Description:FIELD OF THE INVENTION:

The present invention relates to synergistic insecticidal composition comprising a) component (A) Fluxametamide or its agrochemically acceptable salts, esters and derivative; b) component (B) Diafenthiuron or its agrochemically acceptable salts, esters and derivatives; c) component (C) at least one insecticide selected from neonicotinoid group; and d) one or more inactive excipients. The present invention further relates to process of preparing said composition and its use as insecticide.

BACKGROUND OF THE INVENTION:

Fluxametamide [4-[5-(3,5-dichlorophenyl)-4,5-dihydro-5-(trifluoromethyl)-3-isoxazolyl]-N-[(methoxyamino)methylene]-2-methylbenzamide] is an insecticide chemical to control Lepidoptera species, leaf miners, thrips, whitefly, and mites in tea crops. Fluxametamide is a novel isoxazoline insecticide with a wide spectrum of control. Fluxametamide potently inhibits the specific binding of [3H]ethynylbicycloorthobenzoate (EBOB) to housefly-head membranes, suggesting that fluxametamide affects insect γ-aminobutyric acid (GABA)-gated chloride channels. Fluxametamide inhibited agonist responses in both the GABA-gated chloride and glutamate-gated chloride channels (GluCls) expressed in Xenopus oocytes in the nanomolar range, indicating that this insecticide is a ligand-gated chloride channel (LGCC) antagonist.

Diafenthiuron (1-tert-butyl-3-(2,6-di-isopropyl-4- phenoxyphenyl)- thiourea is a broad spectrum and acaricide used to protect many agricultural and horticultural crops. It has unique mode of action that paralyzes pests by inhibiting their respiratory system. It is sold under the brand names Derby, Diron, Pegasus, Polar and Polo.

Neonicotinoids are class of neuro-active insecticides chemically similar to nicotine. Neonicotinoids are among the widest-used insecticides in crop protection. They are also widely employed for veterinary purposes including tick and flea control. The first generation of neonicotinoids includes dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram and imidacloprid.

Dinotefuran ((RS)-1-methyl-2-nitro-3-(tetrahydro-3-furylmethyl) guanidine) is a non-repellent insecticide of the neonicotinoid class used to control pests. Its mode of action involves the disruption of the insect's nervous system by inhibiting nicotinic acetylcholine receptors and has been found useful in controlling pyrethroid resistant pests. Dinotefuran acts through contact and ingestion and results in death shortly after contact. Dinotefuran is a fast-acting agent. However, it is more subject to photo degradation.

Acetamiprid, (E)-N’-[(6-chloro-3-pyridyl)methyl]-N2-cyno-N’-methyl acetamidine, is a neonicotinoid insecticide with contact and stomach action against a range of plant pests such as Hemiptera, Thysanoptera and Lepidoptera acting as an agonist of the nicotinic acetylcholine receptor in the insect central nervous system.

Insecticide compositions typically consist of an active ingredient that targets specific pests, along with several inert ingredients that aid in the formulation's effectiveness, stability, and ease of application. The active ingredient is often a chemical compound such that disrupts the biological processes of insects, either by affecting their nervous system or interfering with their metabolic functions. Inert ingredients, which can include solvents, emulsifiers, stabilizers, and carriers, help to dissolve, dilute, or spread the active ingredient more efficiently, ensuring uniform coverage and enhancing its persistence on surfaces. Some formulations may also contain surfactants to improve the spreadability of the insecticide, or fragrances to mask odors. The precise combination of these components is designed to optimize both the potency and safety of the insecticide, ensuring effective pest control while minimizing risks to humans, animals, and the environment.

In general use, the insecticides actives are used in the form of a dilute aqueous composition because it can attain a good interaction with the target organism. However, most active insecticide compounds that are used as insecticides are only sparingly or even insoluble in water. The low solubility of such compounds presents the challenges and difficulties to formulator in formulating pesticide compounds in stable formulations that can be easily stored for a long time, and which still have a high stability and effective activity until end use. This problem especially occurs and may get worsen if more than one active compound is present in the composition.

However, there remains a need for a synergistic insecticidal composition that addresses the limitations of current formulations. Such a composition should effectively overcome existing issues while being amenable to straightforward and cost-effective manufacturing processes. This formulation should provide enhanced insecticidal activity through synergistic interactions among its components yet be simple to produce without requiring complex or resource-intensive production methods.

Therefore, there still exists a need to develop synergistic insecticidal composition, which is stable, synergistic, more effective in control of wide spectrum of insect-pests in crop and environmentally safe.

Another objective of the present invention is to provide a synergistic insecticidal composition one-shot formulation effective for controlling undesired sucking insects, mites and lepidopteran pests on crop.

Yet another objective of the present invention is to provide a synergistic insecticidal composition which is safe to the crops.

Yet another objective of the present invention is to provide a process for the preparation of a synergistic ternary composition comprising the active ingredients of the present invention and excipients suitable for such an insecticidal composition.

Therefore an aspect of the present invention is to provide novel synergistic insecticidal composition comprising a) component (A) fluxametamide or its agrochemically acceptable salts, esters and derivative; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivatives; c) component (C) at least one insecticide selected from neonicotinoid group can provide solution to the above mentioned problems.

Further Inventors of the present invention have surprisingly found that the novel synergistic insecticidal composition comprising a) component (A) fluxametamide or its agrochemically acceptable salts, esters and derivative; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivatives; c) component (C) at least one insecticide selected from neonicotinoid group with suitable formulation provides synergistic effect.

The present invention further relates to process of preparing said composition along with at least one inactive formulation excipients and formulation thereof which overcomes some of the existing problems and can be prepared easily without much complex manufacturing process.

SUMMARY OF THE INVENTION

The main aspect of the present invention provides a synergistic insecticidal composition comprising:
a. Component (A) Fluxametamide, chemically known as 4-[(RS)-5-(3,5-dichlorophenyl)-4,5-dihydro-5-(trifluoromethyl)isoxazol-3-yl]-N-[(EZ)-(methoxyimino)methyl]-o-toluamide;

or its agrochemically acceptable salts, esters and derivative;
b. Component (B) Diafenthiuron chemically known as 1-tert-butyl-3-(2,6-di-isopropyl-4- phenoxyphenyl)- thiourea:

or its agrochemically acceptable salts, esters and derivative;
c. Component (C) at least one insecticide selected from neonicotinoid group; and
d. One or more inactive excipients.

Another aspect of the present invention to provide synergistic insecticidal composition comprises: a) Component (A) fluxametamide or its agrochemically acceptable salts, esters and derivative is in amount of 1.0% to 10.0% w/w; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivative is in amount of 15.0% to 50.0% w/w; and c) component (C) at least one insecticide selected from neonicotinoid group is in amount of 1.0% to 15.0% w/w.

Another aspect of the present invention to provide neonicotinoid group of insecticide is selected from dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid.

Another aspect of the present invention to provide one or more inactive excipients is selected from the group comprising of wetting agent, dispersing agent, disintegrating agent, emulsifier, defoamer, anti-freezing agent, preservative, filler, carrier, thickener/suspending agent, pH stabilizer, anticaking agent, filler, solvent or a combination thereof and other additives, if required in a formulation.

As per one embodiment, formulation for the synergistic insecticidal composition of the present invention is formulated as Water dispersible granules/Wettable granules (WDG/WG), Water soluble granules (SG), Emulsifiable granule (EG), Wettable powder (WP), Water dispersible powder (WDP), Soluble powder (SP), Emulsifiable powder (EP), Oil dispersible powder (OP), Soluble Tablet (ST), Capsule suspension/Micro capsule (CS), Dispersible concentrate (DC), Emulsifiable concentrate (EC), Emulsion water-in-oil (EO), Emulsion oil-in-water (EW), Micro-emulsion (ME), Oil-dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Suspension Concentrate (SC), Suspo-Emulsion (SE), Soluble Liquid/Concentrate (SL), mixed formulation of CS and SC (ZC), mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).

Further aspect of the present invention is to provide synergistic, broad-spectrum control of harmful insects and mites.

DETAILED DESCRIPTION OF THE INVENTION:

In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, similar symbols typically identify similar components, unless context dictates otherwise. The illustrative embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments may be utilized, and other changes may be made, without departing from the spirit or scope of the subject matter presented here. The present technology is also illustrated by the examples herein, which should not be construed as limiting in any way.

As used herein, the terms below have the meanings indicated.

The singular forms "a," "an," and "the" may refer to plural articles unless specifically stated otherwise.

