Abstract: The present invention provides a synergistic composition comprising at least one triazole, at least one neonicotinoid, and at least one pyridine-based pesticide, and a process for preparation of the composition and uses thereof.
DESC:NOVEL SYNERGISTIC COMPOSITION COMPRISING A TRIAZOLE FUNGICIDE AND INSECTICIDE
FIELD OF THE INVENTION
The present invention relates to a novel synergistic composition comprising a synergistically effective amount of at least three actives. More particularly, the present invention relates to a pesticidal composition comprising at least one triazole, at least one neonicotinoid, and pyriproxyfen and a process of preparation thereof.
BACKGROUND OF THE INVENTION
Pesticides are substances used to control pests (Insects, Diseases or weeds). The Food and Agriculture Organization (FAO) has defined pesticide as any substance or mixture of substances intended for preventing, curating, controlling or destroying any pest, including vectors of human or animal disease, unwanted species of plants or animals, causing harm during or otherwise interfering with the production, processing, storage, transport, or marketing of food, agricultural commodities, wood and wood products or animal feedstuffs, or substances that may be administered to animals for the control of insects, arachnids, or other pests in or on their bodies. The term includes substances intended for use as a plant growth regulator, defoliant, desiccant, or agent for thinning fruit or preventing the premature fall of fruit. Also used as substances applied to crops before or after harvest to protect the commodity from deterioration during storage and transport.
Several chemicals such as insecticides, herbicides, fungicides, rodenticides, bactericides, and larvicides and their combination have been developed to control insects and pests. However, more economically efficient and ecologically safe insect control compositions are still being sought. Insecticidal compositions that allow for reduced effective dosage rates, increased environmental safety, and lower incidence of resistance are highly desirable. The rotational application of insect control agents may be adopted as good pest management practice. However, this does not necessarily provide satisfactory insect control.
Various active ingredients are used as solo and binary formulations. However, with extensive and prolonged use of solo and binary formulations, pests develop resistance, and more concentrated formulations are required to be applied, resulting in various adverse effects on plant health and crop yield. With the onset of resistance to pest (s), despite extensive studies on several insecticidal combinations, a synergistic effect is rarely observed.
However, formulating a composition comprising two or more actives faces challenges such as poor solubility of actives, inadequate dissolution, and crystal formation. Additionally, there are compatibility issues with various components, and if the components are not optimally chosen, haziness, separation, and layer formation occur in the formulation. Moreover, these formulations crystallize in cold storage conditions and fail to reform upon returning to ambient temperature. Furthermore, heat storage studies reveal that these formulations experience layering and increased haziness after a certain period.
Therefore, there is need to develop a stable formulation that that is broad-spectrum, environmentally safe, and helps reduce dosage and frequency of application.
OBJECTIVES OF THE INVENTION
The primary objective of the invention is to provide a synergistic composition comprising at least three actives.
Another objective of the present invention is to provide a composition comprising of at least one fungicide, at least one insecticide, and at least one pyridine-based pesticide.
Another objective of the present invention is to provide a process for preparation of the synergistic agrochemical composition.
Another objective of the present invention is to provide a synergistic composition comprising at least one triazole, at least one neonicotinoid, and at least one pyridine-based pesticide.
Another objective of the present invention is to provide a synergistic composition with broad spectrum control of pests and diseases.
Another objective of the present invention is to provide a method for controlling pests and diseases in the agriculture field.
Another objective of the present invention is to provide a novel and effective synergistic composition which is stable at various temperature ranges and variable environmental changes.
Another objective of the present invention is to provide a novel and effective synergistic composition demonstrating high efficacy and high selectivity.
SUMMARY OF THE INVENTION
The following presents a simplified summary of the invention to provide a basic understanding of some aspects of the invention. This summary is not an extensive overview of the present invention. It is not intended to identify the key/critical elements of the invention or to delineate the scope of the invention. Its sole purpose is to present some concept of the invention in a simplified form as a prelude to a more detailed description of the invention presented later.
Accordingly, the present invention aims to provide a synergistic composition comprising at least three active compounds. The three actives are selected from group comprising of at least one triazole fungicide, at least one neonicotinoid insecticide, and at least one pyridine-based pesticide.
In an aspect, the present invention provides a process for preparation of the synergistic composition comprising of at least one triazole, at least one neonicotinoid, and at least one pyridine-based pesticide.
In another aspect of the present invention, the synergistic composition comprises of (a) at least one triazole in an amount in the range of 0.1-80% by weight, (b) at least one neonicotinoid in an amount in the range of 0.1-80% by weight, and (c) at least one pyridine-based pesticide in an amount in the range of 0.1-80% by weight.
In another aspect of the present invention, the synergistic composition comprises:
(a) at least one triazole fungicide in an amount in the range of 0.1 to 80% by weight of the composition;
(b) acetamiprid in an amount in the range of 0.1 to 80% by weight of the composition;
(c) pyriproxyfen in an amount in the range of 0.1 to 80% by weight of the composition; and
(d) one or more agriculturally acceptable excipient.
In a preferred aspect, the present invention composition comprises:
a) acetamiprid;
b) pyriproxyfen; and
c) at least one triazole fungicide.
In another aspect, the composition comprises
a) acetamiprid in the range of 1 to 30% by weight of the composition;
b) pyriproxyfen in the range of 0.1 to 30% by weight of the composition;
c) at least one triazole fungicide in the range of 0.1 to 30% by weight of the composition; and
d) at least one agriculturally acceptable excipient.
In another aspect of the present invention, the synergistic composition comprises (a) at least one triazole, (b) at least one neonicotinoid and (c) pyriproxyfen.
In another aspect of the present invention, the synergistic composition comprises (a) at least one triazole, (b) acetamiprid and (c) at least one pyridine-based pesticide.
In another aspect of the present invention, the synergistic composition comprises (a) at least one triazole, (b) acetamiprid and (c) pyriproxyfen.
In another aspect of the present invention, the triazole fungicide is selected from tebuconazole, flutriafol, propiconazole and difenoconazole.
In another aspect of the present invention, the agriculturally acceptable excipient is selected from the group comprising a carrier, a binder, a disintegrating agent, dispersants or dispersing agent, a wetting agent, a pH modifier, a humectant, a thickener, a biocide, a preservative, an anti-freezing agent, a colorant, a defoamer, an emulsifier, a co-solvent, solvent or any combination thereof.
In an aspect, the emulsifier is present in an amount in the range of 0.1 to 20% by weight, the humectant is present in an amount in the range of 0.1 to 15% by weight; and the dispersant is present in an amount in the range of 0.1 to 15% by weight.
In an aspect, the emulsifier may be selected from the group consisting of salts of dodecylbenzene sulphonate, e.g. Ca-salts or amine salts, and sulphonates of other C11-C16 alkylbenzenes, alkylether sulphates, alkylphenoletherphosphates and ester phosphates; non-ionic surfactants such as alkoxylated alcohols and alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, e.g. ethoxylated castor oil, fatty acid esters, e.g. of sorbitol, and their ethoxylated derivatives, ethoxylated amines, and condensates of glycerol; and catanionic emulsifiers such as a cationic amine, optionally in combination with an alkylsulphonate or ether sulphonate or ether phosphate, alkoxylated alcohols; alkoxylated alkylphenols; ethoxylated fatty acids; ethoxylated vegetable oils; ethoxylated tristyrylphenol; fatty acid esters of sorbitol and ethoxylated derivatives thereof; ethoxylated amines and condensates of glycerol; sulfonated alkylbenzenes in the range C11-C16 and salts thereof; alkylether sulphates; alkyletherphosphates; alkylphenoletherphosphates; or combinations thereof; salts of phosphate esters of ethoxylated tristyrylphenol; salts of sulphated ethers of ethoxylated tristyrylphenol; or a catanionic system, wherein a cationic amine is present in combination with an alkylsulphonate, an alkylethersulphonate, an ether sulphate, or an ether phosphate such as an alkyletherphosphate, nonylphenol polyethoxy ethanols, castor oil polyglycol ethers, polyadducts of ethylene oxide and polypropylene, tributyl phenoxy polyethoxy ethanol, octyl phenoxy polyethoxy ethanol or combination thereof.
In yet another aspect, the humectant is selected from the group consisting of urea, humic acid, glycerol, lactose or combination thereof; and the dispersant is selected from the group consisting of acrylic graft copolymer, alcohols, C9-11-iso-, C10-rich, ethoxylated, tristyrylphenol ethoxylate phosphate ester, poly(oxy-1,2-ethanediyl), a-sulfo-?-[2,4,6-tris(1- phenylethyl)phenoxy]-, ammonium salt, poly(oxy-1,2-ethanediyl), a-phosphono-? 2,4,6-tris(1-phenylethyl)phenoxy-, alkoxylated alcohol, naphthalene and alkyl naphthalene sulphonic acids formaldehyde condensate, sodium salt, alkyl aryl ethylene oxide condensates, sodium lignosulphonates, sodium dibutylnaphthalenesulphonate, poly aryl phenyl ether phosphate, tristyryl phenol ethylated/ acrylic graft copolymer/ ethoxylated tristryl phenol sulphate, naphthalene sulfonic acid, sodium salt condensate with formaldehyde, ethoxylated oleyl cetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol, EO-PO block copolymers, graft copolymers or combination thereof.
In another aspect, the synergistic composition of the present invention may be formulated as Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG), Emulsion water-in-oil (EO), Emulsifiable powder (EP), Emulsion for seed treatment (ES), Emulsion oil-in-water (EW), Flowable concentrate for seed treatment (FS), Granules (GR), Micro-emulsion (ME), Nano-emulsion, Oil dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Oil dispersible powder (OP), Suspension concentrate (SC), Suspension concentrate for direct application (SD), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC) or a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).
In another aspect, the present invention provides a process for preparing a synergistic composition comprising the steps of (a) weighing and transferring a solvent and a co-solvent in a beaker; (b) adding acetamiprid in the solvent under continuous stirring and at a controlled temperature in the range of 45°C and 50°C to obtain a homogeneous solution; (c) reducing the temperature to 25°C after complete dissolution; (d) adding pyriproxyfen and at least one triazole fungicide to the mixture of step (c) at an ambient temperature and under continuous stirring till uniform dissolution; (e) adding and mixing dispersing agent, emulsifier, humectant and colorant to the mixture of step (d); and (f) homogenizing the mixture of step (e) to obtain a stable emulsion.
In another aspect, the present invention provides a synergistic composition that is stable, environmentally safe and possesses enhanced efficacy for broad spectrum control of pests and diseases.
Other aspects, advantages, and salient features of the invention will become apparent to those skilled in the art from the following detailed description, which, details the invention in different embodiments.
DETAILED DESCRIPTION OF THE INVENTION
The definitions provided herein below for the terminologies used in the present disclosure are for illustrative purposes only and, in no manner, limit the scope of the present invention disclosed in the present disclosure.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention pertains. Other process and materials similar, or equivalent, to those described herein may be used in the practice of the present invention.
It is to be noted that, as used in the specification, the singular forms “a”, “an” and “the” include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to a composition containing “a compound” includes a mixture of two or more compounds. It should also be noted that the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise.
The use of terms “including,” “comprising,” or “having” and variations thereof herein; are meant to encompass the items listed thereafter and equivalents thereof as well as additional items. Further, the use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results. Furthermore, the term "may" be used herein in a permissive sense (i.e. meaning having the potential to), rather than the mandatory sense, (i.e. meaning must).
The terms “formulation” and “composition” as used herein convey the same meaning and may be used interchangeably.
The terms “process” and “method” as used herein convey the same meaning and may be used interchangeably.
The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total solution or composition unless otherwise specified.
The term “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.
The term “active ingredient” (a.i.) or “active agent” used herein refers to that component of the composition responsible for control of insect pests.
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.
As used herein, the term “fungicide”, refers to any chemical substance used to kill parasitic fungi or their spores.
