Claims:CLAIMS
We claim;
1. A novel Suspension Concentrate agrochemical composition comprising:
a. Tolfenpyrad present in an amount of 1% - 20% w/w;
b. an insecticide Fipronil present in an amount of 1% - 20% w/w;
c. another insecticide selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 w/w;
d. a methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane, a super wetting-spreading-penetrating agent is present in an amount of 1% to 10% w/w; and
e. one or more formulation excipients.

2. The novel Suspension Concentrate agrochemical composition as claimed in claim 1, wherein combination of active ingredient is selected from
i. Tolfenpyrad 8% + Fipronil 3% + Abamectin 0.6%;
ii. Tolfenpyrad 8 %+ Fipronil 3% + Fenpyroximate 2%;
iii. Tolfenpyrad 8% + Fipronil 3% + Hexythiazox 2%;
iv. Tolfenpyrad 8% + Fipronil 3% + Etoxazole 3%;
v. Tolfenpyrad 8% + Fipronil 3% + Cyenopyrafen 5%;
vi. Tolfenpyrad 8% + Fipronil 3% + Cyflumetofen 10%;
vii. Tolfenpyrad 8% + Fipronil 3% + Clofentezine 6%;
viii. Tolfenpyrad 8% + Fipronil 3% + Pyridaben 6%;
ix. Tolfenpyrad 8% + Fipronil 3% + Bifenazate 6%;
x. Tolfenpyrad 6.4% + Fipronil 2.4% + Diafenthiuron 18%;
xi. Tolfenpyrad 8% + Fipronil 3% + Dimpropyridaz 5%;
xii. Tolfenpyrad 8% + Fipronil 3% + Spiropidion 5%;
xiii. Tolfenpyrad 8% + Fipronil 3% + Spirotetramat 5%;
xiv. Tolfenpyrad 8% + Fipronil 3% + Spiromesifen 8%;
xv. Tolfenpyrad 8% + Fipronil 3% + Spinosad 3%;
xvi. Tolfenpyrad 8% + Fipronil 3% + Spinetoram 3%;
xvii. Tolfenpyrad 10.6% + Fipronil 4% + Fluxametamide 1%;
xviii. Tolfenpyrad 8% + Fipronil 3% + Chlorfenpyr 5%;
xix. Tolfenpyrad 8% + Fipronil 3% + Fenazaquin 10%;
xx. Tolfenpyrad 10.6% + Fipronil 4% + Broflanilide 1%;
xxi. Tolfenpyrad 8% + Fipronil 3% + Flonicamid 4%;
xxii. Tolfenpyrad 8% + Fipronil 3% + Clothianidin 3%;
xxiii. Tolfenpyrad 8% + Fipronil 3% + Thiamethoxam 3%;
xxiv. Tolfenpyrad8% + Fipronil 3% + Dinotefuran 2% .

3. The novel Suspension Concentrate agrochemical composition as claimed in claim 2, wherein preferred combinations of active ingredients in the composition comprises:
i. Tolfenpyrad 8% + Fipronil 3% + Abamectin 0.6%;
ii. Tolfenpyrad 8 %+ Fipronil 3% + Fenpyroximate 2%;
iii. Tolfenpyrad 8% + Fipronil 3% + Hexythiazox 2%;
iv. Tolfenpyrad 8% + Fipronil 3% + Etoxazole 3%;
v. Tolfenpyrad 8% + Fipronil 3% + Cyenopyrafen 5%;
vi. Tolfenpyrad 8% + Fipronil 3% + Spiromesifen 8%;
vii. Tolfenpyrad 8% + Fipronil 3% + Flonicamid 4%.

4. The novel Suspension Concentrate agrochemical composition as claimed in claim 1, wherein Suspension Concentrate formulation comprises
i. Tolfenpyrad present in an amount of 1% - 20% w/w;
ii. An insecticide Fipronil present in an amount of 1% - 20% w/w;
iii. Another insecticide selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 w/w;
iv. super wetting-spreading-penetrating agent present in an amount of 1 to 10 w/w;
v. dispersing agent I present in an amount of 2 to 8 %w/w;
vi. dispersing agent II present in an amount of 0.1 to 2 %w/w;
vii. suspending agent present in an amount of 0.1 to 2 %w/w;
viii. anti-foaming agent present in an amount of 0.01 to 2 %w/w;
ix. preservative present in an amount of 0.01 to 1.5 %w/w;
x. anti-freezing agent present in an amount of 1 to 10 %w/w;
xi. thickener present in an amount of 0.01 to 2 %w/w ;
xii. Diluent present in an amount of 60 to 80 %w/w.

5. The novel Suspension Concentrate agrochemical composition as claimed in claim 1 or 4, wherein super wetting-spreading-penetrating agent is selected from Methylated seed oil, polyalkyleneoxide modified trisiloxane; Methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane; Methylated seed oil, trisiloxane ethoxylate; Methylated seed oil, polyoxyethylene methyl polysiloxane;
Methylated seed oil, polyether polymethyl siloxane copolymer; Methylated seed oil, polyether modified polysiloxane.

6. The novel Suspension Concentrate agrochemical composition as claimed in claim 1 or 4, wherein seed oil any one or mixture of two or more selected from soybean (Glycine max) oil, groundnut (Arachis hypogaea) oil, rapeseed (Brassica napus subspecies) oil, mustard (Brassica juncea) oil, sesame (Sesamum indicum) oil, Corn (Zea mays) oil, rice (Oryza sativa) bran oil, castor (Ricinum communis) seed oil, cotton (Gossypium hirsutum) seed oil, linseed (Linum usitatissimum), coconut (Cocos nucifera) oil, Kapok (Ceiba pentandra) oil, Papaya (Carica papaya) seed oil, Tea seed (Camellia oleifera) oil, sunflower (Helianthus annuus) oil, safflower (Carthamus tinctorius) seed oil, Eucalyptus (Eucalyptus globulus) oil, Olive (Olea europaea) oil, Jatropha (Jatropha curcas) oil, Garlic acid (Allium sativum), Ginger oil (Zingiber officinale), D-limonene, Citronella oil or Ceylon ironwood (Mesua ferrea) oil.

7. The novel Suspension Concentrate agrochemical composition as claimed in claim 6, wherein preferred seed oils are sunflower oil, soybean oil, rapeseed oil, mustard oil or their blend.

8. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein dispersing agent is selected from Ethylene-propylene oxide block copolymer, Sodium salt of polycarboxylate, Naphthalenesulfonic acid, sodium salt condensated with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide.

9. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein suspending agent is selected from aluminum magnesium silicate, attapulgite clay.

10. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein anti-foaming agent is selected from polydimethyl siloxane, silicone oil, silicone compound, silicone antifoam emulsion, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound.

11. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein anti-freezing agent is selected from ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride.

12. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein Preservative is selected from 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one.

13. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein thickener is selected from xanthan gum, PVK, carboxymethyl celluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch.

14. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein humectant is selected from urea, humic acid, glycerol, lactose.

