Sign In to Follow Application
View All Documents & Correspondence

Synergistic Insecticidal Composition Of Pyriproxyfen, Tolfenpyrad And Diamide, And Process Of Preparation Thereof

Abstract: ABSTRACT A diamide insecticidal composition of pyriproxyfen, tolfenpyrad and preparation method thereof The present invention relates to a diamide insecticidal composition of pyriproxyfen, tolfenpyrad and preparation method thereof and agrochemically acceptable excipients and a process of preparing said composition. The present invention further relates to an insecticidal composition that offers broad spectrum control of insect-pests and mites in one shot application, gives residual control i.e. longer duration of control, prevents or causes delayed development of resistance to insects against insecticides with a specific site/ mode of action, gives synergistic control i.e. grams of active ingredients required are less to achieve desired level of control, gives immediate protection to crops, has improved rain-fastness properties, is environment-friendly, and is safe to the crops.

Get Free WhatsApp Updates!
Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
11 August 2022
Publication Number
07/2024
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

RAJDHANI PETROCHEMICALS PRIVATE LIMITED
6, Lalita Complex, Rasala Road, Navrangpura, Ahmedabad-380009, Gujarat, India.

Inventors

1. PATEL, Dipakkumar
6, Lalita Complex, Rasala Road, Navrangpura, Ahmedabad-380009, Gujarat, India.
2. SHAH, Kenal V
6, Lalita Complex, Rasala Road, Navrangpura, Ahmedabad-380009, Gujarat, India.
3. SHAH, Bhavesh V
6, Lalita Complex, Rasala Road, Navrangpura, Ahmedabad-380009, Gujarat, India.
4. DABODHIA, Kawarlal
6, Lalita Complex, Rasala Road, Navrangpura, Ahmedabad-380009, Gujarat, India.

Specification

DESC:FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. TITLE OF THE INVENTION: “A diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof”
2. APPLICANT:
(a) Name : RAJDHANI PETROCHEMICALS PRIVATE LIMITED
(b) Nationality : INDIAN
(c) Address : 6, LALITA COMPLEX, RASALA ROAD, NAVRANGPURA, AHMEDABAD-380009 Gujarat, India
PROVISIONAL
The following specification describes the invention. þCOMPLETE
The following specification particularly describes the invention and the manner in which it is to be performed.


FIELD OF INVENTION
The present invention relates to a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof . More specifically, the present invention relates to an insecticidal composition comprising bioactive amounts of pyriproxyfen or its agrochemically acceptable salts thereof, tolfenpyrad or its agrochemically acceptable salts thereof, one or more insecticide/s selected from the group of diamides, and agrochemically acceptable excipients; and a process of preparing said composition which is environment-friendly and provides synergistic and broad spectrum control of insect-pests and mites in one shot application.

BACKGROUND OF THE INVENTION
Since the practice of agriculture began, humans have battled pests and diseases that threaten the sustainable food supply. In the process of agricultural production, plant diseases and pests damage the roots, stems, leaves and other parts of plants, as well as fruit, seeds, tubers and other reproductive organs, so that the crop yield sharply reduces, and the quality drops seriously. The protection of crops and its produce from insect pest damage is essential in agriculture produce enhancement. Each year, insects, plant pathogens, and weeds, destroy more than 40% of all food production. The challenge of growing enough food to feed the world’s expanding population has driven the need to improve crop yield and quality through the control of a wide range of insect pests.
At present, in agricultural production, the application of pesticides is an important means to prevent and control plant diseases and insect pests. Insecticides are pesticides that are formulated to kill, harm, repel or mitigate one or more species of insect. The modes of action of insecticides are classified by the Insecticide Resistance Action Committee (IRAC).
However, a major problem with insecticides is the tendency of some target insect populations to develop resistance as their susceptible members are killed off and those resistant strains that survive, multiply eventually perhaps to form a majority of the population. With the repeated use of a large number of existing pesticides and the improper application of pesticides by some farmers, there is a relatively large resistance to the existing common pesticides, and the difficulty of chemical control becomes increasingly greater. The development and manufacture of effective, safe to humans, and environment-friendly pesticides has been a challenge to feed the growing population of our planet.
Combination of insecticides are used to broaden the spectrum of control of insects, to improve the pest control with synergistic effect, reduce dosage, thereby reducing environmental impact, decrease chances of resistance development and to enhance residual control to lesser the number of sprays for crop protection and minimizing the pesticidal load in ecosystem.
WO 20211155106 relates to pyridine compounds for controlling invertebrate pests. This disclosure relates to certain pyridine compounds, their N-oxides, salts and compositions suitable for agronomic and nonagronomic uses, and methods of their use for controlling invertebrate pests in agronomic and nonagronomic environments.
WO 20211067678 relates to an insecticidal composition comprising 2 wt.% to 50 wt.% of diamide insecticide active ingredient and a phosphate ester.
CN112616845A relates to a pesticide composition containing pyrazolecarboxamide insecticide and application of pesticide composition. It discusses pesticide composition containing pyrazolyl amide insecticides, comprising dimpropyridaz, of chemical formula 1-(1,2 dimethylpropyl)-N- Ethyl-5-methyl-N-pyridazin-4-yl-pyrazole-4-carboxamide and at least an active compound selected from a group of compounds.
US 202110267207 Al relates to combinations of ryanodine receptor ligand inhibitor insecticides in combination with at least one Nicotinic Acetylcholine receptor agonist/antagonist and at least another insecticidal compound.
There is however a need for improvement of these combinations. The insecticides currently in use are not that effective; and, due to their prolonged indiscriminate and non-judicious use, many insect-pests have developed resistance to such commonly used insecticides. The use of insecticides for the prevention and control of insect-pests is thereby becoming increasingly difficult.
There is a long felt need to develop effective pesticidal combinations for controlling the harmful pests in plants that demonstrate high efficacy, are environmentally safe and can be advantageously formulated. The present inventors have developed an effective pesticidal combination which ameliorates the aforesaid shortcomings of the prior art.

OBJECT OF THE INVENTION
The principal object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof.
Another object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that gives broad spectrum control of insect-pests and mites in one shot application.
Further object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that gives residual control i.e. longer duration of control.
Another object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof which prevents or causes delayed development of resistance to insects against insecticides with a specific site/ mode of action.
Further object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that gives synergistic control; i.e. grams of active ingredients required are less to achieve desired level of control.
Another object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that gives immediate protection to crops.
Further object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that has improved rain-fastness properties.
Another object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof with environment-friendly formulations; i.e. formulations are without organic solvent as carrier.
Yet another object of the present invention is to provide a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof that is safe to the crops.
Still another object of the present invention is to provide a process of preparing a stable and non-phytotoxic formulation.

SUMMARY OF THE INVENTION
In light of the foregoing background, the following presents a simplified summary of the present disclosure in order to provide a basic understanding of some aspects of the disclosure. This summary is not an extensive overview of the disclosure. It is not intended to delineate the scope of the disclosure. The following summary merely presents some concepts of the disclosure in a simplified form as a prelude to the more detailed description provided below.
The present invention provides a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof comprising bioactive amounts of pyriproxyfen or its agrochemically acceptable salts thereof, tolfenpyrad or its agrochemically acceptable salts thereof, one or more insecticide/s selected from the group of diamides, and agrochemically acceptable excipients; and a process of preparing said composition.
The formulation for the insecticidal composition is selected from Capsule suspension (CS), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion, oil in water (EW), Jambo balls or bags (bags in water soluble pouch), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (SC), Suspo-emulsion (SE), Soluble concentrate (SL), Wettable granule/Water dispersible granule (WG/WDG), Water soluble granule (SG), Water soluble powder (SP), Wettable powder (WP), A mixed formulation of CS and SC (ZC), A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granule (GR) / Soil Applied Granules (SAG), and Controlled release granules (CR).
The process for preparing the present insecticidal composition can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However, all such variations and modifications are still covered by the scope of present invention.
The present invention provides a diamide insecticidal composition of pyriproxyfen and tolfenpyrad and preparation method thereof which offers broad spectrum control of insect-pests and mites in one shot application, gives residual control i.e. longer duration of control, prevents or causes delayed development of resistance to insects against insecticides with a specific site/ mode of action, gives synergistic control i.e. grams of active ingredients required are less to achieve desired level of control, gives immediate protection to crops, has improved rain-fastness properties, is environment-friendly, and is safe to the crops.

DETAILED DESCRIPTION OF THE INVENTION
Before explaining the present invention in detail, it is to be understood that the invention is not limited in its application to the details of the parts illustrated. The invention is capable of other embodiments, as described above and of being practiced or carried out in a variety of ways. It is to be understood that the phraseology and terminology employed herein is for the purpose of description and not to limitation. The invention can have various embodiments and they can be performed as described in the following pages of the complete specification.
The terms and words used in the following description are not limited to the bibliographical meanings, but, are merely used by the inventors to enable a clear and consistent understanding of the invention. Accordingly, it should be apparent to those skilled in the art that the following description of exemplary embodiments of the present invention are provided for illustration purpose only and not for the purpose of limiting the scope of the invention.
It is to be understood that the singular forms "a", "an", and "the" include plural reference unless the context clearly dictates otherwise.
Features that are described and/or illustrated with respect to one embodiment can be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used in this specification is taken to specify the presence of stated features, steps or components but does not preclude the presence or addition of one or more other features, steps, components or groups thereof.
"Bioactive amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.
As used herein, “weight percent”, “wt-%”, “percent by weight”, “% by weight”, and variations thereof refer to the concentration of a substance as the weight of that substance divided by the total weight of the composition and multiplied by 100. It is understood that, as used here, “percent”, “%”, and the like are intended to be synonymous with “weight percent”, “wt-%”, etc.
The term "insects" as used herein, includes all organisms in the class "Insecta".
The term "animal pest" includes arthropods, gastropods, and nematodes. Preferred animal pests according to the invention are arthropods, preferably insects and arachnids, in particular insects. Insects, which are of particular relevance for crops, are typically referred to as crop insect pests.
The term "insecticidal" as used herein, refers to the ability of an insecticide to increase mortality or inhibit growth rate of insects.
To "control" or "controlling" pests means to inhibit, through a toxic effect, the ability of pests to survive, grow, feed, and/or reproduce, or to limit pest related damage or loss in crop plants. To "control" pests can or can not mean killing the pests, although it preferably means killing the pests.
The term 'plants' as used herein, refers to all physical parts of a plant, including seeds, seedlings, saplings, roots, tubers, stems, stalks, foliage and fruits. The term "plant" is to be understood as including wild type plants and plants, which have been modified by either conventional breeding, or mutagenesis or genetic engineering, or by a combination thereof.
The term "crop" refers to both, growing and harvested crops.
The present invention provides a diamide insecticidal composition of pyriproxyfen, tolfenpyrad and diamide, comprising 5% to 15% w/w pyriproxyfen or its agrochemically acceptable salts, 5% to 15% w/w tolfenpyrad or its agrochemically acceptable salts, 1% to 20% w/w at least one insecticide selected from diamide group, and agrochemically acceptable excipients.
Pyriproxyfen, (2-[1-(4-phenoxyphenoxy) propan-2-yloxy]pyridine) is an insect growth regulator.

