DESC:FIELD OF THE INVENTION
The present invention relates to the field of pest control and insecticides. More specifically, it pertains to a synergistic insecticidal composition that combines nitenpyram, pyriproxyfen, and tolfenpyrad for enhanced efficacy against a wide range of insect pests.

BACKGROUND OF THE INVENTION
Insecticides are agrochemicals in the pesticide family which are used to control insects by killing them or preventing their 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 by controlling 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.
Insecticides work differently based on their mode of actions; some disrupt the nervous system, whereas others damage the exoskeletons, others repel or control insects. Insecticides application helps in managing and mitigating insects; thereby guaranteeing crop protection and preventing yield loss.
Processes for formulating insecticidal agents and compositions have been developed to control insect pests and in practice have been used for a single or a mixed agent. However, processes for economically efficient and ecologically safe insect control compositions are still being sought. A process for the preparation of insecticidal compositions which allows for reduced effective dosage rates, increased environmental safety and lower incidence of insect resistance are highly desirable. Although the rotational application of insect control agents having different modes of action may be adopted for good pest management practice, this approach does not necessarily give satisfactory insect control. Further, even though combinations of insect control agents have been studied, a high synergistic action has not always been found. Obtaining an insecticidal composition which demonstrates no cross-resistance to existing insecticidal agents, no toxicity problems and little negative impact on the environment is extremely difficult.
IN201721029744 discloses insecticidal composition comprising of Fipronil, Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide.
Insecticides are used widely and very frequently in commercial agriculture and has enabled an enormous increase in crop yields and product quality which ultimately increased the ease to farmers in terms of economic advantage as well as ease of farming activities.
There are many combinations of insecticides known in the art for the control of soil borne pests. However, there is a need for improvement of these combinations. Single and multiple insecticide combinations used over a long period of time have resulted in resistance. With the onset of resistance to certain pests, there is a need in the art for a novel combination of insecticides that decrease chances of resistance and improve the spectrum of disease and pest control.

OBJECT OF THE INVENTION
One objective of the present invention is to provide a synergistic insecticidal combination of (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad.
Another objective of the present invention is to provide a synergistic insecticidal composition comprising of (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad with suitable agrochemical additives.
Another objective of the present invention is to provide a synergistic insecticidal composition of (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad formulated as emulsifiable concentrate (EC), micro emulsion (ME), and wettable powder (WP).
Yet another objective of the present invention is to provide a synergistic insecticidal composition useful for insect control with enhanced crop protection and delayed dominance of the resistant strains of pests.
Yet another objective of the present invention is to provide a synergistic insecticidal composition that can improve biological performance in a single application and minimize occupational exposure and hazards.
Yet another objective of the present invention is to provide a synergistic insecticidal composition that is effective against a wide variety of chewing, boring and sucking insects.
In yet another objective of the present invention is to provide improved combinations of insecticides that promote plant health.

