Abstract: The present disclosure relates to a fungicidal composition containing azoxystrobin and tricyclazole, wherein the ratio of the amount of azoxystrobin to the amount of tricyclazole ranges from 1: 1 to 1: 9. The present disclosure further provides a fungicidal formulation containing the fungicidal composition, in an amount ranging from 5 to 95 % of the total weight of the formulation and at least one excipient, in an amount ranging from 5 to 95 % of the total weight of the formulation, selected from the group consisting of carriers, dispersing agents, wetting agents, surfactants, stabilizers, thickeners, binders, defoamers, anti-caking agents, anti-freezing agents and optionally vehicles. The formulation is in at least one dosage form selected from the group consisting of water dispersible granules, wettable powder and suspension concentrate. The present disclosure also relates to a process for the preparation of the fungicidal composition.
DESC:FIELD
The present disclosure relates to a fungicidal composition.
BACKGROUND
Azoxystrobin is a fungicide belonging to the strobilurin class of fungicides. Azoxystrobin is a protectant, curative, eradicant, translaminar and systemic fungicide. Azoxystrobin inhibits spore germination, mycelial growth and shows antisporulant activity. Azoxystrobin is used to control fungal diseases in a wide range of field crops, fruits, nuts, vegetables, ornamentals and the like. Azoxystrobin possesses a broad spectrum of antifungal activity. It has the ability to protect against the four big groups of fungal diseases i.e. Ascomycota: Septoria; Deuteromycota: Pyricularia (rice harvesting); Basidiomycota: Stripe rust; and Oomycota: Water mould (grape harvesting).
Azoxystrobin is widely used in farming, particularly wheat farming. More frequent use of azoxystrobin includes early and late blights (Phytophthora infestans and Alternaria solani) of potatoes and tomatoes, downy mildew (Plasmopara viticola) and black rot (Guignardia bidwellii) of vines, downy mildew (Pseudoperonospora cubensis) of cucurbits, scab (Venturia inaequalis) of apples, Sigatoka (Mycosphaerella spp.) of bananas and melanose (Diaporthe citri) of citrus. Azoxystrobin is also used for foliar application and for seed treatment.
IUPAC name of azoxystrobin is Methyl (2E)-2-{2-[6-(2-cyanophenoxy) pyrimidin-4-yloxy] phenyl}-3-methoxyacrylate. The structure of azoxystrobin is given herein below as Formula 1.
Formula 1
Tricyclazole is a fungicide belonging to the triazole class of fungicides. Tricyclazole is a systemic fungicide for protecting rice. Tricyclazole is used to control rice blast (Pyricularia oryzae) in transplanted and direct-seeded rice at a dose of 100 g/ha. Tricyclazole is applied in the form of a flat drench, transplant root soak, and foliar application. One or two applications by one or more of these methods gives a season-long control of the disease in rice. The IUPAC name of tricyclazole is 5-Methyl-1, 2, 4-triazolo [3, 4-b] [1, 3] benzothiazole. The structure of tricyclazole is given herein below as Formula 2.
Formula 2
Two or more fungicides are often combined to get an additive effect of their fungicidal activities. Fungicidal compositions with combination of azoxystrobin with difenoconazole, tricyclazole with difenoconazole, and trifloxystrobin with tricyclazole are known as fungicidal mixtures. However, a need still exists for an alternative fungicidal combination which provides enhanced fungicidal activity.
Accordingly, the present disclosure provides a fungicidal composition which demonstrates enhanced fungicidal activity due to synergistic effect.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a fungicidal composition.
Yet another object of the present disclosure is to provide a fungicidal composition demonstrating synergistic activity.
Still another object of the present disclosure is to provide a fungicidal formulation comprising the fungicidal composition.
Yet another object of the present disclosure is to provide a process for the preparation of the fungicidal formulation.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure provides a fungicidal composition containing azoxystrobin and tricyclazole, wherein the ratio of the amount of azoxystrobin to the amount of tricyclazole ranges from 1: 1 to 1: 9. The present disclosure further provides a fungicidal formulation containing the afore-stated composition, in an amount ranging from 5 to 95 % of the total weight of the formulation and at least one excipient, in an amount ranging from 5 to 95 % of the total weight of the formulation, selected from the group consisting of carriers, dispersing agents, wetting agents, surfactants, stabilizers, thickeners, binders, defoamers, anti-caking agents, anti-freezing agents and optionally vehicles. Typically, the formulation is in at least one dosage form selected from the group consisting of water dispersible granules, wettable powder and suspension concentrate. The present disclosure still further provides a process for the preparation of the fungicidal composition.
DETAILED DESCRIPTION
The disclosure will now be described with reference to the accompanying embodiments which do not limit the scope and ambit of the disclosure. The description provided is purely by way of example and illustration.
The embodiments herein and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the embodiments herein.
The present disclosure, in one aspect, provides a fungicidal composition containing azoxystrobin and tricyclazole in a ratio ranging from 1: 1 to 1: 9. The inventors of the present disclosure surprisingly found that the mixture of azoxystrobin and tricyclazole in the afore-mentioned range demonstrates synergistic action in the prevention and control of plant diseases related to fungal infestations. The phenomenon exhibited by a mixture of two or more agents to mutually affect each other and display an activity that is greater than the sum of their individual activities is designated as synergism.
The ratio of the amount of azoxystrobin to the amount of tricyclazole in the fungicidal composition depends on sensitivity and resistance of the plants, time of application, climatic conditions and soil conditions.
The synergistic fungicidal composition of the present disclosure can be used as a fungicidal agent for the protection of plant and plant products.
In accordance with another aspect, the present disclosure provides a fungicidal formulation containing the afore-stated fungicidal composition and at least one excipient. The total amount of the fungicidal composition in the formulation ranges from 5 to 95 % of the total weight of the formulation whereas the total amount of the excipient(s) in the formulation ranges from 5 to 95 % of the total weight of the formulation. Furthermore, the formulation is in a dosage form selected from the group consisting of water dispersible granules, wettable powder and suspension concentrate.
The formulation of the present disclosure has been found to demonstrate synergistic fungicidal activity. The inventors of the present disclosure have particularly found that the formulation shows good synergistic activity when azoxystrobin is present in an amount ranging from 11 to 35 % of the total weight of the formulation and tricyclazole is present in an amount ranging from 20 to 50 % of the total weight of the formulation.
The excipient is selected from the group consisting of carriers, dispersing agents, wetting agents, surfactants, stabilizers, thickeners, binders, defoamers, anti-caking agents and anti-freezing agents. The present formulation optionally contains vehicles.
