Stable synergistic herbicidal composition comprising an elemental sulphur and at least one bioactive oil

Abstract

The present invention relates to a novel biopesticidal combination comprising elemental sulphur and at least one bioactive oil and / or their constituents having an effective control of various pests including fungal and insect pests. The present invention further relates to a biopesticidal composition comprising of an effective amount of elemental sulphur; an effective amount of at least one bioactive oil and / or their constituents and at least one agrochemically acceptable excipient.

Description

[0001] NOVEL BIOPESTICIDAL COMPOSITION

[0002] TECHNICAL FIELD

[0003] The present invention relates to a novel biopesticidal combination comprising elemental sulphur and at least one bioactive oil and / or their constituents having an effective control of various pests including fungal and insect pests. The present invention further relates to a biopesticidal composition comprising of an effective amount of elemental sulphur; an effective amount of at least one bioactive oil and / or their constituents and at least one agrochemically acceptable excipient.

[0004] BACKGROUND

[0005] The background description includes information that may be useful in understanding the present invention. It is not an admission that any of the information provided herein is prior art or relevant to the presently claimed invention, or that any publication specifically or implicitly referenced is prior art.

[0006] Global crop production has surged since the Green Revolution, yet in some regions, yields remain stagnant or declining. Meanwhile, rising populations and living standards have significantly increased food demand. Pesticides and mineral fertilizers have been instrumental in boosting yields and food security, but their excessive use has led to severe environmental and human health risks.

[0007] The extensive application of synthetic chemical pesticides has led to significant environmental concerns, with growing awareness about chemical residues contaminating food, water sources, and natural ecosystems. Many of these substances pose risks due to their toxicity, potential carcinogenic effects, and harmful impact on human, animal, and aquatic life. Furthermore, the increasing resistance of pests to conventional pesticides has diminished their effectiveness, complicating pest management strategies. Stricter regulatory measures have further restricted the availability of many synthetic pesticides, driving the need for safer and more sustainable alternatives.Natural pesticides derived from minerals, plants, and microorganisms generally exhibit lower environmental persistence and reduced bioaccumulation compared to synthetic chemicals. For instance, low-toxicity plant oils (biological oil), can be one of the alternatives to conventional pesticides. However, some of these natural materials can also pose risks to non-target organisms including beneficial insects, wildlife, and even humans. In addition, certain plant oil may leave residues or provide comparatively lower efficacy than conventional synthetic products under specific conditions. Careful management is therefore essential to ensure both efficacy and environmental protection.

[0008] Elemental sulphur is a cost-effective agricultural input, serving as both a fertilizer and a natural pesticide. It enhances nutrient uptake, improves soil health, and is certified for organic farming. However, traditional sulphur formulations face challenges such as poor dispersion, residue build up, instability, and incompatibilities when combined with other pesticides.

[0009] Given the increasing demand for sustainable and effective crop protection solutions, there is a clear need for a biopesticidal combination that addresses the shortcomings of conventional sulphur products while aligning with modem agricultural.

[0010] The combination of sulphur with bioactive oil and their constituents represents a novel approach to overcoming the limitations of existing solutions. Bioactive oil and their compounds such as Fatty acids and their derivatives provide exceptional chemical stability, biodegradability, and enhanced compatibility with agricultural applications. Unlike synthetic carriers, these bioactive oils facilitate superior spreadability, reduce residue formation, and improve the dispersion of sulphur particles, leading to increased formulation stability and efficacy. Additionally, this bioactive oil and their constituents exhibit inherent pesticidal and plant-protective properties, making them ideal functional excipients in sulphur formulations. This innovative combination offers a stable, environmentally friendly, and efficient alternative to synthetic pesticides, providing an integrated solution for pest and disease management in agriculture.

[0011] SUMMARY OF THE INVENTIONAn object of the present invention is to provide novel biopesticidal combination comprising elemental sulphur and at least one bioactive oil and / or their constituents having and effective control of various pests including fungal and insect pests.

[0012] The present invention further relates to a biopesticidal composition comprising of an effective amount of elemental sulphur; an effective amount of at least one bioactive oil and their constituents and at least one agrochemically acceptable excipient.

[0013] The present invention also relates to a biopesticidal composition comprising of elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil selected from the group comprising of jojoba oil, garlic oil, anise oil, basil oil, nutmeg oil, rosemary oil, camphor oil, cedarwood oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0014] The invention also relates to a process of preparing a biopesticidal composition comprising of elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0015] The invention furthermore relates to a method for treatment of the plant, plant propagation material, locus, parts thereof or the soil against pests or diseases or managing pesticidal resistance or reducing pesticidal residue by application of a biopesticidal composition comprising of an effective amount of elemental sulphur; an effective amount of at least one bioactive oil and / or their constituents.

[0016] Various objects, features, aspects and advantages of the inventive subject matter will become more apparent from the following detailed description of preferred embodiments.

[0017] DETAILED DESCRIPTION

[0018] In describing the embodiments of the invention, specific terminology is resorted for sake of clarity. However, it is not intended that the invention be limited to specific terms so selectedand it is to be understood that each specific term includes all technical equivalents that operate in a similar manner to accomplish a similar purpose.

[0019] All technical and scientific terms used herein have the same meanings as commonly understood by someone ordinarily skilled in the art to which the present subject matter belongs.

[0020] The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure.

