DESC:FIELD OF THE INVENTION:

The present invention relates to synergistic insecticidal composition comprising of Fipronil, Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide. The present invention also relates to the method of preparing the said synergistic composition comprising of Fipronil, Neonicotinoids (Neonics) Clothianidin, Thiamethoxamand at least one more insecticide Cartap, Thiocyclam, Chlorantraniliprole, Flubendiamide.

BACKGROUND OF THE INVENTION

Fipronil is a broad-spectrum insecticide that belongs to the phenylpyrazole chemical family. Fipronil is known as 5-amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-((trifluoromethyl)sulfinyl)-1H-pyrazole-3-carbonitrile, having molecular formula C12H4Cl2F6N4OS. The chemical structure of Fipronil is as below;

EP 295 217 A and EP 352 944 A describe a class of 1-N-arylpyrazole-based insecticides. A particular compound of this class is 5-amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-((trifluoromethyl)sulfinyl)-1H-pyrazole-3-carbonitrile, also known as Fipronil. Fipronil disrupts the insect central nervous system by blocking GABA-gated chloride channels and glutamate-gated chloride channels. Fipronil has proven to be particularly effective as a parasiticide against crop parasites and against mammal ectoparasites, in particular fleas, ticks, flies and myiases.

Neonicotinoids (neonics) are a relatively new type of insecticide, used since many years to control a variety of pests, especially sap-feeding insects.

Neonics are systemic insecticide which are taken up by the plant and transported to all the tissues (leaves, flowers, roots and stems, as well as pollen and nectar). Products containing neonics can be applied at the root (as seed coating or soil drench) or sprayed onto crop foliage. The insecticide toxin remains active in the plant for many weeks, protecting the crop season-long.

Previously people have tried many alternatives and option to overcome this problem and as a result developed poly mixture of insecticide, use of non-toxic ingredients and developing novel formulations which provides effective amount of the insecticide and at the required part only. However the use of poly mixture containing large number of insecticide poses a problem in many was like preparing formulation of multiple insecticides with different chemical properties and behavior and physical properties. It also creates challenge for the formulator in term of compatibility and stability of all the insecticides along with the used excipients in the formulation.

US8404735 describes parasiticidal formulation comprising Fipronil for veterinary use with at least one organic solvent which is not the C1-C6 alcohol co-solvent; and at least one crystallization inhibitor, wherein the total amount of crystallization inhibitor is from 2 to 20% by weight of the formulation.

WO2013126694 discloses a stable, highly-effective topical formulations comprising permethrin, Fipronil and a solvent system that is sufficient to solubilize these two active ingredients and limit degradation of Fipronil to its sulfone, and their uses in topical applications on animals and the environment.

WO2006088653 relates to a method of controlling termites, said method comprising placing at a locus where termite control is needed or expected to be needed, a composition comprising a cellulosic material derived from birch (Betula sp.), a binder, and a termiticide selected from the group consisting of chlorfenapyr, indoxacarb, Fipronil, a pyrethroid and a neonicotinoid.

CN103283769 discloses an insecticidal composition containing dinotefuran, butene-Fipronil and Clothianidin amide. The composition is characterized by taking dinotefuran, butene-Fipronil and Clothianidin amide as effective components, wherein the weight ratio of dinotefuran, butene-Fipronil and Clothianidin amide is 5:3:17. The insecticidal composition provided by the invention taking dinotefuran, butene-Fipronil and Clothianidin amide as the effective components has remarkable synergic effect, and the dosage is reduced while the environmental influence is further reduced.

CN103918698 relates to pesticidal compositions containing Clothianidin and Fipronil and its application in the fight against soil pests. The insecticidal composition comprising the following component parts by weight: 10.0 to 40.0 Clothianidin and Fipronil 2.0 parts to 10.0 parts. Pesticidal compositions containing Clothianidin and Fipronil present invention provides a combination of the two together will be able to give full play to their advantages, can be used to control wireworms and grubs and other soil pests; and a combination of two active ingredients having significant synergies can be achieved to enhance the control effect and delaying resistance role, quick and persistent effectiveness

WO2012101659 describes pesticidal composition comprising an effective amount of a sulphur; an effective amount of at least one insecticide selected from the group consisting of Cartap Fipronil, pirimicarb, buprofezine, thiachloprid, acetamiprid, Clothianidin, diafenthiuron, novaluron, Flubendiamide, spirotetramat, Thiamethoxam, imidacloprid, abamectin, lambda-cyhalothrin or salts thereof, and at least one agrochemically acceptable excipient.

WO2015192717 a synergistic insecticidal composition comprising components (A) at least one neonicotinoid insecticides and (B) at least one pyrethroid insecticides selected from selected from the group consisting of deltamethrin, lambda-cyhalothrin, fenvalerate, permethrin, cypermethrin, bifenthrin, esfenvalerate, etofenprox, cyfluthrin, fenpropathrin, allethrin, cyphenothrin, flucythrinate, flumethrin, imiprothrin, metofluthrin, prallethrin, resmethrin, silafluofen, sumithrin, tefluthrin, tetramethrin, tralomethrin and transluthrin.

However there is no any formulation or composition which can be suitable for targeting insects with effective manner in less concentrated form.

For the reasons mentioned above there does a need to provide further formulation of synergistic combinations comprising Fipronil, Neonicotinoids (Neonics) and at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide having satisfactory insecticidal properties in combination. This object is achieved according to the invention by providing the present composition.

SUMMARY OF THE INVENTION

Accordingly, in a first aspect, the present invention provides a synergistic insecticidal composition comprising (A) Fipronil (B) Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and (C) at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

According to another aspect of the present invention there is provided a synergistic composition comprising (A) 0.1 to 20 % of Fipronil (B) 0.1 to 20 % of Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and (C) 0.1 to 60 % of at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides synergistic insecticidal compositions comprising (A) Fipronil (B) Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and (C) at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

The term “insecticide” or “insecticidal” is similar to “pesticide” or “pesticidal” and is used interchangeably in this whole specification and both convey the same meaning.

Synergism is the cooperative action encountered in combinations of two or more biologically active compounds in which the combined activity of the two or more compounds exceeds the sum of the activities of the compounds when used alone.

The term “Neonicotinoids” and “neonics” conveys the same meaning and can be used interchangeably in this whole specification.

This invention relates to a composition for protecting plants, economically important crops. The present invention relates to plant-protecting active ingredient mixtures having synergistically enhanced action and to a method of improving the health of plants by applying said mixtures to the plants or the locus thereof. One typical problem arising in the Field of pest control lies in the need to reduce the dosage rates of the active ingredient in order to reduce or avoid unfavourable environmental or toxicological effects whilst still allowing effective pest and pathogen control.

Another problem encountered concerns the need to have available pest control agents which are effective against a broad spectrum of pests and pathogens.

Further 3 way mixture type of composition or formulation offers below advantages;
- Provides broad spectrum of insect species control which is not possible with single active.
- Exhibit synergistic activity which increase the effectiveness with low concentration compared to individual active’s effect.
- With 3 active having different mechanism of action, resistant development chances are less and in case resistant is build up for one active, another active can act effectively.
- Reduced work in preparing and applying 3 way mixture compared to preparing 3 individual and applying lead to cost saving and time saving

The present invention relates to a synergistic composition comprising (A) Fipronil (B) Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid and (C) at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

As per one embodiment, the present invention relates to a composition comprising (A) 0.1 to 20 % of Fipronil (B) 0.1 to 20 % of Neonicotinoids (Neonics) ClothianidinThiamethoxamand (C) 0.1 to 60 % of at least one more insecticide CartapThiocyclamChlorantraniliproleFlubendiamideand one or more inactive excipients.

The term "health of a plant" or "plant health" is defined as a condition of the plant and/or its products. As a result of the improved health, yield, plant vigor, quality and tolerance to abiotic or biotic stress are increased. Noteworthy, the health of a plant when applying the method according to the invention, is increased independently of the pesticidal properties of the active ingredients used because the increase in health is not based upon the reduced pest pressure but instead on complex physiological and metabolic reactions which result for example in an activation of the plant's own natural defense system. As a result, the health of a plant is increased even in the absence of pest pressure. Accordingly, in an especially preferred embodiment of the method according to the invention, the health of a plant is increased both in the presence and absence of biotic or abiotic stress factors. The above identified indicators for the health condition of a plant may be interdependent or they may result from each other. An increase in plant vigor may for example result in an increased yield and/or tolerance to abiotic or biotic stress. One indicator for the condition of the plant is the yield. "Yield" is to be understood as any plant product of economic value that is produced by the plant such as grains, fruits in the proper sense, vegetables, nuts, grains, seeds, wood (e.g. in the case of silviculture plants) or even flowers (e.g. in the case of gardening plants, ornamentals). The plant products may in addition be further utilized and/or processed after harvesting.

In an especially preferred embodiment of the invention, the yield of the treated plant is increased.

In another preferred embodiment of the invention, the yield of the plants treated with the composition of invention, is increased synergistically.

According to the present invention, "increased yield" of a plant, in particular of an agricultural, silvicultural and/or horticultural plant means that the yield of a product of the respective plant is increased by a measurable amount over the yield of the same product of the plant produced under the same conditions, but without the application of the mixture according to the invention.

Increased yield can be characterized, among others, by the following improved proper-ties of the plant: increased plant weight, increased plant height, increased biomass such as higher overall fresh weight (FW), increased number of flowers per plant, higher grain yield, more tillers or side shoots (branches), larger leaves, increased shoot growth, increased protein content, increased oil content, increased starch content, increased pigment content, increased leaf are index.

A further indicator for the condition of the plant is the plant vigor. The plant vigor becomes manifest in several aspects such as the general visual appearance. In another especially preferred embodiment of the invention, the plant vigor of the treated plant is increased. In another preferred embodiment of the invention, the plant vigor of the plants treated with the composition of the invention is increased synergistically. Improved plant vigor can be characterized, among others, by the following improved properties of the plant: improved vitality of the plant, improved plant growth, improved plant development, improved visual appearance, improved plant stand (less plant verse/lodging), improved emergence, enhanced root growth and/or more developed root system, enhanced nodulation, in particular rhizobial nodulation, bigger leaf blade, bigger size, increased plant weight, increased plant height, increased tiller number, increased number of side shoots, increased number of flowers per plant, increased shoot growth, increased root growth (extensive root system), increased yield when grown on poor soils or unfavourable climate, enhanced photosynthetic activity (e.g. based on increased stomatal conductance and/or increased C02 assimilation rate), increased stomatal conductance, increased C02 assimilation rate, enhanced pigment content (e.g. chlorophyll content), earlier flowering, earlier fruiting, earlier and improved germination, earlier grain maturity, improved self-defence mechanisms, improved stress tolerance and resistance of the plants against biotic and abiotic stress factors such as fungi, bacteria, viruses, insects, heat stress, cold stress, drought stress, UV stress and/or salt stress, less non-productive tillers, less dead basal leaves, less input needed (such as fertilizers or water), greener leaves, complete maturation under shortened vegetation periods, less fertilizers needed, less seeds needed, easier harvesting, faster and more uniform ripening, longer shelf-life, longer panicles, delay of senescence, stronger and/or more productive tillers, better extractability of ingredients, improved quality of seeds (for being seeded in the following seasons for seed production), better nitrogen uptake, improved reproduction, reduced production of ethylene and/or the inhibition of its reception by the plant.

