DESC:FIELD OF THE INVENTION

The present invention relates to a suspo-emulsion ( SE ) formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) for plant pest control. More particularly, the present invention relates to a suspo-emulsion insecticidal composition with enhanced action for plant pest control, the said insecticidal composition comprises two active chemical compounds i.e. (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C). The present invention also relates to a process for the preparation of the above said suspo-emulsion composition for plant pest control.

Formula (A) (chlorantraniliprole / CAS NO: 500008-45-7)

Formula (B) (Fenobucarb / CAS NO: 3766-81-2)

Formula (C) (Pyriproxyfen / CAS No:-95737-68-1)

BACKGROUND OF THE INVENTION

Insect pests are one of the worst enemies of crops. They cause severe damages to the crops resulting in reduced crop productivity. In heavily infested areas 80 to 90 percent crop damages has been reported. In agrarian countries like India it badly impacts the economy of the country. Controlling crop pest population has been a major issue and various traditional and advanced means are being used to minimize the damage caused by insect pests. Most frequently and widely used method to control insect pests is use of insecticides/pesticides. Continuous use of pesticides and insecticides years after years, in uncontrolled and unscientific manner has resulted in development of resistance in the insect pests and this resistance continues to broaden in spectrum against the number of insecticides/pesticides. Continuous high intensity use of insecticides and pesticides has given rise to some other critical issues like presence of high quantity of insecticide residues in agricultural products, increasing environmental pollution and damage to ecological balance and deteriorating health of consumers.

Therefore, there is a need for an insecticidal formulation that is highly efficient, has slightly toxic, covers a broader spectrum of insects and is environment friendly and economical.

The present invention relates to agrochemical compositions based on suspo-emulsion formulation; their use for application in crop protection flowable formulations for controlling agricultural pests, weeds or diseases and reducing the wash-off of active ingredients by rainfall. Biological efficacy of pesticides is influenced by many factors, particularly the residence time of the pesticide on the treated surface, which is often a plant leaf surface. For example, emulsified oil or water insoluble polymers prepared as emulsions have been used to improve liquid formulation.

A number of chemical agents have been used for controlling plant pest control. However, the problem that plant pest have acquired resistance to the chemical agents becomes remarkable due to frequent use or excessive application, etc., of the chemical agents having similar structures and same functions for controlling the same kinds of pest.

Pesticide compounds are often applied in the form of a dilute aqueous composition in order to achieve a good interaction with the target organism, such as plants, and insects. As most active compounds that are used as pesticides, in particular insecticide/pesticide active compounds, are only sparingly or even insoluble in water, in most of the cases, formulators are often confronted with difficulties in formulating pesticide compounds in stable formulations.

On the other hand, consumers' needs for agricultural chemical-reduced crops and social needs to reduce environmental loads due to agricultural chemicals have now increased. Also, in a farmer's field where the chemicals have been actually used, when two or more kinds of chemicals are used in admixture for the treatment by the tank mix method, there are many risks to lower the effect of the other chemical to be mixed with each other or possibilities to cause chemical damages against plant materials depending on a combination of chemicals where they are not well-suited to each other.

Applicant is desirous to provide suspo-emulsion of insecticidal composition comprising components (compounds) having different basic structures and different functions with well-suited to each other, and a method for controlling plant pest.

Applicant is desirous to provide insecticidal composition in suspo-emulsion form wherein insecticidal composition comprises Chlorantraniliprole of formula (A) as main active chemical compound which is further used in preparing suspo-emulsion combining it with the other chemical compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C).

Chlorantraniliprole of formula (A), also known as 5-bromo-N-[4-chloro-2-methyl-6-(methylcarbamoyl)phenyl]-2-(3-chloropyridin-2-yl)pyrazole-3-carboxamide,(CAS No: 500008-45-7) is a Anthranilic-diamide insecticide.

Chlorantraniliprole has slightly toxic to humans and mammals. Further, it is effective at low use rates. Chlorantraniliprole is commercially available, for example, as Coragen® (available from DuPont™, Coragen is a registered trademark of E. I. du Pont de Nemours and Company).It is board spectrum insecticide for the effective control of Stem borer& Leaf folder for rice, Diamond Back Moth for cabbage, American Boll warm, spotted bollworm & Tobacco caterpillar for Cotton, termite, early shoot borer & Top borer for Sugarcane, Fruit borer for Tomato & Chilli, Green semiloopers &stem fly Girdle Beetle for soyabean, Fruit and shoot borer For Brinjal, Gram pod borer & pod fly for pigeon pea, Pod borer for Bengal gram & Black gram, Fruit borer & caterpillars for Bitter gourd, Fruit borer for Okra, Spotted stem borer, pink stem borer for maize, Tobacco Caterpillar for Ground nut.

Fenobucarb of formula (B), also known as (2-Butan-2-ylphenyl) N-methylcarbamate(CAS No 3766-81-2), is a carbamate insecticide and a pale yellow or pale red liquid in colour having insoluble in water, Fenobucarb is used as an agricultural insecticide for the control of Brown Plant Hopper, Green Leaf hopper in rice and cotton.

Pyriproxyfen of formula (C),also known as 4-Phenoxyphenyl (R/S)-2-(2-pyridyloxy)propylether2-[1-(4-Phenoxyphenoxy)propan-2-yloxy]pyridine(CAS No:-95737-68-1),is a pyridine-based pesticide which is found to be effective against a variety of arthropod. It was introduced to the US in 1996, to protect cotton crops against whitefly and Chilli against Aphids and whitefly It has also been found useful for protecting other crops. It is also used as prevention for flea control on household pets, for killing indoor and outdoor ants and roaches. Pyriproxyfen is a juvenile hormone analog and an insect growth regulator that prevents flea eggs from hatching thus prevents larvae from developing into adulthood and thus rendering them unable to reproduce.

The conventional formulation of pesticides available in market of Chlorantraniliprole, Fenobucarb and Pyriproxyfen, the pesticide formulation are often prepared by use of toxic organic solvents xylene and other, more conventional single product formulations disadvantages. A conventional suspo-emulsion when stored under severe environment conditions at high temperature or low temperature, oil droplets and particles (dispersoids) dispersed in water may sometimes cause a change such as particle growth, separation of an aqueous layer and formation of a hard cake due to aggregation and precipitation of dispersoids, or a change in appearance such as creaming of the formulation, and thus the conventional suspo-emulsion was not necessarily sufficient in storage stability.

The present invention, of stable and synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) and suspo-emulsion formulation has not been reported in any prior art .

SUMMARY OF INVENTION

The present invention is related to a combination insecticidal formulation in a suspo emulsion (SE) form. Insecticidal formulation of this invention is stable, less hazardous, safe to handle, environmentally safe and cost effective. The pesticides used in this formulation act synergistically to cover broader spectrum of pests of crops.

Accordingly, the main object of the present invention is to provide a suspo-emulsion (SE ) formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) for plant pest control.

It is an object of the present invention suspo-emulsion (SE ) formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) in amount of 1% to 10 % (w/w) ( preferably 5 % to 6 %) and (ii) at least one compound selected from Fenobucarb of formula (B) in a amount between 35% to 45 % (w/w) ( preferably 38 % to 42 %)or Pyriproxyfen of formula (C)in a amount between 1% to 10 % (w/w) ( preferably 5 % to 6 %).

It is an object of the present invention to provide a process for the preparation of the suspo-emulsion combination formulation of the present insecticide, comprising the step of:
Preparation suspension concentrate (SC) comprises:-
a) An aqueous dispersion of chlorantraniliprole in amount of 1% to 10 % (w/w), mixture of chlorantraniliprole with of anti-freezing agent ,antifoaming agent and emulsifiers in water ;
b) Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron.
Preparation of Oil-in Water emulsion (EW) comprises:-
a) an emulsion dispersion (Oil-in Water emulsion, EW) of at least one compound selected from Fenobucarb in a range between 35% to 45 % (w/w) or Pyriproxyfen in a amount between 1% to 10 % (w/w) with solvent aromatic hydrocarbon and emulsifiers in water;
Preparation of suspo-emulsion (SE) :-
a) Mixing of (Oil-in Water emulsion, EW) formulation into (suspension concentrate, SC) formulation to prepared suspo-emulsion (SE) Formulation.
b) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers or dispersing agents.
c) Finally adding the viscosity agent & preservative to the suspo-emulsion (SE) to enhance viscosity

In above objective suspo-emulsion formulation according to the invention may additionally comprise: e) penetration promoters, wetting agents, spreading agents and/or retention agents.

