DESC:FIELD OF THE INVENTION:
The present invention relates to oil based suspension concentrate comprising synergistically effective amounts of Haloxyfop and Imazethapyr ester, salt and combinations thereof, wherein said Haloxyfop and Imazethapyr ester, salt and combinations thereof are taken in the mass ratio of 1: 0.77 to 11:8.47. The synergistic herbicide composition can be used for controlling various Graminaceous, sedges and broadleaf weeds and are preferred for oil seeds crops, leguminous crops, fiber crops, and broad leaf crops, and has minimal to zero phytotoxic effect on succeeding crops.

BACKGROUND OF THE INVENTION
The present invention is set within the context of the prior art related to herbicide formulations, particularly those that utilize combinations of herbicidal active ingredients. It should be understood that the following discussion is not intended to imply that the cited prior art is widely known or constitutes common general knowledge in the field, but rather serves to illustrate the technical context in which the present invention resides.
Herbicides are a category of pesticides specifically designed to target and eliminate unwanted plants, commonly referred to as weeds. Selective herbicides are formulated to target specific weed species while leaving desired crops relatively unharmed. These herbicides often function by interfering with the growth of the targeted weeds, with many operating through mechanisms such as plant hormone disruption. Conversely, nonselective herbicides are capable of killing all plant material upon contact and are often used to clear waste grounds or areas with no concern for the surrounding vegetation.
The use of herbicides is widespread, particularly in agriculture and turf management. Some herbicides exhibit rapid degradation in soil, while others possess more persistent properties, resulting in longer environmental half-lives. The varying persistence of herbicides is important in determining their suitability for different applications and environmental conditions.
In the prior art, the use of herbicide mixtures has been identified as offering significant advantages over the application of a single herbicide. These benefits include: (i) an expanded spectrum of weed control or prolonged efficacy over time, (ii) improved crop safety by enabling the use of lower individual doses of multiple herbicides in combination, rather than relying on high-dose applications of a single herbicide, and (iii) a delay in the development of herbicide-resistant weed species. These synergistic effects make herbicide mixtures particularly valuable in contemporary agricultural practices.

In some cases, it may be necessary or advantageous to apply combinations of two or more herbicides simultaneously, particularly when aiming for synergistic interactions beyond simply broadening the control spectrum. Such combinations are commonly administered as tank mixes or package-mixes, with the objective of achieving more rapid weed burn-down and earlier symptomology, thereby enhancing the overall performance and value of the herbicidal product.
Prior research and practical experience have shown that certain herbicidal active ingredients exhibit improved efficacy when combined, a phenomenon known as "synergism." Synergism occurs when the combined effect of two or more herbicides exceeds the expected outcome based on the individual effects of each active ingredient. This enhanced efficacy can result in more effective weed control with lower overall herbicide use, which is beneficial both for crop protection and for mitigating the development of resistance in weed populations.

The prior art clearly demonstrates the utility of herbicide combinations for improved control and safety. However, there remains a need for novel formulations that optimize these synergistic effects while addressing new challenges in weed control, environmental impact, and crop safety. The present invention seeks to advance these objectives by introducing a synergistic composition can be used for controlling various Graminaceous, sedges and broadleaf weeds and are preferred for oil seeds crops, leguminous crops, fiber crops, and broad leaf crops, and has minimal to zero effect on succeeding crops.

Haloxyfop-R-Methyl is a selective Herbicide, absorbed by the foliage and roots, and hydrolysed to Haloxyfop-R, which is translocated to meristematic tissues and inhibits their growth. Haloxyfop-R-methyl is used post-emergence for control of annual and perennial grasses in sugar beet, fodder beet, oilseed rape, potatoes, leaf vegetables, onions, flax, sunflowers, soya beans, vines, strawberries, and other crops.

Imazethapyr belongs to the chemical group Imidazolinone and acts by inhibiting the Acetolactate Synthase (ALS), an enzyme which is Important in protein synthesis within the plant. Imazethapyr is chemically known as 5-ethyl-2-[(RS)-4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl] nicotinic acid and is taken up by the weeds through roots and the leaves.

Some of the prior arts such as Indian patent no. IN390227 discloses an herbicidal composition comprising a tri-combination of Imazethapyr, Chlorimuron ethyl, and Clodinafop Propargyl, where Imazethapyr is present at a concentration of 10%, and Clodinafop Propargyl is used at 20%. These concentrations represent extremely high herbicide loading in the composition.

While the prior art teaches methods for reducing phytotoxicity specifically in broadleaf crops such as Bengal crops and soybeans, it fails to address the significant issue of phytotoxicity observed in graminaceous crops—such as sorghum, maize, and wheat—when grown as subsequent crops after the application of Imazethapyr. High doses of Imazethapyr are known to result in residual toxicity, which adversely affects the growth of graminaceous crops due to the residual herbicide in the soil. The composition disclosed in IN390227 does not provide any solution to mitigate or address the residual phytotoxicity effect on graminaceous crops. This limitation presents a challenge for agricultural practices involving crop rotation or the cultivation of graminaceous crops after herbicide application.

WO2023/187738 discloses a chemical-based herbicidal composition that includes, in addition to the herbicides, antioxidants such as Butylated HydroxyToluene (BHT) or Butylated HydroxyAnisole (BHA). The exemplified composition contains relatively high concentrations of haloxyfop R-methyl (12.8%) and imazethapyr (10%). The loading of herbicide in this formulation is notably high, which may raise concerns regarding the potential for residual toxicity. This composition is characterized as a chemical-based formulation containing both herbicidal active ingredients and chemical excipients, including the aforementioned antioxidants.

It is well established in the prior art that the use of high doses of imazethapyr can lead to significant phytotoxicity in succeeding crops. Specifically, imazethapyr has been shown to cause damage to crops planted after its application, especially graminaceous crops, rendering them unsuitable for cultivation following its use. The presence of high doses of imazethapyr in the composition disclosed in WO2023/187738 poses a risk of phytotoxic effects, which is a significant drawback of this herbicidal formulation. The composition fails to provide a solution to mitigate or control the phytotoxic effects associated with the use of imazethapyr, particularly for succeeding graminaceous crops.

In addition, the formulation disclosed in WO2023/187738 includes high doses of haloxyfop R-methyl, which, similar to imazethapyr, is known to cause phytotoxicity to graminaceous crops when used in higher concentrations. This further exacerbates the problem of crop damage, especially in situations where graminaceous crops are planted following herbicide application.
The lack of a solution for controlling the phytotoxic effects of use of higher doses of imazethapyr and haloxyfop R-methyl in this patent represents a significant limitation, particularly for agricultural practices where crop rotation is common and the safety of subsequent crops is of paramount importance.

The inventors of the present invention have unexpectedly discovered that an herbicidal composition, specifically a greener oil-based suspension concentrate, comprising synergistically effective amounts of Haloxyfop-R-Methyl and Imazethapyr in a mass ratio of 1–11: 0.77–8.47, can be used to effectively control a wide range of graminaceous weeds, sedges, and broadleaf weeds. This formulation is particularly advantageous for use in oilseeds, leguminous crops, fiber crops, and broadleaf crops. Notably, the composition of the present invention achieves effective weed control with significantly lower herbicide dosages compared to prior art formulations.

A key advantage of the present invention is that it does not rely on the use of specific chemicals detrimental to the environment, making it a more sustainable alternative to existing herbicidal compositions. Furthermore, the composition has been observed to have minimal to no phytotoxic effect on broadleaf and graminaceous crops, even when these crops are grown as succeeding crops after the application of the herbicide. This is in stark contrast to the prior art, where herbicides, such as Imazethapyr and/or Haloxyfop, result in residual toxicity that severely impacts the growth of graminaceous crops in subsequent planting cycles.

