Description:FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
[See section 10, Rule 13]

“AGROCHEMICAL COMPOSITION”

Redson Retail & Reality Pvt. Ltd., an Indian company of A-88 Ashok Vihar Phase-I, Delhi - 110052, India

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 the field of pesticides. The present invention in particular relates to a novel, synergistic insecticidal composition comprising as active ingredients, Chlorantraniliprole, Lambda cyhalothrin, Thiamethoxam and Clove oil as a synergist. The present invention further relates to the process of preparation of said composition.

Background of the invention

Protection of crops and its produce from insect pest damage is essential for the enhancement of agriculture produce. Even after the availability of alternative types of pest control, chemical control still remains an important tool for the prevention and control of pests in agriculture, especially the insect pests. Insecticides of varied types and structural groups have been reported in the literature and a large number are in commercial use. However, judicious use of such chemical pesticides is absolutely needed to protect the environment and natural ecosystems. In this regard, application of insecticidal combinations has emerged as an attractive approach to ensure that the chemical load in the environment is reduced. However, not all actives are compatible with each other, and therefore it requires a great amount of experimentation and effort to develop a pesticidal combination which is synergistic, stable and effective in controlling the insect pests in economically important agricultural crops.

CN112715559 A provides an agricultural insecticidal composition containing sulfamide and lambda-cyhalothrin in a weight ratio of (1:100) -(100:1). The invention also provides application of agricultural insecticide in prevention and treatment of lepidoptera pests of vegetables.

CN109303062 A discloses composite type insecticidal granules containing Chlorantraniliprole and thiamethoxam. The active ingredients of the insecticidal granules include Chlorantraniliprole and thiamethoxam in a weight ratio of (0.1 to 15) to (0.4 to 25); the sum of the weight of the Chlorantraniliprole and thiamethoxam being 0.5-40% of the total weight of the composition. However, granules do not stick to foliage or other uneven surfaces and may be hazardous to nontarget species. This is because birds may feed on grain- or seed-like granules or mistake them for “grit” they need to grind up their food. Granules are often bulky and allow low percentage of active ingredient per unit volume.

There is therefore a continued need to develop insecticidal compositions that provides good bioefficacy against target pests, provides a composition with high synergistic action, provides a combination where the dosage of the active ingredients is reduced as compared to the individual recommended dosage, to avoid excess loading of the toxicant to the environment and to negligibly impact environmental safety.

The present invention aims to provide such an insecticidal composition with aforesaid advantageous features. More importantly, the present invention aims at providing a composition wherein the insecticidal activity of the insecticidal composition is considerably higher than the sum of the activities of the individual active compounds and that results in effective control of insect pests in agricultural crops.

Object of the invention
It is an object to provide a novel, stable, synergistic, insecticidal composition comprising Chlorantraniliprole, Lambda cyhalothrin, Thiamethoxam as active ingredients and clove oil as the synergist.

It is yet another object of the present invention to provide an insecticidal composition with enhanced bioefficacy at reduced dosage as compared to individual insecticidal formulations when used individually.

It is yet another object of the present invention to provide an insecticidal composition that is environmentally safe and non-phytotoxic.
It is yet another object of the present invention to provide an insecticidal composition that is effective against lepidopteran pests in agricultural crops, particularly, early shoot borer Chilo infuscatellus in sugarcane crop.

Summary of the invention
Accordingly, in one aspect, the present invention provides a novel, stable, synergistic, environmentally safe, cost-effective insecticidal composition comprising Chlorantraniliprole as first active ingredient, Lambda cyhalothrin as the second active ingredient, Thiamethoxam as the third active ingredient and clove oil acid as the synergist.

In another aspect, the present invention provides a novel, stable, synergistic, environment friendly insecticidal composition that is effective in controlling lepidopteran pests, particularly early shoot borer- Chilo infuscatellus in sugarcane crop.

In another aspect, the present invention provides a stable formulation comprising said insecticidal composition. In a preferred aspect, said insecticidal composition is formulated as an oil dispersion.

In yet another aspect, the present invention provides a process for preparing said insecticidal composition.

Detail description of the invention:
Those skilled in the art will be aware that the invention described herein is subject to variations and modifications other than those specifically described. It is to be understood that the invention described herein includes all such variations and modifications. The invention also includes all such steps, features, compositions and compounds referred to or indicated in this specification, individually or collectively, and all combinations of any two or more of said steps or features.

