DESC:FIELD OF THE INVENTION:
The present invention relates to an insecticidal composition for pest control.
More particularly, the present invention relates to composition comprises
5 compounds (i) Chlorantraniliprole (ii) at least one compound selected from
Thiocyclam hydrogen oxalate or Diafenthiuron and (iii) optionally sulphur. The
present invention relates to Suspension Concentrate (SC) formulation
composition comprises(i) Chlorantraniliprole (ii) Diafenthiuron and Wettable
powder (WP) formulation composition comprises compounds (i)
10 Chlorantraniliprole(ii) Thiocyclam hydrogen oxalate has enhanced action for
plant pest control, having synergistic and superior properties compared to prior
art formulations or mixtures or compositions.
Formula (A) (chlorantraniliprole / CAS NO: 500008-45-7)
15
Formula (B) (Thiocyclam hydrogen oxalate / CAS No.: 31895-22-4)
Page 2 of 49
Formula (C) (Diafenthiuron /CAS No: 80060-09-9) BACKGROUND OF THE INVENTION
A number of chemical agents have been used for controlling plant pest control. 5 However, the problem that plant pest have acquired resistance to the chemical agents becomes remarkable due to frequent use or excessive application, etc., of the chemical agents having similar structures and same functions for controlling the same kinds of pest.
10 On the other hand, consumers' needs for agricultural chemical-reduced crops and social needs to reduce environmental loads due to agricultural chemicals have now increased. Also, in a farmer's field where the chemicals have been actually used, when two or more kinds of chemicals are used in admixture for the treatment by the tank mix method, there are many risks to lower the effect of the 15 other chemical to be mixed with each other or possibilities to cause chemical damages against plant materials depending on a combination of chemicals where they are not well-suited to each other.
20 SUMMARY OF INVENTION: Accordingly, the main objectof the present invention is to provide a plant pest control wherein the said composition comprises compounds (i) Chlorantraniliprole (ii) at least one compound selected from Thiocyclam 25 hydrogen oxalate or Diafenthiuron and (iii) optionally sulphur. It is an object of the present invention to provide improved, stable and ready to use composition for plant pest control comprises compounds (i) Chlorantraniliprole (ii) at least one compound selected from Thiocyclam 30 hydrogen oxalate or Diafenthiuron and (iii) optionally sulphur, having synergistic
Page 3 of 49
and superior properties compared to prior art formulations or mixtures or compositions. Yet it is an object of the present invention to provide a composition for plant pest control comprises compounds (i) Chlorantraniliprole (ii) at least one compound 5 selected from Thiocyclam hydrogen oxalate or Diafenthiuron that will protect crop from pest. It is further an object of the present invention to provide composition for plant pest control comprises compounds (i) Chlorantraniliprole (ii) at least one 10 compound selected from Thiocyclam hydrogen oxalate or Diafenthiuron wherein Wettable powder (WP) formulation comprises compounds (i) Chlorantraniliprole (ii) Thiocyclam hydrogen oxalate; and further Suspension Concentrate (SC) formulation comprises compounds (i) Chlorantraniliprole (ii) Diafenthiuron. 15 Another object of the present invention is to provide Wettable powder (WP) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprolein amount of0.1% to 10% (W/W) (ii) Thiocyclam hydrogen oxalate in amount of30 to 60%(W/W) and (iii) optionally sulphur in amount of 10-30%(W/W). 20 Another object of the present inventionis to provide Suspension Concentrate (SC) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprolein amount of 0.1% to 10% (W/W) (ii) or Diafenthiuronin amount of 10% to 50% (W/W) and (iii) optionally sulphur in amount of 10-25 30%(W/W). Another object of the present invention is to provide a process for the preparation of Wettable powder (WP) or Suspension Concentrate (SC) formulation for plant pest control comprises active chemical compounds (i) Chlorantraniliprole, (ii) at 30
Page 4 of 49
least one compound selected from Thiocyclam hydrogen oxalate of or Diafenthiuron and (iii) optionally sulphur. It is also an object of the present invention to provide a process for preparation of Wettable powder (WP) formulation composition for plant pest control comprises 5 compounds (i) Chlorantraniliprolein amount of 0.1% to 10% (W/W) (ii) Thiocyclam hydrogen oxalate in amount of 30 to 60% (W/W) and (iii) optionally sulphur in amount of 10-30%(W/W). It is an object of the present invention to provide a process for the preparation of 10 the Wettable powder (WP) formulation, comprising step off:
a) Mixing of antifoaming agent and an inert parts by w/w in a blender to form a mass: b) Adding said mass to a mixture of chlorantraniliprole in amount of 1% to 10 % (w/w) and Thiocyclam hydrogen oxalate in amount of 30 % to 60 % (w/w);and optionally sulphur 10-30 % w/w, wetting agent, dispersing agent ,silica, talcum powder , tri-sodium citrate and Lavigated clay parts by weight in a ribbon blender to generate a mixture mass; and c) Dry grinding or micronization of said mixture mass with the help of air jet mill and air classifier mill.
d) Dry grinding of the wettable powder (WP ) in air jet mill and air classifier mill to reduce particle size of the suspension up to less than 25 micron. 15 e) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers and dispersing agents. f) Finally getting the wettable powder (WP) formulation. It is also an object of the present invention to provide a process of preparation of Suspension Concentrate (SC) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprolein amount of 0.1% to 10% (W/W) (ii) or Diafenthiuronin amount of 10% to 50% (W/W) and (iii) optionally sulphur in amount of 10-30%(W/W). 20
Page 5 of 49
It is an object of the present invention to provide a process for the preparation of the Suspension Concentrate (SC), comprising the step of:
a) An aqueous dispersion (suspension concentrate, SC) of chlorantraniliprole in amount of 1% to 10 % (w/w) and diafenthiuron in amount of 10% to 50 % (w/w) and optionally sulphur 10-30 % w/w, mixture of chlorantraniliprole and diafenthiuron and optionally sulphur with of anti-freezing agent ,antifoaming agent and emulsifiers in water b) Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron. c) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers. d) Finally adding the viscosity agent & preservative to the suspension concentrate (SC ) formulation to enhance viscosity It is an object of the present invention to provide improved a Wettable powder 5 (WP) formulation or Suspension Concentrate (SC) formulation, of synergistic insecticidal composition is which stable and ready to use, and has superior properties compared to prior art formulations or mixtures or compositions. It is further an object of the present invention to provide a Wettable powder (WP) 10 formulation or Suspension Concentrate (SC) formulation composition for plant pest control. The further object of the present invention is to provide highly storage-stable Wettable powder (WP) formulation composition for plant pest control comprises 15 two active chemical compounds (i) Chlorantraniliprole, (ii) at least one compound selected from Thiocyclam hydrogen oxalate of or Diafenthiuron, which show excellent storage stability and biological efficacy for use in plant pest control. 20
Page 6 of 49
It is also an object to provide a method of application of composition to the plants to control the plant pest. 5 DETAILED DESCRIPTION OF THE INVENTION: In describing the embodiments of the invention, specific terminology is resorted for the sake of clarity. However, it is not intended that the invention be limited to the specific terms so selected and it is to be understood that each specific term 10 includes all technical equivalents that operate in a similar manner to accomplish a similar purpose. As used herein, the term "synergistic effect" or grammatical variations thereof means and includes a cooperative action encountered in a combination of two or 15 more active compounds in which the combined activity of the two or more active compounds exceeds the sum of the activity of each active compound alone. The term "synergistically effective amount," as used herein, means and includes an amount of two or more active compounds that provide a synergistic effect 20 defined above. The term "pesticidally effective amount," as used herein, means and includes an amount of active pesticide that causes an adverse effect to the at least one pest, wherein the adverse effect may include deviations from natural development, 25 killing, regulation, or the like.