15. The novel Suspension Concentrate agrochemical composition as claimed in claim 4, wherein diluent is water.

16. The novel Suspension Concentrate agrochemical composition as in any of preceding claims, wherein Suspension Concentrate formulation comprises
i. Tolfenpyrad present in an amount of 1% - 20% w/w;
ii. Fipronil present in an amount of 1% - 20% w/w;
iii. an active ingredient selected from Fenpyroximate or Abamectin present in an amount of 0.1 to 30 %w/w;
iv. Methylated seed oil, polyalkyleneoxide modified trisiloxane present in an amount of 1 to 10 %w/w;
v. Ethylene-propylene oxide block copolymer present in an amount of 2 to 8 %w/w;
vi. Sodium salt of polycarboxylate present in an amount of 0.1 to 2 %w/w;
vii. Aluminum magnesium silicate present in an amount of 0.1 to 2 %w/w;
viii. Polydimethylsiloxane present in an amount of 0.01 to 2 %w/w;
ix. 1,2-benzisothiazolin-3(2H)-one present in an amount of 0.01 to 1.5 %w/w;
x. Polypropylene glycol present in an amount of 1 to 10 %w/w;
xi. Xanthum gum present in an amount of 0.01 to 2 %w/w;
xii. Diluent present in an amount of 60 to 80 %w/w.
Dated this 10th day of January 2022
, Description:FIELD OF INVENTION:
The present invention relates to a novel synergistic Suspension Concentrate (SC) composition comprising bioactive amount of component (A) Tolfenpyrad present in an amount of 1% - 20% w/w; component (B) an insecticide Fipronil present in an amount of 1% - 20% w/w; and (C) another insecticide selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 %w/w. The present invention further relates to selection of suitable formulation excipients, process of preparation of the said Suspension Concentrate formulation/composition and its application in the field of agriculture.
BACKGROUND OF THE INVENTION:
These days cultivation of crops and agriculture in general is cost intensive. Receiving a high yield from the cultivated crops is a key. Hence, to achieve higher yield, protecting crops from insect-pests is vital. Hence, the most effective way to control crop insect-pests is the application of pesticides in accordance with the appropriate management practices with proper formulation thereof.
Treating plants with such a pesticides and plant health additives or combination thereof in appropriate formulation helps to reduce the crops/plants damage. Another advantage of treating the plants with the said combination is the improvement in plant growth overall plant health and increase in the crop yield.
Various kinds of agrochemical formulations are developed based upon active ingredients and scope of application thereof. Pesticides for agriculture purpose are available both in the pure form and as well as incorporated into agrochemical formulations, which typically comprise one or more active ingredients (AIs) and additional excipients substances that enhance the effects and facilitate the application thereof, such as carriers, adjuvants or additives. These formulations can be directly applied onto the crops or, more commonly, are applied after being diluted and the spray mixture formed. The formulation type to be used is primarily defined on the basis of physicochemical characteristics of the AI(s) and can be: soluble concentrate (SL), emulsifiable concentrate (EC), emulsion in water (EW), suspension concentrate (SC), suspo-emulsion (SE), micro-emulsion (ME), oil dispersion (OD) or suspension concentrate (SC), dispersible concentrate (DC), capsule suspension (CS), dispersible granules (WG), wettable powder (WP) and others.
The various types of agrochemical formulations are the result of the existence of a large variety of AIs of different chemical natures. For example, a water soluble AI can be easily included into a water based SL while a high melting, water insoluble AI is commonly found in the form of a EC (Emulsifiable concentrate). For this reason, agrochemical formulations are distinct and can contain different inert components.
In recent years, suspension concentrate (SC) formulations have been the subject of studies by companies and formulators because of their advantages with respect to the agronomic performance in the field as compared with conventional formulations. Active ingredients (AIs) formulated in different types of formulations usually exhibit different physicochemical characteristics based on type of formulation they are incorporated in. Suspension concentrates have shown a rapid development in the past, mainly due to their several benefits when compared to other formulations as no dust; no problem of toxicity or flammability due to solvents; good efficiency due to the smaller particle size; low packaging volume. Further suspension concentrates (SC) formulations have technical benefits as easy dilution and application in the field, risk of phytotoxicity or flammability due to solvents reduced, good bio-efficiency due to the fine particle size, good adhesion and penetration into target surface.
Though suspension concentrate (SC) formulation is called as "flowables" formulation it still requires various adjuvants along with formulation excipients. Suspension concentrate (SC) formulation presents several challenges in the process of manufacturing and developing stable and effective formulation with choice of proper formulation excipient or adjuvants. To obtain a good and stable formulation over time, optimal formulation additives are required in addition to optimum processes. There were several development and research done in the filed field of formulation development of suspension concentrate (SC).
Therefore there is further need and scope in the formulation development of the suspension concentrate (SC) formulations comprising one or more active ingredients with better stability profile and increases the synergistic effect of the active ingredients, reduces the toxicity with less introduction of toxic material in environment, which may reduce the dose of the pesticides and eventually produce less chemicals in environment, with better safety profile for contact pesticides.
RU2395201C1 relates to an insecticide composition in the form of suspension concentrate containing as an active substance a combination of imidacloprid and lambda-Cyhalothrin in synergistically effective amounts. Amount of active ingredient is 6-45 wt. %, the ratio of components in it is from 1:5 to 5:1. To increase the effectiveness of the composition additional mineral or vegetable oil and as adhesive aqueous emulsion of acrylic copolymer are included. A method of cultivated plants insect pest control is also described.
CN102396475A relates to a pesticide composition containing cyantraniliprole and abamectin. The weight ratio of cyantraniliprole to abamectin is 1:12 to 12:1; and the cyantraniliprole and abamectin account for 0.5 to 80 percent of the weight of the pesticide composition in total, and agriculturally acceptable surfactant and solid carrier or liquid diluent account for the balance. The pesticide composition can be used for preventing and controlling various ground and underground pests in field crops, fruit trees, vegetables, other special crops and lawns, including lepidopterous pests, homopterous pests, coleopterous pests, dipterous pests and hemipterous pests.
CA2723616C relates to an active compound combination comprising: 6-[trifluormethylpyridin-3-yl]ethyl(methyl)oxido-.lambda.4-sulfanylidencyanamide and at least one compound selected from the group consisting of: acephate, chlorpyrifos-methyl, chlorpyrifos-ethyl, profenofos, triazophos, beta-cyfluthrin, bifenthrin, alpha-cypermethrin, beta-cypermethrin, theta-cypermethrin, zeta-cypermethrin, deltamethrin, gamma-cyhalothrin, lambda-cyhalothrin, dinotefuran, imidacloprid, imidaclothiz, thiacloprid, thiamethoxam, spinosad, spinetoram, abamectin, emamectin-benzoate, milbemectin, pymetrozine, flonicamid, diafenthiuron, chlorfenapyr, flufenoxuron, lufenuron, novaluron, triflumuron, moulting disruptors cyromazine, methoxyfenozide, amitraz, cyflumetofen, cyenopyrafen, fenpyroximate, pyridaben, tebufenpyrad, indoxacarb, metaflumizone, flubendiamide, chlorantraniliprole (rynaxypyr), cyantraniliprole (cyacypyr), buprofezin, pyridalyl, and 4-{[(6-chloropyrid-3-yl)methyl](2,2-difluoroethyl)amino}furan-2(5H)-one, has good insecticidal and acaricidal properties.
There is however a need for improvement of these combinations. Single active combination used over a long period of time has resulted in resistance. With the onset of resistance to certain pests, there is a need in the art for a combination of actives that decrease the chances of resistance and improves the spectrum of insect-pests control.
In general use, the pesticide actives are used in the form of a dilute aqueous composition because it can attain a good interaction with the target organism, such as plants, insect-pests. However, most active pesticide compounds that are used as pesticides are only sparingly or insoluble in water. The low solubility of such compounds present the challenges and difficulties to formulator in formulating pesticide compounds in stable formulations that can be easily stored for a long time and which can still have a high stability and effective activity until end use. This problem especially occurs and may get worsen if more than one active compound is present in the mixture.
Therefore there is further need to formulate the novel suspension concentrate (SC) formulations which increases the synergistic activities between active ingredients by using the appropriate formulation excipients; enhance the duration of control of insect-pests; reduce the doses of active ingredients and thereby minimizing the pesticidal load into the environment; has thermal and chemical stability over a broad range of weather conditions; reduces the toxicity hazards to the applicators, i.e. improves the safety of applicators at the time of handling and spraying the pesticides; and improves leaf penetration of spray droplets, retard evaporation loss and enhance the absorption of active ingredients.
There is however a need for improvement of suspension concentrate (SC) formulations. Many times it has been found that single or combination of active ingredients requires a high loading dose for the better results. Further this will create a higher loading of the pesticides in the environment. Further many of the suspension concentrate (SC) formulations recipe is prone to lose stability when exposed to the higher temperature. In addition there are higher chances of formulation applied gets evaporated resulting in the loss of the active ingredients before penetration.
Therefore, one object of the present invention is to provide novel suspension concentrate formulation of (A) an insecticide Tolfenpyrad present in an amount of 1% - 20% w/w; and component (B) an insecticide Fipronil present in an amount of 1% - 20% w/w; and (C) an insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 %w/w for the control of insect-pest. Another object of the present invention is to provide a method and a composition for controlling insect pests on a full grown plant.
Further object of the present invention is to provide suitable formulation excipients for the present suspension concentrate (SC) formulations in order to produce stable and synergistic formulation.
Another object of the present invention is to provide a method of manufacture and a composition for the suspension concentrate (SC) formulations.
Embodiment of the present invention can ameliorate one or more of the above mentioned problems.
Inventors of the present invention have surprisingly found that the novel synergistic mixture of suspension concentrate (SC) formulations for plant treatment comprising of (A) an insecticide Tolfenpyrad present in an amount of 1% - 20% w/w; and component (B) an insecticide Fipronil present in an amount of 1% - 20% w/w; and (C) an insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 %w/w can provide solution to the above mentioned problems.
SUMMARY OF INVENTION
Therefore an aspect of the present invention provides a novel synergistic Suspension Concentrate (SC) composition comprising bioactive amount of component (A) Tolfenpyrad present in an amount of 1% - 20% w/w; component (B) an insecticide Fipronil present in an amount of 1% - 20% w/w; and (C) another insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 %w/w; along with formulation excipients.
Further aspect of the present invention is to provide novel Suspension Concentrate (SC) formulation that exhibits synergistic activity and stable over wide range of the conditions.
Further aspect of the present synergistic Suspension Concentrate (SC) composition is to provide selection of suitable formulation excipients selected from category of super wetting-spreading-penetrating agent, dispersing agent, dispersing agent, suspending agent, anti-foaming agent preservative, anti-freezing agent, thickener, diluent.