Unless otherwise specified, all terms used in disclosing the invention, including technical and scientific terms, have the meaning as commonly understood by one of the ordinary skill in the art to which the invention belongs. For further guidance, term definitions may be included to better appreciate the teaching of the present invention.

As used herein, the term “plant” refers to any plant or part thereof including serial and subterranean parts of the plant. It is contemplated that the parts of the plant may before example, flowers, fruits or vegetables, shoots, leaves, needles, stalks, stems, fruiting bodies, seeds also roots and that parts of the plants may or may not be attached to the remainder of the plant.

The term “locus” of a plant as used herein is intended to embrace the place on which the plants are growing, where the plant propagation materials of the plants are sown or where the plant propagation materials of the plants will be placed into the soil.

The term “plant propagation material” is understood to denote generative parts of a plant, such as seeds, vegetative material such as cuttings or tubers, roots, fruits, tubers, bulbs, rhizomes and parts of plants, germinated plants and young plants which are to be transplanted after germination or after emergence from the soil. These young plants may be protected before transplantation by a total or partial treatment by immersion.

It is to be understood that the singular forms “a,” “an,” and “the” include plural referents unless the context clearly dictates otherwise.

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.
The term "insects" as used herein, includes all organisms in the class "Insecta."

The term "Insecticidal" as used herein, refers to the ability of a pesticide to increase mortality or inhibit growth rate of insects.

The terms “weight percent”, “wt-%”, “percent by weight”, “% by weight” and variations thereof, as used herein, 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 “synergist” as used herein refers to a material which enhances the activity of other materials such as insecticides so that the overall activity of the composition is greater than the sum of the individual ingredients.

Features that are described and/or illustrated with respect to one embodiment may 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.

Chlorantraniliprole IUPAC name 5-bromo-N-[4-chloro-2-methyl-6-(methylcarbamoyl)phenyl]-2-(3-chloropyridin-2-yl)pyrazole-3-carboxamide was developed world-wide by DuPont belongs to the class of selective insecticides featuring a novel mode of action to control a range of pests of the order Lepidoptera and some other Coleoptera, Diptera and Isoptera species. Chlorantraniliprole opens muscular calcium channels (in particular the ryanodine receptor), rapidly causing paralysis and ultimately death of the sensitive species.

Lambda cyhalothrinIUPAC name ([(R)-cyano-(3-phenoxyphenyl)methyl] 3-[(Z)-2-chloro-3,3,3-trifluoroprop-1-enyl]-2,2-dimethylcyclopropane-1-carboxylate) belongs to the pyrethroid chemical class of pesticides. It is a non-systemic insecticide with contact and stomach action and repellant properties. It gives rapid knockdown and long residual activity. It is very useful for control and management of aphids, Colorado beetles, thrips, lepidoptera larvae, coleoptera larvae and adults, etc. in cereals, hops, ornamentals, potatoes, vegetables, cotton and other crops. It acts on the nervous system of insects and disturbs the function of neurons by interaction with the sodium channels.

Thiamethoxam IUPAC name (EZ)-3-[(2-chlorothiazol-5-yl)methyl]-5-methyl-N-nitro-1,3,5-oxadiazinan-4-imine is a systemic insecticide belonging to the class of neonicotinoids. It has a broad spectrum of activity against many types of insects. It is a contact and stomach poison. It is particularly effective as a seed treatment against soil-dwelling and early season pests. As a seed treatment, the product can be used on a greater number of crops (including cereals) against a broader range of pests.

Oil of clove or clove oil is an essential oil extracted from the clove plant, Syzygiumaromaticum. It is commonly used in aromatherapy and for flavouring food and some medicines. Madagascar and Indonesia are the main producers of clove oil. Clove oil is produced by distilling the dried flower buds that are collected from the clove tree. It may also be derived from flower buds, stems and twigs of Syzygiumaromaticum. The major constituent of the clove oil, eugenol (88.61%) has a phenolic structure which is known to be an important source of potent insecticides, fungicides, herbicides for pest control.

In the present invention, clove oil is being used as a synergist wherein it enhances the efficacy of the insecticidal composition. The present inventors have surprisingly found that the insecticidal efficacy of the mixture is enhanced when clove oil is used in conjunction with the active ingredient combination of Chlorantraniliprole, Lambda cyhalothrin and Thiamethoxam. Thus, a true, unforeseeable synergistic effect is evident in the present insecticidal composition and not just an addition of activities.