Page 7 of 49
As used herein, the term "control" or grammatical variations thereof means and includes regulating the number of living pests or regulating the number of viable eggs of the pests or both. The present invention contains two or more active chemical compounds that 5 mutually complement each other when used together and exhibit synergistic plant pest control capabilities that is greater than the individual compound’s capability to control the plant pest when used alone. Chlorantraniliprole of formula (A), also known as 5-bromo-N-[4-chloro-2-10 methyl-6-(methylcarbamoyl)phenyl]-2-(3-chloropyridin-2-yl) pyrazole-3 carboxamide,(CAS No: 500008-45-7) is a Anthranilic-diamide insecticide. Chlorantraniliprole has low toxicity to humans and mammals. Further, it is effective at low use rates. Chlorantraniliprole is commercially available, for example, as Coragen® (available from Dupont™, Coragen is a registered 15 trademark of E. I. du Pont de Nemours and Company). Thiocyclam hydrogen oxalate of formula (B) (also known as N,N-dimethyltrithian-5-amine;oxalic acid, having CAS No.: 31895-22-4), is an insecticide and effective on pest such as Rice stem borer. Thiocyclam hydrogen 20 oxalate when applied to plant, it enters into the insect system and starts working at the nervous system. Thiocyclam hydrogen oxalate blocks the transmission of information in the larva and treated larva gets quickly paralyzed and stops feeding and damaging the plant which further looses response and tension in its body resulting in quiet death. 25 Diafenthiuron of formula (C) (CAS No: 80060-09-9) is thiourea insecticide and miticide which is mainly used to prevent and kill the pests and mites in cotton, fruit trees, vegetables, ornamental plants, soybeans and other crops. It also can be
Page 8 of 49
used to control the red spideron citrus tree and apple tree, the diamondback moth and other pests of cruciferous vegetables. In one of the embodiment present invention is wettable powder (WP) formulation composition for plant pest control comprises active chemical compounds (i) 5 Chlorantraniliprole, (ii) Thiocyclam hydrogen oxalate of and (iii) optionally sulphur. In one of the embodiment present invention is Suspension concentrate (SC) formulation composition for plant pest control comprises active chemical 10 compounds (i) Chlorantraniliprole, (ii) Diafenthiuron and (iii) optionally sulphur. The said insecticidal composition also comprises optionally sulphur which adds on in the plant nutrient properties and helps in plants growths. Sulphur is a natural element that is toxic to fungus. It is available inseveral formulations 15 including a RTU spray, wettable powder and dust. It is used for the control and prevention of black spot, rusts, leafspots and powdery mildew on roses, other ornamentals, fruits and vegetables. It is also used less frequently as a miticide. Sulphur disrupts the metabolic functioning of fungi and is one of the oldestknown pesticides. 20 Sulphur(S) is an essential plant nutrient required by all crops for optimum production. Plants take up and use S in the sulphate (SO4-S)form, which like nitrate (NO3-N), is very mobile in the soil and is proneto leaching in wet soil conditions, particularly in sandy soils. 25 Sulphur deficiencies are becoming increasingly common in Alberta..(S04). Generally, S is the third most limiting soil nutrient in cereal,oilseed and forage crop production in Alberta. It is third only to nitrogen (N) and phosphorus (P) in fertilizer use in Alberta. 30
Page 9 of 49
It is also an object of the present invention to provide a process for preparation of Wettable powder (WP) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprole in amount of 0.1% to 10% (W/W) (ii) Thiocyclam hydrogen oxalate in amount of 30 to 60% (W/W) and (iii) optionally sulphur in amount of 10-30% (W/W). 5 According to another embodiment of the present invention, there is provided Wettable powder (WP) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprole, (ii) at least one compound selected from Thiocyclam hydrogen oxalate of or Diafenthiuron and (iii) optionally sulphur. 10 Accordingly, the present invention relates to Wettable powder (WP) formulation composition comprising: a) an effective amount of Chlorantraniliprole of formula (A) in a amount between 0.1% to 10% (W/W); 15 b) an effective amount of Thiocyclam hydrogen oxalate of formula (B) in a amount between 30 to 60% or Diafenthiuron of formula (C) in a amount between 10% to 50% (W/W); c) optionally, effective amount of sulphur in a amount between 10-30% (W/W); 20 d) auxiliaries used in preparation of insecticidal composition. It is an object of the present invention to provide a process for the preparation of the Wettable powder (WP) formulation, comprising the step of:
a) Mixing of anti-foaming agent and an inert parts by w/w in a blender to 25 form a mass: b) Adding said mass to a mixture of chlorantraniliprole in amount of 1% to 10 % (w/w) and Thiocyclam hydrogen oxalate in amount of 30 % to 60 % (w/w); and optionally sulphur 10-30 % w/w, wetting agent, dispersing agent ,silica, talcum powder , tri-sodium citrate and Lavigated clay parts by weight in a ribbon blender to generate a mixture mass; and
Page 10 of 49
c) Dry grinding or micronization of said mixture mass with the help of air jet mill and air classifier mill.
d) Dry grinding of the wettable powder (WP) in air jet mill and air classifier mill to reduce particle size of the suspension up to less than 25 micron. e) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers and dispersing agents. Finally getting the wettable powder (WP) formulation. According to another embodiment of the present invention, there is provided process of preparation of Suspension Concentrate (SC) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprolein amount of 5 0.1% to 10% (W/W) (ii) or Diafenthiuronin amount of 10% to 50% (W/W) and (iii) sulphur in amount of 10-30% (W/W).