The term "about," as used herein, is intended to qualify the numerical values which it modifies, denoting such a value as variable within a margin of error. When no particular margin of error, such as a standard deviation to a mean value given in a chart or table of data, is recited, the term "about" should be understood to mean that range which would encompass the recited value and the range which would be included by rounding up or down to that figure as well, taking into account significant figures.

The embodiments, illustratively described herein may suitably be practiced in the absence of any element or elements, limitation or limitations, not specifically disclosed herein. Thus, for example, the terms “comprising,” “including,” “containing,” etc. shall be read expansively and without limitation. Additionally, the terms and expressions employed herein have been used as terms of description and not of limitation, and there is no intention in the use of such terms and expressions of excluding any equivalents of the features shown and described or portions thereof, but it is recognized that various modifications are possible within the scope of the claimed technology. Additionally, the phrase “consisting essentially of” will be understood to include those elements specifically recited and those additional elements that do not materially affect the basic and novel characteristics of the claimed technology. The phrase “consisting of” excludes any element not specified.

The present invention relates a synergistic insecticidal composition comprising:
a. Component (A) fluxametamide;

or its agrochemically acceptable salts, esters and derivative;
b. Component (B) diafenthiuron

or its agrochemically acceptable salts, esters and derivative;
c. Component (C) is at least one insecticide selected from neonicotinoid group consisting of dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid.
d. One or more inactive excipients;

The present invention provides a synergistic insecticidal composition comprising a) Component (A) fluxametamide or its agrochemically acceptable salts, esters and derivative is in amount of 1.0% to 10.0% w/w; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivative is in amount of 15.0% to 50.0% w/w; and c) component (C) at least one insecticide selected from neonicotinoid group is in amount of 1.0% to 15.0% w/w.

The present invention to provide neonicotinoid group of insecticide is selected from dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid.

The composition of the present invention comprises agriculturally acceptable excipients is selected from the group comprising of wetting agent, dispersing agent, disintegrating agent, emulsifier, defoamer, anti-freezing agent, preservative, thickener/suspending agent, pH stabilizer, anticaking agent, rheology modifier, buffering agent, filler, carrier, solvent or a combination thereof and other additives, if required in a formulation.

The synergistic insecticidal composition of the present invention is formulated as Water dispersible granules/Wettable granules (WDG/WG), Water soluble granules (SG), Emulsifiable granule (EG), Wettable powder (WP), Water dispersible powder (WDP), Soluble powder (SP), Emulsifiable powder (EP), Oil dispersible powder (OP), Soluble Tablet (ST), Capsule suspension/Micro capsule (CS), Dispersible concentrate (DC), Emulsifiable concentrate (EC), Emulsion water-in-oil (EO), Emulsion oil-in-water (EW), Micro-emulsion (ME), Oil-dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Suspension Concentrate (SC), Suspo-Emulsion (SE), Soluble Liquid/Concentrate (SL), mixed formulation of CS and SC (ZC), mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).

The composition of the present invention is effective to control various insects-pests belongs to the order Hemiptera, for example, aphid, jassid, leaf hopper, mango hopper, whitefly, mealybug, scale, rice brown plant hopper (BPH), order Lepidoptera, fall army worm, rice stem borer, rice leaf folder, sugarcane early shoot borer, top borer, wheat pink stem borer, fruit borer, pod borer, maruca, cut worm, diamond back moth, looper, semi looper, pink bollworm, brinjal fruit and shoot borer, Spodoptera, Helicoverpa; from the order Coleoptera, white grub, wire worm, epilachna beetle, blue beetle, girdle beetle, rice water weevil; from the order Orthoptera, for example, locust; from the order Thysanoptera, for example, cotton thrips, chilli thrips, black thrips; from the order Isoptera, example-termite; from the order Diptera, for example, shoot fly, stem fly, fruit fly, leaf miner; from the order Acarina, for example, red mite, red spider mite, pink mite, broad mite, purple mite.

The pests may be controlled by contacting the target pest, its food supply, habitat, breeding ground or its locus with a pesticidally effective amount of inventive compositions.

Crops are also to be understood to include those which are obtained by conventional methods of breeding or genetic engineering and contain so-called output traits (e.g. improved storage stability, higher nutritional value and improved flavour).

The composition of the present invention is effective to control various insects, pests and mites infesting the crops like rice, wheat, maize, sugarcane, cotton, okra, brinjal, chilly, tomato, cabbage, cauliflower, tomato, potato, garlic, onion, groundnut, soybean, green gram, black gram, red gram, chickpea, cucumber, melons, apple, mango, papaya, pomegranate, banana, grapes, tea, coffee, cumin, fennel, black pepper, flower crops like rose, marigold etc.

The synergistic insecticidal composition of specific active ingredient has the special advantage of being highly active against insect pests and mites. The present inventors believe that the combination of the present invention surprisingly results in a synergistic action. The combinations of the present invention allow for a broad spectrum of pest control. The broad spectrum of the present combination also provides a solution for preventing the development of resistance.

Active Ingredients Component A Component B Component C
Examples Fluxametamide Diafenthiuron At least one insecticide from neonicotinoid group
% of active ingredients (w/w) 1.0% to 10.0% w/w 15.0% to 50.0% w/w 1.0% to 15.0% w/w

Further, synergistic insecticidal compositions comprising a) component (A) fluxametamide or its agrochemically acceptable salts, esters and derivatives; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivatives; and c) at least one insecticide selected from neonicotinoid group of insecticide, wherein neonicotinoid group of insecticide is dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid; and d) one or more inactive excipients.

In further aspect the present invention relates to ternary insecticidal composition comprising a) component (A) fluxametamide or its agrochemically acceptable salts, esters and derivatives is in range of 1.0% to 10.0% w/w; more preferably in range of 3.0 to 9.0%w/w of the composition; b) component (B) diafenthiuron or its agrochemically acceptable salts, esters and derivatives is in range of 15.0% to 50.0% w/w; more preferably in range of 18.0 to 46.0%w/w of the composition; and c) component (C) at least one insecticide selected from neonicotinoid group of insecticide is in range of 1.0 to 15.0% w/w; more preferably in range 4.0 to 12.0%w/w of the composition, wherein neonicotinoid group of insecticide is dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid

The composition of the present invention comprises agriculturally acceptable excipients is selected from the group comprising of wetting agent, dispersing agent, disintegrating agent, emulsifier, defoamer, anti-freezing agent, preservative, thickener/suspending agent, pH stabilizer, anticaking agent, filler, carrier, solvent or a combination thereof and other additives, if required in a formulation.

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. Non-limiting examples of wetting agents that can be used in the present invention include, but not limited to, tristyryl phenol ethoxylate non-ionic polymer, sodium iso propyl naphthalene sulphonate, alkyl phenyl ethoxylate, aryl phenyl ethoxylate, aryl phenyl ether phosphate, alkoxylated alcohol, ethoxylated fatty alcohol, ethylene oxide-propylene oxide (EO-PO) block copolymer, alkyl aryl sulphonate, alkyl olefin sulfonate, dioctyl succinate, sodium lauryl sulfate, alkyl polyglucoside, sodium alkyl aryl taurate, sorbitol esters, sorbitol oleate, poly aryl phenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate. Ethoxylated alcohol includes natural fatty alcohol (lauryl alcohol ethoxylate, lauryl alcohol alkoxylate), synthetic alcohol ethoxylate (tridecyl alcohol ethoxylate, 2-ethyl hexanol, 2-propylheptanol, isodecyl alcohol, trisiloxane ethoxylate, heptamethyl trisiloxane, modified form includes polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified Tri siloxane, polyalkyleneoxide modified polydimethylsiloxane, may be liquid or powder form.

One or more wetting agents may be used in the present composition. The wetting agent is present in an amount in the range from 1.0% to 10.0% w/w.

Dispersing agents /surfactants are added to prevent agglomeration of solid particles in a liquid and keep them suspended in fluid. Accordingly, the composition of the present invention contains the dispersing agent selected from the group comprising acrylic graft copolymer, examples are methyl methacrylate ethoxylated graft co-polymer, 2-Acrylamido-2-Methylpropane Sulfonic Acid, Sodium methallyl sulfonate, 3-sulfopropyl acrylate potassium salt, 3-sulfopropyl methacrylate potassium salt, 2-hydroxypropyl methacrylate, 2-hydroxypropyl acrylate, 2-hydroxymethyl methacrylate, Polyethylene-g-poly(n-butyl acrylate), poly acrylate copolymer.; polyarylphenyl ether phosphate, Tri styryl phenol ethoxylate, ethoxylated tristryl phenol sulphate, acrylic polymer amine salt, naphthalene sulfonic acid-sodium salt condensate with formaldehyde, alkylated naphthalene sulfonate-sodium salt, ethoxylated oleylcetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol, alkyl sulfonate, styrene acrylic copolymer, alkyl phenol polyglycol ether, sodium lignosulfonate, calcium lignosulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide- polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide.

