DESC:STABLE FORMULATION OF N-(CYANOMETHYL)-4-(TRIFLUOROMETHYL) PYRIDINE-3-CARBOXAMIDE AND METHOD OF PREPARATION

FIELD OF THE INVENTION
The present invention relates to pesticidal compositions. More particularly, the present invention relates to a soluble granule (SG) formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide which has improved solubility.

BACKGROUND OF THE INVENTION
Pests such as aphids, thrips, leafhoppers, planthoppers, and whiteflies pose a threat to field crops due to their piercing-sucking mouthparts. They cause damage by directly feeding on plants and transmitting harmful plant viruses. Aphids, for instance, are major transmitters of plant viruses and are responsible for spreading various viral diseases. Their feeding results in yellowing and curling of leaves, and they can transmit viruses such as African cassava mosaic, bean golden mosaic, tomato yellow leaf curl, and cotton leaf crumple disease. Similarly, thrips puncture plant cells to extract their contents, leading to silvery patches and the drying out of leaves. They may also transmit tospoviruses and Cotton Bud disease. Leafhoppers and planthoppers also suck plant juices, which causes leaf yellowing, curling, and stunted growth, and serve as vectors for numerous plant viruses. Whiteflies, on the other hand, transmit over 100 plant viruses, and their feeding and excretion of honeydew can lead to the growth of sooty mould, which interferes with photosynthesis. The combined damage caused by these piercing-sucking pests through direct feeding and virus transmission can significantly impact crop health, yield, and quality. Therefore, it is essential to implement integrated pest management strategies that include cultural, biological, and selective chemical controls to manage these key pests in field crops effectively.

Chemical pesticides are used in the agricultural field to eliminate or control unwanted pests effectively. Various formulations, such as water-dispersible granules, wettable powder, and suspension concentrate, are used. The existing formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide including WDG and SG have some limitations. For Example, IN297790 discloses a water dispersible granular composition containing up to 90% of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide with other excipients. US8227493 discloses a soluble granule composition containing 45-55% N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide.
Despite some advantages, the existing N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide formulation including the soluble granule formulations have shortcoming that limit their utility and cost effectiveness. Existing soluble granule formulations frequently exhibit inadequate dissolution rates and incomplete solubilisation in water. The poor dissolution often leads to non-uniform distribution of active ingredients in spray solutions, leading to inconsistent pest control efficacy. Also, the incomplete dissolution may also cause localized concentration variations that may lead to phytotoxicity in some areas and inadequate pest control in others.

While soluble granules theoretically offer superior bioavailability compared to suspension-based formulations, current formulations fail to achieve optimal bioavailability due to formulation deficiencies. Poor dissolution characteristics directly translate to reduced bioavailability, negating the primary advantage of the soluble granule format. Further, the available soluble granule formulation is prone to chemical degradation. Such degradation often takes place without any visible indicators, leading to unknowing application of degraded, ineffective products. The inadequate dissolution may lead to practical application difficulties, including equipment clogging, uneven spray patterns, and reduced spray tank cleanout efficiency, which increase labor costs, equipment maintenance requirements, and the risk of cross-contamination when switching between different pesticide applications.

There exists a long-felt need for soluble granule formulations that provide rapid and complete dissolution in water across a range of water quality conditions and temperatures typically encountered in agricultural applications, enhanced bioavailability that maximises the effectiveness of active ingredients while ensuring optimal pest control efficacy with reduced application rates, and superior chemical stability that resists degradation during storage while maintaining active ingredient integrity over extended periods under various environmental conditions. Additionally, there is a need for improved handling that minimise dust generation, reduce inhalation hazards, and facilitate easy and complete cleanout of spray equipment, along with consistent performance that delivers predictable and reliable pest control results across diverse application conditions and pest pressure scenarios. The present invention addresses these long-standing technical challenges. It provides a significant advancement in soluble granule pesticide technology, offering superior performance characteristics that overcome the limitations of existing formulations while providing enhanced economic benefits to agricultural users.
OBJECT OF THE INVENTION
The primary object of the present invention is to provide a soluble granule pesticidal formulation.

Another object of the present invention is to provide a method for preparation of soluble granule pesticidal formulation.

Yet another object of the present invention is to provide a soluble granule formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide.

Yet another object of the present invention is to provide a soluble granule formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide having a penetrant.

Yet another objection of the present invention is to provide a soluble granule formulation with improved solubility and bioavailability.

Still another object of the present invention is to provide a soluble granule formulation with enhanced bio-efficacy.

SUMMARY OF THE INVENTION
The following presents a simplified summary of the invention to provide a basic understanding of some aspects of the invention. This summary is not an extensive overview of the present invention. It is not intended to identify the key/critical elements of the invention or to delineate the scope of the invention. Its sole purpose is to present some concept of the invention in a simplified form as a prelude to a more detailed description of the invention presented later.

Accordingly, the present invention aims to provide a soluble granule pesticidal formulation.

In an aspect, the present invention provides a soluble granule formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide.

In another aspect, the present invention provides a pesticidal formulation comprising N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and at least one agriculturally acceptable additive.
In another aspect, the present invention provides a pesticidal formulation comprising N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, at least one dispersing agent, at least one wetting agent, at least one defoamer; and at least one penetrant.

In another aspect of the present invention, the formulation further comprises at least one carrier.

In another aspect of the present invention, the formulation is in the form of Soluble Granule (SG).

In an aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 10 to 60% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 15 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 20 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 25 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 30 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 35 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 40 to 55% by weight.

In another aspect of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 45 to 55% by weight.

In another aspect of the present invention, the dispersing agent is selected from a group consisting of ‘alpha’-olefin sulfonate; maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9); salt of naphthalene sulphonic acid condensation product; phenol sulphonic acid condensation product; sodium dioctyl sulfosuccinate; sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; ethoxylated polyarylphenol phosphate ester, polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates; polyoxyethylene polyoxypropylene block copolymer phosphate; olefin-copolymer, sodium salt; and/or graft copolymer. Further, the dispersing agent is present in the range of 5 to 9% by weight.

In another aspect of the present invention, the wetting agent is selected from the group consisting of sugar esters; alkyl polyglucoside; polyoxyethylene alkyl ethers; polyoxyethylene alkynyl ether; polyoxyethylene aryl ethers; polyoxyethylene fatty acid esters; polyoxyethylene polyoxypropylene block copolymers; polyoxyethylene polyoxypropylene alkyl ether; polyoxyethylene polyoxypropylene aryl ether; polyoxyethylene alkyl amines; polyoxyethylene fatty acid amide; sodium lauryl sulfate; sodium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates; polyoxyethylene aryl ether sulfates; blend of alkyl sulphate and ethoxylates sulphate salt; amine salt of phosphate tristyryl phenol ethylated; calcium dodecyl benzene sulfonate; sodium naphthalene sulfonate and sodium naphthalene sulfonate formaldehyde condensate. Further, the wetting agent is present in the range of 0.1 to 4% by weight.

In another aspect of the present invention, the defoamer is selected from the group consisting of polysiloxane, polydimethyl siloxane and organic fluorine compounds and is present in the range of 0.1 to 3% by weight.

In further aspect, the penetrant is selected from group consisting of cocoamine propyl amide, silicon-based adjuvants, and esterified and/or etherified polyol alkoxylate compounds. The penetrant is present in the range of 0.1 to 3% by weight.

In another aspect, the carrier is selected from group consisting of natural minerals, synthetic minerals, inorganic salts, urea, solid polyoxyethylene, solid polyoxypropylene, polyethylene, polypropylene, citric acid, trisodium citrate, lactose (4-O-beta-D-Galactopyranosyl-D-glucose), starch, lignin, cellulose, cottonseeds hulls, wheat flour, soybean flour, wood flour, walnut shell flour, plant powders, sawdust, coconut shellflower, corn cob, and/or tobacco stem.
In yet another aspect, the present invention provides a method for preparing the soluble granule formulation comprising the steps of:
mixing N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, at least one dispersing agent, at least one wetting agent, and at least one defoamer to form a mixture;
milling and homogenizing the mixture; and
preparing a dough by adding at least one penetrant and required amount of distilled water to the homogenized mixture and granulating the dough using an extruder to obtain granules.

Other aspects, advantages, and salient features of the invention will become apparent to those skilled in the art from the following detailed description, which, details the invention in different embodiments.

BRIEF DECRIPTION OF DRAWINGS

Figure 1: a flow diagram for process of preparation of the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation.

Figure 2: a pictorial representation for contact angle of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation with penetrant.

Figure 3: a graphical representation for contact angle analysis of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation with penetrant.

Figure 4: a pictorial representation for contact angle of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation without penetrant.

Figure 5: a graphical representation for contact angle analysis of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation without penetrant.

DETAILED DESCRIPTION OF THE INVENTION
The definitions provided herein below for the terminologies used in the present disclosure are for illustrative purpose only and in no manner limit, the scope of the present invention disclosed in the present disclosure.

All technical and scientific phrases or terms used here have the same meanings as those that a person who is skilled in the field of study of the current subject matter would understand. Although other process and materials similar, or equivalent, to those described herein may be used in the practice of the present invention, the preferred materials and process are described herein.

It is to be noted that, as used in the specification, the singular forms “a”, “an”, and “the” include plural referents unless the context dictates otherwise. It should also be noted that the term “or” is generally employed in its sense, including “and/or” unless the content dictates otherwise.

The use of terms “including,” “comprising,” or “having” and variations thereof herein; are meant to encompass the items listed thereafter and equivalents thereof as well as additional items. Further, the use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results. Furthermore, the term “may” be used herein in a permissive sense (i.e. meaning having the potential to), rather than the mandatory sense, (i.e. meaning must).

The terms “preferred” and “preferably” refer to embodiments of the invention that may afford certain benefits under certain circumstances. In an embodiment, the aspects and embodiments described herein shall also be interpreted to replace the clause “comprising” with either “consisting of” or with “consisting essentially of” or with “consisting substantially of”.

The terms “process” and “method” as used herein convey the same meaning and may be used interchangeably.
The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight relative to the weight of the total solution or formulation unless otherwise specified.

The terms “formulation” and “composition”, as used herein, convey the same meaning and may be used interchangeably.
The term “active ingredient” (a.i.) or “active agent” or “actives” used herein refers to that component of the composition responsible for the control of insect pests.

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

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

According to the present invention, “increased yield” of a plant, in particular, of an agricultural, silvicultural and/ or horticultural plant, means that the yield of a product of the respective plant is increased by a measurable amount over the yield of the same product of the plant produced under the same conditions, but without the application of the formulation according to the present invention.

Increased yield may be characterized, among others, by the following improved properties of the plant: increased plant weight, increased plant height, increased biomass such as higher overall fresh weight (FW), increased number of flowers per plant, higher grain yield, more tillers or side shoots (branches), larger leaves, increased shoot growth, increased leaf area index.

Another indicator for the condition of the plant is the “enhanced quality” of a plant and/or its products.

Accordingly, the present invention provides a soluble granule pesticidal formulation and its preparation method.

In an embodiment, the present invention provides a soluble granule pesticidal formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide.

As used herein, the term “N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide” encompasses its agrochemically acceptable salts, derivatives or isomeric form or any other modified form of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide. N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is a systemic insecticide belonging to the pyridinecarboxamides family. It is highly effective against aphids and other piercing-sucking pests, such as thrips, leafhoppers, planthoppers, and whiteflies.

In another embodiment, the present invention provides a pesticidal formulation comprising N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and at least one agriculturally acceptable additive.

The present invention formulation may comprises at least one agriculturally acceptable additives selected from the group comprising of the carrier(s), surfactant(s), wetting agent(s), dispersing agent(s), binder(s), disintegrating agent(s), pH modifier(s), thickener(s), biocide(s), safener(s), penetrant(s), anti-freezing agent(s), defoaming agent(s) / defoamer(s) / antifoaming agent(s) / antifoamer(s), and/or stabilizer(s) or a combination thereof. If desired, the formulation may also contain one or more auxiliaries customary for crop protection formulations.

The present invention provides a soluble granule formulation comprising of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide.

In an embodiment of the present invention, the formulation comprises of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, at least one dispersing agent, at least one wetting agent, at least one penetrant, at least one defoamer and at least one carrier.
In another embodiment of the present invention, the formulation is in the form of Soluble Granule (SG).

In another embodiment of the present invention, the formulation comprises of:
N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide in an amount in the range of 45 to 55% by weight;
at least one dispersing agent in an amount in the range of 5 to 9% by weight;
at least one wetting agent in an amount in the range of 0.1 to 4% by weight;
at least one penetrant in an amount in the range of 0.1 to 2% by weight;
at least one defoamer in an amount in the range of 0.1 to 2.5% by weight; and
at least one carrier in a quantity required to make up 100% by weight.
In a preferred embodiment of the present invention, the formulation comprises of:
N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide in an amount in the range of 45 to 55% by weight;
at least one dispersing agent in an amount in the range of 6 to 8% by weight;
at least one wetting agent in an amount in the range of 1 to 3% by weight;
at least one penetrant in an amount in the range of 0.1 to 1% by weight;
at least one defoamer in an amount in the range of 0.1 to 1% by weight; and
two or more carriers in a quantity required to make up 100% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 15 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 20 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 25 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 30 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 35 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 40 to 55% by weight.

In another embodiment of the present invention, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 45 to 55% by weight.

In another embodiment of the present invention, the formulation has pH in the range of 5 to 9 in 1% aqueous solution.

In another embodiment, the present invention provides a method for preparing a soluble granule pesticidal formulation comprising the steps of (a) charging the required quantity of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, dispersing agent, wetting agent, and defoamer in a pre-blender to obtain a mixture; (b) mixing and milling the mixture of step (a) to obtain a milled mixture; (c) extracting a homogeneous sample from the milled mixture of step (b) for QC analysis; (d) making dough from the sample of step (c), adding penetrant and granulating using an extruder to obtain granules; and (e) drying the granules of step (d) to obtain a soluble granule formulation.

In a preferred embodiment, the present invention provides a method for preparing a soluble granule pesticidal formulation comprising the steps of (a) charging the required quantity of carrier, N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide, dispersing agent, wetting agent, and defoamer in a pre to obtain a mixture; (b) mixing and milling the mixture of step (a) with the help of a Jet mill to obtain a milled mixture; (c) after Jet milling, extracting homogeneous sample from the milled mixture of step (b) for QC analysis; (d) making dough adding penetrant and granulating using an extruder to obtain granules; (e) drying the granules of step (d) with the help of a Fluid bed dryer (FBD) to obtain a soluble granule formulation; (f) drawing the final sample for QC analysis; and (g) packing the finished product as illustrated in FIG. 1.

In another embodiment of the present invention, the method further comprises adding the required amount of demineralized (DM) water for making dough.

Surfactant(s) (a dispersing agent, a wetting agent, a spreader, an adjuvant for penetration enhancement, rain fastness, soil leaching control etc.) are non-ionic or anionic surfactant(s) or a combination of these surfactants. It is preferred to use one or more than one kind of surfactant. Surfactants may be selected from the group comprising of, but not limited to, sugar esters such as sorbitan monolaurate, polyoxyethylene sorbitan monolaurate; alkyl polyglucoside such as decyl glucoside; polyoxyethylene alkyl ethers such as polyoxyethylene lauryl ether or polyoxyethylene coconut fatty alcohol ether; polyoxyethylene alkynyl ether such as 2,4,7,9- tetramethyl-5-decyn-4,7-diol ether; polyoxyethylene aryl ethers such as polyoxyethylene nonylphenyl ether or polyoxyethylene tristyrylphenyl ether; polyoxyethylene fatty acid esters such as polyoxyethylene monolaurate, polyoxyethylene distearate or polyoxyethylene resin acid ester; polyoxyethylene polyoxypropylene block copolymers; polyoxyethylene polyoxypropylene alkyl ether such as polyoxyethylene polyoxypropylene lauryl ether; polyoxyethylene polyoxypropylene aryl ether such as polyoxyethylene polyoxypropylene styrylphenyl ether; polyoxyethylene alkyl amines such as polyoxyethylene stearyl amine; polyoxyethylene fatty acid amide such as lauric acid diethanolamid; fluorinated surfactant; alkyl sulfates such as sodium lauryl sulfate, sodium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates such as sodium polyoxyethylene lauryl ether sulfate; polyoxyethylene aryl ether sulfates such as sodium polyoxyethylene nonylphenyl ether sulfate or ammonium polyoxyethylene tristyrylphenyl ether sulfate; blend of alkyl sulphate and ethoxylates sulphate salt; amine salt of phosphate tristyryl phenol ethylated; aryl sulfonate such as calcium dodecyl benzene sulfonate, sodium naphthalene sulfonate or sodium naphthalene sulfonate formaldehyde condensate; ‘alpha’-olefin sulfonate; maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9); salt of naphthalene sulphonic acid condensation product; phenol sulphonic acid condensation product; alkyl sulfosuccinate such as sodium dioctyl sulfosuccinate; lignin sulfonate such as sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; ethoxylated polyarylphenol phosphate ester, polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates such as polyoxyethylene phenyl ether phosphate or polyoxyethylene nonylphenyl ether phosphate; polyoxyethylene polyoxypropylene block copolymer phosphate; olefin-copolymer, sodium salt; graft copolymer such as polymethyl methacrylate-polyethylene glycol graft copolymer. These surfactants may be used alone or in combination thereof.

In another embodiment of the present invention, the dispersing agent may be selected from the group comprising ‘alpha’-olefin sulfonate; maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9); salt of naphthalene sulphonic acid condensation product; phenol sulphonic acid condensation product; sodium dioctyl sulfosuccinate; sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; ethoxylated polyarylphenol phosphate ester, polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates; polyoxyethylene polyoxypropylene block copolymer phosphate; olefin-copolymer, sodium salt; and/or graft copolymer or combinations thereof.

In another preferred embodiment of the present invention, the dispersing agent is maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9), present in an amount in the range of 5 to 9% by weight of the composition.

In another embodiment of the present invention, the wetting agent may be selected from the group comprising sugar esters; alkyl polyglucoside; polyoxyethylene alkyl ethers; polyoxyethylene alkynyl ether; polyoxyethylene aryl ethers; polyoxyethylene fatty acid esters; polyoxyethylene polyoxypropylene block copolymers; polyoxyethylene polyoxypropylene alkyl ether; polyoxyethylene polyoxypropylene aryl ether; polyoxyethylene alkyl amines; polyoxyethylene fatty acid amide; sodium lauryl sulfate; sodium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates; polyoxyethylene aryl ether sulfates; blend of alkyl sulphate and ethoxylates sulphate salt; amine salt of phosphate tristyryl phenol ethylated; calcium dodecyl benzene sulfonate; sodium naphthalene sulfonate or sodium naphthalene sulfonate formaldehyde condensate or combinations thereof.

