DESC:FIELD OF THE INVENTION
The present invention relates to a stable synergistic agrochemical formulation. More particularly the present invention relates to a synergistic oil dispersion formulation comprising a) profenofos and b) an insecticide selected from acetamiprid or spinetoram. The present invention further relates to selection of suitable formulation excipients, process of preparation of the said oil dispersion formulation and its application in the field of agriculture.
BACKGROUND OF THE INVENTION
Crop protection is the practice of protecting the crop yields from pests, weeds, plant diseases, and other organisms that damage agricultural crops, which is critical from early stages of crop development. Preventing pests and diseases in the entire crop cycle, i.e., from root development to maturing crop, leads to increased crop quality and yield. The control of insects is extremely important in achieving high crop efficiency. Generally, insects are very destructive to crop plants and can significantly reduce crop yields and quality. Insecticides help to minimize this damage by controlling insect pests. For this purpose, in the field of agrochemical industry, numerous formulations are available for delivering active ingredients or combinations, but there is still a continues need to develop new insecticidal combinations which are more effective, less costly, less toxic, environmentally safer and have different sites of action. The use of two or more appropriate active ingredient combinations in specific dose ratios leads to synergism in crop protection.
Profenofos is a widely used organophosphate insecticide known for its contact and stomach action. It is particularly effective against chewing pests and mites in crops such as cotton, vegetables, and rice. Acetamiprid is a neonicotinoid insecticide that acts as an agonist of nicotinic acetylcholine receptors (nAChRs), providing systemic control of sucking pests like aphids, whiteflies, and jassids. Spinetoram, a derivative of the spinosyn class, exhibits a unique mode of action by targeting both nicotinic acetylcholine and GABA receptors, showing efficacy primarily against lepidopteran pests and thrips.
Formulations combining insecticides with complementary modes of action are known to provide broader pest control and help in resistance management. However, conventional formulations such as emulsifiable concentrates (EC), wettable powders (WP), and suspension concentrates (SC) can suffer from limitations such as poor physical stability, inadequate rain-fastness, and potential phytotoxicity. In particular, formulations based on water as the primary carrier may be less effective under certain environmental conditions or when dealing with hydrophobic active ingredients.
Oil dispersion (OD) formulations are a type of non-aqueous suspension in which active ingredients are dispersed in an oil phase. OD formulations are known to offer several advantages, including improved spreading, rain-fastness, reduced volatility, better penetration, and enhanced bioavailability of lipophilic compounds. They may also provide improved shelf life and better compatibility with hydrophobic active ingredients.
Despite these benefits, there is limited availability of stable OD formulations combining Profenofos with either Acetamiprid or Spinetoram. Challenges associated with such combinations include maintaining formulation stability, avoiding chemical degradation of active ingredients, and ensuring consistent biological performance.
There remains a need for the development of oil dispersion formulations that enable effective co-formulation of Profenofos with Acetamiprid or Spinetoram, offering acceptable physical and chemical stability, ease of application, and reliable insecticidal performance across different crop and pest scenarios.

OBJECTS OF THE INVENTION
The primary objective of the present invention is to provide a stable synergistic oil dispersion formulation comprising a) profenofos or agrochemically acceptable salt(s) thereof; and b) an insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof.
Another objective of the present invention is to provide a stable synergistic oil dispersion formulation comprising a) Profenofos or agrochemically acceptable salt(s) thereof; b) an insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof; and c) agriculturally acceptable auxiliaries.
Another object of the present invention is to provide an insecticidal composition that shows synergistic effect against pests.
Another object of the present invention is to provide an insecticidal composition that is stable.
Yet another object of the present invention is to provide a stable synergistic insecticidal formulation with oil(s), solvent(s), surfactant(s)/emulsifier(s), dispersing agent(s), or wetting agent(s) or combination thereof.
Another objective of the present invention is to process for the preparation of profenofos oil dispersion formulation comprising the steps of adding, stirring, milling, collecting, homogenizing and packaging.
Yet another object of the present invention is to provide a stable synergistic insecticidal formulation that has economic significance.
Yet another object of the present invention is to provide a stable synergistic insecticidal formulation that shows technical advancement over the existing insecticides or combination of insecticides.
Further objective of the present invention is to provide an insecticide mixture or combinations which solve at least one of the problems discussed above, like physical and chemical stability, ease of application, and reliable insecticidal performance or combining activity with prolonged insect control and resistance management.
SUMMARY OF THE INVENTION
The present disclosure pertains to the technical field of agricultural compositions and formulations. In particular, the present disclosure pertains to insecticidal compositions and formulations comprising compounds for controlling or preventing insect pests and disease/damages caused by insects in crops.
In an aspect, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof; and
An insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof.
In an aspect, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
An insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof; and
Agriculturally acceptable excipients.
In an aspect, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof is present in the range of 1 to 70% of total weight of composition;
An insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof is present in the range of 0.1 to 20% of total weight of composition; and
Agriculturally acceptable excipients is present in the range of 1 to 60% of total weight of composition.
In one embodiment, the present invention provides a process for the preparation of oil dispersion formulation, wherein the process comprising the steps of:
Step I: Charging and Premixing of Raw Materials
Charging and Premixing of Raw Materials: The required quantity of methylated soybean oil and aromatic solvent (naptha) was weighed and charged into a jacketed formulation vessel using a raw material charging pump.
Next, dispersing agents, wetting agents (e.g., polyalkylene oxide block copolymer and calcium salt of dodecylbenzene sulfonate), and a stabilizer (epoxidized soybean oil) were added to the vessel and stirred for an additional 30 minutes at a temperature maintained below 30?°C.
Subsequently, Profenofos technical was weighed and added slowly into the same vessel under continuous stirring. The mixture was agitated for approximately 30 minutes, maintaining the temperature below 30?°C to ensure uniform dispersion.
Following this, the required quantity of acetamiprid or spinetoram technical was charged in portions into the mixture under continuous agitation to prepare a uniform premix slurry. The slurry was stirred for about 30 minutes to ensure complete wetting and dispersion of the active ingredient.
Step II: Wet Milling Process
The premix slurry was passed through a bead mill containing zirconium beads (size: 1.2–1.4 mm; bulk density ~3.89 g/cm³), occupying approximately 60% of the mill volume. The slurry was subjected to high-shear wet milling until the desired particle size of d90 < 10 µm was achieved. Throughout the process, the temperature was maintained below 25?°C.
Once the target particle size was confirmed by quality control (QC) analysis, the material was transferred to a low-shear mixing vessel for final blending.
Step III: Post Mixing and Homogenization
The milled slurry of (profenofos 50% + Acetamiprid 6%) and (profenofos 50% + spinetoram 9%) was blended in the low-shear vessel. A premix of propylene glycol and styrenated phenol ethoxylate (APE-free, 54 moles) was prepared separately by slightly heating (not exceeding 50?°C) until liquefied. This mixture was then charged into the main vessel and homogenized thoroughly to obtain a uniform and physically stable OD formulation.
In another embodiment, the present invention provides a method for the management of the undesired insect pests or mites and/or phytopathogenic fungi and/or microorganisms, wherein said method comprises the applying oil dispersion according to the present invention to the insect pests or mites and/or phytopathogenic fungi and/or microorganisms.
In another aspect, the present disclosure provides a kit. The kit comprises a plurality of components comprising at least one of the ingredients of the insecticidal combination of the present disclosure.
Various objects, features, aspects, and advantages of the inventive subject matter will become more apparent from the following detailed description of preferred embodiments.
DESCRIPTION OF THE INVENTION
The present specification refers to a synergistic insecticidal composition for crop protection.