The improvement of the plant vigor according to the present invention particularly means that the improvement of any one or several or all of the above mentioned plant characteristics are improved independently of the pesticidal action of the mixture or active ingredients (components).

Another indicator for the condition of the plant is the "quality" of a plant and/or its products.
In an especially preferred embodiment of the invention, the quality of the treated plant is increased.

In another preferred embodiment of the invention, the quality of the plants treated with composition of present invention is increased synergistically.

According to the present invention, enhanced quality means that certain plant characteristics such as the content or composition of certain ingredients are increased or improved by a measurable or noticeable amount over the same factor of the plant produced under the same conditions, but without the application of the mixtures of the present invention. Enhanced quality can be characterized, among others, by following improved properties of the plant or its product: increased nutrient content, increased protein content, increased content of fatty acids, increased metabolite content, increased carotenoid content, increased sugar content, increased amount of essential amino acids, improved nutrient composition, improved protein composition, improved composition of fatty acids, improved metabolite composition, improved carotenoid composition, improved sugar composition, improved amino acids composition, improved or optimal fruit color, improved leaf color, higher storage capacity, higher processability of the harvested products.

Another indicator for the condition of the plant is the plant's tolerance or resistance to biotic and/or abiotic stress factors. Biotic and abiotic stress, especially over longer terms, can have harmful effects on plants. Biotic stress is caused by living organisms while abiotic stress is caused for example by environmental extremes. According to the present invention, "enhanced tolerance or resistance to biotic and/or abiotic stress factors" means that certain negative factors caused by biotic and/or abiotic stress are diminished in a measurable or noticeable amount as compared to plants exposed to the same conditions, but without being treated with a mixture according to the invention and that the negative effects are not diminished by a direct action of the mixture according to the invention on the stress factors, e.g. by its fungicidal or insecticidal action which directly destroys the microorganisms or pests, but rather by a stimulation of the plants' own defensive reactions against said stress factors.

As per one embodiment, the composition of present invention is effective to control or manage insect, pests listed below;

Insects from the order of the Lepidoptera, for example Agrotis ypsilon, Alabama argillacea, Anticarsia gemmatalis, Cacoecia murinana, Capua reticulana, Chilo auricilius, Chilo infuscatellus, Chilo partellus, Chilo sacchariphagus, Chilo suppressalis, Choristoneura fumiferana, Choristoneura occidentalis, Cirphis unipuncta, Cnaphalocrocis medinalis, Cydia pomonella, Diatraea saccharalis, Dendrolimus pini, Diaphania nitidalis, Earias vittella, Earias insulana, Elasmopalpus lignosellus, Emmalocera depressella, Eupoecilia ambiguella, Evetria bou-liana, Exelastis atomosa, Feltia subterranea, Galleria mellonella, Grapholitha funebrana, Helicoverpa armigera, Helicoverpa virescens, Helicoverpa zea, Hellula undalis, Hibernia defoliaria, Hyphantria cunea, Hyponomeuta malinellus, Keiferia lycopersicella, Laphygma exigua, Leucinodes orbonalis, Leucoptera coffeella, Leucoptera scitella, Lithocol-letis blancardella, Lobesia botrana, Loxostege sticticalis, Lymantria dispar, Lymantria monacha, Lyonetia clerkella, Malacosoma neustria, Mamestra brassicae, Marasmia pantalis, Maruca vitrata, Maruca testulalis, Mythimna separata, Orgyia pseu-dotsugata, Ostrinia nubilalis, Panolis flammea, Pectinophora gossypiella, Peridroma saucia, Phalera bucephala, Phthorimaea operculella, Phyllocnistis citrella, Pieris bras-sicae, Plathypena scabra, Plutella xylostella, Pseudoplusia includens, Rhyacionia frus-trana, Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata, Scrobipalpula absoluta, Sesamia inferens, Sitotroga cerealella, Sparganothis pilleriana, Spilosoma obliqua, Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Thaumatopoea pityocampa, Tortrix viridana, Trichoplusia ni, Tryporyza novella, Tuta absoluta and Zeiraphera Canadensis. Beetles (Coleoptera), for example Adoretus bicolor, Agrilus sinuatus, Agriotes lineatus, Agriotes obscu-rus, Amphimallus solstitialis, Anisandrus dispar, Anthonomus grandis, Anthonomus pomorum, Anomala benghalensis, Aphthona euphoridae, Apogonia aerea, Athous haemorrhoidalis, Atomaria linearis, Blasto-phagus piniperda, Blitophaga undata, Bruchus rufimanus, Bruchus pisorum, Bruchus lentis, Byctiscus betulae, Cassida nebulosa, Cerotoma trifurcata, Cetonia aurata, Ceuthorrhynchus assimilis, Ceuthorrhynchus napi, Chaetocnema tibialis, Chiloloba acuta, Conoderus vespertinus, Crioceris asparagi, Ctenicera ssp., Diabrotica longicornis, Diabrotica semipunctata, Diabrotica punctata, Diabrotica speciosa, Diabrotica virgifera, Dicladispa armigera, Epila-chna varivestis, Epitrix hirtipennis, Eutinobothrus brasiliensis, Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Hylobius abietis, Hypera brunneipennis, Hypera postica, Ips typographus, Lema bilineata, Lema melanopus, Leptinotarsa decemlineata, Lepidiota stigma, Limonius califomicus, Lissorhoptrus oryzophilus, Maladera indica, Melanotus communis, Meligethes aeneus, Melolontha hippocastani, Melolontha melolontha, Oberea brevis, Oulema oryzae, Ortiorrhynchus sulcatus, Otiorrhynchus ovatus, Phaedon cochleariae, Phyllobius pyri, Phyllotreta chrysocephala, Phyllophaga sp., Phyllopertha horticola, Phyllotreta nemorum, Phyllotreta striolata, Popillia japonica, Sitona lineatus and Sito-philus gran aria, flies, mosquitoes (Diptera), e.g. Atherigona orientalis, Calliphora vicina, Ceratitis capitata, Chrysomya bezziana, Chrysomya hominivorax, Chrysomya macellaria, Chrysops discalis, Chrysops silacea, Chrysops atlanticus, Cochliomyia hominivorax, Contarinia sorghicola Cordylobia anthropophaga, Culicoides furens, Culiseta inornata, Culiseta melanura, Dacus cucurbi-tae, Dacus oleae, Dasineura brassicae, Delia antique, Delia coarctata, Delia platura, Delia radicum, Dermatobia hominis, Fannia canicularis, Geomyza Tripunctata, Gaster-ophilus intestinalis, Glossina morsitans, Glossina palpalis, Glossina fuscipes, Glossina tachinoides, Haematobia irritans, Haplodiplosis equestris, Hippelates spp., Hylemyia platura, Hypoderma lineata, Leptoconops torrens, Liriomyza sativae, Liriomyza trifolii, Lucilia caprina, Lucilia cuprina, Lucilia sericata, Lycoria pectoralis, Mansonia titillanus, Mayetiola destructor, Melanagromyza obtuse, Muscina stabulans, Oestrus ovis, Ophiomyia phaseli, Opomyza florum, Orseolia oryzae, Oscinella frit, Pegomya hysocyami, Phorbia antiqua, Phorbia brassicae, Phor-bia coarctata, Phlebotomus argentipes, Psorophora columbiae, Psila rosae, Psoro-phora discolor, Prosimulium mixtum, Rhagoletis cerasi, Rhagoletis pomonella, Sar-cophaga haemorrhoidalis, Sarcophaga sp., Simulium vittatum, Stomoxys calcitrans, Tabanus bovinus, Tabanus atratus, Tabanus lineola, and Tabanus similis, Tipula ol-eracea, and Tipula paludosa, thrips (Thysanoptera), e.g. Dichromothrips corbetti, Dichromothrips ssp , Frankliniella fusca, Frankliniella occidentalis, Frankliniella tritici, Scirtothrips citri, Scirtothrips dorsalis, Thrips oryzae, Thrips palmi and Thrips tabaci, termites (Isoptera), e.g. Calotermes flavicollis, Coptotermes formosanus, Heterotermes aureus, Leucotermes flavipes, Microtermes obesi, Odontotermes obesus, Reticulitermes flavipes, Termes natalensis. cockroaches (Blattaria - Blattodea), e.g. Blattella germanica, Penplaneta americana, Periplaneta japonica and Blatta orientalis, true bugs (Hemiptera), e.g. Acrosternum hilare, Acyrtho-siphon pisum, Acyrthosiphon onobrychis, Adelges laricis, Aleurolobus barodensis, Amrasca biguttula biguttula, Amrasca devastans, Amritodus atkinsoni, Aphidula nasturtii, Aphis fabae, Aphis forbesi, Aphis pomi, Aphis gossypii, Aphis crassivora, Aphis grossulariae, Aphis schneideri, Aphis spiraecola, Aphis sambuci, Aulacorthum solani, Bemisia argentifolii, Bemisia tabaci, Brachycaudus cardui, Brachy-caudus helichrysi, Brachycaudus persicae, Brachycaudus prunicola, Brevicoryne brassicae, Capitophorus horni, Cavalerius sweeti, Cerosipha gossypii, Ceratovacuna lanigera, Chaetosiphon fragaefolii, Cicadulina spp., Clavigralla gibbosa, Cryptomyzus ribis, Dreyfusia nordmannianae, Dreyfusia piceae, Dysdercus cingulatus, Dysaphis radicola, Dysaulacorthum pseudosolani, Dysaphis plantaginea, Dysaphis pyri, Empoasca fabae, Hyalopterus pruni, Hyperomyzus lactucae, Idioscopus spp. Leptoglossus phyllopus, Leptocorisa acuta, Lygus lineolaris, Lygus pratensis, Macrosiphum avenae, Macrosiphum euphorbiae, Ma-crosiphon rosae, Megoura viciae, Melanaphis pyrarius, Metopolophium dirhodum, My-zus persicae, Myzus ascalonicus, Myzus cerasi, Myzus varians, Nezara viridula, Nasonovia ribis-nigri, Nilaparvata lugens, Nephotettix virescens, Nephotettix nigropictus, Pemphigus bursarius, Perkinsiella saccharicida, Peregrinus maidis, Phorodon humuli, Planococcus spp., Pseudococcus spp., Pyrilla perpusilla, Psylla mail, Psylla piri, Rhopalomyzus ascalonicus, Rhopalosiphum maidis, Rhopalosi-phum padi, Rhopalosiphum insertum, Saccharicoccus sacchari, Sappaphis mala, Sappaphis mail, Schizaphis graminum, Schizoneura lanuginosa, Sitobion avenae, Sogatella furcifera, Trialeurodes vaporariorum, Toxoptera aurantiia, Psylla spp., Rhopalosiphum spp., Sitobion spp., ants, bees, wasps, sawflies (Hymenoptera), e.g. Athalia rosae, Atta cephalotes, Atta capiguara, Atta cephalotes, Atta laevigata, Atta robusta, Atta sexdens, Atta texana, Crematogaster spp., Hoplocampa minuta, Hoplocampa testudinea, Monomorium pha-raonis, Solenopsis geminata, Solenopsis invicta, Solenopsis richteri, Solenopsis xyloni, Pogonomyrmex barbatus, Pogonomyrmex californicus, Pheidole megacephala, Dasy-mutilla occidentalis, Bombus spp. Vespula squamosa, Paravespula vulgaris, Paraves-pula pennsylvanica, Paravespula germanica, Dolichovespula maculata, Vespa crabro, Polistes rubiginosa, Camponotus floridanus, and Linepithema humile, crickets, grasshoppers, locusts (Orthoptera), e.g. Acheta domestica, Gryllotalpa gryllo-talpa, Locusta migratoria, Melanoplus bivittatus, Melanoplus femurrubrum, Melanoplus mexicanus, Melanoplus sanguinipes, Melanoplus spretus, Nomadacris septemfasciata, Schistocerca americana, Schistocerca gregaria, Dociostaurus maroccanus, Tachycines asynamorus, Oedaleus senegalensis, Zonozerus variegatus, Hieroglyphus daganensis, Kraussaria angulifera, Calliptamus italicus, Chortoicetes terminifera, and Locustana pardalina, Arachnoidea, such as arachnids (Acarina), e.g. of the families Argasidae, Ixodidae and Sarcoptidae, such as Amblyomma americanum, Amblyomma variegatum, Ambryomma maculatum, Argas persicus, Boophilus annulatus, Boophilus decoloratus, Boophilus microplus, Dermacentor silvarum, Dermacentor andersoni, Dermacentor variabilis, Hyalomma truncatum, Ixodes ricinus, Ixodes rubicundus, Ixodes scapularis, Ixodes holocyclus, Ixodes pacificus, Ornithodorus moubata, Ornithodorus hermsi, Ornithodo-rus turicata, Ornithonyssus bacoti, Otobius megnini, Dermanyssus gallinae, Psoroptes ovis, Rhipicephalus sanguineus, Rhipicephalus appendiculatus, Rhipicephalus evertsi, Sarcoptes scabiei, and Eriophyidae spp. such as Aculus schlechtendali, Phyllocoptrata oleivora and Eriophyes sheldoni; Tarsonemidae spp. such as Phytonemus pallidus and Polyphagotarsonemus latus; Tenuipalpidae spp. such as Brevipalpus phoenicis; Tetra-nychidae spp. such as Tetranychus cinnabarinus, Tetranychus kanzawai, Tetranychus pacificus, Tetranychus telarius and Tetranychus urticae, Panonychus ulmi, Panony-chus citri, and Oligonychus pratensis; Araneida, e.g. Latrodectus mactans, and Loxos-celes reclusa, fleas (Siphonaptera), e.g. Ctenocephalides felis, Ctenocephalides canis, Xenopsylla cheopis, Pulex irritans, Tunga penetrans, and Nosopsyllus fasciatus, silverfish, firebrat (Thysanura), e.g. Lepisma saccharina and Thermobia domestica,centipedes (Chilopoda), e.g. Scutigera coleoptrata, millipedes (Diplopoda), e.g. Narceus spp., Earwigs (Dermaptera), e.g. forficula auricularia, lice (Phthiraptera), e.g. Pediculus humanus capitis, Pediculus humanus corporis, Pthi-rus pubis, Haematopinus eurystemus, Haematopinus suis, Linognathus vituli, Bovicola bovis, Menopon gallinae, Menacanthus stramineus and Solenopotes capillatus. Plant parasitic nematodes such as root-knot nematodes, Meloidogyne arenaria, Meloi-dogyne chitwoodi, Meloidogyne exigua, Meloidogyne hapla, Meloidogyne incognita, Meloidogyne javanica and other Meloidogyne species; cyst nematodes, Globodera rostochiensis, Globodera pallida, Globodera tabacum and other Globodera species, Heterodera avenae, Heterodera glycines, Heterodera schachtii, Heterodera trifolii, and other Heterodera species; seed gall nematodes, Anguina funesta, Anguina tritici and other Anguina species; stem and foliar nematodes, Aphelenchoides besseyi, Aphelen-choides fragariae, Aphelenchoides ritzemabosi and other Aphelenchoides species; sting nematodes, Belonolaimus longicaudatus and other Belonolaimus species; pine nematodes, Bursaphelenchus xylophilus and other Bursaphelenchus species; ring ne-matodes, Criconema species, Criconemella species, Criconemoides species, and Me-socriconema species; stem and bulb nematodes, Ditylenchus destructor, Ditylenchus dipsaci, Ditylenchus myceliophagus and other Ditylenchus species; awl nematodes, Dolichodorus species; spiral nematodes, Helicotylenchus dihystera, Helicotylenchus multicinctus and other Helicotylenchus species, Rotylenchus robustus and other Roty-lenchus species; sheath nematodes, Hemicycliophora species and Hemicriconemoides species; Hirshmanniella species; lance nematodes, Hoplolaimus columbus, Hoplolai-mus galeatus and other Hoplolaimus species; false root-knot nematodes, Nacobbus aberrans and other Nacobbus species; needle nematodes, Longidorus elongates and other Longidorus species; pin nematodes, Paratylenchus species; lesion nematodes, Pratylenchus brachyurus, Pratylenchus coffeae, Pratylenchus curvitatus, Pratylenchus goodeyi, Pratylencus neglectus, Pratylenchus penetrans, Pratylenchus scribneri, Pratylenchus vulnus, Pratylenchus zeae and other Pratylenchus species; Radinaphelenchus cocophilus and other Radinaphelenchus species; burrowing nematodes, Radopholus similis and other Radopholus species; reniform nematodes, Rotylenchulus reniformis and other Rotylenchulus species; Scutellonema species; stubby root nematodes, Tri-chodorus primitivus and other Trichodorus species; Paratrichodorus minor and other Paratrichodorus species; stunt nematodes, Tylenchorhynchus claytoni, Tylenchorhyn-chus dubius and other Tylenchorhynchus species and Merlinius species; citrus nematodes, Tylenchulus semipenetrans and other Tylenchulus species; dagger nematodes, Xiphinema americanum, Xiphinema index, Xiphinema diversicaudatum and other Xi-phinema species; and other plant parasitic nematode species.