It is an object of the present invention to provide improved a suspo-emulsion formulation, of synergistic insecticidal composition is which stable and ready to use, and has superior properties compared to prior art formulations or mixtures or compositions.

It is further an object of the present invention to provide a suspo-emulsion composition that will protect crop from pest.

Yet it is an object of the present invention to provide a suspo-emulsion composition for plant pest control wherein the said composition comprises two active chemical compounds (i) Chlorantraniliprole of formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C).

It is also an object of the present invention to provide a synergistic suspo-emulsion composition for plant pest control, the said composition mainly comprises: (i) Chlorantraniliprole of formula (A) and (ii) Fenobucarb of formula (B).

It is also an object of the present invention to provide a synergistic suspo-emulsion composition for plant pest control, the said composition mainly comprises: (i) Chlorantraniliprole of formula (A) and (ii) Pyriproxyfen of formula (C).

Another object of the present invention is to provide a process for the preparation of suspo-emulsion composition for plant pest control.

The further object of the present invention is to provide highly storage-stable suspo-emulsion formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C), which show excellent storage stability and biological efficacy for use in plant pest control.

It is also an object to provide a method of application of composition to the plants to control the plant pest.

DETAILED DESCRIPTION OF THE INVENTION:

In describing the embodiments of the invention, specific terminology is resorted for the sake of clarity. However, it is not intended that the invention be limited to the specific terms so selected and it is to be understood that each specific term includes all technical equivalents that operate in a similar manner to accomplish a similar purpose.

As used herein, the term "synergistic effect" or grammatical variations thereof means and includes a cooperative action encountered in a combination of two or more active compounds in which the combined activity of the two or more active compounds exceeds the sum of the activity of each active compound alone.

The term "synergistically effective amount," as used herein, means and includes an amount of two or more active compounds that provide a synergistic effect defined above.

The term "pesticidally effective amount," as used herein, means and includes an amount of active pesticide that causes an adverse effect to the at least one pest, wherein the adverse effect may include deviations from natural development, killing, regulation, or the like.

As used herein, the term "control" or grammatical variations thereof means and includes regulating the number of living pests or regulating the number of viable eggs of the pests or both.

A suspo-emulsion formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) wherein oil droplets of a liquid pesticidal ingredient and particles of a solid pesticidal ingredient are dispersed together in water, and these ingredients are stably dispersed together in water.

The present inventors have studied in view of these circumstances and found that a suspo-emulsion containing a Propylene Glycol ( Anti freezing agent),modified naphthalene sulphonic acid condensate sodium salt, Acrylate copolymer, Poly-alkoxylated butyl ether, is a formulation having excellent storage stability, which suppresses the particle growth of dispersoids, namely, oil droplets of a liquid pesticidal ingredient and particles of a solid pesticidal ingredient, and also cause neither aggregation nor separation of dispersoids, nor formation of a hard cake, nor a change in appearance, during storage at high temperature and low temperature. Thus, the present invention has been completed. Namely, the present invention will be shown.
The active and inert ingredients in formulation of present invention are dispersed in aqueous solution, preferably water, to compose a stable and safe insecticide suspension.

The inert ingredients include wetting agents and dispersing agents, anti-freezing agents, anti-foaming agents.

In one particular embodiment, a of the present invention is to provide a suspo-emulsion formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) for plant pest control.

The present invention contains two active chemical compounds that mutually complement each other when used together and exhibit synergistic plant pest control capabilities that is greater than the individual compound’s capability to control the plant pest when used alone.

The present innovators have comprehensively and successfully investigated the possibility of developing a synergistic suspo-emulsion composition comprising: (i) Chlorantraniliprole of formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C).

According to the first embodiment of the present invention, there is provided a suspo-emulsion composition for plant pest control wherein composition may comprise two active chemical compounds i.e. (i)Chlorantraniliprole of formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C).

According to another embodiment of the present invention a suspo-emulsion formulation compositions comprising
Preparation suspension concentrate (SC) comprises:-
a) An aqueous dispersion (suspension concentrate, SC) of chlorantraniliprole in amount of 1% to 10 % (w/w), mixture of chlorantraniliprole with of anti-freezing agent ,antifoaming agent and emulsifiers in water ;
b) Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron.
Preparation of Oil-in Water emulsion (EW) comprises:-
a) an emulsion dispersion (Oil-in Water emulsion, EW) of at least one compound selected from Fenobucarb in an amount between 35% to 45 % (w/w) or Pyriproxyfen in an amount between 1% to 10 % (w/w) with solvent aromatic hydrocarbon and emulsifiers in water;
Preparation of suspo-emulsion (SE) :-
a) Mixing of (Oil-in Water emulsion, EW) formulation into (suspension concentrate, SC) formulation to prepared suspo-emulsion (SE) Formulation.
b) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers or dispersing agents.
c) Finally adding the viscosity agent & preservative to the suspo-emulsion (SE) to enhance viscosity

In an embodiment, suspo-emulsion formulation according to the invention may additionally comprise: e) penetration promoters, wetting agents, spreading agents and/or retention agents.

The composition of the present invention also contains auxiliaries tobe used in stage-(i) and stage-(ii) in the process for preparing suspo-emulsion composition. In order to prepare stable, ready to use suspo-emulsion compositions, Auxiliaries may be selected from but not limited to emulsifiers or dispersing agent, antifreeze agents, antifoaming agents, viscosity agents, fillers, stabilizers.

For the purpose of suspo-emulsion composition, organic solvent and auxiliaries may be selected from the list provided in the following paragraphs:

At least one organic solvent is selected from water, aromatic hydrocarbongroup, ethylacetate, ethyleneglycol, glycerine,heptane, hexamethylphosphoramide (HMPA), Hexamethylphosphoroustriamide(HMPT), methanol, methyl t-butyl ether (MTBE), Toluene, Ortho-xylene, Meta-xylene, Para-xylene, Mix-xylene, Acetone, and Acetonitrile .

At least one emulsifiers agent is selected from a group comprising modified naphthalene sulphonic acid condensate sodium salt, Acrylate copolymer, poly-alkoxylated butyl ether, phenyl naphthalene sulphonates, ethoxylated alkyl phenols, ethoxylated fatty acids, alkoxylated linear alcohols, glyceryl esters, maleic anhydride co-polymers, condensation product of aryl sulphonic acids, addition product of ethylene oxide and fatty acid esters, lignin derivatives, naphthalene formaldehyde condensates, sodium salts of iso-decylsulfosuccinic acid half ester, Blend of modified poly ethanoxy ether and sulphated anionic surfactant, blend of alcohol alkoxylates & methyl methacrylate polymer, blend of di alkyl ate naphthalene sulphonic acid sodium salt, sodium alkyl benesulfonates, sodium salts of sulfonates naphthalene, ammonium salts of Sulfonated naphthalene, salts of poly acrylic acids, salts of phenol Sulfonic acid and salts of naphthalene Sulfonic acids.

At least one anti-freezing agent selected from a group comprising anti-freezing agent selected from a group comprising of propylene glycol, diethylene glycol, Mono ethylene glycol, poly ol, polyvinyl alcohols and polyethylene glycols, 1,2- Propylene glycol, mono propylene glycol, 1,2-propanediot.

Anti freeze agents such as Propylene glycol ( polyols ) are added in an amount ranging from 0.1- 8 % w/w based on the weight of the insecticidal combination to avoid the freezing of the liquid insecticide upon application so as to enhance the duration of activity of the said insecticidal composition on the pests.

At least one anti foaming agent selected from a group comprising is silicon based emulsion, silicon Defoamer, Dimethyl polysiloxane or alcohol based antifoam agent.
Antifoam, preferably silicon or alcohol based, is added in an amount ranging from 0.1-5% w/w based on the weight of the insecticidal suspension. Anti foam agents are significant when the ingredients in the suspension are mixed or ground so as to avoid the occurrence of froth during particle size reduction of the ingredients.

