Abstract: ABSTRACT: The present invention contemplates novel formulation of Diafenthiuron and Spirotetramat. The present invention also relates to process for preparing the said formulation comprising Diafenthiuron and Spirotetramat and one or more inactive excipients. The present invention also contemplates use of the formulation comprising Diafenthiuron and Spiorotetramat as crop protectant against insects like Hemiptera, Homoptera, Thysanoptera and phytophagous mites. The list of crops which can be protected by the present invention are Cotton (Gossypium spp.), Rice (Oryza sativa), Wheat (Triticum aestavum), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea) and Rape seed (Brassica napus), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Lentils (Lens culinaris), Okra (Abelmoschus esculentus) , Brinjal (Solanum melongena), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Chilly (Capsicum annum), Cucumber (Cucumis sativus) and Melons (Cucumis melo) Apple (Melus domestica), Mango (Mangifera indica ), Banana (Musa spp.), Grapes (Vitis vinifera), Pomegranate (Punica granatum) , Oranges (Citrus spp.), Tea (Camellia sinensis).
DESC:FIELD OF THE INVENTION:
The present invention contemplates novel formulation of Diafenthiuron and Spirotetramat. The present invention also relates to process for preparing the said formulation comprising Diafenthiuron and Spirotetramat and one or more inactive excipients. The present invention also contemplates use of the formulation comprising Diafenthiuron and Spiorotetramat as crop protectant against Hemiptera, Homoptera, Thysanoptera and phytophagous mites. Hemiptera and Homoptera selected form the group comprising Aphis gossypii, Aphis crassivora, Aphis fabae, Aphis pomi, Acyrthosiphon pisum, Myzus persicae, Lipaphis erysimi, Macrosiphum avenae, Rhopalosiphummaidis, Sitobion avenae, Diaphornia citri, Psylla mali,Nilaparvata lugens, Bemisia tabaci, Emposca spp., Amrasca biguttula biguttula, Maconellicoccus hirsutus, Phenacoccus solenopsis, Aonidiella aurantii; Thysanoptera selected form the group comprising Thrips tabaci, Thrips palmi, Scirtothrips dorsalis, Frankliniella occidentalis; phytophagous mites selected form the group comprising Tetranychidae, Tarsonemidae, Aleyrodidae, Aphididae. .
The list of crops which can be protected by the present invention are Cotton (Gossypium spp.), Rice (Oryza sativa), Wheat (Triticum aestavum), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea) and Rape seed (Brassica napus), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Lentils (Lens culinaris), Okra (Abelmoschus esculentus) , Brinjal (Solanum melongena), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Chilly (Capsicum annum), Cucumber (Cucumis sativus) and Melons (Cucumis melo) Apple (Melus domestica), Mango (Mangifera indica ), Banana (Musa spp.), Grapes (Vitis vinifera), Pomegranate (Punica granatum) , Oranges (Citrus spp.), Tea (Camellia sinensis)..
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 Bacillus thuringiensis biocidal 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 nonpersistent 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 Ryania speciosa (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.
Diafenthiuron was first disclosed in GB2060626. Diafenthiuron, chemically known as 1-tert-butyl-3-(2,6-di-isopropyl-4-phenoxyphenyl)thiourea or N-[2,6-bis(1-methylethyl)-4-phenoxyphenyl]-N'-(1,1-dimethylethyl)thiourea and having chemical structure as below;
Diafenthiuron acts after conversion by either light, or in vivo, to the corresponding carbodiimide, which is an inhibitor of mitochondrial respiration. Mode of action as insecticide and acaricide which kills larvae, nymphs and adults is by contact and/or stomach action; also shows some ovicidal action. It is commonly used as insecticide and acaricide effective against phytophagous mites (tetranychidae, tarsonemidae), aleyrodidae, aphididae and jassidae on cotton, various field and fruit crops, ornamentals and vegetables. Also controls some leaf-feeding pests in cole crops (Plutella xylostella), soya beans (Anticarsia gemmatalis) and cotton (Alabama argillacea).
Spirotetramat was first disclosed in US6114374. Spirotetramat is chemically known as cis-4-(ethoxycarbonyloxy)-8-methoxy-3- (2,5-xylyl)-1-azaspiro[4.5] dec-3-en-2-one and having chemical structure as below;
Spirotetramat belongs to the chemical class of KETON OLS, subclass tetramic acid derivatives, intended for use as an insecticide on a range of agricultural crops. The pesticidal mechanism of action is disruption of lipogenesis as a result of inhibition of acetyl CoA carboxylase.
Spirotetramat is taken up by the plant and then carried around the plant, including into roots and newly-forming shoots, giving sucking insect pest like aphids and whitefly an unpleasant surprise. The compounds work by inhibiting lipid biosysnthesis, affecting reproduction in adults and especially juveniles.
Spirotetramat inhibits lipogenesis in treated insects, resulting in decreased lipid contents, growth inhibition of younger insects, and reduction in ability of adult insects to reproduce.
Spirotetramat is active against aphids, whiteflies, scales, mealybugs, psylla, phylloxera, thrips, and mites.
The main concern with the use of insecticide is the development of resistance by the insects for that particular insecticide and at the end one has to apply more concentrated formulation of the insecticide. The high amount of insecticide 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 insecticide, use of nontoxic ingredients and developing novel formulations which provides effective amount of the insecticide and at the required part only.
However the use of poly mixture containing large number of insecticide poses a problem in many was like preparing formulation of multiple insecticides with different chemical properties and behavior and physical properties. It also creates challenge for the formulator in term of compatibility and stability of all the insecticides along with the used excipients in the formulation.
WO2012101659 discloses a pesticidal composition comprising an effective amount of a sulphur; an effective amount of at least one insecticide selected from the group consisting of cartap, pirimicarb, buprofezine, thiachloprid, acetamiprid, clothianidin, Diafenthiuron, novaluron, flubendiamide, spirotetramat, thiamethoxam, imidacloprid, abamectin, lambda-cyhalothrin or salts thereof, and at least one agrochemically acceptable excipient.