Another aspect of the present invention is to provide synergistic Suspension Concentrate (SC) formulation comprising of Super Wetting-spreading-penetrating agent selected from- Methylated seed oil, polyalkyleneoxide modified trisiloxane; Methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane; Methylated seed oil, trisiloxane ethoxylate; Methylated seed oil, polyoxyethylene methyl polysiloxane; Methylated seed oil, polyether polymethyl siloxane copolymer; Methylated seed oil, polyether modified polysiloxane.
The present synergistic Suspension Concentrate (SC) composition comprising bioactive amount of component (A) an insecticide Tolfenpyrad; and component (B) an insecticide Fipronil; and (C) an insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam described herein is obtained by a process comprising steps of :
1. Preparation of gum solution by charging thickening agent along with preservative in water followed by homogenizing to prepare gum solution.
2. Charging water with dispersing agent. Homogenize dispersing agent and suspending agent for 45-60 minutes in high shear homogenizer.
3. To formed premix all the active ingredients homoginized to prepare uniform slurry.
4. Grinding the antifoaming agent till the desired particle size achieved.
5. Finally adding 2% gum solution and Methylated seed oil, polyalkyleneoxide modified trisiloxane (super wetting-spreading-penetrating agent) to this formulation to prepare the final Suspension Concentrate (SC) formulation and sending to QC for quality check.
DETAIL DESCRIPTION OF THE INVENTION:
Formulation technology in the field of an agriculture is now seen as an “enabling technology” which can provide safe and effective products which are convenient to use. It can also modify the toxicity of active ingredients and improve their ability to target a specific pest. At a time when the discovery of new agrochemical compounds is more difficult and certainly a high risk and expensive operation, formulation technology can extent the useful patent life of an active ingredient. It can also provide a competitive edge by improving product quality of existing formulations, or by introducing a new formulation of an active ingredient.
Suspension concentrate (SC) formulations consist of having a solid active ingredient dispersed in water. SCs have grown in popularity due to benefits such as absence of dust, ease of use and effectiveness when compared to other formulation types such as emulsifiable concentrate (EC) and wettable powder (WP). To formulate a stable SC, the active ingredient must remain insoluble under all temperature conditions.
The suspension concentrates (SC) formulation consist of Stable dispersion of micronized active ingredient in water. Most of the pesticides are delivered to the target site by spray application in agriculture and public health sectors. The water based Suspension Concentrate formulation provide easy application with elimination of disadvantages and risks posed by solvent based EC formulation like flammability, dermal toxicity and phytotoxicity.
Suspension concentrates (SC) formulation has advantage as easy dilution and application in the field; risk of phytotoxicity or flammability due to solvents reduced good bio-efficiency due to the fine particle size, good adhesion and penetration into target surface. The water based SC formulations do not contain any organic solvent and minimizes environmental pollution by evaporation of solvents.
Further SC formulation has benefits as water based hence it provides good safety and user convenience, suitable for many active ingredients with low water solubility, absence of dust, absence of flammable liquids, small particle size of the active ingredient, adjuvants can be built-in for bio enhancement
Large volume of conventional EC and WP formulations are used in agriculture and public health. The developed SC formulation may have good potential as effective and safer alternative to existing EC, WP formulations.
Suspension Concentrate (SC) formulation presents several challenges in preparation and manufacturing phase. To obtain a good and stable formulation over time, optimal formulation additives are required in addition to optimum processes. Particular attention must be given to choice of all the formulation excipients. Its dispersion and activation are key to the stability of the formulation over time.
Some important requirement of the formulation excipients are perfectly dispersiblility of active ingredients in aqueous phase, no phase separation, easy milling, with no agglomeration, excellent stable dilution, good coverage and penetration, even distribution through the whole formulation, provide the right yield value of active ingredients.
Therefore an aspect of the present invention provides a synergistic agrochemical Suspension Concentrate (SC) composition comprising bioactive amount of (A) Tolfenpyrad; and component (B) an insecticide Fipronil; and (C) another insecticide selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam.
Further aspect of the present invention is to provide novel agrochemical Suspension Concentrate (SC) formulation comprising ternary insecticidal composition with formulation excipients shows synergistic activity and stability over wide range of the conditions.
In an especially preferred embodiment of the invention, the yield of the treated plant is increased.
In another preferred embodiment of the invention, the yield of the plants treated according to the method of the invention, is increased synergistically.
The term "synergistic", as used herein, refers the combined action of two or more active
agents blended together and administered conjointly that is greater than the sum of their individual effects.
Further aspect of the present invention is to provide synergistic agrochemical Suspension Concentrate (SC) formulation comprising formulation excipients from the category of super wetting-spreading-penetrating agent, dispersing agent, dispersing agent, suspending agent, anti-foaming agent preservative, anti-freezing agent, thickener, diluent.
The present inventors believe that the combination of the present invention synergistic agrochemical Suspension Concentrate (SC) composition comprising bioactive amount of bioactive amount of component (A) Tolfenpyrad; and component (B) an insecticide Fipronil; and (C) another insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam surprisingly results in synergistic activity.
The combination of the present invention allows for a broad spectrum of insect-pest control and has surprisingly improved plant vigour and yield. The broad spectrum of the present combination also provides a solution for preventing the development of resistance.
The synergistic agrochemical mixture has very advantageous curative, preventive and systemic insecticidal properties for protecting cultivated plants. As has been mentioned, said active ingredient composition can be used to inhibit or destroy the insect-pests that occur on plants or parts of plants of useful crops. The synergistic agrochemical composition of specific active ingredient has the special advantage of being highly active against insect pests that mostly occur on plant parts.
The present invention will be used to control the following insects-pests.
The major insects pests are belongs to the order Hemiptera, for example, rice leafhopper/green leaf hopper (GLH) Nephotettix nigropictus, rice brown plant hopper (BPH) Nilaparvata lugen, rice backed plant hopper (WBPH) Sogatella furcifera, Apple Mealy bug Phenococcus aceris, bean aphid Aphis fabae, black citrus aphid Toxoptera aurantii, citrus black scale Saissetia oleae, cabbage aphid Brevicoryne brassicae, Lipaphis erysimi, citrus red scale Aonidiella aurantii, yellow scale Aonidiella citrine, citrus mealybug Planococcus citri, corn leaf aphid Rhopalosiphum maidis, aphid Aphis gossypii, jassid Amrasca biguttula biguttla, mealy bug Planococcus spp. And Pseudococcus spp., cotton stainer Dysdercus suturellus, whitefly Bemisia tabaci, cowpea aphid Aphis crassivora, grain aphid Sitobion avenae, golden glow aphid Uroleucon spp., grape mealybug Pseudococcus maritimus, green peach aphid Myzus persicae, greenhouse whitefly Trialeurodes vaporariorum, papaya mealy bug Pracoccus marginatus, pea aphid Acyrthosiphon pisum, sugarcane mealybug Saccharicoccus sacchari, potato aphid Myzus persicae, potato leaf hopper Empoasca fabae, cotton whitefly Bemisia tabaci, tarnished plant bug Lygus lineolaris, wooly apple aphid Eriosoma lanigerum, mango hopper Amritodus atkinsoni, Idioscopus spp. ; order Lepidoptera, army worm Mythimna unipuncta, asiatic rice borer Chilo suppressalis, beet armyworm Spodoptera exigua, black cutworm Agrotis ipsilon, bollworm Helicoverpa armigera , cabbage looper Trichoplusia ni, codling moth Cydia pomonella, croton caterpillar Achea janata, diamond backmoth Plutella xylostella, cabbage worm Pieris rapae, pink bollworm Pectinophora gossypiella, sugarcane borer Diatraea saccharalis, sugarcane early shoot borer Chilo infuscatellus tobacco budworm Heliothis virescens, tomato fruitworm Helicoverpa zea, velvet bean caterpillar Anticarsia gemmatalis, yellow stem borer Scirpophaga incertulas, spotted bollworm Earias vittella, rice leaffolder Cnaphalocrocis medinalis, pink stem borer Sesamia spp., tobacco leafeating caterpillar Spodoptera litura; brinjal fruit and shoot borer Leucinodes orbonalis, bean pod borer Maruca vitrata, Maruca testulalis, armyworm Mythimna separata, cotton pinkbollworm Pectinophora gossypiella, citrus leafminer Phyllocnistis citrella, cabbage butterfly Pieris bras-sicae, diamond backmoth Plutella xylostella, paddy stem borer Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata, wheat stem borer Sesamia inferens, Sitotroga cerealella, Spilosoma obliqua, fall armyworm Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Trichoplusia ni, Tryporyza nivella, Tryporyza incertulas, Tuta absoluta.
from the order Coleoptera, for example, apple twig borer Amphicerus spp., corn root worm Diabrotica virgifera, cucumber beetle diabrotica balteata, boll weevil Anthonomus grandis, grape flea beetle Altica chalybea, grape root worm Fidia viticola, grape trunk borer Clytoleptus albofasciatus, radish flea beetle Phyllotreta armoraciae, maize weevil Sitophilus zeamais, northern corn rootworm Diabrotica barberi, rice water weevil Lissorhoptrus oryzophilus, Anthonomus grandis, Bruchus lentis, Diabrotica semipunctata, Diabrotica virgifera, Dicladispa armigera, Epila-chna varivestis, various species of white grubs are Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotreta chrysocephala, Popillia japonica etc; from the order Orthoptera, for example, Gryllotalpa spp., Locusta spp., and Schistocerca is spp.; from the order Thysanoptera, for example, Thrips- Frankliniella spp., Thrips palmi, Thrips tabaci, Thrips parvispinus, Scirtothrips dorsalis; termites (Isoptera), e.g. Calotermes flavicollis, Coptotermes formosanus, Heterotermes aureus, Leucotermes flavipes, Microtermes obesi, Odontotermes obesus, Reticulitermes flavipes, Termes natalensis; from the order Heteroptera, for example, Dysdercus spp., Leptocorisa spp., from the order Hymenoptera, for example, Solenopsis spp. ; from the order Diptera, for example, Antherigona soccata, Dacus spp., Liriomyza spp., Melanagromyza spp., from the order Acarina, for example, Aceria mangiferae, Brevipalpus spp., Eriophyes spp., Oligonychus mangiferus, Oligonychus punicae, Panonychus citri, Panonychus ulmi, Polyphagotarsonemus latus, Tarsonemus spp., Tetranychus urticae, Tetranychus cinnabarinus.
The mixtures according to the invention can be applied to any and all developmental stages of pests, such as egg, larva, pupa, and adult. The pests may be controlled by contacting the target pest, its food supply, habitat, breeding ground or its locus with a pesticidally effective amount of the inventive mixtures or of compositions comprising the mixtures.
Examples of the crops on which the present compositions may be used include GMO (Genetically Modified Organism) and Non GMO traits, hybrids and conventional varieties of Cotton (Gossypium spp.), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Oat (Avena sativa), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum), Sugarbeet (Beta vulgaris), Soybean (Glycin max), Groundnut/Peanut (Arachis hypogaea), Sunflower (Helianthus annuus), Mustard (Brassica juncea), Rape seed (Brassica napus), Sesame (Sesamum indicum), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Red gram (Cajanus cajan), French bean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus), Onion (Allium cepa L.), Tomato (Solanum lycopersicun), Potato (Solanum tuberosum), Sweet potato (Ipomoea batatas), Chilly (Capsicum annum), Bell pepper (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus), Muskmelons (Cucumis melo), Watermelon (Citrullus lanatus), Bottle gourd (Lagenaria siceraria), Bitter gourd (Momordica charantia), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica rapa rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punica granatum), Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Black Pepper (Piper nigrum), Mentha ( Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold ( Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis), Gerbera ( Gerbera jamesonii), Carnation (Dianthus caryophyllus).