DEFINITIONS
The foregoing definitions provided herein for the terminologies used in the present disclosure are for illustrative purpose only and in no manner limit, the scope of the present invention disclosed in the present disclosure.
It will be understood that the terminology used herein is for the purpose of describing embodiments only and is not intended to be limiting. As used in this specification, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, the reference to "a surfactant" includes one or more of such surfactants.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one ordinary skilled in the art to which the invention pertains. Although other methods and materials similar, or equivalent, to those described herein can be used in the practice of the present invention, the preferred materials and methods are described herein.
The term “crop” shall include a multitude of desired plants or an individual 5 plant growing at a locus. As used herein, the term “plant” and “crop” have been used interchangeably throughout the present disclosure. Said term refers to all physical parts of a plant including foliage/leaves, seeds, seedlings, saplings, roots, tubers, stems, stalks, and fruits.
The term “control” or “controlling” or “prevent” or “preventing” a insect pests refers to inhibiting or reducing the growth, reducing the ability of insect pests to grow or reproduce or proliferate or spread, including killing (e.g., causing the morbidity or mortality, or reduced fecundity) of insects and insect eggs and larvae.
As used herein, the terms "comprises", "comprising", "includes", "including", or any other variation thereof, are intended to cover a non-exclusive inclusion, subject to any limitation explicitly indicated. For example, a composition or a method that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, or method.
As used herein, the terms "consisting of' or "consisting essentially of' or "consisting substantially of' are intended to cover a non-exclusive inclusion, subject to any limitation explicitly indicated. In these embodiments, the combination or composition described includes or comprises or consists of or consists essentially of or consists substantially of the specific components recited therein, to the exclusion of other insecticides or adjuvants or excipients not specifically recited therein.
As used herein, the term "composition" or "formulation" or “combination” or “mixture” can be used interchangeably, unless stated otherwise, is meant to encompass, and are not limited to, compositions or formulations containing the combination of profenofos,and acetamiprid or spinetoram.
As used herein, the term "additive(s)" or “agriculturally acceptable additives” or "auxiliaries" or "agriculturally acceptable carrier(s)" or “excipients” or “agriculturally acceptable excipients” can be used interchangeably and refers to inert substances which are commonly used as diluent, to provide stability or to increase the activity profile of the composition or formulation with or without having agrochemical activity.
As used herein, the term "surfactant(s)" means a compound that, when dissolved in a liquid, reduces the surface tension of the liquid, which reduces the interfacial tension between two liquids, or which reduces surface tension between a liquid and a solid.
As used herein, the term "stabilizer(s)" refers to a substance capable of imparting resistance against physical or chemical deterioration or deformulation.
As used herein, the term "biocide(s)" refers to a substance used to protect against unwanted plants, animals, or microorganisms.
As used herein, the term "defoaming agent(s)" refers to a chemical additive that reduces and hinders the formation of foam in the industrial process liquids, semi-solids, or solids. The terms defoaming agent and anti-foaming agent can be used interchangeably.
As used herein, the term "thickener(s)" refers to a polymeric material, which at a low concentration increases the viscosity of an aqueous solution and helps to stabilize the composition.
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. Unless otherwise specified, % refers to % weight; and % weight refers to % of the weight of the respective component with respect to the total weight of the composition.
The term “synergism” or “synergistic” as used in this specification refers to the interaction between two or more active compounds or other factors to produce a combined effect greater than the sum of their separate effects. The present invention involves the mixture of three active ingredients which has increased efficacy when compared to individual use and admixture of those components.
As used herein, the term "effective amount" means the amount of the active substances in the compositions to achieve an observable effect on growth, including the effects of necrosis, death, retardation, prevention, and removal, destruction, or otherwise diminishing the occurrence and activity of the target organism. The effective amount can vary for the various compositions used in the present invention. An effective amount of the compositions will also vary according to the prevailing conditions such as desired pesticidal effect and duration, weather, target species, locus, mode of application, and the like.
As used herein, the term “profenofos” encompasses profenofos or its agriculturally acceptable salt(s), derivative(s) or any other modified form of profenofos.
As used herein, the term “acetamiprid” encompasses acetamiprid or its agriculturally acceptable salt(s), derivative(s) or any other modified form of acetamiprid.
As used herein, the term “spinetoram” encompasses spinetoram or its agriculturally acceptable salt(s), derivative(s) or any other modified form of spinetoram.
As used herein, the term “% disease control” refers to the % control and prevention of a disease in crops.
Each of the aspects described above may have one or more embodiments.
Each of the embodiments described hereinafter may apply to one or all the aspects described hereinabove. These embodiments are intended to be read as being preferred features of one or all the aspects described hereinabove. Each of the embodiments described hereinafter applies to each of the aspects described hereinabove individually.
Conventional insecticides have typical spectrums and effects, which are limited to certain insects and their residual activities are sometimes poor and not satisfactorily maintained for prolonged period, and those satisfactory insecticidal effects cannot be practically achieved. Even though some insecticides may bear satisfactory insecticidal effects, they further require improvements in respect of environment and health safety and are also demanded to achieve a high insecticidal effect at a smaller dosage and lack resistance management.
In pursuit of the above, we found that this objective in part or totally can be achieved by the combination of active compounds defined at the outset. Moreover, it is observed that simultaneous application of active compounds jointly or separately or successive application of an active compound, one or more compounds enhanced insect control more than those of the individual active ingredients. The present inventors have intensively studied to solve these problems and found that by combining insecticide compositions having profenofos in different formulations and percentages have astonishing effects of controlling insects and by reducing amount of dosage than those of using an active compound alone.
In view of the above defined objectives, the present invention provides an oil dispersion formulation comprising a) profenofos or agrochemically acceptable salt(s) thereof; and b) an insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof.
In one embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
An insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof; and
Agriculturally acceptable excipients.
In an aspect of the present embodiment, the agriculturally acceptable excipients are selected from oil(s), solvent(s), surfactant(s)/emulsifier(s), dispersing agent(s), or wetting agent(s) or combination thereof.
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
Acetamiprid or agrochemically acceptable salt(s) thereof; and
Agriculturally acceptable excipients.
In an aspect of the present embodiment, the oil dispersion formulation of the present invention comprises profenofos or agrochemically acceptable salt(s) and acetamiprid or agrochemically acceptable salt(s), wherein the ratio of profenofos to acetamiprid is in the range from 1:100 to 100:1, preferably 1:50 to 50:1, more preferably 1:10 to 10:1.
In another aspect of the present embodiment, the oil dispersion formulation of the present invention comprises the content of profenofos is in the range of 1 to 70 % by weight of the total formulation, preferably 1 to 60% of total weight of formulation; more preferably 1to 55% of total weight of formulation; and the content of acetamiprid is in the range of 0.1 to 20 % by weight of the total formulation, preferably 0.1 to 15% of total weight of formulation, more preferably 0.1 to 10% of total weight of formulation.
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
Spinetoram or agrochemically acceptable salt(s) thereof; and
Agriculturally acceptable excipients.
In an aspect of the present embodiment, the oil dispersion formulation of the present invention comprises profenofos or agrochemically acceptable salt(s) and spinetoram or agrochemically acceptable salt(s), wherein the ratio of profenofos to spinetoram is in the range from 1:100 to 100:1, preferably 1:50 to 50:1, more preferably 1:10 to 10:1.
In another aspect of the present embodiment, the oil dispersion formulation of the present invention comprises the content of profenofos is in the range of 1 to 70 % by weight of the total formulation, preferably 1 to 60% of total weight of formulation; more preferably 1to 55% of total weight of formulation; and the content of spinetoram is in the range of 0.1 to 20 % by weight of the total formulation, preferably 0.1 to 15% of total weight of formulation, more preferably 0.1 to 10% of total weight of formulation.
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
Acetamiprid or agrochemically acceptable salt(s) thereof;
One or more oils and/or solvents;
One or more surfactant(s)/emulsifier(s);
One or more dispersing agent(s);
One or more wetting agent(s), and
Optionally agriculturally acceptable additives.
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
Spinetoram or agrochemically acceptable salt(s) thereof;
One or more oils and/or solvents;
One or more surfactant(s)/emulsifier(s);
One or more dispersing agent(s);
One or more wetting agent(s), and
Optionally agriculturally acceptable additives.
In yet another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof in the range of 1 to 70%;
Acetamiprid or agrochemically acceptable salt(s) thereof in the range of 0.1 to 20%;
One or more oils and/or solvents in the range of 1 to 80%;
One or more surfactant(s)/emulsifier(s) in the range of 0.1 to 30%;
One or more dispersing agent(s) in the range of 0.1 to 30%;
One or more wetting agent(s) in the range of 0.1 to 30%; and
Optionally agriculturally acceptable additives in the range of 0 to 75%.
In yet another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof in the range of 1 to 70%;
Spinetoram or agrochemically acceptable salt(s) thereof in the range of 0.1 to 20%;
One or more oils and/or solvents in the range of 1 to 80%;
One or more surfactant(s)/emulsifier(s) in the range of 0.1 to 30%;
One or more dispersing agent(s) in the range of 0.1 to 30%;
One or more wetting agent(s) in the range of 0.1 to 30%; and
Optionally agriculturally acceptable additives in the range of 0 to 75%.
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos : 50.00%
Acetamiprid: 6.00%
Amorphous silicon dioxide : 4.32%
Atlas™ G-5002 L (Polyalkylene oxide block copolymer) :7.00%
Rhodacal® 60BER (dodecylbenzene sulfonate calcium salt): 7.00%
(Makstab ESO/Unistab-P) Epoxidized soybean oil: 2.00%
Bentonite clay : 0.1%
Propylene Glycol (1,2-propanediol): 3.00%
Emthox PS 5400: 2.00%
Solvesso 150 (Solvent Naptha): 10.00%
Methylated soybean oil: Q.S to make
In another embodiment, the present invention provides a stable synergistic oil dispersion formulation comprising:
Profenofos : 50.00%
Spinetoram : 9.00%
Amorphous silicon dioxide : 4.32%
Atlas™ G-5002 L (Polyalkylene oxide block copolymer) :7.00%
Rhodacal® 60BER (dodecylbenzene sulfonate calcium salt): 7.00%
(Makstab ESO/Unistab-P) Epoxidized soybean oil: 2.00%
Bentonite clay : 0.1%
Propylene Glycol (1,2-propanediol): 3.00%
Emthox PS 5400: 2.00%
Solvesso 150 (Solvent Naptha): 10.00%
Methylated soybean oil: Q.S to make
The oil dispersion formulation of the present invention further comprises agriculturally acceptable additive(s) are selected from the group comprising solid carrier(s), liquid carrier(s), gaseous carrier(s), binder(s), disintegrating agent(s), pH adjuster(s), thickener(s), preservative(s), anti-caking agent(s), anti-freezing agent(s), defoaming agent(s), extender(s), stabilizer(s) and/or coloring agent(s) or a combination thereof. The formulation may also contain if desired, one or more other customary for crop protection formulations.
The oil(s) which can be used in the oil dispersion formulation of the present invention is selected from the group comprising of, but not limited to, Paraffinic hydrocarbons, petroleum oil or its derivatives, vegetable oil or its derivatives, seed oil or its derivatives, mineral oil or its derivatives, animal oil or its derivatives, plant oil or its derivatives, light paraffin oil or its derivatives, animal oil or derivatives, or a combination thereof. However, those skilled in the art will appreciate that it is possible to utilize other water immiscible solvents without departing from the scope of the present invention.
The mineral oil or petroleum oil can be selected from one or more oil of aliphatic or isoparaffinic series, mixtures of aromatic and aliphatic hydrocarbons, halogenated aromatic or aliphatic hydrocarbons. Paraffinic oil can be selected from linear or branched C8 to C30 paraffins e.g. such as octane, nonane, decane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, their mixtures, or mixtures thereof with higher boiling homologs, such as hepta-, octa-, nonadecane, eicosane, heneicosane, docosane, tricosane, tetracosane, pentacosane, and the branched chain isomers thereof, unsubstituted or substitutedaromatic or cycloaliphatic C7 to C18 hydrocarbon compounds such as mono- or polyalkylsubstituted benzenes, or mono- or polyalkyl-substituted naphthalenes, or transesterification products thereof, liquid esters of C1 to C12 alcohols such as butanol, n-octanol, ioctanol, dodecanoi, cyclopentanol, cyclohexanol, cyclooctanol, ethylene glycol or propylene glycol with C2 to C12 carboxylic or polycarboxylic acids, such as caproic acid, capric acid, caprylic acid, pelargonic acid, succinic acid and glutaric acid; or with aromatic carboxylic acids such as benzoic acid, toluic acid, salicylic acid and phthalic acid, liquid amides of Cl to C5 amines, alkylamines or alkanolamines with C6 to Cl8 carboxylic acids, or derivatives thereof. Esters which can be used in the oil dispersions of the invention are benzyl acetate, caproic acid ethyl ester, pelargonic acid ethyl ester, benzoic acid methyl or ethyl ester, salicylic acid methyl, propyl, or butyl ester, diesters of phthalic acid with saturated aliphatic or alicyclic C1 to C12 alcohols, such as phthalic acid dimethyl ester, dibutyl ester, diisooctyt ester, or liquid amides of C1-C3 amines, alkylamines or alkanolamines with C6 - C18 carboxylic acids or derivatives or mixtures thereof. However, those skilled in the art will appreciate that it is possible to utilize other mineral or pertroleum oils without departing from the scope of the present invention.
The vegetable oils can be one or more seed oil. The vegetable oils can also include one or more of soybean oil, methylated soybean oil, rape seed oil, olive oil, castor oil, sunflower seed oil, coconut oil, com oil, cotton seed oil, linseed oil, palm oil, peanut oil, safflower oil, sesame oil, kapok oil, papaya oil, camellia oil, rice bran oil, tung oil and the like; and esters of the above vegetable oils, or transesterification products thereof such as soybean oil methyl esters, ethyl esters, propyl esters, butyl esters or derivatives thereof. The animal oil can be one or more of whale oil, cod-liver oil, or mink oil. Preferably, the oil(s) present in an amount in the range from 1 to 80% w/w.
However, those skilled in the art will appreciate that it is possible to utilize other vegetable or animal oils without departing from the scope of the present invention.
The solvent(s) as used in the oil dispersion formulation of the present invention is selected from the group comprising, but not limited to, water and organic solvents such as saturated hydrocarbons such as pentane, hexane, heptane, octane, and cyclohexane, unsaturated hydrocarbons such as benzene, toluene, ethylbenzene, solvent C9 and xylene, carbon tetrachloride, chloroform, dichloromethane, chlorobutane, halogenated saturated hydrocarbons such as bromobutane, chloropentane, bromopentane, chlorohexane, bromohexane, chlorocyclohexane, bromocyclohexane, halogenated unsaturated hydrocarbons such as chlorobenzene, dichlorobenzene, trichlorobenzene, methanol, ethanol, propanol, isopropanol alcohols such as butanol and tert-butyl alcohol, carboxylic acids such as formic acid, acetic acid and propionic acid, dimethyl ether, diethyl ether and methyl-te ethers suchal as tert-butyl ether, tetrahydrofuran, tetrahydropyran, dioxane, etc., amines such as trimethylamine, triethylamine, N,N,N'N'-tetramethylethylenediamine, pyridine, N,N-dimethylformamide, N,Nexamples include amides such as dimethylacetamide, N,N-diethylacetamide, and N-methylmorpholine oxide, mixtures of aromatic and aliphatic hydrocarbons, such as solvents of the Solvesso series, e.g.Solvesso 100, Solvesso 150 or Solvesso 200 (ExxonMobil Chemicals), of the Solvarex/Solvaro series (TotalFinaElf) or of the Caromax series, e.g. Caromax 28 (Petrochem Carless). Further, include one or more of C2-C4-alkyl lactates, in particular from glycerin triacetate, ethyl lactate, n-propyl lactate and isopropyl lactate. In one embodiment solvent is selected from C6-C10-alkyl lactates, such as n-hexyl lactate, 1-ethylhexyl lactate, 1-methylhepytyl lactate, 1,3- dimethylhexyl lactate, 2-methylheptyl lactate, 2,4-dimethylhexyllactate, 2,2,4-trimethylpentyl lactate, n-octyl lactate, 2-ethylhexyl lactate, n-nonyl lactate, 1-methyloctyl lactate, 2-methyloctyl lactate, 1- methylnonyl lactate, 2-propylheptyl lactate and n-decyl lactate, 2,2,4- trimethylpentyl lactate, butyl lactate, isopropyl myristate, hexylene glycol, dioxane, d-limonene, a C1-C14 saturated straight-chain alcohol, isopropyl alcohol, 2-butanol, isobutyl alcohol, tertiary butyl alcohol, 2-butoxyethanol, 2- phenylethanol, diacetone alcohol, ?-butyrolactone, nitromethane, acetophenone, triacetin, pyridine, water, toluene, xylene, petroleum naphtha, crop oil, acetone, methyl ethyl ketone, cyclohexanone, acetic anhydride, acetonitrile, acetophenone, amyl acetate, 2-butanone, chlorobenzene, cyclohexane, cyclohexanol, alkyl acetates, diacetonalcohol, 1,2-dichloropropane, diethanolamine, pdiethylbenzene, abietate, diethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol methyl ether, N,N-dimethyl formamide, dimethyl sulfoxide, 1,4-dioxane, dipropylene glycol, dipropylene glycol methyl ether, dipropylene glycol dibenzoate, diproxitol, alkyl pyrrolidinone, ethyl acetate, 2-ethyl hexanol, ethylene carbonate, 1,1,1-trichloroethane, 2-heptanone, alpha pinene, dlimonene, ethylene glycol, ethylene glycol butyl ether, ethylene glycol methyl ether, gammabutyrolactone, glycerol, glycerol diacetate, glycerol monoacetate, glycerol triacetate, hexadecane, hexylene glycol, isoamyl acetate, isobornyl acetate, isooctane, isophorone, isopropyl benzene, isopropyl myristate, lactic acid, laurylamine, mesityl oxide, methoxy-propanol, methyl isoamyl ketone, methyl isobutyl ketone, methyl laurate, methyl octanoate, methyl oleate, methylene chloride, m-xylene, n-hexane, n-octylamine, octadecanoic acid, octyl amine acetate, oleic acid, oleylamine, oxylene, phenol, polyethylene glycol (PEG400), propionic acid, propylene glycol, propylene glycol monomethyl ether, p-xylene, toluene, triethyl phosphate, triethylene glycol, xylene sulfonic acid, paraffin, mineral oil, trichloroethylene, perchloroethylene, ethyl acetate, amyl acetate, butyl acetate, methanol, ethanol, isopropanol, and higher molecular weight alcohols such as amyl alcohol, tetrahydrofurfuryl alcohol, hexanol, octanol, etc. ethylene glycol, propylene glycol, glycerine, Nmethyl-2-pyrrolidinone, and the like. The green solvent may include any solvent which is naturally occurring and which has been found not harm the environment when used on an industrial scale. The green solvent may include water, glycerin triacetate, ethyl lactate or an alcohol based solvent (e.g., ethanol). Any of the above mentioned solvent can be used either alone or combination thereof.
The solvent C9 is aromatic hydrocarbon solvent which is comprised of a petroleum naphtha refinery stream, "solvent naphtha (petroleum), light aromatic", from which the other, more chemically pure members of this category are isolated. Preferably, the solvent present in an amount in the range from 1 to 80% w/w.
The surfactant(s)/emulsifiers as used in the oil dispersion formulation of the present invention is a nonionic or anionic surfactants or a combination of these surfactants. It is preferred to use one or more than one kind of surfactant. The surfactant(s) is selected from the group comprising, but not limited to, sugar esters such as sorbitan monolaurate, polyoxyethylene sorbitan monolaurate; C1-C30 alkylcarboxylate, C1-C20 hydroxyalkylcarboxylate, polymer containing carboxylate, arylcarboxylate, alkylx (e.g. aliphatic di- and tricarboxylates) having 2 to 32 carbon atoms, such as aconitic acid, adipic acid, aspartic acid, citric acid, fumaric acid, galactaric acid, glutamic acid, glutaric acid, oxoglutaric acid, maleic acid, malic acid, malonic acid, oxalate, sebacic acid, succinic acid, tartaric acid; alkyl polyglucoside such as decyl glucoside; polyoxyethylene alkyl ethers such as polyoxyethylene lauryl ether, or polyoxyethylene coconut fatty alcohol ether; polyoxyethylene alkynyl ether such as polyoxyethylene 2,4,7,9-tetramethyl-5-decyn-4,7-diol ether; polyoxyethylene aryl ethers such as polyoxyethylene nonylphenyl ether or polyoxyethylene tristyrylphenyl ether; polyoxyethylene vegetable oil ethers such as polyoxyethylene castor oil or polyoxyethylene hydrogenated castor oil; vegetable oil ethoxylate; natural or synthetic ethoxylated fatty alcohols, natural or synthetic, ethoxylated and propoxylated fatty alcohols, ethoxylated and propoxylated shortchain alcohols, C6-C20 linear and branched alcohol ethoxylates, C6-C20 alcohol propoxylates, C6-C20 ethoxylated alcohols, C6-C20 propoxylated alcohols; ethoxylated fatty acids, ethoxylated castor oil, ethoxylated sorbitan esters, ethoxylated esterified sorbitols, ethoxylated alkylphenols, ethoxylated tristyrylphenols and ethoxylated fatty amines, polyoxyethylene fatty acid esters such as polyoxyethylene monolaurate, polyoxyethylene distearate or polyoxyethylene resin acid ester; polyoxyethylene polyoxypropylene (EO-PO) block copolymers such as Pluronic; polyoxyethylene polyoxypropylene alkyl ether such as polyoxyethylene polyoxypropylene lauryl ether; polyoxyethylene polyoxypropylene aryl ether such as polyoxyethylene polyoxypropylene styrylphenyl ether; a modified styrene acrylic polymer, polyoxyethylene alkyl amines such as polyoxyethylene stearyl amine; polyoxyethylene fatty acid amide such as lauric acid diethanolamid; fluorinated surfactant; alkyl sulfates such as sodium lauryl sulfate; sodium alkylbenzene sulfonate, calcium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates such as sodium polyoxyethylene lauryl ether sulfate; polyoxyethylene aryl ether sulfates such as sodium polyoxyethylene nonylphenyl ether sulfate or ammonium polyoxyethylene tristyrylphenyl ether sulfate; aryl sulfonate such as calcium benzene sulfonate calcium dodecyl benzene sulfonate, sodium naphthalene sulfonate, sodium salt of naphthalene sulfonate condensate (MORWET D-425) or sodium naphthalene sulfonate formaldehyde condensate; poly aryl phenyl ether sulphate ammonium salt; 'alpha'-olefin sulfonate; lauryl sulfosuccinate, laureth sulfosuccinate, laureth-5 sulfosuccinate, al ricinoleamide MEA sulfosuccinate, undecylenearnide MEA sulfosuccinate, diisobutyl sulfosuccinate, dioctyl sulfosuccinate, dihexyl sulfosuccinate, dicyclohexyl sulfosuccinate, diisodecyl sulfosuccinate, diisotridecyl sulfosuccinate, di-2-ethylhexyl sulfosuccinate, di-2-methylamyl sulfosuccinate, dimethylamyl sulfosuccinate, dibutylhexyl sulfosuccinate, diisooctyl sulfosuccinate or their alkali metal salts, sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates such as polyoxyethylene phenyl ether phosphate; polyoxyethylene alkyl phenyl ether phosphate; graft copolymers such as polymethyl methacrylate-polyethylene glycol graft copolymer. These surfactants may be used alone or combination thereof.
The suitable stabilizing surfactants include anionic, cationic, nonionic and amphoteric surfactants, block polymers and polyelectrolytes. Further on, polysaccharide (e.g. starch, starch derivatives, cellulose derivatives, xanthan gum, and gelatin) may be used as stabilizing surfactants. Preferred stabilizing surfactants are nonionic surfactants (preferably alkoxylates, such as comb polymers) and/or block polymers, and EO-PO block copolymers. Mixtures of aforementioned stabilizing surfactants are also suitable. On the other hand, surfactants may act as detergents, wetting agents, emulsifiers, foaming agents, dispersants, spreader, adjuvant for penetration enhancement, rain fastness, or soil leaching control etc. Preferably, the surfactant(s)/emulsifiers present in an amount in the range from 0.1 to 30% w/w.
The wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading.
The wetting agent(s) as used in the oil dispersion formulation of the present invention is selected from the group comprising, but not limited to, one or more of dioctyl sulfosuccinate, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether sulfonates, non-ionic ethoxylated, ethoxylated polyarylphenol, dialkylsuccinate, sodium blend of alkyl naphthalene sulfonate, sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate, naphthalene alkyl aryl sulphonate, dioctyl sulfosuccinate, sodium dioctyl sulphosuccinate, sodium lauryl sulfonate, phosphate ester, sodium alkyl naphthalene sulfonate, ethylene oxide/propylene oxide block copolymer, polyarylphenyl ether phosphate, ethoxylated fatty alcohol, or combination thereof. Preferably, the wetting agent(s) are selected from EO-PO block copolymer, Atlox 4914, and Genapol PF 40. Preferably, the wetting agent(s) present in an amount in the range from 0.1 to 30% w/w.
The dispersing agent(s) as used in the oil dispersion formulation of the present invention is selected from the group comprising, but not limited to, one or more polycarboxylates, alkyl naphthalene sulfonates, naphthalene sulphonate derivative, naphthalene sulfonate of formaldehyde condensate, phenol sulphonic acid condensates, ligno sulphonates, methyl oleyl taurates, silica poly ether copolymer and poly vinyl alcohols, sodium salt of naphthalene sulfonate condensate, atloxal Metasperse 550S, mixture of salt of naphthalene sulphonic acid and phenol sulphonic acid condensate, sulfonated aromatic polymer, sodium salt preferably sodium salt of naphthalene sulfonate condensate, castor oil ethoxylate. Further, includes combination of low HLB and high HLB surfactants selected from ethylene oxide propylene oxide block polymers, poly alkaline glycol ether (Atlox 1400, Atlox 1500), calcium dodecyl benzene sulfonate (Rhodocal 60BER), tristyrylphenol ethoxylate (Sophrophor BSU), blends of linear calcium sulfonate and non-alkylphenol non-ionic surfactants (Toximul 3479F), butyl polyalkylene oxide block copolymer (Toximul 8320), acrylic copolymer, graft copolymer, lignin based sulfonate, amine salt of phosphate tristyryl phenol ethoxylated copolymer condensate of ethylene and propylene oxide (Atlox 4894), copolymer condensate of ethylene oxide with methyl methacrylate (Atlox 4913), polyalkylene oxide block copolymer (Atlox G-5000), polyalkylene oxide block copolymer (Atlox G5002L), alkylphenol polyglycol ethers, tristryrylphenol polyglycol ethers, phosphated or sulphated derivatives of these, nonionic random polymeric (Atlox 4914), calcium alkyl benzene sulphonate in 2-ethylhexanol (Calsogen 4814), n-C12 alkyl benzene sulfonate calcium salt, n-C12 alkyl benzene sulfonate calcium salt (Phenylsulfonat CAL) and calcium dodecyl benzene sulphonated (Rhodocal 60 BER), preferably poly alkaline glycol ethers. Preferably, the dispersing agent(s) are selected from Emthox PS 5400, Atlox 4912, and Atlox Metasperse 550S. Preferably, the dispersing agent(s) present in an amount in the range from 0.1 to 30% w/w.
The stabilizer(s) as used in the oil dispersion formulation of the present invention is selected from the group comprising, but not limited to, drying agent such as zeolite, quick lime or magnesium oxide; antioxidant agent such as phenol type, amine type, sulfur type or phosphorus type; or ultraviolet absorber such as salicylic acid type or a benzophenone type; or methylated soybean oil, epoxidized soybean oil; or peroxide compounds such as hydrogen peroxide and organic peroxides, alkyl nitrites such as ethyl nitrite and alkyl glyoxylates such as ethyl glyoxylate, zeolite, Butylated hydroxytoluene (BHT), Butylated hydroxyanisole (BHA), Tocopherols, antioxidants such as phenol compounds, phosphoric acid compounds and the like; ultraviolet absorbers such as benzophenone compounds or derivatives thereof. However, those skilled in the art will appreciate that it is possible to utilize other conventionally known stabilizers without departing from the scope of the present invention. These stabilizers may be used alone or in combination thereof.
As used herein, the term "thickener" or "rheology modifier" refers to a polymeric material, which at a low concentration increases the viscosity of an aqueous solution and helps to stabilize the composition.
The thickener(s) is selected from the group comprising of, but not limited to, water-soluble polymer and inorganic fine powder, wherein water-soluble polymer such as xanthan gum, welan gum, guar gum, polyvinyl alcohol, carboxymethylcellulose, polyvinylpyrrolidone, carboxyvinyl polymer, acrylic polymer, starch derivative or polysaccharide; or an inorganic fine powder selected from high purity silica, bentonite, white carbon, Amorphous silicon dioxide. These thickeners may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises xanthan gum as thickener. The thickener is present in an amount in the range from 0.01 to 3.0% w/w.
Anti-freezing agent used herein for present Oil dispersion (OD) formulation include but not limited ethylene glycol, propane diols, glycerine or the urea, glycol (Monoethylene glycol, Diethylene glycol, Polypropylene glycol, Polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate, sodium chloride.
Rheology modifiers as used herein includes but are not limited to organic derivative of a hectorite clay (like Benton 38, Benton 27, Benton 1000), xanthan gum, vegetable oil derivatives such as blend of vegetable oil base (SURFOM ESP 8105), guar gum, locust bean gum, carrageenan, alginates, methyl cellulose, carboxyethyl sodium carboxymethylcellulose, hydroxyethyl cellulose, modified starches; other polysaccharides and modified polysaccharides, polyethylene alcohol, glycerol alkyl resins and cellulose derivatives, natural oils, mineral oils such as kyros oil and the fumed silicas such as Aerosil R974, Aerosil 200, Aerosil 972, Aerosil R816, Aerosil 300 etc.
As used herein, the term "defoaming agent" or "defoamer" or "anti-foaming agent" refers to an excipient that reduces and hinders the formation of foam in the liquid, semi-solid, or solid formulations.
The defoamer(s) is selected from the group comprising of, but not limited to, silicone compounds such as dimethyl polysiloxane emulsion and organic fluorine compounds. These defoaming agents may be used alone or in combination thereof. Preferably, the synergistic insecticidal composition comprises dimethyl polysiloxane emulsion as defoamer. The defoamer is present in an amount in the range from 0.01 to 2.0% w/w.
As used herein, the term "biocide" refers to an agent that prevents spoilage from bacteria, yeasts and fungi.
Biocide is selected from the group comprising of, but not limited to, 20% aqueous dipropylene glycol solution of 1,2-benzisothiazolin-3-one (Proxel GXL), formaldehyde, isothiazolinone or a combination thereof. The biocide is added to the composition of the present invention for its preservation against spoilage from bacteria, yeasts and fungi. The biocide is present in an amount in the range from 0.01 to 0.50% w/w.
The liquid carrier(s) is selected from the group comprising, but not limited to, water; alcohols such as ethanol, propanol, butanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, benzyl alcohol, glycerin; polyol ethers such as ethylene glycol monopropyl ether, diethylene glycol monomethyl ether, dipropylene glycol dimethyl ether; ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone; ethers such as dipropyl ether, dioxane, tetrahydrofuran, aliphatic hydrocarbons such as normal paraffin, isoparaffin, kerosene, mineral oil; aromatic hydrocarbons such as xylene, toluene, naphthene, solvent naphtha, solvent C9, solvent C10, solvent C12, solvesso 100, solvesso 150, solvesso 200; chlorinated aliphatic or aromatics hydrocarbons such as chlorobenzene, chloroethylene, methylene chloride; esters such as ethyl acetate, diisopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gammabutyrolactone, gamma-valerolactone, epsilon-caprolactone; amides such as dimethylformamide, Nmethylpyrrolidone, N-octylpyrolidone, N,N-dimethyldecanamide; nitriles such as acetonitrile; organosulfur compound such as dimethyl sulfoxide; vegetable oils such as soybean oil, rapeseed oil, cotton seed oil. These liquid carriers may be used alone or in combination.
The gaseous carrier(s) is selected from the group comprising, but not limited to, liquefied petroleum gas, air, nitrogen, carbon dioxide or dimethyl ether. These gaseous carriers may be used alone or in combination thereof.
The penetrant(s) as used in the oil dispersion formulation of the present invention is selected from the group comprising, but not limited to, one or more of alcohol, glycol, glycol ether, ester, amine, alkanolamine, amine oxide, quaternary ammonium compound, triglyceride, fatty acid ester, fatty acid ether, N-methyl pyrrolidone, dimethylformamide, dimethyl acetamide, dimethyl sulfoxide, polyoxyethylenetrimethylolpropanemonooleate, polyoxyethylenetrimeth ylolpropanedioleate, polyoxyethylenetrimethylolpropanetrioleate, polyoxyethylenesorbitanmonooleate, polyoxyethylene sorbitol hexaoleate and methylated soybean oil. However, those skilled in the art will appreciate that it is possible to utilize different penetrants without departing from the scope of the present invention.
In one embodiment, the present invention provides a process for the preparation of an oil dispersion formulation, wherein the process comprising the steps of:
(a) mixing surfactant(s)/emulsifier(s), dispersing agent(s), wetting agent(s), and optionally agrochemically acceptable additives to oils and/or solvents or combination thereof with continuous stirring to form a homogeneous mixture;
(b) adding profenofos or agrochemically acceptable salt(s) thereof to the above homogeneous mixture obtained in step (a) with constant stirring to form a homogeneous mixture;
(c) adding acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof to the above homogeneous mixture obtained in step (b) with constant stirring to form a homogeneous mixture; and
(d) adding the remaining oils and/or solvent or combination thereof with constant stirring till a homogeneous mass obtained.
The formulations this way produced show excellent storage stability properties regarding physiochemical parameters, including stability of the active ingredients, reduced bleeding, and complete redispersibility.
The present invention further provides an oil dispersion (OD) formulation of profenofos or agrochemically acceptable salt(s) thereof and acetamiprid or agrochemically acceptable salt(s) thereof for the control of a wide variety of undesired insect pests.
The present invention further provides an oil dispersion (OD) formulation of profenofos or agrochemically acceptable salt(s) thereof and spinetoram or agrochemically acceptable salt(s) thereof for the control of a wide variety of undesired insect pests.The composition exhibits enhanced insecticidal efficacy through synergistic interaction, providing broad-spectrum control against chewing, sucking, caterpillar, and borer pests in crops such as cotton, vegetables, cereals, and pulses.
The oil dispersion formulation of the present invention also provides a nonagronomic (other than field crops) application such as application on horticultural crops (e.g., greenhouse, nursery or ornamentalal plants not grown in a field), residential, commercial and industrial structures, turf (e.g., sod farm, pasture, golf course, lawn, sports field, etc.).
In one embodiment, the oil dispersion (OD) formulation disclosed herein is employed for the control of a broad spectrum of harmful pathogens, insect pests, and mites, and offers several significant advantages, such as:
The ability to manage a wider array of pest and disease pressures, including those requiring insecticidal, fungicidal, or acaricidal intervention;
Enabling a single, uniform application of the formulation rather than requiring separate treatments with insecticides and fungicides;
Enhancing crop health outcomes in comparison to the effects observed with individual or sequential applications of insecticides and fungicides;
Providing prolonged residual activity following application.
Additionally, the OD formulation of the present invention exhibits enhanced storage stability and extended shelf life due to its water-free, oil-based composition, which prevents hydrolytic degradation of the active ingredients. As a foliar spray, this formulation adheres better to plant surfaces, leading to improved rain-fastness which is a critical feature for agricultural pesticides used in variable environmental conditions.
In another embodiment, the invention provides an OD formulation that demonstrates improved efficacy against target pests and pathogens when compared to the performance of the individual actives alone. This formulation is also effective for promoting plant health when applied to crops, crop parts, propagation materials, or to the sites where these are cultivated.
In some embodiments, the insecticidal OD formulation for controlling or preventing insects and insect eggs and larvae.
In yet another embodiment, the OD formulation is particularly effective for controlling a wide variety of insect pests, mites, and pathogenic organisms in numerous crop types. These include cereals (such as wheat, rice, barley, triticale, oats, mushrooms), root crops (e.g., sugar beet, fodder beet), fruit crops (e.g., apples, apricots, pears, plums, peaches, cherries, strawberries, raspberries, blackberries, and others), legumes (such as lentils, peas, soybeans, and alfalfa), oilseed crops (e.g., canola, mustard, sunflower, olive, palm, coconut, castor), cucurbits (e.g., melons, cucumbers, squashes), fiber crops (e.g., cotton, flax, jute), citrus fruits (e.g., oranges, lemons, mandarins), vegetables (e.g., spinach, lettuce, tomatoes, cabbage, okra, carrots, onions, potatoes, peppers), lauraceous crops (e.g., avocado, camphor), energy crops (e.g., sugarcane, corn), as well as other economically important plants including tobacco, coffee, tea, bananas, grapes, hops, stevia, natural rubber, ornamental plants, and forest species. It is also suitable for use on plant propagation materials such as seeds and crop harvests.
In one embodiment, the method of combating harmful fungi depending on the type of compound and the desired effect, the application rates of the mixture of according to the invention are preferably from 5 to 1000 g/ha, most preferably from 10 to 750 g/ha, in particular from 20 to 500 g/ha.
In preferred embodiment, the method of combating pests (insects, acarids or nematodes) depending on the type of compound and the desired effect, the application rates of the mixture according to the invention are from, preferably from 20 to 1000 g/ha, more preferably from 10 to 750 g/ha, in particular from 20 to 500 g/ha.
In an embodiment, the present invention provides a method for improving crop health (phyto-tonic effect), comprising treating a plant with an pesticidally effective amount of oil dispersion formulation of the present invention. The oil dispersion formulation of the present invention also widens the spectrum and said to have longer residual effect against undesired pathogenic microorganisms, insect pests and mites. The oil dispersion formulation is also able to increase plant health.
The OD formulation described herein offers multiple additional benefits, including:
Enhanced performance compared to conventional formulations evaluated during trials;
Economic advantages for growers through increased yields and reduced number of applications;
Decreased occupational exposure risks to farmers, as fewer sprays are required;
Improved formulation stability during storage;
Absence of phytotoxic effects;
Reduced spraying frequency, leading to lower water consumption.
The insecticidal combinations of the present disclosure may be provided as a kit of parts such that individual insecticides of the kit may be tank mixed, alone or together, before spraying. In some embodiments, the kit of parts may contain profenofos, at least one insecticide selected from Acetamiprid, spinetoram, such that the 2 components may be tank mixed, alone or together, before spraying.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
EXAMPLES
The present invention is further illustrated by the following examples. These examples describe possible preferred embodiments for illustrative purposes only, but they do not limit the scope of the invention. Certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention. These laboratory scale experiments can be scaled up to industrial/ commercial scale.

