Fungicidal compound, fungicidal composition, use of same, plant seed, and methods for controlling disease or one or more phytopathogenic fungi, for treating seed, and for controlling damage and / or yield loss caused by one or more phytopathogenic fungi
Patent Information
- Application Number
- PCT/BR2026/050066
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2025-02-21
- Filing Date
- 2026-02-12
- Publication Date
- 2026-08-27
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Figure BR2026050066_27082026_PF_FP_ABST
Abstract
Description
FUNGICIDAL COMPOUND, FUNGICIDAL COMPOSITION, USE THEREOF, PLANT SEED AND METHODS FOR CONTROLLING A DISEASE OR ONE OR MORE PHYTOPATHOGENIC FUNGI, FOR SEED TREATMENT AND FOR CONTROLLING DAMAGE AND / OR YIELD LOSS CAUSED BY ONE OR MORE PHYTOPATHOGENIC FUNGI. TECHNICAL FIELD
[0001] The invention relates to the technical field of agrochemistry and, in particular, to a fungicidal compound, a fungicidal composition comprising the same, its use in seed protection, plant seed and methods for controlling a disease, for controlling one or more phytopathogenic fungi, for seed treatment and for controlling damage and / or yield loss caused by one or more phytopathogenic fungi. STATE OF THE ART
[0002] Fungal diseases in crops represent a global threat to food security and biodiversity, as fungi are highly resistant microorganisms. Although this problem is not new, fungal diseases still pose a widespread threat to various plant species, especially wheat, corn, rice, potatoes, and soybeans. Environmental, genetic, and biological factors directly or indirectly affect plant vitality.
[0003] Nanotechnology is a field of science that studies the manipulation of matter at the atomic and molecular levels. In agriculture, nanotechnology has been applied in various areas, such as the development of pesticides and fungicides.
[0004] Polyoxometalates (POMs) of some transition metals, such as tungsten, vanadium, molybdenum, and niobium, are attracting considerable interest due to their unique structural properties and peculiar chemical reactivities. These properties open new avenues for the development of multifunctional materials for applications in various fields, such as agrochemicals, medicine, and materials science.
[0005] The polyoxometalate family can be divided into two groups: the isopolyanions, having the general formula ([MxOy] aThe POM cluster is composed of hexa- and deca-metal ions, which have a configuration similar to the Lindqvist type, and heteropolyanions ([XzMxOy]^). There are no chemical limitations for X and M by definition. The element X is called primary, central, or heteroatom. In general, any element can participate as element X in a POM cluster, provided there are no strict physical restrictions for this position. On the other hand, elements M are called secondary, peripheral, or additional.
[0006] Among POMs, polyoxoniobates are less explored when compared to polyoxotungstates, polyoxovanadates, and polyoxomolybdates, which are easily formed over a wide pH range simply by acidification. SUMMARY OF THE INVENTION
[0007] The present invention relates to a fungicidal compound that is a polyoxoniobate.
[0008] Optionally, polyoxoniobate is either an isopolyniobate or a heteropolyniobate.
[0009] Optionally, the heteroatom contained in the heteropolyniobate is phosphorus.
[0010] Optionally, polyoxoniobate is combined with copper.
[0011] Optionally, the polyoxoniobate is [Nbn(H2O)n(PO4)n(OH)2n(Oxi)3n] y ' (poly(aqua)phospho-hydroxy-n(oxy)niobate) or [Nb n (H2O)n(PO4)n(OH)n(Oxi)3nCu] x " (copper II poly(aqua)phospho-hydroxy-n(oxy)niobate).
[0012] The present invention is also related to a fungicidal composition comprising the fungicidal compound of the present invention.
[0013] Optionally, the fungicidal composition may also include an agriculturally acceptable carrier.
[0014] Optionally, the agriculturally acceptable vehicle is a polar solvent.
[0015] Alternatively, water is an acceptable agricultural vehicle.
[0016] The present invention is also related to the use of the fungicidal compound or fungicidal composition of the present invention for seed protection against one or more phytopathogenic fungi.
[0017] Optionally, the seed is a legume seed.
[0018] Optionally, the seed can be a soybean seed.
[0019] Optionally, the phytopathogenic fungus is selected from the group consisting of Alternaria, Aspergillus, Albugo, Apiognomonia, Armiilaria, Bipolaris, Botryosphaeria, Blumeriella, Bremia, Blumeria, Basidiophara, Botrytis, Cladosporium, Cochliobolus, Corynespora, Cercospora, Cofietotrichum, Discuta, Didymella, Drechslera, Eisinoem, Eutypa, Erysiphe, Exserohiium, Fusarium, Golovínomyces, Goeodes, Gymnosporangium. Gibberella, Hemileia, Helminthosporium, Leveillula, Macrophomina, Monosporascus, Monilinia, Magnaporthe, Mycosphaerella, Neofabraea, Phakopsora, Phomopsis, Podosphaera, Penícillium, Phaeosphaeria, Pyrenophora, Puccinia, Pythium, Phytophthora, Peronospora, Pseudoperonospora, Pseudocercosporella, Plasmopara, Plasmodiophora, Phoma, Pyricularia, Rhizopus, Ramuiaria, Rhyncosporium, Rhizoctonia, Schizothyrium, Septoria, Scierotinia, Sphaerotheca, Stagonospora, Sclerotium, Tilletia, Tritici, Uncinula, Uromyces. Ustilago, Verticillium, Venturia, Wilsonomyces,
[0020] Optionally, the fungus is of the genus Fusarium.
[0021] Optionally, the fungus is of the species Fusarium pallidoroseum.
[0022] The present invention also relates to a plant seed coated and / or treated with the fungicidal compound or with the fungicidal composition of the present invention.
[0023] Optionally, the plant seed is a legume seed.
[0024] Optionally, the plant seed is a soybean seed.
[0025] The present invention also relates to a method for controlling a disease caused by a phytopathogenic fungus, comprising treating / coating a seed with the fungicidal compound or with the fungicidal composition of the present invention.
[0026] The present invention also relates to a method for controlling one or more phytopathogenic fungi, comprising applying the fungicidal compound or fungicidal composition of the present invention to a seed.
[0027] The present invention also relates to a method for treating seeds against one or more phytopathogenic fungi, comprising the steps of mixing the fungicidal compound or fungicidal composition of the present invention with one or more seeds.
[0028] The present invention also relates to a method for controlling damage and / or yield loss caused by one or more phytopathogenic fungi, comprising the steps of applying the fungicidal compound or fungicidal composition of the present invention to a seed and planting the seed. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 illustrates an MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] calorimetric assay performed during a short exposure period of 6 hours with the compound PNb53.
[0030] Figure 2 illustrates the MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] calorimetric assay performed during a short exposure period of 6 hours with the compound PNb53-C.
[0031] Figure 3 illustrates the MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] calorimetric assay performed during a long 24-hour exposure period of the PNb53 compound.
[0032] Figure 4 illustrates the MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] calorimetric assay performed during a long 24-hour exposure period of the PNb53-C compound.
[0033] Figure 5 illustrates the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) on the incidence of seeds infected by Fusarium pallidoroseum.
[0034] Figure 6 illustrates the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) on the germination percentage of seeds infected (between 87.00 and 94.50%) by Fusarium pallidoroseum.
[0035] Figure 7 shows photographs of the blotter test comparing the effect of soybean seed treatment with fungicides PNb53 and PNb53-C and the standard. Where T1 is the inoculated control, T2 is the standard sample (100 mL p. / 100 kg of seed), T3 is the sample with PNb53 (100 mL p. / 100 kg of seed), T4 is the sample with PNb53 (200 mL p. / 100 kg of seed), T5 is the sample with PNb53 (400 mL p. / 100 kg of seed), T6 is the sample with PNb53-C (100 mL p. / 100 kg of seed), T7 is the sample with PNb53-C (200 mL p. / 100 kg of seed), T8 is the sample with PNb53-C (400 mL p. / 100 kg of seed).
[0036] Figure 8 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PN 53-C) on the Emergence Speed Index (ESI) in a greenhouse test conducted in trays.
