Description:FIELDOFDISCLOSURE
The present disclosure relates to the field of agricultural insecticides. Specifically, it provides an insecticidal composition comprising a combination of active ingredients, namely Etofenprox, Diafenthiuron, and Acetamiprid, and methods of preparing and using such compositions. The present disclosure aims to provide enhanced control of a variety of insect pests affecting crops, with a synergistic effect that improves efficacy compared to individual components.
BACKGROUND OF THE DISCLOSURE
In agriculture, managing insect pests is crucial to ensure high crop yield and quality. Various crops, including cotton and chili, are prone to damage from a range of insect pests, such as whiteflies, thrips, aphids, and mites. These pests not only damage the crops by feeding on plant sap but also act as vectors for diseases, further impacting crop health. Consequently, farmers and agricultural experts are constantly seeking more effective and reliable solutions to combat these insect infestations.
Traditionally, pest control has relied on the use of single active ingredient insecticides or simple tank mixtures of insecticides. While these approaches can be effective, they often have limitations, including the development of pest resistance, lower efficacy, and the need for higher dosages to achieve the desired level of control. Additionally, tank mixtures of insecticides may not always result in a stable and uniform product, leading to inefficiencies in application and reduced pest control performance.
Over time, many pests have developed resistance to widely used insecticides, reducing the effectiveness of conventional treatments. This phenomenon is a major concern in integrated pest management and sustainable agriculture, necessitating the development of novel insecticidal compositions that can overcome resistance and offer reliable, long-term pest control. Moreover, the agricultural industry is increasingly focused on developing environmentally friendly formulations that are stable, safe, and easy to handle and apply.
The active ingredients in the present disclosure comprises Etofenprox, Diafenthiuron, and Acetamiprid which have been extensively used in pest management due to their distinct modes of action. Etofenprox is a pyrethroid ether insecticide that disrupts the nervous system of insects, leading to paralysis and death. Diafenthiuron functions as an oxidative phosphorylation inhibitor, effectively controlling mites, whiteflies, and other pests. Acetamiprid, a neonicotinoid insecticide, binds to nicotinic acetylcholine receptors, causing hyperexcitation and paralysis in insects. Each of these active ingredients offers unique advantages; however, when used alone, their efficacy may be limited by pest resistance or other environmental factors.
ETOFENPROX
Etofenprox with CAS registration number 80844-07-1 is a derivative of an aromatic ether that is 3-phenoxybenzyl ether of 2-(4-ethoxyphenyl)-2-methylpropan-1-ol. It has the role as a pyrethroid ether insecticide. It is functionally related to a 2-(4-ethoxyphenyl)-2-methylpropan-1-ol.
It has an IUPAC name1-ethoxy-4-[2-methyl-1-[(3phenoxyphenyl)methoxy]propan-2-yl]benzenehaving chemical structure as:

ETOFENPROX

DIAFENTHIURON
Diafenthiuron with CAS registration no 80060-09-9, It is a thiourea acaricide, a thiourea insecticide.which is used to control mites, aphids and whitefly in cotton. It has a role as an oxidative phosphorylation inhibitor and an insecticide.
It has an IUPAC name 1-tert-butyl-3-[4-phenoxy-2,6-di(propan-2-yl)phenyl]thioureahaving chemical structure as:

DIAFENTHIURON
ACETAMIPRID:
Acetamiprid with CAS registration number 135410-20-7 is a pyridylmethylamine, neonicotinoid insecticide. It is a systemic insecticide, and it acts by binding to the acetylcholine site on nicotinoyl acetylcholine receptors (nAChRs), causing a range of symptoms from hyperexcitation to lethargy and paralysis in the insects. Acetamiprid controls insect species such as Hemiptera, Thysanoptera and Lepidoptera.
It has an IUPAC name (E)-N-[(6-chloro-3-pyridyl)methyl]-N'-cyano-N-methylacetamidine having chemical structure as below:

ACETAMIPRID
The present disclosure addresses the above-mentioned challenges by combining Etofenprox, Diafenthiuron and Acetamiprid in a carefully formulated composition. The combination provides a synergistic effect, meaning the combined action of these ingredients is greater than the sum of their individual effects. This synergy allows for lower dosages, enhanced insecticidal performance, and a broader spectrum of pest control. Furthermore, the disclosure incorporates specialized formulation techniques, such as suspo-emulsion (SE) and oil dispersion (OD), to ensure the stability, homogeneity, and effectiveness of the insecticidal composition.
The present disclosure not only improves pest control but also addresses the need for formulations that are stable under various environmental conditions, easy to mix and apply, and safe for non-target organisms when used as directed. By reducing the likelihood of resistance development and minimizing the environmental impact, the disclosure offers a sustainable and efficient solution for pest management in agriculture.
The existing problems and limitations in the current agricultural pest management techniques that the present disclosure seeks to address:
1. Development of Pest Resistance:
a. Many pests have developed resistance to single active ingredient insecticides, making them less effective over time.
b. Conventional insecticides often require increased dosages to achieve the same level of pest control, which is unsustainable and increases the risk of environmental contamination.
c. The frequent use of single-action insecticides leads to the rapid evolution of resistant pest populations, reducing long-term pest management efficacy.
2. Limited Spectrum of Pest Control:
a. Single active ingredient insecticides or basic tank mixtures may not be effective against a broad range of insect pests, leading to incomplete control.
b. Farmers often need to use multiple products to target different pests, which increases costs and complicates pest management practices.
c. Existing solutions may fail to control certain pests like whiteflies, thrips, aphids, and mites effectively in crops like cotton and chili.
3. Suboptimal Synergy in Tank Mixes:
a. Tank mixtures of individual insecticides do not always exhibit true synergistic effects. The combination may result in antagonistic or merely additive effects, which do not significantly enhance pest control.
b. Inconsistent performance of tank mixes can be attributed to the instability of the combined components, leading to inadequate pest control and uneven application.
4. Stability Issues in Formulations:
a. Existing insecticidal formulations often suffer from stability issues, especially under varying environmental conditions such as high or low temperatures.
b. Instability can lead to the separation of active ingredients, reduced efficacy, and challenges in storage and transport.
c. Unstable formulations are harder to apply uniformly, affecting the overall effectiveness of pest control measures.
5. Need for Higher Dosages:
a. Due to the lack of synergistic action, traditional formulations or single active ingredient products may require higher dosages to achieve effective pest control.
b. Increased dosages not only raise the cost of pest management but also heighten the risk of crop phytotoxicity and environmental damage, including potential harm to beneficial insects and non-target organisms.

6. Environmental and Safety Concerns:
a. The use of higher concentrations of insecticides contributes to environmental pollution and poses health risks to farm workers and consumers.
b. There is a growing need for formulations that are effective at lower concentrations, minimizing environmental impact while maintaining pest control efficacy.
c. Safety concerns also arise from formulations that produce harmful residues or have poor degradability, necessitating safer and more eco-friendly options.
7. Application Challenges and Inconsistent Results:
a. Some existing formulations are difficult to mix or apply, leading to inconsistent distribution of the insecticide on crops.
b. Poorly mixed insecticides may form clumps or separate into different phases, making uniform application challenging and reducing the effectiveness of the treatment.
c. The variability in application quality can result in areas of the crop being under protected, leaving them vulnerable to pest damage.
8. Economic Inefficiency:
a. The need for multiple insecticides or repeated applications due to inadequate control increases the financial burden on farmers.
b. Inefficient pest management practices can lead to significant crop losses and reduced profitability for farmers.
c. A more effective, stable, and broad-spectrum insecticidal composition can reduce overall costs and enhance agricultural productivity.
The present disclosure aims to overcome these limitations by providing a synergistic insecticidal composition of Etofenprox, Diafenthiuron and Acetamiprid, ensuring high efficacy at lower dosages, broad-spectrum pest control, formulation stability, and minimal environmental impact.
OBJECTIVEOFTHEDISCLOSURE
The main objective of the disclosure is to provide a synergistic insecticidal composition combining Etofenprox, Diafenthiuron and Acetamiprid that enhances pest control efficacy beyond the sum of individual effects.