In another preferred embodiment of the present invention, the wetting agent is salt of naphthalene sulphonic acid condensation product, present in an amount in the range of 0.1 to 4% by weight of the composition.

Defoaming agent(s) / defoamer(s) / antifoaming agent(s) / antifoamer(s) may be selected from the group comprising of, but not limited to, silicone compounds such as polysiloxane, polydimethyl siloxane and organic fluorine compounds. These defoaming agent(s) / defoamer(s) / antifoaming agent(s) / antifoamer(s) may be used alone or in combination thereof.

In another preferred embodiment of the present invention, the defoamer is silicone compounds present in an amount in the range of 0.1 to 2.5% by weight of the composition.

Penetrant(s) increase the efficacy of pesticides by helping them reach the target site, improving the overall performance of the formulation. Examples include esterified and/or etherified polyol alkoxylates, aliphatic sulfones, acyclic sulfones, sulfones, sulfoxides, biosurfactants, glycolipids, lipopeptides, cocoamine propyl amide and dimethyl sulfoxide (DMSO) or combinations thereof.

In another preferred embodiment of the present invention, the penetrant is cocoamine propyl amide, present in an amount in the range of 0.1 to 2.5% by weight of the composition.

The carrier(s) may be solid or liquid carrier(s). Solid carriers(s) or filler(s) may be selected from the group comprising of, but not limited to, natural minerals such as quartz, talc, kaolin, pyrophyllite, montmorillonite, attapulgite, bentonite, kieselguhr, chalk, zeolite, calcite, sericite, acid clay, diatomaceous earth, natural rock, Fuller’s earth, meerschaum, gibbsite, dolomite or pumice; synthetic minerals such as precipitated silica, fumed silica, sodium silicate, alumina, aluminium hydroxide; inorganic salts such as calcium carbonate, ammonium sulfate or other ammonium salts, sodium sulfate, potassium chloride; organic materials such as urea, solid polyoxyethylene, solid polyoxypropylene, polyethylene, polypropylene, citric acid (2-hydroxypropane-1,2,3-tricarboxylic acid), trisodium citrate (Trisodium 2-hydroxypropane-1,2,3-tricarboxylate), lactose (4-O-beta-D-Galactopyranosyl-D-glucose), starch, lignin, cellulose, cottonseeds hulls, wheat flour, soybean flour, wood flour, walnut shell flour, plant powders, sawdust, coconut shellflower, corn cob, tobacco stem. These solid carriers may be used alone or in combination thereof.

Liquid carrier(s) is selected from the group comprising of, but not limited to, water; alcohols such as ethanol, propanol, n-octanol, isopropanol ethylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, glycerine; polyol ethers such as ethylene glycol monopropyl ether, diethylene glycol monomethyl ether, dipropylene glycol dimethyl ether; ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone; ethers such as dipropyl ether, dioxane, tetrahydrofuran; aliphatic hydrocarbons such as normal paraffin, isoparaffin, kerosene, mineral oil; aromatic hydrocarbons such as xylene, toluene, naphthalene, solvent naphtha, solvent C9, solvent C10, solvent C12, solvesso 100, solvesso 150, solvesso 200; chlorinated aliphatic or aromatic hydrocarbons such as chlorobenzene, chloroethylene, methylene chloride; esters such as ethyl acetate, diisopropyl phthalate, dimethyl adipate, methyl oleate, methyl tallowate; lactones such as gamma-butyrolactone; amides such as dimethylformamide, N-methyl-2-pyrrolidone, N-octylpyrolidone, N,N-dimethyldecanamide; nitriles such as acetonitrile; organosulfur compound such as dimethyl sulfoxide. These liquid carriers may be used alone or in combination thereof.
In another preferred embodiment of the present invention, the carrier is selected from citric acid, trisodium citrate and/or 4-O-beta-D-Galactopyranosyl-D-glucose or combinations thereof.

In one exemplary embodiment of the present invention, the carrier may be present in the “Quantum Satis” i.e., Q.S quantity.

In an exemplary embodiment, the formulation comprises N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, anionic surfactants, carriers and defoamers.

In another preferred embodiment, the formulation comprises N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9), salt of naphthalene sulfonic acid condensation product, citric acid, trisodium citrate, 4-O-beta-D-galactopyranosyl-D-glucose, and polydimethylsiloxane.

In another preferred embodiment, the formulation comprises N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9), salt of naphthalene sulfonic acid condensation product, cocoamine propyl amide, citric acid, trisodium citrate, 4-O-beta-D-galactopyranosyl-D-glucose, and polydimethylsiloxane.

In another embodiment, the soluble granule formulation of the present invention has improved solubility and bioavailability.

In another embodiment, the soluble granule formulation of the present invention possesses enhanced bioefficacy.

In another embodiment, the soluble granule formulation of the present invention provides a broad spectrum of control over diseases and pests in various agricultural crops.
In another embodiment, the soluble granule formulation of the present invention enhanced crop yield without any phytotoxicity.

The lists of crops which can be protected by the formulation of the present invention are GMO (Genetically Modified Organism) and Non GMO varieties of Cotton (Gossypium spp.), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum), Sugarbeet (Beta vulgaris), Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus) , Onion (Allium cepa L.), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Sweet potato (Ipomoea batatas), Chilli (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus), Muskmelons (Cucumis melo), Watermelon (Citrullus lanatus), Bottle gourd (Lagenaria siceraria), Bitter gourd (Momordica charantia), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica rapa subsp rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punica granatum), Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Fenugreek (Trigonella foenumgraecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), Mentha (Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold ( Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis), Gerbera (Gerbera jamesonii), Carnation (Dianthus caryophyllus).

The formulation of the present invention can be used to control the insects from the order of the Lepidoptera, for example cutworm Agrotis ypsilon, sugarcane shoot borer Chilo infuscatellus, sugarcane stalk borer Chilo partellus, sugarcane internode borer Chilo sacchariphagus, paddy/rice stem borer, Chilo suppressalis, rice leaffolder Cnaphalocrocis medinalis, apple colding moth Cydia pomonella, okra fruit borer Earias vittella, Earias insulana, Tomato fruit borer Helicoverpa armigera, tobacco budworm Helicoverpa virescens, corn earworm Helicoverpa zea, cabbage webworm Hellula undalis, Brinjal fruit and shoot borer Leucinodes orbonalis, bean pod borer Maruca vitrata, Maruca testulalis, armyworm Mythimna separata, cotton pinkbollworm Pectinophora gossypiella, citrus leafminer Phyllocnistis citrella, cabbage butterfly Pieris bras-sicae, diamond backmoth Plutella xylostella, paddy stem borer Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata, wheat stem borer Sesamia inferens, Sitotroga cerealella, Spilosoma obliqua, Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Trichoplusia ni, Tryporyza novella, Tuta absoluta.

Beetles (Coleoptera), for example Anthonomus grandis, Bruchus lentis, Diabrotica semipunctata, Diabrotica virgifera, Dicladispa armigera, Epila-chna varivestis, Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotreta chrysocephala, Popillia japonica.
Flies, mosquitoes (Diptera), e.g. Atherigona orientalis, Calliphora vicina, Dacus cucurbi-tae, Liriomyza trifolii, Melanagromyza obtuse.

Thrips (Thysanoptera), e.g. Dichromothrips ssp, Frankliniella occidentalis, Scirtothrips citri, Scirtothrips dorsalis, Thrips oryzae, Thrips palmi and Thrips tabaci.

Termites (Isoptera), e.g. Calotermes flavicollis, Coptotermes formosanus, Heterotermes aureus, Leucotermes flavipes, Microtermes obesi, Odontotermes obesus, Reticulitermes flavipes, Termes natalensis.

True bugs (Hemiptera), e.g. Cotton leafhopper Amrasca biguttula biguttula, Amrasca devastans, Mango hopper Amritodus atkinsoni, Idioscopus spp., cotton aphid Aphis gossypii, groundnut aphid Aphis crassivora, whitefly Bemisia argentifolii, Bemisia tabaci, cabbage aphid Brevicoryne brassicae, red gram bug Clavigralla gibbosa, leaf hopper Empoasca fabae, Lygus pratensis, Macrosiphum avenae, Myzus persicae, Nilaparvata lugens (brown planthopper), Nephotettix virescens, Nephotettix nigropictus, Planococcus spp., Pseudococcus spp., Pyrilla perpusilla, Rhopalosiphum maidis, Saccharicoccus sacchari, Sitobion avenae, Sogatella furcifera (Whitebacked plant- hopper), Cicadella viridis (green leaf hopper), Trialeurodes vaporariorum, Toxoptera aurantiia, Psylla spp., Rhopalosiphum spp.

Arachnoidea, such as arachnids (Acarina/ plant mites), e.g. of the families Argasidae, Ixodidae and Sarcoptidae, such as Amblyomma variegatum, Ambryomma maculatum, Boophilus microplus, Eriophyidae spp. such as Aculus schlechtendali, Phyllocoptrata oleivora and Eriophyes sheldoni; Tarsonemidae spp. such as Phytonemus pallidus and Polyphagotarsonemus latus; Tenuipalpidae spp. such as Brevipalpus phoenicis; Tetra-nychidae spp. such as Tetranychus cinnabarinus, Tetranychus kanzawai, Tetranychus pacificus, Tetranychus telarius and Tetranychus urticae, Panonychus ulmi, Panony-chus citri, and Oligonychus pratensis; Araneida, e.g. Latrodectus mactans, and Loxos-celes reclusa.

The present invention is further described in light of the following experiments which are set forth for illustration purposes only and not to be construed for limiting the scope of the invention. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.

EXAMPLES
The examples below are given solely for the purpose of illustration and are not to be construed as limitations of the present invention, as many variations thereof are possible without departing from the spirit and scope of the invention.

Example 1: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (50%) SG Formulation

Table 1: Soluble Granule (SG) formulation of 50% N-(cyanomethyl)-4-(tri fluoro methyl) pyridine-3-carboxamide

S. No. Ingredients Function Quantity in % W/W CAS No.
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Technical Active Ingredient 10 – 55 158062-67-0
2 Maleic acid, polymer with diisobutene, sodium salt Dispersing Agent 5 - 9 37199-81-8
3 Salt of Naphthalene Sulphonic Acid condensation product. Wetting Agent 0.1 - 4 NA
4 Cocoamine Propyl Amide Penetrant 0.1 - 2 68140-01-2
5 Citric Acid Carrier 0.1 - 1.0 77-92-9
6 Trisodium citrate Carrier 8 - 12 6132-04-3
7 4-O-beta-D-Galactopyranosyl-D-glucose Carrier QS 64044-51-5
8 Polydimethylsiloxane Defoamer 0.1 - 3 9016-00-6

Process for preparation of the formulation: The formulation was prepared by weighing the required quantities of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (technical grade), dispersing agent, wetting agent, and defoamer. These components were then combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The resulting mixture was subsequently subjected to milling using a Jet Mill to achieve the desired particle size distribution. A representative, homogeneous sample was drawn from the milled mixture for quality control (QC) analysis. Upon confirmation that the sample met quality standards, penetrant and the requisite volume of demineralized (DM) water were added to the mixture to form a dough-like mass. This dough was then subjected to granulation using an extruder, resulting in the formation of granules. The obtained granules were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Example 2: Preparation process of Soluble Granule (SG) formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (50%)

Table 2: Ingredients used for preparation of Soluble Granule (SG) formulation
S. No. Ingredients Function Quantity for 1000 kg
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech (96% Purity) Active Ingredient 531.25
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 70.00
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 20.00
4 Cocoamine Propyl Amide
(Ethomeen C/25) Penetrant 10.00
5 Tri-sodium citrate Carrier 100.00
6 Citric Acid Carrier 10.00
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier 253.75
8 Polydimethylsiloxane
(Sag 1572/AFE 3101) Defoamer 5.00

Process for preparation of the formulation: Weighed accurately the required amount of lactose, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Technical, Sokalan CP 9, Tamol FBP-1, Trisodium citrate and Citric acid in a pre-blender and mixed to obtain a mixture. The mixture was milled with the help of a Jet Mill. Next, a homogeneous sample was drawn from the milled mixture for QC analysis. After the conformation of quality, a dough was made by adding Ethomeen C/25 and required amount of demineralized (DM) water to the mixture. Further, granulation of the mixture was done using an extruder to obtain granules. Next, the granules were dried via Fluid bed dryer (FBD) to obtain final product. The final sample was drawn for QC analysis and the finished product was packed after conformation of quality.

Table 3: Quality Control (QC) Analysis of Physiochemical Properties
S. No. Test Parameters Specifications Refer BIS/ISO
Spec. no./other
1 Description The material shall be in the form of light brown colour free flowing granules. Naked eye observation under natural light
2 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Content (% by mass) 48.50 – 52.50 In house method
3 pH (of 1.0% Aq. Solution) 6.0 to 9.0 CIPAC MT 75.3
4 Persistent Foaming (of 1.0% solution in 342 ppm Hard Water) 50.0 ml CIPAC MT 47.3
5 Wet sieve test passes through IS 45µ sieve 99.0 % Min. IS 6940: 1982
6 Solubility (of 1.0 % in 342 ppm Hard Water) Material shall be completely soluble CIPAC MT 157

Quality assessments were carried out on the prepared formulation. The formulation complied with all required specification. As evident from above Table 3, the formulation exhibited a light brown coloration and consisted of freely flowing granules. When dissolved in water to prepare a 1% aqueous solution, the pH of the formulation was found to be within the range of 6.0 to 9.0. Furthermore, the formulation demonstrated complete solubility in water, indicating the absence of any insoluble residue.

Stability evaluations were subsequently performed to assess the robustness of the formulation under defined storage and testing conditions. The data obtained from these studies confirmed that the formulation retained its physical and chemical stability throughout the duration of the testing period. Notably, the enhanced solubility and stability observed are attributable to the synergistic effect of the specific combination of dispersing agent, wetting agent, and penetrant incorporated into the formulation. Thus, it is evident that the formulation not only meets the requisite quality parameters but also demonstrates improved solubility and stability characteristics, thereby affirming its suitability and efficacy for the intended application.

Example 3: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (50%) SG Formulation

Table 4: Soluble Granule (SG) formulation of 50% N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Technical Active Ingredient 50.0
2 Maleic acid, polymer with diisobutene, sodium salt Dispersing Agent 7.0
3 Salt of Naphthalene Sulphonic Acid condensation product. Wetting Agent 2.0
4 Cocoamine Propyl Amide Penetrant 1.0
5 Citric Acid Carrier 1.0
6 Trisodium citrate Carrier 10.0
7 4-O-beta-D-Galactopyranosyl-D-glucose Carrier QS
8 Polydimethylsiloxane Defoamer 0.5

Process for preparation of the formulation: Weighed the required amount of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Technical, dispersing agent, wetting agent and defoamer in a pre-blender and mixed to obtain a mixture. The mixture was milled with the help of a Jet Mill. Next, a homogeneous sample was drawn from the milled mixture for QC analysis. After the conformation of quality, a dough was made by adding penetrant and required amount of demineralized (DM) water to the mixture. Further, granulation of the mixture was done using an extruder to obtain granules. Next, the granules were dried via Fluid bed dryer (FBD) to obtain soluble granule formulation.

Table 5: Storage Stability Data
S. No. Test Parameters Result
At Room Temp. At High Storage Temp (After 14 days)
1 Description Light brown colour granules Light brown colour granules
2 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide
content (% by mass) 50.12 50.26
3 1% aq. pH 7.19 7.23
4 Number of Inversion 22 23
5 Solubility test Completely soluble Completely soluble
6 Bulk density 0.5233 NA

As seen in Tables 4 and 5, a soluble granule (SG) formulation comprising 50% (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) was developed and characterized. The resulting formulation, as detailed in Table 5, was obtained as light-brown-coloured granules. When dispersed in water to form a 1% aqueous solution, the formulation exhibited a pH in the range of 6.0 to 9.0. The formulation demonstrated high solubility in water, yielding a homogeneous solution without observable insoluble matter. In addition, the formulation exhibited excellent storage stability, maintaining its physicochemical properties and meeting all specified quality parameters after prolonged storage at room temperature, as well as after 14 days at elevated temperature. The enhanced stability of the formulation is attributed to the inclusion of a dispersing agent, a wetting agent, and a penetrant at optimized concentrations within the composition.

Example 4: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation at varying concentration of surfactants and penetrant.

Example 4(a):

Table 6: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation with low concentration of dispersing agent and high concentration of penetrant
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 51
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 4
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 3
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The formulation was prepared by weighing the required amounts of carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform mixture. This mixture was then subjected to milling using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was withdrawn from the milled mixture and subjected to quality control (QC) analysis. Upon confirmation that the sample met quality requirements, the penetrant and the necessary quantity of demineralized (DM) water were added to form a dough-like mass. The resulting mixture was subsequently granulated using an extruder to obtain granules. Finally, the granules were dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 7: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules not free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 48.50 – 52.50 50.12
3 1% aq. pH 5.0 to 9.0 7.16
4 Number of Inversion 30 No. Max. 35
5 Solubility test Completely soluble Not soluble

The formulation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG, as illustrated in Tables 5 and 6, was prepared with a reduced concentration of dispersing agent and an elevated concentration of penetrant, diverging from the previously specified compositional range. As a result of this modification, the obtained product was in the form of brown-coloured granules that did not possess the desired free-flowing characteristics and exhibited poor solubility in water, as reflected in the results presented in Table 6. The formulation failed to pass the solubility test and did not meet the required descriptive standards. These findings demonstrate that increasing the concentration of the penetrant while decreasing the concentration of the dispersing agent results in a formulation that does not meet the necessary quality specifications.

Example 4(b):
Table 8: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation with high concentration of both dispersing agent and penetrant
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 51
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 10
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 5
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The formulation process commenced with the weighing of the required amounts of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform mixture. The resulting mixture was subsequently milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was drawn from the milled mixture and subjected to quality control (QC) analysis. Upon confirmation that the quality parameters were met, the penetrant and the requisite quantity of demineralized (DM) water were added to the mixture to form a dough-like mass. This mass was then granulated using an extruder to produce granules, which were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 9: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules not free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 48.50 – 52.50 50.12
3 1% aq. pH 5.0 to 9.0 7.22
4 Number of Inversion 30 No. Max. 17
5 Solubility test Completely soluble Completely soluble

The N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation described in Tables 8 and 9 was prepared with elevated concentrations of both dispersing agent and penetrant, diverging from the specified compositional range. As a consequence of these adjustments, the resulting granules were brown in colour, lacked the desired free-flowing characteristics, and demonstrated poor solubility in water, as detailed in Table 9. The formulation failed the solubility test and did not meet the descriptive requirements. These results indicate that increasing the concentrations of both the dispersing agent and penetrant adversely affects the physical properties and solubility of the formulation, rendering it non-compliant with the required specifications.

