DESC:FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10; rule 13)

1. TITLE OF THE INVENTION – SYNERGISTIC PESTICIDAL FORMULATION OF FLUBENDIAMIDE AND FLONICAMID

2. Applicant(s)
a) NAME: MEGHMANI ORGANICS LIMITED
b) NATIONALITY: INDIAN
c) ADDRESS: MEGHMANI HOUSE, BEHIND SAFAL PROFITAIRE, CORPORATE ROAD, PRAHLADNAGAR, AHMEDABAD, GUJARAT, INDIA-380015

3. PREAMBLE TO THE DESCRIPTION
COMPLETE SPECIFICATION
The following specification describes the invention and the manner in which it is to be performed

SYNERGISTIC PESTICIDAL FORMULATION OF FLUBENDIAMIDE AND FLONICAMID

FIELD OF THE INVENTION:
The present invention relates to a synergistic pesticidal formulation comprising Flubendiamide and Flonicamid. The present invention particularly relates to a synergistic pesticidal formulation comprising Flubendiamide and Flonicamid and at least one inactive ingredient, wherein the said composition is suspension concentrate (SC), Wettable Powder (WP) and Wettable Dispersible Granule (WG) formulation and the process of preparation thereof.

BACKGROUND OF THE INVENTION:

Pesticides are the chemicals which are applied on plants to kill or eliminate fungus, bacteria, insects, snails, slugs, or weeds. Pesticides are broadly used in agriculture and have facilitated a massive increase in yield of crops and productivity.

Flonicamid (IKI220; N-cyanomethyl-4-trifluoromethylnicotinamide), a pyridine carboxamide compound, is a novel systemic insecticide with selective activity against hemipterous pests, such as aphids and whiteflies, and thysanopterous pests like thrips. It disrupts insect chordotonal organs that can affect hearing, balance, movement to cause cessation of feeding, but the specific target site of the chemical is unknown. Flonicamid is very active against aphids, regardless of differences in species, stages and morphs. Flonicamid has no negative impact on pollinating insects or natural enemies, and thus, Flonicamid provide a new option for integrated pest management programs. Flonicamid also has a good toxicological, environmental and ecotoxicological properties.

Flonicamid is having molecular formula C9H6F3N3O and molecular weight is 229.16 g/mol and having water solubility of 5.2 g/L at 20oC. Flonicamid is stable at pH 4 and pH 5. The amide TFNG-AM is formed from this reaction (under alkaline conditions) and can then be hydrolyzed to TFNG (N-(4- trifluoromethylnicotinoyl) glycine).

Flonicamid was first disclosed in EP0580374B1 and chemically represented as below structure:

Flonicamid is the only insecticide from IRAC (Insecticide Resistance Action Committee) Group 29 class. Flonicamid rapidly inhibits the feeding behavior of aphids, and has better action through ingestion than by contact which is unique compared to existing insecticides.

Flonicamid is useful to provide protection in crops like Soybean, Fruit trees, Cereals, Potatoes, Cotton, Vegetables, Ornamentals, etc.

Flonicamid is commercially marketed as a soluble or wettable granule containing 50% Flonicamid, which is to be mixed with water before spraying.

Flubendiamide is the first example of benzene di-carboxamide or phthalic acid diamide insecticides, discovered by Nihon Nohyaku and developed jointly with Bayer Crop Science. It is also the first example of a practical insecticide which activates ryanodine receptors.

The IUPAC name of Flubendiamide is 1- N-[4-(1, 1, 1, 2, 3, 3, 3-heptafluoropropan-2-yl) -2- methyl phenyl] -3-iodo-2- N- (2-methyl-1-methylsulfonylpropan-2-yl) benzene-1, 2-dicarboxamide and the molecular formula is C23H22F7IN2O4S. The relative Molecular mass of Flubendiamide is 682.39 g/ mol.
Flubendiamide belongs to the phthalic acid diamide chemical class, a ryanodine receptor agonist, which activates ryanodine-sensitive intracellular calcium release channels in insect neurons. Flubendiamide shares its mode of action with chlorantraniliprole, another diamide insecticide. The release of calcium causes muscle contraction, resulting in the death of the insect. This mode of action has been shown to be highly specific to insect ryanodine receptors and not to affect mammalian ryanodine receptors.

Flubendiamide was first disclosed as an active ingredient in US20100310518 A1 where in Flubendiamide was combined to other Beneficial Species from the orders or suborders of the Araneae, Acari, Dermaptera, Hymenoptera, Coleoptera, Neuroptera, Thysanoptera, Heteroptera, Diptera, Hemiptera, Dermaptera and/or Parasitiformes or at least one bacteria strain or at least one virus strain for the effective control of unwanted pests. This limits the treatment of the above invention to only insects. The above invention does not prevent the infection by pathogenic fungi.