Thus, the present invention provides an environmentally friendly and highly effective solution for controlling weeds without causing the phytotoxic effects commonly associated with the high-dose herbicide compositions disclosed in the prior art. This represents a significant advancement in herbicide formulation, especially in terms of crop safety, environmental sustainability, and the broader applicability of the herbicide across various crop types.

SUMMARY OF THE INVENTION
As established in prior art, the use of Imazethapyr, whether as a single herbicide or in combination with other herbicides such as Clodinafop Propargyl or Haloxyfop R-methyl, is often limited due to its detrimental effects on succeeding crops. The present invention addresses this challenge by focusing on reducing the residual impact of Imazethapyr on subsequent crops while preserving its herbicidal efficacy on the current crop. Notably, this is achieved without the use of environmentally harmful chemicals, making the composition more sustainable and safer for crop rotation and environmental health.

Accordingly, in main aspect, the present invention provides oil based suspension concentrate comprising synergistically effective amounts of Haloxyfop and ester thereof and Imazethapyr and salts thereof, wherein said Haloxyfop and esters thereof, and Imazethapyr and salts thereof are taken in the mass ratio of 1-11: 0.77-8.47.

Another aspect of the present invention provides oil based suspension concentrate i.e. oil dispersion composition of synergistic agrochemical composition comprising bioactive amount of Haloxyfop-R-Methyl and Imazethapyr wherein said composition is prepared by using greener oils and solvents.

Another aspect of the present invention provides oil based suspension concentrate of Haloxyfop-R-Methyl and Imazethapyr that can be used to effectively control a wide range of graminaceous weeds, sedges, and broadleaf weeds. This formulation is particularly advantageous for use in oilseeds, leguminous crops, fiber crops, and broadleaf crops.

In yet another aspect, the composition of the present invention achieves effective weed control with significantly lower herbicide dosages with minimal to zero phytotoxic effect on succeeding crops with high herbicidal efficacy on the current crop.

DETAILED DESCRIPTION OF THE INVENTION
While prior art demonstrates the utility of herbicides and combinations for improved weed control and crop safety, it fails to address the issue of phytotoxicity in succeeding crops, particularly with high doses of Imazethapyr and Haloxyfop R-methyl. These herbicides, when used at high concentrations, cause significant damage to graminaceous crops planted afterward, hindering crop rotation and posing challenges for sustainable agriculture. The lack of a solution for mitigating these phytotoxic effects remains a key limitation in existing herbicide formulations.

In recent years, oil-based suspension concentrate (OBSC) also known as Oil dispersion (OD) formulations have attracted significant attention from companies and formulators due to their advantages in agronomic performance compared to conventional formulations. Active ingredients (AIs) formulated in different types of formulations often exhibit distinct physicochemical properties, influenced by the type of formulation in which they are incorporated. This variation in performance can be attributed to the presence of oil, such as mineral or vegetable oil, and emulsifiers in OBSC formulations, which act as penetration adjuvants when applied in the field. These adjuvants enhance the absorption of AIs by the plant, making OBSC formulations "adjuvanted" formulations that do not require additional adjuvants in the spray mixture, thus ensuring agronomic effectiveness.

However, despite being considered an adjuvanted formulation, OBSC still requires the addition of various adjuvants and excipients during manufacturing. One of the challenges of OBSC formulations lies in the development of stable, effective formulations with the appropriate selection of excipients and adjuvants. To achieve long-term stability, optimal formulation additives, in addition to ideal manufacturing processes, are necessary. Significant research has been dedicated to the development of OBSC formulations, particularly concerning the dispersion and activation of active ingredients, which are critical to maintaining the formulation’s stability over time. The solvents or carriers used in these formulations, which have traditionally been petroleum-based or aromatic, are increasingly being replaced by vegetable oils.

While the use of vegetable oils as formulation excipients in OBSC formulations offers certain benefits, they present challenges due to their inherent stability issues when combined with active ingredients. Additionally, many OBSC formulations tend to use high doses of active ingredients, which may lead to higher pesticidal loads in the environment. Furthermore, OBSC formulations often suffer from lower thermal and chemical stability under a broad range of conditions, increasing the toxicity hazards to applicators and decreasing overall safety during handling and spraying. Some OBSC formulations also exhibit insufficient leaf penetration of spray droplets, which can increase evaporation loss and limit the absorption of active ingredients.

There is a clear need for novel OBSC formulations that address these issues, providing better stability profiles, enhanced synergistic effects between active ingredients, reduced environmental impact, and improved crop safety. Specifically, there is a need for formulations that reduce the toxicity risks associated with higher pesticide doses, lower the pesticidal load on the environment, and improve safety for applicators during pesticide application.
The present invention aims to fill this gap by providing an oil-based suspension concentrate formulation that enhances the synergistic activities of the active ingredients, improves weed control efficacy, reduces the necessary dose of active ingredients, and minimizes the environmental pesticide load. The novel formulation also offers improved thermal and chemical stability across a wide range of conditions, reduces toxicity hazards to applicators, and enhances leaf penetration of spray droplets, thus reducing evaporation loss and improving the absorption of active ingredients.

Furthermore, OBSC formulations offer several advantages over conventional formulations, such as emulsifiable concentrates (ECs) and water dispersible granules (WDGs). EC formulations are facing increasing regulatory pressure to replace toxic, flammable solvents with safer alternatives, and the novel OBSC formulation meets these needs. Its oil content provides a favorable eco-toxicological profile, ensuring high biological efficacy while remaining non-toxic and non-flammable. Compared to EC formulations, the novel OBSC formulation offers superior biological performance without relying on toxic solvents.

Suspension concentrate (SC) formulations, although safe, typically struggle to enhance the biological efficacy of the active ingredients due to their aqueous base. In contrast, the novel OBSC formulation, with its oil content, guarantees improved biological results, especially for water-sensitive active ingredients. It represents the optimal solution for liquid formulations of such ingredients. Moreover, oil based suspension concentrate (OBSC) formulations offer significant advantages over WDG formulations, providing high efficacy at a lower cost, making them more economically viable.

The development of stable and effective OBSC formulations remains a challenge, particularly in selecting the appropriate excipients. It is crucial to choose excipients that are perfectly dispersible in oil, resist phase separation, allow for easy milling without agglomeration, promote excellent oil emulsification, and ensure stable dilution. Additionally, the formulation should provide uniform distribution of the active ingredients, ensuring optimal coverage, penetration, and yield.

Therefore, the present invention provides a novel OBSC formulation that addresses these challenges and delivers enhanced performance in weed control, reduced environmental impact, and improved safety for both the environment and the applicator.

Therefore, an aspect of the present invention provides a synergistic agrochemical Oil based suspension concentrate composition comprising haloxyfop and ester thereof, and imazethapyr and salts thereof.

Before the present invention is described, it is to be understood that this application is not limited to the particular systems, and methodologies described, as there can be multiple possible embodiments which are not expressly illustrated in the present disclosure. It is also to be understood that the terminology used in the description is for the purpose of describing the particular versions or embodiments only and is not intended to limit the scope of the present application. This summary is not intended to identify essential features of the claimed subject matter nor is it intended for use in determining or limiting the scope of the claimed subject matter.

