DESC:
FIELD OF INVENTION
The present invention relates to synergistic insecticidal composition comprising Spirotetramat and Insecticide selected from flupyrimin or benzpyrimoxan. The present invention more particularly relates to insecticidal compositions and a method of preparation thereof.

BACKGROUND OF THE INVENTION
Spirotetramat is described in WO98/05638, chemical name is 4- (ethoxycarbonyloxy) -8-methoxy-3- (2, 5- dimethylphenyl) -1-azaspiro W, 5] - dec-3-en-2-one is an insecticide, its mechanism interference pests fat synthesis, blocking the energy metabolism, are anti neonicotinoids selection of species management. Spirotetramat withdrawing the unique property, is so far the only insecticide having the absorption bidirectional conducting properties, throughout the body can be moved downward in direction of plants, bark and foliage arrival, and to control a crop on the interior of the fruit skin pests. This unique absorption properties to protect the newborn stems, leaves and roots, preventing eggs and larvae of insects; long duration, can provide effective prevention and control of up to eight weeks, high efficacy, broad spectrum control of pests can be effectively control a variety of sucking insects such as aphids, thrips, psyllids, mealybugs, scale insects and whiteflies; applicable major crops include cotton, soybean, citrus, tropical fruit, nuts, grapes, hops, potatoes and vegetables; natural enemies security: important beneficial insects such as ladybugs, hover flies and parasitic wasps have good selectivity.

Flupyrimin is described in WO2012/029672 (Indian counterpart 4123/KOLNP/2012).

Benzpyrimoxan has a unique chemical structure which contains benzyloxy and cyclic acetal groups on pyrimidine moiety (5-(1,3-dioxan-2-yl)-4-[4(trifluoromethyl)benzyloxy]pyrimidine). Benzpyrimoxan disclosed in WO2013/115391 (Indian Patent IN302827 (1680/KOLNP/2014)).

The present inventors have surprisingly developed an insecticidal composition comprising Spirotetramat and Insecticide selected from flupyrimin or benzpyrimoxan which increase the yield and plant vigour of the treated plant.

Advantages of the present invention
• The insecticidal composition of the present invention is a Broad-spectrum, high-efficient, low-toxic and low-residue composition.
• The insecticidal composition of the present invention is not liable to generate resistance in pests, is safe to human, livestock, plants and natural enemies, has a significant synergistic effect, can reduce a use amount of effective components and a use cost, can delay generation of the resistance in the pests, can effectively reduce environmental pollution and pesticide residue, is free of pesticide hazard and low-toxic in human and other mammals.
• The insecticidal composition of the present invention is free of chronic toxin, and has significant killing effects on sucking insects like aphids, jassids, thrips, mealy bugs, hoppers and plant mites.

OBJECTS OF THE INVENTION

It is an object of the present invention to provide an insecticidal composition comprising comprising Spirotetramat and Insecticide selected from flupyrimin or benzpyrimoxan.

It is another object of the present invention to provide an insecticidal composition comprising comprising Spirotetramat and Insecticide selected flupyrimin or benzpyrimoxan which improve the yield and plant vigour of the treated plant.

SUMMARY OF THE INVENTION
According to an aspect of the present invention there is provided a synergistic insecticidal composition comprising:

I) Spirotetramat in the range from 0.1 to 50% by weight of the composition; and
II) Insecticide in the range from 0.1 to 50% by weight of the composition wherein the said insecticide is selected from flupyrimin or benzpyrimoxan.

DETAILED DESCRIPTION OF THE INVENTION

The present invention relates to insecticidal mixtures of Spirotetramat and Insecticide selected from flupyrimin or benzpyrimoxan.

In an embodiment of the present invention there is provided an insecticidal composition of comprising:

I) Spirotetramat;
II) Insecticide selected from flupyrimin or benzpyrimoxan; and
III) one or more inactive excipients.

