FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
THE PATENT RULES, 2003
COMPLETE SPECIFICATION
[See Section 10 and Rule 13]
Title of the invention: AN INSECTICIDAL COMPOSITION
Name of the Applicant: UPL LIMITED
Nationality: India
Address: UPL House, 610 B/2, Bandra Village, Off
Western Express Highway, Bandra-East,
Mumbai-400051, India
2
Field of the Invention
The present disclosure relates to an agrochemical composition. More particularly,
the present disclosure relates to an insecticidal composition 5 with good stability and
dispersibility and a method for controlling insects using said composition.
Background of the Invention
Fipronil (chemical name 5-amino-1-[2,6-dichloro-4-(trimethylmethyl)sulfinyl]-1H10
pyrazole-3-carbonitrile), represented by formula I, is a member of another relatively
new class of pesticides, the phenylpyrazole insecticides. Fipronil is photolyzed into
several degradates represented by desulfinyl fipronil and fipronil sulfone in the
field. Fipronil is also rapidly metabolized to fipronil sulfone in plants.
15 Formula I
Pymetrozine, chemically known as 6-methyl-4-{(E)-pyridin-3-ylmethylidene)
amino}-4, 5- dihydro-1, 2, 4-triazin-3(2H)-one represented by formula II, is a
selective insecticide. 􀀳􀁜􀁐􀁈􀁗􀁕􀁒􀁝􀁌􀁑􀁈􀀃􀁌􀁖􀀃􀁄􀁑􀀃􀁈􁂇􀁈􀁆􀁗􀁌􀁙􀁈􀀃􀁆􀁋􀁈􀁐􀁌􀁆􀁄􀁏􀀃􀁄􀁊􀁄􀁌􀁑􀁖􀁗􀀃􀁓􀁏􀁄􀁑􀁗-sucking
20 􀁌􀁑􀁖􀁈􀁆􀁗􀁖􀀃􀁖􀁘􀁆􀁋􀀃􀁄􀁖􀀃􀁄􀁓􀁋􀁌􀁇􀁖􀀏􀀃􀁚􀁋􀁌􀁗􀁈􀃀􀁌􀁈􀁖􀀏􀀃􀁏􀁈􀁄f hoppers, and plant hoppers that damage
crops such as rice, vegetables, cotton, wheat, and fruit trees and has been used
in integrated pesticide programs and management.
Formula II
5
10
15
20
3
Water Dispersible Granules (WDGs) are solid, non-dusty formulations which
disperse or dissolve quickly when added to water in a spray tank to give a fine
particle suspension. WDGs are important delivery vehicles for active
agrochemicals because, unlike emulsion concentrates, they are solvent-free, do
not have dusting problems like wettable 􀁓􀁒􀁚􀁇􀁈􀁕􀁖􀀃􀀋􀀺􀀳􀂶􀁖􀀌􀀏􀀃􀁄􀁑􀁇􀀃􀁆􀁄􀁑􀀃􀁅􀁈􀀃􀁗􀁕􀁄􀁑􀁖􀁓􀁒􀁕􀁗􀁈􀁇􀀃 5
􀁐􀁒􀁕􀁈􀀃 􀁈􀁆􀁒􀁑􀁒􀁐􀁌􀁆􀁄􀁏􀁏􀁜􀀃 􀁗􀁋􀁄􀁑􀀃 􀁖􀁘􀁖􀁓􀁈􀁑􀁖􀁌􀁒􀁑􀀃 􀁆􀁒􀁑􀁆􀁈􀁑􀁗􀁕􀁄􀁗􀁈􀁖􀀃 􀀋􀀶􀀦􀂶􀁖􀀌􀀑􀀃 􀀤􀁏􀁖􀁒􀀏􀀃 the packaging
􀁐􀁄􀁗􀁈􀁕􀁌􀁄􀁏􀀃􀁘􀁖􀁈􀁇􀀃􀁉􀁒􀁕􀀃􀀺􀀧􀀪􀂶􀁖􀀃􀁌􀁖􀀃􀁅􀁌􀁒􀁇􀁈􀁊􀁕􀁄􀁇􀁄􀁅􀁏􀁈, 􀁚􀁋􀁌􀁏􀁖􀁗􀀃􀁌􀁗􀀃􀁌􀁖􀀃􀁑􀁒􀁗􀀃􀁗􀁋􀁈􀀃􀁆􀁄􀁖􀁈􀀃􀁚􀁌􀁗􀁋􀀃􀀺􀀳􀂶􀁖􀀃􀁄􀁑􀁇􀀃
􀀶􀀦􀂶􀁖􀀑􀀃
10 When agrochemicals have a relatively similar water solubility profile and
preparation; storage and shipping in a commercially acceptable form can be
relatively easier. However, many agrochemicals having diverse solubility profiles
are required to be combined in a single composition based on the desired biological
effect. Such agrochemicals when combined together to form WDG, disintegration
15 of such WDG becomes the major concern which is to be addressed.