Indian patent application 753/MUM/2012, discloses a composition comprising an effective amount of lambda cyhalothrin in the range of 0.5% to 12%; an effective amount of Diafenthiuron in the range of 15% to 70% wherein the ratio of lambda cyhalothrin to Diafenthiuron is in the range of 1:4 to 1:35; and at least one agrochemical excipient.
WO 2010/020477 describes insecticidal compositions comprising Diafenthiuron and a crop safener, and to the use of such compositions in controlling insects in crops of useful plants. The invention further extends to combination packages of Diafenthiuron and crop safener.
US 6,485,736 discloses microcapsules and to a process for their production. More particularly, this invention relates to encapsulated droplets of a liquid material which is substantially insoluble in water, wherein the encapsulating agent is a shell wall containing disulfide units, thereby forming an environmentally sensitive, variable release wall. Further, this invention relates to the processes for the production of such microcapsules and methods for their use.
US 8,652,997 describes an active compound combinations, in particular a fungicidal and/or insecticidal composition, comprising Isotianil (3,4-dichloro-N-(2-cyanophenyl)-5-isothiazolecarboxamide, CAS No 224049-04-1) and at least one further insecticide of the group of cyclic ketoenols (including Spirotetramat) and optionally one further insecticide of the neonicotinoids.
US 20130345052 describes an agricultural composition comprising at least one insecticidal active ingredient selected from cartap, fipronil, pirimicarb, buprofezine, thiachloprid, acetamiprid, clothianidin, chloropyrifos, diafenthiuron, novaluron, flubendiamide, Spirotetramat, thiamethoxam, imidacloprid or salts thereof in the range of 0.1% to 10% of the total composition, elemental sulphur in the range of 30% to 90% of the total composition, zinc in the range of 2% to 20% of the total composition; and at least one agrochemically acceptable excipient.
CN 101755816 discloses an insecticidal composition. The active ingredients of the composition comprise spirotetramat and bifenthrin in a mass ratio of 40:1 to 1:80. The compounding of spirotetramat and the bifenthrin produces an obvious synergistic effect and can reduce the dosage of the active ingredients and medicament application times and delay the generation of pesticide resistance of pests.
CN 102484995 discloses an insecticidal composition and a preparation thereof. The insecticidal composition comprises spirotetramat and one ingredient selected from nitenpyram, chlopyrifos, acetamiprid or imidacloprid.
WO2011138968 discloses a method for controlling planthoppers, which comprises a step of directly applying an effective amount of spirotetramat to a rice paddy in which a rice plant is growing.
However still there is a need for a formulation of specific insecticides 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 formulation of Diafenthiuron and Spirotetramat as described herein can provide solution to the above problems by showing synergistic effect.
SUMMARY OF THE INVENTION
The present invention relates to a novel insecticidal formulation which comprises of Diafenthiuron and Spirotetramat.
The present invention also relates to a novel formulation of Diafenthiuron and Spirotetramat which shows synergistic effect.
Further the present invention also relates to process for preparing the novel formulation comprising Diafenthiuron and Spirotetramat.
The present invention also contemplates use of the formulation comprising Diafenthiuron and Spiorotetramat as crop protectant against Hemiptera, Homoptera, Thysanoptera and phytophagous mites. Wherein Hemiptera and Homoptera comprises Aphis gossypii, Aphis crassivora, Aphis fabae, Aphis pomi, Acyrthosiphon pisum, Myzus persicae, Lipaphis erysimi, Macrosiphum avenae, Rhopalosiphummaidis, Sitobion avenae, Diaphornia citri, Psylla mali,Nilaparvata lugens, Bemisia tabaci, Emposca spp., Amrasca biguttula biguttula, Maconellicoccus hirsutus, Phenacoccus solenopsis, Aonidiella aurantii; Thysanoptera comprises Thrips tabaci, Thrips palmi, Scirtothrips dorsalis, Frankliniella occidentalis; phytophagous mites comprises Tetranychidae, Tarsonemidae, Aleyrodidae, Aphididae..
The list of crops which can be protected by the present invention are Cotton (Gossypium spp.), Rice (Oryza sativa), Wheat (Triticum aestavum), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea) and Rape seed (Brassica napus), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Lentils (Lens culinaris), Okra (Abelmoschus esculentus) , Brinjal (Solanum melongena), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Chilly (Capsicum annum), Cucumber (Cucumis sativus) and Melons (Cucumis melo) Apple (Melus domestica), Mango (Mangifera indica ), Banana (Musa spp.), Grapes (Vitis vinifera), Pomegranate (Punica granatum) , Oranges (Citrus spp.), Tea (Camellia sinensis).
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides formulation comprising Diafenthiuron and Spirotetramat with one or more inactive excipients.
The term “pesticide” or “pesticidal” is similar to “insecticide” or “insecticidal” and used interchangeably in this whole specification.
The pesticidal or insecticidal formulation 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.
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.
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.
Formulation of the present invention can be in any of the form described above.
Diafenthiuron and Spirotetramat which is active ingredient for the present formulation are present in ratio of 15:1 to 1:15.
The formulation of the present invention in addition to Diafenthiuron and Spirotetramat 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 formulations to facilitate dispersion and suspension during manufacture, and to ensure the particles re-disperse into water in a spray tank. They are widely used in wettable powders, suspension concentrates and water-dispersible granules. Surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier to re-aggregation of particles. The most commonly used surfactants are anionic, non-ionic, or mixtures of the two types. For wettable powder formulations, the most common dispersants are sodium lignosulphonates. For suspension concentrates, very good adsorption and stabilization are obtained using polyelectrolytes, such as sodium naphthalene sulphonate formaldehyde condensates. Tristyrylphenol ethoxylate phosphate esters are also used. Non-ionics such as alkylarylethylene oxide condensates and EO-PO block copolymers are sometimes combined with anionics as dispersants for suspension concentrates. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. These have very long hydrophobic ‘backbones’ and a large number of ethylene oxide chains forming the ‘teeth’ of a ‘comb’ surfactant. These high molecular weight polymers can give very good long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces. Examples of dispersants used herein include but not limited to sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate 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 comprising of polyethylene glycols, methoxypolyethylene glycols, polypropylene glycols, polybutylene glycols, glycerin and ethylene glycol or mixtures thereof.