Crops are to be understood as also including those crops which have been rendered tolerant to herbicides or classes of herbicides (e.g. ALS-, GS-, EPSPS-, PPO-, ACCase- and HPPD-inhibitors) by conventional methods of breeding or by genetic engineering. An example of a crop that has been rendered tolerant to imidazolinones, e.g. imazamox, by conventional methods of breeding is Clearfield® summer rape (canola). Examples of crops that have been rendered tolerant to herbicides by genetic engineering methods include e.g. glyphosate- and glufosinate-resistant maize varieties commercially available under the trade names RoundupReady® and LibertyLink®.

Crops are also to be understood as being those which have been rendered resistant to harmful insects by genetic engineering methods, for example Bt maize (resistant to European corn borer), Bt cotton (resistant to cotton boll weevil) and also Bt potatoes (resistant to Colorado beetle). Examples of Bt maize are the Bt 176 maize hybrids of NK® (Syngenta Seeds). The Bt toxin is a protein that is formed naturally by Bacillus thuringiensis soil bacteria. Examples of toxins, or transgenic plants able to synthesise such toxins, are described in EP-A-451 878, EP-A-374 753, WO 93/07278, WO 95/34656, WO 03/052073 and EP-A-427 529. Examples of transgenic plants comprising one or more genes that code for an insecticidal resistance and express one or more toxins are KnockOut® (maize), Yield Gard® (maize), NuCOTIN33B® (cotton), Bollgard® (cotton), NewLeaf® (potatoes), NatureGard® and Protexcta®. Plant crops or seed material thereof can be both resistant to herbicides and, at the same time, resistant to insect feeding (“stacked” transgenic events). For example, seed can have the ability to express an insecticidal Cry3 protein while at the same time being tolerant to glyphosate.

Crops are also to be understood to include those which are obtained by conventional methods of breeding or genetic engineering and contain so-called output traits (e.g. improved storage stability, higher nutritional value and improved flavour).

Other useful plants include turf grass for example in golf-courses, lawns, parks and roadsides, or grown commercially for sod, and ornamental plants such as flowers or bushes.

More particularly in further aspect of the present invention provides the Suspension Concentrate formulation of agrochemical composition comprising bioactive amounts of Compound A: Tolfenpyrad present in an amount of 1% - 20% w/w; Compound B: an insecticide Fipronil present in an amount of 1% - 20% w/w; Compound C: an insecticide compound selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam present in an amount of 0.1 to 30 %w/w.

Active Ingredients
Compound A
Compound B
Compound C
Examples Tolfenpyrad Fipronil An insecticide selected from Abamectin, Broflanilide, Bifenazate, Chlorfenapyr, Clofentazine, Clothianidin, Cyenopyrafen, Cyflumetofen, Diafenthiuron, Dimpropyridaz, Dinotefuran, Etoxazole, Fenpyroximate, Fenazaquin, Flonicamid, Fluxametamide, Hexythiazox, Pyridaben, Spinetoram, Spinosad, Spiromesifen, Spiropidion, Spirotetramat, Spirodiclofen, Thiamethoxam.
% of Active Ingredient 1 to 20% w/w 1 to 20% w/w
0.1 to 30% w/w

The process for preparing the present synergistic mixture can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However all such variations and modifications are covered by the scope of the present invention.
The composition of the present invention in addition to bioactive amounts of active ingredients further comprises of formulation excipients including but not limited to Super Wetting-spreading-penetrating agent, Dispersing agent, Suspending agent, Anti-foaming agent, Anti-freezing agent, Preservatives, Thickeners, Humectant, Diluent/Solvent.
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. Wetting agents are used for two main functions in agrochemical formulations: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules.
Examples of Super Wetting-spreading-penetrating agent for Suspension Concentrate (SC) formulation includes but not limited Methylated seed oil, polyalkyleneoxide modified trisiloxane; Methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane; Methylated seed oil, trisiloxane ethoxylate; Methylated seed oil, polyoxyethylene methyl polysiloxane; Methylated seed oil, polyether polymethyl siloxane copolymer; Methylated seed oil, polyether modified polysiloxane.
The seed oil may be any one or mixture of two or more selected from soybean (Glycine max) oil, groundnut (Arachis hypogaea) oil, rapeseed (Brassica napus subspecies) oil, mustard (Brassica juncea) oil, sesame (Sesamum indicum) oil, Corn (Zea mays) oil, rice (Oryza sativa) bran oil, castor (Ricinum communis) seed oil, cotton (Gossypium hirsutum) seed oil, linseed (Linum usitatissimum), coconut (Cocos nucifera) oil, Kapok (Ceiba pentandra) oil, Papaya (Carica papaya) seed oil, Tea seed (Camellia oleifera) oil, sunflower (Helianthus annuus) oil, safflower (Carthamus tinctorius) seed oil, Eucalyptus (Eucalyptus globulus) oil, Olive (Olea europaea) oil, Jatropha (Jatropha curcas) oil, Garlic acid (Allium sativum), Ginger oil (Zingiber officinale), D-limonene, Citronella oil or Ceylon ironwood (Mesua ferrea) oil. The preferred seed oils are sunflower oil, soybean oil, rapeseed oil, mustard oil or their blend.

A dispersant or a dispersing agent is a substance which adsorbs 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 formulations to facilitate dispersion and suspension during manufacture, and to ensure the particles re-disperse into water in a spray tank. They are widely used in wettable powders, suspension concentrates and water-dispersible granules. Surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier to re-aggregation of particles. The most commonly used surfactants are anionic, non-ionic, or mixtures of the two types. For wettable powder formulations, the most common dispersants are sodium lingo sulphonates. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. These have very long hydrophobic ‘backbones’ and a large number of ethylene oxide chains forming the ‘teeth’ of a ‘comb’ surfactant. These high molecular weight polymers can give very good long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces.
Examples of dispersants or dispersing agent used herein for Suspension Concentrate (SC) formulation includes but not limited to Ethylene-propylene oxide block copolymer, Sodium salt of polycarboxylate, Naphthalenesulfonic acid, sodium salt condensated with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide;
Examples of suspending agent used herein for Suspension Concentrate (SC) formulation includes but not limited to aluminum magnesium silicate, attapulgite clay.
Examples of Antifoaming agent used herein for Suspension Concentrate (SC) formulation includes but not limited to polydimethyl siloxane, silicone oil, silicone compound, silicone antifoam emulsion, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound.
Examples of Anti-freezing agent used herein for Suspension Concentrate (SC) formulation includes but not limited to ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride.
Examples of Preservative used herein for Suspension Concentrate (SC) formulation includes but not limited to 11,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one.
Examples of Thickeners used herein for Suspension Concentrate (SC) formulation includes but not limited to xanthan gum, PVK, carboxymethyl celluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch.
Examples of Diluent/Solvent used herein for Suspension Concentrate (SC) formulation includes water.
While the foregoing written description of the invention enables one of ordinary skill to make and use what is considered presently to be the best mode thereof, those of ordinary skill will understand and appreciate the existence of variations, combinations, and equivalents of the specific embodiment, method, and examples herein. The invention should therefore not be limited by the above described embodiment, method, and examples, but by all embodiments and methods within the scope and spirit of the invention. The invention shall now be described with reference to the following specific examples. It should be noted that the example(s) appended below illustrate rather than limit the invention, and that those skilled in the art will be able to design many alternative embodiments without departing from the scope of the present invention.
These and other aspects of the invention may become more apparent from the examples set forth herein below. These examples are provided merely as illustrations of the invention and are not intended to be construed as a limitation thereof.
EXAMPLE 1:
Recipe A-Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Novel)
Chemical composition Percent (w/w)
Tolfenpyrad a.i. 8.00
Fipronil a.i. 3.00
Fenpyroximate a.i. 2.00
Methylated seed oil, polyalkyleneoxide modified trisiloxane (super wetting-spreading-penetrating agent) 4.50
Ethylene-propylene oxide block copolymer (dispersing agent I) 4.50
Sodium salt of polycarboxylate (dispersing agent II) 1.00
Aluminum magnesium silicate (suspending agent) 0.50
Polydimethylsiloxane (anti foaming agent) 0.30
1,2-benzisothiazolin-3(2H)-one (preservative) 0.20
Polypropylene glycol (anti freezing agent) 5.00
Xanthum gum (thickner) 0.15
Diluent water 70.85
Total 100.00