[0021] The expression of various quantities in terms of “%” or %wt. or “% w / w” or “%w / v” means the percentage by weight, relative to the weight of the total formulation or composition unless otherwise specified.

[0022] As used herein, the term “agrochemical” used herein is understood to denote an agricultural chemical such as pesticides, fungicides, insecticides, acaricides, herbicides, nematicides, plant growth regulators and can be used interchangeably.

[0023] As used herein, the term "effective amount" refers to an amount of the compound that, when ingested, contacted with or sensed, is sufficient to achieve a good level of control. As used herein, the phrase "agrochemically acceptable" means earners which are known and accepted in the art for the formation of formulations for agricultural or horticultural use.

[0024] Reference throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.The terms “ambient temperature” and “room temperature” as utilized herein shall generally mean any suitable temperature found in a laboratory or other working quarter, and is generally not below about 15°C nor above about 30° C.

[0025] The physicochemical studies of the compositions / formulation is performed according to the CIPAC standard method.

[0026] The term AHS refer to Accelerated heat stability (AHS), wherein experimental studies are carried out to determine the stability of the composition after 14 days of preparing the said composition at a temperature of 54°C.

[0027] The term “plant” refers to all physical parts of a plant, including shoots, leaves, needles, stalks, stems, fruit bodies, fruits, seeds, roots, tubers and rhizomes.

[0028] The term “crop” shall include a multitude of desired crop plants or an individual crop plant growing at a locus.

[0029] As used herein, the phrase "excipients" means excipients which are known and accepted in the art for formation of formulations for agricultural or horticultural use.

[0030] As used herein, the term "bioactive oil" refers to naturally occurring organic oil and their constituents with pesticidal, insecticidal, fungicidal, or plant-protective properties. Bioactive oil, as described in this invention, belong to various chemical classes, including but not limited to phenylpropanoids are aromatic compounds known for their insecticidal and antifungal activities. Examples include anethole, safrole, and myristicin from: anise, basil, camphor, and nutmeg. Jojoba oil a mixture of long-chain mono-unsaturated wax esters derived from fatty acids and fatty alcohols having carbon chain lengths predominantly from C20 to C24, including as a major component (Z)-eicos-ll-enyl (Z)-eicos- 11 -enoate (1 l-(Eicosenoic acid) plus monounsaturated omega-9 fatty acid. Sulfur-Containing bioactives are organosulfur compounds with insecticidal and fungicidal effects. Examples include allicin and diallyl sulfide from garlic, cedrol, cedrene bioactives from cedarwood oil.A first aspect of the invention relates to a novel biopesticidal combination comprising of an effective amount of elemental sulphur; an effective amount of at least one bioactive oil and / or their constituents.

[0031] According to an embodiment, the biopesticidal combination comprises an elemental sulphur and at least one bioactive oil and their constituents in the ratio of from about 60: 1 to about 1:10.

[0032] According to an embodiment, the bioactive oil is selected from the group consisting of jojoba oil, garlic oil, anise oil, basil oil, nutmeg oil, rosemary oil, camphor oil, cedarwood oil and / or their constituents.

[0033] According to an embodiment, the elemental sulphur is present in 1% to 90%wt. of the total composition. According to an embodiment, the elemental sulphur is present in 5% to 80%wt. of the total composition. According to an embodiment, the elemental sulphur is present in 10% to 80%wt. of the total composition.

[0034] According to another embodiment, the bioactive oil is present in 0.1% to 50% wt. of the total composition. According to an embodiment, the bioactive oil is present in 1% to 50% wt. of the total composition. According to an embodiment, the bioactive oil is present in 1% to 40% wt. of the total composition.

[0035] In another embodiments, the biopesticidal combination comprises at least one agrochemically acceptable excipient.

[0036] According to another embodiment, the agrochemically acceptable excipients can include surfactants, wetting agents, dispersing agents, emulsifiers, diluents, pigments, structuring agents, thickeners, suspending agents, anti-freezing agents, rheology modifiers, biocides, tackifier, sticking agents, stabilisers, antifoaming agents, fillers or mixtures thereof. However, those skilled in the art will appreciate that it is possible to utilize additional excipients without departing from the scope of the present invention. The agrochemically acceptable excipients are commercially manufactured and available through various companies.According to an embodiment, the agrochemically acceptable excipients are present in a concentration range of 1% to 80% wt. of the total composition.

[0037] According to an embodiment, the surfactants which are used in the composition include one or more anionic, non-ionic, and / or polymeric surfactants and can be employed as emulsifying agents, wetting agents, dispersing agents, or for other purposes.

[0038] The anionic surfactants include, but are not limited to, lignosulfonates, naphthalene sulfonates, aromatic sulfonate-formaldehyde condensates, alkylaryl sulfonates, sulfosuccinates, alkyl sulfonates, alkyl ether sulfates, polycarboxylate dispersants, phosphate ester, sodium lignosulfonate, calcium ligno sulfonate, potassium lignosulfonate, ammonium lignosulfonate, kraft ligno sulfonates, including grades having low or high degrees of sulfonation, modified lignosulfonates (oxidized, desugared, or sulfonation-enhanced grades), sodium dibutylnaphthalene sulfonate, diisopropylnaphthalene sulfonate (alkali metal or ammonium salts) salts of alkylnaphthalene sulfonic acids, naphthalene monosulfonate and disulfonate salts, aromatic sulfonate-aldehyde condensation products, alkali metal salt of naphthalene sulfonate condensate, salts of condensation products of naphthalene sulfonic acid and formaldehyde, salts of condensation products of phenol sulfonic acid and formaldehyde, salts of condensation products of naphthalene sulfonic acid, phenol sulfonic acid, and formaldehyde, mixtures of naphthalene sulfonate-formaldehyde and phenol sulfonateformaldehyde condensates, alkylaryl sulfonates, sodium dioctyl sulfosuccinate, sodium a-olefin sulfonate, sodium lauryl sulfate (SLS), sodium laureth sulfate (SLES), alkyl or alkylaryl phosphate esters (sodium or ammonium salts) or mixtures thereof.

