DESC:FORM 2

THE PATENTS ACT, 1970
(SECTION 39 OF 1970)
&
The Patents Rules, 2003

COMPLETE SPECIFICATION
(Section 10 and Rule 13)

SYNERGETIC WDG FORMULATIONS, PROCESS FOR PREPARING AND USE THEREOF

We, COROMANDEL INTERNATIONAL LIMITED,
an Indian company incorporated under Companies Act of 1956, having its principal place of business at Coromandel House, Sardar Patel Road, Secunderabad – 500 003, Telangana, India.

The following specification particularly describes the invention and the manner in which it is to be performed:

FIELD OF THE INVENTION
The present invention relates to insecticidal water dispersible granule (WDG) composition comprising combination of phenylpyrazole derivative and organophosphate.

The present invention also relates to water dispersible granule composition comprising combination of phenylpyrazole derivative, organophosphate, wetting agent and dispersing agent.

The present invention specifically relates to water dispersible granule composition comprising combination Fipronil and Acephate, wetting agent, dispersing agent and other agrochemical auxiliaries.

The present invention specifically relates to water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 1 : 60 to 10 : 40 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

The present invention preferably relates to water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 5 : 50 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

The present invention also relates to a process for the preparation of water dispersible granule composition comprising combination of Fipronil and Acephate wherein the granules are prepared by extrusion process.

BACKGROUND OF THE INVENTION
Fipronil is a broad-spectrum insecticide which belongs to the phenylpyrazole chemical family. Fipronil disrupts the insect central nervous system by blocking GABA-gated chloride channels and glutamate-gated chloride (GluCl) channels. Fipronil is an insecticide used to control a broad range of insect pests mainly in horticultural crops and it is a chiral molecule. Fipronil is an isomeric mixture of two enantiomers (±; S/R). Fipronil was first registered for use by the United States Environmental Protection Agency (U.S.EPA) in May 1996.

Fipronil is chemically known as 5-Amino-1-[2,6-dichloro-4-(trifluoromethyl) phenyl]-4-[(trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile and has the following structure:

Acephate is an organophosphate insecticide currently registered for use on a variety of field, fruit, and vegetable crops (e.g., cotton, tobacco, cranberries, mint); in food handling establishments; on ornamental plants both in greenhouses and outdoors (e.g., nonbearing fruit trees, Christmas trees, and cut flowers); and in and around the home. Acephate was first registered in 1973 for ornamental uses, and in 1974 for food uses (agricultural crops).

Acephate is chemically known as Acetylphosphoramidothioic acid O, S-dimethyl ester and is depicted by the structure given below :

Acephate products were sold as powders, liquids, granules, tablets, and in water-soluble packets. Acephate, a water-soluble insecticide readily absorbed by plant roots and foliage to give systemic control of feeding insects. Insect pests are generally controlled more effectively by Acephate through ingestion than by contact.

Fipronil is used to control ants, beetles, cockroaches, fleas, ticks, termites, mole crickets, thrips, rootworms, weevils, and other insects. Uses for individual fipronil products vary widely. Always read and follow the label when applying pesticide products.

Fipronil is used in granular turf products, seed treatments, topical pet care products, gel baits, liquid termiticides, and in agriculture.

Acephate is an organophosphate insecticide currently registered for use on a variety of field, fruit, and vegetable crops (e.g., cotton, tobacco, cranberries, mint); in food handling establishments; on ornamental plants both in greenhouses and outdoors (e.g., non-bearing fruit trees, Christmas trees, and cut flowers); and in and around the home.

Though, conventionally each of these Active ingredients are used individually, combination product is not approved which has applications compared to the mono product. Hence, there is increased interest in the use of Active ingredients in combination to give synergistic results.

The given below prior-art references show the use of combinations of fipronil and Acephate in different ratios.

CN 1102023 C discloses combination of fipronil compound pesticide containing Fipronil: 0.5-10%, Acephate: 40-85%.

CN 103766394 A discloses acephate compound pesticide which is characterized by comprising the components by the weight percentage: 40% of acephate, 0.5% of fipronil, and the balance being a solvent and an auxiliary agent; the solvent is selected from xylene, water or dichloromethane; the auxiliary agent includes an emulsifier selected from one or more of polyoxyethylene nonyl phenyl ether, alkyl benzene calcium sulfate and phenethyl phenyl polyoxyethylene-polyoxypropylene ether.