Example 1: Oil Dispersion of Profenofos and Acetamiprid
Component Name Content (% w/w)
Profenofos (Active ingredient) 50.00%
Acetamiprid (Active ingredient) 6.00%
Amorphous silicon dioxide 4.32%
Atlas™ G-5002 L (Polyalkylene oxide block copolymer) 7.00%
Rhodacal® 60BER (dodecylbenzene sulfonate calcium salt) 7.00%
(Makstab ESO/Unistab-P) Epoxidized soybean oil 2.00%
Bentonite clay 0.1%
Propylene Glycol (1,2-propanediol) 3.00%
Emthox PS 5400 (Styrenated phenol ethoxylate with 54 moles of ethylene oxide) 2.00%
Solvesso 150 (Solvent Naptha) 10.00%
Methylated soybean oil Q.S to make
Total 100% w/w
Example 2: Oil Dispersion of Profenofos and Spinetoram
Component Name Content (% w/w)
Profenofos (Active ingredient) 50.00%
spinetoram (Active ingredient) 9.00%
Amorphous silicon dioxide 4.32%
Atlas™ G-5002 L (Polyalkylene oxide block copolymer) 7.00%
Rhodacal® 60BER (dodecylbenzene sulfonate calcium salt) 7.00%
(Makstab ESO/Unistab-P) Epoxidized soybean oil 2.00%
Bentonite clay 0.1%
Propylene Glycol (1,2-propanediol) 3.00%
Emthox PS 5400 (Styrenated phenol ethoxylate with 54 moles of ethylene oxide) 2.00%
Solvesso 150 (Solvent Naptha) 10.00%
Methylated soybean oil Q.S to make
Total 100% w/w