According to another embodiment of the present invention, there is provided a process for the preparation of the Suspension Concentrate (SC), comprising the 10 step of:
a) An aqueous dispersion (suspension concentrate, SC) of chlorantraniliprole in amount of 1% to 10 % (w/w) and diafenthiuron in amount of 10% to 50 % (w/w) and optionally sulphur 10-30 % w/w, mixture of chlorantraniliprole and diafenthiuron and optionally sulphur with of anti-freezing agent ,anti-foaming agent and emulsifiers in water b) Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron. c) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers. d) Finally adding the viscosity agent & preservative to the suspension concentrate (SC ) formulation to enhance viscosity According to another embodiment of the present invention, there is provided suspension concentrate (SC) formulation composition for plant pest control 15
Page 11 of 49
comprises compounds (i) Chlorantraniliprole, (ii) at least one compound selected from Thiocyclam hydrogen oxalate of or Diafenthiuron and (iii) optionally sulphur. Accordingly, the present invention relates to Suspension concentrate (SC) 5 formulation composition comprising: i. an effective amount of Chlorantraniliprole of formula (A) in a amount between 0.1% to 10% (W/W); ii. an effective amount of Thiocyclam hydrogen oxalate of formula (B) in a amount between 30 to 60% (W/W) or Diafenthiuron of formula (C) in a 10 amount between 10% to 50% (W/W); iii. optionally, effective amount of sulphur in a amount between 10-30%(W/W); iv. auxiliaries used in preparation of insecticidal composition. 15 The composition of the present invention also contains auxiliaries to be used in the process for preparing insecticidal composition. In order to prepare stable, ready to use Suspension concentrate (SC) and wettable powder (WP) formulation of insecticide compositions, Auxiliaries maybe selected from but not limited to emulsifiers or dispersing agent,wetting agents, anti-freezing agents, antifoaming 20 agents and viscosity agents. At least one emulsifieris selected from a group comprising of modified naphthalene sulphonic acid condensate sodium salt, acrylate co-polymer, poly-alkoxylated butyl ether, phenyl naphthalene sulphonates, ethoxylated alkyl phenols, ethoxylated fatty acids, alkoxylated linear alcohols, glyceryl esters, maleic anhydride co-polymers, condensation product of aryl sulphonic acids, addition product of ethylene oxide and fatty acid esters, lignin derivatives, naphthalene formaldehyde condensates, sodium salts of iso-decylsulfosuccinic acid half ester, Blend of modified poly ethanoxy ether and sulphated anionic surfactant, blend of alcohol alkoxylates& methyl methacrylate polymer, blend of
Page 12 of 49
dialkylate naphthalene sulphonic acid sodium salt, sodium alkyl benesulfonates, sodium salts of sulfonates naphthalene, ammonium salts of sulfonated naphthalene, salts of poly acrylic acids, salts of phenol sulfonic acid and salts of naphthalene sulfonic acids. At least one binding agent is selected from polyvinyl alcohols, phenyl naphthalene sulphonate, lignin derivatives, poly vinyl pyrrolidone, poly alkyl pyrrolidone, carboxymethylcellulose, xanthan gum, poly oxylated fatty acids, poly ethoxylated fatty alcohols, ethylene oxide copolymer, propylene oxide 5 copolymer, polyethylene glycols and polyethylene oxides. Atleast one wetting agent is selected from a group comprising poly oxy alkylene alkyl ether, poly oxy alkylene alkyl phenyl ether sulfonates, dialkylsuccinate, Sodium blend of alkyl naphthalene sulfonate, Sodium Dioctyl sulphosuccinate & sodium lauryl sulfonate preferably blend of alkyl naphthalene sulfonate etc.
At least one dispersing agent is selected from group comprising poly carboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, ligno sulphonates, methyl oleyl taurates ,silica poly ether copolymer and poly vinyl alcohols, Sodium salt of naphthalene sulfonate condensate, Mixture of salt of naphthalene sulphonic acid and phenol sulphonic acid condensate, Sulfonated aromatic polymer, Sodium salt preferably sodium salt of naphthalene sulfonate condensate, castor oil ethoxylate. At least one anti-foaming agent selected from a group comprising silicon based emulsion, silicon defoamer, Dimethyl polysiloxane or alcohol based anti-foam agent. There are other auxillieries such as filler, additives, preservative agent or stabilizers have been used in the said composition. 10
Page 13 of 49
At least one filler may be selected from but not limited to water ,Zinc sulfate(ZNSO4), Ferrous sulfate (FeSO4), Copper Sulfate (CuSO4), Ammonium Sulfate ((NH4)2SO4), bentonites, sub-betonites, attapulgites, kaolinites, montmorillonites, bauxite, hydrated aluminas, calcined aluminas, diatomaceous earth, chalk, fuller’s earth, dolomite, kiesulguhr, loess, prophyllites, talc, 5 vermiculites, limestone, natural and syntheticsilicates, silica and china clay. At least one additive may be selected from but not limited to macronutrients, micronutrients, minerals and urea groups, wherein macronutrients are selected from group consisting of nitrogen,phosphorous, calcium, potassium and 10 magnesium and the micronutrients are selected from the group consisting of zinc, iron,manganese, copper, boron, cobalt, vanadium, selenium, silicon and nickel. In another embedment, wettable powder (WP) formulation insecticide composition comprises (i) Chlorantraniliprole (ii) Thiocyclam hydrogen oxalate 15 may be provided as follows: Table : 1 Name of Content in Composition Amount of component (%)
Chlorantraniliprole Technical ( Purity 95.7 % w/w )
1-10 %
Thiocyclam Hydrogen oxalate Technical ( Purity 95 % w/w )
30-60 %
Emulsifier
0.1-10 %
Wetting agent
0.1-20 %
Filler
10-50 % (Quantity sufficient )
Anti-foaming agent
0.1-5 %
Dispersing agent
0.1-20 %
Optionally sulphur
10-30 %
Page 14 of 49
In another embedment, Suspension concentrate (SC) formulation composition for plant pest control comprises compounds (i) Chlorantraniliprole (ii) Diafenthiuron as follows: 5 Table : 2 Name of Content in Composition Amount of component (%)
Chlorantraniliprole Technical ( Purity 95.7 % w/w )
1-10 %
Diafenthiuron Technical ( Purity 97.2 % w/w )
10-50 %
Anti freezing agent
0.1-15%
Anti foaming agent
0.1-5 %
One or more Emulsifier
0.1-10 %
Fillers
10-70 % (Quantity sufficient )
Preservative agent or stabilizer
0.1-5%
Viscosity agent
0.1-8%
Optionally sulphur
10-30 % In another embedment, water dispersible granule(WDG) insecticide composition comprising (i) Chlorantraniliprole (ii) at least one compound selected from 10 Thiocyclam hydrogen oxalate or diafenthiuron and(iii) optionally sulphur may be provided as follows:
Table :3 15 Name of Content in Composition Amount of component (%)
Chlorantraniliprole
0.1-10%
Thiocyclam hydrogen oxalate or diafenthiuron
10-60%
Page 15 of 49
optionally Sulphur
10-30%
Dispersing agent
0.1-20%
Wetting agent
0.1-20%
Binding agent
0.1-5%
Suspending agent
1-15%
Deforming agent or antifoaming agent
0.1-5%
Preservative agent or stabilizer
0.1-5%
Filler
10-70% or Q.S
Example 1: Preparation of chlorantraniliprole (~5 %) + Thiocyclam hydrogen oxalate (~ 45 %) Wettable powder (WP) formulation: Table : 4 5
S.No
Raw Material Name
Inputs Qty (gm.)