US 10,492,489 B2 generically enables combination of different active ingredients. However, the specific compositions of Fipronil and Acephate combination are not disclosed.

Water dispersible granules are a solid, non-dusty granular formulation which disperses or dissolves quickly when added to water in the spray tank to give a fine particle suspension. They provide a system for delivering solid active ingredients to a target organism. They allow for the production of highly-concentrated formulations which are wettable and easily disintegrated on contact with water. Water dispersible granules are an attractive alternative to wettable powder (WP) formulations due to their reduction in dust production.

Accordingly, there is a need in the art to provide Water dispersible granule compositions of combinations which environmentally safer and stable insecticidal / acaricidal compositions having two active ingredients with different physical and chemical properties, which are environmentally safe, easy and effective combination formulation of two active with enhanced efficacy and stable product during storage.

It was surprisingly and unexpectedly found by the present inventors that a selective combination composition of two active ingredients comprising Fipronil, Acephate, wetting agent, dispersing agent and other agrochemical auxiliaries, possesses enhanced efficacy, improved penetration and long duration control of phytopathogens as compared to its other traditional formulations with long storage stability across a wide temperature range and having no adverse impact on photosynthetic activity in plant and fruit quality.

OBJECTIVE OF INVENTION
The main objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of phenylpyrazole derivative and organophosphate.

Another objective of the present invention is to provide a water dispersible granule composition comprising combination of phenylpyrazole derivative, organophosphate, wetting agent and dispersing agent.

Another objective of the present invention is to provide a water dispersible granule composition comprising combination Fipronil and Acephate, wetting agent, dispersing agent and other agrochemical auxiliaries.

Another objective of the present invention is to provide a water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 1 : 60 to 10: 40 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

Another objective of the present invention is to provide a water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 5 : 50 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

Another objective of the present invention is to provide a process for the preparation of water dispersible granule composition comprising combination of Fipronil and Acephate wherein the granules are prepared by extrusion process.

SUMMARY OF INVENTION
Accordingly, the present invention provides insecticidal water dispersible granule composition comprising combination of phenylpyrazole derivative and organophosphate.

In one embodiment, the present invention provides a water dispersible granule composition comprising combination of phenylpyrazole derivative, organophosphate, wetting agent and dispersing agent.

In another embodiment, the present invention provides a water dispersible granule composition comprising combination Fipronil and Acephate, wetting agent, dispersing agent and other agrochemical auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 1 : 60 to 10 : 40 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 5 : 50 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising;
1 to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent, and
0.1 to 70% (w/w) of other agrochemical additives / auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising;
1% to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of naphthalene sulphonates blend,
1% to 15% (w/w) of naphthalene sulphonates condensate, and
0.1% to 70% (w/w) of other additives / auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising;
1% to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of sodium isopropyl naphthalene sulfonate,
1% to 15% (w/w) of sodium salt of naphthalene sulfonate condensate, and
0.1% to 70% (w/w) of other additives / auxiliaries.

In another embodiment, the present invention provides a water dispersible granule composition comprising;
1% to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of wetting agent or,
1% to 15% (w/w) of dispersing agent,
0.5% to 30% (w/w) of disintegrating agent,
0.1 to 10% (w/w) of defoamer, and
5% to 50% (w/w) of inert fillers.

In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising;
1 to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of sodium isopropyl naphthalene sulfonate,
1% to 15% (w/w) of sodium salt of naphthalene sulfonate,
0.5% to 30% (w/w) of ammonium sulphate,
0.1 to 10% (w/w) of absorbed polydimethyl siloxane, and
5% to 50% (w/w) of hydrous aluminosilicate.

In another embodiment, the present invention provides a process for preparing water dispersible granule composition comprising the steps of:
a. blending active ingredients, wetting agent, dispersing agent along with other auxiliaries to obtain a homogenous mixture,
b. milling the blended mixture to obtain particles of size in the range of 10-15 µ,
c. mixing the milled material with water to make a dough, and
d. extruding the dough obtain in step (c) and drying the granules.

