AN INSECTICIDAL COMPOSITION AND A PROCESS FOR PREPARATION THEREOF

FIELD

The present disclosure relates to an insecticidal composition and a process for preparation thereof.

DEFINITIONS

As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used indicate otherwise. Insecticide: An insecticide is a substance or a mixture of substances intended for preventing, destroying or controlling any insect, including vectors of human or animal disease, or animals causing harm or interfering with the production, processing, storage, transport or marketing of food, agricultural commodities, wood and wood products or animal feedstuffs, or substances which may be administered to animals for the control of insects, arachnids or other pests in or on their bodies.

Acaricide: Acaricides are pesticides that kill members of the arachnid subclass Acari, which includes ticks and mites.

Neonicotinoid: Neonicotinoids are a class of neuro-active insecticides that disrupts an insect's nervous system by inhibiting nicotinic acetylcholine receptors. BACKGROUND

The use of insecticides to control insects in crops is a universal practice. Insecticides are commonly applied to plants, as liquid or solid compositions. This practice has gained a high degree of commercial success because it has been shown that such control can increase crop yield. Intensive application of insecticides can cause the development of insecticide resistance in pest/insect species. Due to this resistance there is a remarkable decrease in the crop yield. Pest/insect species evolve insecticide resistance via natural selection: the most resistant specimens survive and pass on their genetic traits to their offspring. Such resistance is increasing globally and thus invariably reduces the crop yield.

Therefore, effective use of insecticides, require sound management, in view of increasing insects / pests resistance, environmental hazards and worker exposure concerns. In order to maximize crop production, it is necessary to protect crops from insects/pests. The incidence of development of resistance to a combination of insecticides reduces when compared to use of a single insecticide.

Thus, there exists a need for combination products involving insecticides which can be applicable in the field of agriculture for better protection and growth of crops and other plants.

Combinations containing different insecticides compositions have been practiced in the art, but problems with the physical stability of such combinations have caused issues with respect to the application and efficacy in many cases.

OBJECTS Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:

It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.

Another object of the present disclosure is to provide an insecticidal composition. Still another object of the present invention is to provide an improved, stable and ready to use insecticidal composition having a synergistic effect.

Yet another object of the present disclosure is to provide a process for preparing the insecticidal composition.

Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure. SUMMARY

The present disclosure in an aspect provides an insecticidal composition effective against insects including arachnids. The insecticidal composition comprises Dinotefuran, Diafenthiuron and agrochemically acceptable excipients. Typically, the ratio of Dinotefuran to Diafenthiuron is in the range of 1 :0.5 to 1: 10.

The present disclosure in another aspect provides a process for preparing an insecticidal composition. The process comprises blending pre-determined amounts of Diafenthiuron, and a first set of agrochemically acceptable excipients to obtain a first mixture. The first mixture is then ground in a jet mill to obtain a wettable powder. The wettable powder is blended with pre-determined amounts of Dinotefuran, and a second set of agrochemically acceptable excipients to obtain a second mixture. The second mixture is blended with pre-determined amounts water, and a third set of agrochemically acceptable excipients to obtain a dough, which is extruded to obtain granules having a particle size in the range of 0.5 mm to 2 mm. The granules are dried to obtain the insecticidal composition. In a further aspect, the present disclosure further provides a kit-of-parts. The kit-of-parts configurable as an agrochemical composition adapted to be stored, transported, and discharged for treatment of plants, its habitat, soil, a crop or a crop field. The kit-of-parts comprises (a) a first insecticidal component comprising Diafenthiuron in an amount 5 mass to 52 mass of the total mass of the composition along with a first set of agrochemically acceptable excipients in the form of a wettable powder, (b) a second insecticidal component comprising Dinotefuran in an amount 3 mass to 10 mass of the total mass of the composition along with a second set of agrochemically acceptable excipients and a third set of agrochemically acceptable excipients, and (c) an instruction manual comprising instructions for mixing the first and second insecticidal components in a predetermined ratio and treating the plants, its habitat, soil, a crop or a crop field.

The synergistic action of Dinotefuran and Diafenthiuron, along with the specific combination of the ingredients used provides improved sticking property, and high attrition resistance. The suspensibility and sticking properties of the insecticidal composition of the present disclosure result in improved bio-efficacy. DETAILED DESCRIPTION

In recent years there is a need to increase the efficacy of acaricides and insecticides by broadening their spectrum, for effectively controlling the growth of different pests or insects simultaneously. The present disclosure envisages an insecticidal composition and a process for preparation thereof.

The composition comprises an acaricidal compound, a neonicotinoid compound and agrochemically acceptable excipients. The insecticides having different modes of action, when used in combination are more effective and have higher potency and activity level as compared to the use of individual pesticides. Typically, the acaricidal compound is Diafenthiuron and the neonicotinoid compound is Dinotefuran.