Storage Stability Study:
Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Novel)

Storage stability-Recipe A-Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Novel)
Laboratory storage stability for 14 days
Parameters Specification (in house) Initial At 54±2 0C At 0±2 0C
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.62 8.38 8.52
Fipronil a.i. (% w/w) 2.85 to 3.30 3.26 3.06 3.12
Fenpyroximate a.i. (% w/w) 1.90 to 2.20 2.17 2.10 2.14
Tolfenpyrad suspensibility (%) 80 98.20 96.80 97.80
Fipronil suspensibility (%) 80 98.60 97.40 98.20
Fenpyroximate suspensibility (%) 80 98.00 96.80 97.50
pH range (1% aq. Suspension) 5.5 to 8.0 7.05 7.00 7.05
Pourability (%) 95 98.20 97.60 98.00
Specific gravity 1.05-1.10 1.07 1.06 1.07
Viscosity at spindle no.62,20 rpm 350-800 cps 600 610 600
Particle size (micron) D50<3, D90<10 2.1,7.4 2.1, 7.6 2.1, 7.4
Persistent foam ml (after 1 minute) max. 60 nil 3 nil
Room temperature storage stability up to 12 months
Parameters Specification (in house) Initial 1 month 6 month 12 month
Tolfenpyrad a.i. (% w/w) 5.70 to 6.60 8.62 8.60 8.56 8.51
Fipronil a.i. (% w/w) 9.50 to 10.50 3.26 3.25 3.22 3.08
Fenpyroximate a.i. (% w/w) 3.16 to 3.66 2.17 2.15 2.14 2.1
Tolfenpyrad suspensibility (%) 80 98.20 98.00 97.60 96.60
Fipronil suspensibility (%) 80 98.60 98.20 97.50 97.40
Fenpyroximate suspensibility (%) 80 98.00 97.40 97.00 96.80
pH range (1% aq. Suspension) 5.5 to 8.0 7.05 7.05 7.05 7.1
Pourability (%) 95 98.20 98.00 97.70 97.50
Specific gravity 1.05-1.10 1.07 1.07 1.07 1.06
Viscosity at spindle no. 62, 20 rpm 350-800 cps 470 470 460 440
Particle size (micron) D50<3, D90<10 2.1, 7.4 2.1,7.4 2.2, 7.5 2.2, 7.6
Persistent foam in ml (after 1 minute) max. 60 nil nil nil 3

The novel SC formulation recipe of Tolfenpyrad 8% + Fipronil 3% + Fenpyroximate 2% meets the all in-house specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Procedure: Manufacturing process for Suspension Concentrate formulation

Step 1 2% Gum Solution: Charge Xanthan gum (2.0 kg) and 1,2-benzisothiazoline-3-one (2.0 kg) into 96 kg water and homogenize. It should be made 12-18 hour prior to use.
Step 2 Charge DM water (50.85 liter) and 1,2-propylene glycol (5 kg) into designated vessel and mix thoroughly.
Step 3 Add Ethylene-propylene oxide block copolymer (4.5 kg), Sodium salt of polycarboxylate (1kg) and Aluminium magnesium silicate (0.5 kg) into the vessel having water and homogenize the contents for 45 – 60 minutes using high shear homogenizer
Step 4 Then add Tolfenpyrad technical (8 kg), Fipronil technical (3 kg) and Fenpyroximate technical (2 kg) to this premix slowly and homogenized to get uniform slurry ready for grinding.
Step 5 Before grinding half the quantity of Polydimethylsiloxane (0.15 kg) was added and then material was subjected to grinding in Dyno mill till desired particle size is achieved.
Step 6 Add remaining Polydimethyl siloxane (0.15 kg) antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7 Finally add 20.0 kg of 2% gum solution and 4.5 kg of Methylated seed oil, polyalkyleneoxide modified trisiloxane (super wetting-spreading-penetrating agent) to this formulation and send to QC for quality check.

General Recipe
Recipe B-Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Conventional)

Chemical composition Percent (w/w)
Tolfenpyrad a.i. 8.00
Fipronil a.i. 3.00
Fenpyroximate a.i. 2.00
Polyoxyethylene styryl phenyl ehter and polyoxyethylene alkyl aryl ether (wetting cum dispersing agent) 4.00
Sodium Lignosulfonate (dispersing agent) 1.00
Silica (suspending agent) 1.00
Polydimethylsiloxane (antifoaming agent) 0.50
1,2-benzisothiazolin-3(2H)-one (preservative) 0.30
Polypropylene glycol (antifreezing agent) 5.00
Xanthum gum (thickner) 0.15
Water (diluent) 68.72
Total 100.00

Storage Stability Study:
Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Conventional)
Storage stability-Recipe B-Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Conventional)
Laboratory storage stability for 14 days
Parameters Specification (in house) Initial At 54±2 0C At 0±2 0C
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.12 8.40
Fipronil a.i. (% w/w) 2.85 to 3.30 3.30 3.03 3.18
Fenpyroximate a.i. (% w/w) 1.90 to 2.20 2.20 2.02 2.10
Tolfenpyrad suspensibility (%) 80 95.40 88.40 92.60
Fipronil suspensibility (%) 80 95.30 89.50 93.80
Fenpyroximate suspensibility (%) 80 96.20 90.20 94.60
pH range (1% aq. Suspension) 5.5 to 8.0 7.00 6.80 7.0
Pourability (%) 95 95.00 93.60 94.80
Specific gravity 1.05-1.10 1.05 1.06 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 600 770 660
Particle size (micron) D50<3, D90<10 2.2, 8.0 3.4, 11.5 3.1, 10.5
Persistent foam ml (after 1 minute) max. 60 nil 5 nil
Room temperature storage stability up to 12 months
Parameters Specification (in house) Initial 1 month 6 month 12 month
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.46 8.22 8.10
Fipronil a.i. (% w/w) 2.85 to 3.30 3.30 3.22 3.12 3.02
Fenpyroximate a.i. (% w/w) 1.90 to 2.20 2.20 2.18 2.06 2.02
Tolfenpyrad suspensibility (%) 80 95.40 94.40 93.20 92.50
Fipronil suspensibility (%) 80 95.30 94.60 94.00 93.60
Fenpyroximate suspensibility (%) 80 96.20 95.80 95.00 94.50
pH range (1% aq. Suspension) 5.5 to 8.0 7.00 7.00 6.90 6.80
Pourability (%) 95 95.00 94.80 94.00 93.60
Specific gravity 1.05-1.10 1.05 1.05 1.05 1.05
Viscosity at spindle no. 62, 20 rpm 350-800 cps 600 630 680 740
Particle size (micron) D50<3, D90<10 2.2, 8.1 2.5, 8.6 3.2, 10.1 3.4, 10.8
Persistent foam in ml (after 1 minute) max. 60 3 5 10 30

The conventional SC formulation recipe of Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% does not meets the pourability and particle size criteria for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

EXAMPLE 2:
Innovative Recipe
Recipe A1-Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Novel)
Chemical composition Percent (w/w)
Tolfenpyrad a.i. 8.00
Fipronil a.i. 3.00
Abamectin a.i. 0.60
Methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane (super wetting-spreading-penetrating agent) 5.00
Ethylene-propylene oxide block copolymer (dispersing agent I) 4.50
Sodium salt of polycarboxylate (dispersing agent II) 1.00
Aluminum magnesium silicate (suspending agent) 0.50
Polydimethylsiloxane (antifoaming agent) 0.30
1,2-benzisothiazolin-3(2H)-one (preservative) 0.20
Polypropylene glycol (antifreezing agent) 5.00
Xanthum gum (thickner) 0.15
water (diluent) 71.75
Total 100.00

Storage Stability Study:
Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Novel)

Storage stability-Recipe A1-Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Novel)

