DESC:SYNERGISTIC HERBICIDAL COMBINATION OF HALOXYFOP AND OXYFLUORFEN
FIELD OF THE INVENTION
The present invention relates to the field of agrochemicals. More particularly, the present invention relates to a synergistic herbicidal emulsifiable concentrate comprising a) haloxyfop; and b) oxyfluorfen. Further, the present invention relates to a synergistic herbicidal combination which is used for controlling undesirable plants and weeds. The present invention further relates to a process for preparing such composition and a method of using such composition effectively.
BACKGROUND OF THE INVENTION
Control of weeds is extremely important in achieving high crop efficiency. Herbicides help to minimize crop damage by controlling the growth of weeds. The use of two or more appropriate active ingredients in specific dose ratios leads to synergism in crop protection. In addition to this, often highly destructive weeds can be difficult to control and may develop resistance to commercial herbicides. Many products are commercially available for these purposes, but there is still a continues need to develop new herbicidal combinations which are more effective, less costly, less toxic, environmentally safer and have different sites of action.
Onion (Allium cepa) is a crucial crop in India, significantly contributing to the agricultural economy and exports. In 2024, onion production in India faced a decline of approximately 19.84%, dropping to 242.12 lakh tons due to unfavorable weather conditions and pest infestations. Weeds pose a significant challenge to onion cultivation due to the crop’s slow initial growth and limited competitiveness. These weeds not only reduce bulb quality and complicate harvesting but also serve as hosts for pests and diseases. Hence, making effective weed control is crucial for optimal yield and quality.
The biggest challenge in field of crop protection is to reduce the dosage rate of active ingredients to diminish or circumvent environmental or toxicological effects without compromising on effective crop protection against weeds, in addition to long lasting and broad-spectrum of weed control. Another challenge is to reduce the excessive application of solo chemical compounds or herbicide which invariably helps in rapid selection of weeds and aid in developing natural or adapted resistance against the active compound in question.
Therefore, it is indeed necessary to use the herbicide combinations in lower doses, fast acting with the different modes of action that can provide long lasting control against broad spectrum weed control and check the resistance development in weeds. The composition should have high synergistic action, no cross resistance to existing herbicides, avoid excess loading of the toxicant to the environment and negligible impact to environmental safety. A need also exists for synergistic herbicidal compositions which could be physico-compatible formulations in the form of storage stable, safely packed, ready to use formulation.
Haloxyfop and oxyfluorfen are well-known herbicides with complementary modes of action provide broad-spectrum of weed control. Several studies and literature describe the about this combination.
CN102349527 describes a herbicidal composition comprising haloxyfop combined with one or more diphenyl ether herbicides, sulfonylurea herbicides, or benzothiadiazinone herbicides. This document exemplifies haloxyfop and oxyfluorfen in dispersible oil suspension. Dispersible oil suspension of this combination has drawbacks, such as the instability from particle sedimentation, the challenge of re-dispersing settled particles, component layering or separation, poor coverage from large particle size, and worries about the environmental impact depending on the oil used, particularly if the suspension is not properly formulated with the right dispersants to mitigate the problem of oil slick formation.
Haloxyfop and oxyfluorfen are widely used as herbicides, targeting grass and broadleaf weeds, respectively. However, their combination in an EC formulation presents several challenges like, haloxyfop is lipophilic, while oxyfluorfen has limited solubility in conventional organic solvents. Incompatibility can lead to sedimentation, crystallization, or layering over time. Both active ingredients degrade under UV exposure, reducing effectiveness.
The present invention overcomes these challenges by providing a emulsifiable concentrate (EC) formulation with optimized solvents, emulsifiers, and stabilizers to ensure long-term stability, economic and field efficacy.
OBJECTS OF THE INVENTION
The main objective of the present invention is to provide a synergistic herbicidal emulsifiable concentrate comprising a) haloxyfop; and b) an oxyfluorfen.
Another object of the present invention is to provide a herbicidal mixture or combination which solves at least one of the major problems discussed above like improving the formulation safety, storage stability, reducing the cost of the combination and addressing the transportation difficulties with improved environmental safety by reducing toxicity and residue deposit in soil and in crops by providing a stable, easy-to-use EC formulation of haloxyfop and oxyfluorfen that offers an enhanced herbicidal performance and mitigates the phytotoxicity without the need of additional crop safeners or plant health additives.
Yet another objective of the present invention is to provide a synergistic herbicidal composition which offers a broader and more complete spectrum of weed control.
Yet another objective of the present invention is to provide a synergistic herbicidal composition which provides better control of weeds at lower use rates, and which gives good residual control.
Yet another object of the present invention is to provide a method of improving the plant health or increasing yield in a crop by the application of a synergistic herbicidal combination.
The present inventive formulation provides enhanced broad-spectrum weed control that efficiently targets broadleaf and grassland weeds. The new formulation has increased stability and shelf life by avoiding deterioration, haziness, and phase separation. Having superior absorption and adherence to plant surfaces, it also exhibits reduced phytotoxicity.
The details of one or more embodiments of this disclosure are set forth in the accompanying description below and other features, objects, and advantages will be apparent from the description.
SUMMARY OF THE INVENTION
The present invention provides a synergistic emulsifiable concentrate composition comprising:
a) haloxyfop or an agriculturally acceptable salts or esters thereof;
b) oxyfluorfen;
c) at least one agrochemical acceptable excipient.
The present invention relates to particularly in specific selected amount of haloxyfop in an amount of 1 to 25% w/w and oxyfluorfen in an amount of 5 to 25% w/w, along with agriculturally acceptable adjuvants in particular amounts.
In accordance with one aspect of the present invention, provided is a synergistic emulsifiable concentrate composition comprising active content of haloxyfop in an amount of 1 to 25% w/w and active content of oxyfluorfen in an amount of 5 to 25 % w/w.
Yet another aspect of the present invention is having synergistic emulsifiable concentrate formulation with significant broad-spectrum bio-efficacy, stable, safety upon use, environmental protection, low toxicity and not creating phytotoxicity to any part of the plant. Therefore, one aspect of present invention is to use adjuvant particularly the emulsifier, solvent and/or co-solvent which results present emulsifiable concentrate having excellent rain fastness property and emulsification property after application.
It is another object and advantage of the present invention to provide a synergistic herbicidal composition which provides superior control and treatment of weeds compared to individual haloxyfop and oxyfluorfen and having enhanced bio-efficacy then other early post and post emergence present in market.
It is a further object and advantage of the present invention to provide a synergistic emulsifiable composition which provides longer duration control of weeds in Onion crop, which helps in reducing the multiple herbicide application cost of farmers.
Yet another aspect of the present invention is to prepare composition in the form easy to use for farmers and can be prepared without much complex manufacturing process.
In accordance with another aspect of the present invention, there is provided a process / method for preparing herbicidal composition, the process comprising the step of mixing the active compound combination of Haloxyfop and Oxyfluorfen with emulsifiers and / or solvents or other formulation ingredients or acceptable carriers.
In accordance with another aspect of the present invention, there is provided method(s) for effectively controlling weeds infestation in useful crops, in particularly of an Onion crop, comprising the step of treating a locus with a composition comprising haloxyfop and oxyfluorfen.
The composition according to the present invention can be used against a large number of agronomically important weeds, such as (Echinochloa colona (Jungle rice), Echinochloa crus-galli (Barnyard grass), Dactyloctenium aegyptium (Crowfoot grass), Cynodon dactylon (Bermuda grass), Eleusine indica (Goosegrass), and Setaria glauca (Yellow foxtail)) and broadleaf species (Amaranthus viridis (Green amaranth), Trianthema portulacastrum (Horse purslane), Digera arvensis (False amaranth), Chenopodium album (Common lambsquarters), Portulaca oleracea (Common purslane), Parthenium hysterophorus (Congress grass), and Cleome viscosa (Asian spiderflower)) and sedges (Cyperus rotundus (Purple nutsedge), Cyperus esculentus (Yellow nutsedge), and Fimbristylis miliacea (Grass-like fimbry)). The composition according to the invention is suitable for all methods of application conventionally used in agriculture, e.g. Early post and post -emergence application. The composition according to the invention is suitable especially for controlling weeds in onion crops.
Other objects and advantages of the present invention will be apparent to those skilled in the art from the description and appended claims provided below.
DETAILED DESCRIPTION OF THE INVENTION
The present disclosure / specification refers to a synergistic herbicidal composition and the process for the preparation for crop protection. As used herein, the terms “comprises”, “comprising”, “includes”, “including”, “has”, “having”, “contains”, “containing”, “characterized by” or any other variation thereof, are intended to cover a non-exclusive inclusion, subject to any limitation explicitly indicated. For example, a composition, mixture, process or method that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, mixture, process or method.