Clove oil has been procured from a commercial source (Yunnan lorraine Aromatic Products Co., Ltd, headquartered at Room B-26,No.3 Jingkai Road Kunming Nation-Class, Economic & Tech Development Zone, Kunming, Yunnan, China) and no biological material has been used in the present invention.

Embodiments of the present invention provide insecticidal combination and composition comprising said combination that possess an enhanced efficacy over the individual active ingredient compounds, when used in isolation.

The present invention thus provides an insecticidal composition comprising a) Chlorantraniliprole as the first active ingredient b) Lambda cyhalothrin as the second active ingredient c) Thiamethoxam as the third active ingredient and clove oil as the synergist wherein Chlorantraniliprole is present in an amount ranging from 2-35% w/w, Lambda cyhalothrin is present in an amount ranging from 2-25% w/w, Thiamethoxam is present in an amount ranging from8-40% w/w and the synergist clove oil is present in an in amount ranging from 0.1-2% w/w of the insecticidal composition.

In a preferred embodiment, Chlorantraniliprole is present in an amount 6% w/w, Lambda cyhalothrin is present in an amount 4% w/w, Thiamethoxam is present in an amount 15% w/w and clove oil is present in an amount of 0.5%w/w of the insecticidal composition.

In an embodiment, the Insecticidal composition of the present invention comprising the said actives exhibits synergistic effect in control of lepidopteran pests in agricultural crops, particularly Early shoot borer-chiloinfuscatellus on sugarcane crop.

In an embodiment, the insecticidal composition of the present invention may be applied to a variety of agricultural crops including but not limited to Sugarcane, Rice, Chili, Maize, Tomato, Cotton, Brinjal, Okra and Capsicum.

In an embodiment, the insecticidal composition of the present invention may be used to control early shoot borer chiloinfuscatellus on sugarcane crop.

In an embodiment, the insecticidal composition of the present invention further comprises at least one agriculturally acceptable excipient. In an embodiment, at least one excipient is selected from the group consisting of at least a wetting agent, at least a dispersing agent, at least an emulsifier, at least a solubilizer, at least a solvent and combinations thereof. In a preferred embodiment, the insecticidal composition of the present invention is formulated as an oil dispersion formulation.

In a more preferred embodiment, the insecticidal composition of the present invention is formulated in the form of an oil dispersion formulation comprising a wetting agent, a dispersing agent, an emulsifier, a solubilizer, a modifier and a solvent.

In an embodiment, the wetting agent is selected from the group comprising alkylphenylpolyoxyethylene ether, isotridecyl alcohol ethoxylate and combinations thereof.

In a preferred embodiment, the wetting agent is alkyl phenyl polyoxyethylene ether. In an embodiment, the wetting agent is present in an amount ranging from 0.5-4% w/w of the insecticidal composition.

In an embodiment, the dispersing agent is selected from the group consisting of polyalkyl phenol ether sulphate, behenyl alcohol ethoxylate, nonyl phenol ethoxylate, styrenated phenol ethoxylate, oleyl cetyl alcohol ethoxylate, Tridecylalcohol ethoxylate, sodium naphthalene formaldehyde sulphonate, phenol sulphonate sodium, sodium lauryl ether sulphonate and combinations thereof. Preferably, the dispersing agent is block copolymer of polyethylene glycol and 12-hydroxystearic acid.

In an embodiment, the dispersing agent is present in an amount ranging from 3-10%w/w of the insecticidal composition.

In an embodiment, the emulsifier is selected from the group comprising ethoxylated nonylphenols, reaction products of alkylphenols with ethylene oxide and/or propylene oxide, ethoxylated arylalkylphenols, furthermore ethoxylated and propoxylatedarylalkylphenols, and sulphated or phosphated arylalkyl ethoxylates or -ethoxy- propoxylates, where sorbitan derivatives, such as polyethylene oxide-sorbitan fatty acid esters and sorbitan fatty acid esters, and combinations thereof.

In an embodiment, the emulsifier is present in an amount ranging from 2-8 %w/w of the insecticidal composition.

In an embodiment, the suitable solubilizers are solvents which promote the dissolution of the active compound in the main solvent or prevent its precipitation. Examples are polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylated castor oil, and polyoxyethylated sorbitan ester and combinations thereof.

In an embodiment, the solubilizer is present in an amount ranging from 1-8 % w/w of the insecticidal composition.

In an embodiment, the modifier improves the formulation's stability, flow properties, and overall performance. The modifier is selected from the group comprising bentinite, Attapulgite, precipitated silica, synthetic clay and combinations thereof.