Accordingly, in one embodiment, the present invention provides oil based suspension concentrate comprising synergistically effective amount of Haloxyfop and Imazethapyr, ester, salt and combinations thereof, wherein said Haloxyfop and Imazethapyr ester, salt and combinations thereof are taken in the mass ratio of 1: 0.77 to 11:8.47.

In another embodiment, the present invention provides oil based suspension concentrate formulation of synergistic agrochemical composition comprising Haloxyfop-R-Methyl or an agriculturally acceptable salt or ester thereof and imazethapyr that controls harmful weeds, wherein the composition is prepared by using greener oils and solvents.

In an embodiment the formulation or composition can also be prepared in other physical forms such as water dispersible granules (WDG).

In an embodiment the present invention provides oil based suspension concentrate of Haloxyfop-R-Methyl and Imazethapyr that can be used to effectively control a wide range of graminaceous weeds, sedges, and broadleaf weeds. This formulation is particularly advantageous for use in oilseeds, leguminous crops, fiber crops, and broadleaf crops. The composition is effective for control of weed in the crops selected from Soybean (Glycin max), Peanut (Arachis hypogaea), Green gram (Vigna radiate), Black gram (Vigna mungo), Green Gram (Vigna radiata), Chickpea (Cicer arietinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), French bean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Cotton (Gossypium spp.), Sugarcane (Saccharum officinarum), Castor (Ricinus communis), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus), Tomato (Solanum lycopersicum), Chilly (Capsicum annum), Sunflower (Helianthus annuus), Safflower (Carthamus tinctorium), Rapeseed(Brassica napus) and genetically modified version of all the crops mentioned above etc.

In an embodiment the composition of present invention controls all kind of Monocots, Dicots weeds and Sedges. The most common weeds controlled are selected from:
Grasses (Monocot):
Acrachne racemose, Acalypha strumarium, Abutilon theophrastii ,Brachiaria eruciformis, Cynodon dactylon, Chloris virgata, Cynotis sp, Cyanotis axiallaris Dactyloctenium aegyptium, Digitaria sanguinalis , Digitaria adscendens, Dinebra arabica, Dinebra retroflexa, Eragrostis japonica, Echinochloa crusgalli, Echinochloa Colona, Eleusine Indica, Euphorbia hirta Setaria faberii, Setaria spp, Imperator cylindrical, Leptocloa chinensis, Panicum dicotomiflorum, Panicum repens, Panicum isochmi,, Pnicum isochmi Sorghum halepense, Xanthium pensylvanicum etc.
Broadleaf Weeds (Dicot):
Ageratum conyzoides, Amaranthus rudis, Amaranthus viridis, Amaranthus spinosus, Acalypha ciliate, Acalypha strumarium, Altenanthera sessilis, Celosia argentea, Croton sparsiflorus, Commelina benghalensis, Commelina communis, Convolvulus arvensis, Cleome gynanadra, Cleome viscosa, Corchprus sp, Celosia argentea, Dinebra sp., Digera muricata, Digera arvensis, Digera muricata, Eclipta alba, Euphorbia geniculate, Galinsoga parviflora, Phyllanthus niruri, Panicum sp., Parthenium hysterophorus, Portulaca oleracea, Polygonum alatum, Parthenium hysterophorus, Trianthema portulaca, Trianthema monogyna etc.
Sedges: Cyperus sp.

The novel oil-based suspension concentrate formulation significantly improves the penetration of spray droplets, reduces evaporation loss, and enhances the absorption of active ingredients into weed leaves. This formulation increases the spreading properties on leaf surfaces, ensuring better wetting of waxy leaf surfaces found in some tough-to-kill weeds. This accelerates the speed of kill and boosts the overall efficacy against challenging weed species.
Additionally, the novel formulation of present invention improves rainfast properties, which is especially crucial during the rainy season to maintain the efficacy of the applied herbicide. By enhancing the rainfastness, the formulation ensures that herbicides remain effective even under adverse weather conditions.
The formulation also enhances the synergistic effects between active ingredients, allowing for the reduction of active ingredient doses, thereby minimizing the pesticidal load in the environment. This contributes to more sustainable agricultural practices with less chemical residue.
A key advantage of the novel formulation of present invention is that it is free from aromatic solvents, which not only improves safety for applicators but also reduces the environmental burden by eliminating the need for these toxic solvents. This makes the formulation safer for both the applicator and the environment.
Moreover, the novel formulation of present invention ensures superior crop safety due to the absence of aromatic solvents. It also offers improved stability during storage, as it utilizes oils such as Pongamia oil (>220°C flash point), Palm oil (>240°C), Jojoba oil (>290°C), Mahua oil (>230°C), and other vegetable oils (>200°C flash point). These high flash point oils make the novel oil based suspension concentrate more stable and safer for storage at elevated temperatures, ensuring reliable performance under a wide range of conditions.

Overall, the novel formulation of present invention exhibits excellent thermal and chemical stability, further enhancing its reliability and effectiveness across diverse environmental conditions.

In one another embodiment, the composition of the present invention in addition to bioactive amounts of active ingredients further comprises inactive excipients including but not limited to Super Wetting-spreading- penetrating agent, carrier or solvent, dispersant or dispersing agent, emulsifying agent, anti-freezing agent, anti-foam agent, preservatives and buffering agent.

In another embodiment, the super wetting-spreading-penetrating agent used herein for present oil based suspension concentrate include but not limited to Polyalkyleneoxide modified Heptamethyl trisiloxane (Modified trisiloxane).

List of inactive agents which may be used in the present invention are listed below but not limited to (Table 1):
Inactive excipients used in Oil based suspension concentrate formulation:
Table -1
Excipients Function Quantity (% w/w)
Fatty alcohol ethoxylate, trisiloxanes, non-ionic acid ethoxylate, PSPO base ethoxylate, calcium sulfonated salt, condensed naphthalene sulfonate, propoxylated Ethoxylated copolymer monoalkylether (ethylhexanol), alkyl sulfonates, alkyl benzene sulfonates, alkyl aryl sulfonates, alkylphenolalkoxylates, tristyrylphenol ethoxylates, natural or synthetic fatty ethoxylate alcohols, natural or synthetic fatty acid alkoxylates, natural or synthetic fatty alcohols alkoxylates, alkoxylated alcohols (such as n-butyl alcohol poly glycol ether), block copolymers (such as ethylene oxide-propylene oxide block copolymers and ethylene oxide-butylene oxide block copolymers), fatty acid-polyalkylene glycol condensates, polyamine-fatty acid condensates, polyester condensates, salts of polyolefin condensates, sodium ligno sulfonate, sodium ploycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, 5 polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide. dispersing agent 1-20%
Saturated esterified vegetable oil, unsaturated esterified vegetable oil, esterified methyl soyate oil, Methyl oleate, edible oil, non-edible oil, palm oil, esterified essential oil, esterified non-essential oil. solvents 0.1-90%
silicone oil, silicone compound, dimethyl siloxane, poly dimethyl siloxane, oil based antifoam, polydimethylsiloxane. Antifoaming agent 0.1-3%
ethylene glycol, propane diols, glycerine or the urea, glycol (Monoethylene glycol, Diethylene glycol, Polypropylene glycol, Polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate. Anti-freezing 0.1-20%
Fused Silica Antisettling agent 0.1-8%
Organic silicates Rheological modifier 0.1-30%

In an embodiment, said Haloxyfop R-methyl: Imazethapyr is present between 1-11% w/w of total composition, and Imazethapyr is present between 0.77-8.47% w/w of total composition.