The viscosity enhancing agents is selected from a group comprising, xanthan gum, gelatin, poly vinyl pyrrolidone, polyvinyl alcohol, sodium methyl cellulose, Poly vinyl pyrrolidone (PVP K-30), silicon oil compound and guar gum.

Though there are list of fillers known in the art, used in the suspo-emulsion composition, Inventors of the present invention has used mainly water (Demineralized water/DM Water) as filler for suspo-emulsion composition.

Viscosity modifier agent may be added for adjusting viscosity of the suspo-emulsion composition for example but limited to Xanthan gum. The other examples of viscosity agent/modifier is a group comprising Xanthan gum, gelatin, poly vinyl pyrrolidone, polyvinyl alcohol, sodium methyl cellulose, Poly vinyl pyrrolidone (PVP K-30), silicon oil compound and guar gum.

Anti foaming is silicon based emulsion, silicon Defoamer, Dimethyl polysiloxane or alcohol based antifoam agent.
The formulation thus prepared with varying amounts of wetting agents, dispersing agents were subjected to stability study and the optimum dose of the ingredients was selected. Formulation selected after various permutations and combination of ingredients was found to be stable and the best stable formulation was checked for parameters of description, suspensibility, dispersibility, pourability, viscosity, pH, under conditions of ambient temperature, heat stability and cold conditions at 10°C.

In general, Synergistic suspo-emulsion insecticidal composition comprising (i) Chlorantraniliprole of formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) may be provided as follows:

Table : 1

Name of Content in Composition Range of component (%)
Chlorantraniliprole 1-10%
Fenobucarb or Pyriproxyfen 1-45%
Anti-freezing agent 0.1-8%
Solvent(s) 5-35 %
Polymerization inhibitor 0.1-5%
Emulsifier 0.1-8%
Filler 30-80%
(Quantity sufficient )
Antifoaming 0.1-5%
Stabilizer 0.1-5%
Viscosity modifier agent 0.1-8%

Accordingly, synergistic composition comprising (i) Chlorantraniliprole of formula (A) and (ii) Fenobucarb of formula (B) may be provided as follows:

Table : 2

Name of Content in Composition Range of component (%)
Chlorantraniliprole 1-10%
Fenobucarb 35-45%
Anti-freezing agent 0.1-8%
Solvent(s) 5-35%
Polymerization inhibitor 0.1-5%
Emulsifier 0.1-8%
Filler 30-80%
(Quantity sufficient )
Antifoaming 0.1-5%
Stabilizer 0.1-5%
Viscosity modifier agent 0.1-8%

In a similar manner, synergistic composition comprising (i) Chlorantraniliprole of formula (A) and (ii) Pyriproxyfen of formula (C) may be provided as follows:

Table : 3

Name of Content in Composition Range of component (%)
Chlorantraniliprole 1-10%
Pyriproxyfen 1-10%
Anti-freezing agent 0.1-8%
Solvent(s) 5-35%
Polymerization inhibitor 0.1-5%
Emulsifier 0.1-8%
Filler 30-80 %
(Quantity sufficient )
Antifoaming 0.1-5%
Stabilizer 0.1-5%
Viscosity modifier agent 0.1-8%

An aqueous suspo-emulsion composition is a mixture of water-insoluble active ingredients dispersed in an aqueous solution, where one (or more) of the active ingredients is in suspension form and one (or more) of the active ingredients is in emulsion form. The formulation is intended for dilution into water prior to spray application. Mixtures of active ingredients are often used to provide a broader spectrum of pest control. Formulating the active ingredients together eliminates the need for tank mixing (which can lead to incompatibilities). Like other aqueous liquid formulations, suspo-emulsions are easy to handle and measure, dust free, non-flammable and offer good miscibility with water.

According to second embodiment of the present invention, there is also a process provided for the preparation of suspo-emulsion composition for controlling plant pest.

The selection of insecticide, quantity of each content of additives/auxiliaries, particle size of insecticide compounds in the said suspo-emulsion composition plays an important role in treating plant pest control.

Detailed embodiment on Best mode of experiment, Suspo-emulsion insecticidal composition, selection of particle size of one or more contents of the composition and process for preparing the said insecticidal composition and other supporting information along with results if any, may be described in detail at the time of filing complete application.

ADVANTAGES OF THE PRESENT INVENTION

The Suspo-emulsion insecticidal compositions of the present invention may show a broad spectrum activity against various insect-pest (for example, bollworms, Whitefly, aphids, Jassids, thrips, mite, stem borer, leaf folder, termite, early & top shoot borer, diamond back moth, Green Semiloopers, Stem fly, Girdle beetle, pod borer and fruit & shoot borer and various Lepidoptera &Coleopteran etc.) including insects resistant to chemicals, and shows excellent controlling effects (synergistic controlling effects) which could never be expected from a single component alone.

? Also, it shows high plant insects controlling effects against existing insects resistant to chemicals, and no chemical damage against plants can be admitted.
? It also shows activity against Brown plant hopper, green leaf hopper, stem borer, leaf folder, early & top shoot borer, termite, bollworms, Whitefly, aphids, Jassids, fruit &shoot borer, diamond back moth, Green Semiloopers, Stem fly, Girdle beetle, tobacco caterpiller, fruit borer and various Lepidoptera& sucking insects.
? The said suspo-emulsion insectidal composition may be useful but not limited onto the plants such as paddy, sugarcane, cotton, cabbage, cauliflower, tobacco, tomatoes, chilli, brinjal, okra, potatoes, leafy vegetables, oil crops, soybean, flowering ornamentals vine crops and fruit trees.

Example 1:Preparation of chlorantraniliprole (~5 %) + Fenobucarb (~ 40 %)
suspo-emulsion (SE) formulation:

Table : 4

S. No Raw Material Name Inputs Qty (gm.)
1 Chlorantraniliprole Technical ( Purity 95.7 % w/w ) 13.607 gm.
2 Fenobucarb technical ( purity 98 % w/w) 105.78 gm
3 Propylene Glycol ( P.G ) Anti freezing agent 12.5 gm.
4 FLK ( Unitop ) ( Preservative ) 3.25 gm.
5 Anti-foaming agent 0.25 gm.
6 modified naphthalene sulphonic acid condensate sodium salt (emulsifier ) 5 gm.
7 Acrylate copolymer(emulsifier ) 15gm (5 + 10)
8 Water (D M Water) ( Quantity sufficient ) (Filler) 78.75 gm.
9 Formaldehyde ( 40 % in water ) 1 gm.
10 Gum( xanthan gum ,1 % solution in water ) 2.5 gm
11 Solvent C-9 12.5 gm
12 Poly-alkoxylated butyl ether(emulsifier ) 1.25 gm
Total Qty 251.387 gm

Preparation of part-A : Process of Preparation of chlorantraniliprole (~5% w/w)
Suspension concentrate (SC) formulation:-

The chlorantraniliprole Technical (Qty 13.6 gm) was added reactor containing in water ( Qty 63.75 gm ),FLK (Unitop) (Qty :3.25 g,)propylene glycol (P.G.) (Qty 12.5 gm) with modified naphthalene sulphonic acid condensate sodium salt (Qty 5 gm) and Acrylate copolymer (Qty 5 gm) with stirring for 10-15minutes at room temperature (Temperature 30 ±5 OC). Further Anti-foaming agent (Qty 0.25 gm) was charged into reaction vessel with continue stirring for 50-55 minutes at room temperature (Temperature 30 ±5°C).

The above mixture was wet grinded in bead mill at temperature 15-16°C, (this process for minimized /reduce particle size of part –A mixture below ~25 micron. After wet grinding particle size was determined by sieve test (99 % min material pass through 25 micron sieve test).

Preparation of part-B: Preparation of Fenobucarb (~40 % w/w) (oil-in-water emulsion) (EW) formulation:-

Fenobucarb technical (Purity 98 %) (Qty 105.78 gm) was charged into reaction vessel with solvent C-9 (Qty 12.5 gm).The Acrylate copolymer (Qty 10 gm) and Poly-alkoxylated butyl ether (Qty 1.25 gm) was charged into reaction vessel with continue stirring for 10 -15 minutes at room temperature (Temperature 30 ±5 OC). Finally water (Qty 15 gm) water was charged into reaction vessel and stirring for 10 -15 minutes at room temperature (Temperature 30 ±5 OC), stirring for another 50 minutes for all material will homogenized.