Another important object of the present disclosure is to deliver broad-spectrum pest control that effectively targets a variety of insect pests, including whiteflies, thrips, aphids, and mites, across different crops like cotton and chili.
Another object of the present disclosure is to reduce the likelihood of pest resistance by utilizing a multi-component approach, thereby decreasing the dependence on single-action insecticides.
Yet another object of the present disclosure is to ensure stability of the formulation under various environmental conditions, minimizing separation or degradation of active ingredients for consistent performance.
Yet another object of the present disclosure is to lower the required dosage levels while maintaining effective pest control, reducing potential Phytotoxicity to crops and minimizing environmental impact.
Yet another object of the present disclosure is to provide an easy-to-mix and apply formulation that ensures uniform distribution on crops, improving application efficiency and overall pest control results.
Yet another object of the present disclosure is to create an environmentally safer alternative by minimizing harmful residues, thus reducing health risks for farmers, consumers, and non-target organisms.

SUMMARY OF THE DISCLOSURE
The present disclosure introduces a novel insecticidal composition comprising Etofenprox, Diafenthiuron and Acetamiprid, designed to enhance pest control efficacy, broaden the range of target pests, and improve formulation stability for agricultural applications.
In an aspect of the present disclosure, the composition can be formulated into various forms, including a suspo-emulsion (SE) or oil dispersion (OD). For the SE formulation, Etofenprox is initially mixed with emulsifiers to create an oil phase, while Diafenthiuron and Acetamiprid are combined with dispersing agents and biocides in an aqueous phase. The two phases are meticulously blended under controlled conditions, followed by pH adjustment and stabilization, resulting in a homogeneous and stable emulsion with optimized particle size. This ensures consistent and effective application across crops.
In another aspect of the present disclosure, the OD formulation involves dispersing all three active ingredients in a carefully selected oil medium, alongside emulsifiers, antifreezing agents, and rheology modifiers. The mixture undergoes homogenization and bead milling to achieve uniform particle distribution, followed by the addition of stabilizing agents to enhance long-term formulation stability. This process yields a product that demonstrates excellent efficacy, with minimal risk of phase separation or degradation over time.
In an aspect of the present disclosure, the insecticidal composition includes precise ratios of Etofenprox (7.2%), Diafenthiuron (29.7%), and Acetamiprid (6.0%), complemented by emulsifiers, dispersing agents, and stabilizers to achieve a stable suspo-emulsion (SE) formulation. The formulation process involves two critical phases: the creation of an Etofenprox oil phase through the blending of polyalkoxylated butyl ether block co-polymer and ethoxylated tristyrylphenol at ambient temperature, and the preparation of an aqueous phase containing Diafenthiuron and Acetamiprid in a pre-mixing vessel with additional surfactants and stabilizers. Homogenization and particle size reduction ensure uniform dispersion of active ingredients.
In another aspect of the present disclosure, the composition is developed as an oil dispersion (OD) formulation. This process involves mixing the active ingredients with various emulsifiers, anti freezing agents, and rheology modifiers in a pre-mixing vessel. The active ingredients are dispersed in the solvent, followed by controlled particle size reduction and stabilization.
The present disclosure further emphasizes maintaining stability across varied storage conditions, achieving efficient pest control with reduced active ingredient concentrations, and providing a solution that minimizes the risk of pest resistance. The present disclosure’s formulation approach promises significant advancements in agricultural pest management by offering a robust, effective, and environmentally safer insecticidal solution.
DETAILED DESCRIPTION OF THE DISCLOSURE
With respect to the use of substantially any plural and/or singular terms herein, those having skill in the art can translate from the plural to the singular and/or from the singular to the plural as is appropriate to the context and/or application. The various singular/plural permutations may be expressly set forth herein for sake of clarity. The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results. Throughout this specification, the word “comprise”, or variations such as “comprises” or “comprising” or “containing” or “has” or “having”, or “including but not limited to” wherever used, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
Reference throughout this specification to “some embodiments”, “one embodiment” or “an embodiment” means that a particular feature, structure or characteristic described in connection with the embodiment may be included in at least one embodiment of the present disclosure. Thus, the appearances of the phrases “in some embodiments”, “in one embodiment” or “in an embodiment” in various places throughout this specification may not necessarily all refer to the same embodiment. It is appreciated that certain features of the disclosure, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the disclosure, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub-combination.
The term “about” as used herein encompasses variations of +/-5% and more preferably +/-2.5%, as such variations are appropriate for practicing the present disclosure. The nature of the disclosure and the manner in which it is performed is clearly described in the specification. The disclosure has various components, and they are clearly described in the detailed description.
For convenience, before further description of the present disclosure, certain terms employed in the specification, and examples are collected here. These definitions should be read in the light of the remainder of the disclosure and understood as by a person of skill in the art.The terms used herein have the meanings recognized and known to those of skill in the art, however, for convenience and completeness, particular terms and their meanings are setforth below.
a. Biocide: A substance that controls harmful organisms through chemical or biological means. In this context, biocides are used to prevent the growth of unwanted microbes in insecticidal formulations, thereby ensuring product stability.
b. Emulsifier: A chemical agent that helps to stabilize a mixture of two immiscible liquids, such as oil and water, by reducing the surface tension between them. Emulsifiers are essential in creating stable and uniform insecticidal formulations.
c. Dispersing Agent: A chemical additive used to improve the distribution of solid particles in a liquid medium. It prevents clumping and ensures uniform dispersion of active ingredients in insecticidal formulations.
d. Antifoaming Agent: A substance that reduces or prevents the formation of foam during the mixing or application of liquid formulations. Foam can interfere with the effectiveness and handling of insecticidal sprays.
e. Rheology Modifier: An agent that alters the flow properties (viscosity) of a liquid formulation, ensuring that it can be easily applied while maintaining stability. Rheology modifiers prevent sedimentation and phase separation in insecticidal compositions.
f. Phytotoxicity: The degree to which a substance is toxic to plants, causing damage such as yellowing, wilting, or necrosis. The present disclosure includes evaluating the potential phytotoxic effects of the insecticidal composition on crops like cotton and chili.
g. Synergistic Effect: A phenomenon where the combined effect of two or more substances is greater than the sum of their individual effects. In the context of the present disclosure, the combination of Etofenprox, Diafenthiuron, and Acetamiprid exhibits a synergistic effect, providing enhanced pest control.
Abbreviations:
• SE- Suspo emulsion
• OD- Oil dispersion
• SC- Suspension concentrate
• FS- Flowable suspension for seed treatment
• WDG- Water-dispersible granule
• WP- Wettable powder
All processes described in this disclosure may be performed in any suitable sequence, unless explicitly stated otherwise or clearly contradicted by the context. The use of examples or exemplary language (e.g., “such as”) in relation to specific embodiments is solely for the purpose of illustrating the disclosure and should not be interpreted as limiting the scope of the disclosure as defined by the claims. No part of this specification should be construed to imply that any non-claimed element is essential to the implementation of the disclosure.
Accordingly, the present disclosure provides an insecticidal composition comprising a synergistic blend of Etofenprox, Diafenthiuron, and Acetamiprid, formulated to offer superior pest control and enhanced formulation stability.
In an aspect, the present disclosure provides a formulation comprising the insecticide composition, the formulation is selected from a suspension concentrate (SC), a flowable suspension for seed treatment (FS), an oil-dispersion (OD), a suspo-emulsion (SE), a water-dispersible granule (WDG), a wettable powder (WP), etc.
In an embodiment, the insecticidal composition, wherein the Etofenprox ranging from 0.1% to 30.0% by weight of the formulation.
In an embodiment, the composition, wherein Diafenthiuron ranging from 0.1% to 50.0% by weight of the formulation.
In an embodiment, the composition, wherein Acetamiprid in an amount ranging from 0.1% to 30.0% by weight.
In an embodiment, the composition further comprises 0.1% to 20.0% by weight of an emulsifier, which can be selected from ethoxylated propoxylated alcohols, alkylphenol ethoxylates, alkoxylated tristyrylphenols, calcium dodecylbenzenesulfonate, or mixtures such as fatty acid polyethylene glycol ester, ethoxylated fatty acids, castor oil ethoxylate, and alkoxylated phosphate esters.
In an embodiment, a dispersing agent is included in the composition at 0.1% to 20.0% by weight, chosen from polymeric ester dispersants, ethoxylated polyarylphenol phosphate ester, sodium salt of naphthalene sulfonate, acrylic copolymer, nonionic proprietary surfactant blends, or similar compounds.
In an embodiment, the composition ranges 0.01% to 5.0% by weight of an antifoaming agent, such as polydimethylsiloxane or its emulsified form.