[0039] In an embodiment, the anionic surfactant is present in a range from 0.1% to 40% wt. of the total composition. According to an embodiment, the anionic surfactant is in the range of 1% to 30%wt. of the total composition.

[0040] The non-ionic surfactants include, but are not limited to, sorbitan trioleate 20, 40, 60, 80, castor oil ethoxylate, glycerol monooleate, sorbitan monooleate, fatty alcohol ethoxylates (EO 2-3, C12-C18), propylene glycol fatty ester, polyoxyethylene sorbitan tristearate, fatty alcohol ethoxylates (EO 5-9, C12-C15), nonylphenol ethoxylates (EO 2-5), polysorbate 20, 40, 60, 80 polyethylene glycol fatty esters, tri- styrylphenol ethoxylates (TSP EO), EO-PO blockcopolymers (pluronic F-68, F-127, P-123), EO-PO block copolymers (pluronic L-44, L-62), EO-PO block copolymers (hydrophobic ally modified, low EO), amine ethoxylates, poly-alkoxylated butyl ether or mixtures thereof.

[0041] In an embodiment, the non-ionic surfactant is present in a range from 0.1% to 40% wt. of the total composition. According to an embodiment, the non-ionic surfactant is in the range of 1% to 30%wt. of the total composition.

[0042] The polymeric surfactants include, but are not limited to, polyethylene glycol (PEG)-based polymers, sodium polyacrylates, copolymer of polyacrylates, polycarboxylates, polyethyleneimine (PEI) derivatives, polyacrylamides and derivatives, polyvinylpyrrolidone (PVP) and copolymers, polyvinyl alcohols (PVA), acrylic polymers, comb polymer, copolymer of acrylic acid, methacrylamide, dimethylaminoethyl methacrylate, polyether modified trisiloxane, or mixtures thereof.

[0043] According to an embodiment, the polymeric surfactant is present in a range from 0.1% to 40% wt. of the total composition. According to an embodiment, the polymeric surfactant is in the range of 1% to 30% wt. of the total composition.

[0044] According to an embodiment, the anti-freezing agents which are used in the composition include one or more sodium chloride, potassium chloride, sodium gluconate, polyvinyl alcohol (PVA), polyethylene glycol (PEG 200-600), glycerol (Glycerin), propylene glycol (1,2-propanediol), sorbitol.

[0045] According to an embodiment, the anti-freezing agents is present in a concentration ranging from 0.1% to 15% wt. of the total composition.

[0046] According to an embodiment, the anti-foaming agents which are used in the composition include one or more dimethylpolysiloxane, silicon oil.

[0047] According to an embodiment, the anti-foaming agents is present in a concentration ranging from 0.1% to 30% w / w of the composition.

[0048] According to an embodiment, the rheology modifiers which are used in the composition include one or more aluminosilicate clay, magnesium aluminum silicate, amorphous silica, magnesium or aluminum hydroxides, hydrated magnesium silicate, layered double hydroxide,microbial polysaccharide (xanthomonas campestris), seed of cyamopsis tetragonoloba, seed of Ceratonia siliqua, agar-agar gum, carboxymethyl cellulose, sodium alginate.

[0049] According to an embodiment, the rheology modifiers present in a concentration ranging from 0.1% to 10% wt. of the composition.

[0050] According to an embodiment, the biocides which are used in the composition include one or more benzo thiazolinone, benzalkonium chloride (BAC), sodium pyrithione.

[0051] According to an embodiment, the biocide is present in a concentration ranging from 0.1% to 10% wt. of the composition.

[0052] According to an embodiment, the fillers which are used in the composition include one or more kaolin clay, bentonite, attapulgite clay, fuller’s earth, talc, calcium carbonate, magnesium carbonate, precipitated silica, diatomaceous earth, silica gel, fumed silica, zeolites, perlite powder, hydrophobic silica.

[0053] According to an embodiment, the fillers present in a concentration ranging from 0.1% to 40% wt. of the composition.

[0054] According to an embodiment, water is used as a diluent to dilute the active ingredient to a desired concentration. Water used is purified water and includes deionized water and / or distilled water.

[0055] In a second aspect, the present invention relates to a biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0056] According to an embodiment the present invention relates to a biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil selected from the group comprising of jojoba oil, garlic oil, anise oil, basil oil, nutmeg oil, rosemary oil, camphor oil, cedarwood oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient. The composition has particles in the size range of 0.1 micron to 100 microns.According to an embodiment the present invention relates to a biopesticidal composition comprising of an elemental sulphur in the range of l%w to 90% wt. of the total composition; at least one bioactive oil selected from the group comprising of jojoba oil, garlic oil, anise oil, basil oil, nutmeg oil, rosemary oil, camphor oil, cedarwood oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient selected from the group comprising of surfactant, anti-freezing agent, anti-foaming agent, rheology modifier, biocides, filler, diluents and combinations thereof in an amount in the range of 1% to 80 % wt. of the total composition.

