92% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 13.5% + Indoxacarb 8% EC) at 750 ml / ha showed 72.77% reduction at 3DAA, 83.70% at 7DAA, and 95.22% at 10DAA. Whereas, the solo application of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb shows lower reduction rates in okra plants.

[0306] Table 28(b): Effect of Insecticide on Okra Aphids at 3, 7 and 10 days of application

[0307]

[0308]

[0309]

[0310] As seen in Table 28(b), the highest percentage control was observed with FE3 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 76.55% reduction at 3 DAA, 84.98% reduction at 7 DAA, and 96.48% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed reductions of 75.39% at 3DAA, 84.82% at 7DAA, and 96.23% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 13.5% + Indoxacarb 8% EC) at 750 ml / ha showed 73.43% reduction at 3DAA, 84.51% at 7DAA, and 95.09% at 10DAA. Whereas, the solo application of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb shows lower reduction rates in okra plants.

[0311] Table 28(c): Effect of Insecticide on Okra Fruit Borer at 3, 7 and 10 days of application

[0312]

[0313]

[0314] As seen in Table 28(c), the highest percentage control was observed with FE3 (N- (Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 20% + Indoxacarb 12% SC) at 500ml / ha, with 79.31% reduction at 3 DAA, 90.52% reduction at 7 DAA, and 94.58% reduction at 10 DAA. This was closely followed by FE6 (N-(Cyanomethyl)-4-(trifluoromethyl)pyridine-3 -carboxamide 17% + Indoxacarb 10% WDG) at 600 ml / ha, which showed reductions of 78.71% at 3DAA, 89.35% at 7DAA, and 93.24% at 10DAA. Similarly, FE9 (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide 13.5% + Indoxacarb 8% EC) at 750 ml / ha showed 76.43% reduction at 3DAA, 88.21% at 7DAA, and 92.52% at 10DAA. Whereas, the solo application of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and Indoxacarb shows lower reduction rates in okra plants.

[0315] Table 29: Synergistic effect of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide + Indoxacarb against okra jassids, okra aphids and okra fruit borer

[0316]

[0317]

[0318] Example 28: Evaluation of phytotoxicity in cotton and okra crops.

[0319] Visual observations were recorded at 3, 7, and 10 days after application (DAA) of the tested product. The parameters observed were leaf injury at the tip / surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting, rated on a 0-10 scale as shown in the table below. A total of 20 plants per plot were observed.

[0320]

[0321]

[0322] Phytotoxic studies

[0323] Evaluation of phytotoxicity in coton crops

[0324] Table 30(a): Phytotoxic effects of various treatment on coton crops after 3DAA at recommended dose.

[0325]

[0326]

[0327] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0328] Table 30(b): Phytotoxic effects of various treatment on cotton crops after 7DAA at recommended dose.

[0329]

[0330] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E- Epinasty, H-Hyponasty, W-wiltingTable 30(c): Phytotoxic effects of various treatment on cotton crops after 10DAA at recommended dose.

[0331]

[0332] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0333] Table 30(d): Phytotoxic effects of various treatment on cotton crops after 3DAA at double dose.

[0334]

[0335] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0336] Table 30(e): Phytotoxic effects of various treatment on cotton crops after 7DAA at double dose.

[0337]

[0338]

[0339] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0340] Table 30(f): Phytotoxic effects of various treatment on cotton crops after 10DAA at double dose.

[0341]

[0342] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0343] Evaluation of phytotoxicity in okra cropsTable 31(a): Phytotoxic effects of various treatment on cotton crops after 3DAA at recommended dose.

[0344]

[0345] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0346] Table 31(b): Phytotoxic effects of various treatment on cotton crops after 7DAA at recommended dose.

[0347]

[0348]

[0349] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0350] Table 31(c): Phytotoxic effects of various treatment on cotton crops after 10 DAA at recommended dose.

[0351]

[0352]

[0353] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0354] Table 31(d): Phytotoxic effects of various treatment on cotton crops after 3DAA at double dose

[0355]

[0356]

[0357] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0358] Table 31(e): Phytotoxic effects of various treatment on cotton crops after 7 DAA at double dose.

[0359]

[0360]

[0361] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0362] Table 31(f): Phytotoxic effects of various treatment on cotton crops after 10DAA at double dose.

[0363]

[0364]

[0365] DAA - Days after application, L-Leaf injury on tips / surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting

[0366] As seen in Tables 30(a-f) and 3 l(a-f), there is no phytotoxicity associated with the treatment of any of the ingredients on the plants, suggesting that the said composition is completely safe to use. The present invention provides a novel and synergistic combination of N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and indoxacarb. While the present specification illustrates various concentrations across which enhanced results are observed, in particular, the suspension concentrate (N-(Cyanomethyl)-4-(trifluoromethyl) pyridine -3 -carboxamide 20% + Indoxacarb 12%) when applied at a dosage of 5001 / ha shows the best results in reducing pests on both cotton and okra plants.