The term “combination” can be replaced with the words “mixture” or “composition” defined or refers to as combining two or more active ingredients formulated in desired formulations. The term “pesticide” as used in this specification refers to a substance or mixture of substances intended for preventing, destroying, repelling, or mitigating any pest or weeds which causes damage to the crop. Herbicides, insecticides, and fungicides are mainly used as pesticides which control weeds, insect pests and disease-causing pathogens, respectively that eventually lead to high yield from the crops. The term “Herbicides” as used in this specification refers to a substance or mixture of substances used to kill, control or eliminate unwanted plants or vegetation, commonly known as weeds that cause economic damage the crops and ornamental plants. The term “synergism” as used in this specification refers to the interaction between two or more active components or other factors that produce a combined effect or properties which is greater than the sum of their separate effects or properties. Thus, the present invention involves the mixture of two active ingredients which have increased efficacy and broad spectrum of weed control when compared to individual use and admixture of those components. The expression of various quantities in the terms of “% w/w” means the percentage by weight, relative to the weight of the total composition unless otherwise specified. The expression of various quantities in the terms of “g.a.i/ha” means the gram active ingredient per hectare. The term “adjuvants” is similar to “inactive excipients” or “excipients” or “agriculturally acceptable adjuvants or “agrochemical acceptable excipients” or agriculturally acceptable excipients” and used interchangeably in this whole specification. In accordance with the present invention, the synergistic composition comprises one or more agriculturally acceptable adjuvants.
The inventors of the present invention conducted extensive study and came up with suitable composition comprising effective amounts of specific adjuvants. The present invention involves the mixture of active ingredients selected from haloxyfop and oxyfluorfen in emulsifiable concentrate (EC) formulation and are described herein thereof. The present invention involves the mixture of two active ingredients which are classified under aryloxy phenoxy propionate herbicides and diphenyl ether herbicides and are described herein thereof.
Aryloxyphenoxypropionate (AOPP) are a selective, systemic and post-emergence class of herbicides that inhibit the synthesis of fatty acids and destroy the membrane structure by inhibiting the activity of acetyl-CoA carboxylase (ACCase) in the chloroplasts of weeds to achieve herbicidal effects. Haloxyfop is a selective, systemic, broad-spectrum commodity herbicide of aryloxy phenoxy propionate class for the control of grass weeds. Originally it was produced as a racemic mixture. The R-isomer is the herbicidal active compound. Mode of action is eliminating the weeds by inhibiting lipid synthesis and inducing oxidative stress. Preferably haloxyfop involves inhibiting the enzyme acetyl coenzyme A carboxylase (ACCase) by converting acetyl-CoA to malonyl-CoA, which is essential for lipid synthesis in plants ultimately leading to the death of grassy weeds. After application, susceptible grassy weeds treated with Haloxyfop exhibit symptoms such as chlorosis (yellowing), necrosis (tissue death), stunting, and death of unwanted weeds. These symptoms result from the disruption of lipid synthesis and subsequent impairment of vital cellular processes. Another component is the diphenyl ethers class of herbicide which belongs to one of the most important agricultural herbicide groups. Diphenyl ethers class are broad spectrum, contact, pre- and post-emergence class of herbicide. Diphenyl ethers herbicides inhibit the protoporphyrinogen oxidase, an enzyme which catalyzes the oxidation of a key porphyrin intermediate on the biosynthetic pathway to chlorophyll, the pigment of photosynthesis. It controls selected grasses, sedges and broad leaf weeds. Oxyfluorfen is a selective pre and post emergent herbicide used to control certain annual broadleaf and grassy weeds in vegetables, fruit, cotton, ornamentals and on non-crop areas. Mode of action is by inhibiting the protoporphyrinogen oxidase, leading to irreversible cell membrane damage. It is a contact herbicide, and light is required for it to affect target plants.
In an embodiment of the present invention provides a synergistic herbicidal composition comprising:
a) haloxyfop or an agriculturally acceptable salt or ester thereof; and
b) oxyfluorfen.
In one embodiment of the present invention, haloxyfop is (±)-2-[4-[[3-chloro-5 (trifluoromethyl)-2-pyridinyl]oxy]phenoxy]propanoic acid and possesses the following structure:

In another embodiment of the present invention, haloxyfop also refers to an enantiomer of (±)-2-[4-[[3-chloro-5-(trifluoromethyl)-2-pyridinyl]oxy]phenoxy]propanoic acid, or a mixture of enantiomers thereof. In one embodiment, haloxyfop refers to (R)-(+)-2-[4-[[3- chloro-5-(trifluoromethyl)-2-pyridinyl]oxy]phenoxy]propanoic acid, which is also commonly known as haloxyfop-P. In another embodiment, haloxyfop refers to (5)-(-)-2-[4-[[3-chloro-5-(trifluoromethyl)-2-pyridinyl]oxy]phenoxy]propanoic acid.
In yet another embodiment of the present invention, an agriculturally acceptable ester or salt of haloxyfop encompasses all the agriculturally acceptable esters or salts of haloxyfop known in the art or provided herein. In one embodiment, the agriculturally acceptable salt of haloxyfop is a sodium salt (e.g., haloxyfop-sodium). In one embodiment, the agriculturally acceptable ester of haloxyfop is a methyl ester (e.g., haloxyfop-methyl or haloxyfop-P-methyl) or a 2-ethoxyethyl (etotyl) ester (e.g., haloxyfop-etotyl or haloxyfop-P-etotyl).
In an embodiment of the present invention, unless otherwise indicated, oxyfluorfen is 2-chloro-l-(3-ethoxy4-nitrophenoxy)-4-(trifluoromethyl)benzene and possesses the following structure:

Oxyfluorfen is a broad-spectrum, pre- and post-emergent herbicide used to control certain annual weeds in vegetables, fruit and other crops which inhibit protoporphyrinogen oxidase, leading to irreversible cell membrane damage.
In another embodiment of the present invention provides a synergistic herbicidal composition comprising:
a) haloxyfop or an agriculturally acceptable salt or ester thereof; and
b) oxyfluorfen.
wherein, haloxyfop is Haloxyfop-R-methyl.
In yet another embodiment of the present invention provides a synergistic herbicidal composition comprising:
a) haloxyfop or an agriculturally acceptable salt or ester thereof; and
b) oxyfluorfen.
wherein the weight ratio of haloxyfop to oxyfluorfen is from (1-25) : (5-25).
In yet another embodiment of the present invention provides a synergistic herbicidal composition comprising:
a) haloxyfop or an agriculturally acceptable salt or ester thereof; and
b) oxyfluorfen
c) at least one agrochemical acceptable excipient.
In one embodiment, an agrochemical acceptable excipient can be selected from but not limited to the group comprising liquid medium, surfactant, stabilizer, anti-freezing agent, anti-foaming agent, anticaking agent, dispersing agent, adjuvant and other auxiliaries. These are selected according to the respective types of formulation requirements, and which will facilitate in the preparation of different formulations.
The another aspect of the present embodiment, synergistic herbicidal composition comprising a combination of haloxyfop and oxyfluorfen; wherein haloxyfop and oxyfluorfen are present in the weight ratio of (1-25) : (5-25).
In another embodiment, the emulsifiable concentrate (EC) formulation of the present invention comprises:
a) haloxyfop;
b) oxyfluorfen;
c) emulsifier(s);
d) adjuvants;
e) solvent(s).
In yet another embodiment, the emulsifiable concentrate (EC) formulation of the present invention comprises:
a) about 1 to 25% haloxyfop by weight of the formulation;
b) about 5 to 25% oxyfluorfen by weight of the formulation;
c) about 5 to 30% emulsifier(s) by weight of the formulation;
d) about 0.5 to 15% adjuvant by weight of the formulation;
e) about 5% to 80 % solvent (Solvent C IX) by weight of the formulation.
In yet another embodiment, the emulsifiable concentrate (EC) formulation of the present invention preferably comprises:
a) about 9 % haloxyfop-R-methyl by weight of the formulation;
b) about 11.5 % oxyfluorfen by weight of the formulation;
c) about 0.1 to 10 % Calcium dodecyl benzene sulphonate by weight of the formulation;
d) about 0.1 to 10 % phenol styrenated by weight of the formulation;
e) about 0.1 to 10 % solvent naphtha (petroleum), heavy aromatic
f) about 0.1 to 10 % castor oil ethoxylate
g) about 5% to 80 % solvent (Solvent C IX) by weight of the formulation.

In another embodiment, the emulsifiable concentrate (EC) formulation of the present invention comprises:
a) about 9 % haloxyfop-R-methyl by weight of the formulation;
b) about 11.5 % oxyfluorfen by weight of the formulation;
c) about 5 % calcium dodecyl benzene sulphonate by weight of the formulation;
d) about 5 % phenol styrenated by weight of the formulation;
e) about 5 % solvent naphtha (petroleum), heavy aromatic by weight of the formulation;
f) about 5 % castor oil ethoxylate by weight of the formulation;
g) about 5% to 80 % solvent (Solvent C IX) by weight of the formulation.
In one embodiment of the present invention provides the process for preparing the emulsifiable concentrate (EC) composition.
Yet another embodiment of the present invention provides a process for the preparation of Emulsifiable concentrate (EC) compositions comprising the steps of: adding the required quantity of solvent C-IX into a clean and dry reactor and stir it slowly; adding the required quantity of oxyfluorfen under continuous stirring; adding the required quantity of haloxyfop slowly while stirring; adding the required quantity of emulsifier(s) slowly under continuous stirring; continuing the stirring for 1 hour to get desired homogenous bio effective emulsifiable concentrate solution comprising haloxyfop and oxyfluorfen. The sample was filtered, and the final composition was packed in the designated containers.