Flubendiamide is chemically represented as below structure:

Flubendiamide is having water solubility of 29.9 µg/ L at 20 °C. Flubendiamide is the insecticide from IRAC (Insecticide Resistance Action Committee) Group 28 class.

In India or anywhere in the world, in agricultural production, using synthetic or chemical agent is the most effective means in order to control plant pest. However, the main disadvantage of the such insecticide or pesticide is that on long run, the insects or pets develop the resistance to that insecticide or pesticide and as a result to produce effective result, higher concentration of the insecticide or pesticide is to be used. Here again using higher dose of insecticide or pesticide may result in some detrimental effect to soil as well as environment. Therefore in general practice, usually combination of pesticide with another pesticide or another herbicide or fungicide is used in different concentration as per requirement.

However, when combination of one or more pesticide are used, the main challenge comes is to develop a formulation or composition which is stable, easy to use and effective.

There are few formulations of Flonicamid and Flubendiamide either reported individually as well in combination with other pesticides.

IN 202017024614 describes pesticidal composition comprising Flonicamid and D-limonene as active ingredients, in a mixing weight ratio of Flonicamid to D-limonene of from 1:150 to 1:1. This prior art does not comprise Flubendiamide in the combination of Flonicamid.

IN 320049 discloses a water-based pesticidal suspension comprising (a) Flonicamid, (b) buprofezin, (c) a polycarboxylate, (d) at least one sulfonate type surfactant selected from the group consisting of an alkyl sulfosuccinate, a lignosulfonate, a C8-18 alkylbenzene sulfonate and a C8-18 alkyl diphenyl ether disulfonate, (e) a sodium alkyl naphthalene sulfonate condensed with formaldehyde, and water, wherein, in the suspension, the content of the active ingredients consisting of the component (a) Flonicamid and the component (b) buprofezin is from 5 to 60 wt%, the content of the component (c) polycarboxylate is from 0.1 to 10 wt%, the content of the component (d) the sulfonate type surfactant is from 0.1 to 20 wt% and the content of the sodium alkyl naphthalene sulfonate condensed with formaldehyde as the component (e) is from 0.1 to 10 wt%, and wherein the weight ratio of the active ingredients to the polycarboxylate is from 1:0.005 to 1:2, the weight ratio of the active ingredients to the sulfonate type surfactant as the component (d) is from 1:0.005 to 1:4, the weight ratio of the active ingredients to the sodium alkyl naphthalene sulfonate condensed with formaldehyde is from 1:0.005 to 1:2.

IN 357838 relates to a synergistic pesticidal composition comprising component (A) Flubendiamide component (B) at least one Strobilurin fungicides from Trifloxystrobin, Azoxystrobin and component (C) at least one more triazole fungicide selected from Difenoconazole, Epoxiconazole, Flutriafol, Hexaconazole, Propiconazole, Prothioconazole, Tebuconazole, Tricyclazole and one or more inactive excipients. This prior art does not comprise Flonicamid in combination with Flubendiamide in an insecticidal composition.

However, there is no formulation or composition available where Flubendiamide and Flonicamid are combined in a single formulation which is stable and yet effective.

Inventors of present invention have arrived to a pesticidal formulation of Flubendiamide and Flonicamid in the form of Suspension Concentrate, Wettable Powder and Wettable Dispersible Granule formulation which is stable, effective and overcome all the problems mentioned in prior art as described herein.

OBJECT OF THE INVENTION

The main objective of the present invention is to provide a pesticidal formulation of Flubendiamide and Flonicamid which is stable.

The main objective of the present invention is to provide a pesticidal formulation of Flubendiamide and Flonicamid which reduces the harmful effects to environment.

The main objective of the present invention is to provide a pesticidal formulation of Flubendiamide and Flonicamid which is effective against crop pests.

The main objective of the present invention is to provide a pesticidal formulation of Flubendiamide and Flonicamid which is easy to manufacture.

The main objective of the present invention is to provide a pesticidal formulation of Flubendiamide and Flonicamid which is effective and in use at the field.

SUMMARY OF THE INVENTION

The main aspect of the invention is to provide a synergistic pesticidal formulation of Flubendiamide and Flonicamid.

Another aspect of the present invention is to provide pesticidal suspension concentrate formulation of Flubendiamide and Flonicamid with one or more inactive ingredients.

Yet another aspect of the present invention is to provide to a synergistic pesticidal formulation comprising Flubendiamide and Flonicamid and at least one inactive ingredient, wherein the said composition is suspension concentrate (SC), Wettable Powder (WP) and Wettable Dispersible Granule (WG) formulation and the process of preparation thereof.

DESCRIPTION OF THE INVENTION

The present invention is all about providing a pesticidal formulation of Flubendiamide and Flonicamid.