[0057] According to an embodiment, the present invention relates to a biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; bioactive oil is jojoba oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0058] According to an embodiment, the present invention relates to a biopesticidal composition comprising of an elemental sulphur in the range of 10% to 85% wt. of the total composition; bioactive oil is jojoba oil and / or their constituents in the range of 1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0059] According to an embodiment, the biopesticidal composition of the present invention is a homogeneous physical mixture of elemental sulphur, at least one bioactive oil, and one or more agrochemically acceptable excipients. As used herein, the term “homogeneous” refers to a uniform distribution of the individual components throughout the composition at a macroscopic level, achieved through mechanical mixing, high-shear emulsification, and / or wet milling. The components remain physically associated in the form of a suspension, emulsion, or suspo-emulsion, without undergoing any chemical reaction, covalent bonding, or structural modification. Accordingly, the composition does not constitute a chemically reacted product or new chemical entity, but rather a stable physical formulation in which each component retains its original chemical identity and functionality.

[0060] According to an embodiment, the biopesticidal composition is in the form of a solid or a liquid.According to an embodiment, the biopesticidal composition of the present invention is formulated as one or more of Capsule suspension (CS), dry capsulated suspension (DC), Dispersible concentrate (DC), Powder for dry seed treatment (DS), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion for foliar spray (ES), Emulsion, oil in water (EW), Flowable suspension / concentrate for foliar spray (FS), Granule / soil applied (GR), Controlled (Slow or Fast) release granules (CR), Micro-emulsion (ME), Suspension concentrate (flowable concentrate) (SC), Suspo-emulsion (SE), Water dispersible granule (WG or WDG), Wettable powder (WP), Water dispersible powder for slurry treatment (WS), A mixed formulation of CS and SC (ZC), a mixed formulation of CS and SE (ZE) or a mixed formulation of CS and EW (ZW) or dust.

[0061] According to an embodiment, the biopesticidal composition can include at least one further pesticidal active ingredient or fertilizer or nutrient. However, those skilled in the art will appreciate that it is possible to utilize other active ingredient without departing from the scope of the present invention.

[0062] According to an embodiment, the further active ingredient is present in the range of 0.1% to 85% wt. of the total composition.

[0063] According to another embodiment, the invention relates to a process for preparing the biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0064] According to another embodiment, the invention relates to a process for preparing the biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient in the form of suspension concentrate, the process comprising of:

[0065] i. Preparing a per-mix slurry by mixing a defined quantity of surfactants and other excipients, as required, in water under agitation;ii. adding the mixture of a defined quantity of sulphur powder and at least one bioactive oil to the pre-mix obtained in step (i) to form a slurry;

[0066] iii. wet milling the slurry of step (ii) to obtain a desired particle size distribution; iv. adding balanced quantity of other excipients such as rheological modifiers, stabilizers, etc., as required to produce a final homogenous product in the form of suspension concentrate.

[0067] According to an embodiment, the present invention provides a process for preparing a suspension concentrate comprising:

[0068] i. preparing an aqueous premix by dispersing one or more excipients selected from surfactants, antifreeze, defoamer, and biocide in water under high-speed agitation to obtain a uniform dispersion;

[0069] ii. charging the bioactive oil into the premix of step (i) using a high-shear homogenizer at 10,000 to 25,000 RPM to form a stable emulsion with oil droplets less than 1 micron;

[0070] iii. adding elemental sulphur powder into the emulsion of step (ii) under high shear to form a slurry, followed by wet milling the slurry using a bead mill to achieve a desired particle size distribution;

[0071] iv. subjecting the slurry of step (iii) to wet bead milling under temperature-controlled conditions and subsequently adding in the remaining water and at least one rheological modifier to obtain a final product having the desired viscosity.

[0072] According to an embodiment, the present invention provides a process for preparing the biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient in the form of a suspo-emulsion, the process comprising:

[0073] i. preparing an organic phase comprising at least one bioactive oil and one or more surfactants;

[0074] ii. preparing an aqueous phase by dispersing at least one surfactant, at least one anti freezing agent, at least one biocide, and at least one anti-foaming agent or a mixtures thereof in a defined quantity of water;iii. charging organic phase of step (i) and emulsifier into the aqueous phase of step (ii) under high-shear mixing at a rate of 1,000 to 25,000 RPM to obtain a stable emulsion having a droplet size of less than 1 micron;

[0075] iv. dispersing sulphur powder into the emulsion of step (iii) under high-shear mixing at approximately 10,000 RPM to obtain a uniform slurry followed by wet milling the slurry using a bead mill to achieve a desired particle size;

[0076] v. subjecting the slurry of step (iv) to wet bead milling under temperature-controlled conditions and adding water and at least one rheological modifier to obtain a final product having viscosity of less than 2000 cP.

[0077] In some embodiments, the suspension is micronized until a particle size distribution of D90 less than 30p is obtained.

[0078] In some embodiments, the suspension is micronized until a particle size distribution of D50 less than lOp is obtained.