In another embodiment of the present invention there is provided an insecticidal composition comprising Spirotetramat and Insecticide selected from flupyrimin or benzpyrimoxan with the following mass percentage of the composition:

Sr. No. Raw material Concentration range (w/w %)
i Spirotetramat 0.1 to 50
ii Insecticide selected from flupyrimin or benzpyrimoxan 0.1 to 50

The insecticidal composition of the present invention may be formulated in the forms given below:

Capsule suspension (CS), Dispersible concentrate (DC), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion for seed treatment (ES), Emulsion, oil in water (EW), Flowable suspension/concentrate for seed treatment (FS), Granule/ soil applied (GR), Controlled (Slow or Fast) release granules (CR)Solution for seed treatment (LS), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (= flowable concentrate) (SC), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Water soluble powder (SP), Water dispersible granule (WG or WDG), Wettable powder (WP), Water dispersible powder for slurry treatment (WS), A mixed formulation of CS en SC (ZC), A mixed formulation of CS en SE (ZE), A mixed formulation of CS en EW (ZW).

In a preffered embodiment of the present invention the composition may be formulated as Water dispersible granule (WG or WDG) or Suspension concentrate (SC).

In another embodiment the composition of the present invention further comprises inactive excipients.

The list of inactive excipients for WDG and SC formulation are as follows:

Water dispersible granule (WDG)
Dispersing agents Naphthalenesulfonic acid, sodium salt condensated with formaldehyde, polyalcoxylated alkylphenol, naphthalenesulfonic acid formaldehyde condensate, methylnaphtaline-formaldehyde-condensate sodium salt, napthalene condensates, lignosulfonates, polyacrylates and phosphate esters, calcium lignosulfonate, lignin sulfonate sodium salt
Wetting agents sodium N-methyl-N-oleoyl taurate,Alkylated naphtalene sulfonate, sodium salt, mixture of isomers of dibutylnaphthalene sulphonic acid sodium salt, sodium diisopropylnaphthalenesulphonate,Sodium Lauryl sulfate, Dioctyl sulfate, alkyl naphthalene sulfonates, phosphate esters, sulphosuccinates and nonionics such as tridexyl alcohol ethoxylate, alkyl or alkaryl sulfonates such as alkylbenzene sulfonates, alpha olefin sulfonate and alkyl naphthalene sulfonates, ethoxylated or non-ethoxylated alkyl or alkyaryl carboxylates, alkyl or alkyaryl phosphate esters, alkylpolysaccharide; di or mono alkyl sulfosuccinate derivatives, alpha olefin sulfonates, alkyl naphthalene sulfonates, dialkyl sulphosuccinates, butyl, dibutyl, isopropyl and diisopropyl naphthalene sulfonate salts, C12 alkyl benzene sulfonate or C10-C16 alkyl benzene sulfonate
Antifoaming agent Polydimethylsiolxane
Carrier China Clay, Silica,Lactose anhydrous,Ammonium sulfate,Sodium sulfate anhydrous,Corn starch,Urea,EDTA,Urea formaldehyde resin,Diatomaceous earth, kaolin, bentonite, kieselguhr, Fuller's earth, Attapulgite clay, , bole, loess, talc, chalk, dolomite, limestone, lime, calcium carbonate, powdered magnesia, magnesium oxide, magnesium sulfate, sodium chloride, gypsum, calcium sulfate, pyrophyllite, silicates and silica gels; fertilizers such as, for example, ammonium sulfate, ammonium phosphate, ammonium nitrate and urea; natural products of vegetable origin such as, for example, grain meals and flours, bark meals, wood meals, nutshell meals and cellulosic powders; and synthetic polymeric materials such as, for example, ground or powdered plastics and resins, bentonites, zeolites, titanium dioxide, iron oxides and hydroxides, aluminium oxides and hydroxides, or organic materials such as bagasse, charcoal, or synthetic organic polymers
Disintegrating agent citric acid, succinic acid or the sodium bicarbonate.
Suspension concentrate (SC)
Wetting agent Ethylene oxide/propylene oxide block copolymer, Polyarylphenyl ether phosphate, Ethoxylated Fatty Alcohol, Sodium dioctyl sulfosuccinate, sodium lauryl sulfate and sodium dodecyl benzene sulfonate, alkyldiphenylsulfonates, sodium isopropyl naphthalene sulfonate,Alkylnaphthalene sulfonate etc
Dispersing agent Alkylated naphthalene sulfonate, sodium salt, Sodium salt of naphthalene sulfonate condensate, Sodium Ligno sulfonate,Sodium ploycarboxylate,EO/PO based copolymer, Phenol sulfonate, Sodium Methyl Oleoyl Taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide
Suspending agent Aluminum Magnesium Silicate, Bentonite clay, Silica, Attapulgite clay
Antifoaming agent silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound,Silicone antifoam emulsion, Dimethylsiloxane, Polydimethyl siloxane,Vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane etc
Antifreezing agent ethylene glycol, propane diols, glycerine or the urea,Glycol (Monoethylene glycol, Diethylene glycol, Polypropylene glycol, Polyethylene glycol), Glycerine, Urea, Magnesium sulfate Heptahydrate, Sodium Chloride etc
Preservative 1,2-benzisothiazolin-3(2H)-one, sodium salt, Sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, Formaldehyde, Sodium o-phenylphenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one
Thickner Xanthan gum, PVK, carboxymethylcelluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethylcellulose, Sodium Polyacrylate, modified starch