The inventive composition of present invention can be applied to any and all developmental stages of pests, such as egg, larva, pupa, and adult. The pests may be controlled by contacting the target pest, its food supply, habitat, breeding ground or its locus with a pesticidally effective amount of the inventive mixtures or of compositions comprising the mixtures.

The inventive composition of present invention are highly effective in controlling insect pests, In Sugarcane crop- Termites Odontotermes spp., Coptotermes spp., Heterotermes spp., Leucotermes spp., Microtermes obesi, Whitegrub, Holotrichia consanguinea, Holotrichia serrata, Maladera insanabilis, Brahmina spp., Melolontha spp., Lepidiota spp., Anomala spp., Phyllognathus spp., Leucopholis spp., Wireworms, Limonius spp., Agriotes spp., Early shoot borer Chilo infuscatellus, Pink borer Sesamia inferens, Top shoot borer Scirpophaga excerptalis, Root borer Emmalocera depressella, Internode borer: Chilo sacchariphagus indicus, Stalk borer Chilo auricilius, White woolly aphid Ceratovacuna lanigera, Black bug Cavelerius sweeti, Whitefly Aleurolobus barodensis, Pyrilla Pyrilla perpusilla, Mealybug Saccharicoccus sacchari. In rice/paddy crop- Termites, root weevil Lissorhoptus oryzophilus, Echinocnemus oryzae, Hydronomodius molitor, stem borer, Chilo suppressalis, Schirpophaga incertulas, Sesamia inferens, Hoppers, Nilaparvata lugens, Sogatella furcifella, Nephotettix nigropictus, Gall midge, Orseolia oryzae, Leaffolder Cnaphalocrocis medinalis, Rice bug, Leptocorisa spp., Stink bug, Nezara spp., Rice Hispa, Dicladispa armigera, Caseworm Nymphula depuctalis, whorl maggot, Hydrellia spp., black bug, Scotinophara coarctata, armyworm, Mythimna separate, Mole cricket Gryllotalpa spp., Stem maggot, Chlorops oryzae and soil earthworm (oligochaeta).

The list of crops which can be suitable for protection by the present formulation are GMO (Genetically Modified Organism) and Non GMO varieties of Cotton (Gossypium spp.), Jute (Corchorus oliotorus), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Ragi (Eleusine coracana), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum) , Sugarbeet (Beta vulgaris), Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Castor (Ricinus communis), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (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), 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 subsp rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), 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), Fenugreek (Trigonella foenum-graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), 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).

The concentration of (A) Fipronil (B) Neonicotinoids (Neonics) ClothianidinThiamethoxamand (C) at least one more insecticide CartapThiocyclamChlorantraniliproleFlubendiamidedepends on many factors, including the type and the occurrence of the pests to be controlled. For each application, the optimum ratios and total amounts to be employed can in each case be determined by routine experimentation.

The present invention was arrived after experiments and trials to arrive to an effective and yet safe composition with different active ingredients.

An “effective amount” is an amount of active ingredient or a combination of active ingredients that is effective to prevent or reduce damage to a plant caused by any pest or to repel, deter or destroy a pest or to cause an adverse effect to an individual insect or an insect population, including, for example, deviations from natural development, killing, regulation, and the like. Suitable adjuvants or carriers should not be phytotoxic to valuable crops, particularly at the concentrations employed in applying the compositions for pest control in the presence of crops, and should not react chemically with pesticidal components of the mixture or other composition ingredients.

The composition of present invention can be in the form of Suspension Concentrate (SC), Suspo emulsion (SE), Capsule Suspension (CS), Oil Dispersion (OD), mixed formulation of CS and SC (ZC), a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granules (Soil Applied Granules), Controlled Release Granules (CR Granules), Slow release and Fast release microsphere Granules (MS Granules), Water Soluble Granules (SG), Water dispersible granule (WDG or WG), Jumbo ball formulation, Water soluble bag formulation, Wettable Powder (WP), Soluble Powder (SP).

In a preferred embodiment, the composition of present invention is selected from Water dispersible Granules (WG), Water Soluble Granules (SG), Controlled release granules (CR) and Suspension concentrate (SC).

As per one embodiment, the present invention composition is to be applied by any of below mentioned application method:

Broadcasting provides effective control of the flow of Granules such as Controlled Release Granules (CR), Slow release and Fast release Microsphere Granules (MS) by manually (by hand), power operated granules spreader, by machine operated soil granules spreader. It can be a sand mix or fertilizer mix broadcasting. Broadcasting can be done before or after crop sowing, planting or transplanting or at the time of land preparation. In sugarcane, broadcasting can be done manually by mixing it with sand or fertilizer and by spreading over cane sett, in open furrow before covering it with soil at the time of planting. In rice, broadcasting can be done manually by mixing it with sand or fertilizer after transplanting the crop.

