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An Acaricidal Insecticidal Composition And A Process Of Preparation Thereof

Abstract: The present disclosure envisages a composition comprising Bifenthrin and Propargite in a suspoemulsion form. The composition further comprises at least one surfactant, at least one stabilizer , at least one viscosity modifying agent , at least one anti-freezing agent, at least one carrier and at least one anti-foaming agent. The present disclosure also envisages a process for preparing the suspoemulsion composition.

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Patent Information

Application #
Filing Date
22 January 2015
Publication Number
36/2016
Publication Type
INA
Invention Field
AGROCHEMICALS
Status
Email
dewan@rkdewanmail.com
Parent Application
Patent Number
Legal Status
Grant Date
2021-09-07
Renewal Date

Applicants

INDOFIL INDUSTRIES LIMITED
Kalpataru Square, 4th Floor, Kondivita Road, Off: Andheri-Kurla Road Andheri (E) Mumbai-400,059, Maharashtra, India

Inventors

1. RAO JAYPRAKASH GOPALKRISHNAN
Gokulnagari Nx, K-5/502 Near Tulsidhara, Khadakpada, Kalyan(W)-421301 Maharashtra, India
2. PATIL SEEMA ABHIJIT
Gokulnagari Nx, K-6/701 Near Tulsidhara, Khadakpada, Kalyan(W)-421301 Maharashtra, India
3. THAKUR SHRAVANEE SACHIN
Moraj, M-Type 4th Floor, Flat No.403,Co.Op.Housing Society Panvel-410206, Maharashtra, India

Specification

DESC:FIELD
The present disclosure relates to a suspoemulsion insecticidal composition.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used indicate otherwise.
Acaricide: Acaricides are pesticides that kill members of the arachnid subclass Acari, which includes ticks and mites.
Rainfastness: Rainfastness is a pesticide’s ability to withstand rainfall and is an important factor affecting the efficacy of foliar-applied pesticides.
Suspoemulsion: Suspoemulsion is a mixture of an emulsion and a suspension, which is formulated to allow the application of two active ingredients, one being solid and the other an immiscible liquid.
Emulsion Concentrate: Emulsion concentrate is an oil-in water emulsion where the active ingredient is dissolved in oil.
Suspension concentrate: Suspension concentrate is a suspension of the active ingredient in water.
BACKGROUND
In order to maximize food production, it is necessary to protect crops from insects/pests. Numerous chemicals such as organochlorines, organophosphates, organosulfurs, carbamates, formamidines, dinitrophenols, organotins, pyrethroid, phenylpyrazoles, pyrroles, pyrazoles and the like are used, to control/manage the insects/pests. Insecticides when used in combinations are more effective with higher potency and activity level as compared to the individual insecticides.

Propargite is a sulfite ester of acaricide having the molecular formula C19H26O4S which is a brownish-yellow, oily, viscous liquid; miscible in organic solvents such as hexane, toluene, dichloromethane, methanol and acetone. Propargite is used to control phytophagous mites (particularly in the motile stages) on a variety of crops including vines, fruit trees (e.g. top fruit, stone fruit and citrus fruit), hops, nuts, tomatoes, vegetables, ornamental plants, cotton, maize, peanuts and sorghum. Propargite binds to plant cuticle giving good rainfastness and long residual contact activity.

Propargite
Propargite is a non-systemic acaricide with contact action which inhibits oxidative phosphorylation of a target organism.
Bifenthrin is a pyrethroid insecticide having the molecular formula C23H22ClF3O2. It is a white, waxy solid having a faint sweet smell and is poorly soluble in water. Bifenthrin is soluble in acetone, chloroform, dichloromethane, diethyl ether and toluene, and slightly soluble in heptane and methanol. Bifenthrin is used to control a broad range of foliar pests on a variety of crops including cereals, citrus, cotton, fruit, grapes, ornamental plants and vegetables. Bifenthrin is effective against a wide range of pests belonging to the order Coleoptera, Diptera, Heteroptera, Homoptera, Lepidoptera and Orthoptera. Bifenthrin is also capable of controlling some species belonging to the subclass Acarina. In India, Bifenthrin is currently registered for use on cotton, rice, tea and apple crops.