[0037] Figure 9 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) on the shoot length of seedlings (cm) in a test conducted in trays in a greenhouse.
[0038] Figure 10 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) on the root length of seedlings (in cm) in a test conducted in trays in a greenhouse.
[0039] Figure 11 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) on the control of Fusarium pallidoroseum during seed germination. The test was carried out in trays in the greenhouse.
[0040] Figure 12 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) to control Fusarium pallidoroseum on the fresh weight of the aerial part and roots of plants grown in trays in the greenhouse.
[0041] Figure 13 shows the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides (Maxim Advanced, PNb53 and PNb53-C) to control Fusarium pallidoroseum on the dry weight of the aerial part and roots of plants grown in trays in the greenhouse.
[0042] Figure 14 shows photographs of the emergence test in trays comparing the effect of treating soybean seeds with the fungicides PNb53 and PNb53-C and the control. On the left is a photograph of the plant and on the right are abnormal and normal specimens, where: T1 is the inoculated control; T2 contains Maxim advanced (100 ml p. / 100 Kg of seed); T3 contains PNb53 (100 mL p. / 100 Kg of seed); T4 contains PNb53 (200 mL p. / 100 Kg of seed); T5 contains PNb53 (400 mL p. / 100 Kg of seed); T6 contains PNb53-C (100 mL p. / 100 Kg of seed); T7 contains PNb53-C (200 mL p. / 100 Kg of seed); T8 contains PNb53-C (400 mL p, / 100 Kg of seed) and T9 is the control without inoculum. DETAILED DESCRIPTION
[0043] The present invention relates to a compound from the polyoxoniobate group. Inventors discovered that polyoxoniobates exhibit fungicidal activity when applied to plant seeds.
[0044] The group of compounds defined here as "polyoxoniobate" should be understood as a class of compounds based on the transition metal Nb. 5+ in a high oxidation state, interconnected by bridging oxygens and containing -oxo groups (O 2- terminals.
[0045] Polyoxoniobates can be further divided into isopolyniobates and heteropolyniobates. Isopolyniobates have chains composed of niobium atoms bonded to oxygen atoms. In the final compound, another type of atom may be found, but these are considered ligands and are not part of the isopolyniobate structure. Heteropolyniobates, on the other hand, have an atom other than niobium in their structure, the heteroatom, which can correspond to practically all elements of the periodic table, with the exception of the noble gases.
[0046] The polyoxoniobates of the present invention can be obtained by any known process, using any niobium compound as starting material, such as, but not limited to, niobium oxide, niobium pentoxide, niobic acid, and niobium phosphate.
[0047] In a particular embodiment of the present invention, the starting material is a niobium phosphate, resulting in a heteropolyniobaium comprising phosphorus heteroatoms in its chain.
[0048] The polyoxoniobates of the present invention can also be combined with cations. In a particular embodiment of the present invention, the polyoxoniobate is combined with copper cations (Cu). 2+ ).
[0049] In a particular embodiment of the present invention, copper cations are obtained from copper salts selected from, but not limited to, the group consisting of copper hydroxide, copper oxychloride, copper chloride, cuprous oxide, copper nitrate, copper sulfate, or tribasic copper sulfate.
[0050] In a preferred embodiment of the present invention, the fungicidal composition comprises [Nbn(H2O)n(PÓ4)n(OH)2n(Oxi)3n] y “ (poly(aqua)phospho-hydroxy-n(oxy)niobate) and / or [Nbn(H2O)n(PO4)n(OH) n (Oxy)3nCu] x '(poly(aqua)phospho-hydroxy-n(oxy)niobate copper II) as active ingredient(s).
[0051] The compound identified by the molecular formula [Nbn(H2O)(PO4)n(OH)2n(Oxi)3n] y ' is also referred to here as “PNb53”.
[0052] The compound identified by the molecular formula [Nbn(H2O)n(PO4)n(OH)n(Oxi)3nCu] x ' is also referred to here as “PNb53-C”.
[0053] The present invention also relates to a fungicidal composition comprising the fungicidal compound(s) defined above.
[0054] In a particular embodiment of the present invention, the fungicidal composition may contain only one polyoxyniobate or any combination of two or more polyoxyniobates, whether isoniobates or heteroniobates.
[0055] The fungicidal compositions of the present invention may further comprise at least one agriculturally acceptable carrier. The expression "agriculturally acceptable carrier" should be understood as; a substance, material or ingredient that is compatible with the active ingredient(s) of the fungicidal composition described herein, at least for the purposes for which said composition will be used, It can be included in the composition to effectively and viably distribute the active ingredient(s) to the seeds. It does not cause any harm to the seed, germinated plant, crop and / or soil to which the composition will be applied.
[0056] The quantitative and qualitative selection of one or more agriculturally acceptable vehicles can be made by a technician in the field based on the intended application of the composition, as well as the active ingredients, based on their knowledge in the area.
[0057] Fungicidal compositions can be used in any conventional form, for example, as a soluble powder, as a concentrate, as a solution, as an emulsion, as granules, or in any other technically feasible form in combination with agriculturally acceptable carriers.
[0058] In a particular embodiment of the present invention, the agriculturally acceptable carrier is a polar solvent. In another preferred embodiment of the present invention, the polar solvent is selected from the group consisting of 1,3-butylene glycol, 2-pyrrolidone, acetone, acetonitrile, an aliphatic alcohol, an aliphatic carboxylic acid alkyl ester, cyclohexanone, di- and triglycols, diacetone alcohol, dialkyl ketone, diethylene glycol, diglylene, DMF, DMSO, ethanol, ethyl acetate, formamide, furfuryl alcohol, gamma-butyrolactone, glycerol, glycofurol, a glycol ether, glycol, hexamethylene glycol, isopropanol, methyl ethyl ketone, N-methylpyrrolidone, pentamethylene glycol, phosphoric acid esters, polyethylene glycol, polyethylene glycols, polyhydroxylated alkanes, propanol, propylene carbonate, propylene glycol, pyrrhidine, pyrrhidine, Sulfolane, tetrahydrofuran, tetramethylene glycol, thiodiglycol and / or triethylene glycol and combinations thereof.In an even more preferable embodiment, the agriculturally acceptable vehicle is water.
[0059] In a particular embodiment of the present invention, the fungicidal composition comprises an effective and non-phytotoxic amount of one or more polyoxoniobates. The expression "effective and non-phytotoxic amount" should be understood as a sufficient quantity of the compound capable of controlling or eliminating a phytopathogenic fungus without resulting in any damage or symptoms of phytotoxicity in the seed to be treated or in the crop obtained therefrom. This quantity may vary depending on the polyoxoniobates included in the fungicidal composition, the fungus to be controlled / eliminated, the type of seed to be treated, as well as the climatic conditions of the planting site. Determining this quantity is within the capabilities of a person skilled in the art with knowledge in the field.
[0060] In a particular embodiment of the present invention, the amount of polyoxoniobate(s) in the fungicidal composition is from 1 to 99% w / w relative to the total weight of the composition. In a preferred embodiment, the amount of polyoxoniobate(s) in the fungicidal composition is from 1 to 50% w / w relative to the total weight of the composition. In a further preferred embodiment, the amount of polyoxoniobate(s) in the fungicidal composition is from 1 to 20% w / w relative to the total weight of the composition. In a further preferred embodiment, the amount of polyoxoniobate(s) in the fungicidal composition is from 5 to 15% w / w relative to the total weight of the composition.
[0061] In a particular embodiment of the present invention, the concentration of the composition is in the range of 10 to 500 g L⁻¹. 1 In a preferred embodiment, the concentration of the composition is in the range of 50 to 200 g.L⁻¹ 1In an even more preferred embodiment, the concentration of the composition is in the range of 75 to 150 g / L. -1 .
[0062] In a particular embodiment of the present invention, the composition has an acidic pH. In a preferred embodiment, the pH of the composition is in the range of 0 to 5. In a further preferred embodiment, the pH of the composition is in the range of 1 to 2.