Seed treatment to seeds, plant propagating materials, Foliar application / spraying, Soil drenching, Through drip irrigation, Nursery bed application, mixing in to soil or other plant growing media in protected cultivations, green houses, net houses, poly houses.

As per one embodiment of the invention, the % w/w of the different active ingredients are as listed in below:

% of components varies from
(A) Fipronil (B) Neonicotinoids (C) Insecticides
Fipronil Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid Cartap Hydrochloride Thiocyclam
Bifenthrin
Chlorpyrifos Chlorantraniliprole
Flubendiamide

0.1 to 20% 0.1 to 20 % 0.1 to 60%

Inactive excipient or customary adjuvants, that are often used in agrochemical compositions, and that can be included in various compositions described herein, include, but are not limited to, dispersing agents, wetting agent, antifoam agents, biocide, anti-freezing agent, suspension aid, thickening agents (also referred to as “thickeners”), quick coating agent or sticking agents (also referred to as “stickers” or “binders”),

A dispersant is a substance which adsorbs onto the surface of particles and helps to preserve the state of dispersion of the particles and prevents them from re-aggregating. Dispersants are added to agrochemical formulations to facilitate dispersion and suspension during manufacture, and to ensure the particles re-disperse into water in a spray tank. They are widely used in wettable powders, suspension concentrates and water-dispersible granules. Surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier to re-aggregation of particles. The most commonly used surfactants are anionic, non-ionic, or mixtures of the two types. For wettable powder formulations, the most common dispersants are sodium lignosulphonates. For suspension concentrates, very good adsorption and stabilization are obtained using polyelectrolytes, such as sodium naphthalene sulphonate formaldehyde condensates. Tristyrylphenolethoxylate phosphate esters are also used. Non-ionics such as alkylarylethylene oxide condensates and EO-PO block copolymers are sometimes combined with anionics as dispersants for suspension concentrates. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. These have very long hydrophobic ‘backbones’ and a large number of ethylene oxide chains forming the ‘teeth’ of a ‘comb’ surfactant. These high molecular weight polymers can give very good long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces. Examples of dispersants used herein include but not limited to sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenolethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers or mixtures thereof.

Anti-freezing agent as used herein can be selected from the group consisting of polyethylene glycols, methoxypolyethylene glycols, polypropylene glycols, polybutylene glycols, glycerin and ethylene glycol.

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. Generally, there are two types of anti-foam agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.

A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading. Wetting agents are used for two main functions in agrochemical formulations: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules. Examples of wetting agents used in wettable powder, suspension concentrate, and water-dispersible granule formulations include but not limited to sodium lauryl sulphate; sodium dioctylsulphosuccinate; alkyl phenol ethoxylates; and aliphatic alcohol ethoxylates or mixtures thereof.

Suspension aid in the present description 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. This carrier is hence generally inert, and it must be agriculturally acceptable, in particular to the plant being treated. The carrier may be solid (clays, natural or synthetic silicates, silica, resins, waxes, solid fertilizers, and the like or mixtures thereof) or liquid (water, alcohols, ketones, petroleum fractions, aromatic or paraffinic hydrocarbons, chlorinated hydrocarbons, liquefied gases, and the like or mixtures thereof).

Biocides / Microorganisms cause spoilage of formulated products. Therefore anti-microbial agents are used to eliminate or reduce their effect. Examples of such agents include, but are not limited to: propionic acid and its sodium salt; sorbic acid and its sodium or potassium salts; benzoic acid and its sodium salt; p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates or mixtures thereof.

Thickeners or gelling agents are used mainly in the formulation of suspension concentrates, emulsions and suspoemulsions to modify the rheology or flow properties of the liquid and to prevent separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixtures.

The quick coating agent can be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, polsaccharides such as starch and cellulose derivatives, vinylal- cohol, vinylacetate and vinylpyrrolidone polymers and copolymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymersand mixtures thereof. Examples of preferred polymers are acrylate polymers such as poly(methacrylate), poly( ethyl methacrylate ), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below , poly(styrene-co maleic anhydride), cellulosic polymers such as ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono-, di-, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), alkyd resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present method include biodegradable polyesters, starch, polylactic acid -starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch ester aliphatic polyester blends, modified corn starch, polycaprolactone, poly(n-amylmethacrylate), wood rosin, polyan- hydrides, polyvinylalcohol, polyhydroxybutyrate-valerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof.

Buffering agent as used herein is selected from group consisting of calcium hydroxyapatite, Pottasium Dihydrogen Phosphate, Sodium Hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphates, amine monomers, lactate dehydrogenase and magnesium hydroxide.

The solvent for the formulation of the present invention may include water, water-soluble alcohols and dihydroxy alcohol ethers. The water-soluble alcohol which can be used in the present invention may be lower alcohols or water-soluble macromolecular alcohols. The term "lower alcohol", as used herein, represents an alcohol having 1-4 carbon atoms, such as methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol, etc. Macromolecular alcohol is not limited, as long as it may be dissolved in water in a suitable amount range, e.g., polyethylene glycol, sorbitol, glucitol, etc. The examples of suitable dihydroxy alcohol ethers used in the present invention may be dihydroxy alcohol alkyl ethers or dihydroxy alcohol aryl ethers. The examples of dihydroxy alcohol alkyl ether include ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, dipropylene glycol ethyl ether, etc. The examples of dihydroxy alcohol aryl ethers include ethylene glycol phenyl ether, diethylene glycol phenyl ether, propylene glycol phenyl ether, dipropylene glycol phenyl ether, and the like. Any of the above mentioned solvent can be used either alone or in combination thereof.

The process for preparing the present insecticidal composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the composition. However all such variation and modification is still covered by the scope of present invention.

EXAMPLES

Example 1: Fipronil 0.5%+Clothianidin 1%+Cartap hydrochloride 5% CR Granules (Controlled Release Granules)

chemical composition % (w/w)
FFipronil a.i. 0.50
CClothianidin a.i. 1.00
CCartap hydrochloride a.i. 5.00
Polyaryl phenol ethoxylate & calcium dodecyl benzene solphonate Blend 1.00
Phosphoric acid 0.05
Polycarboxylates 1.00
Diacetone alcohol 2.00
Urea Formaldehyde resin 2.50
Polyvinyl pyrrolidone 0.50
China Clay 5.00
River sand Q.S.
TOTAL 100.00

Procedure:

Step 1 Charge required quantity of filler in booth mixer.
Step 2 Charge required quantity of technical material and homogenise.
Step 3 Now spray solution of binding agents and slowly in atomized form.
Step 4 Homogenise and dry the the material to form irregular granules of spherical shape
Step 5 Now add required quantity of filler and spray remaining binding agent.
Step 6 Homogenise and send sample to lab for final analysis.

Storage stability data:

Storage stability Study-Fipronil 0.5%+Clothianidin 1%+Cartap hyrdrochloride 5% CGR (Controlled Release Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
FFipronil content percent by mass 0.48 to 0.55 0.54 0.52 0.54
CClothianidin content percent by mass 0.95 to 1.1 1.05 1.03 1.04
CCartap hydrochloride content percent by mass 4.75 to 5.5 5.08 5.06 5.08
pH (1% in DM water) 6 to 8 7.11 7.08 7.11
bulk Density (g/ml) 0.4 to 0.8 0.58 0.58 0.58
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
FFipronil content percent by mass 0.48 to 0.55 0.54 0.54 0.53
CClothianidin content percent by mass 0.95 to 1.1 1.05 1.05 1.04
CCartap hydrochloride content percent by mass 4.75 to 5.5 5.08 5.08 5.07
pH (1% in DM water) 6 to 8 7.11 7.10 7.09
bulk Density (g/ml) 0.4 to 0.8 0.58 0.58 0.58
moisture content max. 2% 1.10% 1.01% 1.02%

Example 2: Fipronil 0.5%+Clothianidin 1%+thiocylam hydrogen oxalate 5% CR Granules (Controlled Release Granules)

chemical composition % (w/w)
FFipronil a.i. 0.50
CClothianidin a.i. 1.00
TThiocyclam hydrogen oxalate a.i. 5.00
Polyaryl phenol ethoxylate & calcium dodecyl benzene solphonate Blend 1.00
Phosphoric acid 0.05
Polycarboxylates 1.00
Diacetone alcohol 2.00
Urea formaldehyde resin 2.00
Polyvinyl pyrrolidone 0.50
China Clay 5.00
River sand Q.S.
TOTAL 100.00

Procedure: As per Example 1

Storage stability data:

Storage stability Study-Fipronil 0.5%+Clothianidin 1%+Thiocyclam hydrogen oxalate 5% CGR (Controlled Release Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
FFipronil content percent by mass 0.48 to 0.55 0.53 0.51 0.53
CClothianidin content percent by mass 0.95 to 1.1 1.06 1.04 1.05
TThiocyclam hydrogen oxalate content percent by mass 4.75 to 5.5 5.11 5.09 5.10
pH (1% in DM water) 6 to 8 7.05 7.01 7.03
bulk Density (g/ml) 0.4 to 0.8 0.58 0.58 0.58
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
FFipronil content percent by mass 0.48 to 0.55 0.53 0.53 0.52
CClothianidin content percent by mass 0.95 to 1.1 1.06 1.06 1.05
TThiocyclam hydrogen oxalate content percent by mass 4.75 to 5.5 5.11 5.10 5.10
pH (1% in DM water) 6 to 8 7.05 7.04 7.05
bulk Density (g/ml) 0.4 to 0.8 0.58 0.58 0.58
moisture content max. 2% 1.20% 1.15% 1.12%

Example 3: FFipronil 5%+CClothianidin 10%+CCartap hydrochloride 50% SG (soluble granules)

chemical composition % (w/w)
Fipronil a.i. 5.00
Clothianidin a.i. 10.00
Cartap hydrochloride a.i. 50.00
Polycarboxylates 5.00
Sodium lauryl sulfate 3.00
silicon antifoam 0.50
Lactose 10.00
Corn Starch Q.S.
TOTAL 100.00

Procedure:
Step 1 Charge required quantity of all ingredients in ribbon blender.
Step 2 Homogenise material for 20 minutes to achieve homogeneous powder.
Step 3 Pass this homogenised material through hammer mill/ pin mill to reduce particle size.
Step 4 Homogenise grinder material for another 20 minutes.
Step 5 Send homogenised sample to QC lab for approval.
Step 6 Once material is approved from QC add required quantity of moisture for dough formation.
Step 7 Pass this dough through basket extruder to produce water soluble granules.
Step 8 Send final sample to QC for approval.

