DESC:FIELD OF THE INVENTION:

The present invention relates to novel composition of Pymetrozine and Thifluzamide in synergistic bioactive amounts. The present invention also relates to process for preparing the said composition comprising of Pymetrozine and Thifluzamide in synergistic bioactive amounts and with one or more inactive excipients.

BACKGROUND OF THE INVENTION

Pesticides are chemicals that may be used to kill fungus, bacteria, insects, plant diseases, snails, slugs, or weeds among others. These chemicals can work by ingestion or by touch and death may occur immediately or over a long period of time.

Insecticides are a type of pesticide that is used to specifically target and kill insects. Some insecticides include snail bait, ant killer, and wasp killer.

An insecticide is a substance used to kill insects. They include ovicides and larvicides used against insect eggs and larvae, respectively. Insecticides are used in agriculture, medicine, industry and by consumers.

Insecticides can be classified by many ways. One of many classifications is as below:

Systemic insecticides are those in which the active ingredient is taken up, primarily by plant roots, and transported (translocated) to locations throughout the plant, such as growing points, where it can affect plant-feeding pests. Systemic insecticides move within the vascular tissues, either through the xylem (water-conducting tissue) or the phloem (food-conducting tissue) depending on the characteristics of the material.
Contact insecticides are toxic to insects when brought into direct contact. Efficacy is often related to the quality of pesticide application, with small droplets (such as aerosols) often improving performance.

Natural insecticides, such as nicotine, pyrethrum and neem extracts are made by plants as defenses against insects. Nicotine-based insecticides are widely used in the US and Canada, but are barred in the European Union.

Plant-incorporated protectants(PIPs) are systemic insecticides produced by transgenic plants. For instance, a gene that codes for a specific Bacillusthuringiensisbiocidal protein was introduced into corn and other species. The plant manufactures the protein which kills the insect when consumed.

Inorganic insecticides are contact insecticides that manufactured with metals and include arsenates, copper and fluorine compounds, which are now seldom used, and sulfur, which is commonly used.

Organic insecticides are contact insecticides that comprise the largest numbers of pesticides available for use today.

The mode of action describes how the pesticide kills or inactivates a pest. It provides another way of classifying insecticides. Mode of action is important in understanding whether an insecticide will be toxic to unrelated species, such as fish, birds and mammals.

Insecticidal classes which covers majority of the insecticides are as below:

Organophosphates and carbamates
Organophosphates target the insect's nervous system. Organophosphates interfere with the enzymes acetylcholinesterase and other cholinesterases, disrupting nerve impulses and killing or disabling the insect. Organophosphate insecticides and chemical warfare nerve agents (such as sarin, tabun, soman, and VX) work in the same way. Organophosphates have a cumulative toxic effect to wildlife, so multiple exposures to the chemicals amplify the toxicity.

Carbamate insecticides have similar mechanisms to organophosphates, but have a much shorter duration of action and are somewhat less toxic.

Organochlorides
The best-known organochloride, DDT (Dichlorodiphenyltrichloroethane), was created by Swiss scientist Paul Müller. For this discovery, he was awarded the 1948 Nobel Prize for Physiology or Medicine. DDT was introduced in 1944. It functions by opening sodium channels in the insect's nerve cells. The contemporaneous rise of the chemical industry facilitated large-scale production of DDT and related chlorinated hydrocarbons.

Neonicotinoids
Neonicotinoids are synthetic analogues of the natural insecticide nicotine (with much lower acute mammalian toxicity and greater field persistence). These chemicals are acetylcholine receptor agonists. They are broad-spectrum systemic insecticides, with rapid action (minutes-hours). They are applied as sprays, drenches, seed and soil treatments. Treated insects exhibit leg tremors, rapid wing motion, stylet withdrawal (aphids), disoriented movement, paralysis and death. Imidacloprid may be the most common.

Pyrethroids
Pyrethroid pesticides mimic the insecticidal activity of the natural compound pyrethrum. These compounds are non-persistent sodium channel modulators and are less toxic than organophosphates and carbamates. Compounds in this group are often applied against household pests.

Ryanoids
Ryanoids are synthetic analogues with the same mode of action as ryanodine, a naturally occurring insecticide extracted from Ryaniaspeciosa (Flacourtiaceae). They bind to calcium channels in cardiac and skeletal muscle, blocking nerve transmission.

Plant-incorporated protectants
Transgenic crops that act as insecticides began in 1996 with Bt corn that produces the Cry protein, derived from the bacterium Bacillus thuringiensis, which is toxic to moth larvae such as the European corn borer. The technique has been expanded to include the use of RNA interference RNAi that fatally silences crucial insect genes. RNAi likely evolved as a defense against viruses. Midgut cells in many larvae take up the molecules and help spread the signal. The technology can target only insects that have the silenced sequence, as was demonstrated when a particular RNAi affected only one of four fruit fly species. The technique is expected to replace many other insecticides, which are losing effectiveness due to the spread of pesticide resistance.

Fungi serve as the planet's decomposers by breaking down organic material in nature, while many form healthy symbiotic relationships with plants in the soil. Unfortunately some fungi develop parasitic relationships with plants where the plant is harmed making it important to have the proper fungicide to minimize those effects.

Fungi are plants which obtain their nutrition from an organic carbon source. The body of the fungus secretes enzymes which degrade the organic substrate on which they are growing and yield smaller entities. These in turn are absorbed into the body of the fungus and are metabolized and provide energy to carry on vital processes.

Fungicides can either be contact, translaminar or systemic. Contact fungicides are not taken up into the plant tissue, and protect only the plant where the spray is deposited; translaminar fungicides redistribute the fungicide from the upper, sprayed leaf surface to the lower, unsprayed surface; systemic fungicides are taken up and redistributed through the xylem vessels. Few fungicides move to all parts of a plant. Some are locally systemic, and some move upwardly.

Fungicides also can be classified based upon their chemical composition. Chemically, organic molecules are those that contain carbon atoms in their structure whereas inorganic molecules do not. Many of the first fungicides developed were inorganic compounds based on sulfur or metal ions such as copper, tin, cadmium and mercury that are toxic to fungi. Copper and sulfur are still widely used. Most other fungicides used today are organic compounds and thus contain carbon. The term "organic" as used here is based on chemistry terminology and differs from "organic" used to describe a system of agriculture that strives to be holistic and to enhance agro ecosystem health.

Fungicides kill fungi by damaging their cell membranes, inactivating critical enzymes or proteins, or by interfering with key processes such as energy production or respiration. Others impact specific metabolic pathways such as the production of sterols or chitin. In recent developments, the newly developed fungicides are unique in that they do not directly affect the pathogen itself. Many of new fungicides elicit a response from the host plant known as "systemic acquired resistance" (SAR). These SAR inducers basically mimic chemical signals in plants that activate plant defense mechanisms such as the production of thicker cell walls and anti-fungal proteins. The utility of SAR inducers, however, has been limited so far since many pathogens are capable of over-powering such defenses.

Fungicide resistance is a stable, heritable trait that results in a reduction in sensitivity to a fungicide by an individual fungus. This ability is obtained through evolutionary processes. Fungicides with single-site mode of action are at relatively high risk for resistance development compared to those with multi-side mode of action. Most fungicides being developed today have a single-site mode of action because this is associated with lower potential for negative impact on the environment, including non-target organisms.

When fungicide resistance results from modification of a single major gene, pathogen subpopulations are either sensitive or highly resistant to the pesticide. Resistance in this case is seen as complete loss of disease control that cannot be regained by using higher rates or more frequent fungicide applications. This type of resistance is commonly referred to as "qualitative resistance."

The control of phytopathogenic fungi is of great economic importance since fungal growth on plants or on parts of plants inhibits production of foliage, fruit or seed, and the overall quality of a cultivated crop.