In an embodiment, the modifier is present in an amount ranging from 0.5-7 % w/w of the insecticidal composition.

In an embodiment, water immiscible solvents include aromatic and non-aromatic hydrocarbons, halogenated aromatic and non-aromatic hydrocarbons, petroleum distillates, aromatic and non-aromatic ethers, esters or amides, oils or mixtures thereof. In a further embodiment, the oils can be one or more of a mineral oil, petroleum oil, vegetable oil or animal oil or derivatives or mixtures thereof. In an embodiment, the solvent is methyl oleate. However, those skilled in the art will appreciate that it is possible to utilize other water immiscible solvents without departing from the scope of the present invention.

In an embodiment, the insecticidal composition is formulated in a form selected from the group comprising water-soluble concentrates (SL), emulsifiable concentrates (EC), emulsions (EW), micro-emulsions (ME), Suspension concentrates (SC), oil-based suspension concentrates (OD), flowable suspensions (FS), water-dispersible granules (WG), water-soluble granules (SG), wettable powders (WP), water soluble powders (SP), granules (GR), encapsulated granules (CG), fine granules (FG), macrogranules (GG), dry flowables (DF), aqueous Suspo-emulsions (SE), capsule suspensions (CS) and microgranules (MG). In a preferred embodiment, the Insecticidal composition is in the form of suspension concentrates (SC), water-dispersible granule (WDG) and wettable powder (WP).In a preferred embodiment, the insecticidal composition of the present invention is formulated as an oil dispersion.

In a preferred embodiment, the insecticidal composition of the present invention is formulated as an oil dispersion as it is a non-aqueous formulation with high biological efficacy ideal for active ingredients which have relatively less solubility in water. An oil dispersion (OD) formulation is a solid active ingredient dispersed in oil. The oil can vary from paraffinic to aromatic solvent types and vegetable oil or methylated seed oils. Ideally the active ingredient is uniformly suspended in the oil phase.

ODs are an excellent delivery system for water sensitive active ingredients due to their better spray retention, spreading and foliar uptake as the carrier oil often acts as an adjuvant.

Other benefits associated with oil dispersion formulation are listed below:

1. Especially suited to hydrolytically unstable actives allowing them to be formulated as liquid formulations.
2. The oil continuous phase acts as a built-in adjuvant.
3. The oil adjuvant can provide both penetration enhancement and spray retention enhancement.
4. Does not need preserving (water free)
5. Retards evaporation loss and enhances absorption of active ingredients;
6. Improved rain fast properties.

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

Example 1: Preparation of Insecticidal composition as oil dispersion (OD)
The following compositions have been prepared which are given below-

Table 1:Insecticidal composition as oil dispersion (OD)
Composition I1 I2 I3 I4 I5 I6 I7 I8 I9 I10
B 6 4 15 0 1.5 5 4 2 4 58.5

C 6 4 15 0.5 1.5 5 4 2 4 58
D 4 3 10 0.4 1.5 5 4 2 4 66.1
E 5 4 12.5 0.4 1.5 5 4 2 4 61.6
F 8 7 20 0.8 1.5 5 4 2 4 47.7
G 35 3 10 0.4 1.5 5 4 2 4 35.1
H 3 35 10 0.4 1.5 5 4 2 4 35.1
J 3 3 40 0.4 1.5 5 4 2 4 37.5
K 15 15 15 2 1.5 5 4 2 4 38
L 10 5 10 2 1.5 5 4 2 4 58

C1-a 6 4 15 0.5 0.5 5 4 2 4 59
C1-b 6 4 15 0.5 1.5 3 4 2 4 60
C1-c 6 4 15 0.5 1.5 5 2 2 4 60
C1-d 6 4 15 0.5 1.5 5 4 1 4 59
C1-e 6 4 15 0.5 1.5 5 4 2 0.5 61.5

D1-a 4 3 10 0.4 0.5 5 4 2 4 67.1
D1-b 4 3 10 0.4 1.5 3 4 2 4 68.1
D1-c 4 3 10 0.4 1.5 5 2 2 4 68.1
D1-d 4 3 10 0.4 1.5 5 4 1 4 67.1
D1-e 4 3 10 0.4 1.5 5 4 2 0.5 69.6