Storage stability data:

Storage stability Study-Fipronil 5%+Clothianidin 10%+Cartap hydrochloride 50% SG (Soluble Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
FFipronil content percent by mass 4.75 to 5.5 5.26 5.21 5.24
CClothianidin content percent by mass 9.5 to 10.5 10.25 10.22 10.25
CCartap hydrochloride content percent by mass 47.5 to 52.5 50.41 50.36 50.39
pH 6 to 8 7.05 7.07 7.05
bulk Density (g/ml) 0.40 to 0.8 0.55 0.55 0.55
moisture Content max. 2% 1.1 0.9 1.1
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
FFipronil content percent by mass 4.75 to 5.5 5.26 5.25 5.24
CClothianidin content percent by mass 9.5 to 10.5 10.25 10.24 10.24
CCartap hydrochloride content percent by mass 47.5 to 52.5 50.41 50.39 50.38
pH (1% in DM water) 6 to 8 7.05 7.05 7.06
bulk Density (g/ml) 0.40 to 0.8 0.55 0.55 0.55
moisture Content max. 2 % 1.1 1 1

Example 4: FFipronil 5%+CClothianidin 10%+ CChlorantraniliprole 5% WG (Water dispersible granules)

chemical composition % (w/w)
FFipronil a.i. 5.00
CClothianidin a.i. 10.00
CChlorantraniliprole a.i. 5.00
Alkylated naphthalene sulfonate, sodium salt 6.00
Polyacrylate polymer sodium salt 3.00
Sodium alkyl naphthalene sulfonate blend 2.00
Silicone antifoam 1.00
Lactose 10.00
Corn starch 20.00
China Clay Q.S.
TOTAL 100.00

Procedure:
Step 1 Charge the required quantity of filler, wetting agent, dispersing agent, and suspending agent, & technical in premixing blender for homogenization for 30 minutes.
Step 2 Pre-blended material is than grinded through Jet mill/ air classifier mills. Finely grinded material is blended in post blender till it becomes homogeneous. (for approx.. 1.5 hr)
Step 3 Homogeneous material is analysed. After getting approval from QC dept. material is unloaded into 25 kg. HDPE bag with LDPE liner inside.
Step 4 Finely grinded powder is mixed with required quantity of water to form extrudable dough.
Step 5 Dough is passed through extruder to get granules of required size.
Step 6 Wet granules are passed through Fluidised bed drier and further graded using vibrating screens.
Step 7 Final product is sent for QC approval.
Step 8 After approval material is packed in required pack sizes.

Storage stability data:

Storage stability Study-Fipronil 5%+Clothianidin 10%+Chlorantraniliprole 5% WG (Water Dispersible Granules)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
FFipronil content percent by mass 4.75 to 5.5 5.12 5.05 5.11
CClothianidin contnet percent by mass 9.5 to 10.5 10.06 10.04 10.06
CChlorantraniliprole content percent by mass 4.75 to 5.5 5.16 5.10 5.15
FFipronil suspensibility percent min. 70 96.85 93.15 96.31
CClothianidin suspensibility percent min. 70 95.62 92.41 95.22
CChlorantraniliprole suspensibility percent min. 70 96.26 93.69 94.06
pH range (1% aq. Suspension) 5.5 to 7.5 7.06 7.02 7.05
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.2 99.1 99.2
bulk density (g/ml) 0.4 to 0.8 0.47 0.47 0.47
moisture content percent by mass max. max. 2% 1.2 0.8 1.1
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
FFipronil content percent by mass 4.75 to 5.5 5.12 5.11 5.1
CClothianidin contnet percent by mass 9.5 to 10.5 10.06 10.05 10.05
CChlorantraniliprole content percent by mass 4.75 to 5.5 5.16 5.15 5.14
FFipronil suspensibility percent min. 70 96.75 96.61 95.26
CClothianidin suspensibility percent min. 70 95.25 95.01 93.96
CChlorantraniliprole suspensibility percent min. 70 95.87 94.56 94.15
pH range (1% aq. Suspension) 5.5 to 7.5 7.06 7.05 7.04
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.2 99.2 99.1
bulk density (g/ml) 0.4 to 0.8 0.47 0.47 0.47
moisture content percent by mass max. max. 2% 1.2 1.1 1

Example 5: FFipronil 5%+CClothianidin 10%+ FFlubendiamide 7.5% WG (Water Dispersible granules)

chemical composition % (w/w)
FFipronil a.i. 5.00
CClothianidin a.i. 10.00
FFlubendiamide a.i. 7.50
Alkylated naphthalene sulfonate, sodium salt 6.00
Polyacrylate polymer sodium salt 3.00
Sodium alkyl naphthalene sulfonate blend 2.00
Silicone antifoam 1.00
Lactose 10.00
Corn starch 20.00
China Clay Q.S.
TOTAL 100.00

Procedure: As per Example 4

Storage stability data:

Storage stability Study-FFipronil 5%+CClothianidin 10%+FFlubendiamide 7.5% WG (Water Dispersible Granules)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
FFipronil content percent by mass 4.75 to 5.5 5.18 5.14 5.17
CClothianidin contnet percent by mass 9.5 to 10.5 10.28 10.22 10.26
FFlubendiamide content percent by mass 7.13 to 8.25 7.62 7.59 7.62
FFipronil suspensibility percent min. 70 97.51 93.54 96.59
CClothianidin suspensibility percent min. 70 97.45 93.11 96.36
FFlubendiamide suspensibility percent min. 70 96.17 91.52 95.69
pH range (1% aq. Suspension) 5.5 to 7.5 7.06 7.03 7.06
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.2 99.1 99.2
bulk density (g/ml) 0.4 to 0.8 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.2 0.8 1.2
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
FFipronil content percent by mass 4.75 to 5.5 5.18 5.18 5.16
CClothianidin contnet percent by mass 9.5 to 10.5 10.27 10.27 10.25
FFlubendiamide content percent by mass 7.13 to 8.25 7.62 7.61 7.61
FFipronil suspensibility percent min. 70 97.24 96.52 96.03
CClothianidin suspensibility percent min. 70 97.11 96.33 95.56
FFlubendiamide suspensibility percent min. 70 95.69 95.61 95.12
pH range (1% aq. Suspension) 5.5 to 7.5 7.06 7.06 7.05
wettability sec. max. 60 8 8 9
wet sieve (45 micron) percent by mass min. 98.5 99.2 99.2 99.1
bulk density (g/ml) 0.4 to 0.8 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.2 1.1 1

Example 6: FFipronil 5%+CClothianidin 10%+ CChlorantraniliprole 5% SC (suspension concentrate)

chemical composition % (w/w)
Fipronil a.i. 5.00
Clothianidin a.i. 10.00
Chlorantraniliprole a.i. 5.00
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
D.M. Water Q.S.
TOTAL 100.00

Procedure:
Step 1 Gum Solution should be made 12-18 hour prior to use. Take required quantity of water, biocide, and defoamer and homogenise, then slowly add gum powder to it and stir till complete dissolution.
Step 2 Charge required quantity of DM water need to be taken in designated vessel for Suspension concentrate production.
Step 3 Add required quantity of Wetting agent, antifreeze, dispersing agent & suspending agents and homogenise the contents for 45 – 60 minutes using high shear homogeniser.
Step 4 Then add technical and other remaining adjuvants excluding ‘thickener’ are added to it and homogenised to get uniform slurry ready for grinding.
Step 5 Before grinding half the quantity of antifoam was added and then material was subjected to grinding in Dyno mill till desired particle size is achieved.
Step 6 Half quantity of the antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7 Finally add gum solution to this formulation and send to QC for quality check.

Storage stability data:

Storage stability Study-FFipronil 5%+CClothianidin 10%+CChlorantraniliprole 5% SC (Suspension Concentrate)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.13 5.09 5.12
Clothianidin contnet percent by mass 9.5 to 10.5 10.28 10.16 10.28
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.19 5.14 5.17
Fipronil suspensibility percent min. 80 98.52 96.51 97.88
Clothianidin suspensibility percent min. 80 98.14 95.28 96.16
Chlorantraniliprole suspensibility percent min. 80 99.11 96.25 98.5
pH range (1% aq. Suspension) 5.5 to 7.5 6.99 6.97 6.99
pourability 95% min. 97.5 97.1 97
specific gravity 1.05-1.15 1.07 1.07 1.07
viscosity at spindle no. 62, 20 rpm 350-800 cps 450 455 490
particle size (micron) D50<3, D90<10 2.2,8.1 2.7,8.5 2.5,8.3
persistent foam ml (after 1 minute) max. 60 2 5 2
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.13 5.13 5.12
Clothianidin contnet percent by mass 9.5 to 10.5 10.28 10.27 10.25
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.19 5.17 5.16
Fipronil suspensibility percent min. 80 98.38 98.31 98.1
Clothianidin suspensibility percent min. 80 98.05 97.82 97.5
Chlorantraniliprole suspensibility percent min. 80 99.02 98.78 98.25
pH range (1% aq. Suspension) 5.5 to 7.5 6.99 6.98 6.98
pourability 95% min. 97.5 97.5 97.4
specific gravity 1.05-1.15 1.07 1.07 1.07
viscosity at spindle no. 62, 20 rpm 350-800 cps 450 451 453
particle size (micron) D50<3, D90<10 2.2,8.1 2.2,8.1 2.3,8.5
persistent foam ml (after 1 minute) max. 60 2 2 3

Example 7: Fipronil 5%+Clothianidin 10%+ Flubendiamide 7.5% SC (suspension concentrate)

chemical composition % (w/w)
Fipronil a.i. 5.00
Clothianidin a.i. 10.00
Flubendiamide 7.50
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
D.M. Water Q.S.
TOTAL 100.00

Procedure: As per Example 6

Storage stability data:

Storage stability Study-Fipronil 5%+Clothianidin 10%+Flubendiamide 7.5% SC (Suspension Concentrate)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.24 5.21 5.23
Clothianidin contnet percent by mass 9.5 to 10.5 10.36 10.22 10.35
Flubendiamide content percent by mass 7.13 to 8.25 7.58 7.53 7.57
Fipronil suspensibility percent min. 80 98.51 94.23 98.26
Clothianidin suspensibility percent min. 80 96.51 94.78 95.02
Flubendiamide suspensibility percent min. 80 97.01 92.02 96.52
pH range (1% aq. Suspension) 5.5 to 7.5 6.98 6.99 6.98
pourability 95% min. 97.6 96.2 96.0
specific gravity 1.05-1.15 1.07 1.08 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 460 466 490
particle size (micron) D50<3, D90<10 2.5,8.6 2.7,8.8 2.7,8.9
persistent foam ml (after 1 minute) max. 60 5 10 5
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.24 5.23 5.23
Clothianidin contnet percent by mass 9.5 to 10.5 10.35 10.33 10.30
Flubendiamide content percent by mass 7.13 to 8.25 7.58 7.56 7.55
Fipronil suspensibility percent min. 80 98.04 97.97 97.89
Clothianidin suspensibility percent min. 80 96.47 96.41 96.33
Flubendiamide suspensibility percent min. 80 96.85 96.81 96.65
pH range (1% aq. Suspension) 5.5 to 7.5 6.98 6.98 6.99
pourability 95% min. 97.5 97.1 96.3
specific gravity 1.05-1.15 1.07 1.07 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 460 462 464
particle size (micron) D50<3, D90<10 2.5,8.6 2.5,8.6 2.6,8.7
persistent foam ml (after 1 minute) max. 60 5 7 7