Preparation of part-C:(Mixing of part-B into part-A): Process of chlorantraniliprole (~5 %) + Fenobucarb (~ 40 %) suspo-emulsion (SE) formulation: -

(Mixing of Fenobucarb (~40 % w/w) (oil-in-water emulsion) (EW) formulation into chlorantraniliprole (~5% w/w) Suspension concentrate (SC) formulation):-

Mixing of Part –B into Part –A with continuously high speed stirring was done at room temperature. The gum solution (xanthan gum 1 % solution in water) (Qty ~ 2.5 gm) was added to maintain viscosity between 50 to 55 sec. Once viscosity is adjust then formaldehyde 40 % solution in water (Qty 1 gm) was added as a preservative. Further chlorantraniliprole (~5 %) + Fenobucarb (~ 40 %) suspo-emulsion (SE) formulation of off white colored viscous liquid was obtained, having suspensibility of chorantraniliprole&fenubucarb~92 %and Viscosity = 410 cps and Particle size (By Malvern master sizer ):- D(50 ) = 1.843 µm, D(90 ) = 3.733 µm, pH=6.02

Example 2: Stability data of formulation of chlorantraniliprole (~5 %) + Fenobucarb (~ 40 %) suspo-emulsion(SE) formulation (Example 1)

The stability data of formulation of chlorantraniliprole (~5 %) + Fenobucarb (~ 40 %) suspo-emulsion (SE) formulation prepared in Example 1

Table :5 STORAGE STABILITY DATA

Parameter Specification
(In House) Initial Heat Stability study at 54± 2OC for 14 Days Cold Storage stability study at 0 ± 2OC for 14 Days

Description White to off white colored viscous liquid. Complies Complies Complies
Chlorantraniliprole ( A.I. Content ) 4.5 to 6 % w/w
(by HPLC ) Complies Complies Complies
Chlorantraniliprole ( Suspensibility ) Min 80 %
(by HPLC ) Complies Complies
Complies
Fenobucarb
( A.I. Content ) 38 to 42 % w/w (by HPLC ) Complies Complies Complies
Fenobucarb
(Suspensibility) Min 80 % Complies Complies Complies
pH. 5-9 Complies Complies Complies
Viscosity ( cps ) 375 to 600 cps Complies Complies Complies

The results were found satisfactory and this formulation is passing in all physicochemical properties.

Example 3: Preparation of chlorantraniliprole (~5 %) + Pyriproxyfen (~ 5 %) suspo-emulsion (SE) formulation

Table : 6

S. No Raw Material Name Inputs Qty (gm.)
1 Chlorantraniliprole Technical ( Purity 95.7 % w/w ) 16.3 gm.
2 Pyriproxyfen technical ( purity 98 % w/w) 16.4 gm
3 Propylene Glycol ( P.G ) ( Anti freezing agent ) 5 gm.
4 FLK ( Unitop )( Preservative ) 3.75 gm.
5 Anti-foaming agent 0.25 gm.
6 modified naphthalene sulphonic acid condensate sodium salt (emulsifier ) 6 gm.
7 Acrylate copolymer(emulsifier ) 18 gm (12+ 6 )
8 Water (D M Water) ( Q.S ) (Filler) 195.6 gm
9 Formaldehyde ( 40 % in water ) 1 gm.
10 Gum( xanthan gum ,1 % solution in water ) 2.5 gm.
11 Solvent C-9 15 gm.
13 Poly-alkoxylated butyl ether(emulsifier ) 1.5 gm
Total Qty 281.2 gm

Preparation of part-A :Preparation of chlorantraniliprole (~5% w/w) Suspension concentrate (SC) formulation:-

The chlorantraniliprole Technical (Qty 16.3 gm.) was added reactor containing in propylene glycol (P.G.) (Qty 5 gm) in water (Qty120.6gm) with modified naphthalene sulphonic acid condensate sodium (Qty 6gm) FLK (Unitop) (Qty :3.75 gm,) and Acrylate copolymer (Qty 6gm) with stirring for 10-15minutes at room temperature (Temperature 30 ±5 OC). Further Anti-foaming agent (Qty 0.3gm) was charged into reaction vessel with continue stirring for 50-55 minutes at room temperature (Temperature 30 ±5°C).

The above mixture was wet grinded in bead mill at temperature 15-16°C, (this process for minimized /reduce particle size of part –A mixture below ~25 micron. After wet grinding particle size was determined by sieve test (99 % min material pass through 25 micron sieve test).

Preparation of part-B :Preparation of Pyriproxyfen (~5 % w/w) (oil-in-water emulsion) (EW) formulation:-

Pyriproxyfen technical (Purity 98 %) (Qty 16.4 gm) was charged into reaction vessel with Solvent C-9 (Qty15 gm). The Acrylate copolymer (Qty 12gm) and Poly-alkoxylated butyl ether (Qty 1.5 gm) was charged into reaction vessel with continue stirring for 10 -15 minutes at room temperature (Temperature 30 ±5 OC). Finally water (Qty 75gm) was charged into reaction vessel and stirring for 10 -15 minutes at room temperature (Temperature 30 ±5 OC), stirring for another 50 minutes for all material will homogenized.

Preparation of part-C: (Mixing of part-B into part-A) Process of chlorantraniliprole (~5 %) + Pyriproxyfen (~ 5 %) suspo-emulsion (SE) formulation: -

(Mixing of Pyriproxyfen (~5 % w/w) (oil-in-water emulsion) (EW) formulation into chlorantraniliprole (~5% w/w) Suspension concentrate (SC) formulation):-

Mixing of Part –B into Part –A with continuously high speed stirring was done at room temperature. The gum solution (xanthan gum 1 % solution in water) (Qty ~ 2.5 gm) was added to maintain viscosity between 50 to 55 sec. Once viscosity is adjust then formaldehyde 40 % solution in water (Qty 1 gm) was added as a preservative. Further chlorantraniliprole (~5 %) + Pyriproxyfen (~5 %)suspo-emulsion (SE) formulation of off white colored viscous liquid was obtained, having Chlorantraniliprole suspensibility of about 92.31%,Pyriproxyfen suspensibility of about 91.59%and Viscosity = 450 cps and Particle size (By Malvern master sizer ):- D(50 ) = 1.976 µm, D(90 ) = 4.990 µm, pH=6.5

Example 3: The stability data of formulation of chlorantraniliprole (~5 %) + Pyriproxyfen (~ 5 %) suspo-emulsion (SE) formulation

Table 7: STORAGE STABILITY DATA:-

Parameter Specification
(In House) Initial Heat Stability study at 54± 2OC for 14 Days Cold Storage stability study at 0 ± 2OC for 14 Days

Description White to off white coloured viscous liquid. Complies Complies Complies
Chlorantraniliprole ( A.I. Content ) 5 to 6 % w/w
( by HPLC ) Complies Complies Complies
Chlorantraniliprole ( Suspensibility ) Min 80 %
( by HPLC ) Complies Complies Complies
Pyriproxyfen
( A.I. Content ) 5 to 6% w/w
( by HPLC ) Complies Complies Complies
Pyriproxyfen
( Suspensibility ) Min 80 % Complies Complies Complies
pH. 5-9 Complies Complies Complies
Viscosity ( cps ) 375 to 600 cps Complies Complies Complies

The results were found satisfactory and this formulation is passing in all physicochemical properties.

Bio field trial:

Evaluation of bio-efficacy and Phytotoxicity of Chlorantraniliprole 5% + Pyriproxyfen 5% SE on Brinjal, chilli, okra for the control of pests like white fly, aphids, fruit borer & shoot borer.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE (Code:- C+P-01)

Objective:
(i) To determine the bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against White fly, Aphids, Fruit borer & shoot borer of brinjal, chilli & okra crop.

(ii) To determine Phytotoxicity of Chlorantraniliprole 5% + Pyriproxyfen 5% SE on brinjal, chilli & okra crop.