The carrier is included to act as a diluent or a bulking agent in the formulation. The carrier is selected from the group consisting of clay, precipitated silica, minerals and talc.
The dispersing agent is used for uniformly dispersing the ingredients, especially the active ingredients, throughout the dosage form. The dispersing agent is selected from the group consisting of sodium lignosulfonate, calcium lignosulfonate, sodium salt of alkyl naphthalene sulfonate, sulfonated aromatic polymer sodium salt, polycarboxylic acid homopolymer, sodium salt of polycarboxylic acid homopolymer, polycarboxylic acid copolymer and sodium salt of polycarboxylic acid copolymer. Typically, the alkyl group has 1 to 20 carbon atoms and the aromatic group in the sulfonated aromatic polymer sodium salt having 1 to 20 carbon atoms.
The wetting agents increase the spreading and penetrating properties of a liquid on and within the formulation by lowering its surface tension. The wetting agent of the present disclosure is selected from the group consisting of non-ionic surfactant, anionic surfactant and combinations thereof. The non-ionic surfactants are alcohol alkoxylates having moles of ethylene oxide in the range of 9 to 15. The anionic surfactants are selected from the group consisting of alkyl naphthalene sulfonate, alkyl naphthalene sulfonate condensate, sodium lauryl sulphate and sodium dodecyl benzene sulfonate. The alkyl group typically comprises 1 to 20 carbon atoms.
The surfactants help in reducing the surface tension and are selected from the group consisting of alkyl ethylene oxide condensates, aryl ethylene oxide condensates, alkyl propylene oxide condensates, aryl propylene oxide condensates, alkylethoxylates and arylethoxylates. Typically, the alkyl and aryl groups have 1 to 20 carbon atoms.
The stabilizers prevent the formulation from microbial spoiling and are selected from the group consisting of propylene glycol, formaldehyde, methyl parahydroxybenzoate, propyl parahydroxybenzoate, 2-bromo-2-nitro-propane-1, 3-diol, sodium benzoate, glutaraldehyde, o-phenylphenol, benzisothiazolinones, 5-chloro-2-methyl-4-isothiazolin-3-one, pentachlorophenol and 2-4-dichlorobenzylalcohol.
The thickeners give a thick consistency to the formulation and are selected from the group consisting of xanthan gum, guar gum, gum arabic and cellulose derivatives. The cellulose derivatives are selected from the group consisting of cellulose acetate, cellulose nitrate, cellulose xanthate, cellulose butyrate, cellulose benzoate, cellulose phthalate, cellulose anthranilate, carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxylethyl cellulose, cellulose sulfate, cellulose phosphate, lignosulfonates, tall oils and terpenes.
The binder binds the ingredients in the composition together to give it the desired strength. The binder is selected from the group consisting of polyvinyl alcohol, polyvinyl-pyrrolidone, polyacrylamides, dextrose, sucrose and lactose.
The defoamer causes prevents foaming of the formulation and is selected from the group consisting of polydimethylsiloxane powder and polydimethylsiloxane liquid.
The anti-caking agent prevents cake formation in the formulation during storage and is selected from the group consisting of clays, precipitated silicas and metal stearates. The metal stearates are selected from the group consisting of zinc stearate, calcium stearate, magnesium stearate and aluminum stearate.
The anti-freezing agent prevents solidification and/ or freezing of the formulation after use or during storage and is selected from the group consisting of ethylene glycol, propylene glycol, glycerin and urea.
The formulation of the present disclosure optionally includes a vehicle to give desired consistency to the formulation or its intermediates. The vehicle used in the present formulation is water.
In one embodiment of the present disclosure, the formulation is in the form of water dispersible granules and includes azoxystrobin and tricyclazole in a ratio ranging from 1: 1 to 1: 9, at least one wetting agent, at least one dispersing agent, at least one defoamer, at least one carrier, at least one vehicle, at least one anti-caking agent and at least one binder. The water dispersible granules have particle size ranging from 100 to 2500 microns.
In another embodiment of the present disclosure the formulation is in the form of wettable powder and includes azoxystrobin and tricyclazole in a ratio ranging from 1: 1 to 1: 9, at least one wetting agent, at least one dispersing agent, at least one carrier and at least one defoamer.
In yet another embodiment of the present disclosure the formulation is in the form of a suspension concentrate and includes azoxystrobin and tricyclazole in a ratio ranging from 1: 1 to 1: 9, at least one vehicle, at least one wetting agent, at least one dispersing agent, at least one defoamer, at least one anti-freezing agent, at least one stabilizer and at least one thickener.
In accordance with yet another aspect, the present disclosure provides a process for the preparation of the fungicidal formulation. The process initially includes admixing the active ingredients to form a mixture of actives. Azoxystrobin and tricyclazole is admixed in a ratio ranging from 1: 1 to 1: 9. In one embodiment, azoxystrobin and tricyclazole are pre-pulverized and then admixed. The resulting mixture of actives is then processed depending on the dosage form of the formulation to be prepared.
Water dispersible granules can be prepared by using any of the processing techniques provided herein below.
In one embodiment, at least one vehicle, at least one wetting agent, at least one dispersing agent, at least one defoamer and at least one carrier are added to and mixed with the mixture of actives, at a mixing speed ranging from 2500 to 3500 rpm for a time period ranging from 20 to 30 minutes to obtain a slurry. The slurry is milled to obtain milled slurry containing particulate matter of size ranging from 1 to 15 microns. The milled slurry is then blended with at least one anti-caking agent, at least one binder, at least one defoamer and at least one vehicle at a blending speed of 1500 rpm to 2500 rpm for a time period ranging from 20 to 40 minutes to obtain a homogenous slurry. Typically, the homogenous slurry contains 35 to 60% solids. The homogenous slurry is dried followed by sieving to obtain water dispersible granules having granule size ranging from 100 to 850 microns. In the present embodiment, the method of drying is selected from the group consisting of spray drying and fluidized bed drying. In this embodiment, the mixture of actives is prepared by admixing non pre-pulverized azoxystrobin and non-pre-pulverized tricyclazole; thereby necessitating the step of milling the slurry.