E1-a 5 4 12.5 0.4 0.5 5 4 2 4 62.6
E1-b 5 4 12.5 0.4 1.5 3 4 2 4 63.6
E1-c 5 4 12.5 0.4 1.5 5 2 2 4 63.6
E1-d 5 4 12.5 0.4 1.5 5 4 1 4 62.6
E1-e 5 4 12.5 0.4 1.5 5 4 2 0.5 65.1

F1-a 8 7 20 0.8 0.5 5 4 2 4 48.7
F1-b 8 7 20 0.8 1.5 3 4 2 4 49.7
F1-c 8 7 20 0.8 1.5 5 2 2 4 49.7
F1-d 8 7 20 0.8 1.5 5 4 1 4 48.7
F1-e 8 7 20 0.8 1.5 5 4 2 0.5 51.2

C2-a 6 4 15 0.5 0.5 5 4 2 4 59
C2-b 6 4 15 0.5 2.5 3 4 2 4 59
C2-c 6 4 15 0.5 2.5 5 2 2 4 59
C2-d 6 4 15 0.5 2.5 5 4 1 4 58
C2-e 6 4 15 0.5 2.5 5 4 2 0.5 60.5

D2-a 4 3 10 0.4 0.5 5 4 2 4 67.1
D2-b 4 3 10 0.4 2.5 3 4 2 4 67.1
D2-c 4 3 10 0.4 2.5 5 2 2 4 67.1
D2-d 4 3 10 0.4 2.5 5 4 1 4 66.1
D2-e 4 3 10 0.4 2.5 5 4 2 0.5 68.6

E2-a 5 4 12.5 0.4 0.5 5 4 2 4 62.6
E2-b 5 4 12.5 0.4 2.5 3 4 2 4 62.6
E2-c 5 4 12.5 0.4 2.5 5 2 2 4 62.6
E2-d 5 4 12.5 0.4 2.5 5 4 1 4 61.6
E2-e 5 4 12.5 0.4 2.5 5 4 2 0.5 64.1

F2-a 8 7 20 0.8 0.5 5 4 2 4 48.7
F2-b 8 7 20 0.8 2.5 3 4 2 4 48.7
F2-c 8 7 20 0.8 2.5 5 2 2 4 48.7
F2-d 8 7 20 0.8 2.5 5 4 1 4 47.7
F2-e 8 7 20 0.8 2.5 5 4 2 0.5 50.2

C3-a 6 4 15 0.5 0.5 2.5 4 2 4 61.5
C3-b 6 4 15 0.5 2.5 3 4 2 4 59
C3-c 6 4 15 0.5 2.5 2.5 2 2 4 61.5
C3-d 6 4 15 0.5 2.5 2.5 4 1 4 60.5
C3-e 6 4 15 0.5 2.5 2.5 4 2 0.5 63

D3-a 4 3 10 0.4 0.5 2.5 4 2 4 69.6
D3-b 4 3 10 0.4 2.5 3 4 2 4 67.1
D3-c 4 3 10 0.4 2.5 2.5 2 2 4 69.6
D3-d 4 3 10 0.4 2.5 2.5 4 1 4 68.6
D3-e 4 3 10 0.4 2.5 2.5 4 2 0.5 71.1

E3-a 5 4 12.5 0.4 0.5 2.5 4 2 4 65.1
E3-b 5 4 12.5 0.4 2.5 3 4 2 4 62.6
E3-c 5 4 12.5 0.4 2.5 2.5 2 2 4 65.1
E3-d 5 4 12.5 0.4 2.5 2.5 4 1 4 64.1
E3-e 5 4 12.5 0.4 2.5 2.5 4 2 0.5 66.6

F3-a 8 7 20 0.8 0.5 2.5 4 2 4 51.2
F3-b 8 7 20 0.8 2.5 3 4 2 4 48.7
F3-c 8 7 20 0.8 2.5 2.5 2 2 4 51.2
F3-d 8 7 20 0.8 2.5 2.5 4 1 4 50.2
F3-e 8 7 20 0.8 2.5 2.5 4 2 0.5 52.7

C4-a 6 4 15 0.5 0.5 2.5 2 2 4 63.5
C4-b 6 4 15 0.5 2.5 3 2 2 4 61
C4-c 6 4 15 0.5 2.5 2.5 2 2 4 61.5
C4-d 6 4 15 0.5 2.5 2.5 2 1 4 62.5
C4-e 6 4 15 0.5 2.5 2.5 2 2 0.5 65