One or more dispersing agents are used in the synergistic insecticidal composition of the present invention. The dispersing agent is present in an amount in the range from 1.0% to 25.0% w/w.

Defoamer is generally added to the composition to prevent foam formation as the foam prevents the efficient filling of a container. Suitable defoamer used herein, but not limited to, Siloxane polyalkyleneoxide, polydimethylsiloxane, polysiloxane emulsion, vegetable oil-based antifoam, magnesium stearate or a combination thereof and present in an amount in range from 0.1% to 5.0% w/w.

An anti-freezing agent is generally added to the composition, to prevent the aqueous compositions from freezing. Suitable anti-freezing agents useful herein, but not limited to ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride etc. The anti-freezing agent is present in an amount in the range from 0.1 to 10% w/w.

A biocide is added to the composition for its preservation against spoilage from bacteria, yeasts and fungi. Suitable biocides useful herein, but not limited to, include benzisothiazolin-3-one, formaldehyde, sodium benzoate, sodium o-phenyl phenate, potassium sorbate, copper pyrithione, zinc pyrithione, 2-bromo-2-nitropropane-1,3-diol, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or a combination thereof, and is present in an amount in the range from 0.01 to 1% w/w.

It is necessary to add a thickener to the composition to reduce the tendency of the composition to disperse when sprayed and decrease the likelihood of it being rinsed off from the crops. The synergistic insecticidal composition comprises a thickener selected from the group comprising polysaccharides such as xanthan gum, sodium carboxymethyl cellulose, hydroxymethyl cellulose, sodium polyacrylate, bentonite clay, attapulgite clay, aluminium magnesium silicate, hydroxy propyl cellulose, polyvinyl alcohols, modifier starch, acacia gum, gelatin or a combination thereof and is present in an amount in the range from 0.01 to 5% w/w.

The solvent and cosolvent used in the present invention is selected from the group comprising of demineralized (DM) water, alcohols such as ethanol, propanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, acetophenone, glycerin, polyol ethers such as ethylene glycol monopropyl ether, diethylene glycol, monomethyl ether, Di propylene 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; heavy aromatic hydrocarbons such as Mixture of heavy aromatic naphtha hydrocarbon C-9 to C-16, xylene, toluene, naphthalene, solvent naphtha, solvent C9, solvent C10, solvent C12, solvesso 100, solvesso 150, solvesso 200; carboxamide; aliphatic or aromatic hydrocarbons such as chlorobenzene, chloroethylene, methylene chloride; esters such as ethyl acetate, Di isopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; alkyl amide, amides such as dimethylformamide, alkyl pyrrolidone, N-methyl-2-pyrrolidone, N-octyl pyrrolidone, N,N-dimethyldecanamide, N, N-dimethyloctanamide, N, N-dimethylamine, N,N-dimethylmethanamide; nitriles such as acetonitrile; organosulfur compound such as alkyl sulfoxide, dimethyl sulfoxide, mineral oil, methylated seed oil-methyl ester of palm oil/soybean oil/castor oil/cotton seed oil/blend of two or seed oil. The solvent may be used alone or in combination and is present in an amount quantity sufficient (QS) required to make 100% w/w formulation. Castor oil ethoxylate 40 moles is non-ionic surfactant that is derived from castor oil. It has variety of uses such as emulsifier, wetting agent, dispersing agent, additive, antistatic agent and as a solvent.

The composition of the present invention may also comprise agriculturally acceptable additives selected from the group comprising of carrier(s), binder(s), disintegrating agent(s), pH stabilizer, anticaking agent, humectant, wall forming material or a combination thereof. The composition may also contain if desired, one or more auxiliary’s customary for crop protection compositions.

Disintegrating agent is inert materials such as clays, bentonite, diatomaceous, colloidal silica, kaolin which swell by water absorption improve in dispersibility. Water soluble salts such as potassium phosphate, ammonium sulphate, sodium sulphate, sodium citrate or urea can be also used as disintegrating agent in an amount in the range from 1% to 25% w/w.

pH stabilizers may include sodium hydroxide, potassium hydrogen phosphate salt solution, acetic acid & sodium acetate, ammonia & ammonium chlorides, citric acid, benzoic acid, salicylic acids, hydrochloric acid, phosphoric acid, sodium citrate, soda ash, calcium carbonate, carboxylic acids, 2,6-di-tert-butyl-p-cresol, butylhydroxyanisole (BHT), epoxidized soybean oil (ESBO), methyl oleate, potassium carbonate, potassium hydroxide, sodium hydroxide and sodium dihydrogen phosphate dihydrate or combination thereof. Optionally stabilizer present in an amount in the range from 0.05 to 2% w/w.

Anti-caking agents are used to prevent caking, which is the formation of lumps. They also make packaging, transport, flowability, and consumption easier. The anticaking agent may be selected from silica/silicone dioxide, calcium silicate, sodium ferrocyanide. Calcium stearate. Optionally anti-caking agents are present in an amount in the range from 0.1 to 10% w/w.

The binder is water soluble, water swellable or combinations of both. The binder is a water-
soluble binder selected from a group consisting of poly ethylene wax, poly vinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol, polyethylene oxide, polyethoxylated fatty acids, polyesters, polyamides, poly carbonates, poly urea, poly urethanes, styrene copolymer, butadiene copolymers, polyethoxylated alcohols, acrylate polymer such as polymethacrylate, poly ethyl methacrylate, poly methyl methacrylate, acrylate copolymers and styrene-acrylic copolymers or mixtures of thereof, a natural gum, lignosulphonate, and a combination thereof. The binder is a water swellable binder selected from a group consisting of China clay, bentonite, fuller’s earth, zeolite, quartz, precipitated silica, palygorskite, sepiolite, halloysite, and a combination thereof. Binder is present in an amount in the range from 0.1 to 10% w/w. Precipitated silica acts as carrier material, absorbing and holding the active ingredient while maintaining a free-flowing, easily dispersible powder form, enhancing wettability by improving water contact, and often providing anti-caking properties to prevent clumping, making it crucial for consistent application of the pesticide when mixed with water for spraying on crops.

A filler/carrier selected from the group comprising sand, silica, precipitated silica, bentonite, attapulgite, ceramic, montmorillonite, pumice, sepiolite, diatomaceous earth, clay, dolomite, calcite, silicon dioxide, china clay/kaolin clay, talc, starch, zinc and its salts (zinc sulphate, zinc oxide, zinc lactate gluconate, zinc polyflavonoid), iron and its salt (ferrous sulphate), copper and salts, sulphur, humic acid and salt, fulvic acid and salt, amino acids, sea weed extracts, chitosan or a combination thereof. It presents in an amount quantity sufficient (QS) required to make 100% w/w formulation.

Wall forming material for encapsulation or Capsule suspension (CS) or microcapsule technology that uses membrane forming wall material to embed the core materials that needs to be protected to form tiny particles, which can protect the core material from adverse environment and effectively plays its biological active functions. The wall forming material/ capsule making monomers may be selected from Tetramethylene diisocyanate, Penta methylene diisocyanate, hexamethylene diisocyanate, toluene diisocyanate, 4,4-diphenylmethene diisocyanate (MDI), polymethylene polyphenylene isocyanate, 2,4,4’-diphenyl ether tri-isocyanate, 3,3’-dimethyl-4,4’-diphenyl diisocyanate, 3,3’-dimethoxy-4,4’-diphenyl diisocyanate, 1,5-naphthylene diisocyanate and 4,4’4"-triphenylmethane tri-isocyanate, toluene diisocyanate or polymethylene polyphenylisocyanate, polyurethane comprising of polyfunctional iso cyanate and a polyamine in polarized form;, Diethylene triamine, Ammonia, hexamine, ethylenediamine, propylene-1,3-diamine, tetramethylenediamine, pentamethylenediamine, 1,6-hexamethylenediamine, diethylenetriamine, triethylenetetramine, tetra ethylene pentaamine, pentaethylenehexamine, 4,9-dioxadodecane-1, 12-diamine, 1,3- phenylenediamine, 2,4- and 2,6-toluenediamine and 4,4’-diaminodiphenylmethane, 1,3-phenylenediamine, 2,4- and 2,6-toluenediamine, 4,4′-diaminodiphenylmethane, 1,5-diaminonaphthalene, 1,3,5-triaminobenzene, 2,4,6-triaminotoluene, 1,3,6-triaminonaphthalene, 2,4,4′-triaminodiphenyl ether, 3,4,5-triamino-1,2,4-triazole and 1,4,5,8-tetraminoanthraquinone. It presents in an amount in the range from 0.1 to 5% w/w.