Water-based formulations often cause foam during mixing operations in production. In order to reduce the tendency to foam, anti-foam agents are often added either during the production stage or before filling into bottles. Generally, there are two types of anti-foam agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.
A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading. Wetting agents are used for two main functions in agrochemical formulations: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules. Examples of wetting agents used in wettable powder, suspension concentrate, and water-dispersible granule formulations include but not limited to sodium lauryl sulphate; sodium dioctyl sulphosuccinate; alkyl phenol ethoxylates; and aliphatic alcohol ethoxylates or mixtures thereof.
Suspension aid in the present description denotes a natural or synthetic, organic or inorganic material with which the active substance is combined in order to facilitate its application to the plant, to the seeds or to the soil. This carrier is hence generally inert, and it must be agriculturally acceptable, in particular to the plant being treated. The carrier may be solid (clays, natural or synthetic silicates, silica, resins, waxes, solid fertilizers, and the like or mixtures thereof) or liquid (water, alcohols, ketones, petroleum fractions, aromatic or paraffinic hydrocarbons, chlorinated hydrocarbons, liquefied gases, and the like or mixtures thereof).
Biocides / Microorganisms cause spoilage of formulated products. Therefore anti-microbial agents are used to eliminate or reduce their effect. Examples of such agents include, but are not limited to: propionic acid and its sodium salt; sorbic acid and its sodium or potassium salts; benzoic acid and its sodium salt; p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates or mixtures thereof.
Thickeners or gelling agents are used mainly in the formulation of suspension concentrates, emulsions and suspoemulsions to modify the rheology or flow properties of the liquid and to prevent separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixtures thereof.
The quick coating agent can be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, polsaccharides such as starch and cellulose derivatives, vinylal- cohol, vinylacetate and vinylpyrrolidone polymers and copolymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymers and mixtures thereof. Examples of preferred polymers are acrylate polymers such as poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below , poly(styrene-co maleic anhydride), cellulosic polymers such as ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono-, di-, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), alkyd resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present method include biodegradable polyesters, starch, polylactic acid -starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch ester aliphatic polyester blends, modified corn starch, polycaprolactone, poly(n-amylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyrate valerate, 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, magnesium hydroxide or mixtures thereof.
The solvent for the formulation of the present invention may include water, water-soluble alcohols and dihydroxy alcohol ethers. The water-soluble alcohol which can be used in the present invention may be lower alcohols or water-soluble macromolecular alcohols. The term "lower alcohol", as used herein, represents an alcohol having 1-4 carbon atoms, such as methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol, etc. Macromolecular alcohol is not limited, as long as it may be dissolved in water in a suitable amount range, e.g., polyethylene glycol, sorbitol, glucitol, etc. The examples of suitable dihydroxy alcohol ethers used in the present invention may be dihydroxy alcohol alkyl ethers or dihydroxy alcohol aryl ethers. The examples of dihydroxy alcohol alkyl ether include ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, dipropylene glycol ethyl ether, etc. The examples of dihydroxy alcohol aryl ethers include ethylene glycol phenyl ether, diethylene glycol phenyl ether, propylene glycol phenyl ether, dipropylene glycol phenyl ether, and the like. Any of the above mentioned solvent can be used either alone or in combination thereof.
WDG formulations 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 formulations 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 formulation 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 Diafenthiuron and Spirotetramat 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 stirring for about 4 hr to obtain homogeneous formulation.
The process for preparing the present novel formulation can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the formulation. However all such variation and modification is still covered by the scope of present invention.
ZC formulation can be prepared by a) preparing SC formulation of one ingredient. B) Preparing CS formulation of another ingredient and finally mixing SC and CS formulation with stirring to obtain the final ZC formulation.
The list of insects which can be controlled by the present formulations are Hemiptera, Homoptera, Thysanoptera and phytophagous mites. Wherein Hemiptera and Homoptera comprises Aphis gossypii, Aphis crassivora, Aphis fabae, Aphis pomi, Acyrthosiphon pisum, Myzus persicae, Lipaphis erysimi, Macrosiphum avenae, Rhopalosiphummaidis, Sitobion avenae, Diaphornia citri, Psylla mali,Nilaparvata lugens, Bemisia tabaci, Emposca spp., Amrasca biguttula biguttula, Maconellicoccus hirsutus, Phenacoccus solenopsis, Aonidiella aurantii; Thysanoptera comprises Thrips tabaci, Thrips palmi, Scirtothrips dorsalis, Frankliniella occidentalis; phytophagous mites comprises Tetranychidae, Tarsonemidae, Aleyrodidae, Aphididae.
The list of crops which can be protected by the present invention are Cotton (Gossypium spp.), Rice (Oryza sativa), Wheat (Triticum aestavum), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea) and Rape seed (Brassica napus), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Lentils (Lens culinaris), Okra (Abelmoschus esculentus) , Brinjal (Solanum melongena), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Chilly (Capsicum annum), Cucumber (Cucumis sativus) and Melons (Cucumis melo) Apple (Melus domestica), Mango (Mangifera indica ), Banana (Musa spp.), Grapes (Vitis vinifera), Pomegranate (Punica granatum) , Oranges (Citrus spp.), Tea (Camellia sinensis).
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.