Further, physico-chemical stability of agrochemical compositions is the biggest
concern while formulating. Selecting suitable surfactants is critical to achieve a
physically and chemically stable formulation with appropriate shelf life. Therefore,
20 it is highly desirable to develop a formulation which is stable over long periods of
time, does not deteriorate under severe storage conditions, being less phytotoxic
to plants and are environmentally friendlier than conventional formulations.
Disintegration is frequently a prerequisite for the efficient dispersion of WDGs in
25 water and also an important index for evaluating the performance of WDGs. It is
known that the WDGs with weak bonding proved to facilitate rapid disintegration
and dispersion. Also, another factor influencing disintegration is the porosity and
the package rate of the surfactant on the pesticide particles surface.
30 There is still no comprehensive and systematic theory for the WDG disintegration
mechanism, and researchers mainly depend on their experience to improve the
disintegration property, which restricts the development of a high-performance
WDG pesticide. Water wetting the surface and diffusing to the inner space of
4
WDGs have been identified as steps necessary in any disintegration process, so
an appropriate porosity is essential for WDGs to achieve sufficient disintegration.
Thus, there is a need for a new and improved WDG formulation which is stable
and useful as pest control agents which provides 5 knock-down activity with
prolonged control, that is, fast action with long lasting action. The present invention
addresses this problem and other needs existing in the art.
Summary of the invention
10 In one aspect the present invention provides an insecticidal composition
comprising:
i) at least one agrochemical active ingredient selected from a hydrophilic
agrochemical active ingredient, a hydrophobic agrochemical active ingredient
and combinations thereof;
15 ii) a surfactant combination comprising a copolymer and an organosulfate;
wherein the composition does not comprise an inorganic salt.
In one aspect the present invention provides an insecticidal composition
comprising:
20 i) at least one agrochemical active ingredient selected from a hydrophilic
insecticidal compound, a hydrophobic insecticidal compound and
combinations thereof;
ii) a surfactant combination comprising a copolymer and an organosulfate;
wherein the composition does not comprise an inorganic salt.
25
In another aspect the present invention provides an insecticidal composition
comprising:
i) at least one hydrophilic agrochemical active ingredient selected from the
pyridine organic class of compounds;
30 ii) at least one hydrophobic agrochemical active ingredient selected from phenyl
pyrazole, diamide, triazine, pyrethroids, oxadiazine and thiourea class of
compounds;
iii) a surfactant combination comprising a copolymer and alkyl sulphate or salts
thereof;
5
wherein the composition does not comprise an inorganic salt.
In another aspect the present invention provides a water dispersible granular
composition comprising:
i) at least one hydrophilic agrochemical active 5 ingredient selected from the
pyridine organic class of compounds;
ii) at least one hydrophobic agrochemical active ingredient selected from phenyl
pyrazole, diamide, triazine, pyrethroids, oxadiazine and thiourea class of
compounds;
10 iii) a surfactant combination comprising a copolymer and alkyl sulphate or salts
thereof;
wherein the composition does not comprise an inorganic salt.
In one aspect the present invention provides a water dispersible granule
15 composition comprising:
i) pymetrozine;
ii) fipronil; and
iii) a surfactant combination comprising alkyl sulphate or salts thereof and a
copolymer;
20 wherein the composition does not contain an inorganic salt.
In another aspect the present invention provides a process for preparation of an
insecticidal composition comprising at least one agrochemical active ingredient
selected from a hydrophilic agrochemical active ingredient, a hydrophobic
25 agrochemical active ingredient and combinations thereof, wherein the composition
does not comprise an inorganic salt.
In another aspect the present invention provides use of an insecticidal composition
for controlling insects, the composition comprising at least one agrochemical active
30 ingredient selected from a hydrophilic agrochemical active ingredient, a
hydrophobic agrochemical active ingredient and combinations thereof, wherein the
composition does not comprise an inorganic salt.
6
In another aspect the present invention provides a method of controlling pests by
applying an effective amount of water dispersible granular composition to pests or
to their locus, the composition comprising at least one agrochemical active
ingredient selected from a hydrophilic agrochemical active ingredient, a
hydrophobic agrochemical active ingredient and combinations 5 thereof, wherein the
composition does not comprise an inorganic salt.
In another aspect the present disclosure provides a method of increasing the yield
of the crop comprising applying the present insecticidal composition to a crop, or
10 to plant propagation material or to the surface of agricultural produce.
In another aspect, the present disclosure provides a kit comprising a plurality of
components, each of which components may include at least one, or more, of the
ingredients of the insecticidal combination/composition of the present disclosure.
15
Additional features and advantages of the present invention will be apparent from
the detailed description that follows, which illustrates by way of example, the most
preferred features of the present invention which are not to be construed as limiting
the scope of the invention described herein.
20
Detailed description of the invention
The following description is provided to assist in a comprehensive understanding
of exemplary embodiments of the invention. It includes various specific details to
assist in that understanding but these are to be regarded as merely exemplary.