The composition may also contain if desired, one or more auxiliary’s customary for crop protection compositions.

The synergistic composition comprising of a) component (A) fluxametamide present in an amount of 1.0% to 10.0% w/w of the composition; b) component (B) diafenthiuron present in an amount of 15.0% to 50.0% w/w and c) component (C) at least one insecticide selected from neonicotinoid group present in an amount of 1.0% to 15.0% w/w; and d) one or more inactive excipients.

The synergistic present composition provides the following advantages:
• Increased efficacy than their individual counterparts or their mixtures, thus allows a substantial reduction in the application rates of each of these active ingredients, while
maintaining good efficacy and thereby reducing costs and residue problems.
• The present compositions provide an improved and extended wide spectrum control of insect-pest & mite, reduced insecticide application rates and costs, less stringent use restrictions, and improved selectivity.
• Delays the emergence of resistant species/strains.
• Minimizes risk of development of resistance and achieves effective and
economical control of undesired insects.
• 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.
• Better storage stability.
• Non-phytotoxic and environment friendly.

The process for preparing the present novel synergistic composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the formulation. However, all such variation and modification are still covered by the scope of present invention.

While the foregoing written description of the invention enables one of ordinary skill to make and use what is considered presently to be the best mode thereof, those of ordinary skill will understand and appreciate the existence of variations, combinations, and equivalents of the specific embodiment, method, and examples herein. The invention should therefore not be limited by the above described embodiment, method, and examples, but by all embodiments and methods within the scope and spirit of the invention. The invention shall now be described with reference to the following specific examples. It should be noted that the example(s) appended below illustrate rather than limit the invention, and that those skilled in the art will be able to design many alternative embodiments without departing from the scope of the present invention.

These and other aspects of the invention may become more apparent from the examples set forth herein below. These examples are provided merely as illustrations of the invention and are not intended to be construed as a limitation thereof.

EXAMPLES:

WG formulation
Compositions Percent (w/w)
Fluxametamide technical 1 to 10
Diafenthiuron technical 15 to 50
At least one neonicotinoid insecticide 1 to 15
Wetting agent 1 to 8
Dispersing agent 1 to 20
Disintegrating agent 2 to 15
Antifoaming agent 0.1 to 2
Binder 0.1 to 5
Carrier & filler qs

SC formulation
Compositions Percent (w/w)
Fluxametamide technical 1 to 10
Diafenthiuron technical 15 to 50
At least one neonicotinoid insecticide 1 to 15
Dispersing agent 2 to 15
Wetting agent 1 to 10
Anti-foaming agent 0.1 to 5
Anti-freezing agent 0.1 to 5
Rheology modifier 0.05 to 2
Thickener 0.1 to 5
Preservative 0.1 to 1
DM water q.s.

WP formulation
Compositions Percent (w/w)
Fluxametamide technical 1 to 10
Diafenthiuron technical 15 to 50
At least one neonicotinoid insecticide 1 to 15
Wetting agent 1 to 10
Dispersing agent 1 to 20
Anticaking agent 1 to 10
Carrier qs

EXAMPLE 1: Method of Preparation of WDG formulation of Fluxametamide 6% + Diafenthiuron 40% + Dinotefuran 7%

Table 1: Fluxametamide 6%+Diafenthiuron 40%+Dinotefuran 7% WG
S.No. Compositions Function Percent (w/w)
1 Fluxametamide technical (93.5% purity) Active ingredient 6.42
2 Diafenthiuron technical (96% purity) Active ingredient 41.67
3 Dinotefuran technical (97% purity) Active ingredient 7.22
4 Sodium salt of naphthalene sulfonate condensate Dispersing agent 5.00
5 Potassium laurate Dispersing agent 1.00
6 Sodium lauryl sulphate Wetting agent/stabilizer 2.00
7 Ammonium sulphate Disintegrating agent 5.00
8 Polydimethylsiloxane Antifoaming Agent 0.50
9 Corn starch Filler 10.00
10 Lactose Binder 0.50
11 China clay Carrier 20.70
Total 100.00

Process for manufacturing of 100 kg batch of Fluxametamide 6%+Diafenthiuron 40%+Dinotefuran 7% WG
Step 1-Charge 20.70 kg of China clay, 0.5 kg of lactose, 10 kg of corn starch, 0.5 kg of polydimethyl siloxane, 5 kg of ammonium sulphate, 2 kg of sodium lauryl sulphate, 1 kg of potassium laurate, 5 kg of sodium salt of naphthalene sulfonate condensate in premixing blender for homogenization for 30 minutes.
Step 2-Now add 7.22 kg of dinotefuran technical, 41.67 kg of diafenthiuron technical and 6.42 kg of fluxametamide technical and again homogenize for 30 more minutes.
Step 3-Pre-blended material is then grinded through Jet mill until a mean particle size of below 10 microns obtained. Finely grinded material is blended in post blender till it becomes homogeneous.
Step 4-Finely grinded powder is mixed with required quantity of water to form extrudable dough.
Step 5-Dough is passed through extruder to get granules having a particle size in the range of 0.5 mm to 2 mm.
Step 6-Wet granules are passed through fluid bed dryer and further graded using vibrating screens.
Step 7-Final product is sent for QC approval.
Step 8-After approval material is packed in required pack sizes.

Table 2: Storage stability: Fluxametamide 6%+Diafenthiuron 40%+Dinotefuran 7% WG
Parameters T0 (initial) T1 (AHS),for 14 days at 0C T2- for three months at 40 0C
Fluxametamide content (%) (-5% to +10% range) 7.04 7.02 7.02
Diafenthiuron content (%) (-5% to +5% range) 43.70 43.70 43.69
Dinotefuran content (%) (-5% to +10% range) 7.89 7.88 7.87
wettability (60 second, maximum) 12 12 12
suspensibility (minimum 70%) 95.80 95.40 95.40
pH range (5.5 to 7.5, 1% aq. Suspension) 6.9 6.9 6.9

The composition was evaluated for its stability. The composition was determined at T0, and under accelerated heat stability (AHS) conditions for 14 days at 54°C designated as T1. The stability was also evaluated after 3 months, at 40°C, designated as T2.

WG formulation of Fluxametamide 6%+Diafenthiuron 40%+Dinotefuran 7% The material is dry and free flowing granules and meets all the storage stability criteria-active ingredient content, wettability, suspensibility, pH 1% solution.
EXAMPLE 2: Method of Preparation of WDG formulation of Fluxametamide 6% + Diafenthiuron 40% + Acetamiprid 6%

Table 3: Fluxametamide 6%+Diafenthiuron 40%+Acetamiprid 6% WG
S. no. Compositions Function Percent (w/w)
1 Fluxametamide technical (93.5% purity) Active ingredient 6.42
2 Diafenthiuron technical (96% purity) Active ingredient 41.67
3 Acetamiprid technical (99% purity) Active ingredient 6.06
4 Dialkyl naphthalene sulphate sodium salt Wetting agent 2.50
5 Modified Sodium lignosulphonate Dispersing agent 7.00
6 Ammonium Sulphate Disintegrating agent 8.00
7 Polydimethylsiloxane Defoamer 1.00
8 Corn Starch Filler 15.00
9 Lactose Binder 1.00
10 China clay Carrier 11.36
Total 100.00

Storage stability:
WG formulation of Fluxametamide 6%+Diafenthiuron 40%+Acetamiprid 6% WG meets all the storage stability criteria-active ingredient content, wettability, suspensibility and pH 1% solution.