In accordance with one aspect of the present disclosure there is provided an insecticidal composition effective against insects including arachnids. The composition comprises Dinotefuran, Diafenthiuron, and agrochemically acceptable excipients. Typically, the composition can be in at least one dosage form selected from the group consisting of water dispersible granules, wettable powder, microemulsion, and suspension concentrate. In one embodiment, the insecticidal composition is in the form of water dispersible granules having a particle size in the range of 0.5 mm to 2 mm.

The ratio of Dinotefuran and Diafenthiuron can be in the range of 1 :0.5 to 1 :10. In an embodiment, the ratio of Dinotefuran and Diafenthiuron is 1 :6.

Diafenthiuron, also known as l-tert-butyl-3-(2, 6-diisopropyl-4-phenoxyphenyl)thiourea is a chemical compound belonging to the class of thioureas, having the chemical formula C2 ₃ H ₃ 2N2OS. It acts by inhibiting the ATP synthesis.

Diafenthiuron Dinotefuran, also known as (RS)-l-methyl-2-nitro-3-(tetrahydro-3-furylmethyl) guanidine is an insecticide of the neonicotinoid class, and its mechanism of action involves disruption of the insect's nervous system by inhibiting nicotinic acetylcholine receptors.

In an embodiment of the present disclosure, the insecticidal composition comprises Dinotefuran in an amount in the range of 3 mass to 10 mass of the total mass of the composition, Diafenthiuron in an amount in the range of 5 mass to 52 mass of the total mass of said composition and an agrochemically acceptable excipients.

In accordance with the embodiment of the present disclosure, the agrochemically acceptable excipients are selected from the group consisting of a binder; a dispersing agent; a wetting agent; a carrier; an anti-caking agent; a defoamer; and a stabilizer In an embodiment of the present disclosure, the binder is in an amount in the range of 0.1 mass to 15 mass of the total mass of the composition, the dispersing agent is in an amount in the range of 1 mass to 20 mass of the total mass of the composition, the wetting agent is in an amount in the range of 0.5 mass to 3 mass of the total mass of the composition, the carrier is in an amount in the range of 1 mass to 50 mass of the total mass of the composition, the anti-caking agent is in an amount in the range of 0.1 mass to 3 mass of the total mass of the composition, the defoamer is in an amount in the range of 0.1 % to 2 % of the total mass of the composition, and the stabilizer is in an amount in the range of 0.1 mass to 3 mass % of the total mass of the composition.

In an embodiment, the binder can be at least one selected from the group consisting of polyvinyl alcohol, polyvinylpyrrolidone, polyacrylamides, dextrose, sucrose, malt dextrin and lactose, sodium carboxymethyl cellulose, cross linked sodium carboxymethyl cellulose and starch, hydroxy propyl methyl cellulose, and composite blend of poly-vinyl pyrrolidone and methyl-vinyl ether/maleic acid half ester neutralized copolymer (2-butenedioic acid (2Z) monobutyl ester, polymer with methoxyethene sodium salt). The binder binds the ingredients in the composition together and also aids in sticking/adhering of the composition to the leaves, for better control of insects. In an embodiment, the binder is hydroxy propyl methyl cellulose, and composite blend of poly-vinyl pyrrolidone and methyl-vinyl ether/maleic acid half ester neutralized copolymer (2-butenedioic acid (2Z) monobutyl ester, polymer with methoxyethene sodium salt), having a ratio of 1 : 1. The dispersing agent can be at least one selected from the group consisting of sodium lignosulfonate, calcium lignosulfonate, sodium salt of alkyl naphthalene sulfonate, sulfonated aromatic polymer sodium salt, polycarboxylic acid homopolymer, sodium salt of polycarboxylic acid homopolymer, polycarboxylic acid copolymer, ethylene oxide/Propylene oxide (EO/PO) block copolymers, sodium salt of polycarboxylic acid copolymer, sodium poly (naphthalene formaldehyde) sulfonate, high molecular weight polymeric ionic dispersant and Kraft lignosulphonates. The dispersing agent aids in the uniform dispersion of the active ingredients throughout the dosage form.

The wetting agent can be at least one selected from the group consisting of non-ionic surfactant, anionic surfactant and combinations thereof. The non-ionic surfactant can be at least one selected from the group consisting of, but not limited to, alcohol ethoxylates having moles of ethylene oxide in the range of 8 to 13. The anionic surfactant can be at least one selected from the group consisting of alkyl naphthalene sulfonate, dialkyl naphthalene sulfonates, alkyl naphthalene sulfonate condensate, sodium lauryl sulphate, sodium dodecyl benzene sulfonate and Sulfosuccinic acid Bis (2-ethyl hexyl) ester sodium salt. The wetting agent can be at least one selected from the group consisting of alkyl ethylene oxide condensates, aryl ethylene oxide condensates, alkyl propylene oxide condensates, aryl propylene oxide condensates, alkylethoxylates and arylethoxylates. Typically, the alkyl group and aryl group in the wetting agent can be a C ₁ -C2 ₀ alkyl group or C ₁ -C2 ₀ aryl group. The wetting agent is used to wet the ingredients of the composition by water by lowering the surface tension.