25 Accordingly, those of ordinary skill in the art will recognize that various changes
and modifications of the embodiments described herein can be made without
departing from the scope of the invention. In addition, descriptions of well-known
functions and constructions are omitted for clarity and conciseness.
30 The terms and words used in the following description and claims are not limited
to the bibliographical meanings but are merely used by the inventor to enable a
clear and consistent understanding of the invention. Accordingly, it should be
apparent to those skilled in the art that the following description of exemplary
7
embodiments of the present invention are provided for illustration purpose only and
not for limiting the scope of the invention.
􀀬􀁗􀀃 􀁌􀁖􀀃 􀁗􀁒􀀃 􀁅􀁈􀀃 􀁘􀁑􀁇􀁈􀁕􀁖􀁗􀁒􀁒􀁇􀀃 􀁗􀁋􀁄􀁗􀀃 􀁗􀁋􀁈􀀃 􀁖􀁌􀁑􀁊􀁘􀁏􀁄􀁕􀀃 􀁉􀁒􀁕􀁐􀁖􀀃 􀂳􀁄􀀏􀂴􀀃 􀂳􀁄􀁑􀀏􀂴􀀃 􀁄􀁑􀁇􀀃 􀂳􀁗􀁋􀁈􀂴􀀃 􀁌􀁑􀁆􀁏􀁘􀁇􀁈􀀃 􀁓􀁏􀁘􀁕􀁄􀁏􀀃
referents unless the context 5 clearly dictates otherwise.
Features that are described and/or illustrated with respect to one embodiment may
be used in the same way or in a similar way in one or more other embodiments
and/or in combination with or instead of the features of the other embodiments. As
10 used herein, the terms "comprises," "comprising," "includes," "including," "has,"
"having," "contains", "containing," "characterized by" or any other variation thereof,
are intended to cover a non-exclusive inclusion, subject to any limitation explicitly
indicated.
15 Recitation of ranges of values are merely intended to serve as a shorthand method
of referring individually to each separate value falling within the range, unless
otherwise indicated herein, and each separate value is incorporated into the
specification as if it were individually recited herein. The endpoints of all ranges
are included within the range and independently combinable. It is understood that
20 where a parameter range is provided, all integers within that range, and tenths
􀁗􀁋􀁈􀁕􀁈􀁒􀁉􀀏􀀃􀁄􀁕􀁈􀀃􀁄􀁏􀁖􀁒􀀃􀁓􀁕􀁒􀁙􀁌􀁇􀁈􀁇􀀑􀀃􀀩􀁒􀁕􀀃􀁈􀁛􀁄􀁐􀁓􀁏􀁈􀀏􀀃􀂳􀀓􀀑􀀔-􀀛􀀓􀀈􀂴􀀃􀁌􀁑􀁆􀁏􀁘􀁇􀁈􀁖􀀃􀀓􀀑􀀔􀀈􀀏􀀃􀀓􀀑􀀕􀀈􀀏􀀃􀀓􀀑􀀖􀀈􀀏􀀃􀁈􀁗􀁆􀀑􀀃
􀁘􀁓􀀃􀁗􀁒􀀃􀀛􀀓􀀈􀀑􀀃􀀷􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀂳􀀈􀀃􀁅􀁜􀀃􀁚􀁈􀁌􀁊􀁋􀁗􀂴􀀃􀀋􀁓􀁈􀁕􀁆􀁈􀁑􀁗􀀃􀁅􀁜􀀃􀁚􀁈􀁌􀁊􀁋􀁗􀀌􀀃􀁒􀁕􀀃􀀈􀀃􀁚􀀒􀁚􀀃􀁄􀁖􀀃􀁘􀁖􀁈􀁇􀀃􀁋􀁈􀁕􀁈􀁌􀁑􀀏􀀃
unless otherwise defined, relates to the relative weight of the respective
component based on the total weight of the composition.
25
􀂳􀀤􀁅􀁒􀁘􀁗􀂴􀀃 􀁒􀁕􀀃 􀂳􀁄􀁓􀁓􀁕􀁒􀁛􀁌􀁐􀁄􀁗􀁈􀁏􀁜􀂴􀀃 􀁄􀁖􀀃 􀁘􀁖􀁈􀁇􀀃 􀁋􀁈􀁕􀁈􀁌􀁑􀀃 􀁌􀁖􀀃 􀁌􀁑􀁆􀁏􀁘􀁖􀁌􀁙􀁈􀀃 􀁒􀁉􀀃 􀁗􀁋􀁈􀀃 􀁖􀁗􀁄􀁗􀁈􀁇􀀃 􀁙􀁄􀁏􀁘􀁈􀀃 􀁄􀁑􀁇􀀃
means within an acceptable range of deviation for the particular value as
determined by one of ordinary skill in the art, considering the measurement in
question and the error associated with measurement of the particular quantity (i.e.,
30 􀁗􀁋􀁈􀀃􀁏􀁌􀁐􀁌􀁗􀁄􀁗􀁌􀁒􀁑􀁖􀀃􀁒􀁉􀀃􀁗􀁋􀁈􀀃􀁐􀁈􀁄􀁖􀁘􀁕􀁈􀁐􀁈􀁑􀁗􀀃􀁖􀁜􀁖􀁗􀁈􀁐􀀌􀀑􀀃􀀃􀀩􀁒􀁕􀀃􀁈􀁛􀁄􀁐􀁓􀁏􀁈􀀏􀀃􀂳􀁄􀁅􀁒􀁘􀁗􀂴􀀃􀁆􀁄􀁑􀀃􀁐􀁈􀁄􀁑􀀃􀁚􀁌􀁗􀁋􀁌􀁑􀀃
one or more standard deviations, or within ± 10% or ± 5% of the stated value.