Table : 8

Details of Experiment
a) Test chemical Chlorantraniliprole 5% + Pyriproxyfen 5% SE
b) Crop Brinjal, Chilli, Okra
c) Location Bhilapur, Vadodara, Gujarat
d) Target pests White fly, Aphids, Fruit borer, Shoot borer
e) Plot size 3.0 m × 3.0 m
f) Design RBD (Randomized Block Design)
g) Treatment 7(Seven); Table 1
h) Number of reapplication 03
i) Application method Spray by knapsack sprayer fitted with flat fan nozzle (5 liter)
j) Water volume used 500 liters/ha

Table :9: Treatment details for bio-efficacy of different insecticide:

SR. No. Treatment Dosage Formulation
(A.I. gm/ha)
1. Chlorantraniliprole 5% + Pyriproxyfen 5% SE (1 ml) 25+25= 50
2. Chlorantraniliprole 5% + Pyriproxyfen 5% SE (0.8 ml) 20+20=40
3. Chlorantraniliprole 5% + Pyriproxyfen 5% SE (0.6 ml) 15+15=30
4. Chlorantraniliprole 5% + Pyriproxyfen 5% SE (1.2 ml) 30+30=60
5. Chlorantraniliprole 18.5% SC 30
6. Pyriproxyfen 10% EC 50
7. Untreated control (water only) -

Example 4: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Brinjal whitefly.
Table : 10

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of whitefly/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day 3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1ml/L) 25 + 25 23 16.10 5.75 4.60 3.45 3.91 83%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.8ml/L) 20 + 20 20 15.40 6.40 4.80 3.60 5.20 74%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.6ml/L) 15 + 15 21 17.85 8.61 6.72 6.30 8.40 60%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1.2ml/L) 30 + 30 25 12.50 5.50 2.75 1.50 3.25 86%
Chlorantraniliprole 18.5% SC 30 24 22.8 23.04 22.56 22.80 22.80 5%
Pyriproxyfen 10%EC 50 23 17.25 7.59 5.98 5.06 5.52 76%
Untreated control - 22 20.68 19.14 17.82 17.38 18.48 16%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited whitefly pest control 85, 94 per cent after 7 days and 83, 86 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of whitefly after 7 and 15 days of spray.

Example 5: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Brinjal Aphids.

Table : 11

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Aphids/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1ml/L) 25 + 25 27 14.04 6.21 2.97 2.43 3.24 88%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.8ml/L) 20 + 20 29 17.11 8.12 4.06 3.48 4.64 84%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.6ml/L) 15 + 15 30 21.60 14.40 9.6 8.70 10.80 64%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1.2ml/L) 30 + 30 29 12.18 4.64 2.03 1.16 2.61 91%
Chlorantraniliprole 18.5% SC 30 28 25.76 27.90 26.32 26.04 26.60 5%
Pyriproxyfen 10%EC 50 27 18.36 9.72 7.56 4.32 5.13 81%
Untreated control - 29 25.52 22.91 20.88 20.01 21.46 26%

Results :

? Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Aphids pest control 91, 96 per cent after 7 days and 88, 91 per cent after 10 days of spray.
? Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Aphids after 7 and 15 days of spray.

Example 6: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Brinjal Fruit borer.
Table : 12

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Fruit borer/plant (5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1ml/L) 25 + 25 7 5.25 4.06 2.94 2.03 2.52 64%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.8ml/L) 20 + 20 9 7.29 5.76 4.86 3.51 3.78 58%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=0.6ml/L) 15 + 15 7 6.09 5.04 4.69 3.64 4.13 41%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 8 5.52 3.52 2.48 1.28 1.76 78%
Chlorantraniliprole 18.5% SC 30 9 7.20 5.76 5.76 3.24 3.69 59%
Pyriproxyfen 10% EC 50 8 7.12 6.48 6.00 5.92 6.08 16%
Untreated control - 7 6.37 6.23 5.74 5.67 5.88 16%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Fruit borer pest control 71, 84 per cent after 7 days and 64, 78 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Fruit borer after 7 and 15 days of spray.

Example 7: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Brinjal Shoot borer.

Table : 13

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Shoot borer/plant (5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE (F=1ml/L) 25 + 25 12 8.64 5.88 3.12 1.68 2.28 81%
Chlorantraniliprole 5%+ Pyriproxyfen 5%SE (F=0.8ml/L) 20 + 20 11 8.58 6.16 4.62 3.41 3.96 64%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 13 10.79 8.71 7.93 5.59 7.02 46%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 11 7.04 3.96 1.98 0.88 1.21 89%
Chlorantraniliprole 18.5% SC 30 12 9.12 6.24 4.92 9.90 10.50 65%
Pyriproxyfen 10% EC 50 11 10.34 9.57 9.24 9.13 5.04 16%
Untreated control - 13 12.48 11.57 11.18 10.92 11.44 12%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Shoot borer pest control 86, 92 per cent after 7 days and 81, 89 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Shoot borer after 7 and 15 days of spray.

REPORT OF PHYTO-TOXICITTY EVALUATION ON BRINJAL CROP
Evaluation of phyto-toxicity effect of suspo-emulsion formulation of insecticidal composition of Chlorantraniliprole 5% and Pyriproxyfen 5% on 50,40,30 & 60 gm/ha on brinjal crop.

TABLE-14 :Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein clearing, Wilting before and after spraying of CLSL sample C+P-01 on Brinjal crop:

Treatment DAS of observation
Before spray 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3
T1 0 0 0 1 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 1 1 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

*DAS= Days After spray
C+P-01=Chlorantraniliprole 5% + Pyriproxyfen 5% SE
Treatment:
T1= C+P-01 (25+25) F=1ml/L
T2= C+P-01 (20+20) F=0.8ml/L
T3= C+P-01 (15+15) F=0.6ml/L
T4= C+P-01 (30+30) F=1.2ml/L
T5 =Untreated control (Water only)

Conclusion:

Results of phyto-toxicity evaluation trial are given in table 14. As per results we are concluded that different doses of Chlorantraniliprole 5% + Pyriproxyfen 5% SE were cause Negligible phytotoxic symptoms on brinjal plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5% + Pyriproxyfen 5% SE is safe to use on brinjal at the dosage from 50, 40, 30 & 60 gm/ha.

The present invention relates to a suspo-emulsion formulation of synergistic insecticidal composition comprising (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C) for plant pest control. More particularly, the present invention relates to a suspo-emulsion insecticidal composition with enhanced action for plant pest control, the said insecticidal composition comprises two active chemical compounds i.e. (i) chlorantraniliprole of Formula (A) and (ii) at least one compound selected from Fenobucarb of formula (B) or Pyriproxyfen of formula (C). The present invention also relates to a process for the preparation of the above said suspo-emulsion composition for plant pest control.

Example 8:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Chilli whitefly.
Table : 15

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of whitefly/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day 3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 18 11.70 8.28 4.68 2.16 2.70 85%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 20 14.60 10.80 8.40 4.40 5.00 75%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 19 15.01 11.78 10.64 8.17 9.31 51%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 20 11.60 6.80 3.80 1.60 2.00 90%
Chlorantraniliprole 18.5% SC 30 19 15.96 15.01 14.06 13.87 14.25 24%
Pyriproxyfen 10% EC 50 18 12.78 9.18 6.48 6.48 3.94 78%
Untreated control - 18 15.66 14.58 14.04 13.68 14.22 21%

Results :
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited whitefly pest control 88, 92 per cent after 7 days and 85, 90 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of whitefly after 7 and 15 days of spray.

Example 9:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Chilli Aphids.

Table : 16

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Aphids/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 22 14.96 10.56 7.04 3.30 3.96 82%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 21 15.12 12.81 9.03 5.46 6.72 68%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 19 14.82 13.68 10.83 7.98 8.93 53%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 22 11.88 9.24 3.52 1.54 2.42 89%
Chlorantraniliprole 18.5% SC 30 21 18.69 18.27 17.85 17.22 17.43 17%
Pyriproxyfen 10% EC 50 19 13.49 10.83 6.84 4.56 5.51 71%
Untreated control - 20 18.20 17.80 17.20 16.60 17.40 13%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Aphids pest control 85, 93 per cent after 7 days and 82, 89 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Aphids after 7 and 15 days of spray.