In another embodiment of the present invention there is provided a method of preparing a stable, low toxic formulation of the present invention.

The method of application of the insecticidal composition of the present invention includes foliar spray, Seed treatment or treatment to planting materials, soil application.

The lists of crops which can be protected by the insecticidal composition of the present invention are GMO (Genetically Modified Organism) and Non GMO varieties of Cotton (Gossypium spp.), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), 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), 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 insecticidal composition of the present invention can be used to control the Insects from the order of the Lepidoptera, for example cutworm Agrotis ypsilon, sugarcane shoot borer Chilo infuscatellus, sugarcane stalk borer Chilo partellus, sugarcane internode borer Chilo sacchariphagus, paddy/rice stem borer, Chilo suppressalis, rice leaffolder Cnaphalocrocis medinalis, apple colding moth Cydia pomonella, okra fruit borer Earias vittella, Earias insulana, Tomato fruit borer Helicoverpa armigera, tobacco budworm Helicoverpa virescens, corn earworm Helicoverpa zea, cabbage webworm Hellula undalis, Brinjal fruit and shoot borer Leucinodes orbonalis, bean pod borer Maruca vitrata, Maruca testulalis, armyworm Mythimna separata, cotton pinkbollworm Pectinophora gossypiella, citrus leafminer Phyllocnistis citrella, cabbage butterfly Pieris bras-sicae, diamond backmoth Plutella xylostella, paddy stem borer Scirpophaga excerptallis, Scirpophaga incertulas, Scirpophaga innotata, wheat stem borer Sesamia inferens, Sitotroga cerealella, Spilosoma obliqua, Spodoptera frugiperda, Spodoptera littoralis, Spodoptera litura, Trichoplusia ni, Tryporyza novella, Tuta absoluta.

Beetles (Coleoptera), for example Anthonomus grandis, Bruchus lentis, Diabrotica semipunctata, Diabrotica virgifera, Dicladispa armigera, Epila-chna varivestis, Holotrichia bicolor, Holotrichia consanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotreta chrysocephala, Popillia japonica.

Flies, mosquitoes (Diptera), e.g. Atherigona orientalis, Calliphora vicina, Dacus cucurbi-tae, Liriomyza trifolii, Melanagromyza obtuse.

Thrips (Thysanoptera), e.g. Dichromothrips ssp, Frankliniella occidentalis, 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.

True bugs (Hemiptera), e.g. Cotton leafhopper Amrasca biguttula biguttula, Amrasca devastans, Mango hopper Amritodus atkinsoni, Idioscopus spp., cotton aphid Aphis gossypii, groundnut aphid Aphis crassivora, whitefly Bemisia argentifolii, Bemisia tabaci, cabbage aphid Brevicoryne brassicae, red gram bug Clavigralla gibbosa, leaf hopper Empoasca fabae, Lygus pratensis, Macrosiphum avenae, Myzus persicae, Nilaparvata lugens, Nephotettix virescens, Nephotettix nigropictus, Planococcus spp., Pseudococcus spp., Pyrilla perpusilla, Rhopalosiphum maidis, Saccharicoccus sacchari, Sitobion avenae, Sogatella furcifera, Trialeurodes vaporariorum, Toxoptera aurantiia, Psylla spp., Rhopalosiphum spp.