1
Chlorantraniliprole Technical ( Purity 95.7 % w/w )
13.65 gm
2
Thiocyclam Hydrogen oxalate Technical ( Purity 95 % w/w )
118.95 gm
3
Blend of dialkylate naphthalene sulphonic acid sodium salt ( Emulsifier)
20 gm
4
Acrylate co-polymer ( Emulsifier )
6.25 gm
5
Sodium Ligno sulphonate (SLS) ( Wetting agent )
6.25 gm
6
Silica ( Filler )
28 gm
7
Talcum powder ( Filler )
60.50 gm
8
Total Qty
253.6 gm
Preparation of chlorantraniliprole (~5 %) + Thiocyclam hydrogen oxalate (~ 45 %) Wettable powder (WP) formulation
Charge The chlorantraniliprole Technical (Qty 13.65gm) and thiocyclam 10 hydrogen oxalate Technical (Qty 118.95 gm)into the blender with Blend of dialkylate naphthalene sulphonic acid sodium salt(Qty 20gm),Acrylate
Page 16 of 49
copolymer (Qty6.25gm), sodium ligno sulphonate (SLS) (Qty 6.25 gm), silica (Qty 28 gm) and Talcum powder (Qty 60.5 gm) with dry grinding of wettable powder (WP) to reduce particle size of the WP formulation is less than 25 microns.
5
Further chlorantraniliprole (~5 %) + Thiocyclam hydrogen oxalate (~ 45 %) wettable powder (WP) formulation of off white colored solid powder was obtained, having suspensibility of chlorantraniliprole & Thiocyclam hydrogen oxalate more than 95 %and Particle size (By Malvern master sizer ):- D(50 ) = 1.978 µm, D(90 ) = 5.410 µm, 10
Example 2: The stability data of formulation of chlorantraniliprole (~5 %) +
Thiocyclam hydrogen oxalate (~ 45 %) (WP) Wettable powder formulation (Example 1) 15
Table :5 STORAGE STABILITY DATA
Parameter
Specification
(In House)
Initial
Heat Stability study at 54± 2OC for 14 Days
Cold Storage stability study at 0 ± 2OC for 14 Days
Description
White to off white colored viscous liquid.
Complies
Complies
Complies
Chlorantraniliprole ( A.I. Content )
5 to 6 % w/w
( by HPLC )
Complies
Complies
Complies
Page 17 of 49
Chlorantraniliprole ( Suspensibility )
Min 80 %
( by HPLC )
Complies
Complies
Complies
Thiocyclam hydrogen oxalate
( A.I.Content )
43 to 47 % w/w
( by HPLC )
Complies
Complies
Complies
Thiocyclam hydrogen oxalate
( Suspensibility )
Min 80 %
Complies
Complies
Complies
pH(1% Aqueous solution )
2-7
Complies
Complies
Complies
Wettability (second)
5-30 Sec
Complies
Complies
Complies
Wet sieve test
( 75 µm)
Min 99 % pass through sieve test
Complies
Complies
Complies
The results were found satisfactory and this formulation is passing in all physicochemical properties.
Example 3: Process of Preparation of chlorantraniliprole (~5 %) + 5
Diafenthiuron (~ 25 %) Suspension concentrate (SC) formulation
Table : 6
S.No
Raw Material Name
Inputs Qty (gm.)
1
Chlorantraniliprole Technical ( Purity 95.7 % w/w )
21.73 gm.
2
Diafenthiuron Technical ( Purity 97.2 % w/w )
100.8 gm.
3
Propylene Glycol ( P.G ) ( Anti freezing agent)
40 gm.
4
Anti foaming agent
4 gm.
5
Modified naphthalene sulphonic acid condensate sodium
8 gm.
Page 18 of 49
salt ( Emulsifier )
6
Blend of alcohol alkoxylated and methyl methacrylate polymer ( Emulsifier )
10 gm.
7
Water (Filler)
193.4 gm.
8
Formaldehyde ( 40 % in water )
2 gm.
9
Gum( xanthan gum ,1 % solution in water )
20 gm.
10
Total Qty
399.93 gm
Preparation of chlorantraniliprole (~5 %) + Diafenthiuron (~ 25 %) Suspension concentrate (SC) formulation:-
The chlorantraniliprole Technical (Qty21.73 gm.) and diafenthiuron technical 5 (Qty 100.8 gm) was added to the reactor containing in propylene glycol (P.G.) (Qty40gm) in water (Qty193.4gm)with modified naphthalene sulphonic acid condensate sodium salt (Qty 8 gm) and blend of alcohol alkoxylated & methyl methacrylate polymer (Qty 10gm) with stirring for 10-15minutes at room temperature (Temperature 30 ±5 °C). Further Anti-foaming (Qty4gm) was 10 charged into reaction vessel with continue stirring for 50-55 minutes at room temperature (Temperature 30 ±5°C).
The above mixture was wet grinded in bead mill at temperature 15-16°C( This process for minimized /reduce particle size of Suspension below ~25 microns 15 after wet grinding particle size was determined by sieve test (99 % min material pass through 25 micron sieve test )
Further chlorantraniliprole (~5 %) + Diafenthiuron (~25 %) suspension concentrate (SC) formulation of off white colored viscous liquid was obtained, 20 having suspensibility of chlorantraniliprole & diafenthiuron more than 95 %,viscosity 421 cps and Particle size (By Malvern master sizer ):- D(50 ) = 1.963 µm, D(90 ) = 4.142 µm,
Page 19 of 49
Example 3: The stability data of formulation of chlorantraniliprole (~5 %) +
Diafenthiuron (~ 25 %) (SC) Suspension concentrate 5 formulation
Table 7: STORAGE STABILITY DATA:-
Parameter
Specification
In House
Initial
Heat Stability study at 54± 2OC for 14 Days
Cold Storage stability study at 0 ± 2OC for 14 Days
Description
White to off white colored viscous liquid.
Complies
Complies
Complies
Chlorantraniliprole ( A.I.Content )
4.5 to 6 % w/w
( by HPLC )
Complies
Complies
Complies
Chlorantraniliprole ( Suspensibility )
Min 80 %
( by HPLC )
Complies
Complies
Complies
Diafenthiuron
( A.I.Content )
24 to 26 % w/w ( by HPLC )
Complies
Complies
Complies
Page 20 of 49
Diafenthiuron
( Suspensibility )
Min 80 %
Complies
Complies
Complies
pH.
5-9
Complies
Complies
Complies
Viscosity ( cps )
375 to 600 cps
Complies
Complies
Complies
The results were found satisfactory and this formulation is passing in all physicochemical properties.
Bio field trial: 5
Evaluation of bio-efficacy and Phytotoxicity of Chlorantraniliprole 5% + Diafenthiuron 25% SC on Cotton for the control of pests like white fly, aphids, Jassids, Thrips, bollworm.
Chlorantraniliprole 5% + Diafenthiuron 25% SC 10
Objective:
(i) To determine the bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC against white fly, aphids, Jassids, Thrips, bollworm of Cotton crop. 15
(ii) To determine Phytotoxicity of Chlorantraniliprole 5% + Diafenthiuron 25% SC on Cotton crop.