The carrier can be at least one selected from the group consisting of clay calcium carbonate, minerals, perlite and talc. Typically, the clay can be selected from kaolinite clay, and bentonite clay. The carrier acts as a diluent or a bulking agent in the composition.

The anti-caking agent can be at least one selected from the group consisting of clays, precipitated silica and metal stearates. The anti-caking agent is used to prevent cake formation in the composition during storage. The defoamer can be at least one selected from the group consisting of polydimethylsiloxane powder and polydimethylsiloxane liquid. The defoamer is used to prevent foaming of the composition.

The stabiliser can be at least one selected from the group consisting of butylated hydroxy toluene, epoxidized soybean oil and acrylic emulsion based products.

In an embodiment of the present disclosure, insecticidal composition comprises 8.4 mass of Dinotefuran having a purity of 99.1 % with respect to the total mass of the composition, 51 mass of Diafenthiuron having a purity of 96 % with respect to the total mass of the composition, 1 mass of composite blend of poly-vinyl pyrrolidone and methyl-vinyl ether/maleic acid half ester neutralized copolymer (2-butenedioic acid (2Z) monobutyl ester, polymer with methoxyethene sodium salt) with respect to the total mass of the composition, 1 mass of hydroxy propyl methyl cellulose with respect to the total mass of the composition, 1 mass of sulfosuccinate sodium salt with respect to the total mass of the composition, 3 mass of naphthalene sulfonic acid polycondensate sodium salt with respect to the total mass of the composition, 5 mass of sodium salt of acid resin copolymer with respect to the total mass of the composition, 1 mass of sodium carboxymethyl cellulose with respect to the total mass of the composition, 25.3 mass of kaolin with respect to the total mass of the composition, 3 mass of perlite with respect to the total mass of the composition, 0.1 mass of butylated hydroxy toluene with respect to the total mass of the composition, and 0.2 mass of silicon with respect to the total mass of the composition. In accordance with another aspect of the present disclosure there is provided a process for preparing the insecticidal composition effective against insects including arachnids. The process involves the following steps:

Initially, pre-determined amounts of Diafenthiuron, and a first set of agrochemically acceptable excipient are blended to obtain a first mixture.

The first set of agrochemically acceptable excipients comprises a carrier and a wetting agent.

The first mixture is ground in a jet mill to obtain a wettable powder, having a particle size in the range of 2 micron to 5 micron.

The wettable powder is blended with pre-determined amounts of Dinotefuran, and a second set of agrochemically acceptable excipients to obtain a second mixture, having a particle size in the range of 2 micron to 8 micron. The second set of agrochemically acceptable excipients comprises a dispersing agent, a sticking agent, a binder, a carrier, and a stabilizer.

The second mixture is blended with pre-determined amounts of water, and a third set of agrochemically acceptable excipients to obtain a dough. The third set of agrochemically acceptable excipients comprise an anti-caking agent, and a defoamer.

The dough is extruded to obtain granules having a particle size in the range of 0.5 mm to 2 mm.

The granules are then dried at a temperature in the range of 35 °C to 65 °C to obtain the insecticidal composition. In an embodiment, the granules are dried at a temperature of 40 °C.

The granules can be dried in a fluid bed dryer or tray dryer.

Typically, the moisture content in the insecticidal composition of the present disclosure can be less than 2% and the granule size can be in the range of 0.5 mm to 2 mm.

Typically, the insecticidal composition prepared by the process of the present disclosure is in the form of wettable powder or granules and is adapted to be mixed with water, at least one defoamer to obtain a suspension concentrate, prior to application.

In an embodiment of the present disclosure, the carrier used to prepare the first mixture and the second mixture is same. In another embodiment of the present disclosure, the carrier used to prepare the first mixture and the second mixture is different. The present disclosure is further described in light of the following laboratory scale experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. These laboratory scale experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial/commercial scale. Experimental Details

Experiment- 1: Preparation of the insecticidal composition in accordance with the present disclosure

The insecticidal composition in accordance with the present disclosure was prepared by the 5 following general procedure. The specific ingredients used and the amount of the ingredients

used is summarized in Table- 1.