It mimics insect juvenile growth hormone and halts development during metamorphosis and larval development, thereby stopping young insects from maturing into adults. It can affect an insect if it is touched or eaten and mostly affects young insects and eggs. It is rarely toxic to adult insects. It can concentrate in female flea ovaries, causing non-viable eggs to be produced. It disturbs egg-laying and egg-hatch and keeps young insects from growing into adult forms. This prevents target insects from multiplying. It has been registered for use in pesticides by the Environmental Protection Agency (EPA) since 1995.
Tolfenpyrad, (4-chloro-5-ethyl-2-methyl-N-[[4-(4-methylphenoxy) phenyl] methyl] pyrazole-3-carboxamide) is a pyrazole insecticide, and was discovered by Mitsubishi Chemical Corporation in 1991. It is an aromatic amide obtained by formal condensation of the carboxyl group of 4-chloro-3-ethyl-1-methylpyrazole-5-carboxylic acid with the amino group of 1-[4-(4-methylphenoxy) phenyl] methylamine. Tolfenpyrad is a meti acaricide/insecticide with contact mode of action. The compound acts mainly through the inhibition of the mitochondrial electron transport system.

As a pesticide, tolfenpyrad has relatively broad activity against egg, larval, nymphal and adult stages of various arthropods (including Hemiptera, Coleoptera, Diptera, Lepidoptera, Thysanoptera and Acarina), and has been applied to various infested crops. Tolfenpyrad halts feeding damage immediately and oviposition within hours after application. It has an excellent know-down effect; pests are controlled usually within 24 to 48 hours. This chemical was developed in Japan and was first approved in 2002; it has been registered for commercial use in several countries.
Diamide insecticides selectively acting on insect ryanodine receptors (RyR) were launched to the market more than 10 years ago. Particularly targeted for the control of lepidopteran pest species in diverse agronomic and horticultural cropping systems, they are now globally registered in many countries and provide reliable control levels in most settings. One or more insecticide(s) is selected from the diamides group including, but not limited to, ryanodine receptor modulators; chlorantraniliprole, cyantraniliprole, cyclaniliprole, tetraniliprole, and flubendiamide.
The combination of the present invention is formulated in a manner which suits the specific application. The formulation is selected from Capsule suspension (CS), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion, oil in water (EW), Jambo balls or bags (bags in water soluble pouch), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (SC), Suspo-emulsion (SE), Soluble concentrate (SL), Wettable granule/Water dispersible granule (WG/WDG), Water soluble granule (SG), Water soluble powder (SP), Wettable powder (WP), A mixed formulation of CS and SC (ZC), A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granule (GR) / Soil Applied Granules (SAG), Controlled release granules (CR).

More particularly, the formulation is selected from oil dispersion (OD), suspo-emulsion (SE) and suspension concentrate (SC).

Lists of agrochemically acceptable excipients used in the oil dispersion (OD) formulation:

The OD formulation of the present invention comprises agrochemically acceptable excipients including, but not limited to, wetting-spreading-penetrating agents, solvents, emulsifiers, dispersing agents, stabilizers, anti-foaming agent, anti-freezing agent, preservatives, buffering agent, and optionally polar cosolvents.

The wetting-spreading-penetrating agents for oil dispersion (OD) is selected from but not limited to the group consisting of , organic silicone, trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxane heptamethyl, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, or mixture thereof. The organosilicone agents have super ability of spreading by drastically reducing the water surface tension. These enhance wetting and absorption of active ingredient through stomatal penetration. This will improve a spray application by modifying the wetting and spreading characteristics, the result being a more uniform spray deposit even at reduced spray volume. It also ensures thorough coverage without excessive runoff of the spray. They are safe to the human beings and environment. The most preferred super wetting-spreading-penetrating agent is polyalkyleneoxide modified heptamethyl trisiloxane (modified trisiloxane).

The solvent for oil dispersion (OD) is selected from but not limited to the group consisting of, blend of pongamia oil and palm oil; blend of pongamia oil and mahua oil; blend of pongamia oil and jojoba (Simmondsia chinensis); blend of pongamia oil and vegetable oil; blend of palm oil and mahua oil; blend of palm oil and jojoba oil; blend of palm oil and vegetable oil; blend of pongamia oil, palm oil and mahua oil; blend of pongamia oil, palm oil and jojoba oil; and blend of pongamia oil, palm oil and vegetable oil. The vegetable oil can be any one or mixture of two or more selected from soybean (Glycine max) oil, groundnut (Arachis hypogaea) oil, rapeseed (Brassica napus subspecies) oil, mustard (Brassica juncea) oil, sesame (Sesamum indicum) oil, corn (Zea mays) oil, rice (Oryza sativa) bran oil, castor (Ricinum communis) seed oil, cotton (Gossypium hirsutum) seed oil, linseed (Linum usitatissimum), coconut (Cocos nucifera) oil, sunflower (Helianthus annuus) oil, safflower (Carthamus tinctorius) seed oil, eucalyptus (Eucalyptus globulus) oil, olive (Olea europaea) oil, jatropha (Jatropha curcas) oil, kapok (Ceiba pentandra) oil, papaya (Carica papaya) seed oil, tea seed (Camellia oleifera) oil, garlic acid (Allium sativum), ginger oil (Zingiber officinale), d-limonene, citronella oil or ceylon ironwood (Mesua ferrea) oil. As solvent for the present formulation, the oil mixtures can be alkylated or ethoxylated or epoxylated or esterified. For example, methyl ester of pongamia oil and vegetable oil, methyl ester of palm oil and vegetable oil, methyl ester of pongamia oil and palm oil, methyl ester of pongamia oil, palm oil and vegetable oil or mixture thereof.

The emulsifier for oil dispersion (OD) is selected from but not limited to the group consisting of , castor oil ethoxylates, alcohol ethoxylates, fatty acid ethoxylates, sorbitan ester ethoxylates, sulphosuccinate, calcium salts of dodecylbenzene sulphonate, alkylammonium salts of alkylbenzene sulphonate, alkylsulphosuccinate salts, ethylene oxide-propylene oxide block copolymers, ethoxylated alkylamines, octylphenol ethoxylate, ethoxylated alkyl phenols, ethoxylated sorbitol oleates, polyoxyethylene sorbitan monolaurate or mixture thereof.

The surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier for re-aggregation of particles. The dispersing agent for oil dispersion (OD) is selected from but not limited to the group consisting of, preparation of condensed naphthalene sulfonate, propoxylated ethoxylated copolymer monoalkylether (ethylhexanol), alkyl sulfonates, alkyl benzene sulfonates, alkyl aryl sulfonates, alkylphenolalkoxylates, tristyrylphenol ethoxylates, natural or synthetic fatty ethoxylate alcohols, natural or synthetic fatty acid alkoxylates, natural or synthetic fatty alcohols alkoxylates, alkoxylated alcohols, n-butyl alcohol poly glycol ether, block copolymers, ethylene oxide-propylene oxide block copolymers ethylene oxide-butylene oxide block copolymers, fatty acid-polyalkylene glycol condensates, polyamine-fatty acid condensates, polyester condensates, salts of polyolefin condensates, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide or mixture thereof.

The stabilizer for oil dispersion (OD) is selected from but not limited to the group consisting of, hectorite clay, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.

The antifoaming agent for oil dispersion (OD) is selected from but not limited to the group consisting of, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane or mixture thereof.

The anti-freezing agent for oil dispersion (OD) is selected from but not limited to the group consisting of , ethylene glycol, propane diols, glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, glycerine, urea, magnesium sulfate heptahydrate, sodium chloride or mixture thereof.

The preservative for oil dispersion (OD) is selected from but not limited to the group consisting of, 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenylphenate, 5-chloro-2-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, butyl hydroxyl toluene or mixture thereof.

The buffering agent for oil dispersion (OD) is selected from but not limited to the group consisting of, citric acid, sodium carbonate, sodium bicarbonate, sulphuric acid, hydrochloric acid, sodium hydroxide, potassium hydroxide, acetic acid, sorbic acid or mixture thereof.

The polar cosolvent can be optionally present, for oil dispersion (OD) is selected from but not limited to the group consisting of, cyclohexanone, acetophenone, butanol, n-octanol, n-propanol, 1-hexanol, propylene carbonate, n-methyl-2-pyrrolidone or mixture thereof.

However, those skilled in the art will appreciate that it is possible to utilize additional agrochemically acceptable excipients without departing from the scope of the present invention. Such agrochemically acceptable excipients can be in the range from 1% to 99% of the total weight of the composition.

More particularly, the present invention also refers to the method for preparation of oil dispersion (OD) formulation as describing the following steps:

Manufacturing process for oil dispersion (OD) formulation:

Part A-Preparation of the liquid premix
Step 1- The oil (methyl ester of pongamia oil and vegetable oil; or methyl ester of palm oil and vegetable oil; or methyl ester of pongamia oil and palm oil; or methyl ester of pongamia oil, palm oil, and vegetable oil) is charged as a solvent, with or without co-solvent into a vessel with an anchor stirrer.
Step 2- The emulsifier(s)/super wetting-spreading-penetrating agent(s) (polyalkyleneoxide modified heptamethyl trisiloxane) and dispersing agent(s) are added under stirring condition until all the ingredients get completely dissolved.

Part B-Preparation of the slurry
Step 1- the liquid premix is charged into a second vessel which is equipped with a cooling and heating device of a high shear stirrer.
Step 2- The active ingredient(s) are added and homogenized thoroughly. The mixture is pre-milled and a particle size distribution is achieved by the final milling practised along with a bead mill/sand mill/attritor as required by the specification.

Part C-Preparation of the Thickener gel
Step 1- The remaining oil is charged to the vessel which is equipped with a high shear stirrer.
Step 2- Add gradually The thickening agent is gradually added by throughout maintaining high-shear mixing. The stirring is continued until thoroughly mixed.
Step 3- The thickener(s) is added under stirring condition. Further, the gel is allowed to get swell whilst maintaining the mixing.

Part D-Preparation of the final formulation
Step 1- The thickener gel solution is added into milled slurry and the mixture is dispersed by using a high shear stirrer.
Step 2- The finished formulation is checked with specification.
Step 3- The material is packed in its required package sizes when approved.
The process for preparing the present diamide insecticidal composition can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However, all such variation and modification is still covered by the scope of present invention.

Lists of agrochemically acceptable excipients used in the suspo-emulsion (SE) formulation:

The SE formulation of the present invention comprises agrochemically acceptable excipients including, but not limited to, super wetting cum spreading agent cum penetrant cum co-solvent, green solvent cum emulsifier, wetting agent cum penetrant, dispersing agent, suspending agent, anti-freezing agent, antifoaming agent, preservatives, thickeners, stabilizer, and buffering agent.