D4-a 4 3 10 0.4 0.5 2.5 2 2 4 71.6
D4-b 4 3 10 0.4 2.5 3 2 2 4 69.1
D4-c 4 3 10 0.4 2.5 2.5 2 2 4 69.6
D4-d 4 3 10 0.4 2.5 2.5 2 1 4 70.6
D4-e 4 3 10 0.4 2.5 2.5 2 2 0.5 73.1

E4-a 5 4 12.5 0.4 0.5 2.5 2 2 4 67.1
E4-b 5 4 12.5 0.4 2.5 3 2 2 4 64.6
E4-c 5 4 12.5 0.4 2.5 2.5 2 2 4 65.1
E4-d 5 4 12.5 0.4 2.5 2.5 2 1 4 66.1
E4-e 5 4 12.5 0.4 2.5 2.5 2 2 0.5 68.6

F4-a 8 7 20 0.8 0.5 2.5 4 2 4 51.2
F4-b 8 7 20 0.8 2.5 3 4 2 4 48.7
F4-c 8 7 20 0.8 2.5 2.5 2 2 4 51.2
F4-d 8 7 20 0.8 2.5 2.5 4 1 4 50.2
F4-e 8 7 20 0.8 2.5 2.5 4 2 0.5 52.7

C5-a 6 4 15 0.5 0.5 2.5 2 2 2 65.5
C5-b 6 4 15 0.5 2.5 3 2 2 2 63
C5-c 6 4 15 0.5 2.5 2.5 2 2 2 63.5
C5-d 6 4 15 0.5 2.5 2.5 2 1 2 64.5
C5-e 6 4 15 0.5 2.5 2.5 2 2 0.5 65

D5-a 4 3 10 0.4 0.5 2.5 2 2 2 73.6
D5-b 4 3 10 0.4 2.5 3 2 2 2 71.1
D5-c 4 3 10 0.4 2.5 2.5 2 2 2 71.6
D5-d 4 3 10 0.4 2.5 2.5 2 1 2 72.6
D5-e 4 3 10 0.4 2.5 2.5 2 2 0.5 73.1

E5-a 5 4 12.5 0.4 0.5 2.5 2 2 2 69.1
E5-b 5 4 12.5 0.4 2.5 3 2 2 2 66.6
E5-c 5 4 12.5 0.4 2.5 2.5 2 2 2 67.1
E5-d 5 4 12.5 0.4 2.5 2.5 2 1 2 68.1
E5-e 5 4 12.5 0.4 2.5 2.5 2 2 0.5 68.6

F5-a 8 7 20 0.8 0.5 2.5 4 2 2 53.2
F5-b 8 7 20 0.8 2.5 3 4 2 2 50.7
F5-c 8 7 20 0.8 2.5 2.5 2 2 2 53.2
F5-d 8 7 20 0.8 2.5 2.5 4 1 2 52.2
F5-e 8 7 20 0.8 2.5 2.5 4 2 0.5 52.7
Wherein I1= Chlorantraniliprole, I2= Lambda cyhalothrin, I3= Thiamethoxam, I4=Clove oil, I5=Wetting agent, I6=Dispersing agent, I7=Emulsifier, I8=Solubilizer, I9=Precipitate silica, and I10=Solvent.
Preparation method of OD:
Step 1: Dispersing and wetting agent were first diluted in the solvent(Methyl oleate) and solubilized by high- speed mixer and grind for homogeneous mixture Step 2: Add Chlorantraniliprole technical, Thiamethoxam technical followed by Lambda cyhalothrin technical and clove oil to the above mixture to obtain a homogenous mass.
Step 3: The above mixed mass is subjected to grinding in sand mill. Grinding is carried out until a mean particle size of <5 micron is obtained. Emulsifier and solubilizer are then added in the desired quantity.
Step 4: Add precipitate silica under low stirring and mix well. After mixing till homogeneous, check for quality parameter. If ok pack as desire packing or transfer to storage vessel.
Example 2: Field evaluation of the bio efficacy of the present Insecticidal composition and comparison with other compositions (not forming part of the invention)
Various Insecticidal composition prepared as per the present invention and other compositions (not forming part of the invention) were tested for their bioefficacy against early shoot borer on a local variety of sugarcane crop. The plants were aligned in a plot size of 50 sq. meter in a random block design. The trials were carried out at Saharanpur, Uttar Pradesh in the Rabi season 2022-23 at a temp 35? at 75% relative humidity and non-windy conditions. The application of all Insecticidal compositions (prepared as per the present invention as well as those compositions not forming part of the invention) was foliar (over the top) and was carried out 2 times at 20 days interval.

