DESC:A STABLE INSECTICIDAL COMPOSITION AND PREPARATION PROCESS THEREOF

FIELD OF THE INVENTION
The present invention relates to the field of agricultural pesticides and, more particularly, to a stable insecticidal composition and process of preparation thereof.

BACKGROUND OF THE INVENTION
Controlling invertebrate pests is essential for improved crop efficiency in economically important crops. These pest not only inflict damage on growing and harvested agronomic crops but also lead substantial reductions in crop yields. The pest management strategies to manage invertebrate pests involve using single active components or mixtures of two or more active compounds. However, there remains a significant demand for more cost-effective and stable insecticidal compositions.

Further, repeated and prolonged application of single compounds often leads to the development of resistance against the active compounds. Normally, such pests develop cross-resistance against other actives with the same or similar mode of action. Hence, there is a need for combinations of actives belonging to different classes and groups to allow for a broader disease control spectrum that combines curative and preventive actives and is stable.

There is an urgent need for a stable, synergistic, and environment friendly insecticidal composition. The composition should provide effective control across a wide array of insect pests, thereby preventing the emergence of resistant strains. Furthermore, it should also offer a broad-spectrum activity that minimizes the number of chemicals applied in fields, aligning with sustainable agricultural practices. Another critical factor for the composition is their stability under diverse environmental conditions, including the ability to remain effective at low temperatures where conventional actives may degrade or perform sub-optimally. This stability ensures that the composition's efficacy is preserved from the point of manufacture through to application, irrespective of climatic variations.

The present invention provides a composition that not only counteracts the resilience tactics of pests through a multi-class active strategy but also ensures consistent performance across a comprehensive temperature spectrum.
OBJECTIVES OF THE INVENTION
The primary objective of the invention is to provide an insecticidal composition with an improved spectrum of activity.

Another objective of the present invention is to provide insecticidal composition for resistance management.

Another objective of the present invention is to provide a stable, synergistic insecticidal composition.

Another objective of the present invention is to provide a stable synergistic insecticidal composition, especially at low temperatures.

Yet another objective of the present invention is to provide a synergistic insecticidal composition with improved stability for extended shelf life.

Another objective of the present invention is to provide a process for preparation of the synergistic insecticidal composition.

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

SUMMARY OF THE INVENTION

The present invention aims to provide an insecticidal composition comprising dinotefuran, bifenthrin, an emulsifying system and a co-solvent.

In another aspect of the present invention the emulsifying system comprises a blend having Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol NP Ethoxylate, heavy aromatic & Triethylene Glycol Monoethyl Ether, Castor Oil Ethoxylate, and n-Butanol.

In yet another aspect of the present invention, the emulsifying system comprises a blend having Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol, NP Ethoxylate, Heavy Aromatic & Triethylene Glycol Monoethyl Ether.
In further aspect of the present invention, the insecticidal composition comprises of
dinotefuran is present in an amount of 1 to 40% by weight;
bifenthrin is present in an amount of 1 to 40% by weight;
the emulsifying system is present in an amount of 1 to 30% by weight; and
the co-solvent is present in an amount of 1 to 60% by weight.

In a preferred embodiment of the present invention, the co-solvent is N-Methyl-2-pyrrolidone.

In further aspect of the present invention, the insecticidal composition comprises of: dinotefuran;
bifenthrin;
an emulsifying system;
a co-solvent; and
a solvent.

In another aspect of the present invention, the solvent is a mixed isomer of benzene, 1, 2, 4-trimethyl and benzene, ethylmethyl (C9 Solvent).

In further aspect of the present invention, the composition further comprises carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, stabilizers or any combination thereof.

In another aspect, the present invention provides a process for preparation of insecticidal composition, the process comprises of
a) weighing of required quantity of co-solvent;
b) adding dinotefuran to co-solvent under stirring to form a mixture;
c) sequentially adding a solvent and bifenthrin to the above mixture under continuous stirring; and
d) adding an emulsifying system into the mixture of step c) under stirring to obtain a final insecticidal composition.

In an aspect of the present invention, the mixture of step b) is stirred at a speed of 100 RPM for a duration ranging from 40-60 minutes.
In yet another aspect of the present invention, the composition comprises addition of carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, stabilizers or any combination thereof.

DETAILED DESCRIPTION OF THE INVENTION
The terms “formulation” and “composition” as used herein convey the same meaning and may be used interchangeably.

The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total solution or composition, unless otherwise specified.

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

The term “active ingredient” (a.i.) or “active agent” or “actives” used herein refers to that component of the composition responsible for the control of insect pests.

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

As used herein, the term “insecticide” or “pesticide”, refers to any chemical substance used to destroy or kill, inhibit, or otherwise adversely affect insect pests.

As used herein, the term "stable" refers to chemical and/or physical stabilization of an active compound.

As used herein, the term “Low temperatures” refers to a temperature below 10° C, preferably below 5° C, more preferable below 0° C, and most preferably it is -10° C.

Accordingly, the present invention aims to provide a synergistic insecticidal composition comprising at least one active compound selected from pyrethroid compounds and neonicotinoid compounds.

In another embodiment, the present invention provides a process for the preparation of a synergistic composition comprising dinotefuran and at least one pyrethroid compound.

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

In another exemplary embodiment, the composition comprises neonicotinoid compounds in the range of 1 to 60% w/w of the composition and pyrethroid compounds in the range of 1-50% w/w of the composition.

In an exemplary embodiment, the present invention provides a synergistic insecticidal composition comprising dinotefuran and bifenthrin.

In an exemplary embodiment, the synergistic insecticidal composition of the present invention is stable over a wide range of temperatures.

In another exemplary embodiment, the synergistic insecticidal composition of the present invention is efficacious and stable at low-temperatures.

The inventors have surprisingly found that the composition in the aforementioned weight percentage ranges provides a synergistic effect.

In an embodiment, the synergistic insecticidal composition comprises of dinotefuran in the range of 1 to 40% by weight and bifenthrin in the range of 1 to 40% by weight.

In an embodiment, the synergistic insecticidal composition comprises of dinotefuran, bifenthrin, and an emulsifying system.

In an embodiment, the synergistic insecticidal composition comprises of dinotefuran, bifenthrin, an emulsifying system and a co-solvent.
In another embodiment of the present invention, the synergistic insecticidal composition comprises of dinotefuran is present in an amount of 1 to 40% by weight, bifenthrin is present in an amount of 1 to 40% by weight, the emulsifying system is present in an amount of 1 to 30% by weight, and the co-solvent is present in an amount of 1 to 60% by weight.

An emulsification or emulsifying system or ES comprises a unique blend of multiple surfactants. These surfactants have optimal hydrophilic-lipophilic balance (HLB) values and possess both hydrophilic and lipophilic properties. This combination ensures the composition achieves superior stability and enhances its physicochemical properties. Additionally, the interactions of these surfactants improve performance, maximizing the effectiveness of the agrochemical composition in agricultural applications. This enhances the stability of the emulsion and optimizes the delivery and action of agrochemical products on crops, resulting in more reliable and effective agricultural solutions.

The emulsifying system comprises a blend having Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol NP Ethoxylate, heavy aromatic & Triethylene Glycol Monoethyl Ether, Castor Oil Ethoxylate, and n-Butanol.

In an embodiment, the emulsifying system comprises a blend having a Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol, NP Ethoxylate, Heavy Aromatic & Triethylene Glycol Monoethyl Ether.

In another embodiment, the co-solvent is selected from N-Methyl-2-pyrrolidone, N-Butyl-2-pyrrolidone, Dimethylsulfoxide (DMSO) or any combination thereof.

In a preferred embodiment, the co-solvent is N-Methyl-2-pyrrolidone.

In another embodiment of the present invention, the synergistic insecticidal composition comprises of dinotefuran, bifenthrin, an emulsifying system, a co-solvent, and a solvent.

In another embodiment, the solvent is mixed isomer of benzene, 1, 2, 4-trimethyl and benzene, ethylmethyl (C9 Solvent).

In an optional embodiment of the present invention, the synergistic insecticidal composition may comprise one or more of carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, stabilizers.

Further, the present invention provides a process for preparing the synergistic insecticidal composition, the process comprises of
a) weighing of required quantity of co-solvent;
b) adding dinotefuran to co-solvent under stirring to form a mixture;
c) sequentially adding a solvent and bifenthrin to the above mixture under continuous stirring; and
d) adding an emulsifying system into the mixture of step c) under stirring to obtain a final insecticidal composition.

In another exemplary embodiment, the synergistic composition of the present invention may be formulated as Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsifiable granule (EG), Emulsion water-in-oil (EO), Emulsifiable powder (EP), Emulsion for seed treatment (ES), Emulsion oil-in-water (EW), Flowable concentrate for seed treatment (FS), Granules (GR), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (OF), Oil miscible liquid (OL), Oil dispersible powder (OP), Suspension concentrate (SC), Suspension concentrate for direct application (SD), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC) or a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW).