In an embodiment, a rheology modifier is present in the composition, ranging from 0.1% to 20.0% by weight, and can include precipitated silica, fumed silica, bentonite, xanthan gum, carboxymethyl cellulose, or other thickening agents.
In an embodiment, Super-Wetting-spreading-penetrating agent is present in the composition, ranging from 0.1% to 5.0% by weight, is blend of methylated seed oil-organic silicone compound may be selected from methylated seed oil-polyalkyleneoxide modified trisiloxane, methylated seed oil-polyalkyleneoxide modified polydimethylsiloxane, methylated seed oil-20 trisiloxane ethoxylate, Polyalkyleneoxide modified heptamethyltrisiloxane methylated seed oil-polyoxyethylene methyl polysiloxane, methylated seed oil-polyether polymethyl siloxane copolymer, methylated seed oil-polyether modified polysiloxane.
In an embodiment, the solvent component ranging up to 95.0% of the composition by weight, and it may consist of demineralized water, N-alkyl-pyrrolidone, or oil media such as methyl or ethyl esters of vegetable oils.
In an embodiment, a biocide is ranging up to 3.0% by weight of the formulation, and suitable options are 1,2-benzisothiazolin-3-one or formaldehyde-based solutions.
In an embodiment, an anti freezing agent can be incorporated, ranging up to 15% by weight, and may include ethylene glycol, propane-1,2-diol, urea, or similar compounds.
In an embodiment, a stabilizing agent is present in the composition, up to 5% by weight, and examples include epoxidized soybean oil, butylated hydroxy toluene, or similar stabilizers.
In an embodiment, a PH stabilizers is present in the composition, up to 5% by weight, and examples include sodium pyrophosphate, sodium acetate, sodium oxalate, sodium carbonate, sodium bicarbonate, trisodium phosphate, citric acid, trisodium citrate, monoethanol amine, triethanol amine, triethylamine, dibasic esters selected from dimethyl succinate, dimethyl glutarate, dimethyl adipate, ortho phosphoric acid, oxalic acid, citric acid, hydrochloric acid.
In one individual embodiment, the insecticidal composition includes Etofenprox in amounts ranging from 0.1% to 30.0% by weight, Diafenthiuron from 0.1% to 50.0% by weight, and Acetamiprid from 0.1% to 30.0% by weight. The composition further contains emulsifiers in the range of 0.1% to 20.0% by weight, selected from ethoxylated propoxylated alcohols, alkylphenol ethoxylates, and tristyrylphenol ethoxylates, and dispersing agents in the range of 0.1% to 20.0% by weight, such as polymeric ester dispersants and acrylic copolymers. It also includes antifoaming agents from 0.01% to 5.0% by weight, typically consisting of polydimethylsiloxane, rheology modifiers from 0.1% to 20.0% by weight, such as bentonite or xanthan gum, and a solvent that balances the composition to 100%, which may include water or oil-based solvents.
In an specific embodiment, the present disclosure provides a suspo-emulsion (SE) formulation where Etofenprox is present at 7.2% by weight, Diafenthiuron at 29.7% by weight, and Acetamiprid at 6.0% by weight. This formulation also includes a total of 4.0% emulsifiers comprising polyalkoxylated butyl ether and ethoxylated tristyrylphenol, 4.0% dispersing agents including a nonionic surfactant blend and acrylic copolymer, and 6.5% of propane-1,2,3-triol as an antifreezing agent. The SE formulation is further stabilized using 0.1% dipropylene glycol solution of 1,2-benzisothiazolin-3-one as a biocide, 0.3% polydimethylsiloxane emulsion as an antifoaming agent, and 0.06% Rhodopol 23 as a rheology modifier, with demineralized water making up the balance.
In another specific embodiment, the composition is prepared as an oil dispersion (OD) formulation that includes 7.2% Etofenprox, 29.7% Diafenthiuron, and 6.0% Acetamiprid. This OD formulation comprises a total of 12.0% emulsifiers, which include castor oil ethoxylate and calcium dodecylbenzenesulfonate, 1.0% dispersing agents made up of polymeric ester dispersant and ethoxylated polyarylphenol phosphate ester, and 2.0% propane-1,2,3-triol as an antifreezing agent. Additionally, the formulation incorporates 1.0% polyalkyleneoxide modified heptamethyltrisiloxane as an adjuvant, 0.3% polydimethylsiloxane as an antifoaming agent, and 3.0% rheology modifiers such as fumed silica and bentonite clay, with the remaining balance made up of methyl ester of vegetable oil as the solvent.
In an embodiment, the SE formulation is prepared through a process where Etofenprox is first mixed with emulsifiers to create an oil phase. Diafenthiuron and Acetamiprid are then combined with dispersing agents, biocides, and antifreezing agents in demineralized water to form an aqueous phase. The oil and aqueous phases are then blended under continuous stirring, followed by pH adjustment and stabilization using rheology modifiers to ensure the composition’s homogeneity and stability.
Another embodiment details the preparation of the OD formulation, where Etofenprox, Diafenthiuron, and Acetamiprid are dispersed in an oil medium with selected emulsifiers, antifreezing agents, and dispersants. This mixture undergoes homogenization and bead milling to achieve a consistent particle size distribution, after which stabilizers and rheology modifiers are added to maintain the formulation's integrity and prevent separation over time.
Yet another embodiment covers alternative forms of the composition, such as suspension concentrate (SC), flowable suspension for seed treatment (FS), water-dispersible granule (WDG), and wettable powder (WP). These variations are achieved by adjusting the emulsifier, dispersing agent, solvent, and other components to optimize the composition for different agricultural applications.
In yet another embodiment, the formulation is designed to minimize environmental impact, using biodegradable solvents and reducing toxic residues. The composition is prepared to ensure compatibility with agricultural safety standards, providing effective pest control with minimal risk to non-target organisms and the environment. The present disclosure emphasizes efficiency and sustainability, with lower application rates and reduced need for repeated treatments.
In an embodiment, the weight percentage of Etofenprox in the composition ranges from 0.1% to 30.0%, the weight percentage of Diafenthiuron ranges from 0.1% to 30.0%, and the weight percentage of Acetamiprid ranges from 0.1% to 30.0%, including specific combinations such as:
The present disclosure provides several significant advantages in optimizing the formulation of the insecticidal composition, particularly through the synergistic interaction of Etofenprox, Diafenthiuron, and Acetamiprid, which collectively enhance efficacy and stability. One of the primary benefits lies in the precise balancing of active ingredients, allowing for lower dosages without sacrificing effectiveness. This precise formulation reduces the likelihood of pest resistance and minimizes the impact on non-target organisms, promoting sustainable agricultural practices.
A major advantage is the improved pest control performance achieved through the synergistic effect, where the combined action of the active ingredients surpasses their individual effects. This synergy translates to enhanced control of a broad spectrum of pests, leading to more effective crop protection and reduced need for repeated applications. Furthermore, the formulation is designed to be highly stable, with emulsifiers, dispersing agents, and rheology modifiers carefully selected to prevent phase separation and ensure uniform application. This stability reduces waste and simplifies handling and storage, making the product highly practical for farmers.
Additionally, the ability to tailor the composition within the specified ranges allows for flexibility in addressing different pest challenges and environmental conditions. The careful selection of solvents and adjuvants ensures optimal spread and penetration on plant surfaces, maximizing efficacy while minimizing residue. The composition’s low environmental footprint, achieved through reduced active ingredient usage and biodegradable components, contributes to a safer, more eco-friendly approach to pest management.
In summary, the present disclosure’s balanced and synergistic formulation delivers key advantages such as enhanced pest control efficacy, improved formulation stability, reduced environmental impact, and greater application efficiency. This makes it not only a highly effective solution for crop protection but also a sustainable and economically beneficial option for large-scale agricultural use.
It is to be understood that the foregoing descriptive matter is illustrative of the disclosure and not a limitation. While considerable emphasis has been placed herein on the particular features of this disclosure, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. Those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein. Similarly, additional embodiments and features of the present disclosure will be apparent to one of ordinary skill in art based upon description provided herein.
Descriptions of well-known/conventional methods/steps and techniques are omitted so as to not unnecessarily obscure the embodiments herein. Further, the disclosure herein provides for examples illustrating the above-described embodiments, and in order to illustrate the embodiments of the present disclosure certain aspects have been employed. The examples used herein for such illustration are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the following examples should not be construed as limiting the scope of the embodiments herein.
EXAMPLES
Example 1: Suspo-emulsion (SE) Formulation and process of preparation thereof-
The Suspo-emulsion (SE) formulation was meticulously prepared in accordance with the present disclosure, utilizing the components outlined in Table 1.
Table 1: Suspo-emulsion (SE) Formulation
Component Composition (%w/w) Remark
Etofenprox 7.2 Active Ingredient
Diafenthiuron 29.7 Active Ingredient
Acetamiprid 6.0 Active Ingredient
Polyalkoxylated butyl ether block co-polymer 2.00 Emulsifier
Ethoxylatedtristyrylphenol 2.00 Emulsifier
Nonionic proprietary surfactant blend 2.00 Dispersing agent
Acrylic copolymer 2.00 Dispersing agent
Propane-1,2,3-triol 6.50 Anti freezing Agent
Dipropylene glycol solution of 1,2-benzisothiazolin-3-one 0.10 Biocide
Polydimethylsiloxane emulsion 0.30 Antifoaming agent
Citric acid 0.2 pH stabilizer
Sodium benzoate 0.5 Stabilizing agent
Rhodopol 23 0.06 Rheology modifier
Demineralizedwater Q.S Solvent