EXAMPLE 3: Manufacturing process of Profenofos 50% + Acetamiprid 6% Oil dispersion (OD) formulation:
Active ingredients profenofos and acetamiprid were weighed as per Example 1.
Step I: Charging and Premixing of Raw Materials
The required quantity of methylated soybean oil and aromatic solvent (naptha) was weighed and charged into a jacketed formulation vessel using a raw material charging pump.
Next, dispersing agents, wetting agents (e.g., polyalkylene oxide block copolymer and calcium salt of dodecylbenzene sulfonate), and a stabilizer (epoxidized soybean oil) were added to the vessel and stirred for an additional 30 minutes at a temperature maintained below 30?°C.
Subsequently, Profenofos technical was weighed and added slowly into the same vessel under continuous stirring. The mixture was agitated for approximately 30 minutes, maintaining the temperature below 30?°C to ensure uniform dispersion.
Following this, the required quantity of Acetamiprid technical was charged in portions into the mixture under continuous agitation to prepare a uniform premix slurry. The slurry was stirred for about 30 minutes to ensure complete wetting and dispersion of the active ingredient.
Step II: Wet Milling Process
The premix slurry was passed through a bead mill containing zirconium beads (size: 1.2–1.4 mm; bulk density ~3.89 g/cm³), occupying approximately 60% of the mill volume. The slurry was subjected to high-shear wet milling until the desired particle size of d90 < 10 µm was achieved. Throughout the process, the temperature was maintained below 25?°C.
Once the target particle size was confirmed by quality control (QC) analysis, the material was transferred to a low-shear mixing vessel for final blending.
Step III: Post Mixing and Homogenization
The milled slurry of Profenofos 50% + Acetamiprid 6% was blended in the low-shear vessel. A premix of propylene glycol and styrenated phenol ethoxylate (APE-free, 54 moles) was prepared separately by slightly heating (not exceeding 50?°C) until liquefied. This mixture was then charged into the main vessel and homogenized thoroughly to obtain a uniform and physically stable OD formulation.
EXAMPLE 4:
Manufacturing process of Profenofos 50% + spinetoram 9% Oil dispersion (OD) formulation:
Active ingredients profenofos and spinetoram were weighed as per Example 2.
Step I: Charging and Premixing of Raw Materials
The required quantity of methylated soybean oil and aromatic solvent (naptha) was weighed and charged into a jacketed formulation vessel using a raw material charging pump.
next, dispersing agents, wetting agents (e.g., polyalkylene oxide block copolymer and calcium salt of dodecylbenzene sulfonate), and a stabilizer (epoxidized soybean oil) were added to the vessel and stirred for an additional 30 minutes at a temperature maintained below 30?°C.
Subsequently, Profenofos technical was weighed and added slowly into the same vessel under continuous stirring. The mixture was agitated for approximately 30 minutes, maintaining the temperature below 30?°C to ensure uniform dispersion.
Following this, the required quantity of spinetoram technical was charged in portions into the mixture under continuous agitation to prepare a uniform premix slurry. The slurry was stirred for about 30 minutes to ensure complete wetting and dispersion of the active ingredient.
Step II: Wet Milling Process
The premix slurry was passed through a bead mill containing zirconium beads (size: 1.2–1.4 mm; bulk density ~3.89 g/cm³), occupying approximately 60% of the mill volume. The slurry was subjected to high-shear wet milling until the desired particle size of d90 < 10 µm was achieved. Throughout the process, the temperature was maintained below 25?°C.
Once the target particle size was confirmed by quality control (QC) analysis, the material was transferred to a low-shear mixing vessel for final blending.
Step III: Post Mixing and Homogenization
The milled slurry of Profenofos 50% + spinetoram 9% was blended in the low-shear vessel. A premix of propylene glycol and styrenated phenol ethoxylate (APE-free, 54 moles) was prepared separately by slightly heating (not exceeding 50?°C) until liquefied. This mixture was then charged into the main vessel and homogenized thoroughly to obtain a uniform and physically stable OD formulation.
Example 5: Stability Study of Profenofos 50% + Spinetoram 9% OD Formulation
The oil dispersion formulation comprising Profenofos 50% w/w and Spinetoram 9% w/w demonstrated excellent physical and chemical stability under various storage conditions. The formulation retained its active ingredient content, viscosity, particle size, and physical homogeneity over a prolonged period. It exhibited no significant degradation, crystallization, or phase separation. These results indicate that the composition is suitable for commercial use and storage, maintaining its efficacy and application characteristics, including redispersibility, rain-fastness, and shelf stability.