The detailed description set forth below is intended as a description of exemplary embodiments and is not intended to represent the only forms in which the exemplary embodiments may be constructed and/or utilized. The description sets forth the functions and the sequence of steps for constructing and/or operating the exemplary embodiments. However, it is to be understood that the same or equivalent functions and sequences which may be accomplished by different exemplary methods are also intended to be encompassed within the spirit and scope of the invention.

As defined herein, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs. Although any process and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are now described.

As stated in the present invention herein, the singular forms “a”, “an” and “the” specifically, also encompass the plural forms of the terms to which they refer, unless the content clearly dictates otherwise. The term “about” is used herein to means approximately, in the region of, roughly, or around.

As stated herein, that it follows in a transitional phrase or in the body of a claim, the terms “comprise(s)” and “comprising” are to be interpreted as having an open-ended meaning. That is, the terms are to be interpreted synonymously with the phrases “having at least” or “including at least”.

As used herein, the terms "pesticidal effect" and "pesticidal activity" mean any direct or indirect action on the target pest that results in reduced feeding damage on the seeds, roots, shoots and foliage of plants grown from treated seeds as compared to plants grown from untreated seeds.

As used herein, the term “dispersing agent” means that a substance which added to a suspension of solid or liquid particles in a liquid to improve the separation of the particles and to prevent their settling or clumping.

As used herein, the term “suspending agent” means that a liquid substance which promotes dispersion or solid particles or which can hold a solid substance in suspension.

As used herein the term “wetting agents” are agents which lower the surface tension of water by a considerable amount, although they may be present only in very low concentration. It is well within the competence of those skilled in the art to determine whether a particular surface-active agent (surfactant) is a wetting agent or not.

As used herein the term “anti-freezing agent” means that an additive that, when added to a water-based formulation, will reduce the freezing point of the formulation.

As used herein the term “anti-foaming agent” means that an additive that reduces and hinders the formation of foam in industrial process liquids.

As used herein the term “thickening agent” means that a substance which can increase the viscosity of a liquid without substantially changing its other properties.

As used herein the term “biocide” means that a chemical substance or microorganism intended to destroy, deter, render harmless, or exert a controlling effect on any harmful organism.

The main embodiment of the present invention is to provide stable pesticidal Suspension Concentrate, Wettable Powder and Wettable Dispersible Granule formulation of Flubendiamide and Flonicamid with one or more inactive ingredient.

Another main embodiment of the present invention, provides a pesticidal formulation comprising:
a) Flonicamid,
b) Flubendiamide,
c) One or more dispersing agent,
d) One or more suspending agent,
e) One or more wetting agent,
f) Anti-freezing agent,
g) Adjuvants

As per one embodiment, Flonicamid is present in the range of 15-40% w/w and Flubendiamide is present in the range of 15-40% w/w.

As per one embodiment, dispersing agent for the pesticidal combination of Flonicamid and Flubendiamide of the present invention is selected from group consisting of sodium salt of alkylated naphthalene sulfonate, sodium naphthalene sulfonate formaldehyde condensates, modified styrene Acrylic polymer, Polydimethylsiloxane, Tristyryl phenol ethoxylate phosphate esters, non-ionic such as alkyl aryl ethylene oxide condensates and EO-PO block copolymers, sodium lignosulfonates; sodium naphthalene sulfonate formaldehyde condensates; Tristyryl phenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alkyl ethoxylates; EO-PO block copolymers; and graft copolymers or combination thereof in the concentration range of 0.5 to 5 % w/w.

As per one embodiment, wetting agent for the pesticidal combination of Flonicamid and Flubendiamide of the present invention is selected from group consisting of poly aryl alkoxylated phosphate esters and their potassium salts sodium dioctyl sulfosuccinates, and ethoxylated fatty alcohols, aliphatic alcohol ethoxylates, Trisiloxane ethoxylate, sodium lauryl sulfate; or combination thereof in the concentration range of 0.5-3% w/w.

As per one embodiment, suspending agent for the present invention is selected from group consisting of Polyalkoxylated butyl ether, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxymethyl cellulose, succino glycan, polycarboxylate polymer thickener, preferably (preferably slightly) crosslinked polyacrylate, xanthan gum, Silicon Dioxide, colloidal silicon dioxide or combination thereof in the concentration range of range of 0.5-3% w/w.

As per one embodiment, anti-freezing agent for the present invention is selected from group consisting of glycerin, propylene glycol, polyethylene glycol and ethylene glycol in the concentration range of 4-8% w/w.

As per one embodiment, the pesticidal formulation also contains one or more additional adjuvants selected from anti foaming agent, biocide, thickening agent, and vehicle in the concentration range of 1-10% w/w.

