DESC:FORM 2

THE PATENTS ACT 1970
(SECTION 39 OF 1970)

&

THE PATENT RULES, 2003

COMPLETE SPECIFICATION
(Section 10 and Rule 13)

SYNERGISTIC INSECTICIDAL COMPOSITION OF INDOXACARB AND TOLFENPYRAD

We, COROMANDEL INTERNATIONAL LIMITED,
an Indian company incorporated under the Companies Act, 1956, and validly existing under the Companies Act, 2013. Having its registered office at Coromandel House, Sardar Patel Road,
Secunderabad – 500 003, Telangana, India

The following specification particularly describes the invention and the manner in which it is to be performed.
FIELD OF THE INVENTION
The present invention relates to a synergistic insecticidal composition comprising of indoxacarb and tolfenpyrad. Particularly the present invention relates to suspension concentrate (SC) of indoxacarb and tolfenpyrad with one or more agrochemical additives in synergistically effective amounts and a process thereof.

BACKGROUND OF THE INVENTION
Insecticides are agrochemicals in the pesticide family used to control insects by killing them or preventing the establishment or proliferation of those considered harmful. They play a key role in agriculture and public health by improving the yield and productivity of crops caused by pests and by reducing the rate of vector-borne diseases by killing or affecting growth and development of vectors such as mosquitoes, houseflies, tsetse flies, sand flies, cockroaches, etc.

They are pesticides formulated for repelling, killing, harming, or mitigating insects from crops and other agri-food sources such as ranches, poultry farms, etc. Insecticides work differently based on their mode of actions; some disrupt the nervous system, whereas others damage the exoskeletons, others repel or control them. Insecticides application helps in managing and mitigating insects; thereby guaranteeing crop protection and preventing yield loss.

Indoxacarb is a non-organophosphorus oxadiazine insecticide developed by DuPont that is considered a safe substitute for organophosphate insecticides. It has a mode of action against insect pests. It works as a sodium channel blocker resulting in paralysis and death of targeted pests. This insecticide has been reported to have a good field activity against a number of lepidoptera as well as certain homoptera and coleoptera insects.

Indoxacarb is chemically known as methyl 7-chloro-2,5-dihydro-2-[[(methoxycarbonyl)[4-(trifluoromethoxy) phenyl] amino] carbonyl] indeno[1,2-e] [1,3,4]oxadiazine-4a(3H)-carboxylate. It’s preparation and use are disclosed in US 5,462,938 and as the following chemical structure:

Tolfenpyrad is a pesticide developed by Mitsubishi Chemical (presently Nihon Nohyaku Co.) that was first approved in 2002 in Japan under the trade name of Hachi-hachi. It is used against a broad range of pests such as hemiptera, coleoptera, diptera, lepidoptera, thysanoptera and acarina. It is especially effective against pests that are resistant to existing insecticides such as organophosphates and carbamates because it possesses a new mode of action: inhibition of complex I in the respiratory electron-transfer chain of mitochondria.

Tolfenpyrad is chemically known as 4-chloro-3-ethyl-1-methyl-N-[4-(4-methylphenoxy)-1H-benzyl]pyrazol-5-carboxamide. It’s preparation and use are disclosed in US 5,039,693 and has the following chemical structure:

Japanese patent application No. JP 2006131516, Nippon disclosed the pest control agent wettable powder, Emulsion compositions containing tolfenpyrad in combination with one or more other compounds having insecticidal activity including indoxacarb.

Chinese patent application No. CN 102630677, Guangxi disclosed ultra-low volume liquids (ULV) formulations of indoxacarb and tolfenpyrad.

Even though the existing prior art has already disclosed different composition comprising of indoxacarb and tolfenpyrad, there is no specific disclosure available on the synergistic composition of indoxacarb and tolfenpyrad in suspension concentrate formulation.

The inventors of the present invention have surprisingly found that the suspension concentration formulation of the two active components indoxacarb and tolfenpyrad has its own benefits such as it has lower application rate that not only reduces the amount of an active substance required for application, but as a rule, also reduces the amount of formulation auxiliaries required. Both reduce the economic outlay and improve the eco-friendliness of the insecticide treatment.

OBJECT OF THE INVENTION
It is an object of the present invention to provide a synergistic insecticidal composition comprising of indoxacarb and tolfenpyrad.

It is another object of the present invention to provide a suspension concentrate (SC) comprising of indoxacarb and tolfenpyrad with one or more agrochemical additives.

It is yet another object of the present invention to provide a process for the preparation of a suspension concentrate (SC) of indoxacarb and tolfenpyrad.

SUMMARY OF THE INVENTION
The present invention provides a synergistic insecticidal composition comprising indoxacarb and tolfenpyrad.