Table : 8 20
Details of Experiment
a) Test chemical
Chlorantraniliprole 5% + Diafenthiuron 25% SC
Page 21 of 49
b) Crop
Cotton
c) Location
Karjan, Vadodara, Gujarat
d) Target crops
white fly, aphids, Jassids, Thrips, bollworm
e) Plot size
3.0 m × 3.0 m
f) Design
RBD (Randomized Block Design)
g) Treatment
7(Seven); Table 1
h) Number of reapplication
03
i) Application method
Spray by knapsack sprayer fitted with flat fan nozzle (5 Liter)
j) Water volume used
500 liters/ha
Table :9: Treatment details for bio-efficacy of different insecticide:
SR. No.
Treatment
Dosage Formulation
(A.I. gm/ha)
1.
Chlorantraniliprole 5% + Diafenthiuron 25% SC (1 ml)
25+125= 150
2.
Chlorantraniliprole 5% + Diafenthiuron 25% SC (0.8 ml)
20+100=120
3.
Chlorantraniliprole 5% + Diafenthiuron 25% SC (0.6 ml)
15+75=90
4.
Chlorantraniliprole 5% + Diafenthiuron 25% SC (1.2 ml)
30+150=180
5.
Chlorantraniliprole 18.5% SC
30
6.
Diafenthiuron 50% WP
300
7.
Untreated control (water only)
-
Example 4: Bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC 5
Page 22 of 49
against Cotton whitefly.
Table : 10
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of whitefly/leaf (15 leaves/ 5 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+ Diafenthiuron 25% SC (F=1ml/L)
25 + 125
18
11.70
7.56
4.86
2.34
2.88
84%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC (F=0.8ml/L)
20 + 100
17
13.09
9.86
6.29
3.74
4.59
73%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC (F=0.6ml/L)
15 + 75
16
13.12
11.84
9.28
8.32
8.64
46%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC (F=1.2ml/L)
30 + 150
17
8.84
5.27
2.72
0.68
1.36
92%
Chlorantranilipr
30
17
15.4
14.9
14.1
13.9
14.2
16%
Page 23 of 49
ole 18.5% SC
7
6
1
4
8
Diafenthiuron 50% WP
300
18
13.68
9.72
5.94
4.14
4.50
75%
Untreated control
-
16
15.36
14.72
14.40
13.92
14.08
12%
Results :
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose were at as per they exhibited whitefly pest control 87, 96 per cent after 7 days 5 and 84, 92 per cent after 10 days of spray.
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Diafenthiuron 50% WP @ 10 300 for control of whitefly after 7 and 15 days of spray.
Example 5: Bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC
against Cotton Aphids.
15
Table : 11
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of Aphids /leaf (15 leaves/ 5 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+
25 + 125
22
15.84
12.54
5.28
2.64
3.08
86%
Page 24 of 49
Diafenthiuron 25% SC
(F=1ml/L)
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.8ml/L)
20 + 100
24
18.96
14.88
7.68
5.28
6.24
74%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.6ml/L)
15 + 75
25
21.00
19.50
15.50
11.75
13.25
47%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1.2ml/L)
30 + 150
24
13.68
9.36
3.36
0.96
2.16
91%
Chlorantraniliprole 18.5% SC
30
23
21.39
20.24
19.09
18.17
18.86
18%
Diafenthiuron 50% WP
300
22
16.28
12.98
6.16
4.62
5.06
77%
Untreated control
-
23
21.62
21.16
20.93
20.70
21.39
7%
Results :
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose were at as per they exhibited Aphids pest control 88, 96 per cent after 7 days 5 and 86, 91 per cent after 10 days of spray.
Page 25 of 49
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Diafenthiuron 50% WP @ 300 for control of Aphids after 7 and 15 days of spray. 5
Example 6: Bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC
against Cotton Jassids.
Table : 12 10
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of Jassids/leaf (15 leaves/ 5 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1ml/L)
25 + 125
29
19.14
13.92
6.67
2.90
3.77
87%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.8ml/L)
20 + 100
28
19.88
14.84
10.64
6.16
7.28
74%
Chlorantraniliprole 5%+ Diafenthiuron
15 + 75
29
23.78
21.17
17.11
12.47
13.92
52%
Page 26 of 49
25% SC
(F=0.6ml/L)
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1.2ml/L)
30 + 150
31
16.74
9.92
5.27
1.24
2.17
93%
Chlorantraniliprole 18.5% SC
30
28
24.92
23.52
23.52
20.78
21.56
23%
Diafenthiuron 50% WP
300
30
20.10
15.30
10.80
6.00
6.60
78%
Untreated control
-
28
26.32
25.76
24.92
24.36
24.64
12%
Results :
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose were at as per they exhibited Jassids pest control 90, 96 per cent after 7 days 5 and 87, 93 per cent after 10 days of spray.
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Diafenthiuron 50% WP 10 @ 300 for control of Jassids after 7 and 15 days of spray.
Example 7: Bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC
against Cotton Thrips. 15
Table : 13
Page 27 of 49
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of Thrips/leaf (15 leaves/ 5 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1ml/L)
25 + 125
16
8.64
5.12
2.08
0.48
0.64
96%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.8ml/L)
20 + 100
18
12.42
8.46
3.78
2.52
3.06
83%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.6ml/L)
15 + 75
17
12.92
8.84
5.44
4.08
4.76
72%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1.2ml/L)
30 + 150
18
7.56
3.78
1.62
0.36
0.54
97%
Chlorantraniliprole 18.5% SC
30
17
15.30
14.96
14.45
12.92
13.43
21%
Diafenthiuron 50% WP
300
18
11.52
7.02
3.42
2.16
2.88
84%
Page 28 of 49
Untreated control
-
16
15.04
14.72
14.40
14.08
14.24
11%
Results :
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and 5 Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose were at as per they exhibited Thrips pest control 97, 98 per cent after 7 days and 96, 97 per cent after 10 days of spray.
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose 10 showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Diafenthiuron 50% WP @ 300 for control of Thrips after 7 and 15 days of spray.
15 Example 8: Bio-efficacy of Chlorantraniliprole 5% + Diafenthiuron 25% SC
against Cotton Bollworm.
Table : 14
20
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of Bollworm /plant (5 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+
25 + 125
6
25.38
3.12
1.68
0.96
1.08
82%
Page 29 of 49
Diafenthiuron 25% SC
(F=1ml/L)
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.8ml/L)
20 + 100
7
5.46
4.13
2.24
1.47
1.68
76%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=0.6ml/L)
15 + 75
5
4.10
3.40
2.85
2.60
2.70
46%
Chlorantraniliprole 5%+ Diafenthiuron 25% SC
(F=1.2ml/L)
30 + 150
7
3.64
2.31
0.98
0.42
0.56
92%
Chlorantraniliprole 18.5% SC
30
6
4.56
3.42
1.74
1.20
1.32
78%
Diafenthiuron 50% WP
300
7
6.65
6.51
6.44
6.09
6.23
11%
Untreated control
-
6
5.76
5.64
5.58
5.46
5.52
8%
Results :
• Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose were at as per they exhibited bollworm pest control 84, 94 per cent after 7 5 days and 82, 92 per cent after 10 days of spray.