[0063] The fungicidal composition of the present invention is also stable under normal temperature and pressure conditions, being stable at room temperature (18 to 30°C).
[0064] In a particular embodiment of the present invention, the fungicidal compound and / or the fungicidal composition can be used for seed protection against one or more phytopathogenic fungi.
[0065] In a particular preferred embodiment of the present invention, the seed is a field crop seed, such as, for example, but not limited to, corn, soybean, cotton, tomato, oilseeds, rice, wheat, beet, sugarcane, oats, rye, barley, triticale, beans, chickpeas, lentils, peanuts or peas.
[0066] In a particular preferred embodiment of the present invention, the seed is a legume seed. In a further preferred embodiment, the seed is a soybean seed.
[0067] Os fítopathogênicos a serem controlled / eliminated fungi com o uso da composizione fungicide da presente invenção podem ser qualquer um selecciona dentre o grupo consistindo em Alternaria, Aspergillus, Albugo, Apiognomonia, Armillaria, Bipolaris, Botryosphaeria, Blumeríella, Bremia, Blumeria, Basidiophara, Botrytis, Cladosporium, Cochliobolus, Corynespora, Cercospora, Colletotríchum, Discuta, Didymella, Drechslera, Elsinoë, Eutypa, Erysiphe, Exserohilum, Fusarium, Golovinomyces, Goeodes, Gymnosporangium, Gibberella, Hemileia, Heiminthosporium, Leveillula, Macrophomina, Monosporascus, Monilinia, Magnaporthe, Mycosphaerella, Neofabraea, Phakopsora, Phomopsis, Podosphaera, Penicillium, Phaeosphaeria, Pyrenophora, Puccinia, Pythium, Phytophthora, Peronospora, Pseudoperonospora, Pseudocercosporeila, Plasmopara, Piasmodiophora, Phoma, Pyricularia, Rhizopus, Ramularia, Rhyncosporium, Rhizoctonia, Schizothyrium, Septoria, Sclerotinia, Sphaerotheca, Stagonospora, Sclerotium, Tilletia, Tritici,Uncinula, Uromyces, Ustilago, Verticillium, Venturia, Wilsonomyces,
[0068] In a particular preferred embodiment of the present invention, the fungicidal composition is used against one or more fungi of the genus Fusarium. In an even more preferred embodiment, the fungicidal composition is used against one or more fungi of the genus Fusarium pallidoroseum.
[0069] The treatment / coating of seeds with the fungicidal compound and / or the fungicidal composition of the present invention can be done by any method known in the art. After treatment, the seed presents itself with at least a portion of its outer surface coated and / or treated with the fungicidal compound and / or the fungicidal composition of the present invention, the coating forming a protective nanofilm.
[0070] The term "coated and / or treated" should be understood as the fungicidal compound being primarily on the surface of the seed after application of the same or the fungicidal composition, although a portion of said compound or fungicidal composition may penetrate the seed, depending on the application method.
[0071] Thus, in a particular embodiment of the present invention, the present invention relates to a plant seed coated and / or treated with the fungicidal compound or fungicidal composition described herein.
[0072] In a particular preferred embodiment of the present invention, the plant seed is a seed of a leguminous plant coated and / or treated with the fungicidal compound or fungicidal composition of the present invention. In an even more preferred embodiment, the plant seed is a soybean seed coated and / or treated with the fungicidal compound or fungicidal composition of the present invention.
[0073] The invention also relates to a method for controlling a disease caused by a phytopathogenic fungus, comprising treating a seed with the fungicidal compound or fungicidal composition as described herein.
[0074] The invention also relates to a method for controlling one or more phytopathogenic fungi, comprising applying the fungicidal compound or fungicidal composition described herein to a seed.
[0075] The invention also relates to a method for treating seeds against one or more phytopathogenic fungi, comprising the step of mixing the fungicidal compound or fungicidal composition described herein with one or more seeds.
[0076] The invention also relates to a method for controlling damage and / or yield loss caused by phytopathogenic fungi, comprising the steps of applying the fungicidal compound or fungicidal composition described herein to a seed and planting the seed.
[0077] In a particular embodiment of the present invention, the dose of the fungicidal compound applied in any of the methods described above is generally between 50 and 500 mL / 100 kg of seed. In a preferred embodiment, the dose is between 100 and 400 mL / 100 kg of seed.
[0078] It should be understood that the doses specified here are illustrative examples. A qualified professional, based on their expertise, will know how to adapt the application doses according to the nature of the plant / crop being treated.
[0079] The fungicidal compounds of the present invention, as well as compositions comprising them, are compatible with use in agriculture, given that they are not ecologically toxic, that is, they do not possess ecotoxicity.
[0080] Thus, the fungicidal compounds of the present invention and the compositions comprising them have low or no environmental impact, being ecologically sustainable and helping to preserve the environment.
[0081] The present invention can be better understood through the following non-limiting examples. EXAMPLES OF IMPLEMENTATION Example 1: Examples of processes for obtaining polyoxoniobates 1.1. Examples of PNb53 procurement processes
[0082] In the first step (step “a”), niobium phosphate can be mixed with water, forming a solution with a concentration that can vary between 1 and 5 g / L of niobium.
[0083] Next, the solution obtained in step “a” can be mixed with a solution of oxalic acid or hydrogen peroxide, in a concentration that can vary between 10 and 50% (w / w), obtaining a polyoxoniobate solution (step “b”).
[0084] In step “c”, the polyoxoniobate solution obtained in step “b” can be mixed with water.
[0085] The solution obtained in step “c” can be stirred between 10 and 100 rpm for a period that can vary from 5 to 120 minutes. 1.2. Examples of PNb53 procurement processes
[0086] In the first step (step “a”), niobium phosphate can be mixed with water, forming a solution with a concentration that can vary between 1 and 5 g / L of niobium.
[0087] Next, the solution obtained in step “a” can be mixed with a solution of oxalic acid or hydrogen peroxide, in a concentration that can vary between 10 and 50% (w / w), obtaining a polyoxoniobate solution (step “b”).
[0088] In step "c", the polyoxoniobate solution obtained in step "b" can be mixed with water.
[0089] In step “d”, the solution obtained in step “c” can be mixed with an aqueous solution of copper sulfate at a concentration that can vary between 0.5 and 1.5 g / L in a ratio that can vary between 1:2 and 2:1 v / v of polyoxoniobate to cations.
[0090] The solution obtained in step “d” can be stirred between 10 and 100 rpm for a period that can vary from 5 to 120 minutes. Example 2: Characterization of polyoxoniobates 2.1. Poly(aqua)phospho-hydroxy-n(oxy) niobate (PNb53)
[0091] For the physicochemical properties tests, poly(aqua)phospho-hydroxy-n(oxy)niobate (PNb53), with the molecular formula [Nbn(H2O)n(PO4)n(OH)2n(Oxi)3nP], at a concentration of 100 g.L⁻¹ 1 The composition used in the assay comprised 10% w / w poly(aqua)phospho-hydroxy-n(oxy)niobate and 90% w / w water.
[0092] The test results are shown in Table 1. Table 1. Physicochemical properties of poly(aqua)phospho-hydroxy-n(oxy)niobate (PNb53). Physicochemical properties Result Appearance: Translucent yellow liquid solution; Odor: Characteristic; pH: 1.0-1.5 Flammability: Non-flammable; Apparent density: 1.05 g / mL; Decomposition temperature: 150-200°C Risk of explosion. Non-explosive. Reactivity: Stable under normal temperature and pressure conditions. Chemical stability: Stable at room temperature (18 ai). 30°C 2.2. Copper(II) poly(aqua)phosphohydroxy-n(oxy)niobate (PNb53-C)
[0093] For the physical-chemical property tests, copper(II) poly(aqua)phosphohydroxy-n(oxy)niobate (PNb53-C), with the molecular formula [Nbn(H2O)n(PO4)n(OH)f ! (O i)3i-> Cu] x ', at a concentration of 100 g.L' 1The composition used in the assay comprised 10% w / w poly(aqua)phospho-hydroxy-n(oxy)niobate and 90% w / w water.