Diafenthiuron, a carrier and a wetting agent were charged into a Sigma blender, and blended for 30 minutes to obtain a first mixture. The first mixture was ground in a jet mill to obtain a wettable powder, having a particle size in the range of 2 to 5 microns. The wettable powder

10 was then blended with Dinotefuran, dispersing agent, binder, carrier, and stabilizer, in a

ribbon blender and blended for 2 hours to obtain a second mixture. The second mixture was then blended with an anti-caking agent, defoamer and water in a dough maker to obtain a dough. The dough was extruded using a basket extruder to obtain granules having granule size in the range of 0.5 mm to 2 mm, which was then dried in a fluid bed dryer at 40 °C to

15 obtain the insecticidal composition.

Table-1: Examples of the insecticidal composition prepared in accordance

with the present disclosure*

Example Dl Kaolin SDS D2 Polymer NAS CMC P-20 HPMC Perlite Lactose BHT Silicon Water Suspensibility Suspensibility- No. (%w/w) AHS

(%w/w)

1 8.3 55 2 8.4 10 10 3 0.1 0.2 15 92% 90%

2 16.6 46.7 2 8.4 10 10 ^{1 1 1} 3 — 0.1 0.2 15 93% 90%

3 24.9 38.4 2 8.4 10 10 ^{1 1 1} 3 — 0.1 0.2 15 93% 91 %

4 33.1 31.2 2 8.4 10 10 3 —

^{1 1 1} 0.1 0.2 15 94% 91 %

5 41.1 22.9 ¹ 8.4 10 10 ^{1 1 1} 3 — 0.1 0.2 15 93% 92%

6 51 25.3 ¹ 8.4 5 3 ^{1 1 1} 3 0.1 0.2 15 90% 87%

7 51 26.3 ¹ 8.4 5 3 —

^{1 1} 3 — 0.1 0.2 15 90% 89%

8 51 26.3 ¹ 8.4 5 3 ¹ 1 — 3 — 0.1 0.2 15 94% 80%

9 51 25.3 8.4 5 3 3 3 0.1 0.2 15 95% 75%

10 51 27.4 8.4 5 3 1 3 0.2 15 95% 94% 1 8.4 1 10 3 0.1 0.2 15 93% 75%

* All the quantities are given in grams (g).

Dl=Diafenthiuron; D2= Dinotefuron; SDS= Sulfosuccinate sodium salt; Polymer= Sodium salt of acid resin copolymer; NAS=Naphthalene sulfonic acid polycondensate sodium salt; CMC= sodium carboxymethyl cellulose; P-20= composite blend of poly-vinyl pyrrolidone and methyl-vinyl ether/maleic acid half ester neutralized copolymer (2-butenedioic acid (2Z) monobutyl ester, polymer with methoxyethene sodium salt) ; BHT= butylated hydroxy toluene; HPMC: Hydroxy propyl methyl cellulose having molecular weight in the range of 10000 to 1500000, AHS- accelerated storage studies.

Storage study of the insecticidal composition of the present disclosure:

The storage studies of the insecticidal composition of the present disclosure was carried out as per CIPAC procedure method no MT 46.3 and are provided in Table- 1.

A sample (20 g) was placed in glass bottle fitted with a polyethylene insert which was subsequently closed and placed in an oven at 54+2° C for 14 days. After 14 days samples were removed from the oven and allowed to reach the room temperature.

From Table- 1 it is observed that the insecticidal composition of Examples 1 to 7 and 10 are stable and there is no significant drop in suspensibility even after accelerated storage study (AHS), whereas in compositions 8, 9, and 11 a drop in suspensibility is observed. In composition of Examples 1 to 7, the combination of 3 % NAS, 5 % polymer + 1 % SDS + 1% CMC + binders (1 % HPMC + 1 % P-20) surprisingly prevented the drop in suspensibility even after the accelerated storage study. In composition 10, the combination of 3 % NAS, 5 % polymer + 1% SDS + 1 % CMC, also prevented the drop in suspensibility. In the composition of Example-11, it is seen that the combination of 10 % NAS, 1 % polymer, 1% SDS + 1 % CMC is unstable and a drop in suspensibility is observed. In composition 8, a combination of surfactants, CMC and binder P-20 is used, which is unstable and a drop in suspensibility is observed. In the composition of Example- 9, a combination of surfactants and lactose is used, which is unstable and a drop in suspensibility is observed. It is evident from the results obtained in Table- 1 that the combination of surfactants and the amount of surfactants used in the present disclosure is important for imparting stability to the insecticidal composition.

Study of the sticking property of the insecticidal composition of the present disclosure: The percentage retention (sticking property) of the insecticidal composition of the present disclosure was determined using the following method.

5 g of Dinotefuran + Diafenthiuron WG mixture of Examples 1-9 was weighed in a 50 mL volumetric flask and water was added to form a suspension. Clean glass slides were tarred on a Mettler balance and 5 g of suspension was added to the glass plate, and the exact weight of the material added was determined. The slides were air dried under a laboratory hood. The slides containing the dried material were washed with 10 mL of water and also with 25 mL of water (water was applied from a pipette on the slides kept at an angle of 45°). The washed slides were air dried and the residue quantified by gravimetric method. The result obtained is summarized in Table-2. It is observed that more the residue on the glass plate, more is the sticking property of the compositions.