Process for Preparing the Suspo-emulsion (SE) Formulation:
The preparation of suspo-emulsion formulation was completed in three phases-
1. Preparation of Etofenprox Oil Phase-
The active ingredient Etofenprox was mixed with the polyalkoxylated butyl ether block co-polymer and ethoxylated tristyrylphenol under stirring to form the Etofenprox oil phase.
2. Preparation of Aqueous Phase of Diafenthiuron and Acetamiprid-
In demineralized water, the constituents, namely the dipropylene glycol solution of 1,2-benzisothiazolin-3-one, polydimethylsiloxane emulsion, propane-1,2,3-triol, nonionic proprietary surfactant blend, and acrylic copolymer as mentioned in Table 1, were added into a clean pre-mixing vessel fitted with a homogenizer. All the ingredients were mixed for a sufficient time with the homogenizer to obtain a uniform mixture. The active ingredients, Acetamiprid and Diafenthiuron, were then added to this mixture, and mixing was continued for an adequate duration with the homogenizer to form a slurry. The slurry was passed through a jacketed bead mill with chilled water circulation for particle size reduction, achieving an aqueous phase of Diafenthiuron and Acetamiprid with a desirable particle size of d(90) < 20 microns. The aqueous phase of Diafenthiuron and Acetamiprid was collected into a mixing vessel equipped with a stirrer.
3. Final step preparation of Suspo-emulsion (SE) Formulation-
The Etofenprox oil phase was added to the aqueous phase of Diafenthiuron and Acetamiprid under continuous agitation for an optimal amount of time at room temperature. A suitable quantity of pH adjuster, stabilizer, and Rhodopol 23 was then introduced into the mixture. The mixture was continuously agitated for the appropriate duration to form the insecticidal Suspo-emulsion (SE) formulation.
Example 2: Oil Dispersion (OD) Formulation-
The Oil Dispersion (OD) Formulation was meticulously prepared in accordance with the present disclosure, utilizing the components outlined in Table 2.
Table 2: Oil Dispersion (OD) Formulation
Component Composition (%w/w) Remark
Etofenprox 7.2 Active Ingredient
Diafenthiuron 29.7 Active Ingredient
Acetamiprid 6.0 Active Ingredient
Castor oil ethoxylate(10 mole) 6.00 Emulsifier
Calcium dodecylbenzenesulfonate 2.00 Emulsifier
Mixture of fatty acid polyethylene glycol ester 4.00 Emulsifier
Polymeric ester dispersant 0.5 Dispersing agent
Ethoxylated polyarylphenol phosphate ester 0.5 Dispersing agent
Propane-1,2,3-triol 2.00 Antifreezing Agent
Polyalkyleneoxide modified heptamethyltrisiloxane 1.00 Super-Wetting-spreading-penetrating agent
Polydimethylsiloxane 0.30 Antifoaming agent
Fumed silica 1.50 Rheology modifier
Citric acid 0.10 pH stabilizer
Bentonite clay 1.50 Rheology modifier
Methyl ester of vegetable oil Balance to 100 Solvent