[0094] The test results are presented in Table 2. Table 2. Physicochemical properties of poly(aqua)phospho-hydroxy-n(oxy) copper(II) niobate (PNb53). Physicochemical properties Result Appearance: Translucent greenish liquid solution. Odor: Characteristic. pH 1.0-1.8 Flammability: Non-flammable Apparent density 1.05 g / mL | Decomposition temperature 150-200 °C Risk of explosion: Non-explosive Stable reactivity under normal temperature and pressure conditions. Chemical stability: Stable at room temperature (18 to 1 30°C) | Example 3: MTT calorimetric assay [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] 3.1. Testing Principle
[0095] The MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium] calorimetric assay is used to determine the viability of cultured cells after exposure to the test sample. The assay is based on the reduction of MTT, a water-soluble yellow salt, by the effect of the metabolic activity of mitochondrial enzymes linked to NADH and NADPH, forming insoluble formazan crystals, blue or purple in color, which are quantified by spectrophotometer. Under optimized conditions, the absorbance value obtained is directly proportional to the number of live cells. 3.2. Endpoint
[0096] Cell viability is determined by the activity of mitochondrial enzymes, measured by the production of formazan salt from MTT. It is expressed as a percentage of the negative control. 3.3. Endpoint Value
[0097] Cell viability (%) is calculated as the ratio (treated QD) / (negative control OD) * 100%, where: OD: optical density; and the wavelength is 570nm. 3.4. Cell lineage
[0098] The cell line used in the test was epithelial cells derived from human lung carcinoma (A549). Cultures were performed in DMEM medium with 10% Qualified Fetal Bovine Serum. 3.5 Tests and results
[0099] The test was performed with a short exposure period of 6 hours, as shown in Tables 3 and 4 and Figures 1 and 2, and a long exposure period of 24 hours, as shown in Figures 3 and 4 and Tables 5 and 6, for the PNb53 (sample 1) and PNb53-C (sample 2) samples, respectively.
[0100] In the case of short-term exposure, the measured endpoint is considered cell death. In the case of long-term exposure, the test substance may exert its effect on cells as cell death or inhibition of cell proliferation. According to ISO 10993-5 (2009), for a sample to be considered cytotoxic there must be a reduction in viability greater than 30% in the evaluated cell line. Therefore, the graphs were marked with a dashed line at the point where 70% of cell viability is indicated. The points on the lines of the graphs are representative of the Mean ± Standard Deviation (SD). Table 3. Sample 1 (PNb53) with an exposure time of 6 hours. Concentration OD 570 Viability (%) _ (pg / mL) _ Mean ± SD Mean ± SD Control: Zero 0.911 ± 0.061 100 C1 = 875 0.944 ± 0.076 103.6 ± 6.2 C2 = 437.5 0.932 ± 0.033 102.5 ± 5.8 C3 = 218.8 0.926 ± 0.022 101.9 ± 4.9 C4 = 109.4 0.960 ± 0.070 105.7 ± 10.6 C5 = 54.7 0.953 ± 0.042 105.0 ± 9.0 C6 = 27.3 0.928 ± 0.037 102.1 ± 5.9 C7 = 13.7 0.946 ± 0.031 104.2 ± 7.8 Table 4. Sample 2 (PNb53-C) with an exposure time of 6 hours. Concentration OD 570. Viability (%) (pg / ml). Mean ± SD. Mean ± SD. Control; Zero 0.847 ± 0.032 100 Cl = 875 0.865 + 0.119 107.3 ± 9.7 C2 = 437.5 0.926 ± 0.113 112.2 ± 7.9 03 = 218.8 0.967 ± 0.096 115.0 ± 6.3 04 = 109.4 0.910 ± 0.056 107.1 ± 2.9 C5 = 54.7 0.895 + 0.040 102.0 ± 6.7 C6 = 27.3 0.915 + 0.072 107.1 ± 5.3 C7 = 13.7 0.869 ± 0.005 101.6 ± 3.7 Table 5. Sample 1 (PNb53) with 24-hour exposure time. Concentration OD 570 Viability (%) (pg / mL) Mean ± SD Mean ± SD Control: Zero 1.548 ± 0.126 100 C1 = 875 1.453 + 0.102 94.1 ± 7.4 C2 = 437.5 1.714 ± 0.128 110.7 ± 1.5 03 = 218.8 1.609 ± 0.120 104.0 ± 3.0 04 = 109.4 1.530 ± 0.095 98.9 ± 2.0 C5 = 54.7 1.572 ± 0.072 101.8 ± 7.1 C6 = 27.3 1.576 ± 0.075 102.0 ± 5.1 C7 = 13.7 1.427 ± 0.041 92.4 ± 4.9 Table 6. Sample 2 (PNb53-C) with 24-hour exposure time. Concentration OD 570. Viability (%) (pg / ml). Mean ± SD. Mean ± SD. Control: Zero. 1.529 ± 0.057. 100 C1 = 875 1.604 ± 0.132 104.9 ± 5.6 02 = 437.5 1.529 ± 0.081 100.0 ± 1.7 03 = 218.8 1.440 ± 0.079 94.2 ± 4.9 04 = 109.4 1.527 ± 0.031 100.0 + 3.3 C5 = 54.7 1.542 ± 0.065 100.9 ± 1.8 C6 = 27.3 1.495 ± 0.057 97.8 ± 2.1 C7 = 13.7 1.419 ± 0.084 92.8 ± 3.4
[0101] This test was performed according to the ISO 10993-5 (2009) and ECVAM (number 17) protocol. After performing the MTT cytotoxicity test using the human lung cell line (A-549), it was found that samples 1 (PNb53) and 2 (PNb53-C) at the 7 (seven) concentrations evaluated, namely: 875; 437.5; 218.8; 109.4; 54.7; 27.3; 13.7 pg / mL, were not cytotoxic. According to ISO 10993-5 (2009), for a sample to be considered cytotoxic, there must be a reduction in viability greater than 30% in the evaluated cell line. Example 4: Phytotoxicity Assay [0102)0 The objective of this trial was to evaluate the effects of the test substances on plants during the critical early stages of their development. For this purpose, the seeds of a terrestrial plant species were exposed to a test substance during the germination, emergence, and early seedling growth stages. The effects measured included percentage of emergence, number of emerged plants, seedling survival, seedling length, and seedling biomass. In addition, qualitative phytotoxic effects were observed and evaluated.
[0103] The duration of the experiment was 5 days, at a temperature of 20°C, with concentrations of 1% of the compounds PNb53 and PNÕ53-C. Ten seeds of the species Lactuca sativa were used for each replicate, with a total of four replicates per treatment (Table 7).
[0104] Two experimental designs were used for this trial: seeds incubated in petri dishes and filter paper; and seeds incubated in petri dishes and Tropical Artificial Soil. The Tropical Artificial Soil was prepared in the following proportion: 70% quartz sand, 20% kaolin, 10% sieved coconut fiber (Table 8). Table 7. Germinated Lactuca sativa seeds on filter paper after 5 days of exposure. Replica Control PNb53 PNb53-C #1 10 0 0 #2 7 0 0 #3 9 0 0 #4 9 0 0 Average 87.5% 0% 0% Table 8. Lactuca sativa seeds germinated in Tropical Artificial Soil after 5 days of exposure. Replica Control PNb53 PNb53" C #1 8 8 10 _ #2 _ 9 _ 9 _ 8 #3 10 7 6 #4 9 8 9 [ Average] 90.0% | 80.0% | 82.5% |
[0105] The substances tested (PNb53 1% and PNb53-C 1%) did not cause statistically significant negative effects on Lactuca sativa seeds when incubated in petri dishes with Tropical Artificial Soil. However, when incubated in petri dishes containing filter paper as a substrate, the treated groups (PNb53 1% and PNb5-C 1%) did not favor the germination of Lactuca sativa seeds.