As used herein, the term “insecticide” or “pesticide”, refers to any chemical substance used to destroy/kill, inhibit or otherwise adversely affect the insect pests.
As used herein, the term “pyridine-based pesticide”, refers to any chemical substance used is effective against a variety of insects.
As used herein, the active ingredient encompasses its agrochemically acceptable salts, derivatives, or any other modified form.
Accordingly, the present invention aims to provide a stable synergistic agrochemical composition comprising at least three active compounds selected from at least one triazole fungicide, at least one neonicotinoid insecticide, and at least one pyridine-based pesticide.
The composition of the present invention comprises of acetamiprid, pyriproxyfen; and at least one triazole fungicide.
In an embodiment, the present invention provides a process for preparing a synergistic composition comprising at least one triazole fungicide, at least one neonicotinoid insecticide, and at least one pyridine-based pesticide.
In another embodiment of the present invention, the triazole fungicide is selected from tebuconazole, flutriafol, propiconazole and difenoconazole.
In another embodiment of the present invention, the triazole fungicide is present in an amount in the range of 0.1-80%, preferably in the range of 0.1 to 50%, more preferably in the range of 0.1 to 30% by weight of the composition.
In another embodiment of the present invention, the neonicotinoid is acetamiprid present in an amount in the range of 0.1-80%, preferably in the range of 1 to 50%, more preferably in the range of 1 to 30% by weight of the composition.
In another embodiment of the present invention, the pyridine-based pesticide is pyriproxyfen present in an amount in the range of 0.1-80%, preferably in the range of 0.1 to 50%, more preferably in the range of 0.1 to 30% by weight of the composition.
In yet another embodiment, the present invention provides a synergistic composition comprising of (a) at least one triazole fungicide selected from tebuconazole, flutriafol, propiconazole and difenoconazole; (b) acetamiprid; and (c) pyriproxyfen.
In an embodiment, the composition may comprises of acetamiprid, pyriproxyfen; at least one triazole fungicide; and at least one agriculturally acceptable excipient.
In a preferred embodiment of the present invention, the synergistic composition comprises (a) tebuconazole, (b) acetamiprid, and (c) pyriproxyfen.
In another preferred embodiment of the present invention, the synergistic composition comprises (a) flutriafol, (b) acetamiprid, and (c) pyriproxyfen.
In another preferred embodiment of the present invention, the synergistic composition comprises (a) propiconazole, (b) acetamiprid, and (c) pyriproxyfen.
In another preferred embodiment of the present invention, the synergistic composition comprises (a) difenoconazole, (b) acetamiprid, and (c) pyriproxyfen.
In another preferred embodiment of the present invention, the synergistic composition comprises:
(a) at least one triazole fungicide selected from tebuconazole, flutriafol, propiconazole and difenoconazole, present in an amount in the range of 0.1 to 30% by weight of the composition;
(b) acetamiprid in an amount in the range of 1 to 30% by weight of the composition;
(c) pyriproxyfen in an amount in the range of 0.1 to 30% by weight of the composition; and
(d) at least one agriculturally acceptable excipient.
The inventors have surprisingly found that the composition at the aforementioned weight percentage ranges provides synergistic effect.
In another embodiment, the synergistic composition of the present invention may be formulated as Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG), Emulsion water-in-oil (EO), Emulsifiable powder (EP), Emulsion for seed treatment (ES), Emulsion oil-in-water (EW), Flowable concentrate for seed treatment (FS), Granules (GR), Micro-emulsion (ME), Nano-emulsion, Oil dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Oil dispersible powder (OP), Suspension concentrate (SC), Suspension concentrate for direct application (SD), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC) or a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).
In a preferred embodiment, the composition of present invention may be formulated as Dispersible concentrate (DC).
In another embodiment of the present invention, the agriculturally acceptable excipient is selected from the group comprising a carrier, a binder, a disintegrating agent, dispersants or dispersing agent, a wetting agent, a pH modifier, a humectant, a thickener, a biocide, a preservative, an anti-freezing agent, a colorant, a defoamer, an emulsifier, a co-solvent, solvent or any combination thereof.
In another embodiment of the present invention, the emulsifier is ethoxylated castor oil present in an amount in the range of 0.1 to 20%, preferably in the range of 0.1 to 15%.
In another embodiment of the present invention, the humectant is urea present in an amount in the range of 0.1 to 20%, preferably in the range of 0.1 to 15%.
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 re-aggregating. 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 often employed are anionic, non-ionic, or mixes of the two. Sodium lingo sulphonates are the most often used dispersants in wettable powder compositions.
Dispersant(s) or dispersing agent(s) may be selected from the group comprising of, but not limited to dispersing agent is selected from the group comprising acrylic co-polymer solution, alcohols, C9-11-iso-, C10-rich, ethoxylated, fatty alcohol ethoxylate, sodium lignosulfonate, blend of alkyl phenol ethoxylate, polyarylphenol ethoxylates and tristyrylphenol ethoxylates, or any combination thereof.
In another embodiment of the present invention, the dispersing agent is present in an amount in the range of 0.1 to 20%, preferably in the range of 0.1 to 15%, more preferably in the range of 0.1 to 12% by weight of the composition.
Emulsifier(s) or emulsifying agent(s) may be selected from the group comprising of, but not limited to Acrylic Co-Polymer Solution, Alcohols, C9-11-iso-, C10-rich, ethoxylated, blend of alkyl aryl sulphonate, nonylphenol, ethoxylated, isobutanol & solvent naphtha (Petroleum) light aromatics, ethopropoxylated polyarylphenol, branched calcium dodecyl benzene sulphonates, tristyryl phenol-polyethylene glycol ether, polyoxyethylene sorbitan mono laurate, fatty alcohol ethoxylate, poly oxyethylenated triglycerides & alcohol ethoxylate/blend polymeric non-ionic surfactants or equivalent, ethoxylate CO-20, Agnique® BP NP-4030 EO-PO Poly, Agnique® CP 72 L, Agnique® 10 CSO 40-U, Agnique® CSO-20, Agnique® CSO-36 Ethox Castor Oil, Agnique® DDL Dispersant, IG Surf® 2370 SC, IG Surf® 2380.
In another embodiment of the present invention, the emulsifier may be present in an amount in the range of 0.1 to 20% by weight of the composition.
Anti-freezing agent(s) may be selected from the group comprising of, but not limited to glycols, mono-ethylene glycol, di-ethylene glycol, propylene glycol, polyethylene glycols, methoxy polyethylene glycols, polypropylene glycols, polybutylene glycols, glycerine and ethylene glycol. Water-based formulations often cause foam during mixing operations in production. In order to reduce the tendency of foaming; anti-foaming agents are often added either during the production stage or before filling into 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 nonsilicone 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.
Antifoaming agent(s) may be selected from the group comprising of, but not limited to silicon emulsion based anti-foam agents, Siloxane polyalkyleneoxide, Polydimethyl Siloxane, trisiloxane ethoxylates and mixtures thereof.
A wetting agent is a substance that, when added to a liquid, increases its spreading or penetrating ability by lowering the interfacial tension between the liquid and the surface it is spreading on. Wetting agent(s) may be selected from the group comprising of, but not limited to alcohols, C9-11-iso-, C10-rich, ethoxylated, and/or blend of alkyl phenol ethoxylate.
Thickener(s) may be selected from the group comprising of, but not limited to, water-soluble polymer and inorganic fine powder, wherein water-soluble polymer such as xanthan gum, arabic 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, white carbon. These thickeners may be used alone or in combination thereof.
Preservative may be selected from the group comprising of, but not limited to, 20% aqueous dipropylene glycol solution of 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.
Colorant(s) may include one or more inorganic or organic pigments, or metal effect agents, or combinations thereof. Examples of suitable pigments include titanium dioxide white, carbon black, lamp black, black iron oxide, red iron oxide, yellow iron oxide, brown iron oxide (a blend of red and yellow oxide with black), phthalocyanine green, phthalocyanine blue, blue dye, amaranth, erythrosine, tartrazine, fast green FCF, brilliant blue FCF, Prussian blue, alizarin dye, azo dye, organic red pigment (such as naphthol red, quinacridone red and toluidine red), quinacridone magenta, quinacridone violet, DNA orange, and organic yellow pigment (such as Hansa yellow) and combinations thereof.
In another embodiment of the present invention, the colorant may be present in the range of 0.001% to 0.1% by weight of the composition.
A carrier is an inert solid or liquid material; the active ingredients or mixtures comprising actives are mixed with the carrier. The carrier helps deliver the active ingredient uniformly. Water, organic solvents, clay, sand, limestone, gypsum, fine powders or granules such as minerals such as kaolin clay, attapulgite clay, bentonite, montmorillonite, acid white clay, pyrophyllite, talc, diatomaceous earth, dioxosilane, oxo(oxoalumanyloxy) alumane, hydrate granules; 4-O-beta-D-Galactopyranosyl-D-glucose, lactose or any combination thereof are used as a carrier.
In another embodiment of the present invention, the carrier may be present in the range of 1 to 15% by weight of the composition.
Solvent(s) or co-solvent(s) may be selected from the group comprising of, but not limited to, water, demineralized water (DM); alcohols such as ethanol, 2-butoxyethanol, 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 aromatic, solvent C9, solvent C10, 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, diisopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; amides such as dimethyl formamide, N-methyl-2-pyrrolidone, N-octyl pyrrolidone, N, N dimethyl decanamide, N,N-Dimethyl heptanamide, N,N-diethyl heptanamide, N,N-Dimethyl octanamide, N,N-Diethyl octanamide, N,N-dimethyl nonanamide, N,N-Diethyl nonanamide, N,N-Diethyl decanamide, N,NDimethyl undecanamide, N,N-Diethyl undecanamide, N,N-Dimethyl dodecanamide, N,N-Diethyl dodecanamide; nitriles such as acetonitrile; organo sulfur compounds.
In another embodiment of the present invention, the co-solvent may be present in the range of 1 to 30% by weight of the composition.
In another embodiment of the present invention, the solvent may be present in the “Quantum Satis” i.e., Q.S quantity.
In an embodiment, the emulsifier may be selected from emulsifiers containing salts of dodecylbenzene sulphonate, e.g. Ca-salts or amine salts, and sulphonates of other C11-C16 alkylbenzenes, alkylether sulphates, alkyl phenol ether phosphates and ester phosphates; non-ionic surfactants such as alkoxylated alcohols and alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, e.g. ethoxylated castor oil, fatty acid esters, e.g. sorbitol, and their ethoxylated derivatives, ethoxylated amines, and condensates of glycerol; and catanionic emulsifiers such as a cationic amine, optionally in combination with an alkylsulphonate or ether sulphonate or ether phosphate, alkoxylated alcohols; alkoxylated alkylphenols; ethoxylated fatty acids; ethoxylated vegetable oils; ethoxylated tristyrylphenol (tristyrlphenol with 16 moles EO), tristyrylphenolpolyglycolether-phosphate, fatty acid esters of sorbitol and ethoxylated derivatives thereof; ethoxylated amines and condensates of glycerol; sulfonated alkylbenzenes in the range C11-C16 and salts thereof; alkylether sulphates; alkyl ether phosphates; alkyl phenol ether phosphates; or combinations thereof; salts of phosphate esters of ethoxylated tristyrylphenol; salts of sulphated ethers of ethoxylated tristyrylphenol; or a catanionic system, wherein a cationic amine is present in combination with an alkyl sulphonate, an alkyl ether sulphonate, an ether sulphate, or an ether phosphate such as an alkyl ether phosphate, nonylphenol polyethoxyethanols, castor oil polyglycol ethers, polyadducts of ethylene oxide and polypropylene, tributyl phenoxy polyethoxy ethanol, octyl phenoxy polyethoxy ethanol, or mixtures thereof.