Stability Data Table:
Test Condition Test Interval Appearance Profenofos (% w/w) Spinetoram (% w/w) pH (1% aq.) Viscosity (cP @25°C) Particle Size d90 (µm) Remarks
25?±?2°C (Ambient) Initial (0 M) Homogeneous, free flowing 50.00 9.00 6.5 550 7.5 Within specification
25?±?2°C (Ambient) 3 Months No separation 49.8 8.9 6.4 555 7.6 Stable
25?±?2°C (Ambient) 6 Months No change 49.6 8.8 6.3 560 7.7 Stable
54?±?2°C (Accelerated) 14 Days Slight thickening 49.5 8.7 6.1 600 8.0 Acceptable, stable under stress
54?±?2°C (Accelerated) 21 Days Slight separation* 49.3 8.6 6.0 615 8.2 Redispersible, no adverse change
54?±?2°C (Accelerated) 30 Days Slight separation 49.1 8.5 5.9 620 8.4 Acceptable
0–5°C (Cold Storage) 7 Days No crystallization 49.9 8.9 6.4 540 7.5 Passed cold stability test
The oil dispersion (OD) formulation comprising Profenofos 50% w/w and Spinetoram 9% w/w demonstrates excellent physicochemical stability under both ambient and accelerated storage conditions. The formulation retains its homogeneity, active ingredient integrity, and dispersibility, with no significant changes in viscosity, pH, or particle size distribution over time. The OD system, being water-free and oil-based, effectively enhances the shelf-life and rain-fastness of the active ingredients while maintaining redispersibility and consistent field performance. These results affirm the robustness and commercial viability of the formulation for broad-spectrum pest management in various crops, offering improved user safety, reduced application frequency, and enhanced crop protection.
Example 6: Stability Study of Profenofos 50% + Acetamiprid 6% OD Formulation
The oil dispersion formulation comprising Profenofos 50% w/w and Acetamiprid 6% w/w exhibited robust stability across ambient, accelerated, and cold storage conditions. The physical and chemical integrity of the formulation remained intact, showing no signs of phase separation, active ingredient degradation, or adverse changes in viscosity and particle size. These results confirm the formulation’s suitability for extended storage and field application, with additional benefits of enhanced residual activity, rain-fastness, and plant safety.
Stability Data Table:
Test Condition Test Interval Appearance Profenofos (% w/w) Acetamiprid (% w/w) pH (1% aq.) Viscosity (cP @25°C) Particle Size d90 (µm) Remarks
25?±?2°C (Ambient) Initial (0 M) Homogeneous, free flowing 50.00 6.00 6.7 545 7.4 Within specification
25?±?2°C (Ambient) 3 Months No separation 49.8 5.9 6.6 550 7.5 Stable
25?±?2°C (Ambient) 6 Months No change 49.6 5.8 6.5 555 7.6 Stable
54?±?2°C (Accelerated) 14 Days Slight thickening 49.4 5.7 6.3 595 7.9 Acceptable, stable under stress
54?±?2°C (Accelerated) 21 Days Slight separation* 49.2 5.6 6.1 610 8.1 Re-dispersible, no adverse change
54?±?2°C (Accelerated) 30 Days Slight separation 49.0 5.5 6.0 620 8.3 Acceptable
0–5°C (Cold Storage) 7 Days No crystallization 49.9 5.9 6.6 540 7.4 Passed cold stability test
The oil dispersion (OD) formulation containing Profenofos 50% w/w and Acetamiprid 6% w/w demonstrates excellent physicochemical stability under a range of storage conditions, including ambient, accelerated, and cold temperatures. The formulation retains its homogeneity, dispersibility, and active ingredient content over time, with no significant phase separation, crystallization, or degradation. The OD system’s oil-based composition ensures enhanced shelf life, rain-fastness, and prolonged residual efficacy. These results validate the formulation’s robustness, making it suitable for commercial agricultural use across diverse climatic regions, with the added benefit of reducing spray frequency and improving crop health.
Example: 7 - BIO-EFFICACY STUDIES:
Methodology:
The different combinations of Profenofos have been evaluated against different major insect pests of different crops. The insecticidal combinations and solo molecules as individual were taken into note and the efficacy of all the molecules are evaluated and the synergistic effect of the combinations were drawn out using Colby ratio. The experiment and treatment details are mentioned in Table 1a, 1b and 1c along with the target pest against which the molecules were tested. The evaluated crops are first divided into plots for each treatment and replicated following Randomized Block Design. The spraying method followed was foliar application with the help of a knapsack sprayer and two sprays are done with an interval of 10 Days. The combinations are even tested against any signs of Phytotoxicity on the respective crops.
GENERAL INFORMATION:
Crops Chilli; Maize; and Paddy
Irrigated / Rainfed Irrigated