The emulsifier in the present invention has an important role in making present emulsifiable concentrate storage stable at different temperature conditions, and bioeffective. Basically, emulsifier allows the active ingredient in the solvents to mix with water to form an emulsion. Hence, due to the particular selection of emulsifier, present emulsifiable concentrate has good rain fastness property, wherein it has been adequately dried or has been absorbed by plant tissues so that it will still be effective after rainfall or irrigation and hydrolytic stability, wherein the ability of ingredients to withstand chemical decomposition in the presence of water when the instant invention is diluted with water for application. Further instant emulsifiable concentrate is stable even at lower atmospheric conditions of 0-10o C, making it suitable for colder conditions.
Synergistic emulsifiable concentrate composition of present invention comprises emulsifier which can be selected from the group comprising of, Pentadecyl phenol ethoxylate, Phenol styrenated (61788-44-1), Poly (oxy-1,2- ethanediyl), Tristyrylphenol ethoxylated, alpha-(tris(1-phenylethyl)phenyl-omega-hydroxy, calcium dodecyl benzene sulphonates (26264-06-2), Solvent naphtha petroleum heavy aromatic (64742-94-5), calcium salt of linear alkyl benzene sulphinic acid, lauryl alcohol ethoxylate, nonyl phenol ethoxylate, castor oil ethoxylate (61791-12-6), petroleum, blend of anionic & non-ionic surfactant and combination thereof, present in an amount in between 5% to 30% weight percent ratio with respect to said emulsifiable concentrate. According to preferred embodiment emulsifier used in the present invention is present in an amount in between 5% to 25% weight percent ratio with respect to said emulsifiable concentrate
Solvent and/or co-solvent used in present invention can be selected from the group comprising of, C9 aromatic solvent(Aromatic hydrocarbon mixture (Solvent C-IX)), NMP, DMF, Benzene, Xylenes, Cumene, 1,2,4-trimethyl-Benzene, 1,3,5-trimethyl-Benzene, ethylmethyl-benzene, ethyltoluene mixed isomers, Solvent naphtha, petroleum, light aromatic and combination thereof present in an amount in between 5% to 80 % weight percent ratio with respect to said concentrate. According to preferred embodiment solvent used in present invention present in an amount in between 10 % to 75% weight percent ratio with respect to said concentrate, wherein preferably solvent present in an amount in between 20% to 75% weight percent ratio with respect to said composition and co-solvent in an amount in between 0 to 30% weight percent ratio with respect to said composition.
An effective amount of emulsifier, solvent and / or co-solvent in the present invention leads the pesticides to enter the plant leaf after application of formulation with penetration occurring primarily through the leaf cuticle. The mechanism involved in penetration and movement into leaves via the leaf cuticle is by diffusion. Hence, emulsifier, solvent and / or co-solvent of present invention provides spreadable and translaminar property to the formulation which gives excellent synergistic mode of action in effective control of the target pest
Optionally, present emulsifiable concentrate comprises stabilizer can be selected one or more from 2,6-di-tert-butyl-p-cresol, butylhydroxyanisole, butylated hydroxytoluene (BHT), epoxidized soybean oil (ESBO) and methyl oleate. Optionally, anti-foaming agent to prevent formation of foam can be used in the present invention can be selected from the group comprising silicon defoamer, polydimethylsiloxane, polymethylhydrosiloxane and cyclomethicones. The antifoaming agent may facilitate spraying of insecticide while reducing the chances of the sprayer becoming clogged with foam or entrained air. Optionally, the present invention comprises anti-microbial agent selected from the group comprising of benzisothiazolinone, methylisothiazolinone, copper pyrithione, zinc pyrithione, commercially available with trade name PROXEL GXL®, which is a 20% aqueous dipropylene glycol solution of 1,2- benzisothiazolin-3-one.
The present invention provides a synergistic herbicidal composition having haloxyfop and oxyfluorfen and purpose thereof. The synergy of this herbicidal composition has two main effective components of haloxyfop and oxyfluorfen. This herbicidal composition acts by inhibiting the activity of acetyl-CoA carboxylase (ACCase) in the chloroplasts and inhibiting protoporphyrinogen oxidase, an enzyme which catalyzes the oxidation of a key porphyrin intermediate on the biosynthetic pathway to chlorophyll can generate efficient synergism in pre-emergence, early-post or post- emergence stages of crops and can enable broad spectrum satisfactory weed control and protect the several crop from sedges, grasses and broad leaf weeds for prolonged period of time at lower dose with no phytotoxic effect. Their different modes of actions, target two different sites resulting in effectiveness, crop safety and environmental friendliness as they are applied at doses lower than they were applied alone on the crop and increasing the probability of this herbicidal mixture as a valuable tool in weed control. It also prevents the weed crops from rejuvenation and further regeneration.
The composition according to the invention can be used against a large number of agronomically important weeds, such as (Echinochloa colona (Jungle rice), Echinochloa crus-galli (Barnyard grass), Dactyloctenium aegyptium (Crowfoot grass), Cynodon dactylon (Bermuda grass), Eleusine indica (Goosegrass), and Setaria glauca (Yellow foxtail)) and broadleaf species (Amaranthus viridis (Green amaranth), Trianthema portulacastrum (Horse purslane), Digera arvensis (False amaranth), Chenopodium album (Common lambsquarters), Portulaca oleracea (Common purslane), Parthenium hysterophorus (Congress grass), and Cleome viscosa (Asian spiderflower)) and sedges (Cyperus rotundus (Purple nutsedge), Cyperus esculentus (Yellow nutsedge), and Fimbristylis miliacea (Grass-like fimbry)).
Another embodiment of the present invention, the synergistic herbicidal composition of present invention used in different dose ratios shows effective weed control in broad spectrum of weeds and increases the crop yield, quality, and lesser dose ratios and shows no phytotoxicity compared to single components, admixture of those two components and other available market standards. By this the herbicidal composition of present invention archives synergistic effect along with economic value products and improved environmental safety by reducing toxicity and residue deposit in soil and in crops.
In another embodiment of the present invention, a method of controlling annual grasses, sedges and broad leaf weeds comprising synergistic herbicidal composition applying to the location of weed in effective amount.
In another embodiment of the present invention, the composition is used to manage weeds in crops by applying the formulation as early post and post-emergent to the weed populations at a rate of 900–1200 ml / ha.
In a preferred embodiment of the the present invention, the composition is used to manage weeds in crops by applying the formulation as early post and post-emergent to the weed populations at a rate of 975–1170 ml / ha.
In another embodiment of the present invention, the herbicidal composition obtained from the present invention, is used to control broadleaf weeds, sedges and annual grasses in rice, wheat, fruits, roots, tubers, vegetables, maize, grains, sugarcane, cereals, field crops, onion and various other crops for general weed control.
In another embodiment of the present invention, the synergistic herbicidal composition can be applied to early post-emergence or post-emergence stages for weed control by conventional spraying methods, such as foliar application etc., over the target areas of weeds or vegetation at same time avoiding excessive drift or runoff of the composition securing thorough coverage.
In another embodiment of the present invention, other alternative formulations other than described herein can be prepared using conventional processes and different methods known in the art by selecting appropriate agrochemical acceptable excipient(s) to get the suitable desired formulation of present invention combination.
Advantages of Present Invention:
1. The synergistic herbicidal composition of present invention can be used in early post-emergence, or post-emergence stages for effective weed control to increase the yield of crops compared to single components of composition, admixture of those components and market standards. This will help the farmers in controlling weeds in the entire crop cycle without any environmental pollution.
2. The innovative and synergistic herbicidal composition of present invention has different modes of actions, target two different sites resulting in effectiveness and provides better and broader spectrum of weed control in agricultural and non-agricultural fields.
3. The synergistic herbicidal composition of present invention is effective against broader spectrum of unwanted weeds compared to single component and market standards without any environmental pollution.
4. The synergistic herbicidal composition of the present invention avoids or reduces the damage of crops and shows no phytotoxicity.
It is to be understood that this disclosure is not limited to a particular compositions or specific constituents, which can, of course, vary and that the terminology used herein is for the purpose of describing embodiments only and is not intended to be limiting the scope of the invention. As used in this specification, the singular forms "a," "an," and "the" include plural referents unless the content clearly dictates otherwise, and equivalents thereof known to those skilled in the art and so forth. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this disclosure pertains. Although any methods and materials similar or equivalent to those described herein can be used in the practice for testing of the disclosure(s), of appropriate materials and methods are described herein.
EXAMPLES:
EXAMPLE 1: Formulations of Synergistic Herbicidal Composition of the Present Invention
TABLE 1: Emulsifiable Concentrate (EC) Formulation
S. No Ingredients Content (%w/w)
1 Haloxyfop-R-methyl 9
2 Oxyfluorfen 11.50
3 Calcium dodecyl benzene sulphonate 0.1 -10
4 Phenol styrenated 0.1 -10
5 Solvent naphtha (petroleum), heavy aromatic 0.1 -10
6 Castor oil ethoxylate 0.1 - 10
7 Aromatic Hydrocarbon Mixture (Solvent C-IX) Q.S. to make 100 %
Total 100

EXAMPLE 2: Process for Preparing the Emulsifiable Concentrate (EC) Composition:
i. adding the required quantity of solvent C-IX into a clean and dry reactor and start stirring;
ii. adding the required quantity of oxyfluorfen slowly, under continuous stirring;
iii. adding the required quantity of haloxyfop-R-methyl under continuous stirring;
iv. adding the required quantity of emulsifier under continuous stirring;
v. continuing the stirring for 1 hour to get desired homogenous bio effective emulsifiable concentrate solution comprising haloxyfop-R-methyl and oxyfluorfen.