The following examples are meant to illustrate the present invention. The examples are presented to exemplify the invention and are not to be considered as limiting the scope of invention.

EXAMPLES
Example 1: Flubendiamide + Flonicamid Suspension Concentrate Formulation
Table 1.1: Composition of Flubendiamide + Flonicamid SC
Sr No. Chemical Composition Percent (% w/w)
1 Flonicamid Tech. (Purity-98.00%) 20.60
2 Flubendiamide Tech. (Purity-98.00%) 20.60
3 Modified Styrene Acrylic Polymer 3.00
4 Ethoxylated Fatty Alcohol 2.00
5 Polyalkoxylated butyl ether 0.50
6 Alkylated naphthalene sulfonate, sodium salt 0.50
7 Tri siloxane ethoxylate 2.00
8 Poly dimethyl siloxane 0.50
9 Silicon Dioxide 0.50
10 Polysaccharides 0.20
11 1,2-benzisothiazol-3-one 0.25
12 Vegetable Oil 8.00
13 Polypropylene glycol 5.00
14 DM Water 36.35
Total 100.00

Table 1.2: Heat stability for 14 days at 54 degrees centigrade & cold stability 7 days at 0 degrees centigrade
Parameters Specification (In house) Initial Heat Stability at 54±2 degrees centigrade Cold Stability at 0±2 degrees centigrade
Flonicamid content % w/w 19.00 to 21.00 20.25 20.28 20.12
Flubendiamide content % w/w 19.00 to 21.00 20.21 20.18 20.20
Flonicamid suspensibility % mini. 80 98.45 98.43 98.51
Flubendiamide suspensibility % mini. 80 99.10 98.90 99.05
pH range (1% aqueous suspension) 5.50 to 7.50 7.10 7.05 7.11
Pourability 95% min. 98.50 98.10 97.97
Specific gravity 1.10- 1.20 1.17 1.178 1.171
Viscosity at spindle no. 62,20 rpm 350-800 cps 630 632 630
Particle size (micron) D50<3, D90<10 2.2, 5.9 2.3,
6.1 2.4,
6.5
Persistent foam ml (after 1 minute) max. 60 5 6 5

Table 1.3: Room Temperature storage stability up to 12 months
Parameters Specification (in house) 1 month 6 months 12 months
Flonicamid content % w/w 19.00 to 21.00 20.21 20.17 20.19
Flubendiamide content % w/w 19.00 to 21.00 20.2 20.22 20.21
Flonicamid suspensibility % mini. 80 98.12 98.38 98.43
Flubendiamide suspensibility % mini. 80 98.92 99.00 98.95
pH range (1% aqueous Suspension) 5.50 to 7.50 7.05 7.04 7.02
Pourability 95% min. 98.76 98.52 98.25
Specific gravity 1.10- 1.20 1.172 1.178 1.179
Viscosity at spindle no. 62,20 rpm 350-800 cps 627 638 640
Particle size (micron) D50<3, D90<10 2.1,
5.6 2.2,
5.9 2.3,6.0
Persistent foam ml (after 1 minute) max. 60 9 5 6

Process of Preparation of Flubendiamide and Flonicamid SC solution:
a) A gum solution was prepared by adding 1,2-benzisothiazol-3-one to De-Mineralized water;
b) The step (a) solution was stirred for 10 min and then polysaccharides were added;
c) The step (b) solution was stirred for about 3 hours and the vessel was heated at 50? and the solution was allowed to stand for 3 hours before using;
d) De-Mineralized water was charged in a vessel and agitated;
e) Then modified styrene Acrylic polymer, Alkylated naphthalene sulfonate, sodium salt, Polyalkoxylated butyl ether, Silicon Dioxide, Ethoxylated Fatty Alcohol, Trisiloxane ethoxylate, Polypropylene glycol, vegetable oil, Polydimethylsiloxane was added into the step (d) solution and mixed for half an hour;
f) Flonicamid and Flubendiamide was added to step (e) and mixed;
g) The step (f) solution was homogenized under high shear homogenization;
h) The material of step (g) was Milled/ Grinded through bead milling and required particle size was achieved;
i) The milled material of step (h) was collected in a post mixing vessel;
j) The gum solution of step (c) was added into the milled material of step (i) and stirred till got completely homogenized solution;
k) The final solution of step (j) was stored into the suitable container.