Bifenthrin
Bifenthrin is effective by contact or by ingestion by the insects. Bifenthrin affects the central and peripheral nervous system of a target insect by interfering with sodium channel gating. Bifenthrin works by interfering with a nerve cell's ability of the targeted insect to send a normal signal by jamming open tiny gates on the cell that need to open and close rapidly to carry the message.
Mixtures containing different insecticide/pesticide compositions have been practiced in the art, but problems with the physical stability of such mixtures have caused application and efficacy issues and consequently in many cases, it is necessary to mix the active ingredients prior to application/use.
There is, therefore, felt a need for a synergistic insecticidal-acaricidal composition which is compatible and stable over long periods.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
It is an object of the present disclosure to provide an acaricidal-insecticidal composition.
It is another object of the present disclosure to provide an acaricidal-insecticidal composition in a suspoemulsion form.
It is a further object of the present invention to provide an improved, stable and ready to use acaricidal-insecticidal composition having a synergistic effect.
It is yet another object of the present disclosure to provide a process for preparing a suspoemulsion composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure envisages a suspoemulsion composition comprising Bifenthrin in an amount ranging from 2 to 25% of the total mass of the composition, Propargite in an amount ranging from 30 to 60% of the total mass of the composition, at least one surfactant in an amount ranging from 1 to 10% of the total mass of the composition, at least one stabilizer in an amount ranging from 0.5 to 3% of the total mass of the composition, at least one anti-freezing agent in an amount ranging from 1 to 7% of the total mass of the composition, at least one carrier in an amount ranging from 10 to 15% of the total mass of the composition, at least one viscosity modifying agent in an amount ranging from 0.1 to 0.5% of the total mass of the composition, and at least one anti-foaming agent in an amount ranging from 0.1 to 1% of the total mass of the composition.
The suspoemulsion composition of the present disclosure optionally comprises at least one filler, at least one wetting agent, at least one emulsifying agent, at least one dispersing agent and at least one suspending agent.
The present disclosure also envisages a process for preparing the suspoemulsion composition.
DETAILED DESCRIPTION
In recent years there is a need to increase the efficacy of the pesticides and insecticides by broadening the spectrum by combination products for controlling different pests and insects. Single active ingredient formulations rarely meet such broad-spectrum requirements. Moreover such combinational products have several additional advantages such as elimination of tank mixing prior to use; reduction in inventory products; saving in time and money; and a reduction in the number of times the crop is sprayed. Often this problem goes unnoticed and results in inconsistent application of both the pesticide and insecticide, yielding inadequate efficacy of both.
Accordingly, there exists a need to develop a solution for overcoming the above mentioned drawbacks and which is safe and effective.
The inventors of the present disclosure envisaged a suspoemulsion composition comprising at least one acaricidal compound, at least one insecticidal compound and at least one excipient.
In accordance with one aspect of the present disclosure there is provided a suspoemulsion composition comprising:
? (2-methyl-3-phenylphenyl)methyl (1RS,3RS)-3-[(Z)-2-chloro-3,3,3-trifluoroprop-1-enyl]-2,2-dimethylcyclopropane-1-carboxylate (Bifenthrin) in an amount ranging from 2 to 25% of the total mass of the composition;
? 2-(4-tert-butylphenoxy)cyclohexyl prop-2-yne-1-sulfonate (Propargite) in an amount ranging from 30 to 60% of the total mass of the composition;
? at least one surfactant in an amount ranging from 1 to 10% of the total mass of the composition;
? at least one stabiliser in an amount ranging from 0.5 to 3% of the total mass of the composition;
? at least one anti-freezing agent in an amount ranging from 1 to 7% of the total mass of the composition;
? at least one carrier solvent in an amount ranging from 5 to 15% of the total mass of the composition;
? at least one viscosity modifying agent in an amount ranging from 0.1 to 0.5% of the total mass of the composition; and
? at least one anti-foaming agent in an amount ranging from 0.1 to 1% of the total mass of the composition.
Typically, the surfactant can be selected from the group consisting of, but not limited to, anionic surfactant, cationic surfactant and non-ionic type surfactant. Typically, the surfactant is selected from the group consisting of, but not limited to, lignosulphonate, sodium formaldehyde condensates polymer salt, naphthalene formaldehyde condensate sodium salt, ethoxylated polyarylphenol phosphate amine salt, condensation products of ethylene oxide with alkyl phenols such as octyl phenol, nonyl phenol, ethoxylated tristyrylphenol, alcohol ethoxylates, castor oil ethoxylates, calcium alkyl benzene sulfonates and proprietary blended emulsifiers such as geronol SCRTM (blend of non ionic surfactant).
Typically, the stabilizer can be selected from the group consisting of, but not limited to, formaldehyde, methyl parahydroxybenzoate, propyl parahydroxybenzoate, 2-bromo-2-nitro-propane-1, 3-diol, sodium benzoate, glutaraldehyde, o-phenylphenol, benzisothiazolinones, 5-chloro-2-methyl-4-isothiazolin-3-one, pentachlorophenol and 2-4-dichlorobenzylalcohol.
Typically, the anti-freezing agent can be selected from the group consisting of, but not limited to, ethylene glycol, propylene glycol, glycerin and urea.
Typically, the carrier can be selected from the group consisting of, but not limited to, aromatic solvents such as solvesso ™ 200, solvesso ™ 200 nd, and ketonic solvents such as cyclohexanone and alcoholic solvents such as butanol, propanol, octanol and water. Solvesso ™ 200 and solvesso ™ 200 nd are a complex combination of hydrocarbons obtained from distillation or aromatic streams and consists mostly of aromatic hydrocarbons having carbon numbers in the range of C9 to C16.
Typically, the viscosity modifying agent can be selected from the group consisting of, but not limited to, xanthan gum, guar gum, and gum arabic, bentonite type clays and cellulose derivatives. The cellulose derivatives are selected from the group consisting of, but not limited to, cellulose acetate, cellulose nitrate and cellulose xanthate.
Typically, the anti-foaming agent can be selected from the group consisting of, but not limited to, polydimethylsiloxane powder and polydimethylsiloxane liquid.
In one embodiment of the present disclosure, the composition comprises Bifenthrin, Propargite, at least one surfactant, at lease one antifreeze agent, at lease one stabiliser, at least one viscosity modifiying agent, at least one antifoaming agent and at least one carrier.
In a preferred embodiment of the present disclosure, there is provided a process for preparing the suspoemulsion composition.
The present disclosure also envisages a process for preparation of the suspoemulsion composition.
In one embodiment of the present disclosure, the process involves the following steps:
In a reaction vessel a predetermined amount of Bifenthrin technical is pre-mixed with a solvent at a speed of 200 to 400 rpm for two hours at a temperature ranging from 20 to 30 °C to obtain a homogenized mixture. At least one antifreezing agent, at least one antifoaming agent and at least one surfactant are added in predetermined amounts to the reaction vessel containing the homogenized mixture, followed by stirring to obtain a second mixture.
The second mixture is then charged slowly with a predetermined amount of Propargite technical at a speed of 1800 to 2200 rpm for 20 to 50 minutes at 20 to 40°C followed by adding a predetermined quantity of water at an optimum temperature and speed followed by addition of at least one stabilizer, at least one anti foaming agent and at least one viscosity modifying agent at a speed of 1500 to 2500 rpm for 60 to 120 minutes to obtain the suspoemulsion composition of the present disclosure.
The present disclosure is further described in light of the following laboratory scale experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial/commercial scale.
Experiments:
The suspoemulsion compositions were prepared by using the ingredients of the present invention in different appropriate quantities as given in experiments 1 to 5.
Experiment 1:
In a reaction vessel, 68g Solvesso™ 200 ND was added. To this reaction vessel containing the Solvesso™ 200 ND, 26.8g of Bifenthrin technical (active pyrethroid ingredient) was added slowly with continuous stirring at 300 rpm for two hours at 25°C, followed by the addition of 25g of propylene glycol, 14g of ethoxylated polyarylphenol phosphate amine salt, 14g of ethoxylated tristyrylphenol and 1g of silicone emulsion (dimethyl siloxane reacted with silica) to obtain a mixture A. Further, 280g of Propargite technical was charged slowly in the reaction vessel containing the mixture A at 1800 rpm for 35 minutes at 30°C to obtain a homogenous mass. The temperature of the homogenous mass was maintained at 30°C and 64.2g of water was charged very slowly into the homogenous mass and stirred at 1800 rpm for two and half hours to obtain a mixture B. The particle size was analyzed by Malvern particle size analyser and the average particle size of mixture B was in the range of 1.5 to 1.8 micron.
To this mixture B, 1g of silicone emulsion (dimethyl siloxane reacted with silica), 5gm of Xanthan gum solution and 1g of benizothiazolinone were added and stirred at 1800 rpm for one and half hour to obtain the suspoemulsion composition of the present disclosure.
The viscosity of the suspoemulsion composition analysed at 60 rpm using spindle 3 was 3000 centipoise (cps). Further the sample was subjected to accelerated storage study for 14 days at 54°C. The stability data has been summarised in Table-1.
Table-1
Parameters Day of formulation After ageing for 14 days at 54 °C
Propargite content (%w/w) 52.1% 51.6%
Bifenthrin content (%w/w) 5.09% 5.04%
Wet sieve test ( 75 micron sieve ) retention on sieve 0.4% 0.5%
Pourability (Rinsed residue) % by mass analysed as per CIPAC method 1.7% 1.8%