Arachnoidea, such as arachnids (Acarina/ plant mites), e.g. of the families Argasidae, Ixodidae and Sarcoptidae, such as Amblyomma variegatum, Ambryomma maculatum, Boophilus microplus, 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.

The mixtures according to the invention can be applied to any and all developmental stages of pests, such as egg, nymph, 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

Manufacturing Process:
WG (Water Dispersible Granules)

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 requied pack sizes.

SC (Suspension Concentrate):

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.

EXAMPLES

The present invention will now be explained in detail by reference to the following formulation examples and a test example, which should not be construed as limiting the scope of the present invention.

Formulation recipe
1. Suspension concentrate (SC) formulation of Spirotetramat 7.5%+ Flupyrimin 10.0%
Chemical composition % (w/w)
Spirotetramat a.i. 7.50
Flupyrimin a.i. 10.00
Ethoxylated fatty alcohol 3.50
Acrylic graft copolymer 3.00
Alkylated napthalene sulfonate, sodium salt 0.50
Precipitated Silica 0.50
Polydimethyl siloxane 0.30
1,2-benzisothiazol-3-one 0.20
Glycol 5.00
Xanthan gum 0.15
Polyalkoxylated butyl ether 1.00
D.M. Water q.s.
Total 100.00

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
Spirotetramat content percent by mass 7.125 to 8.250 7.52 7.50 7.51
Flupyrimin content percent by mass 9.5 to 10.5 10.2 10.1 10.2
Spirotetramat suspensibility percent min. 80 96.14 95.15 96.03
Flupyrimin suspensibility percent min. 80 97.16 97.10 96.80
pH range (1% aq. Suspension) 4.0 to 6.5 5 5 5
Pourability 95% min. 97.4 97.2 96.5
specific gravity 1.05-1.10 1.05 1.05 1.05
viscosity at spindle no. 62, 20 rpm 350-800 cps 510 518 520
particle size (micron) D50<3, D90<10 2.2,8.6 2.4,8.8 2.5,8.9
persistent foam ml (after 1 minute) max. 60 nil 5 nil
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Spirotetramat content percent by mass 7.125 to 8.250 7.52 7.52 7.51
Flupyrimin content percent by mass 9.5 to 10.5 10.2 10.2 10.15
Spirotetramat suspensibility percent min. 80 96.17 95.13 95.32
Flupyrimin suspensibility percent min. 80 97.16 96.10 96.20
pH range (1% aq. Suspension) 4.0 to 6.5 7.12 7.14 7.08
Pourability 95% min. 97.4 97.4 97.3
specific gravity 1.05-1.10 1.05 1.05 1.05
viscosity at spindle no. 62, 20 rpm 350-800 cps 515 520 523
particle size (micron) D50<3, D90<10 2.2,8.6 2.2,8.6 2.2,8.7
persistent foam ml (after 1 minute) max. 60 nil nil 2

2. Suspension concentrate (SC) formulation of Spirotetramat 7.5%+ Benzpyrimoxan 10.0%
Chemical composition % (w/w)
Spirotetramat a.i. 7.50
Benzpyrimoxan a.i. 10.00
Ethoxylated fatty alcohol 3.50
Acrylic graft copolymer 3.00
Alkylated napthalene sulfonate, sodium salt 0.50
Precipitated Silica 1.00
Polydimethyl siloxane 0.30
1,2-benzisothiazol-3-one 0.20
Glycol 5.00
Xanthan gum 0.15
Polyalkoxylated butyl ether 1.00
D.M. Water q.s.
Total 100.00