Example 2: Flubendiamide + Flonicamid Wettable Dispersible Granule Formulation
Table 2.1: Composition of Flubendiamide + Flonicamid WG
Sr No. Chemical Composition Percent (% w/w)
1 Flonicamid Tech. (Purity- 98.00%) 30.85
2 Flubendiamide Tech (Purity- 98%) 30.85
3 Sodium salt of sulphonate naphthalene formaldehyde condensate 5.00
4 Sodium Alkyl naphthalene sulphonate condensate 3.00
5 Polycarboxylate Sodium salt 5.00
6 Sodium Lauryl sulphate 5.00
7 Alkylated naphthalene sulfonate, sodium salt 5.00
8 Poly dimethyl siloxane 0.50
9 sodium sulphate anhydrous 7.00
10 Hydrated Aluminum Silicate 7.80
11 Total 100.00

Table 2.2: Heat stability for 14 days at 54 degrees centigrade & cold stability 7 days at 0 degrees centigrade
Parameters Specification (in house) Initial Heat stability at 54±2 degrees centigrade Cold stability at 0±2 degrees centigrade
Flonicamid content % w/w 28.50 to 31.50 30.27 30.25 30.27
Flubendiamide content % w/w 28.50 to 31.50 30.31 30.19 30.21
Flonicamid suspensibility % mini. 80 96.54 96.48 96.52
Flubendiamide suspensibility % mini. 80 95.83 95.27 95.64
pH range (1% aqueous suspension) 5.50 to 7.50 6.98 6.95 6.96
Wettability sec max. 60 11 11 12
Wet sieve (45 micron) % w/w min. 98.5 99.53 99.58 99.57
Bulk density (g/ml) 0.45 to 0.85 0.64 0.65 0.64
Moisture content % w/w max. max. 2% 1.1 1.05 1.11
Degree of Dispersion 30 Max. 25 26 25

Table 2.3: Room Temperature storage stability up to 12 months
Parameters Specification (in house) 1 month 6 months 12 months
Flonicamid content % w/w 28.50 to 31.50 30.23 30.25 30.28
Flubendiamide content % w/w 28.50 to 31.50 30.29 30.17 30.16
Flonicamid suspensibility % mini. 80 96.45 96.43 96.42
Flubendiamide suspensibility % mini. 80 95.61 95.57 95.36
pH range (1% aqueous Suspension) 5.50 to 7.50 6.96 6.92 6.9
Wettability sec max. 60 11 12 11
Wet sieve (45 micron) % w/w min. 98.5 99.58 99.6 99.56
Bulk density (g/ml) 0.45 to 0.85 0.75 0.74 0.75
Moisture content % by mass max. max. 2% 1.1 1.05 1.11
Degree of Dispersion 30 Max. 23 25 26

Process of Preparation of Flubendiamide and Flonicamid WG formulation:
Step I: Preparation of Powder
a) Charge Flubendiamide technical and Flonicamid technical and other inactive ingredients as per recipe in table 4.2 in pre-blender and mix properly for 30- 45 minutes.
b) Pre-blender of materials as mentioned in step a) is carried out for one hour. Powder shall be homogeneous before jet milling /ACM 30 milling.
c) The Pre-mix of step b) is then feed continuously to air jet mill/ACM 30 Mill.
d) Check the particle size of milled material obtained in step c). The milled material is homogenized in post blender by blending for 1 hour.
Step II: Preparation of Granules: Take a required quantity of water and the milled material in step d) to make dough for extrusion and then dried and sieved. After completion of sieving, the samples of granules obtained are stored for QC analysis.

Example 3: Flubendiamide + Flonicamid Wettable Powder Formulation
Table 3.1: Composition of Flubendiamide + Flonicamid WP
Chemical Composition Percent (% w/w)
1 Flonicamid Tech. (Purity- 98.00%) 35.95
2 Flubendiamide Tech (Purity- 98%) 35.95
3 Sodium salt of sulphonate naphthalene formaldehyde condensate 5.00
4 Sodium Alkyl naphthalene sulphonate condensate 3.00
5 Sodium Lauryl sulphate 5.00
6 Poly dimethyl siloxane 0.50
7 sodium sulphate anhydrous 5.00
8 Hydrated Aluminum Silicate 9.60
9 Total 100.00

Table 3.2: Heat stability for 14 days at 54 degrees centigrade & cold stability 7 days at 0 degrees centigrade
Parameters Specification (in house) Initial Heat stability at 54±2 degrees centigrade Cold stability at 0±2 degrees centigrade
Flonicamid content % w/w 33.25 to 36.75 35.29 35.18 35.24
Flubendiamide content % w/w 33.25 to 36.75 35.21 35.11 35.14
Flonicamid suspensibility percent mini. 80 94.21 94.17 94.23
Flubendiamide suspensibility percent mini. 80 93.67 93.43 93.51
pH range (1% aq Suspension) 5.50 to 7.50 7.1 7.12 7.07
Wettability sec max. 60 36 35 27
Wet sieve (45 micron) percent by mass min. 98.5 99.17 99.04 99.11
Bulk density (g/ml) 0.30 to 0.60 0.4 0.39 0.41
Moisture content percent by mass max. max. 2% 1.1 1.05 1.11
Persistent foam ml (after 1 minute) max. 60 42 39 40