Process for Preparing the Oil Dispersion (OD) Formulation:
In methyl ester of vegetable oil, the constituents—namely polyalkyleneoxide modified heptamethyltrisiloxane, polydimethylsiloxane, propane-1,2,3-triol, castor oil ethoxylate (10 mole), calcium dodecylbenzenesulfonate, ethoxylated polyarylphenol phosphate ester, a mixture of fatty acid polyethylene glycol ester, and polymeric ester dispersant were added into a clean pre-mixing vessel equipped with a homogenizer. All the ingredients were mixed for a sufficient time with the homogenizer to obtain a uniform mixture.
The active ingredients, Etofenprox, Diafenthiuron, and Acetamiprid, were then introduced into the obtained mixture, and mixing was continued for an adequate duration with the homogenizer to form a slurry. The slurry was passed through a jacketed bead mill with chilled water circulation for particle size reduction, achieving a milled slurry with the desired particle size of d(90) < 20 microns. The milled slurry was subsequently collected into a post-mixing vessel fitted with a stirrer.
To the milled slurry, the pH stabilizer, bentonite clay, and fumed silica were added under stirring in the post-mixing vessel. Mixing was continued for a sufficient time to ensure proper incorporation, resulting in the formation of the insecticidal Oil Dispersion (OD) formulation.
Example 3: Oil Dispersion (OD) Formulation-
The Oil Dispersion (OD) Formulation was meticulously prepared in accordance with the present disclosure, utilizing the components outlined in Table 3.
Table 3: Oil Dispersion (OD)Formulation
Component Composition (%w/w) Remark
Etofenprox 7.2 Active Ingredient
Diafenthiuron 29.7 Active Ingredient
Acetamiprid 6.0 Active Ingredient
Ethoxylated polyarylphenol phosphate ester 0.5 Dispersing agent
Polydimethylsiloxane 0.30 Antifoaming agent
Citric acid 0.1 pH stabiliser
Sodium benzoate 0.5 Stabilising agent
Prop-UP 2.0 Rheology modifier
Emulsion All OD Q.S Proprietary blend of solvent and emulsifiers
Process for Preparing the Oil Dispersion (OD) Formulation:
Add polydimethylsiloxane, ethoxylated polyarylphenol phosphate ester and active ingredients, Etofenprox, Diafenthiuron, and Acetamiprid, were then introduced into the obtained mixture, and mixing was continued for an adequate duration with the homogenizer to form a slurry. The slurry was passed through a jacketed bead mill with chilled water circulation for particle size reduction, achieving a milled slurry with the desired particle size of d(90) < 20 microns. The milled slurry was subsequently collected into a post-mixing vessel fitted with a stirrer were added into a clean pre-mixing vessel equipped with a homogenizer. All the ingredients were mixed for a sufficient time with the homogenizer to obtain a uniform mixture.
To the milled slurry, the pH stabilizer, stabilising agent and rheology modifier were added under stirring in the post-mixing vessel. Mixing was continued for a sufficient time to ensure proper incorporation, resulting in the formation of the insecticidal Oil Dispersion (OD) formulation.
Example 4: Bioefficacy of an Insecticidal Composition and thereof (Etofenprox + Diafenthiuron + Acetamiprid) on cotton and chilli crops.
Synergistic effect was checked using Colby’s method for ternary mixes. In the Colby’s method, for a given combination of three active components, E (expected efficacy) can be expressed as:
E = A + B + C – (AB + AC + BC) + (ABC)
1000 100

Where, E = expected efficacy,
A, B and C = the efficacy of three active ingredients A, B and C at a given dose.
Synergy ratio (R) = Experimentally observed efficacy (O)
Expected efficacy (E)
If the synergism ratio (R) between observed and expected is >1 then synergy is exhibited, if R=1 then the effect is additive and if R<1 then the mix is antagonistic.
The experimental data was statistically analysed by Randomized Block Design (RBD) (One factor analysis) using OPSTAT HAU statistical software. The results are expressed as Mean ± SE (standard error) and data was statistically analysed by one-way Analysis of variance (ANOVA), with the level of significance set at p < 0.01.
Phytotoxicity observations
For the evaluation of phytotoxicity on cotton & chilli crops, observations were made by observing the temporary or long lasting damage to the leaves if any viz., yellowing, wilting, necrosis, epinasty and hyponasty at 5, 10 and 15 DAS of the synergistic insecticidal composition of the present invention. Crop injury was observed on visual rating from 0-10 scale as presented in Table 4.
Table 4.Phytotoxicity rating scale
Rating Crop Injury (%) Description
0 - No symptoms
1 1-10 Slight discoloration
2 11-20 More severe, but not lasting
3 21-30 Moderate and more lasting
4 31-40 Medium and lasting
5 41-50 Moderately heavy
6 51-60 Heavy
7 61-70 Very heavy
8 71-80 Nearly destroyed
9 81-90 Destroyed
10 91-100 Completely destroyed

Cotton (Gossypium spp.) is one of the most important fiber and cash crop of India. It is a good source of fibre and edible oil and plays a dominant role in the industrial and agricultural economy of the country. Insect pests infesting cotton can cause significant damage to the crop, leading to lower yields and economic losses. The cotton crop is home to a variety of insects, the most damaging of which is bollworms and sucking pests. Important sucking insect pests of cotton crop are jassid (Amrascabiguttulabiguttula), whitefly (Bemisiatabaci), thrips (Thrips tabaci) and aphid (Aphis gossypii).
Table 5: Effect of different treatments on the population of whitefly in cotton.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Whitefly per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 9.13 (3.18) 9.53 (3.24) 11.37 (3.51) 13.03 (3.74) 32.55 28.39 - -
2 Diafenthiuron 50% WP 300 600 6.57 (2.75) 6.47 (2.73) 7.77 (2.95) 9.20 (3.19) 54.25 49.45 - -
3 Acetamiprid 20% SP 60 300 7.83 (2.97) 8.13 (3.02) 9.73 (3.27) 11.13 (3.48) 42.45 38.83 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 1.90 (1.70) 1.50 (1.57) 1.90 (1.70) 2.30 (1.81) 89.39 87.36 1.08 1.12
5 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 40.30 + 162.50 + 35.10 650 3.60 (2.14) 3.67 (2.15) 3.87 (2.20) 4.87 (2.42) 74.06 73.26 0.90 0.94
6 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 46.50 + 187.50 + 40.50 750 3.20 (2.04) 3.23 (2.05) 3.40 (2.09) 4.23 (2.28) 77.12 76.74 0.93 0.98
7 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 52.70 + 212.50 + 45.90 850 3.00 (1.98) 2.90 (1.97) 3.20 (2.04) 4.17 (2.27) 79.48 77.11 0.96 0.99
8 Untreated Check - - 13.17 (3.76) 14.13 (3.89) 16.60 (4.19) 18.20 (4.38) - - - -
CD at 5% - - 0.19 0.17 0.16 0.22 - - - -
SE (m) - - 0.06 0.05 0.05 0.07 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray
Among all the treatments the tank-mix combinations of Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha was observed with highest per cent controlof the population of whitefly recorded with 89.39% and87.36% control at 5th and 10th day after spray, respectively followed by Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% @ 52.70 + 212.50 + 45.90 gm a.i./ha, Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% @ 46.50 + 187.50 + 40.50 gm a.i./ha and Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%@ 40.30 + 162.50 + 35.10 gm a.i./ha. All the doses of pre-mix formulation of Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%applied @52.70 + 212.50 + 45.90 gm a.i./ha,46.50 + 187.50 + 40.50 gm a.i./ha and 40.30 + 162.50 + 35.10 gm a.i./ha observed with 77.11%, 76.74% and 73.26% reduction over untreated control at 10th DAS, respectively.
All the doses of Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @300 gm a.i./ha (49.45%), Acetamiprid 20% SP@ 60 gm a.i./ha (38.83%) and Etofenprox 10% EC @ 75 gm a.i./ha (28.39%) against whitefly of cotton at 10th day after spray. Among the treatments only tank-mix combination of Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha showed synergistic effect with the synergistic ratio 1.12 (>1) at 10 DAS. (Table 5).