In an embodiment, the stabilizer may be selected from butylated hydroxytoluene (BHT), epoxidized soybean oil (ESBO), and epichlorohydrin.
In another embodiment, the anti-freezing agent may be selected from the ethylene glycol, propane diols, glycerine, urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate, sodium chloride, or mixtures thereof. In an embodiment, the anti-foaming agent may be selected from silicone oil, silicone compound, C10-C20 saturated fatty acid compounds or C8-C10 aliphatic alcohols, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane, or mixtures thereof.
In an embodiment, the preservative may be selected from propionic acid and its sodium salt, sorbic acid and its sodium or potassium salt, benzoic acid and its sodium salt, p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate;and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2- methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates or mixtures thereof. In an embodiment, the thickeners may be selected from water-insoluble particulates and water-soluble polymers. It is possible to produce suspo-emulsion formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenan; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of thickeners are based on modified starches, polyacrylates, polyvinyl 20 alcohol and polyethylene oxide or mixtures.
In an embodiment, the wetting agent may be selected from organosilicone surfactants including trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, polyalkyleneoxide modified heptamethyl trisiloxane, heptamethyl trisiloxane ethoxylate, polyether modified polysiloxane, 10 mole ethylene oxide adduct of octylphenol, or mixtures thereof. Each of these may or may not be in modified form, may be liquid or powder form or mixture thereof.
In an embodiment, the anti-freezing agent may be selected from ethylene glycol, propane diols, glycerine, urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate, sodium chloride, or mixtures thereof. In an embodiment, the anti-foaming agent may be selected from silicone oil, silicone compound, C10-C20 saturated fatty acid compounds or C8-C10 aliphatic alcohols, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane, or mixtures thereof.
In yet another aspect, the humectant may be selected from the group consisting of urea, humic acid, glycerol, lactose or combination thereof; and the dispersant may be selected from the group consisting of acrylic graft copolymer, alcohols, C9-11-iso-, C10-rich, ethoxylated, tristyryl phenol ethoxylate phosphate ester, poly(oxy-1,2-ethanediyl), a-sulfo-?-[2,4,6-tris(1- phenylethyl) phenoxy]-, ammonium salt, poly(oxy-1,2-ethanediyl), a-phosphono-? 2,4,6-tris(1-phenylethyl)phenoxy-, alkoxylated alcohol, naphthalene and alkyl naphthalene sulphonic acids formaldehyde condensate, sodium salt, alkyl aryl ethylene oxide condensates, sodium lignosulphonates, sodium dibutyl naphthalene sulphonate, poly aryl phenyl ether phosphate, tristyryl phenol ethylated/ acrylic graft copolymer/ ethoxylated tristryl phenol sulphate, naphthalene sulfonic acid, sodium salt condensate with formaldehyde, ethoxylated oleyl cetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol, EO-PO block copolymers, graft copolymers or combination thereof. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. The synthetic polymer exhibits crystal growth inhibition properties. These have very long hydrophobic backbones and a large number of ethylene oxide chains forming the “teeth of a comb” surfactant. These high molecular weight polymers may give long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces. Examples of dispersants used herein include but not limited to sodium lignosulphonates, poly aryl phenyl ether phosphate, tristyryl phenol ethylated/ acrylic graft copolymer/ ethoxylated tristryl phenol sulphate, naphthalene sulfonic acid, Sodium dibutylnaphthalenesulphonate, sodium salt condensate with formaldehyde, ethoxylated oleyl cetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol; and graft copolymers or mixtures thereof.
Thickeners, gelling agents, and viscosity modifier are commonly used in the formulation of suspension concentrates, emulsions, and suspoemulsions to alter the rheology or flow properties of the liquid and to avoid separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents are classified as either water-insoluble particles or water-soluble polymers. Clay and silicas may be used for preparing suspension concentrate compositions. These materials include, but are limited to, montmorillonite (e.g., bentonite), magnesium aluminum silicate, and attapulgite. For many years, water-soluble polysaccharides have been used as thickening, and gelling agents. Natural extracts of seeds and seaweed, as well as synthetic derivatives of cellulose or mixtures thereof, are the most often utilized polysaccharides. Guar gum, locust bean gum, Carrageenan, xanthan gum, alginates, methyl cellulose, sodium carboxymethyl cellulose (SCMC), hydroxyethyl cellulose (HEC) or combination thereof are examples of these materials. Other anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol, polyethylene oxide or any combination thereof. These auxiliaries can be added depending on the specific requirements of formulations.
In another embodiment, the present invention provides a process for preparing a synergistic composition comprising the steps of (a) weighing and transferring a solvent and a co-solvent in a beaker; (b) adding acetamiprid in the solvent under continuous stirring and at a controlled temperature in the range of 45°C and 50°C to obtain a homogeneous solution; (c) reducing the temperature to 25°C after complete dissolution; (d) adding pyriproxyfen and at least one triazole fungicide to the mixture of step (c) at an ambient temperature and under continuous stirring till uniform dissolution; (e) adding and mixing dispersing agent, emulsifier, humectant and colorant to the mixture of step (d); and (f) homogenizing the mixture of step (e) to obtain a stable emulsion.
EXAMPLES
Below are the various examples for preparing different formulations according to the present invention. However, the below examples 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: Dispersible Concentrate (DC) Composition
Example 1(a):
Table 1: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8% Pyriproxyfen and 12.5% Tebuconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Tebuconazole Active 12.5%
4 N, N-Dimethyldecanamide Co-Solvent 20.0%
5 Ethoxylated Castor Oil Emulsifier 12.0%
6 Polyarylphenol ethoxylated Dispersant 3.0%
7 Tristyrylphenol Ethoxylates 5.0%
8 Urea Humectant 3.0%
9 Optionally - Blue Dye Colorant 0.001%
10 Water Carrier 5.0%
11 2-Butoxyethanol Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed accurately N, N-Dimethyldecanamide and 2-Butoxyethanol, and it was transferred to a beaker. Next, Acetamiprid technical was added to the solvent under continuous stirring at a controlled speed of 100 RPM while maintaining the temperature between 45°C and 50°C. The mixture was stirred for another 20 mins until complete dissolution, reducing the temperature25°C. The next steps involve adding Pyriproxyfen technical and Tebuconazole technical to the mixture under continuous stirring and at a controlled temperature to obtain a homogeneous solution. Further, the ethoxylated castor oil, urea, dispersant and colourant were added to the mixture and stirred continuously. The mixture was homogenized at 1400 RPM for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 2: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Liquid Liquid
2 Color without Blue dye Yellow Yellow
3 Color with Blue Dye Blue Blue
4 Odor Aromatic Aromatic
5 pH 1 % Aq. Solution 5.0-8.5 6.58
6 Density at 20°C g/ml 1.0 g/ml ± 0.05 0.993 g/ml
7 Dispersion Stability Stable Stable
8 Solubility in water Dispersible Dispersible
Table 3: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Color without Blue Dye Yellow Yellow
Color with Blue Dye Blue Blue
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Tebuconazole AI % 5.00
8.28
12.55 4.97
8.25
12.51
pH 1 % Aq. Solution 6.66 6.69
Dispersion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
The above tables 1-3 disclose a composition comprising Acetamiprid A.I., Pyriproxyfen A.I. and Tebuconazole A.I. The obtained composition, as characterized in Table 2, is a liquid with a yellow colour, aromatic odour, and a pH range of 5.0 to 8.5 in a 1% aqueous solution. The composition has a density of 1.0 g/ml ± 0.05. Further, the composition exhibits excellent accelerated storage stability, showing positive results for all parameters after 14 days at 25°C and after 14 days at 54°C under accelerated heat storage conditions (AHS). Furthermore, the composition exhibits cold stability at 0°C for 7 days, with no significant changes in its properties, demonstrating its reliability and long-term stability. This stability is achieved by adding a dispersant and an emulsifier, ethoxylated castor oil, to the composition. These compounds facilitate the breakdown of particle aggregates, providing uniform dispersion of active ingredients. As a result, the composition exhibits enhanced dispersion stability and improved efficacy. Additionally, the composition also comprises urea as a humectant. Urea enhances moisture retention, ensuring optimal crop hydration, resulting in vigorous growth and improved crop health.
Example 1(b):
Table 4: Dispersible Concentrate (DC) composition of 3.5% Acetamiprid, 8.5% Pyriproxyfen and 14% Tebuconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 3.5%
2 Pyriproxyfen Active 8.5%
3 Tebuconazole Active 14%
4 N,N-Dimethyldecanamide Co-Solvent 22%
5 Ethoxylated Castor Oil Emulsifier 15.0%
6 Polyarylphenol ethoxylated Dispersant 4.0%
7 Tristyrylphenol Ethoxylates Dispersant 5.0%
8 Water Carrier 6.0%
9 Urea Humectant 2.5%
10 Blue Dye (Optionally) Colorant 0.001%
11 2-Butoxyethanol Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed accurately N, N-Dimethyldecanamide and 2-Butoxyethanol, and it was transferred to a beaker. Next, Acetamiprid technical was added to the solvent under continuous stirring at a controlled speed of 100 RPM while maintaining the temperature between 45°C and 50°C. The mixture was stirred for another 20 mins until complete dissolution, then the temperature was reduced to 25°C. The next steps involve adding Pyriproxyfen technical and Tebuconazole technical to the mixture under continuous stirring and at a controlled temperature to obtain a homogeneous solution. Further, the ethoxylated castor oil, urea, dispersant and colourant were added to the mixture and stirred continuously. The mixture was homogenized at 1400 RPM for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 5: Physiochemical Properties of the composition
S. No. Test Parameters 0 days @25°C
1 Physical state Clear Liquid
2 Color without blue dye Yellow
3 Color with blue dye Blue
4 Odor Aromatic
5 Acetamiprid AI %
Pyriproxyfen AI %
Tebuconazole AI % 3.56
8.54
14.3
6 pH 1 % Aq. Solution 6.73
7 Density at 20°C g/ml 1.00 g/ml
8 Dispersion Stability Stable
9 Cold stability @ 0ºC for 7 days Passes
Example 1(c):
Table 6: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 12.5% Flutriafol
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Flutriafol Active 12.5%
4 Solvent N, N-Dimethyldecanamide Co-Solvent 15.0%
5 Ethoxylated Castor Oil Emulsifier 12.0%
6 Polyarylphenol ethoxylated Dispersant 5.0%
7 Tristyrylphenol Ethoxylates 4.0%
8 Urea Humectant 4.0%
9 Blue Dye Colorant 0.001%
10 Water Carrier 7.0%
11 N-Methylpyrrolidone Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed accurately N, N-Dimethyldecanamide and 2-Butoxyethanol, and it was transferred to a beaker. Next, Acetamiprid technical was added to the solvent under continuous stirring at a controlled speed of 100 RPM while maintaining the temperature between 45°C and 50°C. The mixture was stirred for another 20 mins until complete dissolution, then the temperature was reduced to 25°C. The next steps involve adding Pyriproxyfen technical and Flutriafol technical to the mixture under continuous stirring and at a controlled temperature to obtain a homogeneous solution. Further, the ethoxylated castor oil, urea, dispersant and colourant were added to the mixture and stirred continuously. The mixture was homogenized at 1400 RPM for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 7: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Liquid Liquid
2 Color without blue dye Yellow Yellow
3 Color with blue dye Blue Blue
4 Odor Aromatic Aromatic
5 pH 1 % Aq. Solution 5.0-8.5 6.58
6 Density at 20°C g/ml 1.0 g/ml ± 0.05 0.993 g/ml
7 Dispersion Stability Stable Stable
8 Solubility in water Dispersible Dispersible
Table 8: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Color without Blue dye Yellow Yellow
Color with Blue dye Blue Blue
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Flutriafol AI % 5.00
8.15
12.56 4.98
8.11
12.52
pH 1 % Aq. Solution 6.85 6.93
Dispersion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
The above tables 6-8 disclose a composition comprising Acetamiprid A.I., Pyriproxyfen A.I. and Flutriafol A.I. As characterized in Table 7, the obtained composition is a liquid with a yellow colour, aromatic odour, and a pH range of 5.0 to 8.5 in a 1% aqueous solution. The composition has a density of 1.0 g/ml ± 0.05. Further, the composition exhibits excellent accelerated storage stability, showing positive results for all parameters after 14 days at 25°C and after 14 days at 54°C under accelerated heat storage conditions (AHS). Furthermore, the composition exhibits cold stability at 0°C for 7 days, with no significant changes in its properties, demonstrating its reliability and long-term stability. This stability is achieved by adding a dispersant and an emulsifier, ethoxylated castor oil, to the composition. These compounds facilitate the breakdown of particle aggregates, providing uniform dispersion of active ingredients. As a result, the composition exhibits enhanced dispersion stability and improved efficacy. Additionally, the composition also comprises urea as a humectant. Urea enhances moisture retention, ensuring optimal crop hydration, resulting in vigorous growth and improved crop health.