The super wetting cum spreading agent cum penetrant cum co-solvent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, blend of methylated or ethylated seed oil, organo-silicone surfactant and emulsifier cum surfactant. The methylated or ethylated seed oil includes any one or blend of two or more seed oil. The seed oil can be selected from but not limited to soybean (Glycine max) oil, groundnut (Arachis hypogaea) oil, rapeseed (Brassica napus subspecies) oil, mustard (Brassica juncea) oil, sesame (Sesamum indicum) oil, corn (Zea mays) oil, rice (Oryza sativa) bran oil, castor (Ricinum communis) seed oil, cotton (Gossypium hirsutum) seed oil, linseed (Linum usitatissimum), coconut (Cocos nucifera) oil, kapok (Ceiba pentandra) oil, papaya (Carica papaya) seed oil, tea seed (Camellia oleifera) oil, sunflower (Helianthus annuus) oil, safflower (Carthamus tinctorius) seed oil, eucalyptus (Eucalyptus globulus) oil, olive (Olea europaea) oil, jatropha (Jatropha curcas) oil, garlic (Allium sativum) oil, ginger (Zingiber officinale) oil, d-limonene, citronella oil or ceylon ironwood (Mesua ferrea) oil, mahua (Madhuca longifolia) oil. The content of methylated or ethylated seed oil varies from 60 to 80% w/w. The organosilicone surfactant includes trisiloxane ethoxylate, polyalkyleneoxide modified trisiloxane, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, polyalkyleneoxide modified heptamethyl trisiloxane, and polyether modified polysiloxane. It can be liquid or powder form. The content of organo silicone surfactant varies from 20 to 35% w/w. Emulsifier cum surfactant, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulphate, sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate, and alkyl phenol ethoxylate, (1 to 5% w/w) added to bridge the vegetable seed oil and organosilicon surfactant. Example of super wetting cum spreading agent cum penetrant cum co-solvent include, but not limited to, blend of methylated seed oil (75% w/w) and polyalkyleneoxide modified trisiloxane (20% w/w) and ethoxylated fatty alcohol (5% w/w), blend of methylated seed oil (73% w/w) and polyalkyleneoxide modified heptamethyl trisiloxane (23% w/w) and sodium dioctyl sulfosuccinate (4% w/w), blend of methylated rapeseed oil (72% w/w) and polyether modified polysiloxane (25% w/w) and sodium lauryl sulphate (3% w/w) or mixture thereof.

The green solvent cum emulsifier for suspo-emulsion (SE) is selected from the group consisting of but not limited to, N,N decanamide chemistry (Armid series), propylene carbonate (Jeffsol series) or 2 ethylhexyl lactate base solvent (purasolve series). The examples of N,N decanamide chemistry (Armid series) are N,N-Dimethyloctanamide, N,N-Dimethylethylamine, N,N-Dimethylethanamide, N,N-Dimethylmethanamide Dimethylformamide or mixture thereof.

The wetting agent cum penetrant for suspo-emulsion (SE) is selected from the group consisting of but not limited to, polyoxyethylene, polyhydric alcohol. The polyoxyethylene surfactant can, for example, be a polyoxyethylene alkyl phenyl ether, a polyoxyethylene fatty acid ester, formalin condensate of a polyoxyethylene alkyl phenyl ether, a polyoxyethylene alkyl ether, a polyoxyethylene aryl ether, polyoxyethylene (mono-, di- or tri-)phenyl phenyl ether, polyoxyethylene (mono-, di- or tri-)benzyl phenyl ether, polyoxypropylene (mono-, di- or tri-)benzyl phenyl ether, polyoxyethylene (mono-, di- or tri-)styryl phenyl ether, polyoxypropylene (mono-, di- or tri-)styryl phenyl ether, a polymer of polyoxyethylene (mono-, di- or tri-)styryl phenyl ether, a polyoxyethylene/polyoxypropylene block polymer, an alkylpolyoxyethylene/polyoxypropylene block polymer ether, an alkylphenylpolyoxyethylene/polyoxypropylene block polymer ether, a polyoxyethylene bisphenyl ether, a polyoxyethylene resinate, a polyoxyethylene fatty acid amide, an alkylphenoxy polyethoxy ethanol, polyoxyethylene nonylphenoxy ether, a polyoxyethylene alkylamine or a polyoxyethylene rosin ester. Specific examples of the polyoxyethylene alkyl phenyl ether include polyoxyethylene nonyl phenyl ether, polyoxyethylene nonyl phenoxy ether, 4-nonylphenyl-polyethylene glycol, octylphenoxypolyethoxyethanol, polyoxyethylene nonyl pheno, polyoxyethylene octyl phenyl ether, polyoxyethylene styryl phenyl ether and polyoxyethylene alkyl phenyl ether. Specific examples of the polyoxyethylene fatty acid ester include a lanolin fatty acid polyethylene glycol ester, a polyoxyethylene C16-C18 fatty acid ester, a polyoxyethylene resinate and a polyoxyethylene fatty acid ester. Specific examples of the polyoxyethylene alkylamine include polyoxyethylene oleylamine. Specific examples of the polyoxyethylene alkyl ether include polyoxyethylene tridecyl ether, an alkyl aryl polyoxyalkene ether, and N,N-bis2-omega-hydroxypolyoxyethylene alkylamine. The polyhydric alcohol surfactant can, for example, the polyhydric alcohol surfactant include a polyoxyethylenehexitan fatty acid ester, a polyoxyethylene sorbitan fatty acid ester, a sorbitan fatty acid ester, mixture with a polyoxyethylene fatty acid ester and dialkyldimethylammonium polynaphthylmethanesulfonate, polyethylene glycol isotridecyl ester, polyethylene glycol monooleate, polyethylene glycol monostearate and a mixture of a polyhydric alcohol fatty acid ester and a polyhydric alcohol polyethylene oxide fatty acid ester. The preferred wetting agent cum penetrants are a polymer of polyoxyethylene (mono-, di- or tri-)styryl phenyl ether, a polyoxyethylene/polyoxypropylene block polymer, polyoxyethylene nonyl phenyl ether, a polyoxyethylenehexitan fatty acid ester, a polyoxyethylene sorbitan fatty acid ester, a sorbitan fatty acid ester, mixture with a polyoxyethylene fatty acid ester and a dialkyldimethylammonium polynaphthylmethanesulfonate, polyethylene glycol isotridecyl ester or mixture thereof.

The dispersing agent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, polyesters, polyamides, polycarbonates, polyurea and polyurethanes, acrylic polymers and copolymers, styrene copolymers, butadiene copolymers, polysaccharides, starch and cellulose derivatives, vinylalcohol, vinylacetate and vinylpyrrolidone polymers and co=polymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymers and mixtures thereof. Examples of preferred polymers are acrylate polymers, poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below, poly(styrene-co maleic anhydride), cellulosic polymers, ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono, di, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), polyarylphenyl ether sulphate ammonium salt, alkyl resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present invention include biodegradable polyesters, starch, polylactic acid starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch ester-aliphatic polyester blends, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof. The examples of dispersing agents are alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO block copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, and nonylphenol polyglycol ether with 9-10 moles ethylene oxide or mixture thereof.

The suspending agent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, aluminum magnesium silicate, bentonite clay, silica, silicone dioxide, and attapulgite clay or mixture thereof.

The anti-freezing agent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, and polyethylene glycol), propane diols, glycerin, urea, magnesium sulfate heptahydrate, and sodium chloride or mixture thereof.

The antifoaming agent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone emulsion, vegetable oil based antifoam, and tallow based fatty acids or mixture thereof.

The preservative for suspo-emulsion (SE) is selected from the group consisting of but not limited to, 1,2-benzisothiazol-3(2H)-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2- methyl-4-isothiazolin-3-one, propionic acid and its sodium salt, sorbic acid and its sodium or potassium salt, benzoic acid and its sodium salt, p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide, sodium benzoate, potassium sorbate, para hydroxy benzoates or mixture thereof.

The thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clay and silica. Examples of these types of materials include, but not limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds, synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but not limited to, guar gum, locust bean gum, carrageenan, xanthan gum, alginates, methyl cellulose, sodium carboxymethyl cellulose (SCMC), hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixture thereof.

The stabilizer for suspo-emulsion (SE) is selected from the group consisting of but not limited to, butylated hydroxytoluene (BHT), epoxidized soybean oil (ESBO), epichlorohydrin or mixture thereof.

The buffering agent for suspo-emulsion (SE) is selected from the group consisting of but not limited to, calcium hydroxyapatite, potassium dihydrogen phosphate, sodium hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphates, amine monomers, lactate dehydrogenase, magnesium hydroxide or mixture thereof.

However, those skilled in the art will appreciate that it is possible to utilize additional agrochemically acceptable excipients without departing from the scope of the present invention. Such agrochemically acceptable excipients can be in the range from 1% to 99% of the total weight of the composition.

More particularly, the present invention also refers to the method for preparation of suspo-emulsion (SE) formulation as describing the following steps:

Manufacturing process for suspo-emulsion (SE) formulation:

Step 1: Gel solution preparation
The thickening agent is added in to DM water followed by preservative and homogenized until dissolved completely andto be kept for 12-18 hours prior to use.

Step 2: Emulsifiable concentrate (EC) premix
The green solvent cum emulsifier and wetting/spreading/co-solvent is charged into a vessel and a required quantity of technical (active ingredient 1) is added and mixed until completely homogenized.

Step 3: Suspension concentrate (SC) Premix:
The required quantity of DM water is charged into a designated vessel for suspension concentrate production.
The dispersing agent(s), wetting cum penetrating agent and antifreezing agent(s) are added and homogenized the contents for 45 – 60 minutes using high shear homogeniser.
Further, the required quantity of technical (active ingredient 2)and suspending agent(s) are added into this premix and homogenized for 30-45 minutes.
A required quantity of antifoaming agent(s) is added and the material is grinded in dyno mill till desired particle size is achieved.
The remaining quantity of antifoaming agent(s) is added after milling to avoid foaming.

Step 4: SE formulation:
The SC premix is charged into other vessel while the EC premix is added into SC and homogenized slowly to avoid phase change. Further, the gel solution is added and the final product is ready.

Lists of agrochemically acceptable excipients used in the suspension concentrate (SC) formulation:

The wetting agent for suspension concentrate (SC) is selected from the group consisting of ethylene oxide/propylene oxide block copolymer, polyarylphenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulfate and sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate, organosilicons surfactants, wetting-spreading-penetrating agent trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified trisiloxane, polyalkyleneoxide modified polydimethylsiloxane, trisiloxane ethoxylate, polyoxyethylene methyl polysiloxane, polyether polymethyl siloxane copolymer, polyether modified polysiloxane; can or cannot be in modified form, can be liquid or powder form or mixture thereof.

The dispersing agent for suspension concentrate (SC) is selected from the group consisting of naphthalenesulfonic acid, sodium salt condensated with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide or mixture thereof.
The suspending agent for suspension concentrate (SC) is selected from the group consisting of aluminum magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.

The antifoaming agent for suspension concentrate (SC) is selected from the group consisting of silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethyl siloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane or mixture thereof.

The anti-freezing agent for suspension concentrate (SC) is selected from the group consisting of ethylene glycol, propane diols, glycerin or the urea, glycol,monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, glycerin, urea, magnesium sulfate heptahydrate, sodium chloride or mixture thereof.

The preservatives for suspension concentrate (SC) is selected from the group consisting of 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one or mixture thereof.

The thickeners for suspension concentrate (SC) is selected from the group consisting of xanthan gum, PVK, carboxymethyl celluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch, acacia gum or mixture thereof.

The humectant for suspension concentrate (SC) is selected from the group consisting of urea, humic acid, glycerol, lactose or mixture thereof.