In an optional embodiment, the oil based suspension concentrate of the present invention further comprises of effective adjuvants to improve efficacy.

In another preferred embodiment, the compositions of the present invention do not require addition of any antioxidants or stabilizers.

In one another embodiment, the oil based suspension concentrate is prepared by mixing active ingredients i.e. Haloxyfop-R-methyl, and Imazethapyr and inert ingredients and premixing of all ingredients in high shear homogenizer at 25-30°C. It is then followed by wet milling of all ingredients at 25-30°C in bead mill (2-3 milling required). It is then followed by post blending in high shear homogenizer at 25-30°C followed by unloading and packing of material.

Similarly, the Water dispersible granules (WDG) can be applied after disintegration and dispersion in water. Water dispersible granules can be formed by a) agglomeration, b) spray drying, or c) extrusion techniques.

WDG formulations offer a number of advantages in packaging, ease of handling and safety. The WDG are preferably of uniform size, and which are free flowing, low dusting and readily disperse in water to form a homogenous solution of very small particles which may pass through conventional spray nozzles. Ideally WDG formulations when dispersed in water under gentle agitation for five minutes have residues of less than 0.01% on a 150 µm sieve screen and less than 0.5% on a 53 µm screen. The granules can usually be measured accurately by volume which is convenient for the end user.

The process for preparing the present agrochemical composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the composition. However, all such variation and modification are still covered by the scope of present invention.

In another embodiment, the composition can optionally be prepared as water dispersible granules formulation comprising further inactive ingredients selected from one or more of:
a) dispersing agent selected from the group comprising Sodium salt of naphthalene sulfonate condensate, Modified polyacrylate copolymer, Sodium polycarboxylate, Sodium Ligno sulfonate, Alkyl naphthalene sulfonate condensate, sodium salt, Fatty acids methyltauride, sodium salt and Polyacrylate co-polymer, and wherein the weight ratio of dispersing agent is 0.5-10% w/w of total composition,
b) co-dispersant selected from Alcohol block co-polymer, and wherein the weight ratio of co-dispersing agent is 0.5-10% w/w of total composition,
c) wetting agent selected from the group comprising of Blend of naphthalene sulfonate condensate, Sodium dodecylbenzene sulfonate, Sodium lauryl sulfate, Blend of alkyl naphthalene sulfonate and anionic wetting agent, Sodium n-butyl naphthalene sulfonate, Sodium isopropyl naphthalene sulfonate, and Blend of sodium alkyl aryl sulfonates, and wherein the weight ratio of wetting agent is 0.5-10% w/w of total composition,
d) anticaking and suspending agent is selected from Silicon dioxide, Precipitated silica, Urea formaldehyde resin and Urea-methanol, and wherein the weight ratio of anticaking and suspending agent is 0.5-10% w/w of total composition,
e) fillers selected from Ammonium Sulphate, Lactose, China clay/ Kaolin, Titanium dioxide, Talcum powder, and Diatomaceous earth, and wherein the weight ratio of fillers is 0.1-90% w/w of total composition,
f) de-foaming agent or anti-foaming agent selected from Siloxane polyalkyleneoxide, and wherein the weight ratio of anti-foaming agent is 0.2 to 1.0% w/w of total composition.
g) adjuvants selected from Alcohol Ethoxylates C9-C11, Mixture of C12-15, ethoxylated, Sulfosuccinates, and wherein the weight ratio of adjuvants is 1-5% w/w of total composition, and
the composition may further comprise binder selected from Polyvinylpyrrolidone and is present in the weight ratio of 2-10% w/w of total composition.

In one another embodiment, the water dispersible granules (WDG) formulation is prepared by mixing active and inactive ingredients and Pre-Blending for the preparation of homogenized mixture of active & Inert ingredient in blender followed by milling this homogenized mixture in ACM-30. Mixing in post blender and unloading the homogenous material for granulation. Dough formation is done in sigma mixture and then Granular formation through extruder. Transferring the granules in FBD for removal of excess water followed by transferring in vibro shifter. After this the final product is collected and packed.

As disclosed in prior art, it is common practice to incorporate stabilizers and/or safeners into herbicidal formulations to mitigate the phytotoxic effects of Imazethapyr. However, this approach is contrary to the innovative concept of the present invention. In a preferred embodiment, the compositions of the present invention do not require the addition of any antioxidants, safeners, or stabilizers, thereby simplifying the formulation and avoiding the need for additional chemical components.

Although implementations for invention have been described in a language specific to structural features and/or methods, it is to be understood that the description or any part thereof are not necessarily limited to the specific features or methods described. Rather, the specific features and methods are/will be disclosed in the examples/complete specification of implementations for the invention.

EXAMPLES
The present invention will now be explained in detail by reference to the following formulation examples and a test example, which should not be construed as limiting the scope of the present invention.
Example 1: Oil based suspension concentrate of Haloxyfop R-methyl 9.8 % + Imazethapyr 7.5% (AAVP-HI02)
Chemical Composition Function % w/w
Haloxyfop-R- methyl Active 9.8
Imazethapyr Active 7.5
Fatty alcohol ethoxylate Dispersant 12
Organic Silicates Rheological Modifier 10
Fused Silica Antisettling agent 3
polydimethylsiloxane Antifoamer 2
ethylene glycol Antifreeze 6
Methyl Soyate solvent QS

Stability study of Haloxyfop-R- methyl ester 9.8% + Imazethapyr 7.5% Oil based suspension concentrate (Table 2):
Table 2:
Parameters Specification
(In house) Initial Stability (for 14 days)
54±2 0C 0±20C
Description Off white colour granules Complies Complies Complies
Haloxyfop-R-methyl content, %m/m 9.31 to 10.29 10.05 9.98 10.05
Imazethapyr content, %m/m 7.13 -8.25 8.20 8.10 8.20
Haloxyfop-R-methyl Suspensibility, %m/m Min. 80 94.52 94.12 94.36
Imazethapyr Suspensibility percent, %m/m Min. 80 98.47 98.58 99.16
pH range (1% aq. Suspension) 4-6 5.21 5.36 5.38
Persistent Foaming in ml Max. 60 40 40 46
Viscosity at spindle no. 63, 60 rpm 200-400 cps 320 330 337

The novel oil based suspension concentrates of Haloxyfop-R- methyl ester 9.8% + Imazethapyr 7.5% meets all in-house specifications for storage stability studies in laboratory (at 54±2oC & at 0±2oC for 14 days).

Example 2: Water dispersible granules (WG or WDG) formulation of Haloxyfop R-methyl 9.8 % + Imazethapyr 7.5% (AAVP-HI01)
Chemical Composition Percent (% w/w)
Haloxyfop-R- methyl ester 9.8
Imazethapyr 7.5
Fatty acids methyltauride, sodium salt 8.00
Sodium Lignosulfonate 4.00
Sodium Alkyl Naphthalene sulfonate , 10.0
Ammonium sulphate 12.0
Mixture of C12-15, ethoxylated 2
Silicone antifoam 2.0
Precipitated Silica 5.0
China Clay QS

Stability study of Haloxyfop-R- methyl ester 9.8% + Imazetahpyr 7.5% Water Dispersible
Granule (WDG or WG) composition (Table 3):
Table 3:
Parameters Specification (In house) Initial Stability (for 14 days)

At 54 ± 2 0C At 0 ±20C
Description Off white colour granules Complies Complies Complies
Haloxyfop-R-methyl ester content percent by mass 9.31 to 10.29 9.87 9.80 9.86
Imazethapyr content percent by mass 7.13 -8.25 7.59 7.56 7.59
Haloxyfop-R-methyl ester suspensibility percent by mass, Min. 70 94.52 94.12 94.36
Imazethapyr suspensibility percent by mass, Min. 70 94.47 93.58 94.16
Wettability in seconds, Max. 60 16 17 17
Wet sieving, passing
through 75 micron IS
sieve, percent by mass min. 98 99.6 99.3 99.5
Persistent Foaming in ml, Max. 60 27 28 26
Moisture content, percent by mass, Max. 2 1 0.7 1

The WDG formulation of present invention comprising Haloxyfop-R- methyl ester 9.8% + Imazethapyr 7.5% meets all in-house specifications for storage stability studies in laboratory (at 54±2oC & at 0±2oC for 14 days).