EXAMPLES
Example 1
Oil Dispersion
COMPOSITIONS DIAFENTHIURON 30% + SPIROTETRAMAT 2% OD DIAFENTHIURON 25% + SPIROTETRAMAT 3% OD DIAFENTHIURON 20% + SPIROTETRAMAT 4% OD DIAFENTHIURON 17.5% + SPIROTETRAMAT 7% OD DIAFENTHIURON 1% + SPIROTETRAMAT 15% OD
Diafenthiuron (96%) 31.25 26.04 20.80 18.23 1.04
Spirotetramat (95%) 2.11 3.16 4.21 7.37 15.79
Ethoxylated Oleyl-Cetyl Alcohol 3.00 3.00 3.00 3.00 3.00
Polyalkylene glycol ether 1.50 1.50 1.50 1.50 1.50
Polyvinylpyrrolidone 1.00 1.00 1.00 1.00 1.00
Calcium alkyl benzene sulfonate 3.50 3.50 3.50 3.50 3.50
Castor oil ethoxylates 2.50 2.50 2.50 2.50 2.50
Silicon based antifoam 0.50 0.50 0.50 0.50 0.50
Soyabean oil 54.64 58.80 62.99 62.40 71.17
TOTAL 100.00 100.00 100.00 100.00 100.00
Procedure:
Step 1 Charge required quantity of vegetable oil in vessel and add polyvinyl pyrrollidone, mix well for 30 minutes using high shear homogenizer and pass through horizontal bead mill.
Step 2 Add required quantity of Wetting agent, dispersing agent & suspending agents and homogenise 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 2
Suspo Emulsion
COMPOSITION DIAFENTHIURON 25% + SPIROTETRAMAT 4% SE DIAFENTHIURON 20% + SPIROTETRAMAT 5% SE
Diafenthiuron (96%) 26.04 20.83
Spirotetramat (95%) 4.21 5.26
Acrylic graft copolymer 3.00 3.00
Polyalkoxy alkyl ethers 1.50 1.50
Glycol 5.00 5.00
1,2-Benzisothiazolin-3-one 0.10 0.10
Polysaccharide 0.13 0.13
Silicon based antifoam 1.00 1.00
PPt silica 1.00 1.00
DM water 58.02 62.18
TOTAL 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 Oil phase is made by mixing required quantity of oil soluble emulsifier in required quantity of oil/ solvent, still till all raw materials homogenize and then add active component/ technical to it. Make a homogeneous solution by stirring under high shear for 45 to 60 minutes.
Step 3 Simultaneously make aqueous phase by mixing surfactants, antifreeze, antifoam, filler/ suspending agent, & colorant/ dye in water. Once homogenize add technical (water insoluble) to this solution and form a slurry using high shear homogenizer for 60 minutes.
Step 4 Once both phases are ready add Oil phase to aqueous phase slowly under high shear homogenization.
Step 5 After complete addition stir the mixture for 60 more minutes under high shear stirring.
Step 6 Pass homogenized material from above step to Bead mill/ Dyno mill for 2-3 cycles and provide sample to QC lab.
Step 7 Upon approval for particle form lab, gum solution was added and final sample is provided to QC for approval.
Example 3
Water Dispersible Granules
COMPOSITION DIAFENTHIURON 60% + SPIROTETRAMAT 4% WG DIAFENTHIURON 50% + SPIROTETRAMAT 8% WG DIAFENTHIURON 40% + SPIROTETRAMAT 10% WG DIAFENTHIURON 2% + SPIROTETRAMAT 30% WG
Diafenthiuron (96%) 62.50 52.08 41.66 2.08
Spirotetramat (95%) 4.21 8.42 10.53 31.58
Sodium salt of Phenol sulphonic acid condensate 2.00 2.00 2.00 2.00
Styrine acrylic polymer 4.00 4.00 4.00 4.00
Sodium alkylnaphthalene sulfonate, formaldehyde condensate 5.00 5.00 5.00 5.00
Silicone based antifoam 1.00 1.00 1.00 1.00
Colorant/Dye 3.00 3.00 3.00 3.00
PPT silica 6.00 6.00 6.00 6.00
Starch 4.00 4.00 4.00 4.00
China clay 7.0 7.0 7.0 7.0
Lactose 1.29 7.50 15.81 34.34
TOTAL 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 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 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
Wettable Powders
COMPOSITION DIAFENTHIURON 40% + SPIROTETRAMAT 8% WP DIAFENTHIURON
30% + SPIROTETRAMAT 10% WP
Diafenthiuron (96%) 41.66 31.25
Spirotetramat (95%) 8.42 10.52
Sodium salt of Phenol sulphonic acid condensate 2.00 2.00
Styrine acrylic polymer 4.00 4.00
Sodium ligno sulphonate 2.00 2.00
Polyvinyl pyrollidone 1.50 1.50
PPT silica 17.00 17.00
Kaolin 23.42 31.73
TOTAL 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 analysed. After getting approval from QC dept. material is unloaded into 25 kg. HDPE bag with LDPE liner inside.
Example 5
Stability Studies
a) Oil Dispersion (DIAFENTHIURON 20% + SPIROTETRAMAT 4%)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days Room Temperature
Parameters In House 1st day 15th day 15th day 12 months 36 months
Description Off white Complies Complies Complies Complies Complies
Spirotetramat Content 3.8 - 4.4 4.2 4.1 4.2 4.15 4
Spirotetramat Suspensibility 70% minimum 96.1 96 92.5 96.1 93
Diafenthiuron Content 19.0-21.0 20.5 20.4 20.5 20.45 20
Diafenthiuron Suspensibility 80 % minimum 97.2 97 97.1 97.2 97
pH 6.0 – 7.5 7 7.1 7.1 7 7.1
Particle size D50 <3, D90 <10 2.8 8.1 2.8 8.1 2.8 8.1 2.8 8.1 2.8 8.1
Pourability 95 % min 97 97 96.8 97 97
Specific gravity 1.02 – 1.09 1.05 1.05 1.05 1.05 1.05
Viscosity 350 -900 cps 500 510 520 500 510
From the above it is evident that the oil dispersion formulation comprising of Diafenthiuron and Spirotetramat is stable.
