Abstract: The present invention relates to herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl along with one or more inactive excipients. The present invention offer advantage of less chemical exposure and control on wide variety of weeds.
DESC:FIELD OF THE INVENTION:
The present invention relates to herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof along with one or more inactive excipients. The present invention also relates to process for preparing the said composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof along with one or more inactive excipients.
BACKGROUND OF THE INVENTION
The control of undesired vegetation is extremely important in order to achieve high crop efficiency. In many cases, herbicides have an effect against a spectrum of weeds; however, these herbicides may not be effective against certain type of other weeds, which may also be present in the crop to be protected. Therefore, there is a strong need for composition of two or more herbicides.
Herbicide(s), also commonly known as weed killers, are chemical substances used to control unwanted plants. In some cases, herbicidal active ingredients have been shown to be more effective in combination than when applied individually and this is referred to as "synergism." As described in the Herbicide Handbook of the Weed Science Society of America, Seventh Edition, 1994, p. 318, "'synergism' is an interaction of two or more factors such that the effect when combined is greater than the predicted effect based on the response of each factor applied separately."
The effectiveness of herbicides depends inter alia on the nature of the herbicide employed, its application rate, the preparation, the respective to the harmful plants, the climatic and soil conditions and the like. Another criterion is the duration of the action, or the degradation rate of the herbicide. Considerations include if appropriate, changes in the sensitivity of harmful plants to an active compound which may occur on prolonged use or geographically limited. Such changes manifest themselves as more or less pronounced loss in activity and can be only partially offset by higher herbicide application rates.
Because of the large number of possible influencing factors, there is virtually no individual active compound which combined the desired properties for different requirements, in particular with regard to the harmful plants and the climatic zones in itself. Then there is the constant need to achieve the effect with ever lower herbicide application rates. A lower application rate reduces not only the required for the application amount of a drug, but usually reduces the amount of formulation auxiliaries required. Both reduce the economic expense and improve the ecological compatibility of the herbicide treatment.
Propaquizafop was first disclosed in US 4687849 and chemically known as 2-isopropylideneaminooxyethyl (R)-2-[4-(6-chloroquinoxalin-2-yloxy) phenoxy] propionate and having chemical structure as below
Propaquizafop is a synthetic compound and belongs to the aryloxyphenoxy propionate family. Propaquizafop acts as a systemic herbicide of annual and perennial grasses. It quickly gets absorbed through the leaves and translocated to the meristematic growing regions of the plants, where it inhibits cell growth and division through the inhibition of ACCase inhibition.
WO2014181281 relates to an herbicidal mixture for controlling undesired vegetation, specifically to a herbicidal mixture comprising a synergistic combination of propaquizafop and imazethapyr.
CN104621121 discloses a mixed herbicide containing picloram and propaquizafop, belonging to the technical field of herbicides. The herbicide is prepared by taking picloram and propaquizafop as main effective components, wherein the mass ratio of picloram to propaquizafop is (0.1-80): (0.1-80).
CN104012552 relates to the technical field of pesticides and discloses a soybean field herbicide composition. The composition comprises two active components, namely fluthiacet-ethyl and propaquizafop, wherein the weight ratio of the two active components is 1:192 to 4:3; the two active components account for 5-75 mass percent of the herbicide composition.
However still there is a need for a herbicidal composition 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 herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl with one or more inactive excipients described herein in can provide solution to the above mentioned problems.
SUMMARY OF THE INVENTION
Accordingly, in a first aspect of the present invention provides a herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof with one or more inactive excipients.
Accordingly, in a second aspect, the present invention provides a method of preparing the herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof with one or more inactive excipients.
Accordingly, in a third aspect, the present invention provides a method of protecting a crop from unwanted vegetation here called as weed by applying a herbicidal composition defined in the first aspect.
Accordingly, in an anoter aspect, the present invention provides emulsifiable concentrate of herbicidal composition comprising synergistically effective amount of A) Propaquizafop, which is 0.1 to 25% by weight; B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl effective amount, which is 0.1 to 25% by weight and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof effective amount, which is 0.1 to 50% by weight; with 0.1 to 10% by weight of Alkyl polyethylene glycol ether; 0.1 to 10% w/w by weight of Polyvinylpyrrolidone; an amount of at least one water-immiscible solvent sufficient to keep the active ingredient mixture in solution and an emulsifying surfactant system in an amount sufficient to form an emulsion when the formulation is added to sovent, wherein the amount of the emulsifying surfactant system is between 1 and 10 % by weight.
Accordingly, in a another aspect, the present invention provides effective control of many grasses and broad leaf weeds which are not controlled by many herbicides or combinations of herbicides for weed controls.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof with one or more inactive excipients.
"Effective amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.
The term “formulation” and “composition” as used herein conveys the same meaning and can be used interchangeably.
The formulation or composition of the present invention can be in various physical forms, for example in the form of a dustable powder (DP), a gel, a wettable powder (WP), a granule (GR) (such as an emulsifiable granule (EG) or more particularly a water-dispersible granule (WG)), a water-dispersible tablet (WT), an emulsifiable concentrate (EC), a micro- emulsifiable (ME) concentrate, an oil-in-water emulsion (EW), an oil flowable (e.g. a spreading oil (SO)), an aqueous dispersion (e.g. aqueous suspension concentrate (SC)), an oily dispersion (OD), a suspo-emulsion (SE), a capsule suspension (CS), a soluble liquid, a water-soluble concentrate (with water or a water-miscible organic solvent as carrier), an impregnated polymer film, or jumbo formulation.
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.
In one of the embodiment of the present invention the method of application of the formulation comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof are by broadcasting in standing water by manual or by machine. Broadcasting can be done as direct granules broadcasting or mixing with sand or mixing with fertilizer, spraying with manual or machine operated knapsack sprayer, back pack sprayer, jumbo ball application, and Shaker bottle application.
In one of the embodiment of the present invention on method of application of the formulation comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof the time of application or formulations are applied before or after crop plants sowing or transplanting, or before weed germination or after weed germination.
Herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof which are bio active ingredients for the present formulation are present in ratio as described below;
Component A B C
Active Propaquizafop
Clodinafop Propargyl
Quizalofop-P-Ethyl
Quizalofop-P-Tefuryl
Fenoxaprop-P-Ethyl
Fluazifop-P-Butyl Acifluorfen
Fomesafen
Lactofen
Imazethapyr
Imazamox
Chlorimuron Ethyl
Ratio 0.1 to 25% 0.1 to 25% 0.1 to 50%
The compositions according to the invention control vegetation on non-crop areas very efficiently, especially at high rates of application.
As per one embodiment, the herbicicdal composition of present, invention conncetration of component A) Propaquizafop is in the range from 0.1 to 25% component B) at least one herbicide is in the range from 0.1 to 25% and component C) at least one more herbicide, is in the range from 0.1 to 50%
As per anoter embodiment, the herbicicdal emulsifiable concentrate (EC) composition of present, invention conncetration of component A) Propaquizafop is in the range from 0.1 to 25% component B) at least one herbicide is in the range from 0.1 to 25% and component C) at least one more herbicide, is in the range from 0.1 to 50% and Alkyl polyethylene glycol ether is present in the range from 0.1 to 10% w/w and Polyvinylpyrrolidone is present in the range form 0.1 to 10% w/w.
The compositions according to the invention are applied to the plants mainly by spraying. Here, the application can be carried out using, for example, water as carrier by customary spraying techniques using spray liquor amounts of from about 50 to 1000 l/ha (for example from 200 to 600 l/ha). The herbicidal compositions may also be applied by the low-volume or the ultra-low- volume method, or in the form of microgranules. The herbicidal compositions according to the present invention can be applied post- emergence. If any active ingredient of the inventive compositions, is less well tolerated by certain crop plants, application techniques may be used in which the herbicidal compositions are sprayed, with the aid of the spraying equipment, in such a way that as far as possible they do not come into contact with the leaves of the sensitive crop plants, while the active compounds reach the leaves of undesirable plants growing underneath, or the bare soil surface (post- directed, lay-by).
Moreover, it may be advantageous to apply the compositions of the present invention on their own or jointly in combination with other crop protection agents, for example with agents for controlling pests or phytopathogenic fungi or bacteria or with groups of active compounds which regulate growth. Also of interest is the miscibility with mineral salt solutions which are employed for treating nutritional and trace element deficiencies. Non-phytotoxic oils and oil concentrates can also be added.
When employed in plant protection, the amounts of active substances applied, i.e. active ingredient components A, B and C without formulation auxiliaries, are, depending on the kind of effect desired, from 0.1 to 10000 grams per hectare (g/ha), preferably from 0.5 to 1000 g/ha, more preferably from 5 to 500 g/ha and in particular from 5 to 200 g/ ha.
According to the invention the amount of formulated product applied depending upon the kind of effect desired, from 1 to 10000 ml or g per hectare, preferable from 10 to 5000 ml or g per hectare, more preferably from 100 to 2000 ml or g per hectare.
The synergistic herbicidal composition can be applied as post emergence, means after crop and weed germination. The best results can be obtained when applied at 10 to 30 days after sowing of crops.
In another embodiment of the present invention the composition comprising synergistically effective amonts of component A) Propaquizafop, component B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and component C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof are effective for control of weed in the crops selecetd from Soybean (Glycin max), Peanut (Arachis hypogaea), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), French bean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Cotton (Gossypium spp.), Sugarcane (Saccharum officinarum) , Castor (Ricinus communis), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus) , Tomato (Solanum lycopersicun), Chilly (Capsicum annum) and genetically modified version of all the crops mentioned above.
Moreover, the synergistic herbicidal mixtures according to the invention may also be employed for controlling harmful plants in modified crops. These modified crops are obtained by genetic engineering methods or by breeding, and—as a rule—they are distinguished by particular, advantageous properties, for example by resistance to certain crop protection agents (for example glyphosate. 2,4-D, dicamba tolerant crops like soybean, corn etc.), resistance to plant diseases or pathogens causing plant diseases such as particular insects or microorganism such as fungi, bacteria or viruses.
In one embodiment of the present invention, the composition of present invention controls all kind of Monocots, Dicots and Sedges weeds. The most common weeds controlled are selected from Abutilon indicum, Acalypha indica, Acanthospermum hispidum, Achyranthes aspera, Aerva tomentosa, Ageratum conyzoides, Alhagi camelorum, Amaranthus hybridus, Amaranthus spinosus, Amaranthus viridis, Ammannia baccifera, Anagallis arvensis, Argemone mexicana, Artemisia nilagiricia, Asphodelus tenuifolius, Avena fatua, Avena ludoviciana, Bidens pilosa, Boerhaavia diffusa, Boerhavia repanda, Brassica kaber, Bromus tectorum, Calotropis gigantea, Cannabis sativa, Carthamus axyacantha, Cassia tora, Celosia argentea, Centella asiatica, Chenopodium album, Chenopodium murale, Chloris barbata, Chrozophora rottlerii, Cichorium intybus, Cirsium arvense, Clitoria ternatea, Cnicus arvensis, Commelina benghalensis, Commelina communis, Convolvulus arvensis, Conyza canadensis, Corchorus acutangulus, Coronopus didymus, Crotalaria serice, Cucumis callosus, Cuscuta campestris, Cuscuta chinensis, Cynodon dactylon, Cyanotis axillaris, Cyperus esculenthus, Cyperus iria, Cyperus rotundus, Dactyloctenium aegyptium, Datura stramonium, Daucus carota, Digera arvensis, Digitaria sanguinalis, Dinebra retroflexa, Echinochola colonum, Echinochola crusgalli, Eclipta alba, Eichhornia crassipes, Elephantopus scaber, Eleusine indica, Eragrostis major, Euphorbia geniculata, Euphorbia hirta, Fimbristylis miliacea, Fumaria indica, Gynandropsis gynandra, Heliotropium indicum, Indigofera glandulosa, Ipomea aquatica, Lantana camara, Lathyrus aphaca, Launaea asplenifolia, Launaea nudicaulis, Leucas aspera, Marsilea quadrifoliata, Medicago denticulate, Mimosa pudica, Melilotus alba, Melilotus indica, Ocimum canum, Oenothera biennis, Opuntia dillenil, Orobanche ramosa, Oryza longistaminata, Oryza sativa, Oxalis corniculata, Oxalis latifolia, Parthenium hysterophorus, Paspalum sanguinale, Phalaris minor, Phyllanthus niruri, Physalis minima, Polypogon monspeliensis, Portulaca oleracea, Prosopis juliflora, Rumex dentatus, Saccharum spontaneum, Stearia glauca, Seteria viridis, Sida spinosa, Silene antirrhina, Sisymbrium irio, Solanum nigrum, Solanum surattense, Sonchus oleraceous, Sorghum halepense, Spergula arvensis, Sphenocleazeylanica Gaertn, Striga asiatica, Tagetes minuta, Trianthema monogyna, Trianthema portulacastrum, Tribulus terrestris, Trigonelia polycerata, Vernonia cinerea, Vicia sativa and Xanthium strumarium.