Measured quantity of the chemical was added to required volume of water @ 375 lit. /ha for spray. The spray tank was filled with ½ the quantity of clean required volume of water and then the measured chemical (according to the dose) was added followed by the rest half quantity of water. The solution was stirred well before application and through coverage was ensured.
EVALUATION OF BIO-EFFICACY IN SUGARCANE
For Sugarcane early shoot borer:
Count the number of dead hearts from whole plot at 10 DA1A, 20 DA1A and 10 DA2A and 20 DA2A

Percent control: Per-cent control of Live Population was calculated based on no. of live Sucking pest and Spodoptera litura population. Formula is given below.

C – T
Percent control = …………. × 100
C
Where C = No. of Dead Hearts in control plot
T = No. of Dead Hearts in treated plot

Table 2: Bio efficacy of various mixtures of Chlorantraniliprole + Lambda cyhalothrin + Thiamethoxam + Clove oil on Sugarcane:
No. Product Dose/Ha Number of Dead Hearts in 100 sqm (Early Shoot Borer)
10 DA1A % Control 20 DA1A % Control 10 DA2A % Control 20 DA2A % Control
T-1 Untreated 45 30 35 50
T-2 Composition B 750 ml 17 62.22 21 30 22 37.14 24 52
T-3 Composition B 1000 ml 15 66.67 13 56.67 14 60 12 76
T-4 Composition B 1250 ml 14 68.89 10 66.67 9 74.29 9 82
T-5 Composition C 750 ml 7 84.44 6 80 3 91.43 8 84
T-6 Composition C 1000 ml 3 93.33 2 93.33 1 97.14 2 96
T-7 Composition C 1250 ml 2 95.56 1 96.67 1 97.14 1 98
T-8 Composition D 750 ml 22 51.11 17 43.33 15 57.14 16 68
T-9 Composition D 1000 ml 20 55.56 14 53.33 12 65.71 14 72
T-10 Composition D 1250 ml 18 60 10 66.67 10 71.43 12 76
T-11 Composition E 750 ml 9 80 15 50 17 51.43 19 62
T-12 Composition E 1000 ml 7 84.44 10 66.67 14 60 12 76
T-13 Composition E 1250 ml 5 88.89 8 73.33 6 82.86 10 80
T-14 Composition F 750 ml 10 77.78 5 83.33 6 82.86 5 90
T-15 Composition F 1000 ml 5 88.89 3 90 3 91.43 3 94
T-16 Composition F 1250 ml 4 91.11 2 93.33 2 94.29 1 98
T-17 Chlorantraniliprole 18.5 SC “Coragen” 375 ml 5 88.89 6 80 4 88.57 4 92
T-18 Thiamethoxam 25 WG “Extra Super” 1000 gm 12 73.33 14 53.33 12 65.71 19 62
T-19 Lambda cyhalothrin 5 EC “Karate” 1000 ml 22 51.11 12 60 12 65.71 16 68
T-20 Clove Oil 5 EC 500 ml 35 22.22 22 26.67 24 31.43 26 48
The bio efficacy of insecticidal composition C is similar for the compositionsof C1 a-e, C2a-e,…Cn a-e. Similarly, the efficacy of composition of D, E, and F would also be similar to Dn a-e, En a-e, Fn a-e wherein n is an integer.
Example 3: Evaluation of Phytotoxicity
Visual observations were recordedat10 and 20 days after application. The parameters observed were leaf injury on tip/surface, necrosis, vein clearing, epinasty, hyponasty and wilting. For the rating on phytotoxicity the core Scale of 0 – 10 was followed for leaf injury on tips/surface.
Table 3: Phytotoxicity symptoms scoring and rating for leaf injury on tip/surface
Leaf injury on tips/surface Rating
0% 0
1-10% 1
11-20% 2
21-30% 3
31-40% 4
41-50% 5
51-60% 6
61-70% 7
71-80% 8
81-90% 9
91-100% 10