In another embodiment, at least one vehicle, at least one wetting agent, at least one defoamer, at least one dispersing agent and at least one carrier are added to and mixed with the mixture of actives at a mixing speed of 2500 to 3500 rpm, for a time period ranging from 20 minutes to 30 minutes to obtain a slurry. The slurry is then blended with at least one anti-caking agent, at least one binding agent, at least one defoamer and at least one vehicle at a blending speed ranging from 1500 to 2500 rpm, for a time period ranging from 20 to 40 minutes to obtain a homogenous slurry. The homogenous slurry is then dried followed by sieving to obtain water dispersible granules having granule size ranging from 100 to 500 microns. In the present embodiment, the method of drying is selected from the group consisting of spray drying and fluidized bed drying. In this embodiment, the mixture of actives is prepared by admixing pre-pulverized azoxystrobin and pre-pulverized tricyclazole and consequently the step of milling the slurry is obviated.
In yet another embodiment, the mixture of actives is blended with at least one wetting agent, at least one dispersing agent and at least one carrier at a blending speed ranging from 10 to 25 rpm for a time period ranging from 20 to 40 minutes. The blended mixture is further blended with at least one vehicle and at least one defoamer at a blending speed ranging from 10 to 35 rpm for a time period ranging from 10 to 20 minutes to obtain a dough. The dough is extruded to obtain wet granules which are dried by fluidized bed drying. The dried granules are subjected to sieving to obtain water dispersible granules having granule size ranging from 375 to 2500 microns.
In order to prepare the fungicidal formulation in the form of wettable powder, the mixture of actives is blended with at least one wetting agent, at least one dispersing agent, at least one carrier and at least one defoamer at a blending speed ranging from 10 to 30 rpm and for a time period ranging from 110 to 130 minutes. In this embodiment, the mixture of actives is prepared by admixing pre-pulverized azoxystrobin (1 to 7 microns) and pre-pulverized tricyclazole (1 to 10 microns).
In order to prepare the fungicidal formulation in the form of suspension concentrate at least one vehicle, at least one wetting agent, at least one defoamer and at least one anti-freezing agent are added to and mixed with the mixture of actives at a mixing speed ranging from 2500 to 3500 rpm, for a time period ranging from 30 minutes to 40 minutes to obtain a slurry. The slurry is milled to obtain milled slurry containing particulate matter of size ranging from 1 to 15 microns. The milled slurry is blended with at least one defoamer, at least one stabilizer, at least one thickener, at least one dispersing agent and at least one vehicle at a blending speed of 2500 rpm to 3500 rpm for a time period ranging from 90 to 110 minutes to obtain the suspension concentrate. In this embodiment, the mixture of actives is prepared by admixing non pre-pulverized azoxystrobin and non-pre-pulverized tricyclazole; thereby necessitating the step of milling the slurry.
The present disclosure is further illustrated herein below with the help of the following experiments. The experiments used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of embodiments herein. The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. These laboratory scale experiments can be scaled up to industrial/commercial scale.
Index of ingredients:
Table 1. Index of ingredients
Surfactant A
(wetting agent) sodium alkyl naphthalene sulfonate (Supragil WP from Solvay )
Surfactant B
(wetting agent) sulfonated naphthalene condensate, sodium salt (Supragil MNS 90 from Solvay )
Surfactant C
(dispersing agent) modified ligno sulfonate (from MeadWestvaco)
Surfactant D
(dispersing agent) sodium ligno sulfonate (Borresperse NA)
Surfactant E
(dispersing agent) Sulfonated aromatic polymer sodium salt (Morwet D-425 from Akzonobel)
Surfactant F
(wetting agent) sodium alkyl naphthalene sulfonate (Morwet IP from Akzonobel)
Polymer 1 poly-vinyl alcohol
Polymer 2 composite blend of poly-vinyl pyrrolidone and methyl-vinyl ether/ maleic acid half ester neutralized copolymer (2-butenedioic acid (2Z) - monobutyl ester, polymer with methoxyethene, sodium salt)
Anti-caking agent 1 precipitated silica
Carrier 1 china clay
Carrier 2 ammonium sulfate
Carrier 3 sodium sulfate
Defoamer 1 non-silicone oil (Auchtel Products)
Defoamer 2 poly-dimethyl siloxane (Dow Chemicals)
Adhesive 1/ Binder Dextrose
Stabilizer 1 Benzisothiazolinone
Thickener solution Xanthan gum
Example 1: Process for the preparation of water dispersible granules (Embodiment 1 - Spray drying)
458 g of tricyclazole and 243 g of azoxystrobin were admixed with 1000 g of water along with 20 g of Surfactant F, 2 g of Defoamer 1, 20 g of Surfactant E, 20 g of Surfactant C, 80 g of Surfactant D and 144 g of Carrier 1 in a Repulp tank fitted with a homogenizer manufactured by Remi motors Ltd. The homogenizer was operated at 3000 rpm for 25 minutes to obtain slurry. The slurry was pumped by using double diaphragm pump to a wet mill (Dynomill) at a flow rate of 75 ml/min. The milling was continued till the desired particle size was obtained (1 to 7 micron). The particle size was analyzed by Malvern particle size analyzer. The finely milled slurry was pumped to a blend tank to which 8 g of anticaking agent, 2 g of adhesive 1 and 3 g of Defoamer 1 were added. The mixture was blended at 2000 rpm for 30 minutes to obtain homogeneous slurry. Additional water was added so that solid particulate matter was maintained between 45 to 56 % .The percentage of particulate matter was checked by Loss on drying method.
The slurry was then spray dried in a spray dryer where the inlet temperature was maintained from 200 to 210 °C and the output temperature was maintained from 85 to 95 °C temperature. The granules obtained were sieved through a sieve shaker to obtain granules of size ranging from 100 to 500 microns in diameter. The spray dried spherical granules contained moisture less than 2%.
EXAMPLE 2: Process for the preparation of water dispersible granules (Embodiment 1 - Fluidized bed drying)
358 g of tricyclazole and 143 g of azoxystrobin were admixed with 1000 g of water along with 20 g of Surfactant F, 2 g of Defoamer 1, 40 g of Surfactant E, 20 g of Surfactant C, 80 g of Surfactant D and 124 g of carrier 1 in a Repulp tank fitted with homogenizer manufactured by Remi Motors Ltd. The homogenizer was operated at 3000 rpm for 25 minutes to obtain slurry. The slurry was pumped by using double diaphragm pump to a wet mill (Dynomill) at the flow rate of 75 ml/min. The milling was continued till the desired particle size was obtained (1 to 7 micron). The particle size was analyzed by Malvern particle size analyzer. The finely milled slurry was pumped to a blend tank to which 8 g of anticaking agent, 2 g of polymer 1 and 3 g of Defoamer 1 were added. The slurry blended at 3000 rpm for 30 minutes to obtain homogeneous slurry. Additional water was added so that solid particulate matter was maintained between 40 to 50 %. The percentage of particulate matter was checked by Loss on drying method.