An aspect of the present invention is to provide a suspension concentrate (SC) comprising as its active ingredients indoxacarb present in a range from 5% to 10% (w/w), tolfenpyrad present in a range from 20% to 30% (w/w) and one or more agrochemical additives in a range from 20% to 80% (w/w).

In another aspect of the present invention provides a suspension concentrate (SC) comprising indoxacarb in 7% (w/w), tolfenpyrad in 25% (w/w) and one or more agrochemical additives in a range from 20% to 80% (w/w).

In an aspect of the present invention, the agrochemical additives are selected from the group comprising of a wetting agent, a dispersing agent, an anti-freezing agent, a viscosity modifier, a biocide, a defoamer, a buffer and a base.

In an aspect of the present invention, the wetting agent is selected from the group comprising of ethoxylated TSP-phosphate ester, ethoxylated polyaryl phenol phosphate amine salt, amine salt of polyaryl phenyl ether phosphate and nonionic proprietary surfactant blend, present in an amount of 1% to 5 % (w/w).

In an aspect of the present invention, a dispersing agent is selected from the group comprising of EO/PO Polymeric dispersant, polyoxy alkylene glycol butyl ether, sulfated polyaryl phenol ethoxylate ammonium salt, polyoxyethylene-polyoxy propylene block polymer, and methyl methacrylate graft copolymer, present in an amount of 1% to 5% (w/w).

In an aspect of the present invention, an antifreezing agent is selected from the group comprising of propylene glycol, acrylate copolymer or its combination thereof, present in an amount of 10% to 15% (w/w).

In an aspect of the present invention, the viscosity modifier is selected from the group comprising of hydrated magnesium aluminosilicate and xanthan gum, present in an amount of 5% to 15% (w/w).

In an aspect of the present invention, the biocide is selected from the group comprising of 1,2-benzisothiazol-3(2H)-one and 2-methyl-(2H)-isothiazol-3-one, present in an amount of 0.01% to 0.2% (w/w).

In an aspect of the present invention, the defoamer is selected from polydimethyl siloxane antifoam emulsion and other silicones, present in an amount of 0.1% to 1% (w/w).

In an aspect of the present invention, the buffer is selected from the group comprising of phosphate buffer (e.g., disodium hydrogen phosphate) and acetate buffer, present in an amount of 0.5% (w/w).

In an aspect of the present invention, the base is distilled water, present in an amount of 40% to 50% (w/w).

In an aspect of the present invention provides a suspension concentrate (SC) comprising
(a) indoxacarb in a range from 5% to 10% (w/w),
(b) tolfenpyrad in a range from 20% to 30% (w/w),
(c) biocide in a range from 0.01% to 0.2% (w/w).
(d) wetting agent in a range from 1% to 5 % (w/w),
(e) dispersing agent in a range from 1% to 5% (w/w),
(f) antifreezing agent in a range from 10% to 15% (w/w),
(g) viscosity modifier in a range from 5% to 15% (w/w).\,
(h) defoamer in a range from 0.1% to 1% (w/w),
(i) buffer in an amount of 0.5% (w/w),
(j) base in an amount of 40% to 50% (w/w).

The present invention also provides a process for the preparation of a suspension concentrate (SC) comprising of indoxacarb and tolfenpyrad comprising the steps of:

a) preparing an aqueous slurry by mixing antifreezing agent and dispersing agent in a pre-mixer (Vessel No.1) and then adding biocide, defoamer and a base followed by actives
b) wet milling the pre-mixer slurry by passing through the dyno-mill at a temperature less than 30oC and collecting the material in a post-mixer (Vessel No.2),
c) preparing 2% gel suspension by mixing viscosity agent, antifreezing agent, buffer, and a base, and
d) gelling the wet milled slurry (a mixture post-mixer slurry and 2% gel suspension) and stirring the mixture for 3 hours to form homogenized suspension concentrates.

The present invention also provides a process for the preparation of a suspension concentrate (SC) comprising of Indoxacarb and Tolfenpyrad comprising the steps of:
a) preparing an aqueous slurry by mixing propylene glycol and EO/PO polymeric dispersant in a pre-mixer (Vessel No.1) and then adding 1,2-Benzisothiazol-3(2H)-one, polydimethylsiloxane antifoam emulsion and distilled water followed by Indoxacarb and Tolfenpyrad.
b) wet milling the pre-mixer slurry by passing through the dyno-mill at a temperature less than 30oC and collecting the material in a post-mixer (Vessel No.2),
c) preparing 2% gel suspension by mixing xanthan gum, propylene glycol, disodium hydrogen phosphate, and distilled water, and
d) gelling the wet milled slurry (a mixture post-mixer slurry and 2% gel suspension) and stirring the mixture for 3 hrs. to form homogenized suspension concentrates.