RESULTS:
Evaluation of the present herbicidal composition under field condition for bio-efficacy and phytotoxicity:

The herbicidal formulations designated as AAVP-HI01 (which contains Haloxyfop-R methyl at 9.8% + Imazethapyr at 7.5% in water-dispersible granules) and AAVP-HI02 (with Haloxyfop-R methyl at 9.8% +Imazethapyr at 7.5% in oil dispersion) with different treatments were assessed for their effectiveness against grasses, sedges, and broad-leaved weeds in soybean crop. This evaluation was compared to solo formulations as well as various combination formulations serving as standard checks across different recipe types, including SC, EC, ME, and SL. Phytotoxicity due to application of the herbicidal compositions on Soybean crop was also evaluated. A field experiment was conducted in Bidar, Karnataka on the Soybean crop during Kharif season 2023. The crop was raised with recommended package of practices. Soybean variety - DSB-21 was sown on July 9, 2023, in rows, 30 cm apart. The experiment was conducted in randomised block design consisting of a total of 14 treatments. The experiment was replicated thrice.
The detail of the experiment is mentioned hereunder:
Plot size: 25 sq. mt. (with 1 m buffer between plots to avoid drift of chemicals)
Application Time: 15 DAS (Days after sowing)
Spray Volume: 500 Liter water per hectare
Application Equipment: Manually operated knapsack sprayer fitted with flat fat nozzle
Agronomic practices: All the required agronomic practices followed except herbicidal application.
Method of Application: Foliar spray
Treatment detail:
T. No. Treatments Dose g or ml /ha
T1 AAVP-HI01 900
T2 AAVP-HI01 1000
T3 AAVP-HI01 1100
T4 AAVP-HI01 1200
T5 AAVP-HI02 900
T6 AAVP-HI02 1000
T7 AAVP-HI02 1100
T8 AAVP-HI02 1200
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825
T10 Fomesafen 12% + Quizalofop ethyl 3% SC 1500
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5
T12 Haloxyfop R-Methyl 10.5% EC 1250
T13 Imazethapyr 10% SL 1000
T14 Untreated Control -

Observations:
Weed control Efficiency (WCE%): Species wise weed count was recorded at 15 ,30 and 45 DAA (Days after application) by using (100 cm x 100 cm=1 m2) quadrant treatment wise in minimum 4 places randomly selected in the plot / replication. The average of each variable was used together with the sum of all the variables per plot to calculate the percentage of control.
The % weed control (WCE) observed was calculated as follows:
Weed Control Efficiency (%) = (A-B)/A X 100

A= Mean weed count in untreated control
B = Mean weed count in treated plot
The major weed flora in experimental field was Echinochloa colona, Dinebra retroflexa, Digitaria sangunalis, Cyperus spps, Amaranthus viride, Portulaca oleracea, Parthenium hysterophorus, Commelina benghalensis, Trianthema portulacastrum

Colby’s Method: The combined effect of herbicidal combinations is the sum of their individual effects. Colby’s method is an approach to evaluate the synergistic, additive, or antagonistic effects due to the interactions of two herbicides as a combination
Colby’s method calculates expected response, and a ratio is calculated between expected response and observed response.
The formula for expected response is as follows-
E = (X+ Y- ((X*Y /100)
X: Herbicide 1
Y: Herbicide 2
The observed response is the actual percent control achieved.

Colby’s ratio = Observed response (O)/Expected response (E).

If the ratio is,
< 1 = Antagonistic effect; 1= Additive effect; > 1 = Synergistic effect

Phytotoxicity: Visual observations on phytotoxicity parameters viz. yellowing, stunting, necrosis, epinasty and hyponasty were recorded after 3, 7, 14, and 21 days of application on the basis of given phytotoxicity rating scale:

Phytotoxicity Rating Scale (PRS)
Table 4:
Crop response/ Crop injury Rating
0-00 0
1-10% 1
11-20% 2
21-30% 3
31-40% 4
41-50% 5
51-60% 6
61-70% 7
71-80% 8
81-90% 9
91-100% 10

Yield and Yield Attributing Characteristics
Observations on grain yield and yield attributing parameters were observed at harvest of Soybean crop.

Table 5: Oil based suspension concentrate of Haloxyfop R-methyl + Imazethapyr with different concentrations and their respective efficacy @ dose 1000ml/ hac.
Haloxyfop R-methyl (%w/w) Imazethapyr (% w/w) Formulation stability Weed control efficiency Phytotoxicity on succeeding crops Sorghum

Yellowing Necrosis
7.0 10.0 complies 91.75 1 0
11.0 5.0 complies 55.32 1 1
5.0 8.0 complies 62.09 0 0
8.0 8.0 complies 88.07 0 0
6.0 6.0 complies 40.15 0 0

Effect of the herbicide’s application on the succeeding Crop
The effect following the application of different treatment of the herbicide’s composition along with the standard checks on the follow -up crop Green Gram was evaluated and observation on germination percentage, number of pods/plant and seed yield of green gram crop was evaluated. Observation on phytotoxicity symptoms like yellowing, stunting, necrosis, epinasty, hyponasty was also recorded at 7,14, 21 and 28 days after sowing.

Evaluation of safety of the herbicidal formulation having one of the components as ACCase Inhibitors and other ALS inhibitor on crops like Rice, Sorghum, Maize, which are sown as succeeding crop.
Separate trials were undertaken with the different treatments of the herbicidal formulations designated as AAVP-HI01 (which containing Haloxyfop-R methyl at 9.8% + Imazethapyr at 7.5% in water-dispersible granules form) and AAVP-HI02 (with Haloxyfop-R methyl 9.8% +Imazethapyr 7.5% in oil dispersion form) along with solo formulations and few combinations as standard checks to evaluated the safety on few cereal crops like Rice, Sorghum, Maize, which are not tolerant to ACCase Inhibitors and ALS inhibitors. These crops were sown as a succeeding crop after Soybean crop where the AAVP-HI01 (which containing Haloxyfop-R methyl at 9.8% + Imazethapyr at 7.5% in water-dispersible granules form) and AAVP-HI02 (with Haloxyfop-R methyl 9.8% +Imazethapyr 7.5% in oil dispersion form) was used to control the weeds.