Storage stability of suspension concentrate of Spirotetramat 7.5%+ Benzpyrimoxan 10.0%
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
Spirotetramat content percent by mass 7.125 to 8.250 7.51 7.5 7.5
Benzpyrimoxan content percent by mass 9.5 to 10.5 10.1 10 10.1
Spirotetramat suspensibility percent min. 80 97.17 96.53 96.15
Benzpyrimoxan suspensibility percent min. 80 97.26 97.14 97.1
pH range (1% aq. Suspension) 4.0 to 6.5 5.5 5.5 5.5
Pourability 95% min. 97.5 97.1 96.2
specific gravity 1.05-1.10 1.06 1.06 1.06
viscosity at spindle no. 62, 20 rpm 350-800 cps 520 525 522
particle size (micron) D50<3, D90<10 2.1,8.1 2.3,8.5 2.5,9.1
persistent foam ml (after 1 minute) max. 60 5 5 2
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Spirotetramat content percent by mass 7.125 to 8.250 7.51 7.51 7.5
Benzpyrimoxan content percent by mass 9.5 to 10.5 10.1 10.1 10
Spirotetramat suspensibility percent min. 80 97.25 96.7 96.5
Benzpyrimoxan suspensibility percent min. 80 97.4 97.3 97.1
pH range (1% aq. Suspension) 4.0 to 6.5 5.5 5.5 5.5
Pourability 95% min. 97.5 97.5 97.3
specific gravity 1.05-1.10 1.06 1.06 1.06
viscosity at spindle no. 62, 20 rpm 350-800 cps 525 523 520
particle size (micron) D50<3, D90<10 2.1,8.1 2.1,8.2 2.2,8.3
persistent foam ml (after 1 minute) max. 60 5 5 2

Formulation recipe
3. Water dispersible granule (WG) formulation of Spirotetramat 7.5%+ Flupyrimin 10.0%
Chemical composition % (w/w)
Spirotetramat a.i. 7.50
Flupyrimin a.i. 10.00
Sodium Polycarboxylate 6.00
sodium salt of sulphonate napthalene formaldehyde condensate 3.00
Alkylated naphthalene sulfonate, sodium salt 2.00
Corn starch 20.00
Lactose 30.00
Silicon Antifoam 0.50
Silicon Dioxide 3.00
China clay Q.S
Total 100.00

Storage stability of Water Dispersible Granules (WG) of Spirotetramat 7.5%+ Flupyrimin 10.0%
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
Spirotetramat content percent by mass 7.125 to 8.250 7.52 7.51 7.51
Flupyrimin content percent by mass 9.5 to 10.5 10.25 10.15 10.2
Spirotetramat suspensibility percent min. 70 97.05 96.95 96.14
Flupyrimin suspensibility percent min. 70 96.02 95.62 95.51
pH range (1% aq. Suspension) 4.0 to 6.5 5.30 5.50 5.30
wettability sec. max. 60 9 10 10
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.4 1.2 1.1
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Spirotetramat content percent by mass 7.125 to 8.250 7.52 7.52 7.51
Flupyrimin content percent by mass 9.5 to 10.5 10.25 10.24 10.2
Spirotetramat suspensibility percent min. 70 97.05 96.95 96.14
Flupyrimin suspensibility percent min. 70 97.05 96.95 96.14
pH range (1% aq. Suspension) 4.0 to 6.5 5.30 5.50 5.30
wettability sec. max. 60 9 10 10
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.4 1.2 1.1


Formulation recipe
4. Water dispersible granule (WG) formulation of Spirotetramat 7.5%+ Benzpyrimoxan 10.0%
Chemical composition % (w/w)
Spirotetramat a.i. 7.50
Benzpyrimoxan a.i. 10.00
Sodium Polycarboxylate 6.00
sodium salt of sulphonate napthalene formaldehyde condensate 3.00
Alkylated naphthalene sulfonate, sodium salt 2.00
Corn starch 20.00
Lactose 30.00
Silicon Antifoam 0.50
Silicon Dioxide 3.00
China clay Q.S
Total 100.00