Pymetrozine was first disclosed in US4931439 and US4996325.Pymetrozine is chemically known as (E)-4,5-dihydro-6-methyl-4-(3-pyridylmethyleneamino)-1,2,4-triazin-3(2H)-one and having chemical structure as below;

The mode of action of Pymetrozine in insects has not been precisely determined biochemically, but it may involve effects on neuroregulation or nerve-muscle interaction. Physiologically, it appears to act by preventing these insects from inserting their stylus in to the plant tissue.

Pymetrozine is selective against Homoptera, causing them to stop feeding. Pymetrozine is used in control of aphids and whitefly in vegetables, potatoes, ornamentals, cotton, deciduous and citrus fruit, tobacco, hops; both juvenile and adult stages are susceptible and also control planthoppers in rice. Pymetrozine application rates vary from 150 g/ha on potatoes to 200-300 g/ha on ornamentals, tobacco and cotton; 10-30 g/hl on vegetables, fruit and hops. Pymetrozine is available in market with Dispersible powder (DP); Granule (GR); Wettable powder (WP); Water dispersible granules (WG) formulation.

Thifluzamide was first disclosed in US5045554. Chemically Thifluzamide is known as 2',6'-dibromo-2-methyl-4'-trifluoromethoxy-4-trifluoromethyl-1,3-thiazole-5-carboxanilide. Chemical structure of Thifluzamide is as below;

Thifluzamide is highly active against Basidiomycete fungi, in particular Rhizoctonia solani, primarily in rice, potatoes, and turf markets.

The main concern with the use of pesticide is the development of resistance by the pests for that particular pesticide and at the end one has to apply more concentrated formulation of the pesticide. The high amount of pesticide may results in the toxicity to human beings as well as has bad effect on environment.

Previously people have tried many alternatives and option to overcome this problem and as a result developed poly mixture of pesticide, use of non-toxic ingredients and developing novel formulations which provides effective amount of the pesticide and at the required part only.

However the use of poly mixture containing large number of pesticides poses a problem in many was like preparing formulation of multiple pesticides with different chemical properties and behavior and physical properties. It also creates challenge for formulator in term of compatibility and stability of all the pesticide along with used excipients in the formulation.

US 6,486,157 relates to a novel method of controlling pests in and on transgenic crops of useful plants with pymetrozine; profenofos; a benzoylurea-derivative, especially lufenuron; or a carbamate-derivative, especially fenoxycarb.

EP 2422620 A1 disclose a novel pesticide compositions of ethiprole and pymetrozine with good insecticidal, acaricidal, nematicidal activities. In use, a pesticidally effective amount of a composition of the ethiprole and pymetrozine for protecting a seed and/or shoots and foliage of a plant grown from the seed from damage by an animal pest, the method comprising treating an unsown seed with above composition, wherein the weight ratio of ethiprole and pymetrozine is between 25:1 and 1:100 .

Indian patent application 1302/MUMNP/2012 relates to an agrochemical mixture for increasing the health of a plant, comprising as active ingredients 1) a herbicidal compound (I) selected from the group consisting of: (i) Benzoic acids, selected from chloramben, dicamba and 2,3,6-TBA; (ii) Pyridine carboxyiic acids, selected from clopyralid, fluroxypyr, picloram and triclopyr; (iii) Quino-line carboxyiic acids, selected from quinclorac and quinmerac; (iv) benazolin-ethyl; and 2) a fungicidal compound (II) selected from the group consisting of N-(3",4",5"-trifluorobiphenyl-2-yl)- 3-difluoromethyH -memyi-lH-pyrazole-4-carboxamide (common name: fluxapyroxad), N-[2-(4"-trifluoromemylthio)-biphenyi]-3-difluoromethyl-l -methyi-1 H-pyrazole-4-carboxamide, -N-(3",4"-dichloro-5-fiuorobiphenyl-2-yl)-3-difluoromethyl-l-memylpyrazoIe-4-carboxamide (common name: bixafen), N-[2-(l,3-dirnethylbutyl)-phenyI]-l,3-dimethyl-5-fluoro-l H-pyrazole-4-carboxamide (common name: penfluien), N-(2-bicyclopropyl-2-yl-phenyi)-3- difluoromethyl-1 -methyl-I H-pyrazoIe-4-carboxamide (common name: sedaxane), N- [I,2,3,4-tetrahydro-9-(l -memvlethyl)-l,4-methanonaphthalen-5-yl]-3-(difluoromethyl)- 1 -methyl-1 H-pyrazole-4-carboxamide (common name: isopy-razam), N-[2-(l,3-dimethyibutyl)-3-thienyl]-l -methyi-3-(trifluoromethyl)-l H-pyrazole-4-carboxamide (common name: penthiopyrad), boscalid, fluopyram, flutolanil, furametpyr, mepronil and thifluzamide in synergistically effective amounts.

Chines patent application CN 103329892 relates to pesticide for controlling rice sheath blight diseases and false smut, in particular to a suspending agent of thifluzamide and tebuconazole composite pesticide and a preparation method of the suspending agent. The suspending agent is prepared by the following ingredients in parts by weight: 20 parts of thifluzamide, 32 parts of tebuconazole, 18 parts of emolsifier and 30 parts of solvent.

However still there is a need for a composition of specific pesticide which overcomes some of the existing problems and can be prepared easily without much complex manufacturing process.

Inventors of the present invention have surprisingly found that the novel composition of Pymetrozine and Thifluzamide as described herein in can provide solution to the above mentioned problems.

SUMMARY OF THE INVENTION

The present invention relates to a novel pesticidal composition which comprises of Pymetrozine and Thifluzamide in synergistic bioactive amounts.

Further the present invention also relates to process for preparing the novel composition comprising bioactive amounts of Pymetrozine and Thifluzamide with one or more inactive excipients.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides novel composition comprising of Pymetrozine and Thifluzamide in synergistic bioactive amounts with one or more inactive excipients.

"Bioactive amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.

The insecticidal and/or fungicidal composition can be classified as below:

a) Dry - Sprayable
a.1) WP – Wettable powders:
A solid pesticide formulation – micronized to powder form and typically applied as suspended particles after dispersion in water.

a.2) WG or WDG – Water dispersible granule:
A pesticidal formulation consisting of granules to be applied after disintegration and dispersion in water. Water dispersible granules can be formed by a) agglomeration, b) spray drying, or c) extrusion techniques. It can also be termed as water soluble granules (WSG) or soluble granules (SG).

b) Liquid Sprayable
b.1) SL – Soluble Concentrate:
A soluble concentrate is in powder form intended for dilution with water or directly in solution from. In both the case, the end result will be clear solution of the insecticide in the water without any visible un-dissolved particles.

b.2) SC – Suspension Concentrate
A stable suspension of solid pesticide(s) in a fluid usually intended for dilution with water before use. For a good formulation or ideal SC formulation, it should be stable and do not sediment over time.

b.3) EC – Emulsifiable Concentrate
A solution of a pesticide with emulsifying agents in a water insoluble organic solvent which will form an emulsion when added to water. In most of the case it is oil in water type emulsion to make it easy for application. EC formulation should be storage stable without any visible cracking of emulsion.

b.4) ME – Microemulsion
A solution of a pesticide with emulsifying agents in a water insoluble organic solvent which will form a solution/emulsion when added to water. The difference between EC and ME is the particle size of the actives in the final form.

b.5) OD – Oil Dispersion
Oil dispersions (OD) are one type of liquid formulation which is stable suspensions of active ingredients in a water-immiscible fluid which may contain other dissolved active ingredients and is intended for dilution with water before use.

b.6) CS – Capsule Suspension
Suspension of micro-encapsulated active ingredient in an aqueous continuous phase, intended for dilution with water before use.

b.7) SE- Suspension emulsion
A suspension emulsion or suspo emulsion (SE) consists of an organic phase with a dissolved active ingredient and an aqueous suspension phase, in which the active ingredient is dispersed in water.

b.8) Dispersible concentrate (DC)
Dispersible concentrate (DC) is a liquid homogeneous formulation to be applied as a solid dispersion after dilution in water. There are many formulations which contains the part characteristics of EC and part characteristics of DC.

c) Dry – Spreadable Granule
Dry spreadable granules are dry granules which can be applied with a dry spreader to a target area and later when such granules get exposed to water via, for example, rain or irrigation, will not only readily disintegrate, but actively spread on solid substrates so as to achieve disintegration area diameter to original granule diameter ratios.