[0106] The phytotoxicity assay using Lactuca sativa seeds in soil showed that the substances PNb531% and PNb53-C 1% did not present negative effects on germination in the first 5 days of development. The tested substances were classified as non-toxic under the tested conditions. Example 5: Acute Toxicity Test with Earthworms
[0107] The aim of this assay was to evaluate the acute ecotoxicity to earthworms of the species Eisenia fétida and / or Eisenia andrei, using soil samples and chemical substances. This method consisted of exposing adult earthworms of the species Eisenia fétida and / or Eisenia andrei to various concentrations of the sample in a static assay, for a period of 14 days. Toxicity was determined by comparing the lethality of the test organisms with the control organisms, under the same assay conditions.
[0108] The duration of the experiment was 14 days, at a temperature of 24°C; a photoperiod of 12:12 and concentrations of 1% PNb53 and PNb53-C. Ten adult Eisenia andrei organisms were used for each replicate. The substrate used was Tropical Artificial Soil (70% quartz sand, 20% kaolin, 10% sieved coconut fiber - Table 9). Table 9. Count of living organisms in each replicate. Control PNb53 PNb53-C #1 10 10 10 #2 10 10 10 #3 10 7 10 #4 I 10 10
[0109] A one-way ANOVA test for comparison of means was performed, and no statistically significant differences were found between the groups tested. Therefore, both substances (PNb53 and PNb53-C) were considered non-toxic to Eisenia andrei within the 14-day exposure interval.
[0110] In replicate PNb53 #3, at the end of the test, 7 live earthworms were found, but 3 dead earthworms were not found. According to protocol, missing earthworms are considered dead.
[0111] The substances tested (PNb53 1% and PNb53~C 1%) did not show acute toxicity to earthworms of the species Eisenia andrei exposed for a period of 14 days. The substances tested were classified as non-toxic under the conditions tested. Example 6: Escape Test with Worms
[0112] The aim of the experiment was to evaluate the habitat function of soils and the influence of contaminants and chemicals on the behavior of earthworms.
[0113] Ten adult earthworms (Eisenia andrei or Eisenia f tida species) were used and simultaneously exposed to control soil and contaminated soil or soil containing the test substances. Test soil and control soil were placed inside the test container, and the earthworms could choose between the test soil and the control soil.
[0114] The experiment was conducted over 3 days at a temperature of 24°C, with a 12:12 photoperiod, at PNb53 concentrations of 1% and PNb53-C. The substrate used was Tropical Artificial Soil (70% quartz sand, 20% kaolin, 10% sieved coconut fiber).
[0115] The organisms did not exhibit escape behavior in relation to the soil treated with PNb53, since, on average, 60.2% of the organisms remained in the test soil.
[0116] The organisms did not exhibit escape behavior in relation to the soil treated with PNb53-C, since, on average, 43.8% of the organisms remained in the test soil.
[0117] The substances tested (PNb53 and PNb53-C) did not cause negative effects on soil habitat functions at a concentration of 1%. The substances tested were classified as non-toxic under the conditions tested. Example 7: Reproduction Trial with Earthworms
[0118] The objective of this study was to evaluate the effects of chemical substances in the soil on the reproduction of earthworms of the species Eisenia fétida or Eisenia andrei. To this end, adult earthworms were exposed to a variety of concentrations of chemical substances, either mixed into the soil or applied to the soil using procedures consistent with the standard use of the chemical product under test.
[0119] The method of application was specific to the purpose of the test. The range of test concentrations was selected to encompass those likely to cause sublethal and lethal effects over an eight-week period.
[0120] The mortality and growth effects on adult worms were determined after 4 weeks of exposure. The adults were then removed from the soil, and the effects on reproduction were evaluated after another 4 weeks by counting the number of offspring present in the soil.
[0121] The experiment was conducted over 8 weeks at a temperature of 25°C, with a 12:12 photoperiod, at concentrations of PNb53 1% and PNb53-C 1%, using 10 adult organisms (Eisenia andrei) for each replicate. Artificial soil (70% quartz sand, 20% kaolin, 10% sieved sphagnum moss) was used as a substrate. The results obtained are shown in Tables 10 and 11. Table 10. Count of live adult organisms after 4 weeks of experimentation. Replica Control PNb53 PNb53-C #1 10 10 10 #2 10 10 10 #3 10 10 10 #4 10 10 10 I #5 10 10 Table 11. Count of live juvenile organisms after 8 weeks of testing. Control Replicas PNb53 PNb53-C #1 35 41 20 #2 14 54 32 #3 35 46 15 #4 48 70 12 #5 32 48 23
[0122] Regarding the number of adult organisms observed at the midpoint of the trial (4 weeks), there was no loss or mortality. A one-way ANOVA test was performed, and no statistically significant differences were found between the Control and PNb53-C groups. However, the PNb53 treatment showed a statistically significant increase in the number of juveniles observed at the end of the trial when compared to the other groups.
[0123] The substance PNb53-C 1% did not show a statistically significant difference when compared to the control. However, the substance PNb53 1% resulted in a significant increase in the number of juveniles after 8 weeks when compared to the other groups. The substances tested were classified as non-toxic under the tested conditions. Example 8: Acute oral toxicity tests in rats of the polynobates PNb53 and PNb53-C
[0124] In these studies, three young, healthy, nulliparous, non-pregnant adult female Wistar rats (Rattus norvegicus), 9 weeks old, were used for each compound tested. The animals were used after inspection and acclimatized to laboratory conditions for at least 5 days, according to SOP-M 0225 and SOP-M 0226. Feeding was withheld the day before the application of the test item. Each animal was identified by a mark on its tail. The temperature of the animals' room was maintained at 22°C (± 30°C), as well as the relative humidity between 30 and 70%. Photoperiods were programmed in sequential cycles of 12 hours of light and 12 hours without light, and air changes were scheduled for 10 to 15 / hour. The animals were individually weighed before the application of the test item (day 0), on the 70th day after the administration of the test item, and at the end of the treatment (140th day). The animals in this study were sacrificed in a CO2 and O2 chamber.o Euthanasia method (cervical dislocation), according to POP-M 0133.
[0125] The test items were administered undiluted. The volumes of the test items administered to each animal were calculated according to their respective body weight, determined on the day of treatment. Administration was performed by gavage, using an appropriate cannula attached to a syringe. The animals were given access to food ad libitum again 3 hours after application.
[0126] The animals were dosed in a single-stage procedure using three female animals with a dose of 5000 mg / kg of PNb53 and three female animals with a dose of 5000 mg / kg of PNb53-C. Initially, the test items were administered to only one animal; as no clinical signs or mortality were observed 48 hours after application to the first animal, two more animals were tested.
[0127] According to the results obtained and in accordance with the methodology used, the polyoxoniobates from the PNb53 and PNb53-C tests showed an oral LD50 >5000 mg / Kg of body weight, being classified as Category 5 / Unclassified according to the Globally Harmonized System (GHS) for the classification of chemicals. Example 9: Efficiency and agronomic practicality of PNb53 and PNb53-C in seed treatment for the control of Fusarium pallidoroseum in soybean (Glycine max L.) crops.
[0128] The objective of this trial was to evaluate the efficiency and agronomic practicality of PNb53 and PNb53-C, in seed treatment, for the control of Fusarium pallidoroseum in soybean crops, as well as to record possible phytotoxic effects of the treatments on said crop. 9.1. Evaluation trial of PNb53 and PNb53-C in soybean seeds
[0129] For the assay, the seeds were inoculated with the pathogen, where the multiplication of the fungus Fusarium pallidoroseum was carried out in 9cm diameter petri dishes containing PDA medium and maintained in an incubation chamber at 25 °C ± 2 °C and a 12-hour photoperiod for seven days, according to the methodology suggested by TANAKA, MAS., MENTEN, JOM & MARIANNO, MJA Artificial inoculation of cotton seeds with Colletotrichum gossypii var. cephalosporioides and seed infection as a function of exposure time to the pathogen. Summa Phytopathologica 15:232-237. 1989. In each plate containing the fungus, 10 grams of seeds were placed directly in contact with the surface of the colonies. The plates were shaken so that the entire surface of the seeds came into contact with the fungal colony and then incubated for 48 hours. After this period, the seeds were dried at room temperature for 24 hours.The inoculated seeds were then mixed with the non-inoculated seeds, aiming to obtain a homogeneous mixture with a 20% incidence of the pathogen.