DESCRIPTION OF THE INVENTION
The following detailed description is presented to enable any person skilled in the art to make and use the invention. For purposes of explanation, specific nomenclature is set forth to provide a thorough understanding of the present application. However, it will be apparent to one skilled in the art that these specific details are not required to practice the invention. Descriptions of specific applications are provided only as representative examples. The present application is not intended to be limited to the embodiments shown but is to be accorded the widest possible scope consistent with the principles and features disclosed herein.

It is to be noted that, as used in the specification, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to a composition containing “a compound” includes a mixture of two or more compounds. It should also be noted that the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise.

Similarly, the words "comprise", "comprises", and "comprising" are to be interpreted inclusively rather than exclusively. Likewise, the terms "include", "including" and "or" should all be construed to be inclusive, unless such a construction is clearly prohibited from the context. However, the embodiments provided by the present disclosure may lack any element that is not specifically disclosed herein. Thus, a disclosure of an embodiment defined using the term "comprising" is also a disclosure of embodiments "consisting essentially of” and "consisting of” the disclosed components. Where used herein, the term "example", particularly when followed by a listing of terms, is merely exemplary and illustrative and should not be deemed to be exclusive or comprehensive. Any embodiment disclosed herein can be combined with any other embodiment disclosed herein unless explicitly indicated otherwise.

The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total solution or composition unless otherwise specified.

As used herein, the terms “insecticide” may be understood to include pesticides specifically used to destroy one or more species of insects.

As used herein, the term “synergistic composition” may be understood to include effective combination of more than one agrochemical that allows the application of the said agrochemical in a much lower dosage, which results in a less dosage treatment for the crops.

As used herein, the term “agrochemical additives” may be understood to include a range of surfactants, dispersing agents, organic or inorganic pigments, solvents, de-solvents, defoamers, and emulsions, crystallization inhibitors, viscosity modifiers, suspending agents, dyes, antioxidants, foaming agents, light absorbers, mixing aids, neutralizers or pH adjusting substances and buffers, corrosion inhibitors, fragrances, wetting agents, absorption enhancers, micronutrients, plasticizers, lubricants, thickeners, anti-freezing agents, sterilization agents among others.

In an embodiment of the present invention, an insecticidal composition comprises of indoxacarb and tolfenpyrad.

In an embodiment of the present invention, an insecticidal composition comprises of indoxacarb, tolfenpyrad and one or more agrochemical additives.

In an embodiment of the invention, the present invention provides a method for preparing an insecticidal composition of indoxacarb and tolfenpyrad.

The compositions of the present invention are formulated into various formulations such as water soluble liquid (SL), an emulsifiable concentrate (EC), an emulsion (EW), a microemulsion (ME), a suspension concentrates (SC), an oil-based dispersions (OD), a flowable suspension (FS), water dispersible powder for slurry seed treatment (WS), water-soluble granule (SG), water dispersible granules (WDG), water dispersible powder (WP), a granule (GR), encapsulated granule (CG), a fine granule (FG), a macrogranule (GG), suspoemulsion (SE), capsule suspension (CS) and a microgranule (MG). Preferably, the synergistic insecticidal composition can be formulated as suspension concentrate (SC) formulation.

In an embodiment of the present invention, a suspension concentrate (SC) composition comprises indoxacarb present in a range from 5% to 10% (w/w), tolfenpyrad present in a range from 20% to 30% (w/w) and one or more agrochemical additives in a range from 20% to 80% (w/w).

In an embodiment of the present invention, the agrochemical additives are selected from the group comprising of a wetting agent, a dispersing agent, an anti-freezing agent, a viscosity modifier, a biocide, a defoamer, a buffer and a base.

As used herein, the term “wetting agent” may be understood as a chemical substance which is typically a surfactant used to reduce the surface tension of the water by penetrating in between the water molecules and thus reducing the cohesion between them. The waxy surface of many insects, fungi and plants makes it difficult for most water-based pesticides solution to penetrate to their target. Hence, these wetting agents help the solution to spread on the leaf surface thus increasing their efficiency. These agents aid in the milling process.

Accordingly, the composition of the present invention contains a wetting agent suitable for use in the present invention selected from the group comprising of ethoxylated TSP-phosphate ester, ethoxylated polyaryl phenol phosphate amine salt, amine salt of polyaryl phenyl ether phosphate and nonionic proprietary surfactant blend, present in an amount of 1% to 5 %(w/w).

As used herein, the term “dispersing agent” may be understood as a chemical substance, which is typically a surfactant, that is added to a suspension of solid or liquid particles in a liquid (such as a colloid or emulsion) to improve the separation of the particles and to prevent their settling or clumping. They can disperse active ingredients in the formulation and prevent agglomeration after dispersal in water.