The composition of the present invention comprising synergistically effective amounts of component A) Propaquizafop, component B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and component C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl 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. 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 formulations often cause foam during mixing operations in production. In order to reduce the tendency to foam, anti-foam agents are often added either during the production stage or before filling into bottles. Generally, there are two types of anti-foam agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.
A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading. Wetting agents are used for two main functions in agrochemical formulations: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules. Examples of wetting agents used in wettable powder, suspension concentrate, and water-dispersible granule formulations include but not limited to sodium lauryl sulphate; sodium dioctylsulphosuccinate; alkyl phenol ethoxylates; and aliphatic alcohol ethoxylates and the salts thereof which are standard in agricultureor 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 suspo-emulsions to modify the rheology or flow properties of the liquid and to prevent separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixtures.
The quick coating agent can be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, 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 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.
In one of the embodiment of the present invention, composition synergistically effective amounts of component A) Propaquizafop, component B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and component C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl are mixed with solvent and is homogenized with other surfactants and stabilizers. Thereafter, this mixture is applied to adsorbing material in a coating pan followed by mixing at a rotating speed of 25 rpm for 10 min, thereby obtaining a granular agrochemical formulation. Optionally it is sprayed on adsorbing porous carrier and then extruded in jumbo granules by using extrusion technique.
Inactive excipients as mentioned below can also be used based on formulation.
Inactive excipients used in SE formulation
Name Function
n- Octanol Solvent
Octyl Phenol Ethoxylate Wetting agent & Emulsifier
Polyoxyethylene (8) nonyl phenol Wetting agent & Emulsifier
Acrylic graft copolymer Dispersing agent
Ethoxylated Fatty Alcohol Co-dispersant/Wetting agent
Polyalkoxy alkyl ether Dispersing agent & Emulsifier
Ethylene oxide/propylene oxide block copolymer Dispersing agent & Emulsifier
Sodium salt of naphthalene sulfonate condensate Dispersing agent
Trisiloxane ethoxylate Spreader & Wetting agent
Silicone antifoam emulsion Antifoam
Silicone dioxide Suspending aid, Ant caking agent
Polysaccharide Rheology Modifier,Thickner
Sodium dioctyl sulfosuccinate Wetting agent & Emulsifier
Polyarylphenyl ether phosphate Dispersing agent & Wetting agent
DiEthylene Glycol Antifreezing Agent
MonoEthylene Glycol Antifreezing Agent
Polypropanil Glycol Antifreezing Agent
1,2-benzisothiazolin-3-one Biocide/Preservative
Sodium benzoate Biocide/Preservative
2-bromo-2-nitropropane-1,3-diol Biocide/Preservative
Formaldehyde Biocide/Preservative
Inactive excipients used in WG and WP formulation
Sodium salt of naphthalene sulfonate condensate Dispersing Agent
Modified polyacrylate copolymer Dispersing Agent
Sodium polycarboxylate Dispersing Agent
Sodium Ligno sulfonate Dispersing Agent
Alkyl naphthalene sulfonate condensate, sodium salt Dispersing Agent
Polyacrylate co-polymer Dispersing Agent, Stabilizer, Emulsifier
Alcohol block co-polymer Co-dispersant
Blend of naphthalene sulfonate condensate & phenol sulfonate condensate Wetting Agent & Dispersing Agent
blend of naphthalene sulfonate condensate Wetting Agent
Sodium dodecylbenzene sulfonate Wetting Agent
Sodium lauryl sulfate Wetting Agent
Blend of alkyl naphthalene sulfonate and anionic wetting agent Wetting Agent
Sodium n-butyl naphthalene sulfonate Wetting Agent
Sodium isopropyl naphthalene sulfonate Wetting Agent
Blend of sodium alkyl aryl sulfonates Wetting Agent
Corn starch Binder, Filler
Silicon dioxide Suspending agent, Anti-caking Agent, Filler
Urea formaldehyde resin / Urea-methanol Anti caking agent
Lactose Filler
China clay/ Kaolin Filler
Titanium dioxide Filler
Talcum powder Filler
Diatomaceous earth Filler
Polyvinylpyrrolidone Binder
Silicone antifoam emulsion Defoaming agent
Fatty amine ethoxylate Wetting agent, Dispersing agent, Stabilizers, Sanitizers, Defoaming agent
Inactive excipients used in ME formulation
N,N-Dimethyldecanamide Green Solvent
N-Methylpyrrolidone Solvent
Cyclohexane Solvent
Ethoxylated TristyrylPhenol Dispersing Agent,Emulsifier
Polyalkoxylated butyl ether Wetting & Dispersing agent,Emulsifier
DiEthylene Glycol Antifreezing Agent
MonoEthylene Glycol Antifreezing Agent
Polypropanil Glycol Antifreezing Agent
Glycerene Antifreezing Agent
PolyEthylene Glycol Antifreezing Agent
Silicone antifoam emulsion Antifoam
Trisiloxane ethoxylate Spreader & Wetting agent
1,2-benzisothiazolin-3-one Biocide/Preservative
Sodium benzoate Biocide/Preservative
2-bromo-2-nitropropane-1,3-diol Biocide/Preservative
Formaldehyde Biocide/Preservative
Inactive excipients used in EC formulation
Mixture of heavy aromatic hydrocarbons / C IX Solvent
Xylene Solvent
n-Butanol (NBA) Solvent
Solvent - C-9 Solvent
N-Methyl-2-pyrrolidone Solvent / Co-solvent
Polyaryl Phenol Ethoxylate Emulsifiers, Wetting agents, Dispersants, Stabilizers
Calcium Dodecyl Benzene Sulphonate Emulsifier
Blend of Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate Emulsifier
Alkyl polyethylene glycol ether Spreader, Sticker, Penetrant, Surface tension reducer
Polyvinylpyrrolidone Sticker, Surface tension reducer, Binder
Inactive excipients used in OD formulation
N,N-Dimethyldecanamide Solvent
Unsaturated Fatty alcohol, Ethoxylated Non Ionic Emulsifier
Calcium Alkyl Benzen Sulphonate Anionic Emulsifier
Ethoxylated TristyrylPhenol Dispersing Agent,Emulsifier
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer Emulsifier and anti-flocculant
Polyamide Rheology Modifier,Thickner
fatty acid methyl ester Green solvent & carrier
Trisiloxane ethoxylate Spreader & Wetting agent
Polyacrylate co-polymer Dispersing Agent
Polyarylalkylphenol polyethylene glycol phosphoric acid ester Dispersing Agent
The process for preparing the present novel synergistic composition 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.
The scope of present invention covers composition as mentioned below;
Active Ingredient I Active Ingredient II Active Ingredient III Preferred A.I.(%) in formulation Formulation per Hectare (g or ml) Preferred Formulation
Active Ingredient I Active Ingredient II Active Ingredient III
Propaquizafop Clodinafop Propargyl Acifluorfen 6.0% 1.0% 16.5% 1000 EC
Propaquizafop Clodinafop Propargyl Acifluorfen 6.0% 1.0% 16.5% 1000 OD
Propaquizafop Clodinafop Propargyl Fomesafen 6.0% 1.0% 18.0% 1000 EC
Propaquizafop Clodinafop Propargyl Fomesafen 8.0% 1.0% 24.0% 750 EC
Propaquizafop Clodinafop Propargyl Fomesafen 5.0% 1.0% 16.0% 1000 ME
Propaquizafop Clodinafop Propargyl Lactofen 6.0% 1.0% 18.0% 1000 EC
Propaquizafop Clodinafop Propargyl Lactofen 6.0% 1.0% 18.0% 1000 OD
Propaquizafop Clodinafop Propargyl Imazethapyr 10.0% 2.0% 15.0% 500 EC
Propaquizafop Clodinafop Propargyl Imazethapyr 2.50% 0.50% 3.75% 2000 ME
Propaquizafop Clodinafop Propargyl Imazethapyr 10.0% 2.0% 15.0% 500 WG
Propaquizafop Clodinafop Propargyl Imazethapyr 10.0% 2.0% 15.0% 500 WP
Propaquizafop Clodinafop Propargyl Imazamox 5.0% 1.0% 7.5% 1000 EC
Propaquizafop Clodinafop Propargyl Imazamox 10.0% 2.0% 15.0% 500 WG
Propaquizafop Clodinafop Propargyl Imazamox 10.0% 2.0% 15.0% 500 WP
Propaquizafop Clodinafop Propargyl Chlorimuron Ethyl 12.0% 2.0% 1.8% 500 WG
Propaquizafop Clodinafop Propargyl Chlorimuron Ethyl 10.0% 2.0% 1.8% 500 WP
Propaquizafop Clodinafop Propargyl Chlorimuron Ethyl 10.0% 2.0% 1.8% 500 SE
Propaquizafop Quizalofop-P-Ethyl Acifluorfen 5.0% 2.0% 16.5% 1000 EC
Propaquizafop Quizalofop-P-Ethyl Fomesafen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Quizalofop-P-Ethyl Lactofen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Quizalofop-P-Ethyl Imazethapyr 4.0% 2.0% 7.5% 1000 EC
Propaquizafop Quizalofop-P-Ethyl Imazethapyr 4.0% 2.0% 7.5% 1000 SE
Propaquizafop Quizalofop-P-Ethyl Imazethapyr 2.0% 1.0% 3.75% 2000 ME
Propaquizafop Quizalofop-P-Ethyl Imazamox 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Quizalofop-P-Ethyl Imazamox 5.0% 2.0% 7.5% 1000 SE
Propaquizafop Quizalofop-P-Ethyl Chlorimuron Ethyl 10.0% 4.0% 1.8% 500 SE
Propaquizafop Quizalofop-P-Tefuryl Acifluorfen 5.0% 2.0% 16.5% 1000 EC
Propaquizafop Quizalofop-P-Tefuryl Fomesafen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Quizalofop-P-Tefuryl Lactofen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Quizalofop-P-Tefuryl Imazethapyr 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Quizalofop-P-Tefuryl Imazamox 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Quizalofop-P-Tefuryl Chlorimuron Ethyl 5.0% 2.0% 0.9% 1000 SE
Propaquizafop Fenoxaprop-P-Ethyl Acifluorfen 5.0% 2.0% 16.5% 1000 EC
Propaquizafop Fenoxaprop-P-Ethyl Fomesafen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Fenoxaprop-P-Ethyl Lactofen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Fenoxaprop-P-Ethyl Imazethapyr 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Fenoxaprop-P-Ethyl Imazamox 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Fenoxaprop-P-Ethyl Chlorimuron Ethyl 5.0% 2.0% 0.9% 1000 SE
Propaquizafop Fluazifop-P-Butyl Acifluorfen 5.0% 2.0% 16.5% 1000 EC
Propaquizafop Fluazifop-P-Butyl Fomesafen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Fluazifop-P-Butyl Lactofen 5.0% 2.0% 18.0% 1000 EC
Propaquizafop Fluazifop-P-Butyl Imazethapyr 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Fluazifop-P-Butyl Imazamox 5.0% 2.0% 7.5% 1000 EC
Propaquizafop Fluazifop-P-Butyl Chlorimuron Ethyl 5.0% 2.0% 0.9% 1000 SE
EC Emulsifiable Concentrate, OD Oil Dispersion, ME Micro Emulsion, WG
Water Dispersible Granules, WP Wettable Powder, SE Suspo Emulsion
As per one embodiment, the preferred herbicidal composition is in the form of Emulsifiable Concentrate.