In another embodiment of the present invention, the synergistic composition may comprise one or more inactive excipients selected from, but not limited to, the group comprising carrier(s), surfactant(s), binder(s), disintegrating agent(s), dispersants or dispersing agent(s), wetting agents, pH modifier(s), thickener(s), biocide(s), emulsifier(s), preservative(s), anti-freezing agent(s), antifoaming agent(s), defoamers colorant(s), inert fillers, light absorbers, mixing aids, solvents, pH-modifying substances and buffers, corrosion-inhibitors, fragrances, protective colloids, and/or stabilizer(s), liquid and solid fertilizers or a combination thereof.

In an exemplary embodiment, the insecticidal composition of the present invention is formulated in the form of an emulsion concentrate comprising actives, an emulsifying system, solvents, and co-solvents.

In another exemplary embodiment, the insecticidal composition of the present invention is formulated in the form of an emulsion concentrate comprising actives, an emulsifying system, solvents, co-solvents, or one or more of carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, and stabilizers.

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

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

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

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

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

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

Antifoaming agents or defoamers suitable for realizing the compositions or formulations according to the present disclosure includes, but not limited to, silicone oils, polymethylsiloxane, simethicone octanol, magnesium stearate and combinations thereof. It is also possible to use a mixture of one or more of these antifoaming agents.

Inert fillers suitable for realizing the compositions or formulations according to the present disclosure include, but are not limited to, inorganic particles such as carbonates, silicates, and oxides, organic substances, such as urea formaldehyde condensates, kaolin, rutile, silicon dioxide, highly disperse silica, silica gels, precipitated silica, colloidal silica, attapulgite china clay, and natural and synthetic silicates, talc and the likes or any combination thereof.

The solvents that may be used for realizing the compositions and formulations of the present disclosure include, but are not limited to, water, water soluble solvents, alcohols, water insoluble solvents, organic solvents, and the like or combinations thereof. The solvent may be present in an amount of about 1-80% w/w of the composition.

Solvent(s) or Co-solvent may be selected from the group comprising of, but not limited to, water, demineralized water (DM); alcohols such as ethanol, propanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, glycerine; polyol ethers such as ethylene glycol monopropyl ether, diethylene glycol monomethyl ether, dipropylene glycol dimethyl ether; ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone; ethers such as dipropyl ether, dioxane, tetrahydrofuran; aliphatic hydrocarbons such as normal paraffin, isoparaffin, kerosene, mineral oil; aromatic hydrocarbons such as xylene, toluene, naphthalene, solvent naphtha, solvent C9, solvent C10, solvent C12, solvesso 100, solvesso 150, solvesso 200; chlorinated aliphatic or aromatic hydrocarbons such as chloro benzene, chloro ethylene, methylene chloride, benzene, 1, 2, 4-trimethyl and benzene, ethylmethyl (C9 Solvent); esters such as ethyl acetate, di-isopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; amides such as dimethyl formamide, N-methyl-2-pyrrolidone (NMP), N-octyl pyrrolidone, N, N dimethyl decanamide; nitriles such as acetonitrile; cyclohexane, dimethyl formamide, isophorone and N-methyl pyrrolidone; organo sulfur compounds.

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

Dispersing agent(s) may be selected from the group comprising, but not limited to, acrylic co-polymer solution, alcohols, C9-11-iso-, C10-rich, and ethoxylated.

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

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

Wetting agent(s) may be selected from the group comprising, but not limited to, alcohols, C9-11-iso-, C10-rich, and ethoxylated.

Thickener(s) may be selected from the group comprising, but not limited to, water-soluble polymer and inorganic fine powder, wherein water-soluble polymer such as xanthan gum, welan gum, guar gum, polyvinyl alcohol, carboxy methylcellulose, polyvinyl pyrrolidone, carboxyvinyl polymer, acrylic polymer, starch derivative, or polysaccharide; or an inorganic fine powder selected from high purity silica, bentonite, or white carbon. These thickeners may be used alone or in combination.

Preservatives may be selected from the group comprising, but not limited to, 20% aqueous dipropylene glycol solution of 1, 2-benzisothiazolin-3-one, formaldehyde potassium sorbate, 4-hydroxybenzoic acid esters, 2-methyl-4-isothiazolin-3-one, and 5-chloro-2-methyl-4-isothiazolin-3-one.

In another exemplary embodiment, the present invention provides a process for the preparation of synergistic compositions comprising the following steps: (a) charging a vessel with the required quantity of NMP and stirring at 100 rpm; (b) adding the required quantity of actives and stirring until fully dissolved; (c) adding emulsifiers while stirring; (d) drawing samples for quality checks.

As per one embodiment, the synergistic composition comprising dinotefuran, bifenthrin, an emulsifying system, and a co-solvent with one or more inactive excipients, wherein active ingredients are present in concentration as described below;
Ingredients Function QTY
Dinotefuran Active 1-40%
Bifenthrin Active 1-40%
N-Methyl-2-pyrrolidone (NMP) Co-Solvent 1-60%
Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Polyoxyethylene ether of Cardanol
NP Ethoxylate,
Heavy Aromatic
& Triethylene Glycol Monoethyl Ether
Castor Oil Ethoxylate,
n-Butanol

Emulsifying system

1-30%
mixed isomer of benzene, 1,2,4-trimethyl and benzene, ethylmethyl (Aromatic Solvent C-9) Solvent QS to make 100 ML

EXAMPLES

Below are examples of different composition in accordance with the present invention. However, the below examples are given solely for the purpose of illustration and are not to be construed as limitations of the present invention, as many variations thereof are possible without departing from the spirit and scope of the invention.

Example 1:

Table 1: Emulsion Concentrate (EC) Composition of 22% Dinotefuran and 5.5% Bifenthrin

S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 22.0%
2. Bifenthrin Active 5.50%
3. N-Methyl-2-pyrrolidone (NMP) Co-Solvent 45.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Polyoxyethylene ether of Cardanol, NP Ethoxylate,
Heavy Aromatic,
Triethylene Glycol Monoethyl Ether
&
Blend of Calcium Salt of Alkyl Benzene Sulfonate
Castor Oil Ethoxylate,
n-Butanol

Emulsifying system

12.0%
5. mixed isomer of benzene, 1,2,4-trimethyl and benzene, ethylmethyl (Aromatic Solvent C-9) Solvent QS to make 100 ML
TOTAL 100 ML
Process for preparation of the composition:

Required quantity of N-Methyl-2-pyrrolidone (NMP) was weighed in a beaker, and then the desired amount of Dinotefuran was added. The mixture was stirred at 100 RPM for about 40 minutes until it was fully dissolved. Following this, the required quantity of Solvent C-9 and Bifenthrin were added to the mixture while continuously stirring until the mixture dissolved completely. After that, emulsifiers were added and continuously stirred for another 20 minutes to obtain an emulsion concentrate (EC). Finally, the obtained composition is packed after analysis.

Table 2: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 6.53
5. Flash point Above 24.5 ºC 44ºC
6. Density at 20 0C g/ml 1.05 g/ml ± 0.02 1.045 g/ml
7. Emulsion Stability Stable Stable
8. Solubility in water Emulsifiable Emulsifiable

Table 3: Storage Stability Observation
Test Parameters 0 days @25°C 14 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Dinotefuran AI %
Bifenthrin AI % 22.04
5.55 22.01
5.54
pH 1 % Aq. Solution 5.0-8.5 6.13
Flash point Above 24.5ºC Complies
Density at 25 0C g/ml 1.05 g/ml 1.05 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 2:

Table 4: Emulsion Concentrate (EC) Composition of 20% Dinotefuran and 20% Bifenthrin

S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 20.0%
2. Bifenthrin Active 20.0%
3. Dimethyl sulfoxide (DMSO) Co-Solvent 20.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Polyoxyethylene ether of Cardanol,
NP Ethoxylate,
Heavy Aromatic
& Triethylene Glycol Monoethyl Ether
&
Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Castor Oil Ethoxylate,
n-Butanol Water Soluble emulsifying system 12.0%
5. N-Methyl-2-pyrrolidone (NMP) Solvent QS to make 100 ML
TOTAL 100 ML

Process for the preparation of the composition:

Weighing the required amount of NMP in a beaker, followed by adding required quantity of Dinotefuran and stirring the mixture at 100 RPM for 40 minutes until it was fully dissolved. Thereafter adding specified amount of DMSO and Bifenthrin to the mixture while stirring continuously until it dissolved completely. After that, the required amount of emulsifying system and stirred continuously for another 20 minutes to obtain an emulsion concentrate (EC).