Dry spreadable granules should possess good hardness and an ability to maintain integrity upon normal, commercial handling in a dry spreading operation and yet be capable of quickly disintegrating or scattering upon what may be a minimal exposure to water, such as, for example, a light rain.

d) GR – Soil applied Granule on inert or fertilizer carrier
This formulation is in the form of granules which can be applied on inert carrier or the carrier which is fertilizer.

e) Mixed formulation

e.1) ZC Formulation (Mix of CS and SC)
“ZC formulation” is the international denominations adopted by the FAO (Food and Agricultural Organization of the United Nations) to designate "stable aqueous suspension of microcapsules and solid fine particles"

ZC is a mixed formulation of CS and SC and is a stable aqueous suspension of microcapsules and solid fine particles, each of which contains one or more active ingredients. The formulation is intended for dilution into water prior to spray application. Formulating the active ingredients together eliminates the need for tank mixing, which can lead to incompatibility, and facilitates control of a wider range of pests with fewer applications. Like other aqueous liquid formulations, ZC formulations are easy to handle and measure, dust free, non-flammable and offer good miscibility with water.

One or more of the active ingredients is encapsulated for various purposes, such as to increase the residual biological activity, or to reduce the acute toxicity, or to obtain a physical or chemically stable water-based formulation. The purpose determines whether the “free” active ingredient and the “release rate” are relevant properties of a specific product.

The term WDG, DG, WSG and SG are synonyms and can be used inter changeably and convey the same meaning.

The term composition and formulation are synonyms and can be used inter changeably and convey the same meaning.

Composition of the present invention can be in any of the form described above.

Pymetrozine and Thifluzamide which are active ingredients for the present compositionare present in ratio of 20: 1 to 1:20; preferably are in ratio of 10:1 to 1:10 and most preferably are present in ratio of 1: 2 to 2:1.

The novel composition of Pymetrozine and Thifluzamide is effective for management of mixed infestation of various sucking insects and fungal diseases in following crops. In rice, it is useful for control of sheath blight, blast, brown spot diseases along with hoppers. In Potato, it can be used for control of black scurf, aphids and jassid. In chilly crop it can be used for control of root rot, thrips and aphid.

The novel composition of the present invention can be used for 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), Castor (Ricinus communis), Green gram (Vigna radiate), 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), Caluflower (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) and Melons (Cucumis melo), 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)

The present composition preferably is active against normally sensitive and resistant species and against all or some stages of development.

The Insects-pests includes are from the class Insecta, from the order Coleoptera, for example, Agriotes spp., Anobium punctatum, Anthonomus spp., Anthrenus spp., Bruchidius obtectus, Bruchus spp., Cassida spp., Cerotoma trifurcata, Conoderus spp.,Cosmopolites spp., Diabrotica spp., Dichocrocis spp., Dicladispa armigera, Epilachna spp., Gnathocerus cornutus, Hypothenemus spp., Lachnosterna consanguinea, Lasioderma serricorne, Latheticus oryzae, Lathridius spp., Lema spp., Leptinotarsa decemlineata, Leucopteraspp., Lissorhoptrus oryzophilus, Melanotus spp., Melolontha spp., Oryzaephilus surinamensis, Oryzaphagus oryzae, Phyllotreta spp., Rhizopertha dominica, Sitophilus oryzae, Tribolium spp., Trogoderma spp., from the order Diptera, for example, Agromyza spp., Asphondylia spp., Bactrocera spp., Contarinia spp., Dacus oleae, Drosophila spp., Liriomyza spp., Musca spp., Tetanops spp., Tipula spp.; from the order Heteroptera, for example, Leptocorisa spp., Leptocorisa varicornis, Lygus spp., Miridae, from the order Homoptera, for example, Acizzia spp., Acyrthosipon spp., Amrasca spp., Aonidiella spp., Aphis spp., Aulacorthum solani, Bemisia tabaci, Brevicoryne brassicae, Carneocephala fulgida, Ceratovacuna lanigera, Coccus spp., Cryptomyzus ribis, Dialeurodes citri, Diaphorina citri, Drosicha spp., Empoasca spp., Geococcus coffeae, Idiocerus spp., Lipaphis erysimi, Macrosiphum spp., Myzus spp., Nephotettix spp., Nettigoniclla spectra, Nilaparvata lugens, Phenacoccus spp., Phylloxera spp., Planococcus spp., Pseudococcus spp., Psylla spp., Pyrilla spp., Rastrococcus spp., Rhopalosiphum spp., Saissetia spp., Sogatella furcifera, Toxoptera spp., Trialeurodes vaporariorum, from the order Hymenoptera, for example, Athalia spp., Diprion spp., Solenopsis invicta, from the order Isoptera, for example, Coptotermes spp., Cornitermes cumulans, Cryptotermes spp., Incisitermes spp., Microtermes obesi, Odontotermes spp., Reticulitermes spp.; from the order Lepidoptera, for example, Agrotis spp., Anarsia spp., Anticarsia spp., Chilo spp., Cnaphalocerus spp., Maruca testulalis, Scirpophaga spp., Sesamia inferens, Trichoplusia spp., Tuta absoluta, from the order Thysanoptera, for example, Anaphothrips obscurus, Baliothrips biformis, Drepanothrips reuteri, Enneothrips flavens, Frankliniella spp., Heliothripsspp., Hercinothrips femoralis, Rhipiphorothrips cruentatus, Scirtothrips spp., Taeniothrips cardamomi, Thrips spp.

Below diseases can be controlled by composition of the present invention:
The diseases caused by powdery mildew pathogens, for example Blumeria graminis, Podosphaera leucotricha, Sphaerotheca fuliginea, Uncinula necator, diseases caused by rust disease pathogens, for example Gymnosporangium sabinae, Hemileia vastatrix, Phakopsora pachyrhizi and Phakopsora meibomiae, Puccinia recondite, Puccinia triticina, Puccinia graminis, Uromyces appendiculatus, diseases caused by pathogens from the group of the Oomycetes, Algubo candida, Bremia lactucae, Peronospora pisi, Phytophthora infestans, Plasmopara viticola, Pseudoperonospora humuli or Pseudoperonospora cubensis, Pythium ultimum, leaf blotch diseases and leaf wilt diseases caused, for example, Alternaria solani, Cercospora oryzae, Cladiosporium cucumerinum, Cochliobolus sativus, Drechslera spp., Cochliobolus miyabeanus, Colletotrichum lindemuthanium, Gloeosporium laeticolor, Glomerella cingulata, Guignardia species, Guignardia bidwelli, Leptosphaeria maculans, Leptosphaeria nodorum, Magnaporthe grisea, Microdochium nivale, Mycosphaerella graminicola, Phaeosphaeria nodorum, Pyrenophora teres, Pyrenophora tritici repentis, Ramularia areola, Rhynchosporium secalis, Septoria apii, Septoria lycopersii, Venturia inaequalis. Root and stem diseases caused, for example by Corticium graminearum, Fusarium oxysporum, Gaeumannomyces graminis, Rhizoctonia solani, Sarocladium oryzae, Sclerotium oryzae, Tapesia acuformis, Thielaviopsis basicola.