[0130] The seeds used in the trials were treated in polyethylene bags, where the dosages of the products were first added (also referred to here by the letter “p.” - concentrations of 100g / L of PNb53 and 100g / L of PNb53-C), supplemented with water until a volume of solution equivalent to 500 mL / 100 kg of seeds was reached, mixed, and then the seeds were placed in the bags and agitated until complete coverage and homogenization (Table 12 and Figure 5).
[0131] For the blotter test, 100 seeds per replicate were used, with four replicates per treatment, totaling 400 seeds. In each gerbox (11.0 cm x 11.0 cm x 3.5 cm), four sheets of filter paper moistened with water were placed, and 20 seeds were distributed. The seeds were incubated for seven days at a temperature of 20°C ± 2°C and a 12 / 12 hour fluorescent light / dark cycle. After this period, using a stereoscopic microscope and a biological microscope, the number of seeds infected by Fusarium pallidoroseum was counted, and the incidence of seeds infected by the pathogen was calculated. The percentage of seed germination was also counted to verify the effect of the pathogen interfering with seed germination (Table 13, Figure 6, and Figure 7). Table 12. Treatments for the evaluation trial of PNb53 and PNb53~C, in seed treatment, in soybean cultivation. DOSAGES PRODUCTS aia / 100kg 1 p. / 100kg 2 1. 0 0 i Inoculated Witness 2. MAXIM ADVANCED 2 + 2 + 15 100 í (fludioxonil + metalaxyl-M + thiabendazole) i 3- 10 100 PNb53 i 4. 20 200 PNb53 5. 40,400 PNb53 6. 10 100 PNb53-C 7. 20 200 PNb53-C 8. 40,400 PNb53-C 1 a.i. / 100kg = grams of active ingredient ('a.') per 100 kg of seeds 2 p. / 100kg - milliliters of product ("p.") per 100 kg of seed Table 13. Effect of soybean seed treatment (cv. M 5917 IPRO) with fungicides on the control of Fusarium pallidoroseum in seeds, evaluated by the Blotter Test method. INCIDENCE OF SEED TREATMENTS % INFECTED (%) 1 / 2GERMINATION 1 ' 3 Dosages Products (ml_ p. / 100 kg Fusarium pallidoroseum without) 1 - 0 20.50 (0) a 87.00 (0) b Inoculated witness 2 100 12.50 (39) ab 91.00 (5) ab MAXIM ADVANCED 3. 100 19.00 (7) a 87.00 (0) b PNb53 4. 200 12.50 (39) ab 89.00 (2) ab PNb535. 400 12.50 (39) ab 94.50 (9) a PNb53 6. 100 14.50 (29) ab 92.00 (6) ab PNb53-C 7. 200 12.00 (41) ab 92.00 (6) ab PNb53-C 8. 400 10.00 (51) b 91.50 (5) ab PNb53-C CV (%) 12.97 3.35 1 Average of four repetitions per treatment. Values followed by the same letter do not differ from each other by Tukey's test at 5% probability. Values in parentheses indicate the differences (%) in relation to the control without fungicide. 2 Analysis of Variance performed after transforming the original data for x I. 3 / Analysis of Variance performed after transforming the original data to arcsine % / 100.
[0132] Based on the blotter test evaluation, the products showed control for Fusarium pallidoroseum in soybean seeds, although only the highest dose of PNb53-C (400 mL / 100 kg of seeds, with 10% incidence) differed significantly from the inoculated control, which showed 20.50% incidence. Even the standard, with 12.50% incidence, showed 39% control and did not differ from the control, with the 200 and 400 mL doses of PNb53 showing the same control as the standard. The 100 and 200 mL doses of PNb53-C had similar behavior to the standard, with 29% and 41% control, respectively.
[0133] In the germination assessment using the Blotter Test, where the pathogen acts directly on the seeds, the inoculated control showed 87% germination, and the fungicide treatments showed variations from 87% (100 mL of PNb53) to 94.50% (400 mL of PNb53), with the latter differing significantly from the inoculated control. 9.2. Tray test in a greenhouse
[0134] For the greenhouse tray trial, 100 seeds were sown in plastic trays (405 mm x 260 mm x 70 mm = 7.4 dm³). 3 ), containing, as a substrate, a 2:1 mixture of washed medium sand and Plantmax® commercial compost, and the seeds were divided so that each tray represented two replicates of 50 seeds.
[0135] The commercial substrate used was Plantmax®, indicated for the production of seedlings of forest species. According to the manufacturer, the compound contains: pine bark, fine and superfine granule vermiculite, and humus.
[0136] The chemical composition of the commercial substrate Plantmax® was detailed in the Embrapa research and development bulletin (2012), containing: nitrogen (0.49 dag. kg⁻¹). 1 ); P2O2 (0.41 dag.kg' 1 ); K2O (0.38 dag.kg' 1 ); calcium (0.90 dag. g 1 ); magnesium (1.78 dag.kg" 5 ), sulfur (0.27 dag.kg 1 ), iron (2.00 dag.kg" 1 ); carbon (10.7 dag.kg" 1 ); copper (36.5 mg.kg" 1 ): zinc (45 mg. kg" 1 ); manganese (215 mg.kg" 1 ) and boron (13.8 mg.kg' 1(SERRANO, LA L; FANTON, CJ; MARTINS, AG Organic substrates and slow-release fertilizer in the production of early-maturing dwarf cashew seedlings. Research and Development Bulletin, ISSN 1679-6543, November, 2012).
[0137] Percentage of emergence assessments were performed periodically, from the emergence of the first seedlings until emergence stabilized. The trial was conducted until 28 days after sowing, when all seedlings were carefully removed from the trays, washed in running water, and then the shoot and root length of 25 randomly selected seedlings were evaluated. The percentage of germination and the percentage of normal and abnormal seedlings were assessed based on the total percentage of germinated seedlings.
[0138] With the seedling emergence assessments, the Emergence Speed Index (ESI) was determined (Figure 8), calculated according to MAGUIRE, 1962 by equation (1) where E1, E2 and En represent the number of normal seedlings counted in the first, second and last count. N1, N2 and Nn - number of days after the implementation of the test (MAGUIRE, JD Speed of germination aid in selection and evaluation for seedling emergence and vigor. Crop Science, Madison, v.2, n.2, p. 176-177, 1962). IVE = E1 / N1 + E2 / N2 +... + En / Nn (1)
[0139] The fresh and dry mass of the seedlings from each treatment was also evaluated, divided into shoot and root system, taking all the seedlings from the plots and then dividing by the number of seedlings. For dry mass, the seedlings were left to dry in an oven until constant weight. The temperature and relative humidity data obtained in the greenhouse during the experiment are described in Table 14. Table 14. Daily temperature, precipitation, and relative humidity data collected in the greenhouse during the experiment. Day Temp. Min. (°C) Temp. Max,(°C) i Precip. (mm)* RH (%) 1 17.2 33.6 3.0 62.5 2 14.6 31.3 i 3.0 59.0 3 9.2 30.7 i 3.0 56.0 4 9.3 30.6 3.0 54.5 I 5 12.5 31.6 3.0 55.0 6 17.2 31.9 3.0 51.0 i 7 17.2 30.8 3.0 63.5 8 15.0 31.5 3.0 63.5 9 15.1 32.0 i 3.0 60.0 | 10 15.2 32.0 3.0 62.5 11 16.4 32.4 3.0 62.0 12 15.7 32.1 3.0 61.5 i 13 19.7 32.9 i 3.0 55.5 14 19.5 32.5 i 3.0 51.5 15 16.9 33.7 i 3.0 56.5 16 17.6 32.0 I 3.0 63.0 17 18.0 32.0 | 3.0 65.0 18 15.5 28.0 i 3.0 73.0 i 19 12.5 31.3 3.0 61.5 20 13.4 33.0 3.0 59.5 21 14.7 32.6 3.0 57.0 22 14.3 33.8 3.0 57.0 23 15.1 33.6 3.0 56.0 24 15.1 33.7 3.0 55.5 | 25 15.6 33.9 3.0 54.5 | 26 15.9 33.9 3.0 54.5 27 18.1 33.0 i 3.0 55.0 28 20.5 22.3 3.0 73.0 29 16.1 30.1 3.0 71.5 * Precipitation supplied through sprinkler irrigation.