Table 5: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 6.47
5. Flash point Above 24.5 ºC Complies
6 Density at 20 ºC g/ml 1.07g/ml ± 0.02 1.068 g/ml
7. Emulsion Stability Stable Stable
8. Solubility in water Emulsifiable Emulsifiable

Table 6: Storage Stability Observation
Test Parameters 0 days @25°C 14 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Flash point Above 24.5ºC Complies
pH 1 % Aq. Solution 6.78 6.50
Density at 25 0C g/ml 1.07 g/ml 1.06 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 3:
Table 7: Emulsion Concentrate (EC) Composition of 10% Dinotefuran and 15% Bifenthrin

S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 10.0%
2. Bifenthrin Active 15.0%
3. N-Butyl-2-pyrrolidone (NMP) Co-Solvent 40.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Polyoxyethylene ether of Cardanol, NP Ethoxylate,
Heavy Aromatic,
Triethylene Glycol Monoethyl Ether & Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Castor Oil Ethoxylate,
n-Butanol

Emulsifying system

13.0%
5. mixed isomer of benzene, 1,2,4-trimethyl and benzene, ethylmethyl (Aromatic Solvent C-9) Solvent QS to make 100 ML
TOTAL 100 ML

Process for the preparation of the composition:
Weighing the required quantity of NMP in a beaker, the required amount of Dinotefuran was added and the mixture was stirred at 100 RPM for 40 minutes, ensuring it fully dissolves. Then, the specified quantity of Solvent C-9 along with Bifenthrin was added to the mixture while continuously stirring until the mixture dissolved completely. After that, the necessary emulsifiers were added and continuously stirred for another 20 minutes to obtain an emulsion concentrate (EC). The material is packed after analysis.

Table 8: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 6.33
5. Flash point Above 24.5 ºC 45 ºC
6. Density at 25 0C g/ml 1.05 g/ml ± 0.02 1.051 g/ml
7. Emulsion Stability Stable Stable
8. Solubility in water Emulsifiable Emulsifiable

Table 9: Storage Stability Observation
Test Parameters 0 days @25°C 15 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Dinotefuran AI %
Bifenthrin AI % 10.08
15.04 10.01
15.24
pH 1 % Aq. Solution 5.0-8.5 7.13
Flash point Above 24.5ºC Complies
Density at 25 0C g/ml 1.05 g/ml 1.04 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 4:
Table 10: Emulsion Concentrate (EC) Composition of 28% Dinotefuran and 3.5% Bifenthrin
S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 28.0%
2. Bifenthrin Active 3.5%
3. N-Methyl-2-pyrrolidone (NMP) Co-Solvent 50.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate
Polyoxyethylene ether of Cardanol,
NP Ethoxylate,
Heavy Aromatic,
Triethylene Glycol Monoethyl Ether
&
Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Castor Oil Ethoxylate,
n-Butanol

Emulsifying system

15.0%
5. mixed isomer of benzene, 1,2,4-trimethyl and benzene, ethylmethyl (Aromatic Solvent C-9) Solvent QS to make 100 ML
TOTAL 100 ML

Process for the preparation of the composition:

Weighing the required quantity of NMP and Dinotefuran, transferred into a beaker and the mixture was stirred at 100 RPM for 40 minutes until it dissolved completely. Then, the required quantity of Solvent C9 and Bifenthrin were added to the mixture while continuously stirring until the mixture dissolved completely. After that, the necessary emulsifiers were added and stirred for another 20 minutes to obtain an emulsion concentrate (EC).

Table 11: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 6.82
5. Flash point Above 24.5ºC 45ºC
6. Density at 25 0C g/ml 1.05 g/ml ± 0.02 1.055 g/ml
7. Emulsion Stability Stable Stable
8. Solubility in water Emulsifiable Emulsifiable

Table 12: Storage Stability Observation
Test Parameters 0 days @25°C 14 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Dinotefuran AI %
Bifenthrin AI % 28.04
3.55 28.02
3.54
pH 1 % Aq. Solution 5.0-8.5 6.24
Flash point Above 24.5ºC Complies
Density at 25 0C g/ml 1.04 g/ml 1.04 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 5:

Table 13: Emulsion Concentrate (EC) Composition of 8.5% Dinotefuran and 25% Bifenthrin
S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 8.5%
2. Bifenthrin Active 25.0%
3. Dimethyl sulfoxide (DMSO) Co-Solvent 20.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol, NP Ethoxylate, Heavy Aromatic, Triethylene Glycol Monoethyl Ether &
Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Castor Oil Ethoxylate,
n-Butanol Emulsifying system 14.5%
5. N-Methyl-2-pyrrolidone (NMP) Solvent QS to make 100 ML
6. TOTAL 100 ML

Process for the preparation of the composition:

In a beaker, the required quantity of NMP was weighed and then the required amount of Dinotefuran was added. The mixture was stirred at 100 RPM for 40 minutes to ensure it was fully dissolved. Next, the DMSO and Bifenthrin were added to the mixture while continuously stirring until the mixture completely dissolved. After that, the emulsifying system was added and continuously stirred for another 20 minutes to obtain an emulsion concentrate (EC).
Table 14: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 7.01
5. Flash point Above 24.5 ºC Complies
6. Emulsion Stability Stable Stable
7. Solubility in water Emulsifiable Emulsifiable

Table 15: Storage Stability Observation
Test Parameters 0 days @25°C 14 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Flash point Above 24.5ºC Complies
pH 1 % Aq. Solution 7.04 7.01
Density at 25 0C g/ml 1.05 g/ml 1.04 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 6:

Table 16: Emulsion Concentrate (EC) Composition of 17.5% Dinotefuran and 24.5% Bifenthrin

S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 17.5%
2. Bifenthrin Active 24.5%
3. N-Methyl-2-pyrrolidone (NMP) Co-Solvent 35.0%
4. Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Polyoxyethylene ether of Cardanol,
NP Ethoxylate,
Heavy Aromatic,
Triethylene Glycol Monoethyl Ether
&
Blend of Calcium Salt of Alkyl Benzene Sulfonate,
Castor Oil Ethoxylate,
n-Butanol

Emulsifying system 20%
5. mixed isomer of benzene, 1,2,4-trimethyl and benzene, ethylmethyl (Aromatic Solvent C-9) Solvent QS to make 100 ML
6. TOTAL 100 ML

Process for the preparation of the composition:
Weighing the required quantity of NMP, Dinotefuran was added to a beaker, and the mixture was stirred at 100 RPM for 40 minutes, ensuring it was fully dissolved. Then, the specified quantity of Solvent C-9 and Bifenthrin were added to the mixture under continuous stirring until the complete dissolution. After that, the necessary emulsifiers were added and stirred for another 20 minutes to obtain an emulsion concentrate (EC).

Table 17: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Liquid
2. Color Yellow Yellow
3. Odor Aromatic Aromatic
4. pH 1 % Aq. Solution 5.0-8.5 7.1
5. Flash point Above 24.5 ºC 42 ºC
6. Density at 20 0C g/ml 1.05 g/ml ± 0.02 1.026 g/ml
7. Emulsion Stability Stable Stable
8. Solubility in water Emulsifiable Emulsifiable

Table 18: Storage Stability Observation
Test Parameters 0 days @25°C 15 Days @54°C
Physical state Clear Transparent Liquid Clear Transparent Liquid
Color Yellow Yellow
Odor Aromatic Aromatic
Flash point Above 24.5ºC Complies
pH 1 % Aq. Solution 5.0-8.5 7.10
Density at 25 0C g/ml 1.06 g/ml 1.06 g/ml
Emulsion Stability Stable Stable
Cold stability @ 0ºC for 7 days Passes Passes

Example 7: Composition with other solvents
Table 19: Emulsion Concentrate (EC) Composition of 20% Dinotefuran and 20% Bifenthrin with other solvents
S. No. Ingredients Function Quantity in %W/V
1. Dinotefuran Active 20.0%
2. Bifenthrin Active 20.0%
3. n-Butanol Co-Solvent 45.0%
4. Butylated hydroxytoluene (BHT) Preservative 1.0%
5. Blend of alkyl aryl sulfonate, nonyl phenol, ethoxylated, isobutanol and solvent naphtha (petroleum) light aromatics Emulsifier 12.0%
6. Aromatic Solvent C-9 Solvent QS to make 100 ML
TOTAL 100 ML

Process for the preparation of the composition:

Required amount of n-Butanol was measured and transferred to a beaker, then stirred at 100 RPM. The active ingredients, Dinotefuran and Bifenthrin, along with the preservative BHT and emulsifier were added to the beaker while stirring continuously for two hours. It was observed that Dinotefuran does not dissolve completely. Thus, the experiment was terminated.