As per one embodiment, the emulsifieable concentrate (EC) contains Alkyl polyethylene glycol ether and Polyvinylpyrrolidone.
Further as per preferred embodiment, the emulsifieable concentrate (EC) contains Alkyl polyethylene glycol ether is present in the range from 0.1 to 10% w/w and Polyvinylpyrrolidone is present in the range form 0.1 to 10% w/w.
As per preferred embodiment, the excipient Alkyl polyethylene glycol ether and Polyvinylpyrrolidone in emulsifieable concentrate (EC) is playing important role. As per study and analysis, it has been observed that when Emulsifiable concentrate (EC) contains Alkyl polyethylene glycol ether and Polyvinylpyrrolidone in desired concentration mentioned above, the formulation exhibit good long term stability. In contrast when the Emuslfiable Concetrate (EC), does not contain Alkyl polyethylene glycol ether and Polyvinylpyrrolidone, the formulation does not provide desired stability. Moreover the novel formulation of Emuslfiable Concetrate (EC) of synergistic combination of present invention also enhanced the bio efficacy against weed in field conditions also.
The invention is further illustrated in the following examples, which should not be construed as further limiting the scope of the invention.
EXAMPLE
Example 1: (Recipe 1) Propaquizafop 6%+Clodinafop Propargyl 1% +Fomesafen 18%-EC (Emulsifiable Concentrate)
Composition Percentage (w/w)
Propaquizafop (95% purity) 6.52
Clodinafop Propargyl (95% purity ) 1.26
Fomesafen (95% purity) 19.16
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
Alkyl polyethylene glycol ether 1.50
Polyvinylpyrrolidone 1.00
N-Methyl-2-pyrrolidone 15.00
Solvent - C-9 48.56
TOTAL 100.00
Procedure:
Step 1 Charge half quantity of solvent and then mix the technical into this solvent untill completely soluble.
Step 2 Now add Emulsifier and other adjuvents dose as per screening ration.
Step 3 Now add remaining solvent to this mixture
Step 4 Final product is sent for QC approval.
Step 5 After approval material is packed in requied pack sizes.
Storage stability-Propaquizafop 6%+Clodinafop Propargyl 1%+Fomesafen 18% EC (Emulsifiable Concentrate) formulation
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 to Yellowish liquid Complies Complies Complies
Propaquizafop content 5.70 - 6.30 6.22 6.15 6.21
Clodinafop Propargyl content 0.95 - 1.05 1.05 1.01 1.03
Fomesafen content 17.10 - 18.9 18.34 18.25 18.33
Emulsion stability Max 1ml creaming or sediment PASS PASS PASS
pH 5.0-7.0 6.7 6.48 6.5
Specific gravity 1-1.5 1.03 1.03 1.03
Room temperature storage data
Specification Study Duration
Parameters In house 1 month 3 month 6 month 9 month 12 month
Description Off-white to Yellowish liquid Complies Complies Complies Complies Complies
Propaquizafop content 5.70 - 6.30 6.22 6.21 6.2 6.2 6.19
Clodinafop Propargyl content 0.95 - 1.05 1.03 1.03 1.02 1.03 1.02
Fomesafen content 17.10 - 18.9 18.34 18.33 18.31 18.3 18.3
Emulsion stability Max 1ml creaming or sediment PASS PASS PASS PASS PASS
pH 5.0-7.0 6.5 6.5 6.49 6.49 6.49
Specific gravity 1.03 1.03 1.03 1.03 1.03 1.03
Example 1.A: (Recipe 2) Propaquizafop 6%+Clodinafop Propargyl 1% +Fomesafen 18%-EC (Emulsifiable Concentrate)
Composition Percentage (w/w)
Propaquizafop (95% purity) 6.52
Clodinafop Propargyl (95% purity ) 1.26
Fomesafen (95% purity) 19.16
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
N-Methyl-2-pyrrolidone 15.00
Solvent - C-9 51.06
TOTAL 100.00
Procedure: As per Example 1
Storage stability: Propaquizafop 6%+Clodinafop Propargyl 1% +Fomesafen 18%-EC (Emulsifiable Concentrate)
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 6.28 5.95 6.26
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.05 1.01 1.02
Fomesafen content (% w/w) 17.10 - 18.9 18.23 18.01 18.2
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.11 7.07 7.08
Cold test separation or creaming max 2 ml after 1 hour Complies 3ml 3ml
Flash point Above 24.5 0C 43 43 43
Room Temperature storage data
Parameters Specification (In house) Study Duration
1 month 3 month 6 month 9 month 12 month
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 6.27 6.25 6.21 6.1 6.01
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.05 1.04 1.03 1.03 0.99
Fomesafen content (% w/w) 17.10 - 18.9 18.22 18.19 18.17 18.14 18.09
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies Complies 3 ml
pH (5% in DM water) 6.0 - 8.0 7.10 7.09 7.09 7.11 7.15
Cold test separation or creaming max 2 ml after 1 hour Complies Complies Complies Complies Complies
Flash point Above 24.5 0C 43 43 43 43 43
Example 2: (Recipe 3) Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 24%-EC (Emulsifiable Concentrate)
Composition Percentage (w/w)
Propaquizafop (95% purity) 8.63
Clodinafop Propargyl ( 95% purity) 1.26
Fomesafen 95% purity) 25.47
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
N-Methyl-2-pyrrolidone 16.00
Alkyl polyethylene glycol ether 1.50
Polyvinylpyrrolidone 1.00
Solvent - C-9 39.14
TOTAL 100.00
Procedure: As per Example 1
Storage stability: Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 24%-EC (Emulsifiable Concentrate)
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 8.17 8.08 8.15
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.07 1.05 1.06
Fomesafen content (% w/w) 17.10 - 18.9 24.19 24.11 24.18
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.24 7.15 7.24
Cold test separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 0C 43 43 43
Room Temperature Storage data
Parameters Specification (In house) Study Duration
1 month 3 month 6 month 9 month 12 month
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 8.17 8.17 8.16 8.16 8.14
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.07 1.07 1.07 1.07 1.06
Fomesafen content (% w/w) 17.10 - 18.9 24.18 24.17 24.17 24.15 24.14
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.22 7.21 7.22 7.23 7.24
Cold test separation or creaming max 2 ml after 1 hour Complies Complies Complies Complies Complies
Flash point Above 24.5 0C 43 43 43 43 43
Example 2.A: (Recipe 4) Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 24%-EC (Emulsifiable Concentrate)
Composition Percentage (w/w)
Propaquizafop (95% purity) 8.63
Clodinafop Propargyl ( 95% purity) 1.26
Fomesafen 95% purity) 25.47
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
N-Methyl-2-pyrrolidone 16.00
Solvent - C-9 41.64
TOTAL 100.00
Procedure: As per Example 1
Storage stability: Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 24%-EC (Emulsifiable Concentrate)
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 8.21 8.01 8.15
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.06 0.97 1.02
Fomesafen content (% w/w) 17.10 - 18.9 24.52 24.19 24.45
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.32 7.22 7.27
Cold test separation or creaming max 2 ml after 1 hour Complies 3ml 3ml
Flash point Above 24.5 0C 43 43 43
Room Temperature Storage data
Parameters Specification (In house) Study Duration
1 month 3 month 6 month 9 month 12 month
Description Pale yellow to Yellowish stable clear liquid. It shall be free from extraneous visible matter. Complies Complies Complies Complies Complies
Propaquizafop content (% w/w) 5.70 - 6.60 8.20 8.19 8.18 8.18 8.16
Clodinafop Propargyl content (% w/w) 0.95 - 1.10 1.06 1.06 1.06 1.05 1.05
Fomesafen content (% w/w) 17.10 - 18.9 24.51 24.48 24.41 24.38 24.35
Emulsion stability Max. 2ml creaming or sediment after 1 hour Complies Complies Complies Complies 3 ml
pH (5% in DM water) 6.0 - 8.0 7.31 7.29 7.28 7.26 7.25
Cold test separation or creaming max 2 ml after 1 hour Complies Complies Complies Complies Complies
Flash point Above 24.5 0C 43 43 43 43 43
Example 3: Propaquizafop 10% + Clodinafop Propargyl 2% + Imazethapyr 15% EC (Emulsifiable Concentrate) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 10.74
Clodinafop Propargyl ( 95% purity) 3.31
Imazethapyr ( 95% purity) 16.00
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
Alkyl polyethylene glycol ether 1.50
Polyvinylpyrrolidone 1.00
N-Methyl-2-pyrrolidone 35.00
Solvent - C-9 25.45
TOTAL 100.00
Procedure: As per Example 1
Storage stability-Propaquizafop 10%+Clodinafop Propargyl 2%+Imazethapyr 15% EC (Emulsifiable Concentrate) formulation
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 to Yellowish liquid Complies Complies Complies
Propaquizafop content 9.5-10.5 10.32 10.15 10.32
Clodinafop Propargyl content 1.9-2.1 2.08 2.03 2.08
Imazethapyr content 14.25-15.75 15.48 15.19 15.45
Emulsion stability Max 1ml creaming or sediment PASS PASS PASS
pH 5.0-7.0 5.95 5.87 6.1
Specific gravity 1-1.1 1.03 1.03 1.03
Room temperature storage
Specification Study Duration
Parameters In house 1 month 3 month 6 month 9 month 12 month
Description Off-white to Yellowish liquid Complies Complies Complies Complies Complies
Propaquizafop content 9.5-10.5 10.31 10.3 10.28 10.27 10.25
Clodinafop Propargyl content 1.9-2.1 2.08 2.08 2.07 2.07 2.05
Imazethapyr content 14.25-15.75 15.46 15.45 15.39 15.35 15.28
Emulsion stability Max 1ml creaming or sediment PASS PASS PASS PASS PASS
pH 5.0-7.0 5.95 5.95 5.91 5.91 5.89
Specific gravity 1.03 1.03 1.03 1.03 1.03 1.03
Example 4: Propaquizafop 5% + Quizalofop-P-Ethyl 2% + Fomesafen 18%-EC (Emulsifiable Concentrate) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 5.47
Quizalofop-P-Ethyl ( 95% purity) 2.31
Fomesafen (95% purity) 19.16
Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate 7.00
Alkyl polyethylene glycol ether 1.50
Polyvinylpyrrolidone 1.00
N-Methyl-2-pyrrolidone 15.00
Solvent C-9 48.56
TOTAL 100.00
Procedure: As per Example 1