Design RBD
No. of treatments Chilli: 10 treatments
Maize & Paddy: 6 treatments
No. of replications Chilli: 3 replications
Maize & Paddy: 4 replications
Plot size 5 m x 5 m
No. of Sprays Two sprays
Spray interval 10 days
Water volume 500 l/ha
Equipment used Knapsack sprayer

Table 1a. Treatment Details (CHILLI)
T.No Treatment Combination Dose (gm or ml/ha)

T1 Profenofos 50% EC 1000
T2 Acetamiprid 20% SP 100
T3 Spinetoram 11.7% SC 250
T4 Profenofos 50% +Acetamiprid 6% OD 400
T5 Profenofos 50% +Acetamiprid 6% OD 500
T6 Profenofos 50% + Acetamiprid 6% OD 600
T7 Profenofos 50% + Spinetoram 9% OD 400
T8 Profenofos 50% + Spinetoram 9% OD 500
T9 Profenofos 50% + Spinetoram 9% OD 600
T10 Untreated Check -
Table 1b. Treatment Details (MAIZE)
T.No Treatment Combination Dose (gm or ml/ha)

T1 Profenofos 50% EC 1000
T2 Spinetoram 11.7% SC 250
T3 Profenofos 50% + Spinetoram 9% OD 400
T4 Profenofos 50% + Spinetoram 9% OD 500
T5 Profenofos 50% + Spinetoram 9% OD 600
T6 Untreated Check -
Table 1c. Treatment Details (PADDY)
T.No Treatment Combination Dose (gm or ml/ha)

T1 Profenofos 50% EC 1000
T2 Acetamiprid 20% SP 100
T3 Profenofos 50% + Acetamiprid 6% OD 400
T4 Profenofos 50% + Acetamiprid 6% OD 500
T5 Profenofos 50% + Acetamiprid 6% OD 600
T6 Untreated Check -
Method of Observations:
Pest observations: select 5 random plants in the plot and the pest population/pest damage symptoms are recorded and then the pest population or percentage damage will be calculated.
The observations were taken 1 day before spraying and at 3, 7, 10 days after spray for Thrips in chilli, Fall armyworm in maize and Brown plant hopper in paddy crop respectively.
Take the observation on the crop safety of the insecticide i.e., Phytotoxicity / softener observation of insecticide after application at 5 and 10 Days after application.
The yield data from crops is taken plot wise and equated to t/ha.
Parameters of Observations:
The pest infestation in different crops are calculated as follows –
Thrips Scirtothrips dorsalis (Chilli):
The thrips infestation is measured as number of thrips per 3 leaves per plant, the data is recorded from 5 random plants, and the average thrips/plant is calculated.
Fall Armyworm Spodoptera frugiperda (Maize):
The fall armyworm infestation is measured as number of larvae per plant, the data is recorded from 5 random plants, and the average larval/plant is calculated.
Brown Plant Hopper Nilaparvata lugens (Paddy):
The brown plant hopper infestation is measured as number of hoppers (nymphs or adults) from basal portion of hill, the data is recorded from 10 random hills, and the average bph/hill is calculated.

Percent reduction over control:
In all the pest populations calculated, the percent reduction over control has been calculated to identify the potency of the pesticide above untreated control. The percent reduction is calculated by the following formula –
% Reduction (%ROC) = ( % control in untreated-% control in treatment )/(% control in untreated)× 100
Colby’s Method:
The combined effect of Pesticidal combinations is the sum of their individual effects. Colby’s method is an approach to evaluate the synergistic, additive, or antagonistic effects due to the interactions of two pesticides as a combination.
Colby’s method calculates expected response, and a ratio is calculated between expected response and observed response.
The formula for expected response is as follows-
two-way combination -
E = (A+B) - ((A*B)/100)
A represents pesticide 1, B represents pesticide 2
The observed response is the actual percent control achieved
Colby’s ratio = Observed response (O)/Expected response (E).
If the ratio is,
< 1 = Antagonistic effect
= Additive effect
> 1 = Synergistic effect
Results:
The different insecticide combinations of Profenofos viz., Profenofos 50% + Spinetoram 9% OD, and Profenofos 50% + Acetamiprid 6% OD formulations applied at three doses 400, 500 and 600 gm or ml/ha were effective in managing a wide range of insect pests, so the different pests and crops in the field experiments were enlisted below,
Chilli - Thrips (Scirtothrips dorsalis)
Maize -Fall armyworm (Spodoptera frugiperda)
Paddy -Brown Plant Hopper (Nilaparvata lugens)
Example - 7.1: Chilli – Thrips
Table 2. Synergistic Effect of Profenofos Combinations on Thrips Infestation on Chilli Crop
T.No Treatment Combination Dose
(gm or ml/ha) % Reduction in Infestation
Expected (E) Observed (O)
T1 Profenofos 50% EC 1000 43.64
T2 Acetamiprid 20% SP 100 38.33
T3 Spinetoram 11.7% SC 250 45.11
T4 Profenofos 50% + Acetamiprid 6% OD 400 65.25 80.87
(O/E) 1.24
T5 Profenofos 50% + Acetamiprid 6% OD 500 65.25 89.40
(O/E) 1.37
T6 Profenofos 50% + Acetamiprid 6% OD 600 65.25 90.50
(O/E) 1.39
T7 Profenofos 50% + Spinetoram 9% OD 400 69.07 80.11
(O/E) 1.16
T8 Profenofos 50% + Spinetoram 9% OD 500 69.07 91.64
(O/E) 1.33
T9 Profenofos 50% + Spinetoram 9% OD 600 69.07 91.44
(O/E) 1.32
The efficacy of Profenofos 50% EC + Acetamiprid 6% OD and Profenofos 50% + Spinetoram 9% OD at 400, 500, 600ml/ha were evaluated against Scirtothrips dorsalis (thrips) in chilli crop through thrips infestation. The study was conducted in a randomized block design with net plot size of 5m x 5m. The crop was raised by following all the agronomic practices, two consecutive sprays were done with knapsack sprayer with 10 days spray interval (Table 2).
The thrips population, the percent reduction in thrips over control was calculated at the end of each spray, the percent reduction in thrips infestation at the end of second spray has been presented in Table 2. The results indicate that the insecticidal combinations were highly effective against thrips management in chilli when applied in two-way combination than when applied alone. The results revealed Profenofos 50% + Acetamiprid 6% OD combination achieved 80.87%, 89.40% and 90.50% reduction in infestation over control in 400, 500, 600ml/ha doses. While Profenofos 50% + Spinetoram 9% OD combination observed 80.11%, 91.64% and 91.44% reduction in infestation over control in 400, 500, 600ml/ha doses respectively.
The percent reduction in infestation over control in solo treatments displayed a reduction between < 50% which was moderate but not significant control which was not satisfactory or considerable control. The present combination Profenofos 50% + Acetamiprid 6% in OD and Profenofos 50% + Spinetoram 9% OD at 400, 500, 600ml/ha doses were highly promising in managing thrips in chilli by recording a synergistic effect with a Colby ratio of >1.2 and >1.15 respectively.
Similarly, the efficacy trend of the combinations in managing thrips in chilli over the span of two sprays was shown in the table below, where the combinations showed >50% reduction in infestation over control by the end of first spray which gradually increased to >80% reduction in infestation over control by the end of two sprays (Table 3).