Accordingly, the composition of the present invention contains a dispersing agent suitable for use in the present invention selected from the group comprising of EO/PO Polymeric dispersant, polyoxy alkylene glycol butyl ether, sulfated polyaryl phenol ethoxylate ammonium salt, polyoxyethylene-polyoxy propylene block polymer, and methyl methacrylate graft copolymer, present in an amount of 1% to 5% (w/w).

As used herein, the term “anti-freezing agent” may be understood as a chemical substance which prevents the said formulation from freezing.

Accordingly, the composition of the present invention contains an anti-freezing agent suitable for use in the present invention are selected from the group comprising of propylene glycol, acrylate copolymer or its combination thereof, present in an amount of 10% to 15% (w/w).

As used herein, the term “viscosity modifier” may be understood as a chemical substance used to alter the viscosity or the thickness of a liquid. These are the substances that alter the fluid resistance to flow.

Accordingly, the composition of the present invention contains a viscosity modifier suitable for use in the present invention are selected from the group comprising of hydrated magnesium aluminosilicate and xanthan gum, present in an amount of 5% to 15%(w/w).

As used herein, the term “biocide” may be understood as a chemical substance used to destroy, deter, render harmless or exert a controlling effect on any harmful organism. The addition of these biocides to the agricultural formulations helps to prevent the possible growth of micro-organisms for longer duration.

Accordingly, the composition of the present invention contains a biocide suitable for use in the present invention are selected from the group comprising of 1,2-benzisothiazol-3(2H)-one and 2-methyl-(2H)-isothiazol-3-one, present in an amount of 0.01% to 0.2% (w/w).

As used herein, the term “defoamer” may be understood as a chemical additive which is used to reduce and hinder the formation of foam in the liquid formulations.

Accordingly, the composition of the present invention contains a defoamer suitable for use in the present invention are selected from the group comprising of polydimethyl siloxane antifoam emulsion and other silicones, present in an amount of 0.1% to 1% (w/w).

As used herein, the term “buffer” may be understood as substances that adjust the pH of a solution. They can be either weak acids or weak bases or mixtures thereof that make a buffer solution.

Accordingly, the composition of the present invention contains a buffer suitable for use in the present invention is selected from the group comprising of phosphate buffer (e.g., disodium hydrogen phosphate) and acetate buffer, present in an amount of 0.5% (w/w).

Accordingly, the composition of the present invention contains a base suitable for use in the present invention is distilled water, present in an amount of 40% to 50% (w/w).

The present invention also provides a process for the preparation of a suspension concentrate (SC) comprising of indoxacarb and tolfenpyrad comprising the steps of:
a) preparing an aqueous slurry by mixing antifreezing agent and dispersing agent in a pre-mixer (Vessel No.1) and then adding biocide, defoamer and a base followed by actives
b) wet milling the pre-mixer slurry by passing through the dyno-mill at a temperature less than 30oC and collecting the material in a post-mixer (Vessel No.2),
c) preparing 2% gel suspension by mixing viscosity agent, antifreezing agent, buffer, and a base, and
d) gelling the wet milled slurry (a mixture post-mixer slurry and 2% gel suspension) and stirring the mixture for 3 hrs. to form homogenized suspension concentrates.

The present invention also provides a process for the preparation of a suspension concentrate (SC) comprising of Indoxacarb and Tolfenpyrad comprising the steps of:
a) preparing an aqueous slurry by mixing propylene glycol and EO/PO polymeric dispersant in a pre-mixer (Vessel No.1) and then adding 1,2-Benzisothiazol-3(2H)-one, polydimethylsiloxane antifoam emulsion, and distilled water followed by Indoxacarb and Tolfenpyrad.
b) wet milling the pre-mixer slurry by passing through the dyno-mill at a temperature less than 30oC and collecting the material in a post-mixer (Vessel No.2),
c) preparing 2% gel suspension by mixing xanthan gum, propylene glycol, disodium hydrogen phosphate and distilled water and
d) gelling the wet milled slurry (a mixture post-mixer slurry and 2% gel suspension) and stirring the mixture for 3 hrs. to form homogenized suspension concentrates.

The present invention provides a synergistic insecticidal composition of indoxacarb and tolfenpyrad, with an enhanced efficacy that would not be possible using the individual active compounds otherwise.

In yet another aspect, of the present invention provides with a synergistic composition comprising of indoxacarb and tolfenpyrad in suspension concentrate (SC) formulation with an improved stability and ready to use insecticidal composition, having superior bio-efficacy compared to the individual formulations.

The present invention is related to an insecticidal composition indoxacarb and tolfenpyrad which results in synergistic mixture that is more effective than the individual compounds at the considered doses. The composition of the present invention decreases application rates of each of the active ingredients and is non-phytotoxic.