8
􀀤􀁖􀀃􀁘􀁖􀁈􀁇􀀃􀁋􀁈􀁕􀁈􀁌􀁑􀀃􀁗􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀀅􀁓􀁏􀁄􀁑􀁗􀀅􀀃􀁒􀁕􀀃􀂳􀁆􀁕􀁒􀁓􀂴􀀃􀁕􀁈􀁉􀁈􀁕􀁖􀀃􀁗􀁒􀀃􀁚􀁋􀁒􀁏􀁈􀀃􀁓􀁏􀁄􀁑􀁗􀁖􀀏􀀃􀁓􀁏􀁄􀁑􀁗􀀃􀁒􀁕􀁊􀁄􀁑􀁖􀀃􀀋􀁈􀀑􀁊􀀑􀀏􀀃
leaves, stems, twigs, roots, trunks, limbs, shoots, fruits etc.), plant cells, and plant
seeds. This term also encompasses plant crops such as fruits.
􀀷􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀂳􀁏􀁒􀁆􀁘􀁖􀂴􀀃􀁄􀁖􀀃􀁘􀁖􀁈􀁇􀀃􀁋􀁈􀁕􀁈􀁌􀁑􀀃􀁇􀁈􀁑􀁒􀁗􀁈􀁖􀀃􀁗􀁋􀁈􀀃􀁙􀁌􀁆􀁌􀁑􀁌􀁗􀁜􀀃􀁒􀁕􀀃􀁄􀁕􀁈􀁄􀀃􀁇􀁈􀁖􀁌􀁊􀁑􀁄􀁗􀁈􀁇􀀃􀁉􀁒􀁕􀀃􀁊􀁕􀁒􀁚􀁗􀁋􀀃 5
of a desired crop susceptible to or likely to be susceptible to infestation by insects,
and in which control of the insect is desired. The locus includes the vicinity of
desired crop plants wherein insect infestation has either occurred or is most likely
to occur or is yet to occur.
10
􀀷􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀂳􀁌􀁑􀁖􀁈􀁆􀁗􀁌􀁆􀁌􀁇􀁄􀁏􀁏􀁜􀀃􀁈􀁉􀁉􀁈􀁆􀁗􀁌􀁙􀁈􀀃􀁄􀁐􀁒􀁘􀁑􀁗􀂴􀀃􀁐􀁈􀁄􀁑􀁖􀀃􀁗􀁋􀁈􀀃􀁄􀁐􀁒􀁘􀁑􀁗􀀃􀁒􀁉􀀃􀁗􀁋􀁈􀀃􀁆􀁒􀁐􀁓􀁒􀁖􀁌􀁗􀁌􀁒􀁑􀀃
needed to achieve an observable adverse effect on growth, including the effects of
necrosis, death, retardation, prevention, and removal, destruction, insect pest
mortality, insect pest weight loss, insect pest reduced plant defoliation, and other
15 behavioural and physical changes of an insect pest after feeding and exposure for
an appropriate length of time.
The term "agriculturally acceptable amount of active" refers to an amount of an
active that kills or inhibits the pest on which control is desired, in an amount not
20 significantly toxic to the plant being treated.
􀀷􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀀅􀁌􀁑􀁖􀁈􀁆􀁗􀁖􀀅􀀃􀁌􀁑􀁆􀁏􀁘􀁇􀁈􀁖􀀃􀁄􀁏􀁏􀀃􀁒􀁕􀁊􀁄􀁑􀁌􀁖􀁐􀁖􀀃􀁌􀁑􀀃􀁗􀁋􀁈􀀃􀁆􀁏􀁄􀁖􀁖􀀃􀀅􀀬􀁑􀁖􀁈􀁆􀁗􀁄􀂴􀀑􀀃􀀬􀁑􀁖􀁈􀁆􀁗􀁌􀁆􀁌􀁇􀁄􀁏􀀃􀁕􀁈􀁉􀁈􀁕􀁖􀀃
to the ability of a substance to increase mortality and/or inhibit the growth rate of
insects.
