Description:FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. TITLE OF THE INVENTION: “A spinosad and insecticide(s) wettable granule composition and process for preparation thereof”
2. APPLICANT:
(a) Name : RAJDHANI PETROCHEMICALS PRIVATE LIMITED
(b) Nationality : INDIAN
(c) Address : 6, LALITA COMPLEX, RASALA ROAD, NAVRANGPURA, AHMEDABAD-380009 Gujarat, India
PROVISIONAL
The following specification describes the invention. þ COMPLETE
The following specification particularly describes the invention and the manner in which it is to be performed.

FIELD OF INVENTION
The present invention relates to a spinosad and insecticide(s) wettable granule composition and process for preparation thereof. More specifically, the present invention relates to an insecticidal composition comprising bioactive amounts of spinosad or its agrochemically acceptable salts thereof, one or more compound selected from a group of insecticides, and agrochemically acceptable excipients; and a process for preparing said composition which is effective against lepidopteran, thysanopteran, dipteran and hemipteran insects and is stable in terms of stability, efficacy and being less prone to UV degradation of the active ingredient/s.

BACKGROUND OF THE INVENTION
Since the practice of agriculture began about 10,000 years ago in the fertile crescent of Mesopotamia, mankind has battled pests and diseases that threaten the sustainable food supply. Invertebrate pests and in particular insects, arachnids and nematodes destroy growing and harvested crops and attack wooden dwelling and commercial structures, thereby causing large economic loss to the food supply and to property. In the process of agricultural production, plant diseases and pests damage the roots, stems, leaves and other parts of plants, as well as fruit, seeds, tubers and other reproductive organs, so that the crop yield sharply reduces, and the quality drops seriously.
The first recorded use of pesticides is about 4500 years ago by Sumerians who used sulfur compounds to control insects and mites. The evolution of pesticides is classified into five single phases, namely, before 1000: early pest management; 1000–1850: use of plant, animal, or mineral derivatives; 1850–1940: use of inorganic products and industrial by-products; 1940–1970: use of synthetic organic compounds; 1970-present: use of lower-risk synthetic organic compounds. When organic chemistry was introduced to the pesticide science field after World War II, the door of industrial pesticide science was opened. In the past century, various kinds of pesticides have been launched throughout the world.
At present, in agricultural production, the application of pesticides is an important means to prevent and control plant diseases and insect pests. A lot of chemicals for control of crop diseases are used in cultivation of agricultural and horticultural crops. With the repeated use of a large number of existing pesticides and the improper application of pesticides by some farmers, there is a relatively large resistance to the existing common pesticides, and the difficulty of chemical control becomes increasingly greater.
Combining effective ingredients of different action mechanisms into a compound pesticide is an effective and quick way to deal with pest resistance problems. The compounding of different active ingredients that complement each other, can expand the control spectrum, comprehensively and effectively control pests and diseases, and become a popular application form in production practice. In particular, synergistic insecticides interact with each other so that the combined effect is better than the sum of the effects of the individual use effects. Therefore, in practical use, it can have a multiplier effect and is more favored by users.
The development and manufacture of effective, safe to humans, and environment-friendly pesticides has been a challenge to feed the growing population of our planet. The development of pesticides that pose a lower risk to natural enemies and useful organisms and are compatible with IPM (Integrated Pest Management) is also an important target. Moreover, due to public perception of chemical insecticides’ adverse effects and environmental safety, the commercialization and use of highly active and competitive microbial insecticides have gradually increased.
CN111616156A relates to an abamectin-spinosad nano suspending agent and a preparation method thereof, and belongs to the technical field of insecticide preparation.
CN104186479A relates to an insecticidal composition containing chlorantraniliprole and spinosad. In practical application, the insecticidal composition is prepared into one of water emulsions, micro-emulsions, suspensions, wettable powders or water-dispersible granules.
CN103918673A relates to an insecticidal composition containing a compound improved from chlorantraniliprole and a biological-source insecticide. The compositions comprise an active composition A and an active composition B, wherein the active composition A is the compound improved from chlorantraniliprole, and the active composition B is any one compound selected from avermectin, spinosad, spinetoram and emamectin benzoate.
However, some disadvantages of microbial insecticides include variable field performance, high production costs, short residual activity, and shelf life among others. Furthermore, ultraviolet (UV) spectrum from solar radiation inactivates most microbial insecticides. In general, direct exposure of microbial insecticides to solar radiation negatively affects viability and infectivity, mainly due to DNA denaturation and/or generation of highly reactive oxygen radicals. Solar radiation, primarily in the ultraviolet (UV) portion (300 – 400 nm) causes both mutagenic and lethal changes in nucleic acids. The main consequence of UV action is the formation of a dimer from adjacent pyrimidines on the same strand, which become unstable (may transfer most of its extra energy by collision to an adjacent molecule) and reactive (formation of new bonds). Thus, the alteration of the DNA blocks its replication, and causes the death of the microorganism. Therefore, solar radiation has been the responsible for the rapid loss of activity of Bacillus thuringiensis, baculoviruses, microsporidia, and fungi products among many crops. UV inactivation is especially true when microbial are sprayed on foliage. Using aerial application, more pathogens are exposed to UV (on top of leaf surface), whereas using ground application, much entomopathogens are deposited underside of leaves and are less exposed to UV. Since UV radiation is always an important inactivating factor for entomopathogenic microorganisms in field, there are many research groups working to improve residual activity after application. The use of adjuvants or improved formulations can address UV inactivation.
Indian Patent No. 356584 relates to natural origin insecticidal composition containing UV photodegradation arrester.
However, for the reasons such as insufficient control efficacy, restriction of its use due to the development of resistance in insects against insecticides, phytotoxicity and contamination to plants, or toxicity to human beings, beasts, fishes and the like, many of them cannot be said to be satisfactory control chemicals. There are many different formulations possible as well. Wettable granule (WG) formulations can be difficult to apply in a uniform and even manner. Generally WG formulation has poor spreading properties as compared to liquid formulations like suspension concentrate (SC), suspo-emulsion (SE), soluble concentrate (SL), etc.
Hence, there is still a need for a novel, stable, safer, high potential, synergistic broad spectrum composition with better spreading properties, which exhibits least photo degradation of the active ingredient and less residue leading to least chemical environmental pollution.
The preceding discussion of the background art is intended to facilitate an understanding of the present invention only. The discussion is not an acknowledgement or admission that any of the material referred to is or was part of the common general knowledge as at the priority date of the application.

OBJECT OF THE INVENTION
The principal object of the present invention is to provide a spinosad and insecticide(s) wettable granule composition and process for preparation thereof.
Another object of the present invention is to provide a pesticidal composition comprising bioactive amounts of spinosad or its agrochemically acceptable salts thereof, one or more compound selected from a group of insecticides, UV photo degradation arrester, wetting-spreading-penetrating agent, and agrochemically acceptable excipients; and a process for preparing said composition.
Another object of the present invention is to provide a pesticidal composition that is stable in terms of stability, efficacy and being less prone to UV degradation of the active ingredient/s.
Another object of the present invention is to provide a pesticidal composition which provides residual control of insect-pests due to enhanced stability.
Yet another object of the present invention is to provide a pesticidal composition which provides broad spectrum of activities, i.e. effective against lepidopteran, thysanopteran, dipteran and hemipteran insects.
Yet another object of the present invention is to provide a pesticidal composition that has improved leaf penetration of spray droplets, retarded evaporation loss and enhanced absorption of active ingredients.
Yet another object of the present invention is to provide a pesticidal composition that has synergism in terms of bioefficacy.
Further object of the present invention is to provide a pesticidal composition that has increased spreading properties on leaf surfaces and better wetting of waxy leaf surfaces.
Further object of the present invention is to provide a pesticidal composition that has improved rainfast properties.
Further object of the present invention is to provide a process for preparing a stable and non-phytotoxic composition.
Further object of the present invention is to provide a pesticidal composition that is safe to the crops, environment and applicator.

SUMMARY OF THE INVENTION
In light of the foregoing background, the following presents a simplified summary of the present disclosure in order to provide a basic understanding of some aspects of the disclosure. This summary is not an extensive overview of the disclosure. It is not intended to delineate the scope of the disclosure. The following summary merely presents some concepts of the disclosure in a simplified form as a prelude to the more detailed description provided below.
The present invention provides a synergistic pesticidal composition comprising bioactive amounts of spinosad or its agrochemically acceptable salts thereof, one or more compound selected from a group of insecticides, UV photo degradation arrester, wetting-spreading-penetrating agent, and agrochemically acceptable excipients; and a process for preparing said composition. In practical application, the pesticidal composition is prepared as wettable granule (WG).
The process for preparing the present spinosad and insecticide(s) wettable granule formulation can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However, all such variation and modification is still covered by the scope of present invention.
The present invention provides spinosad composition that has synergism in terms of bioefficacy, is effective against lepidopteran, thysanopteran, dipteran and hemipteran insects, is stable in terms of stability, efficacy and being less prone to UV degradation of the active ingredient, has residual control of insect-pests due to enhanced stability, has improved leaf penetration of spray droplets, retarded evaporation loss and enhanced absorption of active ingredients, has increased spreading properties on leaf surfaces, better wetting of waxy leaf surfaces, improved rainfastness properties, and is safe to the crops, environment and applicator.
DETAILED DESCRIPTION OF THE INVENTION
Before explaining the present invention in detail, it is to be understood that the invention is not limited in its application to the details of the parts illustrated. The invention is capable of other embodiments, as described above and of being practiced or carried out in a variety of ways. It is to be understood that the phraseology and terminology employed herein is for the purpose of description and not to limitation. The invention may have various embodiments and they may be performed as described in the following pages of the complete specification.
The terms and words used in the following description are not limited to the bibliographical meanings, but, are merely used by the inventors to enable a clear and consistent understanding of the invention. Accordingly, it should be apparent to those skilled in the art that the following description of exemplary embodiments of the present invention are provided for illustration purpose only and not for the purpose of limiting the scope of the invention.
It is to be understood that the singular forms "a", "an", and "the" include plural reference unless the context clearly dictates otherwise.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used in this specification is taken to specify the presence of stated features, steps or components but does not preclude the presence or addition of one or more other features, steps, components or groups thereof.
"Bioactive amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.
As used herein, “weight percent”, “wt-%”, “percent by weight”, “% by weight”, and variations thereof refer to the concentration of a substance as the weight of that substance divided by the total weight of the composition and multiplied by 100. It is understood that, as used here, “percent”, “%”, and the like are intended to be synonymous with “weight percent”, “wt-%”, etc.
The term "insects" as used herein, includes all organisms in the class "Insecta".
The term "animal pest" includes arthropods, gastropods, and nematodes. Preferred animal pests according to the invention are arthropods, preferably insects and arachnids, in particular insects. Insects, which are of particular relevance for crops, are typically referred to as crop insect pests.
The term "pesticidal" as used herein, refers to the ability of a pesticide to increase mortality or inhibit growth rate of pests.
The term "insecticidal" as used herein, refers to the ability of a insecticide to increase mortality or inhibit growth rate of insects.
To "control" or "controlling" pests means to inhibit, through a toxic effect, the ability of pests to survive, grow, feed, and/or reproduce, or to limit pest related damage or loss in crop plants. To "control" pests may or may not mean killing the pests, although it preferably means killing the pests.
The term 'plants' as used herein, refers to all physical parts of a plant, including seeds, seedlings, saplings, roots, tubers, stems, stalks, foliage and fruits. The term "plant" is to be understood as including wild type plants and plants, which have been modified by either conventional breeding, or mutagenesis or genetic engineering, or by a combination thereof.
The term "crop" refers to both, growing and harvested crops.
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 soybean (resistant to lepidopteran and coleopteran pests). 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 flavor).
The present invention provides a spinosad and insecticide(s) wettable granule composition comprising 3 to 50% w/w spinosad or its agrochemically acceptable salts, 1 to 50% w/w one or more insecticides from various groups, 0.5 to 2.5% w/w UV photo degradation arrester, 1.5 to 6% w/w wetting-spreading-penetrating agent, and agrochemically acceptable excipients.
Spinosad is a mixture of spinosyn A and spinosyn D, two naturally occurring metabolites from the soil bacterium, Saccharopolyspora spinosa. The chemical structures of spinosyn A [2- ((6- Deoxy-2, 3, 4 –tri –O –methyl –a –L -mannopyranosyl) oxy)-13- ((5-(dimethylamino) tetrahydro -6- methyl -2H –pyran -2- yl) oxy)-9-ethyl-2,3,3a,5a,5b,6,9,10,11,12,13,14,16a,16b- tetradecahydro-14-methyl-1H-as- indaceno(3,2-d)oxacyclododecin-7,15- dione] and spinosyn D [2-((6-Deoxy-2,3,4-tri-O-methyl-a-L-mannopyranosyl)oxy)-13-((5-(dimethylamino)tetrahydro-6-methyl-2H-pyran-2-yl) oxy)-9-ethyl-2,3,3a,5a,5b,6,9,10,11,12,13,14,16a,16b- tetradecahydro-4, 14-dimethyl-1H- as-indaceno(3,2-d)oxacyclododecin-7,15-dione] are as follows.