Observation on Phytotoxicity symptoms on the succeeding crops viz. Sorghum, Maize and Rice crops were observed on 7, 14, 21 and 28 days after sowing.
Table 6: Effect of treatments on Weed Control Efficiency in Soybean Crop against Grassy Weeds
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at WCE (%) at WCE (%) at Percent control of total grassy weeds (%)
15 DAA 30DAA 45 DAA
T1 AAVP-HI01 900 84.33 82.52 80.32 82.39
T2 AAVP-HI01 1000 85.36 84.43 82.88 84.22
T3 AAVP-HI01 1100 86.78 86.04 83.71 85.51
T4 AAVP-HI01 1200 89.25 88.50 85.23 87.66
T5 AAVP-HI02 900 89.48 88.00 82.54 86.67
T6 AAVP-HI02 1000 92.58 91.40 86.94 90.31
T7 AAVP-HI02 1100 94.96 92.78 87.96 91.90
T8 AAVP-HI02 1200 96.03 94.32 89.56 93.30
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825 82.23 81.08 76.96 80.09
T10 Fomesafen 12% + Quizalofop ethyl 3% SC 1500 81.76 79.46 77.95 79.72
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5 78.22 77.19 74.90 76.77
T12 Haloxyfop R-Methyl 10.5% EC 1250 62.21 59.40 55.03 58.88
T13 Imazethapyr 10 % SL 1000 52.92 50.48 46.74 50.05
T14 Untreated Control - 0.00 0.00 0.00 0.00

*DAA: Days after application

Table 7: Effect of treatments on Weed Control Efficiency in Soybean Crop against Broadleaf Weeds

Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at WCE (%) at WCE (%) at Total Broad leaf weeds control (%)
15 *DAA 30DAA 45 DAA
T1 AAVP-HI01 900 75.09 73.82 66.79 71.90
T2 AAVP-HI01 1000 79.78 77.44 71.79 76.33
T3 AAVP-HI01 1100 83.95 82.04 78.44 81.48
T4 AAVP-HI01 1200 87.45 85.41 83.05 85.30
T5 AAVP-HI02 900 79.75 78.11 73.29 77.05
T6 AAVP-HI02 1000 91.51 89.15 84.30 88.32
T7 AAVP-HI02 1100 94.23 93.12 90.81 92.72
T8 AAVP-HI02 1200 96.99 95.00 92.91 94.97
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825 83.73 79.61 64.93 76.09
T10 Fomesafen 12% + Quizalofop ethyl 3% SC 1500 81.19 75.94 60.68 72.60
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5 79.21 72.95 54.45 68.87
T12 Haloxyfop R-Methyl 10.5% EC 1250 4.18 7.02 6.26 5.82
T13 Imazethapyr 10 % SL 100 69.99 66.29 62.66 66.31
T14 Untreated Control - 0.00 0.00 0.00 0.00
*DAA means days after treatment.

Table 8: Effect of treatments on Weed Control Efficiency in Soybean Crop against Sedges
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at WCE (%) at WCE (%) at Total Sedges control (%)
15 DAA 30DAA 45 DAA
T1 AAVP-HI01 900 75.53 73.63 64.36 71.17
T2 AAVP-HI01 1000 79.23 76.92 69.61 75.25
T3 AAVP-HI01 1100 80.81 78.81 75.00 78.21
T4 AAVP-HI01 1200 83.45 80.22 77.00 80.22
T5 AAVP-HI02 900 79.05 78.34 75.83 77.74
T6 AAVP-HI02 1000 81.16 80.06 78.45 79.89
T7 AAVP-HI02 1100 84.51 82.42 80.94 82.62
T8 AAVP-HI02 1200 85.92 83.36 82.32 83.87
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825 74.47 69.86 66.71 70.35
T10 Fomesafen 12% + Quizalofop ethyl 3% SC 1500 73.06 67.66 59.53 66.75
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5 71.83 64.05 56.91 64.26
T12 Haloxyfop R-Methyl 10.5% EC 1250 1.76 3.61 3.18 2.85
T13 Imazethapyr 10% SL 1000 71.30 68.76 57.87 65.98
T14 Untreated Control - 0.00 0.00 0.00 0.00
*DAA means days after treatment.

Table 9: Synergistic activity of herbicidal compositions on grassy weeds in Soybean crop at 15 DAA

Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

15 DAA
T1 AAVP-HI01 900 84.33 1.03
T2 AAVP-HI01 1000 85.36 1.04
T3 AAVP-HI01 1100 86.78 1.06
T4 AAVP-HI01 1200 89.25 1.09
T5 AAVP-HI02 900 89.48 1.09
T6 AAVP-HI02 1000 92.58 1.13
T7 AAVP-HI02 1100 94.96 1.16
T8 AAVP-HI02 1200 96.03 1.17
T9 Haloxyfop R-Methyl 10.5% EC 1200 62.21 0.76
T10 Imazethapyr 10% SL 1000 52.92 0.64
*DAA means days after treatment.

Table 10: Synergistic activity of herbicidal compositions on grassy weeds in Soybean crop at 30 DAA
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

30 DAA
T1 AAVP-HI01 900 80.32 1.06
T2 AAVP-HI01 1000 82.88 1.09
T3 AAVP-HI01 1100 83.71 1.10
T4 AAVP-HI01 1200 85.23 1.12
T5 AAVP-HI02 900 82.54 1.09
T6 AAVP-HI02 1000 86.94 1.14
T7 AAVP-HI02 1100 87.96 1.16
T8 AAVP-HI02 1200 89.56 1.18
T9 Haloxyfop R-Methyl 10.5% EC 1200 55.03 0.72
T10 Imazethapyr 10% SL 1000 46.74 0.61
*DAA means days after treatment.

Table 11: Synergistic activity of herbicidal compositions on grassy weeds in Soybean crop at 45 DAA
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

45 DAA
T1 AAVP-HI01 900 82.39 1.04
T2 AAVP-HI01 1000 84.22 1.06
T3 AAVP-HI01 1100 85.51 1.08
T4 AAVP-HI01 1200 87.66 1.10
T5 AAVP-HI02 900 86.67 1.09
T6 AAVP-HI02 1000 90.31 1.14
T7 AAVP-HI02 1100 91.90 1.16
T8 AAVP-HI02 1200 93.30 1.17
T9 Haloxyfop R-Methyl 10.5% EC 1200 58.88 0.74
T10 Imazethapyr 10% SL 1000 50.05 0.63
*DAA means days after treatment.

Table 12: Synergistic activity of herbicidal compositions on total grassy weeds in Soybean crop
Tr. No.
Treatments Application Rate
(g or ml /ha) Percent control of total grassy weeds (%) Colby Ratio

T1 AAVP-HI01 900 82.13 1.03
T2 AAVP-HI01 1000 84.08 1.06
T3 AAVP-HI01 1100 85.51 1.07
T4 AAVP-HI01 1200 87.54 1.10
T5 AAVP-HI02 900 86.67 1.09
T6 AAVP-HI02 1000 89.89 1.13
T7 AAVP-HI02 1100 91.04 1.14
T8 AAVP-HI02 1200 92.67 1.16
T9 Haloxyfop R-Methyl 10.5% EC 1200 59.00 0.74
T10 Imazethapyr 10% SL 1000 50.12 0.63
DAA means days after treatment.

Table 13: Synergistic activity of herbicidal compositions on broad leaf weeds in Soybean crop at 15 DAA
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

15 DAA
T1 AAVP-HI01 900 75.09 1.05
T2 AAVP-HI01 1000 79.78 1.12
T3 AAVP-HI01 1100 83.95 1.18
T4 AAVP-HI01 1200 87.45 1.23
T5 AAVP-HI02 900 79.75 1.12
T6 AAVP-HI02 1000 91.51 1.28
T7 AAVP-HI02 1100 94.23 1.32
T8 AAVP-HI02 1200 96.99 1.36
T9 Haloxyfop R-Methyl 10.5% EC 1200 4.18 0.06
T10 Imazethapyr 10% SL 1000 69.99 0.98
DAA means days after treatment.