Example 4(c):

Table 10: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation with low concentration of dispersing agent and high concentration of wetting agent
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 51
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 5
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 5
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 1
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The process for preparing the formulation involved accurately weighing the required quantities of the carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform mixture. The resulting mixture was then subjected to milling using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was drawn from the milled mixture and analyzed for quality control (QC) parameters. Upon confirmation that the sample met the requisite quality standards, the penetrant and the required amount of demineralized (DM) water were added to the mixture to form a dough-like mass. This mass was subsequently granulated using an extruder to produce granules. The granules were then dried using a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 11: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 48.50 – 52.50 50.20
3 1% aq. pH 5.0 to 9.0 7.22
4 Number of Inversion 30 No. Max. 30
5 Solubility test Completely soluble Not soluble

The (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 50% SG formulation, as described in Tables 10 and 11, was prepared using a higher concentration of wetting agent and a lower concentration of dispersing agent than the specified composition. As a result of these modifications, the formulation yielded brown-coloured granules that demonstrated poor solubility in water, as shown in Table 11. Consequently, the formulation failed to meet the required quality specifications and did not pass the solubility test. These results indicate that increasing the amount of wetting agent while decreasing the dispersing agent has an adverse effect on the solubility and overall performance of the formulation.
Example 5: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation at high concentration of active content.

Example 5(a):

Table 12: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 65% SG Formulation
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 66
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 1
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The preparation of the formulation commenced with the weighing of the required amounts of carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) technical grade, dispersing agent, wetting agent, and defoamer. These ingredients were combined in a pre-blender and thoroughly mixed to obtain a uniform mixture. This mixture was subsequently milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was then drawn from the milled mixture for quality control (QC) analysis. Upon confirmation of compliance with quality standards, the penetrant and the requisite quantity of demineralized (DM) water were added to the mixture to form a dough-like mass. The resulting dough was then granulated using an extruder to produce granules, which were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 13: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 63.05 – 68.25 65.11
3 1% aq. pH 5.0 to 9.0 7.96
4 Number of Inversion 30 No. Max. 36
5 Solubility test Completely soluble Not soluble

The N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 65% SG formulation, as presented in Tables 12 and 13, was prepared with an increased concentration of the active ingredient, thereby deviating from the specified compositional range. As a result of this modification, the formulation yielded brown-coloured granules that demonstrated poor solubility in water, as indicated in Table 13. Consequently, the formulation failed to meet the required quality specifications and did not pass the solubility test. These results indicate that a higher concentration of the active content has an adverse effect on the solubility and overall suitability of the formulation.

Example 5(b):

Table 14: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 90% SG Formulation
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 91
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 3
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 0.5
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 0.5
5 Citric Acid Carrier 0.2
6 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
7 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The process for preparing the formulation began with the weighing of the required amounts of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform mixture. The resulting mixture was then milled using a Jet Mill to achieve the desired particle size. A homogeneous sample was withdrawn from the milled mixture and subjected to quality control (QC) analysis. Upon confirmation that the quality parameters were met, the penetrant and the requisite quantity of demineralized (DM) water were added to the mixture to form a dough-like mass. This mass was then granulated using an extruder to produce granules, which were subsequently dried using a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 15: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 87.30 – 94.50 90.24
3 1% aq. pH 5.0 to 9.0 8.03
4 Number of Inversion 30 No. Max. 46
5 Solubility test Completely soluble Not soluble

The N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 90% SG formulation, as described in Tables 14 and 15, was prepared with a significantly increased concentration of active ingredient, thereby deviating from the specified compositional range. As a result of this modification, the formulation produced brown-coloured granules that exhibited poor solubility in water, as indicated by the data presented in Table 15. Consequently, the formulation failed to meet the required quality specifications and did not pass the solubility test. These findings indicate that an excessively high concentration of active content adversely impacts the solubility and overall acceptability of the formulation.

Example 6: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation at low concentration of active content.

Example 6(a):

Table 16: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 35% SG Formulation
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 36
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 1
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The preparation of the formulation commenced with the accurate weighing of the required amounts of carrier (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide), technical grade; dispersing agent; wetting agent; and defoamer. These ingredients were combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The resulting mixture was then subjected to milling using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was drawn from the milled mixture and analyzed for quality control (QC) to confirm compliance with the required standards. Upon confirmation of quality, the penetrant and the requisite quantity of demineralized (DM) water were added to the mixture to form a dough-like mass. This mass was subsequently granulated using an extruder to produce granules, which were then dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 17: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 33.25 – 36.75 35.19
3 1% aq. pH 5.0 to 9.0 7.65
4 Number of Inversion 30 No. Max. 20
5 Solubility test Completely soluble Completely soluble

Observation: The formulation successfully passed all conducted tests, meeting the required quality parameters and specifications.

Example 6(b):

Table 18: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 10% SG Formulation
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 11
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Cocoamine Propyl Amide (Ethomeen C/25) Penetrant 1
5 Tri-sodium citrate Carrier 10
6 Citric Acid Carrier 1
7 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
8 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The process for preparing the formulation began with the accurate weighing of the required amounts of carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The resulting mixture was subsequently milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was then withdrawn from the milled mixture and subjected to quality control (QC) analysis. Upon confirmation that the mixture met the specified quality parameters, the penetrant and the requisite quantity of demineralized (DM) water were added to form a dough-like mass. This mass was then granulated using an extruder to produce granules, which were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.
Table 19: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 9.50 – 10.50 10.16
3 1% aq. pH 5.0 to 9.0 7.52
4 Number of Inversion 30 No. Max. 20
5 Solubility test Completely soluble Completely soluble

Observation: The formulation passed in all parameters.

Example 7: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (50%) SG Formulation without Penetrant

Table 19: Soluble Granule (SG) formulation of 50% N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide without Penetrant

S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 51
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Tri-sodium citrate Carrier 10
5 Citric Acid Carrier 1
6 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
7 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The preparation of the formulation commenced with the accurate weighing of the required amounts of carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) technical grade, dispersing agent, wetting agent, and defoamer. These ingredients were combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The resulting mixture was then milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was withdrawn from the milled mixture and subjected to quality control (QC) analysis. Upon confirmation of compliance with quality standards, a dough was prepared, and the mixture was subsequently granulated using an extruder to obtain granules. The granules were then dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 21: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 48.50 – 52.50 50.18
3 1% aq. pH 5.0 to 9.0 7.41
4 Number of Inversion 30 No. Max. 25
5 Solubility test Completely soluble Completely soluble

As disclosed in Tables 20 and 21, a (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 50% SG formulation was prepared without the inclusion of a penetrant. The resulting formulation, as detailed in Table 21, comprised light brown-coloured granules exhibiting a pH range of 5.0 to 9.0 in a 1% aqueous solution. The formulation demonstrated high solubility in water, yielding a homogeneous solution. This favourable solubility profile was achieved by incorporating a dispersing agent and a wetting agent at specific concentrations within the composition. Accordingly, the overall performance of the formulation is considered acceptable.

Example 8: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (without penetrant) at high concentration of active content.
Example 8(a):

Table 22: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 65% SG Formulation (without penetrant)

S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 66
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Tri-sodium citrate Carrier 10
5 Citric Acid Carrier 1
6 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
7 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The process for preparing the formulation commenced with the accurate weighing of the required quantities of carrier, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) technical grade, dispersing agent, wetting agent, and defoamer. These ingredients were combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The mixture was then milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was withdrawn from the milled mixture for quality control (QC) analysis. Upon confirmation of compliance with quality parameters, a dough was prepared, and the mixture was granulated using an extruder to obtain granules. These granules were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 23: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 63.05 – 68.25 65.12
3 1% aq. pH 5.0 to 9.0 7.63
4 Number of Inversion 30 No. Max. 40
5 Solubility test Completely soluble Not soluble

The (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 65% SG formulation without penetrant, as described in Tables 22 and 23, was prepared with an increased concentration of active ingredient, deviating from the specified composition. As a result of this modification, the formulation produced brown-coloured granules that demonstrated poor solubility in water, as evidenced by the data presented in Table 23. Consequently, the formulation failed the solubility test. It did not meet the required quality specifications, indicating that a higher concentration of active content, in the absence of a penetrant, adversely affects the solubility and overall suitability of the formulation.

Example 8(b):

Table 24: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 90% SG Formulation (without penetrant)
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 91
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 3
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 0.5
4 Citric Acid Carrier 0.2
5 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
6 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The preparation of the formulation began with the accurate weighing of the required quantities of carrier N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide), technical grade; dispersing agent; wetting agent; and defoamer. These components were combined in a pre-blender and thoroughly mixed to obtain a uniform blend. The mixture was then milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was subsequently withdrawn from the milled mixture for quality control (QC) analysis. Upon confirmation that the quality parameters were met, a dough was prepared, and the mixture was granulated using an extruder to form granules. The resulting granules were then dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 25: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 87.30 – 94.50 90.19
3 1% aq. pH 5.0 to 9.0 7.58
4 Number of Inversion 30 No. Max. 46
5 Solubility test Completely soluble Not soluble

The (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 90% SG formulation without penetrant, as presented in Tables 24 and 25, was prepared with a high concentration of active ingredient, deviating from the specified compositional range. As a result of this modification, the formulation yielded brown-coloured granules that demonstrated poor solubility in water, as indicated by the data in Table 25. Consequently, the formulation failed to meet the required quality specifications and did not pass the solubility test. These results indicate that a high concentration of active content, in the absence of a penetrant, adversely affects the solubility and overall suitability of the formulation.

Example 9: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (without penetrant) at low concentration of active content.

Example 9(a):
Table 26: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 35% SG Formulation (without penetrant)

S. No. Ingredients Function Qunatity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 36
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Tri-sodium citrate Carrier 10
5 Citric Acid Carrier 1
6 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
7 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The formulation process commenced with the accurate weighing of the required amounts of carrier, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide technical grade, dispersing agent, wetting agent, and defoamer. These components were combined in a pre-blender and thoroughly mixed to achieve a uniform blend. The resulting mixture was then milled using a Jet Mill to obtain the desired particle size distribution. A homogeneous sample was withdrawn from the milled mixture for quality control (QC) analysis. Upon confirmation of compliance with quality standards, a dough was prepared, and the mixture was granulated using an extruder to form granules. The granules were subsequently dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 27: Physiochemical Properties of the Formulation
S. No. Test Parameters Specifications Result
1 Description Light brown to brown colour free flowing granules Brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 33.25 – 36.75 35.21
3 1% aq. pH 5.0 to 9.0 7.51
4 Number of Inversion 30 No. Max. 27
5 Solubility test Completely soluble completely soluble

Observation: Formulation passed in all test.
Example 9(b):

Table 28: N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 10% SG Formulation (without penetrant)
S. No. Ingredients Function Quantity in % W/W
1 N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide Tech Active Ingredient 11
2 Maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9) Dispersing Agent 7
3 Salt of Naphthalene Sulphonic Acid condensation product (Tamol FBP 1) Wetting Agent 2
4 Tri-sodium citrate Carrier 10
5 Citric Acid Carrier 1
6 4-O-beta-D-Galactopyranosyl-D-glucose (Lactose) Carrier QS
7 Polydimethylsiloxane (Sag 1572/AFE 3101) Defoamer 0.5
Total Batch size kg 100

The required quantities of carrier N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, technical grade, dispersing agent, wetting agent, and defoamer were accurately weighed and combined in a pre-blender, then thoroughly mixed to obtain a uniform blend. The resulting mixture was milled using a Jet Mill to achieve the desired particle size distribution. A homogeneous sample was withdrawn from the milled mixture for quality control (QC) analysis. Upon confirmation of quality, a dough was prepared, and the mixture was granulated using an extruder to form granules. The granules were then dried in a fluid bed dryer (FBD) to yield the final soluble granule formulation.

Table 29: Physiochemical Properties of the Formulation
S. No. Test Specifications Result
1 Description Light brown to brown colour free flowing granules Light brown colour granules free flowing
2 N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide content
(% by mass) 9.50 – 10.50 10.14
3 1% aq. pH 5.0 to 9.0 7.33
4 Number of Inversion 30 No. Max. 24
5 Solubility test Completely soluble Completely soluble

Observation: The formulation passed in all parameters.

Example 10: Evaluation of Bio-efficacy and Phytotoxicity Study of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG formulation (with and without penetrant) against Aphids, Jassids, Thrips & Whiteflies in Chilli crop.

TRIAL 1: Laboratory Experimental Details
Season Rabi (2024-25)
Location Mastakatti Village, Koppal District, Karnataka
Crop Chilli
Variety Yashaswini Hybrid Chilli (Mahyco)
Pests under study Aphids- Aphis gossypii
Thrips- Scirtothrips dorsalis/ Thrips tabaci
Whitefly- Bemisia tabaci
Jassids- Amrasca devastans/ Amrasca bigutulla bigutulla
Chemical Tested N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (F001)
Area Required 1170 sq. m [6m x 5m= 30m2 Per plot]
Plot size 6m x 5m= 30m2
Number of Replication 3
Date of sowing 11/12/2024
Volume of spray fluid 500 L
Number of spray 2
Spray Schedule 1st Spray: 25/12/2024
2nd Spray: 09/01/2025
Date of Harvest 31/03/2025

Table 30: Treatment Details
S. No. Treatment Details Dosage/ha
A.I. (gm) Formulation (gm) Dilution in water (L)
T-1 F001 10% SG without penetrant 20 200 500
T-2 F001 10% SG with penetrant 20 200 500
T-3 F001 35% SG without penetrant 70 200 500
T-4 F001 35% SG with penetrant 70 200 500
T-5 F001 50% SG without penetrant 100 200 500
T-6 F001 50% SG with penetrant 100 200 500
T-7 Std check-N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% WG 100 200 500
T-8 Std check-N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG 100 200 500
T-9 Control - - -
*Note: T-7 & T-8 are commercially available products

Methodology:
The experiment was laid out in randomized block design (RBD), replicating thrice with a single plot area of 6 x 5 m2.
The required quantity of the insecticide was dissolved in 500 litres of water per hectare and applied uniformly using a knapsack sprayer at the first appearance of insect pests to ensure complete canopy coverage.
Observations for Aphids, Jassids, Thrips, and Whiteflies populations were recorded a day prior to the first spray application. Post-treatment pest counts were taken on the 3rd, 7th, 10th, and 14th days after application.
This observation schedule was repeated following each subsequent round of application. Pest population data were collected from ten randomly tagged plants per plot or replication.

Table 31: RBD Distribution

Replication-1 Replication-2 Replication-3
T-5 T-4 T-7
T-8 T-9 T-3
T-1 T-2 T-9
T-6 T-8 T-5
T-9 T-6 T-2
T-7 T-1 T-6
T-3 T-5 T-8
T-4 T-3 T-4
T-2 T-7 T-1

Observation:
Evaluation was done based on the following observations:
Insect severity on three leaves per plant in ten tagged plants at 3, 7, 10, and 14 days after spray.
Population of Aphids, Jassids, Thrips & Whiteflies before and after each application.
Percent insect control
Bio-effectiveness of insecticide doses
Fruiting body Damage (%): Total number of damaged bolls per 15 bolls recorded.

= (Number of damaged bolls)/(Total number of bolls recorded) x 100
Yield: Total yield in quintals per ha.
Effect on Natural enemies: Total number of natural enemies per ten tagged plants.
Phytotoxicity: Number of plant Epinasty, Hyponasty, Necrosis, Vein clearing, wilting per ten tagged plants in a plot. (Ranging from 0: No symptoms of phytotoxicity to 10: Complete death)

Table 32: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on population of Aphids in Chilli crop
Treatment Dose (gai/ha) Number of aphids/ 3 leaves/ plant after first spray ROC Number of aphids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG without Penetrant 20 16.47 15.60 14.73 13.53 12.93 45.51 11.73 10.53 9.33 8.60 73.24
(4.12) (4.01) (3.90) (3.75) (3.67) (3.50) (3.32) (3.14) (3.02)
T2-F001 10% SG with Penetrant 20 16.20 15.13 13.73 12.73 11.93 49.72 11.33 10.13 9.13 8.20 74.48
(4.09) (3.95) (3.77) (3.64) (3.53) (3.44) (3.26) (3.10) (2.95)
T3-F001 35% SG without Penetrant 70 16.40 14.73 13.20 12.13 11.00 53.65 10.20 9.73 8.40 7.80 75.73
(4.11) (3.90) (3.70) (3.55) (3.39) (3.27) (3.20) (2.98) (2.88)
T4-F001 35% SG with Penetrant 70 16.60 14.00 12.80 11.93 10.53 55.62 9.93 8.53 7.73 7.33 77.18
(4.14) (3.81) (3.65) (3.53) (3.32) (3.23) (3.01) (2.87) (2.80)
T5-F001 50% SG without Penetrant 100 16.33 13.80 12.33 11.53 10.13 57.30 9.33 8.00 7.20 6.60 79.46
(4.10) (3.78) (3.58) (3.47) (3.26) (3.14) (2.92) (2.77) (2.66)
T6-F001 50% SG with Penetrant 100 16.67 12.73 10.93 10.00 8.80 62.92 7.93 6.73 5.93 5.20 83.82
(4.14) (3.64) (3.38) (3.24) (3.05) (2.90) (2.69) (2.54) (2.39)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 16.20 14.13 12.73 11.80 10.33 56.46 9.67 8.33 7.53 6.93 78.42
(4.09) (3.83) (3.64) (3.51) (3.29) (3.19) (2.97) (2.83) (2.73)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 16.73 14.40 13.00 12.20 10.80 54.49 9.93 8.73 7.93 7.40 76.97
(4.15) (3.86) (3.67) (3.56) (3.36) (3.23) (3.04) (2.90) (2.81)
T9-Control - 16.80 18.20 20.20 22.13 23.73 25.13 27.27 30.20 32.13
(4.16) (4.32) (4.55) (4.76) (4.92) (5.06) (5.27) (5.54) (5.71)
C.D. NS 0.413 0.531 0.403 0.451 0.58 0.705 0.56 0.476
SE(m) - 0.141 0.181 0.137 0.153 0.197 0.24 0.191 0.162

As shown in Table 32, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations resulted in a significant reduction of aphid populations compared to the untreated control. The inclusion of a penetrant consistently enhanced the efficacy of all formulations and application rates. The most pronounced control was achieved with the 50% SG formulation at 100 g/ha in combination with a penetrant, resulting in the highest reduction in aphid count and a ROC of 83.82% following the second spray. Lower-dose treatments, such as the 10% SG at 20 gai/ha, were less effective, particularly in the absence of a penetrant. Notably, formulations of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide combined with a penetrant consistently outperformed the standard check treatments (50% WG and SG), highlighting the superior efficacy of F001 50% SG with Penetrant, especially when applied in conjunction with a penetrant.