Spinosad is a broad-spectrum insecticide used to control Lepidoptera larvae (caterpillars), Diptera (flies), Thysanoptera (thrips), Coleoptera (beetles) and many other crop-damaging pests. It is registered for use in over 82 countries for more than 250 crops encompassing most of the crop groupings such as row crops, e.g. cotton, soybean, rice; tree fruits, e.g. pome, stone and citrus; tree nuts e.g. walnut, almond; small fruits, e.g. grape, strawberry; leafy and brassica vegetables, e.g. lettuce, cole crop; fruiting vegetables, e.g. tomato, pepper; curcurbits, e.g. cucumber, melon; bulb, root and tuber vegetables, e.g. onion, carrot, potato; legumes, e.g. dry and succulent peas and beans; forages, e.g. alfalfa, forage grasses and pastures; other; e.g. coffee, tea, plantation, turf, trees, and ornamentals in nurseries and greenhouses, and commercial aquatic plants, control of fire ants, and stored grains. It is stable at typical use and storage temperatures. It has contact activity on virtually all life stages of a pest including egg, larvae and adult. Eggs must be sprayed directly but larvae and adults can be effectively dosed through contact with treated surfaces. Spinosad is most effective when eaten by insect pests. Foliar formulations of spinosad are not highly systemic; however, translaminar activity is evident in some crops. In general, more movement and penetration is seen with younger and rapidly growing leaves. Limited root uptake may also occur under certain conditions and environments. Spinosad residue on plant foliage appears to be harmless to foraging honeybees once dry and has minimal impact on most other beneficial insects.
One or more insecticide(s) is selected from emamectin benzoate, abamectin, indoxacarb, methoxyfenozide, tebufenozide, chromafenozide, broflanilide, cyproflanilide, fluxametamide, isocycloseram, afoxolaner, esafoxolaner, fluralaner, lotilaner, sarolaner, chlorantraniliprole, cyantraniliprole, cyclaniliprole, tetraniliprole, tetrachlorantraniliprole, tyclopyrazoflor, cyhalodiamide, flubendiamide, fluchlordiniliprole, tiorantraniliprole, dichloromezotiaz, fenmezoditiaz, lambda cyhalothrin, bifenthrin, clothianidin, thiamethoxam, fipronil, profenofos, diafenthiuron, flonicamid, fenpyroximate, hexythiazox, etoxazole and cyenopyrafen.
Spinosad, abamectin and emamectin benzoate are fermentation products. Factors affecting UV radiation include geographical location, season, and time of the day. The sun’s rays are strongest at the equator, where the sun is most directly overhead and UV rays travel the least distance through the atmosphere. Ozone also is naturally thinner in the tropics compared to the mid- and high-latitudes, so there is less ozone to absorb the UV radiation as it passes through the atmosphere. Addition of UV photo degradation arrester helps in preventing further degradation of products. The UV photo degradation arrester that also acts as stability enhancer is selected from, but not limited to, zinc oxide and titanium dioxide.
The super wetting-spreading-penetrating agents used in wettable granule formulations is selected from, but not limited to, organic silicone, which includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxane heptamethyl, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, or mixture thereof. The organosilicone agents have super ability of spreading by drastically reducing the water surface tension. These enhance wetting and absorption of active ingredient through stomatal penetration. This will improve a spray application by modifying the wetting and spreading characteristics, the result being a more uniform spray deposit even at reduced spray volume. It also ensures thorough coverage without excessive runoff of the spray. It makes the water surface tension lower down. They are safe to the human beings and environment. The most preferred super wetting-spreading-penetrating agent is polyalkyleneoxide modified heptamethyl trisiloxane.
The present invention further comprises agrochemically acceptable excipients including, but not limited to, dispersing agents, anti-foaming agents, carriers, humectants, binding agents, and anti-caking agents.
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 dispersants used herein include but not limited to sodium polycarboxylate (sodium polyacrylate), naphthalene sulfonic acid, sodium salt condensates with formaldehyde, polyalcoxylated alkylphenol, naphthalene sulfonic acid formaldehyde condensate, methyl naphthalene-formaldehyde-condensate sodium salt, naphthalene condensates, lignosulfonates, calcium lignosulfonate, sodium lignosulfonate, sodium alkyl naphthalene sulfonate, sodium lignosulfonate-sulfomethylated. Dispersant can be used in the range of 5 to 20% w/w of the composition. The preferred dispersing agents are sodium lignosulfonate, sodium alkyl naphthalene sulfonate, sodium lignosulfonate-sulfomethylated. These provide excellent wetting, dispersing, hydrotroping and medium to low foaming, and offer acid and base stability, hard water tolerance and high temperature stability.
Water-based formulations often cause foam during mixing operations in production. In order to reduce the tendency to foam, anti-foam agents are often added either during the production stage or before filling into bottles. The function of the anti-foam agent is to displace the surfactant from the air-water interface. Anti-foaming agent as used herein can be selected from the group comprising of silicone emulsion, perfluoroalkylphosphonic acids, perfluoroalkylphosphinic acids and perfluoroaliphatic polymeric esters or mixtures thereof. Anti-foaming agent can be used in the range of 0.25 to 1% w/w of the composition. The preferred antifoaming agent is polydimethylsiloxane.
Carrier denotes a natural or synthetic, organic or inorganic material with which the active substance is combined in order to facilitate its application to the plant, to the seeds or to the soil. It is generally inert, and it must be agriculturally acceptable, in particular to the plant being treated. The carrier is selected from, but not limited to clay, silica, lactose monohydrate, sodium sulfate anhydrous, corn starch, urea, EDTA, urea formaldehyde resin, diatomaceous earth, kaolin, bentonite, kieselguhr, fuller's earth, attapulgite clay, bole, loess, talc, chalk, dolomite, limestone, lime, calcium carbonate, powdered magnesia, magnesium oxide, magnesium sulphate, sodium chloride, gypsum, calcium sulphate, pyrophyllite, silicates and silica gels; fertilizers such as, for example, ammonium sulphate, ammonium phosphate, ammonium nitrate and urea; natural products of vegetable origin such as, for example, grain meals and flours, bark meals, wood meals, nutshell meals and cellulosic powders; and synthetic polymeric materials such as, for example, ground or powdered plastics and resins, bentonites, zeolites, titanium dioxide, iron oxides and hydroxides, aluminium oxides and hydroxides, or organic materials such as bagasse, charcoal, or synthetic organic polymers. Carrier can be used in the range to 30 to 70% w/w of the composition.
Suitable humectant is selected from, but not limited to humic acid, glycerol, lactose, and sodium sulphate anhydrous. Humectants can be used in the range to 1 to 10% w/w of the composition.
The binding agent used herein includes, but not limited to, sucrose, synthetic and natural gums, synthetic polymers such as poly vinyl acetate, cellulose derivatives-methyl cellulose, EOPO (Ethylene oxide/propylene oxide, polyethylene glycols, polyethylene oxide, polyethoxylated fatty acids or alcohols, sorbitol or urea. Binding agent can be used in the range to 0.5 to 2% w/w of the composition.
The anti-caking agent used herein includes, but not limited to, amorphous silica, sodium or ammonium phosphates, sodium carbonate/bicarbonate, sodium acetate, sodium metasilicate, magnesium or zinc sulfates, magnesium hydroxide, sodium alkylsulfosuccinates. Anti-caking agent can be used in the range to 0.2 to 1% w/w of the composition.
However, those skilled in the art will appreciate that it is possible to utilize additional agrochemically acceptable excipients without departing from the scope of the present invention. Such agrochemically acceptable excipients can be in the range from 40% to 90% of the total weight of the composition.
In practical application, the pesticidal composition is formulated as wettable granule (WG) by addition of organosilicone as a wetting agent which improves spreading and penetrating properties.

The process for preparing wettable granule (WG) formulation comprises following steps:
a) 3% to 50% w/w spinosad and 1% to 50% w/w one or more insecticide(s) are taken in a blender,
b) 0.5% to 2.5% w/w UV photo degradation arrester, 1.5% to 6% w/w wetting-spreading-penetrating agent, 5% to 20% w/w dispersing agent, 0.25% to 1% w/w anti-foaming agent, 30% to 70% w/w carrier, 1% to 10% w/w humectants, 0.5% to 2% w/w binding agent, and 0.2% to 1% w/w anti-caking agent are added in to step a) and mixed till its complete homogenization,
c) said homogenized mixture of step b) is milled till required wet sieve and post blended again for homogeneity,
d) homogenous material obtained in step c) is passed through extruder for granulation,
e) above prepared granules in step d) are passed through fluid bed dryer to remove excess moisture,
f) after moisture removal, the prepared granules are transferred to vibro shifter,
g) final material is collected from the vibro shifter.
The process for preparing the present synergistic composition can be modified accordingly by any person skilled in the art based on the knowledge of manufacturing the formulation. However, all such variation and modification is still covered by the scope of present invention.