Storage Stability- Propaquizafop 5% + Quizalofop-P-Ethyl 2% + Fomesafen 18%-EC (Emulsifiable Concentrate) formulation
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 to Yellowish liquid Complies Complies Complies
Propaquizafop content 4.75-5.25 5.22 5.06 5.2
Quizalofop-P-Ethyl content 1.9-2.1 2.09 2.04 2.09
Fomesafen content 17.1-18.9 18.6 18.2 18.6
Emulsion Stabilty Max 1ml creaming or sediment PASS PASS PASS
pH (1%) 5.0-7.0 6.32 6.19 6.32
Specific gravity 0.95-1.05 1.01 1.01 1.01
Room temperature storage
Specification Study Duration
Parameters In house 1 month 3 month 6 month 9 month 12 month
Description Off-white to Yellowish liquid Complies Complies Complies Complies Complies
Propaquizafop content 4.75-5.25 5.22 5.2 5.19 5.19 5.17
Quizalofop-P-Ethyl content 1.9-2.1 2.09 2.08 2.07 2.07 2.07
Fomesafen content 17.1-18.9 18.6 18.59 18.51 18.45 18.41
Emulsion Stabilty Max 1ml creaming or sediment PASS PASS PASS PASS PASS
pH (1%) 5.0-7.0 6.32 6.32 6.32 6.3 6.3
Specific gravity 0.95-1.05 1.01 1.01 1.01 1.01 1.01
Example 5: Propaquizafop 5%+Quizalofop-P-Ethyl 2% +Acifluorfen 16.5%- EC (Emulsifiable Concentrate) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 5.47
Clodinafop Propargyl ( 95% purity) 2.31
Acifluorfen (85% purity) 19.65
N,N Dimethyl decanamide 10.00
Unsaturated fatty alcohol ethoxylates 4.00
Calcium alkyl benzene sulfonate 5.00
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer 3.00
ethoxylated polyaryl alcohol 7.00
Polyamide 3.00
Adjuvant containing trisiloxane ethoxylate 1.00
Rapeseed oil fatty acid methyl ester 39.57
TOTAL 100.00
Storage Stability- Propaquizafop 5% + Quizalofop-P-Ethyl 2% + Acifluorfen 16.5%-EC (Emulsifiable Concentrate) formulation
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 to Yellowish liquid Complies Complies Complies
Propaquizafop content 4.75-5.25 5.19 5.11 5.19
Quizalofop-P-Ethyl content 1.9-2.1 2.07 2.02 2.07
Acifluorfen content 15.675-17.325 17.05 16.77 17.05
Emulsion Stability Max 1ml creaming or sediment PASS PASS PASS
pH (1%) 5.0-7.0 6.95 6.85 6.95
Specific gravity 0.95-1.05 1.02 1.02 1.02
Room temperature storage
Specification Study Duration
Parameters In house 1 month 3 month 6 month 9 month 12 month
Description Off-white to Yellowish liquid Complies Complies Complies Complies Complies
Propaquizafop content 4.75-5.25 5.19 5.18 5.18 5.17 5.17
Quizalofop-P-Ethyl content 1.9-2.1 2.06 2.06 2.06 2.06 2.05
Aciflourfen content 15.675-17.325 17.05 17.04 17.03 17.03 17.02
Emulsion Stability Max 1ml creaming or sediment PASS PASS PASS PASS PASS
pH (1%) 5.0-7.0 6.95 6.95 6.95 6.92 6.92
Specific gravity 0.95-1.05 1.02 1.02 1.02 1.02 1.02
Example 6: Propaquizafop 6%+Clodinafop Propargyl 1% +Acifluorfen 16.5%- OD (Oil Dispersion) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 6.53
Clodinafop Propargyl ( 95% purity) 1.26
Acifluorfen (85% purity) 19.65
N,N Dimethyl decanamide 12.00
Unsaturated fatty alcohol ethoxylates 6.00
Calcium alkyl benzene sulfonate 5.00
ethoxylated polyaryl alcohol 7.00
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer 3.00
Polyamide 3.00
Alkyl polyethylene glycol ether 2.00
Rapeseed oil fatty acid methyl ester 34.56
TOTAL 100.00
Procedure:
Step 1 Charge required quantity of vegetable oil in vessel and add polyvinyl pyrrollidone, mix well for 30 minutes using highshear homogeniser.
Step 2 Add required quantity of Wetting agent, dispersing agent & suspending agents and homogenise the contents for 45 – 60 minutes using high shear homogeniser.
Step 3 Then add technical materials and homogenise for further 30 minutes.
Step 4 Now pass this homogenised material through horizontal bead mill to get required particle size.
Step 5 Add remaining amount of vegetable oil and gum solution and stirr for 20 minutes using homogeniser.
Step 6 After completion sample is sent to QC for A.I. & particle size analysis.
Step 7 After approval from QC, material is transferred to storage tank till packing.
Storage Stability- Propaquizafop 6%+Clodinafop Propargyl 1% +Acifluorfen 16.5%- OD (Oil Dispersion) formulation
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 to Yellowish to flowable liquid Complies Complies Complies
Propaquizafop content 5.70 - 6.30 6.25 6.16 6.23
Propaquizafop suspensibility Mini 80% 90.18 89.9 90.15
Clodinafop Propargyl content 0.95 - 1.05 1.02 1.01 1.02
Clodinafop Propargyl suspensibility Mini 80% 89.78 89.52 89.75
Acifluorfen content 15.675-17.325 16.75 16.68 16.74
Acifluorfen suspensibility Mini 80% 93.88 93.52 93.82
pH 5.0-7.0 6.21 6.05 6.2
Particle size D50 <3, D90 <10 D50 2.2, D90 8.1 D50 2.7, D90 8.9 D50 2.5, D90 8.65
Pourability Mini 95% 99.6 99.1 99.6
Specific gravity 1.02 – 1.15 1.13 1.13 1.13
Viscosity 300-800 470 490 481
Room temperature torage
Specification Study Duration
Parameters In house 1 month 3 month 6 month 9 month 12 month
Description Off-white to Yellowish to flowable liquid Complies Complies Complies Complies Complies
Propaquizafop content 5.70 - 6.30 6.25 6.24 6.23 6.21 6.2
Propaquizafop suspensibility Mini 80% 90.18 90.1 90.01 89.87 89.54
Clodinafop Propargyl content 0.95 - 1.05 1.02 1.02 1.02 1.02 1.01
Clodinafop Propargyl suspensibility Mini 80% 89.78 89.75 89.65 89.52 89.41
Acifluorfen content 15.675-17.325 16.75 16.74 16.74 16.73 16.73
Acifluorfen suspensibility Mini 80% 93.88 93.86 93.74 93.5 93.44
pH 4.5-7.0 6.2 6.2 6.2 6.2 6.19
Particle size D50 <3, D90 <10 D50 2.2, D90 8.1 D50 2.4, D90 8.6 D50 2.2, D90 8.1 D50 2.7, D90 8.7 D50 2.9, D90 8.9
Pourability Mini 95% 99.6 99.6 99.6 99.5 99.5
Specific gravity 1.02 – 1.15 1.13 1.13 1.13 1.13 1.13
Viscosity 300-800 470 470 475 475 482
Example 7: Propaquizafop 2.5% + Clodinafop Propargyl 0.5% + Imazethapyr 3.75% ME (Micro Emulsion) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 2.84
Clodinafop Propargyl (95% purity) 0.73
Imazethapyr (95% purity) 4.16
Tetrahydrofurfuryl Alcohol 12.00
Ethoxylated Tristrylphenol 10.00
Polyoxyethelene (20) sorbitan monolaurate 15.00
Mono Ethylene Glycol 5.00
1,2-benzisothiazolin-3-one 0.10
D.M. Water 50.17
TOTAL 100.00
Procedure:
Step 1 Aqueous phase:Charge 90% of total quanitiy of water in a vessel and then add preservative and MEG and stirr well till clear solution
Step 2 Organic Phase: In other vessel add solvent and Technical and then recommended surfactant slowly and mix completely under stirring
Step 3 Now under moderate stirring add this oil phase into aqueous phase and let mix till completely homogeneous
Step 4 Add the remaining amount of water and mix until homogeneous
Step 5 Filter through a 50 mesh into an appropriate container
Step 6 Final product is sent for QC approval.
Step 7 After approval material is packed in requied pack sizes.
Storage stability-Propaquizafop 2.5%+Clodinafop Propargyl 0.5%+Imazethapyr 3.75% ME (Micro Emulsion) formulation
Parameters Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
In House
Description Colourless to slight turbid solution Complies Complies Complies
Propaquizafop content 2.375-2.625 2.59 2.52 2.59
Clodinafop Propargyl content 0.475-0.525 0.52 0.51 0.52
Imazethapyr content 3.563-3.938 3.81 3.76 3.80
PH(1% D.M.Water) 5.0-7.0 6.54 6.44 6.5
Specific gravity 0.98-1.02 1.01 1.01 1.01
Room temperature storage
Parameters Specification Study Duration
In house 1 month 3 month 6 month 9 month 12 month
Description Colourless to slight turbid solution Complies Complies Complies Complies Complies
Propaquizafop content 2.375-2.625 2.59 2.59 2.58 2.57 2.55
Clodinafop Propargyl content 0.475-0.525 0.52 0.52 0.52 0.52 0.52
Imazethapyr content 3.563-3.938 3.81 3.79 3.78 3.77 3.77
PH (1% DM Water) 5.0-7.0 6.54 6.54 6.52 6.52 6.51
Specific gravity 1.01 1.01 1.01 1.01 1.01 1.01
Example 8: Propaquizafop 2% + Quizalofop-P-Ethyl 1% + Imazethapyr 3.75% ME (Micro Emulsion) formulation
Composition Percentage (w/w)
Propaquizafop (95% purity) 2.31
Quizalofop-P-Ethyl (95%purity) 1.26
Imazethapyr ( 95% purity) 4.16
Tetrahydrofurfuryl Alcohol 12.00
Ethoxylated Tristrylphenol 8.00
POE (20) sorbitan monolaurate 15.00
Mono Ethylene Glycol 5.00
1,2-benzisothiazolin-3-one 0.10
D.M. Water 52.17
TOTAL 100.00
Procedure: As above
Storage Stability- Propaquizafop 2% + Quizalofop-P-Ethyl 1% + Imazethapyr 3.75% ME (Micro Emulsion) formulation
Parameters Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
In House
Description Colourless to slight turbid solution Complies Complies Complies
Propaquizafop content 1.9-2.1 2.07 2.02 2.07
Quizalofop-P-Ethyl content 0.95-1.05 1.03 1.01 1.03
Imazethapyr content 3.563-3.938 3.83 3.78 3.82
pH(1% D.M.Water) 5.0-7.0 6.75 6.67 6.75
Density 1.0-1.6 1.02 1.02 1.02
Room temperature storage
Parameters Specification Study Duration
In house 1 month 3 month 6 month 9 month 12 month
Description Colourless to slight turbid solution Complies Complies Complies Complies Complies
Propaquizafop content 1.9-2.1 2.07 2.06 2.06 2.06 2.05
Quizalofop-P-Ethyl content 0.95-1.05 1.03 1.03 1.02 1.02 1.02
Imazethapyr content 3.563-3.938 3.82 3.79 3.78 3.77 3.77
pH(1% D.M.Water) 5.0-7.0 6.75 6.75 6.74 6.74 6.73
Denisty 1.0-1.6 1.02 1.02 1.02 1.02 1.02
Example 9: Propaquizafop 12% + Clodinafop Propargyl 2% + Chlorimuron Ethyl 1.8% WG (Water Dispersible Granules)
Composition Percentage (w/w)
Propaquizafop (95% purity) 12.84
Clodinafop Propargyl (95%purity) 2.31
Chlorimuron Ethyl (95%purity) 2.10
Alkylated naphthalene sulfonate, sodium salt 5.00
Sodium Lauryl Sulfate 3.00
PPT silica 2.00
Silicon antifoam 0.50
Corn starch 28.00
Lactose 25.00
China Clay 10.00
Ammonium sulphate 9.25
TOTAL 100.00
Procedure:
Step 1 Charge the required quantity of filler, wetting agent, dispersing agent, and suspending agent, & technical in premixing blender for homogenization for 30 minutes.