25
The term "control" or "controlling" insects refers to inhibition of insects, through a
toxic effect, the ability of insect pests to survive, grow, feed, and/or reproduce, or
to limit insect-related damage or loss in crop plants. To "control" insects may or
may not mean killing the insects, although it preferably means reducing insect
30 population by killing the insects.
􀀷􀁋􀁈􀀃􀁗􀁈􀁕􀁐􀀃􀂵􀁖􀁗􀁄􀁅􀁏􀁈􀂶􀀃􀁕􀁈􀁉􀁈􀁕􀁕􀁈􀁇􀀃􀁗􀁒􀀃􀁋􀁈􀁕􀁈􀁌􀁑􀀃􀁕􀁈􀁉􀁈􀁕􀁖􀀃􀁗􀁒􀀃􀁆􀁋􀁈􀁐􀁌􀁆􀁄􀁏􀀃􀁄􀁑􀁇􀀒􀁒􀁕􀀃􀁓􀁋􀁜􀁖􀁌􀁆􀁄􀁏􀀃􀁖􀁗􀁄􀁅􀁌􀁏􀁌􀁝􀁄􀁗􀁌􀁒􀁑􀀃
of the active ingredients in the composition and desired suspensibility and
9
dispersibility of the composition by maintaining homogeneity of the components
that impart longer shelf life.
The term AHS refer to Accelerated heat stability (AHS), wherein experimental
studies are carried out to determine the stability 5 of the composition after 14 days
of preparing the said composition at a temperature of 54°C.
The physicochemical studies of the compositions/formulation is performed
according to the CIPAC standard method.
10
The present disclosure provides an insecticidal composition, particularly the
composition comprising a combination of insecticides and their use for controlling
the targeted insects. The disclosure also relates to a method for preparing the
composition that is stable at varied storage conditions as well as a method for
15 controlling insect pests using the present insecticidal compositions comprising the
same.
The present insecticidal combinations and compositions are useful for protecting
plants and plant parts, for controlling insect infestation, for increasing harvest
20 yields, and/or for improving the quality of the harvested material.
Accordingly, the present invention provides an insecticidal composition comprising
a pesticidally effective amount of an active ingredient with specific surfactant
combinations to prevent degradation of active compounds. The present
25 composition is formulated as water dispersible granular formulation. Surprisingly,
the present inventors found that the surfactant combination present in the
composition comprising sodium alkyl sulphate and a copolymer provide an
improved disintegration profile of water dispersible granules prepared according to
the present invention. The present composition is free of inorganic salt. It is
30 observed that selection of the specific surfactant combination intensely, without the
presence of an inorganic salt enhances the disintegration profile of compositions.
In the present composition the active ingredients remain fully dispersed, such that
the formulation thereafter maintains a stable dispersion that is suitable for spraying.
Additionally, the present formulation has good wetting capacity.
10
In an embodiment, the present invention provides an insecticidal composition
comprising:
a) at least one agrochemical active ingredient selected from a hydrophilic
agrochemical active ingredient, a hydrophobic 5 agrochemical active ingredient and
combinations thereof; and
b) a surfactant combination comprising a copolymer and an organosulfate;
wherein the composition does not comprise an inorganic salt.
10 In an embodiment, the present invention provides an insecticidal composition
comprising:
a) at least one agrochemical active ingredient selected from a hydrophilic
insecticidal compound, a hydrophobic insecticidal compound and combinations
thereof; and
15 b) a surfactant combination comprising a copolymer and an organosulfate;
wherein the composition does not comprise an inorganic salt.
In an embodiment, the agrochemical active ingredient is selected from hydrophilic
agrochemical active ingredients.
20
In an embodiment the hydrophilic agrochemical active ingredient is selected from
the group comprising pyridine organic compounds, neonicotinoids,
dithiocarbamates, phthalimides, or triazines, their derivatives and salts thereof.
25 In an embodiment, the hydrophilic agrochemical active ingredient include but not
limited to, flonicamid, acephate, pymetrozine, emamectin-benzoate acetamiprid,
imidacloprid, thiamethoxam, spinosad and salts thereof.
In a preferred embodiment of the present invention, the hydrophilic agrochemical
30 active ingredient is selected from flonicamid, pymetrozine or acephate.
According to an embodiment of the present invention, hydrophilic agrochemical
active ingredient is pymetrozine.
11
In an embodiment, the present composition comprises from about 0.1% w/w to
about 90% w/w hydrophilic agrochemical active ingredient of the total weight of the
composition.
In an embodiment, the present composition comprises from 5 about 1% w/w to about
80% w/w hydrophilic agrochemical active ingredient of the total weight of the
composition.
In an embodiment, the present composition comprises from about 5% w/w to about
10 80% w/w hydrophilic agrochemical active ingredient of the total weight of the
composition.
In an embodiment, of the present invention, the present composition comprises
from about 5% w/w to about 50% w/w hydrophilic agrochemical active ingredient
15 of the total weight of the composition.