Ear and panicle diseases (including corn cobs) caused, for example, by Alternaria spp., Apergillus flavus, Cladosporium cladosporioides, Claviceps purpurea, Fusarium culmorum, Gibberella zeae, Monographella nivalis, Septoria nodorum, diseases caused by smut fungi, Sphacelotheca reiliana, Tilletia caries, T. controversa, Urocystis occulta, Ustilago nuda, U. nuda tritici,fruit rot caused, for example, by Aspergillus flavus, Botrytis cinerea, Penicillium expansum and P. purpurogenum, Sclerotinia sclerotiorum, Verticilium alboatrum.

Seed and soilborne decay, mould, wilt, rot and damping-off diseases caused, for example, by Alternaria brassicicola, Aphanomyces euteiches, Ascochyta lentis, Apergillus flavus, Cladosporium herbarum, Cochliobolus sativus, (Conidiaform: Drechslera, Bipolaris Syn: Helminthosporium), Colletotrichum coccodes, Fusarium culmorum, Gibberella zeae, Macrophomina phaseolina, Monographella nivalis, Penicillium expansum, Phoma lingam, Phomopsis sojae, Phytophthora cactorum, Pyrenophora graminea, Pyricularia oryzae, Pythium ultimum, Rhizoctonia solani, Rhizopus oryzae, Sclerotium rolfsii, Septoria nodosum, Typhula incarnate, Verticillium dahlia, Cancers, galls and witches' broom caused, for example, by Nectria galligena, wilt diseases caused Monilinia taxa, leaf blister or leaf curl diseases caused by Exobasidium vexans, Taphrina deformans. Decline diseases of wooden plants caused, for example, by Phaemoniella clamydospora, Phaeoacremonium aleophilum and Fomitiporia mediterranea; Eutypa dyeback, caused for example by Eutypa lata; Ganoderma diseases caused for example Ganoderma boninense, Rigidoporus diseases caused for example by Rigidoporus lignosus.

As per one embodiment the novel composition of present invention used for control of insects in rice selected from stem borer (Chilo suppressalis, Diatraea lineolata, Elasmopalpus lignosellus, Scirpophaga incertulas, Sesamia cretica, Sesamia inferens), Planthoppers (Laodelphax striatellus, Nilaparvata lugens, Sogatella furcifera, Tagosodes orizicolus, Nephotettix cincticeps, Nephotettix virescens, Nephotettix nigropictus), Rice gall midge (Orseolia oryzae), Rice leaffolder (Cnaphalocrocis medinalis, Marasmia patnalis, Marasmia bilinealis, Marasmia suspicalis), Rice bug (Leptocorisa acuta, Leptocorisa biguttata, Lepotcorisa chinensis), Stink bug (Oebalus pugnax, Oebalus poecila, Oebalus ypsilon-griseus), Rice hispa (Dicladispa armigera), Rice water weevil (Lissorhoptrus oryzophilus), Rice thrips (Stenchaetothrips biformis, Haplothrips aculeatus), Rice caseworm (Nymphula depunctalis), Rice whorl maggot (Hydrellia philippina), Rice leaf miner (Hydrellia griseola), Rice stem maggot (Hydrellia sasakii), Rice black bug (Scotinophara coarctata, Scotinophara lurida), Common army worm ( Mythimna unipuncta), Rice swarming caterpillar (Spodoptera mauritia acronyctoides), fall armyworm (Spodoptera frugiperda), rice root aphid (Tetraneura nigriabdominalis) and control of insects in potato selected from Potato Aphid, Jassid and Whitefly.

As per another embodiment of the present invention, novel formulation of the present invention is used to control of fungi in rice selected from Sheath spot ( Ceratobasidium oryzae-sativae, Rhizoctonia oryzae-sativae [anamorph]), Black kernel (Curvularia lunata Cochliobolus lunatus [teleomorph], Blast (Pyricularia grisea, Pyricularia oryzae, Magnaporthe grisea [teleomorph]), Brown spot (Cochliobolus miyabeanus Bipolaris oryzae [anamorph]), Crown sheath rot (Gaeumannomyces graminis), Downy mildew (Sclerophthora macrospora), Eyespot (Drechslera gigantean), False smut (Ustilaginoidea virens), Kernel smut (Tilletia barclayana =Neovossia horrid), Leaf smut (Entyloma oryzae), Leaf scald (Microdochium oryzae), Narrow brown leaf spot (Cercospora janseana = Cercospora oryzae, Sphaerulina oryzina [teleomorph]), Pecky rice/Kernel spotting (Cochliobolus miyabeanus, Curvularia spp., Fusarium spp., Microdochium oryzae, Sarocladium oryzae), Root rots (Fusarium spp., Pythiurm spp., Pythium dissotocum, Pythium spinosum), Seedling blight (Cochliobolus miyabeanus, Curvularia spp., Fusarium spp., Rhizoctonia solani, Sclerotium rolfsii), Sheath blight (Thanatephorus cucumeris, Rhizoctonia solani [anamorph]), Sheath rot (Sarocladium oryzae), Sheath spot (Rhizoctonia oryzae), Alternaria padwickii leaf spot and control of fungi in potato selected from Potato Early blight, Tuber rot and Cercospora leaf spot.

The novel composition of the present invention in addition to Pymetrozine and Thifluzamide, further comprises inactive excipients including but not limited to dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents (also referred to as “stickers” or “binders”) and buffering agent.

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 compositions 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 compositions, 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. Nonionics 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 compositions 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 compositions: 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 compositions 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 composition 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 compositions 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 agentcan be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, polysaccharides such as starch and cellulose derivatives, vinylalcohol, 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 invention 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 esteraliphatic polyester blends, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof.

Buffering agent as used herein is selected from group consisting of calcium hydroxyapatite, Potassium 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 composition 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 wettable dry granules (WDG) can be applied after disintegration and dispersion in water. Water dispersible granules can be formed by a) agglomeration, b) spray drying, or c) extrusion techniques.

WDG compositions offer a number of advantages in packaging, ease of handling and safety. The WDG are preferably of uniform size and which are free flowing, low dusting and readily disperse in water to form a homogenous solution of very small particles which may pass through conventional spray nozzles. Ideally WDG compositions when dispersed in water under gentle agitation for five minutes have residues of less than 0.01% on a 150 µm sieve screen and less than 0.5% on a 53 µm screen. The granules can usually be measured accurately by volume which is convenient for the end user.

The SC composition can be prepared by below described method;
STEP-I: Adding anti-microbial agent and gum in water under continuous stirring followed by slow addition. Continuing stirring until homogeneous dispersion is formed.
STEP-II: Mixing anti-freezing agent, dispersant, wetting agent, anti-microbial agent and anti-foaming agent in water for 30 minute until homogeneous solution is formed. Finally add Pymetrozine and Thifluzamide is added slowly under continuous stirring at 30 minute till homogeneous dispersion is obtained. Milling the slurry through bead mill until required particle size is achieved.
Step-III: Adding rest of water, anti-foaming agent and gum solution under continuous stirring to get desired viscosity of the suspension. Continue the stirring for about 4 hr. to obtain homogeneous composition.