Table 3.3: Room Temperature storage stability up to 12 months
Parameters Specification (in house) 1 month 6 months 12 months
Flonicamid content % w/w 33.25 to 36.75 35.23 35.19 35.17
Flubendiamide content % w/w 33.25 to 36.75 35.21 35.15 35.12
Flonicamid suspensibility % mini. 80 94.25 94.23 94.14
Flubendiamide suspensibility % mini. 80 93.61 93.27 93.16
pH range (1% aqueous suspension) 5.50 to 7.50 7.05 7.12 7.1
Wettability sec max. 60 38 32 35
Wet sieve (45 micron) percent by mass min. 98.5 99.18 99.06 99.02
Bulk density (g/ml) 0.30 to 0.60 0.41 0.41 0.42
Moisture content % by mass max. max. 2% 1.13 1.17 1.19
Persistent foam ml (after 1 minute) max. 60 45 42 43

Process of Preparation of Flubendiamide and Flonicamid WP formulation:
a) Charge Flubendiamide technical and Flonicamid technical and other inactive ingredients as per recipe in table 4.2 in pre-blender and mix properly for 30- 45 minutes.
b) Pre-blender of materials as mentioned in step a) is carried out for one hour. Powder shall be homogeneous before jet milling /ACM 30 milling.
c) The Pre-mix of step b) is then feed continuously to air jet mill/ACM 30 Mill.
d) Check the particle size of milled material obtained in step c). The milled material is homogenized in post blender by blending for 1 hour.
e) The final powder product is stored and sent for QC analysis.

Example 4: Field Trial Studies
Field trial experiments were conducted to evaluate the efficacy of Flubendiamide and Flonicamid formulations in comparison to its solo applications.

The observations were recorded by counting the no. of pests before the treatment, after 7 days of treatment and after 15 days of treatment on the crops. The % percent population reduction/ control of pests was calculated by below formula:

Example 4.1: Efficacy of Flubendiamide 20% + Flonicamid 20% SC on Rice BPH* (Nilaparvata lugens) population control.
Location: Bellary, Karnataka, India
Season: Kharif- 2021
Crop: Rice
Date of Transplanting: 03/08/2021
Date of application: 24/09/2021
Treatment details Dose Pre-Treatment 7 DAT
** 15 DAT % Reduction / Control
T1 Flubendiamide 20% + Flonicamid 20% SC 250 ml/ha 26.50 16.75 13.25 47.83
T2 Flubendiamide 20% + Flonicamid 20% SC 300 ml/ha 25.25 8.75 5.50 75.22
T3 Flubendiamide 20% + Flonicamid 20% SC 350 ml/ha 23.50 9.00 4.75 76.09
T4 Flubendiamide 39.35% SC 50 ml/ha 23.75 20.75 13.00 41.30
T5 Flonicamid 50% WDG 150 g/ha 23.25 19.75 14.25 40.87
T6 Untreated control 26.00 31.75 25.75 ---
CV*** (%) 13.34 15.44 26.66
CD**** 5% 5.74 4.78 5.91
Note: *BPH: Brown Plant Hopper, **DAT: Days After Treatment, ***CV= Co-efficient of Variation, **** CD= Critical Difference

The results of the above experiment show that the suspension concentrate formulation of Flubendiamide 20% and Flonicamid 20% show synergistic effect in terms of % Population reduction/ Control of BPH in Rice.

Example 4.2 (a) Efficacy of Flubendiamide 30% + Flonicamid 30% WG on Cotton whitefly (Bemisia tabaci) population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 05/07/2021
Date of application: 04/09/2021
Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 30% + Flonicamid 30% WG 175 g/ha 15.25 11.50 13.25 24.45
T2 Flubendiamide 30% + Flonicamid 30% WG 200 g/ha 15.75 6.00 5.75 64.13
T3 Flubendiamide 30% + Flonicamid 30% WG 225 g/ha 16.25 5.25 5.00 68.71
T4 Flubendiamide 39.35% SC 50 ml/ha 16.75 11.25 11.75 29.79
T5 Flonicamid 50% WG 150 g/ha 16.50 9.25 10.00 41.24
T6 Untreated control 16.00 16.25 16.50 0.00
CV** (%) 22.58 30.50 28.04
CD*** 5% 6.32 5.26 5.06
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, *** CD= Critical Difference

The results of the above experiment show that the Water Dispersible Granule formulation of Flubendiamide 30% and Flonicamid 30% show synergistic effect in terms of % Population reduction/ Control of whiteflies in cotton.