SUMMARY OF THE INVENTION
The present invention provides a novel insecticidal composition that synergistically combines nitenpyram, pyriproxyfen, and tolfenpyrad. This composition demonstrates enhanced insecticidal activity, effectively controlling a broad spectrum of insect pests while also offering reduced toxicity to non-target organisms.
In an aspect of the present invention, a synergistic insecticidal composition comprising of (a) nitenpyram present in a range from 5% (w/w) to 15% (w/w), (b) pyriproxyfen present in a range from 5% (w/w) to 15% (w/w), (c) tolfenpyrad present in a range from 5% (w/w) to 25% (w/w), and suitable agrochemical additives is provided.
In an aspect of the present invention, the synergistic insecticidal composition is formulated as emulsion concentrate (EC), micro emulsion (ME), and wettable powder (WP).
In an aspect of the present invention, the synergistic insecticidal composition formulated as emulsion concentrate (EC) or micro emulsion (ME) contains suitable agrochemical additives selected from an emulsifier, a stabilizer, and a solvent.
In an aspect of the present invention, an emulsifier is selected from the group comprising of linear or branched alkylbenzene sulfonates, alcohol ether sulfates, calcium salt of dodecyl benzene sulphonates, non-ionic surfactant blend, ethoxylated and alkoxylated fatty acids, tristyryl phenol ethoxylate with 16 EO, ethoxylated amines, ethoxylated alcohol, alkyl and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylates, alkoxylated alcohol, Calcium alkyl aryl sulphonate, Polyaryl phenol ethoxylate sulphate ammonium salt and a combination thereof, present in an amount of 1 to 15% (w/w).
In an aspect of the present invention, the stabilizer is epoxidized soya bean oil (ESO) present in an amount of 1% to 2% (w/w).
In an aspect of the present invention, the solvent is selected from solvent C9 (heavy aromatic solvent naphtha (petroleum)), dipropylene glycol linear monomethyl ether (DPM), and distilled water, present in Q. S.
In another aspect of the present invention, the synergistic insecticidal composition is formulated as wettable powder (WP).
In another aspect of the present invention, the synergistic insecticidal composition in form of wettable powder contains suitable agrochemical additives selected from a wetting agent, a dispersing agent, an anticaking agent, a defoamer, and a filler.
In another aspect of the present invention, the wetting agent is selected from butylated naphthalene sulphonic acid and dioctyl sulphosuccinate, sodium alpha olefin sulphonates, and sodium di-isopropyl naphthalene sulphonates, present in an amount of 1% to 5% (w/w).
In another aspect of the present invention, the dispersing agent is selected from sodium salt of naphthalene sulphonates formaldehyde condensate, and modified styrene acrylic polymer, present in an amount of 1% to 5% (w/w).
In another aspect of the present invention, the Anti caking agent is silicon dioxide or precipitated silica, present in an amount of 1% to 5% (w/w).
In another aspect of the present invention, the defoamer is polydimethylsiloxane present in an amount of 1% to 2% (w/w).
In another aspect of the present invention, the filler is china clay, present in Q.S.
In yet another aspect the present invention provides insecticidal composition useful for enhanced insect control with enhanced crop protection and delayed dominance of the resistant strains of pests.
In yet another aspect the present invention provides a synergistic insecticidal composition that can improve biological performance in a single application and minimize occupational exposure and hazards.
In yet another aspect the present invention provides an improved combination of insecticides for the control of chewing, boring and sucking insects.
In yet another aspect the present invention provides improved combinations of insecticides that promote plant health.
In yet another aspect the present invention provides a process for the preparation of a synergistic insecticidal composition comprising of nitenpyram, pyriproxyfen, and tolfenpyrad.

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 insecticides that allows the application of the said insecticides 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, emulsifiers, crystallization inhibitors, viscosity modifiers, suspending agents, dyes, antioxidants, foaming agents, mixing aids, neutralizers or pH adjusting substances and buffers, wetting agents, absorption enhancers, micronutrients, plasticizers, lubricants, thickeners, anti-freezing agents, and sterilization agents among others.
The present invention aims to develop a novel insecticidal combination of nitenpyram, pyriproxyfen, and tolfenpyrad with suitable agrochemical additives.
Nitenpyram is a synthetic, nicotine-related insecticide, and has an effect on the nicotinic acetylcholine receptors. This compound is an insect neurotoxin belonging to the class of neonicotinoids which works by blocking neural signaling of the central nervous system. It does so by binding irreversibly to the nicotinic acetylcholine receptor (nACHr) thereby stopping the flow of ions in the postsynaptic membrane of neurons leading to paralysis and death.
Nitenpyram has been used on many commercial crops, such as cotton and corn, and can be applied in various ways. Commonly used techniques are dusting and seed treatment. Seed treatment allows for a long-lasting immunity against insects damaging the crops. The use of nitenpyram has been shown to be highly effective in protecting crops, as it's generally less toxic for non-target organisms, while killing off crop destroying insects. It is used for controlling aphids, thrips, leafhoppers, whiteflies, and other sucking insects on rice and glasshouse crops.
Nitenpyram is a neonicotinoid insecticide known for its rapid action against a variety of insects. It is chemically known as (E)-N1-[(6-Chloropyridin-3-yl)methyl]-N1-ethyl-N'1-methyl-2-nitroethene-1,1-diamine, and has following structure:

Pyriproxyfen is an insect growth regulator that disrupts the development of juvenile insects. It is chemically known as 2-((1-(4-Phenoxyphenoxy)propan-2-yl)oxy)pyridine, and has the following structure:

Tolfenpyrad is a contact insecticide that inhibits an organism's energy metabolism and can also act as a contact fungicide. It was first registered by U.S. Environmental Protection Agency (EPA) for greenhouse use in 2010. In 2013 tolfenpyrad was approved by EPA for outdoor use in vegetables, fruit, and row crops.
Tolfenpyrad is a broad-spectrum insecticide with a unique mode of action. It is chemically known as 4-chloro-3-ethyl-1-methyl-N-[4-(p-tolyloxy) benzyl] pyrazole-5-carboxamide and has following structure:

In an embodiment of the present invention, an insecticidal combination of (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad is provided.
In an embodiment of the present invention, a synergistic insecticidal composition comprises of (a) nitenpyram present in a range from 5% (w/w) to 15% (w/w), (b) pyriproxyfen present in a range from 5% (w/w) to 15% (w/w), (c) tolfenpyrad present in a range from 5% (w/w) to 25% (w/w), and suitable agrochemical additives is provided.
The novel insecticidal composition of the present invention may be formulated into various formulations such as Granular composition (GR), Capsule suspension (CS), Dispersible concentrate (DC), Dustable powder (DP), Powder for dry seed treatment (DS), Emulsifiable/Emulsion concentrate (EC), Emulsifiable granule (EG), Emulsifiable water-in-oil (EO), Emulsifiable powder (EP), Emulsifiable for seed treatment (ES), Emulsifiable oil-in-water Soluble concentrate (SL), Micro emulsion (ME), Spreading oil (SO), Water soluble powder (SP), Water soluble tablet (ST), Ultra-low volume (ULV) suspension, Tablet (TB), Ultra-low volume (ULV) liquid, Water dispersible granules (WG), Wettable powder (WP), Water dispersible powder for slurry seed treatment (WS), Water dispersible tablet (WT), a mixed formulation of CS and SC (ZC), a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW). Preferably, the composition of the present invention is formulated as emulsifiable concentrate (EC), micro emulsion (ME), and wettable powder (WP).
In a preferred embodiment of the present invention, the synergistic insecticidal composition is formulated as emulsifiable concentrate (EC) and micro emulsion (ME).
Emulsifiable concentrates are one of the most common formulation types for agrochemical products. Formulators prefer to prepare emulsifiable concentrates for active ingredients that have low water solubility. An emulsifiable concentrate can be prepared by dissolving the active ingredient in an organic solvent along with sufficient surfactants.
Suitable agrochemical additives may be solid or liquid and the preferred additives used in emulsifiable concentrate (EC) and micro emulsion (ME) formulation process, are for example an emulsifier, a stabilizer, and a solvent.
Accordingly, the composition of the present invention contains an emulsifier selected from the group comprising of linear or branched alkylbenzene sulfonates, alcohol ether sulfates, calcium salt of dodecyl benzene sulphonates, non-ionic surfactant blend, ethoxylated and alkoxylated fatty acids, tristyryl phenol ethoxylate with 16 EO, ethoxylated amines, ethoxylated alcohol, alkyl and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylates, alkoxylated alcohol, Calcium alkyl aryl sulphonate, Polyaryl phenol ethoxylate sulphate ammonium salt and a combination thereof, present in an amount of 1 to 15% (w/w).
Accordingly, the composition of the present invention contains a stabilizer. Stabilizer suitable for use in the present invention is epoxidized soya bean oil (ESO) present in an amount of 1% to 2% (w/w).
Accordingly, the composition of the present invention contains a solvent. Solvents suitable for use in the present invention are C9 (heavy aromatic solvent naphtha (petroleum)), dipropylene glycol linear monomethyl ether (DPM), and distilled water, present in Q. S.
In another embodiment of the present invention, the synergistic insecticidal composition is formulated as wettable powder (WP).
Suitable agrochemical additives may be solid or liquid and the preferred additives used in formulating process for wettable powder, are for example a wetting agent, a dispersing agent, an anticaking agent, a defoamer, and a filler.
A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading.
Accordingly, the composition of the present invention contains a wetting agent selected from the group comprising of butylated naphthalene sulphonic acid and dioctyl sulphosuccinate, sodium alpha olefin sulphonates, and sodium di-isopropyl naphthalene sulphonates, present in an amount of 1% to 5% (w/w).
A dispersant or a dispersing agent is a substance which absorbs onto the surface of particles and helps to preserve the state of dispersion of the particles and prevents them from re-aggregating. Dispersants are added to agrochemical compositions to facilitate dispersion and suspension during manufacture, and to ensure that the particles re-disperse into water in a spray tank.
Accordingly, the composition of the present invention contains a dispersing agent selected from the group comprising of sodium salt of naphthalene sulphonates formaldehyde condensate, and modified styrene acrylic polymer, present in an amount of 1% to 5% (w/w).
An anticaking agent suitable for the purpose of the present invention is silicon dioxide or precipitated silica, present in an amount of 1% to 5% (w/w).
Defoamer is a chemical reagent developed for defoaming, and foam suppression based on the principle of foaming. The defoamer suitable for the purpose of the present invention is Polydimethylsiloxane, present in an amount of 1% to 2% (w/w).
A filler refers to solid chemicals that are added to a pesticide formulation to aid in the delivery of the active ingredient. Accordingly, the composition of the present invention contains a filler china clay, present in Q.S.
In yet another embodiment, the invention provides a method for preparing an insecticidal composition of (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad and suitable agrochemical additives as an emulsion concentrate (EC), micro emulsion (ME), and wettable powder (WP) formulation.
The present invention is further illustrated by the following examples which are provided merely to be exemplary of the inventions and are not intended to limit the scope of the invention. Certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention.
Examples:

Example 1: Nitenpyram 7.5% + Pyriproxyfen 7.5% + Tolfenpyrad 10% EC
S. No. Composition Function Charge in (%)
1. Nitenpyram (Technical) Active ingredient 7.50
2. Pyriproxyfen (Technical) Active ingredient 7.50
3. Tolfenpyrad (Technical) Active ingredient 10.0
4. Alkoxylated alcohol and Ca-DDBS Emulsifier 3.0
5. Tristyryl phenol ethoxylate with 16 EO Emulsifier 4.0
6. Epoxy soya oil Stabilizer 1.0
7. Dipropylene glycol linear monomethyl ether (DPM) Solvent Q. S.

Manufacturing process:
Step 1: According to the batch size, raw materials were mixed in following order.
• Solvent
• Pyriproxyfen technical
• Tolfenpyrad technical
• Nitenpyram technical
Step 2: Dissolving all three active ingredients in a solvent under continuous stirring,
Step 3: Adding required quantity of emulsifiers to the above mixture under stirring conditions for 30 min,
Step 4: Finally adding required amount of stabilizer to the above solution and continue stirring for another 30 min to get emulsifiable concentrate formulation,
Step 5: Submitting the sample for quality control for complete analysis, and
Step 6: Packing the material in suitable bottle.

Example 2: Nitenpyram 15% + Pyriproxyfen 15% + Tolfenpyrad 25% EC
S. No. Composition Function Charge in (%)
1. Nitenpyram (Technical) Active ingredient 15.0
2. Pyriproxyfen (Technical) Active ingredient 15.0
3. Tolfenpyrad (Technical) Active ingredient 25.0
4. Castor oil ethoxylates Emulsifier 5.0
5. Calcium dodecylbenzene sulfonate Emulsifier 3.0
6. Epoxy soya oil Stabilizer 1.0
7. Solvent C9 Solvent Q. S.

The manufacturing procedure for formulation of Example 2 is similar to the one described in Example 1.

Example 3: Nitenpyram 5% + Pyriproxyfen 5% + Tolfenpyrad 5% EC
S. No. Composition Function Charge in (%)
1. Nitenpyram (Technical) Active ingredient 5.0
2. Pyriproxyfen (Technical) Active ingredient 5.0
3. Tolfenpyrad (Technical) Active ingredient 5.0
4. Epoxy soya oil Stabilizer 1.0
5. Castor oil ethoxylates Emulsifier 5.0
6. Calcium dodecylbenzene sulfonate Emulsifier 5.0
7. Solvent C9 Solvent Q. S.

The manufacturing procedure for formulation of Example 3 is similar to the one described in Example 1.