Table 33: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on population of Thrips in Chilli crop
Treatment Dose (gai/ha) Number of thrips/ 3 leaves/ plant after first spray ROC Number of thrips/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG without Penetrant 20 12.53 11.80 11.33 10.73 10.20 50.65 9.60 9.13 8.33 7.40 72.18
(3.61) (3.51) (3.44) (3.35) (3.27) (3.18) (3.10) (2.97) (2.81)
T2-F001 10% SG with Penetrant 20 12.20 11.13 10.40 9.80 9.20 55.48 8.40 7.33 6.80 6.53 75.44
(3.56) (3.41) (3.30) (3.21) (3.11) (2.98) (2.80) (2.70) (2.65)
T3-F001 35% SG without Penetrant 70 13.07 10.93 10.13 9.53 8.80 57.42 8.13 7.73 6.40 5.93 77.69
(3.68) (3.38) (3.26) (3.17) (3.05) (2.94) (2.87) (2.63) (2.54)
T4-F001 35% SG with Penetrant 70 12.40 9.93 9.20 8.40 7.80 62.26 6.73 5.93 5.20 4.60 82.71
(3.59) (3.23) (3.11) (2.98) (2.88) (2.69) (2.54) (2.39) (2.26)
T5-F001 50% SG without Penetrant 100 12.60 9.73 8.93 8.33 7.33 64.52
6.40 5.73 5.00 4.53 82.96
(3.62) (3.20) (3.07) (2.97) (2.80) (2.63) (2.50) (2.35) (2.24)
T6-F001 50% SG with Penetrant 100 12.73 8.80 8.13 7.40 6.20 70.00 5.53 4.93 4.40 4.13 84.46
(3.64) (3.05) (2.94) (2.81) (2.59) (2.46) (2.33) (2.21) (2.15)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 12.60 9.80 9.33 8.53 7.60 63.23 6.80 6.20 5.40 4.73 82.21
(3.62) (3.21) (3.14) (3.01) (2.85) (2.70) (2.59) (2.43) (2.29)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 13.13 10.20 9.73 8.93 7.93 61.61 7.33 6.93 5.80 5.00 81.20
(3.69) (3.27) (3.20) (3.07) (2.90) (2.80) (2.73) (2.51) (2.35)
T9-Control - 12.47 14.20 16.27 18.73 20.67 22.73 23.40 24.40 26.60
(3.60) (3.83) (4.09) (4.39) (4.60) (4.82) (4.89) (4.99) (5.21)
C.D. NS 0.707 0.624 0.598 0.634 0.717 0.62 0.705 0.898
SE(m) - 0.241 0.213 0.204 0.216 0.244 0.211 0.24 0.306

As presented in Table 33, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations demonstrated improved efficacy in reducing thrips populations, with substantial declines observed following treatment. The addition of a penetrant notably enhanced the performance of all tested formulations, mirroring the results seen with aphid control. The most effective control was achieved with the 50% SG formulation at 100 gai/ha combined with a penetrant, resulting in an ROC of 84.46% after the second spray, thereby surpassing both standard check treatments. Overall, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide formulations used in conjunction with a penetrant consistently achieved marked reductions in thrips populations. In contrast, lower doses applied without a penetrant exhibited limited efficacy, underscoring the critical role of both dosage and formulation composition in optimizing pest management outcomes.

Table 34: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on population of Whiteflies in Chilli crop
Treatment Dose (gai/ha) Number of whiteflies/ 3 leaves/ plant after first spray ROC Number of whiteflies/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG without Penetrant 20 10.40 9.93 9.40 8.80 8.53 44.35 7.93 7.40 6.73 6.40 70.46
(3.30) (3.23) (3.15) (3.05) (3.01) (2.90) (2.81) (2.69) (2.63)
T2-F001 10% SG with Penetrant 20 10.27 9.33 8.60 7.93 7.40 51.74 6.93 6.40 6.20 5.80 73.23
(3.28) (3.14) (3.02) (2.90) (2.81) (2.73) (2.63) (2.59) (2.51)
T3-F001 35% SG without Penetrant 70 10.33 9.00 8.40 7.60 7.33 52.17 6.60 6.13 5.93 5.60 74.15
(3.29) (3.08) (2.98) (2.85) (2.80) (2.66) (2.58) (2.54) (2.47)
T4-F001 35% SG with Penetrant 70 11.07 8.40 7.53 6.80 6.40 58.26 5.93 5.60 5.33 4.93 77.23
(3.40) (2.98) (2.83) (2.70) (2.63) (2.54) (2.47) (2.42) (2.33)
T5-F001 50% SG without Penetrant 100 10.20 8.13 7.00 6.20 5.80 62.17 5.53 5.20 5.00 4.73 78.15
(3.27) (2.94) (2.74) (2.59) (2.51) (2.46) (2.39) (2.35) (2.29)
T6-F001 50% SG with Penetrant 100 10.40 7.60 6.80 6.00 5.33 65.22 5.00 4.73 4.33 4.00 81.54
(3.30) (2.85) (2.70) (2.55) (2.42) (2.35) (2.29) (2.20) (2.12)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 10.13 8.53 7.33 6.53 6.20 59.57 5.80 5.53 5.13 4.93 77.23
(3.26) (3.01) (2.80) (2.65) (2.59) (2.51) (2.46) (2.37) (2.33)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 10.27 8.80 7.73 6.93 6.60 56.96 6.13 5.73 5.33 5.20 76.00
(3.28) (3.05) (2.87) (2.73) (2.66) (2.58) (2.50) (2.42) (2.39)
T9-Control - 10.67 12.20 13.67 14.53 15.33 17.40 19.40 20.73 21.67
(3.34) (3.56) (3.76) (3.88) (3.98) (4.23) (4.46) (4.61) (4.71)
C.D. NS 0.611 0.576 0.766 0.591 0.694 0.815 0.714 0.697
SE(m) - 0.208 0.196 0.261 0.201 0.236 0.277 0.243 0.237

As demonstrated in Table 34, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations exhibited high efficacy against whiteflies, with performance further enhanced by the inclusion of a penetrant. The most effective treatment was the 50% SG formulation at 100 gai/ha with penetrant, achieving an ROC of 81.54% following the second spray. Consistent with results observed for aphids and thrips, formulation in combination with a penetrant produced superior control of whitefly populations. The efficacy of the F001 formulations in these top-performing treatments exceeded that of the standard checks, underscoring its potential as a reliable option for integrated whitefly management.

Table 35: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on population of Jassids in Chilli crop
Treatment Dose (gai/ha) Number of jassids/ 3 leaves/ plant after first spray ROC Number of jassids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG without Penetrant 20 8.13 7.80 7.20 6.73 6.33 51.28 5.93 5.40 4.80 4.60 72.18
(2.94) (2.88) (2.77) (2.69) (2.61) (2.54) (2.43) (2.30) (2.26)
T2-F001 10% SG with Penetrant 20 8.27 7.33 6.60 6.13 5.73 55.90 5.20 4.73 4.40 4.20 74.60
(2.96) (2.80) (2.66) (2.58) (2.50) (2.39) (2.29) (2.21) (2.17)
T3-F001 35% SG without Penetrant 70 8.67 6.93 6.53 5.93 5.53 57.44 5.00 4.60 4.33 4.00 75.81
(3.03) (2.73) (2.65) (2.54) (2.46) (2.35) (2.26) (2.20) (2.12)
T4-F001 35% SG with Penetrant 70 8.73 6.33 5.80 5.20 4.80 63.08 4.13 3.93 3.60 3.40 79.44
(3.04) (2.61) (2.51) (2.39) (2.30) (2.15) (2.11) (2.02) (1.97)
T5-F001 50% SG without Penetrant 100 8.33 6.20 5.73 5.13 4.53 65.13 3.80 3.73 3.47 3.20 80.65
(2.97) (2.59) (2.50) (2.37) (2.24) (2.07) (2.06) (1.99) (1.92)
T6-F001 50% SG with Penetrant 100 8.27 5.80 5.00 4.33 4.00 69.23 3.53 3.13 2.80 2.73 83.47
(2.96) (2.51) (2.35) (2.20) (2.12) (2.01) (1.91) (1.82) (1.80)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 8.20 6.40 5.87 5.33 4.93 62.05 4.20 4.00 3.73 3.60 78.23
(2.95) (2.63) (2.52) (2.42) (2.33) (2.17) (2.12) (2.06) (2.02)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 8.33 6.80 6.00 5.73 5.20 60.00 4.60 4.20 3.93 3.93 76.21
(2.97) (2.70) (2.55) (2.50) (2.39) (2.26) (2.17) (2.11) (2.11)
T9-Control - 8.27 9.00 10.27 11.40 13.00 14.60 15.60 16.53 16.53
(2.96) (3.08) (3.28) (3.45) (3.67) (3.89) (4.01) (4.13) (4.13)
C.D. NS 0.683 0.695 0.782 0.745 0.721 0.757 0.682 0.67
SE(m) - 0.233 0.237 0.266 0.254 0.246 0.258 0.232 0.228

As shown in Table 35, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (F001) formulations significantly reduced jassid populations, with the highest efficacy observed for the 50% SG formulation at 100 gai/ha with penetrant, achieving 83.47% control after the second spray. Treatments incorporating a penetrant consistently outperformed those without it, and mid-to high-dose applications (35–50% SG) demonstrated superior effectiveness. Across all evaluated treatments, F001 formulations outperformed the standard checks, underscoring their potential as superior agents for jassid control.

Table 36: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on Natural Enemies in Chilli Crops
Treatment Dose (gai /ha) Number of spiders per Plant Number of coccinellids per Plant
First Spray Second Spray First Spray Second Spray
PTC 3 DAS 7 DAS 7 DAS 10 DAS PTC 3 DAS 7 DAS 7 DAS 10 DAS
T1-F001 10% SG without Penetrant 20 1.27 1.20 1.20 1.07 1.07 1.93 1.87 1.80 1.73 1.73
(1.33) (1.30) (1.30) (1.25) (1.25) (1.56) (1.54) (1.52) (1.49) (1.49)
T2-F001 10% SG with Penetrant 20 1.33 1.27 1.33 1.27 1.20 1.87 1.80 1.80 1.73 1.73
(1.35) (1.33) (1.35) (1.33) (1.30) (1.54) (1.52) (1.52) (1.49) (1.49)
T3-F001 35% SG without Penetrant 70 1.40 1.33 1.27 1.27 1.13 1.87 1.80 1.73 1.67 1.67
(1.38) (1.35) (1.33) (1.33) (1.28) (1.54) (1.52) (1.49) (1.47) (1.47)
T4-F001 35% SG with Penetrant 70 1.40 1.33 1.27 1.20 1.07 2.00 1.93 1.87 1.73 1.67
(1.38) (1.35) (1.33) (1.30) (1.25) (1.58) (1.56) (1.54) (1.49) (1.47)
T5-F001 50% SG without Penetrant 100 1.33 1.27 1.20 1.13 1.13 1.93 1.87 1.73 1.67 1.73
(1.35) (1.33) (1.30) (1.28) (1.28) (1.56) (1.54) (1.49) (1.47) (1.49)
T6-F001 50% SG with Penetrant 100 1.27 1.20 1.13 1.07 1.07 1.87 1.80 1.73 1.60 1.60
(1.33) (1.30) (1.28) (1.25) (1.25) (1.54) (1.52) (1.49) (1.45) (1.45)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 1.33 1.27 1.27 1.20 1.13 1.87 1.73 1.73 1.67 1.67
(1.35) (1.33) (1.33) (1.30) (1.28) (1.54) (1.49) (1.49) (1.47) (1.47)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 1.27 1.20 1.20 1.13 1.00 2.00 1.93 1.87 1.73 1.67
(1.33) (1.30) (1.30) (1.28) (1.22) (1.58) (1.56) (1.54) (1.49) (1.47)
T9-Control - 1.40 1.53 1.67 1.67 1.73 1.93 2.00 2.07 2.13 2.13
(1.38) (1.43) (1.47) (1.47) (1.49) (1.56) (1.58) (1.60) (1.62) (1.62)
C.D. NS NS NS NS NS NS NS NS NS NS
SE(m) - - - - - - - - - -

As indicated in Table 36, the application of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) had minimal impact on populations of natural enemies, i.e., spiders and coccinellids within the chilli ecosystem. Across all doses and formulations, including treatments with and without penetrant, the population levels of these beneficial insects remained relatively stable, with only a slight decline observed compared to the untreated control. Importantly, no statistically significant differences were detected among the various treatments, confirming that F001 is safe for natural enemies and does not disrupt the ecological balance in chilli fields.

Table 37: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) on Chilli Yield
Treatment Dose (gai /ha) Yield
(t/ha) Increase in yield over control (%) Yield Profit Common cost Cost per Insecticide Cost per treatment Net Return Total Cost Cost benefit Ratio


T1-F001 10% SG without Penetrant 20 3.23 36.62 53,350.00 16,000.00 153.636 599.18 36750.82 16599.18 2.21
(1.93)
T2-F001 10% SG with Penetrant 20 3.27 38.03 53,900.00 16,000.00 153.98 600.52 37299.48 16600.52 2.25
(1.94)
T3-F001 35% SG without Penetrant 70 3.65 54.23 60,225.00 16,000.00 424.316 1654.83 42570.17 17654.83 2.41
(2.04)
T4-F001 35% SG with Penetrant 70 3.83 61.97 63,250.00 16,000.00 424.66 1656.17 45593.83 17656.17 2.58
(2.08)
T5-F001 50% SG without Penetrant 100 3.98 68.31 65,725.00 16,000.00 586.724 2288.22 47436.78 18288.22 2.59
(2.12)
T6-F001 50% SG with Penetrant 100 4.20 77.46 69,300.00 16,000.00 587.068 2289.57 51010.43 18289.57 2.79
(2.15)
(2.27)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 3.82 61.41 63,030.00 16,000.00 1704 1704 45326.00 17704.00 2.56
(2.08)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 3.60 52.11 59,400.00 16,000.00 398.836 1555.46 41844.54 17555.46 2.38
(2.02)
T9-Control - 2.37 39,050.00 16,000.00 - - 23050.00 16000.00 1.44
(1.69)
C.D. 0.168
SE(m) 0.057
As shown in Table 37, the evaluation of various formulations and doses of F001 on chilli yield demonstrated that the 50% SG formulation at 100 gai/ha was the most effective, particularly when applied with a penetrant (T6), resulting in the highest yield of 4.20 t/ha and an 77.46% increase over the untreated control. Overall, the 35% and 50% SG formulations (T3–T6) significantly outperformed other doses, with yield increases ranging from 54.23% to 77.46%. In contrast, lower doses, such as the 10% SG formulations (T1 and T2), were less effective, resulting in yield gains of between 36.62% and 38.03%. Compared to the standard check treatments (50% WG and SG), which produced yield increases of 61.41% and 52.11%, respectively. The untreated control recorded the lowest yield at 2.37 t/ha, highlighting the substantial benefit of F001 applications in enhancing chilli productivity.

Analysis across multiple datasets demonstrates that the inclusion of a penetrant significantly enhances both the efficacy and economic viability of F001 insecticide formulations, particularly when applied at optimal doses. Among all treatments evaluated, F001 50% SG with penetrant at 100 g/ha consistently achieved the highest cost-benefit ratio (2.79) and the greatest net return, reflecting superior profitability. Other formulations, such as F001 35% SG with penetrant, also showed significant improvements in yield and cost efficiency compared to their counterparts without penetrant. In every case, treatments incorporating penetrant outperformed both the untreated control and the standard check treatments N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% WG/SG), confirming that the penetrant additive substantially contributes to improved pest control and overall plant performance. Therefore, F001 50% SG with penetrant at 100 g/ha is identified as the most economically effective option among all treatments tested.

Table 38: Evaluation of Phytotoxicity of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (with and without penetrant) in Chilli crop

Visual observations were recorded on 1, 3, 5, 7, and 10 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below.

Score Phytotoxicity (percent) Score Phytotoxicity (percent)
0 No phytotoxicity 5 41-50
1 1-10 6 51-60
2 11-20 7 61-70
3 21-30 8 71-80
4 31-40 9 & 10 Complete Destruction

Table 39: Phytotoxic effect of various treatments on Chilli crop
Treatment Dose (g /ha) First Spray Second Spray
1 DAS 3 DAS 5 DAS 7 DAS 10 DAS 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
T1-F001 10% SG without Penetrant 20 0 0 0 0 0 0 0 0 0 0
T2-F001 10% SG with Penetrant 20 0 0 0 0 0 0 0 0 0 0
T3-F001 35% SG without Penetrant 70 0 0 0 0 0 0 0 0 0 0
T4-F001 35% SG with Penetrant 70 0 0 0 0 0 0 0 0 0 0
T5-F001 50% SG without Penetrant 100 0 0 0 0 0 0 0 0 0 0
T6-F001 50% SG with Penetrant 100 0 0 0 0 0 0 0 0 0 0
*DAS – Days After Spray

As shown in Table 39, the phytotoxicity evaluation of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations in chilli demonstrated that all tested formulations and doses of F001 (ranging from 10 to 100 gai/ha) exhibited no phytotoxic effects on chilli plants. Across both the first and second sprays, and on all observation days (1, 3, 5, 7, and 10 DAS), no symptoms such as chlorosis, necrosis, and leaf deformation, or wilting were recorded. This suggests that F001 is safe for use on cotton at the evaluated doses and does not negatively impact plant health.

Example 11: Evaluation of Bio-efficacy and Phytotoxicity Study of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (with penetrant) against Aphids, Jassids, Thrips & Whiteflies in Cotton crop.