EXAMPLE 3: Method of Preparation of SC formulation Fluxametamide 3% + Diafenthiuron 20% + Dinotefuran 4%

Table 4: Fluxametamide 3%+Diafenthiuron 20%+Dinotefuran 4% SC
S.No. Compositions Function Percent (w/w)
1 Fluxametamide technical (93.5% purity) Active ingredient 3.21
2 Diafenthiuron technical (96% purity) Active ingredient 20.83
3 Dinotefuran technical (97% purity) Active ingredient 4.12
4 Acrylic Graft Copolymer (polymethyl methacrylate-polyethylene glycol graft copolymer) Dispersing agent 5.00
5 Alkyl naphthalene sulfonate formaldehyde condensate Dispersing agent 1.00
6 Tri siloxane ethoxylate Wetting agent 2.50
7 Aluminum magnesium silicate Suspending agent 0.50
8 Polydimethylsiloxane Anti-foaming agent 0.40
9 Propylene Glycol Anti-freezing agent 5.00
10 1,2-benzisothiazolin-3(2H)-one Preservative 0.20
11 Precipitate Silica Rheology modifier 0.40
12 Xanthan gum/Polysaccharide Thickener 0.20
13 Demineralized water Solvent 56.63
Total 100.00

Process for manufacturing of 100 kg batch of Fluxametamide 3%+Diafenthiuron 20%+Dinotefuran 4% SC
Weighing the raw materials according to the batch size as follows
Step 1: Preparation of gum solution: Dissolve 2 kg of 1,2-benzisothiazolin-3(2H)-one into 96 kg of Demineralized (DM) water. Now add 2 kg of Polysaccharide slowly and stir till completely dissolved to form a solution. This gum solution was made 12 to 18 hours prior to use.
Step 2: Take 46.63 kg of DM water and 5 kg of propylene glycol into designated vessel and mix thoroughly. Add 1 kg of Alkyl naphthalene sulfonate formaldehyde condensate and 5 kg of (polymethyl methacrylate-polyethylene glycol graft copolymer) into the vessel having water and homogenize the contents for 45 to 60 minutes using high shear homogenizer.
Step 3: Then 3.21 kg of fluxametamide tech., 20.83 kg of diafenthiuron tech. and 4.12 kg of dinotefuran tech., 0.4 kg of precipitated silica and 2.5 kg of Tri siloxane ethoxylate were added and homogenized to get a uniform slurry for grinding.
Step 4: Then half of the quantity of polydimethyl siloxane was added to the slurry and then the slurry was subjected to three cycles of grinding in a bead mill till desired particle size achieved. Remaining half of the quantity of polydimethyl siloxane was added after the grinding process.
Step 5: Finally, 10 kg of remaining gum solution added and homogenize it to obtain the title formulation.
Step 6: Sending the sample to the quality analysis;
Step 7: Packing the formulated material in suitable packaging.
Table 5: Storage stability of Fluxametamide 3%+Diafenthiuron 20%+Dinotefuran 4% SC
Parameters T0 (initial) T1 (AHS),for 14 days at 0C T2- for three months at 40 0C
Fluxametamide content (%) (-5% to +10% range) 3.50 3.49 3.48
Diafenthiuron content (%) (-5% to +5% range) 20.78 20.77 20.76
Dinotefuran content (%) (-5% to +10% range) 4.08 4.06 4.06
Suspensibility (minimum 80%) 98.60 98.40 98.20
pH range (7 to 10, 1% aq. Suspension) 7.00 7.00 7.00
Pourability (95% minimum) 98.30 98.10 98.00
Viscosity at spindle no. 62, 20 rpm (350 to 800 cps) 650 660 650
Particle size (D50<3, D90<10 micron) 2.2, 8.2 2.2, 8.3 2.2, 8.3

The composition was evaluated for its stability. The composition was determined at T0, and under accelerated heat stability (AHS) conditions for 14 days at 54°C designated as T1. The stability was also evaluated after 3 months, at 40°C, designated as T2.

The composition meets all the required storage stability criteria- technical content (%), suspensibility, pH, pourability, viscosity and particle size.

EXAMPLE 4: Method of Preparation of SC formulation of Fluxametamide 3% + Diafenthiuron 20% + Clothianidin 6%

Table 6: Fluxametamide 3%+Diafenthiuron 20%+Clothianidin 6% SC
S.No. Ingredients Description Content
(% w/w)
1 Fluxametamide technical (93.5% purity) Active Ingredient 3.21
2 Diafenthiuron technical (96% purity) Active Ingredient 20.83
3 Clothianidin technical (98% purity) Active Ingredient 6.12
4 Tri siloxane ethoxylate Wetting agent 5.00
5 Ethoxylated tristrylphenol Dispersing agent 4.00
6 Sodium naphthalene sulphonate formaldehyde condensates Dispersing agent 1.51
7 Attapulgite clay Suspending agent 0.30
8 1,2-benzisothiazolin-3(2H)-one Preservative 0.15
9 1,2-propylene glycol Anti freezing agent 3.90
10 Precipitated Silica Rheology modifier 0.50
11 Polydimethylsiloxane Anti foaming agent 0.30
12 Xanthan gum/Polysaccharide Thickener 0.15
13 Demineralized water Solvent 54.03
Total 100.00

The composition of Fluxametamide 3%+Diafenthiuron 20%+Clothianidin 6% SC meets all the required storage stability criteria- technical content (%), suspensibility, pH, pourability, viscosity and particle size.

EXAMPLE 5: Method of Preparation of WP formulation: Fluxametamide 6.4%+Diafenthiuron 36%+Acetamiprid 6%

Table 7: Fluxametamide 6.4%+Diafenthiuron 36%+Acetamiprid 6% WP
S.No. Compositions Function Percent (w/w)
1 Fluxametamide technical (93.5% purity) Active ingredient 6.84
2 Diafenthiuron technical (96% purity) Active ingredient 37.50
3 Acetamiprid technical (99% purity) Active ingredient 6.06
4 Condensed alkyl naphthalene sulfonate sodium salt Dispersing agent 10.00
5 Ethoxylated fatty alcohol Wetting agent 2.00
6 Precipitated silica Anticaking agent 5.00
7 China clay Carrier 32.59
Total 100.00

Process for manufacturing of 100 kg batch of Fluxametamide 6.4%+Diafenthiuron 36%+Acetamiprid 6% WP
Step 1-Charge 32.59 kg of China clay, 5 kg of precipitated silica, 2 kg of ethoxylated fatty alcohol, 10 kg of condensed alkyl naphthalene sulfonate sodium salt in premixing blender for homogenization for 30 minutes.
Step 2-Now add 37.5 kg of diafenthiuron technical, 6.84 kg of fluxametamide technical and 6.06 kg of acetamiprid technical and again homogenize for 30 minutes.
Step 2-Pre-blended material is then grinded through Jet mill/ air classifier mills. Finely grinded material is blended in post blender till it becomes homogeneous. (for approx. 1.5 hr.).
Step 3-Final product is sent for QC approval.
Step 4-After approval material is packed in required pack sizes.

The composition of Fluxametamide 6.4%+Diafenthiuron 36%+Acetamiprid 6% WP meets all in-house specification for storage stability studies in laboratory (for 14 days) and room temperature (for 3 months).

EXAMPLES 6

BIOLOGICAL EXAMPLES:

Evaluation of synergistic effect of insecticidal composition of the present invention:
The synergism between two or three pesticidal compounds can be evaluated as per the method given by S R Colby. Calculating Synergistic and Antagonistic Responses of Herbicide Combinations, published online by Cambridge University Press: 12 June 2017, pp. 20-22 (Weeds, Journal of The Weed society of America, Volume 15, January 1967, Issue 1, Page 20-22).

Experiment 1: Control of sucking pests in Okra crop.
Crop: Okra
Plot size: 8 m x 7 m.
Pests: Whitefly (Bemisia tabaci), Jassid (Amrasca devastans)
Crop stage: 61 days.
Application method: Foliar spray with battery operated backpack sprayer.
Spray volume: 500 liters per hectare.
Methodology: Whitefly (nymph & adults) and Jassid (nymph & adults) are sucking insects, mostly present on lower surface of leaf and suck the cell sap. Observations recorded by counting the number of insects per leaf, three leaves each one from upper, middle and lower canopy of plant, ten plants per plot. Insect control (as an observed value) calculated by given formula.