Table 20: Physiochemical Properties of the Composition
S. No. Test Parameters Specifications Results
1. Physical state Liquid Failed
2. Color Yellow Failed
3. Odor Aromatic Failed
4. pH 1 % Aq. Solution 5.0-8.5 Failed
5. Flash point Above 24.5 ºC Failed
7. Emulsion Stability Stable Failed
8. Solubility in water Emulsifiable Failed

It was observed that the active ingredient Dinotefuran did not dissolve in n-butanol. Further, the composition exhibited negative characteristics in several critical parameters, including physical state, Color, and odour, which do not meet acceptable standards. Thus, the composition without the co-solvent, solvent and emulsifying system of the present invention did not achieve the intended outcome and failed.
Example 8:
TRIAL 1: Evaluation of bio-efficacy of the insecticidal composition of Dinotefuran and Bifenthrin against Paddy Stem Borer (Scirpophaga incertulas)

Season Kharif
Location Panchedu, Nellore, Andhra Pradesh
Crop Paddy
Age of Crop 25 days (after transplanting)
Temperature Range during Trial 25-30 °C
Variety MTU 1010
Single plot size 5 x 5 =25 m2
Date of Transplanting/Sowing 11/6/2023
Number of applications 1
Date of application 8/7/2023
Target Pest Yellow Stem Borer (Scirpophaga incertulas)
Method of application Spraying

Table 21: Treatment details of the composition of actives.
Treatment No. Treatment Details AI gm/Ha Dose gm or ml/Ha?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 55+13.75 250
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 110 + 27.5 500
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 165 + 41.25 750
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 55+13.75 250
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 110 + 27.5 500
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 165 + 41.25 750
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 55+13.75 275 + 137.5
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 110 + 27.5 550 + 275
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 165 + 41.25 825 + 412.5
T10 Dinotefuran 20 % SG 55.00 275
T11 Dinotefuran 20 % SG 110.00 550
T12 Dinotefuran 20 % SG 165.00 825
T13 Bifenthrin 10% EC 13.75 137.5
T14 Bifenthrin 10% EC 27.50 275
T15 Bifenthrin 10% EC 41.25 412.5
T16 Control Nil Nil
*ES - Emulsifying System, CE - conventional emulsifier

Methodology
The experiment was conducted under field conditions at Panchedu, Nellore, Andhra Pradesh, focusing on the paddy hybrid “MTU 1010”. The experimental design followed a Randomized Block Design (RBD) with three replications. Each plot covered an area of 25 square meters for precise measurements. As per the treatment schedule, the test samples were applied at pest appearance using 500 litres of water per hectare with a knapsack sprayer.

Observation
Pre-count Pest observation was taken before the spray application. Pest counts were recorded by randomly selecting five plants per replication and noting insect population for each replication. Observations were recorded on the 5th, 10th, and 15th days after the spray application.

Table 22: Effectiveness of different treatments against Paddy Stem Borer.
S. No. Treatments Dose gm or ml/Ha? Effectiveness of different treatments against Paddy Stem Borer
Dead heart Percent (%) Percent reduction over Control (%)
Pre-count 5 DAA 10 DAA 15 DAA 5 DAA 10 DAA 15 DAA
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 11.49 2.43 2.10 2.54 79.62 83.91 80.42
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 9.99 1.77 1.21 2.32 85.20 90.71 82.13
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 10.84 0.74 0.86 1.63 93.80 93.40 87.42
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 10.37 3.31 3.50 4.21 72.29 73.16 67.49
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 10.76 2.62 2.87 4.12 78.07 78.03 68.20
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 10.04 2.09 2.24 3.48 82.52 82.85 73.18
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 9.53 3.48 5.10 5.09 70.85 60.94 60.73
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 10.74 2.81 4.01 4.86 76.43 69.29 62.52
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 10.07 2.01 2.90 3.94 83.14 77.80 69.59
T10 Dinotefuran 20 % SG 275 10.67 6.89 8.07 7.52 42.33 38.16 41.97
T11 Dinotefuran 20 % SG 550 9.86 6.28 7.52 7.45 47.41 42.41 42.51
T12 Dinotefuran 20 % SG 825 9.80 5.30 7.26 7.00 55.63 44.36 46.02
T13 Bifenthrin 10% EC 137.5 10.21 5.55 6.83 7.46 53.53 47.64 42.45
T14 Bifenthrin 10% EC 275 10.90 4.90 6.38 6.67 58.96 51.10 48.52
T15 Bifenthrin 10% EC 412.5 11.70 3.68 5.71 5.91 69.19 56.22 54.39
T16 Control Nil 11.68 11.94 13.05 12.96 0.00 0.00 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Table 23: Synergistic effect of different treatments against Paddy Stem Borer at 10 DAA.
S. no. Treatment details Dose (ml or gm/Ha) % Reduction over control of paddy stem borer 10 DAA
Observed Expected Ratio Synergy
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 83.91 67.62 1.24 Yes
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 90.71 71.84 1.26 Yes
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 93.40 75.64 1.23 Yes
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 73.16 67.62 1.08 Yes
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 78.03 71.84 1.09 Yes
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 82.85 75.64 1.10 Yes
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275+137.5 60.94 67.62 0.90 No
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550+275 69.29 71.84 0.97 No
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825+412.5 77.80 75.64 1.03 Yes
T10 Dinotefuran 20 % SG 275 38.16 - - -
T11 Dinotefuran 20 % SG 550 42.41 - - -
T12 Dinotefuran 20 % SG 825 44.36 - - -
T13 Bifenthrin 10% EC 137.5 47.64 - - -
T14 Bifenthrin 10% EC 275 51.10 - - -
T15 Bifenthrin 10% EC 412.5 56.22 - - -
T16 Control Nil 0.00 - - -
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

It is apparent from the above data that there is significant reduction in dead heart symptoms caused by Scirpophaga incertulas in Treatments 3 and 2, with reductions of 93.40% and 90.71%, respectively. These treatments demonstrated a notable decrease in the Scirpophaga incertulas population compared to the control. Additionally, Treatment 3 (Dinotefuran 220 + Bifenthrin 55 g/L EC (ES)) at 750 ml was the most effective in reducing the Scirpophaga incertulas population.

Table 24: Yield study on Paddy Stem Borer
S. no. Treatment details Dose (ml or gm/Ha) Yield T/Ha Percent increase over control (%)
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 7.12 11.28
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 7.13 11.46
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 7.31 14.24
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 250 6.92 8.16
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 500 6.96 8.68
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 750 6.99 9.20
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 6.84 6.94
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 6.88 7.47
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 6.90 7.81
T10 Dinotefuran 20 % SG 275 6.58 2.78
T11 Dinotefuran 20 % SG 550 6.64 3.82
T12 Dinotefuran 20 % SG 825 6.69 4.51
T13 Bifenthrin 10% EC 137.5 6.67 4.17
T14 Bifenthrin 10% EC 275 6.68 4.34
T15 Bifenthrin 10% EC 412.5 6.80 6.25
T16 Control Nil 6.40 0.00

Observation: The treatments with the Emulsifiable Concentrate composition of the present invention resulted in increased crop yield, implying that the present composition is synergistic and bio-effective.

Example 9:
TRIAL 2: Evaluation of bio-efficacy of the insecticidal composition of Dinotefuran and Bifenthrin against Paddy Leaf folder.
Season Kharif 2023
Location Basapattana (Gangavathi)
Crop Paddy
Age of Crop 60 days
Temperature Range during Trial 25 to 30?
Variety Kaveri sona
Single plot size 5x5 (25 m2)
Date of Transplanting/Sowing 17/08/2023
Number of applications 1
Date of application 17/10/2023
Target Pest Leaf Folder (Cnaphalocrocis medinalis)
Method of application Spraying

Table 25: Treatment details of the composition of actives.
Treatment No. Treatment Detail AI gm/Ha Dose gm or ml/Ha?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 55+13.75 250
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 110 + 27.5 500
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 165 + 41.25 750
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 55+13.75 250
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 110 + 27.5 500
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 165 + 41.25 750
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 55+13.75 275 + 137.5
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 110 + 27.5 550 + 275
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 165 + 41.25 825 + 412.5
T10 Dinotefuran 20 % SG 55.00 275
T11 Dinotefuran 20 % SG 110.00 550
T12 Dinotefuran 20 % SG 165.00 825
T13 Bifenthrin 10% EC 13.75 137.5
T14 Bifenthrin 10% EC 27.50 275
T15 Bifenthrin 10% EC 41.25 412.5
T16 Control Nil Nil

Methodology
The experimental design followed a Randomized Block Design (RBD) with three replications. Each plot covered an area of 25 square meters, for precise measurements to be taken. The test samples, according to the treatment schedule, were applied at pest appearance using 500 liters of water per hectare with a knapsack sprayer.

Observation
Pre-count Pest observation was taken before the spray application. Pest counts were recorded by randomly selecting five hills per treatment and recorded population of leaf folder for each hill. Observations were recorded on the 3rd, 7th, and 15th days after the spray application.