More particularly, the present invention also refers to the method for preparation of suspension concentrate formulation as describing the following steps:

Manufacturing process for suspension concentrate (SC) formulation:
Step 1: Gel preparation: A required quantity of water is charged to a vessel which is equipped with a high shear stirrer whilst the agitation is initiated. A required amount of preservative(s) is added and mixed to form a homogenous mixture. A required amount of thickener(s) is added and mixed vigorously to achieve wetness.
Step 2: A required quantity of water is charged to a vessel which is equipped with a bulk agitator and a high shear homogenizer; initiated the agitation. Further, a required amount of an anti freezing agent(s) is added and mixed to achieve uniformity. Moreover, the antifoaming agent(s) is added whilst ensuring that it is well dispersed. The wetting and dispersing agent(s) are added and mixed to achieve uniformity whilst ensuring that the dispersing agent is fully dispersed.
Step 3: The active ingredients are added and the agitation of the vessel contents are continued until all the components get dissolved. The pre-mix is milled through a colloid mill and subsequently through a dyno mill to meet the specified particle size.
Step 4: The remaining antifoaming agent(s) is added to this SC mill base to a vessel which is equipped with the bulk agitator and mixed to achieve uniformity. The required amount of 2% aqueous pre-gel and suspending agent(s) are added and the agitation is continued until the formulation is homogeneous and has reached the target viscosity.
Step 5: The final product is submitted for QC approval.
Step 6: The material is packed in its required package sizes when received approval.

EXAMPLES
The present invention has been described with reference to specific embodiment which is merely illustrative and not intended to limit the scope of the invention as defined in the present complete specification.

Biological Examples:
The diamide insecticidal action of the inventive mixtures can be demonstrated by the experiments below. A synergistic effect exists wherever the action of a combination (ready-mix) or tank mix of active ingredient is greater than the sum of the action of each of the components alone. Therefore, a diamide insecticidal effective amount or an effective amount of a diamide insecticidal composition or combination is an amount that exhibits greater pesticide activity than the sum of the pesticide activities of the individual components.

In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two or three active components can be calculated as follows:

The objective of the present studies is to study the synergism, residual control, spectrum of activity and benefits of compositions comprising of pyriproxyfen, tolfenpyrad and at least one insecticide selected from group of diamide were analyzed.

Example 1: Control of insect-pests in okra crop.
Crop : Okra
Location : Chaklasi, Nadiad, Gujarat
No. of treatments : 24
Crop age : 65 days after sowing.
Spray water volume : 430 liter per hectare
Method of application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.

Observation methods:
Whitefly (Bemesia tabaci) control (%): Count the number of live whitefly (nymphs and adults) per leaf, record the observations from 3 leaves per plant and 10 plants per plot.

Jassid (Amrasca biguttula biguttula) control (%): count the number of live jassid (nymphs and adults) per leaf, record the observations from 3 leaves per plant and 10 plants per plot. Record the observations on 7th day after application.

Fruit borer (mixed infestation of Spodoptera exigua & Helicoverpa armigera) larval control (%): Count the number of live larvae per plant. Record observations from 10 plants per plot on 7th day after application.

Marketable fruit count: count the number of healthy marketable fruits per plant, record the observations from 5 plants per plant.

T1: Composition of pyriproxyfen 6%+ tolfenpyrad 12%+ chlorantraniliprole 2.5% SE
Ingredient Function Percent (w/w)
Pyriproxyfen tech. active ingredient 1 6.00
Tolfenpyrad tech. active ingredient 2 12.00
Chlorantraniliprole tech. active ingredient 3 2.50
Polyarylphenyl anionic ether sulfate, ammonium salt emulsifier 1.50
N,N decanamide solvent 5 to 10
Acrylic graft copolymer dispersing agent 3.00
Sodium salt of polycarboxylate dispersing agent 4.50
Aluminum magnesium silicate suspending agent 0.50
Polydimethylsiloxane anti foaming agent 0.20
1,2-benzisothiazolin-3(2H)-one preservative 0.15
Polypropylene glycol anti freezing agent 5.00
Xanthan gum thickner 0.15
Diluent water carrier 49.50
Total 100.00

T1: Storage stability-pyriproxyfen 6%+ tolfenpyrad 12%+ chlorantraniliprole 2.5% SE
Laboratory storage stability for 14 days
Parameters (in-house) Specification Initial at 54±2 0C at 0±2 0C
Pyriproxyfen tech. 5.70 to 6.60 6.50 6.25 6.6
Tolfenpyrad tech. 11.40 to 12.60 12.50 12.3 12.50
Chlorantraniliprole tech. 2.375 to 2.75 2.70 2.60 2.69
Pyriproxyfen suspensibility (%) 80 98.90 97.50 98.50
Tolfenpyrad suspensibility (%) 80 99.00 97.90 98.60
Chlorantraniliprole suspensibility (%) 80 98.50 97.60 98.30
pH range (1% aq. Suspension) 5.5 to 8.5 7.50 7.50 7.55
Pourability (%) 95 98.20 98.20 97.80
Specific gravity 1.00-1.10 1.05 1.05 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 550 560 560
Particle size (micron) D50<3, D90<10 2.1,8.2 2.2,8.5 2.1,8.2
Persistent foam ml (after 1 minute) max. 60 nil nil nil

T1: Room temperature storage stability
Parameters (in-house) Specification Initial 3 month 6 month
Pyriproxyfen tech. 5.70 to 6.60 6.50 6.50 6.47
Tolfenpyrad tech. 11.40 to 12.60 12.50 12.50 12.48
Chlorantraniliprole tech. 2.375 to 2.75 2.70 2.70 2.69
Pyriproxyfen suspensibility (%) 80 98.90 98.90 98.50
Tolfenpyrad suspensibility (%) 80 99.00 99.00 98.60
Chlorantraniliprole suspensibility (%) 80 98.50 98.50 98.30
pH range (1% aq. Suspension) 5.5 to 8.5 7.50 7.50 7.55
Pourability (%) 95 98.20 98.20 97.80
Specific gravity 1.00-1.10 1.05 1.05 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 550 550 560
Particle size (micron) D50<3, D90<10 2.1,8.2 2.1,8.2 2.1,8.2
Persistent foam ml (after 1 minute) max. 60 nil nil nil
The composition of pyriproxyfen 6%+ tolfenpyrad 12%+ chlorantraniliprole 2.5% SE (suspo emulsion) meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 °C & At 0±2 °C for 14 days) and room temperature (for 6 months).

T1: Manufacturing process for 100 kg batch of pyriproxyfen 6%+ tolfenpyrad 12%+ chlorantraniliprole 2.5% SE (suspo emulsion)

Step 1:2% Gum solution: 2 kg xanthan gum and 2 kg 1,2-benzisothiazoline-3-one are charged into 96 kg water and was homogenized. The above mentioned mixture was prepared 12-18 hours prior its use.
Step 2: EC premix- 15.0 kg of methylated Soyabean oil & & iso-octyl phenoxy polyethoxy ethanol was added into other vessel having slow stirring. Further, 6.0 kg of pyripoxyfen technical (melted) is added and mixed properly for 30-45 minutes.
Step 3: 42.0 kg of DM water and 5 kg of 1,2-propylene glycol were charged into designated vessel and mixed thoroughly.
Step 4: 0.5 kg of aluminum magnesium silicate, 3.0 kg of acrylic graft copolymer, 4.50 kg of sodium salt of polycarboxylate and 0.10 kg of polydimethylsiloxane were added into the vessel having water and the contents were homogenised for 45 – 60 minutes using high shear homogeniser.
Step 5: 12.0 kg of tolfenpyrad technical and 2.50 kg of chlorantraniliprole technical is added slowly to this premix and homogenised to achieve uniform slurry ready for grinding.
Step 6: Half of the quantity of antifoam was added prior grinding and then the material was subjected dyno mill for grinding till desired particle size is achieved.
Step 7; The remaining 0.10 kg of polydimethyl siloxane antifoam was added after the completion of grinding process and prior the sampling for in process analysis.
Step 8: The EC premix under slow stirring is mixed to this milled slurry and homogenized for 30-45 minutes.
Step 9: 7.5 kg of 2% gum solution is added to this formulation and sent to QC for quality check.

Table 1: Treatment details
Treatment number Treatment details gram active ingredients per hectare
T1 Pyriproxyfen 6%+Tolfenpyrad 12%+Chlorantraniliprole 2.5% SE 60+120+25
T2 Pyriproxyfen 6%+Tolfenpyrad 12%+Cyantraniliprole 5% SE 60+120+50
T3 Pyriproxyfen 6%+Tolfenpyrad 12%+Tetraniliprole 3% SE 60+120+30
T4 Pyriproxyfen 6%+Tolfenpyrad 12%+Cyclaniliprole 3% SE 60+120+30
T5 Pyriproxyfen 6%+Tolfenpyrad 12%+Flubendiamide 3.5% SE 60+120+35
T6 Pyriproxyfen 6%+Chlorantraniliprole 2.5% SC 60+25
T7 Pyriproxyfen 6%+Cyantraniliprole 5% OD 60+50
T8 Pyriproxyfen 6%+Tetraniliprole 3% SC 60+30
T9 Pyriproxyfen 6%+Cyclaniliprole 3% SE 60+30
T10 Pyriproxyfen 6%+Flubendiamide 3.5% SC 60+35
T11 Tolfenpyrad 12%+Chlorantraniliprole 2.5% SC 120+25
T12 Tolfenpyrad 12%+Cyantraniliprole 5% SC 120+50
T13 Tolfenpyrad 12%+Tetraniliprole 3% SC 120+30
T14 Tolfenpyrad 12%+Cyclaniliprole 3% SE 120+30
T15 Tolfenpyrad 12%+Flubendiamide 3.5% SC 120+35
T16 Pyriproxyfen 6%+Tolfenpyrad 12% SC 60+120
T17 Pyriproxyfen 10% EC 60
T18 Tolfenpyrad 15% EC 120
T19 Chlorantraniliprole 18.5% w/w (20% w/v) SC 25
T20 Cyantraniliprole 10.26% w/w (10% w/v) OD 50
T21 Tetraniliprole 18.18% w/w (20% w/v) SC 30
T22 Cyclaniliprole 4.55% w/w (5% w/v) SL 30
T23 Flubendiamide 39.35% w/w (48% w/v) SC 35
T24 UTC (Untreated Control) -

T1 to T5-present compositions, T6 to T16-conventional combinations and T17 to T23-market available products.

Table 2a: Jassid and whitefly control in okra crop

Treatment number Jassid control (%) Whitefly control (%)
Observed Expected Colby's ratio Synergism (Y/N) Observed Expected Colby's ratio Synergism (Y/N)
T1 86.4 82.23 1.05 Y 83.2 77.68 1.07 Y
T2 91.8 86.40 1.06 Y 97.2 94.99 1.02 Y
T3 86.2 82.15 1.05 Y 85.2 78.24 1.09 Y
T4 89.8 83.98 1.07 Y 84.6 77.35 1.09 Y
T5 88.2 82.49 1.07 Y 83.6 77.68 1.08 Y
T6 53.6 55.13 0.97 65.8 62.43 1.05
T7 54.6 57.71 0.95 77.2 74.89 1.03
T8 51.8 54.92 0.94 66.8 63.37 1.05
T9 56.6 59.54 0.95 63.4 61.86 1.02
T10 53.2 55.78 0.95 65.6 62.43 1.05
T11 68.8 66.97 1.03 53.2 52.72 1.01
T12 70.4 68.87 1.02 69.4 68.40 1.01
T13 69.0 66.82 1.03 54.4 53.91 1.01
T14 72.2 70.22 1.03 52.8 52.00 1.02
T15 69.8 67.45 1.03 53.6 52.72 1.02
T16 81.6 78.70 1.04 75.4 71.96 1.05
T17 46.2 52.8
T18 60.4 40.6
T19 16.6 20.4
T20 21.4 46.8
T21 16.2 22.4
T22 24.8 19.2
T23 17.8 20.4
T24 0.0 0.0

All the present compositions (T1 to T5) provide synergistic control of key sucking pests, i.e., jassid and whitefly in okra crop on 7th day after application. The value of control observed was higher than all the conventional combinations (T6 to T16), market available products (T17 to T23) and untreated check (T24).