The results indicate that the suspoemulsion composition of the present disclosure was stable after the accelerated study thus indicating a stable homogeneous suspoemulsion composition having the desired shelf life.
Experiment 2:
In a reaction vessel, 68g Solvesso™ 200ND was added. To this reaction vessel containing the Solvesso 200™ ND, 26.8g Bifenthrin technical (active pyrethroid ingredient) was added slowly with continuous stirring at 300 rpm for two hours at 25 °C, followed by the addition of 25g of propylene glycol, 8g of polyoxyethylene alkyl ether (Atlox™ 4894), 10g of polymethyl methacrylate polyethylene glycol graft copolymer and 1g of silicone emulsion (dimethyl siloxane reacted with silica) to obtain a mixture A.
Further, 280g of Propargite technical was charged slowly in the reaction vessel containing the mixture A at 1800 rpm for 35 minutes at 30°C to obtain a homogenous mass. The temperature of the homogenous mass was maintained at 30°C and 74.2 g of water was charged very slowly into the homogenous mass and stirred at 1800 rpm for two hours to obtain a mixture B. The particle size was analyzed by Malvern particle size analyser and the average particle size of mixture B was in the range of 1.5 to 1.8 micron.
To this mixture B, 1g of silicone emulsion (dimethyl siloxane reacted with silica), 5gm of Xanthan gum solution and 1g of benzisothiazolinone were added and stirred at 1800 rpm for one and half hour to obtain the suspoemulsion composition of the present disclosure. The suspoemulsion composition when kept still for 30 minutes, separated into two phases indicating that the blend of polyoxyethylene alkyl ether (Atlox™ 4894) and polymethyl methacrylate polyethylene glycol graft copolymer at the desired ratio is not forming a stable homogeneous product.
Experiment 3:
In a reaction vessel, 68g Solvesso™ 200 ND was added. To this reaction vessel containing the Solvesso™ 200 ND, 26.8g Bifenthrin technical (active pyrethroid ingredient) was added slowly with continuous stirring at 300 rpm for two hours at 25 Py°C, followed by the addition of 25g of propylene glycol, 9.5g of polyoxyethylene alkyl ether (Atlox™ 4894), 10g of polymethyl methacrylate polyethylene glycol graft copolymer and 1g of silicone emulsion (dimethyl siloxane reacted with silica) to obtain a mixture A.
Further, 280g of Propargite technical was charged slowly in the reaction vessel containing the mixture A at 1800 rpm for 35 minutes at 30°C to obtain a homogenous mass. The temperature of the homogenous mass was maintained at 30°C and 72.7 g of water was charged very slowly into the homogenous mass and stirred at 1800 rpm for two hours to obtain a mixture B. The particle size was analyzed by Malvern particle size analyser and the average particle size of mixture B was in the range of 1.5 to 1.8 micron.
To this mixture B, 1g of silicone emulsion (dimethyl siloxane reacted with silica), 5gm of Xanthan gum solution and 1g of benzisothiazolinone were added and strirred at 1800 rpm for one and half hour to obtain the suspoemulsion composition of the present disclosure. The suspoemulsion composition when kept still for 30 minutes, separated into two phases indicating that the blend of polyoxyethylene alkyl ether (Atlox™ 4894) and polymethyl methacrylate polyethylene glycol graft copolymer at the desired ratio is not forming a stable homogeneous product.
Experiment 4:
In a reaction vessel, 68g Solvesso™ 200 ND was added. To this reaction vessel containing the Solvesso™ 200 ND,26.8g Bifenthrin technical (active pyrethroid ingredient) was added slowly with continuous stirring at 300 rpm for two hours at 25 °C, followed by the addition of 25g of propylene glycol, 9.5g of ethoxylated polyarylphenol phosphate amine salt (sorprophpr™ 3d33), 10g of tristyrylphenol ethoxylate phosphate ester and 1g of silicone emulsion (dimethyl siloxane reacted with silica) to obtain a mixture A.
Further, 280g of Propargite technical was charged slowly in the reaction vessel containing the mixture A at 1800 rpm for 35 minutes at 30°C to obtain a homogenous mass. The temperature of the homogenous mass was maintained at 30°C and 72.7 g of water was charged very slowly into the homogenous mass and stirred at 1800 rpm for two hours to obtain a mixture B. The particle size was analyzed by Malvern particle size analyser and the average particle size was in the range of 1.5 to 1.8 micron.
To this mixture B, 1g of silicone emulsion (dimethyl siloxane reacted with silica), 5gm of Xanthan gum and 1g of benzisothiazolinone were added and stirred at 1800 rpm for one and half hour to obtain the suspoemulsion composition of the present disclosure. The suspoemulsion composition when kept still for 30 minutes, separated into two phases indicating that the blend of ethoxylated polyarylphenol phosphate amine salt and tristyrylphenol ethoxylate phosphate ester at the desired ratio is not forming a stable homogeneous product.
Experiment 5:
The suspoemulsion composition was prepared as per experiment no. 1 but the process conditions were changed with respect to speed of mixing during the addition of water and the temperature. There was an increase in the viscosity as the speed was increased, which resulted in a gel like structure. The observations are summarised in Table 2.
Table 2
Temperature Speed of stirrer Viscosity in centipoise (cps) Particle size in micron Remark
30 °C
1800 rpm 3000 cps 1.65 Homogeneous free flowing Mixture obtained.
2200 rpm 3200 cps 1.81 Homogeneous free flowing Mixture obtained.
3200 rpm 4300 cps 2.30 Viscous gel like material obtained.
4200 rpm 5000 cps 2.75 Viscous gel like material obtained.
20 °C 1800 rpm 3200 cps 2.05 Homogeneous free flowing Mixture obtained
2200 rpm 3300 cps 2.11 Homogeneous free flowing Mixture obtained
3200 rpm 4400 cps 2.58 Viscous gel like material obtained.
4200 rpm 5200 cps 3.21 Viscous gel like material obtained.
35 °C 1800 rpm 2800 cps 1.79 Homogeneous free flowing Mixture obtained
2200 rpm 3100 cps 1.89 Homogeneous free flowing Mixture obtained
3200 rpm 4000 cps 2.29 Viscous gel like material obtained.
4200 rpm 4800 cps 2.65 Viscous gel like material obtained.