In another embodiment, the present invention provides a process for preparing water dispersible granule composition comprising the steps of:
a. blending Fipronil, hydrous aluminosilicate, sodium isopropyl naphthalene sulfonate, sodium salt of naphthalene sulfonate condensate, absorbed polydimethyl siloxane to obtain a homogenous mixture,
b. milling mixture obtained in step (a) and blending for 20 minutes,
c. blending Acephate and precipitated silicon dioxide for 20 minutes,
d. mixing the milled materials with water to make a dough, and
e. extruding the dough obtain in step (d) and drying the granules.

DETAILED DESCRIPTION OF THE INVENTION
The term "comprising", which is synonymous with "including", "containing", or "characterized by" here is defined as being inclusive or open-ended, and does not exclude additional, unrecited elements or method steps, unless the context clearly requires otherwise.

The present invention provides water dispersible granule composition comprising combination of Fipronil and Acephate in the weight ratio of 1 : 60 to 10 : 40 of first active ingredient to the second active ingredient, preferably in the weight ratio of 5 : 50. However, variables of the ratios of each of the active ingredients can be used and the selection of the particular amount is dependent upon many factors including, for example, type of formulations, the crop, disease sought to be controlled and environmental conditions. The selection of the proper quantity of active agent to be applied, however, is within the expertise of one skilled in the art.

The combination compositions of the present invention can be used on a number of fruits, wines, hops and ornamental varieties such as lemons and oranges. T product is also used as a foliar application in labeled crops.

The composition of the present invention could be applied to plants, seeds, fruits, soil as preventive and curative state.

The wetting agent is a compound that facilitates rapid wetting of the powder when added to the water. The wetting agent employed in the formulation composition is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.

The wetting agents as used in the present invention are selected from and not limited to polycondensation product of naphthalene sulfonic acid, which is alkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, sodium isopropyl naphthalene sulfonate (Morwet IP), dialkyl naphthalene sulphonate sodium salt (Supragil WP), sodium alkyl naphthalene sulfonate blend (Morwet 3028), salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, salts of polyarylether sulphates such as tristyrylphenolethoxylate sulphate salts, alkoxylated alkylphenols and alcohols as well as block copolymers of ethyleneoxide and propylene oxide. Preferred wetting agents used in the composition of the present invention are sodium isopropyl naphthalene sulfonate (Morwet IP), dialkyl naphthalene sulphonate sodium salt (Supragil WP), sodium alkyl naphthalene sulfonate blend (Morwet 3028).

The wetting agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 1 to 10% of the total weight of the composition.

The wetting agent may also be used as a dispersing agent.

The compositions of the present invention contain dispersing agents selected from and not limited to sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers, polycarboxylates, sodium salt of naphthalene sulfonate condensate (Morwet D-425), condensed methyl naphthalene sulfonate sodium salt (Supragil MNS-90). Preferred dispersing agents used in the composition of the present invention are sodium salt of naphthalene sulfonate condensate (Morwet D-425), condensed methyl naphthalene sulfonate sodium salt (Supragil MNS-90).

The dispersing agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 2% to 10% of the total weight of the composition.

The disintegrating agents as used in the present invention are selected from and not limited to microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenyl sulphonates, sodium starch glycolate, sodium lignin sulfonate, sodium lauryl sulfate, combinations of carbonates with solid acids, agar, starch, hydroxypropylstarch, sodium alginate, carboxymethyl starch ether, gum arabic, gum tragacanth, gelatin, casein, crystalline cellulose, carboxymethylcellulose calcium, Tween, Pluronic, sodium laurate, carboxylic resins, potassium chloride, sodium chloride, urea, anionic surfactants, calcium chloride, magnesium chloride, aluminum chloride, glucose, lactose, sodium glutamate, sodium inosinate, dextrin, blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof). Preferred disintegrating agent is ammonium sulphate.

The disintegrating agents present in the composition of the present invention are in the range of 0.5% to 30%, more preferably 2% to 25% of the total weight of the composition.

The defoamer as used herein is selected from and not limited to absorbed polydimethyl siloxane, stearates; silicones (SILFOAM®, SILFAR®, PULPSIL® and WACKER® AK) and ethoxylates. The defoamer is preferably polydimethyl siloxane (Rhodosil EP-6703).

The defoamers present in the composition of the present invention are in the range of 0.1% to 10%, more preferably 0.1% to 5% of the total weight of the composition.