The process for preparing the present novel 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: Suspension Concentrate (SC) formulation
COMPOSITIONS Pymetrozine 20%+ Thifluzamide 1% SC Pymetrozine 15%+ Thifluzamide 10% SC Pymetrozine 12.5%+ Thifluzamide 9% SC Pymetrozine 12.5%+ Thifluzamide 7% SC Pymetrozine 12.5%+ Thifluzamide 5% SC Pymetrozine 10%+ Thifluzamide 9% SC Pymetrozine 10%+ Thifluzamide 7% SC Pymetrozine 10%+ Thifluzamide 5% SC Pymetrozine 1%+ Thifluzamide 20% SC
Pymetrozine (95%) 21.60 16.30 13.60 13.60 13.60 11.00 11.00 11.00 1.80
Thifluzamide (95%) 1.60 11.00 10.00 7.90 5.80 10.00 7.90 5.80 21.60
Ethoxylated Fatty Alcohol 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00
Nonionic polyalkylene glycol ether 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50
Acrylic graft copolymer 3.00 3.00 3.00 3.00 3.00 3.00 3.00 3.00 3.00
Alkylated naphtalene sulfonate, sodium salt 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50
Bentonite Clay 1.50 1.50 1.50 1.50 2.00 1.50 2.00 2.00 1.50
Silicone antifoam 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50
Benzisothiazoline 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20
Glycol 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00
Polysaccharides 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15
Water 63.5 59.35 63.05 65.15 66.8 65.65 67.25 69.35 63.25
TOTAL 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00

Procedure:
Step 1 Gum Solution should be made 12-18 hour prior to use. Take required quantity of water, biocide, and defoamer and homogenize, 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 Flowable concentrate/ Suspension concentrate/ Flowable slurry production.
Step 3 Add required quantity of Wetting agent, dispersing agent & suspending agents, colourant/deye and homogenize the contents for 45 – 60 minutes using high shear homogenizer.
Step 4 Then add technical and other remaining adjuvants excluding ‘antifreeze & thickeners’ are added to it and homogenized to get uniform slurry ready for grinding.
Step 5 Before grinding half the quantity of antifoam was added and then material was subjected to three cycles of grinding in Dyno mill.
Step 6 Half quantity of the antifoam was added along with antifreeze after grinding process completes and before sampling for in process analysis.

Example 2: Oil Dispersion (OD) formulation
COMPOSITIONS Pymetrozine 12.5% + Thifluzamide 9% OD Pymetrozine 12.5% + Thifluzamide 7.5% OD Pymetrozine 12.5% + Thifluzamide 5% OD Pymetrozine 10% + Thifluzamide 7.5% OD Pymetrozine 10% + Thifluzamide 5% OD
Pymetrozine (95%) 13.60 13.60 13.60 11.00 11.00
Thifluzamide (95%) 10.00 8.20 5.80 8.20 5.80
2-pyrrolidinone, 1-ethenylhexadecyl-, homopolymer 2.00 2.00 2.00 2.00 2.00
Tristyrenephenole with 16 moles EO 3.00 3.00 3.00 3.00 3.00
Dodecyl benzene sulphonic acid sodium salt 5.00 5.00 5.00 5.00 5.00
Fatty alcohol ethoxylate 5.00 5.00 5.00 5.00 5.00
Silicondioxide 0.16 0.16 0.16 0.16 0.16
Cyclohexanone 10.00 10.00 10.00 10.00 10.00
Methylated Rape Seed Oil 51.24 53.04 55.44 55.64 58.04
TOTAL 100.00 100.00 100.00 100.00 100

Procedure:
Step 1 Charge required quantity of vegetable oil in vessel and add polyvinyl pyrrollidone, mix well for 30 minutes using highshear homogenizer and pass through horizontal bead mill.
Step 2 Add required quantity of Wetting agent, dispersing agent & suspending agents and homogenize the contents for 45 – 60 minutes using high shear homogenizer.
Step 3 Then add technical materials and homogenize for further 30 minutes.
Step 4 Now pass this homogenized material through horizontal bead mill to get required particle size.
Step 5 After completion of grinding cycles sample is sent to QC for A.I. & particle size analysis
Step 6 After approval from QC, material is transferred to storage tank till packing.

Example 3: Water Dispersible Granules (WG) formulation
COMPOSITIONS Pymetrozine 25% + Thifluzamide 18% WDG Pymetrozine 25% + Thifluzamide 16% WDG Pymetrozine 25% + Thifluzamide 14% WDG Pymetrozine 20% + Thifluzamide 18% WDG Pymetrozine 20% + Thifluzamide 16% WDG Pymetrozine 20% + Thifluzamide 14% WDG
Pymetrozine (95%) 26.80 26.80 26.80 21.60 21.60 21.60
Thifluzamide (95%) 19.50 17.40 15.25 19.50 17.40 15.25
Sodium salt of Phenol sulphonic acid condensate 3.00 3.00 3.00 3.00 3.00 3.00
Polyacrylate co-polymer 6.00 6.00 6.00 6.00 6.00 6.00
Sodium alkylnaphthalenesulfonate, formaldehyde condensate 3.00 3.00 3.00 3.00 3.00 3.00
Silicone based antifoam 0.50 0.50 0.50 0.50 0.50 0.50
Polyvinyl pyrollidone 1.25 1.25 1.25 1.25 1.25 1.25
Starch 10.00 10.00 15.00 15.00 15.00 15.00
China clay 30.0 32.1 29.20 30.2 32.25 34.40
TOTAL 100.00 100.00 100.00 100.00 100.00 100.00

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 analyzed. After getting approval from QC dept. material is unloaded into 25 kg. HDPE bag with LDPE liner inside.
Step 4 Finely grinded powder is mixer 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 Fluidized 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.

Example 4: Stability Study
4.1) Storage stability Study Data of Pymetrozine 12.5% + Thifluzamide 7% SC (Suspension Concentrate)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
Parameters In House
Description Off-white liquid Complies Complies Complies
Pymetrozine Content 11.875-13.125 12.8 12.5 12.7
Pymetrozine Suspensibility Mini 80% 99 98 99
Thifluzamide Content 6.65-7.7 7.5 7.3 7.45
Thifluzamide Suspensibility Mini 80% 98 98 99
pH 5.0-9.0 8 8 8
Particle size D50 <3, D90 <10 2.5, 8 2.5, 8 2.9, 8.9
Pourability 95 % min 97 96 97
Specific gravity 1.05 – 1.15 1.1 1.1 1.1
Viscosity 350 -900 cps 500 510 530

Room temperature storage study
Specification Study Duration
Parameters In House 1st day 6 month 12 months 36 months
Description Off-white liquid Complies Complies Complies Complies
Pymetrozine Content 11.875-13.125 12.8 12.8 12.77 12.3
Pymetrozine Suspensibility Mini 80% 99 99 99 96
Thifluzamide Content 6.65-7.7 7.5 7.5 7.5 7.1
Thifluzamide Suspensibility Mini 80% 98 98 98 98
pH 5.0-9.0 8 8 8 8
Particle size D50 <3, D90 <10 2.5, 8 2.5, 8 2.5, 8 2.5, 8
Pourability 95 % min 97 97 97 96
Specific gravity 1.05 – 1.15 1.1 1.1 1.1 1.1
Viscosity 350 -900 cps 500 500 500 510

4.2) Storage stability Study Data of Pymetrozine 12.5% + Thifluzamide 7% OD (Oil Dispersion)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
Parameters In House
Description Off-white liquid Complies Complies Complies
Pymetrozine Content 11.875-13.125 12.8 12.5 12.7
Pymetrozine Suspensibility Mini 80% 99 98 99
Thifluzamide Content 6.65-7.7 7.5 7.3 7.45
Thifluzamide Suspensibility Mini 80% 98 98 99
pH 5.0-9.0 8 8 8
Particle size D50 <3, D90 <10 2.5, 8 2.5, 8 2.9, 8.9
Pourability 95 % min 97 96 97
Specific gravity 1.05 – 1.15 1.1 1.1 1.1
Viscosity 350 -900 cps 700 680 690

Room temperature storage study
Specification Study Duration
Parameters In house 1st day 6 month 12 months 36 months
Description Off-white liquid Complies Complies Complies Complies
Pymetrozine Content 11.875-13.125 12.8 12.8 12.77 12.3
Pymetrozine Suspensibility Mini 80% 99 99 99 96
Thifluzamide Content 6.65-7.7 7.5 7.5 7.5 7.1
Thifluzamide Suspensibility Mini 80% 98 98 98 98
pH 5.0-9.0 8 8 8 8
Particle size D50 <3, D90 <10 2.5, 8 2.5, 8 2.5, 8 2.5, 8
Pourability 95 % min 97 97 97 96
Specific gravity 1.05 – 1.15 1.1 1.1 1.1 1.1
Viscosity 350 -900 cps 700 700 700 680