Laboratory storage stability for 14 days
Parameters Specification (in house) Initial Stability at 54±2 0C Stability at 0±2 0C
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.42 8.58
Fipronil a.i. (% w/w) 2.85 to 3.30 3.26 3.14 3.24
Abamectin a.i. (% w/w) 0.57 to 0.66 0.65 0.62 0.64
Tolfenpyrad suspensibility (%) 80 98.60 97.50 98.20
Fipronil suspensibility (%) 80 98.40 97.20 98.00
Abamectin suspensibility (%) 80 98.60 97.50 98.10
pH range (1% aq. Suspension) 5.5 to 8.0 7.05 7.05 7.05
Pourability (%) 95 98.80 98.20 98.50
Specific gravity 1.05-1.10 1.05 1.05 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 550 520 540
Particle size (micron) D50<3, D90<10 2.1, 8.5 2.1, 8.4 2.1, 8.5
Persistent foam ml (after 1 minute) max. 60 nil 1 nil
Room temperature storage stability up to 12 months
Parameters Specification (in house) Initial 1 month 6 months 12 months
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.65 8.62 8.57
Fipronil a.i. (% w/w) 2.85 to 3.30 3.26 3.26 3.25 3.25
Abamectin a.i. (% w/w) .57 to 0.66 0.65 0.65 0.65 0.62
Tolfenpyrad suspensibility (%) 80 98.60 98.60 98.40 98.00
Fipronil suspensibility (%) 80 98.40 96.40 98.40 98.20
Abamectin suspensibility (%) 80 98.60 98.60 98.30 98.20
pH range (1% aq. Suspension) 5.5 to 8.0 7.05 7.05 7.05 7.00
Pourability (%) 95 98.80 98.80 98.60 98.50
Specific gravity 1.05-1.10 1.05 1.05 1.05 1.05
Viscosity at spindle no. 62, 20 rpm 350-800 cps 550 550 530 520
Particle size (micron) D50<3, D90<10 2.1, 8.5 2.1, 8.5 2.1, 8.6 2.2, 8.7
Persistent foam in ml (after 1 minute) max. 60 nil nil nil 2

The novel SC formulation recipe of Tolfenpyrad 8% + Fipronil 3% + Abamectin 0.6% meets the all in-house specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Procedure: Manufacturing process for Suspension Concentrate formulation

Step 1 2% Gum Solution: Charge Xanthan gum (2.0 kg) and 1,2-benzisothiazoline-3-one (2.0 kg) into 96 kg water and homogenize. It should be made 12-18 hour prior to use.
Step 2 Charge DM water (51.75 liter) and 1,2-propylene glycol (5 kg) into designated vessel and mix thoroughly.
Step 3 Add Ethylene-propylene oxide block copolymer (4.5 kg), Sodium salt of polycarboxylate(1kg) and Aluminium magnesium silicate (0.5 kg) into the vessel having water and homogenize the contents for 45 – 60 minutes using high shear homogenizer
Step 4 Then add Tolfenpyrad technical (8 kg), Fipronil technical (3 kg) and Abamectin technical (0.6 kg) to this premix slowly and homogenized to get uniform slurry ready for grinding.
Step 5 Before grinding half the quantity of Polydimethylsiloxane (0.15 kg) was added and then material was subjected to grinding in Dyno mill till desired particle size is achieved.
Step 6 Add remaining Polydimethyl siloxane (0.15 kg) antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7 Finally add 20.0 kg of 2% gum solution and 4.5 kg of Methylated seed oil, polyalkyleneoxide modified trisiloxane (super wetting-spreading-penetrating agent) to this formulation and send to QC for quality check.

General Recipe
Recipe B1-Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Conventional)

Chemical composition Percent (w/w)
Tolfenpyrad a.i. 8.00
Fipronil a.i. 3.00
Abamectin a.i. 0.60
Dioctyl sulfosuccinate (wetting agent) 2.00
Ethylene-propylene oxide block copolymer (dispersing agent I) 4.50
Sodium salt of polycarboxylate (dispersing agent II) 1.50
Aluminum magnesium silicate (suspending agent) 1.00
Polydimethylsiloxane (antifoaming agent) 0.30
1,2-benzisothiazolin-3(2H)-one (preservative) 0.20
Polypropylene glycol (antifreezing agent) 5.00
Xanthum gum (thickner) 1.50
Water (diluent) 72.40
Total 100.00

Storage Stability Study:
Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Conventional)
Storage stability-Recipe B1-Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC (Conventional)
Laboratory storage stability for 14 days
Parameters Specification (in house) Initial Stability at 54±2 0C Stability at 0±2 0C
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.08 8.32
Fipronil a.i. (% w/w) 2.85 to 3.30 3.26 3.02 3.16
Abamectin a.i. (% w/w) 0.57 to 0.66 0.65 0.61 0.62
Tolfenpyrad suspensibility (%) 80 96.20 95.60 94.20
Fipronil suspensibility (%) 80 96.50 95.80 94.80
Abamectin suspensibility (%) 80 96.40 95.20 93.80
pH range (1% aq. Suspension) 5.5 to 8.0 7.00 6.90 6.95
Pourability (%) 95 95.00 93.60 94.20
Specific gravity 1.05-1.10 1.05 1.05 1.05
Viscosity at spindle no.62,20 rpm 350-800 cps 650 760 690
Particle size (micron) D50<3, D90<10 2.1, 8.6 3.7, 11.2 3.2, 10.2
Persistent foam ml (after 1 minute) max. 60 nil 8 2
Room temperature storage stability up to 12 months
Parameters Specification (in house) Initial 1 month 6 months 12 months
Tolfenpyrad a.i. (% w/w) 7.60 to 8.80 8.65 8.62 8.30 8.04
Fipronil a.i. (% w/w) 2.85 to 3.30 3.26 3.18 3.08 3.02
Abamectin a.i. (% w/w) .57 to 0.66 0.65 0.63 0.62 0.60
Tolfenpyrad suspensibility (%) 80 96.20 95.40 95.00 94.20
Fipronil suspensibility (%) 80 96.50 95.80 94.80 94.20
Abamectin suspensibility (%) 80 96.40 95.60 94.20 93.80
pH range (1% aq. Suspension) 5.5 to 8.0 7.00 7.00 6.95 6.90
Pourability (%) 95 95.00 95.00 92.40 90.20
Specific gravity 1.05-1.10 1.05 1.05 1.05 1.05
Viscosity at spindle no. 62, 20 rpm 350-800 cps 650 650 720 780
Particle size (micron) D50<3, D90<10 2.1, 8.6 2.3, 8.7 3.0, 9.8 3.4, 10.6
Persistent foam in ml (after 1 minute) max. 60 8 10 15 28

The conventional SC formulation recipe of Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% does not meets the pourability and particle size criteria for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
EXAMPLE 3:
Lists of preferred combinations and ratio of active ingredients for novel SC formulation:
Compound A Compound B Compound C Active ingredients (%) Formulation Strength (%) Formulation Type
A B C
Tolfenpyrad Fipronil Abamectin 8 3 0.6 11.60 Novel SC
Tolfenpyrad Fipronil Fenpyroximate 8 3 2 13.00 Novel SC
Tolfenpyrad Fipronil Hexythiazox 8 3 2 13.00 Novel SC
Tolfenpyrad Fipronil Etoxazole 8 3 3 14.00 Novel SC
Tolfenpyrad Fipronil Cyenopyrafen 8 3 5 16.00 Novel SC
Tolfenpyrad Fipronil Cyflumetofen 8 3 10 21.00 Novel SC
Tolfenpyrad Fipronil Clofentezine 8 3 6 17.00 Novel SC
Tolfenpyrad Fipronil Pyridaben 8 3 6 17.00 Novel SC
Tolfenpyrad Fipronil Bifenazate 8 3 6 17.00 Novel SC
Tolfenpyrad Fipronil Diafenthiuron 6.4 2.4 18 26.80 Novel SC
Tolfenpyrad Fipronil Dimpropyridaz 8 3 5 16.00 Novel SC
Tolfenpyrad Fipronil Spiropidion 8 3 5 16.00 Novel SC
Tolfenpyrad Fipronil Spirotetramat 8 3 5 16.00 Novel SC
Tolfenpyrad Fipronil Spiromesifen 8 3 8 19.00 Novel SC
Tolfenpyrad Fipronil Spinosad 8 3 3 14.00 Novel SC
Tolfenpyrad Fipronil Spinetoram 8 3 3 14.00 Novel SC
Tolfenpyrad Fipronil Fluxametamide 10.6 4 1 15.60 Novel SC
Tolfenpyrad Fipronil Chlorfenpyr 8 3 5 16.00 Novel SC
Tolfenpyrad Fipronil Fenazaquin 8 3 10 21.00 Novel SC
Tolfenpyrad Fipronil Broflanilide 10.6 4 1 15.60 Novel SC
Tolfenpyrad Fipronil Flonicamid 8 3 4 15.00 Novel SC
Tolfenpyrad Fipronil Clothianidin 8 3 3 14.00 Novel SC
Tolfenpyrad Fipronil Thiamethoxam 8 3 3 14.00 Novel SC
Tolfenpyrad Fipronil Dinotefuran 8 3 2 13.00 Novel SC

Biological Examples:
A synergistic effect exists wherever the action of a combination of active ingredient is greater than the sum of the action of each of the components alone. Therefore, a synergistically effective amount or an effective amount of a synergistic composition or combination is an amount that exhibits greater pesticidal activity than the sum of the pesticidal activities of the individual components.
In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two or three active components can be calculated as follows:

FIELD BIO-EFFICACY STUDIES:
The novel SC (Suspension Concentrate) formulation of Tolfenpyrad + Fipronil + Insecticide has been developed in the laboratory and evaluated for its efficacy, residual control and rain-fast action in comparison with prior art formulations and tank mixes.