Table 26: Effectiveness of different treatments against Paddy Leaf folder.
S. No. Treatments Dose g or ml/ha Effectiveness of different insecticide against Paddy Leaf Folder
Percent (%) reduction over control
Pre-count 3 DAA 7 DAA 15 DAA
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 1.47 76.92 83.78 78.38
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 1.40 84.62 89.19 81.08
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 1.53 88.46 94.59 83.78
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 1.60 69.23 81.08 67.57
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 1.33 73.08 83.78 70.27
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 1.67 80.77 86.49 72.97
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 1.53 53.85 59.46 56.76
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 1.60 57.69 70.27 64.86
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 1.67 65.38 78.38 70.27
T10 Dinotefuran 20 % SG 275 1.33 11.54 18.92 13.51
T11 Dinotefuran 20 % SG 550 1.73 15.38 21.62 16.22
T12 Dinotefuran 20 % SG 825 1.20 26.92 37.84 27.03
T13 Bifenthrin 10% EC 137.5 1.73 46.15 54.05 45.95
T14 Bifenthrin 10% EC 275 1.13 50.00 56.76 48.65
T15 Bifenthrin 10% EC 412.5 1.80 53.85 59.46 54.05
T16 Control Nil 1.73 0.00 0.00 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Table 27: Synergistic effect of different treatments against Paddy Leaf folder at 7 DAA.
S.no. Treatment details Dose (ml or gm/Ha) % Reduction
over control of Paddy Leaf folder 7DAA
Observed Expected Ratio Synergy
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 83.78 62.75 1.34 Yes
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 89.19 66.11 1.35 Yes
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 94.59 74.80 1.26 Yes
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 81.08 62.75 1.29 Yes
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 83.78 66.11 1.27 Yes
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 86.49 74.80 1.16 Yes
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 59.46 62.75 0.95 No
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 70.27 66.11 1.06 Yes
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 78.38 74.80 1.05 Yes
T10 Dinotefuran 20 % SG 275 18.92
T11 Dinotefuran 20 % SG 550 21.62
T12 Dinotefuran 20 % SG 825 37.84
T13 Bifenthrin 10% EC 137.5 54.05
T14 Bifenthrin 10% EC 275 56.76
T15 Bifenthrin 10% EC 412.5 59.46
T16 Control Nil 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Results
The Leaf folder population ranged from 1-2 individuals per leaf prior to treatment. The mean leaf folder population reduction was the highest in plots treated with Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at a 750 ml dose, achieving a 94.59% reduction, followed by a reduction of 89.19% in plots treated with Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at a 500 ml dose.

Table 28: Yield study on Paddy Leaf folder
S. no. Treatment details Dose (ml or gm/Ha) Yield T/Ha Percent increase over control (%)
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 7.10 20.34
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 7.20 22.03
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 7.39 25.24
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 250 6.92 17.33
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 500 6.97 18.08
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 750 7.01 18.83
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 6.82 15.63
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 6.84 16.01
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 6.91 17.14
T10 Dinotefuran 20 % SG 275 6.57 11.30
T11 Dinotefuran 20 % SG 550 6.67 12.99
T12 Dinotefuran 20 % SG 825 6.72 13.94
T13 Bifenthrin 10% EC 137.5 6.68 13.18
T14 Bifenthrin 10% EC 275 6.70 13.56
T15 Bifenthrin 10% EC 412.5 6.78 14.88
T16 Control Nil 5.90 0.00

Observation: The treatments with the Emulsifiable Concentrate composition of the present invention resulted in increased crop yield, implying that the present composition is synergistic and bio-effective.

Example 10:
Table 29: Effect of different treatments on natural enemy population on Paddy
S. No.? Treatment details? Dose gm or ml/Ha? Effect of insecticide treatment on natural enemy population
Dragon Flies Spider
Pre count 5 DAA 10 DAA? 15 DAA? Pre count 5 DAA 10 DAA? 15 DAA?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 4.33 4.67 4.67 4.00 7.67 7.33 8.00 7.33
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 4.00 4.33 4.33 4.00 7.00 6.67 7.00 6.33
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 3.33 4.33 3.67 4.33 6.67 7.00 6.67 6.33
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 4.00 4.33 4.67 4.33 7.33 7.33 6.67 7.00
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 3.67 3.67 4.00 4.00 7.33 6.33 7.00 6.33
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 3.33 4.67 4.67 4.33 7.33 6.67 6.67 6.33
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 4.33 4.33 3.33 3.00 7.33 7.33 7.00 6.00
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 3.33 3.67 4.67 4.33 6.33 6.33 6.67 7.00
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 3.67 3.67 4.33 3.67 7.00 6.33 6.33 6.33
T10 Dinotefuran 20 % SG 275 4.33 4.33 4.67 4.67 6.67 7.00 7.33 7.33
T11 Dinotefuran 20 % SG 550 4.00 4.33 4.33 4.33 6.67 7.33 6.67 6.33
T12 Dinotefuran 20 % SG 825 3.67 4.67 4.00 4.00 7.33 6.33 7.00 6.33
T13 Bifenthrin 10% EC 137.5 3.33 3.67 3.33 4.00 6.33 6.33 7.00 6.00
T14 Bifenthrin 10% EC 275 4.33 4.33 4.33 4.33 7.67 7.00 7.00 7.33
T15 Bifenthrin 10% EC 412.5 3.33 4.33 4.33 3.00 7.33 7.33 8.00 6.33
T16 Control Nil 4.00 3.67 4.00 4.00 6.33 6.33 6.33 7.33
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Result
The present invention composition is safe on natural enemies in paddy ecosystems. There is no difference in natural enemy population count between any of the treatments and the untreated control.

Example 11: Evaluation of Phytotoxicity of the present composition on Paddy.
Visual observations were recorded at 7, 14 and 21 days after the application (DAA) of tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty and wilting based on 0-10 scale given in below table. A total of 20 plants per plot were observed.

Table 30: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
Leaf injury on tips /surface? Rating?
0%? 0?
1-10%? 1?
11-20%? 2?
21-30%? 3?
31-40%? 4?
41-50%? 5?
51-60%? 6?
61-70%? 7?
71-80%? 8?
81-90%? 9?
91-100%? 10?

Table 31: Phytotoxic effect of various treatments on Paddy after 7 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 7 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 32: Phytotoxic effect of various treatments on Paddy after 14 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 14 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 33: Phytotoxic effect of various treatments on Paddy after 21 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 21 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 34: Phytotoxic effect of various treatments on Paddy after 7 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 7 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?
Table 35: Phytotoxic effect of various treatments on Paddy after 14 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 14 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 36: Phytotoxic effect of various treatments on Paddy after 21 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 21 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Tables 31 to 33 above indicate that application of Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) in all doses showed no phytotoxicity symptoms like leaf injury on tips, leaf injury on the surface, wilting, vein clearing, necrosis, epinasty and hyponasty in paddy crop. Further, as evident from tables 34, 35 and 36, the application of Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) at even double dose shows no phytotoxicity. Thus, applying the present invention composition may be considered completely safe for paddy crops.

Example 12:
TRIAL 3: Evaluation of bio-efficacy of the insecticidal composition of Dinotefuran and Bifenthrin against Cotton Jassids.
Season Kharif 2023
Location Khargone (MP)
Crop Cotton
Age of Crop 55 days
Temperature Range during Trial 25-30 °C
Variety Asha 1
Single plot size 5 x 5 =25 m2
Date of Transplanting/Sowing 15/06/2023
Number of applications 1
Date of application 09/08/2023
Target Pest Jassids
Method of application Spraying

Table 37: Treatment details of the composition of actives.
Treatment No. Treatment Details AI gm/Ha Dose gm or ml/Ha?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 55+13.75 250
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 110 + 27.5 500
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 165 + 41.25 750
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 55+13.75 250
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 110 + 27.5 500
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 165 + 41.25 750
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 55+13.75 275 + 137.5
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 110 + 27.5 550 + 275
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 165 + 41.25 825 + 412.5
T10 Dinotefuran 20 % SG 55.00 275
T11 Dinotefuran 20 % SG 110.00 550
T12 Dinotefuran 20 % SG 165.00 825
T13 Bifenthrin 10% EC 13.75 137.5
T14 Bifenthrin 10% EC 27.50 275
T15 Bifenthrin 10% EC 41.25 412.5
T16 Control Nil Nil
*ES - Emulsifying System, CE - conventional emulsifier

Methodology
The experiment was conducted under field conditions at Khargone, Madhya Pradesh on cotton hybrid “Asha 1”. The experimental design followed a Randomized Block Design (RBD) with three replications. Each plot covered an area of 25 square meters, for precise measurements to be taken, 5 plants were tagged per treatment and pest count taken prior to the application. The test samples, according to the treatment schedule, were applied at pest appearance using 500 liters of water per hectare with a knapsack sprayer?fitted with hollow cone nozzle.

Observation
Pre-count Pest observation was taken before the spray application. Pest counts were recorded by randomly selecting five plants per treatment and counting number of jassids per leaf. Observations were recorded on the 3rd, 7th, and 15th days after the spray application.