Example 4.2 (b) Efficacy of Flubendiamide 30% + Flonicamid 30% WG on Cotton Thrips (Thrips tabaci) population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 05/07/2021
Date of application: 04/08/2021
Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 30% + Flonicamid 30% WG 175 g/ha 15.75 10.00 11.25 51.43
T2 Flubendiamide 30% + Flonicamid 30% WG 200 g/ha 16.00 5.50 4.00 78.29
T3 Flubendiamide 30% + Flonicamid 30% WG 225 g/ha 17.50 6.50 3.75 76.57
T4 Flubendiamide 39.35% SC 50 ml/ha 15.25 9.75 10.50 53.71
T5 Flonicamid 50% WDG 150 g/ha 16.00 9.50 10.00 55.43
T6 Untreated control 17.25 20.00 23.75 -
CV** (%) 13.10 15.30 23.69
CD*** 5% 3.71 2.72 4.34
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, ***CD= Critical Difference

The results of the above experiment show that the Water Dispersible Granule formulation of Flubendiamide 30% and Flonicamid 30% show synergistic effect in terms of % Population reduction/ Control of Thrips in cotton.

Example 4.2 (c) Efficacy of Flubendiamide 30% + Flonicamid 30% WG on Cotton Leaf Hoppers (Amrasca biguttula biguttula) population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 05/07/2021
Date of application: 13/08/2021
Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 30% + Flonicamid 30% WG 175 g/ha 7.25 8.75 8.00 28.72
T2 Flubendiamide 30% + Flonicamid 30% WG 200 g/ha 6.75 3.00 3.25 73.40
T3 Flubendiamide 30% + Flonicamid 30% WG 225 g/ha 6.00 2.75 2.50 77.66
T4 Flubendiamide 39.35% SC 50 ml/ha 6.00 9.75 7.25 27.66
T5 Flonicamid 50% WDG 150 g/ha 6.25 8.50 7.50 31.91
T6 Untreated control 6.50 12.25 11.25 -
CV** (%) 28.14 41.66 37.74
CD*** 5% 3.16 5.44 4.35
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, ***CD= Critical Difference

The results of the above experiment show that the Water Dispersible Granule formulation of Flubendiamide 30% and Flonicamid 30% show synergistic effect in terms of % Population reduction/ Control of Leaf hoppers in cotton.

Example 4.3 (a) Efficacy of Flubendiamide 35% + Flonicamid 35% WP on Cotton whitefly population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 07/07/2021
Date of application: 06/09/2021
Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 35% + Flonicamid 35% WP 150 g/ha 16.00 5.50 6.25 64.39
T2 Flubendiamide 35% + Flonicamid 35% WP 175 g/ha 16.25 3.75 2.25 81.82
T3 Flubendiamide 35% + Flonicamid 35% WP 200 g/ha 15.50 3.25 2.00 84.09
T4 Flubendiamide 39.35% SC 50 ml/ha 15.75 7.75 11.25 42.42
T5 Flonicamid 50% WDG 150 g/ha 16.00 9.00 9.00 45.45
T6 Untreated control 15.25 15.75 17.25 -
CV** (%) 29.97 37.90 34.70
CD*** 5% 8.24 4.95 4.83
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, *** CD= Critical Difference

The results of the above experiment show that the Wettable Powder formulation of Flubendiamide 35% and Flonicamid 35% show synergistic effect in terms of % Population reduction/ Control of whiteflies in cotton.

Example 4.3 (b) Efficacy of Flubendiamide 35% + Flonicamid 35% WP on Cotton Thrips population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 07/07/2021
Date of application: 06/08/2021
Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 35% + Flonicamid 35% WP 150 g/ha 11.25 9.00 5.75 37.89
T2 Flubendiamide 35% + Flonicamid 35% WP 175 g/ha 12.00 3.75 2.75 72.63
T3 Flubendiamide 35% + Flonicamid 35% WP 200 g/ha 11.50 2.75 3.00 75.79
T4 Flubendiamide 39.35% SC 50 ml/ha 12.50 8.50 6.25 37.89
T5 Flonicamid 50% WDG 150 g/ha 12.75 9.00 7.00 32.63
T6 Untreated control 12.25 12.00 11.75
CV** (%) 25.02 32.21 15.83
CD*** 5% 5.24 4.20 1.53
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, *** CD= Critical Difference

The results of the above experiment show that the Wettable Powder formulation of Flubendiamide 35% and Flonicamid 35% show synergistic effect in terms of % Population reduction/ Control of thrips in cotton.