Thus it was observed that the temperature and the stirring speed play an important role in obtaining a stable suspoemulsion composition. The ideal stirring speed was observed to be in the range of 1800 to 2200 rpm and optimum temperatures were in the range of 20 to 35 °C. At higher speed, there was an increase in the viscosity and gelling of the composition was observed.
Experiment 6:
Cotton plants heavily infested by jassids, aphids, mites and whiteflies were treated by spraying:
i. a preparation containing only Propargite as the active ingredient;
ii. a preparation containing only Bifenthrin as the active ingredient; and
iii. the suspoemulsion composition of the present disclosure.
When the preparation containing only Propargite is used, an effective reduction in mite was observed with little effect on whitefly. Similarly, when the preparation containing only Bifenthrin was used, only the whitefly infestation was controlled with little effect on the mite infestation. When the suspoemulsion composition of the present disclosure comprising both Propargite and Bifenthrin was used, both the mite and whitefly were effectively controlled along with jassids, aphids. Further, it was also observed that a higher kill percentage for the mite was observed when the suspoemulsion composition of the present disclosure comprising Propargite and Bifenthrin was used when compared to the preparation containing only Bifenthrin.
Similarly, it was also observed that a higher kill percentage for the whiteflies was observed when the suspoemulsion composition of the present disclosure comprising Propargite and Bifenthrin was used when compared to the preparation containing only Propargite.
Hence, a synergistic activity is obtained using the suspoemulsion composition of the present disclosure as compared to the active compounds (Propargite and Bifenthrin) when applied individually.
Bioefficacy and Phytotoxicity evaluation on Cotton (variety Rasi -659).
Field trials were conducted to evaluate Propargite 50% + Bifenthrin 5% suspoemulsion (SE) against sucking pests, jassids, aphids, mites and whiteflies in cotton field. Two sprays of Propargite 50% + Bifenthrin 5% SE were given at 15 days interval starting with the initiation of sucking pest infestation.
Propargite 50% + Bifenthrin 5% SE was sprayed using a knapsack sprayer at 500 L of spray solution per hectare. 1st spray was conducted on the 65th day after sowing and 2nd spray was conducted on the 80th day after sowing.
Jassids, aphids, thrips, whiteflies and mite population were recorded at pre-treatment and at 3, 5, 7, 10 and 14 days of each spraying from 5 leaves from 5 tagged plants in each treatment. The treatment details are summarised in Table 3.
Table 3
No. Treatment compositions Dose rates (g.ai. /Ha) Dose rates (ml/gm/Ha)
T1 Propargite 50% + Bifenthrin 5% SE 500+ 50.0 1000
T2 Propargite 50% + Bifenthrin 5% SE 550 + 55.0 1100
T3 Propargite 50% + Bifenthrin 5% SE 575+57.5 1150
T4 Bifenthrin 10% EC 62.5 625
T5 Propargite 57% EC 627 1100
T6 Imidacloprid 20% SL 20 100
T7 Spiromesifen 24% SC 96 400
T8 Untreated Check (Control) - -
EC = Emulsifiable concentrate, SL = Soluble (liquid) and SC = Suspension concentrate
The experimental data was statistically analysed by Completely Randomized Design (factorial CRD) and Randomized Complete Block Design (RCBD) using MSTAT statistical software in a microcomputer. The results are expressed as Mean ± SE (standard error) and data was statistically analysed by one-way Analysis of variance (ANOVA), with the level of significance set at p < 0.01. The mean values adjusted by Duncan’s Multiple Range Test (DMRT).
RESULT & DISCUSSION:
a) Jassids :
The observations of the use of the treatment compositions on jassids are summarized in Table 4.
Among all the dose rates, significantly superior mortality was observed in Propargite 50% + Bifenthrin 5% SE treated plots at 555+55.0 and 575+57.5 g.a.i/ha. There was no significant difference between Propargite 50% + Bifenthrin 5% SE at 555 +55.0 and 575+57.5 g.a.i/ha treatments. Combination treatments of Propargite 50% + Bifenthrin 5% SE showed better efficacy compared to the solo applications of Propargite at 627 ga.i/ha and Bifenthrin at 62.5 ga.i/ha against jassids.
Table 4: Effect of Propargite 50% + Bifenthrin 5% against Cotton Jassids
Sr. No. Treatments Dose g.ai/ha Dose (ml /gm/ha) % Mortality of jassid population after treatment
3days 5 days 7 days 10 days 14 days
1. Propargite 50% + Bifenthrin 5% SE 500 + 50.0 1000 78.89 85.78 80.56 71.24 60.12
(62.72)b (67.93)b (63.91)c (57.75)d (50.87)d
2. Propargite 50% + Bifenthrin 5% SE 555 + 55.0 1100 85.12 97.17 99.12 89.32 79.87
(67.74)a (80.34)a (87.62)a (70.89)a (63.24)a
3. Propargite 50% + Bifenthrin 5% SE 575 + 57.5 1150 86.11 98.12 100.00 90.21 81.22
(68.11)a (81.59)a (87.89)a (71.66)a (63.80)a
4. Bifenthrin 10% EC 62.5 625 77.99 85.98 81.32 74.32 65.32
(62.79)b (68.71)b (64.34)c (59.50)c (53.67)c
5. Propargite 57% EC 627 1100 12.32 15.33 17.89 16.22 15.22
(20.78)d (23.25)c (24.68)d (24.22)e (23.19)e
6. Imidacloprid 20 % SL 20 100 75.23 84.98 85.11 79.32 69.78
(62.16)c (67.96)b (67.30)b (61.65)b (55.25)b
7. Spiromesifen 24% SC 96 400 11.98 13.12 14.89 15.67 14.39
(20.75)e (22.99)e (23.12)d (23.79)e (23.01)e
8. Control -- -- 0 0 0 0 0
(0.00)e (0.00)d (0.00)e (0.00)f (0.00)f
CD (p=0.05) 0.561 1.302 2.546 1.018 0.86
SE(m) 0.1 0.535 2.048 0.327 0.233
Means followed by a common letter do not differ Pd"0.05 by Duncan's multiple range test
Data based on means of two sprays and three replicates each. Figures in parenthesis are arcsine transformed values.
a = 1st performing dose rate;
b = 2nd performing dose rate;
c = 3rd performing dose;
d = 4th performing dose rate;
e = 5th performing dose rate;
f = 6th performing dose rate;
g = 7th performing dose rate; and
CD (p=0.05) = Critical difference at 5% probability.
If two dose rates show a, they are at par with each other.
b) Aphids :
The observations of the use of the treatment compositions on aphids are summarized in Table 5.
Among all the dose rates, significantly superior mortality was observed in Propargite 50% + Bifenthrin 5% SE treated plots at 555+55.0 and 575+57.5 g.a.i/ha. There was no significant difference between Propargite 50% + Bifenthrin 5% SE at 555 +55.0 and 575+57.5 g.a.i/ha treatments. Combination treatments of Propargite 50% + Bifenthrin 5% SE showed better efficacy compared to the solo applications of Propargite at 627 ga.i/ha and Bifenthrin at 62.5 ga.i/ha against aphids.
Table 5: Effect of Propargite 50% + Bifenthrin 5% against Cotton Aphids
Sr. No. Treatments Dose g.ai/ha Dose (ml /gm/ha) % Mortality of Aphids population after treatment
3days 5 days 7 days 10 days 14 days