The slurry was spray dried in a fluidized bed equipment containing 100 g of ground tricyclazole and 100 g of ground azoxystrobin as base materials for seeding purpose. The inlet air temperature of the spray nozzle was maintained at 85 to 100 °C, the product temperature was maintained at 35 to 45° C, the outlet temperature of the spray nozzle was maintained at 40 °C during spraying and the final effective temperature of the product was at 70 °C during drying. The resulting dried granules were sieved through a sieve shaker moved at thirty oscillations per minutes to obtain granules having size ranging from 100 to 850 microns. The sieved granules contained moisture less than 2%.
EXAMPLE 3: Process for the preparation of water dispersible granules (Embodiment 2)
458 g of tricyclazole was pulverized using a pulverizer at a feed rate of 10 to 20 g/min to obtain pulverized tricyclazole having particle size in the range of 1 to 7 microns. 243 g of azoxystrobin was pulverized using a pulverizer at a feed rate of 10 to 30 g/min to obtain pulverized azoxystrobin having particle size in the range of 1 to 10 microns. The thus pre-pulverized 458 g of tricyclazole and pre-pulverized 243 g of azoxystrobin was admixed with 1000 g of water along with 25 g of Surfactant F, 2 g of Defoamer 1, 25 g of Surfactant E, 25 g of Surfactant C, 75 g of Surfactant D and 134 g of Carrier 1 in a Repulp tank fitted with a homogenizer manufactured by Remi Motors Ltd. The homongenizer was operated at 3000 rpm for 25 minutes to obtain slurry. This slurry was pumped to a mix blend tank to which 8 g of anticaking agent, 2 g of Adhesive 1 and 3 g of Defoamer 1 were added. The slurry was blended at 2000 rpm for 30 minutes to obtain homogeneous slurry. Additional water was added so that the content of the solid particulate matter was maintained between 45 to 56 %. The percentage of the particulate matter was checked by Loss on drying method.
The slurry was then spray dried in a spray dryer where the inlet temperature was maintained at 200 to 210 °C and the output temperature was maintained at 85 to 95 °C. The granules obtained were sieved through a sieve shaker to obtain granules of size ranging from 100 to 500 microns in diameter. The spray dried spherical granules contained moisture less than 2%.
EXAMPLE 4: Process for the preparation of water dispersible granules (Embodiment 3)
486 g of tricyclazole was milled in a pulverizer at a rate of 100 g/minute. 274 g of azoxystrobin was milled in a pulverizer at a rate of 150 g/minute. The pre-pulverized tricyclazole and pre-pulverized azoxystrobin were blended with 20 g of Surfactant A, 80 g of Surfactant B, 40 g of Surfactant C, 59 g of Carrier 1 and 40 g of carrier 2 for half an hour at 20 rpm after which 80 g of water was added along with 1 g of Defoamer 2 followed by blending for 15 minutes at 30 rpm to obtain dough. The dough was passed through an extruder to obtain wet granules which were dried in fluidized bed equipment. The inlet air temperature was maintained at 75 °C and the product temperature was maintained in the range of 55 to 60 °C. The dried granules were sieved through 10 mesh and 40 mesh sieves in a sieve shaker moved at twenty oscillations per minute. The sieved granules contained moisture less than 2%.
EXAMPLE 5: Process for the preparation of water dispersible granules (Embodiment 3)
458 g of tricyclazole and 243 g of azoxystrobin were mixed in a blender to obtain a mixture of actives. The mixture was pulverized at a rate of 50 g/minute to obtain particle size in the range of 1 to 7 microns. The mixture was blended with 40 g of Surfactant F, 50 g of Surfactant E, 30 g of Surfactant C, 50 g of Surfactant D, 118 g of Carrier 1 and 10 g of polymer 2 for half an hour at 20 rpm. To this, 80 g of water was then added along with 1 g of Defoamer 2 and blended for 15 minutes at 30 rpm to obtain dough. The dough was passed through an extruder equipment to obtain wet granules. The wet granules were dried in a fluidized bed equipment where the inlet air temperature was maintained at 75 °C and the product temperature was maintained in the range of 55 to 60 °C. The dried granules were sieved through 10 mesh and 40 mesh sieves in a sieve shaker moved at twenty oscillations per minute. The sieved granules contained moisture less than 2%.
EXAMPLE 6: Process for the preparation of water dispersible granules (Embodiment 3)
458 g of tricyclazole was milled in a pulverizer at a rate of 100 g/minute. 348 g of azoxystrobin was milled in a pulverizer at a rate of 150 g/minute. The pulverized tricyclazole and azoxystrobin were blended with 50 g of Surfactant F, 50 g of Surfactant E, 34 g of Surfactant C, 49 g of Surfactant D and 10 g of polymer 2 for half an hour at 20 rpm. 80 g of water was then added along with 1 g of Defoamer 2 and blended for 15 minutes at 30 rpm to obtain dough. The dough was passed through an extruder equipment to obtain wet granules. The wet granules were dried in a fluidized bed equipment where the inlet air temperature was maintained at 75 °C and the product temperature was maintained in the range of 55 to 60 °C. The dried granules were sieved through 10 mesh and 40 mesh sieves in a sieve shaker moved at twenty oscillations per minute. The sieved granules contained moisture less than 2%.
Table 2. Composition of formulations (water dispersible granules) prepared by the processes of Example 1 - 6
Ingredient Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Percent on dry basis
Tricyclazole 45.8% 45.8% 45.8% 48.6% 45.8% 45.8%
Azoxystrobin 24.3% 24.3% 24.3% 27.4% 24.3% 34.8%
Surfactant A ---- ---- ---- 2.0% ---- ----
Surfactant B ---- ---- ---- 8.0% ---- ----
Surfactant C 2.0% 2.0% 2.5% 4.0% 3.0% 3.4%
Surfactant D 8.0% 8.0% 7.5% ---- 5.0% 4.9%
Surfactant E 2.0% 4.0% 2.5% ---- 5.0% 5.0%
Surfactant F 2.0% 2.0% 2.5% ---- 4.0% 5.0%
Carrier 1 14.4% 12.4% 13.4% 5.9% 11.8% ----
Carrier 2 ---- ---- ---- 4.0% ---- ----
Anticaking agent 1 0.8% 0.8% 0.8% ---- ---- ----
Adhesive 1 0.2% ---- 0.2% ---- ---- ----
Defoamer 1 0.5% 0.5% 0.5% ---- ---- ----
Defoamer 2 ---- ---- ---- 0.1% 0.1% 0.1%
Polymer 2 ---- 0.2% - ---- ---- 1.0% 1.0%
Characterization:
The formulations prepared by the processes of Examples 1 – 6 (water dispersible granules) were characterized for parameters such as active content, suspensibility, wetting out time, dust content and moisture content. The parameters were determined before and after aging at 54 ? 2?c for 14 days. The results obtained are provided herein below in the form of Table 3.