EXAMPLE 3: Stability Study
Stability study of present invention a synergistic emulsifiable concentrate herbicidal composition was done for 14 days at ±54oC. Analysis of before heat stability test (BHST) and after heat stability test (AHST) was compared. Results revealed that present synergistic emulsifiable concentrate herbicidal compositions is stable. There is no specific active ingredient deterioration was observed in emulsifiable concentrate. Stability results are tabulated in Table -2.
TABLE 2: Stability Results
S No. Test Parameters / Specifications Composition Example
BHST* AHST*
1 Description: (Specification: Clear homogeneous stable liquid free from extraneous matter) Complies Complies
2 Active ingredient; Haloxyfop R-Methyl
(min. 8.1 to max. 9.90) 9.35 9.34
Active ingredient. Oxyfluorfen
(min. 10.81 to max. 12.19) 11.95 11.93
3 pH 1% aq. Solution (3.0 to 7.5) 5.68 5.87
4 Emulsion Stability Complies Complies
5 Cold stability 0°C Complies Complies
* BHST = before heat stability test (BHST); AHST = after heat stability test

EXAMPLE 4: Bio Efficacy and Phytotoxicity Tests of the Present Invention
Methodology:
When the crop is in its initial developmental stages the crop experiences high invasion of weed flora and upon their incursion, they compete with the crop parallelly for nutrients, light and other resources causing hinderance to crop growth and effects the productivity of the crop. Hence, timely management of weeds plays an important role in gaining good qualitative and quantitative yield.
TABLE 3: Details of Field Trials
Project Bio-efficacy and Phyto-toxicity evaluation of Haloxyfop 9% + Oxyfluorfen 11.50% EC against weeds in onion crop
Objective a) Bio-efficacy and Phyto-toxicity evaluation of Haloxyfop 9% + Oxyfluorfen 11.50% EC against weeds in onion crop.
b) Effect of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation on follow-up crop – Black gram
Product to be tested Herbicide
Crop Onion (Allium spp)
Variety Recommended variety
Target weeds Digitaria sanguinalis, Echinochloa colonum,
Trianthema portulacastrum, Portulaca oleracea, Amaranthus viridae, Cyprus rotundus, Fimbristylis miliaceae
Design RBD
Replications 3
Plot size 25-50 SQM
Time of spraying early post emergence / post emergence
Equipment for spraying Knap sack sprayer fitted with flat fan nozzle
The combined use of haloxyfop and oxyfluorfen as an herbicidal mixture offers a synergistic weed control strategy, enhancing efficacy and reducing the risk of resistance. The dual action of these herbicides provides a more comprehensive approach to weed management, targeting different biochemical pathways in weeds and ensuring improved onion crop performance. This combination not only broadens the spectrum of weed control but also maintains a more sustainable agricultural practice by reducing the chances of weed adaptation. By integrating herbicidal mixtures into onion farming, Indian agriculture can achieve better productivity, addressing both weed-related challenges and the need for higher yields despite fluctuating climatic conditions.
Table 4. Treatment Details
Treatments Treatment detail Dose / ha (ml / ha)
T1 Haloxyfop 9% + Oxyfluorfen 11.5% EC 780
T2 Haloxyfop 9% + Oxyfluorfen 11.5% EC 975
T3 Haloxyfop 9% + Oxyfluorfen 11.5% EC 1170
T4 Haloxyfop 10.5% EC 1200
T5 Oxyfluorfen 23.5% EC 850
T6 Propaquizafop 5% + Oxyfluorfen 12% EC 874
T7 Quizalofop ethyl 4% + Oxyfluorfen 6% EC 1000
T8 Hand weeding --
T9 Untreated Control --
Parameters of Observation:
The weeds controlled in each treatment are calculated as % weed controlled over untreated or controlled plot. The percent weed control is calculated by the following formula –

The weeds biomass build-up in treatments is calculated to know the weed control index of each treatment. The WCI – Weed Control Index is calculated by the following formula –

Synergism is the interaction or cooperation of two or more organizations, substances, or other agents to produce a combined effect greater than the sum of their separate effects. As described in the Herbicide Handbook of the Weed Science Society of America, Ninth Edition, 2007, p. 429, “synergism” [is] an interaction of two or more factors such that the effect when combined is greater than the predicted effect based on the response to each factor applied separately.
Colby's formula is applied to determine synergistic effect, as provided in WEEDS 1967, 15, 22.
E = (X + Y) – [(X × Y) / 100]
Wherein,
X= individual response of Haloxyfop
Y= individual response of Oxyfluorfen
E (Expected Control %) = expected (or predicted) control of combination of (X) + (Y) when applied
O (Observed Control %) = observed control of combination of (X) + (Y) when applied
Ratio: Observed Control % / Expected Control %
For Synergy, O/E > 1, means synergism observed.
Results:
The different types and species of weeds found in this experiment in onion (Allium spp) crop field were enlisted below,
Grasses: Digitaria sanguinalis, Echinochloa colonum.
Broad Leaved Weeds: Trianthema portulacastrum, Portulaca oleracea, Amaranthus viridae.
Sedges: Cyprus rotundus; Fimbristylis miliaceae

Table 5. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against grassy weeds.
Treatments Dose
(ml / ha) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average Percent
Weed
Control Colby’s ratio
D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c
T1 780 45.67 14.67 11 5 9 4 2 1 3 3 6.25 3.25 90.67 91.39 1.05 1.00
T2 975 47.00 15.33 4 3 2 2 0 0 3.45 2 2.3625 1.75 96.47 95.36 1.12 1.04
T3 1170 47.33 15.00 0 0 0 0 0 0 3.03 5 0.7575 1.25 98.87 96.69 1.15 1.06
T4 1200 46.67 16.33 34 12 21 9 24 11 26 14 26.25 11.5 60.82 69.54 0.71 0.76
T5 850 46.00 15.67 32 11 19 8 21 10 24 13 24 10.5 64.18 72.19 0.75 0.79
T6 874 46.33 14.33 39 15 41 16 7 5 11 9 24.5 11.25 63.43 70.20 0.74 0.77
T7 1000 48.33 14.67 40 16 44 19 49 22 53 27 46.5 21 30.60 44.37 0.36 0.48
T8 -- 46.00 14.00 1 1 1 2 22 2.5 19 6 10.75 2.875 83.96 92.38 - -
T9 -- 47.67 16.33 55 26 62 34 71 41 80 50 67 37.75 - - - -
DAA – Days after application; D. s – Digitaria sanguinalis; E. c – Echinochloa colonum
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against grassy weeds, specifically Digitaria sanguinalis (D.s) and Echinochloa colonum (E.c), was evaluated based on different doses of the herbicidal mixture, solo herbicide of the combination and market standards (competitor products) as different treatments while also checking the effect of manual practice of hand weeding and an untreated check for comparison. The pre-count of grassy weed populations before herbicide application was similar across treatments, with values ranging from 45.67 to 48.33 weeds per square meter for D. sanguinalis and 14.00 to 16.33 for E. colonum. A significant reduction in weed population was observed in treated plots compared to the untreated control, particularly at higher doses. Among all the treatments, T3 – Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha demonstrated the highest efficacy, completely eliminating both Digitaria sanguinalis and Echinochloa colonum by the 7th and 14th days after application (DAA) and maintaining near-complete suppression up to 35 DAA, resulting in an average weed control efficacy of 98.87% for D. sanguinalis and 96.69% for E. colonum over control plot. Similarly, the colby’s ratios of 1.15 and 1.06 respectively indicate a synergistic effect of the formulation. Haloxyfop 9% + Oxyfluorfen 11.5% EC 975 ml/ha also showed excellent control, with weed counts dropping to zero by 14 DAA and maintaining suppression up to 35 DAA, achieving 96.47% and 95.36% control of D. sanguinalis and E. colonum, respectively. The lowest herbicidal mixture dose - Haloxyfop 9% + Oxyfluorfen 11.5% EC 780 ml/ha provided slightly lower but still effective weed control, with an average efficacy of 90.67% for D. sanguinalis and 91.39% for E. colonum, showing gradual reduction over time.
Moderate weed control was observed in treatments T4 – Haloxyfop 10.5% EC (1200 ml/ha), T5 - Oxyfluorfen 23.5% EC (850 ml/ha), and T6 - Propaquizafop 5% + Oxyfluorfen 12% EC (874 ml/ha), which showed higher weed survival rates compared to the more effective treatments. T4 - Haloxyfop 10.5% EC (1200 ml/ha) recorded 60.82% and 69.54% control for D. sanguinalis and E. colonum, respectively. While, Oxyfluorfen 23.5% EC (850 ml/ha), and T6 - Propaquizafop 5% + Oxyfluorfen 12% EC (874 ml/ha) exhibited similar trends with control levels of 64.18% to 72.19%. Notably, T7 - Quizalofop ethyl 4% + Oxyfluorfen 6% EC (1000 ml/ha) performed the worst among the treated plots, showing only 30.60% control of D. sanguinalis and 44.37% for E. colonum, with the weed population increasing significantly by 35 DAA. The untreated control (T9) recorded the highest weed count, with no reduction in weed numbers, confirming the impact of the herbicide in the treated plots. The results indicate that Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (T3) and 975 ml/ha (T2) provided the most effective control of grassy weeds, significantly reducing their populations and demonstrating a strong synergistic effect, as reflected in the Colby’s ratio above 1.0. Lower doses such as Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha (T1) and Oxyfluorfen 23.5% EC at 850 ml/ha (T5) also contributed to substantial weed suppression, while solo Haloxyfop 10.5% EC 1200 ml/ha was less effective. These findings highlight the optimal dose range for effective grassy weed control in onion crops.