Example 4: Nitenpyram 7.5% + Pyriproxyfen 7.5% + Tolfenpyrad 10% ME
S. No. Composition Function Charge in (%)
1. Nitenpyram (Technical) Active ingredient 7.5
2. Pyriproxyfen (Technical) Active ingredient 7.5
3. Tolfenpyrad (Technical) Active ingredient 10.0
4. Non-ionic surfactant blend (UNITOX NPR) Emulsifier 3.0
5. Castor oil ethoxylates Emulsifier 7.0
6. Calcium dodecylbenzene sulfonate Emulsifier 5.0
7. Distilled water Solvent 1.0
8. Dipropylene glycol linear monomethyl ether (DPM) Solvent Q. S.

Manufacturing process:
Step 1: According to the batch size, raw materials were mixed in following order.
• Solvent
• Pyriproxyfen technical
• Tolfenpyrad technical
• Nitenpyram technical
Step 2: Dissolving all three active ingredients in a solvent under continuous stirring,
Step 3: Adding required quantity of emulsifiers to the above mixture under stirring conditions for 30 min,
Step 4: Finally adding required amount of distilled water to the above solution and continue stirring for another 30 min to get microemulsion formulation,
Step 5: Submitting the sample for quality control for complete analysis, and
Step 6: Packing the material in suitable bottle.

Example 5: Nitenpyram 15% + Pyriproxyfen 15% + Tolfenpyrad 25% ME
S. No. Composition Function Charge in (%)
1. Nitenpyram Active ingredient 15.0
2. Pyriproxyfen Active ingredient 15.0
3. Tolfenpyrad Active ingredient 25.0
4. Calcium alkyl aryl sulphonate Emulsifier 5.0
5. Tristyryl phenol ethoxylates Emulsifier 3.0
6. Polyaryl phenol ethoxylate sulphate ammonium salt Emulsifier 2.0
7. Distilled water Solvent 1.0
8. Dipropylene glycol linear monomethyl ether (DPM) Solvent Q. S.

The manufacturing procedure of formulation of Example 5 is similar to the manufacturing process described in Example 4.

Example 6: Nitenpyram 7.5% + Pyriproxyfen 7.5% + Tolfenpyrad 10% WP
S. No. Composition Function Charge in (%)
1. Nitenpyram (Technical) Active ingredient 7.5
2. Pyriproxyfen (Technical) Active ingredient 7.5
3. Tolfenpyrad (Technical) Active ingredient 10.0
4. Butylated naphthalene sulphonic acid and dioctyl sulphosuccinate Wetting agent 4.0
5. Sodium salt of Naphthalene Sulphonates formaldehyde condensate Dispersing agent 3.0
6. Polydimethylsiloxane Defoamer 1.0
7. Precipitated Silica Anti caking agent 3.0
8. China clay Filler Q.S.

Procedure of preparation of Nitenpyram 7.5% + Pyriproxyfen 7.5% + Tolfenpyrad
10% WP
Step 1: Grinding tolfenpyrad technical and pyriproxyfen technical separately in air jet mill.
Check their particle size, if d90 value is <10µm then use it for further process. If it is >10µm further grind the material in air jet mill.
Step 2: According to the batch size, all raw materials were mixed in following order.
• Tolfenpyrad technical (grounded)
• Pyriproxyfen technical (grounded)
• Nitenpyram technical
• Anticaking agent
• Wetting agent
• Dispersing agent
• Defoamer
• Filler
Step 3: Pre-mixing the sample in a ribbon blender for 2 hrs.
Step 4: Submitting the sample for quality control for complete analysis, and
Step 5: Packing the material in suitable bottle.

Efficacy study for combination of Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % in Emulsifiable concentrate (EC) form:

SYNERGY STUDIES:
A synergistic effect exists whenever the action of an active ingredient combination is greater than the sum of the actions of the individual components.
After calculating % disease control, the synergism was calculated by the below formula: The synergistic pesticidal action of the inventive mixtures is calculated by Colby’s formula. Appropriate analysis of plant response to pesticide combination is critical in determining the type of activity observed. The most widely used model is the 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) ***
The synergistic action expected for a given combination of three active components can be calculated as follows:
(AB + AC + BC) ABC
Expected (E) = A + B + C - +
100 10000

Where:
“E” represents expected percentage of pesticidal control for the combination of the three active ingredients at defined doses (for example equal to A, B and C, respectively).
“A” is the percentage of pesticidal control observed by compound A at a defined dose.
“B” is the percentage of pesticidal control observed by the compound B at a defined dose.
“C” is the percentage of pesticidal control observed by the compound C at a defined dose.
The synergistic action expected for a given combination of two active components can be calculated as follows:
AB
Expected (E) = A + B -
100
Where:
“A” is Percentage of pesticidal control observed by compound A.
“B” is Percentage of pesticidal control observed by compound B.