Table 1: Most preferred composition (spinosad + insecticide) and formulations thereof for the present invention
spinosad insecticide active ingredients (%) Formulation Strength (%) Formulation Type
spinosad Insecticide
Spinosad Emamectin benzoate 16 3 19.00 WG
Spinosad Abamectin 16 3 19.00 WG
Spinosad Indoxacarb 16 16 32.00 WG
Spinosad Methoxyfenozide 8 24 32.00 WG
Spinosad Tebufenozide 8 24 32.00 WG
Spinosad Chromafenozide 16 24 40.00 WG
Spinosad Broflanilide 40 8 48.00 WG
Spinosad Cyproflanilide 40 10 50.00 WG
Spinosad Fluxametamide 16 12 28.00 WG
Spinosad Isocycloseram 20 25 45.00 WG
Spinosad Fluralaner 20 10 30.00 WG
Spinosad Chlorantraniliprole 30 12 42.00 WG
Spinosad Cyantraniliprole 22.5 22.5 45.00 WG
Spinosad Cyclaniliprole 30 20 50.00 WG
Spinosad Tetraniliprole 30 20 50.00 WG
Spinosad Tetrachlorantraniliprole 30 20 50.00 WG
Spinosad Tyclopyrazoflor 30 20 50.00 WG
Spinosad Cyhalodiamide 30 20 50.00 WG
Spinosad Flubendiamide 30 13.33 43.33 WG
Spinosad Tolfenpyrad 10 20 30.00 WG
Spinosad Dichloromezotiaz 10 12 22.00 WG
Spinosad Lambda cyhalothrin 22.5 10 32.50 WG
Spinosad Bifenthrin 22.5 20 42.50 WG
Spinosad Clothianidin 22.5 20 42.50 WG
Spinosad Thiamethoxam 22.5 20 42.50 WG
Spinosad Dinotefuran 22.5 10 32.50 WG
Spinosad Fipronil 30 30 60.00 WG
Spinosad Profenofos 3.6 36 39.60 WG
Spinosad Flonicamid 22.5 25 47.50 WG
Spinosad Fenpyroximate 26.67 10 36.67 WG
Spinosad Hexythiazox 13.3 5 18.30 WG
Spinosad Etoxazole 26.67 20 46.67 WG
Spinosad Cyenopyrafen 13.3 15 28.30 WG

Table 2: Most preferred composition (spinosad + insecticide + insecticide) and formulations thereof for the present invention
Spinosad Insecticide 1 Insecticide 2 active ingredients (%) Formulation Strength (%) Formulation Type
Spinosad Insecticide 1 Insecticide 2
Spinosad Abamectin Chlorantraniliprole 24 4.8 12 40.80 WG
Spinosad Abamectin Cyantraniliprole 24 4.8 30 58.80 WG
Spinosad Abamectin Tetraniliprole 24 4.8 20 48.80 WG
Spinosad Abamectin Cyclaniliprole 24 4.8 20 48.80 WG
Spinosad Abamectin Broflanilide 48 9.6 9.6 67.20 WG
Spinosad Abamectin Tolfenpyrad 12 2.4 30 44.40 WG
Spinosad Abamectin Fluxametamide 24 4.8 20 48.80 WG
Spinosad Abamectin Methoxyfenozide 12 2.4 40 54.40 WG
Spinosad Emamectin benzoate Chlorantraniliprole 24 4.8 12 40.80 WG
Spinosad Emamectin benzoate Cyantraniliprole 24 4.8 30 58.80 WG
Spinosad Emamectin benzoate Tetraniliprole 24 4.8 20 48.80 WG
Spinosad Emamectin benzoate Cyclaniliprole 24 4.8 20 48.80 WG
Spinosad Emamectin benzoate Broflanilide 48 9.6 9.6 67.20 WG
Spinosad Emamectin benzoate Tolfenpyrad 12 2.4 30 44.40 WG
Spinosad Emamectin benzoate Fluxametamide 24 4.8 20 48.80 WG
Spinosad Emamectin benzoate Methoxyfenozide 12 2.4 40 54.40 WG
Spinosad Tolfenpyrad Chlorantraniliprole 12 30 6 48.00 WG
Spinosad Tolfenpyrad Cyantraniliprole 12 30 15 57.00 WG
Spinosad Tolfenpyrad Tetraniliprole 12 30 10 52.00 WG
Spinosad Tolfenpyrad Cyclaniliprole 12 30 10 52.00 WG
Spinosad Tolfenpyrad Broflanilide 12 30 2.4 44.40 WG
Spinosad Tolfenpyrad Fluxametamide 12 30 10 52.00 WG
Spinosad Tolfenpyrad Methoxyfenozide 6 15 20 41.00 WG
Spinosad Fluxametamide Chlorantraniliprole 12 10 6 28.00 WG
Spinosad Fluxametamide Cyantraniliprole 12 10 15 37.00 WG
Spinosad Fluxametamide Tetraniliprole 12 10 10 32.00 WG
Spinosad Fluxametamide Cyclaniliprole 12 10 10 32.00 WG
Spinosad Fluxametamide Broflanilide 12 10 2.4 24.40 WG
Spinosad Fluxametamide Methoxyfenozide 6 5 20 31.00 WG
Spinosad Diafenthiuron Chlorantraniliprole 3 18 1.5 22.50 WG
Spinosad Diafenthiuron Cyantraniliprole 3 18 3.75 24.75 WG
Spinosad Diafenthiuron Tetraniliprole 3 18 2.5 23.50 WG
Spinosad Diafenthiuron Cyclaniliprole 3 18 2.5 23.50 WG
Spinosad Diafenthiuron Broflanilide 3 18 0.6 21.60 WG
Spinosad Diafenthiuron Methoxyfenozide 3 18 10 31.00 WG

The amount of a composition according to the invention to be applied, will depend on various factors, such as the subject of the treatment, such as, for example plants, soil or seeds; the type of treatment, such as, for example spraying, dusting or seed dressing; the purpose of the treatment, such as, for example prophylactic or therapeutic control; in case of insect control, the type of insects or mites to be controlled or the application time. This amount of the composition of the present invention to be applied can be readily deduced by a skilled agronomist.
Application to the seeds is carried out before sowing, either directly on the seeds or after having pregerminated the latter. Suitable application methods include inter alia soil treatment, seed treatment, in furrow application, and foliar application. Soil treatment methods include drenching the soil, drip irrigation (drip application onto the soil), dipping roots, tubers or bulbs, or soil injection. Seed treatment techniques include seed dressing, seed coating, seed dusting, seed soaking, and seed pelleting. In furrow applications typically include the steps of making a furrow in cultivated land, seeding the furrow with seeds, applying the pesticidally active composition to the furrow, and closing the furrow. Foliar application refers to the application of the pesticidally active composition to plant foliage, e.g. through spray equipment.
The rates of application vary within wide limits and depend on the nature of the soil, the method of application, the crop plant, the pest to be controlled, the prevailing climatic conditions, and other factors governed by the method of application, the time of application and the target crop.
The present invention is suitable for use in protecting crops, plants, plant propagation materials, such as seeds, or sailor water, in which the plants are growing, from attack or infestation by animal pests. Therefore, the present invention also relates to a plant protection method, which comprises contacting crops, plants, plant propagation materials, such as seeds, or soil or water, in which the plants are growing, to be protected from attack or infestation by animal pests, with a pesticidally effective amount of the present invention.
Examples of the crops on which the present compositions is used or applied 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). 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.
The present invention is also suitable for use in combating or controlling animal pests. Therefore, the present invention also relates to a method of combating or controlling animal pests, which comprises contacting the animal pests, their habitat, breeding ground, or food supply, or the crops, plants, plant propagation materials, such as seeds, or soil, or the area, material or environment in which the animal pests grow, with a pesticidally effective amount of the present invention.
The present invention is used to control the following insects-pests. The major insects pests belong 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.); to the order Lepidoptera, army worm (Mythimna unipuncta), asiatic rice borer (Chilo suppressalis), beet armyworm (Spodoptera exigua), fall armyworm (Spodoptera frugiperda), 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 medinali), 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 separate), cotton pinkbollworm (Pectinophora gossypiella), citrus leafminer (Phyllocnistis citrella), cabbage butterfly (Pieris brassicae), diamond backmoth (Plutella xylostella), paddy stem borer (Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata), wheat stem borer (Sesamia inferens, Sitotroga cerealella, Spilosoma oblique), fall armyworm (Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Trichoplusia ni, Tryporyza nivella, Tryporyza incertulas, Tuta absoluta); to 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, Epilachna varivestis), various species of white grubs are (Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotreta chrysocephala, Popillia japonica) etc; to the order Orthoptera, for example, Gryllotalpa spp., Locusta spp., and Schistocerca is spp.; to 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; to the order Heteroptera, for example, Dysdercus spp., Leptocorisa spp., to the order Hymenoptera, for example, Solenopsis spp.; to the order Diptera, for example, Antherigona soccata, Dacus spp., Liriomyza spp., Melanagromyza spp., to 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, and Tetranychus cinnabarinus.
The composition 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 composition of the present invention.
Benefits of the present invention include synergism in terms of bioefficacy, broad spectrum of activities, i.e. effective against lepidopteran, thysanopteran, dipteran and hemipteran insects, stable in terms of stability, efficacy and being less prone to UV degradation of the active ingredient, residual control of insect-pests due to enhanced stability, improved leaf penetration of spray droplets, retarded evaporation loss and enhanced absorption of active ingredients, increased spreading properties on leaf surfaces, better wetting of waxy leaf surfaces, improved rainfast properties, and safe to the crops, environment and applicator.
The invention is illustrated more in detail in the following examples. The examples describe and demonstrate embodiments within the scope of the present invention. These examples are given solely for the purpose of illustration and are not to be construed as limitations of the present invention, as many variations thereof are possible without departing from the spirit and scope of the invention.
EXAMPLES
Example 1
Spinosad 16%, Emamectin benzoate 3%, WG formulation with zinc oxide 1%
Ingredients Percent (w/w)
Spinosad a.i. 16.00 15.20 16.80
Emamectin benzoate a.i. 3.00 2.85 3.30
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.00
Sodium polyacrylate (dispersing agent II) 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 3.00
Zinc oxide (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00
Urea formaldehyde resin (carrier) 15.00
China clay (carrier) 46.50
Total 100.00

Procedure:
a) Spinosad and one or more insecticide/s (here, emamectin benzoate) were taken in a blender,
b) UV photo degradation arrestor, wetting-spreading-penetrating agent, dispersing agent, anti-foaming agent, carrier, humectants, binding agent, and anti-caking agent (here, zinc oxide, polyalkyleneoxide modified heptamethyltrisiloxane, alkyl naphthalene sulfonate, sodium salt, sodium polyacrylate, polydimethyl siloxane, sodium sulphate anhydrous, urea formaldehyde resin, and china clay) were added to step a) and mixed till its complete homogenization,
c) homogenized mixture of step b) was milled till required wet sieve and was post blended again for homogeneity,
d) homogenous material obtained in step c) was passed through extruder for granulation,
e) above prepared granules in step d) were passed through fluid bed dryer to remove excess moisture,
f) after moisture removal, the prepared granules were transferred to vibro shifter,
g) final material was collected from the vibro shifter.