Table 6. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against biomass of grassy weeds.
Treatments Dose (gm / L) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average Weed Control Index
D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c D.s E.c
T1 780 11.74 3.77 2.83 1.29 2.31 1.03 0.76 0.66 1.56 2.09 1.87 1.27 89.17 86.96
T2 975 12.08 3.94 1.03 0.77 0.51 0.66 0.00 0.00 1.00 1.77 0.64 0.80 96.31 91.75
T3 1170 12.17 4.23 0.00 0.00 0.00 0.00 0.00 0.00 1.33 0.44 0.33 0.11 98.07 98.87
T4 1200 12.00 4.20 8.74 3.08 5.40 2.31 6.17 2.83 6.68 3.60 6.75 2.96 60.82 69.54
T5 850 11.83 4.03 8.23 2.83 4.88 2.06 5.40 2.57 6.17 3.34 6.17 2.70 64.18 72.19
T6 874 11.91 3.68 10.03 3.86 10.54 4.11 1.80 1.29 2.83 2.31 6.30 2.89 63.43 70.20
T7 1000 12.43 3.77 10.28 4.11 11.31 4.88 12.60 5.66 13.62 6.94 11.95 5.40 30.60 44.37
T8 -- 11.83 3.60 0.26 0.26 0.26 0.51 5.66 0.64 4.88 1.54 2.76 0.74 83.96 92.38
T9 -- 12.25 4.20 14.14 6.68 15.94 8.74 18.25 10.54 20.57 12.85 17.22 9.70 - -
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against the biomass of grassy weeds, particularly Digitaria sanguinalis (D.s) and Echinochloa colonum (E.c), was assessed across multiple treatment doses over different time intervals. The pre-treatment weed biomass was relatively uniform across treatments, ranging between 11.74–12.43 g/m² for D. sanguinalis and 3.60–4.23 g/m² for E. colonum, establishing a consistent baseline for evaluating the herbicide's effectiveness. The highest level of weed suppression was observed in T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha, where biomass reduction was complete by 7 and 14 days after application (DAA), maintaining 0.00 g/m² for both weed species up to 28 DAA, with a minor resurgence observed at 35 DAA (1.33 g/m² for D. sanguinalis and 0.44 g/m² for E. colonum). The Weed Control Index (WCI) for T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC 1170 ml/ha was 98.07% and 98.87% for D. sanguinalis and E. colonum respectively, confirming this as the most efficacious treatment. The treatment, T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC 975 ml/ha followed closely, showing near-complete suppression of weed biomass by 14 DAA, with minimal regrowth observed at 35 DAA, and achieving WCI values of 96.31% for D. sanguinalis and 91.75% for E. colonum. Similarly, T1 - Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780 ml/ha effectively suppressed weed biomass, reducing it to 1.87 g/m² and 1.27 g/m² for D. sanguinalis and E. colonum respectively, by the end of the observation period, resulting in WCI values of 89.17% and 86.96%.
Conversely, treatments, solo Haloxyfop 10.5% EC @ 1200 ml/ha (T4), Oxyfluorfen 23.5% EC @ 850 ml/ha (T5), and market standard - T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) exhibited moderate weed suppression, with significant weed regrowth after initial reductions. In T4 (Haloxyfop 10.5% EC @ 1200 ml/ha), weed biomass remained relatively high at 35 DAA (6.75 g/m² for D. sanguinalis and 2.96 g/m² for E. colonum), leading to a lower WCI of 60.82% and 69.54%, respectively. The solo Oxyfluorfen 23.5% EC @ 850ml/ha (T5) and T6 - Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha also showed suboptimal control, with final WCI values of 64.18% and 72.19% (T5 – Oxyfluorfen 23.5% EC); and 63.43% and 70.20% (T6 - Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha), indicating that these doses were less effective at sustained weed suppression. The least effective herbicidal treatment was T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha), which exhibited a rapid resurgence of weed biomass by 28 and 35 DAA, resulting in a WCI of only 30.60% for D. sanguinalis and 44.37% for E. colonum, indicating insufficient control. The untreated control (T9) experienced continuous weed growth, with biomass increasing to 20.57 g/m² for D. sanguinalis and 12.85 g/m² for E. colonum by 35 DAA, confirming the necessity of herbicidal intervention. Interestingly. These findings indicate that Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha (T3) is the optimal dose for achieving maximum grassy weed suppression, while Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha (T2) also provides effective control. Lower doses Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780ml/ha (T1) remain viable options, but remaining treatments (T4–T7) were less effective, likely due to factors such as herbicide tolerance, regrowth, or limited residual activity.

Table 7. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against broad leave weeds.
Treatment Dose
(g or l / ha) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average % Weed Control Colby’s Coefficient
T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v
T1 780 113 21 30 4 0 0 2 0 0 5 3 1.89 9 5 3 5 2 1.22 96.16 95.83 97.95 1.18 1.00 1.03
T2 975 115 25 33 3 0 0 2 0 0 4 1.2 1.4 8 3 2 4.25 1.05 0.85 96.74 97.81 98.57 1.19 1.02 1.04
T3 1170 110 24 37 3 0 0 1 0 0 4 1 1.2 5 2 3 3.25 0.75 1.05 97.50 98.44 98.24 1.20 1.03 1.03
T4 1200 118 27 35 89 15 18 56 10 11 47 7 9 58 10 13 62.5 10.5 12.75 52.02 78.13 78.57 0.64 0.82 0.83
T5 850 122 30 33 77 15 16 44 8 13 38 5 10 45 9 17 51 9.25 14 60.84 80.73 76.47 0.75 0.84 0.81
T6 874 121 27 35 35 20 11 10 18 8 15 7 9 21 13 14 20.25 14.5 10.5 84.45 69.79 82.35 1.04 0.73 0.87
T7 1000 120 25 32 54 13 13 12 10 14 18 16 22 22 17 27 26.5 14 19 79.65 70.83 68.07 0.98 0.74 0.72
T8 -- 125 28 35 0 0 0 3 2 5 5 7 14 11 12 16 4.75 5.25 8.75 96.35 89.06 85.29 0.00 - -
T9 -- 121 29 34 124 34 41 127 41 56 132 55 66 138 62 75 130.25 48 59.5 - - - 0.00 - -
T. p - Trianthema portulacastrum; P. o – Portulaca oleracea; A.v – Amaranthus viridae
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation in controlling broad-leaved weeds, specifically Trianthema portulacastrum (T.p), Portulaca oleracea (P.o), and Amaranthus viridis (A.v), was evaluated across multiple treatment doses, solo molecules of same herbicidal mixture, market standards (competitor products), manual practice-hand weeding and a comparative of an untreated control plot over different observation periods. The pre-treatment weed density was relatively uniform across treatments, ranging between 110–125 plants/m² for Trianthema portulacastrum, 21–30 plants/m² for Portulaca oleracea, and 30–37 plants/m² for Amaranthus viridis, providing a consistent baseline for evaluating herbicide efficacy. The highest weed suppression was observed in T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha), where weed density was reduced significantly within 7 DAA, with complete control of Portulaca oleracea and Amaranthus viridis, while Trianthema portulacastrum showed a minimal presence (3 plants/m²). By 14 DAA, weed densities were further suppressed to near-zero levels, and at 35 DAA, the final weed counts remained low, with Trianthema portulacastrum at 3.25 plants/m², Portulaca oleracea at 0.75 plants/m², and (Amaranthus viridis at 1.05 plants/m². The weed control percentage for T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha) was 97.50% (Trianthema portulacastrum), 98.44% (Portulaca oleracea), and 98.24% (Amaranthus viridis), confirming this treatment as the most effective. Similarly, T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha) also exhibited strong control, with weed counts reduced to 4.25 plants / m² (Trianthema portulacastrum), 1.05 plants/m² (Portulaca oleracea), and 0.85 plants / m² (Amaranthus viridis) at 35 DAA, achieving a weed control efficacy of 96.74%, 97.81%, and 98.57%, respectively. Colby’s coefficient for T3 -Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170ml/ha (1.20, 1.03, and 1.03) and T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha (1.19, 1.02, and 1.04) further confirmed a strong synergistic herbicidal interaction, maximizing weed suppression.