4.3) Storage stability Study of Pymetrozine 25% + Thifluzamide 14% WG(Water Dispersible Granules)
Specification Initial Heat stability study at 54+2 0C for 14 days Cold storage stability at 0+2 0C for 14 days
Parameters In House
Description White to off-white granules Complies Complies Complies
Pymetrozine Content 23.75-26.25 25.5 25.3 25.45
Pymetrozine Suspensibility 70 % minimum 98% 97% 98%
Thifluzamide Content 13.3-14.7 14.5 14.3 14.5
Thifluzamide Suspensibility 70 % minimum 98% 97% 98%
pH 5.0-9.0 8.5 8.5 8.5
Wet-sieve (45 micron sieve) Mini 99.5% 99.8 99.8 99.8
Bulk density 0.35 -0.45 0.4 0.4 0.4
Wettability 60 Sec Max 20 24 20

Room temperature storage study
Specification Study Duration
Parameters In house 1st day 6 month 12 months 36 months
Description White to off-white granules Complies Complies Complies Complies
Pymetrozine Content 23.75-26.25 25.5 25.5 25.5 25.1
Pymetrozine Suspensibility 70 % minimum 98% 98% 98% 94%
Thifluzamide Content 13.3-14.7 14.5 14.5 14.49 14.3
Thifluzamide Suspensibility 70 % minimum 98% 98% 98% 97%
pH 5.0-9.0 8.5 8.5 8.5 8.7
Wet-sieve (45 micron sieve) Mini 99.5% 99.8 99.8 99.8 99.8
Bulk density 0.35 -0.45 0.4 0.4 0.4 0.4
Wettability 60 Sec Max 20 20 20 28

Example 5: Field efficacy trials
Rice (Oryza sativa L.) is the primary source of food for more than half of the world’s population. Occurrence of diseases and insect pests together in rice demands the necessity of fungicidal and insecticidal application at the same place and time. In many endemic areas, sheath blight, brown plant hopper (BPH), leaf folder and stem borer occur at the same stage of the crop growth. Therefore, a combined application of effective fungicides and insecticides is a practical necessity. Farmers in coastal belt of south and east Indian state, are regularly going for 2-3 sprays in rice crop, and mixed combinations of fungicides and insecticides is a common practice in view of labor shortage. Keeping this in view, the study was undertaken with novel compositions of Pymetrozine along with Thifluzamide with different ratio to find their efficacy on Sheath blight and Brown Plant Hopper (BPH). The field study was carried out to evaluate the interaction effect of Pymetrozine and Thifluzamide on rice sheath blight and brown hopper (BPH). The testing samples with various novel formulations with different ratio of Pymetrozine and Thifluzamide were developed at in-house R&D laboratory.
The key objective of this experiment was:
1. To find out the interaction effect of (insecticidal and fungicidal action) on rice sheath blight and brown plant hopper
2. To study the impact of novel formulations with different ration on beneficial / predatory insects in rice crop eco-system
3. To find out the impact on crop yield.
Table 1: Sample compositions comprising of Pymetrozine and Thifluzamide, their formulations and use rate
Sr.No. Sample Code Type of Formulation A.I.(%) in formulation Formulation per Hectare (g or ml) Active Ingredient/Hectare Ratio of Pymetrozine : Thifluzamide
Pymetrozine Thifluzamide Pymetrozine Thifluzamide

1 PT1 SC 20.0% 1.0% 1000 200 10 20 : 1
2 PT2 SC 15.0% 7.5% 1000 150 75 2 : 1
3 PT3 SC 12.5% 9.0% 1000 125 90 1.4 : 1
4 PT4 SC 12.5% 7.0% 1000 125 70 1.8 : 1
5 PT5 SC 12.5% 5.0% 1000 125 50 2.5 : 1
6 PT6 SC 10.0% 9.0% 1000 100 90 1.1 : 1
7 PT7 SC 10.0% 7.0% 1000 100 70 1.4 : 1
8 PT8 SC 7.5% 15.0% 1000 75 150 1 : 2
9 PT9 SC 1.0% 20.0% 1000 10 200 1 : 20
10 PT10 OD 15.0% 7.5% 1000 150 75 2 : 1
11 PT11 OD 12.5% 7.5% 1000 125 75 1.7 : 1
12 PT12 OD 12.5% 5.0% 1000 125 50 2.5 : 1
13 PT13 OD 10.0% 7.5% 1000 100 75 1.33 : 1
14 PT14 OD 7.5% 15.0% 1000 75 150 1 : 2
15 PT15 WG 30.0% 15.0% 500 150 75 2 : 1
16 PT16 WG 25.0% 16.0% 500 125 80 1.6 : 1
17 PT17 WG 25.0% 14.0% 500 125 70 1.8 : 1
18 PT18 WG 20.0% 18.0% 500 100 90 1.1 : 1
19 PT19 WG 20.0% 16.0% 500 100 80 1.25 : 1
20 PT20 WG 12.5% 25.0% 500 62.5 125 1 : 2
21 PRS 1 WG 50.0% _ 400 200 _ _
22 PRS 2 SC _ 24.0% 375 _ 90 _
23 PRS 3 WG+SC 50.0% 24.0% 400+375 200 90 _
24 PRS 4 WG+SC 50.0% 24.0% 250+375 125 90 _
25 PRS 5 WG+SC 50.0% 24.0% 250+290 125 70 _
26 PRS 6 WG+SC 50.0% 24.0% 200+375 100 90 _
27 PRS 7 WG+SC 50.0% 24.0% 200+290 100 70
_
28 Untreated Control _ _ _ _ _ _
_

Note:
A. I. -Active Ingredient, g- Gram, ml –milli liter, SC- Suspension Concentrate, OD –Oil Dispersion, WDG -Water Dispersible Granules, PT1 to PT20- Laboratory Samples of Pymetrozine and Thifluzamide
The experiment was conducted in coastal area of southern state of Andhra Pradesh state. The experiment was conducted in Randomized Block used with 7 m x 7 m net plot size and 30 sets of treatments including one Untreated check and seven sets of prior art samples. The Rice crop was raised with all standard agronomic practices. Spraying was done with back pack sprayer with 500 liter of water spray volume. The experiment initiated as soon as infestation of Brown Plant Hopper (Nilaparvata lugens) and Sheath blight (Rhizoctonia solani). The observations was recorded by counting the no. of hoppers per hill (25 hills per plot) and percent disease severity data collected by observing 100 tillers per plot. The observations were recorded at before spraying and 3, 7 and 10 days after spraying.The field observations were presented in below table. The observations on beneficial insects i.e. Spider and Predatory insects were also recorded along with hopper count and disease rating. The efficacies of various treatments were also judged at the time of harvest by considering grain yield.
% BPH Control = 100 - Number of BPH in treated plot x 100
Number of BPH in Untreated plot

Observation Methodology for Sheath Blight disease:
Observe 100 tillers per plot, representing entire plot.
Rate visually the disease by following below rating

Score Description
0 No Infection
1 Vertical spread of diseases up to 20% of plant height
3 Vertical spread of diseases up to 21-30% of plant height
5 Vertical spread of diseases up to 31-45% of plant height
7 Vertical spread of diseases up to 46-65% of plant height
9 Vertical spread of diseases >66% of plant height

Calculate PDI (%) = Sum of numerical rating x _100_____
Total no of plant observed x Max. Grade

Table 2- Rice Brown Plant Hopper (BPH) control and Sheath blight disease severity