b) Supso emulsion (Diafenthiuron 20% + Spirotetramat 5%)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days Room Temperature
Parameters In House 1st day 15th day 15th day 12 months 36 months
Description Off-white Complies Complies Complies Complies Complies
Diafenthiuron Content 19.0-21.0 20.5 20.3 20.5 20.45 20.1
Diafenthiuron Suspensibility 70% minimum 96.1 96 96.1 96.1 96
Spirotetramat Content 4.5-6.0 5.3 5.2 5.3 5.28 5.1
Spirotetramat Suspensibility 80 % minimum 97.2 97.2 97.2 97.2 97.2
pH 6.0 – 7.5 7 7 7 7 7
Particle size D50 <3, D90 <10 2.8 8.1 2.8 8.1 2.8 8.1 2.8 8.1 2.8 8.1
Pourability 95 % min 97 97 97 97 97
Specific gravity 1.02 – 1.09 1.05 1.05 1.05 1.05 1.05
Viscosity 350 -900 cps 500 500 500 500 500
From the above it is evident that the suspo emulsion formulation comprising of Diafenthiuron and Spirotetramat is stable.
c) Water Dispersible Granules (Diafenthiuron 50% + Spirotetramat 8%)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Room Temperature
Parameters In House 1st day 15th day 12 months 36 months
Description off-white to brownish granules Complies Complies Complies Complies
Diafenthiuron Content 47.5-52.5 50.8 50.4 50.6 50.2
Diafenthiuron Suspensibility 70% minimum 96.5 96.5 96.5 96.5
Spirotetramat Content 6.4-8.8 8.5 8.3 8.49 8.1
Spirotetramat Suspensibility 80 % minimum 97 97 97 97
pH 6.0-7.5 7.5 7.5 7.5 7.5
Wet-sieve(45 micron sieve) Mini 99.5% 99.7 99.7 99.7 99.7
Bulk density 0.35 -0.45 0.4 0.4 0.4 0.4
Wettability 60 Sec Max 15 15 15 15
From the above it is evident that the water dispersible granules formulation comprising of Diafenthiuron and Spirotetramat is stable.
d) Wettable Powders (Diafenthiuron 30% + Spirotetramat 10%)
Specification Initial Heat stability study at 54 + 2 0C for 14 days Room Temperature
Parameters In House 1st day 15th day 12 months 36 months
Description off-white to light brown powder Complies Complies Complies Complies
Diafenthiuron Content 28.5-31.5 30.9 30.5 30.85 30.25
Diafenthiuron Suspensibility 70% minimum 96.5 96.5 96.5 96.5
Spirotetramat Content 9.5-10.5 10.8 10.5 10.72 10.3
Spirotetramat Suspensibility 80 % minimum 97 97 97 97
pH 6.0-7.5 7.5 7.5 7.5 7.5
Wet-sieve(45 micron sieve) Mini 99.5% 99.7 99.7 99.7 99.7
Bulk density 0.35 -0.45 0.4 0.4 0.4 0.4
Wettability 60 Sec Max 20 20 20 20
From the above it is evident that the wettable powders formulation comprising of Diafenthiuron and Spirotetramat is stable.
Example 6
Field Efficacy Trial
The present formulations are also evaluated for their efficacy trials and the details of results are provided below in the examples.
The present study relates to the active ingredient formulations comprising Diafenthiuron and Spirotetramt. One typical problem arising in the field of harmful insect control lies in the need to reduce the dose rate of active ingredient in order to reduce or avoid unfavorable environment or toxicological effects whilst still allowing effective harmful insect-pest control.
Various formulations of Diafenthiuron and Spirotetramat with different active ingredient ratio were developed in-house. These samples were evaluated for their-
1. Efficacy, to find out optimum use rate of both active ingredient to ensure highest efficacy with minimal impact on environment
2. To find out the spectrum of activity (to control more than one harmful insects at a time)
3. Safety to beneficial insects in crop ecosystem
4. Resistance management
Table 1: Sample compositions comprising of Diafenthiuron and Spirotetramat, their formulations and use rate
Sample Code Type of Formulation A.I.(%) in formulation Formulation per Hectare (g or ml) Active Ingredient/Hectare Ratio of Diafenthiuron : Spirotetramat
Diafenthiuron Spirotetramat Diafenthiuron Spirotetramat
DS1 OD 30.0% 2.0% 1000 300 20 15 : 1
DS2 OD 25.0% 3.0% 1000 250 30 8.33 : 1
DS3 OD 20.0% 4.0% 1000 200 40 5 : 1
DS4 OD 17.5% 7.0% 1000 175 70 2.5 : 1
DS5 OD 1.0% 15.0% 1000 10 150 1 : 15
DS6 SE 25.0% 4.0% 1000 250 40 6.25 : 1
DS7 SE 20.0% 5.0% 1000 200 50 4 : 1
DS8 WG 60.0% 4.0% 500 300 20 15 : 1
DS9 WG 50.0% 8.0% 500 250 40 6.25 : 1
DS10 WG 40.0% 10.0% 500 200 50 4 : 1
DS11 WG 2.0% 30.0% 500 10 150 1 : 15
DS12 WP 40.0% 8.0% 500 200 40 5 : 1
DS13 WP 30.0% 10.0% 500 150 50 3 : 1
DFN14 WP 50% 600 300
SPT OD 15% 500 75
Tank mix WP+OD 50% 15% 600+500 300 75
Untreated Check _ _
Observations:
Brinjal (Solanum melongena) is an important vegetable crop cultivated in many countries. It attacked by a number of insects pests from vegetative to harvesting stage. Among the important key pests of Brinjal, the sucking pests viz., leafhopper, Amrasca biguttula biguttula (Ishida), aphid, Aphis gossypii (Glover), whitefly Bemisia tabaci (Gennadius) and thrips, Thrips tabaci (Linnman) cause severe damage and serious threat to the crop growth and yield. These sucking pests also responsible for wide spread infection of MLO (Mycoplasma like Organism) which causes little leaf disease in Brinjal. Therefore chemical control is necessary to keep the population of sucking pests below ETL. In the present study some novel formulations of insecticides have been used to test their efficacy against the sucking pests.