Storage stability of Water Dispersible Granules (WG) of Spirotetramat 7.5%+ Benzpyrimoxan 10.0%
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
Spirotetramat content percent by mass 7.125 to 8.250 7.55 7.52 7.55
Benzpyrimoxan contnet percent by mass 9.5 to 10.5 10.2 10.1 10.2
Spirotetramat suspensibility percent min. 70 97.05 96.95 96.14
Benzpyrimoxan suspensibility percent min. 70 96.02 95.62 95.51
pH range (1% aq. Suspension) 4.0 to 6.5 5.80 5.80 5.70
wettability sec. max. 60 9 10 10
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.4 1.2 1.1
Room temperature storage stability up to 12 months
Parameters specification (in house) 1 month 6 month 12 month
Spirotetramat content percent by mass 7.125 to 8.250 7.55 7.54 7.53
Benzpyrimoxan contnet percent by mass 9.5 to 10.5 10.2 10.20 10.18
Spirotetramat suspensibility percent min. 70 97.05 96.95 96.14
Benzpyrimoxan suspensibility percent min. 70 96.02 95.62 95.51
pH range (1% aq. Suspension) 4.0 to 6.5 5.80 5.80 5.70
wettability sec. max. 60 9 10 10
wet sieve (45 micron) percent by mass min. 98.5 99.5 99.2 99.3
bulk density (g/ml) 0.45 to 0.65 0.48 0.48 0.48
moisture content percent by mass max. max. 2% 1.4 1.2 1.1

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

To study the synergistic effect of Spirotetramat and insecticide selected from flupyrimin and benzpyrimoxan, field trial was conducted in paddy (Oryza sativa) crop to evaluate the bio-efficacy against brown plant hopper (BPH) Nilaparvata lugens.

Experiment 1: Control of brown plant hopper (BPH), Nilaparvata lugen in paddy/rice crop.
Crop & Variety : Paddy, Gurjari
Location : Umreth, Anand, Gujarat
Treatments : Elevan (11)
Replication : Three
Plot size : 30 m2 (6 m x 5 m)
Crop Stage at spraying: Panicle emergence stage (77 days after transplanting)
Method of Application: Foliar spray with back pack sprayer fitted with hollow cone nozzle
Agronomic Practices: Fertilizer, irrigation, inter culturing and weeding done as per the crop requirement.
Observation Methods:
Record the number of brown plant hopper (nymph+adult) per hill. Such ten hills per plot at before spray and 5th and 10th day after spray application (DAA). The bio efficacy data was recorded from First spray. Second spray was given after 15 days of first spray and yield data were recorded and presented in terms of kg per plot.
Calculate percent insect control and then calculate Colby ratio to study synergism.

Table 1: Treatment composition
Treatment Number Treatment Details Formulation (Per Hectare) Active Ingredient (g/h)

T1 Spirotetramat 7.5%+Flupyrimin 10% SC 500 ml 37.5+50
T2 Spirotetramat 7.5%+Benzpyrimoxan 10% SC 500 ml 37.5+50
T3 Spirotetramat 5%+Flupyrimin 15% SC 500 ml 25+75
T4 Spirotetramat 5%+Benzpyrimoxan 15% SC 500 ml 25+75
T5 Spirotetramat 5% SC 500 ml 25
T6 Spirotetramat 7.5% SC 500 ml 37.5
T7 Flupyrimin 10% SC 500 ml 50
T8 Flupyrimin 15% SC 500 ml 75
T9 Benzpyrimoxan 10% SC 500 ml 50
T10 Benzpyrimoxan 15% SC 500 ml 75
T11 Untreated control (UTC) 0 0
SC- Suspension concentrate

Table 2: BPH (%) Control
Treatment Details % BPH Control Observed % BPH Control Expected Colby Ratio o/e
5 DAA 10 DAA 5 DAA 10 DAA 5 DAA 10 DAA
T1 98.6 90.2 78.67 65.66 1.25 1.37
T2 97.3 91.4 84.32 75.74 1.15 1.21
T3 98.2 92.6 79.93 63.49 1.23 1.46
T4 96.8 90.5 85.52 72.27 1.13 1.25
T5 51.4 36.4
T6 60.2 48.6
T7 46.4 33.2
T8 58.7 42.6
T9 60.6 52.8
T10 70.2 56.4
T11 0.0 0.0
DAA- Days After Application
The field trial results shows synergistic activity of spirotetramat+flupyrimin and spirotetramat+benzpyrimoxan in terms of BPH (Paddy Brown Plant Hopper) control (% insect control and duration of control, i.e. residual control) (Colby ratio > 1).
Table 3: Grain yield
Treatment Number Treatment Details Formulation (Per Hectare) Active Ingredient (g/h) Grain Yield (kg/plot) % Yield increase over Untreated