Experiment 1: Synergistic control of Okra thrips (Thrips tabaci) and mites (Tetranychus urticae)
Crop & Variety : Okra
Location : Durg, Chhattishgarh
Treatments : 32
Plot size : 16 sq.m.
Crop age : 66 days
Spray water volume : 500 liter per hectare
Method of Application: Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Agronomic Practices : All agronomic practices followed as per the crop requirement.
Observation Methods:
Thrips (Scirtothrips dorsalis) control (%):
Count the number of live thrips per twigs by shaking it gently over piece of paper. Record the observations from 4 twigs per plant and 10 plants per plot. Calculate thrips control (%) as;

Mite (Polyphagotarsonemus latus) control (%):
Record the number of motile stages of mite per spot, 4 spots per plant and 10 plants per plot. Calculate mite control (%) as;

Thrips and Mite control (%) data were used to check the synergism by applying Colby’s.
Fruit yields : Count the number of healthy fruits per plant. Record the observations from 5 plants per plot.

Table 1: Treatment details
Treatment Number Treatment details gram active per hectare
T1 Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC 80+30+20
T2 Tolfenpyrad 8%+Fipronil 3%+Hexythiazox 2% SC 80+30+20
T3 Tolfenpyrad 8%+Fipronil 3%+Etoxazole 3% SC 80+30+30
T4 Tolfenpyrad 8%+Fipronil 3%+Abamectin 0.6% SC 80+30+6
T5 Tolfenpyrad 8%+Fipronil 3%+Cyenopyrafen 5% SC 80+30+50
T6 Tolfenpyrad 8%+Fipronil 3%+Spiromesifen 8% SC 80+30+80
T7 Tolfenpyrad 8%+Fipronil 3%+Fluxametamide 0.75% SC 80+30+7.5
T8 Tolfenpyrad 15% SC+Fenpyroximate 5% SC 80+20
T9 Tolfenpyrad 15% SC+Hexythiazox 5.45% EC 80+20
T10 Tolfenpyrad 15% SC+Etoxazole 10% SC 80+30
T11 Tolfenpyrad 15% SC+Abamectin 1.9% EC 80+6
T12 Tolfenpyrad 15% SC+Cyenopyrafen 30% SC 80+50
T13 Tolfenpyrad 15% SC+Spiromesifen 22.9% SC 80+80
T14 Tolfenpyrad 15% SC+Fluxametamide 10% EC 80+7.5
T15 Fipronil 18.87% SC+Fenpyroximate 5% SC 30+20
T16 Fipronil 18.87% SC+Hexythiazox 5.45% EC 30+20
T17 Fipronil 18.87% SC+Etoxazole 10% SC 30+30
T18 Fipronil 18.87% SC+Abamectin 1.9% EC 30+6
T19 Fipronil 18.87% SC+Cyenopyrafen 30% SC 30+50
T20 Fipronil 18.87% SC+Spiromesifen 22.9% SC 30+80
T21 Fipronil 18.87% SC+Fluxametamide 10% EC 30+7.5
T22 Tolfenpyrad 15% SC+Fipronil 18.87% SC 80+30
T23 Tolfenpyrad 15% SC 80
T24 Fipronil 18.87% SC (Regent Gold)* 30
T25 Fenpyroximate 5% SC (Tata Neon)* 20
T26 Hexythiazox 5.45% EC (Maiden)* 20
T27 Etoxazole 10% SC (Borneo)* 30
T28 Abamectin 1.9% EC (Abacin)* 6
T29 Cyenopyrafen 30% SC (Kunochi)* 50
T30 Spiromesifen 22.9% SC (Oberon)* 80
T31 Fluxametamide 10% EC (Gracia)* 7.5
T32 Untreated Check (UTC) -

T1 to T7 were novel ready mix SC formulation. T8 to T22 were conventional tank mixes. * Brand name.
Table 2: Synergistic control of Chilli Thrips and Mites.
Treatment Number Thrips control (%) at 5 DAA Mite control (%) at 5 DAA
Observed control Expected control Colby's ratio Synergism (Y/N) Observed control Expected control Colby's ratio Synergism (Y/N)
T1 96.4 90.09 1.07 Yes 96.2 91.32 1.05 Yes
T2 95.8 90.00 1.06 Yes 95.8 90.81 1.05 Yes
T3 94.4 89.38 1.06 Yes 94.6 90.35 1.05 Yes
T4 98.8 92.53 1.07 Yes 96.4 90.86 1.06 Yes
T5 96.2 89.08 1.08 Yes 93.8 89.89 1.04 Yes
T6 94.6 89.35 1.06 Yes 95.4 90.26 1.06 Yes
T7 98.2 92.38 1.06 Yes 89.8 88.96 1.01 Yes
T8 77.2 78.36 0.99 No 82.4 85.86 0.96 No
T9 76.4 78.16 0.98 No 81.6 85.04 0.96 No
T10 74.4 76.82 0.97 No 80.4 84.28 0.95 No
T11 80.2 83.70 0.96 No 79.6 85.11 0.94 No
T12 75.4 76.15 0.99 No 78.4 83.53 0.94 No
T13 73.6 76.75 0.96 No 79.6 84.13 0.95 No
T14 81.2 83.37 0.97 No 77.2 82.03 0.94 No
T15 68.8 70.32 0.98 No 71.4 76.91 0.93 No
T16 67.4 70.05 0.96 No 71.2 75.56 0.94 No
T17 65.6 68.21 0.96 No 69.8 74.33 0.94 No
T18 74.2 77.65 0.96 No 70.6 75.69 0.93 No
T19 65.8 67.30 0.98 No 67.4 73.11 0.92 No
T20 64.2 68.12 0.94 No 69.2 74.09 0.93 No
T21 74.8 77.19 0.97 No 64.8 70.65 0.92 No
T22 80.2 84.70 0.95 No 72.6 76.91 0.94 No
T23 66.6 62.4
T24 54.2 38.6
T25 35.2 62.4
T26 34.6 60.2
T27 30.6 58.2
T28 51.2 60.4
T29 28.6 56.2
T30 30.4 57.8
T31 50.2 52.2
T32 0.0 0.0
DAA-days after application
Table 2a. Chilly fruit yield
Treatment number Number of healthy fruits per plant Increase (%) in healthy fruits over T32

T1 44.8 154.5
T2 43.6 147.7
T3 41.8 137.5
T4 44.4 152.3
T5 41.8 137.5
T6 42.6 142.0
T7 43.0 144.3
T8 34.8 97.7
T9 35.2 100.0
T10 36.2 105.7
T11 35.8 103.4
T12 34.4 95.5
T13 33.8 92.0
T14 35.0 98.9
T15 36.2 105.7
T16 32.8 86.4
T17 33.6 90.9
T18 35.2 100.0
T19 34.4 95.5
T20 32.2 83.0
T21 35.2 100.0
T22 34.2 94.3
T23 31.4 78.4
T24 28.8 63.6
T25 27.8 58.0
T26 28.4 61.4
T27 27.6 56.8
T28 29.2 65.9
T29 25.8 46.6
T30 26.4 50.0
T31 25.4 44.3
T32 17.6 0.0

The novel ready mix SC formulations of Tolfenpyrad+Fipronil+Insecticide (T1 to T7) provides synergistic control of chilly thrips and mites on 5th days after application as compared to all conventional treatments (T8 to T31). The novel SC formulations of Tolfepyrad+Fipronil+Insecticide (T1 to T7) also produces higher number of green chilly fruits as compared to all conventional treatments (T8 to T31).