The field trial was conducted to evaluate the efficacy of various formulations of premixes of Diafenthiuron and Spirotetramat. Trial was conducted with R.B.D design with 5 m X 5 m net plot size. Brinjal was raised with all standard agronomic practices. Spraying was done with manual operated back pack sprayer with 750 liter of water spray volume. The observations was recorded by counting the no. of sucking insects (whitefly, jassid and thrips) per leaf, three leaves per plant and five plants per plot. The observations were recorded at before spraying, 7 and 14 days after spraying. The field observations were presented in below table. The observations on beneficial insects i.e. Coccinella spp. and Chrysopa spp. were also recorded along with harmful insects to assess the harmful impact of all formulations on beneficial insects. The efficacy of various treatments were also judged by little leaf disease incidence and harvest of marketable fruit yield.
Table 2- Efficacy of various formulations of Diafenthiuron and Spirotetramat mixtures against sucking pests of Brinjal Crop
Sample Code Type of Formulation Active Ingredient/Hectare Number of Insects per leaf
Diafenthiuron Spirotetramat Whitefly, Bemisia tabaci Jassid, Amrasca biguttula biguttula Thrips, Thrips tabaci
1 DBT 7 DAT 14 DAT 1 DBT 7 DAT 14 DAT 1 DBT 7 DAT 14 DAT
DS1 OD* 300 20 22 4 6 16 3 8 8 3 7
DS2 OD 250 30 19 3 5 14 2 4 7 2 5
DS3 OD 200 40 25 2 4 18 2 3 11 1 4
DS4 OD 175 70 23 1 2 15 1 3 9 2 7
DS5 OD 10 150 17 2 2 16 1 6 10 3 8
DS6 SE** 250 40 20 2 4 14 3 5 8 3 5
DS7 SE 200 50 27 2 2 17 1 4 9 1 4
DS8 WG# 300 20 21 1 4 15 1 7 7 2 5
DS9 WG 250 40 24 1 3 18 2 3 11 1 2
DS10 WG 200 50 18 3 6 13 3 5 10 1 4
DS11 WG 10 150 24 2 5 16 2 7 9 4 5
DS12 WP## 200 40 26 0 2 17 1 3 13 3 4
DS13 WP 150 50 23 1 2 15 2 3 12 3 4
DFN14 WP 300 -- 25 15 34 15 12 30 8 7 20
SPT OD -- 75 23 16 40 14 14 34 10 6 18
Tank mix WP+OD 300 75 28 14 29 17 10 26 8 5 17
Untreated Check 25 38 55 16 24 47 12 20 33
Note: DBT –Days Before Treatment, DAT –Days After Treatment, OD* –Oil Dispersion, SE** -Suspo Emulsion, WG# -Wettable Granule, WP## Wettable Powder,
Observations:
All the ready mix formulation of Diafenthiuron and Spirotetramat were found to be highly effective against sucking insects pests like whitefly, Jassid and Thrips in Brinjal cropp, as compared to their individual use as well as their onsite tank mixer. The formulation ratio of Diafenthiuron and Spirotetramat i.e. 8.33:1 to 3:1 provides excellent efficacy with longer residual control which will be helpful in reducing the no. of spray and thereby reducing the load of active ingredient in the environment.
Table 3- Effect of insecticidal treatments on beneficial insects
Sample Code Type of Formulation Active Ingredient/Hectare Beneficial Insects Population before and after sprays
Diafenthiuron Spirotetramat Coccinella spp. Chrysopera spp.
1 DBT 7 DAT 14 DAT 1 DBT 7 DAT 14 DAT
DS1 OD 300 20 2 6 8 7 7 14
DS2 OD 250 30 4 5 7 6 8 13
DS3 OD 200 40 3 4 8 5 9 12
DS4 OD 175 70 2 5 7 6 8 13
DS5 OD 10 150 4 6 9 7 7 12
DS6 SE 250 40 3 5 7 6 8 14
DS7 SE 200 50 2 4 8 5 9 12
DS8 WG 300 20 3 5 9 8 8 13
DS9 WG 250 40 4 6 8 7 7 12
DS10 WG 200 50 4 5 7 6 8 13
DS11 WG 10 150 3 5 8 5 9 14
DS12 WP 200 40 2 6 9 6 8 13
DS13 WP 150 50 3 5 8 7 7 12
DFN14 WP 300 4 4 3 8 7 6
SPT OD 75 3 4 4 5 6 5
Tank mix WP+OD 300 75 4 3 3 6 5 6
Untreated Check 3 6 8 7 9 13
Note: DBT –Days Before Treatment, DAT –Days After Treatment, OD* –Oil Dispersion, SE** -Suspo Emulsion, WG# -Wettable Granule, WP## Wettable Powder
The field observation on beneficial insects suggests all ready mix formulations of Diafenthiuron and Spirotetramat, i.e. OD, SE, WG and WP formulations are found highly safer for both species of beneficial insects i.e. Coccinella spp. and Chyrsopa spp. The commercially available formulations of Diafenthiuron i.e. WP and Spirotetramat i.e. OD and their onsite tank mixing found toxic to the both beneficial insects species. This is very important for resistance management point of view and also to harness the benefits of nature in pest management.