In addition, by treating the insecticidal composition of the present invention in the soil, it becomes possible to simultaneously control pests inhabiting the soil and pests inhabiting the ground. In addition, in this method, since the dosage and the number of times of application of the active ingredient are reduced and the long-lasting effect persists, it is possible to provide a comprehensive control method.

The following examples describes the nature of the invention which are given only for the purpose of illustrating the present invention in more detail and are not limitative and relate to solutions, which have been particularly effective on bench scale.

EXAMPLES:

Preparation of indoxacarb and tolfenpyrad in a suspension concentrate (SC) form:
The composition of indoxacarb and tolfenpyrad in a suspension concentrate (SC) form is prepared by following steps as below:
Step 1: Preparation of Aqueous Slurry
10 parts by weight of antifreezing agent, 2.0 parts by weight of dispersing agent were taken in Vessel No.1 (pre-mixer). To this 0.08 parts of biocide, 4.0 parts by weight of defoamer and 45.02 parts by weight of base were added. The mixture was stirred for 15 minutes and then 2.0 parts by weight of antifreezing agent added. The stirring was continued for 15 min and then added 7.0 parts by weight of indoxacarb active ingredient, followed by added 25.0 parts by weight of tolfenpyrad active ingredient. The mixture was stirred for homogenization (the mixture should be thoroughly homogenized) for 30 min.

Step 2: Wet Milling of Slurry
The wet slurry from Vessel No 1 passed through Dyno-Mill at a temperature less than 30oC and material was collected in Vessel No.2 (post-Mixer). Continuous stirring was maintained in both the vessels to avoid sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 5 µ. If the d90 is higher than > 5µ then grind the mixture further till the PSD value complies the specification. The sample was collected in Vessel No.2 under homogenization.
Step 3: Preparation of 2.0% Xanthan gum gel suspension
Adding 2.0 parts by weight of xanthan gum (viscosity modifier) in 4.0 parts by weight of propylene glycol (antifreezing agent) and then added 0.05 part by weight 1,2-Benzisothiazol-3(2H)-one (biocide), 0.5 parts by weight of disodium hydrogen phosphate (buffer) and 45.02 parts of water (base). The mixture was stirred until got lumps free homogeneous mixture and keep this gel as such for 4-5 hours to get a translucent homogeneous gel.
Step 4: Gelling of Wet Milled Slurry
The required quantity of xanthan gum gel suspension (prepared above) was added to the wet slurry in Vessel No 2 and the mixture was stirred for 3 hours for homogenization. The sample was checked for complete analysis and packed in COEX Bottle.
The process illustrated above may be used for preparation of other composition indoxacarb and tolfenpyrad in a suspension concentrate (SC) form.

Example-1: Composition of indoxacarb 7% and tolfenpyrad 25% SC
S. No. Ingredients Function Quantity (in %w/w)
1. Indoxacarb @ 96.6% Active ingredient 7.0
2. Tolfenpyrad @ 97% Active ingredient 25.0
3. EO/PO polymeric dispersant Dispersing agent 2.0
4. Propylene glycol Antifreezing agent 10.0
5. Acrylate copolymer Antifreezing agent 2.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.08
7. Xanthan gum Viscosity modifier 8.0
8. Polydimethylsiloxane antifoam emulsion Defoamer 0.4
9. Disodium hydrogen phosphate Buffer 0.5
10. Distilled water Base 45.02
Total 100

Example-2: Composition of indoxacarb 7% and tolfenpyrad 25% SC
S. No. Ingredients Function Quantity (in %w/w)
1. Indoxacarb @ 96.6% Active ingredient 7.0
2. Tolfenpyrad @ 97% Active ingredient 25.0
3. Ethoxylated TSP-phosphate ester Wetting agent 2.0
4. Polyoxyalkylene glycol butyl ether Dispersing agent 2.0
5. Propylene glycol Antifreezing agent 10.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.1
7. Xanthan gum Viscosity modifier 10.0
8. Polydimethylsiloxane antifoam emulsion Defoamer 0.5
9. Distilled water Base 43.4
Total 100

Example-3: Composition of indoxacarb 7% and tolfenpyrad 25% SC
S. No. Ingredients Function Quantity (in %w/w)
1. Indoxacarb @ 96.6% (b) 7.0% Active ingredient 7.0
2. Tolfenpyrad @ 97% (b) 25% Active ingredient 25.0
3. Sulfated polyaryl phenol ethoxylate ammonium salt Dispersing agent 2.0
4. Ethoxylated polyaryl phenol phosphate amine salt Wetting agent 2.0
5. Propylene glycol Antifreezing agent 10.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.1
7. Xanthan gum Viscosity modifier 10.0
8. Polydimethylsiloxane antifoam emulsion Defoamer 0.5
9. Distilled water Base 43.4
Total 100