Example 2
Spinosad 16%, Emamectin benzoate 3%, WG formulation with titanium oxide 1%
Ingredients Percent (w/w)
Spinosad a.i. 16.00
Emamectin benzoate a.i. 3.00
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.00
Sodium polyacrylate (dispersing agent II) 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 3.00
Titanium dioxide (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00
Urea formaldehyde resin (carrier) 15.00
China Clay (carrier) 46.50
Total 100.00

Procedure: as per Example 1

Example 3
Spinosad 16%, Emamectin benzoate 3%, WG formulation with kojic acid 1%
Ingredients Percent (w/w)
Spinosad a.i. 16.00
Emamectin benzoate a.i. 3.00
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.00
Sodium polyacrylate (dispersing agent II) 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 3.00
kojic acid (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00
Urea formaldehyde resin (carrier) 15.00
China Clay (carrier) 46.50
Total 100.00

Procedure: as per Example 1

Example 4
Spinosad 16%, Emamectin benzoate 3%, WG formulation without UV photo degradation arrestor (conventional)
Ingredients Percent (w/w)
Spinosad a.i. 16.00
Emamectin benzoate a.i. 3.00
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.00
Sodium polyacrylate (dispersing agent II) 6.00
Sodium Lauryl sulfate (wetting agent) 3.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00
Urea formaldehyde resin (carrier) 15.00
China Clay (carrier) 47.50
Total 100.00
Procedure: as per Example 1

Example 5
Spinosad 22.5%, Cyantraniliprole 22.5%, WG formulations with different concentration of super wetting-spreading-penetrating agent
Ingredients Formulations
SPCY-WG-1 SPCY-WG-2 SPCY-WG-3 SPCY-WG-4
Percent (w/w)
Spinosad a.i. 22.50 22.50 22.50 22.50
Cyantraniliprole a.i. 22.50 22.50 22.50 22.50
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.50 3.50 3.50 3.50
Sodium polyacrylate (dispersing agent II) 6.00 6.00 6.00 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 2.00 3.00 4.00 5.00
Zinc oxide (UV photo degradation arrestor) 1.00 1.00 1.00 1.00
Polydimethyl siloxane (antifoaming agent) 0.50 0.50 0.50 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00 6.00 6.00 6.00
Urea formaldehyde resin (carrier) 15.00 15.00 15.00 15.00
China Clay (carrier) 21.00 20.00 19.00 18.00
Total 100.00 100.00 100.00 100.00

Procedure: as per Example 1

Example 6
Spinosad 22.5%, Cyantraniliprole 22.5%, WG (SPCY-5-conventional)
Ingredients Percent (w/w)
Spinosad a.i. 22.50
Cyantraniliprole a.i. 22.50
Alkyl naphthalene sulfonate, sodium salt (dispersing agent I) 3.50
Sodium polyacrylate (dispersing agent II) 6.00
Sodium Lauryl sulfate (wetting agent) 4.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 6.00
Urea formaldehyde resin (carrier) 15.00
China Clay (carrier) 20.00
Total 100.00

Procedure: as per Example 1

Example 7
Spinosad 20%+Chlorantraniliprole 15% WG
Ingredients Percent (w/w)
Spinosad a.i. 20.00
Chlorantraniliprole a.i. 15.00
Sodium Alkyl naphthalene sulfonate (dispersing agent) 0.50
Sodium lignosulfonate (dispersing agent) 3.00
Sodium lignosulfonate, sulfomethylated (dispersing agent) 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 3.00
Zinc oxide (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Amorphous silica (anti caking agent) 0.50
Sucrose (binding agent) 1.00
Clay (carrier) 8.00
Lactos monohydrate (carrier) 41.50
Total 100.00

Procedure: as per Example 1

Example 8
Composition of Spinosad 16%+Abamectin 3% WG (SA-WG-190)
Ingredients Percent (w/w)
Spinosad a.i. 16.00
Abamectin a.i. 3.00
Sodium lignosulfonate (dispersing agent I) 5.00
Sodium polyacrylate (dispersing agent II) 7.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 3.00
Titanium dioxide (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 4.00
Sucrose (binding agent) 1.00
Amorphous silica (anti caking agent) 0.50
Lactose monohydrate (carrier) 10.00
China Clay (carrier) 49.00
Total 100.00

Procedure: as per Example 1

Example 9
Composition of Spinosad 10%+Tolfenpyrad 20% WG
Ingredients Percent (w/w)
Spinosad a.i. 10.00
Tolfenpyrad a.i. 20.00
Sodium lignosulfonate (dispersing agent I) 3.00
Sodium polyacrylate (dispersing agent II) 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 4.00
Titanium dioxide (UV photo degradation arrestor) 1.00
Polydimethyl siloxane (antifoaming agent) 0.50
Sodium sulphate anhydrous (carrier cum humectant) 4.00
Sucrose (binding agent) 1.00
Amorphous silica (anti caking agent) 0.50
Lactose monohydrate (carrier) 10.00
China Clay (carrier) 40.00
Total 100.00

Active ingredients purity on 100% basis

Procedure: as per Example 1
Example 10
Composition of Spinosad 24%+Abamectin 4.8%+Chlorantraniliprole 12% WG
Ingredients Percent (w/w)
Spinosad a.i. 24.00
Abamectin a.i. 4.80
Chlorantraniliprole a.i. 12.00
Sodium Alkyl naphthalene sulfonate 0.50
Sodium lignosulfonate 3.00
Sodium lignosulfonate, sulfomethylated 6.00
Polyalkyleneoxide modified heptamethyltrisiloxane (super wetting-spreading-penetrating agent) 5.00
Titanium oxide (UV photo degradation arrestor) 2.50
Amorphous silica 0.50
Sucrose 1.00
Clay 8.00
Lactose monohydrate 32.70
Total 100.00

Active ingredients purity on 100% basis

Procedure: as per Example 1

Example 11
Storage stability study of Example 1
Laboratory storage stability of Example 1 for 14 days
Parameters Specification (in house) Initial At 54±20C At 0±20C
Spinosad content percent by mass 15.20 to 16.80 16.25 16.10 16.22
Emamectin benzoate contnet percent by mass 2.85 to 3.30 3.15 3.08 3.13
Spinosad suspensibility percent min. 70 97.75 95.02 97.52
Emamectin benzoate suspensibility percent min. 70 95.36 94.15 94.56
pH range (1% aq. Suspension) 6.5 to 8.5 7.5 7.6 7.5
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.5 0.5 0.5
moisture content percent by mass max. max. 3% 2.5 2.6 2.5

Room temperature storage stability of Example 1 up to 12 months
Parameters Specification (in house) 1 month 6 months 12 months
Spinosad content percent by mass 15.20 to 16.80 16.50 16.40 16.22
Emamectin benzoate contnet percent by mass 2.85 to 3.30 3.18 3.10 3.08
Spinosad suspensibility percent min. 70 97.90 97.70 97.52
Emamectin benzoate suspensibility percent min. 70 95.36 94.15 94.56
pH range (1% aq. Suspension) 6.5 to 8.5 7.5 7.5 7.55
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.5 0.5 0.5
moisture content percent by mass max. max. 3% 2.5 2.5 2.5

Example 12
Storage stability study of Example 2
Conclusion:
Spinosad 16%+Emamectin benzoate 3% WG meets all in-house specifications for storage stability parameters i.e. active ingredients, suspensibility, pH, wettability, wet sieve, bulk density and moisture content in laboratory (at 54±20C & At 0±20C for 14 days) and room temperature (for 12 months).

Example 13
Storage stability study of Example 3
Conclusion:
Spinosad 16%+Emamectin benzoate 3% WG meets all the in-house specifications for storage stability parameters i.e. active ingredients, suspensibility, pH, wettability, wet sieve, bulk density and moisture content in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Example 14
Storage stability study of Example 8
Spinosad 16%+Abamectin 3% WG meets all the in-house specifications for storage stability parameters i.e. active ingredients, suspensibility, pH, wettability, wet sieve, bulk density and moisture content in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Example 15
Storage stability study of Example 9
The composition of Spinosad 10%+Tolfenpyrad 20% WG meets all the in-house specifications for storage stability parameters i.e. active ingredients, suspensibility, pH, wettability, wet sieve, bulk density and moisture content in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Example 16
Storage stability study of Example 10
The composition of Spinosad 24%+Abamectin 4.8%+Chlorantraniliprole 12% WG meets all the in-house specifications for storage stability parameters i.e. active ingredients, suspensibility, pH, wettability, wet sieve, bulk density and moisture content in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).

Example 17
To study the effect of different UV photo degradation arrestor on WG formulation of spinosad and insecticide of Examples 1-4 and conventional SE formulation
Crops : Okra
Target pests : Fruit borer larvae, Helicoverpa armigera
No. of Treatments : six
Plot size : 40 m2
Crop stage : 80 days old crop
Spray time : 12 PM to 2 PM, bright sunshine hours
Spray Volume : 500 litres water per hectare
Application Equipment: Manually operated knapsack sprayer fitted with hollow cone nozzle
Fruit borer larval control (%): Count the number of live larvae plant. Record the observations from 10 plants per plot at 0, 3, 7, 10, 14 and 18 DAA (days after application). Calculate the larval control (%) as below;

The larval control data (observed value) used in Colby’s formula to calculate the synergism.
Table 3: Effect of UV photo degradation arrestor on bioefficacy
Treatment details with application rate (ml or g per hectare) Fruit borer larval control (%)
3 DAA 7 DAA 10 DAA 14 DAA 18 DAA
T1-Spinosad 16%+Emamectin benzoate 3% WG with zinc oxide 1% (Example 1), 250 g 100.0 98.6 94.2 86.2 75.6
T2-Spinosad 16%+Emamectin benzoate 3% WG with titanium dioxide 1% (Example 2), 250 g 100.0 98.0 92.8 83.6 70.2
T3-Spinosad 16%+Emamectin benzoate 3% WG with kojic acid 1% (Example 3), 250 g 100.0 96.6 88.4 76.4 54.2
T4-Spinosad 16%+Emamectin benzoate 3% WG (conventional) (Example 4), 250 g 99.2 94.8 79.6 65.2 40.6
T5-Spinosad 16%+Emamectin benzoate 3% SE (conventional), 250 ml 98.4 88.6 70.2 51.2 32.8
T6-UTC (Untreated Check) 0.00 0.0 0.0 0.00 0.0

T4 and T5 were conventional treatment (as per reference CN103918673A)
Conclusion:
The field trial results show compositions of Example 1 and Example 2 provide higher control of okra fruit borer larvae and also duration of control (residual control) as compared to compositions of Example 3 and Example 4 and their tank mixes. The efficacy and residual control observed was highest in composition of Example 1 followed by composition of Example 2 followed by composition of Example 3. The increase in efficacy and residual control observed in T1 and T2 was because of minimal UV photo degradation of spinosad and emamectin benzoate in the field condition. Zinc oxide and titanium dioxide were more effective UV photo degradation arrestor than kojic acid.