Table 6: Effect of different treatments on the population of whitefly in cotton.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Whitefly per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 7.80 (2.96) 9.57 (3.25) 10.77 (3.43) 12.33 (3.65) 33.41 29.39 - -
2 Diafenthiuron 50% WP 300 600 6.07 (2.65) 6.83 (2.79) 7.90 (2.98) 9.37 (3.21) 52.44 46.37 - -
3 Acetamiprid 20% SP 60 300 6.77 (2.78) 8.17 (3.02) 9.03 (3.16) 10.60 (3.40) 43.16 39.31 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 1.53 (1.59) 1.67 (1.63) 1.67 (1.63) 2.20 (1.78) 88.40 87.40 1.07 1.13
5 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 46.80 + 193.05 + 39 650 2.77 (1.94) 3.07 (2.01) 3.57 (2.13) 4.40 (2.32) 78.65 74.81 0.95 0.97
6 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 54 + 222.75 + 45 750 1.23 (1.49) 1.27 (1.50) 1.00 (1.41) 1.50 (1.57) 91.18 91.41 1.11 1.18
7 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 61.20 + 252.45 + 51 850 1.03 (1.42) 1.10 (1.44) 0.83 (1.35) 1.20 (1.48) 92.34 93.13 1.12 1.20
8 Untreated Check - - 11.53 (3.54) 14.37 (3.92) 15.67 (4.08) 17.47 (4.29) - - - -
CD at 5% - - 0.18 0.18 0.16 0.21 - - - -
SE (m) - - 0.06 0.06 0.05 0.07 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray

Among all the doses of combination and individual treatments, Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 61.20 + 252.45 + 51 gm a.i./hawas observed with highest per cent control of whitefly population recorded with 93.13% control at 10th DAS and found at par with Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 54 + 222.75 + 45 gm a.i./ha (91.41%) and Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha (87.40%) followed by Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 46.80 + 193.05 + 39 gm a.i./ha (74.81%) at 10th DAS.
All the doses of Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @300 gm a.i./ha (46.37%), Acetamiprid 20% SP@ 60 gm a.i./ha (39.31%) and Etofenprox 10% EC @ 75 gm a.i./ha (29.39%) against whitefly of cotton at 10th day after spray. Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 54 + 222.75 + 45 gm a.i./ha showed synergistic effect with the synergistic ratio1.18 (>1) at 10 DAS. (Table 6).

Table 7: Effect of different treatments on the population of whitefly in cotton.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Whitefly per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 9.26 (3.20) 9.60 (3.25) 11.47 (3.53) 12.40 (3.66) 32.55 29.55 - -
2 Diafenthiuron 50% WP 300 600 6.63 (2.76) 6.63 (2.76) 8.07 (3.01) 9.03 (3.16) 53.40 48.67 - -
3 Acetamiprid 20% SP 60 300 7.60 (2.93) 8.03 (3.00) 9.93 (3.30) 10.80 (3.43) 43.56 38.64 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 1.67 (1.63) 1.63 (1.61) 1.80 (1.67) 2.17 (1.77) 88.52 87.69 1.07 1.12
5 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 53.30 + 227.50 + 44.20 650 3.33 (2.08) 3.50 (2.11) 3.90 (2.21) 5.07 (2.46) 75.41 71.21 0.91 0.91
6 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 61.50 + 262.50 + 51 750 1.27 (1.50) 1.13 (1.45) 1.03 (1.42) 1.37 (1.53) 92.04 92.23 1.11 1.18
7 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 69.70 + 297.50 + 57.80 850 1.00 (1.41) 0.90 (1.37) 0.60 (1.26) 1.10 (1.44) 93.68 93.75 1.13 1.20
8 Untreated Check - - 13.17 (3.76) 14.23 (3.90) 16.70 (4.20) 17.60 (4.31) - - - -
CD at 5% - - 0.18 0.17 0.14 0.16 - - - -
SE (m) - - 0.06 0.05 0.04 0.05 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray
Among all the doses of combination and individual treatments, Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 69.70 + 297.50 + 57.80 gm a.i./hawas observed with highest per cent control of whitefly recorded with 93.75% control and found at par with Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 61.50 + 262.50 + 51 gm a.i./ha (92.23%) and Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha (87.69%) followed by Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 53.30 + 227.50 + 44.20 gm a.i./ha (71.21%) at 10th DAS.
All the doses of Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @ 300 gm a.i./ha (48.67%), Acetamiprid 20% SP@ 60 gm a.i./ha (38.64%) and Etofenprox 10% EC @ 75 gm a.i./ha (29.55%) against whitefly of cotton at 10th day after spray. T4, T6& T7showed synergistic effect with the synergistic ratio 1.12, 1.18& 1.20 (>1) at 10 DAS, respectively. (Table 7).

Table 8: Effect of different treatments on the population of thrips in chilli.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Thrips per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 4.20 (2.27) 4.77 (2.40) 5.40 (2.52) 7.10 (2.84) 36.44 31.51 - -
2 Diafenthiuron 50% WP 300 600 2.90 (1.97) 3.13 (2.03) 3.60 (2.14) 4.80 (2.40) 58.22 53.70 - -
3 Acetamiprid 20% SP 60 300 3.60 (2.14) 4.10 (2.25) 4.67 (2.37) 6.17 (2.67) 45.33 40.51 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 0.73 (1.31) 0.57 (1.25) 0.70 (1.30) 1.23 (1.49) 92.44 88.10 1.08 1.08
5 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 40.30 + 162.50 + 35.10 650 1.57 (1.59) 1.70 (1.63) 1.77 (1.66) 2.53 (1.87) 77.33 75.56 0.90 0.93
6 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 46.50 + 187.50 + 40.50 750 1.47 (1.56) 1.47 (1.56) 1.43 (1.56) 2.10 (1.76) 80.44 79.74 0.94 0.98
7 Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% 52.70 + 212.50 + 45.90 850 1.37 (1.53) 1.33 (1.52) 1.37 (1.53) 2.00 (1.73) 82.22 80.71 0.96 0.99
8 Untreated Check - - 6.40 (2.72) 7.50 (2.91) 8.27 (3.04) 10.37 (3.37) - - - -
CD at 5% - - 0.20 0.19 0.20 0.20 - - - -
SE (m) - - 0.06 0.06 0.06 0.06 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray

Among all the treatments the tank-mix combinations of Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha was observed with highest per cent controlof the population of thrips recorded with 92.44% and88.10% control at 5th and 10th day after spray, respectively followed by Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% @ 52.70 + 212.50 + 45.90 gm a.i./ha, Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% @ 46.50 + 187.50 + 40.50 gm a.i./ha andEtofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4% @ 40.30 + 162.50 + 35.10 gm a.i./ha. All the doses of pre-mix formulation of Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%applied @52.70 + 212.50 + 45.90 gm a.i./ha,46.50 + 187.50 + 40.50 gm a.i./ha and 40.30 + 162.50 + 35.10 gm a.i./ha observed with 80.71%, 79.74% and 75.56% reduction over untreated control at 10th DAS, respectively.
All the doses of Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @300 gm a.i./ha (53.70%), Acetamiprid 20% SP@ 60 gm a.i./ha (40.51%) and Etofenprox 10% EC @ 75 gm a.i./ha (31.51%) against thrips of chilli at 10th day after spray. Among the treatments only tank-mix combination of Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha showed synergistic effect with the synergistic ratio 1.08 (>1) at 10 DAS. (Table 8).