Example 1(d):
Table 9: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 5% Difenoconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Difenoconazole Active 5%
4 N, N-Dimethyldecanamide Co-Solvent 5%
5 Castor oil Ethoxvlate Emulsifier 12.0%
6 Sodium Lignosulfonate Dispersant 1.0%
7 Blend Of Alkyl Phenol Ethoxylate Dispersant 15.0%
8 Urea Humectant 3.0%
9 Blue Dye (Optional) Colorant 0.001%
10 Water Carrier 5.0%
11 NMP Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed accurately N, N-Dimethyldecanamide and 2-Butoxyethanol, and it was transferred to a beaker. Next, Acetamiprid technical was added to the solvent under continuous stirring at a controlled speed of 100 RPM while maintaining the temperature between 45°C and 50°C. The mixture was stirred for another 20 mins until complete dissolution, reducing the temperature25°C. The next steps involve adding Pyriproxyfen technical and Difenoconazole technical to the mixture under continuous stirring and at a controlled temperature to obtain a homogeneous solution. Further, the ethoxylated castor oil, urea, dispersant and colourant were added to the mixture and stirred continuously. The mixture was homogenized at 1400 RPM for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 10: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Clear Liquid Clear Liquid
2 Color without blue dye Brownish Yellow Brownish Yellow
3 Color with blue dye Blue Blue
4 Odor Aromatic Aromatic
5 pH 1 % Aq. Solution 4.0 – 6.0 4.58
6 Density at 20°C g/ml 1.08g/ml ± 0.05 1.07g/ml
7 Dispersion Stability Stable Stable
8 Solubility in water Dispersible Dispersible
Table 11: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Color without blue dye Brownish Yellow Brownish Yellow
Color with blue dye Blue Blue
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Difenoconazole AI % 4.96
8.37
5.18 4.93
8.33
5.15
pH 1 % Aq. Solution 4.62 4.60
Dispersion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
The above tables 9-11 disclose a composition comprising Acetamiprid A.I., Pyriproxyfen A.I. and Difenoconazole A.I. As characterized in Table 10, the obtained composition is a liquid with a brownish-yellow colour, aromatic odour, and a pH range of 4.0 to 6.0 in a 1% aqueous solution. The composition has a density of 1.08 g/ml ± 0.05. Further, the composition exhibits excellent accelerated storage stability, showing positive results for all parameters after 14 days at 25°C and after 14 days at 54°C under accelerated heat storage conditions (AHS). Furthermore, the composition exhibits cold stability at 0°C for 7 days, with no significant changes in its properties, demonstrating its reliability and long-term stability. This stability is achieved by adding a dispersant and an emulsifier, ethoxylated castor oil, to the composition. These compounds facilitate the breakdown of particle aggregates, providing uniform dispersion of active ingredients. As a result, the composition exhibits enhanced dispersion stability and improved efficacy. Additionally, the composition also comprises urea as a humectant. Urea enhances moisture retention, ensuring optimal crop hydration, resulting in vigorous growth and improved crop health.
Example 1(e):
Table 12: Dispersible Concentrate (DC) composition of 3.8% Acetamiprid, 7.0% Pyriproxyfen and 10.5% Prothioconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 3.8%
2 Pyriproxyfen Active 7.0%
3 Prothioconazole Active 10.5%
4 NMP Co-Solvent 20.0%
5 Castor oil Ethoxvlate Emulsifier 10.0%
6 Polyarylphenol ethoxylated Dispersant 5.0%
7 Tristyrylphenol Ethoxylates 4.0%
8 Urea Humectant 1.2%
9 Blue Dye (Optional) Colorant 0.001%
10 Water Carrier 5.0%
11 2-Butoxyethanol Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed accurately N, N-Dimethyldecanamide and 2-Butoxyethanol, and it was transferred to a beaker. Next, Acetamiprid technical was added to the solvent under continuous stirring at a controlled speed of 100 RPM while maintaining the temperature between 45°C and 50°C. The mixture was stirred for another 20 mins until complete dissolution, reducing the temperature25°C. The next steps involve adding Pyriproxyfen technical and Prothioconazole technical to the mixture under continuous stirring and at a controlled temperature to obtain a homogeneous solution. Further, the ethoxylated castor oil, urea, dispersant and colourant were added to the mixture and stirred continuously. The mixture was homogenized at 1400 RPM for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 13: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Liquid Liquid
2 Color without blue dye Yellow Yellow
3 Color with blue dye Blue Blue
4 Odor Aromatic Aromatic
5 pH 1 % Aq. Solution 5.0-8.5 6.8
6 Density at 20 °C g/ml 1.0 g/ml ± 0.05 €1.03 g/ml
7 Dispersion Stability Stable Stable
8 Solubility in water Dispersible Dispersible
Table 14: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Colour Yellow Yellow
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Prothioconazole AI % 3.86
7.08
10.56 3.85
7.05
10.53
pH 1 % Aq. Solution 6.78 6.86
Dispersion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
The above tables 12-14 disclose a composition comprising Acetamiprid A.I., Pyriproxyfen A.I. and Prothioconazole A.I. As characterized in Table 13, the obtained composition is a liquid with a yellow colour, aromatic odour, and a pH range of 5.0 to 8.5 in a 1% aqueous solution. The composition has a density of 1.0 g/ml ± 0.05. Further, the composition exhibits excellent accelerated storage stability, showing positive results for all parameters after 14 days at 25°C and after 14 days at 54°C under accelerated heat storage conditions (AHS). Furthermore, the composition exhibits cold stability at 0°C for 7 days, with no significant changes in its properties, demonstrating its reliability and long-term stability. This stability is achieved by adding a dispersant and an emulsifier, ethoxylated castor oil, to the composition. These compounds facilitate the breakdown of particle aggregates, providing uniform dispersion of active ingredients. As a result, the composition exhibits enhanced dispersion stability and improved efficacy. Additionally, the composition also comprises urea as a humectant. Urea enhances moisture retention, ensuring optimal crop hydration, resulting in vigorous growth and improved crop health.
Example 2: Micro-emulsion Concentrate (ME) Composition
Example 2(a):
Table 15: Micro-emulsion Concentrate (ME) composition of 4.0% Acetamiprid, 7.2% Pyriproxyfen and 12.0% Tebuconazole
S. No. Ingredients Quantity In % W/W
1 Acetamiprid A.I 4.0%
2 Pyriproxyfen A.I. 7.2%
3 Tebuconazole A.I. 12%
4 Sodium Lignosulfonate 0.1%
5 Polyarylphenol ethoxylated 3.5%
6 Tristyrylphenol Ethoxylates 4.5%
7 Castor oil ethoxylate 10.0%
8 Urea 2.0%
9 N, N-Dimethyldecanamide 20.0%
10 Water 5.0%
11 N-Methyl-2-pyrrolidone Q.S.
Process for preparation of the composition: Prepare a solvent phase by accurately weighing the required amount of N-Methyl-2-pyrrolidone (NMP) and N, N-Dimethyldecanamide and transferring it to a beaker. The mixture was stirred at a speed of 100 RPM. Next, Acetamiprid, Pyriproxyfen, and Tebuconazole technical were added to the mixture under continuous stirring to obtain a homogeneous solution. The next step involves preparing an organic phase by adding and mixing water, urea and sodium lignosulfonate to obtain a mixture. The mixture was stirred for about 20 minutes to ensure complete dissolution. Further, the organic phase was added to the solvent phase under continuous stirring to obtain a mixture. The dispersant and castor oil ethoxylate were added to the mixture and stirred for another 20 minutes to ensure thorough dispersion and uniform emulsification. The material was packed after passing quality analysis.
Table 16: Physiochemical Properties of the composition
S. No. Test Parameters Specification
1 Physical state Liquid
2 Colour Yellow to Brown
3 Odor Aromatic
4 Emulsion Stability Stable
5 pH (1% aqua sol.) 4.0 – 6.0
6 Flash point Above 24.5ºC
7 Density at 20°C g/ml 1.04 g/ml ± 0.1
Table 17: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Colour Brown Brown
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Tebuconazole AI % 4.07
7.06
12.10 4.05
7.04
12.08
pH 1 % Aq. Solution 4.68 4.79
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
Example 2(b):
Table 18: Micro-emulsion Concentrate (ME) composition of 5.4% Acetamiprid, 6.5% Pyriproxyfen and 11.0% Difenoconazole
S. No. Ingredients Quantity In % W/W
1 Acetamiprid A.I 5.4%
2 Pyriproxyfen A.I. 6.5%
3 Difenconazole A.I. 11%
4 Polyarylphenol ethoxylated 5.5%
5 Tristyrylphenol Ethoxylates 6.0%
6 Castor oil ethoxylate 14.0%
7 Urea 1.9%
8 N, N-Dimethyldecanamide 17.0%
9 Water 5.0%
10 N-Methyl-2-pyrrolidone Q.S.
Process for preparation of the composition: Prepare a solvent phase by accurately weighing the required amount of N-Methyl-2-pyrrolidone (NMP) and N, N-Dimethyldecanamide and transferring it to a beaker. The mixture was stirred at a speed of 100 RPM. Next, Acetamiprid, Pyriproxyfen, and Difenoconazole technical were added to the mixture under continuous stirring to obtain a homogeneous solution. The next step involves preparing an organic phase by adding and mixing water, urea and sodium lignosulfonate to obtain a mixture. The mixture was stirred for about 20 minutes to ensure complete dissolution. Further, the organic phase was added to the solvent phase under continuous stirring to obtain a mixture. The dispersant and castor oil ethoxylate were added to the mixture and stirred for another 20 minutes to ensure thorough dispersion and uniform emulsification. The material was packed after passing quality analysis.
Table 19: Physiochemical Properties of the composition
S. No. Test Parameters Specification
1 Physical state Liquid
2 Colour Yellow to Brown
3 Odor Aromatic
4 Emulsion Stability Stable
5 pH (1% aqua sol.) 4.0 – 6.0
6 Flash point Above 24.5ºC
7 Density at 20°C g/ml 1.04 g/ml ± 0.1
Table 20: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Colour Brown Brown
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Difenoconazole AI % 5.48
6.56
11.07 5.45
6.54
11.05
pH 1 % Aq. Solution 4.86 4.95
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
Example 2(c):
Table 21: Micro-emulsion Concentrate (ME) composition of 4.8% Acetamiprid, 7.0% Pyriproxyfen and 10.2% Flutriafol
S. No. Ingredients Quantity In % W/W
1 Acetamiprid A.I 4.8%
2 Pyriproxyfen A.I. 7%
3 Flutriafol A.I. 10.2%
4 Polyarylphenol ethoxylated 4%
5 Tristyrylphenol Ethoxylates 5.5%
6 Castor oil ethoxylate 11%
7 Urea 1.5%
8 2-Butoxyethanol 4.0%
9 Water 5.0%
10 N-Methyl-2-pyrrolidone Q.S.
Process for preparation of the composition: Prepare a solvent phase by accurately weighing the required amount of N-Methyl-2-pyrrolidone (NMP) and N, N-Dimethyldecanamide and transferring it to a beaker. The mixture was stirred at a speed of 100 RPM. Next, Acetamiprid, Pyriproxyfen, and Flutriafol technical were added to the mixture under continuous stirring to obtain a homogeneous solution. The next step involves preparing an organic phase by adding and mixing water, urea and sodium lignosulfonate to obtain a mixture. The mixture was stirred for about 20 minutes to ensure complete dissolution. Further, the organic phase was added to the solvent phase under continuous stirring to obtain a mixture. The dispersant and castor oil ethoxylate were added to the mixture and stirred for another 20 minutes to ensure thorough dispersion and uniform emulsification. The material was packed after passing quality analysis.