Table 3. Efficacy of Profenofos Combinations against Thrips Infestation on Chilli Crop
Treatments Dose
(gm or
ml/ha) First Spray
(Thrips Population) Second Spray
(Thrips Population)
pre 3 das 7 das 10 das Avg % ROC 3 das 7 das 10 das Avg % ROC
Profenofos 50% EC 1000 20.78 17.22 17 18.89 18.47 21.39 14.56 15 17.34 15.63 43.64
Acetamiprid 20% SP 100 20 16.23 16 18.41 16.88 28.17 15.23 17 19.09 17.11 38.33
Spinetoram 11.7% SC 250 21.04 15.11 15 17.45 15.85 32.54 12.11 16.23 17.34 15.23 45.11
Profenofos 50% + Acetamiprid 6% OD 400 20.04 12.07 12 13.09 12.39 47.29 5.12 5.22 5.58 5.31 80.87
Profenofos 50% + Acetamiprid 6% OD 500 20.23 9.44 9 10.11 9.52 59.50 2.85 2.97 3 2.94 89.40
Profenofos 50% + Acetamiprid 6% OD 600 20.45 9 8.5 9.12 8.87 62.24 2.58 2.62 2.71 2.64 90.50
Profenofos 50% + Spinetoram 9% OD 400 20.55 10.17 9 10.41 9.86 58.04 5.23 5.32 6 5.52 80.11
Profenofos 50% + Spinetoram 9% OD 500 20 8.23 8 9.37 8.53 63.69 2.13 2.33 2.5 2.32 91.64
Profenofos 50% + Spinetoram 9% OD 600 20.22 8 7.45 8.65 8.03 65.82 2 2.45 2.67 2.37 91.44
Untreated Check 21.11 22.33 23 25.17 23.50 0.00 25.87 27.57 29.78 27.74 0.00
SeM± 1.24 0.590
CD 3.63 1.77
Table 4. Phytotoxicity of Profenofos combinations and other insecticides on Chilli Crop
Treatments Days Visual Rating Scale
Yellowing Necrosis Wilting Vein
Clearing Leaf Tip / Margin Dying Stunting / Dwarfing
Profenofos 50% EC @1000ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Acetamiprid 20% SP @100gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Spinetoram 11.7% SC @ 450ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 400ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 500ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 600gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 400ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 500ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 600gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Untreated Check 5 0 0 0 0 0 0
10 0 0 0 0 0 0

The phytotoxic effect of the insecticidal combinations of Profenofos viz., Profenofos 50% + Acetamiprid 6% in OD and Profenofos 50% + Spinetoram 9% OD at all three doses and solo formulations of the same showed no signs of phytotoxicity in the chilli crop. Hence, the combinations are safe for the usage of Thrips management in Chilli crop (Table 4).
Example -7.2: Maize – Fall Armyworm
Table 5. Synergistic Effect of Profenofos Combinations against Fall Armyworm Infestation on Maize Crop
T.No Treatment Combination Dose
(gm or ml/ha) % Reduction in Infestation
Expected (E) Observed (O)
T1 Profenofos 50% EC 1000 57.20
T2 Spinetoram 11.7% SC 250 57.93
T3 Profenofos 50% + Spinetoram 9% OD 400 81.99 88.90
(O/E) 1.08
T4 Profenofos 50% + Spinetoram 9% OD 500 81.99 91.93
(O/E) 1.12
T5 Profenofos 50% + Spinetoram 9% OD 600 81.99 93.80
(O/E) 1.14
The efficacy of Profenofos 50% + Spinetoram 9% OD at three doses of 400, 500, 600ml/ha doses were evaluated against Spodoptera frugiperda (fall armyworm) in maize crop through larval infestation. The study was conducted in a randomized block design with net plot size of 5m x 5m. The crop was raised by following all the agronomic practices, two consecutive sprays were done with knapsack sprayer with 10 days spray interval (Table 5).
The larval population and percent reduction of larvae over control was calculated at the end of each spray, the percent reduction in larval population at the end of second spray has been presented in Table 5. The results indicate that the insecticidal combinations were highly effective against fall armyworm management in maize when applied in two-way combination than when applied alone. The results revealed Profenofos 50% + Spinetoram 9% OD combination achieved 88.90%, 91.93% and 93.80% reduction in infestation over control in 400, 500, 600ml/ha doses respectively. The percent reduction in infestation over control in solo treatments displayed a reduction >55% which was moderate efficacy but not evident for control and not satisfactory or considerable control. The present combination Profenofos 50% + Spinetoram 9% in OD at all three doses were highly promising in managing Fall armyworm in maize by recording a synergistic effect with a Colby ratio of 1.08, 1.12 and 1.14 respectively.
Similarly, the efficacy trend of the combinations in managing fall armyworm in maize over the span of two sprays was shown in the table below, where the combinations showed >60% reduction in infestation over control by the end of first spray which gradually increased to >85% reduction in infestation over control by the end of two sprays (Table 6).
Table 6. Efficacy of Profenofos Combinations against Fall Armyworm Infestation on Maize Crop
Treatments Dose
(gm or ml/ha) First Spray
(Larval Population) Second Spray
(Larval Population)
Pre 3 das 7 das 10 das Ave. % ROC 3 das 7 das 10 das Ave. % ROC
Profenofos 50% EC 1000 1 0.94 0.85 0.9 0.92 32.50 0.81 0.94 1.07 0.94 41.61
Spinetoram 11.7% SC 250 1.07 1 0.88 1 0.96 29.76 0.9 0.98 1.03 0.97 39.75
Profenofos 50% + Spinetoram 9% OD 400 0.93 0.87 0.88 1.02 0.92 32.44 0.89 0.95 1 0.95 41.20
Profenofos 50% + Spinetoram 9% OD 500 1.07 0.6 0.42 0.5 0.51 62.93 0.44 0.68 0.85 0.66 59.21
Profenofos 50% + Spinetoram 9% OD 600 1 0.8 0.5 0.65 0.65 52.44 0.5 0.65 0.77 0.64 60.25
Untreated check - 1.03 0.7 0.5 0.68 0.63 54.15 0.51 0.61 0.68 0.60 62.73
SeM± 0.151 0.112
CD 0.459 0.341

Table 7. Phytotoxicity of Profenofos combinations and other insecticides on Maize
Treatments Days Visual Rating Scale
Yellowing Necrosis Wilting Vein
Clearing Leaf Tip / Margin Dying Stunting / Dwarfing
Profenofos 50% EC @1000ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Spinetoram 11.7% SC @ 450ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 400ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 500ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Spinetoram 9% OD @ 600gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Untreated Check 5 0 0 0 0 0 0
10 0 0 0 0 0 0
The phytotoxic effect of the insecticidal combinations of Profenofos 50% + Spinetoram 9% OD in 400, 500, 600ml/ha doses and solo formulations of the same showed no signs of phytotoxicity in the maize crop. Hence, the combinations are safe for the usage of Fall Armyworm management in Maize crop (Table 7).

Example -7. 3: Paddy– Brown Plant Hopper
Table 8. Synergistic Effect of Profenofos Combinations on Brown Plant Hopper Infestation on Paddy Crop
T.No Treatment Combination Dose
(gm or ml/ha) % Reduction in Infestation
Expected (E) Observed (O)
T1 Profenofos 50% EC 1000 53.80
T2 Acetamiprid 20% SP 100 57.11
T3 Profenofos 50% + Acetamiprid 6% OD 400 80.19 83.72
(O/E) 1.02
T4 Profenofos 50% + Acetamiprid 6% OD 500 80.19 89.85
(O/E) 1.10
T5 Profenofos 50% + Acetamiprid 6% OD 600 80.19 90.14
(O/E) 1.10
The efficacy of Profenofos 50% + Acetamiprid 6% OD at 400, 500, 600ml/ha doses were evaluated against Nilaparvata lugens (brown plant hopper) in paddy crop. The study was conducted in a randomized block design with net plot size of 5m x 5m. The crop was raised by following all the agronomic practices, two consecutive sprays were done with knapsack sprayer with 10 days spray interval (Table 8).
The brown plant hopper population, the percent reduction in hoppers over control was calculated at the end of each spray, the percent reduction in hoppers infestation at the end of second spray has been presented in Table 8. The results indicate that the insecticidal combinations were highly effective against brown plant hoppers management in paddy when applied in two-way combination than when applied alone. The results revealed Profenofos 50% + Acetamiprid 6% OD combination achieved 83.72%, 89.85% and 90.14% reduction in infestation over control in 400, 500, 600ml/ha doses respectively. The percent reduction in infestation over control in solo treatments displayed a reduction up to 50% which was not significant control. The present combination Profenofos 50% + Acetamiprid 6% OD in 400, 500, 600ml/ha doses were highly promising in managing brown plant hopper in paddy by recording a synergistic effect with a Colby ratio of 1.02, 1.10 and 1.10 respectively.
Similarly, the efficacy trend of the combinations in managing brown plant hopper in paddy over the span of two sprays was shown in the table below, where the combinations showed >40% reduction in infestation over control by the end of first spray which gradually increased to >80% reduction in infestation over control by the end of two sprays (Table 9).
Table 9. Efficacy of Profenofos Combinations against Brown Plant Hopper Infestation on Paddy Crop
Treatments Dose
(gm or ml/ha) First Spray
(BPH Population) Second Spray
(BPH Population)
Pre 3 das 7 das 10 das Ave. % ROC 3 das 7 das 10 das Ave. % ROC
Profenofos 50% EC 1000 12.23 11.12 10.23 9.65 12.23 11.12 6.31 6 6.07 7.01 53.80
Acetamiprid 20% SP 100 12 9.45 9 8.68 12 9.45 5.78 5.43 6.13 6.51 57.11
Profenofos 50% + Acetamiprid 6% OD 400 12.09 6.45 5.78 6.51 12.09 6.45 1.02 1.15 1.2 2.47 83.72
Profenofos 50% + Acetamiprid 6% OD 500 12.1 5.15 5 5.42 12.1 5.15 0 0.27 0.47 1.54 89.85
Profenofos 50% + Acetamiprid 6% OD 600 12.07 5.02 4.78 5.38 12.07 5.02 0 0.2 0.4 1.50 90.14
Untreated check - 12.34 12.88 13.45 14 12.34 12.88 14.67 15.78 16.22 15.17 0.00
SeM± 0.833 0.677
CD 2.534 2.058
Table 10. Phytotoxicity of Profenofos Combinations and other Insecticides on Paddy Crop
Treatments Days Visual Rating Scale
Yellowing Necrosis Wilting Vein
Clearing Leaf Tip / Margin Dying Stunting / Dwarfing
Profenofos 50% EC @1000ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Acetamiprid 20% SP @ 100gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 400ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 500ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Profenofos 50% + Acetamiprid 6% OD @ 600gm/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Untreated Check 5 0 0 0 0 0 0
10 0 0 0 0 0 0