T1 Spirotetramat 7.5%+ Flupyrimin 10% SC 500 ml 37.5+50 16.8 64.7
T2 Spirotetramat 7.5%+ Benzpyrimoxan 10% SC 500 ml 37.5+50 17.1 67.6
T3 Spirotetramat 5%+ Flupyrimin 15% SC 500 ml 25+75 16.4 60.8
T4 Spirotetramat 5%+ Benzpyrimoxan 15% SC 500 ml 25+75 17.7 73.5
T5 Spirotetramat 5% SC 500 ml 25 10.7 4.9
T6 Spirotetramat 7.5% SC 500 ml 37.5 11.8 15.7
T7 Flupyrimin 10% SC 500 ml 50 10.8 5.9
T8 Flupyrimin 15% SC 500 ml 75 12.4 21.6
T9 Benzpyrimoxan 10% SC 500 ml 50 11.6 13.7
T10 Benzpyrimoxan 15% SC 500 ml 75 12.8 25.5
T11 Untreated control (UTC) 0 0 10.2 0.0

The field trial results shows higher (>60% increase over untreated) grain yield were obtained from the combination treatment spirotetramat+flupyrimin and spirotetramat+benzpyrimoxan, which much higher compared to their solo treatment.
,CLAIMS:
1. A synergistic insecticidal composition comprising:
I) Spirotetramat in the range from 0.1 to 50% by weight of the composition; and
II) Insecticide in the range from 0.1 to 50% by weight of the composition wherein the said insecticide is selected from flupyrimin or benzpyrimoxan.

2. The synergistic insecticidal composition as claimed in claim 1, wherein the composition further comprises inactive excipients selected from the group consisting of wetting agent, dispersing agent, antifoaming agent, disintegrating agent, preservative, suspending agents, anti-freezing agent, carrier, or thickener.

3. The synergistic insecticidal composition as claimed in claims 1 wherein the formulation is selected from Capsule suspension (CS), Dispersible concentrate (DC), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion for seed treatment (ES), Emulsion, oil in water (EW), Flowable suspension/concentrate for seed treatment (FS), Granule/ soil applied (GR), Controlled (Slow or Fast) release granules (CR)Solution for seed treatment (LS), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (= flowable concentrate) (SC), Suspo-emulsion (SE), Water soluble granule (SG), Soluble concentrate (SL), Water soluble powder (SP), Water dispersible granule (WG or WDG), Wettable powder (WP), Water dispersible powder for slurry treatment (WS), A mixed formulation of CS en SC (ZC), A mixed formulation of CS en SE (ZE), or A mixed formulation of CS en EW (ZW).

4. The synergistic insecticidal composition as claimed in claims 3 wherein the formulation is Water dispersible granule (WG or WDG).
5. The synergistic insecticidal composition as claimed in claims 3 wherein the formulation is Suspension Concentrate (SC).

6. A process for the preparation of synergistic insecticidal composition as claimed in claim 4 comprising the stes of:
i. Blending filler, wetting agent, dispersing agent, suspending agent, and technical in pre-mixing blender for homogenization;
ii. Grinding pre-blended material obtained in step (i) to obtain finely grinded homogeneous material;
iii. Finely grinded powder obtained in step (ii) is mixed with water to form extrudable dough;
iv. Dough is passed through extruder to obtain Water dispersible granules.

7. A process for the preparation of synergistic insecticidal composition as claimed in claim 5 comprising the steps of:
i. Preparing Gum solution;
ii. Wetting agent, antifreeze agent, dispersing agent and suspending agent are homogenised to obtain a mixture;
iii. Adding technical and adjuvants in th mixture obtained in step (ii) followed by homogenizing to obtain uniform slurry;
iv. Adding halfpart of antifoam to the slurry obtained in step (iii);
v. Grinding the material obtained in step (iv);
vi. Adding remaining half part of antifoam in the formulation obtained in step (v);
vii. Adding Gum solution to the formulation obtained in step (v) to obtain the Suspension Concentrate.