Table 22: Physiochemical Properties of the composition
S. No. Test Parameters Specification
1 Physical state Liquid
2 Colour Yellow to Brown
3 Odor Aromatic
4 Emulsion Stability Stable
5 pH (1% aqua sol.) 4.0 – 6.0
6 Flash point Above 24.5ºC
7 Density at 20°C g/ml 1.04 g/ml ± 0.1
Table 23: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Colour Brown Brown
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Flutriafol AI % 4.88
7.26
10.26 4.85
7.25
10.24
pH 1 % Aq. Solution 4.82 4.95
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
Example 2(d):
Table 24: Micro-emulsion Concentrate (ME) composition of 4.0% Acetamiprid, 7.2% Pyriproxyfen and 12.0% Prothioconazole
S. No. Ingredients Quantity In % W/W
1. Acetamiprid A.I 4.0%
2. Pyriproxyfen A.I. 7.2%
3. Prothioconazole A.I. 12%
4. Polyarylphenol ethoxylated 3.0%
5. Tristyrylphenol Ethoxylates 6.5%
6. Castor oil ethoxylate 15.0%
7. Urea 2.5%
8. 2-Butoxy ethanol 8.0%
9. Water 5.0%
10. N-Methyl-2-pyrrolidone Q.S.
Process for preparation of the composition: Prepare a solvent phase by accurately weighing the required amount of N-Methyl-2-pyrrolidone (NMP) and N, N-Dimethyldecanamide and transferring it to a beaker. The mixture was stirred at a speed of 100 RPM. Next, Acetamiprid, Pyriproxyfen, and Prothioconazole technical were added to the mixture under continuous stirring to obtain a homogeneous solution. The next step involves preparing an organic phase by adding and mixing water, urea and sodium lignosulfonate to obtain a mixture. The mixture was stirred for about 20 minutes to ensure complete dissolution. Further, the organic phase was added to the solvent phase under continuous stirring to obtain a mixture. The dispersant and castor oil ethoxylate were added to the mixture and stirred for another 20 minutes to ensure thorough dispersion and uniform emulsification. The material was packed after passing quality analysis.
Table 25: Physiochemical Properties of the composition
S. No. Test Parameters Specification
1 Physical state Liquid
2 Colour Yellow to Brown
3 Odor Aromatic
4 Emulsion Stability Stable
5 pH (1% aqua sol.) 4.0 – 6.0
6 Flash point Above 24.5ºC
7 Density at 20°C g/ml 1.04 g/ml ± 0.1
Table 26: Storage Stability Data
Test Parameters 14 Days @ 25°C 14 Days @ 54°C
Physical state Clear Liquid Clear Liquid
Colour Brown Brown
Odor Aromatic Aromatic
Acetamiprid AI %
Pyriproxyfen AI %
Prothioconazole AI % 4.05
7.28
12.06 4.04
7.27
12.03
pH 1 % Aq. Solution 4.91 5.03
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes
Example 3: Present invention composition without emulsifier and humectant.
Example 3(a):
Table 27: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8% Pyriproxyfen and 12.5% Tebuconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Tebuconazole Active 12.5%
4 Solvent N, N-Dimethyldecanamide Co-Solvent 3.0%
5 Polyoxyethylene sorbitan fatty acid ester Emulsifier 5.0%
6 Ammonium Salt of Polyarylphenyl Ether Sulfate Dispersing agent 12.0%
7 Water Carrier 4.0%
8 Propylene carbonate Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed the required amount of solvent N, N-Dimethyldecanamide, & Propylene carbonate in a beaker. Then Acetamiprid Technical was added to the solvent, and the mixture was stirred at RPM 100 and 52°C temperature for 20 minutes until complete dissolution, then the temperature was reduced to 25°C. The following steps involve adding Pyriproxyfen technical and Tebuconazole technical to the mixture under continuous stirring to obtain a homogeneous solution. Further, the emulsifiers and water were added to the mixture and homogenized at 1400 rpm for 30 minutes to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 28: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Liquid Not completely soluble
2 Color Yellow Yellow
3 Odor Aromatic Aromatic
4 pH 1 % Aq. Solution 5.0-8.5 Failed
5 Density at 20°C g/ml 1.0 g/ml ± 0.05 Failed
6 Dispersion Stability Stable Failed
7 Solubility in water Emulsifiable Failed
Example 3(b):
Table 29: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 12.5% Tebuconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Tebuconazole Active 12.5%
4 Solvent N, N-Dimethyldecanamide Co-Solvent 3.0%
5 Ethoxylate CO 20 Emulsifier 3.0%
6 Polyarylphenol ethoxylated Dispersing agent 8.0%
7 (Ethoxylated tristyrylphenol (Poly(oxy-1,2-ethanediyl), a-[2,4,6-tris(1-phenylethyl) phenyl]-w-hydroxy) Dispersing agent 3.0%
8 Water Carrier 10.0%
9 2-Butoxyethanol Solvent Q.S.
TOTAL 100
Process for preparation of the composition: Weighed the required amount of solvent N, N-Dimethyldecanamide & 2-Butoxyethanol in a beaker. Then Acetamiprid Technical was added to the solvent, and the mixture was stirred at RPM 100 and 52°C temperature for 20 minutes until complete dissolution, then the temperature was reduced to 25°C. The next steps involve adding Pyriproxyfen technical and Tebuconazole technical to the mixture under continuous stirring to obtain a homogeneous solution. Further, the emulsifiers, Ethoxylate CO 20 and water, were added to the mixture and homogenized at 1400 rpm for 30 mins to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 30: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Clear liquid Hazy liquid
2 Color Light to dark yellow Yellow
3 Odor Aromatic Aromatic
4 pH 1 % Aq. Solution 5.0-8.5 Failed
5 Density at 20°C g/ml 1.0 g/ml ± 0.05 Failed
6 Dispersion Stability Stable Failed
7 Solubility in water Emulsifiable Failed
Example 3(c):
Table 31: Dispersible Concentrate (DC) composition of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 12.5% Tebuconazole
S. No. Ingredients Function Quantity In % W/W
1 Acetamiprid Active 4.8%
2 Pyriproxyfen Active 8.0%
3 Tebuconazole Active 12.5%
4 Ethoxylate CO 20 Emulsifier 3.0%
5 Polyethylene Glycol Octylphenyl ether; PEG -10 Octyl Phenol ether Dispersing agent 5.0%
6 (Ethoxylated tristyrylphenol (Poly(oxy-1,2-ethanediyl), a-[2,4,6-tris(1-phenylethyl) phenyl]-w-hydroxy) Dispersing agent 10.0%
7 Water Carrier 0.75%
8 2-Butoxyethanol Solvent Q.S.
TOTAL 100 ML
Process for preparation of the composition: Weighed the required amount of solvent 2-Butoxyethanol in a beaker. Then Acetamiprid Technical was added to the solvent, and the mixture was stirred at RPM 100 and 52°C temperature for 20 minutes until complete dissolution, then the temperature was reduced to 25°C. The following steps involve adding Pyriproxyfen technical and Tebuconazole technical to the mixture under continuous stirring to obtain a homogeneous solution. Further, the emulsifiers, Ethoxylate CO 20 and water, were added to the mixture and homogenized at 1400 rpm for 30 mins to obtain a stable emulsion. The material was packed after passing quality analysis.
Table 32: Physiochemical Properties of the composition
S. No. Test Parameters Specifications Result
1 Physical state Clear liquid Clear liquid
2 Color Light to dark yellow Yellow
3 Odor Aromatic Aromatic
4 pH 1 % Aq. Solution 5.0-8.5 6.92
5 Density at 20 °C g/ml 1.0 g/ml ± 0.05 0.988 hg/ml
6 Dispersion Stability Stable Failed (3 ml sediment)
7 Solubility in water Emulsifiable Dispersible
As evident from Tables 27 to 32, the composition without emulsifier and humectants showed unfavourable results for stability. The composition underwent particle aggregation and sedimentation. This physical change negatively impacted the composition due to increased particle size and reduced dispersion. In contrast, the present invention composition possessed optimal dispersion and better stability, thereby improving the overall performance of the composition.
Example 4: Evaluation of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 12.5% Tebuconazole DC composition for bio-efficacy against Whitefly (Bemisia tabaci) & Alternaria leaf spot in Cotton crop.
TRIAL 1: Experimental Details
Season Kharif
Location Rama Mandi Bathinda (PB)
Crop Cotton
Age of Crop 68 Days
Temperature Range during Trial 29-40°C
Variety RCH-926
Single plot size 25 m2
Date of Transplanting/Sowing 16/05/2024
Number of applications 01
Date of application 24/07/2024
Target Pest Whitefly & Alternaria Leaf spot
Method of application Foliar
Table 33: Treatment Details
S. No. Treatments Active Ingredient (AI) (gm/ha) Dose (ml/ha)
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 60+100+156.25gm 1250 ml
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 60+100gm 300+1000 ml
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 100+156.25gm 1000+ 603 ml
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 60 + 156.25gm 300 + 603 ml
IE5 Acetamiprid 20% SP 60gm 300 ml
IE6 Pyriproxyfen 10% EC 100gm 1000 ml
IE7 Tebuconazole 25.9% EC 156.25 gm 603 ml
IE8 Control - -
• The experiment was laid out in a randomized block design and replicated thrice with a single plot area of 25 m2. The test sample, as per the treatment schedule, was applied at pest appearance using 500 litres of water per hectare using a knapsack sprayer.
• A pre-count was taken prior to the spray conduction. Pests count was recorded from (Area of observation) randomly selected five plants per replication and from three leaves per plant.
• Post-spray application pest count was recorded on the 3rd, 7th, and 10th days after spray application, whereas observation for Alternaria disease incidence was recorded on the 5th, 10th, and 15th days after spray Application.
• Percent reduction in pest population was calculated using a formula Henderson and Tilton gave.
• Percent reduction in Population = 100 × (1-Ta × Cb) / Tb × Ca, where
• Ta = Number of insects after treatment,
• Tb = Number of insects before treatment,
• Ca = Number of insects in untreated check after treatment,
• Cb = Number of insects in untreated check before treatment.
A disease rating scale is also provided for evaluating the percentage of disease control & PDI by using disease rating scale:
Disease Rating scale:
Rating Scale Disease severity & Description
0 No of lesions / discoloration
1 1% area covered with lesions / spots / discoloration
3 1-10% area covered with lesions / spots / discoloration
5 10-25% area covered with lesions / spots / discoloration
7 25-50% area covered with lesions / spots / discoloration
9 > 50% area covered with lesions / spots / discoloration
The scored data will convert into per cent disease index (PDI) using formula given below. The PDI will be subject to statistical analysis.