Table-2: Study of the sticking property of the insecticidal composition of the present disclosure

Ratio of Dinotefuron Binder quantity After spraying with 10 mL After spraying with 25 mL Diafenthiuron of water of water

(%) retention on glass (%) retention on glass plate plate

Example 1 (P-20) 1% (HPMC) 1% 53.7% 29.5% Example 2 P-20) 1% (HPMC) 1% 57.5% 31.1%

Example 3 P-20) 1% (HPMC) 1% 59.88 30.11%

Example 4 P-20) 1% (HPMC) 1% 66.2% 38.4%

Example 5 P-20) 1% (HPMC) 1% 77.2% 61.1%

Example 6 (P-20) 1% (HPMC) 1% 87% 71%

Example 7 (HPMC) 1% 61.1% 31.6%

Example 8 (P-20) % 60% 28.6%

Example 10 44% 22%

It is seen from Table-2 that the percentage retention on the glass plate was 44% for the insecticidal composition without the binder (composition of Example- 10), when 10 mL water was sprayed, and 22 % when 25 mL water was sprayed. When a single binder was used such as HPMC as per composition of Example-7, the percentage retention on glass plates were 61.1 % and 31.61 %, respectively when 10 mL and 25 mL of water was sprayed. When single binder was used such as P-20 as per composition of Example-8, the percentage retention on glass plates were 60 % and 28.6 %, respectively when 10 mL and 25 mL of water was sprayed.

However, it is surprisingly observed that the combination of Binders (1 % P-20 + 1 % HPMC) used in the present disclosure enhances the sticking property of the insecticidal composition as observed in the composition of Example-6 (87 % when 10 mL water was sprayed, and 71 % when 25 mL water was sprayed).

Experiment-2: Study of bioefficacy of the insecticidal composition of the present disclosure

The details of the crop used, the target pests, the application duration, and the treatment details of the insecticidal composition used are summarized in Tables 3 5 and 4 below.

Table-3: Details of the bioefficacy study

0 Table-4: Bio-efficacy Treatment Details:

The bio-efficacy of the ready tank mix formulations of the insecticidal composition of the present disclosure having different ratios of Dinotefuron and Diafenthiuron, namely 1: 1, 1 :2, 1 :4, 1:5, and 1 :6, were studied. Compositions 5 comprising Dinotefuron and Diafenthiuron as the individual insecticide were also tested. The untreated cotton crop was treated as the Control. The bio-efficacy studies were carried out against Whitefly, Thrips, Aphids, Jassids and Mites on Cotton crop. The insecticides were applied as a foliar spray with Knapsack Sprayer fitted with a hollow cone nozzle. Application was initiated with build of 10 pest population to Economical Threshold Level (ETL) in the field. The sprayings were done at 15 days interval.

One day prior of the initiation of the study, pest incidence was recorded, and subsequent observations were recorded after 5, 10 and 15 days of each spray. The Whitefly, Jassids, Thrips and Aphids were counted on 5 pre-tagged plants per plot 15 as 6 leaves selected randomly / plant (2 leaves each from top, middle and bottom).

For Mites, the population per 4 cm was counted using a 10X hand lens with graduated platform, on five leaves from the top portion per plant. The mean value was derived from the treatment and used for Statistical analysis of the data.

Seed cotton from each net plot was recorded at picking and weighed separately for 20 calculating the yield. Three pickings were carried out and at the end of last picking, total yield from each net plot was calculated and computed on a hectare basis (Kg/ha) and statistically analysed the data.

Individual plot wise yield was recorded on different pickings and calculated treatment wise mean yield and converted into yield per hectare (Kg/ha) and 5 statistically analysed the data.

The analysis of variance was calculated by using MS- Excel Computer Program, and the results are summarized in Tables 5 to 9.

Table-5: Bio-efficacy of different Insecticides treatments against Whitefly of

10 Cotton

Figures in parenthesis are arcsine transformed values; DAA- Days after Application; NS-

Non significant; CD - Critical difference (P- probability at 5% level of significance). It is seen from Table-5 there was a uniform population of Whitefly across all the

treatments, at the start of the study. At 5 days after first application, the highest Whitefly population was recorded in the control (6.83/leaf). It is observed that all 5 the insecticide treatments were capable of reducing the Whitefly population as

compared to the untreated control, but the significant lowest number of Whitefly was observed in T5 (0.4/leaf). At 5 days after the second application, the highest Whitefly population was recorded in the control (7.37/leaf). The significant lowest Whitefly population was observed in T5 (0.11/leaf). A similar trend was observed 10 on 10 days after the first and second application, and 15 days after the first

application. It is seen from Table-5 that the treatment T5 recorded the least number of Whitefly at 15 days after second spray (0.30/leaf), followed by T4 (0.78/leaf) and T3 (0.82/leaf). The highest number of Whitefly was recorded in treatment T8 (7.67/leaf) which was the untreated control.