Table 2b: Fruit borer larval control and fruit yield

Treatment number Fruit borer larval control (%) Marketable fruits per 5 plants Increase (%) in marketable fruits over T24
Observed Expected Colby's ratio Synergism (Y/N)
T1 95.8 85.67 1.12 Y 24.6 119.6
T2 94.6 84.01 1.13 Y 25.4 126.8
T3 98.4 86.53 1.14 Y 23.4 108.9
T4 97.2 86.06 1.13 Y 22.8 103.6
T5 96.4 85.74 1.12 Y 22.4 100.0
T6 73.6 70.87 1.04 17.4 55.4
T7 72.4 70.39 1.03 17.2 53.6
T8 73.2 72.62 1.01 16.8 50.0
T9 72.8 71.66 1.02 16.4 46.4
T10 73.2 71.03 1.03 17.0 51.8
T11 84.4 81.99 1.03 19.2 71.4
T12 83.2 81.70 1.02 18.8 67.9
T13 85.6 83.08 1.03 17.6 57.1
T14 83.4 82.48 1.01 18.2 62.5
T15 84.2 82.09 1.03 17.8 58.9
T16 62.6 60.84 1.03 16.4 46.4
T17 20.4 13.8 23.2
T18 50.8 14.2 26.8
T19 63.4 15.4 37.5
T20 62.8 15.2 35.7
T21 65.6 14.6 30.4
T22 64.4 14.2 26.8
T23 63.6 14.4 28.6
T24 0.0 11.2 0.0

All the present compositions (T1 to T5) provide excellent protection against fruit borer larvae and also yielded higher number of marketable fruits per plant as compared to conventional combinations (T6-T16), market available products (T17-T23) and untreated control (T24).

Conclusion: Among the various compositions as shown in Table 1 treatment number T1-T5 are considered to be present compositions which showed excellent synergism and effectiveness against jassid and whitefly on okra crop. In Table 2a the jassid control observed at 7 DAA (days after application) of T1-T5 were 91.8%. Particularly, T2 (91.8%) followed by T4 (89.8%) and T5 (88.2%) showed highest jassid control at 7 DAA. Furthermore, the white fly control observed at 7 DAA of T1-T5 were 97.2%. Particularly, T2 (97.2%) followed by T3 (85.2%) and T4 (84.6%) showed highest whitefly control at 7 DAA. Moreover, the colby’s ratio is found to be >1 which shows stronger synergism of the present compositions to control both of jassid and whitefly.

In addition to that in Table 2b the fruit borer larval control of T1-T5 was 98.4%. Particularly, T3 (98.4%) followed by T4 (97.2%), and T5 (96.4%) showed fruit borer larval control. Further, the number of marketable fruits per 5 plants was found to be 25.4. Particularly, T2 (25.4), T1 (24.6) and T3 (23.4) showed the highest number of marketable fruits per 5 plants. Moreover, the increase in marketable fruits over T24 i.e. (untreated check) was found to be 126.8%. Particularly, T2 (126.8%) followed by T1 (119.6%) and T3 (108.9%) showed increase in marketable fruits over T24 (untreated check) which is an excellent result when compared with the conventional combinations and market available products for field trial. At last but not least the colby’s ratio was found to be >1 which shows stronger synergism of the present compositions to control fruit borer larval.

Example 2: Control of insect-pests in cotton crop.
Crop : Cotton
Location : Rajkot, Gujarat
No. of treatments : 18
Crop age : 86 days after sowing.
Spray water volume : 520 liter per hectare
Method of application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.

Observation methods:
Thrips (Thrips tabaci) control (%): Count the number of live thrips per leaf, record the observations from 3 leaves per plant and 10 plants per plot.

Pink bollworm (Pectinophora gossypiella) damage: Count the number of rosette flower (infected) flower per plant, record the observations from 20 plants per plot, on 10 and 20 days after application.

Healthy fruiting bodies count: Count the number of healthy fruiting bodies (includes squares, flowers, bolls) per plant. Record the observations from 10 plants per plot.

T2: Composition of pyriproxyfen 10%+ tolfenpyrad 12%+ cyantraniliprole 8% OD (oil dispersion)

Ingredients Function Percent (w/w)
Pyriproxyfen tech. active ingredient 1 10.00
Tolfenpyrad tech. active ingredient 2 12.00
Cyantraniliprole tech. active ingredient 3 8.00
Polyoxyethylene sorbitol hexaoleate oil emulsifier 10.00
Ethoxylated sorbitan ester co-emulsifier 8.50
Salts of polyolefin condensates non-aqueous dispersant 2.50
Styrene acrylic polymeer aqueous dispersant 1.50
Silicon antifoam antifoam 0.30
Bentonite clay rheology modifier 1.50
Methylated seed oil carrier 45.70
Total 100.00
technical/active ingredient on 100% purity basis

T2: Room temperature storage stability
Parameters (in-house) Specification Initial 3 month 6 month
Pyriproxyfen tech. 9.50 to 10.50 10.50 10.50 10.47
Tolfenpyrad tech. 11.40 to 12.60 12.50 12.50 12.48
Cyantraniliprole tech. 7.60 to 8.80 8.30 8.30 8.29
Pyriproxyfen suspensibility (%) 80 98.70 98.70 98.60
Tolfenpyrad suspensibility (%) 80 98.90 98.90 98.70
Cyantraniliprole suspensibility (%) 80 98.90 98.90 98.80
pH range (1% aq. Suspension) 4.0 to 6.0 5.50 5.50 5.50
Pourability (%) 95 98.00 98.00 98.00
Specific gravity 1.00-1.10 1.07 1.07 1.07
Viscosity at spindle no.62,20 rpm 350-800 cps 650 650 655
Particle size (micron) D50<3, D90<10 2.0,7.8 2.0,7.8 2.0,7.9
Persistent foam ml (after 1 minute) max. 60 nil nil nil
The composition of pyriproxyfen 10%+ tolfenpyrad 12%+ cyantraniliprole 8% OD meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 °C & At 0±2 °C for 14 days) and room temperature (for 6 months).

T2: Manufacturing process for 100 kg batch of pyriproxyfen 10%+ tolfenpyrad 12%+ cyantraniliprole 8% OD

Step 1: 15% Bentonite clay solution preparation: 15 kg of bentonite clay is added into 85 kg of methylated seed oil and homogenized till it gets completely dissolved. The above mentioned mixture was prepared 12-18 hours prior its use.
Step 2: OD premix: 30.70 kg of methylated seed oil is charged into a designated vessel for OD production.
Step 3: 10.0 kg of polyoxyethylene sorbitol hexaoleate, 1.50 kg of styrene acrylic polymer, 8.50 kg of ethoxylated sorbitan ester, 2.50 kg of salts of polyolefin condensates and 0.15 kg of polydimethyl siloxane were added and homogenized for 45 – 60 minutes using high shear homogeniser.
Step 4: 10.0 kg of pyriproxifen technical, 8.0 kg of cyantraniliprole technical and 12.0 kg of tolfenpyrad technical were added into this premix and homogenized for 30-45 minutes
Step 5: The remaining 0.15 kg of silicon antifoam and 10 kg of 15% bentonite caly solution were added after milling to avoid foaming
Step 6: The final formulation was sent to QC for quality check.

Table 3: Treatment details
Treatment number Treatment details gram active ingredients per hectare
T1 Pyriproxyfen 10%+Tolfenpyrad 12%+Chlorantraniliprole 4% OD 75+90+30
T2 Pyriproxyfen 10%+Tolfenpyrad 12%+Cyantraniliprole 8% OD 75+90+60
T3 Pyriproxyfen 10%+Tolfenpyrad 12%+Tetraniliprole 4.67% OD 75+90+35
T4 Pyriproxyfen 10%+Tolfenpyrad 12%+Cyclaniliprole 4.67% OD 75+90+35
T5 Pyriproxyfen 10%+Tolfenpyrad 12%+Flubendiamide 5.33% OD 75+90+40
T6 Pyriproxyfen 10% EC+Tolfenpyrad 15% EC+Chlorantraniliprole 18.5% SC 75+90+30
T7 Pyriproxyfen 10% EC+Tolfenpyrad 15% EC+Cyantraniliprole 10.26% OD 75+90+60
T8 Pyriproxyfen 10% EC+Tolfenpyrad 15% EC+Tetraniliprole 18.18% SC 75+90+35
T9 Pyriproxyfen 10% EC+Tolfenpyrad 15% EC+Cyclaniliprole 4.55% SL 75+90+35
T10 Pyriproxyfen 10% EC+Tolfenpyrad 15% EC+Flubendiamide 39.35% SC 75+90+40
T11 Pyriproxyfen 10% EC 75
T12 Tolfenpyrad 15% EC 90
T13 Chlorantraniliprole 18.5% w/w (20% w/v) SC 30
T14 Cyantraniliprole 10.26% w/w (10% w/v) OD 60
T15 Tetraniliprole 18.18% w/w (20% w/v) SC 35
T16 Cyclaniliprole 4.55% w/w (5% w/v) SL 35
T17 Flubendiamide 39.35% w/w (48% w/v) SC 40
T18 UTC (Untreated Control) -

T1 to T5-present compositions, T6 to T10-tank mixes of market available products, T11 to T17-market available products.

Table 4: Residual control of thrips and pink bollworm in cotton

Treatment number Thrips control (%) No. of rosette flowers due to pink bollworm/plant Number of healthy fruiting bodies per plant Increase (%) in healthy fruiting bodies over T18
1 DAA 5 DAA 10 DAA 15 DAA after 10 days after 20 days
T1 95.2 90.2 78.6 70.6 0.00 0.00 56.4 120.3
T2 98.8 94.2 87.4 80.2 0.00 0.00 55.3 116.0
T3 96.8 91.4 85.6 75.2 0.00 0.00 54.1 111.3
T4 97.2 92.4 84.8 76.4 0.00 0.00 52.3 104.3
T5 96.6 90.4 81.8 72.4 0.00 0.00 51.3 100.4
T6 87.6 77.6 53.8 33.6 0.42 0.82 48.8 90.6
T7 92.4 86.4 72.4 58.6 0.58 0.96 47.1 84.0
T8 90.4 81.4 66.4 48.6 0.52 0.86 45.6 78.1
T9 87.8 76.2 56.8 42.8 0.46 0.98 44.3 73.0
T10 85.6 70.4 51.2 35.6 0.56 1.14 41.7 62.9
T11 65.4 61.8 50.6 38.8 2.64 4.24 36.5 42.6
T12 78.8 70.6 62.4 50.4 1.18 2.82 38.3 49.6
T13 66.4 45.6 32.8 14.4 0.68 1.14 42.8 67.2
T14 75.8 64.2 48.6 35.2 0.82 1.72 41.2 60.9
T15 68.4 48.2 35.8 19.6 0.74 1.68 40.7 59.0
T16 70.4 50.2 37.4 21.8 0.82 1.86 39.8 55.5
T17 65.6 46.4 32.8 16.2 0.80 1.78 38.6 50.8
T18 0.0 0.0 0.0 0.0 3.58 6.34 25.6 0.0

DAA-days after application. All the present compositions (T1 to T5) provide excellent control of thrips up to 15 days, provides protection against pink bollworm and yielded higher number of healthy fruiting bodies per plant, as compared to tank mixes of market available products (T6 to T10), market available products (T11 to T17) and untreated control (T18).