Table 4- Effect of insecticidal treatments on little leaf disease incidence and fruit yield of brinjal
Sample Code Type of Formulation Active Ingredient/Hectare %Little Leaf incidence Fruit Yield (kg/plot)
Diafenthiuron Spirotetramat
DS1 OD 300 20 5% 31
DS2 OD 250 30 3% 34
DS3 OD 200 40 2% 36
DS4 OD 175 70 3% 33
DS5 OD 10 150 6% 30
DS6 SE 250 40 2% 32
DS7 SE 200 50 1% 36
DS8 WG 300 20 6% 30
DS9 WG 250 40 2% 34
DS10 WG 200 50 2% 35
DS11 WG 10 150 5% 29
DS12 WP 200 40 2% 33
DS13 WP 150 50 3% 28
DFN14 WP 300 15% 22
SPT OD 75 14% 21
Tank mix WP+OD 300 75 11% 24
Untreated Check 24% 15
The efficacy trial data indicates that the incidence of little leaf disease were lower in all the novel formulations of Diafenthiuron and Spirotetramat, i.e. OD, SE, WG and WP as compared to the commercially available formulations of Diafenthiuron i.e. WP and Spirotetramat i.e. OD and their onsite tank mixing. Not only that the marketable fruit yield of brinjal were also harvested more in the treatments of various formulations of Diafenthiuron and Spirotetramat as compared to their solo commercial formulation as well as their onsite mixture.
,CLAIMS:We claim:
1. A novel formulation comprising of Diafenthiuron and Spirotetramat and one or more inactive excipients.
2. A novel formulation as claimed in claim 1 wherein the ratio of Diafenthiuron and Spirotetramat is in the range of 15:1 to 1:15.
3. A novel formulation according to claim 1, wherein inactive excipients selected from the group comprising 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.
4. A novel formulation as claimed in claim 1 or 2 wherein the formulation may be in the form of oil dispersion, water dispersible granules, suspension concentrate and wettable powders.
5. A novel formulation as claimed in claim 4, wherein the amount of the Diafenthiuron and Spirotetramat thereof applied is from 0.1 g/ha to 2000 g/ha.
6. A novel formulation as claimed in any of the preceding claims wherein the said formulation controls Hemiptera, Homoptera, Thysanoptera and phytophagous mites.
7. A novel formulation as claimed in claim 6 wherein the said formulation controls Hemiptera and Homoptera selected form the group comprising Aphis gossypii, Aphis crassivora, Aphis fabae, Aphis pomi, Acyrthosiphon pisum, Myzus persicae, Lipaphis erysimi, Macrosiphum avenae, Rhopalosiphummaidis, Sitobion avenae, Diaphornia citri, Psylla mali,Nilaparvata lugens, Bemisia tabaci, Emposca spp., Amrasca biguttula biguttula, Maconellicoccus hirsutus, Phenacoccus solenopsis, Aonidiella aurantii.
8. A novel formulation as claimed in claim 6 wherein the said formulation controls Thysanoptera selected form the group comprising Thrips tabaci, Thrips palmi, Scirtothrips dorsalis, Frankliniella occidentalis.
9. A novel formulation claimed in claim 6 wherein the said formulation controls phytophagous mites selected form the group comprising Tetranychidae, Tarsonemidae, Aleyrodidae, Aphididae.
10. A novel formulation as claimed in any of the preceding claims wherein the said formulation protects crops selected form the group comprising Cotton (Gossypium spp.), Rice (Oryza sativa), Wheat (Triticum aestavum), Maize (Zea mays), Sorghum (Sorghum bicolor), Sugarcane (Saccharum officinarum) , Soybean (Glycin max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea) and Rape seed (Brassica napus), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Lentils (Lens culinaris), Okra (Abelmoschus esculentus) , Brinjal (Solanum melongena), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Chilly (Capsicum annum), Cucumber (Cucumis sativus) and Melons (Cucumis melo) Apple (Melus domestica), Mango (Mangifera indica ), Banana (Musa spp.), Grapes (Vitis vinifera), Pomegranate (Punica granatum) , Oranges (Citrus spp.), Tea (Camellia sinensis).
11. A novel formulation of Diafenthiuron and Spirotetramat as claimed in any of the preceding claims and exemplified with working examples.
| Section | Controller | Decision Date |
|---|---|---|
| 15 | RESMI C SENAN | 2023-12-30 |
| 25(1) | RESMI C SENAN | 2023-12-30 |
| # | Name | Date |
|---|---|---|
| 1 | 4104-MUM-2014-Response to office action [18-09-2023(online)].pdf | 2023-09-18 |
| 1 | Description(Complete) [18-08-2015(online)].pdf | 2015-08-18 |
| 2 | 4104-MUM-2014-AMMENDED DOCUMENTS [19-08-2023(online)].pdf | 2023-08-19 |
| 2 | Assignment [18-08-2015(online)].pdf | 2015-08-18 |
| 3 | Form 18 [01-07-2016(online)].pdf | 2016-07-01 |