Sample Code Type of Formulation Active Ingredient/Hectare % Brown Plant Hopper Control Sheath Blight (PDI %)
Pymetrozine Thifluzamide 3 DAA 7 DAA 10 DAA 3 DAA 7 DAA 10 DAA
PT1 SC 200 10 93.6 96.8 92.8 8.5 21.9 42.6
PT2 SC 150 75 92.4 95.4 90.4 1.8 2.8 5.0
PT3 SC 125 90 91.2 94.2 89.4 1.2 2.4 3.8
PT4 SC 125 70 91.4 93.8 89.0 1.9 3.2 5.6
PT5 SC 125 50 90.2 94.0 88.2 2.8 4.8 7.5
PT6 SC 100 90 88.2 91.6 85.6 1.4 2.6 3.6
PT7 SC 100 70 88.4 91.0 84.6 1.4 2.5 4.0
PT8 SC 75 150 83.2 84.8 79.2 1.2 2.6 4.8
PT9 SC 10 200 42.6 32.6 20.6 1.8 3.8 6.4
PT10 OD 150 75 93.0 96.0 91.6 1.6 2.6 4.6
PT11 OD 125 75 92.0 95.2 90.2 1.5 3.0 5.1
PT12 OD 125 50 91.6 94.8 89.4 3.4 6.3 9.2
PT13 OD 100 75 89.4 92.8 89.0 1.8 2.5 3.8
PT14 OD 75 150 82.6 85.6 78.2 1.1 2.0 3.2
PT15 WG 150 75 90.2 93.6 88.2 3.2 7.0 9.6
PT16 WG 125 80 88.4 90.6 84.2 3.0 6.8 10.6
PT17 WG 125 70 88.2 89.4 83.6 3.6 7.3 12.4
PT18 WG 100 90 84.2 85.6 80.2 4.2 9.6 16.2
PT19 WG 100 80 83.8 84.8 79.8 4.8 11.6 18.8
PT20 WG 62.5 125 75.6 77.4 70.4 2.2 4.8 9.6
PRS 1 WG 200 _ 84.2 85.8 78.6 22.4 43.9 67.8
PRS 2 SC _ 90 24.6 18.5 10.8 4.6 11.8 20.4
PRS 3 WG+SC 200 90 80.2 79.6 62.4 5.8 10.3 18.6
PRS 4 WG+SC 125 90 72.8 70.6 52.6 6.8 18.7 23.6
PRS 5 WG+SC 125 70 70.4 68.4 47.6 12.6 28.7 41.3
PRS 6 WG+SC 100 90 64.8 62.4 42.8 9.6 23.8 30.5
PRS 7 WG+SC 100 70 65.2 61.6 43.4 15.9 32.8 50.8
Untreated Control _ _ _ 0.0 0.0 0.0 24.8 42.6 72.6

Note: DAA –Days after Application, PDI (%)- Percent Disease Index; PRS(Prior art Sample)

The field experiment results shows high efficacy of novel composition of Pymetrozine and Thifluzamide against Rice Brown Plan Hopper (BPH) and sheath blight disease compared to all the prior art samples and untreated control. The synergistic effect of formulation ratio of Pymetrozine and Thifluzamide varies from 1: 2 to 2: 1, specifically shows very high level of efficacy as well as residual control of both BPH and sheath blight disease. This will help to further reduce the number of applications per crop cycle, good control effect is low in dosage, is safe to the environment and target organism, achieves the one product multi-treatment aim has excellent synergistic effect for controlling rice disease and pests, particularly rice sheath blight and brown plant hopper.
Table 3- Rice Grain Yield
Sample Code Type of Formulation Active Ingredient/Hectare Grain Yield (kg/plot) Estimated Grain Yield (kg/hectare)
Pymetrozine Thifluzamide
PT1 SC 200 10 19.6 4000.0
PT2 SC 150 75 39.8 8122.4
PT3 SC 125 90 40.2 8204.1
PT4 SC 125 70 36.2 7387.8
PT5 SC 125 50 34.4 7020.4
PT6 SC 100 90 33.2 6775.5
PT7 SC 100 70 32.4 6612.2
PT8 SC 75 150 31.6 6449.0
PT9 SC 10 200 29.8 6081.6
PT10 OD 150 75 38.6 7877.6
PT11 OD 125 75 37.4 7632.7
PT12 OD 125 50 34.2 6979.6
PT13 OD 100 75 32.6 6653.1
PT14 OD 75 150 30.8 6285.7
PT15 WG 150 75 35.4 7224.5
PT16 WG 125 80 35.2 7183.7
PT17 WG 125 70 32.0 6530.6
PT18 WG 100 90 31.6 6449.0
PT19 WG 100 80 31.2 6367.3
PT20 WG 62.5 125 32.0 6530.6
PRS 1 WG 200 _ 13.6 2775.5
PRS 2 SC _ 90 16.2 3306.1
PRS 3 WG+SC 200 90 24.6 5020.4
PRS 4 WG+SC 125 90 22.8 4653.1
PRS 5 WG+SC 125 70 20.4 4163.3
PRS 6 WG+SC 100 90 19.6 4000.0
PRS 7 WG+SC 100 70 18.4 3755.1
Untreated Control _ _ _ 10.6 2163.3

The yield data shows Pymetrozine and Thifluzamide has very high level of interaction in terms of pest control as well as grain yield compared to all the prior art samples. All the novel formulations i.e. SC, OD and WDG with the formulation ratio in the range of 1 : 2 to 2 : 1 gives approximately > 30% grain yield increase as compared to all prior art samples.
Table 4- Impact on Spider population and Predatory beetles in Rice crop eco-system

Sample Code Type of Formulation Active Ingredient/Hectare No. of Spider Web per plot No. of Predatory beetles per plot
Pymetrozine Thifluzamide 3 DAA 7 DAA 10 DAA 3 DAA 7 DAA 10 DAA
PT1 SC 200 10 3 6 10 1 4 7
PT2 SC 150 75 4 8 9 3 6 8
PT3 SC 125 90 5 7 11 2 5 8
PT4 SC 125 70 4 6 9 1 4 6
PT5 SC 125 50 3 7 12 2 3 7
PT6 SC 100 90 5 8 10 2 4 7
PT7 SC 100 70 3 8 12 1 3 6
PT8 SC 75 150 4 6 11 2 3 7
PT9 SC 10 200 3 7 12 3 4 8
PT10 OD 150 75 5 6 10 2 3 7
PT11 OD 125 75 4 7 9 1 4 6
PT12 OD 125 50 3 8 10 2 5 7
PT13 OD 100 75 4 8 9 3 4 8
PT14 OD 75 150 5 6 11 2 3 7
PT15 WG 150 75 4 7 9 1 4 6
PT16 WG 125 80 3 8 10 2 4 7
PT17 WG 125 70 4 7 13 3 4 7
PT18 WG 100 90 5 7 12 2 4 6
PT19 WG 100 80 4 8 10 1 5 7
PT20 WG 62.5 125 3 6 11 2 4 6
PRS 1 WG 200 _ 2 3 5 1 3 5
PRS 2 SC _ 90 1 2 4 1 3 4
PRS 3 WG+SC 200 90 1 3 6 0 2 4
PRS 4 WG+SC 125 90 2 4 5 0 1 3
PRS 5 WG+SC 125 70 1 3 4 1 3 4
PRS 6 WG+SC 100 90 2 3 5 0 2 4
PRS 7 WG+SC 100 70 2 4 6 1 3 5
Untreated Control _ _ _ 4 7 11 2 5 8

Spider considered as one of the important bio-agent / predator in rice crop eco-system. Along with spider coccinellids beetles also observed predating on BPH. All the novel formulations SC, OD and WDG of Pymetrozine and Thifluzamide found very safe to the Spider and coccinellids beetles even up to 10 days after application.

Example 2: Experiment against Aphid and Early blight disease in Potato

The efficacy of novel formulations of Pymetrozine and Thifluzamide were also evaluated against Aphid, Myzus persicae and early blight disease, Alternaria solani. Field experiment was carried out in the state of Punjab. The crop was raised with standard agronomic practices.