Table 38: Effectiveness of different treatments against Cotton Jassids.
S. No. Treatments Dose g or ml/ha Effectiveness of different insecticide against cotton jassids
Percent (%) reduction over control
Pre-count 3 DAA 7 DAA 15 DAA
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 3.07 83.64 87.10 81.82
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 3.27 87.27 90.32 85.71
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 3.33 89.09 95.16 87.01
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 3.40 81.82 79.03 75.32
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 3.20 83.64 85.48 77.92
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 3.07 85.45 87.10 80.52
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275+137.5 3.13 76.36 74.19 66.23
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 3.07 78.18 77.42 71.43
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825+412.5 3.27 80.00 80.65 76.62
T10 Dinotefuran 20 % SG 275 3.33 56.36 58.06 51.95
T11 Dinotefuran 20 % SG 550 3.40 58.18 62.90 54.55
T12 Dinotefuran 20 % SG 825 3.20 60.00 66.13 62.34
T13 Bifenthrin 10% EC 137.5 3.07 32.73 35.48 33.77
T14 Bifenthrin 10% EC 275 3.13 45.45 37.10 35.06
T15 Bifenthrin 10% EC 412.5 3.27 45.45 40.32 38.96
T16 Control Nil 3.27 0.00 0.00 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Table 39: Synergistic effect of different treatments against Cotton Jassids at 7 DAA.
S. no. Treatment details Dose (ml or gm/Ha) % Reduction
over control of cotton Jassids 7DAA
Observed Expected Ratio Synergy
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 87.10 72.94 1.19 Yes
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 90.32 76.66 1.18 Yes
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 95.16 79.79 1.19 Yes
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 79.03 72.94 1.08 Yes
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 85.48 76.66 1.12 Yes
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 87.10 79.79 1.09 Yes
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 74.19 72.94 1.02 Yes
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 77.42 76.66 1.01 Yes
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 80.65 79.79 1.01 Yes
T10 Dinotefuran 20 % SG 275 58.06 - - -
T11 Dinotefuran 20 % SG 550 62.90 - - -
T12 Dinotefuran 20 % SG 825 66.13 - - -
T13 Bifenthrin 10% EC 137.5 35.48 - - -
T14 Bifenthrin 10% EC 275 37.10 - - -
T15 Bifenthrin 10% EC 412.5 40.32 - - -
T16 Control Nil 0.00 - - -
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Result
The recorded data revealed that the Jassid population was uniformly distributed across the experimental area prior to the application of treatments. Observations made the day before spraying showed Jassid populations ranging between 3.07 and 3.40 per plant, with no significant differences among the treatments. However, 7 days after application (DAA), all treatments resulted in a significant reduction in Jassid populations compared to the control. Among all the treatments, Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at 750 ml and 500 ml doses proved to be the most effective in reducing the Jassid population.
Table 40: Yield study on Cotton Jassids
S. no. Treatment details Dose (ml or gm/Ha) Yield T/Ha Percent increase over control (%)
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 250 33.31 20.42
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 500 34.36 24.23
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 750 35.29 27.60
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 250 32.23 16.53
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 500 32.91 18.99
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 750 32.93 19.06
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 31.20 12.80
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 32.25 16.58
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 32.46 17.36
T10 Dinotefuran 20 % SG 275 30.12 8.90
T11 Dinotefuran 20 % SG 550 30.57 10.52
T12 Dinotefuran 20 % SG 825 31.01 12.11
T13 Bifenthrin 10% EC 137.5 29.00 4.86
T14 Bifenthrin 10% EC 275 28.86 4.33
T15 Bifenthrin 10% EC 412.5 29.15 5.40
T16 Control Nil 27.66 0.00

Observation: The treatments with the Emulsifiable Concentrate composition of the present invention resulted in increased crop yield, implying that the present composition is synergistic and bio-effective.

Example 13:
TRIAL 4: Evaluation of bio-efficacy of the insecticidal composition of Dinotefuran and Bifenthrin against Cotton Aphids.
Season Kharif 2023
Location Aurangabad (Maharashtra)
Crop Cotton
Age of Crop 54 days
Temperature Range during Trial 20-30 °C
Variety RCH659
Single plot size 5 x 5 =25 m2
Date of Transplanting/Sowing 19/06/2023
Number of applications 1
Date of application 12/08/2023
Target Pest Aphids
Method of application Spraying

Table 41: Treatment details of the composition of actives.
Treatment No. Treatment Details AI gm/Ha Dose gm or ml/Ha?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 55+13.75 250
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 110 + 27.5 500
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 165 + 41.25 750
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 55+13.75 250
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 110 + 27.5 500
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 165 + 41.25 750
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 55+13.75 275 + 137.5
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 110 + 27.5 550 + 275
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 165 + 41.25 825 + 412.5
T10 Dinotefuran 20 % SG 55.00 275
T11 Dinotefuran 20 % SG 110.00 550
T12 Dinotefuran 20 % SG 165.00 825
T13 Bifenthrin 10% EC 13.75 137.5
T14 Bifenthrin 10% EC 27.50 275
T15 Bifenthrin 10% EC 41.25 412.5
T16 Control Nil Nil
*ES - Emulsifying System, CE - conventional emulsifier

Methodology
The experiment was conducted under field conditions at Aurangabad, Maharashtra on cotton hybrid “RCH659”. The experimental design followed a Randomized Block Design (RBD) with three replications. Each plot covered an area of 25 square meters, for precise measurements to be taken, 5 plants were tagged per treatment and pest count taken prior to the application. The test samples, according to the treatment schedule, were applied at pest appearance using 500 liters of water per hectare with a knapsack sprayer?fitted with hollow cone nozzle.

Observation
Pre-count Pest observation was taken before the spray application. Pest counts were recorded by randomly selecting five plants per treatment and counting number of aphids per leaf. Observations were recorded on the 3rd, 7th, and 15th days after the spray application.

Table 42: Effectiveness of different treatments against Cotton Aphids.
S. No. Treatments Dose g or ml/ha Effectiveness of different insecticide against Cotton Aphid
Percent (%) reduction over control
Pre-count 3 DAA 7 DAA 15 DAA
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 8.93 84.16 87.69 78.46
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 9.93 89.11 90.77 82.31
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 8.73 91.09 94.62 85.38
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 8.53 81.19 82.31 73.85
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 9.13 83.17 84.62 76.15
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 9.33 88.12 88.46 80.00
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275+137.5 8.93 77.23 63.85 60.77
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 9.13 79.21 73.85 69.23
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825+412.5 10.33 82.18 82.31 74.62
T10 Dinotefuran 20 % SG 275 9.73 49.50 53.08 50.00
T11 Dinotefuran 20 % SG 550 8.73 52.48 57.69 53.85
T12 Dinotefuran 20 % SG 825 8.93 58.42 62.31 57.69
T13 Bifenthrin 10% EC 137.5 10.53 34.65 38.46 36.15
T14 Bifenthrin 10% EC 275 10.33 36.63 41.54 38.46
T15 Bifenthrin 10% EC 412.5 9.33 39.60 46.92 43.85
T16 Control Nil 10.33 0.00 0.00 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Table 43: Synergistic effect of different treatments against Cotton Aphids at 7 DAA.
S. no. Treatment details Dose (ml or gm/Ha) % Reduction
over control of Cotton Aphid 7 DAA
Observed Expected Ratio Synergy
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 87.69 71.12 1.23 Yes
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 90.77 75.27 1.21 Yes
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 94.62 79.99 1.18 Yes
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 82.31 71.12 1.16 Yes
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 84.62 75.27 1.12 Yes
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 88.46 79.99 1.11 Yes
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275+137.5 63.85 71.12 0.90 No
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 73.85 75.27 0.98 No
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825+412.5 82.31 79.99 1.03 Yes
T10 Dinotefuran 20 % SG 275 53.08 - - -
T11 Dinotefuran 20 % SG 550 57.69 - - -
T12 Dinotefuran 20 % SG 825 62.31 - - -
T13 Bifenthrin 10% EC 137.5 38.46 - - -
T14 Bifenthrin 10% EC 275 41.54 - - -
T15 Bifenthrin 10% EC 412.5 46.92 - - -
T16 Control Nil 0.00 - - -
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Result
The recorded data revealed that the aphid population was uniformly distributed across the experimental area prior to the application of treatments. Observations made the day before spraying showed aphid populations ranging from 8.53 to 10.53 per plant, with no significant differences among the treatments. However, 3 days after application (DAA), all treatments resulted in a significant reduction in aphid populations compared to the control. Among all the treatments, Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at 750 ml and 500 ml doses were the most effective in reducing the aphid population. The above results indicate that among all the treatments, highest percent reduction over control (% ROC) was observed in Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at 750 ml, which was found to be the most effective for the reducing the aphid population.

Table 44: Yield study on Cotton Aphids
S. no. Treatment details Dose (ml or gm/Ha) Yield T/Ha Percent increase over control (%)
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 21.13 24.94
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 21.50 27.11
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 22.17 31.05
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 250 20.13 18.99
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 500 20.58 21.67
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (Conventional) 750 21.14 25.00
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 19.71 16.50
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 20.23 19.61
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 20.47 21.02
T10 Dinotefuran 20 % SG 275 18.24 7.85
T11 Dinotefuran 20 % SG 550 18.87 11.56
T12 Dinotefuran 20 % SG 825 19.40 14.71
T13 Bifenthrin 10% EC 137.5 17.42 2.99
T14 Bifenthrin 10% EC 275 17.61 4.13
T15 Bifenthrin 10% EC 412.5 18.16 7.35
T16 Control Nil 16.92 0.00
Observation: The treatments with the Emulsifiable Concentrate composition of the present invention resulted in increased crop yield, implying that the present composition is synergistic and bio-effective.