Table 9: Effect of different treatments on the population of thrips in chilli.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Thrips per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 4.67 (2.37) 5.40 (2.52) 6.17 (2.67) 7.00 (2.82) 36.22 30.46 - -
2 Diafenthiuron 50% WP 300 600 3.57 (2.13) 3.77 (2.17) 4.33 (2.30) 4.97 (2.44) 55.51 50.66 - -
3 Acetamiprid 20% SP 60 300 4.03 (2.24) 4.53 (2.35) 5.27 (2.50) 5.93 (2.63) 46.46 41.06 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 0.77 (1.32) 0.73 (1.31) 0.90 (1.37) 1.20 (1.48) 91.34 88.08 1.07 1.10
5 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 46.80 + 193.05 + 39 650 1.50 (1.57) 1.60 (1.60) 2.00 (1.73) 2.37 (1.83) 81.10 76.49 0.95 0.95
6 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 54 + 222.75 + 45 750 0.57 (1.24) 0.57 (1.25) 0.70 (1.30) 1.00 (1.41) 93.31 90.07 1.10 1.12
7 Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% 61.20 + 252.45 + 51 850 0.40 (1.18) 0.40 (1.18) 0.63 (1.27) 0.77 (1.32) 95.28 92.38 1.12 1.15
8 Untreated Check - - 7.23 (2.86) 8.47 (3.07) 9.27 (3.20) 10.07 (3.32) - - - -
CD at 5% - - 0.20 0.20 0.17 0.19 - - - -
SE (m) - - 0.06 0.06 0.05 0.06 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray

Among all the doses of combination and individual treatments, Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 61.20 + 252.45 + 51 gm a.i./hawas observed with highest per cent control of thrips population recorded with 92.38% control at 10th DAS and found at par with Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 54 + 222.75 + 45 gm a.i./ha (90.07%) and Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha (88.08%) followed by Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@ 46.80 + 193.05 + 39 gm a.i./ha (76.49%) at 10th DAS.
All the doses of Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @300 gm a.i./ha (50.66%), Acetamiprid 20% SP@ 60 gm a.i./ha (41.06%) and Etofenprox 10% EC @ 75 gm a.i./ha (30.46%) against thrips of chilli at 10th day after spray. Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%@54 + 222.75 + 45 gm a.i./ha showed synergistic effect with the synergistic ratio1.12 (>1) at 10 DAS. (Table 9).

Table 10: Effect of different treatments on the population of thrips in chilli.
Sr. No.
Treatment Compositions Dosage/ha Average no. of Thrips per leaf Per cent reduction over control Colby’s synergistic ratio
Dosage/ha
a.i. (gm) Formulation (gm/ml) 3 DAS 5 DAS 7 DAS 10 DAS % Control
5 DAS % Control
10 DAS 5 DAS 10 DAS
1 Etofenprox 10% EC 75 750 4.23 (2.28) 4.43 (2.33) 5.07 (2.46) 6.00 (2.64) 34.16 31.03 - -
2 Diafenthiuron 50% WP 300 600 3.07 (2.01) 2.90 (1.97) 3.30 (2.07) 4.13 (2.26) 56.93 52.49 - -
3 Acetamiprid 20% SP 60 300 3.57 (2.13) 3.67 (2.15) 4.37 (2.31) 5.10 (2.47) 45.54 41.38 - -
4 Etofenprox 10% EC + Diafenthiuron 50% WP+ Acetamiprid 20% SP 75 + 300 + 60 750+600+300 0.83 (1.35) 0.63 (1.27) 0.60 (1.26) 0.80 (1.33) 90.59 90.80 1.07 1.12
5 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 53.30 + 227.50 + 44.20 650 1.57 (1.59) 1.50 (1.57) 1.67 (1.62) 2.30 (1.81) 77.72 73.56 0.91 0.91
6 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 61.50 + 262.50 + 51 750 0.40 (1.18) 0.37 (1.16) 0.53 (1.23) 0.73 (1.31) 94.55 91.57 1.09 1.13
7 Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8% 69.70 + 297.50 + 57.80 850 0.27 (1.12) 0.23 (1.11) 0.43 (1.19) 0.53 (1.23) 96.53 93.87 1.10 1.16
8 Untreated Check - - 6.07 (2.65) 6.73 (2.77) 7.83 (2.97) 8.70 (3.11) - - - -
CD at 5% - - 0.18 0.19 0.19 0.19 - - - -
SE (m) - - 0.06 0.06 0.06 0.06 - - - -
Figure in parenthesis represents square root transformed value; DAS: Days After Spray

Among all the doses of combination and individual treatments, Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 69.70 + 297.50 + 57.80 gm a.i./hawas observed with highest per cent control of thrips recorded with 93.87% control and found at par with Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 61.50 + 262.50 + 51 gm a.i./ha (91.57%) and Etofenprox 10% EC @ 75 gm a.i./ha + Diafenthiuron 50% WP @ 300 gm a.i./ha + Acetamiprid 20% SP @ 60 gm a.i./ha (90.80%) followed by Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%@ 53.30 + 227.50 + 44.20 gm a.i./ha (73.56%) at 10th DAS.
All the doses of Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%showed better efficacy compared to the individual applications of Diafenthiuron 50% WP @300 gm a.i./ha (52.49%), Acetamiprid 20% SP@ 60 gm a.i./ha (41.38%) and Etofenprox 10% EC @ 75 gm a.i./ha (31.03%) against thrips of chilli at 10th day after spray. T4, T6& T7showed synergistic effect with the synergistic ratio 1.12, 1.13& 1.16 (>1) at 10 DAS, respectively. (Table 10).
Phytotoxicity observations
Various insecticidal compositions of the present invention provided good control of cotton whitefly as well as chilli thrips as compared to the reference products. Further, the use of these insecticidal compositions resulted in better crop condition i.e. fresh green leaves and didn’t produce any phytotoxic symptoms on the plants. Table 8-13 depicts the phytotoxic effects of the various insecticidal compositions of the present invention on cotton and chilli at 5th, 10th and 15th DAS.