Step 2 Pre-blended material is than grinded through Jet mill/ air classifier mills. Finely grinded material is blended in post blender till it becomes homogeneous. (for approx 1.5 hr)
Step 3 Homogeneous material is analysed. After getting approval from QC dept. material is unloaded into 25 kg. HDPE bag with LDPE liner inside.
Step 4 Finely grinded powder is mixe with required quantity of water to form extrudable dough.
Step 5 Dough is passed through extruder to get granules of required size.
Step 6 Wet granules are passed through Fluidised bed drier and further graded using vibrating screens.
Step 7 Final product is sent for QC approval.
Step 8 After approval material is packed in requied pack sizes.
Storage stability Study of Propaquizafop 12%+Clodinafop Propargyl 2%+Chlorimuron Ehtyl 1.8% WDG (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
Propaquizafop content 11.4-12.6 12.28 12.16 12.28
Propaquizafop suspensibility Min. 70% 92.55 90.41 92.5
Clodinafop Propargyl content 1.9-2.1 2.09 2.02 2.09
Clodinafop Propargyl suspensibility Min. 70% 91.8 90.78 91.8
Chlorimuron Ehtyl content 1.71-1.89 1.85 1.81 1.85
Chlorimuron Ehtyl suspensibility Min. 70% 90.12 89.01 90.1
pH (1%) 5.0-7.0 6.35 6.33 6.35
Wet-sieve (45 micron sieve) Mini 98.5% 99.7 99.6 99.7
Bulk density 0.45-0.85 0.55 0.55 0.55
Wettability Max 60 sec 8 9 8
Room temperature storage
Specification Study Duration
Parameters In house 1month 3 month 6 month 9 month 12 month
Description White to off-white granules Complies Complies Complies Complies Complies
Propaquizafop content 11.4-12.6 12.28 12.27 12.25 12.23 12.2
Propaquizafop suspensibility Min 70% 92.45 92.22 92.01 91.88 91.68
Clodinafop Propargyl content 1.9-2.1 2.09 2.08 2.08 2.06 2.05
Clodinafop Propargyl suspensibility Min 70% 91.77 91.71 91.65 91.55 91.43
Chlorimuron Ehtyl content 1.71-1.89 1.85 1.84 1.84 1.84 1.83
Chlorimuron Ehtyl suspensibility Min 70% 90.02 89.99 89.84 89.81 89.69
pH (1%) 5.0-7.0 6.35 6.35 6.35 6.34 6.34
Wet-sieve (45 micron sieve) Mini 98.5% 99.7 99.7 99.7 99.7 99.7
Bulk density 0.45-0.85 0.55 0.55 0.55 0.55 0.55
Wettability Max 60 sec 8 8 8 8 9
Example 10: Propaquizafop 10% + Quizalofop-P-Ethyl 4% + Chlorimuron Ethyl 1.8% SE (Suspo Emulsion) formulation
Ingredient Percentage (w/w)
Propaquizafop 10.74
Quizalofop-P-Ethyl (95% purity) 4.42
Chlorimuron Ethyl ( 95% purity) 2.11
polyalkoxylated butyl ether 2.25
Polyarylphenyl ether sulphate ammonium salt 1.50
Acrylic graft copolymer 3.50
Alkylated naphthalene sulfonate, sodium salt 0.50
Silicone antifoam 1.00
Benzisothiazoline 0.20
Glycol 5.00
Octyl phenol Ethoxylate 1.5 mole 8.00
Polysaccharides 0.25
Water 60.53
TOTAL 100.00
Procedure:
Step 1 Gum Solution should be made 12-18 hour prior to use. Take required quantity of water, biocide, and defoamer and homogenise, then slowly add gum powder to it and stir till complete dissolution.
Step 2 Oil Phase: Technical disolved in solvent and emulsifier.
Step 3 Aqueous phase: Charge 90% of total quanitiy of water in a vessel and then add preservative and MEG and stirr well till clear solution
Step 4 Add required quantity of Wetting agent, dispersing agent & suspending agents and homogenise the contents for 45 – 60 minutes using high shear homogeniser.
Step 5 Then add technical and other remaining adjuvants excluding ‘antifreeze & thickeners’ are added to it and homogenised to get uniform.
Step 6 Now add oil phase in aqueous phase and stirr for 30 minutes using homogeniser.
Step 6 Before grinding half the quantity of antifoam was added and then material was subjected to three cycles of grinding in Dyno mill.
Step 7 Half quantity of the antifoam was added along with antifreeze after grinding process completes and before sampling for in process analysis.
Step 8 Finally add gum solution to this formulation and Send to QC for quality check.
Storage Stability- Propaquizafop 10% + Quizalofop-P-Ethyl 4% + Chlorimuron Ethyl 1.8% SE (Suspo Emulsion) formulation
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
Propaquizafop content 9.5-10.5 10.38 10.18 10.38
Propaquizafop suspensibility Min 80% 92.55 91.4 92.42
Quizalofop-P-Ethyl content 3.8-4.2 4.19 4.09 4.19
Quizalofop-P-Ethyl suspensibility Min 80% 90.26 89.58 90.03
Chlorimuron Ehtyl content 1.71-1.89 1.88 1.83 1.87
Chlorimuron Ehtyl suspensibility Min 80% 93.55 92.26 93.35
pH 5.0-9.0 6.67 6.61 6.65
Particle size D50 <3, D90 <10 2.4, 8.1 2.5, 8.2 2.9, 8.9
Pourability 95 % min 99.1 98.9 98.8
Specific gravity 1.05 – 1.15 1.13 1.14 1.13
Viscosity 350 -900 cps 500 510 530
Room temperature storage
Specification Study Duration
Parameters In House 1 month 3 month 6 month 9 month 12 month
Description Off-white liquid Complies Complies Complies Complies Complies
Propaquizafop content 9.5-10.5 10.36 10.35 10.35 10.34 10.34
Propaquizafop suspensibility Min 80% 92.48 92.26 92.09 91.89 91.78
Quizalofop-P-Ethyl content 3.8-4.2 4.18 4.17 4.16 4.15 4.14
Quizalofop-P-Ethyl suspensibility Min 80% 90.18 90.08 90.01 89.97 89.92
Chlorimuron Ehtyl content 1.71-1.89 1.87 1.87 1.85 1.85 1.84
Chlorimuron Ehtyl suspensibility Min 80% 93.48 93.29 93.17 93.08 92.83
pH 5.0-9.0 6.67 6.67 6.67 6.66 6.66
Particle size D50 <3, D90 <10 2.4, 8.1 2.4, 8.1 2.4, 8.1 2.4, 8.1 2.4, 8.1
Pourability 95 % min 99.1 99.1 99.1 99.1 99.1
Specific gravity 1.05 – 1.15 1.13 1.13 1.13 1.13 1.14
Viscosity 350 -900 cps 500 505 507 510 513
Example 11: Bio Efficacy Trials
The field experiments on present invention concerns a synergistic herbicidal mixture comprising of Propaquizafop, one more herbicide selected from the group of Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl, Fluazifop-P-butyl and one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox, Chlorimuron Ethyl were carried out to evaluate the phyto-toxicity and Bioefficacy against different weed flora existing in various crop eco-system.
Trial 1: Phytotoxicity and Bioefficacy against mixed weed flora in various crops like Soybean (Glycine max), Black gram (Vigna mungo L.), Cluster bean (Cyamopsis tetragonoloba) and Groundnut (Arachis hypogaea)
The field experiments were conducted in Soybean, Black gram, Cluster bean and Groundnut. The experimental details are as below:
Crops & Varieties: Soybean (JS 335), Black gram (UG 135), Cluster bean (HG 884), Groundnut (GG 2). All crops were sown on same farm, not as mixed crops or inter Crop. All the crop varieties were Non GMO.
Experimental design: Randomized block design (R.B.D)
Replications: Four
No. of Treatments: As per treatment details
Plot size: 30 sq. mt.
Application Time: 20 DAS (Days after sowing)
Observations: at 3, 7, 14 and 21 DAA (Days after Application)
Spray Volume: 375 liter water per hectare
Application Equipment: Manually operated knapsack sprayer fitted with flat fat nozzle
Treatment Details:
Table 1: Treatment Details for Phytotoxicity and Bioefficacy
Treatment Details Active Ingredient (g/h) Formulation (ml or g/h)
T1 : Recipe 1-Propaquizafop 6%+Clodinafop Propargyl 1% +Fomesafen 18% EC (improved recipe) 60+10+180 1000
T2 : Recipe 2-Propaquizafop 6%+Clodinafop Propargyl 1% +Fomesafen 18% EC (know recipe) 60+10+180 1000
T3 : Recipe 3-Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 18% EC (improved recipe) 60+7.5+180 750
T4 : Recipe 2-Propaquizafop 8%+Clodinafop Propargyl 1% +Fomesafen 18% EC (known recipe) 60+7.5+180 750
T5 : Prior Art 1-Propaquizafop 10% EC+Fomesafen salt 22.1% SL (tank mix) 60+180 600+815
T6 : Prior Art 2-Clodinafop Propargyl 15% WP+Fomesafen salt 22.1% SL (tank mix) 10+180 66.67+815
T7 : Prior Art 3-Propaquizafop 10% EC + Clodinafop Propargyl 15% WP (tank mix) 60+10 600+66.67
T8 : Propaquizafop 10% EC 60 600
T9 : Clodinafop Propargyl 15% WP 10 66.67
T10 : Fomesafen salt 22.1% SL* 180 815
T11 : Untreated Control (Water Spray) 0 0
Where EC Emulsifiable Concentrate, SL Soluble Liquid, WP Wettable Powder, *Added 0.25% Non Ionic Surfactant
All the required crops, Soybean, Black gram, Cluster bean and Groundnut were raised as per the standard agronomic practices in the field (all crops on same piece of land) to conduct trials to assess phytotoxicity and bioefficacy of inventive mixtures with improved recipe, know recipe and prior art treatments given in Table 1. The trials were laid out in Randomized Block Design (RBD) with different treatments including untreated check (UTC), replicated four times. For each treatment plot size of 30 sq. mt was maintained. The application of different treatments with prescribed doses was done with manually operated knapsack sprayer fitted with flat fan nozzle. The spray volume was used at 375 l/h for spraying. The Untreated check plot was sprayed with water alone. Observations on phytotoxicity viz., leaf scorching, leaf yellowing were recorded at 3, 7, 14 and 21 days after spraying, by adopting 0-10 rating scale as below :
0= No phytotoxicity, 1 =1-10% leaf scorching/yellowing, 2=11-20% leaf scorching/yellowing… 9=81-90% leaf scorching/yellowing, 10=91-100% leaf scorching/yellowing.
Percent phytotoxicity was calculated by following formula:
Sum of all scores
% Phytotoxicity = ------------------------------------------------------------- X 100
Number of samples x highest rating scale
Bioefficacy : Species wise weed count recorded at 7 DAA and 14 DAA (Days after Application) by using 0.25 m2 quadrant treatment wise in minimum 4 places randomly selected in the plot per replication. The species wise weed count further grouped in to Grasses and Broad Leaf weeds (BLW). The average of each variable was used together with the sum of all the variables per plot to calculate the percentage of control.