[0079] In some embodiments, the suspension is micronized until a particle size distribution of D90 less than lOp is obtained.

[0080] In some embodiments, the suspension is micronized until a particle size distribution of D50 less than 5p is obtained.

[0081] According to an another embodiment, the invention relates to a method for preparing the biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient in the form of wettable powder the process comprising

[0082] i. charging elemental sulphur, a dispersing agent, at least one secondary dispersant, at least one wetting agent, at least one anti-caking agent, at least one carrier, and / or inert filler in a high- shear ribbon blender and blending to obtain a uniform powder; ii. during blending, introducing at least one bioactive oil through pressure-atomization nozzle onto the agitated powder to obtain uniform distribution and absorption of the bioactive oil onto the carrier and / or filler particles, thereby forming a homogeneous pre-mix;iii. feeding the pre-mix of step (ii) to a micronizing system to reduce the particle size to the desired particle size range to obtain a wettable powder formulation, followed by secondary blending to obtain a final product.

[0083] In some embodiments, the powder is micronised until a particle size distribution of D90 less than 50p is obtained.

[0084] In some embodiments, the powder is micronised until a particle size distribution of D50 less than lOp is obtained.

[0085] In some embodiments, the micronization step may be carried out by any method or technique commonly known for the skilled person, such as, but not limited to, jet mill, classifier mill, pin mill, air classifier, cyclone separator or dust collection unit.

[0086] According to another embodiment, the invention relates to a method for preparing the biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; and at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient in the form of water dispersible granules the process comprising of:

[0087] i. preparing a pre-mix slurry by mixing a defined quantity of one or more surfactants, elemental sulphur powder and at least one bioactive oil under agitation to obtain a uniform slurry;

[0088] ii. subjecting the slurry of step (i) to wet milling to obtain the desired particle size distribution;

[0089] iii. spray drying the finely milled slurry into a spray dryer under controlled conditions to obtain a dry, free flowing granulated product.

[0090] According to an embodiment, the biopesticidal composition can comprise particles in the size range of 0.1 micron to 50 microns. According to an embodiment, the biopesticidal composition can comprise particles in the size range of 0.1 micron to 30 microns.

[0091] Achieving this fine particle size enhances pesticidal performance, improves suspension stability in spray solutions, and enables rapid wetting in water.According to an embodiment, the present invention provides a method of application of the the biopesticidal composition.

[0092] According to another embodiment of the present invention, the biopesticidal composition can be applied as a foliar spray, soil drenching, seed dressing, application as paste of the targeted plants / trees, broadcasting, spraying, rubbing, atomizing, irrigating, evaporating, dusting, fogging, broadcasting, pouring, mist blowing, soil mixing, foaming, painting, spreading-on, drenching, dipping or drip irrigation.

[0093] According to an embodiment, the invention further relates to the use of the biocidal composition as plant protection and a yield enhancer composition. In addition to promoting plant health and productivity, the composition exhibits improved toxicological and ecotoxicological safety, ensuring minimal impact on users and the environment. It demonstrates superior stability, maintaining its efficacy over extended storage and varying environmental conditions. Furthermore, the composition contributes to reduced residue levels, supporting compliance with regulatory limits, and offers pre -harvest benefits by enhancing crop quality and optimizing harvest timing.

[0094] According to an embodiment, the invention relates to a method of application of an effective amount of the biopesticidal composition, wherein the composition is applied to any and all developmental stages of insect pests, such as egg, nymph, larva, pupa, and adult. The insect pests may be controlled by contacting the target insect pest, habitat, breeding ground or its locus with an effective amount of the novel and inventive composition of the present invention.

[0095] According to another embodiment, examples of crops include groundnut, wheat, barley, rye, oats, soybean, cotton, mustard, sunflower, pulses such as chickpea, red gram, green gram, black gram, fruit Crops include grapes, apple, mango, banana, citrus, pomegranate, strawberry, pear, loquat. Vegetable Crops include chilli, tomato, brinjal, cucumber, bottle gourd, pumpkin, okra, peas, cabbage, cauliflower. Stone Fruits include peach, apricot, cherry, plum, macadamia. Tree Nuts includes almond, pistachio, hazelnut, chestnut, walnut. Ornamental and Plantation Crops includes tea, rose and Nursery plants.According to an embodiment, the biopesticidal composition of the present invention can be used to control the various pests including but not limited to powdery mildew, blight, wilt, white flies, all sucking pest, rust, rot, leaf spot, scab, mites, spider mites, gall mites.

[0096] According to an embodiment, the g a.i. / ha as used herein refers to grams of active ingredient per hectare, wherein the active ingredient represents the combined total amount of elemental sulphur and at least one bioactive oil present in the biopesticidal combination, unless otherwise specifically stated.

[0097] According to another embodiment, the present invention provides a method for controlling growth of fungal disease in a plant, the method comprising applying to the plant, plant part or locus thereof, a biopesticidal combination comprising an elemental sulphur and at least one bioactive oil, wherein the biopesticidal combination is applied at a rate ranging from about 10 g a.i. / ha to about 2000 g a.i. / ha. According to an embodiment, the biopesticidal combination is applied at a rate ranging from about 50 g a.i. / ha to about 750 g a.i. / ha. In a preferred embodiment, the biopesticidal combination is applied at a rate ranging from about 50 g a.i. / ha to about 450 g a.i. / ha.