The inert fillers used in the present invention are selected from and not limited to natural minerals such as calcite, talc, china clay series like hydrous aluminosilicate, and montmorillonite or attapulgite clays including various forms of Bentonite, Kaolin; lactose anhydrous, lactose monohydrate, starches, sodium sulphate, sodium bicarbonate, calcium carbonate, calcium sulphate, calcium phosphate, sodium tripolyphosphate (STPP), woodflours, activated carbon, sugars, diatomaceous earth, cereal flours, fine-grain inorganic solids, and the like. Clays and inorganic solids which may be used include calcium bentonite, perlite, mica, vermiculite, silicas, quartz powder, montmorillonite and mixtures thereof. Sugars which may be useful include dextrin and maltodextrin. Preferred inert fillers are corn starch, hydrous aluminosilicate (China clay) and mixtures thereof.

The inert fillers present in the composition of the present invention are in the range of 5 to 50%, more preferably 10 to 45% of the total weight of the composition.

The WDG composition according to the invention can comprise from 0.5 to 35 wt% of adjuvants commonly used in this field and well known to those expert in the art, such as antidrift agents, adhesives, penetrants, pH modifiers, stickers and spreaders.

The WDG compositions of the present invention can be diluted with water or water solutions of agronomic compounds before use to produce a sprayable composition which is used in treating plants or increasing plant growth, Dilution in water usually results in suspensions, emulsions, suspoemulsions or solutions of the agrochemical active ingredient at a concentration of at least 0.001 g/l.

A particular mode of administering the composition of the present invention is the administration to the aboveground parts of plants, in particular to the leaves thereof (leaf-application). The number of applications and the administered doses are chosen in accordance with the biological and climatic conditions of life of the causative agent. The antifungal compositions though, can also be applied to the soil and get into the plants through the root system (systemic activity), in case the locus of the plants is sprayed with a liquid composition or if the components are added to the soil in a solid formulation e.g. in the form of granulate (soil application).

When using the active compound combinations according to the invention, the application rate can be varied within a relatively wide range, depending on the kind of application. For the treatment of parts of plants, the active-compound combination application rates are generally between 0.1 and 10 000 g/ha, preferably between 100 and 2500 g/ha. For seed dressing, the active compound combination application rates are generally between 0.001 and 50 g per kilogram of seed, preferably between 0.01 and 20 g per kilogram of seed. For the treatment of the soil, the active-compound combination application rates are generally between 0.1 and 10 000 g ha preferably between 1 and 5000 g/ha.

Although the invention has been described above with reference to the disclosed embodiments, those skilled in the art will readily appreciate that the specific embodiments detailed are only illustrative of the invention. It should be understood that various modifications can be made without departing from the spirit of the invention. Accordingly, the invention is limited only by the claims.

EXAMPLES
Example 1: Composition of Acephate + Fipronil WDG
S.No Ingredients/Raw Materials Chemical Name Quantity (% w/w)
1. Acephate Technical@ 97% (b) 50% O,S- dimethyl acetylphosphoramidothioate 51.54
2. Ppt Silica silicon dioxide, precipitated 0.5
3. Fipronil Technical@ 90 (b)5.0% 5-amino-[2,6 –dichloro-4- (trifluoromethyl) phenyl]-4- [(1R,S)- (trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile 5.55
4. Morwet IP sodium isopropyl naphthalene sulfonate 1.0
5. Morwet D-425 sodium salt of naphthalene sulfonate condensate 6.0
6. Rhodosil EP-6703 absorbed polydimethyl siloxane 0.5
7. Ammonium Sulphate ammonium sulphate 20
8. China clay Hydrous aluminosilicate 14.91
Total 100

Manufacturing process:

Step 1: Required quantities of hydrous aluminosilicate, sodium isopropyl naphthalene sulfonate, sodium salt of naphthalene sulfonate condensate, absorbed polydimethyl siloxane, Fipronil were weighed,
Step 2: obtained sample was pre-mixed for 20 minutes in a ribbon blender,
Step 3: sample was milled through air jet milling instrument with inlet pressure 4 kg/cm2 and grinding pressure 6-7 kg/ cm2,
Step 4: the air jetted material was collected and post blended for 20 min,
Step 5: Acephate and precipitated silicon dioxide were weighed and blended in a sigma mixer for 20 min,
Step 6: the air jetted material was added to a sigma blender after 20 min and the process was continued for further 20 min.
Step 7: dough was prepared by adding 2.4% distilled water into the mixture,
Step 8: granules were extruded through Basket extruder,
Step 9: water dispersible granules were collected, dried in FBD @ 45°C, the moisture content was checked and it should be < 1.5%.
Step 10: obtained water dispersible granules of Acephate and Fipronil were packed appropriately.