[0140] All results were subjected to analysis of variance, and those that showed significant differences between treatments were subjected to the mean separation test, Tukey's test at the 5% significance level. All analyses were performed using the statistical software SASM-Agri v.3.2.4. (CANTERI et al., Sasm - Agri: System for analysis and separation of means in agricultural experiments for Scott - Knott, Turey, and Duncan methods, Brazilian Journal of Agricultural Computing, v.1, n. 2, p.18-24, 2001).
[0141] Table 15 presents the effect of soybean seed treatment with the fungicides Maxim Advanced, PNb53, and PNb53-C on the control of Fusarium paidoroseum, on seedling emergence between 0 and 22 days after emergence (DAE) (Figure 14) and emergence speed index in trays (IVE), in a greenhouse; and Table 16 presents the effect of soybean seed treatment with the fungicides Maxim Advanced, PNb53, and PNb53-C on the control of Fusarium paidoroseum, on shoot length (Figure 9) and seedling root length (Figure 10), in a trial conducted in trays in a greenhouse.
[0142] Table 17 presents the effect of treating soybean seeds with the fungicides Maxim Advanced, PNb53, and PNb53-C, for the control of Fusarium pallidoroseum, on the health of seedlings grown in trays in the greenhouse, and Figure 11 represents the effect of treating soybean seeds (cv. M 5917 IPRO) with fungicides, for the control of Fusarium pallidoroseum, on seed germination.
[0143] Table 18 shows the effect of soybean seed treatment for the control of Fusarium pallidoroseum on the fresh weight and dry weight of plants grown in trays in the greenhouse. Table 15. Effect of soybean seed treatment (cv. M 5917 IPRO) with fungicides on the control of Fusarium pallidoroseum, on seedling emergence and emergence speed index in trays, in a greenhouse. TRATAft ÍENTOS EMERGENCY 3E SEEDLINGS IN SAND Dosages Products (ml P. / 100 (0 DA) |(1 DA) (2 DA) (3 DA) (4 DA) (5 DA) (22 DA) IVÊ I kg sem.) 3 1, 0 59,00 f 96,50 98,00 99,00 99,00 99,00 99,00 7,74 | testemunha (0) (0) (0) (0) (0) (0) (0) (0) inoculada n.s. | n.s. n s. n.s. n.s. n.s. n.s. n.s | 2. 100 63,00 91,50 97,00 97,50 97,50 97,50 97,50 7,66 | MAXIM ADVANCED (7) (-5) (-1) (-2) (-2) (-2) (-2) (-1) 3 100 55,50 | 93,00 95,50 95,50 96,00 96,00 96,00 7,48 | PNb53 (-6) (-4) (-3) (-4) (-3) (-3) (-3) (-3) | 4. 200 55,00 91,00 93,50 95,00 95,00 95,00 95,00 7,39 | PNb53 (-7) (-6) (-5) (-4) I (-4) (-4) (-4) (-5) i 5, 400 43,00 88,50 93,50 95,50 96,00 96,00 96,00 7,28 | PNb53 (-27) (-8) (-5) (-4) (-3) (-3) (-3) (-6) 6. 100 50,00 92,00 95,00 96,00 96,00 96,00 96,00 7,41 | PNb53-C (-15) (-5) (-3) (-3) (-3) (-3) (-3) (-4) 7. 200 50,50 | 88,00 92,00 94,00 95,00 95,00 95,00 7.30 | PNb53-C (-14) (-9) (-6) (-5) (-4) (-4) (-4) (-6) | 8. 400 54,50 89,50 95,00 97,00 97,50 97,50 97,50 7,52 i PNb53-C (-8) (-7) (-3) (-2) (-2) (-2) (-2) (-3) 9. 0 40,00 88,00 96,50 98,00 98,50 98,50 98,50 7,40 | testemunha without inoculum (-32) (-9) (-2) (-1) (-1) (-D (-1) (-4) CV (%) 15.16 6.42 8.06 7.39 | 7.66 7.66 7.66 4.06 | 1 Average of four repetitions per treatment. Values in parentheses indicate the differences (%) in relation to the control. Values followed by the same letter do not differ from each other by Tukey's test at 5% probability. 2 Analysis of Variance performed after transforming the original data to arcsin √(x / 100). 3 mL p. / 100 kg sem. - milliliters of product per 100 kilograms of seeds. ns = not significant. Table 16, Effect of soybean seed treatment (cv, M 5917! PRO) with fungicides, in the control of Fusarium pallidoroseum, on the shoot and root length of seedlings, in a trial conducted in trays in a greenhouse. TREATMENTS SEEDLING LENGTH (cm) 1 ' 2 Dosages Products 3 Aerial part Roots (mL p. / 100 kg sem.) I 1 - 0 26.75 (0) ns 26.08 (0) ai Uninformed Witness 2. 100 27.93 (4) 26.93 (3) for MAXIM ADVANCED 3. 100 29.23 (9) 25.93 (-1) a _ PNb53 _ I 4 200 29.95 (12) 27.58 (6) a _ PNb53 _ 5. 400 28.45 (6) 27.03 (4) to PNb53 6. 100 29.32 (10) 25.56 (-2) to PNb53-C 7. 200 28.56 (7) 28.69 (10) a _ PNb53-C _ 8. 400 28.02 (5) 28.50 (9) a _ PNb53-C 0 26.89 (1) 27.21 (4) a I i Witness without inoculum CV (%) 6.37 5.23 1 Average of four repetitions per treatment. Values in parentheses indicate the differences (%) in relation to the control. Values followed by the same letter do not differ from each other by Tukey's test at 5% probability. ns - not significant. 2Analysis of Variance performed without transforming the original data. 3 mL p. / 100 kg sem. ~ milliliters of product per 100 kilograms of seeds.Table 17. Effect of soybean seed treatment (cv. M 5917 IPRO) with fungicides, for the control of Fusarium pallidoroseum, on the health of seedlings grown in trays in the greenhouse. TREATMENTS SEEDLING INCIDENCE (%) 1 Dosages Products (mL p. / 100 kg i Sprouted 3 i Normal Abnormal without.) 1 ii 1. 0 99.00 (0) ns 99.49 (0) ns 0.51 (0) ns Inoculated control 2. 100 97.50 (-2) 99.48 (0) 0.52 (-2) MAXIM ADVANCED 3. 100 96.00 (-3) 100.00 (1) 0.00 (100) PNb53 4. 200 95.00 (-4) 99.49 (0) 0.51 (0) PNb53 5. 400 96.00 (-3) 100.00 (1) 0.00 (100) PNb53 6. 100 96.00 (-3) 100.00 (1) 0.00 (100) PNb53-C 7. 200 95.00 (-4) 100.00 (1) 0.00 (100) PNb53-C 8. 400 97.50 (-2) 100.00 (1) 0.00 (100) PNb53-C 9. Witness without 0 98.50 (-1) 100.00 (1) 0.00 (100) inoculation C. V, (%) 7.66 2.63 20.04 1 Average of four repetitions per treatment. Values in parentheses indicate the differences (%) in relation to the control. Values do not differ significantly between This is determined by analysis of variance. The percentage of normal and abnormal seedlings is relative to the number of seedlings that germinated. ns = not significant 2 ml p. / 100 kg sem. = milliliters of product per 100 kilograms of seeds. Table 18. Effect of soybean seed treatment (cv. M 5917 IPRO) for the control of Fusarium pallidoroseum, on the Fresh Weight and Dry Weight of plants grown in trays in the greenhouse. TREATMENTS FRESH WEIGHT / Plant i DRY WEIGHT / Plant i (9)' (S) 1 I Products Doses Aerial Part | Roots | Aerial Part | Roots (mLp. / 100 kg) seeds) 2 1. 0 2.968 (0) ns i 1.154 (0) i 0.337 (0) ns 0.097 (0) ns | Witness inoculated in ns i 2. I 100 2.930 (-1 ) 1 1.014 (-12) i 0.322(-4 ) 0.077 (-21) i MAXIM ADVANCED | 3. 100 2.953 (0) 1 1.024 (-11); 0.321 (-5) 0.080 (-18) i PNb53 4. i 200 3.113 (5); 1.100 (-5) i 0.341 (1) 0.079 (-18) i PNb53 i 5. i 400 3.157 (6) i 1.157 (0) i 0.346 (3) 0.091 (-6) I PNb53 6. 100 3.061 (3) 1.027 (−6) 0.328 (−3) 0.075 (−22) PNb53-C 3?i22'(5) pÕ^93 E14j1 ÕÍ334 W"" 'TíõwWl PNb53-C 8. i 400 3.053 (3) i 1.223 (6) i 0.338 (0) 0.092 (-5) i PNb53-C 9. | 0 3,012 (1) i 1,024 (-11) i 0,329 (-2) 0,076 (-21) i Witness without inoculum CV (%) 4.87 i 12.88 i 4.99 13.24 ] 1 Average of four repetitions per treatment. Values in parentheses indicate the differences (%) in relation to the control. Values do not differ significantly from each other by analysis of variance. ns = not significant. 2 mL p. / 100 kg seeds = milliliters of product per 100 kilograms of seeds.