Example 8: Fipronil 0.5%+Thiamethoxam 1.25%+Cartap hydrochloride 5% CR Granules (Controlled Release Granules)

chemical composition % (w/w)
Fipronil a.i. 0.50
Thiamethoxam a.i. 1.25
Cartap hydrochloride a.i. 5.00
Polyaryl phenol ethoxylate & calcium dodecyl benzene solphonate Blend 1.00
Phosphoric acid 0.05
Polycarboxylates 1.00
Diacetone alcohol 2.00
Urea Formaldehyde resin 2.50
Polyvinyl pyrrolidone 0.50
China Clay 5.00
River sand Q.S.
TOTAL 100.00

Procedure: As per Example 1

Storage stability data:

Storage stability Study-Fipronil 0.5%+Thiamethoxam 1.25%+Cartap hyrdrochloride 5% CGR (Controlled Release Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 0.48 to 0.55 0.53 0.51 5.52
Thiamethoxam content percent by mass 1.19 to 1.38 1.33 1.31 1.33
Cartap hydrochloride content percent by mass 4.75 to 5.5 5.30 5.17 5.28
pH (1% in DM water) 6 to 8 7.11 7.07 7.11
bulk Density 0.4 to 0.8 0.59 0.59 0.59
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 0.48 to 0.55 0.53 0.53 0.52
Thiamethoxam content percent by mass 1.19 to 1.38 1.33 1.33 1.32
Cartap hydrochloride content percent by mass 4.75 to 5.5 5.30 5.29 5.27
pH (1% in DM water) 6 to 8 7.11 7.10 7.08
bulk Density (g/ml) 0.4 to 0.8 0.59 0.59 0.59
moisture content max. 2% 1.1 1 0.9

Example 9: Fipronil 0.5%+Thiamethoxam 1.25%+thiocylam hydrogen oxalate 5% CR Granules (Controlled Release Granules)

chemical composition % (w/w)
Fipronil a.i. 0.50
Thiamethoxam a.i. 1.25
Thiocyclam hydrogen oxalate a.i. 5.00
Polyaryl phenol ethoxylate & calcium dodecyl benzene solphonate Blend 1.00
Phosphoric acid 0.05
Polycarboxylates 1.00
Diacetone alcohol 2.00
Urea Formaldehyde resin 2.50
Polyvinyl pyrrolidone 0.50
China Clay 5.00
River sand Q.S.
TOTAL 100.00

Procedure: As per Example 1

Storage stability data:

Storage stability Study-Fipronil 0.5%+Thiamethoxam 1.25%+Thiocyclam hydrogen oxalate 5% CGR (Controlled Release Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 0.48 to 0.55 0.52 0.51 0.52
Thiamethoxam content percent by mass 1.19 to 1.38 1.29 1.28 1.29
Thiocyclam hydrogen oxalate content percent by mass 4.75 to 5.5 5.21 5.16 5.21
pH (1% in DM water) 6 to 8 7.28 7.22 7.27
bulk Density 0.4 to 0.8 0.58 0.58 0.58
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 0.48 to 0.55 0.52 0.52 0.51
Thiamethoxam content percent by mass 1.19 to 1.38 1.29 1.29 1.28
Thiocyclam hydrogen oxalate content percent by mass 4.75 to 5.5 5.21 5.21 5.19
pH (1% in DM water) 6 to 8 7.28 7.26 7.25
bulk Density (g/ml) 0.4 to 0.8 0.58 0.58 0.58
moisture content max. 2% 1.3 1.2 1.1

Example 10: Fipronil 5%+Thiamethoxam 12.5%+Cartap hydrochloride 50% SG (soluble granules)

chemical composition % (w/w)
Fipronil a.i. 5.00
Thiamethoxam a.i. 12.50
Cartap hydrochloride a.i. 50.00
Polycarboxylates 6.00
Sodium lauryl sulfate 3.00
silicon antifoam 0.50
Lactose 10.00
Corn Starch Q.S.
Total 100.00

Procedure: As per Example 2

Storage stability data:
Storage stability Study-Fipronil 5%+Thiamethoxam 12.5%+Cartap hydrochloride 50% SG (Soluble Granule)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.35 5.31 5.34
Thiamethoxam content percent by mass 11.88 to 13.13 12.71 12.65 12.70
Cartap hydrochloride content percent by mass 47.5 to 52.5 50.42 50.32 50.41
pH (1% in DM water) 6 to 8 7.08 7.04 7.08
bulk Density (g/ml) 0.4 to 0.8 0.52 0.52 0.52
moisture Content max. 2% 1.2 0.9 1
Room temperature storage stability up to 12 months
parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.35 5.34 5.34
Thiamethoxam content percent by mass 11.88 to 13.13 12.70 12.70 12.68
Cartap hydrochloride content percent by mass 47.5 to 52.5 50.42 50.41 50.38
pH (1% in DM water) 6 to 8 7.08 7.06 7.05
bulk Density (g/ml) 0.4 to 0.8 0.52 0.52 0.52
moisture Content max. 2 % 1.2 1.1 0.9

Example 11: Fipronil 5%+Thiamethoxam 12.5%+ Chlorantraniliprole 5% WG (Water Dispersible granules)

chemical composition % (w/w)
Fipronil a.i. 5.00
Thiamethoxam a.i. 12.50
Chlorantraniliprole a.i. 5.00
Alkylated naphthalene sulfonate, sodium salt 7.00
Polyacrylate polymer sodium salt 3.00
Sodium alkyl naphthalene sulfonate blend 2.00
Silicone antifoam 1.00
Lactose 10.00
Corn starch 20.00
China Clay Q.S.
TOTAL 100.00

Procedure: as per Example 4

Storage stability data:
Storage stability Study-Fipronil 5%+Thiamethoxam 12.5%+Chlorantraniliprole 5% WG (Water Dispersible Granules)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.32 5.14 5.32
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.68 12.58 12.66
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.33 5.29 5.32
Fipronil suspensibility percent min. 70 97.58 93.05 97.15
Thiamethoxam suspensibility percent min. 70 99.21 98.14 98.85
Chlorantraniliprole suspensibility percent min. 70 98.01 94.05 97.36
pH range (1% aq. Suspension) 5.5 to 7.5 6.95 6.94 6.95
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.1 98.9 99.1
bulk density (g/ml) 0.4 to 0.8 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.1 0.9 1.1
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.32 5.31 5.26
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.68 12.66 12.62
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.32 5.32 5.31
Fipronil suspensibility percent min. 70 97.12 97.02 96.56
Thiamethoxam suspensibility percent min. 70 99.08 98.69 98.62
Chlorantraniliprole suspensibility percent min. 70 97.62 97.52 95.01
pH range (1% aq. Suspension) 5.5 to 7.5 6.95 6.94 6.94
wettability sec. max. 60 8 8 9
wet sieve (45 micron) percent by mass min. 98.5 99.1 98.9 98.9
bulk density (g/ml) 0.4 to 0.8 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.1 1.1 1

Example 12: Fipronil 5%+Thiamethoxam 12.5%+ Flubendiamide 7.5% WG (wettalbe granules)

chemical composition % (w/w)
Fipronil a.i. 5.00
Thiamethoxam a.i. 12.50
Flubendiamide a.i. 7.50
Alkylated naphthalene sulfonate, sodium salt 7.00
Polyacrylate polymer sodium salt 3.00
Sodium alkyl naphthalene sulfonate blend 2.00
Silicone antifoam 1.00
Lactose 10.00
Corn starch 20.00
China Clay Q.S.
TOTAL 100.00

Procedure: As per Example 4

Storage stability data:
Storage stability Study-Fipronil 5%+Thiamethoxam 12.5%+Flubendiamide 7.5% WG (Water Dispersible Granules)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.26 5.18 5.24
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.71 12.55 12.69
Flubendiamide content percent by mass 7.13 to 8.25 7.62 7.58 7.61
Fipronil suspensibility percent min. 70 97.52 94.26 96.74
Thiamethoxam suspensibility percent min. 70 95.26 91.45 95.11
Chlorantraniliprole suspensibility percent min. 70 97.47 92.05 95.69
pH range (1% aq. Suspension) 5.5 to 7.5 7.07 7.09 7.07
wettability sec. max. 60 8 9 9
wet sieve (45 micron) percent by mass min. 98.5 99.1 99 99.1
bulk density (g/ml) 0.4 to 0.8 0.47 0.47 0.47
moisture content percent by mass max. max. 2% 1.2 0.8 1.1
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.26 5.24 5.22
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.71 12.69 12.67
Chlorantraniliprole content percent by mass 7.13 to 8.25 7.62 7.59 7.58
Fipronil suspensibility percent min. 70 97.01 96.36 95.14
Thiamethoxam suspensibility percent min. 70 95.23 94.69 94.51
Chlorantraniliprole suspensibility percent min. 70 97.17 96.52 94.36
pH range (1% aq. Suspension) 5.5 to 7.5 7.07 7.07 7.06
wettability sec. max. 60 8 8 9
wet sieve (45 micron) percent by mass min. 98.5 99.1 99.1 99.1
bulk density (g/ml) 0.4 to 0.8 0.47 0.47 0.47
moisture content percent by mass max. max. 2% 1.2 1.2 1.1

Example 13: Fipronil 5%+Thiamethoxam 12.5%+ Chlorantraniliprole 5% SC (suspension concentrate)

chemical composition % (w/w)
Fipronil a.i. 5.00
Thiamethoxam a.i. 12.50
Chlorantraniliprole a.i. 5.00
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
D.M. Water Q.S.
TOTAL 100.00

Procedure: As per Example 6

Storage stability data:
Storage stability Study-Fipronil 5%+Thiamethoxam 10%+Chlorantraniliprole 5% SC (Suspension Concentrate)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.42 5.36 5.41
Thiamethoxam contnet percent by mass 9.5 to 10.5 10.35 10.28 10.33
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.21 5.13 5.21
Fipronil suspensibility percent min. 80 98.14 95.39 97.88
Thiamethoxam suspensibility percent min. 80 99.14 98.16 98.94
Chlorantraniliprole suspensibility percent min. 80 97.89 94.23 97.02
pH range (1% aq. Suspension) 5.5 to 7.5 6.95 6.93 6.95
pourability 95% min. 97.5 97.1 96.8
specific gravity 1.05-1.15 1.08 1.08 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 485 481 491
particle size (micron) D50<3, D90<10 2.3,8.3 2.6,8.7 2.7,8.9
persistent foam ml (after 1 minute) max. 60 5 10 5
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.42 5.41 5.4
Thiamethoxam contnet percent by mass 9.5 to 10.5 10.35 10.33 10.31
Chlorantraniliprole content percent by mass 4.75 to 5.5 5.21 5.19 5.17
Fipronil suspensibility percent min. 80 98.11 97.02 96.06
Thiamethoxam suspensibility percent min. 80 98.14 98.03 97.99
Chlorantraniliprole suspensibility percent min. 80 97.26 96.13 95.87
pH range (1% aq. Suspension) 5.5 to 7.5 6.95 6.94 6.94
pourability 95% min. 97.5 97.4 97.4
specific gravity 1.05-1.15 1.08 1.08 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 485 483 482
particle size (micron) D50<3, D90<10 2.3,8.3 2.3,8.3 2.4,8.5
persistent foam ml (after 1 minute) max. 60 5 7 7