1. Propargite 50% + Bifenthrin 5% SE 500 + 50.0 1000 75.11 80.22 85.78 80.34 70.12
(60.10)c (63.63)d (67.87)d (63.92)d (57.11)c
2. Propargite 50% + Bifenthrin 5% SE 555 + 55.0 1100 78.89 94.22 95.21 90.43 79.87
(63.30)a (76.97)a (77.62)a (72.34)a (63.40)a
3. Propargite 50% + Bifenthrin 5% SE 575 + 57.5 1150 79.99 95.33 95.89 91.88 81.22
(63.48)a (77.38)a (78.19)a (73.03)a (62.67)a
4. Bifenthrin 10% EC 62.5 625 70.12 90.78 91.22 89.88 79.89
(57.74)d (71.96)b (72.72)b (71.53)b (63.41)a
5. Propargite 57% EC 627 1100 8.90 11.32 12.34 10.11 8.92
(17.07)e (17.84)e (20.43)e (19.75)e (18.69)d
6. Imidacloprid 20 % SL 20 100 75.23 84.98 88.32 85.12 73.12
(62.18)b (66.97)c (69.91)c (70.16)c (59.47)b
7. Spiromesifen 24% SC 96 400 8.62 12.12 13.89 10.67 9.39
(17.01)e (17.99)e (20.49)e (19.79)e (18.98)d
8. Control -- -- 0 0 0 0 0
(0.00)f (0.00)f (0.00)f (0.00)f (0.00)f
CD (p=0.05) 0.513 1.102 0.624 0.949 1.983
SE(m) 0.1 0.383 0.123 0.285 1.243
Means followed by a common letter do not differ Pd"0.05 by Duncan's multiple range test
Data based on means of two sprays and three replicates each. Figures in parenthesis are arcsine transformed values.
a = 1st performing dose rate;
b = 2nd performing dose rate;
c = 3rd performing dose;
d = 4th performing dose rate;
e = 5th performing dose rate;
f = 6th performing dose rate;
g = 7th performing dose rate; and
CD (p=0.05) = Critical difference at 5% probability.
If two dose rates show a, they are at par with each other.
c. Mites :
The observations of the use of the treatment compositions on mites are summarized in Table 6.
Among all the dose rates, significantly superior mortality was observed in Propargite 50% + Bifenthrin 5% SE treated plots at 555+55.0 and 575+57.5 g.a.i/ha. There was no significant difference between Propargite 50% + Bifenthrin 5% SE at 555 +55.0 and 575+57.5 g.a.i/ha treatments. Combination treatments of Propargite 50% + Bifenthrin 5% SE showed better efficacy compared to the solo applications of Propargite at 627 ga.i/ha and Bifenthrin at 62.5 ga.i/ha against mites.
Table 6: Effect of Propargite 50% + Bifenthrin 5% against Cotton mites
Sr. No. Treatments Dose g.ai/ha Dose (ml /gm/ha) % Mortality of mite population after treatment
3days 5 days 7 days 10 days 14 days
1. Propargite 50% + Bifenthrin 5% SE 500 + 50.0 1000 69.24 84.24 87.41 85.76 75.45
(56.32)c (66.62)b (69.22)c (67.83)e (56.87)d
2. Propargite 50% + Bifenthrin 5% SE 555 + 55.0 1100 75.34 100 99.53 100 96.93
(60.45)a (87.89)a (88.52)a (89.71)a (82.75)a
3. Propargite 50% + Bifenthrin 5% SE 575 + 57.5 1150 78.11 100 100 100 96.19
(60.52)a (87.89)a (89.71)a (89.71)a (82.94)a
4. Bifenthrin 10% EC 62.5 625 23.22 31.23 28.77 21.33 19.32
(25.56)f (30.62)d (26.47)d (19.27)f (18.95)e
5. Propargite 57% EC 627 1100 75 86.54 87.46 90.33 90.67
(60.08)b (68.49)b (69.34)c (71.88)c (63.32)b
6. Imidacloprid 20% SL 20 100 10.38 12.22 9.32 9.56 8.34
(13.47)e (15.64)e (10.21)e (10.28)g (10.01)f
7. Spiromesifen 24% SC 96 400 33.22 76.12 91.895 94.675 87.39
(35.20)d (60.75)c (72.82)b (76.65)b (57.62)d
8. Control -- -- 0 0 0 0 0
(0.00)f (0.00)f (0.00)f (0.00)h (0.00)g
CD (p=0.05) 0.352 3.116 1.337 0.012 0.804
SE(m) 0.039 3.067 0.565 0.001 0.204
Means followed by a common letter do not differ Pd"0.05 by Duncan's multiple range test
Data based on means of two sprays and three replicates each. Figures in parenthesis are arcsine transformed values.
a = 1st performing dose rate;
b = 2nd performing dose rate;
c = 3rd performing dose;
d = 4th performing dose rate;
e = 5th performing dose rate;
f = 6th performing dose rate;
g = 7th performing dose rate; and
CD (p=0.05) = Critical difference at 5% probability.
If two dose rates show a, they are at par with each other.
d. Whiteflies :
The observations of the use of the treatment compositions on whiteflies are summarized in Table 7.
Among all the dose rates, significantly superior mortality was observed in Propargite 50% + Bifenthrin 5% SE treated plots at 555+55.0 and 575+57.5 g.a.i/ha. There was no significant difference between Propargite 50% + Bifenthrin 5% SE at 555 +55.0 and 575+57.5 g.a.i/ha treatments. Combination treatments of Propargite 50% + Bifenthrin 5% SE showed better efficacy compared to the solo applications of Propargite at 627 ga.i/ha and Bifenthrin at 62.5 ga.i/ha against whiteflies.
Table 7: Effect of Propargite 50% + Bifenthrin 5% against Cotton Whiteflies
Sr. No. Treatments Dose g.ai/ha Dose (ml /gm/ha) % Mortality of mite population after treatment
3days 5 days 7 days 10 days 14 days
1. Propargite 50% + Bifenthrin 5% SE 500 + 50.0 1000 66.23 80.24 83.32 75.76 70.34
(54.47)c (63.60)d (65.89)d (60.51)c (56.98)c
2. Propargite 50% + Bifenthrin 5% SE 555 + 55.0 1100 71.98 91.22 99.89 100 92.93
(58.23)a (73.56)a (89.08)a (89.71)a (74.59)a
3. Propargite 50% + Bifenthrin 5% SE 575 + 57.5 1150 72.23 92.32 100 100 94.19
(58.20)a (73.92)b (89.61)a (89.89)a (74.16)a
4. Bifenthrin 10% EC 62.5 625 67.23 83.32 88.43 76.33 64.32
(55.07)b (65.92)c (67.47)c (61.98)c (54.13)d
5. Propargite 57% EC 627 1100 12.21 12.22 13.32 11.56 13.34
(20.46)e (20.41)f (27.21)f (23.34)e (20.39)e
6. Imidacloprid 20% SL 20 100 12.38 32.22 53.32 51.56 43.34
(20.47)e (28.64)g (47.21)e (45.34)d (38.39)d
7. Spiromesifen 24% SC 96 400 55.62 79.12 93.895 91.67 82.39
(48.23)d (62.81)e (75.76)b (74.17)b (65.26)b
8. Control -- -- 0 0 0 0 0
(0.00)g (0.00)h (0.00)g (0.00)f (0.00)f
CD (p=0.05) 0.258 0.013 0.600 0.603 0.804
SE(m) 0.021 0.001 0.114 0.115 0.204
Means followed by a common letter do not differ Pd"0.05 by Duncan's multiple range test
Data based on means of two sprays and three replicates each. Figures in parenthesis are arcsine transformed values.
a = 1st performing dose rate;
b = 2nd performing dose rate;
c = 3rd performing dose;
d = 4th performing dose rate;
e = 5th performing dose rate;
f = 6th performing dose rate;
g = 7th performing dose rate; and
CD (p=0.05) = Critical difference at 5% probability.
If two dose rates show a, they are at par with each other.
e. Phytotoxicity :
There was no phytotoxicity observed on the cotton crops when the dosage of Propargite 50% + Bifenthrin 5% SE was doubled. The observations are summarized in Table 8.
Table 8: Effect of different treatments on phytotoxicity at 3, 7 and 15 DAA
Treatments Dose
(Form/ acre) Yellowing Necrosis Scorching Epinasty Hyponasty
Days after Application
3 7 15 3 7 15 3 7 15 3 7 15 3 7 15
1. 2000 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
2. 2200 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
3. 2300 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
4. 1250 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
5. 2200 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