15 Table-6: Bio-efficacy of different Insecticides treatments against Jassids of

Cotton

Tr. Treatment Details Dose Dose Pre- count Mean Number of Jassids/leaf

No (g a.i./ha) (mL or g ha)

5 DAA 10 DAA 15 DAA 5 DAA 10 DAA 15 DAA 1" spray 1" spray 1" spray 2 ^nd spray 2 ^nd spray 2 ^nd spray

Ti Dinotefuron 8% + 50 + 50 625 4.67 1.26 1.37 1.12 0.96 1.31 1.37 Diafenthiuron 8% (12.46) (6.43) (6.71) (6.43) (5.61) (6.54) (6.71) WG

T ₂ Dinotefuron 8 % + 50 + 100 625 4.67 0.85 1.08 0.96 0.62 0.83 0.82 Diafenthiuron 16% (12.46) (5.30) (5.95) (5.30) (4.52) (5.24) (5.20) WG

T ₃ Dinotefuron 8% + 50 + 200 625 4.33 0.68 0.89 0.79 0.44 0.57 0.63 Diafenthiuron 32% (12.00) (4.72) (5.40) (4.72) (3.82) (4.31) (4.56) WG

T ₄ Dinotefuron 8% + 50 + 250 625 4.33 0.51 0.77 0.64 0.28 0.43 0.48 Diafenthiuron 40% (12.33) (4.11) (5.02) (3.96) (3.03) (3.77) (3.97) WG

T ₅ Dinotefuron 8% + 50 + 300 625 4.67 0.08 0.17 0.32 0.06 0.12 0.22 Diafenthiuron 48% (12.46) (1.61) (2.33) (1.61) (1.11) (1.98) (2.69) WG

T ₆ Dinotefuron 20% 50 250 4.67 2.27 2.49 1.86 1.49 1.64 1.62 SG (12.46) (8.66) (9.07) (9.48) (7.00) (7.37) (7.31)

T ₇ Diafenthiuron 50% 300 600 4.67 2.71 2.87 2.13 2.14 2.27 2.37 WP (12.46) (9.48) (975) (8.66) (8.42) (8.67) (8.85) τ ₈ Tank Mix 50+300 250 + 600 4.67 1.54 1.43 1.42 1.22 1.44 1.62 (Dinotefuron 20% (12.46) (7.14) (6.87) (6.71) (6.35) (6.86) (7.32) SG +

Diafenthiuron 50%

WP)

τ ₉ Control 4.67 7.00 7.99 8.02 8.03 9.06 9.01

(12.46) (15.33) (16.42) (15.33) (16.46) (17.51) (17.47)

CD (Ρ=0.05) NS 0.41 0.15 0.12 0.17 0.29 0.12

Figures in parenthesis are arcsine transformed values; DAA- Days after Application; NS-

Non significant; CD - Critical difference (P- probability at 5% level of significance).

It is seen from Table-6 that at the time of initiation of trial there was no significant

difference between the treatments, which indicates a uniform prevalence of the

pest. At 5 days after first application, the highest number of Jassids was recorded in control (7.00/leaf). The significant lowest Jassids population was observed in

T5 (0.08/leaf). A similar trend was observed on 10 days after first application. At

15 days after the first application, significantly less number of Jassids was

observed in treatment T5. The highest number of Jassids was recorded in control

(8.02/leaf). At 5 days after second application, there is a significant suppression of

Jassid population in the treatments. Very less number of Jassids were observed in T5 (0.06/leaf) which is lowest and the highest was in untreated control that is T9

(8.03/leaf). A similar trend was observed on 10 days and at 15 days after the

second application. The significant lowest Jassids were observed in treatment T5

(0.22/leaf). The highest population of Jassids was observed in the untreated

control (9.01/leaf).