Based on the insect control observed, expected control calculated by Colby’s formula.
Table 8: Treatment details
S.No. Treatment details Dose per hectare
Ingredients (g) formulation (g)
T1 Control (water spray only) -
T2 Fluxametamide 10% EC 25 250.0
T3 Fluxametamide 10% EC 37.5 75.0
T4 Fluxametamide 10% EC 50 250.0
T5 Diafenthiuron 50% WP 275 550.0
T6 Diafenthiuron 50% WP 250 500.0
T7 Diafenthiuron 50% WP 225 450.0
T8 Dinotefuran 20% SG 50 250.0
T9 Dinotefuran 20% SG 43.75 218.75
T10 Dinotefuran 20% SG 31.25 156.25
T11 Fluxametamide 5%+Diafenthiuron 27.5% SC 50+275 1000
T12 Fluxametamide 10%+Dinotefuran 10% WG 50+50 500
T13 Diafenthiuron 48%+Dinotefuran 8% WG 275+50 625
T14 Pyriproxyfen 8%+Diafenthiuron 18%+Dinotefuran 5% SC 80+180+50 1000
T15 Fluxametamide 4%+Diafenthiuron 44%+Dinotefuran 8% WG 25+275+50 625
T16 Fluxametamide 6%+Diafenthiuron 40%+Dinotefuran 7% WG 37.+250+43.75 625
T17 Fluxametamide 8%+Diafenthiuron 36%+Dinotefuran 5% WG 50+225+31.25 625
T15 to T17 are present compositions; T11 to T14 are prior arts; T2 to T10-market products.
Table 9: Synergistic control of whitefly and jassid in Okra crop
S.No. Whitefly control (%) Jassid control (%)
3rd day 7th day 15th day 3rd day 7th day 15th day
Observed Expected Ratio Observed Expected Ratio
T1 0.00 - - 0.00 0.00 0.00 - - 0.00 0.00
T2 19.48 - - 6.32 0.96 77.56 - - 66.36 52.24
T3 26.48 - - 11.85 1.38 84.78 - - 76.12 63.77
T4 36.82 - - 22.15 8.92 68.75 - - 55.36 40.26
T5 80.52 - - 71.28 58.86 50.86 - - 41.88 27.58
T6 75.28 - - 54.82 47.53 45.67 - - 33.93 20.10
T7 58.42 - - 57.46 33.86 38.85 - - 26.32 11.65
T8 56.38 - - 30.45 12.84 77.48 - - 70.52 58.62
T9 52.28 - - 24.37 9.38 70.73 - - 59.88 44.38
T10 42.86 - - 15.38 3.45 58.86 - - 45.62 27.26
T11 88.85 87.69 1.01 77.26 60.64 86.42 84.64 1.02 72.38 51.72
T12 74.22 72.44 1.02 44.74 18.36 94.58 92.96 1.02 88.95 73.68
T13 92.90 91.50 1.02 79.18 62.75 91.42 88.93 1.03 83.16 67.93
T14 90.85 - - 80.36 71.85 86.26 - - 75.18 56.76
T15 100.00 93.16 1.07 98.63 93.46 100.00 97.52 1.03 100.00 98.88
T16 99.23 91.33 1.09 96.29 91.96 100.00 97.58 1.02 100.00 97.38
T17 98.80 84.99 1.16 94.78 87.53 100.00 92.14 1.09 100.00 95.26

The trial results show present compositions at various doses (T15 and T17) are highly synergistic in terms of efficacy and residual control against whitefly and jassid and provide higher percentage of control as compared with prior art treatments (T11 to T14) and market products (T2 to T10). The Present composition, T15, T16 and T17 gave 100%, 99.23% and 98.80% control of whitefly respectively on 3rd day, which are highest among all the treatments. Similar trend was observed on 7th and 15th day also.

All the doses of present composition, i.e. T15, T16 and T17 provide 100% control of jassid on 3rd and 7th day after application. On 15th day, all the doses of present composition provide >95% control of jassid, which are higher than prior art treatments (T2 to T14). So, it is concluded that present compositions at different doses (T15 to T17) are highly synergistic and provide effective control of whitefly and jassid for longer duration.

Table 10: Effect on beneficial insects
S.No. Beneficial Insect population
lady bird beetle Syrphid fly larvae
3 days 7 days 15 days 3 days 7 days 15 days
T1 1.87 1.89 2.00 0.78 1.12 1.27
T2 1.83 1.83 2.10 0.84 1.16 1.44
T3 1.68 1.85 1.90 0.59 0.99 1.34
T4 1.83 1.92 1.99 0.76 1.12 1.39
T5 1.90 2.03 2.15 0.91 1.21 1.40
T6 1.76 1.99 2.01 0.70 1.04 1.42
T7 2.03 1.90 2.10 0.97 1.13 1.49
T8 1.66 1.89 1.91 0.60 0.92 1.35
T9 1.49 1.67 1.63 0.42 0.74 1.23
T10 1.90 2.13 1.98 0.88 1.15 1.32
T11 1.85 1.97 2.13 0.77 1.07 1.35
T12 1.93 1.86 2.10 0.86 1.13 1.37
T13 1.85 1.89 1.93 0.83 1.00 1.23
T14 1.82 1.88 1.84 0.78 0.92 1.24
T15 1.92 1.98 2.10 0.91 1.18 1.36
T16 1.87 1.91 2.08 0.81 1.24 1.40
T17 1.93 1.98 2.15 0.86 1.20 1.32

Beneficial insects like lady bird beetle and syrphid fly are natural friends as they feed on sucking insect-pests like aphid, jassid, thrips and whitefly. The grub and adult lady bird beetle, and larvae of syrphid fly were present in the trial plot and their populations were assessed along with sucking pests to judge the effect of present compositions on natural/beneficial insects. The results presented in table 3 show present compositions (T15 to T17) were found safe and does not have any negative impact on population of beneficial insect’s lady bird beetle and syrphid fly larvae.

Experiment 2: Residual control of whitefly in brinjal crop.
Crop: Brinjal
Plot size: 10 m x 5m.
Pests: Whitefly (Bemisia tabaci)
Crop stage: 75 days.
Application method: Foliar spray with battery operated backpack sprayer.
Spray volume: 520 liters per hectare.
Observation method: Brinjal is very succulent crop and hosts many sap sucking insects. Among the sap sucking insects, whitefly is major sucking pests infesting the brinjal crop from nursery stage to the till crop removal. Farmer has to spray every week to control whitefly. Observations were recorded as per the method given in experiment 1.
Table 11: Treatment details
S.No Treatment details Dose per hectare
active Ingredients (g) formulation (g)
T1 Control (water spray only) - -
T2 Fluxametamide 10% EC 36 360
T3 Diafenthiuron 50% WP 240 480
T4 Acetamiprid 20% SP 36 180
T5 Dinotefuran 20% SG 48 240
T6 Sulfoxaflor 24% SC 72 300
T7 Clothianidin 50% WDG 72 144
T8 Fluxametamide 6%+Diafenthiuron 40% WG 36+240 600
T9 Fluxametamide 10%+Acetamiprid 10% WG 36+36 360
T10 Fluxametamide 6%+Dinotefuran 8% WG 36+48 600
T11 Fluxametamide 6%+Sulfoxaflor 12% SC 36+72 600
T12 Fluxametamide 10%+Clothianidin 20% SC 36+72 360
T13 Diafenthiuron 40%+Acetamiprid 6% WP 240+36 600
T14 Diafenthiuron 40%+Dinotefuran 8% WG 240+48 600
T15 Diafenthiuron 20%+Sulfoxaflor 6% SC 240+72 1200
T16 Diafenthiuron 20%+Clothianidin 6% SC 240+72 1200
T17 Fluxametamide 6%+Diafenthiuron 40%+Acetamiprid 6% WG 36+240+36 600
T18 Fluxametamide 3%+Diafenthiuron 20%+Dinotefuran 4% SC 36+240+48 1200
T19 Fluxametamide 3%+Diafenthiuron 20%+Sulfoxaflor 6% SC 36+240+72 1200
T20 Fluxametamide 3%+Diafenthiuron 20%+Clothianidin 6% SC 36+240+72 1200
T17 to T20-present compositions; T8 to T16-known binary combinations.
Table 12: Residual control of whitefly in brinjal crop
S.No. Whitefly control (%)
3rd day 7th day 14th day
Observed Expected Ratio Observed Expected Ratio Observed Expected Ratio
T1 0.00 - - 0.00 - - 0.00 - -
T2 26.85 - - 12.38 - - 2.95 - -
T3 74.82 - - 52.26 - - 45.38 - -
T4 50.48 - - 27.92 - - 10.47 - -
T5 55.95 - - 31.16 - - 12.48 - -
T6 60.86 - - 40.84 - - 18.77 - -
T7 50.65 - - 28.36 - - 10.29 - -
T8 83.48 81.58 1.02 57.86 58.17 0.99 42.37 46.99 0.90
T9 65.18 63.78 1.02 35.64 36.84 0.97 10.16 13.11 0.77
T10 69.82 67.78 1.03 38.12 39.68 0.96 11.76 15.06 0.78
T11 72.85 71.37 1.02 47.28 48.16 0.98 18.28 21.17 0.86
T12 65.28 63.90 1.02 35.68 37.23 0.96 9.83 12.94 0.76
T13 89.72 87.53 1.03 63.88 65.59 0.97 47.43 51.10 0.93
T14 90.48 88.91 1.02 66.21 67.14 0.99 48.25 52.20 0.92
T15 92.18 90.14 1.02 68.26 71.76 0.95 51.36 55.63 0.92
T16 90.96 87.57 1.04 64.22 65.80 0.98 48.88 51.00 0.96
T17 100.00 90.88 1.10 90.20 69.85 1.29 86.24 52.54 1.64
T18 100.00 91.89 1.09 92.29 71.20 1.30 86.42 53.61 1.61
T19 100.00 92.79 1.08 95.35 75.25 1.27 90.82 56.94 1.59
T20 100.00 90.91 1.10 97.52 70.03 1.39 93.26 52.45 1.78

The residual control provided by present compositions (T17 to T20) and known binary combinations (T8 to T16) were studied in this experiment.