Example 4.3 (c) Efficacy of Flubendiamide 35% + Flonicamid 35% WP on Cotton Leaf hoppers population control.
Location: Raichur, Karnataka, India
Season: Kharif-2021
Crop: Cotton
Date of sowing: 07/07/2021
Date of application: 16/08/2021

Treatment details Dose Pre-Treatment 7 DAT
* 15 DAT % Reduction / Control
T1 Flubendiamide 35% + Flonicamid 35% WP 150 g/ha 12.75 8.25 8.50 35.58
T2 Flubendiamide 35% + Flonicamid 35% WP 175 g/ha 11.75 4.00 3.75 70.19
T3 Flubendiamide 35% + Flonicamid 35% WP 200 g/ha 13.50 3.50 4.00 71.15
T4 Flubendiamide 39.35% SC 50 ml/ha 11.50 9.25 5.75 42.31
T5 Flonicamid 50% WDG 150 g/ha 11.50 8.00 7.75 39.42
T6 Untreated control 12.50 12.75 13.25
CV** (%) 16.78 42.11 27.88
CD*** 5% 3.58 5.59 3.48
Note: *DAT: Days After Treatment, **CV= Co-efficient of Variation, *** CD= Critical Difference

The results of the above experiment show that the Wettable Powder formulation of Flubendiamide 35% and Flonicamid 35% show synergistic effect in terms of % Population reduction/ Control of Leaf Hoppers in cotton.

From the results in Examples 1-4, the pesticidal combination of Flubendiamide and Flonicamid in SC, WG and WP formulation claimed in the present invention have a synergistic effect on control of pests.

Although the foregoing invention has been described in some way by way of illustration and example of purposes of clarity of understanding, it will be readily apparent to those of ordinary skill in the art in light of the teachings of this invention that certain changes and modifications may be made thereto.
,CLAIMS:We Claim:
1. A synergistic pesticidal formulation of Flubendiamide and Flonicamid comprising:
a) Flonicamid Technical (Purity 98% w/w) in the concentration range of 15-40% w/w,
b) Flubendiamide Technical (Purity 98% w/w) in the concentration range of 15-40% w/w,
c) One or more dispersing agent in the concentration range of 0.5-5% w/w,
d) One or more suspending agent in the concentration range of 0.5-3% w/w,
e) One or more wetting agent in the concentration range of 0.5-3% w/w,
f) Anti-freezing agent in the concentration range of 4-8% w/w,
g) Adjuvants in the concentration range of 1-10% w/w.

2. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein Flonicamid is present in the range of 15-40% w/w and Flubendiamide is present in the range of 15-40% w/w.

3. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein the dispersing agent for the pesticidal combination of Flonicamid and Flubendiamide of the present invention is selected from group consisting of sodium salt of alkylated naphthalene sulfonate, sodium naphthalene sulfonate formaldehyde condensates, modified styrene Acrylic polymer, Polydimethylsiloxane, Tristyryl phenol ethoxylate phosphate esters, non-ionic such as alkyl aryl ethylene oxide condensates and EO-PO block copolymers, sodium lignosulfonates; sodium naphthalene sulfonate formaldehyde condensates; Tristyryl phenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alkyl ethoxylates; EO-PO block copolymers; and graft copolymers or combination thereof in the concentration range of 0.5 to 5 % w/w.

4. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein suspending agent for the present invention is selected from group consisting of Polyalkoxylated butyl ether, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxymethyl cellulose, succino glycan, polycarboxylate polymer thickener, preferably (preferably slightly) crosslinked polyacrylate, xanthan gum, Silicon Dioxide, colloidal silicon dioxide or combination thereof in the concentration range of range of 0.5-3% w/w.

5. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein wetting agent for the pesticidal combination of Flonicamid and Flubendiamide of the present invention is selected from group consisting of poly aryl alkoxylated phosphate esters and their potassium salts sodium dioctyl sulfosuccinates, and ethoxylated fatty alcohols, aliphatic alcohol ethoxylates, Trisiloxane ethoxylate, sodium lauryl sulfate; or combination thereof in the concentration range of 0.5-3% w/w.

6. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein anti-freezing agent for the present invention is selected from group consisting of glycerin, propylene glycol, polyethylene glycol and ethylene glycol in the concentration range of 4-8% w/w.

7. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein the pesticidal formulation also contains one or more additional adjuvants selected from anti foaming agent, biocide, thickening agent, and vehicle in the concentration range of 1-10% w/w.

8. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 1, wherein the combination is formulated as Suspension Concentrate (SC), Water Dispersible Granules (WG) and Wettable Powder (WP).

9. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 8, wherein SC formulation comprises 20% w/w Flubendiamide and 20% w/w Flonicamid.

10. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 8, wherein WG formulation comprises 30% w/w Flubendiamide and 30% w/w Flonicamid.

11. The synergistic pesticidal formulation of Flubendiamide and Flonicamid as claimed in claim 8, wherein WP formulation comprises 35% w/w Flubendiamide and 35% w/w Flonicamid.

Dated this day of November, 2022

Signature:
Name: Patel Ankit (CEO)