Page 30 of 49
• Chlorantraniliprole 5% + Pyriproxyfen 5% SE @ 150 gm (a.i./ha) and Chlorantraniliprole 5% + Diafenthiuron 25% SC @ 180 gm (a.i./ha) dose showed synergistic effect and significantly superior or standard check by separately Chlorantraniliprole 18.5% SC @ 30 and Diafenthiuron 50% WP @ 300 for control of bollworm after 7 and 15 days of spray. 5
REPORT OF PHYTO-TOXICITTY EVALUATION ON COTTON CROP
Evaluation of phyto-toxicity effect of Chlorantraniliprole 5%+ Diafenthiuron 25% SC @ 150,120,90 & 180 gm/ha on cotton crop. 10
Evaluation of phyto-toxicity effect of sample Example ___ on Cotton crop
TABLE-15
15
Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein clearing, Wilting before and after spraying of sample Example ___on Cotton crop:
Treatment
DAS of observation
Before spray
1 DAS
3 DAS
5 DAS
7 DAS
10 DAS
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
T1
0
0
0
1
0
0
0
0
0
0
0
0
0
0
0
0
0
0
T2
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
T3
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
T4
0
0
0
0
1
1
0
0
0
0
0
0
0
0
0
0
0
0
T5
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
*DAS= Days After spray
C+D-01= Chlorantraniliprole 5%+ Diafenthiuron 25% SC 20
T1 C+D-01 (25+125)F=1ml/L
Page 31 of 49
T2 C+D-01 (20+100)F=0.8ml/L
T3 C+D-01 (15+75)F=0.6ml/L
T4 C+D-01 (30+150)F=1.2ml/L
T5 Untreated control(Water only)
5
Conclusion: 10
Results of phyto-toxicity evaluation trial are given in table 15. As per results we are concluded that different doses of Chlorantraniliprole 5%+ Diafenthiuron 25% SC (manufactured by Crop life science limited, Ankleshwar, Gujarat) were cause Negligible phytotoxic symptoms on Cotton plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic 15 effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5%+ Diafenthiuron 25% SC is safe to use on Cotton at the dosage from 150, 120, 90 & 180 gm/ha.
Bio field trial: 20
Evaluation of bio-efficacy and Phytotoxicity of Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP on Rice for the control of pests like Stem borer& Leaf folder.
25
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP
Objective:
(i) To determine the bio-efficacy of Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP against Stem borer & Leaf folder of Rice 30 crop.
Page 32 of 49
(ii) To determine Phytotoxicity of Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP on Rice crop.
Table :16
5
Details of Experiment
a) Test chemical
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP
b) Crop
Rice
c) Location
Misroth, Bhopal, Madhya Pradesh.
C) Target crops
Stem borer& Leaf folder.
d) Plot size
3.0 m × 3.0 m
e) Design
RBD (Randomized Block Design)
f) Treatment
7(Seven); Table 1
g) Number of reapplication
03
h) Application method
Spray by knapsack sprayer fitted with flat fan nozzle (15 Liter)
i) Water volume used
500 liters/ha
Table :17: Treatment details for bio-efficacy of different insecticide:
SR. No.
Treatment
Dosage Formulation
(A.I. gm/ha)
1.
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP (1 ml)
25+225=250
2.
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP (0.8 ml)
20+180=200
3.
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP (0.6 ml)
15+135=150
Page 33 of 49
4.
Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP (1.2 ml)
30+270=300
5.
Chlorantraniliprole 18.5% SC
30
6.
Thiocyclam Hydrogen Oxalate 0.4% GR
500
7.
Untreated control (water only)
-
Example 9: Bio-efficacy of Chlorantraniliprole 5% + Thiocyclam Hydrogen
Oxalate 45% WP against Rice Stem borer.
5
Table :18:
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of stem borer (9 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP (F=1ml/L)
25 + 225
28
15.12
10.36
6.16
2.24
2.80
90%
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP (F=0.8ml/L)
20 + 180
30
20.40
15.60
9.60
4.50
5.40
82%
Page 34 of 49
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP (F=0.6ml/L)
15 + 135
29
23.49
21.17
16.82
14.79
15.66
46%
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP (F=1.2ml/L)
30 + 270
31
17.36
9.92
4.96
1.24
1.86
94%
Chlorantraniliprole 18.5% SC
30
30
22.80
18.30
12.60
10.50
11.1
63%
Thiocyclam Hydrogen Oxalate 0.4% GR
500
32
21.76
17.92
12.16
9.28
10.56
67%
Untreated control
-
29
26.97
25.81
25.23
24.65
24.94
14%
Results :
• Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 250 gm (a.i./ha) and Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 300 gm (a.i./ha) dose were at as per they exhibited stem borer 5 pest control 92, 96 per cent after 7 days and 90, 94 per cent after 10 days of spray.
• Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 250 gm (a.i./ha) and Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 300 gm (a.i./ha) dose showed synergistic effect and 10 significantly superior or standard check by separately Chlorantraniliprole
Page 35 of 49
18.5% SC @ 30 and Thiocyclam Hydrogen Oxalate 0.4% GR @ 500 for control of stem borer after 7 and 15 days of spray.
5
Example 10: Bio-efficacy of Chlorantraniliprole 5% + Thiocyclam
Hydrogen Oxalate 45% WP against Rice Leaf folder
Table :19 10
Treatments
DOSE
gm/ha
Observed Value Before Spray
Observed Value After Spray
% Pest control
Mean of No. of Leaf folder
(9 Plants/ treatment)
1st
2nd
3rd
4th
5th
1 day
3 day
5 day
7 day
10 day
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP
(F=1ml/L)
25 + 225
21
10.29
6.72
3.36
1.05
1.68
92%
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP(F=0.8ml/L)
20 + 180
23
14.26
11.27
7.13
4.37
5.06
78%
Chlorantranilipr
15 +
22
16.2
11.4
9.68
7.92
8.58
61%
Page 36 of 49
ole 5%+ Thiocyclam Hydrogen Oxalate 45% WP
(F=0.6ml/L)
135
8
4
Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP (F=1.2ml/L)
30 + 270
25
8.50
4.00
1.50
1.00
0.75
97%
Chlorantraniliprole 18.5% SC
30
23
14.49
11.73
8.28
5.06
5.52
76%
Thiocyclam Hydrogen Oxalate 0.4% GR
500
24
15.84
12.96
9.36
6.24
6.72
72%
Untreated control
-
22
19.36
18.70
18.48
18.04
18.26
17%
Results :
• Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 250 gm (a.i./ha) and Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 300 gm (a.i./ha) dose were at as per they exhibited Leaf 5 folder pest control 95, 96 per cent after 7 days and 92, 97 per cent after 10 days of spray.
• Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 250 gm (a.i./ha) and Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP @ 300 gm (a.i./ha) dose showed synergistic effect and 10 significantly superior or standard check by separately Chlorantraniliprole
Page 37 of 49
18.5% SC @ 30 and Thiocyclam Hydrogen Oxalate 0.4% GR @ 500 for control of Leaf folder after 7 and 15 days of spray.