In an embodiment, the present composition comprises pymetrozine in a
concentration from about 0.1% w/w to about 90% w/ of the total weight of the
composition.
20
In an embodiment, the present composition comprises pymetrozine in a
concentration from about 1% w/w to about 80% w/w of the total weight of the
composition.
25 In an embodiment, the present composition comprises pymetrozine in a
concentration from about 5% w/w to about 80% w/w of the total weight of the
composition.
In an embodiment, the present composition comprises pymetrozine in a
30 concentration from about 5% w/w to about 50% w/w of the total weight of the
composition.
According to an embodiment of the present invention, said insecticidal
compositions comprise a hydrophobic agrochemical active ingredient.
12
In an embodiment the hydrophobic agrochemical active ingredient is selected from
phenyl pyrazole compound, diamide, triazinone, pyrethroids, oxadiazine, or
thiourea, their derivatives and salts thereof.
5
In an embodiment, the hydrophobic agrochemical active ingredient is selected from
the group comprising fipronil, flubendiamide, clodinafop, metribuzin,
diafenthiauron, indoxacarb, bifenthrin, fluazuron, atrazine, deltamethrin,
rimsulfuron, fomesafen, acifluorfen, azaconazole, azoxystrobin, benalaxyl,
10 benodanil, benzamacril, benzamacryl-isobutyl, bialaphos, binapacryl, biphenyl,
bitertanol, blasticidin-S, bromuconazole, bupirimate, buthiobat, calcium
polysulphide, capsimycin, carbendazim, carboxin, carvone, chinomethionat
(quinomethionat), chlobenthiazone, chlorfenazole, chlorothalonil, chlozolinate,
clozylacon, cufraneb, cymoxanil, cyproconazole, cyprodinil,
15 cyprofuram, debacarb, dichlorophen, diclobutrazol, diclofluanid, diclomezine,
dicloran, diethofencarb, difenoconazole, diafenthiuron, dimethirimol, dithianon,
dodemorph, drazoxolon, ediphenphos, epoxiconazole, etaconazole, ethirimol,
etridiazole, famoxadone, fenapanil, fenarimol, fenbuconazole, fenfuram,
fenitropan, fenpiclonil, fenpropidin, fenpropimorph, fluquinconazole, flurprimidol,
20 flusilazole, flusulphamide, flutolanil, imibenconazole, iminoctadine,
iminoctadinealbesilate, iminoctadine, iprodione, irumamycin, isoprothiolane,
isovaledione, kasugamycin, kresoxim-methyl, meferimzone, mepanipyrim,
mepronil, metalaxyl, metconazole, methasulphocarb, methfuroxam, myclobutanil,
penconazole, pencycuron, phosdiphen, pimaricin, piperalin, polyoxin, polyoxorim,
25 probenazole, prochloraz, procymidone, propamocarb, propanosine-sodium,
propiconazole, propineb, pyrazophos, pyrifenox, pyrimethanil, pyroquilon,
pyroxyfur, and tebuconazole, tecloftalam, tecnazene, tetcyclacis, tetraconazole,
thiabendazole, , thifluzamide, thiophanate-methyl, tricyclazole, tridemorph,
triflumizole, triforine, triticonazole, avermectin lorfenapyr fenazaquin,
30 fenpyroximate, pyrimidifen, pyridaben, tebufenpyrad, tolfenpyrad Diafenthiuron
spirodiclofen, spiromesifen amidoflumet, benclothiaz, benzoximate, bifenazate,
bromopropylate, buprofezin, chinomethionat, chlordimeform, chlorobenzilate,
chloropicrin, clothiazoben, cycloprene, dicyclanil, fenoxacrim, fentrifanil,
flubenzimine, flufenerim, flutenzin, gossyplure, hydramethylnone, japonilure,
13
metoxadiazone, petroleum, piperonyl butoxide, potassium oleate, pyridalyl,
sulphluramid, tetradifon, tetrasul, triarathene, chlorantraniliprole, chlorfenapyr,
clothianidin, cyantraniliprole, diafenthiuron, emamectin benzoate, ethiprole,
flupyradifurone, imidacloprid, indoxacarb, lambda cyhalothrin, lufenuron,
methoxyfenozide, pymetrozine, pyrethrum, 5 bistrifluoron, chlofluazuron,
diflubenzuron, fluazuron, flucycloxuron, flufenoxuron, hexaflumuron, lufenuron,
novaluron, noviflumuron, penfluoron, teflubenzuronchromafenozide, halofenozide,
methoxyfenozide or tebufenozide.
10 In an embodiment the hydrophobic agrochemical active ingredient is selected from
fipronil, flubendiamide, indoxacarb, diafenthiuron and bifenthrin.
In an embodiment the hydrophobic agrochemical active ingredient is fipronil.
15 In an embodiment, the present insecticidal composition comprises from about
0.1% w/w to about 90% w/w hydrophobic agrochemical active ingredient of the
total weight of the composition.