Compositions of examples 2-5 were also prepared using the similar method used for the preparation of example 1 composition.

Example 2: Composition of Acephate + Fipronil WDG
S.No Ingredients/Raw Materials Chemical Name Quantity (% w/w)
1. Acephate Technical@ 97% (b) 50% O,S- Dimethyl acetylphosphoramidothioate 51.54
2. Ppt Silica Silicon Dioxide, Precipitated 0.5
3. Fipronil Technical@ 90 (b)5.0% 5-amino-[2,6 –dichloro-4- (trifluoromethyl) phenyl]-4- [(1R,S)- (trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile 5.55
4. Morwet IP sodium isopropyl naphthalene sulfonate 1.0
5. Morwet D-425 sodium salt of naphthalene sulfonate condensate 6.0
6. Rhodosil EP-6703 absorbed polydimethyl siloxane 0.5
7. Ammonium Sulphate ammonium Sulphate 14.91
8. China clay hydrous aluminosilicate 20
Total 100

Example 3: Composition of Acephate + Fipronil WDG
S.No Ingredients/Raw Materials Chemical Name Quantity (% w/w)
1. Acephate Technical@ 97% (b) 50% O,S- Dimethyl acetylphosphoramidothioate 51.54
2. Fipronil Technical@ 90 (b)5.0% 5-amino-[2,6 –dichloro-4- (trifluoromethyl) phenyl]-4- [(1R,S)- (trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile 5.55
3. Supragil WP dialkyl naphthalene sulphonate
sodium salt 1.0
4. Supragil MNS-90 condensed methyl naphthalene sulfonate sodium salt 6.0
5. Corn starch corn starch 33.3
6. Ammonium sulphate ammonium sulphate 2.61
Total 100

Example 4: Composition of Acephate + Fipronil WDG:
S.No Ingredients/Raw Materials Chemical Name Quantity (% w/w)
1. Acephate Technical@ 97% (b) 50% O,S- Dimethyl acetylphosphoramidothioate 51.54
2. Fipronil Technical@ 90 (b)5.0% 5-amino-[2,6 –dichloro-4- (trifluoromethyl) phenyl]-4- [(1R,S)- (trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile 5.55
3. Supragil WP dialkyl naphthalene sulphonate
sodium salt 1.0
4. Supragil MNS-90 condensed methyl naphthalene sulfonate sodium salt 6.0
5. Rhodorsil EP-6703 absorbed polydimethyl siloxane 0.5
6. Corn Starch corn starch 30.5
7. Ammonium Sulphate Ammonium Sulphate 4.91
Total 100

Example 5: Composition of Acephate + Fipronil WDG:
S.No Ingredients/Raw Materials Chemical Name Quantity (% w/w)
1. Acephate Technical@ 97% (b) 50% O,S- Dimethyl acetylphosphoramidothioate 51.54
2. Fipronil Technical@ 90 (b)5.0% 5-amino-[2,6 –dichloro-4- (trifluoromethyl) phenyl]-4- [(1R,S)- (trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile 5.55
3. Morwet 3028 sodium alkyl naphthalene sulfonate blend 3.0
4. Morwet D-425 sodium salt of naphthalene sulfonate condensate 5.0
5. Ammonium sulphate Ammonium sulphate 7.0
6. Rhodosil EP 6703 Absorbed Polydimethyl siloxane 0.5
7. China clay Hydrous aluminosilicate 27.41
Total 100

Field Trials Data:
The water dispersible granule combination composition of Acephate and Fipronil of the present invention were prepared and field efficacy trials were done in the fields of Cotton and Rice. The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control with the WDG composition of the present invention is greater than the solo compositions and synergistic effect is observed (Ratio of O/E > 1, means synergism observed).

The field efficacy and Sucking Pests control against various insects i.e., Jassids, Thrips, Aphids, The brown planthopper and Stem Borer were observed and compared with solo composition. The combination of Acephate 500 + Fipronil 5 WDG composition has shown excellent efficacy as well as residual control over the both Acephate 75% SP and Fipronil 5% SC solo compositions.