| 3 | 4104-MUM-2014-FORM 13 [19-08-2023(online)].pdf | 2023-08-19 |
| 4 | 4104-MUM-2014-MARKED COPIES OF AMENDEMENTS [19-08-2023(online)].pdf | 2023-08-19 |
| 4 | 4104-MUM-2014-FORM-26 [03-04-2018(online)].pdf | 2018-04-03 |
| 5 | Form-26-GPA-GSP.pdf | 2018-08-11 |
| 5 | 4104-MUM-2014-Written submissions and relevant documents [19-08-2023(online)].pdf | 2023-08-19 |
| 6 | Form 3-IN1457-04-PS-DFN-Spirotetramat.pdf | 2018-08-11 |
| 6 | 4104-MUM-2014-PETITION UNDER RULE 138 [17-08-2023(online)].pdf | 2023-08-17 |
| 7 | Form 2-IN1457-04-PS-DFN-Spirotetramat-Final-16122014.pdf | 2018-08-11 |
| 7 | 4104-MUM-2014-Correspondence to notify the Controller [01-08-2023(online)]-1.pdf | 2023-08-01 |
| 8 | 4104-MUM-2014-Power of Attorney-220915.pdf | 2018-08-11 |
| 8 | 4104-MUM-2014-Correspondence to notify the Controller [01-08-2023(online)].pdf | 2023-08-01 |
| 9 | 4104-MUM-2014-FORM-26 [01-08-2023(online)].pdf | 2023-08-01 |
| 9 | 4104-MUM-2014-OTHERS-230115.pdf | 2018-08-11 |
| 10 | 4104-MUM-2014-OTHERS-220915.pdf | 2018-08-11 |
| 10 | 4104-MUM-2014-PreGrant-HearingNotice-(HearingDate-03-08-2023).pdf | 2023-07-03 |
| 11 | 4104-MUM-2014-FER.pdf | 2019-09-26 |
| 11 | 4104-MUM-2014-Statement and Evidence [06-01-2023(online)].pdf | 2023-01-06 |
| 12 | 4104-MUM-2014-PRE GRANT OPPOSITION FORM [06-03-2020(online)].pdf | 2020-03-06 |
| 12 | 4104-MUM-2014-US(14)-HearingNotice-(HearingDate-13-09-2021).pdf | 2021-10-03 |
| 13 | 4104-MUM-2014-Annexure [28-09-2021(online)].pdf | 2021-09-28 |
| 13 | 4104-MUM-2014-PRE GRANT OPPOSITION DOCUMENT [06-03-2020(online)].pdf | 2020-03-06 |
| 14 | 4104-MUM-2014-OTHERS [06-03-2020(online)].pdf | 2020-03-06 |
| 14 | 4104-MUM-2014-Written submissions and relevant documents [28-09-2021(online)].pdf | 2021-09-28 |
| 15 | 4104-MUM-2014-ABSTRACT [24-03-2020(online)].pdf | 2020-03-24 |
| 15 | 4104-MUM-2014-FER_SER_REPLY [24-03-2020(online)].pdf | 2020-03-24 |
| 16 | 4104-MUM-2014-CLAIMS [24-03-2020(online)].pdf | 2020-03-24 |
| 16 | 4104-MUM-2014-COMPLETE SPECIFICATION [24-03-2020(online)].pdf | 2020-03-24 |
| 17 | 4104-MUM-2014-COMPLETE SPECIFICATION [24-03-2020(online)].pdf | 2020-03-24 |
| 17 | 4104-MUM-2014-CLAIMS [24-03-2020(online)].pdf | 2020-03-24 |
| 18 | 4104-MUM-2014-ABSTRACT [24-03-2020(online)].pdf | 2020-03-24 |
| 18 | 4104-MUM-2014-FER_SER_REPLY [24-03-2020(online)].pdf | 2020-03-24 |
| 19 | 4104-MUM-2014-OTHERS [06-03-2020(online)].pdf | 2020-03-06 |
| 19 | 4104-MUM-2014-Written submissions and relevant documents [28-09-2021(online)].pdf | 2021-09-28 |
| 20 | 4104-MUM-2014-Annexure [28-09-2021(online)].pdf | 2021-09-28 |
| 20 | 4104-MUM-2014-PRE GRANT OPPOSITION DOCUMENT [06-03-2020(online)].pdf | 2020-03-06 |
| 21 | 4104-MUM-2014-PRE GRANT OPPOSITION FORM [06-03-2020(online)].pdf | 2020-03-06 |
| 21 | 4104-MUM-2014-US(14)-HearingNotice-(HearingDate-13-09-2021).pdf | 2021-10-03 |
| 22 | 4104-MUM-2014-FER.pdf | 2019-09-26 |
| 22 | 4104-MUM-2014-Statement and Evidence [06-01-2023(online)].pdf | 2023-01-06 |
| 23 | 4104-MUM-2014-OTHERS-220915.pdf | 2018-08-11 |
| 23 | 4104-MUM-2014-PreGrant-HearingNotice-(HearingDate-03-08-2023).pdf | 2023-07-03 |
| 24 | 4104-MUM-2014-OTHERS-230115.pdf | 2018-08-11 |
| 24 | 4104-MUM-2014-FORM-26 [01-08-2023(online)].pdf | 2023-08-01 |
| 25 | 4104-MUM-2014-Power of Attorney-220915.pdf | 2018-08-11 |
| 25 | 4104-MUM-2014-Correspondence to notify the Controller [01-08-2023(online)].pdf | 2023-08-01 |
| 26 | Form 2-IN1457-04-PS-DFN-Spirotetramat-Final-16122014.pdf | 2018-08-11 |
| 26 | 4104-MUM-2014-Correspondence to notify the Controller [01-08-2023(online)]-1.pdf | 2023-08-01 |
| 27 | Form 3-IN1457-04-PS-DFN-Spirotetramat.pdf | 2018-08-11 |
| 27 | 4104-MUM-2014-PETITION UNDER RULE 138 [17-08-2023(online)].pdf | 2023-08-17 |
| 28 | Form-26-GPA-GSP.pdf | 2018-08-11 |
| 28 | 4104-MUM-2014-Written submissions and relevant documents [19-08-2023(online)].pdf | 2023-08-19 |
| 29 | 4104-MUM-2014-MARKED COPIES OF AMENDEMENTS [19-08-2023(online)].pdf | 2023-08-19 |
| 29 | 4104-MUM-2014-FORM-26 [03-04-2018(online)].pdf | 2018-04-03 |
| 30 | Form 18 [01-07-2016(online)].pdf | 2016-07-01 |
| 30 | 4104-MUM-2014-FORM 13 [19-08-2023(online)].pdf | 2023-08-19 |
| 31 | 4104-MUM-2014-AMMENDED DOCUMENTS [19-08-2023(online)].pdf | 2023-08-19 |
| 31 | Assignment [18-08-2015(online)].pdf | 2015-08-18 |
| 32 | 4104-MUM-2014-Response to office action [18-09-2023(online)].pdf | 2023-09-18 |
| 32 | Description(Complete) [18-08-2015(online)].pdf | 2015-08-18 |
| 1 | 2019-09-2516-34-49_25-09-2019.pdf |