The experiment data presented in Table 12 clearly shows present compositions (T17 to T20) provides higher control of whitefly, and for longer duration (>15 days) in comparison with known binary combinations (T8 to T16). The present compositions will helps the farmer to protect their crop for longer duration and thereby reducing crop protection cost and lowering the active ingredients loading into the environment.

Trial 3: Flea beetle control in cauliflower crop.
Crop: Cauliflower
Plot size: 5 m x 5 m.
Pests: Flea beetle (Phyllotreta Cruciferae)
Crop stage: 48 days.
Application method: Foliar spray with battery operated backpack sprayer.
Spray volume: 400 liters per hectare.
Observation method: Count the number of live beetles per leaf, record the observations from 20 leaves per plot. Calculate beetle control (%) as observed value.

Table 13: Treatment doses
S.No. Treatment details Dose per hectare
active Ingredients (g) formulation (g)
T1 Control (water spray only) - -
T2 Fluxametamide 10% EC 40 400
T3 Diafenthiuron 50% WP 225 450
T4 Thiamethoxam 25% WG 62.5 250
T5 Nitenpyram 20% SC 62.5 312.5
T6 Acetamiprid 20% SP 37.5 187.5
T7 Fluxametamide 6.4%+Diafenthiuron 36% WG 40+225 625
T8 Fluxametamide 16%+Thiamethoxam 25% WG 40+62.5 250
T9 Fluxametamide 16%+Nitenpyram 25% WG 40+62.5 250
T10 Fluxametamide 16%+Acetamiprid 15% WP 40+37.5 250
T11 Diafenthiuron 36%+Thiamethoxam 10% WG 225+62.5 625
T12 Diafenthiuron 36%+Nitenpyram 10% WG 225+62.5 625
T13 Diafenthiuron 36%+Acetamiprid 6% WP 225+37.5 625
T14 Fluxametamide 6.4%+Diafenthiuron 36%+Thiamethoxam 10% WG 40+225+62.5 625
T15 Fluxametamide 6.4%+Diafenthiuron 36%+Nitenpyram 10% WP 40+225+62.5 625
T16 Fluxametamide 6.4%+Diafenthiuron 36%+Acetamiprid 6% WP 40+225+37.5 625
T14 to T16-present compositions; T7 to T13-known binary combinations; T2 to T6-market products.
Table 14: Synergistic control of flea beetle in cauliflower crop
S.No. flea beetle control in cauliflower (%)
3rd day 10th day
Observed Expected Ratio Observed Expected Ratio
T1 0.00 - - 0.00 - -
T2 65.82 - - 55.92 - -
T3 52.38 - - 40.73 - -
T4 65.23 - - 52.38 - -
T5 62.47 - - 50.96 - -
T6 60.36 - - 37.42 - -
T7 84.26 83.72 1.01 71.28 73.87 0.96
T8 89.96 88.12 1.02 77.96 79.01 0.99
T9 88.25 87.17 1.01 75.38 78.38 0.96
T10 87.22 86.45 1.01 70.46 72.41 0.97
T11 84.86 83.44 1.02 68.89 71.78 0.96
T12 83.25 82.13 1.01 68.26 70.93 0.96
T13 81.95 81.12 1.01 60.73 62.91 0.97
T14 100.00 94.34 1.06 100.00 87.56 1.14
T15 100.00 93.89 1.07 98.68 87.19 1.13
T16 101.00 97.39 1.04 99.68 91.89 1.08

Field trial results data presented in Table 14 shows all the present composition (T14 to T16) provide synergistic and residual control (>15 days) of flea beetle infesting cauliflower crop and gave higher percentage of control in comparison with known binary combinations (T7 to T13).
, C , Claims:I/We Claim,
1. A synergistic insecticidal composition comprising:
a. Component (A) Fluxametamide:

or its agrochemically acceptable salts, esters and derivative;
b. Component (B) Diafenthiuron:

or its agrochemically acceptable salts, esters and derivative;
c. Component (C) is selected from at least one insecticide from neonicotinoid group; and
d. One or more inactive excipients.

2. The synergistic insecticidal composition as claimed in claim 1, wherein a) Component (A) Fluxametamide or its agrochemically acceptable salts, esters and derivative is in amount of 1.0% to 10.0%; b) component (B) Diafenthiuron or its agrochemically acceptable salts, esters and derivative is in amount of 15.0% to 50.0% w/w; and c) insecticide component (C) at least one insecticide selected from neonicotinoid group of insecticide is in amount of 1.0% to 15.0% w/w.

3. The insecticidal composition as claimed in claim 1, wherein neonicotinoid group of insecticide is selected from dinotefuran, acetamiprid, sulfoxaflor, clothianidin, thiamethoxam, nitenpyram or imidacloprid.

4. The synergistic insecticidal composition as claimed in claim 1, wherein one or more inactive excipients is selected from the group comprising of wetting agent, dispersing agent, disintegrating agent, emulsifier, defoamer, anti-freezing agent, biocide, thickener/suspending agent, pH stabilizer, anticaking agent, filler, carrier, solvent or a combination thereof and other additives.

5. The synergistic insecticidal composition as claimed in claim 1, wherein the formulation for the said composition is selected from Water dispersible granules/Wettable granules (WDG/WG), Water soluble granules (SG), Emulsifiable granule (EG), Wettable powder (WP), Water dispersible powder (WDP), Soluble powder (SP), Emulsifiable powder (EP), Oil dispersible powder (OP), Soluble Tablet (ST), Capsule suspension/Micro capsule (CS), Dispersible concentrate (DC), Emulsifiable concentrate (EC), Emulsion water-in-oil (EO), Emulsion oil-in-water (EW), Micro-emulsion (ME), Oil-dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Suspension Concentrate (SC), Suspo-Emulsion (SE), Soluble Liquid/Concentrate (SL), mixed formulation of CS and SC (ZC), mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).

6. The synergistic insecticidal composition as claimed in claim 5, wherein the Water dispersible granules/Wettable granules (WDG/WG) formulation comprises:
i. Component (A) Fluxametamide or its agrochemically acceptable salts, esters and derivative present in an amount of 1.0% to 10.0% w/w;
ii. Component (B) Diafenthiuron or its agrochemically acceptable salts, esters and derivative present in an amount of 15.0% to 50.0% w/w;
iii. Component (C) is selected from at least one insecticide from neonicotinoid group in an amount of 1.0% to 15.0% w/w;
iv. Wetting agent in an amount of 1.0% to 8.0 % w/w;
v. Dispersing agent in an amount of 1.0% to 20.0% w/w;
vi. Disintegrating agent in an amount of 2.0% to 15.0% w/w;
vii. Antifoaming agent in an amount of 0.1% to 2.0% w/w
viii. Binder in an amount of 0.1% to 5.0% w/w; and
ix. Carrier & filler are in amount of quantity sufficient.

7. The synergistic insecticidal composition as claimed in claim 5, wherein the Suspension Concentrate (SC) formulation comprises:
i. Component (A) Fluxametamide or its agrochemically acceptable salts, esters and derivative present in an amount of 1.0% to 10.0% w/w;
ii. Component (B) Diafenthiuron or its agrochemically acceptable salts, esters and derivatives present in an amount of 15.0% to 50.0% w/w;
iii. Component (C) is selected from at least one insecticide from neonicotinoid group present in an amount of 1.0% to 15.0% w/w;
iv. Dispersing agent in an amount of 2.0% to 15.0% w/w;
v. wetting agent in an amount of 1.0% to 10.0% w/w;
vi. Anti-foaming agent in an amount of 0.1% to 5.0% w/w;
vii. Anti-freezing agent in amount of 0.1% to 5.0% w/w;
viii. Rheology modifier in amount of 0.05% to 2.0% w/w;
ix. Thickener is in amount of 0.1% to 5.0% w/w;
x. Preservative is in amount of 0.1% to 1.0% w/w; and
xi. Solvent is in amount quantity sufficient.