Table 3. Characterization of formulations (water dispersible granules) prepared by the processes of Example 1 - 6
PARAMETERS Example
1
BA Example
1
AA Example
2
BA Example
2
AA Example
3
BA
Example
3
AA
Example 4
BA Example
4
AA Example
5
BA Example
5
AA Example
6
BA Example
6
AA
Active content (% w/w) Tricyclazole 42.8% 42.7% 42.7% 42.5% 42.9% 42.1% 45.9% 45.8% 42.8% 42.5% 42.9% 42.8%
Active content (% w/w) Azoxystrobin 22.8% 22.6% 22.7% 22.6% 22.8% 22.1% 26.0% 25.9% 22.7% 22.5% 32.7% 32.6%
Suspensibility %w/w 88.6% 88.2% 85.1% 84.3% 81.6% 79.2% 84.22% 84.17% 89.51% 87.13% 85% 82.09%
Wetting out time 3 sec 2 sec 7 sec 8 sec 3 sec 2 sec 3 sec 2 sec 2 sec 3 sec 2 sec 3 sec
Dust content 3 mg 3 mg 7 mg 8 mg 3 mg 3 mg 1 mg 1 mg 1 mg 1 mg 1 mg 1 mg
Moisture content (%w/w) 1.8 1.7 1.9 1.7 1.8 1.7 1.7 1.6 1.5 1.4 1.7 1.6
*BA: Before Aging; *AA: After Aging
EXAMPLE 7: Process for the preparation of wettable powder
458 g of tricyclazole was pulverized using a pulverizer at a feed rate of 10 to 20 g/min to obtain pulverized tricyclazole having particle size in the range of 1 to 7 micron. 243 g of azoxystrobin was pulverized in a jet mill at a feed rate of 10 to 30 g/min to obtain pulverized azoxystrobin having particle size in the range of 1 to 10 microns. Pulverized azoxystrobin and tricyclazole were admixed in a blender along with 50 g of Surfactant A, 80 g of Surfactant B, 40 g of Surfactant D, 128 g of Carrier 1 and 1 g of defoamer 2 in a ribbon blender and blended for 2 hours at 20 rpm to give a homogeneous wettable powder meeting various quality parameters.
Table 4. Composition of wettable powder
Ingredients Example 7
percent on dry basis
Tricyclazole 45.8%
Azoxystrobin 24.3%
Surfactant A 5.0%
Surfactant B 8.0%
Surfactant D 4.0%
Carrier 1 12.8%
Defoamer 2 0.1%
Characterization:
The wettable powder was characterized for parameters such as active content, suspensibility, wetting out time, dust content and moisture content. The parameters were determined before and after aging at 54 ? 2?c for 14 days. The results obtained are provided herein below in the form of Table 5.
Table 5. Characterization of wettable powder
PARAMETERS Example 7
Before Aging Example 7
After Aging
Active content (% w/w) tricyclazole 43.1% 42.8%
Active content (% w/w) Azoxystrobin 22.9% 22.6%
Suspensibility (%w/w) 86.07% 85.14%
Wetting out time 45 sec 40 sec
EXAMPLE 8: Process for the preparation of suspension concentrate
232 g of tricyclazole and 121 g of azoxystrobin was admixed to form a mixture of actives. To this, 300 g of water along with 10 g of Surfactant A, 2.5 g of Defoamer 2 and 100 g of propylene glycol as an anti-freezing agent was added in Repulp tank fitted with homogenizer manufactured by Remi Motors Ltd. The homogenizer was operated at 3000 rpm for 35 minutes to obtain slurry. The slurry was pumped by using double diaphragm pump to a wet mill (Dynomill) at a flow rate of 50 ml/min. The milling was continued till the desired particle size was obtained (1 to 3 micron). Particle size was analyzed by Malvern particle size analyzer. The finely milled slurry was pumped to mix blend tank where 2.5 g of Defoamer 2, 3 g of Stabilizer and 150 g of Thickener solution, 30 g of Surfactant E and 49 g of water were added. The mixture in the mix blend tank was operated at 3000 rpm for 100 minutes to obtain homogeneous slurry.
Table 6. Composition of the suspension concentrate
Ingredient Example 8
percent on dry basis
Tricyclazole 23.2%
Azoxystrobin 12.1%
Surfactant E 3.0%
Surfactant A 1.0%
Propylene glycol 10.0%
Thickener 0.3%
Stabilizer 0.1%
Characterization:
The suspension concentrate was characterized for parameters such as active content and suspensibility. The parameters were determined before and after aging at 54 ? 2?c for 14 days. The results obtained are provided herein below in the form of Table 7.
Table 7. Characterization of suspension concentrate
PARAMETERS Example 8
Before Aging Example 8
After Aging
Active content (% w/w)
Tricyclazole 21.8% 21.5%
Active content (%w/w) Azoxystrobin 11.5% 11.3%
Suspensibility %w/w 93.2% 92.8%
BIO-EFFICACY STUDIES:
The water dispersible granules, wettable powder and suspension concentrate as prepared by using the afore-stated processes were subjected to bio-efficacy studies; details about the same are provided herein below.
Crop : Rice
Variety : MTU-1010
Time of applications : 1st on 45 DAT, 2nd on 60 DAT and 3rd at 75 DAT
Disease Observed : Blast, Sheath blight and False smut
Methodology
The treatments using the afore-stated formulations were imposed at 45 days after transplanting and the second round of spraying was given 15 days after the first spray and third round at 15 days after the second spray. A plot size of 8 x 5 m2 was taken and the spray volume for each plot was 2 L. Disease severity in the plants after treatment was observed 7, 15 and 25 days after cessation of the treatment. Effect of the formulations on diseases such as sheath blight, blast and false smut was evaluated as follows.