However, higher herbicide doses (T4 – Haloxyfop 10.5% EC @ 1200 ml/ha and T5–Oxyfluorfen 23.5% EC @ 850 ml/ha) demonstrated lower efficacy in controlling broad-leaved weeds. In T4 (Haloxyfop 10.5% EC @ 1200ml/ha, weed counts remained relatively high at 35 DAA, with Trianthema portulacastrum at 62.5 plants/m², Portulaca oleracea at 10.5 plants/m², and Amaranthus viridis at 12.75 plants/m², resulting in moderate weed control percentages of 52.02%, 78.13%, and 78.57%, respectively. Similarly, T5 – Oxyfluorfen 23.5% EC @ 850 ml/ha exhibited substantial weed regrowth, particularly for Trianthema portulacastrum (51 plants / m²) and Amaranthus viridis (14 plants / m²), leading to a weed control index of 60.84%, 80.73%, and 76.47%. The least effective treatments were T6 - Propaquizafop 5% + Oxyfluorfen 12% EC (874 ml/ha) and T7 - Quizalofop ethyl 4% + Oxyfluorfen 6% EC (1000 ml/ha), which exhibited persistent weed populations, with weed control percentages ranging between 68.07% and 84.45%, indicating insufficient suppression of broad-leaved weeds. The untreated control (T9) exhibited continuous weed proliferation, with Trianthema portulacastrum increasing to 130.25 plants/m², Portulaca oleracea to 48 plants/m², and Amaranthus viridis to 59.5 plants/m² by 35 DAA, demonstrating the necessity of herbicidal intervention. Based on these results, Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha (T3) emerged as the most effective dose for controlling broad-leaved weeds, followed closely by Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha (T2), while lower doses Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780ml/ha (T1) still provided reasonable control. However, remaining treatments (T4–T7) were less effective, possibly due to factors such as herbicide resistance, reduced residual activity, or weed resurgence.
Table 8. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against biomass of broad-leaved weeds.
Tret
ment Dose
(g or l / ha) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average % Weed Control
T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v T.p P..o A.v
T1 780 31.75 5.25 7.50 0.00 0.00 0.00 0.00 0.00 0.00 1.00 0.40 0.47 3.45 1.23 1.74 1.11 0.41 0.55 97.88 97.75 96.71
T2 975 36.25 6.25 8.25 0.00 0.00 0.00 0.00 0.00 0.00 1.00 0.30 0.35 2.66 0.88 1.05 0.92 0.30 0.35 98.25 98.37 97.92
T3 1170 34.50 6.00 9.25 0.00 0.00 0.00 0.00 0.00 0.00 0.98 0.25 0.30 2.34 2.20 3.00 0.83 0.61 0.83 98.42 96.61 95.09
T4 1200 32.00 6.75 8.75 27.50 6.25 7.50 30.25 8.25 8.50 31.50 9.25 10.75 32.50 10.00 11.75 30.44 8.44 9.63 41.90 53.33 42.67
T5 850 31.25 7.50 8.25 28.25 6.75 7.75 30.00 7.50 9.25 32.00 8.75 11.25 33.00 10.25 12.25 30.81 8.31 10.13 41.18 54.02 39.70
T6 874 32.00 6.75 8.75 5.50 5.00 1.25 4.00 0.50 0.50 5.00 1.75 2.00 7.00 8.00 7.00 5.38 3.81 2.69 89.74 78.91 83.99
T7 1000 32.50 6.25 8.00 18.50 3.25 2.50 3.00 2.25 3.50 4.50 4.00 5.50 5.50 4.25 6.75 7.88 3.44 4.56 84.97 80.99 72.83
T8 -- 33.75 7.00 8.75 0.00 0.00 0.00 0.25 0.25 0.75 1.25 1.75 3.50 2.75 3.00 4.00 1.06 1.25 2.06 97.97 93.09 87.72
T9 -- 40.12 10.12 10.09 43.44 14.32 12.34 49.76 17.66 14.00 56.23 19.12 16.50 60.12 21.22 24.32 52.39 18.08 16.79
T. p – Trianthema portulacastrum; P. o – Portulaca oleracea; A.v – Amaranthus viridae
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against the biomass of broad-leaved weeds was evaluated by assessing its impact on Trianthema portulacastrum (T. p.), Portulaca oleracea (P. o.), and Amaranthus viridis (A. v.) across different treatments and time intervals. The results indicate significant reductions in weed biomass at varying degrees of herbicidal application, demonstrating differential effectiveness among the applied doses.
At 7 days after application (DAA), treatments T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) exhibited complete suppression of weed biomass across all species, with values reaching near zero. In contrast, T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) recorded moderate reductions but failed to achieve complete weed suppression, with T. portulacastrum biomass remaining at 27.50 g and 28.25 g, respectively. The 14 DAA results reflected similar trends, with T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) maintaining complete control, whereas T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) exhibited weed biomass persistence, notably in T. portulacastrum (30.25 g and 30.00 g, respectively). Treatments T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) showed a gradual decline in biomass, with T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) reducing P. oleracea to 0.50 g and A. viridis to 0.50 g, while T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) recorded moderate biomass reduction.
By 28 DAA, the control efficacy of T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) remained high, with only minimal weed resurgence (=1.25 g for any species). However, T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) exhibited considerable weed biomass, particularly in T. portulacastrum (31.50 g and 32.00 g, respectively), signifying reduced herbicidal efficiency at these doses. At 35 DAA, T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) continued to demonstrate superior control, with weed biomass values remaining at a minimum (1.11 g, 0.92 g, and 0.83 g for T. portulacastrum, respectively). Conversely, T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) continued to sustain higher weed biomass (32.50 g and 33.00 g for T. portulacastrum, respectively), indicating less effective suppression. T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) showed moderate levels of weed control, with T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) performing better than T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha), particularly in reducing P. oleracea and A. viridis biomass.
The Weed Control Percentage (WCP) values reaffirmed the efficacy trends, with T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) achieving the highest suppression rates, exceeding 97% across all weed species. Treatments T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) maintained moderate weed control levels, ranging between 72.83% and 89.74%, while T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) exhibited substantially lower efficacy (below 55% in some cases). The untreated control (T9) experienced continuous weed growth, with biomass values increasing substantially over time (52.39 g, 18.08 g, and 16.79 g for T. portulacastrum, P. oleracea, and A. viridis, respectively, by 35 DAA).
Overall, the results confirm that Haloxyfop 9% + Oxyfluorfen 11.5% EC at doses of 780 ml/ha, 975 ml/ha, and 1170 ml/ha exhibited superior efficacy in suppressing broad-leaved weeds, with near-total biomass elimination. The treatments – T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) and T6 - (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) demonstrated moderate weed control, while the remaining treatments paradoxically exhibited lower efficiency, possibly due to reduced selectivity or differential weed response. Thus, Haloxyfop 9% + Oxyfluorfen 11.5% EC at doses 975 ml/ha, and 1170 ml/ha may be recommended for optimal broad-leaved weed management in onion crops.
Table 9. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against Sedges.
Treatments Dose / ha
(gm / L) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average % Weed Control Colby’s Ratio
T1 780 51 19 14 21 29 20.75 73.57 1.09
T2 975 53 15 12 19 25 17.75 77.39 1.14
T3 1170 54 12 10 17 22 15.25 80.57 1.19
T4 1200 50 37 33 43 56 42.25 46.18 0.68
T5 850 52 41 35 48 52 44 43.95 0.65
T6 874 55 28 25 31 48 33 57.96 0.86
T7 1000 52 30 34 42 46 38 51.59 0.76
T8 -- 53 0 0 3 5 2 97.45 -
T9 -- 51 54 67 87 106 78.5 - -
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC against sedges was evaluated across different treatments over multiple time intervals. The pre-treatment (0 DAA) weed counts were relatively uniform across treatments, ranging from 50 to 55 weeds per plot, indicating a consistent baseline infestation. At 7 DAA, a significant decline in sedge populations was observed in T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780 ml/ha), T2 ( Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha), and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha), with T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha recording the lowest weed count (12 weeds), demonstrating its early suppression effectiveness. Conversely, T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) had higher sedge persistence (37 and 41 weeds, respectively), indicating reduced initial efficacy.
By 14 DAA, the downward trend continued, with T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha) showing the lowest weed count (10 weeds), followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha) (12 weeds) and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780 ml/ha) (14 weeds), confirming their superior efficacy in weed suppression. In contrast, T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) (33 weeds) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) (35 weeds) retained a substantial sedge presence, indicating insufficient control. At 28 DAA, weed counts in T1, T2, and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha, 975 ml/ha, and 1170 ml/ha, respectively) remained below 21 weeds, reinforcing their continued suppression capability, while T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) (43 and 48 weeds, respectively) exhibited poor weed control. At 35 DAA, the lowest weed counts were recorded for T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) (22 weeds), T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (25 weeds), and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) (29 weeds), highlighting their sustained effectiveness. However, T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) demonstrated significant sedge regrowth (56 and 52 weeds, respectively), confirming their lower efficacy. The untreated control (T9) exhibited progressive weed proliferation, reaching 106 weeds by 35 DAA.
In terms of weed control efficacy (% WCI), T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) achieved the highest reduction (80.57%), followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (77.39%) and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) (73.57%), demonstrating their superior performance. Treatments T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) exhibited moderate control (57.96% and 51.59%, respectively), while T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) showed poor suppression (46.18% and 43.95%, respectively), confirming their reduced effectiveness.
Colby’s Coefficient analysis provided insights into herbicide interactions. T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) (1.19) exhibited the strongest synergistic effect, followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (1.14) and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) (1.09), reinforcing their effectiveness as combined formulations. Treatments T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) (0.86) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) (0.76) showed moderate interactions, while T4 (Haloxyfop 10.5% EC at 1200 ml/ha) (0.68) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) (0.65) had the lowest synergy values, indicating weaker combined efficacy.