Table 11: Phytotoxic effects of the insecticidal combination of “Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%on cotton
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Table 12: Phytotoxic effects of the insecticidal combination of “Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%on cotton
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Table 13: Phytotoxic effects of the insecticidal combination of “Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%” on cotton
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Table 14: Phytotoxic effects of the insecticidal combination of “Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%” on chilli
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Table 15: Phytotoxic effects of the insecticidal combination of “Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%” on chilli
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Table 16: Phytotoxic effects of the insecticidal combination of “Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%” on chilli
Treatments Phytotoxicity rating
Yellowing Wilting Necrosis Epinasty Hyponasty
Days After Spray
3 7 10 3 7 10 3 7 10 3 7 10 3 7 10
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Conclusion
After evaluation of three formulations i.e., Etofenprox 6.2% + Diafenthiuron 25% + Acetamiprid 5.4%, Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6%and Etofenprox 8.2% + Diafenthiuron 35% + Acetamiprid 6.8%at three different doses (650 ml/ ha, 750 ml/ha &850 ml/ha). Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% @ 750 ml/ha found to be effective against whitefly of cotton and thrips of chilli crops in comparison to Tank mix formulation (Etofenprox 10% EC + Diafenthiuron 50% WP + Acetamiprid 20% SP) as well as solo treatments (Etofenprox 10% EC, Diafenthiuron 50% WP and Acetamiprid 20% SP). Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% @ 750 ml/ha was found at par with higher formulation, higher dose and higher active ingredient.
Therefore, application of Etofenprox 7.2% + Diafenthiuron 29.70% + Acetamiprid 6% @ 750 ml/ha (54 + 222.75 + 45 gm a.i./ ha) formulation can be recommended for effective control of whitefly in cotton and thrips in chilli crops.
, Claims:
1. An insecticidal composition comprising a synergistic combination of-
a. an Etofenprox in an amount ranging from 0.1% to 30.0% by weight;
b. a Diafenthiuron is present in an amount ranging from 0.1% to 50.0% by weight;
c. an Acetamiprid is present in an amount ranging from 0.1% to 30.0% by weight; and
d. agrochemical acceptable excipient.
2. The insecticidal composition as claimed in claim 1, wherein Etofenprox is present in an amount of 7.2% w/w,Diafenthiuron is present in an amount of 29.7% w/w and Acetamiprid is present in an amount of 6 % w/w.
3. The insecticidal composition as claimed in claim 1 wherein, the agrochemically acceptable excipient is Emulsifier, Dispersing agent, Antifreezing Agent, Adjuvant, Antifoaming agent, Super-Wetting-spreading-penetrating agent, Rheology modifier, pH stabilizer, Solvent and Biocide.
4. The insecticidalcomposition as claimed in claim 1, wherein the formulation is selected from a suspension concentrate (SC), flowable suspension for seed treatment (FS), oil dispersion (OD), suspo-emulsion (SE), water-dispersible granule (WDG), or wettable powder (WP).
5. The insecticidal composition as claimed in claim 1, wherein the emulsifier is in an amount ranging from 0.1% to 20.0% by weight, selected from selected from but not limited to ethoxylatedpropoxylated alcohols, alkylphenolethoxylates, alkoxylatedtristyrylphenols, calcium dodecylbenzenesulfonate,Polyalkoxylated butyl ether block co-polymer,ethoxylatedpropoxylatedpolyaryl phenol, ethoxylated fatty acids, fatty alcohol ethoxylates, ethoxylatedricinoleic acid triglycerides, sorbitan trioleate, tridecyl alcohol ethoxylate, castor oil ethoxylate, alkoxylated phosphate ester.
6. The insecticidal composition as claimed in claim 1, wherein the dispersing agent is in an amount ranging from 0.1% to 20.0% by weight, selected from selected from but not limited to polymeric ester dispersants, ethoxylated polyarylphenol phosphate esters, or sodium salt of naphthalene sulfonatecondensate, acrylic copolymer,nonionic proprietary surfactant blend, polycarboxylates, calcium dodecylbenzene sulfonate, sodium lignosulphonate, polystyrenatedacrylated co-polymer, modified styrene acrylic copolymer, salts of phenol sulfonic acids, butyl polyalkylene oxide block co-polymer, mixture of tristyrylphenolethoxylates and polyalkylene oxide derivative of a synthetic alcohol,random co-polymer of alcoxylated polyethylene glycol.
7. The insecticidal composition as claimed in claim 1, wherein the antifoaming agent is in an amount ranging from 0.01% to 5.0% by weight, selected from selected from but not limited to polydimethylsiloxane or polydimethyl siloxane emulsion.
8. The insecticidal composition as claimed in claim 1, wherein the rheology modifier is in an amount ranging from 0.01% to 20.0% by weight, selected from precipitated silica, fumed silica, modified fumed silica, bentonite clay, Rhodopol 23, hydroxymethyl cellulose, carboxymethyl cellulose, xanthan gum, thickening silica, hydrated clay minerals, magnesium aluminium silicates, organic derivative of hectorite clay, hydrophobic fumed silica, polyvinylpyrrolidone.
9. The insecticidal compositionas claimed in claim 1, wherein the solvent component in an amount rangingup to 95.0% of the composition by weight, selected from selected from but not limited to demineralized water or oil media, wherein, oil medium selected from the group comprising, esterified fatty acids selected from methylethyl ester ofvegetable oil triglycerides containing C12–C22 saturated and unsaturated fatty acid.
10. The insecticidal composition as claimed in claim 1, wherein the biocide is in an amount ranging up to3.0% by weight, selected from but not limited to 1,2-benzisothiazolin-3-one or formaldehyde-based solutions or dipropylene glycol solution of 1,2-benzisothiazolin-3-one.
11. The insecticidal composition as claimed in claim 1, wherein the antifreezing agent is in an amount ranging up to 15% by weight, selected from but not limited to ethylene glycol or propane-1,2-diol or propane-1,2,3-triol, urea.
12. The insecticidal composition as claimed in claim 1, wherein the stabilizing agent is in an amount ranging up to 5% by weight, selected from but not limited to epoxidized soyabean oil, butylated hydroxy toluene, ethylenediaminetetraacetic acid.
13. The insecticidal composition as claimed in claim 1, wherein the pH modifier is in an amount ranging up to 5% by weight, selected from but not limited to sodium pyrophosphate, sodium acetate, sodium oxalate, sodium carbonate, sodium bicarbonate, trisodium phosphate, citric acid, trisodium citrate, monoethanol amine, triethanol amine, triethylamine, dibasic esters selected from dimethyl succinate, dimethyl glutarate, dimethyl adipate, ortho phosphoric acid, oxalic acid, citric acid, hydrochloric acid.
14.The insecticidal composition as claimed in claim 1, wherein the the Super-Wetting-spreading-penetrating agent is blend of methylated seed oil-organic silicone compound may be selected from methylated seed oil-polyalkyleneoxide modified trisiloxane, methylated seed oil-polyalkyleneoxide modified polydimethylsiloxane, methylated seed oil-20 trisiloxane ethoxylate, Polyalkyleneoxide modified heptamethyltrisiloxane methylated seed oil-polyoxyethylene methyl polysiloxane, methylated seed oil-polyether polymethyl siloxane copolymer, methylated seed oil-polyether modified polysiloxane.
15. A process for preparing a Suspo-emulsion insecticidal composition comprising the steps of-
a. Mixing Etofenprox with polyalkoxylated butyl ether and ethoxylated tristyrylphenol to create the Etofenprox oil phase.
b. adding dipropylene glycol solution of 1,2-benzisothiazolin-3-one, polydimethylsiloxane emulsion, propane-1,2,3-triol, a nonionic surfactant blend, and acrylic copolymer to demineralized water in a pre-mixing vessel with a homogenizer.
c. homogenizing the mixture until uniform.
d. Acetamiprid and Diafenthiuron, and mixing to obtain a slurry.
e. reducing the particle size of the slurry using a jacketed bead mill to achieve d(90) less than 20 microns.
f. collecting the aqueous phase into a mixing vessel.
g. adding the Etofenprox oil phase to the aqueous phase under continuous agitation.
h. incorporating a pH adjuster, stabilizer, and Rhodopol 23, then agitating to form the insecticidal suspo-emulsion composition.
16. A process for preparing an Oil-dispersion insecticidal composition comprising the steps of-
a. adding polyalkylene oxide modified heptamethyltrisiloxane, polydimethylsiloxane, propane-1,2,3-triol, castor oil ethoxylate, calcium dodecylbenzenesulfonate, ethoxylated polyarylphenol phosphate ester, and a fatty acid polyethylene glycol ester mixture to methyl ester of vegetable oil in a pre-mixing vessel with a homogenizer.
b. mixing until uniform.
c. incorporating Etofenprox, Diafenthiuron, and Acetamiprid, and mixing to create a slurry.
d. reducing the particle size of the slurry using a jacketed bead mill to achieve d(90) less than 20 microns.
e. collecting the milled slurry into a post mixing vessel.
f. adding a pH stabilizer, bentonite clay, and fumed silica under stirring.
g. mixing until homogeneous to form the insecticidal Oil-dispersion formulation.