Example 10:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Chilli Fruit borer.
Table : 17

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Fruit borer/plant (5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 17 10.20 6.29 3.06 1.36 2.04 88%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 18 11.70 7.56 4.68 2.52 3.42 81%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 16 11.68 9.44 7.68 6.72 7.20 55%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 18 8.10 5.04 2.16 0.72 1.26 93%
Chlorantraniliprole 18.5% SC 30 16 11.04 7.84 5.28 4.16 4.80 70%
Pyriproxyfen 10% EC 50 18 16.38 15.66 14.76 14.58 14.94 17%
Untreated control - 17 15.81 14.96 14.79 14.28 14.45 15%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Fruit borer pest control 92, 96 per cent after 7 days and 88, 93 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Fruit borer after 7 and 15 days of spray.

Example 11:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Chilli Shoot borer.
Table : 18

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Shoot borer/plant (5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 17 12.75 9.01 6.46 3.74 4.42 74%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 15 11.85 9.30 6.60 4.35 4.80 68%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 16 12.96 11.68 9.12 7.04 7.68 52%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 15 10.20 6.90 3.45 2.10 2.70 82%
Chlorantraniliprole 18.5% SC 30 17 13.60 11.39 7.82 5.27 6.12 64%
Pyriproxyfen 10% EC 50 16 14.40 14.08 13.60 12.80 13.12 18%
Untreated control - 16 14.72 14.24 13.76 13.60 13.92 13%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Shoot borer pest control 78, 86 per cent after 7 days and 74, 82 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Shoot borer after 7 and 15 days of spray.

REPORT OF PHYTO-TOXICITTY EVALUATION ON CHILLI CROP

Evaluation of phyto-toxicity effect of suspo-emulsion formulation of insecticidal composition of Chlorantraniliprole 5% and Pyriproxyfen 5% SEon 50,40,30& 60 gm/ha on Chilli crop.

TABLE-18 :Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein clearing, Wilting before and after spraying of CLSL sample C+P-01 on Chilli crop:

Treatment DAS of observation
Before spray 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3
T1 0 0 0 0 1 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 1 0 1 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

*DAS= Days After spray
C+P-01=Chlorantraniliprole 5% + Pyriproxyfen 5% SE

Treatment:
T1= C+P-01 (25+25) F=1ml/L
T2= C+P-01 (20+20) F=0.8ml/L
T3= C+P-01 (15+15) F=0.6ml/L
T4= C+P-01 (30+30) F=1.2ml/L
T5 =Untreated control (Water only)
Conclusion:

Results of phyto-toxicity evaluation trial are given in table 18. As per results we are concluded that different doses of Chlorantraniliprole 5% + Pyriproxyfen 5% SE (manufactured by Crop life science limited, Ankleshwar, Gujarat) were cause Negligible phytotoxic symptoms on Chilli plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5% + Pyriproxyfen 5% SE is safe to use on Chilli at the dosage from 50, 40, 30 & 60 gm/ha.

Example 12:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Okra whitefly.

Table : 19

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of whitefly/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 23 15.64 11.96 8.74 4.83 5.52 76%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 22 15.84 14.08 9.46 5.72 7.04 68%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 23 17.94 15.87 12.88 10.12 11.73 49%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 24 13.68 13.68 5.28 2.88 3.60 85%
Chlorantraniliprole 18.5% SC 30 22 20.02 18.92 17.82 17.38 18.04 18%
Pyriproxyfen 10% EC 50 24 17.76 16.08 11.76 7.68 8.40 65%
Untreated control - 23 21.39 20.47 19.78 19.09 19.55 15%

Results :
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited whitefly pest control 79, 88 per cent after 7 days and 76, 85 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @50 for control of whitefly after 7 and 15 days of spray.

Example 13: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Okra Aphids.
Table : 20

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Aphids/leaf (15 leaves/ 5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 18 12.96 9.54 4.68 2.52 3.06 83%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 20 15.40 11.60 6.40 4.80 5.60 72%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 18 15.12 12.96 10.44 9.18 10.08 44%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 19 11.21 6.08 3.42 2.09 2.47 87%
Chlorantraniliprole 18.5% SC 30 18 16.56 15.12 14.40 13.68 14.22 21%
Pyriproxyfen 10% EC 50 19 15.20 12.92 8.17 5.51 6.27 67%
Untreated control - 17 16.32 15.47 14.79 14.28 14.62 14%

Results:

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Aphids pest control 86, 89 per cent after 7 days and 83, 87 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Aphids after 7 and 15 days of spray.

Example 14: Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against okra Fruit borer.
Table : 21

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Fruit borer/plant (5 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 26 14.82 8.06 3.38 1.82 2.60 90%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 27 17.28 11.61 6.21 3.78 4.32 84%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 24 17.76 16.32 11.04 9.84 10.56 56%
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 27 12.42 5.94 3.24 0.81 1.62 94%
Chlorantraniliprole 18.5% SC 30 25 17.75 14.00 10.50 8.25 9.50 62%
Pyriproxyfen 10% EC 50 27 23.22 22.14 21.06 19.98 20.52 24%
Untreated control - 26 22.88 21.84 20.80 20.02 20.54 21%

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Fruit borer pest control 93, 97 per cent after 7 days and 90, 94 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Pyriproxyfen 10% EC @ 50 for control of Fruit borer after 7 and 15 days of spray.

Example 15:Bio-efficacy of Chlorantraniliprole 5% + Pyriproxyfen 5% SE against Okra Shoot borer.

Table : 22

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control Synergy
Mean of No. of Shoot borer/plant (24 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1ml/L) 25 + 25 6 4.44 3.48 1.92 0.96 1.08 82% yes
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.8ml/L) 20 + 20 7 5.53 4.48 3.22 1.61 1.89 73% yes
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=0.6ml/L) 15 + 15 7 5.74 5.11 3.78 2.94 3.22 54% No
Chlorantraniliprole 5%+ Pyriproxyfen 5% SE
(F=1.2ml/L) 30 + 30 8 5.44 3.84 1.92 0.72 0.96 88% yes
Chlorantraniliprole 18.5% SC 30 8 6.48 5.44 3.92 2.56 3.04 62% Yes
Pyriproxyfen 10% EC 50 7 6.58 6.23 6.02 5.88 5.95 15% No
Untreated control - 6 5.76 5.58 5.34 5.22 5.40 10% No

Results :

Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose were at as per they exhibited Shoot borer pest control 84, 91 per cent after 7 days and 82, 88 per cent after 10 days of spray.
Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 50 gm (a.i./ha) and Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 60 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @30 and Pyriproxyfen 10% EC @50 for control of Shoot borer after 7 and 15 days of spray.

REPORT OF PHYTO-TOXICITTY EVALUATION ON OKRACROP
Evaluation of phyto-toxicity effect of suspo-emulsion formulation of insecticidal composition of Chlorantraniliprole 5% and Pyriproxyfen 5% on 50,40,30& 60 gm/ha on Okra crop.

TABLE-23 Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein clearing, Wilting before and after spraying of CLSL sample C+P-01 on okra crop:

Treatment DAS of observation
Before spray 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3
T1 0 0 0 0 1 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 1 0 1 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

*DAS= Days After spray
C+P-01=Chlorantraniliprole 5% + Pyriproxyfen 5% SE
Treatment:
T1= C+P-01 (25+25) F=1ml/L
T2= C+P-01 (20+20) F=0.8ml/L
T3= C+P-01 (15+15) F=0.6ml/L
T4= C+P-01 (30+30) F=1.2ml/L
T5 =Untreated control (Water only)

Conclusion:

Results of phyto-toxicity evaluation trial are given in table 23. As per results we are concluded that different doses of Chlorantraniliprole 5% + Pyriproxyfen 5% SE (manufactured by Crop life science limited, Ankleshwar, Gujarat) were cause Negligible phytotoxic symptoms on Okra plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5% + Pyriproxyfen 5% SE is safe to use on okra at the dosage from 50, 40, 30 & 60 gm/ha.