Conclusion: Among the various compositions as shown in Table 3 treatment number T1-T5 are considered to be present compositions which showed excellent synergism and effectiveness against thrips and pink bollworm control in cotton crop. Further, in Table 4 the control of thrips showed maximum of 98.8% (T2) on 1 DAA (days after application) followed by 94.2% (T2) on 5 DAA, 87.4% (T2) on 10 DAA and 80.2% (T2) on 15 DAA when compared with tank mixes of market available products (T6 to T10), market available products (T11 to T17) and untreated check (T18).

Moreover, in Table 4 the number of rosette flowers (infected) due to pink bollworm is 0 after 10 days and 20 days as well. Furthermore, the number of healthy fruiting bodies per plant was maximum of 56.4. Particularly, (T1) 56.4 followed by (T2) 55.3 and (T3) 54.1. In addition to that the increase in healthy fruiting bodies over (T18) untreated check was 120.3%. Particularly, (T1) 120.3% followed by T2 (116.0%) and (T3) 111.3% which shows effectiveness and synergism of the present compositions as compared to tank mixes of market available products, market products and untreated check.

Example 3: Pod borer larval control in redgram crop.
Crop : Red gram
Location : Sinor, Gujarat
No. of treatments : 13
Crop age : 95 days after sowing.
Spray water volume : 500 liter per hectare
Method of application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.

Observation methods:
Pod borer (Helicoverpa armigera) larval control (%): Count the number of live larvae per plant, record the observations from 10 plants per plot. Calculate larval control (%) as observed value.

Healthy pod count: Count the number of healthy (undamaged) pods per plant. Record the observations from 10 plants per plot.

T5: Composition of pyriproxyfen 5%+ tolfenpyrad 8%+ flubendiamide 3.2% SC (Suspension concentrate)

Ingredients Function Percent (w/w)
Pyriproxyfen tech. active ingredient 1 5.00
Tolfenpyrad tech. active ingredient 2 8.00
Flubendiamide tech. active ingredient 3 3.20
Methylated seed oil, polyalkyleneoxide modified trisiloxane (super wetting-spreading-penetrating agent) super-wetting-spreading-penetrating agent 3.00
Tristyryl phenol ethoxylate phosphate esters (dispersing agent I) dispersing agent 4.50
Sodium salt of polycarboxylate (dispersing agent II) dispersing agent 1.50
Aluminum magnesium silicate (suspending agent) suspending agent 1.00
Polydimethylsiloxane (anti foaming agent) anti foaming agent 0.30
sodium benzoate (preservative) preservative 0.30
Polypropylene glycol (anti freezing agent) anti freezing agent 6.00
Xanthan gum (thickner) thickner 0.30
Diluent water carrier 66.90
Total 100.00
technical/active ingredient on 100% purity basis

T5: Storage stability-pyriproxyfen 5%+ tolfenpyrad 8%+ flubendiamide 3.2% SC
Laboratory storage stability for 14 days
Parameters (in-house) Specification Initial at 54±2 0C at 0±2 0C
Pyriproxyfen tech. 4.75 to 5.50 5.30 5.15 5.3
Tolfenpyrad tech. 7.60 to 8.80 8.40 8.20 8.39
Flubendiamide tech. 3.04 to 3.52 3.50 3.25 3.5
Pyriproxyfen suspensibility (%) 80 97.80 97.00 97.60
Tolfenpyrad suspensibility (%) 80 98.90 98.50 98.70
Flubendiamide suspensibility (%) 80 98.10 98.00 98.10
pH range (1% aq. Suspension) 5.5 to 8.0 6.50 6.60 6.50
Pourability (%) 95 98.50 98.20 98.40
Specific gravity 1.00-1.10 1.05 1.05 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 650 680 655
Particle size (micron) D50<3, D90<10 1.5, 8.1 1.6,8.2 1.5,8.2
Persistent foam ml (after 1 minute) max. 60 nil nil nil

T5: Room temperature storage stability
Parameters (in-house) Specification Initial 3 month 6 month
Pyriproxyfen tech. 4.75 to 5.50 5.30 5.30 5.28
Tolfenpyrad tech. 7.60 to 8.80 8.40 8.40 8.39
Flubendiamide tech. 3.04 to 3.52 3.50 3.50 3.48
Pyriproxyfen suspensibility (%) 80 97.80 97.80 97.60
Tolfenpyrad suspensibility (%) 80 98.90 98.90 98.70
Flubendiamide suspensibility (%) 80 98.10 98.10 98.10
pH range (1% aq. Suspension) 5.5 to 8.0 6.50 6.50 6.50
Pourability (%) 95 98.50 98.50 98.40
Specific gravity 1.00-1.10 1.05 1.05 1.05
Viscosity at spindle no. 62, 20 rpm 350-800 cps 650 650 651
Particle size (micron) D50<3, D90<10 1.5, 8.1 1.5, 8.1 1.5,8.2
Persistent foam in ml (after 1 minute) max. 60 nil nil nil
The composition of pyriproxyfen 5%+ tolfenpyrad 8%+ flubendiamide 3.2% SC meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 °C & At 0±2 °C for 14 days) and room temperature (for 6 months).

T5: Manufacturing process for 100 kg batch of pyriproxyfen 5%+ tolfenpyrad 8%+ flubendiamide 3.2% SC

Step 1: 2% Gum solution: Xanthan gum (2.0 kg) and sodium benzoate (2.0 kg) were charged into 96.0 kg water and homogenized. The above mentioned mixture was preapred 12-18 hours prior its use.
Step 2: DM water (51.90 kg) and 1,2-propylene glycol (6 kg) were charged into designated vessel and mixed thoroughly.
Step 3: Sodium salt of polycarboxylate (1.5 kg), tristyryl phenol ethoxylate phosphate esters (4.5 kg) and aluminum magnesium silicate (1.0 kg) were added into the vessel having water and homogenized for 45 – 60 minutes using high shear homogenizer.
Step 4: Pyriproxifen technical (5.0 kg), tolfenpyrad technical (8.0 kg) and flubendiamide technical (3.20 kg) were added to this premix slowly and homogenized to achieve uniform slurry ready for grinding.
Step 5: Half of the quantity of polydimethylsiloxane (0.15 kg) was added before grinding and then the material was subjected to grind in dyno mill till the desired particle size is achieved.
Step 6: The remaining polydimethyl siloxane (0.15 kg) antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7: 15.0 kg of 2% xanthum gum solution, 3.0 kg of methylated seed oil and polyalkyleneoxide modified trisiloxaneto were added to this formulation and homogenized for 30 minutes.
Step 8: The final formulation was sent to QC for quality check.

Table 5: Treatment details
Treatment number Treatment details gram active ingredients per hectare
T1 Pyriproxyfen 5%+Tolfenpyrad 8%+Chlorantraniliprole 2% SC 62.5+100+25
T2 Pyriproxyfen 5%+Tolfenpyrad 8%+Cyantraniliprole 4.8% SC 62.5+100+60
T3 Pyriproxyfen 5%+Tolfenpyrad 8%+Tetraniliprole 2.8% SC 62.5+100+35
T4 Pyriproxyfen 5%+Tolfenpyrad 8%+Cyclaniliprole 2.8% SC 62.5+100+35
T5 Pyriproxyfen 5%+Tolfenpyrad 8%+Flubendiamide 3.2% SC 62.5+100+40
T6 Pyriproxyfen 10% EC 75
T7 Tolfenpyrad 15% EC 90
T8 Chlorantraniliprole 18.5% w/w (20% w/v) SC 30
T9 Cyantraniliprole 10.26% w/w (10% w/v) OD 60
T10 Tetraniliprole 18.18% w/w (20% w/v) SC 35
T11 Cyclaniliprole 4.55% w/w (5% w/v) SL 35
T12 Flubendiamide 39.35% w/w (48% w/v) SC 40
T13 UTC (Untreated Control) -

T1 to T5-present compositions, T6 to T12-market products and T13 UTC (untreated control)

Table 6: Pod borer larval control in red gram

Treatment number Pod borer larval control (%) Number of healthy pods per plant Increase (%) in healthy pods per plant over T13
Observed Expected Colby's ratio Synergism (Y/N)
T1 100.0 89.77 1.11 Y 93.7 76.1
T2 100.0 88.37 1.13 Y 90.8 70.7
T3 100.0 89.09 1.12 Y 92.6 74.1
T4 98.8 88.60 1.12 Y 91.2 71.4
T5 99.2 88.81 1.12 Y 92.1 73.1
T6 24.4 63.7 19.7
T7 54.6 68.8 29.3
T8 70.2 77.5 45.7
T9 67.4 75.1 41.2
T10 68.2 75.7 42.3
T11 66.8 74.7 40.4
T12 67.4 75.3 41.5
T13 0.0 53.2 0.0

All the present compositions (T1 to T5) provide synergistic control of pod borer larvae and yielded higher number of healthy pods per plant as compared to market products (T6-T12) and untreated check (T13).

Conclusion: Among the various compositions as shown in Table 5 treatment number T1-T5 are considered to be present compositions which showed excellent synergism and effectiveness against pod borer larval control in red gram crop. Further, in Table 6, T1-T5 showed 100% control on pod borer larval control in red gram. In particular, (T1), (T2) and (T3) showed 100% control followed by (T5) 99.2% and (T4) 98.8% as compared to the market products (T6 to T12) and untreated check (T13). Moreover, the numbers of healthy pods per plant were found 93.7. Particularly, (T1) 93.7 followed by (T3) 92.6 and (T5) 92.1 as compared to market products and untreated check. In addition to that, the present compositions also showed 76.1% of increase in healthy pods per plant over (T13) untreated check. In particular, (T1) showed 76.1% followed by (T3) 74.1% and (T5) 73.1% increment in healthy pods per plant over T13 when compared with the market products. At last the colby’s ratio was found to be >1 which shows stronger synergism of the present compositions to control pod borer larval.