Table-7: Bio-efficacy of different Insecticides treatments against Thrips of Cotton

Tr. Treatment Details Dose Dose Pre-count Mean Number of Thrips/leaf

No (g a.iVha) (mL or g/ha)

5 DAA 10 DAA 15 DAA 5 DAA 10 DAA 15 DAA 1" spray 1" spray 1" spray 2 ^nd spray 2 ^nd spray 2 ^nd spray

Ti Dinotefuron 8% + 50 + 50 625 2.92 1.05 1.19 1.30 0.43 0.52 0.94 Diafenthiuron 8% WG (9.80) (5.87) (6.25) (6.55) (3.76) (4.12) (5.57)

T ₂ Dinotefuron 8 % + 50 + 100 625 2.75 0.81 0.85 0.94 0.31 0.44 0.75 Diafenthiuron 16% (9.50) (5.16) (5.26) (5.52) (3.19) (3.78) (4.98) WG

T ₃ Dinotefuron 8% + 50 + 200 625 3.03 0.39 0.64 0.64 0.14 0.33 0.51 Diafenthiuron 32% (10.03) (3.58) (4.57) (4.57) (2.17) (3.31) (4.09) WG τ ₄ Dinotefuron 8% + 50 + 250 625 2.89 0.34 0.32 0.44 0.09 0.21 0.30

Diafenthiuron 40% (9.79) (3.36) (2.64) (3.78) (1.71) (2.63) (3.14)

WG

τ ₅ Dinotefuron 8% + 50 + 300 625 2.86 0.00 0.07 0.11 0.00 0.03 0.12

Diafenthiuron 48% (9.67) (0.00) (1.44) (1.90) (0.00) (0.99) (1.96)

WG

τ ₆ Dinotefuron 20% SG 50 250 2.63 1.62 2.21 2.22 1.02 1.11 1.43

(9.29) (7.28) (8.55) (8.57) (5.80) (6.04) (6.88) τ ₇ Diafenthiuron 50% 300 600 2.88 1.52 1.72 1.85 0.83 0.97 1.30

WP (9.77) (7.08) (7.54) (7.81) (5.24) (5.64) (6.55)

Tg Tank Mix 50+300 250 + 600 2.86 1.33 1.38 1.53 0.61 0.81 1.02

(Dinotefuron 20% SG (9.72) (6.63) (6.75) (7.11) (4.49) (5.17) (5.80)

+ Diafenthiuron 50%

WP)

τ ₉ Control - - 2.98 3.66 4.15 4.13 4.24 4.29 4.31

(9.94) (11.02) (11.76) (11.72) (11.88) (11.95) (11.98)

CD (Ρ=0.05) NS 0.32 0.28 0.20 0.10 0.10 0.06

Figures in parenthesis are arcsine transformed values; DAA- Days after Application; NS-

Non significant; CD - Critical difference (P- probability at 5% level of significance).

5 It is seen from Table-7 that at the time of the initiation of trial, the thrips

population was uniformly present across the plot. At 5 days after first application, the highest number of Thrips was recorded in untreated control (3.66/leaf). The lowest number of Thrips was observed in T5 (0.00/leaf). A similar pattern was recorded on 10 days after the first application. At 15 days after first

10 application, significantly less number of Thrips was observed in treatment T5(0.11/leaf). The highest Thrips was recorded in control (4.13/leaf). At 5 days after the second application, there was a significant suppression of Thrips population in all the insecticide spray treatments. The treatment T5 was found free from Thrips infestation, and the highest population of Thrips was noticed in

15 untreated control T9 (4.24/leaf). A similar trend was observed on 10 days after the second application, and at 15 days after the second application. The lowest number of Thrips was recorded in treatment T5 (0.12/leaf). The highest number of

Thrips was observed in the untreated control (4.31/leaf).

20 Table-8: Bio-efficacy of different Insecticides treatments against Aphids of

Cotton

Figures in parenthesis are arcsine transformed values; DAA- Days after Application; NS- Non significant; CD - Critical difference (P- probability at 5% level of significance).

5

It is seen from Table-8 that, at the time of initiation of the trial, the population of Aphids was uniform across the plot and was building up. At 5 days after the first application, the highest number of aphids was recorded in the untreated control (8.16/leaf). The lowest number of aphids was observed in T5 (0.30/leaf). The population of Aphids in untreated control increased on 10 days after the first application. At 15 days after the first application, there was significantly less number of aphids observed in treatment T5 (0.94/leaf). The highest number of aphids was recorded in the untreated control (14.49/leaf). Five days after the second application, the Aphid population was suppressed in all the treatments except the untreated control. A similar trend was observed at 10 days and at 15 days after the second application. It is seen from Table-8 that the least number of aphids were recorded in treatment T5 (0.07/leaf), and the highest number of 5 aphids was recorded in the untreated control T9 (16.18/leaf).