Leaf Blast:
The percent disease severity was determined using the following IRRI scale. 25 leaves per replication and grade was observed using the following scale. Leaf Blast Severity was calculated using the formula given below:
Leaf blast Severity = (10 x N1) + (20 x N3) + (40 x N5) + (70 x N7) + (100 x N9)
_____________________________________________
Total Number of leaves Observed
Where: N1 – N9 = Number of leaves with scores 1-9
Scale - Observe at maximum tillering stage
Score Symptoms
0 No visible lesions
1 Small brown specs of pin point size or larger brown specks without sporulating center
3 Small, roundish to slightly elongated necrotic sporulating spots, about 1-2 mm in diameter with a distinct brown margin or yellow halo
5 Narrow or slightly elliptical lesions, 1-2 mm in breadth, more than 3 mm long with a brown margin
7 Broad spindle shaped lesion with yellow, brown or purple margin
9 Rapidly coalescing small, whitish, grayish or bluish lesions without distinct margins
Sheath blight:
Sheath blight severity was calculated using the formula given below:
PDI = Sum of all disease Ratings X 100
Total Number of ratings x Maximum Disease grade
Grade Description
0 No Incidence
1 Vertical spread of the lesions up to 20% of plant height
3 Vertical spread of the lesions up to 21-30% of plant height
5 Vertical spread of the lesions up to 31-45% of plant height
7 Vertical spread of the lesions up to 46-65% of plant height
9 Vertical spread of the lesions up to 66-100% of plant height
Results
Disease control: Blast and Sheath blight
• The data in Table 8 shows percent disease severity and percent disease index (PDI) for Blast and Sheath blight for various treatments of Azoxystrobin+Tricyclazole combinations and for individual components Azoxystrobin 25% and Tricyclazole 75%. The disease severity was more in case of untreated control, Azoxystrobin 25% and Tricyclazole 75% plots indicating that the combination product has better activity in controlling the disease-indicating synergistic activity.
• Combination treatments of Azoxystrobin + Tricyclazole (T2, T3, T4, T6 and T7) show disease control at par against and blast and significantly superior to T1 and T5 indicating that at a particular ratio of Azoxystrobin 22.5% + Tricyclazole 42.5% synergism is the best. All the combination treatments comparatively showed better efficacy than individual components Azoxystrobin 25% and Tricyclazole 75%.
Table 8. Effect of different treatments of Azoxystrobin +Tricyclazole on Bioefficacy against Blast, Pyricularia oryzae and sheath blight, Rhizoctonia solani
Treatments Products DOSE (g.ai/Ha) DOSE (g/ml /Ha) Blast Sheath blight
Disease Severity at diff. days interval PDI at diff. days interval
7 15 25 7 15 25
T1 Azoxystrobin 25 + Tricyclazole 45 125+225 500 16.1 18.3 19.8 10 16.1 18.1
T2 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 14.9 16.8 17.6 8.8 14.9 16.7
T3 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 14.7 17.1 18.3 8.9 15.6 16.8
T4 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 14.5 16.4 18.1 9.1 15.8 16.3
T5 Azoxystrobin 32.5 + Tricyclazole 42.5 162.5+212.5 500 16.2 17.9 19.6 10.6 17.1 17.9
T6 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 14.5 17.9 18.1 9.2 15.9 16.9
T7 Azoxystrobin 11.25 + Tricyclazole 21.25 112.5+212.5 1000 13.6 16.1 17.5 9.0 14.8 15.9
T8 Azoxystrobin 25% 125 500 17.1 21.4 27.3 11.2 16.8 18.5
T9 Tricyclazole 75% 225 300 16.9 18.9 21.3 13.9 23.8 27.8
T10 Control 24.8 28.4 33.2 14.3 24.2 30.8
CD 1.3 1.4 1.4 1.0 1.3 1.4
Disease control: False smut
• The data in Table 9 shows percent infected tillers and disease severity for false smut of various treatments of (Azoxystrobin +Tricyclazole) combinations and individual components Azoxystrobin 25% and Tricyclazole 75%. The disease severity was more in case of untreated control, Azoxystrobin 25% and Tricyclazole 75% plots indicating that the combination product has better synergistic effect in controlling the disease.
• Combination treatments of Azoxystrobin + Tricyclazole (T2, T3, T4, T6 and T7) show disease control at par against False smut and significantly superior to T1 and T5 indicating that at a particular ratio of Azoxystrobin 22.5% + Tricyclazole 42.5%, synergism is the best.
• All the combination treatments comparatively showed better efficacy than individual components Azoxystrobin 25% and Tricyclazole 75%.
Yield
Application of different treatments of the combination product (Azoxystrobin +Tricyclazole) significantly affects the yield (Table 9). Among all the treatments, T2, T3, T4, T6 and T7 are at par in terms of yield. All the combinations showed significant yield increase over solo treatments of Azoxystrobin 25% (45.3 q/ha) and Tricyclazole 75% (45.7 q/ha).
Table 9. Effect of different treatments of Azoxystrobin +Tricyclazole on Bio-efficacy against False smut, Ustilaginoidea virens
Treatments Products DOSE (g.ai/Ha) DOSE (g/ml /Ha) Percent infected tillers Disease severity Yield q/Ha
T1 Azoxystrobin 25 + Tricyclazole 45 125+225 500 7.1 9.8 46.2
T2 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 4.9 7.8 49.6
T3 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 5.1 8.1 49.1
T4 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 4.8 7.7 49.8
T5 Azoxystrobin 32.5 + Tricyclazole 42.5 162.5+212.5 500 6.7 9.4 46.6
T6 Azoxystrobin 22.5 + Tricyclazole 42.5 112.5+212.5 500 5.3 8.3 48.2
T7 Azoxystrobin 11.25 + Tricyclazole 21.25 112.5+212.5 1000 4.9 7.9 49.1
T8 Azoxystrobin 25% 125 500 8.3 10.9 45.3
T9 Tricyclazole 75% 225 300 7.6 10.2 45.7
T10 Control 10.1 18 42.8
CD 0.8 1.0 2.2
PHYTOTOXICITY:
Observation recorded on Table 10 shows that different dose combinations of Azoxystrobin +Tricyclazole do not cause any phytotoxic effect on Rice crop.