TRIAL 2: Experimental Details
Season Rabi (2024-25)
Location Mastakatti Village, Koppal District, Karnataka
Crop Cotton
Variety Ajeet-V-5210
Pests under study Aphids- Aphis gossypii
Thrips- Thrips tabaci
Whitefly- Bemisia tabaci
Jassids- Amrasca devastans
Chemical Tested N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (F001)
Area Required 1170 sq. m [6m x 5m= 30m2 Per plot]
Plot size 6m x 5m = 30m2
Number of Replication 3
Date of sowing 12/11/2024
Volume of spray fluid 500 L
Number of Spray 2
Spray Schedule 1st Spray: 11/02/2025
2nd Spray: 25/02/2025
Date of Harvest 05/03/2025, 12/03/2025, 18/03/2025

Table 40: Treatment Details
S. No. Treatment Details Dosage/ha
A.I. (gm) Formulation (gm) Dilution in water (L)
T-1 F001 10% SG 7.5 75 500
T-2 F001 10% SG 15 150 500
T-3 F001 35% SG 26.25 75 500
T-4 F001 35% SG 52.5 150 500
T-5 F001 50% SG 37.5 75 500
T-6 F001 50% SG 75 150 500
T-7 Std check-N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% WG 75 150 500
T-8 Std check-N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG 75 150 500
T-9 Control
*Note: T-7 & T-8 are commercially available products

Methodology:
The experiment was laid out in randomized block design (RBD), replicating thrice with a single plot area of 6 x 5 m2.
The required quantity of the insecticide was dissolved in 500 litres of water per hectare and applied uniformly using a knapsack sprayer at the first appearance of insect pests to ensure complete canopy coverage.
Observations for Aphids, Jassids, Thrips, and Whiteflies populations were recorded a day prior to the first spray application. Post-treatment pest counts were taken on the 3rd, 7th, 10th, and 14th days after application.
This observation schedule was repeated following each subsequent round of application. Pest population data were collected from ten randomly tagged plants per plot or replication
Table 41: RBD Distribution

Replication 1 Replication 2 Replication 3
T 7 T 6 T 9
T 1 T 5 T 3
T 9 T 8 T 7
T 5 T 1 T 2
T 3 T 9 T 6
T 2 T 4 T 8
T 8 T 3 T 5
T 6 T 7 T 1
T 4 T 2 T 4

Observation:
The evaluation was done based on the following observations:
Insect severity on three leaves per plant in ten tagged plants at 3, 7, 10, and 14 days after spray.
Population of Aphids, Jassids, Thrips & Whiteflies before and after each application.
Percent insect control
Bio-effectiveness of insecticide doses
Yield: Total yield in quintals per ha.
Effect on Natural enemies: Total number of natural enemies per ten tagged plants.
Phytotoxicity: Number of plant Epinasty, Hyponasty, Necrosis, Vein clearing, wilting per ten tagged plants in a plot. (Ranging from 0: No symptoms of phytotoxicity to 10: Complete death)

Table 42: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Aphids in Cotton
Treatment Dose (gai/ha) Number of aphids/ 3 leaves/ plant after first spray ROC Number of aphids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 7.50 12.40 11.33 10.60 9.80 8.53 57.89 7.40 6.93 6.33 5.60 78.29
(3.59) (3.44) (3.33) (3.21) (3.01) (2.81) (2.73) (2.61) (2.47)
T2-F001 10% SG 15.00 12.00 11.00 10.40 9.40 7.93 60.86 7.00 5.87 5.47 4.67 81.91
(3.54) (3.39) (3.30) (3.15) (2.90) (2.74) (2.52) (2.44) (2.27)
T3-F001 35% SG 26.25 13.20 10.20 9.80 8.87 7.73 61.84 6.60 5.20 4.60 4.07 84.24
(3.70) (3.27) (3.21) (3.06) (2.87) (2.66) (2.39) (2.26) (2.14)
T4-F001 35% SG 52.50 12.67 8.00 7.20 6.40 5.07 75.00 3.60 2.53 2.00 1.93 92.51
(3.63) (2.92) (2.77) (2.63) (2.36) (2.02) (1.74) (1.58) (1.56)
T5-F001 50% SG 37.50 14.73 9.80 9.20 8.20 6.93 65.79 6.13 4.20 3.67 3.53 86.30
(3.90) (3.21) (3.11) (2.95) (2.73) (2.58) (2.17) (2.04) (2.01)
T6-F001 50% SG 75.00 12.13 6.80 5.87 5.07 3.60 82.24 2.60 1.93 1.73 1.47 94.32
(3.55) (2.70) (2.52) (2.36) (2.02) (1.76) (1.56) (1.49) (1.40)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 75 13.87 10.07 9.27 7.80 6.13 69.74 5.67 4.87 4.20 3.60 86.05
(3.79) (3.25) (3.13) (2.88) (2.58) (2.48) (2.32) (2.17) (2.02)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 75 14.53 10.53 9.60 8.87 7.40 63.49 5.93 5.13 4.53 4.27 83.46
(3.88) (3.32) (3.18) (3.06) (2.81) (2.54) (2.37) (2.24) (2.18)
T9-Control - 13.53 15.27 16.80 18.13 20.27 21.80 22.73 23.67 25.80
(3.75) (3.97) (4.16) (4.32) (4.56) (4.72) (4.82) (4.92) (5.13)
C.D. NS 0.673 0.471 0.48 0.486 0.492 0.554 0.639 0.674
SE(m) - 0.229 0.16 0.163 0.165 0.167 0.189 0.218 0.229

The effectiveness of the present invention formulation was assessed against aphid infestation in cotton crop. As presented in Table 42, the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulations (F001) exhibited strong efficacy against aphids, particularly at higher application rates. Among the treatments, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 75 g ai/ha (T6) was most effective, showing the highest reduction over control (ROC) 82.24% after the first spray and 94.32% after the second spray. This was closely followed by F001 35% SG at 52.5 g ai/ha (T4), with ROC values of 75.00% and 92.51%, respectively. Lower doses such as F001 10% SG (T1 and T2) also performed moderately, with ROC values ranging from 57.89% to 81.91%. In comparison, the standard checks standard checks provided ROC values of 69.74% and 63.49% after the first spray, and 86.05% and 83.46% after the second spray, indicating that several F001 formulations, especially T6 and T4 outperformed the standards. The untreated control consistently showed increasing aphid populations over time, validating the effectiveness of the insecticide treatments.

Table 43: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Thrips in Cotton
Treatment Dose (gai/ha) Number of thrips/ 3 leaves/ plant after first spray ROC Number of thrips/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 7.50 14.13 11.53 10.80 10.00 8.73 57.61 7.60 7.07 6.47 5.80 77.69
(3.83) (3.47) (3.36) (3.24) (3.04) (2.85) (2.75) (2.64) (2.51)
T2-F001 10% SG 15.00 13.87 11.20 10.60 9.60 8.20 60.19 7.33 6.20 5.73 4.73 81.79
(3.79) (3.42) (3.33) (3.18) (2.95) (2.80) (2.59) (2.50) (2.29)
T3-F001 35% SG 26.25 13.47 10.53 10.13 9.20 7.80 62.14 6.87 5.40 4.80 4.27 83.59
(3.74) (3.32) (3.26) (3.11) (2.88) (2.71) (2.43) (2.30) (2.18)
T4-F001 35% SG 52.50 13.47 8.33 7.53 6.60 5.20 74.76 4.80 3.53 3.13 2.73 89.49
(3.74) (2.97) (2.83) (2.66) (2.39) (2.30) (2.01) (1.91) (1.80)
T5-F001 50% SG 37.50 13.40 10.13 9.53 8.53 7.13 65.37 6.33 4.53 4.00 3.67 85.90
(3.73) (3.26) (3.17) (3.01) (2.76) (2.61) (2.24) (2.12) (2.04)
T6-F001 50% SG 75.00 13.80 7.13 6.20 5.33 3.80 81.55 2.80 2.20 1.93 1.67 93.59
(3.78) (2.76) (2.59) (2.42) (2.07) (1.82) (1.64) (1.56) (1.47)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 75 13.87 10.33 9.47 8.13 6.27 69.58 5.80 5.13 4.47 3.80 85.38
(3.79) (3.29) (3.16) (2.94) (2.60) (2.51) (2.37) (2.23) (2.07)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 75 13.40 10.73 9.80 9.20 7.73 62.46 6.20 5.47 4.87 4.47 82.82
(3.73) (3.35) (3.21) (3.11) (2.87) (2.59) (2.44) (2.32) (2.23)
T9-Control - 13.93 15.53 17.13 18.40 20.60 22.13 22.93 23.93 26.00
(3.80) (4.00) (4.20) (4.35) (4.59) (4.76) (4.84) (4.94) (5.15)
C.D. NS 0.469 0.477 0.455 0.483 0.51 0.451 0.617 0.629
SE(m) - 0.16 0.163 0.155 0.164 0.174 0.154 0.21 0.214

The effectiveness of the present invention's formulation in controlling thrips in cotton crops was evaluated. As shown in Table 43, the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) demonstrated efficacy against thrips that closely paralleled their performance against aphids, with the highest application rates yielding the most substantial control. N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 75 g/ha (T6) and 35% SG at 52.5 g/ha (T4) showed the highest effectiveness, reducing thrips populations by 81.55% and 74.76% after the first spray, and by 93.59% and 89.49% after the second spray, respectively. These results were superior to the standard checks which achieved 85.38% and 82.82% control after the second spray. Lower doses, such as N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 10% SG at 7.5 and 15 g/ha, recorded moderate control, with reductions of 57.61and 60.19% after the first spray and up to 81.79% after the second. The untreated control group showed a continual increase in thrips numbers. Overall, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG exhibited strong, dose-dependent thrips suppression, indicating its suitability as an effective alternative to existing standard treatments in cotton pest management.

Table 44: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Cotton Whiteflies
Treatment Dose (gai/ha) Number of whiteflies/ 3 leaves/ plant after first spray ROC Number of whiteflies/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 7.50 13.27 12.33 11.73 11.00 10.33 46.55 9.53 8.20 7.53 6.93 72.04
(3.71) (3.58) (3.50) (3.39) (3.29) (3.17) (2.95) (2.83) (2.73)
T2-F001 10% SG 15.00 14.27 12.13 10.93 10.13 9.40 51.38 8.60 7.80 7.33 6.13 75.27
(3.84) (3.55) (3.38) (3.26) (3.15) (3.02) (2.88) (2.80) (2.58)
T3-F001 35% SG 26.25 13.33 11.33 10.00 9.33 8.53 55.86 7.40 6.73 6.13 5.20 79.03
(3.72) (3.44) (3.24) (3.14) (3.01) (2.81) (2.69) (2.58) (2.39)
T4-F001 35% SG 52.50 13.67 8.40 7.60 6.73 6.00 68.97 5.33 4.73 4.00 3.13 87.37
(3.76) (2.98) (2.85) (2.69) (2.55) (2.42) (2.29) (2.12) (1.91)
T5-F001 50% SG 37.50 13.80 10.40 9.13 8.20 7.60 60.69 6.80 6.13 5.40 4.73 80.91
(3.78) (3.30) (3.10) (2.95) (2.85) (2.70) (2.58) (2.43) (2.29)
T6-F001 50% SG 75.00 13.67 7.93 6.80 5.40 4.73 75.52 4.20 3.60 3.00 2.20 91.13
(3.76) (2.90) (2.70) (2.43) (2.29) (2.17) (2.02) (1.87) (1.64)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 75 13.53 9.93 8.80 8.00 7.33 62.07 6.53 5.73 5.00 4.40 82.26
(3.75) (3.23) (3.05) (2.92) (2.80) (2.65) (2.50) (2.35) (2.21)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 75 14.00 10.13 9.20 8.67 7.93 58.97 7.00 6.33 5.80 5.20 79.03
(3.81) (3.26) (3.11) (3.03) (2.90) (2.74) (2.61) (2.51) (2.39)
T9-Control - 13.40 15.80 16.60 17.53 19.33 20.20 21.40 22.33 24.80
(3.73) (4.04) (4.14) (4.25) (4.45) (4.55) (4.68) (4.78) (5.03)
C.D. NS 0.419 0.648 0.543 0.424 0.315 0.426 0.402 0.562
SE(m) - 0.143 0.221 0.185 0.144 0.107 0.145 0.137 0.191

The effectiveness of the present invention's formulation was evaluated for controlling whiteflies in cotton crops. As indicated in Table 44, the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) demonstrated high efficacy against whiteflies, mirroring the trend observed for aphids and thrips. N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 75 g/ha (T6) and 35% SG at 52.5 g/ha (T4) were the most effective treatments, reducing whitefly populations by 75.52% and 68.97% after the first spray, and by 91.13% and 87.37% after the second spray, respectively. These results outperformed standard checks, which achieved up to 82.26% and 79.03% control. Lower doses of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide, such as the 10% SG at 7.5 and 15 g/ha, exhibited moderate efficacy with up to 75.27% reduction. The untreated control group showed a progressive increase in whitefly populations. Overall, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 50% SG formulation demonstrated strong whitefly suppression, indicating its potential as an effective alternative to standard insecticides in integrated pest management strategies.

Table 45: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Cotton Jassids
Treatment Dose (gai/ha) Number of jassids/ 3 leaves/ plant after first spray ROC Number of jassids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 7.50 11.80 10.67 10.00 9.47 8.87 54.92 8.33 8.07 7.87 6.27 75.07
(3.51) (3.34) (3.24) (3.16) (3.06) (2.97) (2.93) (2.89) (2.60)
T2-F001 10% SG 15.00 11.60 10.47 9.93 9.67 8.67 55.93 8.13 7.67 6.40 5.47 78.25
(3.48) (3.31) (3.23) (3.19) (3.03) (2.94) (2.86) (2.63) (2.44)
T3-F001 35% SG 26.25 12.33 10.07 9.87 9.27 8.33 57.63 7.73 7.07 6.33 4.53 81.96
(3.58) (3.25) (3.22) (3.13) (2.97) (2.87) (2.75) (2.61) (2.24)
T4-F001 35% SG 52.50 12.40 8.67 7.93 7.07 6.80 65.42 5.67 5.00 4.33 3.67 85.41
(3.59) (3.03) (2.90) (2.75) (2.70) (2.48) (2.35) (2.20) (2.04)
T5-F001 50% SG 37.50 12.73 9.73 9.47 8.53 7.93 59.66 7.13 6.47 5.73 4.07 83.82
(3.64) (3.20) (3.16) (3.01) (2.90) (2.76) (2.64) (2.50) (2.14)
T6-F001 50% SG 75.00 13.73 8.27 7.47 6.67 6.07 69.15 5.13 4.33 3.53 2.07 91.78
(3.77) (2.96) (2.82) (2.68) (2.56) (2.37) (2.20) (2.01) (1.60)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 75 13.40 10.27 9.13 8.33 7.67 61.02 6.87 6.07 5.33 3.73 85.15
(3.73) (3.28) (3.10) (2.97) (2.86) (2.71) (2.56) (2.42) (2.06)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 75 13.20 10.47 9.53 9.07 8.27 57.97 7.33 6.67 6.13 4.47 82.23
(3.70) (3.31) (3.17) (3.09) (2.96) (2.80) (2.68) (2.58) (2.23)
T9-Control - 12.67 16.13 16.93 17.87 19.67 20.60 21.73 22.67 25.13
(3.63) (4.08) (4.18) (4.29) (4.49) (4.59) (4.72) (4.81) (5.06)
C.D. NS 0.488 0.463 0.412 0.5 0.493 0.481 0.493 0.554
SE(m) - 0.166 0.158 0.14 0.17 0.168 0.164 0.168 0.189

The effectiveness of the present invention's formulation was assessed for managing jassids in cotton crops. As shown in Table 45, the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) demonstrated high efficacy against jassids. The highest reduction in jassid population was recorded with N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 75 g/ha (T6), achieving 69.15% reduction after the first spray and 91.78% after the second spray. This was followed closely by F001 35% SG at 52.5 g/ha (T4), which showed 65.42% and 85.41% reduction after the first and second sprays, respectively. These results were superior to the standard checks, which recorded up to 85.15% and 82.23% reduction after the second spray. Moderate efficacy was observed at lower doses such as N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 10% SG at 7.5-15 g/ha. The untreated control group saw an increase in jassid populations over time. Overall, the data highlight the strong potential of the present invention formulation for the effective management of jassids, particularly when applied at higher concentrations and dosages.

Table 46: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Natural Enemies in Cotton Crops
Treatment Dose (gai /ha) Number of Spiders per Plant Number of Coccinellids per Plant
First Spray Second Spray First Spray Second Spray
PTC 3 DAS 7 DAS 7 DAS 10 DAS PTC 3 DAS 7 DAS 7 DAS 10 DAS
T1-F001 10% SG 7.50 4.80 4.73 4.60 4.53 4.40 3.93 3.93 3.80 3.73 3.67
(2.30) (2.29) (2.26) (2.24) (2.21) (2.11) (2.11) (2.07) (2.06) (2.04)
T2-F001 10% SG 15.00 4.87 4.67 4.60 4.47 4.40 3.87 3.87 3.80 3.67 3.60
(2.32) (2.27) (2.26) (2.23) (2.21) (2.09) (2.09) (2.07) (2.04) (2.02)
T3-F001 35% SG 26.25 4.80 4.60 4.53 4.40 4.33 4.13 3.80 3.73 3.60 3.53
(2.30) (2.26) (2.24) (2.21) (2.20) (2.15) (2.07) (2.06) (2.02) (2.01)
T4-F001 35% SG 52.50 4.73 4.53 4.47 4.33 4.27 4.07 3.73 3.67 3.53 3.47
(2.29) (2.24) (2.23) (2.20) (2.18) (2.14) (2.06) (2.04) (2.01) (1.99)
T5-F001 50% SG 37.50 4.47 4.47 4.40 4.33 4.20 4.13 3.73 3.60 3.47 3.40
(2.23) (2.23) (2.21) (2.20) (2.17) (2.15) (2.06) (2.02) (1.99) (1.97)
T6-F001 50% SG 75.00 4.60 4.47 4.33 4.27 4.27 3.87 3.67 3.53 3.53 3.33
(2.26) (2.23) (2.20) (2.18) (2.18) (2.09) (2.04) (2.01) (2.01) (1.96)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 75.00 4.47 4.53 4.53 4.33 4.27 4.27 3.73 3.67 3.53 3.47
(2.23) (2.24) (2.24) (2.20) (2.18) (2.18) (2.06) (2.04) (2.01) (1.99)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 75.00 4.67 4.60 4.47 4.40 4.27 4.13 3.80 3.73 3.60 3.53
(2.27) (2.26) (2.23) (2.21) (2.18) (2.15) (2.07) (2.06) (2.02) (2.01)
T9-Control - 4.73 4.87 5.00 5.07 5.13 3.93 4.07 4.13 4.33 4.53
(2.29) (2.32) (2.35) (2.36) (2.37) (2.11) (2.14) (2.15) (2.20) (2.24)
C.D. NS NS NS NS NS NS NS NS NS NS
SE(m) - - - - - - - - - -

The effect of the present invention formulation on natural enemies within cotton crops was evaluated to determine its ecological safety. As indicated in Table 46, application of the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) resulted in minimal impact on the populations of key beneficial insects present in the cotton ecosystem. Two principal natural enemies spiders and coccinellids were monitored following both the first and second applications. Across all tested doses and formulations of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide (SG), only slight and statistically non-significant reductions in the population levels of both natural enemies were observed when compared to the untreated control. The standard check treatments (50% WG/SG) demonstrated similar trends, further confirming that the F001 formulation does not adversely affect natural enemy populations. Therefore, the present invention formulation can be considered ecologically safe and compatible with integrated pest management (IPM) practices in cotton cultivation.