[0144] In seedling emergence assessments in trays, the inoculated control showed a final emergence of 99.00%, and the fungicide treatments did not differ significantly. The variation among fungicides was from 95.00% to 97.50%, and the control without inoculum showed 98.50% emergence.
[0145] The Emergence Speed Index (ESI) was calculated using emergence readings over the days until the number of emerged seedlings stabilized, and there was no significant difference between the inoculated control and the fungicide treatments. The inoculated control had an ESI of 7.74, while the non-inoculated control had an ESI of 7.40, and among the fungicide treatments, the variation was from 7.28 (400 mL dose of PNb53) to 7.66 (Maxim Advanced at a dose of 100 mL);
[0146] In the evaluation of shoot length of seedlings, the treatments that presented the greatest heights were: 200 mL dose of PNb53 (29.95 cm), 100 mL dose of PNb53-C (29.32 cm), 100 mL dose of PNb53 (29.23 cm), although none of the treatments differed statistically from the inoculated control, which presented a length of 26.75 cm (Figure 9).
[0147] In terms of root length, the highest values were observed with the 200 and 400 mL doses of PNb53-C, measuring 28.69 cm and 28.50 cm, respectively, showing no significant difference from the inoculated control (26.08 cm). The 200 and 400 mL doses of PNb53 also had numerically higher values than the inoculated control, measuring 27.58 cm and 27.03 cm, respectively, similar to the Maxim Advanced standard of 26.93 cm, but did not differ statistically.
[0148] In terms of fresh weight of the aerial part per plant, the inoculated control presented 2.968 g and the fungicide treatments showed variations of 2.930 g (Maxim Advanced at 100 mL) and 3.157 g (400 mL of PNb53), without differing significantly. In terms of dry weight of the aerial part, there was also no significant difference (Figure 10).
[0149] In terms of fresh root weight per plant, the inoculated control group weighed 1.154 g, while the fungicide treatments ranged from 0.993 g to 1.223 g, without significant differences (Figure 12). There was also no significant difference in dry root weight (Figure 13).
[0150] No symptoms of phytotoxicity from the fungicides were observed in the soybean crop.
Claims
CLAIMS 1. Fungicidal compound, characterized by being a polyoxoniobate.
2. Fungicidal compound, according to claim 1, characterized in that it is an isopolyniobate or a heteropolyniobate.
3. Fungicidal compound, according to claim 2, characterized in that the heteroatom contained in the heteropolyniobate is a phosphorus atom.
4. Compound according to any one of claims 1 to 3, characterized in that the polyoxoniobate is combined with copper (Cu). 2+ ).
5. Fungicidal compound, according to any one of claims 1 to 4, characterized in that the polyoxoniobate is [Nb ! (OH)2n(Oxi)3 t) ] y ' (poly(aqua)phospho-hydroxy~n(oxy)niobate) and / or [Nbn(H2O)n(PO4)n(OH)n(Oxi)3nCu] x ' (poly(aqua)phospho-hydroxy-n(oxy)niobate copper II).
6. Fungicidal composition, characterized in that it comprises the fungicidal compound as defined in any one of claims 1 to 5.
7. Fungicidal composition, according to claim 6, characterized in that it further comprises an agriculturally acceptable vehicle.
8. Use of a fungicidal compound, as defined in any one of claims 1 to 5, or of a fungicidal composition, as defined in any one of claims 6 and 7, characterized in that it is for seed protection against one or more phytopathogenic fungi.
9. Use according to claim 8, characterized in that the seed is a legume seed.
10. Use according to claim 9, characterized in that the seed is a soybean seed.
11. Use, according to qualquer uma das reivindicações 8 a 10, characterized by the fate of a phytopathogenic fungus selected from a group that consists of Alternaria, Aspergillus, Albugo, Apiognomonia, Armiliaria, Bipolaris, Botryosphaeria, Blumeriella, Bremia, Blumeria, Basidiophara, Botrytis, Cladosporium, Cochlioboius, Corynespora, Cercospora, Colletotríchum, Discula, Didymella, Drechslera, Elsinoë, Eutypa, Erysiphe, Exserohilum, Fusarium, Golovinomyces, Goeodes, Gymnosporangium, Gibberella, Hemileia, Helminthosporium, Leveillula, Macrophomina, Monosporascus, Monilinia, Magnaporthe, Mycosphaerella, Neofabraea, Phakopsora, Phomopsis, Podosphaera, Penicillium, Phaeosphaeria, Pyrenophora, Puccinia, Pythium, Phytophthora, Peronospora, Pseudoperonospora, Pseudocercosporella, Plasmopara, Plasmodiophora, Phoma, Pyrícularia, Rhizopus, Ramularia, Rhyncosporium, Rhizoctonia, Schizothyrium, Septoria, Sclerotinia, Sphaerotheca, Stagonospora, Sclerotium, Tilletia, Tritici, Uncinula, Uromyces,Ustilago, Verticillium, Venturia, Wilsonomyces, 12. Use, according to any one of claims 8 to 11, characterized in that the fungus is of the genus Fusarium.
13. Use, according to any one of claims 8 to 12, characterized in that the fungus is of the species Fusarium pallidoroseum.
14. Plant seed, characterized by being coated and / or treated with a fungicidal compound, as defined in any one of claims 1 to 5, or with a fungicidal composition, as defined in any one of claims 6 to 9.
15. Plant seed, according to claim 16, characterized in that the plant seed is the seed of a leguminous plant.
16. Plant seed, according to claim 17, characterized in that the plant seed is a soybean seed.
17. Method for controlling a disease caused by a phytopathogenic fungus, characterized by comprising treating / coating a seed with a fungicidal compound, as defined in any one of claims 1 to 5, or with a fungicidal composition, as defined in any one of claims 6 and 7.
18. Method for controlling one or more phytopathogenic fungi, characterized by comprising applying a fungicidal compound, as defined in any one of claims 1 to 5, or a fungicidal composition, as defined in any one of claims 6 and 7, to a seed.
19. A method for treating seeds against one or more phytopathogenic fungi, characterized by comprising the step of mixing a fungicidal compound as defined in any one of claims 1 to 5 or a fungicidal composition as defined in any one of claims 6 to 7 with one or more seeds.
20. A method for controlling damage and / or yield loss caused by one or more phytopathogenic fungi, characterized by comprising the steps of applying a fungicidal compound, as defined in any one of claims 1 to 5, or a fungicidal composition, as defined in any one of claims 6 to 7, to a seed and planting the seed.