[0098] According to an embodiment, the present invention further relates to a method of protecting the plant and enhancing the plant yield; the method comprising treating at least one of seeds, seedling, a plant, plant propagation material, locus, parts thereof or to the surrounding soil with effective amount of the biopesticdal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

[0099] According to an embodiment, the invention provides a method for controlling plant pathogenic fungi and / or bacteria, comprising applying to the locus of the plants, simultaneously or sequentially, an effective amount of component (a) and component (b), either: (a) as a preformulated biopesticidal composition, or (b) as a tank mix prepared by mixing an elemental sulphur formulation with at least one bioactive oil and / or their constituents in water prior to application.According to an embodiment, the present invention, the various components of the storage stable biopesticidal composition can be used individually or already partially or completely mixed with one another to prepare the composition according to the invention. It is also possible for them to be packaged and used further as combination composition such as a kit of parts. The method of control of the present invention may be carried out by spraying the suggested tank mixes, or the individual fungicide may be formulated as a kit-of-parts containing various components that may be mixed as instructed prior to spraying.

[0100] In a preferred embodiment of the present invention, a biopesticidal composition comprising (a) an elemental sulphur; (b) at least one bioactive oil and / or their constituents; and (c) a mixture comprising a surfactant is in the form of a kit with single pack or multi pack.

[0101] It has been observed that the combination of elemental sulphur and at least one bioactive oil demonstrated synergistic effect. In addition, the composition of the present invention demonstrates enhanced, efficacious and superior behaviour in the fields. In fact, various advantageous properties associated with the compositions according to the invention, include but are not limited to an advantageous behaviour during formulating and / or upon application, improved stability, improved toxicological and / or ecotoxicological behaviour, improved crop protection and crop yield and other advantages familiar to a person skilled in the art. Through the composition of the present invention, the number of applications or the amount of fertilizers or pesticides are minimized. The composition is highly safe to the user and to the environment.

[0102] EXAMPLES

[0103] The present invention is more particularly described in the following examples that are intended as illustration only, since numerous modifications and variations within the scope of the present invention will be apparent to those skilled in the art. Unless otherwise noted, all parts, percentages and ratios reported in the following examples are on a weight basis, and all ingredients used in the examples were obtained or are available from the chemical suppliers.

[0104] The following examples illustrate the basic methodology and versatility of the present invention.

[0105] Table 1: Suspension Concentrate (SC) formulations of Sulphur + Jojoba Oil (J-oil)

[0106] >

[0107]

[0108] Process: A suspension concentrate is prepared as follows. Preparing an aqueous premix by dispersing surfactants, antifreeze, defoamer, filler and biocide in water under high-speed agitation to obtain uniform dispersion. Charging the bioactive oil slowly into this premix using a high- shear homogenizer at 10,000-25,000 RPM to form a stable emulsion with oil droplets less than 1 micron. Adding elemental sulphur powder into emulsion under high shear to obtain slurry, followed by wet milling the slurry using a bead mill to achieve a solid particle size distribution of D50 less than 2.5 microns and D90 less than 8 microns. The resulting slurry is subjected to mill-base to a finishing vessel and subsequently blending in the remaining water and rheological filler under agitation to obtain a stable suspension concentrate.

[0109] Stability studies

[0110] Table 2: The physicochemical properties and stability observations of the formulation of Example 1 to Example 5 were recorded as follows:

[0111]

[0112] > > > > >

[0113]

[0114] > > > > >

[0115]

[0116] > > > > >

[0117]

[0118] Result: Examples 1 to 5 of the present invention demonstrate good physical stability and storage stability under ambient, cold (0°C), and accelerated (54°C) storage conditions.

[0119] Table 3: Suspo-emulsion (SE) and Suspension Concentrate (SC) formulations of Sulphur + Jojoba Oil (J-Oil)

[0120]

[0121]

[0122] Stability studies:

[0123] Table 4: The physicochemical properties and stability observations of the formulation of Example 6 to Example 10 were recorded as follows:

[0124] > > > > >

[0125]

[0126] > > > > >

[0127]

[0128] > > > >

[0129] >

[0130]

[0131] Result: Examples 6 to 10 of the present invention demonstrate exhibit good physical stability and storage stability under ambient, cold (0°C), and accelerated (54°C) storage conditions.

[0132] Example 11: Sulphur 70% + Jojoba oil 5% WP

[0133]

[0134]

[0135] Process: i. charging elemental sulphur powder, a dispersing agent, secondary dispersant, wetting agent, anti-caking agent or carrier, and inert filler in a high-shear ribbon blender and blending to obtain a uniform powder.

[0136] ii. during blending introducing, at least one bioactive oil through pressure-atomization nozzle onto the agitated powder to obtain uniform distribution and absorption of bioactive oil onto the carrier thereby forming a homogeneous pre-mix. iii. feeding the pre-mix of step (ii) in a micronizing system to reduce the particle size to the desired particle size range to obtain a wettable powder formulation followed by secondary blending to obtain the final product.

[0137] In Vitro Antifungal Assay Against Alternaria alternata

[0138] The antifungal activity of formulation of the present invention Example 11 Sulphur 70% + 5% Jojoba oil WP was evaluated against Alternaria alternata using a standard in vitro method where samples are incorporated into agar to measure fungal mycelial growth inhibition over 11 days at 28±2°C. Colony diameters were measured daily in triplicate for 11 days relative to control plates.