Table 14: Synergistic activity of herbicidal compositions on broad leaf weeds in Soybean crop at 30 DAA
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

30 DAA
T1 AAVP-HI01 900 73.82 1.08
T2 AAVP-HI01 1000 77.44 1.13
T3 AAVP-HI01 1100 82.04 1.19
T4 AAVP-HI01 1200 85.41 1.24
T5 AAVP-HI02 900 78.11 1.14
T6 AAVP-HI02 1000 89.15 1.30
T7 AAVP-HI02 1100 93.12 1.36
T8 AAVP-HI02 1200 95.00 1.38
T9 Haloxyfop R-Methyl 10.5% EC 1200 7.02 0.10
T10 Imazethapyr 10% SL 1000 66.29 0.97
DAA means days after treatment.

Table 15: Synergistic activity of herbicidal compositions on broad leaf weeds in Soybean crop at 45 DAA
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) at Colby Ratio

45 DAA
T1 AAVP-HI01 900 66.79 1.03
T2 AAVP-HI01 1000 71.79 1.10
T3 AAVP-HI01 1100 78.44 1.21
T4 AAVP-HI01 1200 83.05 1.28
T5 AAVP-HI02 900 73.29 1.13
T6 AAVP-HI02 1000 84.30 1.30
T7 AAVP-HI02 1100 90.81 1.40
T8 AAVP-HI02 1200 92.91 1.43
T9 Haloxyfop R-Methyl 10.5% EC 1200 6.26 0.10
T10 Imazethapyr 10% SL 1000 62.66 0.96
DAA means days after treatment

Table 16: Synergistic activity of herbicidal compositions on total broad leaf weeds in Soybean crop
Tr. No.
Treatments Application Rate
(g or ml /ha) Percent control of total broadleaf weeds (%) Colby Ratio

T1 AAVP-HI01 900 71.90 1.05
T2 AAVP-HI01 1000 76.33 1.12
T3 AAVP-HI01 1100 81.48 1.19
T4 AAVP-HI01 1200 85.30 1.25
T5 AAVP-HI02 900 77.05 1.13
T6 AAVP-HI02 1000 88.32 1.29
T7 AAVP-HI02 1100 92.72 1.36
T8 AAVP-HI02 1200 94.97 1.39
T9 Haloxyfop R-Methyl 10.5% EC 1200 5.82 0.09
T10 Imazethapyr 10% SL 1000 66.31 0.97

Table 17: Synergistic activity of herbicidal compositions on sedges in Soybean crop
Tr. No.
Treatments Application Rate
(g or ml /ha) WCE (%) of Sedges Colby Ratio

T1 AAVP-HI01 900 71.17 1.06
T2 AAVP-HI01 1000 75.25 1.12
T3 AAVP-HI01 1100 78.21 1.17
T4 AAVP-HI01 1200 80.22 1.20
T5 AAVP-HI02 900 77.74 1.16
T6 AAVP-HI02 1000 79.89 1.19
T7 AAVP-HI02 1100 82.62 1.23
T8 AAVP-HI02 1200 83.87 1.25
T9 Haloxyfop R-Methyl 10.5% EC 1200 2.85 0.04
T10 Imazethapyr 10% SL 1000 65.98 0.99

Table 18: Effect of the herbicidal treatments on phytotoxicity of Soybean crop
Symptoms Yellowing Necrosis Stunting Epinasty Hyponasty
*Days after application (DAA)
*Days after application (DAA) *Days after application (DAA) *Days after application (DAA) *Days after application (DAA)
Tr. No. *3 7 14 21 3 7 14 21 3 7 14 21 3 7 14 21 3 7 14 21
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T9 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T10 1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T11 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T12 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T13 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T14 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
DAA means days after treatment

Table 19: Effect of the herbicidal treatments on yield and yield parameter of Soybean crop
Tr. No.
Treatments
Application Rate (g or ml/ha) Plant Height (cm) No. of pods per plant Seed Yield
(kg/ha)
T1 AAVP-HI01 900 33.87 25.88 1197
T2 AAVP-HI01 1000 35.42 27.72 1232
T3 AAVP-HI01 1100 36.47 29.85 1245
T4 AAVP-HI01 1200 39.83 31.54 1362
T5 AAVP-HI02 900 37.25 28.32 1292
T6 AAVP-HI02 1000 36.19 34.85 1501
T7 AAVP-HI02 1100 40.52 35.14 1539
T8 AAVP-HI02 1200 39.12 37.24 1610
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825 34.8 27.34 1218
T10 Fomesafen 12% + Quizalofop-ethyl 3% SC 1500 32.54 24.57 1174
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5 31.54 23.19 1121
T12 Haloxyfop R-Methyl 10.5% EC 1250 26.84 21.16 1017
T13 Imazethapyr 10% SL 1000 29.67 22.41 1091
T14 Untreated Control - 24.24 18.58 841

Table 20: Effect of the herbicidal treatments on yield and yield parameter on succeeding crop—Green gram.
Tr. No.
Treatments
Application Rate (g or ml/ha) Germination
(%) No. of pods per plant Seed Yield
(kg/ha)
T1 AAVP-HI01 900 97.8 15.2 417.33
T2 AAVP-HI01 1000 95 17.8 418.67
T3 AAVP-HI01 1100 94.8 14.2 411.00
T4 AAVP-HI01 1200 95.2 16.6 409.00
T5 AAVP-HI02 900 98.8 13.8 402.71
T6 AAVP-HI02 1000 94.2 14.6 407.17
T7 AAVP-HI02 1100 95.7 16.8 421.23
T8 AAVP-HI02 1200 96.4 18.6 406.17
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME 825 92.4 13.4 381.23
T10 Fomesafen 12% + Quizalofop ethyl 3% SC 1500 89.7 12.6 377.90
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC 437.5 90.6 15.8 363.83
T12 Haloxyfop R-Methyl 10.5% EC 1250 97.8 16.6 410.33
T13 Imazethapyr 10% SL 1000 93.5 14.4 381.00
T14 Untreated Control - 98.7 15.4 419.57

Table 21: Effect of the herbicidal treatments on phytotoxicity on succeeding crop- green gram
Symptoms Yellowing Necrosis Stunting Epinasty Hyponasty
*Days after application (DAS)
*Days after application (DAS) *Days after application (DAS) *Days after application (DAS) *Days after application (DAS)
Tr. No. *7 14 21 28 7 14 21 28 7 14 21 28 7 14 21 28 7 14 21 28
T1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T9 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T10 1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T11 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T12 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T13 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T14 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
*DAS means days after treatment.