Percent Disease Incidence (PDI) = Sum of infected Numerical ratings × 100
Total no. of plants × maximum rating scale
Percent disease reduction over control (PDC) was calculated by using the formula given below:
Percent disease reduction over control = PDI of control – PDI of treatment × 100
PDI of treatment
Table 34: Effect of different treatments against Cotton Whitefly (Bemisia tabaci)
S. No. Treatments Dose ml/ha Effectiveness of present invention against Cotton Whitefly
Corrected Per cent control
Pre count (Avg. pest count per leaf) 3 DAA 7 DAA 10 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 16.47 80.58 81.72 83.76
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 17.27 74.82 76.21 78.98
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+ 603 ml 17.27 69.42 70.69 70.70
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 + 603 ml 16.27 64.75 66.55 66.56
IE5 Acetamiprid 20% SP 300 ml 15.67 62.23 63.45 64.01
IE6 Pyriproxyfen 10% EC 1000 ml 16.67 63.31 65.52 65.29
IE7 Tebuconazole 25.9% EC 603 ml 16.93 17.27 19.31 18.15
IE8 Control - 17.20 0.00 0.00 0.00
Table 35: Synergistic effect of present invention composition against Cotton whitefly (Bemisia tabaci)
S. no. Treatment details Dose (ml or gm/Ha) Corrected percent (%) control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 83.76 74.6 1.12 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300 + 1000 ml 78.98 87.5 0.9 No
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000 + 603 ml 70.7 71.58 0.98 No
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 + 603 ml 69.14 70.54 0.98 No
IE5 Acetamiprid 20% SP 300 ml 64.1 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 65.29 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 18.15 0 0 0
The effectiveness of the present invention composition was evaluated against Cotton whitefly (Bemisia tabaci) in cotton crops. The effectiveness was measured as the percentage reduction of whitefly over the control at different intervals, i.e., 3, 7, and 10 days after application (DAA). Table 35 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% at dose 1250ml/ha resulted in the highest efficacy, achieving a percent reduction of 81.72% at 7 DAA and 83.76% at 10 DAA, thereby showing synergy as compared to other treatments.
Table 36: Effect of different treatments against Alternaria leaf spot of Cotton.
S. No. Treatments Dose ml/ha Effectiveness of Present invention against Alternaria leaf spot of cotton.
Percent Disease Control (PDC)
Before Spray PDI 5 DAA 10 DAA 15 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 11.11 69.96 72.22 83.52
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 13.33 4.00 14.81 14.29
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 11.85 54.00 66.67 74.73
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 12.59 52.00 62.96 74.73
IE5 Acetamiprid 20% SP 300 ml 12.59 6.00 12.96 8.79
IE6 Pyriproxyfen 10% EC 1000 ml 14.07 12.00 14.81 10.99
IE7 Tebuconazole 25.9% EC 603 ml 13.33 48.00 57.41 73.63
IE8 Control - 11.85 0.00 0.00 0.00
*PDI: Percent Disease Index
Table 37: Synergistic effect of present invention composition against Alternaria leaf spot of Cotton
S. no. Treatment details Dose (ml or gm/Ha) % Percent Disease Control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 83.52 77.16 1.08 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 14.29 18.81 0.75 No
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 74.73 76.52 0.97 No
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 74.73 75.94 0.98 No
IE5 Acetamiprid 20% SP 300 ml 8.79 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 10.99 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 73.63 0 0 0
Table 37 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% resulted in highest efficacy, achieving percent disease control of 72.22% at 10 DAA and 83.52% at 15 DAA, thereby showing synergy as compared to other treatments.
Example 5: Evaluation of 4.8% Acetamiprid, 8.0% Pyriproxyfen and 12.5% Tebuconazole DC composition for bio-efficacy against Whitefly & Alternaria leaf spot in Cabbage crop.
TRIAL 2: Laboratory Experimental Details
Season Kharif 2024
Location Village-Duradundi, Tq- Gokak, Dist-Belagavi, Karnataka
Crop Cabbage
Age of Crop 25 Days
Temperature Range during Trial 27-38°C
Variety RING (Chiguru Seeds)
Single plot size 25 m2
Date of Transplanting/Sowing 21/07/2024
Number of applications 01
Date of application 14/08/2024
Target Pest Whitefly & Alternaria Leaf spot/Dark leaf spot of cabbage (Alternaria brassicicola)
Method of application Foliar
Table 38: Effect of different treatments against Cabbage Whitefly
S. No. Treatments Dose ml/ha Effectiveness of present invention against Cabbage Whitefly
Corrected Per cent Control
Pre count (Avg. pest count per leaf) 3 DAA 7 DAA 10 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 39.67 85.26 90.53 89.69
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 38.00 81.09 87.33 82.66
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 40.40 67.63 73.89 65.02
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 38.80 66.67 72.52 60.09
IE5 Acetamiprid 20% SP 300 ml 38.47 63.62 68.55 56.95
IE6 Pyriproxyfen 10% EC 1000 ml 40.93 65.87 72.06 61.14
IE7 Tebuconazole 25.9% EC 603 ml 38.67 20.19 11.76 10.91
IE8 Control - 40.93 0.00 0.00 0.00
Table 39: Synergistic effect of present invention composition against Cabbage Whitefly.
S. no. Treatment details Dose (ml or gm/Ha) % Reduction over control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 89.69 77.50 1.16 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 82.66 83.27 0.99 No
IE3 Pyriproxyfen 10% EC + Tebuconazole 25.9% EC 1000+603 ml 65.02 65.38 0.99 No
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 60.09 61.65 0.97 No
IE5 Acetamiprid 20% SP 300 ml 56.95 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 61.14 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 10.91 0 0 0
The effectiveness of the present invention composition was evaluated against Cabbage whitefly. The effectiveness was measured as the percentage reduction of whitefly over the control at different intervals, i.e., 3, 7, and 10 days after application (DAA). Table 39 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% at dose 1250ml/ha resulted in the highest efficacy, achieving a percent reduction of 90.53% at 7 DAA and 89.69% at 10 DAA, thereby showing synergy as compared to other treatments.
Table 40: Effect of different treatments against Alternaria leaf spot of Cabbage.
S. No. Treatments Dose ml/ha Effectiveness of present invention against Alternaria leaf spot of cabbage (Alternaria brassicicola)
Percent Disease Control (PDC)
Before Spray PDI 5 DAA 10 DAA 15 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 14.07 67.16 76.84 83.70
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 14.81 19.40 25.26 25.19
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 15.56 56.72 69.47 78.52
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 + 603 ml 14.81 53.73 66.32 77.04
IE5 Acetamiprid 20% SP 300 ml 15.56 14.93 18.95 17.78
IE6 Pyriproxyfen 10% EC 1000 ml 14.07 8.96 16.84 16.30
IE7 Tebuconazole 25.9% EC 603 ml 15.56 50.75 65.26 76.30
IE8 Control - 15.56 0.00 0.00 0.00
*PDI: Per cent Disease Index
Table 41: Synergistic effect of present invention composition against Alternaria leaf spot of Cabbage
S. no. Treatment details Dose (ml or gm/Ha) % Percent Disease Control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 83.70 79.27 1.06 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 25.19 31.18 0.81 No
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 78.52 80.16 0.98 No
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 77.04 80.51 0.96 No
IE5 Acetamiprid 20% SP 300 ml 17.78 0.00 0.00 0.00
IE6 Pyriproxyfen 10% EC 1000 ml 16.30 0.00 0.00 0.00
IE7 Tebuconazole 25.9% EC 603 ml 76.30 0.00 0.00 0.00
Table 41 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% resulted in the highest efficacy, achieving per cent disease control of 76.84% at 10 DAA and 83.70% at 15 DAA, thereby showing synergy as compared to other treatments.
Example 6: Evaluation of Phytotoxicity of synergistic composition comprising Acetamiprid, Pyriproxyfen, and Tebuconazole in cotton & cabbage crop
Visual observations were recorded 7, 14, and 21 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below. A total of 20 plants per plot were observed.
Table 42: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
?Leaf injury on tips /surface? Rating
0%? 0?
1-10%? 1?
11-20%? 2?
21-30%? 3?
31-40%? 4?
41-50%? 5?
51-60%? 6?
61-70%? 7?
71-80%? 8?
81-90%? 9?
91-100%? 10?
Table 43: Phytotoxic effect of various treatments on cotton and cabbage crop after 7 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 44: Phytotoxic effect of various treatments on cotton and cabbage crop after 14 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 45: Phytotoxic effect of various treatments on cotton and cabbage crop after 21 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 1000+603 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 300 +603 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 603 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 46: Phytotoxic effect of various treatments on cotton and cabbage crop after 7 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 2000+1206 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 600 +1206 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 1206 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 47: Phytotoxic effect of various treatments on cotton and cabbage crop after 14 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 2000+1206 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 600 +1206 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 1206 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 48: Phytotoxic effect of various treatments on cotton and cabbage crop after 21 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Tebuconazole 12.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Tebuconazole 25.9% EC 2000+1206 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Tebuconazole 25.9% EC 600 +1206 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Tebuconazole 25.9% EC 1206 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Tables 43 to 48 above evidence that the application of Acetamiprid, Pyriproxyfen, and Tebuconazole in all doses showed no phytotoxicity symptoms like leaf injury on tips, leaf injury on the surface, wilting, vein clearing, necrosis, epinasty and hyponasty in cotton and cabbage crop. Further, as evident from tables 46, 47 and 48, the application of Acetamiprid, Pyriproxyfen, and Tebuconazole at even double doses shows no phytotoxicity. Thus, applying the present invention composition may be considered completely safe for crops.
Example 7: Evaluation of 4.8% Acetamiprid, 8% Pyriproxyfen, and 5% Difenoconazole DC composition for bio-efficacy against Whitefly & Alternaria leaf spot in Cotton crop.
TRIAL 3: Experimental Details
Season Kharif
Location Rama Mandi Bathinda (PB)
Crop Cotton
Age of Crop 68 Days
Temperature Range during Trial 29-40°C
Variety RCH-926
Single plot size 25 m2
Date of Transplanting/Sowing 16/05/2024
Number of applications 01
Date of application 24/07/2024
Target Pest Whitefly
Method of application Foliar
Table 49: Treatment Details
S. No. Treatments Active Ingredient (AI) (gm/ha) Dose (ml/ha)
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 60+100+62.5gm 1250 ml
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 60+100 gm 300+1000 ml
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 100+62.5 gm 1000+ 250 ml
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 60 + 62.5 gm 300 + 250 ml
IE5 Acetamiprid 20% SP 60 gm 300 ml
IE6 Pyriproxyfen 10% EC 100 gm 1000 ml
IE7 Difenoconazole 25% EC 62.5 gm 250 ml
IE8 Control - -
Table 50: Effect of different treatments against Cotton Whitefly (Bemisia tabaci)
S. No. Treatments Dose ml/ha Effectiveness of present invention against cotton Whitefly (Bemisia tabaci)
Corrected Per cent Control
Pre-count (Avg. pest count per leaf) 3 DAA 7 DAA 10 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 12.67 71.43 77.48 80.69
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 11.73 62.56 69.82 72.53
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 12.00 55.17 64.41 65.67
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 12.73 49.75 62.61 62.66
IE5 Acetamiprid 20% SP 300 ml 12.87 47.29 54.95 56.22
IE6 Pyriproxyfen 10% EC 1000 ml 13.33 47.29 56.76 58.37
IE7 Difenoconazole 25% EC 250 ml 12.40 15.27 17.57 18.45
IE8 Control - 11.73 0.00 0.00 0.00
Table 51: Synergistic effect of present invention composition against Cotton whitefly (Bemisia tabaci)
S. no. Treatment details Dose (ml or gm/Ha) Corrected Per cent % Control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 80.69 73.02 1.1 Yes
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 72.53 81.77 0.88 No
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 65.67 66.05 0.99 No
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 62.66 64.29 0.97 No
IE5 Acetamiprid 20% SP 300 ml 56.22 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 58.37 0 0 0
IE7 Difenoconazole 25% EC 250 ml 18.45 0 0 0
IE8 Control Nil 0 0 0 0
Table 51 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Difenoconazole 5% at dose 1250ml/ha resulted in the highest efficacy, achieving a per cent reduction of 77.48% at 7 DAA and 80.69% at 10 DAA, thereby showing synergy as compared to other treatments.