[0139] Table 5: Antifungal Assay Against Alternaria alternata

[0140]

[0141]

[0142] As shown, Example 11 Sulphur 70% + 5% J oil in WP exhibited superior radial growth inhibition (48.09% at Day 11) compared to solo Sulphur 55% SC (17.06%) and Jojoba oil (-1.24%), demonstrating unexpectedly prolonged antifungal activity.

[0143] Bio-efficacy and phytotoxicity data

[0144] The present invention composition was evaluated for bio efficacy and phytotoxicity for Powdery Mildew in Okra. The findings of the evaluation are summarized below.

[0145] Table 6: Treatments details

[0146]

[0147]

[0148] Sulphur 51% + Jojoba oil 5% combinations were tested at specified concentrations, along with one possible tank mix combinations: Sulphur 51% and Jojoba oil 5%. Additionally, solo individual fungicides, namely Sulphur 51% SC, Jojoba oil 5% and an untreated control, were tested against powdery mildew disease in Okra. The fungicides were applied as foliar spray using a Knapsack Sprayer fitted with a hollow cone nozzle. The observations on Percent Disease Index (PDI) of powdery mildew was calculated. Similarly, the Percent Disease Incidence (PDI) of powdery mildew and Grain discolouration were calculated. The yield was calculated after harvesting. Further, observations on phytotoxicity viz., epinasty, hyponasty, yellowing, necrosis, and leaf tip burning were recorded at 1, 3, 5, 7, 10 and 15 days after fungicide application.

[0149] Assessment of Powdery Mildew (Leveillula laurica) disease incidence:

[0150] A disease infection was then calculated according to the following:

[0151] Disease infection index % (PDI) = X Disease Scores x 100

[0152] Number of plants x Maximum Disease

[0153] assessed Score

[0154] Table 7: Disease rating scale:

[0155]

[0156]

[0157] Observation:

[0158] The incidence of Powdery Mildew was recorded fifteen days after each spraying. Twenty plants in each replicated plot were selected and tagged. The whole plant was observed for scoring the severity. Randomly selected twenty-five plants / replicated plot were evaluated excepting the border rows. The assessment of disease intensity of Powdery Mildew in okra was performed by calculating the score into percent disease index (PDI). The periodic intensity of Powdery Mildew was recorded and were statistically analyzed. The scoring of Powdery Mildew diseases was done based on the following Rating Schemes:

[0159] Table 8: Disease Ratings

[0160]

[0161] Synergy data:

[0162] A, = the percent inhibition of Disease by Fungicide A at Rate 1, and

[0163] B, = the percent inhibition of Disease by B at Rate 1, then

[0164] By (100- Al)

[0165] E= Al + Bl(lOO-Al)

[0166] 100

[0167] Colby Formula by converting the percent inhibition values to percent of control. Colby described the expected growth (E,) after applying the combination of Fungicide A at Rate 1 (Al) and Bioactive oil B at Rate 1 (Bl) by the formula

[0168] El = A1 B 1 / 100where Aland Bl are defined as Disease Control (percent and in revised form of control) rather than inhibition of Disease Control.

[0169] Table 9. Bio-efficacy data against Okra Powdery Mildew disease (1stSeason)

[0170]

[0171] *Data presented in parentheses indicate Angular transformed values; DAA- Days after application

[0172] Table 10. Bio-efficacy data against Okra Powdery Mildew disease (1stSeason)

[0173]

[0174] *Data presented in parentheses indicate Angular transformed values; DAA- Days after applicationTable 11:

[0175] >

[0176]

[0177] Result: The bio-efficacy data from the second spray confirms that the composition of the present invention Example 1 exhibits a significant and consistent synergistic effect. While the expected efficacy based on the Colby formula was calculated at 85.77%, the observed disease reduction for Treatments Tl, T2, and T3 reached significantly higher levels, peaking at 90.44%. The combination of Sulphur and Jojoba oil at the specified ratios provides a potentiation of fungicidal activity that exceeds the cumulative effect of the individual components.

[0178] The synergistic effect of the composition comprising Sulphur 51% + Jojoba oil 5% SC was determined using the Colby method. Based on the bio-efficacy data against Okra Powdery Mildew, the expected efficacy (E) for the combination of Sulphur (75.03% control) and Jojoba oil (45.69% control) was calculated to be 86.44%. This synergy allows for enhanced disease control even at lower application rates of the active ingredients.

[0179] Phy to toxicity: -

[0180] To know the crop tolerance and extent of phytotoxicity, ten plants were randomly selected from each plot and the total number of leaves showing phytotoxic symptoms such as viz., Stunting &Leaf injury on tips / surface, Chlorosis & deformation, Wilting& Scorching, Yellowing &Vein clearing, Necrosis& Crop discoloration, Hyponasty &Epinasty if any were counted on 1, 3, 5, 7 and 10 days after spraying and grading was done as per CIB guidelines adopting 0 -10 scale. A double dose of the test chemical was assessed only for the phytotoxic effect and the double dose treatment T9 was kept by the side of bio-efficacy trial plot to avoid drift into the bio-efficacy plots.Table 12:

[0181]

[0182] Table 13: Phytotoxicity Data:

[0183] &

[0184] &

[0185] &

[0186] &

[0187] & &

[0188] &

[0189] &

[0190] &

[0191] &

[0192] & &

[0193] &

[0194]

[0195] &

[0196] &

[0197] &

[0198] & &

[0199] &

[0200] &

[0201] &

[0202] &

[0203] & &

[0204]

[0205] Result: No symptoms of Chlorosis & deformation, Vein clearing & yellowing, Hyponasty & Epinasty, Necrosis & crop discoloration, Wilting & Stunting, Scorching & leaf injury were observed.