Design: Random Block Design (RBD)
Plot size: 5 mt x 5 mt
Variety: Kufri Pukhraj

Two consecutive applications were made at 7 days interval. The pest and disease assessment were done at 7 days after second application. The data were recorded by counting the number of aphid per leaf and 10 plants per plot. For early blight disease severity, 100 leaflets from the entire plot were randomly assessed and rated visually by rating scale and Percent Disease Index was calculated.

Rating Scale used for evaluation of soybean rust severity

Rating Description
0 No lesion / spot on leaf
1 1% leaf area covered with early blight
3 1.1-10% leaf area covered with early blight
5 10.1-25% leaf area covered with early blight
7 25.1-50% leaf area covered with early blight
9 More than 50% leaf area covered with early blight

Table: 5 Efficacy of novel formulations of Pymetrozine+Thifluzamide on Potato Aphid and Early blight disease

Type of Formulation Active Ingredient/Hectare 7 Days After 2nd application
Pymetrozine Thifluzamide % Aphid control Early Blight (PDI %)
SC 150 75 98.6 0.6
SC 125 90 96.4 0.4
SC 125 70 96.2 0.5
SC 125 50 97.0 0.7
SC 100 90 94.6 1.5
SC 100 70 92.8 1.6
OD 150 75 97.6 0.4
OD 125 75 95.8 0.6
OD 125 50 94.8 0.5
OD 100 75 93.2 1.6
WG 150 75 97.6 1.1
WG 125 80 95.4 1.2
WG 125 70 94.8 1.3
WG 100 90 91.8 1.8
WG 100 80 92.4 1.9
PRS-WG 200 _ 90.8 12.6
PRS-SC _ 90 24.8 5.8
PRS-WG+SC 200 90 85.6 7.8
PRS-WG+SC 150 75 82.0 9.1
PRS-WG+SC 125 90 80.4 8.6
PRS-WG+SC 100 90 74.8 10.2
PRS-WG+SC 100 70 72.6 12.2
Untreated Check _ _ 0.0 23.8

The pest and disease assessment data shows Pymetrozine and Thifluzamide shows synergistic action on Potato Aphid, Myzus persicae and early blight disease, Alternaria solani. The level of insect control as well as disease control was higher compared to all prior art sample.
Table 6: Safety to beneficial insects in Potato crop eco-system
Type of Formulation Active Ingredient/Hectare No. of Beneficial Insects at 7 days After 2nd Application
Pymetrozine Thifluzamide Coccinellids Syrphid Fly
SC 150 75 6 5
SC 125 90 5 3
SC 125 70 7 4
SC 125 50 5 5
SC 100 90 6 4
SC 100 70 8 6
OD 150 75 5 3
OD 125 75 7 4
OD 125 50 6 5
OD 100 75 8 4
WG 150 75 6 5
WG 125 80 7 4
WG 125 70 6 5
WG 100 90 7 4
WG 100 80 8 6
PRS-WG 200 _ 4 2
PRS-SC _ 90 3 2
PRS-WG+SC 200 90 2 1
PRS-WG+SC 150 75 3 2
PRS-WG+SC 125 90 4 2
PRS-WG+SC 100 90 4 3
PRS-WG+SC 100 70 5 3
Untreated Check _ _ 7 5

All the novel formulations of Pymetrozine and Thifluzamide were found safe to the beneficial insects like Coccinellids beetles and Syrphid fly compared to all prior art samples. This will helps in integrated pest management approach and thereby reducing pesticide load in to the environment.

,CLAIMS:CLAIMS

We claim:

1. A novel composition comprising of Pymetrozine and Thifluzamide in synergistic bioactive amounts and one or more inactive excipients.
2. The novel composition as claimed in claim 1 wherein the ratio of Pymetrozine and Thifluzamide is 20: 1 to 1:20.
3. The novel composition as claimed in claim 1 or 2 wherein the ratio of Pymetorzine and Thifluzamide is preferably 10: 1 to 1: 10, most preferably 1: 2 to 2: 1.
4. The novel composition according to claim 1, wherein inactive excipients can be 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.
5. The novel composition as claimed in claim 1 or 4wherein the formulation can be selected from Suspension Concentrate (SC), Oil Dispersion (OD) and Water dispersible granules (WG).
6. The novel composition as claimed in any of the preceding claims, wherein the said formulation is used for control of insects in rice selected from stem borer (Chilo suppressalis, Diatraea lineolata, Elasmopalpus lignosellus, Scirpophaga incertulas, Sesamia cretica, Sesamia inferens), Planthoppers (Laodelphax striatellus, Nilaparvata lugens, Sogatella furcifera, Tagosodes orizicolus, Nephotettix cincticeps, Nephotettix virescens, Nephotettix nigropictus), Rice gall midge (Orseolia oryzae), Rice leaffolder (Cnaphalocrocis medinalis, Marasmia patnalis, Marasmia bilinealis, Marasmia suspicalis), Rice bug (Leptocorisa acuta, Leptocorisa biguttata, Lepotcorisa chinensis), Stink bug (Oebalus pugnax, Oebalus poecila, Oebalus ypsilon-griseus), Rice hispa (Dicladispa armigera), Rice water weevil (Lissorhoptrus oryzophilus), Rice thrips (Stenchaetothrips biformis, Haplothrips aculeatus), Rice caseworm (Nymphula depunctalis), Rice whorl maggot (Hydrellia philippina), Rice leaf miner (Hydrellia griseola), Rice stem maggot (Hydrellia sasakii), Rice black bug (Scotinophara coarctata, Scotinophara lurida), Common army worm ( Mythimna unipuncta), Rice swarming caterpillar (Spodoptera mauritia acronyctoides), fall armyworm (Spodoptera frugiperda), rice root aphid (Tetraneura nigriabdominalis) and control of insects in potato selected from Potato Aphid, Jassid and Whitefly.

7. The novel composition as claimed in any of the preceding claims, wherein the said formulation is used to control of fungi in rice selected from Sheat spot ( Ceratobasidium oryzae-sativae, Rhizoctonia oryzae-sativae [anamorph]), Black kernel (Curvularia lunata Cochliobolus lunatus [teleomorph], Blast (Pyricularia grisea, Pyricularia oryzae, Magnaporthe grisea[3] [teleomorph]), Brown spot (Cochliobolus miyabeanus Bipolaris oryzae [anamorph]), Crown sheath rot (Gaeumannomyces graminis), Downy mildew (Sclerophthora macrospora), Eyespot (Drechslera gigantean), False smut (Ustilaginoidea virens), Kernel smut (Tilletia barclayana =Neovossia horrid), Leaf smut (Entyloma oryzae), Leaf scald (Microdochium oryzae), Narrow brown leaf spot (Cercospora janseana = Cercospora oryzae, Sphaerulina oryzina [teleomorph]), Pecky rice/Kernel spotting (Cochliobolus miyabeanus, Curvularia spp., Fusarium spp., Microdochium oryzae, Sarocladium oryzae), Root rots (Fusarium spp., Pythiurm spp., Pythium dissotocum, Pythium spinosum), Seedling blight (Cochliobolus miyabeanus, Curvularia spp., Fusarium spp., Rhizoctonia solani, Sclerotium rolfsii), Sheath blight (Thanatephorus cucumeris, Rhizoctonia solani [anamorph]), Sheath rot (Sarocladium oryzae), Sheath spot (Rhizoctonia oryzae), Alternaria padwickii leaf spot and control of fungi in potato selected from Potato Early blight, Tuber rot and Cercospora leaf spot.

8. A novel composition of Pymetrozine and Thifluzamide in synergistic bioactive amounts as claimed in any of the preceding claims and exemplified with working examples as disclosed.