Table 47: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Cotton Yield
Treatment Dose (gai /ha) Yield
(q/ha) Increase in yield over control (%) Yield Profit Common cost Cost per Insecticide Cost per treatment Net Return Total Cost Cost benefit Ratio


T1-F001 10% SG 10 10.33 24.00 79,411.67 16,000.00 76.99 300.26 63111.41 16300.26 3.87
(3.29)
T2-F001 10% SG 20 10.67 28.00 81,973.33 16,000.00 153.98 600.52 65372.81 16600.52 3.94
(3.34)
T3-F001 35% SG 35 11.00 32.00 84,535.00 16,000.00 212.33 828.09 67706.91 16828.09 4.02
(3.39)
T4-F001 35% SG 70 12.67 52.00 97,343.33 16,000.00 424.66 1656.17 79687.16 17656.17 4.51
(3.63)
T5-F001 50% SG 50 11.67 40.00 89,658.33 16,000.00 293.534 1144.78 72513.55 17144.78 4.23
(3.49)
T6-F001 50% SG 100 13.67 64.00 1,05,028.33 16,000.00 587.068 2289.57 86738.77 18289.57 4.74
(3.76)
(3.41)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 11.67 40.00 89,658.33 16,000.00 1704 1704 71954.33 17704.00 4.06
(3.49)
T8-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 11.00 32.00 84,535.00 16,000.00 398.836 1555.46 66979.54 17555.46 3.82
(3.39)
T9-Control - 8.33 64,041.67 16,000.00 - - 48041.67 16000.00 3.00
(2.97)
C.D. 0.966
SE(m) 0.329

The effect of the present invention formulation on cotton yield was evaluated, as summarized in Table 47. Application of the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulations (F001) resulted in a significant improvement in cotton yield compared to the untreated control, which recorded a yield of 8.33 q/ha. Among the tested treatments, 50% SG at 75 gai/ha (T6) achieved the highest yield of 13.67 q/ha (64% increase), and this was followed by the 35% SG at 52.5 gai/ha (T4), with a yield of 12.67 q/ha (52% increase). Moderate yield improvements, ranging from 32% to 40%, were observed with standard chemical checks (50% WG and SG), further demonstrating the superior performance of the F001 formulations at appropriate doses. Notably, even the lowest tested dose of F001 (10% SG at 7.5 gai/ha) resulted in a yield of 10.33 q/ha, corresponding to a 24% increase over the control. These results collectively demonstrate the efficacy of the present invention formulation in enhancing cotton yield across a range of application rates.

Cost-Benefit analysis: The economic assessment of the treatments for whitefly control demonstrated that the application of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 75 gai/ha provided the most favourable outcome, yielding the highest cost-benefit ratio of 4.74 and a net return of ?86,738.77 per hectare. This treatment also yielded a substantial 13.67 t/ha, reflecting both high biological efficacy and economic viability. Additionally, 35% SG at 52.5 gai/ha delivered high profitability, with cost-benefit ratios of 4.51. These formulations provided elevated yield returns while maintaining reasonable insecticide costs. The standard check treatment (50% WG) achieved a moderate cost-benefit ratio of 4.06, which was surpassed by several of the F001 formulations. Overall, these results indicate that the F001 formulations, particularly at 50% SG (75 g ai/ha) represent a highly effective and economically advantageous solution for managing whiteflies in cotton cultivation.

Table 48: Evaluation of Phytotoxicity of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG in Cotton crop

Visual observations were recorded on 1, 3, 5, 7, and 10 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below.

Score Phytotoxicity (percent) Score Phytotoxicity (percent)
0 No phytotoxicity 5 41-50
1 1-10 6 51-60
2 11-20 7 61-70
3 21-30 8 71-80
4 31-40 9 & 10 Complete Destruction

Table 49: Phytotoxic effect of various treatments on Cotton crop
Treatment Dose (g /ha) First Spray Second Spray
1 DAS 3 DAS 5 DAS 7 DAS 10 DAS 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
T1-F001 10% SG 7.50 0 0 0 0 0 0 0 0 0 0
T2-F001 10% SG 15.00 0 0 0 0 0 0 0 0 0 0
T3-F001 35% SG 26.25 0 0 0 0 0 0 0 0 0 0
T4-F001 35% SG 52.50 0 0 0 0 0 0 0 0 0 0
T5-F001 50% SG 37.50 0 0 0 0 0 0 0 0 0 0
T6-F001 50% SG 75.00 0 0 0 0 0 0 0 0 0 0
*DAS – Days After Spray

As presented in Table 49, the phytotoxicity evaluation of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) in cotton indicated that all tested formulations and doses of F001 (ranging from 7.5 to 75.0 g/ha) exhibited no phytotoxic effects on cotton plants. Across both the first and second sprays, and on all observation days (1, 3, 5, 7, and 10 DAS), no symptoms such as chlorosis, necrosis, and leaf deformation, or wilting were recorded. This suggests that F001 is safe for use on cotton at the evaluated doses and does not negatively impact plant health

Example 12: Evaluation of Bio-efficacy and Phytotoxicity Study of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (with penetrant) against Aphids, Jassids, Thrips & Whiteflies in Brinjal crop.

TRIAL 3: Experimental Details
Season Rabi (2024-25)
Location Mastakatti Village, Koppal District, Karnataka
Crop Brinjal
Variety Ajeet-V-80
Pests under study Aphids- Aphis gossypii
Thrips- Thrips tabaci
Whitefly- Bemisia tabaci
Jassids- Amrasca devastans/ Amrasca bigutulla bigutulla
Chemical Tested N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide SG (F001)
Area Required 1170 sq. m [6m x 5m= 30m2 Per plot]
Plot size 6m x 5m= 30m2
Number of Replication 3
Date of sowing 03/12/2024
Volume of spray fluid 500 L
Number of Spray 2
Spray Schedule 1st Spray: 12/02/2025
2nd Spray: 27/02/2025
Date of Harvest 29/04/2025

Table 50: Treatment Details
S. No. Treatment Details Dosage/ha
A.I. (gm) Formulation (gm) Dilution in water (L)
T-1 F001 10% SG 10 100 500
T-2 F001 10% SG 20 200 500
T-3 F001 35% SG 35 100 500
T-4 F001 35% SG 70 200 500
T-5 F001 50% SG 50 100 500
T-6 F001 50% SG 100 200 500
T-7 Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 200 500
T-8 Std check – N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 200 500
T-9 Control - - -
*Note: T-7 & T-8 are commercially available products

Methodology:
The experiment was laid out in randomized block design (RBD), replicating thrice with a single plot area of 6 x 5 m2.
The required quantity of the insecticide was dissolved in 500 litres of water per hectare and applied uniformly using a knapsack sprayer at the first appearance of insect pests to ensure complete canopy coverage.
Observations for Aphids, Jassids, Thrips, and Whiteflies populations were recorded a day prior to the first spray application. Post-treatment pest counts were taken on the 3rd, 7th, 10th, and 14th days after application.
This observation schedule was repeated following each subsequent round of application. Pest population data were collected from ten randomly tagged plants per plot or replication

Table 51: RBD Distribution

Replication-1 Replication-2 Replication-3
T-4 T-8 T-6
T-9 T-5 T-5
T-1 T-9 T-9
T-7 T-1 T-7
T-3 T-6 T-1
T-6 T-4 T-3
T-8 T-3 T-8
T-2 T-2 T-4
T-5 T-7 T-2

Observation:
Evaluation was done based on the following observations:
Insect severity on three leaves per plant in ten tagged plants at 3, 7, 10, and 14 days after spray.
Population of Aphids, Jassids, Thrips & Whiteflies before and after each application.
Percent insect control
Bio-effectiveness of insecticide doses
Yield: Total yield in quintals per ha.
Effect on Natural enemies: Total number of natural enemies per ten tagged plants.
Phytotoxicity: Number of plant Epinasty, Hyponasty, Necrosis, Vein clearing, wilting per ten tagged plants in a plot. (Ranging from 0: No symptoms of phytotoxicity to 10: Complete death)

Table 52: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Aphids in Brinjal crop
Treatment Dose (gai/ha) Number of aphids/ 3 leaves/ plant after first spray ROC Number of aphids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 8.13 7.67 7.13 6.53 6.20 46.55 5.53 4.93 4.20 3.53 77.92
(2.94) (2.86) (2.76) (2.65) (2.59) (2.46) (2.33) (2.17) (2.01)
T2-F001 10% SG 20 8.27 7.33 6.87 6.27 5.93 48.85 5.33 4.73 3.93 3.13 80.42
(2.96) (2.80) (2.71) (2.60) (2.54) (2.42) (2.29) (2.11) (1.91)
T3-F001 35% SG 35 8.67 7.00 6.33 6.00 5.53 52.30 5.00 4.40 3.53 2.73 82.92
(3.03) (2.74) (2.61) (2.55) (2.46) (2.35) (2.21) (2.01) (1.80)
T4-F001 35% SG 70 8.20 5.60 4.93 4.40 4.13 64.37 3.73 2.93 2.33 1.73 89.17
(2.95) (2.47) (2.33) (2.21) (2.15) (2.06) (1.85) (1.68) (1.49)
T5-F001 50% SG 50 8.33 6.73 5.93 5.60 5.13 55.75 4.73 4.73 3.20 2.53 84.17
(2.97) (2.69) (2.54) (2.47) (2.37) (2.29) (2.29) (1.92) (1.74)
T6-F001 50% SG 100 8.13 4.60 3.93 3.40 2.80 75.86 2.40 1.80 1.53 1.20 92.50
(2.94) (2.26) (2.11) (1.97) (1.82) (1.70) (1.52) (1.43) (1.30)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 8.67 6.40 5.73 5.13 4.80 58.62 4.40 3.73 3.13 2.40 85.00
(3.03) (2.63) (2.50) (2.37) (2.30) (2.21) (2.06) (1.91) (1.70)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 8.13 6.60 5.80 5.33 5.00 56.90 4.80 4.00 3.60 2.60 83.75
(2.94) (2.66) (2.51) (2.42) (2.35) (2.30) (2.12) (2.02) (1.76)
T9-Control - 8.33 9.00 9.73 10.40 11.60 13.13 14.53 15.33 16.00
(2.97) (3.08) (3.20) (3.30) (3.48) (3.69) (3.88) (3.98) (4.06)
C.D. NS 0.543 0.469 0.532 0.427 0.492 0.477 0.35 0.394
SE(m) - 0.185 0.16 0.181 0.145 0.167 0.163 0.119 0.134

The effectiveness of the present invention's formulation was assessed for controlling aphids in brinjal crops. As shown in Table 52, the efficacy of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) against aphids increased with both concentration and application rate. Lower concentrations, specifically the 10% SG formulation resulted in moderate reductions in aphid populations, achieving reductions of up to 48.85% and 46.55% over the control (ROC) after the first spray, with the effect increasing to 80.42% following the second application. In contrast, higher concentrations such as 35% SG at 70 gai/ha, and 50% SG at 100 gai/ha, achieved substantial reductions in aphid populations, with ROC values of 89.17%, and 92.5%, respectively. These outcomes surpassed those observed for the standard check treatments (50% WG and SG), which achieved ROC values ranging from 83.75% to 85%. The untreated control plots exhibited a continual increase in aphid populations, further underscoring the robust efficacy of the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations in managing aphid infestations in brinjal crops.

Table 53: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Thrips in Brinjal crop
Treatment Dose (gai/ha) Number of thrips/ 3 leaves/ plant after first spray ROC Number of thrips/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 15.47 14.13 13.60 12.00 11.20 47.17 10.53 9.80 8.40 7.73 72.90
(4.00) (3.83) (3.75) (3.54) (3.42) (3.32) (3.21) (2.98) (2.87)
T2-F001 10% SG 20 15.60 13.73 12.53 11.80 10.40 50.94 9.80 8.60 7.93 7.33 74.30
(4.01) (3.77) (3.61) (3.51) (3.30) (3.21) (3.02) (2.90) (2.80)
T3-F001 35% SG 35 15.13 12.60 11.73 11.00 10.20 51.89 9.40 8.33 7.53 6.93 75.70
(3.95) (3.62) (3.50) (3.39) (3.27) (3.15) (2.97) (2.83) (2.73)
T4-F001 35% SG 70 15.40 9.20 8.93 8.13 7.67 63.84 6.53 5.93 5.40 4.80 83.18
(3.99) (3.11) (3.07) (2.94) (2.86) (2.65) (2.54) (2.43) (2.30)
T5-F001 50% SG 50 15.13 11.40 10.93 10.53 9.60 54.72 8.73 7.73 6.60 6.20 78.27
(3.95) (3.45) (3.38) (3.32) (3.18) (3.04) (2.87) (2.66) (2.59)
T6-F001 50% SG 100 15.93 7.80 7.40 6.93 6.00 71.70 5.00 4.60 3.80 3.40 88.08
(4.05) (2.88) (2.81) (2.73) (2.55) (2.35) (2.26) (2.07) (1.97)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 15.40 11.13 10.53 9.80 9.20 56.60 8.53 7.60 6.73 6.20 78.27
(3.99) (3.41) (3.32) (3.21) (3.11) (3.01) (2.85) (2.69) (2.59)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 15.00 11.80 11.00 10.20 9.60 54.72 8.93 8.13 7.73 6.73 76.40
(3.94) (3.51) (3.39) (3.27) (3.18) (3.07) (2.94) (2.87) (2.69)
T9-Control - 15.07 16.80 18.13 19.80 21.20 23.53 25.13 27.33 28.53
(3.95) (4.16) (4.32) (4.51) (4.66) (4.90) (5.06) (5.28) (5.39)
C.D. NS 0.941 0.707 0.559 0.595 0.592 0.559 0.488 0.389
SE(m) - 0.32 0.241 0.19 0.203 0.202 0.191 0.166 0.132

The effectiveness of the present invention's formulation was evaluated for controlling thrips in brinjal crops. As indicated in Table 53, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) effectively managed thrips populations. Lower-dose treatments, such as the 10% SG formulation at 10 and 20 gai/ha, resulted in reduction over control (ROC) values of approximately 47.17% and 50.94% after the first spray and up to 74.3% after the second spray. The highest efficacy was achieved with the 50% SG formulation at 100 gai/ha (ROC 88.08%). These results surpassed those obtained with the standard (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) treatments, which demonstrated ROC values ranging from 76.4% to 78.27%. In contrast, the untreated control group exhibited a marked increase in thrips population, further emphasizing the substantial efficacy of higher-dose SG formulations of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) in managing thrips infestations in brinjal crops.

Table 54: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Whiteflies in Brinjal crop
Treatment Dose (gai/ha) Number of whiteflies/ 3 leaves/ plant after first spray ROC Number of whiteflies/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 18.33 16.53 15.60 14.80 13.33 46.09 12.33 11.00 9.93 8.80 70.67
(4.34) (4.13) (4.01) (3.91) (3.72) (3.58) (3.39) (3.23) (3.05)
T2-F001 10% SG 20 18.20 15.80 15.13 14.73 12.80 48.25 11.93 10.60 9.00 8.20 72.67
(4.32) (4.04) (3.95) (3.90) (3.65) (3.53) (3.33) (3.08) (2.95)
T3-F001 35% SG 35 18.53 14.33 13.93 12.53 11.73 52.56 10.40 10.40 8.33 7.33 75.56
(4.36) (3.85) (3.80) (3.61) (3.50) (3.30) (3.30) (2.97) (2.80)
T4-F001 35% SG 70 18.00 10.33 9.80 9.40 8.20 66.85 7.40 6.53 6.00 5.33 82.22
(4.30) (3.29) (3.21) (3.15) (2.95) (2.81) (2.65) (2.55) (2.42)
T5-F001 50% SG 50 18.47 12.80 12.13 11.60 10.53 57.41 9.60 9.60 7.40 6.40 78.67
(4.36) (3.65) (3.55) (3.48) (3.32) (3.18) (3.18) (2.81) (2.63)
T6-F001 50% SG 100 18.60 9.13 8.20 7.80 6.00 75.74 5.73 5.40 4.67 4.20 86.00
(4.37) (3.10) (2.95) (2.88) (2.55) (2.50) (2.43) (2.27) (2.17)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 18.80 12.73 11.00 10.47 9.80 60.38 9.00 8.13 7.00 6.33 78.89
(4.39) (3.64) (3.39) (3.31) (3.21) (3.08) (2.94) (2.74) (2.61)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 18.00 13.20 11.60 10.93 10.20 58.76 9.53 8.73 7.33 6.73 77.56
(4.30) (3.70) (3.48) (3.38) (3.27) (3.17) (3.04) (2.80) (2.69)
T9-Control - 18.47 19.60 20.80 22.00 24.73 26.07 27.20 28.93 30.00
(4.36) (4.48) (4.62) (4.74) (5.02) (5.15) (5.26) (5.43) (5.52)
C.D. NS 0.656 0.465 0.487 0.366 0.464 0.469 0.564 0.499
SE(m) - 0.223 0.159 0.166 0.125 0.158 0.16 0.192 0.17

The effectiveness of the present invention's formulation in controlling whiteflies in brinjal crops was assessed. As shown in Table 54, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations (F001) demonstrated increased efficacy against whiteflies with higher application doses. Initial treatments with lower concentrations, specifically the 10% SG formulation, provided moderate control, achieving approximately 46-48% reduction over control (ROC) after the first spray and improving to over 70% following the second spray. Markedly greater efficacy was observed with higher doses, such as the 35% SG at 70 gai/ha and the 50% SG at 100 gai/ha, which achieved ROC values of 82.22% and 86%, respectively. These results consistently surpassed those obtained with the standard check treatments (50% formulations), which recorded ROC values of around 78%. The untreated control group exhibited a continual increase in whitefly population, further validating the superior efficacy of the (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG formulations across various pest species in brinjal crops.

Table 55: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Jassids in Brinjal crop

Treatment Dose (gai/ha) Number of jassids/ 3 leaves/ plant after first spray ROC Number of jassids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 10.20 8.93 8.20 7.53 6.93 54.98 6.40 5.93 5.60 5.27 73.22
(3.27) (3.07) (2.95) (2.83) (2.73) (2.63) (2.54) (2.47) (2.40)
T2-F001 10% SG 20 10.27 8.33 7.87 7.20 6.53 57.58 6.00 5.53 5.20 5.00 74.58
(3.28) (2.97) (2.89) (2.77) (2.65) (2.55) (2.46) (2.39) (2.35)
T3-F001 35% SG 35 10.53 7.73 7.33 6.80 6.13 60.17 5.73 5.13 4.80 4.60 76.61
(3.32) (2.87) (2.80) (2.70) (2.58) (2.50) (2.37) (2.30) (2.26)
T4-F001 35% SG 70 10.07 6.20 5.73 5.20 4.60 70.13 4.33 4.00 3.60 3.20 83.73
(3.25) (2.59) (2.50) (2.39) (2.26) (2.20) (2.12) (2.02) (1.92)
T5-F001 50% SG 50 10.40 6.93 6.40 6.20 5.93 61.47 5.40 4.93 4.40 4.13 78.98
(3.30) (2.73) (2.63) (2.59) (2.54) (2.43) (2.33) (2.21) (2.15)
T6-F001 50% SG 100 10.87 5.60 5.00 4.60 3.87 74.89 3.73 3.40 2.73 2.33 88.14
(3.37) (2.47) (2.35) (2.26) (2.09) (2.06) (1.97) (1.80) (1.68)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 10.53 7.00 6.53 6.13 5.80 62.34 5.33 4.93 4.40 4.00 79.66
(3.32) (2.74) (2.65) (2.58) (2.51) (2.42) (2.33) (2.21) (2.12)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 10.80 7.20 6.93 6.60 6.20 59.74 5.80 5.20 4.80 4.33 77.97
(3.36) (2.77) (2.73) (2.66) (2.59) (2.51) (2.39) (2.30) (2.20)
T9-Control - 10.73 11.93 12.80 14.13 15.40 16.73 17.80 18.60 19.67
(3.35) (3.53) (3.65) (3.83) (3.99) (4.15) (4.28) (4.37) (4.49)
C.D. NS 0.743 0.664 0.482 0.389 0.489 0.542 0.587 0.578
SE(m) - 0.253 0.226 0.164 0.133 0.167 0.185 0.2 0.197

The effectiveness of the present invention's formulation was evaluated for managing jassids in brinjal crops. As indicated in Table 55, N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG (F001) formulations exhibited strong efficacy in controlling jassid populations, with effectiveness increasing at higher doses and concentrations. Some highly effective treatments included the 50% SG at 100 gai/ha and the 35% SG at 70 gai/ha, both of which resulted in reductions exceeding 80%. In contrast, lower doses and formulations were less effective. While the standard check treatments N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide showed efficacy, they were generally surpassed by the higher-dose F001 treatments. Collectively, these findings demonstrate that the SG formulations of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide are highly effective in controlling jassid infestations in brinjal crops, particularly at elevated concentrations.