Table 10: Effect of different treatments on phytotoxicity at 3, 7 and 15 DAA
Treatments Dose
(Form./ acre) Yellowing Necrosis Scorching Epinasty Hyponasty
3
D
A
A 7
D
A
A 15
D
A
A 3
D
A
A 7
D
A
A 15
D
A
A 3
D
A
A 7
D
A
A 15
D
A
A 3
D
A
A 7
D
A
A 15
D
A
A 3
D
A
A 7
D
A
A 15
D
A
A
T1 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 1000 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 500 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T9 300 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
*DAA = Days after Application
CONCLUSION:
Considering the efficacy against all diseases the combination treatment of Azoxystrobin 22.5 + Tricyclazole 42.5 (T2), Azoxystrobin 22.5 + Tricyclazole 42.5 (T3), Azoxystrobin 22.5 + Tricyclazole 42.5 (T4), Azoxystrobin 22.5 + Tricyclazole 42.5 (T5) and Azoxystrobin 11.25 + Tricyclazole 21.25 (T6) showed superior performance as compared to solo treatments of Azoxystrobin 25% and Tricyclazole 75%.
This is attributed to the fact that each component is complementary to each other and thus shows synergism in action. Other two combinations were also found to have better effect on the disease complex and yield than the individual products Azoxystrobin 25% and Tricyclazole 75%.
The foregoing description of the specific embodiments will so fully reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.
TECHNICAL ADVANCES AND ECONOMICAL SIGNIFICANCE
The fungicidal formulation of the present disclosure described herein above has several technical advantages including, but not limited to, the realization of:
• The formulation of the present disclosure comprising azoxystrobin and tricyclazole shows synergistic fungicidal activity.
• The composition and formulation of the present disclosure can be used to inhibit or destroy fungal infestation that occurs on plants or on parts of plants such as fruit, blossom, leaves, stems, tubers and roots.
• The composition or formulation can also be used as dressings in the treatment of plant propagation materials such as seeds, fruits, tubers, grains; and plant cuttings such as those of rice, to provide protection against fungus infections as well as against phytopathogenic fungi that occur in the soil.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values ten percent higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification specific to the contrary.
While considerable emphasis has been placed herein on the components and component parts of the preferred embodiments, it will be appreciated that many embodiments can be made and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. These and other changes in the preferred embodiment as well as other embodiments of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation. ,CLAIMS:1. A fungicidal composition comprising azoxystrobin and tricyclazole, wherein the ratio of the amount of azoxystrobin to the amount of tricyclazole ranges from 1: 1 to 1: 9.
2. A fungicidal formulation comprising:
i. the composition as claimed in claim 1, in an amount ranging from 5 to 95 % of the total weight of the formulation; and
ii. at least one excipient, in an amount ranging from 5 to 95 % of the total weight of the formulation, selected from the group consisting of carriers, dispersing agents, wetting agents, surfactants, stabilizers, thickeners, binders, defoamers, anti-caking agents, anti-freezing agents and optionally vehicles.
3. The formulation as claimed in claim 2, wherein azoxystrobin is present in an amount ranging from 11 to 35 % of the total weight of the formulation and tricyclazole is present in an amount ranging from 20 to 50 % of the total weight of the formulation.
4. The formulation as claimed in claim 2, being in at least one dosage form selected from the group consisting of water dispersible granules, wettable powder and suspension concentrate.
5. The formulation as claimed in claim 2, which includes at least one carrier selected from the group consisting of clay, precipitated silica, minerals and talc.
6. The formulation as claimed in claim 2, which includes at least one dispersing agent selected from the group consisting of sodium lignosulfonate, calcium lignosulfonate, sodium salt of alkyl naphthalene sulfonate, sulfonated aromatic polymer sodium salt, polycarboxylic acid homopolymer, sodium salt of polycarboxylic acid homopolymer, polycarboxylic acid copolymer, sodium salt of polycarboxylic acid copolymer; said alkyl group having 1 to 20 carbon atoms and said aromatic group in the sulfonated aromatic polymer sodium salt having 1 to 20 carbon atoms.
7. The formulation as claimed in claim 2, which includes at least one wetting agent selected from the group consisting of primary and secondary alcohol ethoxylates having moles of ethylene oxide in the range of 9 to 15, sodium alkyl naphthalene sulfonate, sodium alkyl naphthalene sulfonate condensate, sodium lauryl sulphate and sodium dodecyl benzene sulfonate; said alkyl group having 1 to 20 carbon atoms.
8. The formulation as claimed in claim 2, which includes at least one surfactant selected from the group consisting of alkyl ethylene oxide condensates, aryl ethylene oxide condensates, alkyl propylene oxide condensates, aryl propylene oxide condensates, alkylethoxylates and arylethoxylates; said alkyl and aryl groups having 1 to 20 carbon atoms.
9. The formulation as claimed in claim 2, which includes at least one stabilizer selected from the group consisting of propylene glycol, formaldehyde, methyl parahydroxybenzoate, propyl parahydroxybenzoate, 2-bromo-2-nitro-propane-1, 3-diol, sodium benzoate, glutaraldehyde, o-phenylphenol, benzisothiazolinones, 5-chloro-2-methyl-4-isothiazolin-3-one, pentachlorophenol and 2-4-dichlorobenzylalcohol.
10. The formulation as claimed in claim 2, which includes at least one thickener selected from the group consisting of xanthan gum, guar gum, gum arabic and cellulose derivatives; said cellulose derivative being at least one selected from the group consisting of cellulose acetate, cellulose nitrate, cellulose xanthate, cellulose butyrate, cellulose benzoate, cellulose phthalate, cellulose anthranilate, carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxylethyl cellulose, cellulose sulfate, cellulose phosphate, lignosulfonates, tall oils and terpenes.
11. The formulation as claimed in claim 2, which includes at least one binder selected from the group consisting of polyvinyl alcohol, polyvinyl-pyrrolidone, polyacrylamides, dextrose, sucrose and lactose.
12. The formulation as claimed in claim 2, which includes at least one defoamer selected from the group consisting of polydimethylsiloxane powder and polydimethylsiloxane liquid.
13. The formulation as claimed in claim 2, which includes at least one anti-caking agent selected from the group consisting of clays, precipitated silicas and metal stearates; said metal stearate being at least one selected from the group consisting of zinc stearate, calcium stearate, magnesium stearate and aluminum stearate.
14. The formulation as claimed in claim 2, which includes at least one anti-freezing agent selected from the group consisting of ethylene glycol, propylene glycol, glycerin and urea.
15. The formulation as claimed in claim 2, which includes at least one vehicle which is water.
16. The formulation as claimed in claim 2, comprising azoxystrobin and tricyclazole, at least one wetting agent, at least one dispersing agent, at least one defoamer, at least one carrier, at least one vehicle, at least one anti-caking agent and at least one binder; said formulation being in the form of water dispersible granules having granule size ranging from 100 to 2500 microns.