Example 14:
TRIAL 5: Evaluation of bio-efficacy of the insecticidal composition of Dinotefuran and Bifenthrin against Cotton Bollworm.
Season Kharif 2023
Location Ambala, Punjab
Crop Cotton
Age of Crop 90 days
Temperature Range during Trial 25-35 °C
Variety F2228
Single plot size 5 x 5 =25 m2
Date of Transplanting/Sowing 19/06/2023
Number of applications 1
Date of application 19/09/2023
Target Pest Bollworm (Helicoverpa armigera)
Method of application Spraying

Table 45: Treatment details of the composition of actives.
Treatment No. Treatment Details AI gm/Ha Dose gm or ml/Ha?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 55+13.75 250
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 110 + 27.5 500
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 165 + 41.25 750
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 55+13.75 250
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 110 + 27.5 500
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 165 + 41.25 750
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 55+13.75 275 + 137.5
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 110 + 27.5 550 + 275
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 165 + 41.25 825 + 412.5
T10 Dinotefuran 20 % SG 55.00 275
T11 Dinotefuran 20 % SG 110.00 550
T12 Dinotefuran 20 % SG 165.00 825
T13 Bifenthrin 10% EC 13.75 137.5
T14 Bifenthrin 10% EC 27.50 275
T15 Bifenthrin 10% EC 41.25 412.5
T16 Control Nil Nil
*ES - Emulsifying System, CE - conventional emulsifier

Methodology
The experiment was conducted under field conditions at Ambala, Punjab. on cotton hybrid “F2228”. The experimental design followed a Randomized Block Design (RBD) with three replications. Each plot covered an area of 25 square meters, for precise measurements to be taken, 5 plants were tagged per treatment and pest count taken prior to the application. The test samples, according to the treatment schedule, were applied at pest appearance using 500 liters of water per hectare with a knapsack sprayer?fitted with hollow cone nozzle.

Observation
Pre-count Pest observation was taken before the spray application. Pest counts were recorded by randomly selecting five plants per treatment and counting number of bollworms per leaf. Observations were recorded on the 3rd, 7th, and 10th days after the spray application.

Table 46: Effectiveness of different treatments against Cotton Bollworm.
S. No. Treatments Dose g or ml/ha Effectiveness of different insecticide against Cotton Bollworm
Percent (%) reduction over control
Pre-count 3 DAA 7 DAA 10 DAA
sT1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 1.47 79.31 85.37 80.95
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 1.40 86.21 90.24 83.33
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 1.53 89.66 95.12 85.71
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 1.60 72.41 82.93 71.43
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 1.33 75.86 85.37 73.81
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 1.67 82.76 87.80 76.19
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275+137.5 1.53 58.62 63.41 61.90
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 1.60 62.07 70.73 69.05
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825+412.5 1.67 68.97 80.49 73.81
T10 Dinotefuran 20 % SG 275 1.33 20.69 26.83 23.81
T11 Dinotefuran 20 % SG 550 1.73 24.14 29.27 26.19
T12 Dinotefuran 20 % SG 825 1.20 34.48 43.90 35.71
T13 Bifenthrin 10% EC 137.5 1.73 51.72 58.54 52.38
T14 Bifenthrin 10% EC 275 1.13 55.17 60.98 54.76
T15 Bifenthrin 10% EC 412.5 1.80 58.62 63.41 59.52
T16 Control Nil 1.87 0.00 0.00 0.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Table 47: Synergistic effect of different treatments against Cotton Bollworm at 7 DAA.

S. no.
Treatment details Dose (ml or gm/Ha) % Reduction
over control of Cotton Bollworm 7 DAA
Observed Expected Ratio Synergy
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 85.37 69.66 1.23 Yes
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 90.24 72.40 1.25 Yes
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 95.12 79.48 1.20 Yes
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 82.93 69.66 1.19 Yes
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 85.37 72.40 1.18 Yes
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 87.80 79.48 1.10 Yes
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 63.41 69.66 0.91 No
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 70.73 72.40 0.98 No
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 80.49 79.48 1.01 Yes
T10 Dinotefuran 20 % SG 275 26.83 - - -
T11 Dinotefuran 20 % SG 550 29.27 - - -
T12 Dinotefuran 20 % SG 825 43.90 - - -
T13 Bifenthrin 10% EC 137.5 58.54 - - -
T14 Bifenthrin 10% EC 275 60.98 - - -
T15 Bifenthrin 10% EC 412.5 63.41 - - -
T16 Control Nil 0.00 - - -
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Result
The data recorded revealed that the population of cotton bollworms remained uniform throughout the experiment area prior to the application of treatments. The observation day before spray showed that bollworm populations varied between 1-2 per plant, respectively, and there was no significant difference among all the treatments. However, after 7 DAA, all the treatments showed a significant reduction in the population of aphids compared to the control. Amongst all the treatments, Dinotefuran 220 + Bifenthrin 55 g/L EC (ES) at 750 ml and 500 ml doses was the most effective for the reduction of cotton bollworm population.

Table 48: Yield study on Cotton Bollworm
S. no. Treatment details Dose (ml or gm/Ha) Yield T/Ha Percent increase over control (%)
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 250 16.47 29.08
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 500 17.40 36.38
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (WSES) 750 17.82 39.65
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 250 15.44 21.01
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 500 15.80 23.83
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (WCE) 750 16.36 28.19
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 15.32 20.05
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 15.60 22.26
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 15.87 24.33
T10 Dinotefuran 20 % SG 275 13.18 3.30
T11 Dinotefuran 20 % SG 550 13.87 8.67
T12 Dinotefuran 20 % SG 825 13.95 9.28
T13 Bifenthrin 10% EC 137.5 13.57 6.31
T14 Bifenthrin 10% EC 275 14.14 10.77
T15 Bifenthrin 10% EC 412.5 14.62 14.52
T16 Control Nil 12.76 0.00

Observation: The treatments with the Emulsifiable Concentrate composition of the present invention resulted in increased crop yield, implying that the present composition is synergistic and bio-effective.

Example 15:
Table 49: Effect of different treatments on natural enemy population on Cotton
S. No.? Treatment details? Dose gm or ml/Ha? Effect of insecticide treatment on natural enemy population
Coccinella septempunctata Chrysoperla carnea
Pre count 5 DAA 10 DAA? 15 DAA? Pre count 5 DAA 10 DAA? 15 DAA?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 1.33 1.67 2.00 2.00 3.33 3.67 4.00 4.00
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 2.33 1.67 1.00 2.00 4.33 3.67 3.00 4.00
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 2.33 1.33 1.67 0.67 4.33 3.33 3.67 2.67
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 1.00 1.67 2.00 1.00 3.00 3.67 4.00 3.00
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 1.33 2.00 1.00 1.67 3.33 4.00 3.00 3.67
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 1.67 1.33 1.67 2.33 3.67 3.33 3.67 4.33
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 2.33 1.33 2.33 2.00 4.33 3.33 4.33 4.00
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 1.33 1.33 0.67 1.33 3.33 3.33 2.67 3.33
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 1.33 1.00 1.67 1.33 3.33 3.00 3.67 3.33
T10 Dinotefuran 20 % SG 275 1.00 1.33 1.33 1.67 3.00 3.33 3.33 3.67
T11 Dinotefuran 20 % SG 550 2.33 1.67 1.67 0.67 4.33 3.67 3.67 2.67
T12 Dinotefuran 20 % SG 825 1.33 1.33 2.00 2.33 3.33 3.33 4.00 4.33
T13 Bifenthrin 10% EC 137.5 1.33 1.67 1.00 2.00 3.33 3.67 3.00 4.00
T14 Bifenthrin 10% EC 275 2.33 1.33 2.33 1.33 4.33 3.33 4.33 3.33
T15 Bifenthrin 10% EC 412.5 1.00 1.67 2.00 1.67 3.00 3.67 4.00 3.67
T16 Control Nil 1.33 1.33 1.00 2.00 3.33 3.33 3.00 4.00
*ES - Emulsifying System, CE - conventional emulsifier, DAA- days after application

Result
The composition of the present invention is safe on natural enemies in cotton ecosystems. There is no difference in natural enemy population count between any of the treatments and the untreated control.

Example 16: Evaluation of Phytotoxicity of the present invention composition on Cotton.

Visual observations were recorded at 7, 14 and 21 days after the application (DAA) of tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty and wilting based on 0-10 scale given in below table. A total of 20 plants per plot were observed.