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
Trial 1: Pests of Cotton:
Cotton (Gossypium hirsutum L.) is the most important cash crop in India with an expanse of 10-11 million hector area under cultivation.
Cotton grows well in almost all areas of the country but is mainly grown in nine states. Major cotton growing states includes Punjab, Haryana, Rajasthan in North India, Maharashtra, Gujarat and Madhya Pradesh in Central India, and Tamil Nadu, Karnataka, Andhra Pradesh and Telangana in South India.
The field efficacy trials were conducted in cotton on cotton sucking pest complex. The sucking pests viz., Aphid, (Aphis gossypii) (Glover), Thrip (Thrips tabaci) (Linnman), Whiteflies (Bemesia tabaci) Leafhopper/Jassids (Amrasca biguttula biguttula) (Ishida) and Mites (Tetranychus neocaledonicus) cause severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield.
The field trial was conducted to evaluate the efficacy of the individual, binary and ternary mixtures of Nitenpyram, Pyriproxyfen and Tolfenpyrad.
Trials were conducted with randomized block design with net plot size of 5m x 8m = 40 Sq mt. Cotton crops were raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liters of water spray volume per hectare at 60 days after sowing. The observations were recorded by counting the nod of sucking insects Jassids, Thrips, Aphids, Whiteflies and Mites) per leaf, six leaves per plant and five plants per plot. The observations were recorded before spraying, 5 DAA and 10 DAA (Days after application).

Table 1: Efficacy of Jassids, Thrips, Mites, White fly and Aphid pests’ control in Cotton
at 5 and 10 Days After Application (DAA):

Compositions
GAI/ha % Insect Control at 5 DAA % Insect Control at 10 DAA
Jassids Thrips Mites White
fly Aphids Jassids Thrips Mites White
fly Aphids
Nitenpyram 25 % SP 80 70.3 61.3 21.2 73.2 69.2 61.1 50.8 14.1 59.8 58.5
Pyriproxyfen 10 % EC 60 44.2 51.2 32.2 77.5 52.2 30.4 39.1 20.5 65.2 40.4
Tolfenpyrad 10 % EC 150 65.4 62.4 69.4 45.7 70.5 49.4 50.6 57.7 31.3 56.2
Nitenpyram 25 % SP + Pyriproxyfen 10 % EC 80 + 60 78.1 70.1 40.1 86.2 74.6 63.45 56.73 26.4 75.06 65.6
Pyriproxyfen 10 % EC + Tolfenpyrad 10 % EC 60 + 150 69.5 70.3 72.2 80.1 81.2 55.72 58.0 58.1 65.4 63.03
Nitenpyram 25 % SP + Tolfenpyrad 10 % EC 80 + 150 82.3 76.2 73.2 78.2 85.1 70.68 60.56 55.4 63.07 71.11
Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC 250 98.6 97.8 92.9 99.1 99.6 96.1 96.7 90.1 98.9 98.2

The trial results in Table 1 show excellent efficacy of Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC combination against sucking pest complex in Cotton. The solo application as well as the combination of two active ingredients tested here against jassids, thrips, mites, whiteflies, aphids were not able to provide satisfactory control of sucking pest complex. Whereas the combination of Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC has shown excellent efficacy as well as residual control on Cotton for all sucking pests.

Table 2: Evaluation of synergy of Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC against Jassids, Thrips, Mites, Whitefly, Aphid at 10 DAA on Cotton