Overall, Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (T3) emerged as the most effective treatment, providing the highest weed suppression (80.57%) with strong synergistic interaction (Colby’s ratio: 1.19). Treatments T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) also demonstrated effective control, achieving weed reductions exceeding 73%. In contrast, remaining treatment applications showed significantly reduced efficacy, likely due to herbicide antagonism or increased weed resistance. Moderate suppression was observed with market standards - T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha), but their efficiency was comparatively lower. Therefore, Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha at a dose of 975–1170 ml/ha is recommended for optimal sedge management, ensuring maximum suppression with a strong synergistic interaction between Haloxyfop and Oxyfluorfen.

Table 10. Efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation against biomass of sedges.
Treatments Dose / ha (gm / L) Pre-count 7 DAA 14 DAA 28 DAA 35 DAA Average % Weed
Control
T1 780 6.42 1.02 1.54 1.77 1.89 2.53 85.28
T2 975 5.74 0.00 0.00 0.98 1.12 1.57 90.87
T3 1170 5.21 0.00 0.00 0.13 1.09 1.29 92.51
T4 1200 8.19 6.59 7.45 8.19 8.99 7.88 54.10
T5 850 7.82 6.49 8.00 8.99 9.32 8.12 52.68
T6 874 7.49 5.32 2.99 3.32 3.49 4.52 73.66
T7 1000 7.16 5.82 3.82 4.49 5.82 5.42 68.42
T8 -- 5.55 0.00 0.00 1.99 2.32 1.97 88.52
T9 -- 7.32 14.56 18.97 21.00 24.00 17.17
The efficacy of Haloxyfop 9% + Oxyfluorfen 11.5% EC against the biomass of sedges was evaluated over multiple time intervals, with significant variations observed across different treatments. The pre-treatment sedge biomass ranged from 5.21 to 8.19 g per plot, ensuring a relatively uniform initial weed pressure. By 7 DAA, the most effective treatments were T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha), both of which completely suppressed sedge biomass to 0.00 g, indicating strong early control. In contrast, T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) showed relatively poor performance, retaining biomass levels of 6.59 g and 6.49 g, respectively.
At 14 DAA, T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975ml/ha) and T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) continued to exhibit full suppression (0.00 g), confirming their sustained impact, while market standards - T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) showed moderate reductions to 2.99 g and 3.82 g, respectively. Meanwhile, T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) displayed increased biomass accumulation (7.45 g and 8.00 g, respectively), indicating suboptimal control. By 28 DAA, minimal biomass recovery was noted in T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) (0.13 g), reinforcing its strong long-term suppression. T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (0.98 g) and T8 (Hand weeding) (1.99 g) also maintained effective control, whereas T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) exhibited near-complete biomass regrowth (8.19 g and 8.99 g, respectively), highlighting their inefficacy.
By 35 DAA, T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) (1.09 g) and T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (1.12 g) sustained their superior weed suppression, followed by T8 (Hand weeding) (2.32 g), confirming their long-term efficacy. However, T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) (8.99 g) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) (9.32 g) exhibited maximum biomass recovery, suggesting herbicide failure or resistance development. T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) (3.49 g) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) (5.82 g) maintained moderate suppression, though with reduced efficacy compared to T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) and T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha). The untreated control (T9) showed an exponential increase in sedge biomass, reaching 24.00 g by 35 DAA, confirming the aggressive nature of unchecked sedge proliferation.
In terms of overall weed biomass reduction efficiency, T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) achieved the highest suppression (92.51%), followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (90.87%) and T8 (Hand weeding) (88.52%), demonstrating their superior efficacy. Moderate control was observed with T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) (73.66%) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) (68.42%), whereas T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) (54.10%) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) (52.68%) provided the lowest levels of biomass reduction, indicating poor herbicidal efficacy. The untreated control (T9) showed continuous biomass accumulation, reinforcing the necessity of effective herbicide intervention.
Overall, Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (T3) proved to be the most effective formulation, offering the highest weed biomass suppression (92.51%), with sustained efficacy over time. The Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha (T2) also exhibited strong control (90.87%), while moderate suppression was achieved by lower doses (T6 (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) and T7 (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha). However, higher-dose applications such as T4 (Haloxyfop 10.5% EC @ 1200 ml/ha) (54.10%) and T5 (Oxyfluorfen 23.5% EC @ 850 ml/ha) resulted in significantly reduced efficacy, suggesting potential antagonistic effects or reduced herbicide absorption. Based on these findings, Haloxyfop 9% + Oxyfluorfen 11.5% EC at a dose range of 975–1170 ml/ha is recommended for optimal sedge biomass management, ensuring prolonged suppression and improved weed control efficiency.
The following images represent the trend of weed density across the different treatments. Conclusively we can clearly observe the effect of Haloxyfop-R-Methyl 10.5% + Oxyfluorfen 23.5% EC significantly controlled the weed density at all three doses was higher than the weed density controlled by individual components.
T1
T2
T3
Un Treated

Table 11. Phytotoxicity of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation on onion.
Treatments Days Visual Rating Scale
Yellowing Necrosis Wilting Vein
Clearing Leaf Tip / Margin Dying Stunting / Dwarfing
Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 780 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 975 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Haloxyfop 9% + Oxyfluorfen 11.5% EC @ 1170 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Haloxyfop 10.5% EC @ 1200 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Oxyfluorfen 23.5% EC @ 850 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Quizalofop Ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha 5 0 0 0 0 0 0
10 0 0 0 0 0 0
Untreated Control 5 0 0 0 0 0 0
10 0 0 0 0 0 0

The data presented evaluates the phytotoxicity of various formulations of Haloxyfop 9% + Oxyfluorfen 11.5% EC on onion, specifically looking at the effects on visual symptoms such as yellowing, necrosis, wilting, vein clearing, leaf tip/margin dying, and stunting/dwarfing. The treatments were applied at different doses, ranging from 750 ml/ha to 1250 ml/ha for the Haloxyfop + Oxyfluorfen combinations, as well as other herbicide combinations such as Propaquizafop + Oxyfluorfen, Quizalofop Ethyl + Oxyfluorfen, and a control group. In all treatments, no phytotoxicity symptoms were observed either at 5 or 10 days after application (DAA). The visual ratings for all treatments, including Haloxyfop 9% + Oxyfluorfen 11.5% EC at doses of 780 ml/ha, 975 ml/ha, 1170 ml/ha, as well as other herbicide combinations (Propaquizafop + Oxyfluorfen, Quizalofop Ethyl + Oxyfluorfen, and Oxyfluorfen), remained at 0 for all symptoms at both 5- and 10-days post-application. This indicates that none of the treatments caused any visible damage or phytotoxicity to the onion plants, suggesting that the formulations and doses used were safe for onions within the observed time frame.
Table 12. Effect of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation on onion yield parameters
Treatments Dose / ha (gm / L) Plant height (cm) Collar thickness (cm) Bulb weight (gm/bulb) Bulb yield (q/ha)
T1 780 21 2.09 55 243
T2 975 24.8 2.2 60 265
T3 1170 22.1 2.4 64 281
T4 1200 20 1.45 48 217
T5 850 20.34 1.54 44 198
T6 874 19 1.77 32 178
T7 1000 18 1.65 25 184
T8 -- 17 1.78 21 167
T9 -- 15 0.9 15 49
The effect of Haloxyfop 9% + Oxyfluorfen 11.5% EC on onion yield parameters varied significantly across different treatment doses. Plant height, collar thickness, bulb weight, and total bulb yield were notably influenced by the application rates of the herbicide formulation. The tallest plants were observed in T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha), with an average height of 24.8 cm, followed by T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) at 22.1 cm, indicating a positive response to these herbicide doses. In contrast, the untreated control (T9) exhibited the shortest plant height (15 cm), suggesting that unchecked weed competition severely impacted crop growth.
Collar thickness, an important indicator of bulb development, followed a similar trend. The highest collar thickness was recorded in T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (2.4 cm), followed by T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha (2.2 cm) and T1 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha (2.09 cm), reflecting improved vegetative growth and nutrient uptake due to effective weed suppression. Conversely, T9 (untreated control) had the lowest collar thickness (0.9 cm), indicating stunted growth due to high weed pressure.
Bulb weight, a crucial yield-determining factor, was highest in T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (64 g per bulb), followed by T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha (60 g per bulb) and T1 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha (55 g per bulb), suggesting that these herbicide treatments created favorable conditions for bulb development. In contrast, T9 (untreated control_ exhibited the lowest bulb weight (15 g per bulb), reaffirming the negative impact of weed competition. Lower herbicide doses, such as T6 - (Propaquizafop 5% + Oxyfluorfen 12% EC @ 874 ml/ha) (32 g) and T7 - (Quizalofop ethyl 4% + Oxyfluorfen 6% EC @ 1000 ml/ha) (25 g), also showed reduced bulb weights, indicating that insufficient weed control could hinder proper bulb formation.
Bulb yield per hectare (q/ha) followed a consistent pattern with bulb weight. The highest yield was recorded in T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (281 q/ha), followed by T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha (265 q/ha) and T1 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha (243 q/ha), highlighting the significant role of effective weed management in enhancing onion productivity. Meanwhile, T9 (untreated control) had the lowest bulb yield (49 q/ha), reflecting severe yield losses due to uncontrolled weed growth. Treatments with higher herbicide doses, such as T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 11.5% EC at 850 ml/ha), resulted in reduced yields (217 q/ha and 198 q/ha, respectively).