In an embodiment, the present composition comprises from about 1% w/w to about
20 80% w/w hydrophobic agrochemical active ingredient of the total weight of the
composition.
In an embodiment, the present composition comprises from about 5% w/w to about
50% w/w hydrophobic agrochemical active ingredient of the total weight of the
25 composition.
In an embodiment, the present composition comprises fipronil in a concentration
from about 0.1% w/w to about 90% w/w of the total weight of the composition.
30 In an embodiment, the present composition comprises fipronil in a concentration
from about 1% w/w to about 80% w/w of the total weight of the composition.
In an embodiment, the present composition comprises fipronil in a concentration
from about 5% w/w to about 50% w/w of the total weight of the composition.
14
In an embodiment, the present composition comprises fipronil in a concentration
from about 5% w/w to about 25% w/w of the total weight of the composition.
In an embodiment of the present invention, said organosulfate is selected from
sodium dodecyl sulfate and potassium 5 or ammonium salts thereof.
In an embodiment, the organosulfate comprises sodium alkyl sulphate.
In an embodiment, the present composition comprises an organosulfate from
10 about 0.1% w/w to about 50% w/w of the total weight of the composition.
In an embodiment, the present composition comprises an organosulfate in a
concentration from about 1% w/w to about 30% w/w of the total weight of the
composition.
15
In an embodiment, the present composition comprises an organosulfate in a
concentration from about 0.5% w/w to about 20% w/w of the total weight of the
composition.
20 In an embodiment, the present composition comprises sodium alkyl sulphate from
about 0.1% w/w to about 50% w/w of the total weight of the composition.
In an embodiment, the present composition comprises sodium alkyl sulphate in a
concentration from about 1% w/w to about 30% w/w of the total weight of the
25 composition.
In an embodiment, the present composition comprises sodium alkyl sulphate in a
concentration from about 0.5% w/w to about 20% w/w of the total weight of the
composition.
30
In an embodiment of the present invention, the copolymer is selected from the
group comprising urea formaldehyde resin, polyurea, polyvinyl chloride,
polyurethanes, polyamide, polyvinyl pyrrolidine, acrylic polymers, polyisocyanate15
cyclic alkylene, polyamine, polyimine, polycarboxylic acids, naturally occurring
polymers, their derivatives and salts thereof.
In an embodiment, the copolymer is urea formaldehyde resin.
5
In an embodiment, the present composition comprises a copolymer from about
0.1% w/w to about 50% w/w of the total weight of the composition.
In an embodiment, the present composition comprises a copolymer from about 1%
10 w/w to about 30% w/w of the total weight of the composition.
In an embodiment, the present composition comprises a copolymer from about
0.5% w/w to about 20% w/w of the total weight of the composition.
15 In an embodiment a copolymer and an organosulfate are present in the
composition in a ratio of 1: 1.66.
In an embodiment, the surfactant combination comprising copolymer and an
organosulfate present in a ratio of about 1:1 or about 1:1.5 or about 1: 2 or about
1:2.5 or about 1:3 or about 1: 3.5 or about 1:4.
20
In preferred embodiment, the surfactant combination comprises a copolymer and
sodium alkyl sulphate present in a ratio 1: 1.5.
In another preferred embodiment, the surfactant combination comprises a
25 copolymer and sodium alkyl sulphate present in a ratio1:2.
In an embodiment, the present insecticide compositions further comprise one or
more dispersants or surfactants, fillers, binding agent, pH-regulating agents,
preservatives, biocides, antifoaming agents, colorants and other formulation aids.
30
The examples of dispersing agents or suspending agent or surfactants include
ionic and nonionic dispersants to enable disintegration of granules in water with
ease, such as salts of polystyrene sulphonic acids, salts of polyvinylsulphonic
acids, salts of naphthalenesulphonic acid/formaldehyde condensates, salts of
16
condensates of naphthalenesulphonic acid, phenolsulphonic acid and
formaldehyde, and salts of lignosulphonic acid, and lignosulphonate, such as
sodium lignosulphonate and modified sodium lignosulfonate; polyethylene
oxide/polypropylene oxide block copolymers, polyethylene glycol ethers of linear
alcohols, reaction products of fatty acids with 5 ethylene oxide and/or propylene
oxide, furthermore polyvinyl alcohol, polyvinylpyrrolidone, copolymers of polyvinyl
alcohol and polyvinylpyrrolidone and copolymers of (meth)acrylic acid and
(meth)acrylic esters, Polycarboxylate & their salts, furthermore alkyl ethoxylates
and alkylarylethoxylates ethoxylated alkylarylphosphated or mixtures.
10
The examples of wetting agents or surfactants include ionic and nonionic wetter to
enable wetting of granules in water with ease e.g. frequently used dispersants are
alkylnaphtalene sulphonates, for instance sodium diisopropylnaphthalene
sulphonate and sodium alkylnaphthalene sulphonate, sulfosuccinate & their salts,
15 alkylaryl ethoxylates, alkyl sulphates & salts thereof, sodium lauryl sulfate or
combination thereof.