Table-9: Bio-efficacy of different Insecticides treatments against Mites of Cotton

Figures in parenthesis are arcsine transformed values; DAA- Days after Application

significant; CD - Critical difference (P- probability at 5% level of significance). It is seen from Table-5 that, at the time of initiation of trial, the population of mites was uniform in the range of 15.07-16.58/ 4 cm ^" across the plots and was building up. At 5 days after the first application, the highest number of mites was recorded in the untreated control (17.63/ 4 cm ^" ). The lowest number of mites was

5 observed in T5 (1.10/ 4cm ^" ). A similar trend was observed at 10 days after the first application. At 15 days after the first application, there was significantly less number of mites observed in treatment T5 (2.08/ 4 cm ^" ). The highest mite

_2

population was recorded in control (18.17/ 4 cm ^" ). At 5 days after the second application, the Mite population was suppressed in all the treatments except in the

10 untreated control and Dinotefuran 20 % SG. The treatment T5 recorded the least

_2 _2

number of mites per cm ^" (0.07/ 4 cm ^" ), which is lowest among all the treatments

_2

and the highest was in the untreated control T9 (17.84/ 4 cm ^" ). A similar trend was observed for 10 days and at 15 days after the second application. The lowest

_2

mite population was observed in treatment T5 (0.23/ 4 cm ^" ), and the highest mite

_2

15 population was observed in the untreated control (19.67/ 4 cm ^" ).

The yield obtained from the cotton crop treated with different insecticidal composition of the present disclosure is summarized in Table- 10.

Table-10: Effect of treatment of different insecticidal composition on Cotton

Yield

Tr. No Treatment Details Dose (g a.i./ha) Dose (mL or g/ha) Yield (kg/ha)

Ti Dinotefuron 8% + Diafenthiuron 8% WG 50 + 50 625 1722

T ₂ Dinotefuron 8 % + Diafenthiuron 16% WG 50 + 100 625 1793

T ₃ Dinotefuron 8% + Diafenthiuron 32% WG 50 + 200 625 1912

T ₄ Dinotefuron 8% + Diafenthiuron 40% WG 50 + 250 625 1961

T ₅ Dinotefuron 8% + Diafenthiuron 48% WG 50 + 300 625 2059

T ₆ Dinotefuron 20% SG 50 250 1628

T ₇ Diafenthiuron 50% WP 300 600 1504

Tank Mix 50+300 250 + 600

T ₈ (Dinotefuron 20% SG + Diafenthiuron 50% 1690 WP)

T ₉ Control - - 1458 CD (P = 0.05) 54.67

CD - Critical difference (P- probability at 5% level of significance).

It is seen from Table- 10 that the treatment by the insecticidal composition of the present disclosure significantly increases the yield as compared to the yield of the untreated Control (1458 Kg/ha). The highest yield was observed in treatment T5 (2059 Kg/ha), which was significant over the rest of the treatments, solo treatment and tank mix combinations. The insecticidal compositions Tl to T5 exhibited higher yield as compared to solo insecticide treatments (T6 and T7) and tank mix combination treatment (T8). Phytotoxicity study of the insecticidal composition of the present disclosure

The treated plants were observed for damages, if any, caused by the application of different treatments by considering the phytotoxic symptoms, namely, leaf injury on tips and leaf surface, wilting, vein clearing, necrosis, epinasty and hyponasty on ten plants per plot. The observations were recorded before spray and 1, 3, 5, 7 and 10 ^th day after applications. The Phytotoxicity study scale on leaf injury on tips and leaf surface the Scale (0-10) used is given below.

Phytotoxicity Rating Scale (PRS)

Crop response/ Crop injury Rating

0-00 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-11: Phyto-toxicity effect of different Insecticide treatments on Cotton

*For phototoxic symptoms- Leaf injury on tips and Leaf surface, Wilting, Vein Clearing, Necrosis, Epinasty and Hyponasty

5 It is seen from Table- 11 that the insecticidal composition of the present disclosure does not have any detrimental effect on the treated cotton plants. Hence, the insecticidal composition of the present disclosure is safe for plants.

It is clearly seen from the above studies that the insecticidal composition of the present disclosure is effective in controlling sucking pests of cotton. The 10 composition comprising Dinotefuran 8% + Diafenthiuron 48% WG provided the most effective control of the sucking pests. The insecticidal composition of the present disclosure provided enhanced efficacy as compared to the commercially available Dinotefuron 20% SG & Diafenthiuron 50% WP and their tank mix combination for controlling sucking pest complex of cotton. Due to the effective control of the pests, treatment with the insecticidal composition of the present disclosure results in higher yield of cotton. There is no phytotoxic effect of the insecticide composition on the cotton crop. The insecticide composition of the present disclosure exhibits synergistic effect in controlling the sucking pests of cotton crop, and can be used effectively and safely used for the management of sucking pests than individual Dinotefuron, Diafenthiuron and tank mix combinations of both.

TECHNICAL ADVANCEMENTS

The present disclosure described herein above has several technical advantages including, but not limited to, the realization of:

- a synergistic insecticidal composition which is stable and is in a ready-to use form;

- a composition having improved sticking property, high attrition resistance, high dispersion when mixed in water and enhanced bio efficacy; and

- an easy and simple process for the preparation of the synergistic insecticidal composition.

Throughout this specification the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.

The use of the expression "at least" or "at least one" suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.

The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.

While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.