% Weed Control =
Mean weed count in – Mean weed control
Untreated plot in treated plot
1- ------------------------------------------------------- X 100
Mean weed count in untreated plot
Table 2: Phytotoxicity comparison
Treatment Details % Leaf Scorching
Soybean Black gram Groundnut
3 DAA 7 DAA 14 DAA 21 DAA 3 DAA 7 DAA 14 DAA 21 DAA 3 DAA 7 DAA 14 DAA 21 DAA
T1 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
T2 10.64 5.26 2.12 0.00 12.84 6.82 3.18 0.00 15.82 10.24 4.62 2.16
T3 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
T4 12.84 4.28 1.28 0.00 14.82 8.36 2.52 0.00 16.82 11.62 5.28 3.20
T5 20.62 15.82 8.28 2.64 23.48 14.62 6.38 1.24 21.28 16.38 6.72 2.16
T6 18.28 9.38 4.82 0.00 19.82 12.48 2.48 0.00 17.74 10.72 4.16 1.06
T7 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
T8 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
T9 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
T10 26.82 18.26 6.82 1.62 22.74 14.62 8.62 3.18 28.84 18.42 10.86 6.34
T11 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
The phytotoxicity observations given in above (Table 2), shows that the inventive mixture with improved recipe of Propaquizafop+Clodinafop Propargyl+Fomesafen (T1 and T3) were found safe to the tested crops like, Soybean, Black gram and Ground nut crop, where as all the prior art samples as well as their solo application were found phyto toxic to soybean, black gram and groundnut. The mixture of Propaquizafop+ Clodinafop Propargyl+ Fomesafen with known recipe (Treatment T2 and T3), shows marginal phytotoxicity which later recover about 14 days after application (14 DAA). The inventive mixture with improved recipe (T1 and T3) of Propaquizafop+ Clodinafop Propargyl+ Fomesafen found safe (non phyto toxic) to the soybean, black gram and groundnut crop.
Table 3: Bioefficacy comparison
Treatment Details % Weed Cotnrol
Soybean Black gram Groundnut
Grasses BLW* Grasses BLW Grasses BLW
7 DAA 14 DAA 7 DAA 14 DAA 7 DAA 14 DAA 7 DAA 14 DAA 7 DAA 14 DAA 7 DAA 14 DAA
T1 100.00 98.28 100.00 98.64 100.00 98.36 100.00 97.32 100.00 97.94 100.00 98.64
T2 86.68 80.28 84.68 77.26 88.44 76.62 85.48 77.38 88.72 78.16 84.66 75.82
T3 99.16 96.24 98.88 96.16 99.12 96.28 98.28 95.68 98.26 96.82 97.28 95.40
T4 83.84 76.74 80.84 72.38 85.18 73.72 82.96 73.56 85.52 74.82 81.72 72.66
T5 81.72 75.72 79.96 70.48 83.28 70.84 80.26 71.64 82.34 71.62 78.82 68.18
T6 18.48 10.62 74.28 68.62 16.18 12.48 78.28 74.40 20.18 14.20 76.48 65.84
T7 80.38 74.58 0.00 0.00 82.18 76.48 0.00 0.00 80.28 70.62 0.00 0.00
T8 74.42 70.44 0.00 0.00 77.18 68.68 0.00 0.00 74.28 64.62 0.00 0.00
T9 16.28 8.38 0.00 0.00 14.10 8.62 0.00 0.00 16.42 10.62 0.00 0.00
T10 5.28 3.28 73.28 64.68 6.82 2.68 74.38 70.16 11.72 4.42 72.38 62.96
T11 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
Weed flora observed: Grasses includes Echinochloa spp., Dinebra retroflex, Digitaria ciliaris, BLW* (Broad Leaf Weeds) includes Commelina benghalensis, Commelina communis, Amaranthus viridis, Euphorbia geniculata, Parthenium hysterophorus, and Phyllanthus niruri.
The Bioefficacy observations given in above (Table 3) shows that the inventive mixture with improved recipe of Propaquizafop+Clodinafop Propargyl+Fomesafen (T1 and T3) provides excellent control of grasses and broad leaf weeds (BLW) compared to all prior art treatments as well as their solo application. The improved recipe of Propaquizafop+Clodinafop Propargyl+Fomesafen (T1 and T3) provides approximately 10 to 20% higher weed control compared to known recipe of Propaquizafop+Clodinafop Propargyl+Fomesafen (T2 and T4).
Trial 2: Bioefficacy evaluation on Soybean, Black gram, Cluster bean, Groundnut
The synergistic pesticide action of the inventive mixtures can be demonstrated by the experiments below. A synergistic effect exists wherever the action of a combination (ready-mix) of active ingredient is greater than the sum of the action of each of the components alone. Therefore a synergistically effective amount or an effective amount of a synergistic composition or combination is an amount that exhibits greater pesticide activity than the sum of the pesticide activities of the individual components. In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two active components can be calculated as follows:
Colby’s Formula:
To study the synergistic effect of the inventive mixtures of Propaquizafop with at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl, Fluazifop-P-butyl and one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox, Chlorimuron Ethyl., various sets of field experiments were conducted in different crops like soybean, black gram, cluster bean and groundnut.
Experiment 1: Synergistic weed control in Soybean
Crop & Variety: Soybean, JS-335
Experimental design: Randomized block design (R.B.D)
Replications: Three
No. of Treatments: Eleven
Plot size: 30 sq. mt.
Application Time: 22 DAS (Days after sowing)
Observations: 15 DAA (Days after Application)
Spray Volume: 400 liter water per hectare
Application Equipment: Hand operated knapsack sprayer fitted with flat fan nozzle
Experiment method: The trials were laid out in Randomized Block design (RBD) with eleven (11) treatments, replicated three times. For each treatment plot size of 30 sq. mt. was maintained. To raise the crops all the agronomic practices were followed as usually adopted. The treatments were applied as per the calculated dosages, using manually operated knap sack sprayer, fitted with flat fan nozzle. The spray volume was used at 400 l/ha for application of all herbicidal treatments. Species wise weed count recorded at 15 DAA (Days after Application) by using 0.25 m2 quadrant treatment wise in minimum 3 places randomly selected in the plot per replication. The species wise weed count further grouped in to Grasses and Broad Leaf weeds (BLW). The average of each variable was used together with the sum of all the variables per plot to calculate the percentage of control.
% Weed Control =
Mean weed count in – Mean weed control
Untreated plot in treated plot
1- ------------------------------------------------------- X 100
Mean weed count in untreated plot
The % weed control data used in Colby’s formula to calculate the synergism between three herbicides.
Table 4: Synergistic weed control in Soybean
Active Ingredients Active Ingredient (g/h) Formulation (ml/h) % Weed Control
Grasses Broad Leaf Total Weeds
Actual Expected Actual Expected Actual Expected Ratio
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP + Fomesafen salt 22.1% SL 60+ 10+ 180 600 ml+ 66.67 g+ 815 ml 98.16 82.05 98.46 87.63 98.74 85.31 1.16
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP + Acifluorfen salt 20.1% SL 60+ 10+ 165 600 ml+ 66.67 g+ 820 ml 97.88 82.39 98.74 88.23 98.26 85.07 1.16
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP 60+ 10 600 ml+ 66.67 g 86.72 80.11 0.00 0.00 62.48 71.49 0.87
Propaquizafop 10% EC+ Fomesafen salt 22.1% SL 60+ 180 600 ml+ 815 ml 80.74 73.50 90.37 87.63 75.48 76.21 0.99
Propaquizafop 10% EC+ Acifluorfen salt 20.1% SL 60+ 165 600 ml+ 820 ml 77.38 74.00 91.17 88.23 74.13 75.82 0.98
Clodinafop Propargyl 15% WP +Fomesafen salt 22.1% SL 10+ 180 66.67 g+ 815 ml 46.83 38.89 91.24 87.63 67.53 68.20 0.99
Clodinafop Propargyl 15% WP +Acifluorfen salt 20.1% SL 10+ 165 66.67g+ 820 ml 45.27 40.04 90.16 88.23 66.83 67.67 0.99
Propaquizafop 10% EC 60 600 ml 70.63 0.00 53.82
Clodinafop Propargyl 15% WP 10 66.67g 32.28 0.00 38.26
Fomesafen salt 22.1% SL* 180 815 ml 9.76 87.63 48.49
Acifluorfen salt 20.1% SL* 165 820 ml 11.46 88.23 47.63
EC Emulsifiable Concentrate, WP Wettable Powder, SL Soluble Liquid.
*Added 0.25% Non Ionic Surfactant
Weed flora: Grasses- Echinochloa spp., Dinebra retroflex, Digitaria ciliaris, BLW – Commelina benghalensis, Commelina communis, Amaranthus viridis, Euphorbia geniculata, Parthenium hysterophorus, and Phyllanthus niruri.
The field study data shows that tank mixes of Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP + Fomesafen salt 22.1% SL and Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP + Acifluorfen salt 20.1% SL gives excellent control of grasses and broad leaf weeds observed in the experimental plot.
Experiment 2: Weed control in Soybean
Crop & Variety: Soybean, NRC-7
Experimental design: Randomized block design (R.B.D)
Replications: Three
No. of Treatments: Eleven
Plot size: 30 sq. mt.
Application Time: 18 DAS (Days after sowing)
Observations: 15 DAA (Days after Application)
Spray Volume: 400 liter water per hectare
Application Equipment: Hand operated knapsack sprayer fitted with flat fan nozzle
Experiment method: as given in experiment 1.
Table 5: Weed control in Soybean
Active Ingredients Active Ingredient (g/h) Formulation (ml/h) % Weed Control
Grasses Broad Leaf Total Weeds
Actual Expected Actual Expected Actual Expected Ratio
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP +Imazethapyr 10% SL 50+ 10+ 75 500 ml+ 66.7 g+ 750 ml 97.4 89.73 97.9 67.63 97.5 85.60 1.14
Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC + Imazethapyr 10% SL 40+ 20+ 75 400 ml+ 400 ml + 750 ml 98.7 81.83 97.4 0.00 99.2 83.30 1.19
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP 50+ 10 500 ml+ 66.7g 89.7 76.20 0.0 0.00 51.3 70.32 0.73
Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC 40+ 20 400 ml + 400 ml 93.1 77.58 0.0 0.00 56.4 75.70 0.74
Propaquizafop 10% EC+ Imazethapyr 10% SL 50+ 75 500 ml+ 750 ml 90.7 87.32 66.5 67.63 81.3 79.05 1.03
Clodinafop Propargyl 15% WP + Imazethapyr 10% SL 10+ 75 66.7 g+ 750 ml 60.8 65.02 68.3 67.63 65.2 66.65 0.98
Quizalofop-P-Ethyl 5% EC+ Imazethapyr 10% SL 20+ 75 400 ml + 750 ml 64.3 67.05 69.6 67.63 71.5 72.70 0.98
Propaquizafop 10% EC 50 500 ml 70.6 0.0 56.8
Clodinafop Propargyl 15% WP 10 66.7 g 19.0 0.0 31.3
Quizalofop-P-Ethyl 5% EC 20 400 ml 23.7 0.0 43.7
Imazethapyr 10% SL* 75 750 ml 56.8 67.6 51.5
EC Emulsifiable Concentrate, WP Wettable Powder, SL Soluble Liquid’
*Added 0.25% Non Ionic Surfactant and 2 g/l Ammonium Sulphate
Weed flora: Grasses- Echinochloa spp., Panicum repens, Brachiaria mutica, BLW – Commelina benghalensis, Cyanotis axillaris, Digera arvensis, Euphorbia geniculata, Acalypha indica.
Observations on efficacy of tank mixes of Propaquizafop 10% EC+ Clodinafop op Propargyl 15% WP +Imazethapyr 10% SL and Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC + Imazethapyr 10% SL shows synergism in terms of weed control of both the grassy and broad leaf weeds in soybean crop.