Example 18
To study the impact of UV rays on degradation of active ingredients of Examples 1-4
To study the impact of UV rays on active ingredients, a xenon radiation chamber as a solar simulator was used. It mimics the sunlight radiation energy levels. The radiation intensity falling on the samples was found to be approximately 2.5 to 3K Lux. This radiation energy simulates the solar radiation and is suitable to carry out photo degradation studies in the analytical testing laboratories.
Testing of appropriate samples of compositions studied using HPLC and samples were prepared as mentioned in Examples 1-4:
Table 4: HPLC Conditions
Column C-18,250*4.6MM,5µ
Mobile phase Acetonitrile: Water: TEA:: 75 :25 :0.1 adjust pH to 7.1 using Phosphoric acid
Flow rate 1.0 ml/min
Injection volume 20 µL
Column temperature Ambient
Wave length 245 nm
Run time Approximate 20 min

Chemicals and reagents: Water HPLC grade, acetonitrile, emamectin benzoate and spinosad standard (known purity), triethyl amine (TEA), phosphoric acid.
Standard solution preparation:
Take 0.1 g weight of spinosad and 0.02 g of emamectin benzoate standard in 100 ml volumetric flask, add approximate 50 ml acetonitrile and sonicate for 5 minutes and allow to attain the room temperature, make up the volume with acetonitrile (A). Transfer 1.0 ml of (A) in 25 ml volumetric flask and make up the volume with mobile phase.

Composition sample preparation:
Take approximate 0.67 g of composition in 100 ml volumetric flask, add 2 ml HPLC water and approximate 50 ml acetonitrile and sonicate for 5 minutes and allow to attain the room temperature, make up the volume with acetonitrile (B). Transfer 1.0 ml of (B) in 25 ml volumetric flask and make up the volume with mobile phase.

Estimation:
Inject 20 µL standard solutions until the standard area does not deviate from each other by more than two percent. Then use the following injection sequence std1, std2, sam1, sam2.
Calculation:
S1 x MS1
Spinosad content (% by mass) = -------------- x P
S2 x MS2
Where,
MS1=Mass in g of reference standard spinosad,
MS2=Mass in g of sample,
S1=Sum of peak area of spinosad A+spinosad D in the chromatogram of sample,
S2=Sum peak area of spinosad A+spinosad D in the chromatogram of standard,
P=Percentage purity of standard spinosad
E1 x ME1
Emamectin benzoate content (% by mass) = --------------- x P
E2 x M2
Where,
ME1=Mass in g of reference standard emamectin benzoate
MS2=Mass in g of sample,
E1=Peak area of emamectin benzoate in the chromatogram of sample,
E2=Peak area of emamectin benzoate in the chromatogram of standard,
P=Percentage purity of standard emamectin benzoate

Table 5: Results - Active ingredients after UV rays exposure
Treatments Exposure period (hours)
0 Hrs 2 Hrs 4 hrs 6 hrs 8 hrs
S (%) EB (%) S (%) EB (%) S (%) EB (%) S (%) EB (%) S (%) EB (%)
Example 1 (zinc oxide) 16.25 3.15 16.25 3.15 16.20 3.12 16.19 3.10 16.15 3.09
Example 2 (titanium dioxide) 16.26 3.16 16.26 3.16 16.20 3.11 16.17 3.07 15.95 3.00
Example 3 (kojic acid) 16.24 3.15 16.24 3.15 16.20 3.10 16.15 3.05 15.85 2.95
Example 4 (conventional) 16.25 3.16 16.24 3.14 16.05 3.10 15.90 2.90 15.50 2.50
S (%) - spinosad, EB (%)-emamectin benzoate
Conclusion:
The photo degradation study with usage of different types of UV degradation arresters shows that the degradation of spinosad and emamectin benzoate were minimal with zinc oxide (Example 1) followed by titanium dioxide (Example 2) and kojic acid (Example 3) after 8 hrs exposure. The degradation of both the active ingredients was highest in composition of Example 4 (conventional). The selection of zinc oxide as a UV photo degradation arrestor to the WG formulation of spinosad and emamectin benzoate resulted in enhanced bio-efficacy and residual control under field conditions.

Example 19
To study the spreading properties of WG formulations of spinosad of Examples 1 and 2, and Examples 5 and 6
Method: Spreading properties test conducted by preparing 1% solution (1 g composition 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 6: Spreading property study
Compositions Room temperature storage
1 month 6 months 12 months
(Spreading diameter in mm)
Spinosad 16%+Emamectin benzoate 3% WG (Example 1) 13 13 11
Spinosad 16%+Emamectin benzoate 3% WG (Example 4 – conventional) 5 5 4

Conclusion:
Spinosad 16%+emamectin benzoate 3% WG (Example 1) shows excellent spreading properties as compared to spinosad 16%+emamectin benzoate 3% WG (Example 4 – conventional). This improves the bio-efficacy under field conditions by enhancing spreading action and penetration and also improves rainfastness properties during rainy days.
Table 7: Spreading property study of different compositions of spinosad 22.5%+cyantraniliprole 22.5% WG
Compositions Room temperature storage
1 month 6 months 12 months
(Spreading diameter in mm)
SC-WG-1 (Polyalkyleneoxide modified heptamethyltrisiloxane 2%) (Example 5) 12 11 10
SC-WG-2 (Polyalkyleneoxide modified heptamethyltrisiloxane 3%) (Example 5) 14 13 12
SC-WG-3 (Polyalkyleneoxide modified heptamethyltrisiloxane 4%) (Example 5) 14 14 12
SC-WG-4 (Polyalkyleneoxide modified heptamethyltrisiloxane 5%) (Example 5) 15 14 13
Spinosad 22.5%+Cyantraniliprole 22.5% WG (conventional) (Example 6) 5 4 3

Conclusion:
The trial results show compositions SC-WG-2, SC-WG-3 and SC-WG-4 provide excellent spreading action as compared to spinosad 22.5% + cyantraniliprole 22.5% WG (conventional).

Example 20
To study the effect of super wetting-spreading-penetrating agent on bio-efficacy performance of Examples 5, 6 and tank mix
Crop : Cauliflower
Location : Umreth, Dist. Anand, Gujarat
Treatments : Seven
Crop age : 72 days after transplanting.
Spray water volume : 500 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Conclusion:
The treatment application (spraying) was done with knap sack sprayer by using 500 litre spray volume. One hour later, the sprayed plants were exposed to 75 mm of simulated rain in one hour. The leaves from respective treatments were collected and put into the PVC/plastic box. 25 larvae (3rd instar) of Spodoptera litura were released into the PVC box containing treated cauliflower leaves and larval mortality was observed on 72 hrs. The % larval control was calculated. Similarly, the treated cauliflower leaves were collected on 3rd, 7th, 10th and 14th days and Spodoptera litura (3rd instar), 25 larvae were released and allowed to feed and % larval mortality was recorded after 72 hrs. The % larval control was calculated.

Table 8: Control of Spodoptera litura on cauliflower (rainfastness study)
Treatment details with application rate per hectare Spodoptera litura larval control (%)
3 DAA 7 DAA 10 DAA 14 DAA
T1-Spinosad 22.5%+Cyantraniliprole 22.5% WG (Example 5: SPCY-WG-1), 100 g 100 98.2 95.8 91.4
T2-Spinosad 22.5%+Cyantraniliprole 22.5% WG (Example 5: SPCY-WG-2), 100 g 100 99.2 96.4 93.2
T3-Spinosad 22.5%+Cyantraniliprole 22.5% WG (Example 5: SPCY-WG-3), 100 g 100 98.4 94.6 91.2
T4-Spinosad 22.5%+Cyantraniliprole 22.5% WG (Example 5: SPCY-WG-4), 100 g 100 98.2 93.6 90.0
T5-Spinosad 22.5%+Cyantraniliprole 22.5% WG (Example 6: SPCY-5-conventional), 100 g 100 94.6 87.6 80.4
T6-Spinosad 45% SC+Cyantraniliprole 10.26% OD (tank mix), 50 ml+225 ml 98.4 90.6 80.2 68.2
T7-UTC (Untreated Check) 0.00 0.0 0.0 0.00
Conclusion:
All the WG formulations of present invention of spinosad 22.5%+Cyantraniliprole 22.5% (Example 5: T1 to T4) provide more than >90% larval control upto 14 DAA, which was much higher than T5 (Example 6: SPCY-5 conventional WG) and their tank mix T6. The addition of polyalkyleneoxide modified heptamethyltrisiloxane as a super wetting-spreading-penetrating agent in WG formulation provides better efficacy even under rainfall condition.

Example 21
To study the synergism between spinosad and insecticide in WG formulations of present invention, on farm tank mixes, and market available products
Crop : Chilli, Pikador variety
Target insects : Thrips (Scirtothrips dorsalis and Thrips parvispinus)
Number of treatments : Fifteen
Plot size : 30 m2
Crop age : 75 days, flowering and fruiting stage
Spray water volume : 500 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods:
Thrips 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. Record the observations on 4, 8 and 12 days after application (DAA). Calculate thrips control (%) as;

Use thrips control (%) data (as observed value) to check the synergism by applying Colby’s formula given below.