The process for preparing the present diamide insecticidal composition can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However, all such variation and modification is still covered by the scope of present invention.
The amount of the present composition to be applied will depend on various factors such as, the subject of the treatment, for example, plants, soil or seeds; the type of treatment, for example, spraying, dusting or seed dressing; the purpose of the treatment, for example, prophylactic or therapeutic control; in case of insect control, the type of insects or mites to be controlled or the application time. This amount of the composition of the present invention to be applied can be readily deduced by a skilled agronomist.
Application to the seeds is carried out before sowing, either directly on the seeds or after having pregerminated the latter. Suitable application methods include, inter alia soil treatment, seed treatment, in furrow application and foliar application. Soil treatment methods include drenching the soil, drip irrigation (drip application onto the soil), dipping roots, tubers or bulbs, or soil injection. Seed treatment techniques include seed dressing, seed coating, seed dusting, seed soaking, and seed pelleting. In furrow applications typically include the steps of making a furrow in cultivated land, seeding the furrow with seeds, applying the pesticidally active composition to the furrow, and closing the furrow. Foliar application refers to the application of the pesticidally active composition to plant foliage, e.g. through spray equipment.
The rates of application vary within wide limits and depend on the nature of the soil, the method of application, the crop plant, the pest to be controlled, the prevailing climatic conditions, and other factors governed by the method of application, the time of application and the target crop.
The lists of crops on which the insecticidal composition of the present invention is used, include, but not limited to, GMO (Genetically Modified Organism) and non GMO traits, hybrids and conventional varieties of cotton (Gossypium spp.), paddy (Oryza sativa), wheat (Triticum aestavum), barley (Hordeum vulgare), maize (Zea mays), sorghum (Sorghum bicolor), oat (Avena sativa), pearl millet (Pennisetum glaucum), sugarcane (Saccharum officinarum), sugarbeet (Beta vulgaris), soybean (Glycin max), groundnut/peanut (Arachis hypogaea), sunflower (Helianthus annuus), mustard (Brassica juncea), rape seed (Brassica napus), sesame (Sesamum indicum), green gram (Vigna radiata), black gram (Vigna mungo), chickpea (Cicer aritinum), cowpea (Vigna unguiculata), red gram (Cajanus cajan), french bean (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), chilly (Capsicum annum), bell pepper (Capsicum annum), garlic (Allium sativum), cucumber (Cucumis sativus), muskmelon (Cucumis melo), watermelon (Citrullus lanatus), bottle gourd (Lagenaria siceraria), bitter gourd (Momordica charantia), radish (Raphanus sativus), carrot (Dacus carota subsp. sativus), turnip (Brassica rapa rapa), apple (Melus domestica), banana (Musa spp.), citrus groups (Citrus spp.), grape (Vitis vinifera), guava (Psidium guajava), 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), black pepper (Piper nigrum), mentha (Mentha spp.), rose (Rosa spp.), jasmine (Jasminum spp.), marigold (Tagetes spp.), common daisy (Bellis perennis), dahlia (Dahlia hortnesis), gerbera (Gerbera jamesonii), and carnation (Dianthus caryophyllus).
Crops are also to be understood as including those crops which have been rendered tolerant to herbicides or classes of herbicides (e.g. ALS-, GS-, EPSPS-, PPO-, ACCase- and HPPD-inhibitors) by conventional methods of breeding or by genetic engineering. An example of a crop that has been rendered tolerant to imidazolinones, e.g. imazamox, by conventional methods of breeding is Clearfield® summer rape (canola). Examples of crops that have been rendered tolerant to herbicides by genetic engineering methods include e.g. glyphosate- and glufosinate-resistant maize varieties commercially available under the trade names RoundupReady® and LibertyLink®.
Crops are also to be understood as being those which have been rendered resistant to harmful insects by genetic engineering methods, for example Bt maize (resistant to European corn borer), Bt cotton (resistant to cotton boll weevil) and also Bt potatoes (resistant to Colorado beetle). Examples of Bt maize are the Bt 176 maize hybrids of NK® (Syngenta Seeds). The Bt toxin is a protein that is formed naturally by Bacillus thuringiensis soil bacteria. Examples of toxins or transgenic plants able to synthesize such toxins, are described in EP-A-451 878, EP-A-374 753, WO 93/07278, WO 95/34656, WO 03/052073 and EP-A-427 529. Examples of transgenic plants comprising one or more genes that code for insecticidal resistance and express one or more toxins are KnockOut® (maize), Yield Gard® (maize), NuCOTIN33B® (cotton), Bollgard® (cotton), NewLeaf® (potatoes), NatureGard® and Protexcta®. Plant crops or seed material thereof can be resistant to herbicides, and at the same time, be resistant to insect feeding (“stacked” transgenic events). For example, seed can have the ability to express an insecticidal Cry3 protein while at the same time being tolerant to glyphosate.
Crops are also to be understood to include those which are obtained by conventional methods of breeding or genetic engineering and contain so-called output traits (e.g. improved storage stability, higher nutritional value and improved flavour).
Other useful plants include turf grass in golf-courses, lawns, parks and roadsides or grown commercially for sod, and ornamental plants such as flowers or bushes.
The diamide insecticidal composition of the present invention is used to control insects-pests and mites. The major insects-pests belong to the order Hemiptera for example, but not limited to, rice leafhopper/green leaf hopper (GLH) (Nephotettix nigropictus), rice brown plant hopper (BPH) (Nilaparvata lugen), rice backed plant hopper (WBPH) (Sogatella furcifera), apple mealy bug (Phenococcus aceris), bean aphid (Aphis fabae), black citrus aphid (Toxoptera aurantii), citrus black scale (Saissetia oleae), cabbage aphid (Brevicoryne brassicae), (Lipaphis erysimi), citrus red scale (Aonidiella aurantii), yellow scale (Aonidiella citrine), citrus mealybug (Planococcus citri), corn leaf aphid (Rhopalosiphum maidis), aphid (Aphis gossypii), jassid (Amrasca biguttula biguttla), mealy bug (Planococcus spp. and Pseudococcus spp.), cotton stainer (Dysdercus suturellus), whitefly (Bemisia tabaci), cowpea aphid (Aphis crassivora), grain aphid (Sitobion avenae), golden glow aphid (Uroleucon spp.), grape mealybug (Pseudococcus maritimus), green peach aphid (Myzus persicae), greenhouse whitefly (Trialeurodes vaporariorum), papaya mealy bug (Pracoccus marginatus), pea aphid (Acyrthosiphon pisum), sugarcane mealybug (Saccharicoccus sacchari), potato aphid (Myzus persicae), potato leaf hopper (Empoasca fabae), cotton whitefly (Bemisia tabaci), tarnished plant bug (Lygus lineolaris), wooly apple aphid (Eriosoma lanigerum), and mango hopper (Amritodus atkinsoni, Idioscopus spp.); to the order Lepidoptera for example, but not limited to, army worm (Mythimna unipuncta), asiatic rice borer (Chilo suppressalis), bean pod borer (Maruca vitrata), beet armyworm (Spodoptera exigua), black cutworm (Agrotis ipsilon), bollworm (Helicoverpa armigera), cabbage looper (Trichoplusia ni), codling moth (Cydia pomonella), croton caterpillar (Achea janata), diamond backmoth (Plutella xylostella), cabbage worm (Pieris rapae), pink bollworm (Pectinophora gossypiella), sugarcane borer (Diatraea saccharalis), sugarcane early shoot borer (Chilo infuscatellus), tobacco budworm (Heliothis virescens), tomato fruitworm (Helicoverpa zea), velvet bean caterpillar (Anticarsia gemmatalis), yellow stem borer (Scirpophaga incertulas), spotted bollworm (Earias vittella), rice leaf-folder (Cnaphalocrocis medinalis), tobacco leaf-eating caterpillar (Spodoptera litura); brinjal fruit and shoot borer (Leucinodes orbonalis), bean pod borer (Maruca vitrata, Maruca testulalis), armyworm (Mythimna separata), citrus leaf-miner (Phyllocnistis citrella), cabbage butterfly (Pieris brassicae), paddy stem borer (Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata), wheat stem borer (Sesamia inferens, Sitotroga cerealella, Spilosoma obliqua), and fall armyworm (Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Tryporyza nivella, Tryporyza incertulas, Tuta absoluta); to the order Coleoptera for example, but not limited to, apple twig borer (Amphicerus spp.), corn root worm (Diabrotica virgifera), cucumber beetle (diabrotica balteata), boll weevil (Anthonomus grandis), grape flea beetle (Altica chalybea), grape root worm (Fidia viticola), grape trunk borer (Clytoleptus albofasciatus), radish flea beetle (Phyllotreta armoraciae), maize weevil (Sitophilus zeamais), northern corn rootworm (Diabrotica barberi), rice water weevil (Lissorhoptrus oryzophilus, Anthonomus grandis, Bruchus lentis, Diabrotica semipunctata, Diabrotica virgifera, Dicladispa armigera, Epilachna varivestis), and various species of white grubs (Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotreta chrysocephala, Popillia japonica); to the order Orthoptera for example, but not limited to, Gryllotalpa spp., Locusta spp., and Schistocerca spp.; to the order Thysanoptera for example, but not limited to, Frankliniella spp., Thrips palmi, Thrips parvispinus, Thrips tabaci and Scirtothrips dorsalis; to the order Heteroptera for example, but not limited to, Dysdercus spp., and Leptocorisa spp., to the order Hymenoptera for example, but not limited to, Solenopsis spp.; to the order Diptera for example, but not limited to, Antherigona soccata, Dacus spp., Liriomyza spp., and Melanagromyza spp., to the order Acarina or arachnida for example, but not limited to, Aceria mangiferae, Brevipalpus spp., Eriophyes spp., Oligonychus mangiferus, Oligonychus punicae, Panonychus citri, Panonychus ulmi, Polyphagotarsonemus latus, Tarsonemus spp., Tetranychus urticae, and Tetranychus cinnabarinus.
The composition of present invention provides a number of benefits such as, broad spectrum of control i.e. controls sucking insects, foliage feeder, internal borers in one shot application - sucking insects belong to hemiptera, homoptera, thysanoptera; foliage feeder and internal borers belong to lepidoptera; mites belongs to arachnida class; residual control i.e. longer duration of control; delayed or prevents development of resistance in insects against insecticides with a specific site/mode of action; synergistic control i.e. gram of active ingredients required are less to achieve desired level of control; immediate protection to crops; rain-fastness; environment-friendly formulations i.e. formulations without organic solvent as carrier; and is safe to the crops.
The present invention has been described with reference to specific embodiment which is merely illustrative and not intended to limit the scope of the invention as defined in the present complete specification.


,CLAIMS:We Claim:

1. A diamide insecticidal composition of 5% to 15% w/w pyriproxyfen, 5% to 15% w/w tolfenpyrad, at least one compound selected from insecticides(s) of diamide group in an amount 1% to 20% w/w and agrochemically acceptable excipients.

2. The diamide insecticidal composition as claimed in claim 1 wherein, insecticide(s) of diamide group is selected from ryanodine receptor modulators, chlorantraniliprole, cyantraniliprole, cyclaniliprole, tetraniliprole, and flubendiamide.

3. The diamide insecticidal composition as claimed in claim 1, wherein the agrochemically acceptable excipients are selected from the group consisting of super wetting spreading penetrating agent(s), emulsifier(s), dispersing agent(s), suspending agent(s), anti-freezing agent(s), antifoaming agent(s), preservative(s), thickener(s), stabilizer(s), buffering agent(s), solvent(s), thickening gelling anti-settling agent(s) humectants(s) and polar co-solvent(s).

4. The diamide insecticidal composition as claimed in claim 1, wherein the agrochemically acceptable excipients are present in the range from 1% to 99% of the total weight of the composition.

5. The diamide insecticidal composition as claimed in claim 1, wherein the composition is in the form of oil dispersion (OD), suspo-emulsion (SE) and suspension concentrate (SC).

6. The diamide insecticidal composition as claimed in claim 3, wherein the wetting-spreading-penetrating agent(s) for oil dispersion (OD) is selected from organic silicone, trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxane heptamethyl, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane and mixture thereof.

7. The diamide insecticidal composition as claimed in claim 3, wherein the solvent(s) for oil dispersion (OD) is selected from blend of pongamia oil and palm oil; blend of pongamia oil and mahua oil; blend of pongamia oil and jojoba (Simmondsia chinensis); blend of pongamia oil and vegetable oil; blend of palm oil and mahua oil; blend of palm oil and jojoba oil; blend of palm oil and vegetable oil; blend of pongamia oil, palm oil and mahua oil; blend of pongamia oil, palm oil and jojoba oil; blend of pongamia oil, palm oil and vegetable oil and mixture thereof.