Experiment 3: Synergistic weed control in Soybean
Crop & Variety: Soybean, JS-335
Experimental design: Randomized block design (R.B.D)
Replications: Three
No. of Treatments: Eleven
Plot size: 42 sq. mt.
Application Time: 17 DAS (Days after sowing)
Observations: 15 DAA (Days after Application)
Spray Volume: 400 liter water per hectare
Application Equipment: Hand operated knapsack sprayer fitted with flat fan nozzle
Experiment method: as given in experiment 1.
Table 6: Weed control in Soybean
Active Ingredients Active Ingredient (g/h) Formulation (ml/h) % Weed Control
Grasses Broad Leaf Total Weeds
Actual Expected Actual Expected Actual Expected Ratio
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP +Chlorimuron Ethyl 25% WP* 60+10+9 600 ml+ 66.7 g+ 37.5 g 97.4 75.26 98.1 68.36 97.7 84.44 1.16
Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC +Chlorimuron Ethyl 25% WP* 50+20+9 500 ml+ 400 ml + 37.5 g 99.1 82.23 98.4 0.00 98.9 85.57 1.16
Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP* 60+10 600 ml+ 66.7g 92.8 75.26 0.0 0.00 50.3 71.56 0.70
Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC* 50+20 500 ml + 400 ml 93.7 77.61 0.0 0.00 52.7 74.77 0.71
Propaquizafop 10% EC+ Chlorimuron Ethyl 25% WP* 50+9 500 ml+ 37.5 g 89.3 68.83 70.4 68.36 72.6 72.78 1.00
Clodinafop Propargyl 15% WP +Chlorimuron Ethyl 25% WP* 10+9 66.7 g+ 37.5 g 26.7 20.62 67.3 68.36 67.8 68.71 0.99
Quizalofop-P-Ethyl 5% EC+Chlorimuron Ethyl 25% WP* 20+9 400 ml + 37.5 g 32.6 28.17 69.5 68.36 71.6 72.24 0.99
Propaquizafop 10% EC 50 500 ml 68.8 0.0 50.3
Clodinafop Propargyl 15% WP 10 66.7 g 20.6 0.0 42.8
Quizalofop-P-Ethyl 5% EC 20 400 ml 28.2 0.0 49.3
Chlorimuron Ethyl 25% WP* 9 37.5 g 0.0 68.4 45.3
EC Emulsifiable Concentrate, WP Wettable Powder
*Added 0.25% Non Ionic Surfactant
Weed flora: Grasses- Echinochloa spp., Digitaria sanguinalis, Eleusine indica, Brachiaria mutica, BLW – Commelina benghalensis, Celocia argentia, Digera arvensis, Euphorbia geniculata, Phyllanthus niruri, Trianthema monogyna.
The percent weed control of both the grasses and broad leaf weeds in the treatment of tank mixes of Propaquizafop 10% EC+ Clodinafop Propargyl 15% WP +Chlorimuron Ethyl 25% WP and Propaquizafop 10% EC+ Quizalofop-P-Ethyl 5% EC +Chlorimuron Ethyl 25% WP were higher than expected weed control.
Experiment 4: Synergistic weed control in Black gram
Crop & Variety: Black gram, LBG 787
Experimental design: Randomized block design (R.B.D)
Replications: Three
No. of Treatments: Eighteen
Plot size: 36 sq. mt.
Application Time: 18 DAS (Days after sowing)
Observations: 15 DAA (Days after Application)
Spray Volume: 400 liter water per hectare
Application Equipment: Hand operated knapsack sprayer fitted with flat fan nozzle
Experiment method: as given in experiment 1.
Table 7: Treatment Details
Compositions Application Rate (ml or g per h) Active Ingredient (g/h)
T1 : Propaquizafop 6% + Clodinafop Propargyl 1% + Acifluorfen-Sodium salt 16.5% OD 1000 60+10+165
T2 :Propaquizafop 5% + Quizalofop-P-Ethyl 2% + Acifluorfen-Sodium salt 16.5% EC 1000 50+20+165
T3 :Propaquizafop 6% + Clodinafop Propargyl 1% + Fomesafen 18% EC 1000 60+10+180
T4 :Propaquizafop 5% + Quizalofop-P-Ethyl 2% + Fomesafen-sodium salt 18% EC 1000 50+20+180
T5 : Propaquizafop 10% + Clodinafop Propargyl 2% + Imazethapyr 15% EC 500 50+10+75
T6 : Propaquizafop 10% + Quizalofop-P-Ethyl 2% + Imazethapyr 15% EC 500 50+10+75
T7 : Propaquizafop 2.5% + Clodinafop Propargyl 0.5% + Imazethapyr 3.75% ME* 2000 50+10+75
T8 : Propaquizafop 2.5% + Quizalofop-P-Ethyl 0.5% + Imazethapyr 3.75% ME* 2000 50+10+75
T9 : Propaquizafop 12% + Clodinafop Propargyl 2% + Chlorimuron Ehtyl 1.8% SE 500 60+10+9
T10 : Propaquizafop 10% + Quizalofop-P-Ethyl 4% + Chlorimuron Ethyl 1.8% SE 500 50+20+9
T11 :Propaquizafop 10% EC 600 60
T12 :Clodinafop Propargyl 15% WP 66.67 20
T13 :Quizalofop-P-Ethyl 5% EC 400 20
T14 :Acifluorfen Sodium salt 20.1% SL 820 165
T15 :Fomfesafen Sodium salt 22.1% SL 815 180
T16 : Imazethapyr 10% SL** 750 75
T17 : Chlorimuron Ethyl 25% WP*** 37.5 9
T18 : Untreated Check (UTC) Water spray -
OD Oil Dispersion, EC Emulsifiable Concentrate, ME Micro Emulsion, SE Suspo Emulsion, WP Wettable Powder, SL Soluble Liquid.
*Added 2 g/l Ammonium Sulphate, **Added 0.25% Non Ionic Surfactant and 2 g/l Ammonium Sulphate, *** Added 0.25% Non Ionic Surfactant.
Table 8: Synergistic weed control in Black gram
Treatments % Weed Control
Grasses Broad Leaf
15 DAA* 30 DAA* 15 DAA* 30 DAA*
T1 97.56 98.92 97.72 98.82
T2 98.65 100 98.22 98.78
T3 97.16 99.48 98.12 99.62
T4 98.58 100 97.42 98.24
T5 97.82 99.88 96.72 97.82
T6 99.42 100 96.28 98.36
T7 98.72 99.87 97.1 98.42
T8 99.24 99.84 97.64 98.26
T9 97.38 98.18 95.72 96.42
T10 98.42 99.24 94.58 96.26
T11 51.28 52.36 0.00 0.00
T12 20.23 20.72 0.00 0.00
T13 40.83 42.48 0.00 0.00
T14 2.18 5.28 51.36 54.70
T15 3.72 4.26 49.75 50.18
T16 50.42 51.72 46.28 47.76
T17 0.00 0.00 40.68 41.92
T18 0.00 0.00 0.00 0.00
*DAA Days after application
Weed flora: Grasses- Echinochloa spp., Dactyloctenium spp., Dinebra spp., Brachiaria mutica, BLW –Amaranthus lividis, Digera arvensis, Euphorbia hirta, Phyllanthus niruri, Physalis minima.
All the inventive ready mixes shows synergistic weed control of grassy weeds and broad leaf weeds in black gram compared to their individual applications.
All the above results show that the percentage of herbicidal control observed for the tank mix combinations as well as ready mix formulations are greater than the expected percentage (Colby Ration O/E). The data shows efficacy on grassy weeds and broad leaf weeds on soybean and black gram is significantly higher than that has been reported in many prior art.
,CLAIMS:We claim;
[CLAIM 1]. A herbicidal composition comprising synergistically effective amounts of A) Propaquizafop, B) at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl and C) at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof with one or more inactive excipients.
[CLAIM 2]. The herbicidal composition as claimed in claim 1 wherein component A is present in ratio of 0.1 to 25%, component B herbicide is present in ratio of 0.1 to 25% and component C one more herbicide is present in ratio of 0.1 to 50%.
[CLAIM 3]. The herbicidal composition as claimed in claim 1-2, wherein inactive excipients is selected from the group consisting of dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents and buffering agent.
[CLAIM 4]. The herbicidal composition as claimed in claim 1-3, wherein the composition are selected from dustable powder (DP), a gel, a wettable powder (WP), a granule (GR) (such as an emulsifiable granule (EG) or more particularly a water-dispersible granule (WG)), a water-dispersible tablet (WT), an emulsifiable concentrate (EC), a micro- emulsifiable concentrate, an oil-in-water emulsion (EW), an oil flowable (e.g. a spreading oil (SO)), an aqueous dispersion (e.g. aqueous suspension concentrate (SC)), an oily dispersion (OD), a suspo-emulsion (SE), a capsule suspension (CS).
[CLAIM 5]. The herbicidal composition as claimed claim 1 or 4, wherein the composition is emulsifiable concentrate (EC).
[CLAIM 6]. The herbicidal compositions as claimed in claim 1 or 4, wherein the composition is Micro Emulsion (ME).
[CLAIM 7]. The herbicidal compositions as claimed in claim 1 or 4, wherein the composition is Water Dispersible Granules (WDG).
[CLAIM 8]. An emulsifiable concentrate of herbicidal composition according to claim 1 comprising:
a) synergistically effective amount of Propaquizafop, which is 0.1 to 25% by weight;
b) synergistically effective amount of at least one herbicide selected from Clodinafop Propargyl, Quizalofop-P-Ethyl, Quizalofop-P-Tefuryl, Fenoxaprop-P-Ethyl and Fluazifop-P-Butyl effective amount, which is 0.1 to 25% by weight;
c) synergistically effective amount of at least one more herbicide selected from Acifluorfen, Fomesafen, Lactofen, Imazethapyr, Imazamox and Chlorimuron Ethyl and salts thereof effective amount, which is 0.1 to 50% by weight;
d) 0.1 to 10% by weight of Alkyl polyethylene glycol ether;
e) 0.1 to 10% w/w by weight of Polyvinylpyrrolidone;
f) an amount of at least one water-immiscible solvent sufficient to keep the active ingredient mixture in solution,
g) an emulsifying surfactant system in an amount sufficient to form an emulsion when the formulation is added to sovent, wherein the amount of the emulsifying surfactant system is between 1 and 10 % by weight.
[CLAIM 9]. The herbicidal composition according to claim 8 wherein emulsifying surfactant are Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate.
[CLAIM 10]. The herbicidal composition according to claim 1 or 8 which comprises:
a) 1 to 20% by weight/weight of Propaquizafop;
b) 0.5 to 10% by weight/weight of Clodinafop Propargyl;
c) 1 to 30% by weight/weight of Fomesafen;
d) 0.1 to 10% by weight/weight of Polyaryl phenol ethoxylate & calcium dodecyl benzene sulfonate;
e) 0.1 to 10% by weight/weight of Alkyl polyethylene glycol ether;
f) 0.1 to 10% by weight/weight of Polyvinylpyrrolidone;
g) 1 to 30% by weight/weight of N-Methyl-2-pyrrolidone; and
h) Solvent.
[CLAIM 11]. The herbicidal composition as claimed in any of the preceding claims, wherein composition to be used for crop selected from selected from Soybean (Glycin max), Peanut (Arachis hypogaea), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), French bean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Cotton (Gossypium spp.), Sugarcane (Saccharum officinarum) , Castor (Ricinus communis), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus) , Tomato (Solanum lycopersicun) , Chilly (Capsicum annum) and genetically modified version of all the crops mentioned above.