17. The formulation as claimed in claim 2, comprising azoxystrobin and tricyclazole, at least one wetting agent, at least one dispersing agent, at least one carrier and at least one defoamer; said formulation being in the form of wettable powder.
18. The formulation as claimed in claim 2, comprising azoxystrobin and tricyclazole, at least one vehicle, at least one wetting agent, at least one dispersing agent, at least one defoamer, at least one anti-freezing agent, at least one stabilizer and at least one thickener; said formulation being in the form of a suspension concentrate.
19. A process for the preparation of a fungicidal formulation; said process comprising the following steps:
i. admixing, optionally pre-pulverized, azoxystrobin and optionally pre-pulverized, tricyclazole in a ratio ranging from 1: 1 to 1: 9 to obtain a mixture of actives;
ii. processing said mixture of actives by a set of process steps to obtain the fungicidal formulation having a dosage form selected from the group consisting of water dispersible granules, wettable powder and suspension concentrate; said process steps selected from the group consisting of:
a. adding to and mixing with the mixture of actives, at least one vehicle, at least one wetting agent, at least one dispersing agent, at least one defoamer and at least one carrier at a mixing speed ranging from 2500 to 3500 rpm for a time period ranging from 20 to 30 minutes to obtain a slurry; milling the slurry to obtain a milled slurry containing particulate matter of size ranging from 1 to 15 microns; blending with the milled slurry, at least one anti-caking agent, at least one binder, at least one defoamer and at least one vehicle at a blending speed of 1500 rpm to 2500 rpm for a time period ranging from 20 to 40 minutes to obtain a homogenous slurry; drying the homogenous slurry followed by sieving to obtain water dispersible granules having granule size ranging from 100 to 850 microns;
b. adding to and mixing with the mixture of actives, at least one vehicle, at least one wetting agent, at least one defoamer, at least one dispersing agent and at least one carrier at a mixing speed of 2500 to 3500 rpm, for a time period ranging from 20 minutes to 30 minutes to obtain a slurry; blending the slurry with at least one anti-caking agent, at least one binding agent, at least one defoamer and at least one vehicle at a blending speed ranging from 1500 to 2500 rpm, for a time period ranging from 20 to 40 minutes to obtain a homogenous slurry; drying the homogenous slurry followed by sieving to obtain water dispersible granules having granule size ranging from 100 to 500 microns;
c. blending the mixture of actives with at least one wetting agent, at least one dispersing agent and at least one carrier at a blending speed ranging from 10 to 25 rpm for a time period ranging from 20 to 40 minutes and at least one vehicle and at least one defoamer at a blending speed ranging from 10 to 35 rpm for a time period ranging from 10 to 20 minutes to obtain a dough; extruding the dough to obtain wet granules; drying the wet granules followed by sieving to obtain water dispersible granules having granule size ranging from 375 to 2500 microns;
d. blending the mixture of actives with at least one wetting agent, at least one dispersing agent, at least one carrier and at least one defoamer at a blending speed ranging from 10 to 25 rpm for a time period ranging from 110 to 130 minutes to obtain wettable powder; and
e. adding to and mixing with the mixture of actives, at least one vehicle, at least one wetting agent, at least one defoamer, at least one anti-freezing agent at a mixing speed ranging from 2500 to 3500 rpm, for a time period ranging from 30 minutes to 40 minutes to obtain a slurry; milling the slurry to obtain milled slurry containing particulate matter of size ranging from 1 to 15 microns; blending with the milled slurry, at least one defoamer, at least one stabilizer, at least one thickener, at least one dispersing agent and at least one vehicle at a blending speed of 2500 rpm to 3500 rpm for a time period ranging from 90 to 110 minutes to obtain suspension concentrate.
20. The process as claimed in claim 19, wherein the step of drying in process steps (a) and (b) is selected from the group consisting of spray drying and fluidized bed drying and the step of drying in process step (c) is fluidized bed drying.
21. The formulation as claimed in claim 2, for the treatment of leaf blast, sheath blight and false smut in plants and plant products.
| # | Name | Date |
|---|---|---|
| 1 | 3334-MUM-2014-FER.pdf | 2021-10-03 |
| 1 | 3334-MUM-2014-FORM 1(28-10-2014).pdf | 2014-10-28 |
| 2 | 3334-MUM-2014-RELEVANT DOCUMENTS [24-02-2021(online)].pdf | 2021-02-24 |
| 2 | 3334-MUM-2014-CORRESPONDENCE(28-10-2014).pdf | 2014-10-28 |
| 3 | FORM-3.pdf | 2018-08-11 |
| 3 | Description(Complete) [16-10-2015(online)].pdf | 2015-10-16 |
| 4 | Indofil-PS-RKD-Draft Final Azo + Tricy.pdf | 2018-08-11 |
| 4 | 3334-MUM-2014-CORRESPONDENCE-(26-04-2016).pdf | 2016-04-26 |
| 5 | Form 18 [05-12-2016(online)].pdf | 2016-12-05 |
| 5 | INDOFIL.pdf | 2018-08-11 |
| 6 | PRE GRANT OPPOSITION DOCUMENT [02-02-2017(online)].pdf | 2017-02-02 |
| 6 | PREGRANT OPPOSITION [02-02-2017(online)].pdf | 2017-02-02 |
| 7 | PRE GRANT OPPOSITION DOCUMENT [02-02-2017(online)].pdf | 2017-02-02 |
| 7 | PREGRANT OPPOSITION [02-02-2017(online)].pdf | 2017-02-02 |
| 8 | Form 18 [05-12-2016(online)].pdf | 2016-12-05 |
| 8 | INDOFIL.pdf | 2018-08-11 |
| 9 | 3334-MUM-2014-CORRESPONDENCE-(26-04-2016).pdf | 2016-04-26 |
| 9 | Indofil-PS-RKD-Draft Final Azo + Tricy.pdf | 2018-08-11 |
| 10 | FORM-3.pdf | 2018-08-11 |
| 10 | Description(Complete) [16-10-2015(online)].pdf | 2015-10-16 |
| 11 | 3334-MUM-2014-RELEVANT DOCUMENTS [24-02-2021(online)].pdf | 2021-02-24 |
| 11 | 3334-MUM-2014-CORRESPONDENCE(28-10-2014).pdf | 2014-10-28 |
| 12 | 3334-MUM-2014-FORM 1(28-10-2014).pdf | 2014-10-28 |
| 12 | 3334-MUM-2014-FER.pdf | 2021-10-03 |
| 1 | 3334searchstrategyE_22-01-2021.pdf |