8. The synergistic insecticidal composition as claimed in claim 5, wherein the wettable powder (WP) formulation comprises:
i. Component (A) Fluxametamide or its agrochemically acceptable salts, esters and derivative present in an amount of 1.0% to 10.0% w/w;
ii. Component (B) Diafenthiuron or its agrochemically acceptable salts, esters and derivatives present in an amount of 15.0% to 50.0% w/w;
iii. Component (C) is selected from at least one insecticide from neonicotinoid group present in an amount of 1.0% to 15.0% w/w;
iv. Wetting agent in an amount of 1.0% to 10.0% w/w;
v. Dispersing agent in an amount of 1.0 % to 20.0% w/w;
vi. Anticaking agent in an amount of 1.0% to 10.0% w/w;
vii. Carrier is in amount quantity sufficient.

9. The synergistic insecticidal composition as claimed in claim 6, claim 7 and claim 8, wherein wetting agent is selected from tristyryl phenol ethoxylate non-ionic polymer, sodium iso propyl naphthalene sulphonate, alkyl phenyl ethoxylate, aryl phenyl ethoxylate, aryl phenyl ether phosphate, alkoxylated alcohol, ethoxylated fatty alcohol, ethylene oxide-propylene oxide (EO-PO) block copolymer, alkyl aryl sulphonate, alkyl olefin sulfonate, dioctyl succinate, sodium lauryl sulfate, alkyl polyglucoside, sodium alkyl aryl taurate, sorbitol esters, sorbitol oleate, poly aryl phenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate. Ethoxylated alcohol includes natural fatty alcohol (lauryl alcohol ethoxylate, lauryl alcohol alkoxylate), synthetic alcohol ethoxylate (tridecyl alcohol ethoxylate, 2-ethyl hexanol, 2-propylheptanol, isodecyl alcohol, trisiloxane ethoxylate, heptamethyl trisiloxane, modified form includes polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified Tri siloxane, polyalkyleneoxide modified polydimethylsiloxane, may be liquid or powder form or a combination thereof in an amount in the range from 1.0% to 10.0% w/w.

10. The synergistic insecticidal composition as claimed in claim 6, claim 7 and claim 8, wherein Dispersing agent is selected from the group comprising acrylic graft copolymer, examples are methyl methacrylate ethoxylated graft co-polymer, 2-Acrylamido-2-Methylpropane Sulfonic Acid, Sodium methallyl sulfonate, 3-sulfopropyl acrylate potassium salt, 3-sulfopropyl methacrylate potassium salt, 2-hydroxypropyl methacrylate, 2-hydroxypropyl acrylate, 2-hydroxymethyl methacrylate, Polyethylene-g-poly(n-butyl acrylate), poly acrylate copolymer.; polyarylphenyl ether phosphate, Tri styryl phenol ethoxylate, ethoxylated tristryl phenol sulphate, acrylic polymer amine salt, naphthalene sulfonic acid-sodium salt condensate with formaldehyde, alkylated naphthalene sulfonate-sodium salt, ethoxylated oleylcetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol, alkyl sulfonate, styrene acrylic copolymer, alkyl phenol polyglycol ether, sodium lignosulfonate, calcium lignosulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide- polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide or a combination thereof in an amount in the range from 1.0% to 20.0% w/w.

11. The synergistic insecticidal composition as claimed in claim 6, claim 7, wherein Anti-foaming agent is selected from Siloxane polyalkyleneoxide, polydimethylsiloxane, polysiloxane emulsion, vegetable oil-based antifoam, magnesium stearate or a combination thereof and present in an amount in range from 0.1% to 5.0% w/w.

12. The synergistic insecticidal composition as claimed in claim 7, wherein Anti freezing agent is selected from ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride or a combination thereof is present in an amount in the range from 0.1 to 10% w/w.

13. The synergistic insecticidal composition as claimed in claim 7, wherein Thickeners/ suspending agent is selected from the group comprising polysaccharides such as xanthan gum, sodium carboxymethyl cellulose, hydroxymethyl cellulose, sodium polyacrylate, bentonite clay, attapulgite clay, aluminum magnesium silicate, hydroxy propyl cellulose, polyvinyl alcohols, modifier starch, acacia gum, gelatin or a combination thereof and is present in an amount in the range from 0.01 to 5% w/w.

14. The synergistic insecticidal composition as claimed in claim 6, wherein disintegrating agent is selected from clays, bentonite, diatomaceous, colloidal silica, kaolin, potassium phosphate, ammonium sulphate, sodium sulphate, sodium citrate or urea or a combination thereof and is present in an amount in the range from 2 to 15% w/w.

15. The synergistic insecticidal composition as claimed in claim 7, wherein solvent is selected from the group comprising of demineralized (DM) water, alcohols such as ethanol, propanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, acetophenone, 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; heavy aromatic hydrocarbons such as Mixture of heavy aromatic naphtha hydrocarbon C-9 to C-16, xylene, toluene, naphthalene, solvent naphtha, solvent C9, solvent C10, solvent C12, solvesso 100, solvesso 150, solvesso 200; carboxamide; aliphatic or aromatic hydrocarbons such as chlorobenzene, chloroethylene, methylene chloride; esters such as ethyl acetate, Di isopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; alkyl amide, amides such as dimethylformamide, alkyl pyrrolidone, N-methyl-2-pyrrolidone, N-octyl pyrrolidone, N,N-dimethyldecanamide, N, N-dimethyloctanamide, N, N-dimethylamine, N,N-dimethylmethanamide; nitriles such as acetonitrile; organosulfur compound such as alkyl sulfoxide, dimethyl sulfoxide, alkylated vegetable oil such as methyl soyate, mineral oil alone or in combination thereof and are in amount of quantity sufficient.

16. The synergistic insecticidal composition as claimed in claim 7, wherein rheology modifier is selected from water-soluble selected from a group consisting of poly ethylene wax, poly vinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol, polyethylene oxide, polyethoxylated fatty acids, polyesters, polyamides, poly carbonates, poly urea, poly urethanes, styrene copolymer, butadiene copolymers, polyethoxylated alcohols, acrylate polymer such as polymethacrylate, poly ethyl methacrylate, poly methyl methacrylate, acrylate copolymers and styrene-acrylic copolymers, a natural gum, lignosulphonate, China clay, bentonite, fuller’s earth, zeolite, quartz, precipitated silica, palygorskite, sepiolite, halloysite, and a combination thereof and are present in amount of 0.05% to 2.0% w/w.

17. The synergistic insecticidal composition as claimed in claim 8, wherein Anti-caking agents selected from silica/silicone dioxide, calcium silicate, sodium ferrocyanide. Calcium stearate. Optionally anti-caking agents are present in an amount in the range from 0.1 to 10% w/w.

18. The synergistic insecticidal composition as claimed in claim 6, wherein binder is water soluble, water swellable or combinations of both, selected from a group consisting of poly ethylene wax, poly vinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol, polyethylene oxide, polyethoxylated fatty acids, polyesters, polyamides, poly carbonates, poly urea, poly urethanes, styrene copolymer, butadiene copolymers, polyethoxylated alcohols, acrylate polymer such as polymethacrylate, poly ethyl methacrylate, poly methyl methacrylate, acrylate copolymers and styrene-acrylic copolymers or mixtures of thereof, a natural gum, lignosulphonate, China clay, bentonite, fuller’s earth, zeolite, quartz, precipitated silica, palygorskite, sepiolite, halloysite, and a combination thereof, is present in an amount in the range from 0.1 to 10% w/w.

19. The synergistic insecticidal composition as claimed in claim 6 and claim 8, wherein, filler/carrier selected from the group comprising sand, silica, precipitated silica, bentonite, attapulgite, ceramic, montmorillonite, pumice, sepiolite, diatomaceous earth, clay, dolomite, calcite, silicon dioxide, china clay/kaolin clay, talc, starch, zinc and its salts (zinc sulphate, zinc oxide, zinc lactate gluconate, zinc polyflavonoid), iron and its salt (ferrous sulphate), copper and salts, sulphur, humic acid and salt, fulvic acid and salt, amino acids, sea weed extracts, chitosan or a combination thereof. It presents in an amount quantity sufficient (QS) required to make 100% w/w formulation.

Dated this 18th day of February, 2025