8. The diamide insecticidal composition as claimed in claim 3, wherein the emulsifier(s) for oil dispersion (OD) is selected from castor oil ethoxylates, alcohol ethoxylates, fatty acid ethoxylates, sorbitan ester ethoxylates, sulphosuccinate, calcium salts of dodecylbenzene sulphonate, alkylammonium salts of alkylbenzene sulphonate, alkylsulphosuccinate salts, ethylene oxide-propylene oxide block copolymers, ethoxylated alkylamines, octylphenol ethoxylate, ethoxylated alkyl phenols, ethoxylated sorbitol oleates, polyoxyethylene sorbitan monolaurate and mixture thereof.

9. The diamide insecticidal composition as claimed in claim 3, wherein the dispersing agent(s) for oil dispersion (OD) is selected from surfactant, condensed naphthalene sulfonate, propoxylated ethoxylated copolymer monoalkylether (ethylhexanol), alkyl sulfonate, alkyl benzene sulfonate, alkyl aryl sulfonate, alkylphenolalkoxylate, tristyrylphenol ethoxylate, natural or synthetic fatty ethoxylate alcohol, natural or synthetic fatty acid alkoxylate, natural or synthetic fatty alcohol alkoxylate, alkoxylated alcohol, n-butyl alcohol poly glycol ether, block copolymer, ethylene oxide-propylene oxide block copolymer, ethylene oxide-butylene oxide block copolymer, fatty acid-polyalkylene glycol condensate, polyamine-fatty acid condensate, polyester condensate, salts of polyolefin condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol- polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide and mixture thereof.

10. The diamide insecticidal composition as claimed in claim 3, wherein the stabilizer(s) for oil dispersion (OD) is selected from hectorite clay, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay and mixture thereof.

11. The diamide insecticidal composition as claimed in claim 3, wherein the antifoaming agent(s) for oil dispersion (OD) is selected from silicone oil, silicone compound, C10~C20 saturated fat acid compound, C8~C10 aliphatic alcohol compound, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane and mixture thereof.

12. The diamide insecticidal composition as claimed in claim 3, wherein the anti-freezing agent(s) for oil dispersion (OD) is selected from ethylene glycol, propane diol, glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, glycerine, urea, magnesium sulfate heptahydrate, sodium chloride and mixture thereof.

13. The diamide insecticidal composition as claimed in claim 3, wherein the preservative(s) for oil dispersion (OD) is selected from 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenylphenate, 5-chloro-2-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, butyl hydroxyl toluene and mixture thereof.

14. The diamide insecticidal composition as claimed in claim 3, wherein the buffering agent(s) for oil dispersion (OD) is selected from citric acid, sodium carbonate, sodium bicarbonate, sulphuric acid, hydrochloric acid, sodium hydroxide, potassium hydroxide, acetic acid, sorbic acid and mixture thereof.

15. The diamide insecticidal composition as claimed in claim 3, wherein the polar cosolvent(s) for oil dispersion (OD) is selected from cyclohexanone, acetophenone, butanol, n-octanol, n-propanol, 1-hexanol, propylene carbonate, n-methyl-2-pyrrolidone and mixture thereof.

16. The diamide insecticidal composition as claimed in claim 3, wherein the wetting-spreading-penetrating agent(s) for suspo-emulsion (SE) is selected from trisiloxane ethoxylate, polyalkyleneoxide modified trisiloxane, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyethylene glycol isotridecyl ester, polyethylene glycol monooleate, polyethylene glycol monostearate, mixture of polyhydric alcohol fatty acid ester, polyhydric alcohol polyethylene oxide fatty acid ester; polymer of polyoxyethylene (mono-, di- or tri-) styryl phenyl ether, polyoxyethylene/polyoxypropylene block polymer, polyoxyethylene nonyl phenyl ether, polyoxyethylenehexitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, sorbitan fatty acid, ester, mixture with polyoxyethylene fatty acid ester, dialkyldimethylammonium polynaphthylmethanesulfonate; polyethylene glycol isotridecyl ester and mixture thereof.

17. The diamide insecticidal composition as claimed in claim 3, wherein the solvent(s) for suspo-emulsion (SE) is selected from N,N-dimethyloctanamide, N,N-dimethylethylamine, N,N-dimethylethanamide, N,N-dimethylmethanamide, acetophenone, g-valerolactone, 2-methyltetrahydrofuran, cyclopentylmethylether, propylene carbonate, 2 ethylhexyl lactate base solvent and mixture thereof.

18. The diamide insecticidal composition as claimed in claim 3, wherein the dispersing agent(s) for suspo-emulsion (SE) is selected from polyester, polyamide, polycarbonate, polyurea, polyurethane, acrylic polymer and copolymer, styrene copolymer, butadiene copolymer, polysaccharide, starch, cellulose derivative, vinylalcohol, vinylacetate, vinylpyrrolidone polymer and copolymer, polyether, epoxy, phenolic, melamine resin, polyolefin and copolymer, acrylate polymer, poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmer, styrene-acrylic copolymer, poly(styrene-co maleic anhydride), cellulosic polymer, ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono, di, triglyceride, poly(vinylpyrrolidone), vinyl acetate polymer and copolymer, poly(alkylene glycol), styrene butadiene copolymer, poly(orthoesters), polyarylphenyl ether sulphate ammonium salt, alkyl resin, biodegradable polyester, starch, polylactic acid starch blend, polylactic acid, poly(lactic acid-glycolic acid) copolymer, polydioxanone, cellulose ester, ethyl cellulose, cellulose acetate butyrate, starch esters, starch ester-aliphatic polyester blend, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydride, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyester, polyhydroxybutyrate, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO block copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide and mixture thereof.

[
19. The diamide insecticidal composition as claimed in claim 3, wherein the suspending agent(s) for suspo-emulsion (SE) is selected from aluminum magnesium silicate, bentonite clay, silica, silicone dioxide, attapulgite clay and mixture thereof.

20. The diamide insecticidal composition as claimed in claim 3, wherein the anti-freezing agent(s) for suspo-emulsion (SE) is selected from glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, propane diol, glycerin, urea, magnesium sulfate heptahydrate, sodium chloride and mixture thereof.

21. The diamide insecticidal composition as claimed in claim 3, wherein the antifoaming agent(s) for suspo-emulsion (SE) is selected from silicone oil, silicone compound, C10~C20 saturated fat acid compound or C8~C10 aliphatic alcohol compound, silicone emulsion, vegetable oil based antifoam, tallow based fatty acid and mixture thereof.

22. The diamide insecticidal composition as claimed in claim 3, wherein the preservative(s) for suspo-emulsion (SE) is selected from 1,2-benzisothiazol-3(2H)-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2- methyl-4-isothiazolin-3-one, propionic acid, propionic acid sodium salt, sorbic acid, sorbic acid sodium or potassium salt, benzoic acid, benzoic acid sodium salt, p-hydroxy benzoic acid sodium salt, methyl p-hydroxy benzoate, biocide, sodium benzoate, potassium sorbate, para hydroxy benzoate and mixture thereof.

23. The diamide insecticidal composition as claimed in claim 3, wherein the thickening, gelling, and anti-settling agent(s) for suspo-emulsion (SE) is selected from natural extract of seeds and seaweeds, synthetic derivatives of cellulose, guar gum, locust bean gum, carrageenan, xanthan gum, alginate, methyl cellulose, sodium carboxymethyl cellulose (SCMC), hydroxyethyl cellulose (HEC), modified starche, polyacrylates, polyvinyl alcohol, polyethylene oxide and mixture thereof.

24. The diamide insecticidal composition as claimed in claim 3, wherein the stabilizer(s) for suspo-emulsion (SE) is selected from butylated hydroxytoluene (BHT), epoxidized soybean oil (ESBO), epichlorohydrin and mixture thereof.

25. The diamide insecticidal composition as claimed in claim 3, wherein the buffering agent(s) for suspo-emulsion (SE) is selected from the group consisting of calcium hydroxyapatite, potassium dihydrogen phosphate, sodium hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphate, amine monomers, lactate dehydrogenase, magnesium hydroxide and mixture thereof.

26. The diamide insecticidal composition as claimed in claim 3, wherein the wetting-spreading-penetrating agent(s) for suspension concentrate (SC) is selected from ethylene oxide/propylene oxide block copolymer, polyarylphenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulfate, sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonate, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate, organosilicon surfactant, trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified trisiloxane, polyalkyleneoxide modified polydimethylsiloxane, trisiloxane ethoxylate, polyoxyethylene methyl polysiloxane, polyether polymethyl siloxane copolymer, polyether modified polysiloxane; in unmodified form and mixture thereof.

27. The diamide insecticidal composition as claimed in claim 3, wherein the dispersing agent(s) for suspension concentrate (SC) is selected from naphthalenesulfonic acid, sodium salt condensated with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide and mixture thereof.

28. The diamide insecticidal composition as claimed in claim 3, wherein the suspending agent(s) for suspension concentrate (SC) is selected from aluminum magnesium silicate, bentonite clay, silica, attapulgite clay and mixture thereof.

29. The diamide insecticidal composition as claimed in claim 3, wherein the antifoaming agent(s) for suspension concentrate (SC) is selected from silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohol compound, silicone antifoam emulsion, dimethyl siloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane and mixture thereof.

30. The diamide insecticidal composition as claimed in claim 3, wherein the anti-freezing agent(s) for suspension concentrate (SC) is selected from ethylene glycol, propane diol, glycerin or the urea, glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, glycerin, urea, magnesium sulfate heptahydrate, sodium chloride and mixture thereof.

31. The diamide insecticidal composition as claimed in claim 3, wherein the preservative(s) for suspension concentrate (SC) is selected from 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one and mixture thereof.

32. The diamide insecticidal composition as claimed in claim 3, wherein the thickener(s) for suspension concentrate (SC) is selected from xanthan gum, PVK, carboxymethyl cellulose, polyvinyl alcohol, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch, acacia gum and mixture thereof.

33. The diamide insecticidal composition as claimed in claim 3, wherein the humectants(s) for suspension concentrate (SC) is selected from urea, humic acid, glycerol, lactose and mixture thereof.

Dated this 2nd day of August, 2023.

Documents

Application Documents

# Name Date
1 202221045925-STATEMENT OF UNDERTAKING (FORM 3) [11-08-2022(online)].pdf 2022-08-11
2 202221045925-PROVISIONAL SPECIFICATION [11-08-2022(online)].pdf 2022-08-11
3 202221045925-PROOF OF RIGHT [11-08-2022(online)].pdf 2022-08-11
4 202221045925-POWER OF AUTHORITY [11-08-2022(online)].pdf 2022-08-11
5 202221045925-FORM FOR SMALL ENTITY(FORM-28) [11-08-2022(online)].pdf 2022-08-11
6 202221045925-FORM FOR SMALL ENTITY [11-08-2022(online)].pdf 2022-08-11
7 202221045925-FORM 1 [11-08-2022(online)].pdf 2022-08-11
8 202221045925-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [11-08-2022(online)].pdf 2022-08-11
9 202221045925-EVIDENCE FOR REGISTRATION UNDER SSI [11-08-2022(online)].pdf 2022-08-11
10 202221045925-DECLARATION OF INVENTORSHIP (FORM 5) [11-08-2022(online)].pdf 2022-08-11
11 202221045925-ENDORSEMENT BY INVENTORS [02-08-2023(online)].pdf 2023-08-02
12 202221045925-CORRESPONDENCE-OTHERS [03-08-2023(online)].pdf 2023-08-03
13 202221045925-COMPLETE SPECIFICATION [03-08-2023(online)].pdf 2023-08-03