Table 56: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Natural Enemies in Brinjal Crops
Treatment Dose (gai/ha) Number of spiders per Plant Number of coccinellids per Plant
First Spray Second Spray First Spray Second Spray
PTC 3 DAS 7 DAS 7 DAS 10 DAS PTC 3 DAS 7 DAS 7 DAS 10 DAS
T1-F001 10% SG 10 1.87 1.73 1.60 1.60 1.33 2.33 2.27 2.20 2.20 2.13
(1.54) (1.49) (1.45) (1.45) (1.35) (1.68) (1.66) (1.64) (1.64) (1.62)
T2-F001 10% SG 20 1.73 1.67 1.60 1.53 1.47 2.13 2.13 2.07 2.07 2.00
(1.49) (1.47) (1.45) (1.43) (1.40) (1.62) (1.62) (1.60) (1.60) (1.58)
T3-F001 35% SG 35 1.67 1.67 1.53 1.47 1.40 2.33 2.27 2.20 2.13 2.07
(1.47) (1.47) (1.43) (1.40) (1.38) (1.68) (1.66) (1.64) (1.62) (1.60)
T4-F001 35% SG 70 2.00 1.60 1.47 1.40 1.40 2.27 2.20 2.13 2.13 2.13
(1.58) (1.45) (1.40) (1.38) (1.38) (1.66) (1.64) (1.62) (1.62) (1.62)
T5-F001 50% SG 50 1.80 1.60 1.47 1.33 1.33 2.33 2.20 2.07 2.07 2.00
(1.52) (1.45) (1.40) (1.35) (1.35) (1.68) (1.64) (1.60) (1.60) (1.58)
T6-F001 50% SG 100 1.87 1.53 1.40 1.27 1.33 2.20 2.13 2.00 1.93 1.87
(1.54) (1.43) (1.38) (1.33) (1.35) (1.64) (1.62) (1.58) (1.56) (1.54)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 1.80 1.60 1.47 1.33 1.33 2.20 2.13 2.07 2.07 2.00
(1.52) (1.45) (1.40) (1.35) (1.35) (1.64) (1.62) (1.60) (1.60) (1.58)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 1.73 1.67 1.53 1.40 1.40 2.27 2.20 2.13 2.07 2.07
(1.49) (1.47) (1.43) (1.38) (1.38) (1.66) (1.64) (1.62) (1.60) (1.60)
T9-Control - 1.93 2.00 2.07 2.13 2.13 2.13 2.27 2.40 2.53 2.60
(1.56) (1.58) (1.60) (1.62) (1.62) (1.62) (1.66) (1.70) (1.74) (1.76)
C.D. NS NS NS NS NS NS NS NS NS NS
SE(m) - - - - - - - - - -

The effect of the present invention formulation on natural enemies in brinjal crops was evaluated to assess its ecological safety. As shown in Table 56, the application of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations had a minimal impact on the populations of key beneficial insects within the brinjal ecosystem. Two principal natural enemies spiders and coccinellids were monitored following the first and second sprays. Across all tested doses and formulations of F001, only slight and statistically non-significant reductions in the populations of both natural enemies were observed compared to the untreated control. The same was observed for the standard check treatments (50% WG/SG), further confirming that the F001 formulations do not adversely affect natural enemy populations. Accordingly, the present invention formulation can be considered ecologically safe and compatible with integrated pest management (IPM) strategies in brinjal cultivation.

Table 57: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Brinjal Yield
Treatment Dose (gai /ha) Yield
(q/ha) Increase in yield over control (%) Yield Profit Common cost Cost per Insecticide Cost per treatment Net Return Total Cost Cost benefit Ratio


T1-F001 10% SG 10 16.00 17.07 2,83,200.00 16,000.00 76.99 300.26 266899.74 16300.26 16.37
(4.06)
T2-F001 10% SG 20 17.67 29.27 3,12,700.00 16,000.00 153.98 600.52 296099.48 16600.52 17.84
(4.26)
T3-F001 35% SG 35 18.67 36.59 3,30,400.00 16,000.00 212.33 828.09 313571.91 16828.09 18.63
(4.38)
T4-F001 35% SG 70 23.33 70.73 4,13,000.00 16,000.00 424.66 1656.17 395343.83 17656.17 22.39
(4.88)
T5-F001 50% SG 50 20.67 51.22 3,65,800.00 16,000.00 293.534 1144.78 348655.22 17144.78 20.34
(4.60)
T6-F001 50% SG 100 24.33 78.05 4,30,700.00 16,000.00 587.068 2289.57 412410.43 18289.57 22.55
(4.98)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% WG 100 21.33 56.10 3,77,600.00 16,000.00 1704 1704 359896.00 17704.00 20.33
(4.67)
T8-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 19.67 43.90 3,48,100.00 16,000.00 398.836 1555.46 330544.54 17555.46 18.83
(4.49)
T9-Control - 13.67 2,41,900.00 16,000.00 - - 225900.00 16000.00 14.12
(3.76)
C.D. 0.890
SE(m) 0.303

The effect of the present invention's formulation on brinjal yield was evaluated, with the results summarised in Table 57. The yield data demonstrate that all N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) treatments significantly increased brinjal yield compared to the untreated control. The highest yield of 24.33 q/ha, corresponding to a 78.05% increase over the control, was achieved with 50% SG formulation at 100 gai/ha. This was closely followed by the 35% SG at 70 gai/ha, with a 70.73% increase in yield. Generally, higher doses of F001 formulations produced greater yield improvements and consistently outperformed the standard check treatments, namely 50% WG (a 56.10% increase) and 50% SG (a 43.90% increase). These findings indicate that the present invention formulation is highly effective in enhancing brinjal yield, particularly at higher concentrations.

Cost-Benefit analysis: The economic evaluation of various N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations and application rates revealed that the 50% SG formulation at 100 gai/ha was the most profitable treatment, yielding the highest cost-benefit ratio of 22.55 and a substantial net return of ?4,12,410.43 per hectare. This was followed by 35% SG at 70 gai/ha with cost-benefit ratios of 22.39. These treatments combined high-yield performance with reasonable insecticide costs, resulting in excellent economic efficiency. The standard check treatments (50% WG and SG) demonstrated moderate performance but were surpassed by several F001 treatments in both net returns and cost efficiency. Collectively, these results demonstrate that the F001 formulation, particularly at optimized doses such as 50% SG at 100 gai/ha, provides a cost-effective and high-return alternative to conventional insecticides.

Table 58: Evaluation of Phytotoxicity of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG in Brinjal crop

Visual observations were recorded on 1, 3, 5, 7, and 10 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below.

Score Phytotoxicity (percent) Score Phytotoxicity (percent)
0 No phytotoxicity 5 41-50
1 1-10 6 51-60
2 11-20 7 61-70
3 21-30 8 71-80
4 31-40 9 & 10 Complete Destruction

Table 59: Phytotoxic effect of various treatments on Brinjal crop
Treatment Dose (gai/ha) First Spray Second Spray
1 DAS 3 DAS 5 DAS 7 DAS 10 DAS 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
T1-F001 10% SG 10 0 0 0 0 0 0 0 0 0 0
T2-F001 10% SG 20 0 0 0 0 0 0 0 0 0 0
T3-F001 35% SG 35 0 0 0 0 0 0 0 0 0 0
T4-F001 35% SG 70 0 0 0 0 0 0 0 0 0 0
T5-F001 50% SG 50 0 0 0 0 0 0 0 0 0 0
T6-F001 50% SG 100 0 0 0 0 0 0 0 0 0 0
*DAS – Days after spray

As presented in Table 59, the phytotoxicity evaluation of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations in brinjal demonstrated that all tested formulations and doses of F001 (ranging from 10 to 100 gai/ha) exhibited no phytotoxic effects on brinjal plants. Across both the first and second sprays, and on all observation days (1, 3, 5, 7, and 10 DAS), no symptoms such as chlorosis, necrosis, and leaf deformation, or wilting were recorded. This suggests that F001 is safe for use on brinjal at the evaluated doses and does not negatively impact plant health

Example 13: Evaluation of Bio-efficacy and Phytotoxicity Study of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulation (with penetrant) against Aphids, Jassids, Thrips & Whiteflies in Chilli crop.

TRIAL 4: Experimental Details
Season Rabi (2024-25)
Location Mastakatti Village, Koppal District, Karnataka
Crop Chilli
Variety Yashaswini Hybrid Chilli (Mahyco)
Pests under study Aphids- Aphis gossypii
Thrips- Scirtothrips dorsalis/ Thrips tabaci
Whitefly- Bemisia tabaci
Jassids- Amrasca devastans/ Amrasca bigutulla bigutulla
Chemical Tested N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide SG formulation (F001)
Area Required 1170 sq. m [6m x 5m= 30m2 Per plot]
Plot size 6m x 5m= 30m2
Number of Replication 3
Date of sowing 11/12/2024
Volume of spray fluid 500 L
Number of spray 2
Spray Schedule 1st Spray: 25/12/2024
2nd Spray: 09/01/2025
Date of Harvest 31/03/2025

Table 60: Treatment Details
S. No. Treatment Details Dosage/ha
A.I. (gm) Formulation (gm) Dilution in water (L)
T-1 F001 10% SG 10 100 500
T-2 F001 10% SG 20 200 500
T-3 F001 35% SG 35 100 500
T-4 F001 35% SG 70 200 500
T-5 F001 50% SG 50 100 500
T-6 F001 50% SG 100 200 500
T-7 Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 200 500
T-8 Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 200 500
T-9 Control - - -
*Note: T-7 & T-8 are commercially available products

Methodology:
The experiment was laid out in randomized block design (RBD), replicating thrice with a single plot area of 6 x 5 m2.
The required quantity of the insecticide was dissolved in 500 litres of water per hectare and applied uniformly using a knapsack sprayer at the first appearance of insect pests to ensure complete canopy coverage.
Observations for Aphids, Jassids, Thrips, and Whiteflies populations were recorded a day prior to the first spray application. Post-treatment pest counts were taken on the 3rd, 7th, 10th, and 14th days after application.
This observation schedule was repeated following each subsequent round of application. Pest population data were collected from ten randomly tagged plants per plot or replication

Table 61: RBD Distribution

Replication-1 Replication-2 Replication-3
T-7 T-6 T-9
T-1 T-5 T-3
T-9 T-8 T-7
T-5 T-1 T-2
T-3 T-9 T-6
T-2 T-4 T-8
T-8 T-3 T-5
T-6 T-7 T-1
T-4 T-2 T-4

Observation:
Evaluation was done based on the following observations:
Insect severity on three leaves per plant in ten tagged plants at 3, 7, 10, and 14 days after spray.
Population of Aphids, Jassids, Thrips & Whiteflies before and after each application.
Percent insect control
Bio-effectiveness of insecticide doses
Yield: Total yield in quintals per ha.
Effect on Natural enemies: Total number of natural enemies per ten tagged plants.
Phytotoxicity: Number of plant Epinasty, Hyponasty, Necrosis, Vein clearing, wilting per ten tagged plants in a plot. (Ranging from 0: No symptoms of phytotoxicity to 10: Complete death)

Table 62: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Aphids in Chilli crop
Treatment Dose (gai/ha) Number of aphids/ 3 leaves/ plant after first spray ROC Number of aphids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 19.80 17.27 15.47 14.33 12.13 52.36 11.00 10.40 9.80 9.20 70.07
(4.51) (4.22) (4.00) (3.85) (3.55) (3.39) (3.30) (3.21) (3.11)
T2-F001 10% SG 20 19.67 16.80 14.87 11.33 10.80 57.59 10.20 9.73 9.27 8.93 70.93
(4.49) (4.16) (3.92) (3.44) (3.36) (3.27) (3.20) (3.13) (3.07)
T3-F001 35% SG 35 20.13 16.33 13.93 11.20 10.40 59.16 9.73 9.40 8.80 8.33 72.89
(4.54) (4.10) (3.80) (3.42) (3.30) (3.20) (3.15) (3.05) (2.97)
T4-F001 35% SG 70 20.00 14.60 12.47 9.93 9.40 63.09 8.20 7.40 7.00 7.00 77.22
(4.53) (3.89) (3.60) (3.23) (3.15) (2.95) (2.81) (2.74) (2.74)
T5-F001 50% SG 50 21.07 15.40 13.67 10.80 10.00 60.73 9.40 8.47 8.20 7.80 74.62
(4.64) (3.99) (3.76) (3.36) (3.24) (3.15) (2.99) (2.95) (2.88)
T6-F001 50% SG 100 19.87 13.27 10.73 8.47 8.20 67.80 7.60 6.40 5.60 4.80 84.38
(4.51) (3.71) (3.35) (2.99) (2.95) (2.85) (2.63) (2.47) (2.30)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 20.00 15.27 13.20 11.27 10.13 60.21 8.87 8.40 8.13 7.73 74.84
(4.53) (3.97) (3.70) (3.43) (3.26) (3.06) (2.98) (2.94) (2.87)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 19.87 15.80 13.80 11.53 10.73 57.85 9.20 8.80 8.60 8.13 73.54
(4.51) (4.04) (3.78) (3.47) (3.35) (3.11) (3.05) (3.02) (2.94)
T9-Control - 19.67 20.20 21.60 23.53 25.47 27.00 28.27 29.27 30.73
(4.49) (4.55) (4.70) (4.90) (5.10) (5.24) (5.36) (5.46) (5.59)
C.D. NS 0.638 0.712 0.679 0.702 0.811 0.727 0.623 0.599
SE(m) - 0.217 0.242 0.231 0.239 0.276 0.248 0.212 0.204

The effectiveness of the present invention's formulation was evaluated for controlling aphids in chilli crops. As shown in Table 62, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations demonstrated excellent efficacy in reducing aphid populations, particularly at higher doses and concentrations. The most effective treatment was the 50% SG formulation at 100 gai/ha, achieving an 84.38% reduction in aphid populations following the second spray. All F001 treatments significantly outperformed the untreated control and provided superior efficacy compared to the standard check treatments (50% WG and 50% SG), which recorded aphid population reductions of 74.84% and 73.54%, respectively. These results indicate a strong dose- and concentration-dependent effect of the present invention formulation in managing aphid infestations in chilli crops.

Table 63: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Thrips in Chilli crop
Treatment Dose (gai/ha) Number of thrips/ 3 leaves/ plant after first spray ROC Number of thrips/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 8.00 7.67 7.20 6.73 6.40 47.54 6.00 5.60 5.13 4.80 69.23
(2.92) (2.86) (2.77) (2.69) (2.63) (2.55) (2.47) (2.37) (2.30)
T2-F001 10% SG 20 7.93 7.40 6.80 6.53 6.13 49.73 5.93 5.73 4.93 4.53 70.94
(2.90) (2.81) (2.70) (2.65) (2.58) (2.54) (2.50) (2.33) (2.24)
T3-F001 35% SG 35 8.67 7.00 6.73 6.33 6.00 50.82 5.73 5.20 4.60 4.13 73.50
(3.03) (2.74) (2.69) (2.61) (2.55) (2.50) (2.39) (2.26) (2.15)
T4-F001 35% SG 70 8.40 6.33 6.00 5.80 5.33 56.28 4.73 4.40 3.80 3.20 79.49
(2.98) (2.61) (2.55) (2.51) (2.42) (2.29) (2.21) (2.07) (1.92)
T5-F001 50% SG 50 8.73 6.80 6.27 6.00 5.80 52.46 5.40 5.00 4.33 3.73 76.07
(3.04) (2.70) (2.60) (2.55) (2.51) (2.43) (2.35) (2.20) (2.06)
T6-F001 50% SG 100 8.33 5.80 5.60 5.20 4.73 61.20 4.20 4.00 3.33 2.80 82.05
(2.97) (2.51) (2.47) (2.39) (2.29) (2.17) (2.12) (1.96) (1.82)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 8.87 6.73 6.40 6.20 6.00 50.82 5.73 5.27 4.80 3.80 75.64
(3.06) (2.69) (2.63) (2.59) (2.55) (2.50) (2.40) (2.30) (2.07)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 8.87 7.00 6.60 6.47 6.20 49.18 5.93 5.40 4.87 4.20 73.08
(3.06) (2.74) (2.66) (2.64) (2.59) (2.54) (2.43) (2.32) (2.17)
T9-Control - 8.73 9.20 10.07 11.20 12.20 13.33 14.33 15.20 15.60
(3.04) (3.11) (3.25) (3.42) (3.56) (3.72) (3.85) (3.96) (4.01)
C.D. NS 0.831 0.675 0.513 0.506 0.738 0.538 0.622 0.681
SE(m) - 0.283 0.23 0.175 0.172 0.251 0.183 0.212 0.232

The effectiveness of the present invention's formulation was evaluated for managing thrips in chilli crops. As detailed in Table 63, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations exhibited high efficacy against thrips, with the greatest effectiveness observed at higher concentrations and application rates. The 50% SG formulation at 100 gai/ha achieved the highest reduction in thrips populations at 82.05%, followed closely by the 35% SG at 70 gai/ha, which provided 79.49% control. In all instances, F001 treatments outperformed the standard insecticides, which provided approximately 75% control. These results indicate that the present invention formulation offers a highly effective solution for thrips management in chilli crops, particularly when applied at higher doses and formulation strengths.