[0367] Table 32: Comparative Formulation Composition: Present Invention vs Conventional Stabilizer and pH-Modifying System

[0368]

[0369] &

[0370]

[0371] Table 32 demonstrates that the only distinguishing feature between the present invention and the comparative composition is the selection of (i) the polymeric stabilizer and (ii) the buffered pH-modifying system comprising sodium hydroxide in combination with potassium dihydrogen phosphate. All other formulation components are identical in both nature and concentration. The comparison clearly establishes that the improvements in stability and performance of the present invention composition.

[0372] Table 33: Accelerated Heat Stability

[0373] & &

[0374]

[0375]

[0376] Particle Size

[0377]

[0378]

[0379]

[0380] Table 33 demonstrates that the composition comprising the claimed stabilizer and pH-modifying system maintains chemical assay, suspensibility, viscosity, particle size distribution, and pH within acceptable limits under both ambient and accelerated storage conditions (54°C). In stark contrast, the comparative composition exhibits severe physical instability (hard caking), drastic loss of suspensibility, assay reduction, pH failure, viscosity non-compliance, and particle instability.

[0381] Table 34: Comparative Formulation Composition: Present Invention vs Conventional Stabilizer and pH-Modifying System

[0382] &

[0383]

[0384] Table 34 demonstrates that the composition comprising the claimed stabilizer and pH-modifying system maintains chemical assay, suspensibility, viscosity, particle size distribution, and pH within acceptable limits under both ambient and accelerated storage conditions (54°C). In stark contrast, the comparative composition exhibits severe physical instability (hard caking), drastic loss of suspensibility, assay reduction, pH failure, viscosity non-compliance, and particle instability.

[0385] Table 35: Accelerated Heat Stability

[0386] & &

[0387]

[0388] < >

[0389]

[0390] Table 35 further confirms the superiority of the claimed composition; even at higher active amounts, the present invention composition maintains assay integrity, high suspensibility (>99%), viscosity compliance, particle size control, and physical homogeneity under accelerated storage. Whereas the composition containing a conventional stabiliser and a pH-modifying agent shows significant degradation, hard caking, reduced suspensibility, assay reduction, and complete failure across multiple regulatory parameters.

[0391] Table 36: Technical Impact of different pH modifying System

[0392]

[0393]

[0394] Table 36 clearly shows that removing sodium hydroxide disrupts the composition, leading to pH drift and increased susceptibility to hydrolytic degradation of both active ingredients. The resulting chemical instability, flocculation tendency, reduced zeta potential, viscosity irregularities, and poor storage robustness evidence the technical effect of the present invention composition.

[0395] Table 37. Comparative Buffer System (pH) Effect

[0396]

[0397] Table 37 demonstrates that neither potassium dihydrogen phosphate alone nor sodium phosphate alone stabilises the composition. The pH-modifying system of the present invention ensures chemical stability, electrostatic particle stabilisation, and long-term storage performance.

[0398] From the foregoing it will be observed that numerous modifications and variations can be effectuated without departing from the true spirit and scope of the novel concepts of the present invention. It is to be understood that no limitations with respect to the specific embodiments illustrated is intended or should be inferred. It should be understood that all such modifications and improvements have been deleted herein for the sake of conciseness and readability but are properly within the scope of the following claims.

Claims

CLAIMS1. An insecticidal composition, comprising:a. N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount ranging from 1-60% w / w;b. Indoxacarb in an amount ranging from 1-15% w / w; andc. a stabilizer in an amount ranging from 0.01-15% w / w.

2. The insecticidal composition as claimed in claim 1, wherein the stabilizer is poly (ethylene glycol-ran-propylene glycol) monobutyl ether.

3. The insecticidal composition as claimed in claim 1 , comprising a pH modifying system, wherein said pH modifying system is present in an amount ranging from 0.01-8% w / w.

4. The insecticidal composition as claimed in claim 1, wherein the pH modifying system comprises a mixture of Sodium hydroxide and Potassium Dihydrogen Phosphate.

5. The insecticidal composition as claimed in claim 1, further comprises at least one agriculturally acceptable excipient,wherein the agriculturally acceptable excipient are selected from dispersing agent, anti -freezing agent, anti -foaming agent, a thickener, rheological modifier, a biocide, a wetting agent, a binder, an emulsifier, a carrier, a solvent, a co-solvent, or a mixture thereof.