Bio field trial:

Evaluation of bio-efficacy and Phytotoxicity of Chlorantraniliprole 5% + Fenobucarb 40% SE on Rice for the control of pests like Stem borer, Leaf folder, BPH(Brown plant hopper) & GLH(Green Leaf hopper).
Chlorantraniliprole 5% + Fenobucarb 40% SE (CODE-C+F-01)

Objective:
(i) To determine the bio-efficacy of Chlorantraniliprole 5% + Fenobucarb 40% SE against Stem borer, Leaf folder, BPH (Brown plant hopper) & GLH(Green Leaf hopper) of Rice crop.

(ii) To determine Phytotoxicity of Chlorantraniliprole 5% + Fenobucarb 40% SE on Rice crop.

Table : 24

Details of Experiment
a) Test chemical Chlorantraniliprole 5% + Fenobucarb 40% SE
b) Crop Rice
c) Location Misroth, Bhopal, Madhya Pradesh

d) Target pests Stem borer, Leaf folder, BPH (Brown plant hopper) & GLH (Green Leaf hopper).
e) Plot size 3.0 m × 3.0 m
f) Design RBD (Randomized Block Design)
g) Treatment 7(Seven); Table 1
h) Number of reapplication 03
i) Application method Spray by knapsack sprayer fitted with flat fan nozzle (15 Liter)
j) Water volume used 500 liters/ha

Table :25: Treatment details for bio-efficacy of different insecticide:

SR. No. Treatment Dosage Formulation
(A.I. gm/ha)
1. Chlorantraniliprole 5% + Fenobucarb 40% SE (1 ml) 25+200= 225
2. Chlorantraniliprole 5% + Fenobucarb 40% SE (0.8 ml) 20+160=180
3. Chlorantraniliprole 5% + Fenobucarb 40% SE (0.6 ml) 15+120=135
4. Chlorantraniliprole 5% + Fenobucarb 40% SE (1.2 ml) 30+240=270
5. Chlorantraniliprole 18.5% SC 30
6. Fenobucarb 50% EC 1000
7. Untreated control (water only) -

Example 16:Bio-efficacy of Chlorantraniliprole 5% + Fenobucarb 40% SE against Rice Stem borer.
Table :26:

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of stem borer (9 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day 3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=1ml/L) 25 + 200 20 15.00 10.06 7.60 3.20 3.80 81%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=0.8ml/L) 20 + 160 19 15.01 11.59 7.98 5.89 6.46 66%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=0.6ml/L) 15 + 120 19 16.53 14.82 11.21 9.88 10.64 44%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=1.2ml/L) 30 + 240 21 13.02 7.98 3.36 0.84 1.68 92%
Chlorantraniliprole 18.5% SC 30 19 14.63 10.64 7.79 3.23 3.8 80%
Fenobucarb 50% EC 1000 21 17.43 14.49 11.13 9.24 9.66 54%
Untreated control - 20 18.40 17.80 17.20 16.60 17.00 15%

Results :

Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose were at as per they exhibited stem borer pest control 84, 96 per cent after 7 days and 81, 92 per cent after 10 days of spray.
Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Fenobucarb 50% EC @ 1000 for control of stem borer after 7 and 15 days of spray.

Example 17:Bio-efficacy of Chlorantraniliprole 5% + Fenobucarb 40% SE against Rice Leaf folder

Table :27:

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of Leaf folder
(9 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day 3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=1ml/L) 25 + 200 20 13.60 10.40 6.60 2.80 3.20 84%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=0.8ml/L) 20 + 160 15 11.40 9.45 6.90 4.80 5.55 63%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=0.6ml/L) 15 + 120 19 15.58 13.87 11.78 10.26 11.21 41%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=1.2ml/L) 30 + 240 25 13.25 9.00 4.75 1.00 1.75 93%
Chlorantraniliprole 18.5% SC 30 23 15.41 16.20 9.60 5.29 5.98 74%
Fenobucarb 50% EC 1000 20 16.20 11.20 9.60 7.80 8.40 58%
Untreated control - 22 20.02 19.36 19.14 18.48 18.70 15%

Results :

Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose were at as per they exhibited Leaf folder pest control 86, 96 per cent after 7 days and 84, 93 per cent after 10 days of spray.
Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Fenobucarb 50% EC @ 1000 for control of Leaf folder after 7 and 15 days of spray.

Example 18: Bio-efficacy of Chlorantraniliprole 5% + Fenobucarb 40% SE against Rice BPH (Brown plant hopper)
Table :28:

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of BPH (9 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=1ml/L) 25 + 200 450 135 49.5 18.00 27.00 31.50 93%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=0.8ml/L) 20 + 160 435 261.00 100.05 47.85 69.60 82.65 81%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=0.6ml/L) 15 + 120 412 296.64 214.24 177.16 189.52 197.76 52%
Chlorantraniliprole 5%+ Fenobucarb 40% SE (F=1.2ml/L) 30 + 240 448 85.12 35.84 8.96 13.44 17.92 96%
Chlorantraniliprole 18.5% SC 30 440 330.00 228.80 158.40 171.60 184.80 58%
Fenobucarb 50% EC 1000 432 250.56 112.32 73.44 86.40 95.04 78%
Untreated control - 425 378.25 348.50 314.50 323.00 327.25 23%

Results :

Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose were at as per they exhibited BPH (Brown plant hopper) pest control 94, 97 per cent after 7 days and 93, 96 per cent after 10 days of spray.
Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Fenobucarb 50% EC @ 300 for control of BPH (Brown plant hopper) after 7 and 15 days of spray.

Example 19:Bio-efficacy of Chlorantraniliprole 5% + Fenobucarb 40% SE against Rice GLH (Green leaf hopper)
Table :29

Treatments DOSE
gm/ha Observed Value Before Spray Observed Value After Spray % Pest control
Mean of No. of GLH (9 Plants/ treatment)
1st 2nd 3rd 4th 5th
1 day
3 day 5 day 7 day 10 day
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=1ml/L) 25 + 200 28 20.44 13.44 6.16 3.08 3.92 86%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=0.8ml/L) 20 + 160 31 24.49 15.81 10.23 6.80 8.06 74%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=0.6ml/L) 15 + 120 29 24.07 22.04 17.98 16.24 17.11 41%
Chlorantraniliprole 5%+ Fenobucarb 40% SE
(F=1.2ml/L) 30 + 240 32 19.84 12.48 5.76 2.56 2.88 91%
Chlorantraniliprole 18.5% SC 30 30 24.00 21.60 18.30 15.60 16.20 46%
Fenobucarb 50% EC 1000 29 22.04 15.08 9.57 5.51 6.38 78%
Untreated control - 31 28.83 27.90 27.28 26.35 26.66 14%

Results :

Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose were at as per they exhibited GLH (Green plant hopper) pest control 89, 92 per cent after 7 days and 86, 91 per cent after 10 days of spray.
Chlorantraniliprole 5% + Fenobucarb 40% SE @ 225 gm (a.i./ha) and Chlorantraniliprole 5% + Fenobucarb 40% SE @ 270 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Fenobucarb 50% EC @ 1000 for control of GLH (Green Leaf hopper) after 7 and 15 days of spray.

REPORT OF PHYTO-TOXICITTY EVALUATION ON RICE CROP

Evaluation of phyto-toxicity effect of suspo-emulsion formulation of insecticidal composition of Chlorantraniliprole 5% and Fenobucarb 40% on 225, 180, 135 &270 gm/ha on Rice crop.