The phytotoxic effect of the insecticidal combinations of Profenofos 50% + Acetamiprid 6% OD in 400, 500, 600ml/ha doses and solo formulations of the same showed no signs of phytotoxicity in the paddy crop. Hence, the combinations are safe for the usage of Brown Plant Hopper management in Paddy crop (Table 9).
Effect of Profenofos Combinations on Crop Yield
The evaluated combinations of Profenofos 50% + Acetamiprid 6% OD and Profenofos 50% + Spinetoram 9% OD at application rates of 400, 500, and 600 mL/ha exhibited a positive impact on crop yield across all tested crops—Chilli, Maize, and Paddy. Yield observations recorded at harvest indicated that plots treated with the combination formulations consistently achieved significantly higher yields compared to control and solo treatment plots. This enhancement in yield suggests not only effective pest suppression but also a probable phytotonic effect attributable to the combination formulations.
The observed increase in productivity can be attributed to:
Improved pest control efficiency,
Reduction in crop damage during critical growth stages,
Better plant vigor and recovery post-infestation,
Possible synergistic enhancement in physiological health of the plant.
These findings collectively affirm the agronomic and economic advantage of using Profenofos-based combination formulations for integrated pest and yield management in key agricultural crops.

Table 11. Effect of Broflanilide Combinations on the Crop Yield
Treatments Dose
(gm or ml/ha) Yield (t/ha)
Chilli Maize Paddy
Profenofos 50% EC 1000 32.40 11.61 42.46
Acetamiprid 20% SP 100 30.99 - 44.52
Spinetoram 11.7% SC 250 35.99 12.28 -
Profenofos 50% + Acetamiprid 6% OD 400 41.21 - 52.60
Profenofos 50% + Acetamiprid 6% OD 500 38.99 - 49.67
Profenofos 50% + Acetamiprid 6% OD 600 40.75 - 50.57
Profenofos 50% + Spinetoram 9% OD 400 41.99 14.83 -
Profenofos 50% + Spinetoram 9% OD 500 39.99 16.28 -
Profenofos 50% + Spinetoram 9% OD 600 41.51 17.84 -
Untreated Check - 25.77 6.17 32.26
SeM± 0.012 0.014 0.004
CD 0.036 0.044 0.013

The above examples and results are intended to illustrate certain specific embodiments of the invention and should not be construed as limiting its broader applicability. It is understood that:
The invention is not limited to the precise compositions or constituent concentrations disclosed herein. Variations in formulation components and ratios may be employed by those skilled in the art without departing from the essence of the invention.
The terminology used throughout this specification is for descriptive purposes only and is not intended to limit the scope of the claims. Unless context dictates otherwise, singular terms include their plural equivalents, and vice versa.
All technical and scientific terms used herein carry their commonly accepted meanings as understood by practitioners skilled in the relevant field.
While specific materials, methods, and field conditions have been described, substitutes and equivalents that achieve substantially similar results are considered within the purview of this disclosure. Any modifications, adaptations, or substitutions of the formulations, test protocols, or crop sequences that are apparent to a person skilled in the art are considered to fall within the scope of the invention as defined by the appended claims.
All patents, published applications, and other references cited in this disclosure are incorporated herein by reference and are considered to indicate the level of ordinary skill in the art relevant to this invention. ,CLAIMS:CLAIMS
We Claim:
1. A stable synergistic insecticidal oil dispersion formulation comprising:
Profenofos or agrochemically acceptable salt(s) thereof;
An insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof; and
One or more agriculturally acceptable excipients.
2. The oil dispersion formulation as claimed in claim 1, agriculturally acceptable excipients are selected from oil(s), solvent(s), surfactant(s)/emulsifier(s), dispersing agent(s), wetting agent(s) and optionally agriculturally acceptable additives.
3. The oil dispersion formulation as claimed in claim 1, wherein a) profenofos or agrochemically acceptable salt(s) thereof is present in the range of 1 to 70% of total weight of formulation, and b) at least one insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof is present in the range of 0.1 to 20% of total weight of formulation.
4. The oil dispersion formulation as claimed in claim 1, wherein said formulation comprising: a) profenofos or agrochemically acceptable salt(s) thereof in the range of 1 to 70%; b) and at least one insecticide selected from acetamiprid or spinetoram or agrochemically acceptable salt(s) thereof is present in the range of 0.1 to 20% of total weight of formulation; c) one or more oils and/or solvents in the range of 1 to 80%; d) one or more surfactant(s)/emulsifier(s) in the range of 0.1 to 30%; e) one or more dispersing agent in the range of 0.1 to 30%; f) one or more wetting agent(s) in the range of 0.1 to 30%; and g) optionally agriculturally acceptable additives in the range of 0 to 75%.
5. The oil dispersion formulation as claimed in claim 1 or 4, wherein said oil is selected from paraffinic hydrocarbons, petroleum oil or its derivatives, vegetable oil or its derivatives, seed oil or its derivatives, mineral oil or its derivatives, animal oil or its derivatives, plant oil or its derivatives, light paraffin oil or its derivatives, animal oil or derivatives, or a combination thereof.
6. The oil dispersion formulation as claimed in claim 1 or 4, wherein said dispersing agent is selected from the group comprising Atlox 4912, polyurethanes, methyl oleyl taurates, phosphated ethoxylated alkylphenols, polyamides, poly vinyl alcohols, styrene copolymers, polylactic acid, alkyl naphthalene sulfonates, phosphated ethoxylated and proproxylated natural or synthetic fatty alcohols, acrylic polymers and copolymers, Atlox Metasperse 550S, castor oil ethoxylate, mixture of salt of naphthalene sulphonic acid and phenol sulphonic acid condensate, poly(lactic acid-glycolic acid) copolymers, sulfonated aromatic polymer, phenol sulphonic acid condensates, ethanolamine fatty amides, phosphated ethoxylated tristyrylphenols, polyurea, polyesters, phosphated ethoxylated natural or synthetic fatty alcohols, sodium salt of naphthalene sulfonate condensate, ligno sulphonates, polycarbonates, phosphated ethoxylated and proproxylated alkylphenols, silica poly ether copolymer, sodium salt of naphthalene sulfonate condensate, Atlox 4916, plant oil ethoxylates, butadiene copolymers, poly carboxylates, or combination thereof.
7. The oil dispersion formulation as claimed in claim 1 or 4, wherein said surfactant/emulsifier is selected from C6-C20 ethoxylated alcohols, C6-C20 propoxylated alcohols, calcium alkyl benzene sulphonates, alkyl sulphonate, ether sulphonate, ether phosphate, alkoxylated alcohols, alkoxylated alkyl phenols, tridecyl alcohol ethoxylate, ethoxylated fatty acids dodecyl benzene sulphonate, sulphonates of other C11-C16 alkyl benzenes, alkyl ether sulphates, alkyl phenol ether phosphates, ester phosphates, natural or synthetic ethoxylated fatty alcohols, natural or synthetic propoxylated fatty alcohols, EO-PO copolymers, ethoxylated fatty acids, ethoxylated castor oil, ethoxylated sorbitan esters, ethoxylated esterified sorbitols, ethoxylated alkylphenols, ethoxylated tristyrylphenols or ethoxylated fatty amines or combination thereof.
8. The oil dispersion formulation as claimed in claim 1 or 4, wherein said solvent is selected from C2-C4-alkyl lactates, alkyl benzenes, alkylnaphthalenes, polyalkylene glycol ethers, fatty acid diesters, fatty alkylamides and diamides, dialkylene carbonates, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, propylene glycol esters of fatty acids, or propylene glycol ester, methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, di-propylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, solvent C9, ethyl lactate, glycerin triacetate, cyclohexanone, di-propylene glycol ethyl ether, ethylene glycol, propane diols, or glycerine or combination thereof.
9. The oil dispersion formulation as claimed in claim 1 or 4, wherein said wetting agent is selected from dioctyl sulfosuccinate, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether sulfonates, dialkylsuccinate, EO-PO block copolymer, Atlox 4914, PF40 Clariant, sodium dioctyl sulphosuccinate, sodium lauryl sulfonate, sodium blend of alkyl naphthalene sulfonate, trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, modified heptamethyl trisiloxane, polyether modified polysiloxane, or combination thereof.
10. A process for preparing an oil dispersion formulation as claimed in claim 1 or 4, wherein said process comprising the steps of:
mixing surfactant(s)/emulsifier(s), dispersing agent(s), wetting agent(s), and optionally agrochemically acceptable additives to oils and/or solvents or combination thereof with continuous stirring to form a homogeneous mixture;
adding profenofos or agrochemically acceptable salt(s) thereof to the above homogeneous mixture obtained in step (a) with constant stirring to form a homogeneous mixture;
adding acetamiprid or spinetoram technical or agrochemically acceptable salt(s) thereof to the above homogeneous mixture obtained in step (b) with constant stirring to form a homogeneous mixture; and
adding the remaining oil(s) and/or solvent(s) or combination thereof with constant stirring till a homogeneous mass obtained.
11. A kit for preparing a synergistic insecticidal oil dispersion formulation, comprising:
(a) a container comprising profenofos or its agrochemically acceptable salt(s);
(b) a container comprising an insecticide selected from acetamiprid or spinetoram or their agrochemically acceptable salt(s);
(c) optionally a container comprising an agriculturally acceptable oil-based carrier composition comprising one or more emulsifier(s), dispersing agent(s), or wetting agent(s),
Wherein, said components are adapted to be mixed prior to application for pest management in agricultural crops.
12. A method for controlling or combating the undesired insect pests or mites and/or insect eggs and larvae and/or microorganisms, wherein said oil dispersion formulation as claimed in claim 1 or 4, is applied to the plants, to parts thereof or to a locus thereof.