Example-4: Composition of indoxacarb 7% and tolfenpyrad 25% SC
S. No. Ingredients Function Quantity (in %w/w)
1. Indoxacarb @ 96.6% Active ingredient 7.0
2. Tolfenpyrad @ 97% Active ingredient 25.0
3. Polyoxyethylene-Polyoxy propylene block polymer Dispersing agent 1.5
4. Amine salt of polyaryl phenyl ether phosphate Wetting agent 1.5
5. Propylene glycol Antifreezing agent 10.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.1
7. Xanthan gum Viscosity modifier 10.0
8. Polydimethylsiloxane antifoam emulsion Defoamer 0.5
9. Distilled water Base 44.4
Total 100

Example-5: Composition of indoxacarb 7% and tolfenpyrad 25% SC
S. No. Ingredients Function Quantity (in %w/w)
1. Indoxacarb @ 96.6% Active ingredient 7.0
2. Tolfenpyrad @ 97% Active ingredient 25.0
3. Nonionic proprietary surfactant blend Wetting agent 1.5
4. Methyl methacrylate graft copolymer Dispersing agent 1.5
5. Propylene glycol Antifreezing agent 10.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.1
7. Xanthan gum Viscosity modifier 10.0
8. Polydimethylsiloxane antifoam emulsion Defoamer 0.5
9. Distilled water Base 44.4
Total 100

Example-6: Efficacy study for combination of indoxacarb and tolfenpyrad in a suspension concentrate (SC) formulation

SYNERGY STUDIES:
The synergistic pesticidal action of the inventive mixtures calculated by Colby’s formula as follows:

The percent insect control was worked out by using below mentioned formula:
Number of Insects in treated plot
% Insect Control = ---------------------------------------------x 100
Number of Insects in untreated plot

After calculating % disease control, the synergism was calculated by below formula:
Appropriate analysis of plant response to herbicide combination is critical in determining the type of activity observed. The most widely used model is one Gowing* derived and Colby** modified. Gowing described a mathematical formula for calculating the predicting response values for pesticide mixtures. He suggested the expected (E) percent inhibition of growth induced by pesticide A plus pesticide B is as follows, *(Jerry Flint et al, 1988)***
If A1 = the percent inhibition of growth by pesticide A at given rate
B1 = the percent inhibition of growth by pesticide B at given rate then,
B1 (100 – A1)
E = A1 +
100
When the percentage of pesticidal control observed for the combination is greater than the expected percentage, there is a synergistic effect. (Ratio of O/E > 1, means synergism observed.)

Reference:

*Gowing, D. P. 1960. Comments on tests of herbicide mixtures. Weeds 8:379–391.
**Colby, S. R. 1967. Calculating synergistic and antagonistic responses of herbicide combinations. Weeds 15:20–22
*** Jerry Flint et al, 1988. Analyzing Herbicide Interactions: A Statistical Treatment of Colby's Method. Weed Technology 2: 304-309

Field Bio-efficacy trials: Pests of Chilli, Pests of Cabbage
Trial 1: Pests of Chilli
Chilli, Capsicum annum L. belongs to the family Solanaceae is one of the important commercial crops grown in India. Nearly 35 species of insect pests occur on chilli which includes thrips, mites, whiteflies, aphids, fruit borers, tobacco caterpillar and other minor pests. The field efficacy trials were conducted on sucking pest complex in chilli. The sucking pests viz., thrips, Scirtothrips dorsalis (Hood) and yellow mite, Polyphagotarsonemus latus (Banks), Aphids Aphis gossypii (Glov) and Lepidopteran pests like Tobacco cater pillar Spodoptera litura (Hubner) and Fruit borer Helicoverpa armigera (Fabricius) cause severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield.
Field trials were conducted to evaluate the efficacy of innovative mixtures i.e., Indoxacarb and Tolfenpyrad against sucking & lepidopterans pests in Chilli. The chilli crop was raised with all standard agronomic practices. The experiments were laid out in a Randomized Block Design (RBD) and replicated thrice with an individual plot size of 5m X 6m. Spraying was done with manual operated knapsack sprayer with 500 liter of water spray volume per hectare at 20-50 days after transplanting. The observations were recorded by counting the number of sucking pests (Thrips, Mites & Aphids) per leaf and number of larvae of lepidopterans pests of Tobacco cater pillar & Fruit borer per plant and five plants per plot. The observations were recorded before spraying, 5 & 10 DAA (Days After Application).
Table 1: Efficacy of thrips, mites, aphids & lepidopteran pests’ control in Chilli at 5 and 10 days after application:

Compositions
GAI/ha % Insect Control at 5 DAA % Insect Control at 10 DAA
Thrips Mites Aphids Spodo
ptera Helico
verpa Thrips Mites Aphids Spodo
ptera Helico
verpa
Tolfenpyrad 15% EC 125 88.6 85.2 89.3 26.3 21.2 85.8 82.7 83.5 23.4 20.1
Indoxacarb 14.5% SC 35 3.1 2.5 3.6 90.6 89.4 2.2 1.9 2.9 82.2 80.4
Indoxacarb 7% + Tolfenpyrad 25% SC 160 95.6 91.7 93.5 91.5 90.3 93.3 90.3 91.5 92.5 90.3
SC- Suspension concentrate, EC – Emulsifiable concentrate, GAI/ha is gram active per hectare, and DAA is days after application.

The trial results in table 1 show excellent efficacy of Indoxacarb 7% + Tolfenpyrad 25% SC combination against sucking pest complex and lepidopteran pests in Chilli. The solo application as well as the combination of two active ingredients tested here against thrips, mites, aphids, spodoptera & helicoverpa. Solo was not able to provide satisfactory control of sucking & lepidopteran pest complex. The combination of Indoxacarb 7% + Tolfenpyrad 25% SC has shown excellent efficacy as well as residual control.

Table 2: Evaluation of synergy of Indoxacarb 7% + Tolfenpyrad 25% SC against Thrips, Mites, Aphids, Spodoptera & Helicoverpa at 10 DAA on Chilli

Compositions
GAI/ha Thrips Mites Aphids Spodoptera Helicoverpa
Exp Obs Exp Obs Exp Obs Exp Obs Exp Obs
Tolfenpyrad 15% EC 125 85.8 82.7 83.5 23.4 20.1
Indoxacarb 14.5% SC 35 2.2 1.9 2.9 82.2 80.4
Indoxacarb 7% + Tolfenpyrad 25% SC 160 86.1 93.3 83.0 90.3 83.9 91.5 86.3 92.5 84.3 90.3
Ratio of O/E - 1.08 1.08 1.09 1.07 1.07
SC- Suspension concentrate, EC – Emulsifiable concentrate, GAI/ha is gram active per hectare, Exp- Expected & Obs.- Observed, and DAA Days after application.

The trial results in table 1 & 2 show synergistic effect of Indoxacarb 7% + Tolfenpyrad 25% SC combination against thrips, mites, aphids, tobacco caterpillar & fruit borer on Chilli crop.

Trial 2: Pests of Cabbage
Cabbage, Brassica oleracea var capitata is a small, leafy biennial producing a compact globular mass of smooth or crinkled leaves wrapped over each other known as head. Nearly 8 species of insect pests occur on cabbage which includes aphids, diamond back moth, Tobacco cater pillar, head borer and other minor pests. The field efficacy trials were conducted on lepidopteran pest’s complex in cabbage. The Lepidopteran pests of diamond back moth Plutella xylostella (Linnaeus), Tobacco cut worm Spodoptera litura (Fab.) and sucking pest of Aphid Myzus persicae (Sulzer) causes severe damage and serious threat to the cabbage crop at early to head development stage and can also affect the crop stand and yield. Diamond back moth is a monophagous pest and tobacco cut worm and aphids are polyphagous and these are widely distributed in tropical, sub-tropical and temperate regions.
Field trials were conducted to evaluate the efficacy of innovative mixtures i.e., Indoxacarb and Tolfenpyrad against lepidopterans & sucking pests in Cabbage. The cabbage crop was raised with all standard agronomic practices. The experiments were laid out in a Randomized Block Design (RBD) and replicated thrice with an individual plot size of 5m X 6m. Spraying was done with manual operated knapsack sprayer with 500 liter of water spray volume per hectare at 20-50 days after transplanting. The observations were recorded by counting the number of larvae per plant and sucking pest per leaf in five plants per plot. The observations were recorded before spraying, 5 & 10 DAA (Days After Application).

Table 3: Efficacy of diamond back moth pest control in Cabbage at 5 and 10 days after application

Compositions
GAI/ha Diamond Back Moth Spodoptera Aphids
% Insect Control
at 5 DAA % Insect Control at 10 DAA % Insect Control at 5 DAA % Insect Control at 10 DAA % Insect Control at 5 DAA % Insect Control at 10 DAA
Tolfenpyrad 15% EC 125 87.6 78.3 24.3 18.6 88.2 85.3
Indoxacarb 14.5% SC 35 53.2 48.4 82.4 77.5 5.3 4.1
Tolfenpyrad 25 % +
Indoxacarb 7 % SC 160 95.3 90.5 96.9 92.5 94.3 92.7
SC- Suspension concentrate, EC – Emulsifiable concentrate, GAI/ha is gram active per hectare, and DAA is days after application.