REPORT OF PHYTO-TOXICITTY EVALUATION ON RICE CROP
5
Evaluation of phyto-toxicity effect of Wettable powder formulation of insecticidal composition of Chlorantraniliprole 5% and Thiocyclam Hydrogen Oxalate 45% WP on 250, 180, 150 & 300 gm/ha on Rice crop.
10
TABLE-20 Symptoms of Leaf injury, Epinasty, Hyponasty, Necrosis, Vein
clearing, Wilting before and after spraying of sample Example ______ on Rice crop:
Treatment
DAS of observation
Before spray
1 DAS
3 DAS
5 DAS
7 DAS
10 DAS
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
R1
R2
R3
T1
0
0
0
1
0
1
0
0
0
0
0
0
0
0
0
0
0
0
T2
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
T3
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
T4
0
0
0
1
1
0
0
0
0
0
0
0
0
0
0
0
0
0
T5
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
15
*DAS= Days After spray
C+T-01=Chlorantraniliprole 5% + Thiocyclam Hydrogen Oxalate 45% WP
Treatment: 20
T1= C+P-01 (25+25) F=1ml/L
Page 38 of 49
T2= C+P-01 (20+20) F=0.8ml/L
T3= C+P-01 (15+15) F=0.6ml/L
T4= C+P-01 (30+30) F=1.2ml/L
T5 =Untreated control (Water only)
5
Conclusion:
Results of phyto-toxicity evaluation trial are given in table 20. As per results we are concluded that different doses of Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP(manufactured by Crop life science limited, 10 Ankleshwar, Gujarat) were cause Negligible phytotoxic symptoms on Rice plant after the spraying, however plants are recover within 7-10 days of application. It may be due to phytotonic effect and weather effect Hence, it may be concluded that Chlorantraniliprole 5%+ Thiocyclam Hydrogen Oxalate 45% WP is safe to use on Rice at the dosage from 250, 200, 150&300gm/ha. ,CLAIMS:CLAIMS We claim; [CLAIM 1]. The novel synergistic insecticidal composition comprises: a) component (A) Chlorantraniliprole in a amount between 1% to 10 % (w/w) b) component (B) at least one pesticide selected from Diafenthiuron in a amount between 10% to 50 % (w/w) or Thiocyclam hydrogen oxalate in a amount between 30 % to 60 % (w/w); c) optionally sulphur in an amount of 10-30% (w/w); d) in active excipients selected form anti-freezing, emulsifiers, antifoaming agent, stabilizing agent, viscosity agent, filler, anticaking agent, wetting and dispersing agent.
[CLAIM 2]. The novel synergistic insecticidal composition formulation as claimed in claim 1, wherein inactive excipients are selected from the group consisting of emulsifiers, anti-freezing agents, antifoaming agents, viscosity agents, fillers, stabilizers,wetting agents, dispersing agent ,anti-caking agent ,binder and inert carrier. [CLAIM 3]. The novel synergistic insecticidal compositionas claimed in claim 1, wherein an effective amount of Chlorantraniliprole in a amount between 1% to 10 % (w/w/) and preferably in a amount between 5 % to 6 % (w/w). [CLAIM 4]. The novel synergistic insecticidal compositionas claimed in claim 1,wherein an effective amount of Thiocyclam hydrogen oxalate in a amount between 30 % to 60 % (w/w) and preferably in a amount between 44 % to 46 % (w/w).
Page 2 of 49
[CLAIM 5]. The novel synergistic insecticidal compositionas claimed in claim 1, wherein an effective amount of Diafenthiuron in a range between 10% to 50 % (w/w) and preferably in a amount between 24 % to 26 % (w/w).
[CLAIM 6]. The novel synergistic insecticidal compositionas claimed in claim 1, wherein preferred formulation are selected form Wettable powder formulation (WP) or Suspension concentrate (SC) formulation. [CLAIM 7]. The novel synergistic insecticidal composition as claimed in claim 1, wherein prepared formulation product of chlorantraniliprole and Diafenthiuron is Suspension concentrate (SC ) formulation. [CLAIM 8]. The novel synergistic insecticidal composition as claimed in claim 7, wherein Suspension concentrate (SC )formulation comprises: a) component (A) Chlorantraniliprole in an amount between 1% to 10 % (w/w) b) component (B) Diafenthiuron in an amount between 10% to 50 % (w/w) c) optionally sulphur in an amount of 10-30% (w/w); d) anti-freezing agent in an amount of 0.1-15 % w/w; e) one or more emulsifiers in an amount of 0.1-10% w/w; f) anti-foaming agent in an amount of 0.1-5 % w/w; g) stabilizing agent in an amount of 0.1-5 % w/w; h) viscosity agent in an amount of 0.1-8 % w/w; i) filler in amount of 10-70 % w/w (Quantity sufficient). [CLAIM 9]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein the process for the preparation of the suspension concentrate (SC ) from, comprising step off:
Page 3 of 49
a) An aqueous dispersion (suspension concentrate, SC) of chlorantraniliprole in amount of 1% to 10 % (w/w) and diafenthiuron in amount of 10% to 50 % (w/w) and optionally sulphur 10-30 % w/w, mixture of chlorantraniliprole and diafenthiuron and optionally sulphur with of anti-freezing agent,antifoaming agent and emulsifiers in water.Wet grinding of the suspension in pressurized bead mill to reduce particle size of the suspension up to less than 25 micron.
b) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers;
c) adding viscosity agent and preservative to the suspension viscosity between 300 to 550 cps . [CLAIM 10]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein emulsifiers is selected from a group comprising of modified naphthalene sulphonic acid condensate sodium salt, acrylate co-polymer, poly-alkoxylated butyl ether, phenyl naphthalene sulphonates, ethoxylated alkyl phenols, ethoxylated fatty acids, alkoxylated linear alcohols, glyceryl esters, maleic anhydride co-polymers, condensation product of aryl sulphonic acids, addition product of ethylene oxide and fatty acid esters, lignin derivatives, naphthalene formaldehyde condensates, sodium salts of iso-decylsulfosuccinic acid half ester, Blend of modified poly ethanoxy ether and sulphated anionic surfactant, blend of alcohol alkoxylates& methyl methacrylate polymer, blend of dialkylate naphthalene sulphonic acid sodium salt, sodium alkyl benesulfonates, sodium salts of sulfonates naphthalene, ammonium salts of sulfonated naphthalene, salts of poly acrylic acids, salts of phenol sulfonic acid and salts of naphthalene sulfonic acids.
Page 4 of 49
[CLAIM 11]. The novel synergistic insecticidal composition as claimed in claim 7 to 8,wherein emulsifiers is selected from a group comprising of modified naphthalene sulphonic acid condensate sodium salt, Acrylate co-polymer, Poly-alkoxylated butyl ether, blend of alcohol alkoxylates& methyl methacrylate polymer, blend of dialkylate naphthalene sulphonic acid sodium salt, Blend of modified poly ethanoxy ether .