Table 4:
S.no. Treatment details Dose (gm)/ha 1 DAA 3 DAA 5 DAA 7 DAA 10 DAA 15 DAA
1 Untreated 0 0 0 0 0 0
2 Composition B 750 ml 0 0 0 0 0 0
3 Composition B 1000 ml 0 0 0 0 0 0
4 Composition B 1250 ml 0 0 0 0 0 0
5 Composition C 750 ml 0 0 0 0 0 0
6 Composition C 1000 ml 0 0 0 0 0 0
7 Composition C 1250 ml 0 0 0 0 0 0
8 Composition D 750 ml 0 0 0 0 0 0
9 Composition D 1000 ml 0 0 0 0 0 0
10 Composition D 1250 ml 0 0 0 0 0 0
11 Composition E 750 ml 0 0 0 0 0 0
12 Composition E 1000 ml 0 0 0 0 0 0
13 Composition E 1250 ml 0 0 0 0 0 0
14 Composition F 750 ml 0 0 0 0 0 0
15 Composition F 1000 ml 0 0 0 0 0 0
16 Composition F 1250 ml 0 0 0 0 0 0
17 Chlorantraniliprole 18.5 SC 375 ml 0 0 0 0 0 0
18 Thiamethoxam 25 WG 1000 gm 0 0 0 0 0 0
19 Lambda cyhalothrin 5 EC 1000 ml 0 0 0 0 0 0
20 Clove oil 5 % EC 500 0 0 0 0 0 0

The foregoing description is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will be readily apparent to those skilled in the art, it is not desired to limit the invention to the exact construction and process shown as described above. Accordingly, all suitable modifications and equivalents may be considered to fall within the scope of the invention as defined by the claims that follow. The words "comprise," "comprising," "include," "including," and "includes" when used in this specification and in the following claims are intended to specify the presence of stated features, integers, components, or steps, but they do not preclude the presence or addition of one or more other features, integers, components, steps, or groups thereof.
, Claims:We Claim:
1. An insecticidal composition comprising:
a) Chlorantraniliprole in an amount ranging from2-35% w/w,
b) Lambda cyhalothrin in an amount ranging from 2-25% w/w and
c) Thiamethoxam in an amount ranging from 8-40%w/w and
d) Clove oil in an amount ranging from 0,1-2%w/w
2. The insecticidal composition as claimed in claim 1, wherein said insecticidal composition further comprises at least one agriculturally acceptable excipient.
3. The insecticidal composition as claimed in claim 1, wherein said insecticidal composition is formulated in a form selected from the group comprising water-soluble concentrates (SL), emulsifiable concentrates (EC), emulsions (EW), micro-emulsions (ME), Suspension concentrates (SC), oil-dispersion (OD), flowable suspensions (FS), water-dispersible granules (WG), water-soluble granules (SG), wettable powders (WP), water soluble powders (SP), dry flowables (DF), granules (GR), encapsulated granules (CG), fine granules (FG), macrogranules (GG), aqueous Suspo-emulsions (SE), capsule suspensions (CS) and microgranules (MG).
4. The insecticidal composition as claimed in claim 1, wherein said insecticidal composition is preferably formulated in the form of an oil dispersion (OD).
5. The insecticidal composition as claimed in claim 4, wherein said insecticidal composition further comprises at least adispersing agent, at least a wetting agent, at least an emulsifying agent, atleast a solubilizer, at least a solvent.
6. The insecticidal composition as claimed in claim 5, wherein said insecticidal composition comprises at least a wetting agent ranging from 0.5-4%w/w, at least a dispersing agent ranging from 3-10 %w/w, at least an emulsifying agent ranging from 2-8% w/w, at least a solubilizer ranging from 1-8%w/wof the insecticidal composition and at least a solvent ranging from 20-65%w/w.
7. The insecticidal composition as claimed in claim 1, wherein Chlorantraniliprole is present in an amount ranging from 2-35%w/w, Lambda cyhalothrin is present in an amount ranging from 2-25% w/w, Thiamethoxam is present in an amount ranging from 8-40% and Clove oil is present in an amount ranging from 0.1-2 % w/w of said insecticidal composition.
8. A method for controlling insect pests in agricultural crop, said method comprising contacting the insect pests with the insecticidal composition as claimed in the preceding claims.
9. A process for preparing an insecticidal composition as claimed in claim 1 in the form of an oil dispersion, said process comprising:
1) Dispersing and wetting agent were first diluted in the solvent (Methyl oleate) and solubilized by high- speed mixer and grinded to obtain a homogeneous mixture.
2) Chlorantraniliprole technical, Thiamethoxam technical followed by Lambda cyhalothrin technical and clove oil was then added to the above mixture to obtain a homogenous mass.
3) The above mixed mass is subjected to grinding in sand mill. Grinding is carried out until a mean particle size of <5 micron is obtained. Emulsifier and solubilizer are then added in the desired quantity.
4) Precipitate silica was added under low stirring and then mixed well.
5) Quality parameter were checked.