Overall, the results indicate that Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (T3) was the most effective treatment, resulting in the highest plant height, collar thickness, bulb weight, and bulb yield. The Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha dose (T2) also performed well, showing slightly lower but comparable yield parameters. However, higher doses such as Haloxyfop 10.5% EC at 1200 ml/ha (T4) and Oxyfluorfen 11.5% EC at 850 ml/ha (T5) negatively impacted onion growth and yield, potentially due to herbicide stress. Based on these findings, Haloxyfop 9% + Oxyfluorfen 11.5% EC at a dose range of 975–1170 ml/ha is recommended for optimal onion yield, ensuring effective weed control without causing adverse effects on crop development.
Table 13. Effect of Haloxyfop 9% + Oxyfluorfen 11.5% EC formulation on follow-up crop – Black gram
Treatments Dose / ha
(gm / ml) % germination Pods / plant Yield
(q / ha)
T1 780 88.00 33.00 947
T2 975 90.00 36.00 1003.00
T3 1170 92.00 39.00 1120.00
T4 1200 77.00 28.00 835.00
T5 850 74.32 29.00 889.00
T6 874 82.33 30.00 814.00
T7 1000 80.08 31.00 855.00
T8 -- 68 27.00 778.00
T9 -- 60 23.00 690.00
The effect of Haloxyfop 9% + Oxyfluorfen 11.5% EC on the follow-up crop, Black gram, was evaluated based on germination percentage, number of pods per plant, and total yield (q/ha). The results indicate that herbicide application at optimal doses positively influenced black gram performance, while higher doses or the absence of weed control led to reduced crop productivity.
Seed germination was highest in T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) at 92%, followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) at 90% and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) at 88%, indicating minimal residual toxicity at these application rates. In contrast, the untreated control (T9) exhibited the lowest germination rate of 60%, likely due to the adverse effects of weed competition. Treatments with higher herbicide doses, such as T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha), resulted in reduced germination rates of 77% and 74.32%, respectively, suggesting potential residual effects of herbicide at these higher concentrations.
The number of pods per plant, a critical determinant of black gram productivity, followed a similar pattern. T3 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha) recorded the highest pod count (39 per plant), followed by T2 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha) (36 per plant) and T1 (Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha) (33 per plant), reflecting improved crop health and growth due to effective weed control in the preceding onion crop. On the other hand, T9 (untreated control) had the lowest pod count (23 per plant), indicating that residual weed pressure negatively impacted reproductive growth. Treatments such as T4 (Haloxyfop 10.5% EC at 1200 ml/ha) and T5 (Oxyfluorfen 23.5% EC at 850 ml/ha) resulted in pod counts of 28 and 29 per plant, respectively, showing a decline due to possible residual effects.
The total yield of black gram (q/ha) was highest in T3 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 1170 ml/ha (1120 q/ha), followed by T2 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 975 ml/ha (1003 q/ha) and T1 - Haloxyfop 9% + Oxyfluorfen 11.5% EC at 780 ml/ha (947 q/ha), highlighting the benefits of weed-free conditions for improved soil fertility and crop productivity. Conversely, the lowest yield was observed in T9 – untreated control (690 q/ha), where high weed infestation from the previous season likely suppressed black gram growth. Higher herbicide doses, such as T4 - Haloxyfop 10.5% EC at 1200 ml/ha (835 q/ha) and T5 - Oxyfluorfen 23.5% EC at 850 ml/ha (889 q/ha), also showed a decline in yield, suggesting potential carryover effects that may have slightly inhibited crop performance.
Overall, the results suggest that Haloxyfop 9% + Oxyfluorfen 11.5% EC at an application rate of 1170 ml/ha (T3) provided the best outcomes for black gram, ensuring high germination, pod formation, and yield. The Haloxyfop 9% + Oxyfluorfen 11.5% EC at an application rate of 975 ml/ha dose (T2) also demonstrated favorable results, while remaining treatments or insufficient weed control (untreated control) negatively impacted the subsequent crop. Therefore, Haloxyfop 9% + Oxyfluorfen 11.5% EC at an optimal application rate of 975–1170 ml/ha is recommended to maximize productivity in a follow-up black gram crop, ensuring effective weed management with minimal residual effects.
The foregoing examples are merely illustrative and are not to be taken as limitations upon the scope of the invention. Various changes and modifications to the disclosed examples will be apparent to those skilled in the art. Such changes and modifications may be made without departing from the scope of the invention. It is to be understood that this disclosure is not limited to a particular compositions or specific constituents, which can, of course, vary and that the terminology used herein is for the purpose of describing embodiments only and is not intended to be limiting the scope of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" include plural referents unless the content clearly dictates otherwise, and equivalents thereof known to those skilled in the art and so forth. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this disclosure pertains. Although any methods and materials similar or equivalent to those described herein can be used in the practice for testing of the disclosure(s), specific examples of appropriate materials and methods are described herein. The examples set forth above are provided to give those of ordinarily skilled in the art a complete description of how to make and use the embodiments of the compositions or specific constituents, methods of practice, and are not intended to limit the scope of what the inventors regard as their invention. Modifications of the above-described modes for carrying out the invention that is obvious to persons skilled in the art are intended to be within the scope of the following claims. All patents and publications mentioned in the specification are indicative of the levels of skill of those skilled in the art to which the disclosure pertains.
While specific embodiments of the present invention are explicitly disclosed herein, the above specification and examples herein are illustrative and not 5 restrictive. It will be understood that various modifications may be made without departing from the spirit and scope of the invention. Many variations of the disclosure will become apparent to those skilled in the art upon review of this specification and the embodiments below. The full scope of the invention should be determined by reference to the embodiments, along with their full scope of equivalents and the specification, along with such variations. Accordingly, other embodiments are within the scope of the following claims. ,CLAIMS:I / We Claim:
1. A synergistic herbicidal emulsifiable concentrate (EC)
formulation comprising:
a) haloxyfop or an agriculturally acceptable salts or esters
thereof;
b) oxyfluorfen;
c) at least one agrochemical acceptable excipient.
2. The composition as claimed in claim 1, wherein, the haloxyfop
includes haloxyfop-R-methyl.
3. The composition as claimed in claim 1, synergistic herbicidal
emulsifiable concentrate (EC) formulation comprising a
combination of haloxyfop and oxyfluorfen; wherein haloxyfop
and oxyfluorfen are present in the weight ratio of (1-25) :
(5-25).
4. The composition as claimed in claim 1, wherein, the weight
ratio of haloxyfop and oxyfluorfen is 9 : 11.5.
5. The composition as claimed in claim 1, wherein, the
agrochemical acceptable excipients are selected from the
group comprising of an emulsifier, wetting agent, an anti-
freezing agent, an anti-foaming agent, a stabilizer, an
adjuvant and solvents.
6. The herbicidal emulsifiable concentrate formulation as
claimed in claim 1, wherein the emulsifiable concentrate
comprises:
a) about 1-25% haloxyfop by weight of the formulation;
b) about 5- 25% oxyfluorfen by weight of the formulation;
c) about 5- 30% emulsifier(s) by weight of the formulation;
d) about 0.5-15% adjuvant by weight of the formulation;
e) about 5-80% solvent by weight of the formulation.
7. The herbicidal emulsifiable concentrate formulation as
claimed in claim 1, wherein the emulsifiable concentrate
comprises:
a) 9 % haloxyfop-R-methyl by weight of the formulation;
b) 11.5 % oxyfluorfen by weight of the formulation;
c) about 5 % calcium dodecyl benzene sulphonate by weight of
the formulation;
d) about 5 % phenol styrenated by weight of the formulation;
e) about 5 % solvent naphtha (petroleum), heavy aromatic by
weight of the formulation;
f) about 5 % castor oil ethoxylate by weight of the
formulation;
g) about 5% to 80 % solvent (Solvent C IX) by weight of the
formulation.
8. A process for preparing the emulsifiable concentrate (EC)
formulation as claimed in claim 1, the process comprising
steps of:
a) adding solvent C-IX into a clean and dry reactor;
b) adding the active ingredients haloxyfop and oxyfluorfen
slowly, under continuous stirring;
c) adding one or more agrochemical acceptable excipients
under continues stirring;
d) continuing the stirring for another one hour to get
desired homogenous bioeffective emulsifiable concentrate
solution comprising haloxyfop and oxyfluorfen.
9. The process for preparing the emulsifiable concentrate (EC)
as claimed in claim 8, wherein the agrochemical acceptable
excipients are selected from the group comprising of an
emulsifier, wetting agent, an anti-freezing agent, an anti-
foaming agent, a stabilizer, an adjuvant and solvents.
10. The composition as claimed in the preceding claims,
formulated as an EC with reducing the phytotoxicity without
the need of additional crop safeners or plant health
additives.
11. The composition as claimed in the preceding claims, wherein
the herbicidal composition is used to control annual
grasses, sedges, and broad leaf weeds in onion crops and
various other crops for general weed control.
12. The composition as claimed in the preceding claims, the
composition is used to manage weeds in crops by applying the
formulation as early post and post-emergent to the weed
populations at a rate of 900–1200 ml/ha.