TABLE-30 Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein clearing, Wilting before and after spraying of CLSL sample C+F-01 on Rice crop:

Treatment DAS of observation
Before spray 1 DAS 3 DAS 5 DAS 7 DAS 10 DAS
R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3 R1 R2 R3
T1 0 0 0 1 1 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 1 0 1 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

*DAS= Days After spray
C+F-01=Chlorantraniliprole 5% + Fenobucarb 40% SE

Treatment:

T1= C+F-01 (25+200) F=1 ml/L
T2= C+F-01 (20+160) F=0.8 ml/L
T3= C+F-01 (15+120) F=0.6 ml/L
T4= C+F-01 (30+240) F=1.2 ml/L
T5= Untreated control (water only)

Conclusion:

Results of phyto-toxicity evaluation trial are given in table 30. As per results we are concluded that different doses of Chlorantraniliprole 5%+ Fenobucarb 40% SE (manufactured by Crop life science limited, Ankleshwar, Gujarat) were cause Negligible phytotoxic symptoms on Rice plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5%+ Fenobucarb 40% SE is safe to use on Rice at the dosage from 225, 180, 135 &270 gm/ha.
,CLAIMS:CLAIMS

We claim;

[CLAIM 1]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition comprises:
a) component (A) Chlorantraniliprole in a amount between 1% to 10 % (w/w)
b) component (B) at least one pesticide selected from Fenobucarb in a amount between 35% to 45 % (w/w) or Pyriproxyfen in a amount between 1% to 10 % (w/w);
c) anti-freezing agent in an amount of 0.1-8 % w/w;
d) one or more emulsifiers in an amount of 0.1-8% w/w;
e) antifoaming agent in an amount of 0.1-5 % w/w;
f) stabilizing agent in an amount of 0.1-5 % w/w;
g) viscosity modifier agent in an amount of 0.1-8 % w/w;
h) filler in amount of 30-80 % w/w (Quantity sufficient);
i) one or more solvent in an amount of 5-35%w/w

[CLAIM 2]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 1, wherein inactive excipients are selected from the group consisting of emulsifiers, antifreezing agents, antifoaming agents, viscosity agents, fillers, stabilizers.

[CLAIM 3]. The suspo-emulsion (SE)formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein the process for the preparation of the suspo-emulsion, comprising step off:
Preparation suspension concentrate (SC) comprises:
a) An aqueous dispersion of chlorantraniliprole in amount of 1% to 10 % (w/w), mixture of chlorantraniliprole with of anti-freezing agent ,antifoaming agent and emulsifiers in water ;
b) Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron.
Preparation of Oil-in Water emulsion (EW) comprises:
a) an emulsion dispersion (Oil-in Water emulsion, EW) of at least one compound selected from Fenobucarb in a amount between 35% to 45 % (w/w) or Pyriproxyfen in a amount between 1% to 10 % (w/w) with solvent aromatic hydrocarbon and emulsifiers in water;
Preparation of suspo-emulsion (SE)
a) Mixing of (Oil-in Water emulsion, EW) formulation into (suspension concentrate, SC) formulation to prepared suspo-emulsion (SE) Formulation.
b) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers or dispersing agents.
c) Finally adding the viscosity agent & preservative to the suspo-emulsion (SE) to enhance viscosity.

[CLAIM 4]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, where in solvent is selected from water, aromatic hydrocarbongroup,ethylacetate,ethyleneglycol,glycerine,heptane,hexamethylphosphoramide(HMPA),Hexamethylphosphoroustriamide(HMPT), methanol, methyl t-butyl ether (MTBE), Toluene, Ortho-xylene, Meta-xylene, Para-xylene, Mix-xylene, Acetone, and Acetonitrile .

[CLAIM 5]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 4, wherein solvent use is preferably aromatic hydrocarbon Solvent C-9.

[CLAIM 6]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 4, wherein solvent is in an amount of 5-35% w/w.

[CLAIM 7]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein emulsifiers is selected from a group comprising of modified naphthalene sulphonic acid condensate sodium salt, Acrylate copolymer, poly-alkoxylated butyl ether, phenyl naphthalene sulphonates, ethoxylated alkyl phenols, ethoxylated fatty acids, alkoxylated linear alcohols, glyceryl esters, maleic anhydride co-polymers, condensation product of aryl sulphonic acids, addition product of ethylene oxide and fatty acid esters, lignin derivatives, naphthalene formaldehyde condensates, sodium salts of iso-decylsulfosuccinic acid half ester, Blend of modified poly ethanoxy ether and sulphated anionic surfactant, blend of alcohol alkoxylates & methyl methacrylate polymer, blend of dialkylate naphthalene sulphonic acid sodium salt, sodium alkyl benesulfonates, sodium salts of sulfonates naphthalene, ammonium salts of Sulfonated naphthalene, salts of poly acrylic acids, salts of Phenolsulfonic acid and salts of naphthalene Sulfonic acids.

[CLAIM 8]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 7, wherein emulsifiers is selected from a group comprising of modified naphthalene sulphonic acid condensate sodium salt, Acrylate co-polymer, Poly-alkoxylated butyl ether, Blend of modified poly ethanoxy ether and sulphated anionic surfactant.

[CLAIM 9]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 7, wherein one or more emulsifiers used are in an amount of 0.1-8 % w/w.

[CLAIM 10]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein anti-freezing agent selected from a group comprising of propylene glycol, diethylene glycol, Mono ethylene glycol, polyol, polyvinyl alcohols and polyethylene glycols, 1,2- Propylene glycol, mono propylene glycol, 1,2-propanediot.

[CLAIM 11]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 10, wherein anti-freezing agent is preferably propylene glycol.

[CLAIM 12]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 10, wherein anti-freezing agent is in an amount of 0.1-8 % w/w.

[CLAIM 13]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein viscosity modifier agent is a group comprising, xanthan gum, gelatine, poly vinyl pyrrolidone, polyvinyl alcohol, sodium methyl cellulose, Poly vinyl pyrrolidone (PVP K-30), silicon oil compound and guar gum.

[CLAIM 14]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 13, wherein viscosity modifier agent is Preferably Xanthan Gum.

[CLAIM 15]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 13, wherein viscosity modifier agent is in an amount of 0.1-8 % w/w.

[CLAIM 16]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein anti foaming agent is silicon based emulsion, silicon Defoamer, Dimethyl polysiloxane or alcohol based antifoam agent.

[CLAIM 17]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 16, wherein anti foaming agent is selected from the group consisting of Dimethyl polysiloxane.

[CLAIM 18]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 16, wherein anti foaming agent is in an amount of 0.1-5 % w/w.

[CLAIM 19]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein filler is water. (Demineralized water)

[CLAIM 20]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 19, wherein filler is in an amount of 30-80% w/w ( Quantity sufficient )

[CLAIM 21]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein Particle size D (50) is less than 5.0 µm & D( 90) is less than 10.0 µm.

[CLAIM 22]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein Viscosity is 300cps to 550cps.

[CLAIM 23]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein synergistic composition comprises:
i. Chlorantraniliprole in an amount between 1-10 %
ii. Fenobucarb in an amount between 35-45 %
iii. Anti-freezing Agent (Propylene glycol) in an amount between 0.1-8 %
iv. Solvent ( solvent C-9) in an amount between 5-35 %
v. One or more emulsifier in an amount between 0.1-8 %
vi. water in amount between 30-80% (Quantity sufficient)
vii. anti-foaming agent in an amount between 0.1-5 %
viii. Stabilizer ( Formaldehyde) in an amount between 0.1-5 %
ix. Viscosity modifier agent ( Xanthan Gum) in an amount between 0.1-8%.
[CLAIM 24]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 23, wherein synergistic chlorantraniliprole (~5 %) and Fenobucarb (~40%) Particle size is:-
i. D(10 ) = 0.737 µm
ii. D(50 ) = 1.843 µm
iii. D(90 ) = 3.733 µm
iv. D( 100 ) = 7.624 µm

[CLAIM 25]. The suspo-emulsion(SE) formulation of synergistic insecticidal composition as claimed in claim 1 or 2, wherein synergistic composition comprises:
i. Chlorantraniliprole in an amount between 1-10 %
ii. Pyriproxyfen in an amount between1-10 %
iii. Ant freezing Agent ( Propylene glycol )in an amount between0.1-8 %
iv. Solvent (solvent C-9) (5-35%)
v. One or more emulsifier in an amount between 0.1-8 %
vi. water in amount between 30-80% (Quantity sufficient)
vii. anti-foaming/ in an amount between 0.1-5 %
viii. Stabilizer ( Formaldehyde) in an amount between 0.1-5 %
ix. Viscosity modifier agent ( Xanthan Gum )in an amount between 0.1-8%.

[CLAIM 26]. The suspo-emulsion (SE) formulation of synergistic insecticidal composition as claimed in claim 25, wherein synergistic chlorantraniliprole (~5 %) and Pyriproxyfen (~5 %) Particle size is:-
i. D(10 ) = 0.714 µm
ii. D(50 ) = 1.976 µm
iii. D(90 ) = 4.990 µm
iv. D(100 ) = 12.691 µm