The trial results in table 3 show excellent efficacy of Indoxacarb 7% + Tolfenpyrad 25% SC combination against lepidopterans and sucking pest complex in Cabbage. The solo application as well as the combination of two active ingredients tested here against diamond back moth, tobacco cut worm and aphids. Solo was not able to provide satisfactory control of lepidopteran and sucking pest complex. The combination of Indoxacarb 7% + Tolfenpyrad 25% SC has shown excellent efficacy as well as residual control.
Table 4: Evaluation of synergy of Indoxacarb 7% + Tolfenpyrad 25% SC against Diamond Back Moth, Tobacco cut worm and Aphids at 10 DAA on Cabbage

Compositions
GAI/ha % Insect Control at 10 DAA
Diamond Back Moth Spodoptera Aphids
Exp Obs Exp Obs Exp Obs
Tolfenpyrad 15% EC 125 -- 78.3 -- 18.6 -- 85.3
Indoxacarb 14.5% SC 35 -- 48.4 -- 77.5 -- 4.1
Tolfenpyrad 25 % +
Indoxacarb 7 % SC 160 88.8 90.5 81.6 92.5 85.9 92.7
Ratio of O/E - 1.01 1.13 1.07
SC- Suspension concentrate, EC – Emulsifiable concentrate, GAI/ha is gram active per hectare, Exp- Expected & Obs- Observed, and DAA Days after application.

The trial results in table 3 & 4 show synergistic effect of Indoxacarb 7% + Tolfenpyrad 25% SC combination against diamond back moth, tobacco cut worm and aphids on Cabbage crop. ,CLAIMS:WE CLAIM:
1. A suspension concentrate (SC) comprising as its active ingredients indoxacarb present in a range from 5% to 10% (w/w), tolfenpyrad present in a range from 20% to 30% (w/w) and agrochemical additives present in a range from 20% to 80% (w/w).

2. The composition as claimed in claim 1, wherein the agrochemical additives are selected from the group comprising of a wetting agent, a dispersing agent, an anti-freezing agent, a viscosity modifier, a biocide, a defoamer, a buffer and a base.

3. The composition as claimed in claim 2, wherein the wetting agent is selected from the group comprising of ethoxylated TSP-phosphate ester, ethoxylated polyaryl phenol phosphate amine salt, amine salt of polyaryl phenyl ether phosphate and nonionic proprietary surfactant blend, present in an amount of 1% to 5 %(w/w).

4. The composition as claimed in claim 2, wherein the dispersing agent is selected from the group comprising of EO/PO Polymeric dispersant, polyoxy alkylene glycol butyl ether, sulfated polyaryl phenol ethoxylate ammonium salt, polyoxyethylene-polyoxy propylene block polymer, and methyl methacrylate graft copolymer, present in an amount of 1% to 5% (w/w).

5. The composition as claimed in claim 2, wherein an antifreezing agent is selected from the group comprising of propylene glycol, acrylate copolymer or its combination thereof, present in an amount of 10% to 15% (w/w).

6. The composition as claimed in claim 2, wherein the viscosity modifier is selected from the group comprising of hydrated magnesium aluminosilicate and xanthan gum, present in an amount of 5% to 15%(w/w).

7. The composition as claimed in claim 2, wherein the biocide is selected from the group comprising of 1,2-benzisothiazol-3(2H)-one, and 2-methyl-(2H)-isothiazol-3-one, present in an amount of 0.01% to 0.2% (w/w).

8. The composition as claimed in claim 2, wherein the defoamer is selected from polydimethyl siloxane antifoam emulsion and other silicones, present in an amount of 0.1% to 1% (w/w).

9. The composition as claimed in claim 2, wherein the buffer is disodium hydrogen phosphate, present in an amount of 0.5%(w/w) and the base is distilled water, present in an amount of 40% to 50% (w/w).

10. A process for preparation of a suspension concentrate (SC) as claimed in claim 1, where the said process comprising the steps of:
a) preparing an aqueous slurry by mixing antifreezing agent and dispersing agent in a pre-mixer (Vessel No.1) and then adding biocide, defoamer and a base followed by actives,
b) wet milling the pre-mixer slurry by passing through the dyno-mill at a temperature less than 30oC and collecting the material in a post-mixer (Vessel No.2),
c) c) preparing 2% gel suspension by mixing viscosity agent, antifreezing agent, buffer, and a base, and
d) gelling the wet milled slurry (a mixture post-mixer slurry and 2% gel suspension) and stirring the mixture for 3 hours to form homogenized suspension concentrates.

Dated this Twenty fourth (24th) day of July, 2023

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