CONCLUSION:
The efficacy of the suspoemulsion composition, i.e. Propargite 50% + Bifenthrin 5% SE at the dose rate of 555+55.0 g.ai/ha showed synergistic effect on controlling jassids, aphids, mites and white flies.
There was no significant difference between Propargite 50% + Bifenthrin 5% SE at 555 +55.0 and 575+57.5 g.a.i/ha treatments. Solo applications of Propargite at 627 g.a.i/ha and Bifenthrin at 62.5 g.a.i/ha showed less mortality in controlling jassids, aphids, mites and white flies when compared to the suspoemulsion composition of the present disclosure (Propargite 50% + Bifenthrin 5% SE at the dose rate of 550 + 55.0 g.ai/ha).
This can be because each component of Propargite and Bifenthrin is complementary to each other which showed a strong synergistic effect in controlling jassids, aphids, mites and white flies.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of:
? a synergistic insecticidal-acaricidal suspoemulsion composition comprising Bifenthrin and Propargite;
? a synergistic insecticidal-acaricidal suspoemulsion composition comprising Bifenthrin and Propargite which is stable and is in a ready-to use form; and
? an easy and simple process for the preparation of the synergistic insecticidal-acaricidal suspoemulsion composition comprising Bifenthrin and Propargite.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation. ,CLAIMS:1. A suspoemulsion composition comprising:
? at least one acaricidal compound;
? at least one insecticidal compound; and
? at least one excipient.
2. A suspoemulsion composition comprising:
? (2-methyl-3-phenylphenyl)methyl (1RS,3RS)-3-[(Z)-2-chloro-3,3,3-trifluoroprop-1-enyl]-2,2-dimethylcyclopropane-1-carboxylate (Bifenthrin) in an amount ranging from 2 to 25% of the total mass of the composition;
? 2-(4-tert-butylphenoxy)cyclohexyl prop-2-yne-1-sulfonate (Propargite) in an amount ranging from 30 to 60% of the total mass of the composition;
? at least one surfactant in an amount ranging from 1 to 10% of the total mass of the composition;
? at least one stabiliser in an amount ranging from 0.5 to 3% of the total mass of the composition;
? at least one viscocity modifying agent in an amount ranging from 0.1 to 0.5% of the total mass of the composition;
? at least one anti-freezing agent in an amount ranging from 1 to 7% of the total mass of the composition;
? at least one carrier in an amount ranging from 5 to 15% of the total mass of the composition; and
? at least one anti-foaming agent in an amount ranging from 0.1 to 1% of the total mass of the composition.