Table 52: Effect of different treatments against Alternaria leaf spot of Cotton.
S. No. Treatments Dose ml/ha Effectiveness of present invention against Alternaria Leaf spot of Cotton.
Per cent (%) Disease reduction over control
Before Spray PDI 5 DAA 10 DAA 15 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 10.37 60.47 68.75 78.76
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 13.33 13.16 16.67 15.94
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 10.37 39.47 62.50 66.67
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 11.11 36.84 58.33 66.67
IE5 Acetamiprid 20% SP 300 ml 9.63 7.89 10.42 11.59
IE6 Pyriproxyfen 10% EC 1000 ml 9.63 5.26 12.50 14.49
IE7 Difenoconazole 25% EC 250 ml 11.85 31.58 52.08 65.22
IE8 Control Nil 8.89 0.00 0.00 0.00
*PDI: Per cent Disease Index
Table 53: Synergistic effect of present invention composition against Alternaria leaf spot of Cotton.
S. no. Treatment details Dose (ml or gm/Ha) % Percent diseases reduction over control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Difenoconazole 5% DC 1250 ml 78.76 71.51 1.1 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 15.94 24.4 0.65 No
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 66.67 70.25 0.94 No
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 66.67 69.25 0.96 No
IE5 Acetamiprid 20% SP 300 ml 11.59 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 14.49 0 0 0
IE7 Difenoconazole 25% EC 250 ml 65.22 0 0 0
IE8 Control - 0 0 0 0
Table 53 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Difenoconazole 5% resulted in the highest efficacy, achieving per cent disease control of 68.75% at 10 DAA and 78.76% at 15 DAA, thereby showing synergy as compared to other treatments.
Example 8: Evaluation of Phytotoxicity of synergistic composition comprising Acetamiprid, Pyriproxyfen, and Difenoconazole in cotton crop
Visual observations were recorded 7, 14, and 21 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below. A total of 20 plants per plot were observed.
Table 54: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
?Leaf injury on tips /surface? Rating
0%? 0?
1-10%? 1?
11-20%? 2?
21-30%? 3?
31-40%? 4?
41-50%? 5?
51-60%? 6?
61-70%? 7?
71-80%? 8?
81-90%? 9?
91-100%? 10?
Table 55: Phytotoxic effect of various treatments on cotton crop after 7 DAA?at recommended dose.
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 250 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 56: Phytotoxic effect of various treatments on cotton crop after 14 DAA?at recommended dose.
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 250 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 57: Phytotoxic effect of various treatments on cotton crop after 21 DAA?at recommended dose.
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 1000+ 250 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 300 + 250 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 250 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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
?
Table 58: Phytotoxic effect of various treatments on cotton crop after 7 DAA?at double dose.
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 2000+ 500 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 600 + 500 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 500 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 59: Phytotoxic effect of various treatments on cotton crop after 14 DAA?at double dose.
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 2000+ 500 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 600 + 500 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 500 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 60: Phytotoxic effect of various treatments on cotton crop after 21 DAA?at double dose.
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% +
Difenoconazole 5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Difenoconazole 25% EC 2000+ 500 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Difenoconazole 25% EC 600 + 500 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 ml 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Difenoconazole 25% EC 500 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Tables 55 to 60 above evidence that the application of Acetamiprid, Pyriproxyfen, and Difenoconazole in all doses showed no phytotoxicity symptoms like leaf injury on tips, leaf injury on the surface, wilting, vein clearing, necrosis, epinasty and hyponasty in cotton and cabbage crop. Further, as evident from tables 58, 59 and 60, the application of Acetamiprid, Pyriproxyfen, and Difenoconazole at even double doses shows no phytotoxicity. Thus, applying the present invention composition may be considered completely safe for crops.
Example 9: Evaluation of 4.8% Acetamiprid, 8% Pyriproxyfen, and 11.5% Flutriafol DC composition for bio-efficacy against Whitefly & Alternaria leaf spot in Cotton crop.
TRIAL 4: Laboratory Experimental Details
Season Kharif
Location Rama Mandi Bathinda (PB)
Crop Cotton
Age of Crop 68 Days
Temperature Range during Trial 29-40°C
Variety RCH-926
Single plot size 25 m2
Date of Transplanting/Sowing 16/05/2024
Number of applications 01
Date of application 24/07/2024
Target Pest Whitefly
Method of application Foliar
Table 61: Treatment Details
S. No. Treatments Active Ingredient (AI) (gm/ha) Dose (ml/ha)
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 60+100+143.75 gm 1250 ml
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 60+100 gm 300+1000 ml
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 100+143.75 1000+575 ml
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 60 + 143.75 300 + 575 ml
IE5 Acetamiprid 20% SP 60 gm 300 gm
IE6 Pyriproxyfen 10% EC 100 gm 1000 ml
IE7 Flutriafol 25% SC 143.75 gm 575 ml
IE8 Control - -
Table 62: Effect of different treatments against Cotton Whitefly (Bemisia tabaci)
S. No. Treatments Dose ml/ha Effectiveness of present invention against Cotton Whitefly (Bemisia tabaci)
Corrected Per cent (%) control
Pre count (Avg. pest count per leaf) 3 DAA 7 DAA 10 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 16.47 80.20 82.76 84.39
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 17.27 74.06 76.90 79.62
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 17.27 68.94 72.76 73.25
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 16.27 65.19 71.38 72.29
IE5 Acetamiprid 20% SP 300 ml 15.67 63.48 65.52 67.52
IE6 Pyriproxyfen 10% EC 1000 ml 16.67 63.48 66.90 69.11
IE7 Flutriafol 25% SC 575 ml 16.93 19.45 20.34 17.20
IE8 Control - 17.20 0.00 0.00 0.00
Table 63: Synergistic effect of present invention composition against Cotton whitefly (Bemisia tabaci)
S. no. Treatment details Dose (ml or gm/Ha) Corrected per cent control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 84.39 75.64 1.11 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 79.62 89.96 0.88 No
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 73.25 74.42 0.98 No
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 72.29 73.1 0.98 No
IE5 Acetamiprid 20% SP 300 ml 64.1 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 65.29 0 0 0
IE7 Flutriafol 25% SC 575 ml 18.15 0 0 0
IE8 Control - 0 0 0 0
Table 63 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% at dose 1250ml/ha resulted in the highest efficacy, achieving a per cent reduction of 82.76% at 7 DAA and 84.39% at 10 DAA, thereby showing synergy as compared to other treatments.
Table 64: Effect of different treatments against Alternaria leaf spot of Cotton.
S. No. Treatments Dose ml/ha Effectiveness of present invention against Alternaria leaf spot of cotton
Per cent (%) Disease control (PDC)
Before Spray PDI 5 DAA 10 DAA 15 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 11.11 71.15 75.41 84.21
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 12.59 7.69 19.67 17.89
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 12.59 55.77 70.49 77.89
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 14.07 53.85 67.21 75.79
IE5 Acetamiprid 20% SP 300 gm 14.81 1.92 6.56 12.63
IE6 Pyriproxyfen 10% EC 1000 ml 14.81 11.54 18.03 14.74
IE7 Flutriafol 25% SC 575 ml 13.33 50.00 62.30 74.74
IE8 Control - 14.07 0.00 0.00 0.00
*PDI- Per cent Disease Index
Table 65: Synergistic effect of present invention composition against Alternaria leaf spot of Cotton.
S. no. Treatment details Dose (ml or gm/Ha) % Disease Reduction over control (PDC)
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 84.21 78.4 1.07 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 17.89 25.5 0.70 No
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 77.89 78.46 0.99 No
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 75.79 77.93 0.97 No
IE5 Acetamiprid 20% SP 300 gm 12.63 0.00 0.00 0.00
IE6 Pyriproxyfen 10% EC 1000 ml 14.74 0.00 0.00 0.00
IE7 Flutriafol 25% SC 575 ml 74.74 0.00 0.00 0.00
IE8 Control - 0.00 0.00 0.00 0.00
Table 65 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% resulted in the highest efficacy, achieving a percent disease control of 75.41% at 10 DAA and 84.21% at 15 DAA, thereby showing synergy as compared to other treatments.
Example 10: Evaluation of 4.8% Acetamiprid, 8% Pyriproxyfen, and 11.5% Flutriafol DC composition for bio-efficacy against Whitefly & Alternaria leaf spot in Cabbage crop.
TRIAL 5: Laboratory Experimental Details
Season Kharif 2024
Location Village-Duradundi, Tq- Gokak, Dist-Belagavi, Karnataka
Crop Cabbage
Age of Crop 25 Days
Temperature Range during Trial 27-38°C
Variety RING (Chiguru Seeds)
Single plot size 25 m2
Date of Transplanting/Sowing 21/07/2024
Number of applications 01
Date of application 14/08/2024
Target Pest Whitefly & Alternaria Leaf spot/Dark leaf spot of cabbage (Alternaria brassicicola)
Method of application Foliar
Table 66: Effect of different treatments against Cabbage Whitefly
S. No. Treatments Dose ml/ha Effectiveness of present invention against Cotton Whitefly (Bemisia tabaci)
Correct Per cent (%) control
Pre count (Avg. pest count per leaf) 3 DAA 7 DAA 10 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 29.53 78.75 88.38 86.69
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 30.53 73.26 83.31 79.55
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 30.13 56.96 70.38 61.76
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 30.40 54.21 67.27 57.14
IE5 Acetamiprid 20% SP 300 gm 31.07 52.01 64.16 54.76
IE6 Pyriproxyfen 10% EC 1000 ml 28.73 52.56 65.63 58.12
IE7 Flutriafol 25% SC 575 ml 29.87 1.28 11.46 9.66
IE8 Control - 28.87 0.00 0.00 0.00
Table 67: Synergistic effect of present invention composition against Cabbage Whitefly.
S. no. Treatment details Dose (ml or gm/Ha) Corrected per cent % control
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 86.69 76.73 1.13 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 79.55 81.06 0.98 No
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 61.76 62.17 0.99 No
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 57.14 59.13 0.97 No
IE5 Acetamiprid 20% SP 300 gm 54.76 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 58.12 0 0 0
IE7 Flutriafol 25% SC 575 ml 9.66 0 0 0
IE8 Control - 0.00 0 0 0
The effectiveness of the present invention composition against Cabbage whitefly by measuring the percentage reduction of whitefly over the control at different intervals, i.e., 3, 7, and 10 days after application (DAA). Table 67 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% at dose 1250ml/ha resulted in the highest efficacy, achieving a percent reduction of 88.38% at 7 DAA and 86.69% at 10 DAA, thereby showing synergy as compared to other treatments.
Table 68: Effect of different treatments against Alternaria leaf spot of Cabbage.
S. No. Treatments Dose ml/ha Effectiveness of PRESENT INVENTION against Alternaria leaf spot of cabbage (Alternaria brassicicola)
Per cent (%) Disease control (PDC)
Before Spray PDI 5 DAA 10 DAA 15 DAA
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 14.07 72.60 79.80 85.19
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 14.81 31.51 30.30 26.67
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 15.56 60.27 72.73 80.00
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 14.81 60.27 69.70 78.52
IE5 Acetamiprid 20% SP 300 gm 15.56 24.66 24.24 19.26
IE6 Pyriproxyfen 10% EC 1000 ml 14.07 19.18 22.22 17.78
IE7 Flutriafol 25% SC 575 ml 15.56 57.53 68.69 77.78
IE8 Control - 15.56 0.00 0.00 0.00
*PDI: Per cent Disease Index
Table 69: Synergistic effect of present invention composition against Alternaria leaf spot of Cabbage
S. no. Treatment details Dose (ml or gm/Ha) % Disease Reduction over control (PDC)
Observed Expected Ratio Synergy
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 85.19 79.92 1.09 Yes
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 26.67 33.61 0.79 No
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 80.00 81.73 0.98 No
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 78.52 82.06 0.96 No
IE5 Acetamiprid 20% SP 300 gm 19.26 0.00 0.00 0.00
IE6 Pyriproxyfen 10% EC 1000 ml 17.78 0.00 0.00 0.00
IE7 Flutriafol 25% SC 575 ml 77.78 0.00 0.00 0.00
IE8 Control - 0.00 0.00 0.00 0.00
Table 69 shows that the present invention composition Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% resulted in the highest efficacy, achieving percent disease control of 79.80% at 10 DAA and 85.19% at 15 DAA, thereby showing synergy as compared to other treatments.