Table 64: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Whiteflies in Chilli crop
Treatment Dose (gai/ha) Number of whiteflies/ 3 leaves/ plant after first spray ROC Number of whiteflies/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 10.00 8.80 8.33 7.73 7.33 48.36 6.80 6.13 5.73 5.33 68.25
(3.24) (3.05) (2.97) (2.87) (2.80) (2.70) (2.58) (2.50) (2.42)
T2-F001 10% SG 20 9.53 8.40 7.80 7.20 6.80 52.11 6.07 5.60 5.20 4.80 71.43
(3.17) (2.98) (2.88) (2.77) (2.70) (2.56) (2.47) (2.39) (2.30)
T3-F001 35% SG 35 9.73 8.07 7.60 7.13 6.53 53.99 5.93 5.33 5.00 4.53 73.02
(3.20) (2.93) (2.85) (2.76) (2.65) (2.54) (2.42) (2.35) (2.24)
T4-F001 35% SG 70 10.13 7.13 6.53 5.93 5.33 62.44 4.93 4.53 3.80 3.20 80.95
(3.26) (2.76) (2.65) (2.54) (2.42) (2.33) (2.24) (2.07) (1.92)
T5-F001 50% SG 50 9.60 7.73 7.40 6.73 6.20 56.34 5.60 5.13 4.80 4.13 75.40
(3.18) (2.87) (2.81) (2.69) (2.59) (2.47) (2.37) (2.30) (2.15)
T6-F001 50% SG 100 10.27 6.53 6.20 5.53 4.93 65.26 4.47 3.80 3.27 2.53 84.92
(3.28) (2.65) (2.59) (2.46) (2.33) (2.23) (2.07) (1.94) (1.74)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 10.20 7.80 7.13 6.53 6.00 57.75 5.80 5.20 4.53 4.00 76.19
(3.27) (2.88) (2.76) (2.65) (2.55) (2.51) (2.39) (2.24) (2.12)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 9.87 8.13 7.53 6.80 6.33 55.40 6.13 5.73 4.80 4.33 74.21
(3.22) (2.94) (2.83) (2.70) (2.61) (2.58) (2.50) (2.30) (2.20)
T9-Control - 9.60 11.07 12.07 13.07 14.20 14.93 15.53 16.00 16.80
(3.18) (3.40) (3.54) (3.68) (3.83) (3.93) (4.00) (4.06) (4.16)
C.D. NS 0.581 0.412 0.645 0.543 0.733 0.602 0.669 0.623
SE(m) - 0.198 0.14 0.22 0.185 0.249 0.205 0.228 0.212

The effectiveness of the present invention's formulation in controlling whiteflies in chilli crops was evaluated. As shown in Table 64, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) applications resulted in significant reductions in whitefly populations, particularly at higher application rates. The most effective treatment was the 50% SG formulation at 100 gai/ha, achieving an 84.92% reduction in whitefly populations. High efficacy was also observed with the 35% SG at 70 gai/ha, which achieved reductions of 80.95%. All F001 treatments outperformed the standard check treatments, which demonstrated an efficacy of approximately 76%. These results indicate that the present invention formulation provides consistent and effective control of whiteflies in chilli crops, with enhanced performance at higher concentrations and application rates.

Table 65: Bio-efficacy Evaluation of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on population of Jassids in Chilli crop
Treatment Dose (gai/ha) Number of jassids/ 3 leaves/ plant after first spray ROC Number of jassids/ 3 leaves/ plant after second spray ROC
PTC 3 DAS 7 DAS 10 DAS 14 DAS 3 DAS 7 DAS 10 DAS 14 DAS
T1-F001 10% SG 10 6.40 6.13 5.80 5.40 5.20 48.34 4.93 4.80 4.40 4.13 70.62
(2.63) (2.58) (2.51) (2.43) (2.39) (2.33) (2.30) (2.21) (2.15)
T2-F001 10% SG 20 6.07 5.93 5.53 5.13 4.80 52.32 4.73 4.53 4.13 3.80 72.99
(2.56) (2.54) (2.46) (2.37) (2.30) (2.29) (2.24) (2.15) (2.07)
T3-F001 35% SG 35 6.80 5.73 5.40 5.00 4.67 53.64 4.40 3.93 3.73 3.53 74.88
(2.70) (2.50) (2.43) (2.35) (2.27) (2.21) (2.11) (2.06) (2.01)
T4-F001 35% SG 70 6.87 4.80 4.60 4.33 3.80 62.25 3.47 3.20 2.73 2.53 81.99
(2.71) (2.30) (2.26) (2.20) (2.07) (1.99) (1.92) (1.80) (1.74)
T5-F001 50% SG 50 6.60 5.33 5.13 4.87 4.53 54.97 4.13 3.73 3.40 3.20 77.25
(2.66) (2.42) (2.37) (2.32) (2.24) (2.15) (2.06) (1.97) (1.92)
T6-F001 50% SG 100 6.47 4.33 4.20 3.80 3.47 65.56 2.93 2.40 2.07 1.93 86.26
(2.64) (2.20) (2.17) (2.07) (1.99) (1.85) (1.70) (1.60) (1.56)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 6.33 5.20 5.13 4.87 4.53 54.97 3.80 3.60 3.33 3.20 77.25
(2.61) (2.39) (2.37) (2.32) (2.24) (2.07) (2.02) (1.96) (1.92)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 6.73 5.53 5.33 5.07 4.80 52.32 4.33 3.80 3.60 3.40 75.83
(2.69) (2.46) (2.42) (2.36) (2.30) (2.20) (2.07) (2.02) (1.97)
T9-Control - 6.60 7.00 8.07 9.00 10.07 11.07 12.20 13.00 14.07
(2.66) (2.74) (2.93) (3.08) (3.25) (3.40) (3.56) (3.67) (3.82)
C.D. NS 0.593 0.804 0.684 0.606 0.5 0.722 0.572 0.52
SE(m) - 0.202 0.274 0.233 0.206 0.17 0.246 0.195 0.177

The effectiveness of the present invention's formulation was evaluated for managing jassids in chilli crops. As indicated in Table 65, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations effectively reduced jassid populations in a dose-dependent manner. The highest level of control was achieved with the 50% SG formulation at 100 gai/ha, resulting in a 86.26% reduction in jassid populations and surpassing the efficacy of standard check treatments. This was followed by 35% SG at 70 gai/ha, achieving reductions above 80%. In contrast, lower doses of the formulations demonstrated moderate efficacy. Overall, these findings establish that the present invention formulation is highly effective in managing jassid infestations in chilli crops, particularly at elevated concentrations.

Table 66: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Natural Enemies in Chilli Crops
Treatment Dose (gai /ha) Number of spiders per Plant Number of coccinellids per Plant
First Spray Second Spray First Spray Second Spray
PTC 3 DAS 7 DAS 7 DAS 10 DAS PTC 3 DAS 7 DAS 7 DAS 10 DAS
T1-F001 10% SG 10 1.53 1.47 1.53 1.47 1.40 1.87 1.87 1.80 1.73 1.73
(1.43) (1.40) (1.43) (1.40) (1.38) (1.54) (1.54) (1.52) (1.49) (1.49)
T2-F001 10% SG 20 1.40 1.33 1.40 1.27 1.27 1.80 1.80 1.87 1.73 1.73
(1.38) (1.35) (1.38) (1.33) (1.33) (1.52) (1.52) (1.54) (1.49) (1.49)
T3-F001 35% SG 35 1.53 1.47 1.40 1.40 1.33 1.73 1.80 1.73 1.67 1.67
(1.43) (1.40) (1.38) (1.38) (1.35) (1.49) (1.52) (1.49) (1.47) (1.47)
T4-F001 35% SG 70 1.47 1.40 1.33 1.33 1.27 1.87 1.80 1.73 1.67 1.60
(1.40) (1.38) (1.35) (1.35) (1.33) (1.54) (1.52) (1.49) (1.47) (1.45)
T5-F001 50% SG 50 1.47 1.40 1.33 1.27 1.20 1.80 1.73 1.67 1.60 1.73
(1.40) (1.38) (1.35) (1.33) (1.30) (1.52) (1.49) (1.47) (1.45) (1.49)
T6-F001 50% SG 100 1.53 1.47 1.40 1.27 1.33 1.73 1.67 1.67 1.60 1.53
(1.43) (1.40) (1.38) (1.33) (1.35) (1.49) (1.47) (1.47) (1.45) (1.43)

T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 1.47 1.40 1.33 1.27 1.20 1.87 1.80 1.73 1.67 1.60
(1.40) (1.38) (1.35) (1.33) (1.30) (1.54) (1.52) (1.49) (1.47) (1.45)
T8-Std check- N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 1.40 1.33 1.33 1.27 1.27 1.93 1.87 1.80 1.73 1.67
(1.38) (1.35) (1.35) (1.33) (1.33) (1.56) (1.54) (1.52) (1.49) (1.47)
T9-Control - 1.53 1.73 1.93 2.00 2.07 1.80 2.07 2.20 2.20 2.27
(1.43) (1.49) (1.56) (1.58) (1.60) (1.52) (1.60) (1.64) (1.64) (1.66)
C.D. NS NS NS NS NS NS NS NS NS NS
SE(m) - - - - - - - - - -

The effect of the present invention formulation on natural enemies in chilli crops was evaluated to assess its ecological safety. As indicated in Table 66, (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations exhibited minimal adverse effects on key beneficial insects (designated as A and B) across all treatments and application rates. While higher doses resulted in slight reductions in the populations of these natural enemies compared to the control, these changes were not statistically significant. The populations of both spiders and coccinellids remained relatively stable throughout the evaluation period, particularly in comparison to the untreated control, which exhibited a natural increase in population over time. Overall, F001 treatments were found to be safe for natural enemies, thereby supporting the maintenance of ecological balance within the chilli crop ecosystem.

Table 67: Effect of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG on Chilli Yield
Treatment Dose (gai /ha) Yield
(t/ha) Increase in yield over control (%) Yield Profit Common cost Cost per Insecticide Cost per treatment Net Return Total Cost Cost benefit Ratio


T1-F001 10% SG 10 3.50 38.16 57,750.00 16,000.00 76.99 300.26 41449.74 16300.26 2.54
(2.00)
T2-F001 10% SG 20 3.67 44.74 60,500.00 16,000.00 153.98 600.52 43899.48 16600.52 2.64
(2.04)
T3-F001 35% SG 35 3.80 50.00 62,700.00 16,000.00 212.33 828.09 45871.91 16828.09 2.73
(2.07)
T4-F001 35% SG 70 4.20 65.79 69,300.00 16,000.00 424.66 1656.17 51643.83 17656.17 2.92
(2.17)
T5-F001 50% SG 50 4.03 59.21 66,550.00 16,000.00 293.534 1144.78 49405.22 17144.78 2.88
(2.13)
T6-F001 50% SG 100 4.40 73.68 72,600.00 16,000.00 587.068 2289.57 54310.43 18289.57 2.97
(2.21)
T7-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% WG 100 3.95 55.92 65,175.00 16,000.00 1704 1704 47471.00 17704.00 2.68
(2.11)
T8-Std check-N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide 50% SG 100 3.85 51.97 63,525.00 16,000.00 398.836 1555.46 45969.54 17555.46 2.62
(2.09)
T9-Control - 2.53 41,800.00 16,000.00 - - 25800.00 16000.00 1.61
(1.74)
C.D. 0.231
SE(m) 0.079

The effect of the present invention formulation on chilli yield was evaluated, as summarized in Table 67. The application of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations resulted in a significant yield enhancement compared to the untreated control, with all treatments demonstrating increases. The highest yield, 4.40 t/ha, was achieved with the 50% SG formulation at 100 gai/ha (T6), corresponding to a 73.68% increase over the control. This was followed by 35% SG at 70 gai/ha (T4), showing yield increases exceeding 64%. These F001 treatments consistently outperformed the standard checks (50% WG and 50% SG formulations), which demonstrated yield improvements of 52% to 56%. The lowest yield improvement among F001 treatments was observed at the minimum dose (T1, 10 gai/ha), with a 38.16% increase over control. Overall, the F001 50% SG formulations were most effective in boosting the chilli yield.

Cost-Benefit analysis: The economic evaluation of treatments under varying environmental conditions or seasons demonstrated that N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide 50% SG at 100 gai/ha consistently emerged as the most economically viable option, achieving the highest cost-benefit ratio of 2.97, a yield of 4.40 t/ha, and a net return of ?54,310.43 per hectare. This was followed by 35% SG at 70 gai/ha, and exhibited strong economic performance, with cost-benefit ratios of 2.92 effectively balancing input costs with substantial yield gains. The standard check treatments demonstrated moderate effectiveness, with cost-benefit ratios of 2.68 and 2.62, which were outperformed by the leading F001 treatments. The control plot resulted in the lowest yield and net return, with a cost-benefit ratio of only 1.61. Overall, these results confirm that (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) 50% SG at 100 gai/ha consistently provides the most economically effective solution for pest management under the evaluated conditions.

Table 68: Evaluation of Phytotoxicity of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG in Chilli crop

Visual observations were recorded on 1, 3, 5, 7, and 10 days after the application (DAA) of the tested product. The parameters observed were leaf injury on tip/surface, stunting, necrosis, chlorosis, vein clearing, epinasty, hyponasty, and wilting based on the 0-10 scale given in the table below.

Score Phytotoxicity (percent) Score Phytotoxicity (percent)
0 No phytotoxicity 5 41-50
1 1-10 6 51-60
2 11-20 7 61-70
3 21-30 8 71-80
4 31-40 9 & 10 Complete Destruction

Table 69: Phytotoxic effect of various treatments on Chilli crop
Treatment Dose (g /ha) First Spray Second Spray
1 DAS 3 DAS 5 DAS 7 DAS 10 DAS 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
T1-F001 10% SG 10 0 0 0 0 0 0 0 0 0 0
T2-F001 10% SG 20 0 0 0 0 0 0 0 0 0 0
T3-F001 35% SG 35 0 0 0 0 0 0 0 0 0 0
T4-F001 35% SG 70 0 0 0 0 0 0 0 0 0 0
T5-F001 50% SG 50 0 0 0 0 0 0 0 0 0 0
T6-F001 50% SG 100 0 0 0 0 0 0 0 0 0 0
*DAS – Days after spray

As indicated in Table 69, the phytotoxicity evaluation of (N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide) SG (F001) formulations in chilli demonstrated that all tested formulations and doses of F001 (ranging from 10 to 100 gai/ha) exhibited no phytotoxic effects on chilli plants. Across both the first and second sprays, and on all observation days (1, 3, 5, 7, and 10 DAS), no symptoms such as chlorosis, necrosis, and leaf deformation, or wilting were recorded. This suggests that F001 is safe for use on cotton at the evaluated doses and does not negatively impact plant health

A contact angle analysis was performed to assess the wetting characteristics of N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide SG formulations with and without the penetrant. Measurements were conducted using the sessile drop method at 0.5% dilution via surface tensiometry. As illustrated in figures 2-3, the penetrant-containing formulation exhibited a mean contact angle of 82.48° (±1.20°). In contrast, the non-penetrant formulation demonstrated a significantly higher mean contact angle of 92.58° (±1.53°) as depicted in figures 4-5.

The observed reduction in contact angle for the formulation with the penetrant confirms that the present invention formulation has enhanced surface wetting properties, improved spreading behavior and superior surface coverage efficiency. Conversely, the contact angle in the absence of penetrant confirms diminished wettability. The contact angle analysis establish that the present invention formulation have significantly enhanced surface-wetting performance, particularly the 50% SG formulation, leading to increased biological efficacy through optimized interfacial contact on plant surfaces.

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

1. A soluble granule formulation comprising:
a. N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide;
b. at least one dispersing agent;
c. at least one wetting agent;
d. at least one defoamer; and
e. at least one penetrant.

2. The formulation as claimed in claim 1, wherein the N-(cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide is present in the range of 10 to 60% by weight.

3. The formulation as claimed in claim 1, wherein the dispersing agent is selected from a group consisting of ‘alpha’-olefin sulfonate; maleic acid, polymer with diisobutene, sodium salt (Sokalan CP 9); salt of naphthalene sulphonic acid condensation product; phenol sulphonic acid condensation product; sodium dioctyl sulfosuccinate; sodium lignosulfonate; polycarboxylic acid sodium salt; N-methyl fatty acid sarcosinate; ethoxylated polyarylphenol phosphate ester, polyoxyethylene alkyl ether phosphate; polyoxyethylene aryl ether phosphates; polyoxyethylene polyoxypropylene block copolymer phosphate; olefin-copolymer, sodium salt; and/or graft copolymer.

4. The formulation as claimed in claim 1, wherein the dispersing agent is present in the range of 5 to 9% by weight.

5. The formulation as claimed in claim 1, wherein the wetting agent is selected from the group consisting of sugar esters; alkyl polyglucoside; polyoxyethylene alkyl ethers; polyoxyethylene alkynyl ether; polyoxyethylene aryl ethers; polyoxyethylene fatty acid esters; polyoxyethylene polyoxypropylene block copolymers; polyoxyethylene polyoxypropylene alkyl ether; polyoxyethylene polyoxypropylene aryl ether; polyoxyethylene alkyl amines; polyoxyethylene fatty acid amide; sodium lauryl sulfate; sodium alkylbenzene sulphonate; polyoxyethylene alkyl ether sulfates; polyoxyethylene aryl ether sulfates; blend of alkyl sulphate and ethoxylates sulphate salt; amine salt of phosphate tristyryl phenol ethylated; calcium dodecyl benzene sulfonate; sodium naphthalene sulfonate and sodium naphthalene sulfonate formaldehyde condensate.

6. The formulation as claimed in claim 1, wherein the wetting agent is present in the range of 0.1 to 4% by weight.

7. The formulation as claimed in claim 1, wherein the defoamer is selected from the group consisting of polysiloxane, polydimethyl siloxane and organic fluorine compounds.

8. The formulation as claimed in claim 1, wherein the defoamer is present in the range of 0.1 to 3% by weight.

9. The formulation as claimed in claim 1, wherein the penetrant is selected from group consisting of cocoamine propyl amide, silicon-based adjuvants, esterified and/or etherified polyol alkoxylate compounds.,

10. The formulation as claimed in claim 1, wherein the penetrant is present in the range of 0.1 to 2% by weight.

11. The formulation as claimed in claim 1, further comprising at least one carrier.

12. The formulation as claimed in claim 11, wherein the carrier is selected from group consisting of natural minerals, synthetic minerals, inorganic salts, urea, solid polyoxyethylene, solid polyoxypropylene, polyethylene, polypropylene, citric acid, trisodium citrate, lactose (4-O-beta-D-Galactopyranosyl-D-glucose), starch, lignin, cellulose, cottonseeds hulls, wheat flour, soybean flour, wood flour, walnut shell flour, plant powders, sawdust, coconut shellflower, corn cob, and/or tobacco stem.

13. A method for preparing a soluble granule formulation comprising the steps of:
a. mixing N-(cyanomethyl)-4-(trifluoromethyl)pyridine-3-carboxamide, at least one dispersing agent, at least one wetting agent, and at least one defoamer to form a mixture;
b. milling and homogenizing the mixture; and
c. preparing a dough by adding at least one penetrant and required amount of distilled water to the homogenized mixture and granulating the dough using an extruder to obtain granules.