Example 14: Fipronil 5%+Thiamethoxam 12.5%+ Flubendiamide 7.5% SC (suspension concentrate)
chemical composition % (w/w)
Fipronil a.i. 5.00
Thiamethoxam a.i. 12.50
Flubendiamide 7.50
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
D.M. Water Q.S.
TOTAL 100.00

Procedure: As per Example 6

Storage stability data:

Storage stability Study-Fipronil 5%+Thiamethoxam 12.5%+Flubendiamide 7.5% SC (Suspension Concentrate)
Laboratory storage stability for 14 days
parameters specification (in house) initial heat stability study at 54±2 0C cold storage stability at 0±2 0C
Fipronil content percent by mass 4.75 to 5.5 5.29 5.18 5.28
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.74 12.68 12.74
Flubendiamide content percent by mass 7.13 to 8.25 7.66 7.63 7.65
Fipronil suspensibility percent min. 80 98.43 96.47 97.95
Thiamethoxam suspensibility percent min. 80 98.85 94.16 97.11
Flubendiamide suspensibility percent min. 80 98.14 93.26 96.87
pH range (1% aq. Suspension) 5.5 to 7.5 7.04 7.06 7.04
pourability 95% min. 97.2 96.7 96.4
specific gravity 1.05-1.15 1.07 1.08 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 463 473 496
particle size (micron) D50<3, D90<10 2.4,8.5 2.6,8.8 2.7,9.1
persistent foam ml (after 1 minute) max. 60 2 7 3
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Fipronil content percent by mass 4.75 to 5.5 5.29 5.27 5.24
Thiamethoxam contnet percent by mass 11.88 to 13.13 12.73 12.73 12.71
Flubendiamide content percent by mass 7.13 to 8.25 7.66 7.65 7.65
Fipronil suspensibility percent min. 80 98.04 97.63 97.53
Thiamethoxam suspensibility percent min. 80 97.99 97.91 97.51
Flubendiamide suspensibility percent min. 80 97.15 97.26 96.85
pH range (1% aq. Suspension) 5.5 to 7.5 7.04 7.05 7.05
pourability 95% min. 97.2 97.2 97.1
specific gravity 1.05-1.15 1.07 1.07 1.08
viscosity at spindle no. 62, 20 rpm 350-800 cps 463 466 468
particle size (micron) D50<3, D90<10 2.4,8.5 2.4,8.5 2.6,8.7
persistent foam ml (after 1 minute) max. 60 2 2 5

Example 15: Bio efficacy trials

Trial 1: Control of Sugarcane insect-pests.
Crop & Variety : Sugarcane
Location : Dhanaula, Dist. Amroha, Uttar Pradesh
Treatments : 20
Plot size : 40 sq. mt. (8 m x 4.5 m)
Spacing : 90 cm row to row
Planting material : 3 budded setts, 4 setts per meter
Date of sowing : 15 March 2017
Date of Application : At the time of planting, 15 March 2017
Method of Application: In furrow application, over the setts and than cover up with soil and irrigated
Date of Harvesting : 10 March 2018
Fertilizer : 100 kg per ha. DAP (diammonium phosphate) as basal dose at plating.
Agronomic Practices : Fertilizer, irrigation, inter culturing, earthing up and weeding done as per the
crop requirement.
Observation Methods:
Germination (%):
The germination (%) was recorded after 45 days of planting using following formula.

Number of emerging shoots
Percent germination of Buds = ---------------------------------------------- X 100
Total number of buds planted

Shoot count:
The number of shoots was counted from 1 mrl (meter row length) from randomly selected 5 spot per plot. The percent increase in shoot over untreated control was calculated by below formula.
Number of shoots in treatment
Percent increase over untreated control = 100 X ____________________________________ - 100
Number of shoots in untreated control

Early shoot borer (Chilo infuscatellus) incidence (%):
Fifty shoots per plot were selected randomly and presence of characteristic “dead heart” (damaged shoots) were recorded to calculate per cent shoot damage by early shoot borer.

Damaged shoots
Percent shoot damage = -------------------------------------------------- X 100
Total number of shoots observed (50)

Plant damage by Termite (Odontotermes spp. And Microtermes spp.) (%):
Ten plants at random from each plot were observed to record the plant damage due to termites at 60, 90 and 120 days after sowing (planting)

Damaged plants
Percent plant damage = ------------------------------------------- X 100
Total number of plants observed

Plant damage by White grub (Holotrichia consanguinea) (%):
Ten plants at random from each plot were observed to record the plant damage due to white grub at 120 and 120 days after sowing (planting).

Damaged plants
Percent plant damage = ------------------------------------------- X 100
Total number of plants observed

White grub larval count:
The soils from three spot (30 cm x 30 cm x 30 cm) at random from each plot were dugged out from root zone taken out and presence of grub / larvae were recorded at 120 days after sowing (planting).
Table 1: Treatment Details
Treatments Treatments Dose (gram active per hectare)
Sample 1 Fipronil 0.5%+Clothianidin 1%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 50+100+500
Sample 2 Fipronil 0.5%+Clothianidin 1%+Bifenthrin 0.5% Granules, 10 kg per ha. 50+100+50
Sample 3 Fipronil 0.5%+Clothianidin 1%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50+100+50
Sample 4 Fipronil 0.5%+Clothianidin 1%+Flubendiamide 0.75% Granules, 10 kg per ha. 50+100+75
Sample 5 Fipronil 0.5%+Clothianidin 1%, Granules, 10 kg per ha. 50+100
Sample 6 Fipronil 0.5%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 50+500
Sample 7 Fipronil 0.5%+Bifenthrin 0.5% Granules, 10 kg per ha. 50+50
Sample 8 Fipronil 0.5%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50+50
Sample 9 Fipronil 0.5%+Flubendiamide 0.75% Granules, 10 kg per ha. 50+75
Sample 10 Clothianidin 1%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 100+500
Sample 11 Clothianidin 1%+Bifenthrin 0.5% Granules, 10 kg per ha. 100+50
Sample 12 Clothianidin 1%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 100+50
Sample 13 Clothianidin 1%+Flubendiamide 0.75% Granules, 10 kg per ha. 100+75
Sample 14 Fipronil 0.5% Granules, 10 kg per ha. 50
Sample 15 Clothianidin 1% Granules, 10 kg per ha. 100
Sample 16 Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 500
Sample 17 Bifenthrin 0.5% Granules, 10 kg per ha. 50
Sample 18 Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50
Sample 19 Flubendiamide 0.75% Granules, 10 kg per ha. 75
UTC Untreated Check (Control) -
Kg- Kilo gram, ha- hectare.

Table 2: Efficacy against Sugarcane Insect-pest, germination (%) and tiller count
Treatments Germination (%) No. of shoots per mrl % Increase of GC over Untreated Control Early shoot borer incidence (%) % Plant Damage by Termite % Plant damage by White grub White grub larvae per cubic feet
45 DAS 45 DAS 45 DAS 60 DAS 60 DAS 90 DAS 120 DAS 120 DAS 120 DAS
Sample 1 100.00 21.40 174.36 0.00 0.12 0.16 1.18 0.00 0.00
Sample 2 100.00 20.80 166.67 1.20 0.15 0.27 1.84 0.00 0.00
Sample 3 100.00 23.30 198.72 0.00 0.12 0.19 1.62 0.00 0.00
Sample 4 100.00 21.20 171.79 0.00 0.10 0.26 1.86 0.00 0.00
Sample 5 96.33 11.50 47.44 6.40 0.36 0.76 5.24 3.14 1.83
Sample 6 91.33 10.60 35.90 6.20 0.42 0.78 6.42 4.82 2.43
Sample 7 89.33 10.30 32.05 5.70 0.76 1.84 9.82 3.28 2.64
Sample 8 86.33 10.90 39.74 3.20 0.82 1.92 8.86 4.82 1.98
Sample 9 84.33 10.70 37.18 3.40 0.62 1.72 7.84 3.96 2.64
Sample 10 83.67 11.20 43.59 4.50 0.92 2.16 10.24 2.86 1.42
Sample 11 80.33 11.10 42.31 6.70 0.36 1.18 7.86 2.42 1.27
Sample 12 84.33 11.80 51.28 3.10 0.72 1.42 10.83 2.94 1.36
Sample 13 82.67 11.40 46.15 3.20 0.82 1.86 9.84 2.38 1.18
Sample 14 75.67 9.40 20.51 8.60 1.12 2.43 10.83 6.85 3.86
Sample 15 77.67 9.70 24.36 10.20 0.62 1.26 8.74 3.83 1.16
Sample 16 73.00 9.20 17.95 9.70 2.63 6.83 12.75 8.73 3.24
Sample 17 70.00 8.10 3.85 11.40 3.18 6.82 14.28 10.28 4.72
Sample 18 75.33 9.50 21.79 6.40 3.28 7.84 15.28 9.86 5.82
Sample 19 72.67 8.80 12.82 6.70 2.96 8.52 14.85 11.38 4.86
UTC 62.67 7.80 - 12.80 4.83 10.73 24.73 15.82 6.84

The field trials data (table 2) shows that novel combinations of Fipronil 0.5%+Clothianidin 1%+Thiocyclam Hydrogen Oxalate 5% Granules, Fipronil 0.5%+Clothianidin 1%+Bifenthrin 0.5% Granules, Fipronil 0.5%+Clothianidin 1%+Chlorantraniliprole 0.5% Granules, Fipronil 0.5%+ Clothianidin 1% + Flubendiamide 0.75% Granules gave excellent germination (100%), about > 166% increase in shoots Cane over control, excellent protection against early shoot borer (no incidence), excellent protection against termite with longer residual control (up to 120 days) and excellent protection against white grub damage (no damage). The visible characters were observed in novel combinations of Fipronil 0.5%+Clothianidin 1%+ Thiocyclam Hydrogen Oxalate 5% Granules, Fipronil 0.5%+Clothianidin 1%+Bifenthrin 0.5% Granules, Fipronil 0.5%+Clothianidin1%+Chlorantraniliprole 0.5% Granules, Fipronil 0.5%+ Clothianidin 1% + Flubendiamide 0.75%ations were increase in number of roots (root mass), more number of secondary and tertiary roots, dark green color of leaf, increased leaf blades width, leaf shinning, stem girth, plant/ shoot height and no lodging compared to other treatments.

Trial 2: Control of Paddy insect-pests.