6. The insecticidal composition as claimed in claim 1, whereinthe dispersing agent is present in an amount ranging from 0.1-20% w / w,the anti -freezing agent is present in an amount ranging from 0.1-15% w / w, the wetting agent is present in an amount ranging from 0.1-15% w / wthe anti -foaming agent is present in an amount ranging from 0.1-2% w / w,the thickener is present in an amount ranging from 0.1-20% w / w,the biocide is present in an amount ranging from 0.1-5% w / w,the wetting agent is present in an amount from 0.1-10% w / w,the binder is present in an amount ranging from 0.1-20% w / w,the emulsifier is present in an amount ranging from 0.1-25% w / w.

7. The insecticidal composition as claimed in claim 1, wherein the insecticide is formulated into 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).

8. A process for preparing an insecticidal composition comprising N-(Cyanomethyl)-4- (trifluoromethyl) pyridine-3 -carboxamide and indoxacarb, the process comprising: a. providing N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and indoxacarb;b. providing an additive system comprising (i) a stabilizer and (ii) a pH-modifying system;c. mixing the N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide and the indoxacarb with the additive system and at least one agriculturally acceptable excipient to form a process mixture; andd. subjecting the process mixture to homogenisation to obtain a formulated composition.

9. The process as claimed in claim 8, wherein the stabilizer comprises poly (ethylene glycol-ran-propylene glycol) monobutyl ether and the pH-modifying system comprises a mixture of sodium hydroxide and potassium dihydrogen phosphate.

10. The process as claimed in any one of claims 8-9, wherein the formulated composition comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in an amount of 1-60 wt.%, indoxacarb in an amount of 1-15 wt.%, the stabilizer in an amount of 0.01-15 wt.%, and the pH-modifying system in an amount of 0.01-8 wt.%.

11. The process as claimed in any one of claims 8-10, wherein the formulated composition is a suspension concentrate (SC), and wherein step (d) comprises:forming the process mixture as an aqueous suspension comprising water;wet-milling the aqueous suspension to obtain a particle size of below 10 pm; and incorporating a rheology modifier and a biocide to obtain the SC,wherein, the SC comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3- carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.01-8 wt.%, stabilizer 0.01-15 wt.%, dispersing agent 1-5 wt.%, rheology modifier 0.1-2 wt.%, and preservative 0.1-2 wt.%.

12. The process as claimed in any one of claims 8-10, wherein the formulated composition is water dispersible granules (WDG), and wherein step (d) comprises:dry-blending the process mixture with a carrier, a wetting agent and a dispersing agent to obtain a dry blend;dry-milling the dry blend; andgranulating and drying the milled material to obtain the WDG,wherein the WDG comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3- carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.01-8 wt.%, stabilizer 0.01-15 wt.%, dispersing agent 1-15 wt.%, stabilizer 0.01-15 wt.%, and pH- modifying system 0.1-2 wt.%.

13. The process as claimed in any one of claims 8-10, wherein the formulated composition is an oil dispersion (OD), and wherein step (d) comprises:dispersing the process mixture in an oil phase comprising an oil and a solvent to obtain a dispersion; andwet-milling the dispersion to obtain the OD,wherein the OD comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3- carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.01-8 wt.%, stabilizer 0.01-15 wt.%, wetting agent 0.5-10 wt.%, and dispersing agent 0.5-10 wt.%.

14. The process as claimed in any one of claims 8-10, wherein the formulated composition is a dispersible concentrate (DC) or an emulsifiable concentrate (EC), and wherein step (d) comprises:dissolving N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 -carboxamide in a solvent system comprising a solvent and optionally a co-solvent to obtain a solution; adding indoxacarb to obtain a homogeneous composition; andincorporating an emulsifier system together with the stabilizer and the pH-modifying system to obtain the DC or the EC,wherein, when the formulation is an EC, the obtained composition is filtered, and wherein the DC and EC comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3- carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.01-8 wt.%, stabilizer 0.01-15 wt.%, emulsifier 5-15 wt.%, and optionally co-solvent 1-30 wt.%.

15. The process as claimed in any one of claims 8-10, wherein the formulated composition is a wettable powder (WP), and wherein step (d) comprises:dry-blending the process mixture with a dispersing agent to obtain a blend; and grinding the blend to obtain particles having a size of below 20 pm, thereby obtaining theWP,wherein the WP comprises N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3 - carboxamide 1-60 wt.%, indoxacarb 1-15 wt.%, pH-modifying system 0.01-8 wt.%, stabilizer 0.01-15 wt.%, and dispersing agent 1-20 wt.%.