3. A suspoemulsion composition comprising:
? (2-methyl-3-phenylphenyl)methyl (1RS,3RS)-3-[(Z)-2-chloro-3,3,3-trifluoroprop-1-enyl]-2,2-dimethylcyclopropane-1-carboxylate (Bifenthrin) in an amount ranging from 2 to 25% of the total mass of the composition;
? 2-(4-tert-butylphenoxy)cyclohexyl prop-2-yne-1-sulfonate (Propargite) in an amount ranging from 30 to 60% of the total mass of the composition;
? at least one surfactant in an amount ranging from 1 to 8% of the total mass of the composition;
wherein said surfactant is selected from the group consisting of anionic surfactant, cationic surfactant and non-ionic type surfactant;
? at least one stabilizer in an amount ranging from 0.5to 3% of the total mass of the composition;
wherein said stabilizer is selected from the group consisting of formaldehyde, methyl parahydroxybenzoate, propyl parahydroxybenzoate, 2-bromo-2-nitro-propane-1, 3-diol, sodium benzoate, glutaraldehyde, o-phenylphenol, benzisothiazolinones, 5-chloro-2-methyl-4-isothiazolin-3-one, pentachlorophenol and 2-4-dichlorobenzylalcohol;
? at least one viscosity modifying agent in an amount ranging from 0.1 to 0.5% of the total mass of the composition;
wherein said viscosity modifying agent is selected from the group consisting of xanthan gum, guar gum, acacia gum and cellulose derivatives;
? at least one anti-freezing agent in an amount ranging from 1 to 7% of the total mass of the composition;
wherein said anti-freezing agent is selected from the group consisting of ethylene glycol, propylene glycol, glycerin and urea;
? at least one carrier in an amount ranging from 5 to 15% of the total mass of the composition;
wherein said carrier is selected from the group consisting of aromatic solvents such as high aromatic solvent naptha, and ketonic solvents such as cyclohexanone and alcoholic solvents such as butanol, propanol, octanol and water;
and
? at least one anti-foaming agent in an amount ranging from 0.1 to 1% of the total mass of the composition;
wherein said anti-foaming agent is selected from the group consisting of polydimethylsiloxane powder and polydimethylsiloxane liquid.
4. The composition as claimed in claim 1, wherein said
? acaricidal compound is 2-(4-tert-butylphenoxy)cyclohexyl prop-2-yne-1-sulfonate (Propargite);
? insecticidal compound is (2-methyl-3-phenylphenyl)methyl (1RS,3RS)-3-[(Z)-2-chloro-3,3,3-trifluoroprop-1-enyl]-2,2-dimethylcyclopropane-1-carboxylate (Bifenthrin); and
? at least one excipient is selected from the group consisting of a surfactant, an anti-freezing agent, a carrier, a stabilizer, a viscosity modifying agent and an anti-foaming agent.
5. The composition as claimed in claim 3 further comprises at least one filler, at least one wetting agent, at least one emulsifying agent, at least one dispersing agent and at least one suspending agent.
6. The composition as claimed in claim 3, wherein said surfactant is selected from the group consisting of lignosulphonate, sodium formaldehyde condensates polymer salt, naphthalene formaldehyde condensate sodium salt, ethoxylated polyarylphenol phosphate amine salt, condensation products of ethylene oxide with alkyl phenols such as octyl phenol, nonyl phenol, ethoxylated tristyrylphenol, alcohol ethoxylates, castor oil ethoxylates, calcium alkyl benzene sulfonates and proprietary blended emulsifiers such as geronol SCRTM (blend of non ionic surfactant).
7. A process for preparing a suspoemulsion composition, said process comprising:
? mixing in a reaction vessel a predetermined amount of Bifenthrin technical with a solvent at a speed of 200 to 400 rpm for two hours at a temperature ranging from 20 to 30 °C to obtain a homogenized mixture;
? adding a predetermined amount of at least one antifreezing agent, at least one antifoaming agent and at least one surfactant are added to said reaction vessel containing said homogenized mixture, followed by stirring at a speed of 400 to 800 rpm for 1 to 2 hours at a temperature ranging from 20 to 30 °C to obtain a second mixture;
? charging said second mixture with a predetermined amount of Propargite technical at a speed of 1800 to 2200 rpm for 20 to 50 minutes at 20 to 40 °C followed by adding a predetermined quantity of water at a temperature ranging from 20 to 40 °C and at a speed of 1500 to 2200 rpm; and
? adding at least one stabilizer, at least one anti foaming agent and at least one viscosity modifying agent and stirring at a speed of 1500 to 2500 rpm for 60 to 120 minutes to obtain said suspoemulsion composition.
8. The process as claimed in claim 7, wherein said predetermined amount of Bifenthrin is in the range of 2 to 25% of the total mass of the composition.
9. The process as claimed in claim 7, wherein said antifreezing agent is in the range of 1 to 7% of the total mass of the composition.
10. The process as claimed in claim 7, wherein said antifoaming agent is in the range of 0.1 to 1% of the total mass of the composition.
11. The process as claimed in claim 7, wherein said at least one surfactant is in the range of 1 to 8% of the total mass of the composition.
12. The process as claimed in claim 7, wherein said predetermined amount of Propargite is in the range of 30 to 60% of the total mass of the composition.
13. The process as claimed in claim 7, wherein said predetermined quantity of water is in the range of 10 to 15% of the total mass of the composition.