Table 50: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
Leaf injury on tips /surface? Rating?
0%? 0?
1-10%? 1?
11-20%? 2?
21-30%? 3?
31-40%? 4?
41-50%? 5?
51-60%? 6?
61-70%? 7?
71-80%? 8?
81-90%? 9?
91-100%? 10?
Table 51: Phytotoxic effect of various treatments on Cotton after 7 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 7 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 52: Phytotoxic effect of various treatments on Cotton after 14 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 14 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 53: Phytotoxic effect of various treatments on Cotton after 21 DAA?at recommended dose.
S. No.? Treatment details? Dose gm or ml/Ha? 21 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 250 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 750 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 250 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 750 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 275 + 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 825 + 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 275 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 825 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 137.5 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 412.5 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 54: Phytotoxic effect of various treatments on Cotton after 7 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 7 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 55: Phytotoxic effect of various treatments on Cotton after 14 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 14 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Table 56: Phytotoxic effect of various treatments on Cotton after 21 DAA?at double dose (2X).
S. No.? Treatment details? Dose gm or ml/Ha? 21 DAA?
L? S? N? C? V? E? H? W?
T1 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 500 0? 0? 0? 0? 0? 0? 0? 0?
T2 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T3 Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T4 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 500 0? 0? 0? 0? 0? 0? 0? 0?
T5 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1000 0? 0? 0? 0? 0? 0? 0? 0?
T6 Dinotefuran 220 g/l + Bifenthrin 55 g/l EC (CE) 1500 0? 0? 0? 0? 0? 0? 0? 0?
T7 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 550 + 275 0? 0? 0? 0? 0? 0? 0? 0?
T8 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1100 + 550 0? 0? 0? 0? 0? 0? 0? 0?
T9 Dinotefuran 20% SG + Bifenthrin 10 % EC (Tank Mix) 1650 + 825 0? 0? 0? 0? 0? 0? 0? 0?
T10 Dinotefuran 20 % SG 550 0? 0? 0? 0? 0? 0? 0? 0?
T11 Dinotefuran 20 % SG 1100 0? 0? 0? 0? 0? 0? 0? 0?
T12 Dinotefuran 20 % SG 1650 0? 0? 0? 0? 0? 0? 0? 0?
T13 Bifenthrin 10% EC 275 0? 0? 0? 0? 0? 0? 0? 0?
T14 Bifenthrin 10% EC 550 0? 0? 0? 0? 0? 0? 0? 0?
T15 Bifenthrin 10% EC 825 0? 0? 0? 0? 0? 0? 0? 0?
T16 Control Nil 0? 0? 0? 0? 0? 0? 0? 0?
*DAA – Days after application, L-Leaf injury on tips/surface, S-stunting, N-Necrosis, C-Chlorosis, V- Vein clearing, E-Epinasty, H-Hyponasty, W-wilting?

Tables 51 to 53 above indicate that application of Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) in all doses showed no phytotoxicity symptoms like leaf injury on tips, leaf injury on the surface, wilting, vein clearing, necrosis, epinasty and hyponasty in cotton crop. Further, as evident from tables 54, 55 and 56, the application of Dinotefuran 220 + Bifenthrin 55 g/l EC (ES) at even double dose shows no phytotoxicity. Thus, applying the present invention composition may be considered completely safe for cotton crops.

Example 17: Evaluation of stability of different compositions

Table 57: Present Invention composition at Low Temperatures
Formulation Example No. Appearance at 25°C after 7 days Appearance at 10°C after 7 days Appearance at 5°C after 7 days Appearance at
0°C after 7 days Appearance at
-10°C after 7 days
Example 1
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 2
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 3
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 4 With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 5
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)

Table 57 shows that the present invention’s compositions are stable across varying temperature spectrums. No sign of crystallization or phase separation was observed, and have excellent water miscibility, confirming the emulsifiable properties. Moreover, the samples stored below 10°C remained liquid throughout the testing period, confirming the stability.

Table 58: Stability at 0°C and -10°C, and solubility in water

Properties Example 1 Example 2 Example 3 Example 4 Example 5
Cold stability @ 0ºC for 7 days Stable Stable Stable Stable Stable
Cold stability @ -10ºC for 7 days Stable Stable Stable Stable Stable
Solubility in Water Emulsifiable Emulsifiable Emulsifiable Emulsifiable Emulsifiable

Table 58 confirms that all the compositions of the present invention exhibit exceptional stability at low temperatures. The composition maintains stable liquid forms, indicative of successful emulsification, allowing for effective delivery of active ingredients without the risk of degradation due to temperature fluctuations. These properties make the formulations particularly suitable for agricultural applications where low-temperature stability is critical.

Example 18

Table 59: Comparative Low Temperature Stability Examples with and without emulsifying system

Formulation Example No. Appearance at 25°C after 7 days Appearance at 10°C after 7 days Appearance at 5°C after 7 days Appearance at 0°C after 7 days Appearance at -10°C after 7 days
Example 1
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 2
With ES
(Present invention composition) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow) Clear Transparent Liquid (Color – Yellow)
Example 7
Composition
Without
ES Haziness
(Phase Separation Issue)
Solid Particles Haziness
(Phase Separation
Issue)
Solid Particles Haziness
(Phase Separation
Issue)
Solid Particles Haziness
(Phase Separation
Issue)
Solid Particles Haziness
(Phase Separation
Issue)
Solid Particles

Composition with ES and without ES were subject to stability tests, specifically by assessing the appearance at various temperatures over 7 days. Examples 1 and 2 (present invention composition) having the ES, the compositions were remarkable stability across all tested temperatures: 25°C, 10°C, 5°C, 0°C, and -10°C. The compositions (examples 1 and 2) were clear, transparent liquid appearance, characterized by a yellow Color, indicating their robustness under the specified conditions.

In contrast, the example 7 (composition without ES) showed noticeable haziness and phase separation at the various temperatures (25°C, 10°C, 5°C, 0°C, and -10°C), thus confirming that said composition was unstable and lacks compatibility.

Therefore, it is evident that the present invention composition with ES is stable across various temperatures, has a desirable appearance, and extends its shelf life.

Further evaluation of the above compositions for stability at 0°C and -10°C, and solubility in water.

Table 60: Stability at 0°C and -10°C, and solubility in water.
Properties Example 1 Example 2 Example 7 Composition Without ES
Cold stability @ 0ºC for 7 days Stable Stable Unstable
Cold stability @ -10ºC for 7 days Stable Stable Unstable
Solubility in Water Emulsifiable Emulsifiable Crystallization in emulsion

Observation:

The compositions were evaluated for cold stability at both 0°C and -10°C for 7 days, alongside assessments of solubility in water.

The composition of the present invention (examples 1 and 2), formulated with ES, had excellent stability, and the emulsions maintained their desired characteristics and showed no signs of instability, demonstrating their resilience at lower temperatures.

However, example 7 (composition without ES) had multiple issues, such as compatibility problems, stability concerns, and evidence of crystallization within the emulsion. Such challenges indicate a marked deterioration in performance when the compositions are prepared without the ES, emphasizing the critical role that ES plays in enhancing the stability and overall quality of the emulsions.

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

1. A insecticidal composition comprising:
dinotefuran;
bifenthrin;
an emulsifying system; and
a co-solvent.

2. The insecticidal composition as claimed in claim 1, wherein the emulsifying system is a blend of Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol NP Ethoxylate, heavy aromatic & Triethylene Glycol Monoethyl Ether, Castor Oil Ethoxylate, and n-Butanol.

3. The insecticidal composition as claimed in claim 1, wherein the emulsifying system is a blend of Calcium Salt of Alkyl Benzene Sulfonate, Polyoxyethylene ether of Cardanol, NP Ethoxylate, Heavy Aromatic & Triethylene Glycol Monoethyl Ether.

4. The insecticidal composition as claimed in claim 1, wherein
dinotefuran is present in an amount of 1 to 40% by weight;
bifenthrin is present in an amount of 1 to 40% by weight;
the emulsifying system is present in an amount of 1 to 30% by weight; and
the co-solvent is present in an amount of 1 to 60% by weight.

5. The insecticidal composition as claimed in claim 1, wherein the co-solvent is N-Methyl-2-pyrrolidone.

6. A insecticidal composition, comprising:
dinotefuran;
bifenthrin;
an emulsifying system;
a co-solvent; and
a solvent.

7. The insecticidal composition as claimed in claim 6, comprising a solvent, the solvent is a mixed isomer of benzene, 1, 2, 4-trimethyl and benzene, ethylmethyl (C9 Solvent).

8. The insecticidal composition as claimed in claims 1 to 7, further comprising carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, stabilizers or any combination thereof.

9. A process for preparation of insecticidal composition, the process comprising:
a) weighing of required quantity of co-solvent;
b) adding dinotefuran to co-solvent under stirring to form a mixture;
c) sequentially adding a solvent and bifenthrin to the above mixture under continuous stirring; and
d) adding an emulsifying system into the mixture of step c) under stirring to obtain a final insecticidal composition.

10. The process as claimed in claim 9, wherein the mixture of step b) is stirred at a speed of 100 RPM for a duration ranging from 40-60 minutes.

11. The process as claimed in claim 9, further comprising the addition of carriers, binders, disintegrating agents, dispersants or dispersing agents, wetting agents, pH modifiers, thickeners, biocides, preservatives, anti-freezing agents, colorants, defoamers, stabilizers or any combination thereof.