[0206] Yield: The Okra crop was harvested at periodical intervals. The yield in quintal per hectare was calculated and recorded.

[0207] Table 14. Yield Data

[0208]

[0209]

[0210] Result: T3 @ (3000 ml / ha) recorded higher okra fruit yield (14.42 t / ha) which was at par with T2 @ (2500 ml / ha) okra fruit yield (14.05 t / ha) and T1 @ (1875 ml / ha) okra fruit yield (13.92 t / ha) as compared to untreated control fruit yield (8.32 t / ha).

[0211] The tank-mix compatibility of product A Sulphur 80% WDG (4g / 250 mb) with various bioactive oils was evaluated using a CIPAC jar test method.

[0212] Table 15:

[0213] <

[0214]

[0215] <

[0216]

[0217] Result: All mixtures showed minor reversible phase separation without caking, residue levels below 0.5% w / w after 200-mesh sieving and required fewer than 12 inversions for complete re-dispersion. The mixtures remained physically stable with uniform dispersion, indicating suitability for co-application and reduced risk of nozzle blockage under field spray conditions.

[0218] Table 16:

[0219]

[0220] Result: A fertilizer-grade WDG containing 90% active ingredient showed 45% residue after 200-mesh sieving and significant sedimentation, indicating poor dispersibility and tank-mix incompatibility.

[0221] From the foregoing it is to be understood that no limitation with respect to the specific embodiments illustrated is intended or should be inferred. It is to be understood that the present invention is susceptible to modifications, changes and adaptations by those skilled in the art. Such modifications, changes, adaptations are intended to be within the scope of the present invention. The above and other features of the present invention will be more clearly described in the complete specification which will be filed pursuant to the present provisional specification.

Claims

Claims:We claim,1. A biopesticidal combination comprising an elemental sulphur and at least one bioactive oil and / or their constituents in a ratio from about 60: 1 to about 1: 10.

2. A biopesticidal composition comprising of an elemental sulphur in the range of 1% to 90% wt. of the total composition; at least one bioactive oil and / or their constituents in the range of 0.1% to 50% wt. of the total composition; and at least one agrochemically acceptable excipient.

3. The biopesticidal composition according to claim 2, wherein an elemental sulphur is in the range of 10% to 85% wt. of the total composition; at least one bioactive oil and / or their constituents is in the range of 1% to 50% wt. of the total composition.

4. The biopesticidal composition according to claims 2 to 3 wherein at least one bioactive oil is selected from the group comprising of jojoba oil, garlic oil, anise oil, basil oil, nutmeg oil, rosemary oil, camphor oil, cedarwood oil and / or their constituents.

5. The biopesticidal composition according to claim 4, wherein at least one bioactive oil is jojoba oil and / or their constituents.

6. The biopesticidal composition according to claims 2 to 5, wherein an elemental sulphur and at least one bioactive oil and / or their constituents is from about 60: 1 to about 1:10.

7. The biopesticidal composition according to claims 2 to 6, wherein the agrochemically acceptable excipients is selected from the group comprising of surfactants, wetting agents, dispersing agents, emulsifiers, diluents, pigments, structuring agents, thickeners, suspending agents, anti-freezing agents, rheology modifiers, biocides, tackifier, sticking agents, stabilisers, antifoaming agents, fillers or mixtures thereof.

8. The biopesticidal composition according to claims 2 to 6, wherein the composition is in the form of capsule suspension (CS), dry capsulated suspension (DC), Dispersible concentrate (DC), powder for dry seed treatment (DS), Emulsifiable concentrate (EC), water in oil Emulsion (EO), Emulsion for foliar spray (ES), oil in water Emulsion (EW), Flowable suspension / concentrate for foliar spray (FS), Granule / soil applied (GR), Controlled (Slow or Fast) release granules (CR), Micro-emulsion (ME), Suspension concentrate (flowable concentrate) (SC), Suspo-emulsion (SE), Water dispersible granule (WG or WDG), Wettable powder (WP), Water dispersible powder for slurry treatment (WS), a mixed formulation of CS and SC (ZC), a mixed formulation of CS and SE (ZE) or a mixed formulation of CS and EW (ZW) or dust.

9. The biopesticidal composition according to claim 8, wherein the composition is in the form of Suspension concentrate (SC), suspo-emulsion (SE), Water dispersible granule (WG or WDG) or Wettable powder (WP).

10. The biopesticidal composition according claims 2 to 9, wherein the composition is present in a form of a tank mix or a pre-formulated (pre-mix ) / ready-mix formulation.

11. A method for controlling phytopathogenic fungi, the method comprising applying an effective amount of the biopesticidal combination or composition as claimed in any one of claims 1 to 10 to the fungi, the plant, the plant propagation material, or the locus, parts thereof.

12. Use of the biopesticidal combination or composition as claimed in any one of claims 1 to 10 for controlling phytopathogenic fungi on plants or plant propagation material.

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