Trial 1: Cotton

Cotton (Gossypium hirsutum L.) is the most important cash crop in India with an expanse of 9-11 million hector area under cultivation. It grows well in almost all areas of the country but mainly grown in nine states major cotton growing states which includes Punjab, Haryana, Rajasthan in North India, Maharashtra, Gujarat & Madhya Pradesh in Central India, and Tamilnadu, Karnataka, Andhra Pradesh in South India.

The field efficacy trials were conducted in cotton on cotton sucking pest complex. The sucking pests viz., Leafhopper, Amrasca biguttula biguttula (Ishida), Aphid, Aphis gossypii (Glover), and Thrip, Thrips tabaci (Linnman) cause severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield.

Field trials were conducted and the efficacy of WDG composition of the present invention was evaluated against sucking pests in Cotton. The cotton crop was raised with all standard agronomic practices. The experiments were laid out in a randomized block design with net plot size of 5m x 8m. Cotton crop was raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liter of water spray volume per hectare at 60 days after sowing. The observations were recorded by counting the no of sucking insects (Jassids, Thrips & Aphids) per leaf, six leaves per plant and five plants per plot. The observations were recorded at before spraying, 10 DAA (Days after application). The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control for the combination is greater than the expected percentage, there is a synergistic effect. (Ratio of O/E > 1, means synergism observed).

Table 1: Sucking Pests control in Cotton against Mites, Thrips, Whitefly adults and Whitefly nymphs
Compositions Dose Gram Active/hectare % Insect Control at 10 DAA
Jassids Thrips Aphids
Acephate +Fipronil 55 % WDG (Example No. 1) 500+50 86.8 94.6 88.5
Acephate 75% SP 500 30.5 33.8 42.5
Fipronil 5% SC 50 36.5 42.5 38.0
WDG Water Dispersible Granule, SP- Soluble powder, SC Suspense Concentrate
The trial results illustrated in Tables 1 shows excellent efficacy of Acephate + Fipronil combination insecticide against sucking pests Jassids, Thrips & Aphids. Solo application as well as the combination of two active ingredients against Jassids, Thrips, and Aphids have been tested. Solo alone was not able to provide satisfactory control of sucking pests. The synergistic effect of Acephate + Fipronil combination against Jassids, Thrips & Aphids has shown excellent efficacy as well as residual control.

Trial 2: Rice Pests:
The brown planthopper (Nilaparvata lugens) is a planthopper species that feeds on rice plants. These insects are among the most important pests of rice, which is the major staple crop for about half the world's population. BPH can also transmit Rice Ragged Stunt and rice Grassy Stunt diseases. Neither disease can be cured.

Stem Borer: Its damage can reduce the number of reproductive tillers. At late infection, plants develop whiteheads. Yellow stemborer (Scirpophaga incertulas) damage can lead to about 20% yield loss in early planted rice crops, and 80% in late-planted crops. White stemborer is an important pest in rainfed wetland rice.

Field trials were conducted to evaluate the efficacy of WDG composition of the present invention against the brown planthopper and stem borer in Rice. The experiments were laid out in a randomized block design with net plot size of 5m x 6m. Rice crop was raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liter of water spray volume per hectare at 45 days after sowing. The observations were recorded by counting the no. of BPH insects per hill and dead hearts count per Sqm. The observations were recorded before spraying, 10 DAA (Days after application). The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control for the combination is greater than the expected percentage, there is a synergistic effect.

Table 2: Pest control in Rice
Compositions Dose Gram Active/hectare % Insect Control at 10 DAA
BPH Stem borer
Acephate 500 + Fipronil 5 WDG (Example No. 1) 500+50 88.75 89.50
Acephate 75% SP 500 45.70 32.88
Fipronil 5% SC 50 37.5 47.5

SP- Soluble powder, WP Wettable Powder, SC Suspense Concentrate, SL Soluble Liquid, WG Wettable granule DAA Days after Application

The trial results illustrated in Table 2, results show excellent efficacy of Acephate + Fipronil combination insecticide against Brown Plant Hopper & Stem borer. Trials were conducted with solo as well as the combination of two active ingredients tested here against Brown plant hopper & Stem borer. Solo alone was not able to provide satisfactory control for both the pests. The synergistic effect of combination of Acephate + Fipronil has shown excellent efficacy against Brown plant hopper as well as stem borer, it also shown good residual control.