Experiment 2: Comparison of Novel SC formulation with conventional SC and tank mixes (Dose reduction)
Crop & Variety : Brinjal
Location : Durg, Chhattishgarh
Treatments : 7
Plot size : 30 sq.m.
Crop age : 72 days after transplanting.
Spray water volume : 500 liter per hectare
Method of Application: Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Agronomic Practices : All agronomic practices followed as per the crop requirement.
Observation Methods:
Jassid (Amrasca biguttula biguttual) control (%):
Count the number of live insests (nymph and adutls) per leaf. Record the observation from 3 leaves per plant and 10 plants per plot. Record the observations at 3, 7, 10 and 14 days after application (DAA). Jassid control (%) as observed value were used to check the synergism by applying Colby’s formula.
Table 3: Treatment details

Treatment Number Treatment details with application Rate (gai/h)
T1 Novel SC Tolfenpyrad 7%+Fipronil 4%+Fenpyroximate 2.5% SC (Novel), 1000 ml (70+40+25 gia/h)
T2 Tolfenpyrad 7%+Fipronil 4%+Fenpyroximate 2.5% SC (Novel), 800 ml (56+32+20 gia/h)
T3 Conventional SC Tolfenpyrad 7%+Fipronil 4%+Fenpyroximate 2.5% SC (Conventional), 1000 ml (70+40+25 gia/h)
T4 Tolfenpyrad 7%+Fipronil 4%+Fenpyroximate 2.5% SC (Conventional), 800 ml (56+32+20 gia/h)
T5 Tank mixes Tolfenpyrad 15% SC+Fipronil 18.87% SC+Fenpyroximate 5% SC (tank mix), (70+40+25 gai/h)
T6 Tolfenpyrad 15% SC+Fipronil 18.87% SC+Fenpyroximate 5% SC (tank mix), (56+32+20 gai/h)
T7 UTC (Untreated Check)

Table 4a: Efficacy and residual control observed with Novel SC, conventional SC and tank mixes against brinjal jassid.
Treatment Number Jassid control (%)
3 DAA 7 DAA 10 DAA 14 DAA
T1 98.6 94.8 89.2 83.6
T2 95.6 90.0 83.2 75.2
T3 97.2 90.6 84.8 74.6
T4 92.6 82.2 74.2 60.6
T5 93.4 84.6 70.2 60.6
T6 85.4 72.6 55.4 40.8
T7 0.0 0.0 0.0 0.0

Table 4b: Efficacy and residual control observed with Novel SC, conventional SC and tank mixes against brinjal jassid
Treatment Number Drop in efficacy due to dose reduction
3 DAA 7 DAA 10 DAA 14 DAA
Novel Formulation (T1-T2) 3.0 4.8 6.0 8.4
Conventional SC (T3-T4) 4.6 8.4 10.6 14.0
Tank mixes (T5-T6) 8.0 12.0 14.8 19.8

The field trial results shows that novel SC formulation provides better efficacy as compared to conventional SC and tank mixes when the dose was reduced from 1000 ml/h to 800 ml/h (i.e. 20%). The efficacy against brinjal jassid drops by 3.0, 4.8, 6.0, 8.4 at 3 DAA, 7 DAA, 10 DAA, 14 DAA respectively in novel SC formulation whereas it drops by 4.6, 8.4, 10.6, 14.0 at 3 DAA, 7 DAA, 10 DAA, 14 DAA respectively in conventional SC. We can conclude that novel SC formulation will helps the farmer by providing better efficacy as compared to conventional SC and tank mixes. The novel SC formulation performs better in comparison with conventional SC and tank mixes even at 20% dose reduction.

Experiment 3: Study of rain fastness properties of novel SC formulation
Crop & Variety : Cauliflower
Location : Durg, Chhattishgarh
Treatments : 4
Plot size : 100 sq.m.
Crop age : 60 days after transplanting.
Spray water volume : 500 liter per hectare
Method of Application: Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Agronomic Practices : All agronomic practices followed as per the crop requirement.
Methods for rain fastness study:
The treatment application (spraying) was done with knap sack sprayer by using 500 liter spray volume. After 60 minutes of spraying, artificial raining was done through overhead sprinkler system in trial plot for 30 minutes which was approximately equal to 10 mm of rainfall (measured by rain gauge). After 24 hrs. of artificial rain, the leaves were collected from treatment and put them into the PVC/plastic box. 20 larvae (3rd instar) of Spodoptera were release into the PVC box containing cauliflower leaves and larval mortality was observed on 72 hrs. The % larval control were calculated. Similar way, the cauliflower leaves were collected on 3rd, 7th, 10th and 14th day and spodoptera (3rd instar, 20 larvae) were released and allow to feed and % larval mortality were recorded after 72 hrs. The % larval control data further used to calculate synergism.

Table 5: Treatment details to study the rain fastness property of novel SC formulation
Treatment Number Treatment details with application Rate (gai/h)
T1 Tolfenpyrad 7.5%+Fipronil 3%+Abamectin 0.75% SC (Novel), 75+30+7.5 gai/h
T2 Tolfenpyrad 7.5%+Fipronil 3%+Abamectin 0.75% SC (Conventional), 75+30+7.5 gai/h
T3 Tolfenpyrad 15% SC+Fipronil 18.87% SC+Abamectin 1.9% EC, 75+30+7.5 gai/h (tank mix)
T4 UTC (Untreated Check)

Table 6a: Spodoptera litura larval control (%) on cauliflower.
Treatment Number Spodoptera litura larval control (%)
1 DAA 3 DAA 7 DAA 10 DAA 14 DAA
T1 100.0 100.0 96.2 90.0 84.8
T2 100.0 96.2 89.4 78.2 60.4
T3 98.2 93.4 84.6 70.6 52.6
T4 0.0 0.0 0.0 0.0 0.0

Table 6b: Spodoptera litura larval control (%) on cauliflower.
Treatment Number Increase in control (T1) over
1 DAA 3 DAA 7 DAA 10 DAA 14 DAA
T2 0.0 3.8 6.8 11.8 24.4
T3 1.8 6.6 11.6 19.4 32.2

The field trial results shows that novel SC formulation (T1) provides excellent rainfast properties by providing 3.8% (at 3 DAA), 6.8% (at 7 DAA), 11.8% (at 10 DAA) and 24.4% (at 14 DAA) higher larval control as compared to conventional SC (T2), and by providing 1.8% (at 1 DAA), 6.6% (at 3 DAA), 11.6% (at 7 DAA), 19.4% (at 10 DAA) and 32.2% (at 14 DAA) higher larval control as compared to tank mix treatments (T3). It can be concluded that novel SC formulation provides excellent rainfast properties as compared to conventional SC and tank mixes.
Experiment 4: Comparison of Novel SC formulation with other conventional formulation
Crop & Variety : Chilly,
Location : Durg, Chhattishgarh
Treatments : 4
Plot size : 50 sq.m.
Crop age : 80 days after transplanting.
Spray water volume : 520 liter per hectare
Method of Application: Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Agronomic Practices : All agronomic practices followed as per the crop requirement.
Observation Methods:
Thrips (Scirtothrips dorsalis) control (%): As given in Experiment 1.
Pod borer (Spodoptera exigua) larval control (%): Count the number of live larvae per plant at 3, 7, 10 and 14 DAA. Calculate larval control (%).
Table 7: Treatment details
Treatment Number Treatment details with application Rate (gai/h)
T1 Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Novel), 80+30+20 gai/h
T2 Tolfenpyrad 16%+Fipronil 6%+Fenpyroximate 4% WG, 80+30+20 gai/h
T3 Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% OD, 80+30+20 gai/h
T4 UTC (Untreated Check)

Table 8: Synergistic control of chilly thrips and pod borer larvae
Treatment Number Thrips control (%) Spodoptera larval control (%)
3 DAA 7 DAA 10 DAA 14 DAA 3 DAA 7 DAA 10 DAA 14 DAA
T1 99.0 92.6 85.8 77.2 100.0 98.4 92.2 88.6
T2 95.4 86.8 78.2 67.8 98.8 90.4 82.6 71.4
T3 96.4 88.4 80.4 69.6 99.6 93.4 85.0 77.6
T4 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

The field trial results shows that novel SC formulation provides higher efficacy and longer duration control of chilly thrips and pod borer larvae as compared to WG and OD formulation. This will helps the farmer to reduce the number of sprays.

Overall summery of field trials:
The field trials results shows many benefits/advantages of novel SC formulations of Tolfenpyrad+Fipronil+Insecticide as compared to their conventional SC, WG, OD formulation and tank mixes.
• Novel SC formulation shows synergism between Tolfenpyrad+Fipronil+Insecticide.
• Novel SC formulation shows strong synergism in comparison with their conventional SC, OD and WG formulations and tank mixes.
• Novel SC formulation provides longer residual control. The longer residual control experienced due to improved spreading properties of spray solution over leaf surface, increase in penetration in to the leaf surface.
• Protection against multiple insect pests i.e. thrips, mites and lepidopteran insects at a time
• Novel SC formulation helps to reduce the doses of active ingredients to get desirable insect control and thereby minimizing the pesticidal load into the environment.
• The improved rain fastness properties of novel SC formulation experienced due to better retention of spray solution over the waxy leaf surface.
• The novel SC formulations meets all the inhouse parameters of storage stability studies.

Spreading properties study:
Method: Spreading properties test conducted by preparing 1% solution (1 ml formulation in 100 ml water). Drop the solution on leaf surface and measure the spreading diameter (mm) after 30 seconds. Spreading diameter measured by graph paper.
Table 1: Spreading properties of Novel SC formulation of Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC

Treatments Room temperature storage
1 month 6 months 12 months
(Spreading diameter in mm)
Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Novel) 25 22 20
Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% SC (Conventional) 14 11 8
Tolfenpyrad 16%+Fipronil 6%+Fenpyroximate 4% WG (conventional) 6 4 3
Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% OD (Conventional) 10 8 4

The novel SC formulations of Tolfenpyrad 8%+Fipronil 3%+Fenpyroximate 2% shows excellent spreading properties. This helps to the bio-efficacy under field condition, ensures quick control of target insect-pests and also improves the rain-fast properties during rainy days.