Crop & Variety : Paddy, BPT-5204
Location : Gangavathi, Dist. Koppal, Karnataka
Treatments : 20
Plot size : 25 sq. mt. (5 m x 5 m)
Date of Transplanting : 10 August 2017
Date of Application : 24 DATP (Days after transplanting)
Method of Application: Manual broadcasting by hand (wearing rubber gloves)
Agronomic Practices : Fertilizer, irrigation, and weed control operation done as per
the crop requirement.

Observation Methods:
Stem borer Incidence (Chilo supressalis) (%):
The stem borer incidence were assessed by dead heart and white ear head symptoms at 45 DATP
and at before harvest respectively.
Dead heart (%): Ten hills per plot were selected randomly to count the number of characteristic
“dead heart” (damaged tiller) and total number of tillers.

Number of dead heart
Dead Heart (%) = ---------------------------------- X 100
Total number of tillers

White ear head (%):
10 hills per plot were selected randomly and presence of white ear head and total number of ear head were recorded before harvest to calculate per cent white ear head.

Number of white ear head
White ear head (%)= --------------------------------------- X 100
Total number of ear head

Effective Tillers:
The number of effective tillers per hill were counted from randomly selected 10 hills per plot at grain filling stage.

Leaf folder incidence (Cnaphalocrosis medinalis) (%):
The incidence of lead folder were recorded as soon as its damage observed in untreated control plot.

Number of damaged leaf let per hill
Leaf folder damage (%)= ------------------------------------------------- X 100
Total number of leaflet per hill

Plant Hopper (Nilaparvata lugens, Sogatella furcifella, Nephotettix nigropictus):
The number of hoppers (nymphs+adults) per hill were recorded from randomly selected 10 hills per plot. The observations were recorded after hopper incidence reached at its peak in untreated control plot. The percent plant hopper controls were recorded by below formula.

Number of Hoppers in treated plot
Plant Hopper control (%) = 100 - ---------------------------------------------------------- X 100
Number of hoppers in untreated control plot

Table 3: Treatment Details
Treatments Treatments Dose (gram active per hectare)
Sample 1 Fipronil 0.5%+Clothianidin 1%+Cartap Hydrochloride 5% Granules, 10 kg per ha. 50+100+500
Sample 2 Fipronil 0.5%+Clothianidin 1%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 50+100+500
Sample 3 Fipronil 0.5%+Clothianidin 1%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50+100+50
Sample 4 Fipronil 0.5%+Clothianidin 1%+Flubendiamide 0.75% Granules, 10 kg per ha. 50+100+75
Sample 5 Fipronil 0.5%+Clothianidin 1%, Granules, 10 kg per ha. 50+100
Sample 6 Fipronil 0.5%+Cartap Hydrochloride 5% Granules, 10 kg per ha. 50+500
Sample 7 Fipronil 0.5%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 50+500
Sample 8 Fipronil 0.5%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50+50
Sample 9 Fipronil 0.5%+Flubendiamide 0.75% Granules, 10 kg per ha. 50+75
Sample 10 Clothianidin 1%+Cartap Hydrochloride 5% Granules, 10 kg per ha. 100+500
Sample 11 Clothianidin 1%+Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 100+500
Sample 12 Clothianidin 1%+Chlorantraniliprole 0.5% Granules, 10 kg per ha. 100+50
Sample 13 Clothianidin 1%+Flubendiamide 0.75% Granules, 10 kg per ha. 100+75
Sample 14 Fipronil 0.5% Granules, 10 kg per ha. 50
Sample 15 Clothianidin 1% Granules, 10 kg per ha. 100
Sample 16 Cartap Hydrochloride 5% Granules, 10 kg per ha 500
Sample 17 Thiocyclam Hydrogen Oxalate 5% Granules, 10 kg per ha. 500
Sample 18 Chlorantraniliprole 0.5% Granules, 10 kg per ha. 50
Sample 19 Flubendiamide 0.75% Granules, 10 kg per ha. 75
UTC Untreated Check (Control) -

Table 4: Efficacy against insect-pest of paddy crop and effective tillers
Treatments Stem borer Incidence (%) Leaf folder damage (%) No. of Effective tillers per hill % Increase in effective tiller per hill over untreated control % Plant Hoppers control
Dead Heart (%) White Ear head (%)
45 DATP Before Harvest 60 DATP 80 DATP 80 DATP 80 DATP
Sample 1 0.00 0.00 0.00 17.60 72.55 86.84
Sample 2 0.00 0.00 0.00 17.80 74.51 88.82
Sample 3 0.00 0.00 0.00 18.20 78.43 87.26
Sample 4 0.00 0.00 0.00 18.10 77.45 86.83
Sample 5 1.28 1.42 3.76 15.30 50.00 78.84
Sample 6 0.48 0.96 2.64 15.20 49.02 56.38
Sample 7 0.42 0.92 2.32 15.40 50.98 54.28
Sample 8 0.24 0.64 1.83 15.70 53.92 52.43
Sample 9 0.30 0.72 1.92 15.50 51.96 50.28
Sample 10 1.32 2.96 4.10 14.80 45.10 69.73
Sample 11 1.24 2.84 3.48 14.60 43.14 68.73
Sample 12 0.96 2.37 2.86 14.50 42.16 68.18
Sample 13 1.07 2.16 3.12 14.70 44.12 67.80
Sample 14 2.64 6.74 6.89 12.60 23.53 28.18
Sample 15 5.84 10.84 18.83 12.20 19.61 66.38
Sample 16 2.42 5.96 5.86 13.10 28.43 13.82
Sample 17 1.84 4.27 4.86 11.60 13.73 20.84
Sample 18 0.96 1.96 3.74 12.60 23.53 14.82
Sample 19 1.12 2.86 4.20 12.30 20.59 10.28
UTC 7.87 16.72 24.32 10.20 0.00 0.00

The field trial observations (table 4) shows that Fipronil 0.5%+Clothianidin 1%+Cartap hydrochloride 5% Granules, Fipronil 0.5%+Clothianidin 1%+ Thiocyclam Hydrogen Oxalate 5% Granules, Fipronil 0.5%+Clothianidin 1%+Chlorantraniliprole 0.5% Granules and Fipronil 0.5%+ Clothianidin 1% + Flubendiamide 0.75% Granules gaves excellent control of stem borer (both in terms of dead heart and white ear head at harvest), leaf folder and plant hoppers (brown plant hopper and white backed plant hoppers) and also produces higher number of effective tillers compared to others treatments. Other visible characters were observed in novel combinations of Fipronil 0.5%+Clothianidin 1%+Cartap hydrochloride 5% Granules, Fipronil 0.5%+Clothianidin 1%+ Thiocyclam Hydrogen Oxalate 5% Granules, Fipronil 0.5%+Clothianidin 1%+Chlorantraniliprole 0.5% Granules, Fipronil 0.5%+ Clothianidin 1% + Flubendiamide 0.75% were increase in number of roots (root mass), more number of secondary and tertiary roots, dark green color of leaf, increased leaf blades width, leaf shinning, stem girth, plant/ shoot height, no lodging and decreased incidence of sheath blight, leaf blast and grain discoloration diseases compared to other treatments.
,CLAIMS:We claim;
[CLAIM 1]. A synergistic insecticidal composition comprising
a) Fipronil;
b) Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid; and
c) at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

[CLAIM 2]. The synergistic insecticidal composition according to claim 1 wherein, composition comprises;
a) 0.1 to 20 % of Fipronil;
b) 0.1 to 20 % of Neonicotinoids (Neonics) selected from Acetamiprid, Dinotefuran, Nitenpyram, Thiacloprid, Clothianidin, Thiamethoxam, Imidacloprid; and
c) 0.1 to 60 % of at least one more insecticide selected from Cartap Hydrochloride, Thiocyclam, Bifenthrin, Chlorpyrifos, Chlorantraniliprole and Flubendiamide and one or more inactive excipients.

[CLAIM 3]. The synergistic insecticidal composition according to claim 1 or 2, wherein inactive excipients are selected from the group consisting of dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents and buffering agent.

[CLAIM 4]. The synergistic insecticidal composition according to claim 1-3, wherein the composition can be selected from Suspension Concentrate (SC), Suspo emulsion (SE), Capsule Suspension (CS), Oil Dispersion (OD), mixed formulation of CS and SC (ZC), a mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granules (Soil Applied Granules), Controlled Release Granules (CR Granules), Slow release and Fast release microsphere Granules (MS Granules), Water Soluble Granules (SG), Water dispersible granule (WDG or WG), Jumbo ball formulation, Water soluble bag formulation, Wettable Powder (WP), Soluble Powder (SP)..

[CLAIM 5]. The synergistic insecticidal composition according to claim 4, wherein the preferable formulations are Water dispersible Granules (WG), Water Soluble Granules (SG), Controlled release granules (CR) and Suspension concentrate (SC).

[CLAIM 6]. The synergistic insecticidal composition according to any of the preceding claims, wherein the composition is effective in controlling insect pests, In Sugarcane crop- Termites Odontotermes spp., Coptotermes spp., Heterotermes spp., Leucotermes spp., Microtermes obesi, Whitegrub, Holotrichia consanguinea, Holotrichia serrata, Maladera insanabilis, Brahmina spp., Melolontha spp., Lepidiota spp., Anomala spp., Phyllognathus spp., Leucopholis spp., Wireworms, Limonius spp., Agriotes spp., Early shoot borer Chilo infuscatellus, Pink borer Sesamia inferens, Top shoot borer Scirpophaga excerptalis, Root borer Emmalocera depressella, Internode borer: Chilo sacchariphagus indicus, Stalk borer Chilo auricilius, White woolly aphid Ceratovacuna lanigera, Black bug Cavelerius sweeti, Whitefly Aleurolobus barodensis, Pyrilla Pyrilla perpusilla, Mealybug Saccharicoccus sacchari. In rice/paddy crop- Termites, root weevil Lissorhoptus oryzophilus, Echinocnemus oryzae, Hydronomodius molitor, stem borer, Chilo suppressalis, Schirpophaga incertulas, Sesamia inferens, Hoppers, Nilaparvata lugens, Sogatella furcifella, Nephotettix nigropictus, Gall midge, Orseolia oryzae, Leaffolder Cnaphalocrocis medinalis, Rice bug, Leptocorisa spp., Stink bug, Nezara spp., Rice Hispa, Dicladispa armigera, Caseworm Nymphula depuctalis, whorl maggot, Hydrellia spp., black bug, Scotinophara coarctata, armyworm, Mythimna separate, Mole cricket Gryllotalpa spp., Stem maggot, Chlorops oryzae and soil earthworm (oligochaeta).

[CLAIM 7]. The synergistic insecticidal composition according to any of the preceding claims, wherein the said composition is effective for GMO (Genetically Modified Organism) and Non GMO varieties of Cotton (Gossypium spp.), Jute (Corchorus oliotorus), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Ragi (Eleusine coracana), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum) , Sugarbeet (Beta vulgaris), Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Castor (Ricinus communis), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (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), 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 subsp rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), 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), Fenugreek (Trigonella foenum-graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), 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).