Documents

Application Documents

# Name Date
1 Power of Attorney [21-01-2016(online)].pdf 2016-01-21
2 Form 6 [21-01-2016(online)].pdf 2016-01-21
3 Description(Complete) [21-01-2016(online)].pdf 2016-01-21
4 Assignment [21-01-2016(online)].pdf_17.pdf 2016-01-21
5 Assignment [21-01-2016(online)].pdf 2016-01-21
6 Other Patent Document [23-09-2016(online)].pdf 2016-09-23
7 Form 8 [07-10-2016(online)].pdf 2016-10-07
8 Form 18 [06-04-2017(online)].pdf 2017-04-06
9 Synergistic_composition_PS_draft2.pdf 2018-08-11
10 FORM 3.pdf 2018-08-11
11 235-MUM-2015-Power of Attorney-250116.pdf 2018-08-11
12 235-MUM-2015-OTHERS-290216.pdf 2018-08-11
13 235-MUM-2015-Form 5-020216.pdf 2018-08-11
14 235-MUM-2015-Form 1-020216.pdf 2018-08-11
15 235-MUM-2015-Correspondence-290216.pdf 2018-08-11
16 235-MUM-2015-Correspondence-250116.pdf 2018-08-11
17 235-MUM-2015-Correspondence-020216.pdf 2018-08-11
18 143-MUM-2015-Form 1-300115.pdf 2018-08-11
19 143-MUM-2015-Correspondence-300115.pdf 2018-08-11
20 235-MUM-2015-FER.pdf 2019-04-09
21 235-MUM-2015-MARKED COPIES OF AMENDEMENTS [04-10-2019(online)].pdf 2019-10-04
22 235-MUM-2015-FORM 13 [04-10-2019(online)].pdf 2019-10-04
23 235-MUM-2015-FER_SER_REPLY [04-10-2019(online)].pdf 2019-10-04
24 235-MUM-2015-COMPLETE SPECIFICATION [04-10-2019(online)].pdf 2019-10-04
25 235-MUM-2015-CLAIMS [04-10-2019(online)].pdf 2019-10-04
26 235-MUM-2015-AMMENDED DOCUMENTS [04-10-2019(online)].pdf 2019-10-04
27 235-MUM-2015-Response to office action [31-08-2020(online)].pdf 2020-08-31
28 235-MUM-2015-Response to office action [31-08-2020(online)]-1.pdf 2020-08-31
29 235-MUM-2015-FORM-26 [10-03-2021(online)].pdf 2021-03-10
30 235-MUM-2015-Correspondence to notify the Controller [10-03-2021(online)].pdf 2021-03-10
31 235-MUM-2015-Written submissions and relevant documents [26-03-2021(online)].pdf 2021-03-26
32 235-MUM-2015-RELEVANT DOCUMENTS [26-03-2021(online)].pdf 2021-03-26
33 235-MUM-2015-PETITION UNDER RULE 137 [26-03-2021(online)].pdf 2021-03-26
34 235-MUM-2015-FORM 13 [26-03-2021(online)].pdf 2021-03-26
35 235-MUM-2015-PatentCertificate07-09-2021.pdf 2021-09-07
36 235-MUM-2015-IntimationOfGrant07-09-2021.pdf 2021-09-07
37 235-MUM-2015-US(14)-HearingNotice-(HearingDate-12-03-2021).pdf 2021-10-03
38 235-MUM-2015-RELEVANT DOCUMENTS [23-07-2022(online)].pdf 2022-07-23
39 235-MUM-2015-RELEVANT DOCUMENTS [23-08-2023(online)].pdf 2023-08-23

Search Strategy

1 235MUM2015searchstrategy_09-04-2019.pdf

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