,CLAIMS:WE CLAIM:
1. A water dispersible granule composition comprising combination of Fipronil and Acephate, wetting agent, dispersing agent and other agrochemical auxiliaries.

2. The water dispersible granule composition as claimed in claim 1, wherein said composition comprising combination of Fipronil and Acephate in the weight ratio of 1 : 60 to 10 : 40 of first active ingredient to the second active ingredient.

3. The water dispersible granule composition as claimed in claim 2, wherein said composition comprising combination of Fipronil and Acephate in the weight ratio of 5 : 50 of first active ingredient to the second active ingredient.

4. The water dispersible granule composition as claimed in claim 1, wherein said composition comprising;
1 to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent, and
0.1 to 70% (w/w) of other agrochemical additives / auxiliaries.

5. The water dispersible granule composition as claimed in claim 1, wherein said composition comprising;
1% to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of wetting agent or,
1% to 15% (w/w) of dispersing agent,
0.5% to 30% (w/w) of disintegrating agent,
0.1 to 10% (w/w) of defoamer, and
5% to 50% (w/w) of inert fillers.

6. The water dispersible granule composition as claimed in claim 5, wherein said composition comprising;
1 to 10 % (w/w) of Fipronil as first active ingredient,
10% to 60% (w/w) of Acephate as second active ingredient,
1% to 15% (w/w) of sodium isopropyl naphthalene sulfonate,
1% to 15% (w/w) of sodium salt of naphthalene sulfonate,
0.5% to 30% (w/w) of ammonium sulphate,
0.1 to 10% (w/w) of absorbed polydimethyl siloxane, and
5% to 50% (w/w) of hydrous aluminosilicate.

7. The water dispersible granule composition as claimed in claim 5, wherein said wetting agent is selected from polycondensation product of naphthalene sulfonic acid, which is alkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, sodium isopropyl naphthalene sulfonate, dialkyl naphthalene sulphonate sodium salt, sodium alkyl naphthalene sulfonate blend, salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, salts of polyarylether sulphates such as tristyrylphenolethoxylate sulphate salts, alkoxylated alkylphenols and alcohols as well as block copolymers of ethyleneoxide and propylene oxide or mixtures thereof.

8. The water dispersible granule composition as claimed in claim 5, wherein said dispersing agent selected from sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers, polycarboxylates, sodium salt of naphthalene sulfonate condensate, condensed methylnaphthalene sulfonate sodium salt or mixtures thereof.

9. The water dispersible granule composition as claimed in claim 5, wherein said disintegrating agent selected from and not limited to microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenyl sulphonates, sodium starch glycolate or mixtures thereof.

10. The water dispersible granule composition as claimed in claim 5, wherein said defoamer is selected from absorbed polydimethyl siloxane, stearates; silicones and ethoxylates or combination thereof.

11. The water dispersible granule composition as claimed in claim 5, wherein said fillers selected from natural minerals such as calcite, talc, china clay series, hydrous aluminosilicate, montmorillonite or attapulgite clays including various forms of bentonite, kaolin; lactose, starches, calcium carbonate, calcium sulphate, calcium phosphate, sodium tripoly phosphate or combinations thereof.

12. A process for preparing water dispersible granule composition comprising the steps of:
a. blending active ingredients, wetting agent, dispersing agent along with other auxiliaries to obtain a homogenous mixture,
b. milling the blended mixture to obtain particles of size in the range of 10-15 µ,
c. mixing the milled material with water to make a dough, and
d. extruding the dough obtain in step (c) and drying the granules.

13. The process for the preparation of insecticidal water dispersible granule composition as claimed in claim 11, wherein said process comprising the steps of:
a. blending Fipronil, hydrous aluminosilicate, sodium isopropyl naphthalene sulfonate, sodium salt of naphthalene sulfonate condensate, absorbed polydimethyl siloxane to obtain a homogenous mixture,
b. milling mixture obtained in step (a) and blending for 20 minutes,
c. blending Acephate and precipitated silicon dioxide for 20 minutes,
d. mixing the milled materials with water to make a dough, and
e. extruding the dough obtain in step (d) and drying the granules.

Dated this Twenty Sixth (26th) day of June, 2021

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Dr. S. Padmaja
Agent for the Applicant
IN/PA/883