[CLAIM 12]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein one or more emulsifiers used are in an amount of 0.1-10 % w/w. [CLAIM 13]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein anti-freezing agent selected from a group comprising of propylene glycol, diethylene glycol, Mono ethylene glycol, polyol, polyvinyl alcohols and polyethylene glycols, 1,2- Propylene glycol, mono propylene glycol, 1,2-propanediot. [CLAIM 14]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein anti-freezing agent is preferably propylene glycol. [CLAIM 15]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein anti-freezing agent is in an amount of 0.1-15 % w/w. [CLAIM 16]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein viscosity agent is a group comprising, xanthan gum, gelatine, poly vinyl pyrrolidone, polyvinyl alcohol, sodium methyl cellulose, Polysaccharide derivative, Poly vinyl pyrrolidone (PVP K-30), silicon oil compound and guar gum.
Page 5 of 49
[CLAIM 17]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein viscosity agent is preferably xanthan Gum. [CLAIM 18]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein viscosity agent is in an amount of 0.1-8 % w/w. [CLAIM 19]. The novel synergistic insecticidal composition as claimed in claim 7 to 8,wherein anti foaming agent is silicon based emulsion, silicon defoamer, Dimethyl polysiloxane or alcohol based antifoam agent. [CLAIM 20]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein anti foaming is selected from the group consisting of Dimethyl polysiloxane. [CLAIM 21]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein anti foaming agent is in an amount of 0.1-5 % w/w.
[CLAIM 22]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein filler is water. (Demineralized water).
[CLAIM 23]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein filler is in an amount of 10-70% w/w (Quantity sufficient).
[CLAIM 24]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein Particle size of less than 25 microns.
Page 6 of 49
[CLAIM 25]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein Particle size D(50) is less than 5.0 µm & D( 90) is less than 10.0 µm.
[CLAIM 26]. The novel synergistic insecticidal composition in a suspension concentrate (SC) form formulation as claimed in claim 25, wherein synergistic chlorantraniliprole (~5 %) and diafenthiuron (~25 %) Particle size is:- i. D(10 ) = 0.743 µm ii. D(50 ) = 1.968 µm iii. D(90 ) = 4.142 µm iv. D( 100 ) = 8.662 µm
[CLAIM 27]. The novel synergistic insecticidal composition as claimed in claim 7 to 8, wherein Viscosity is 300cps to 550cps. [CLAIM 28]. The novel synergistic insecticidal composition as claimed in claim 1, wherein prepared formulation product of chlorantraniliprole and Thiocyclam hydrogen oxalate is Wettable powder formulation (WP). [CLAIM 29]. The novel synergistic insecticidal composition as claimed in claim 28, wherein wettable powder (WP ) formulation comprises: a) component (A) Chlorantraniliprole in an amount between 1% to 10 % (w/w) b) component (B) Thiocyclam hydrogen oxalate in an amount between 30 % to 60 % (w/w); c) optionally sulphur in an amount of 10-30% (w/w); d) one or more emulsifiers in an amount of 0.1-10% w/w; e) antifoaming agent in an amount of 0.1-5 % w/w; f) filler (inert carrier ) in amount of 10-50 % w/w (Quantity sufficient); g) a wetting and dispersing agent in an amount of 0.1-20% w/w;
Page 7 of 49
h) an anticaking agent in an amount of 2-10 % w/w.
[CLAIM 30]. The novel synergistic insecticidal composition as claimed in claim 29, wherein the process for the preparation of the wettable powder (WP ) from, comprising step off:
a) Mixing of antifoaming agent and an inert parts by w/w in a blender to form a mass:
b) Adding said mass to a mixture of chlorantraniliprole in amount of 1% to 10 % (w/w) and Thiocyclam hydrogen oxalate in amount of 30 % to 60 % (w/w);and optionally sulphur 10-30 % w/w, wetting agent, dispersing agent ,silica, talcum powder, tri-sodium citrate and Lavigated clay parts by weight in a ribbon blender to generate a mixture mass; and
c) Dry grinding or micronization of said mixture mass with the help of air jet mill and air classifier mill.
d) Dry grinding of the wettable powder (WP ) in air jet mill and air classifier mill to reduce particle size of the suspension up to less than 25 micron.
e) One or more additives selected from the group consisting of non-ionic or anionic emulsifiers and dispersing agents.
f) Finally getting the wettable powder (WP) formulation.
[CLAIM 31]. The novel synergistic insecticidal composition as claimed in claim 28 to 30, wherein wetting agent is selected from a group comprising poly oxy alkylene alkyl ether, poly oxy alkylene alkyl phenyl ether sulfonates, dialkylsuccinate, Sodium blend of alkyl naphthalene sulfonate, Sodium Dioctyl sulphosuccinate & sodium lauryl sulfonate preferably blend of alkyl naphthalene sulfonate.
[CLAIM 32]. The novel synergistic insecticidal composition as claimed in claim 28 to 30, wherein wetting agent is in amount of 0.1 – 20% w/w.
Page 8 of 49
[CLAIM 33]. The novel synergistic insecticidal compositionas claimed in claim 28 to 30, wherein dispersing agent is selected from group comprising poly carboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, ligno sulphonates, methyl oleyl taurates ,silica poly ether copolymer and poly vinyl alcohols, Sodium salt of naphthalene sulfonate condensate, Mixture of salt of naphthalene sulphonic acid and phenol sulphonic acid condensate, Sulfonated aromatic polymer, Sodium salt preferably sodium salt of naphthalene sulfonate condensate, castor oil ethoxylate.
[CLAIM 34]. The novel synergistic insecticidal composition as claimed in claim 28 to 30, wherein dispersing agent is in amount of 0.1 – 20% w/w.
[CLAIM 35]. The novel synergistic insecticidal compositionas claimed in claim 28 to 30, wherein inert carrier are silica, Hydrophobic silica powder, Colloidal silica and lavigated clay, talcum powder, china clay.
[CLAIM 36]. The novel, synergistic insecticidal composition as claimed in claim 28 to 30, wherein filler for Wettable powder formulation (WP) are Silica , Talcum powder, lavigated clay, china clay.
[CLAIM 37]. The novel synergistic insecticidal compositionas claimed in claim 28 to 30, wherein inert carrier are silica and lavigated clay ,is in an amount of 10-50 % w/w ( Quantity sufficient ).
[CLAIM 38]. The novel synergistic insecticidal compositionas claimed in claim 28 to 30,wherein said mixture are dry grinding in air jet mill and air classifier mill to average particle size of less than 25 microns.
Page 9 of 49
[CLAIM 39]. The novel synergistic insecticidal composition in a wettable powder (WP ) form formulation as claimed in claim 38, wherein synergistic chlorantraniliprole (~5 %) and thiocyclam hydrogen oxalate (~45 %) Particle size is:- i. D(10 ) = 0.723 µm ii. D(50 ) = 1.978 µm iii. D(90 ) = 5.410 µm iv. D(100 ) = 16.398 µm