Example 11: Evaluation of Phytotoxicity of synergistic composition comprising Acetamiprid, Pyriproxyfen, and Flutriafol in cotton & cabbage crop
Visual observations were recorded 7, 14, and 21 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below. A total of 20 plants per plot were observed.
Table 70: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
?Leaf injury on tips /surface? Rating
0%? 0?
1-10%? 1?
11-20%? 2?
21-30%? 3?
31-40%? 4?
41-50%? 5?
51-60%? 6?
61-70%? 7?
71-80%? 8?
81-90%? 9?
91-100%? 10?
Table 71: Phytotoxic effect of various treatments on cotton and cabbage crop after 7 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 575 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 72: Phytotoxic effect of various treatments on cotton and cabbage crop after 14 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 575 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 73: Phytotoxic effect of various treatments on cotton and cabbage crop after 21 DAA?at recommended dose
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 1250 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 300+1000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 1000+575 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 300 +575 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 300 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 1000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 575 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 74: Phytotoxic effect of various treatments on cotton and cabbage crop after 7 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 7 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 2000+1150 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 600 +1150 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 1150 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 75: Phytotoxic effect of various treatments on cotton and cabbage crop after 14 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 14 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 2000+1150 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 600 +1150 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 1150 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Table 76: Phytotoxic effect of various treatments on cotton and cabbage crop after 21 DAA?at double dose
S. No.? Treatment details? Dose Kg/ha? 21 DAA?
L? S? N? C? V? E? H? W?
IE1 Acetamiprid 4.8% + Pyriproxyfen 8% + Flutriafol 11.5% DC 2500 ml 0 0 0 0 0 0 0 0
IE2 Acetamiprid 20% SP + Pyriproxyfen 10% EC 600+2000 ml 0 0 0 0 0 0 0 0
IE3 Pyriproxyfen 10% EC+ Flutriafol 25% SC 2000+1150 ml 0 0 0 0 0 0 0 0
IE4 Acetamiprid 20% SP + Flutriafol 25% SC 600 +1150 ml 0 0 0 0 0 0 0 0
IE5 Acetamiprid 20% SP 600 gm 0 0 0 0 0 0 0 0
IE6 Pyriproxyfen 10% EC 2000 ml 0 0 0 0 0 0 0 0
IE7 Flutriafol 25% SC 1150 ml 0 0 0 0 0 0 0 0
IE8 Control - 0 0 0 0 0 0 0 0
*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?
Tables 71 to 76 above evidence that the application of Acetamiprid, Pyriproxyfen, and Flutriafol in all doses showed no phytotoxicity symptoms like leaf injury on tips, leaf injury on the surface, wilting, vein clearing, necrosis, epinasty and hyponasty in cotton and cabbage crop. Further, as evident from tables 74, 75 and 76, the application of Acetamiprid, Pyriproxyfen, and Flutriafol at even double doses shows no phytotoxicity. Thus, applying the present invention composition may be considered completely safe for crops.
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:We Claim:
1. A synergistic composition comprising:
a. acetamiprid;
b. pyriproxyfen; and
c. at least one triazole fungicide.
2. The synergistic composition as claimed in claim 1, wherein the triazole fungicide is selected from tebuconazole, flutriafol, propiconazole and difenoconazole.
3. The synergistic composition as claimed in claim 1, wherein:
a) acetamiprid in the range of 1 to 30% by weight of the composition;
b) pyriproxyfen in the range of 0.1 to 30% by weight of the composition;
c) at least one triazole fungicide in the range of 0.1 to 30% by weight of the composition; and
d) at least one agriculturally acceptable excipient.
4. The synergistic composition as claimed in claim 3, wherein the agriculturally acceptable excipient is selected from the group comprising a carrier, a binder, a disintegrating agent, dispersants or dispersing agent, a wetting agent, a pH modifier, a humectant, a thickener, a biocide, a preservative, an anti-freezing agent, a colorant, a defoamer, an emulsifier, a co-solvent, solvent or any combination thereof.
5. The synergistic composition as claimed in claim 4, wherein the emulsifier is present in an amount in the range of 0.1 to 20% by weight; the humectant is present in an amount in the range of 0.1 to 15% by weight; and the dispersant is present in an amount in the range of 0.1 to 15% by weight.
6. The synergistic composition as claimed in claim 4, wherein the emulsifier is selected from the group consisting of salts of dodecylbenzene sulphonate, e.g. Ca-salts or amine salts, and sulphonates of other C11-C16 alkylbenzenes, alkylether sulphates, alkylphenoletherphosphates and ester phosphates; non-ionic surfactants such as alkoxylated alcohols and alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, e.g. ethoxylated castor oil, fatty acid esters, e.g. of sorbitol, and their ethoxylated derivatives, ethoxylated amines, and condensates of glycerol; and catanionic emulsifiers such as a cationic amine, optionally in combination with an alkylsulphonate or ether sulphonate or ether phosphate, alkoxylated alcohols; alkoxylated alkylphenols; ethoxylated fatty acids; ethoxylated vegetable oils; ethoxylated tristyrylphenol; fatty acid esters of sorbitol and ethoxylated derivatives thereof; ethoxylated amines and condensates of glycerol; sulfonated alkylbenzenes in the range C11-C16 and salts thereof; alkylether sulphates; alkyletherphosphates; alkylphenoletherphosphates; or combinations thereof; salts of phosphate esters of ethoxylated tristyrylphenol; salts of sulphated ethers of ethoxylated tristyrylphenol; or a catanionic system, wherein a cationic amine is present in combination with an alkylsulphonate, an alkylethersulphonate, an ether sulphate, or an ether phosphate such as an alkyletherphosphate, nonylphenol polyethoxy ethanols, castor oil polyglycol ethers, polyadducts of ethylene oxide and polypropylene, tributyl phenoxy polyethoxy ethanol, octyl phenoxy polyethoxy ethanol or combination thereof;
the humectant is selected from the group consisting of urea, humic acid, glycerol, lactose or combination thereof; and
the dispersant is selected from the group consisting of acrylic graft copolymer, alcohols, C9-11-iso-, C10-rich, ethoxylated, tristyrylphenol ethoxylate phosphate ester, poly(oxy-1,2-ethanediyl), a-sulfo-?-[2,4,6-tris(1- phenylethyl)phenoxy]-, ammonium salt, poly(oxy-1,2-ethanediyl), a-phosphono-? 2,4,6-tris(1-phenylethyl)phenoxy-, alkoxylated alcohol, naphthalene and alkyl naphthalene sulphonic acids formaldehyde condensate, sodium salt, alkyl aryl ethylene oxide condensates, sodium lignosulphonates, sodium dibutylnaphthalenesulphonate, poly aryl phenyl ether phosphate, tristyryl phenol ethylated/ acrylic graft copolymer/ ethoxylated tristryl phenol sulphate, naphthalene sulfonic acid, sodium salt condensate with formaldehyde, ethoxylated oleyl cetyl alcohol, polyalkelene glycol ether, ethoxylated fatty alcohol, EO-PO block copolymers, graft copolymers or combination thereof.
7. The synergistic composition as claimed in claim 1 or 2, wherein the composition is in the form of a 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), Nano-emulsion, 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), and/or a mixed formulation of CS and EW (ZW).
8. A process for preparing a synergistic composition, comprising the steps of:
a) weighing and transferring a solvent and a co-solvent into a beaker;
b) dissolving acetamiprid in the solvents under continuous stirring at a controlled temperature between 45°C to 50°C to obtain a homogeneous solution;
c) cooling the solution to room temperature after the complete dissolution of acetamiprid;
d) adding pyriproxyfen and at least one triazole fungicide into the cooled mixture of step c) under ambient temperature and continuous stirring until uniform dissolution;
e) adding and mixing a dispersing agent, an emulsifier, a humectant and a colorant to the mixture of step (d); and
f) homogenizing the mixture of step (e) to obtain a stable emulsion.
9. The process as claimed in claim 8, wherein the triazole fungicide is selected from tebuconazole, flutriafol, propiconazole and difenoconazole.
10. The process as claimed in claim 8, wherein the emulsifier is present in an amount in the range of 0.1 to 20% by weight; the humectant is present in an amount in the range of 0.1 to 15% by weight; and the dispersing agent is present in an amount in the range of 0.1 to 15% by weight.
| # | Name | Date |
|---|---|---|
| 1 | 202411008694-STATEMENT OF UNDERTAKING (FORM 3) [08-02-2024(online)].pdf | 2024-02-08 |
| 2 | 202411008694-PROVISIONAL SPECIFICATION [08-02-2024(online)].pdf | 2024-02-08 |
| 3 | 202411008694-FORM 1 [08-02-2024(online)].pdf | 2024-02-08 |
| 4 | 202411008694-DECLARATION OF INVENTORSHIP (FORM 5) [08-02-2024(online)].pdf | 2024-02-08 |
| 5 | 202411008694-FORM-26 [12-02-2024(online)].pdf | 2024-02-12 |
| 6 | 202411008694-Proof of Right [14-03-2024(online)].pdf | 2024-03-14 |
| 7 | 202411008694-GPA-160224.pdf | 2024-03-20 |
| 8 | 202411008694-Correspondence-160224.pdf | 2024-03-20 |
| 9 | 202411008694-Others-210324.pdf | 2024-04-12 |
| 10 | 202411008694-Correspondence-210324.pdf | 2024-04-12 |
| 11 | 202411008694-CORRESPONDENCE-OTHERS [07-02-2025(online)].pdf | 2025-02-07 |
| 12 | 202411008694-COMPLETE SPECIFICATION [07-02-2025(online)].pdf | 2025-02-07 |
| 13 | 202411008694-FORM-9 [10-02-2025(online)].pdf | 2025-02-10 |
| 14 | 202411008694-FORM 18 [10-02-2025(online)].pdf | 2025-02-10 |
| 15 | 202411008694-Covering Letter [10-02-2025(online)].pdf | 2025-02-10 |
| 16 | 202411008694-FORM 18A [17-03-2025(online)].pdf | 2025-03-17 |
| 17 | 202411008694-FER.pdf | 2025-05-30 |
| 18 | 202411008694-Proof of Right [08-08-2025(online)].pdf | 2025-08-08 |
| 19 | 202411008694-OTHERS [08-08-2025(online)].pdf | 2025-08-08 |
| 20 | 202411008694-FER_SER_REPLY [08-08-2025(online)].pdf | 2025-08-08 |
| 21 | 202411008694-US(14)-HearingNotice-(HearingDate-25-11-2025).pdf | 2025-10-31 |
| 22 | 202411008694-RELEVANT DOCUMENTS [10-11-2025(online)].pdf | 2025-11-10 |
| 23 | 202411008694-POA [10-11-2025(online)].pdf | 2025-11-10 |
| 24 | 202411008694-FORM 13 [10-11-2025(online)].pdf | 2025-11-10 |
| 25 | 202411008694-Correspondence to notify the Controller [20-11-2025(online)].pdf | 2025-11-20 |
| 1 | 202411008694_SearchStrategyNew_E_searchstrategy-3E_21-05-2025.pdf |