Fruits & Flower count: Count the number of healthy fruits and flowers per plant. Record the observations from 10 plants per plot on 15th day after application.
Table 9: Treatment details
Treatment details Application Rate
Composition (ml or g hectare) g.a.i.* per hectare
T1-Spinosad 16%+Emamectin benzoate 3% WG 250 g 40+7.5
T2-Spinosad 16%+Abamectin 3% WG 250 g 40+7.5
T3-Spinosad 16%+Fluxametamide 12% WG 250 g 40+30
T4-Spinosad 40%+Broflanilide 8% WG 100 g 40+8
T5-Spinosad 45% SC+Emamectin benozate 1.9% EC 88.89 ml+394.74 ml 40+7.5
T6-Spinosad 45% SC+Abamectin 1.9% EC 88.89 ml+394.74 ml 40+7.5
T7-Spinosad 45% SC+Fluxametamide 10% EC 88.89 ml+300 ml 40+30
T8-Spinosad 45% SC+Broflanilide 10% SC 88.89 ml+80 ml 40+8
T9-Spinosad 45% SC 88.89 ml 40
T10-Spinosad 45% SC 160 ml 72
T11-Emamectin benzoate 1.9% EC 394.74 ml 7.5
T12-Abamectin 1.9% EC 394.74 ml 7.5
T13-Fluxametamide 10% EC 300 ml 30
T14-Broflanilide 30% SC 25 ml 8
T15-UTC (Untreated Check) - -

*gram active ingredients
T1 to T4- WG formulations of present invention, T5 to T8-on farm tank mixes, T9 to T14-market available products

Table 10: Synergistic control of chilly thrips
Treatment details Thrips control (%)
4 DAA* 8 DAA* 12 DAA*
Observed Value Expected Value Colby's ratio Observed Value Expected Value Colby's ratio Observed Value Expected Value Colby's ratio Synergism (Y/N)
T1 94.0 86.77 1.08 90.2 71.41 1.26 82.4 45.68 1.80 Y
T2 99.8 89.76 1.11 96.8 77.49 1.25 86.2 50.26 1.72 Y
T3 98.8 89.25 1.11 95.2 74.30 1.28 81.6 42.58 1.92 Y
T4 99.2 88.68 1.12 92.8 72.41 1.28 81.2 41.55 1.95 Y
T5 93.2 86.77 1.07 72.2 71.41 1.01 36.4 45.68 0.80 N
T6 95.8 89.76 1.07 80.2 77.49 1.03 49.8 50.26 0.99 N
T7 94.6 89.25 1.06 79.4 74.30 1.07 40.2 42.58 0.94 N
T8 95.6 88.68 1.08 78.2 72.41 1.08 38.6 41.55 0.93 N
T9 68.2 50.2 26.2
T10 88.4 70.6 46.6
T11 58.4 42.6 26.4
T12 67.8 54.8 32.6
T13 66.2 48.4 22.2
T14 64.4 44.6 20.8
T15 0.00 0.00 0.00

*days after application

Conclusion:
All the WG formulation of present invention of spinosad+insecticide (T1 to T4) provides excellent control of thrips on 4th and 8th DAA and provides synergistic residual control of thrips up to 14 days. The conventional tank mixes (T5 to T8) do not show synergism on 12 DAA.
Table 11: Number of flowers and fruits
Treatment details Number of flowers/plant Increase(%) over T15 Number of fruits/plant Increase(%) over T15
T1 44.3 139.5 50.2 141.3
T2 48.5 162.2 52.7 153.4
T3 47.2 155.1 51.8 149.0
T4 45.8 147.6 51.2 146.2
T5 31.6 70.8 40.6 95.2
T6 36.9 99.5 43.6 109.6
T7 36.2 95.7 42.3 103.4
T8 33.7 82.2 41.2 98.1
T9 26.8 44.9 30.7 47.6
T10 35.9 94.1 37.5 80.3
T11 24.8 34.1 31.3 50.5
T12 28.7 55.1 35.5 70.7
T13 27.4 48.1 34.3 64.9
T14 25.6 38.4 32.6 56.7
T15 18.5 0.0 20.8 0.0
Conclusion:
The treatment of WG formulation of present invention of spinosad+insecticide (T1 to T4) bears significantly higher number of flower and fruits per plant as compared to their tank mixes (T5 to T8). The WG formulation of present invention of spinosad+insecticides provides residual control which helps the farmers to reduce the number of sprays and also produces higher number of flowers and fruits.

Example 22
Bioefficacy comparison of WG formulation of present invention with conventional suspension concentrate (SC) formulation, conventional oil dispersion (OD) formulation, and tank mixes of market available products
Crop : Chilli, Omega variety
Target insects : Fruit borer complex (Helicoverpa armigera and Spdoptera litura), Thrips (Scirtothrips dorsalis & Thrips parvispinus)
Number of treatments : Five
Plot size : 40 m2
Crop age : 68 days, flowering and fruiting stage
Spray water volume : 500 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods:
Thrips control (%): same as given in Example 21.
Fruit borer larval control (%): same as given in Example 17.
Table 12: Field performance of WG formulation of present invention v/s conventional formulations
Treatment details Application Rate Fruit borer larval control (%)
Composition (g or ml per hectare) g.a.i. per hectare 1 DAA 3 DAA 7 DAA 10 DAA 14 DAA
T1-Spinosad 10% + Tolfenpyrad 20% WG 500 g 50+100 100.0 98.6 95.6 88.2 80.4
T2-Spinosad 10% + Tolfenpyrad 20% SC 500 ml 50+100 100.0 97.8 90.4 79.2 68.6
T3-Spinosad 10% + Tolfenpyrad 20% OD 500 ml 50+100 100.0 97.2 89.6 78.4 65.8
T4-Spinosad 45% SC + Emamectin benozate 1.9% EC (tank mix) 111.11 ml+666.67 ml 50+100 97.8 90.4 84.2 68.8 58.6
T5-UTC (Untreated Check) - - 0.00 0.0 0.0 0.00 0.0

T1- WG formulation of present invention, T2-conventional Suspension concentrate (SC) formulation, T3-conventional Oil dispersion (OD) formulation, T4-tank mixes of market available products

Conclusion:
The WG formulation of present invention of spinosad 10%+tolfenpyrad 20% WG provides excellent control (higher control level and residual period) of fruit borer larvae of chilly crop up to 14 DAA as compared to conventional formulations like SC, OD and tank mixes.
Table 13: Thrips control and fruit count
Treatment number Thrips control (%) Number of fruits per plant Increase(%) over T5
7 DAA 14 DAA
T1 88.6 76.80 63.5 123.6
T2 70.2 49.40 51.6 81.7
T3 69.4 46.80 50.4 77.5
T4 62.6 37.80 46.8 64.8
T5 0.0 0.00 28.4 0.0

Conclusion:
The WG formulation of present invention of spinosad 10%+tolfenpyrad 20% WG (T1) provides superior control of chilly thrips and produces more number of chilly fruits per plant as compared to conventional formulations like SC, OD and tank mixes.

Example 23
Effect of spray volume on bioefficacy of WG formulation of present invention, conventional suspo Emulsion (SE), and tank mix of market available product
Crop : Chilli, Omega variety
Target insects : Thrips (Scirtothrips dorsalis and Thrips parvispinus)
Number of treatments : Seven
Plot size : 40 m2
Crop age : 68 days, flowering and fruiting stage
Spray water volume : as given in treatment details
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods:
Thrips control (%): same as given in Example 21.
Table 14: Spray volume and bioefficacy against thrips
Treatment details Dose & spray water volume Thrips control (%)
3 DAA 7 DAA 10 DAA 14 DAA
T1-Spinosad 16%+Abamectin 3% (Composition: SA-WG-190) 250 g in 500 litres 99.6 94.2 89.6 82.8
T2-Spinosad 16%+Abamectin 3% (Composition: SA-WG-190) 250 g in 375 litres 96.8 90.2 83.8 75.4
T3-Spinosad 16%+Abamectin 3% SE 250 ml in 500 litres water 98.4 91.8 84.6 73.2
T4-Spinosad 16%+Abamectin 3% SE 250 ml in 375 litres water 94.6 84.2 73.2 57.6
T5-Spinosad 45% SC+Abamectin 1.9% EC (88.89 ml+394.74 ml) in 500 litres water 95.8 86.4 72.6 58.8
T6-Spinosad 45% SC+Abamectin 1.9% EC (88.89 ml+394.74 ml) in 375 litres water 90.4 77.6 58.8 40.6
T7-UTC (Untreated Check) - 0.00 0.0 0.0 0.00

Table 15: Spray volume and bioefficacy against thrips
Treatment Number Drop in efficacy due to spray volume reduction
3 DAA 7 DAA 10 DAA 14 DAA
T1-T2 2.8 4.0 5.8 7.4
T3-T4 3.8 7.6 11.4 15.6
T5-T6 5.4 8.8 13.8 18.2
T1 & T2- WG formulation of present invention, T3 & T4-Suspo Emulsion (SE) as per reference CN111616156A, T5&T6-tank mix of market available product

Conclusion:
The results of field bioefficacy studies show that bioefficacy against chilly thrips drops by 2.8%, 4%, 5.8% and 7.4% on 3 DAA, 7 DAA, 10 DAA and 14 DAA respectively in WG formulations of present invention when spray volume reduced from 500 litres to 375 litres per hectare i.e. 25% reduction. The drops in bioefficacy were higher in SE formulation and tank mixes. It can be concluded that bioefficacy is not much affected with WG formulation of the present invention, when spray water volume reduces, whereas it was greatly reduced in conventional formulation and tank mixes.

Example 24
Synergistic control of fall armyworm infesting maize crop
Crop : Maize/Corn
Target insects : Fall Armyworm, Spodoptera frugiperda
Number of treatments : Twenty four
Plot size : 24 m2
Crop age : 32
Spray water volume : 400 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods: Calculate larval control (%).
Table 16: Larval control of fall armyworm
Treatment details Composition per hectare g.a.i./ hectare Larval control (%) at 7 DAA
Observed Value Expected Value Colby's ratio
T1-Spinosad 16% + Indoxacarb 16% WG 250 g 40+40 94.6 82.81 1.14
T2-Spinosad 8% + Methoxyfenozide 24% WG 500 g 40+120 97.4 84.62 1.15
T3-Spinosad 8% + Tebufenozide 24% WG 500 g 40+120 95.4 84.36 1.13
T4-Spinosad 16% + Chromafenozide 24% SC 250 g 40+60 94.2 84.53 1.11
T5-Spinosad 5% + Diafenthiuron 25% WG 800 g 40+200 85.2 83.80 1.02
T6-Spinosad 30% + Flubendiamide 13.33% WG 150 g 45+20 98.6 88.11 1.12
T7-Spinosad 30% + Tetraniliprole 20% WG 150 g 45+30 96.8 87.68 1.10
T8-Spinosad 22.5% + Lambda cyhalothrin 10% WG 200 g 45+20 90.8 82.17 1.11
T9-Spinosad 3.6% + Profenofos 36% WG 1250 45+450 91.2 84.39 1.08
T10-Spinosad 10% + Dichloromezotiaz 12% WG 500 g 50+60 95.2 86.03 1.11
T11-Spinosad 45% SC 88.89 ml 40 56.8
T12-Spinosad 45% SC 100 ml 45 64.2
T13-Spinosad 45% SC 111.11 ml 50 68.4
T14-Indoxacarb 15% EC 266.67 ml 40 60.2
T15-Methoxyfenozide 21.8% (24% w/v) SC 500 ml 120 64.4
T16-Tebufenozide 70% WP 171.42 ml 120 63.8
T17-Chromafenozide 80% WP 75 ml 60 64.2
T18-Diafenthiuron 50% WG 400 g 200 48.8
T19-Flubendiamide 20% WG 100 g 20 66.8
T20-Tetraniliprole 18.18% SC (20% w/v) 150 ml 30 65.6
T21-Lambda cyhalothrin 5% EC 400 ml 20 50.2
T22-Profenofos 50% EC 900 ml 450 56.4
T23-Dichloromezotiaz 20% SC 300 ml 60 55.8
T24-UTC (Untreated Check) - - 0.00
T1 to T10- WG formulation of present invention
Conclusion:
All the WG formulations of present invention of spinosad+insecticide (T1 to T10) provide synergistic control of fall army worm infesting maize crop.