[CLAIM 12]. The herbicidal composition as claimed in any of the preceding claims, wherein the composition control weeds selected from Abutilon indicum, Acalypha indica, Acanthospermum hispidum, Achyranthes aspera, Aerva tomentosa, Ageratum conyzoides, Alhagi camelorum, Amaranthus hybridus, Amaranthus spinosus, Amaranthus viridis, Ammannia baccifera, Anagallis arvensis, Argemone mexicana, Artemisia nilagiricia, Asphodelus tenuifolius, Avena fatua, Avena ludoviciana, Bidens pilosa, Boerhaavia diffusa, Boerhavia repanda, Brassica kaber, Bromus tectorum, Calotropis gigantea, Cannabis sativa, Carthamus axyacantha, Cassia tora, Celosia argentea, Centella asiatica, Chenopodium album, Chenopodium murale, Chloris barbata, Chrozophora rottlerii, Cichorium intybus, Cirsium arvense, Clitoria ternatea, Cnicus arvensis, Commelina benghalensis, Commelina communis, Convolvulus arvensis, Conyza canadensis, Corchorus acutangulus, Coronopus didymus, Crotalaria serice, Cucumis callosus, Cuscuta campestris, Cuscuta chinensis, Cynodon dactylon, Cyanotis axillaris, Cyperus esculenthus, Cyperus iria, Cyperus rotundus, Dactyloctenium aegyptium, Datura stramonium, Daucus carota, Digera arvensis, Digitaria sanguinalis, Dinebra retroflexa, Echinochola colonum, Echinochola crusgalli, Eclipta alba, Eichhornia crassipes, Elephantopus scaber, Eleusine indica, Eragrostis major, Euphorbia geniculata, Euphorbia hirta, Fimbristylis miliacea, Fumaria indica, Gynandropsis gynandra, Heliotropium indicum, Indigofera glandulosa, Ipomea aquatica, Lantana camara, Lathyrus aphaca, Launaea asplenifolia, Launaea nudicaulis, Leucas aspera, Marsilea quadrifoliata, Medicago denticulate, Mimosa pudica, Melilotus alba, Melilotus indica, Ocimum canum, Oenothera biennis, Opuntia dillenil, Orobanche ramosa, Oryza longistaminata, Oryza sativa, Oxalis corniculata, Oxalis latifolia, Parthenium hysterophorus, Paspalum sanguinale, Phalaris minor, Phyllanthus niruri, Physalis minima, Polypogon monspeliensis, Portulaca oleracea, Prosopis juliflora, Rumex dentatus, Saccharum spontaneum, Stearia glauca, Seteria viridis, Sida spinosa, Silene antirrhina, Sisymbrium irio, Solanum nigrum, Solanum surattense, Sonchus oleraceous, Sorghum halepense, Spergula arvensis, Sphenocleazeylanica Gaertn, Striga asiatica, Tagetes minuta, Trianthema monogyna, Trianthema portulacastrum, Tribulus terrestris, Trigonelia polycerata, Vernonia cinerea, Vicia sativa and Xanthium strumarium.
[CLAIM 13]. The synergistic herbicidal composition according to any of the preceding claims, wherein composition is to be applied as post emergence and at 10 to 30 days after sowing of crops.
| # | Name | Date |
|---|---|---|
| 1 | 201621017889-PROOF OF ALTERATION [11-04-2025(online)].pdf | 2025-04-11 |
| 1 | 201621017889-RELEVANT DOCUMENTS [26-06-2022(online)].pdf | 2022-06-26 |
| 1 | Power of Attorney [23-05-2016(online)].pdf | 2016-05-23 |
| 2 | 201621017889-RELEVANT DOCUMENTS [26-06-2022(online)].pdf | 2022-06-26 |
| 2 | 201621017889-US(14)-HearingNotice-(HearingDate-15-04-2021).pdf | 2021-10-18 |
| 2 | Form 5 [23-05-2016(online)].pdf | 2016-05-23 |
| 3 | 201621017889-CORRESPONDENCE(IPO)-(CERTIFIED COPY)-(23-09-2021).pdf | 2021-09-23 |
| 3 | 201621017889-US(14)-HearingNotice-(HearingDate-15-04-2021).pdf | 2021-10-18 |
| 3 | Form 3 [23-05-2016(online)].pdf | 2016-05-23 |
| 4 | Description(Provisional) [23-05-2016(online)].pdf | 2016-05-23 |
| 4 | 201621017889-REQUEST FOR CERTIFIED COPY [16-09-2021(online)].pdf | 2021-09-16 |
| 4 | 201621017889-CORRESPONDENCE(IPO)-(CERTIFIED COPY)-(23-09-2021).pdf | 2021-09-23 |
| 5 | 201621017889-REQUEST FOR CERTIFIED COPY [16-09-2021(online)].pdf | 2021-09-16 |
| 5 | 201621017889-POWER OF ATTORNEY-(13-06-2016).pdf | 2016-06-13 |
| 5 | 201621017889-IntimationOfGrant22-05-2021.pdf | 2021-05-22 |
| 6 | 201621017889-PatentCertificate22-05-2021.pdf | 2021-05-22 |
| 6 | 201621017889-IntimationOfGrant22-05-2021.pdf | 2021-05-22 |
| 6 | 201621017889-FORM 5-(13-06-2016).pdf | 2016-06-13 |
| 7 | 201621017889-PatentCertificate22-05-2021.pdf | 2021-05-22 |
| 7 | 201621017889-FORM 3-(13-06-2016).pdf | 2016-06-13 |
| 7 | 201621017889-AMMENDED DOCUMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 8 | 201621017889-AMMENDED DOCUMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 8 | 201621017889-FORM 1-(13-06-2016).pdf | 2016-06-13 |
| 8 | 201621017889-FORM 13 [29-04-2021(online)].pdf | 2021-04-29 |
| 9 | 201621017889-CORRESPONDENCE-(13-06-2016).pdf | 2016-06-13 |
| 9 | 201621017889-FORM 13 [29-04-2021(online)].pdf | 2021-04-29 |
| 9 | 201621017889-MARKED COPIES OF AMENDEMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 10 | 201621017889-MARKED COPIES OF AMENDEMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 10 | 201621017889-Written submissions and relevant documents [29-04-2021(online)].pdf | 2021-04-29 |
| 10 | Description(Complete) [19-05-2017(online)].pdf_454.pdf | 2017-05-19 |
| 11 | 201621017889-ABSTRACT [30-11-2020(online)].pdf | 2020-11-30 |
| 11 | 201621017889-Written submissions and relevant documents [29-04-2021(online)].pdf | 2021-04-29 |
| 11 | Description(Complete) [19-05-2017(online)].pdf | 2017-05-19 |
| 12 | 201621017889-ABSTRACT [30-11-2020(online)].pdf | 2020-11-30 |
| 12 | 201621017889-CLAIMS [30-11-2020(online)].pdf | 2020-11-30 |
| 12 | 201621017889-FORM 18 [08-01-2018(online)].pdf | 2018-01-08 |
| 13 | 201621017889-FORM-26 [06-04-2018(online)].pdf | 2018-04-06 |
| 13 | 201621017889-FER_SER_REPLY [30-11-2020(online)].pdf | 2020-11-30 |
| 13 | 201621017889-CLAIMS [30-11-2020(online)].pdf | 2020-11-30 |
| 14 | 201621017889-FER.pdf | 2020-06-02 |
| 14 | 201621017889-FER_SER_REPLY [30-11-2020(online)].pdf | 2020-11-30 |
| 14 | 201621017889-OTHERS [30-11-2020(online)].pdf | 2020-11-30 |
| 15 | 201621017889-FER.pdf | 2020-06-02 |
| 15 | 201621017889-OTHERS [30-11-2020(online)].pdf | 2020-11-30 |
| 16 | 201621017889-FER.pdf | 2020-06-02 |
| 16 | 201621017889-FER_SER_REPLY [30-11-2020(online)].pdf | 2020-11-30 |
| 16 | 201621017889-FORM-26 [06-04-2018(online)].pdf | 2018-04-06 |
| 17 | 201621017889-FORM 18 [08-01-2018(online)].pdf | 2018-01-08 |
| 17 | 201621017889-FORM-26 [06-04-2018(online)].pdf | 2018-04-06 |
| 17 | 201621017889-CLAIMS [30-11-2020(online)].pdf | 2020-11-30 |
| 18 | 201621017889-FORM 18 [08-01-2018(online)].pdf | 2018-01-08 |
| 18 | Description(Complete) [19-05-2017(online)].pdf | 2017-05-19 |
| 18 | 201621017889-ABSTRACT [30-11-2020(online)].pdf | 2020-11-30 |
| 19 | 201621017889-Written submissions and relevant documents [29-04-2021(online)].pdf | 2021-04-29 |
| 19 | Description(Complete) [19-05-2017(online)].pdf | 2017-05-19 |
| 19 | Description(Complete) [19-05-2017(online)].pdf_454.pdf | 2017-05-19 |
| 20 | 201621017889-CORRESPONDENCE-(13-06-2016).pdf | 2016-06-13 |
| 20 | 201621017889-MARKED COPIES OF AMENDEMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 20 | Description(Complete) [19-05-2017(online)].pdf_454.pdf | 2017-05-19 |
| 21 | 201621017889-FORM 13 [29-04-2021(online)].pdf | 2021-04-29 |
| 21 | 201621017889-FORM 1-(13-06-2016).pdf | 2016-06-13 |
| 21 | 201621017889-CORRESPONDENCE-(13-06-2016).pdf | 2016-06-13 |
| 22 | 201621017889-AMMENDED DOCUMENTS [29-04-2021(online)].pdf | 2021-04-29 |
| 22 | 201621017889-FORM 1-(13-06-2016).pdf | 2016-06-13 |
| 22 | 201621017889-FORM 3-(13-06-2016).pdf | 2016-06-13 |
| 23 | 201621017889-FORM 3-(13-06-2016).pdf | 2016-06-13 |
| 23 | 201621017889-FORM 5-(13-06-2016).pdf | 2016-06-13 |
| 23 | 201621017889-PatentCertificate22-05-2021.pdf | 2021-05-22 |
| 24 | 201621017889-FORM 5-(13-06-2016).pdf | 2016-06-13 |
| 24 | 201621017889-IntimationOfGrant22-05-2021.pdf | 2021-05-22 |
| 24 | 201621017889-POWER OF ATTORNEY-(13-06-2016).pdf | 2016-06-13 |
| 25 | 201621017889-POWER OF ATTORNEY-(13-06-2016).pdf | 2016-06-13 |
| 25 | 201621017889-REQUEST FOR CERTIFIED COPY [16-09-2021(online)].pdf | 2021-09-16 |
| 25 | Description(Provisional) [23-05-2016(online)].pdf | 2016-05-23 |
| 26 | Form 3 [23-05-2016(online)].pdf | 2016-05-23 |
| 26 | Description(Provisional) [23-05-2016(online)].pdf | 2016-05-23 |
| 26 | 201621017889-CORRESPONDENCE(IPO)-(CERTIFIED COPY)-(23-09-2021).pdf | 2021-09-23 |
| 27 | Form 5 [23-05-2016(online)].pdf | 2016-05-23 |
| 27 | Form 3 [23-05-2016(online)].pdf | 2016-05-23 |
| 27 | 201621017889-US(14)-HearingNotice-(HearingDate-15-04-2021).pdf | 2021-10-18 |
| 28 | Form 5 [23-05-2016(online)].pdf | 2016-05-23 |
| 28 | 201621017889-RELEVANT DOCUMENTS [26-06-2022(online)].pdf | 2022-06-26 |
| 28 | Power of Attorney [23-05-2016(online)].pdf | 2016-05-23 |
| 29 | 201621017889-PROOF OF ALTERATION [11-04-2025(online)].pdf | 2025-04-11 |
| 29 | Power of Attorney [23-05-2016(online)].pdf | 2016-05-23 |
| 1 | searchE_01-06-2020.pdf |