Table 22: Safety evaluation of the herbicidal treatments on phytotoxicity on cereal crops when sown after Soybean crop harvest
Tr.
No. Treatments/ Days After Application Sorghum Maize Rice (Nursery)
Yellowing Necrosis Yellowing Necrosis Yellowing
Necrosis

7 14 21 7 14 21 7 14 21 7 14 21 7 14 21 7 14 21
T1 AAVP-HI01 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T2 AAVP-HI01 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T3 AAVP-HI01 1 0 0 0 0 0 1 0 0 0 0 0 1 0 0 0 0 0
T4 AAVP-HI01 1 0 0 1 1 0 1 0 0 1 1 0 1 0 0 0 0 0
T5 AAVP-HI02 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T6 AAVP-HI02 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T7 AAVP-HI02 1 0 0 1 1 0 0 0 0 0 0 0 0 0 0 0 0 0
T8 AAVP-HI02 1 0 0 1 1 0 1 0 0 1 1 0 0 0 0 0 0 0
T9 Haloxyfop-R-methyl 12.8 % + Imazethapyr 10% ME @ 825 ml/ha 3 2 1 2 2 2 1 0 0 1 1 0 0 0 0 0 0 0
T10 Fomesafen 12% + Quizalofop ethyl 3% SC @1500 ml/ha 2 2 1 0 0 0 1 0 0 0 0 0 0 0 0 0 0 0
T11 Quizalofop ethyl 7.5% + Imazethapyr 15% w/w EC @ 437.5 ml/ha 2 1 1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
T12 Haloxyfop R-Methyl 10.5% EC @1250 ml/ha 4 3 2 2 2 2 1 0 0 0 0 0 0 0 0 0 0 0
T13 Imazethapyr 10% SL @1000 ml 2 2 1 0 0 0 1 0 0 0 0 0 0 0 0 0 0 0
T14 Untreated Control 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

RESULT AND DISCUSSION:
From the data in Table 4 it is clearly evident that herbicidal composition represented as AAVP-HI01 and AAVP-HI02 effectively controlled the grassy weeds in Soybean crop and gave more than 80 % control till 45 days after application when compared to the standard checks. However, the oil based suspension concentrates of Haloxyfop R methyl + Imazethapyr (AAVP-HI02) is very effective in controlling the grassy weeds when compared to the WDG formulation of Haloxyfop R methyl + Imazethapyr (AAVP-HI01).

The broadleaf weeds were also effectively controlled in Soybean crop by the herbicidal composition represented as AAVP-HI01 and AAVP-HI02 as presented in Table 6. It has been found that the herbicidal composition (AAVP-HI02) with Oil based suspension concentrate gave more than 90 % control till 45 days after application with 1100 and 1200 ml/ha dose as compared to WDG herbicidal composition AAVP-HI01 which gave more than 78% and 83% control with 1100 and 1200 g/ha dose respectively.

From the data in Table 7, it has been found that the herbicidal composition represented as AAVP-HI01 and AAVP-HI02 gave more than 70 % control of Cyperus spp.in Soybean crop. However, when comparison between WDG herbicidal composition AAVP-HI01 and Oil based suspension concentrate AAVP-HI02 is drawn, it has been found that the OBSC herbicidal composition AAVP-HI02 performed better than the WDG herbicidal composition- AAVP-HI01. The herbicidal composition AAVP-HI02 at 1100 ml and 1200 ml/ha gave more than 82 % control of sedge- Cyperus spp. in Soybean crop.

Additionally, the data shown in Tables 8, 9, 10 and 11 indicate that both herbicidal compositions AAVP-HI01 and AAVP-HI02, in both WDG and OBSC (oil based suspension concentrate) formulations, exhibited a synergistic effect in managing grassy weeds in soybean crops at 15, 30, and 45 days. Similarly, the findings presented in Tables 12, 13, 14, 15 and 16 reveal that AAVP-HI01 and AAVP-HI02, in WDG and OBSC formulations, also produced a synergistic effect in controlling broadleaf weeds in soybean crops over the same time periods. The herbicidal composition AAVP-HI01 and AAVP-HI02 both gave synergistic effect in controlling the sedges in Soybean Crop as indicated from the data presented in Table 17.

No phytotoxicity symptoms like yellowing, necrosis, stunting, epinasty, hyponasty etc. were observed following the application of herbicidal compositions AAVP-HI01 and AAVP-HI02 on any of the observation days. The data indicating the results are detailed in Table 18 and 19.

The herbicidal composition AAVP-HI01 and AAVP-HI02 did not have any residual effect on the succeeding crop Green Gram. No phytotoxicity effects were observed any of the treatment of the herbicidal composition AAVP-HI01 and AAVP-HI02 at any days observed after sowing (Table 20 & 21).

Also, there was no significant difference amongst the various treatments following application on the succeeding crops.

The herbicidal composition AAVP-HI01 and AAVP-HI02 along with standard checks were
evaluated for their safety towards few cereal crops grown as a succeeding crop after Soybean crop in which combination of ACCase + ALS inhibitor herbicides (Haloxyfop R-methyl + Imazethapyr) were used to control weeds. The cereal crops chosen for the study were sorghum, maize, rice (Table 22). It is known that crops belonging to the graminaceous family are not tolerant to ACCase and ALS inhibitor herbicides. Hence, the study was undertaken to see the effect of the herbicidal combination containing ALS and ACCase inhibitor herbicides on the graminaceous crops when they are sown as a succeeding crop after Soybean crop where these herbicidal combinations were meant to be recommended to control the weeds. The crops were observed for yellowing of foliage, necrosis on leaf of the crop and observed for any visible recovery. The results in the Table 22 showed that the herbicidal combination AAVP-HI01 and AAVP-HI02 cause yellowing and necrosis at higher dose of 1100 and 1200 g or ml /ha which got recovered at 14 and 21 days respectively on succeeding crop Sorghum, Maize and Rice crops. The standard checks showed phytotoxic effect on the succeeding crop Maize, Sorghum and it did not recover from the damage after 14 days of sowing.

Thus, the herbicidal combination AAVP-HI01 and AAVP-HI02 is found to be safe for used in crops like Sorghum, Rice and Maize when sown as a succeeding crop.
,CLAIMS:WE CLAIM
1. An oil based suspension concentrate comprising synergistically effective amounts of Haloxyfop and Imazethapyr ester, salt and combinations thereof, wherein said Haloxyfop and Imazethapyr ester, salt and combinations thereof are taken in the mass ratio of 1: 0.77 to 11:8.47.

2. The oil based suspension concentrate as claimed in claim 1, wherein said composition comprises inactive ingredients selected from one or more of dispersing agent, solvent, antifoaming agent, anti-freezing agent, anti-settling agent, rheological modifier and optionally an adjuvant.

3. The oil based suspension concentrate as claimed in claim 2, wherein said dispersing agent is present in the weight ratio of 1-20%w/w of total composition, wherein said solvent is present in the weight ratio of 0.1-90% w/w of total composition, wherein said antifoaming agent is present in the weight ratio of 0.1-3%w/w of total composition, wherein said anti-freezing agent is present in the weight ratio of 0.1-20%w/w of total composition, wherein said anti-settling agent is present in the weight ratio of 0.1-8%w/w of total composition and wherein said rheological modifier is present in the weight ratio of 0.1-30%w/w of total composition.

4. The oil based suspension concentrate as claimed in claims 1 and 2, wherein said solvents are greener solvents and are selected from saturated esterified vegetable oil, unsaturated esterified vegetable oil, esterified methyl soyate oil, Methyl oleate, edible oil, non-edible oil, palm oil, esterified essential oil, and esterified non-essential oil.

5. The oil based suspension concentrate as claimed in claim 1, wherein said Haloxyfop R-methyl is present between 1-11% w/w of total composition.

6. The oil based suspension concentrate as claimed in claim 1, wherein said Imazethapyr is present between 0.77-8.47% w/w of total composition.

7. The oil based suspension concentrate as claimed in claim 1, wherein said composition excludes chemicals selected from antioxidants, safeners and stabilizers.

8. The oil based suspension concentrate as claimed in claim 1, wherein said composition comprises synergistic lower doses of 0.77-8.47% w/w of Imazethapyr and 1-11% of Haloxyfop R-methyl of total composition showing minimal to zero phytotoxicity on succeeding crops.