Example 25
Synergistic control of pod borer larvae in redgram crop by Example 7, other WG formulations of present invention, and conventional formulations
Crop : Redgram
Target insects : Pod borer, Helicoverpa armigera
Number of treatments : Eight
Plot size : 30 m2
Crop age : 96 days, flowering and pod formation stage
Spray water volume : 550 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods: Calculate larval control (%).
Table 17: Pod borer larval control
Treatment details Composition per hectare g.a.i./ hectare Larval control (%)
3 DAA 7 DAA 10 DAA 14 DAA
T1-Spinosad 20% + Chlorantraniliprole 10% WG 200 g 40+20 100.0 96.2 91.8 85.8
T2-Spinosad 20% + Chlorantraniliprole 15% WG (Example 7) 200 g 40+30 100.0 97.8 93.6 88.6
T3-Spinosad 25% + Chlorantraniliprole 10% WG 200 g 45+20 100.0 96.2 92.4 86.6
T4-Spinosad 25% + Chlorantraniliprole 15% WG 200 g 45+30 100.0 98.8 95.2 90.4
T5-Spinosad 25% + Chlorantraniliprole 15% WG (conventional) 200 g 45+30 100.0 95.2 84.2 73.4
T6-Spinosad 25% + Chlorantraniliprole 15% WP (conventional) 200 g 45+30 100.0 94.6 84.8 74.6
T7-Spinosad 25% + Chlorantraniliprole 15% SC (conventional) 200 ml 45+30 100.0 95.4 87.2 78.4
T8-UTC (Untreated Check) 221 g - 0.0 0.0 0.0 0.0

Conclusion:
All the doses of WG formulation of present invention of spinosad+chlorantraniliprole provide higher control of larvae even on 14 DAA as compared to all conventional formulations. Even the lower dosage of WG formulation of present invention provides better efficacy as compared to higher doses of conventional WG, WP and SC formulation.

Example 26
Synergistic control of fruit borer larvae and thrips in chilly crop by WG formulations of present invention, and conventional ready mix formulations
Crop : Chilly
Target insects : Fruit borer and Thrips
Table 18: Treatment details
Treatment number Treatment details Application rate (gram active ingredients per hectare)
T1 Spinosad 24%+Abamectin 4.8%+Chlorantraniliprole 12% WG, 125 g 30+6+15
T2 Spinosad 24%+Emamectin benzoate 4.8%+Chlorantraniliprole 12% WG, 125 g 30+6+15
T3 Spinosad 12%+Tolfenpyrad 30%+Chlorantraniliprole 6% WG, 250 g 30+75+15
T4 Spinosad 12%+Fluxametamide 10%+Chlorantraniliprole 6% WG, 250 g 30+25+15
T5 Spinosad 24%+Chlorantraniliprole 12% SC, 125 ml 30+15
T6 Spinosad 10%+Abamectin 2% SE, 300 ml 30+6
T7 Spinosad 10%+Emamectin benzoate 2 % SE, 300 ml 30+6
T8 Spinosad 6%+Tolfenpyrad 15% SC, 500 ml 30+75
T9 Spinosad 12%+Fluxametamide 10% SE, 250 ml 30+25
T10 Abamectin 2%+Chlorantraniliprole 5% SE, 300 ml 6+15
T11 Emamectin benzoate 2%+Chlorantraniliprole 5% SE, 300 ml 6+15
T12 Tolfenpyrad 15%+Chlorantraniliprole 3% SC, 500 ml 75+15
T13 Fluxametamide 10%+Chlorantraniliprole 6% SC, 250 ml 25+15
T14 Spinosad 45% SC 30
T15 Chlorantraniliprole 18.5% SC 15
T16 Abamectin 1.9% EC 6
T17 Emamectin benzoate 1.9% EC 6
T18 Tolfenpyrad 15% EC 75
T19 Fluxametamide 10% EC 25
T20 UTC (Untreated Control) -
T1 to T4- WG formulations of present invention, T5 to T13-conventional ready mix formulations
SE suspo emulsion, SC suspension concentrate, EC emulsifiable concentrate

Table 19: Synergistic control of fruit borer and thrips in chilly crop
Treatment number Larval control (%) Thrips control (%)
Observed Value Expected value Colby's ratio Observed Value Expected value Colby's ratio
T1 100.0 84.70 1.18 98.4 87.82 1.12
T2 100.0 91.75 1.09 96.4 84.64 1.14
T3 100.0 88.89 1.13 97.2 87.30 1.11
T4 100.0 89.80 1.11 95.4 86.13 1.11
T5 77.4 79.27 0.98 65.8 67.60 0.97
T6 66.8 69.15 0.97 83.4 85.04 0.98
T7 82.4 83.36 0.99 78.8 81.13 0.97
T8 75.8 77.60 0.98 80.8 84.40 0.96
T9 77.2 79.43 0.97 80.2 82.97 0.97
T10 61.4 63.40 0.97 67.8 69.39 0.98
T11 77.4 80.26 0.96 50.4 61.42 0.82
T12 70.4 73.41 0.96 65.6 68.09 0.96
T13 73.2 75.60 0.97 60.4 65.16 0.93
T14 58.2 60.2
T15 50.4 18.6
T16 26.2 62.4
T17 60.2 52.6
T18 46.4 60.8
T19 50.8 57.2
T20 0.0 0.0

Conclusion:
All the WG formulations of present invention (T1 to T4) provide synergistic (colby’s ratio >1) control of fruit borer larvae and thrips as compared to all the conventional ready mix formulations (T5 to T13).
Example 27
Synergistic control of sucking pests complex in chilli
Crop : Chilli
Target insects : Thrips (Scirtothrips dorsalis) and mites (Polyphagotarsonemus latus)
Number of treatments : Ten
Plot size : 25 m2
Crop age : 67 days, flowering and fruiting stage
Spray water volume : 430 litres per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods:
Thrips control (%): same as given in Example 21.
Mite control (%):
Count the number of motile stage of mite per spot with 10x magnifying lense, 4 spot per leaf, 4 leaves per plant and 10 plants per plot. Calculate mite control (%).
Observations were recorded on 7th days after application.
Table 20: Synergistic control of thrips and mites in chilly
Treatment details Formulation per hectare g.a.i per hectare Thrips control (%) Mite control (%) Synergism
Observed Value Expected Value Observed Value Expected Value
T1-Spinosad 26.67% + Fenpyroximate 10% WG 150 40+15 88.6 80.50 75.4 72.38 Yes
T2-Spinosad 13.3% + Hexythiazox 5% WG 150 40+15 86.4 79.44 78.8 73.54 Yes
T3-Spinosad 26.67% + Etoxazole 20% WG 150 40+30 84.2 78.23 80.2 75.37 Yes
T4-Spinosad 13.3% + Cyenopyrafen 15% WG 300 40+45 80.6 77.77 76.6 73.04 Yes
T5-Spinosad 45% SC 88.89 40 62.2 16.8
T6-Fenpyroximate 40% WG 37.5 15 48.4 66.8
T7-Hexythiazox 5.45% (5% w/v) EC 300 15 45.6 68.2
T8-Etoxazole 10% SC 300 30 42.4 70.4
T9-Cyenopyrafen 30% SC 150 45 41.2 67.6
T10-UTC (Untreated Check) - - 0.00 0.00

Conclusion:
The compositions of the present invention (T1 to T4) provide synergistic control of thrips and mites in chilli crop.

Example 28
Synergistic control of sucking pests complex in cotton
Crop : Cotton
Target insects : Thrips (Thrips tabaci) and Jassid (Amrasca bibuttulla biguttulla)
Number of treatments : Ten
Plot size : 50 m2
Crop age : 58 days, flowering and fruiting stage
Spray water volume : 450 liters per hectare
Method of Application : Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle
Observation Methods:
Thrips control (%): same as given in Example 21.
Jassid control (%): Count the number of live jassids per leaf, observe 3 leaves per plant and 10 plant per plot. Calculate jassid control (%).
Observations were recorded on 7th day after application.
Table 21: Synergistic control of thrips and jassid in cotton crop
Treatment details Formulation per hectare g.a.i per hectare Jassid (%) Thrips control (%) Synergism (Yes/No)
Observed Value Expected Value Observed Value Expected Value
T1-Spinosad 22.5%+Flonicamid 25% WG 200 45+50 80.6 77.04 90.2 83.44 Yes
T2-Spinosad 22.5%+Clothianidin 20% WG 200 45+40 78.6 73.33 94.8 87.66 Yes
T3-Spinosad 22.5%+Dinotefuran 10% WG 200 45+20 70.2 66.41 93.6 86.17 Yes
T4-Spinosad 30%+Fipronil 30% WG 150 45+45 65.8 55.10 97.8 92.30 Yes
T5-Spinosad 45% SC 100 45 15.6 76.8
T6-Flonicamid 50% WG 100 50 72.8 28.6
T7-Clothianidin 50% WG 80 40 68.4 46.8
T8-Dinotefuran 20% SG 100 20 60.2 40.4
T9-Fipronil 80% WG 56.25 45 46.8 66.8
T10-UTC (Untreated Check) - - 0.00 0.00

Conclusion:
The compositions of the present invention (T1 to T4) provide synergistic control of thrips and jassid in cotton crop.

To sum up, the composition of the present invention shows synergism between spinosad + insecticide and spinosad + insecticide + insecticide, provides control of broad spectrum of insects pests at a time, provides residual (extended) control as compared to conventional formulations, shows rainfast properties as compared to conventional formulations, has better bioefficacy even at reduced spray water volume, and has enhanced bioefficacy due to super wetting-spreading-penetrating agent and UV photo degradation arrestor.
Although the examples as well as the process for preparation and use has been specifically described, it should be understood that variations in the preferred embodiment/s could be achieved by a person skilled in the art without departing from the spirit of the invention. All substitution, alterations and modification of the present invention which come within the scope of the following claims are to which the present invention is readily susceptible without departing from the spirit of the invention. The scope of the invention should therefore be determined not only with reference to the above description but also with reference to the appended claims along with full scope of equivalents to which such claims are entitled.
, Claims:WE CLAIM:
1. A spinosad and insecticide(s) wettable granule composition comprising 3 to 50% w/w spinosad or its agrochemically acceptable salts, 1 to 50% w/w one or more insecticides, 0.5 to 2.5% w/w UV photo degradation arrester, 1.5 to 6% w/w wetting-spreading-penetrating agent, and agrochemically acceptable excipients.

2. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein one or more insecticides is selected from emamectin benzoate, abamectin, indoxacarb, methoxyfenozide, tebufenozide, chromafenozide, broflanilide, cyproflanilide, fluxametamide, isocycloseram, afoxolaner, esafoxolaner, fluralaner, lotilaner, sarolaner, chlorantraniliprole, cyantraniliprole, cyclaniliprole, tetraniliprole, tetrachlorantraniliprole, tyclopyrazoflor, cyhalodiamide, flubendiamide, fluchlordiniliprole, tiorantraniliprole, dichloromezotiaz, fenmezoditiaz, lambda cyhalothrin, bifenthrin, clothianidin, thiamethoxam, fipronil, profenofos, diafenthiuron, flonicamid, fenpyroximate, hexythiazox, etoxazole and cyenopyrafen.

3. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein the preferred combination for the composition comprises:
i. Spinosad, Emamectin benzoate and one or more inactive excipients, or
ii. Spinosad, Abamectin and one or more inactive excipients, or
iii. Spinosad, Indoxacarb and one or more inactive excipients, or
iv. Spinosad, Methoxyfenozide and one or more inactive excipients, or
v. Spinosad, Tebufenozide and one or more inactive excipients, or
vi. Spinosad, Chromafenozide and one or more inactive excipients, or
vii. Spinosad, Broflanilide and one or more inactive excipients, or
viii. Spinosad, Cyproflanilide and one or more inactive excipients, or
ix. Spinosad, Fluxametamide and one or more inactive excipients, or
x. Spinosad, Isocycloseram and one or more inactive excipients, or
xi. Spinosad, Fluralaner and one or more inactive excipients, or
xii. Spinosad, Chlorantraniliprole and one or more inactive excipients, or
xiii. Spinosad, Cyantraniliprole and one or more inactive excipients, or
xiv. Spinosad, Cyclaniliprole and one or more inactive excipients, or
xv. Spinosad, Tetraniliprole and one or more inactive excipients, or
xvi. Spinosad, Tetrachlorantraniliprole and one or more inactive excipients, or
xvii. Spinosad, Tyclopyrazoflor and one or more inactive excipients, or
xviii. Spinosad, Cyhalodiamide and one or more inactive excipients, or
xix. Spinosad, Flubendiamide and one or more inactive excipients, or
xx. Spinosad, Tolfenpyrad and one or more inactive excipients, or
xxi. Spinosad, Dichloromezotiaz and one or more inactive excipients, or
xxii. Spinosad, Lambda cyhalothrin and one or more inactive excipients, or
xxiii. Spinosad, Bifenthrin and one or more inactive excipients, or
xxiv. Spinosad, Clothianidin and one or more inactive excipients, or
xxv. Spinosad, Thiamethoxam and one or more inactive excipients, or
xxvi. Spinosad, Dinotefuran and one or more inactive excipients, or
xxvii. Spinosad, Fipronil and one or more inactive excipients, or
xxviii. Spinosad, Profenofos and one or more inactive excipients, or
xxix. Spinosad, Flonicamid and one or more inactive excipients, or
xxx. Spinosad, Fenpyroximate and one or more inactive excipients, or
xxxi. Spinosad, Hexythiazox and one or more inactive excipients, or
xxxii. Spinosad, Etoxazole and one or more inactive excipients, or
xxxiii. Spinosad, Cyenopyrafen and one or more inactive excipients, or
xxxiv. Spinosad, Abamectin, Chlorantraniliprole and one or more inactive excipients, or
xxxv. Spinosad, Abamectin, Cyantraniliprole and one or more inactive excipients, or
xxxvi. Spinosad, Abamectin, Tetraniliprole and one or more inactive excipients, or
xxxvii. Spinosad, Abamectin, Cyclaniliprole and one or more inactive excipients, or
xxxviii. Spinosad, Abamectin, Broflanilide and one or more inactive excipients, or
xxxix. Spinosad, Abamectin, Tolfenpyrad and one or more inactive excipients, or
xl. Spinosad, Abamectin, Fluxametamide and one or more inactive excipients, or
xli. Spinosad, Abamectin, Methoxyfenozide and one or more inactive excipients, or
xlii. Spinosad, Emamectin benzoate, Chlorantraniliprole and one or more inactive excipients, or
xliii. Spinosad, Emamectin benzoate, Cyantraniliprole and one or more inactive excipients, or
xliv. Spinosad, Emamectin benzoate, Tetraniliprole and one or more inactive excipients, or
xlv. Spinosad, Emamectin benzoate, Cyclaniliprole and one or more inactive excipients, or
xlvi. Spinosad, Emamectin benzoate + Broflanilide and one or more inactive excipients, or
xlvii. Spinosad, Emamectin benzoate, Tolfenpyrad and one or more inactive excipients, or
xlviii. Spinosad, Emamectin benzoate, Fluxametamide and one or more inactive excipients, or
xlix. Spinosad, Emamectin benzoate, Methoxyfenozide and one or more inactive excipients, or
l. Spinosad, Tolfenpyrad, Chlorantraniliprole and one or more inactive excipients, or
li. Spinosad, Tolfenpyrad, Cyantraniliprole and one or more inactive excipients, or
lii. Spinosad, Tolfenpyrad, Tetraniliprole and one or more inactive excipients, or
liii. Spinosad, Tolfenpyrad, Cyclaniliprole and one or more inactive excipients, or
liv. Spinosad, Tolfenpyrad, Broflanilide and one or more inactive excipients, or
lv. Spinosad, Tolfenpyrad, Fluxametamide and one or more inactive excipients, or
lvi. Spinosad, Tolfenpyrad, Methoxyfenozide and one or more inactive excipients, or
lvii. Spinosad, Fluxametamide, Chlorantraniliprole and one or more inactive excipients, or
lviii. Spinosad, Fluxametamide, Cyantraniliprole and one or more inactive excipients, or
lix. Spinosad, Fluxametamide, Tetraniliprole and one or more inactive excipients, or
lx. Spinosad, Fluxametamide, Cyclaniliprole and one or more inactive excipients, or
lxi. Spinosad, Fluxametamide, Broflanilide and one or more inactive excipients, or
lxii. Spinosad, Fluxametamide, Methoxyfenozide and one or more inactive excipients, or
lxiii. Spinosad, Diafenthiuron, Chlorantraniliprole and one or more inactive excipients, or
lxiv. Spinosad, Diafenthiuron, Cyantraniliprole and one or more inactive excipients, or
lxv. Spinosad, Diafenthiuron, Tetraniliprole and one or more inactive excipients, or
lxvi. Spinosad, Diafenthiuron, Cyclaniliprole and one or more inactive excipients, or
lxvii. Spinosad, Diafenthiuron, Broflanilide and one or more inactive excipients.

4. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein the UV photo degradation arrestor is selected from zinc oxide and titanium dioxide.

5. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein the wetting-spreading-penetrating agent is selected from organic silicone, which includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxane heptamethyl, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, or mixture thereof, more preferably, polyalkyleneoxide modified heptamethyl trisiloxane.

6. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein the agrochemically acceptable excipients comprises dispersing agent, anti-foaming agent, carrier, humectants, binding agent, and anti-caking agent.

7. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the agrochemically acceptable excipients comprises 5 to 20% w/w dispersing agent, 0.25 to 1% w/w anti-foaming agent, 30 to 70% w/w carrier, 1 to 10% w/w humectants, 0.5 to 2% w/w binding agent, and 0.2 to 1% w/w anti-caking agent.

8. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the dispersing agent is selected from sodium polycarboxylate (sodium polyacrylate), naphthalene sulfonic acid, sodium salt condensates with formaldehyde, polyalcoxylated alkylphenol, naphthalene sulfonic acid formaldehyde condensate, methyl naphthalene-formaldehyde-condensate sodium salt, naphthalene condensates, lignosulfonates, calcium lignosulfonate, sodium lignosulfonate, sodium alkyl naphthalene sulfonate, and sodium lignosulfonate-sulfomethylated, more preferably, sodium lignosulfonate, sodium alkyl naphthalene sulfonate, and sodium lignosulfonate-sulfomethylated.

9. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the anti-foaming agent is selected from silicone emulsion, perfluoroalkylphosphonic acids, perfluoroalkylphosphinic acids and perfluoroaliphatic polymeric esters or mixtures thereof, more preferably, polydimethylsiloxane.

10. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the carrier is selected from clay, silica, lactose monohydrate, sodium sulfate anhydrous, corn starch, urea, EDTA, urea formaldehyde resin, diatomaceous earth, kaolin, bentonite, kieselguhr, fuller's earth, attapulgite clay, bole, loess, talc, chalk, dolomite, limestone, lime, calcium carbonate, powdered magnesia, magnesium oxide, magnesium sulphate, sodium chloride, gypsum, calcium sulphate, pyrophyllite, silicates, silica gels, ammonium sulphate, ammonium phosphate, ammonium nitrate urea, grain meals flours, bark meals, wood meals, nutshell meals, cellulosic powders, ground or powdered plastics and resins, bentonites, zeolites, titanium dioxide, iron oxides and hydroxides, aluminium oxides and hydroxides, or organic materials such as bagasse, charcoal, or synthetic organic polymers.

11. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the humectants is selected from humic acid, glycerol, lactose, and sodium sulphate anhydrous.

12. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the binding agent is selected from sucrose, synthetic and natural gums, synthetic polymers such as poly vinyl acetate, cellulose derivatives-methyl cellulose, EOPO (Ethylene oxide/propylene oxide, polyethylene glycols, polyethylene oxide, polyethoxylated fatty acids or alcohols, sorbitol or urea.

13. The spinosad and insecticide(s) wettable granule composition as claimed in claim 6, wherein the anti-caking agent is selected from amorphous silica, sodium or ammonium phosphates, sodium carbonate/bicarbonate, sodium acetate, sodium metasilicate, magnesium or zinc sulfates, magnesium hydroxide and sodium alkylsulfosuccinates.

14. The spinosad and insecticide(s) wettable granule composition as claimed in claim 1, wherein the process for preparing the composition comprises following steps:
a) taking 3% to 50% w/w spinosad and 1% to 50% w/w one or more insecticide(s) in a blender;
b) adding 0.5% to 2.5% w/w UV photo degradation arrester, 1.5% to 6% w/w wetting-spreading-penetrating agent, 5% to 20% w/w dispersing agent, 0.25% to 1% w/w anti-foaming agent, 30% to 70% w/w carrier, 1% to 10% w/w humectants, 0.5% to 2% w/w binding agent, and 0.2% to 1% w/w anti-caking agent into step a) and mixing it till its complete homogenization;
c) milling the homogenized mixture of step b) till required wet sieve and post blending again for homogeneity;
d) passing the homogenous material obtained in step c) through extruder for granulation;
e) transferring the above prepared granules in step d) through fluid bed dryer to remove excess moisture;
f) transferring the granules to vibro shifter after moisture removal;
g) collecting the final material from the vibro shifter.

Dated this 25th June, 2022