Compositions
GAI/ha % Insect Control at 10 DAA
Jassids Thrips Mites Whitefly Aphid
Exp Obs. Exp Obs. Exp Obs. Exp Obs. Exp Obs.
Nitenpyram 25 % SP 80 61.1 50.8 14.1 59.8 58.5
Pyriproxyfen 10 % EC 60 30.4 39.1 20.5 65.2 40.4
Tolfenpyrad 10 % EC 150 49.4 50.6 57.7 31.3 56.2
Nitenpyram 25 % SP + Pyriproxyfen 10 % EC 80 + 60 72.93 63.45 70.04 56.73 31.71 26.4 86.01 75.06 75.27 65.6
Ratio of O/E 0.87 0.81 0.83 0.87 0.87
Pyriproxyfen 10 % EC + Tolfenpyrad 10 % EC 60 + 150 64.79 55.72 69.92 58.0 66.38 58.1 76.1 65.4 73.9 63.03
Ratio of O/E 0.86 0.83 0.88 0.86 0.85
Nitenpyram 25 % + Tolfenpyrad 10 % EC 80 + 150 80.32 70.68 75.7 60.56 63.67 55.4 72.39 63.07 81.83 71.11
Ratio of O/E 0.88 0.80 0.87 0.87 0.87
Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC 250 86.3 96.1 85.2 96.7 71.11 90.1 90.38 98.9 89.17 98.2
Ratio of O/E 1.12 1.13 1.27 1.09 1.10
*Exp- Expected & Obs.- Observed.
The trial results in table 2 show synergistic effect of Nitenpyram 7.5 % + Pyriproxyfen 7.5 % + Tolfenpyrad 10 % EC combination against Jassids, Thrips, Mites, Whitefly & Aphids on Cotton crop. The higher ratio of the observed and the expected efficacy clearly demonstrates the synergistic effect of the combination. ,CLAIMS:We Claim:
1. A synergistic insecticidal composition comprising (a) nitenpyram, (b) pyriproxyfen, and (c) tolfenpyrad and suitable agrochemical additives.

2. The synergistic insecticidal composition as claimed in claim 1, wherein the composition comprises (a) nitenpyram present in a range from 5% (w/w) to 15% (w/w), (b) pyriproxyfen present in a range from 5% (w/w) to 15% (w/w), (c) tolfenpyrad present in a range from 5% (w/w) to 25% (w/w), and suitable agrochemical additives.

3. The synergistic insecticidal composition as claimed in claims 1 and 2, wherein the composition is formulated as an emulsion concentrate (EC), a micro emulsion (ME), and a wettable powder (WP).

4. The synergistic insecticidal composition as claimed in claim 2, wherein the suitable agrochemical additives are selected from an emulsifier, a stabilizer, a solvent, a wetting agent, a dispersing agent, an anticaking agent, a defoamer, and a filler.

5. The synergistic insecticidal composition as claimed in claim 4, wherein the emulsifier is selected from the group comprising of linear or branched alkylbenzene sulfonates, alcohol ether sulfates, calcium salt of dodecyl benzene sulphonates (Ca-DDBS), non-ionic surfactant blend, ethoxylated and alkoxylated fatty acids, tristyryl phenol ethoxylate with 16 EO, ethoxylated amines, ethoxylated alcohol, alkyl and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylates, alkoxylated alcohol, Calcium alkyl aryl sulphonate, Polyaryl phenol ethoxylate sulphate ammonium salt and a combination thereof, present in an amount of 1 to 15% (w/w).

6. The synergistic insecticidal composition as claimed in claim 4, wherein the stabilizer is epoxidized soya bean oil (ESO), present in an amount of 1% to 2% (w/w).

7. The synergistic insecticidal composition as claimed in claim 4, wherein solvent is selected from the group comprising of solvent C9 (heavy aromatic solvent naphtha (petroleum)), dipropylene glycol linear monomethyl ether (DPM), and distilled water, present in Q. S.

8. The synergistic insecticidal composition as claimed in claim 4, wherein the wetting agent is selected from the group comprising of butylated naphthalene sulphonic acid and dioctyl sulphosuccinate, sodium alpha olefin sulphonates, and sodium di-isopropyl naphthalene sulphonates, present in an amount of 1% to 5% (w/w).

9. The synergistic insecticidal composition as claimed in claim 4, wherein the dispersing agent is selected from the group comprising of sodium salt of naphthalene sulphonates formaldehyde condensate, and modified styrene acrylic polymer, present in an amount of 1% to 5% (w/w).

10. The synergistic insecticidal composition as claimed in claim 4, wherein the anti-caking agent is silicon dioxide or precipitated silica, present in an amount of 1% to 5% (w/w), the defoamer is polydimethylsiloxane, present in an amount of 1% to 2% (w/w), and the filler is china clay, present in Q.S.