The binding agent may include any or a combination of polyvinyl alcohols, phenyl
naphthalene sulphonate, lignin derivatives, polyvinyl pyrrolidone,
20 polyalkylpyrrolidone, carboxymethylcellulose, xanthan gum, polyethoxylated fatty
acids, polyethoxylated fatty alcohols, ethylene oxide copolymer, propylene oxide
copolymer, polyethylene glycols and polyethylene oxides, but not limited thereto.
In an embodiment the filler is selected from insoluble fillers and soluble fillers. In
25 an embodiment, the preferred fillers are selected from silica, precipitated silica and
kaolin.
In an embodiment, suitable antifoam is selected from silicones, polysiloxane,
aqueous emulsion of polysiloxane, polydimethoxysiloxane, polydimethylsiloxane,
30 long-chain alcohols and salts of fatty acids.
In an embodiment, suitable colorants (for example in red, blue and green) are,
preferably, pigments, which are sparingly soluble in water, and dyes, which are
water-soluble. Examples are inorganic coloring agents (for example iron oxide,
17
titanium oxide, and iron hexacyanoferrate) and organic coloring agents (for
example alizarin, azo and phthalocyanin coloring agents).
In an embodiment, suitable biocides include benzothiazoles, 1,2-benzisothiazolin-
3-one, sodium dichloro-s-triazinetrione, sodium 5 benzoate, potassium sorbate, 1,2-
phenyl-isothiazolin-3-one, or inter chloroxylenol paraoxybenzoate butyl.
In an embodiment, the present composition is formulated as a solid composition
including, but not limited to, dust, powder, granules, pellets, tablets, dry flowable,
10 wettable powder or water dispersible granules (WDG).
In an embodiment, the present composition is formulated as water dispersible
granules (WDG).
15 Accordingly, the present invention provides a water dispersible granular
composition comprising:
a) at least one agrochemical active ingredient selected from a hydrophilic
agrochemical active ingredient, a hydrophobic agrochemical active ingredient and
combinations thereof; and
20 b) a surfactant combination comprising organosulfate and a copolymer;
wherein the composition does not comprise an inorganic salt.
According to an embodiment of the present invention, the water dispersible
granular composition comprises fipronil and a surfactant combination of a
25 copolymer and sodium alkyl sulphate in a ratio from about 1:1 to about 1:4.
In an embodiment of the present invention, the water dispersible granular
composition comprises pymetrozine and a surfactant combination of a copolymer
and sodium alkyl sulphate in a ratio from about 1:1 to about 1:4.
30
In an embodiment of the present invention, the water dispersible granular
composition comprises fipronil, pymetrozine and a surfactant combination of a
copolymer and sodium alkyl sulphate in a ratio from about 1:1 to about 1:4.
18
In another preferred embodiment, the present invention provides a water
dispersible granular formulation comprising:
i) pymetrozine;
ii) fipronil; and
iii) a surfactant combination of a copolymer and 5 sodium alkyl sulphate in a ratio
from about 1:1 to about 1:4;
wherein the composition does not comprise an inorganic salt.
In another preferred embodiment, the present invention provides a water
10 dispersible granular formulation comprising:
i) 5% w/w to about 80% w/w of pymetrozine;
ii) 5% w/w to about 50% w/w of fipronil; and
iii) a surfactant combination of a copolymer and sodium alkyl sulphate in a ratio
from about 1:1 to about 1:4;
15 wherein the composition does not comprise an inorganic salt.
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 10% w/w to about 90% w/w fipronil, from about 0.1% w/w
to about 20% w/w sodium alkyl sulphate and from about 0.1% w/w to 20% w/w
20 urea-formaldehyde copolymer of the total weight of the composition.
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 10% w/w to about 90% w/w pymetrozine, from about 0.1%
w/w to about 20% w/w sodium alkyl sulphate and from about 0.1% w/w to 20% w/w
25 urea-formaldehyde copolymer of the total weight of the composition.
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 5% w/w to about 50% w/w fipronil, from about 10% w/w to
about 90% w/w pymetrozine, from about 0.1% w/w to about 20% w/w sodium alkyl
30 sulphate and from about 0.1% w/w to 20% w/w urea-formaldehyde copolymer of
the total weight of the composition.
In an embodiment, the present invention provides a stable insecticidalcomposition
comprising from about 5% w/w to about 50% w/w fipronil, from about 10% w/w to
19
about 90% w/w pymetrozine, from about 0.1% w/w to about 20% w/w sodium alkyl
sulphate and from about 0.1% w/w to 20% w/w urea-formaldehyde copolymer of
the total weight of the composition, wherein the composition does not contain
inorganic salt.
5
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 5% w/w to about 50% w/w fipronil, from about 10% w/w to
about 90% w/w pymetrozine, surfactant combination of sodium alkyl sulphate and
urea-formaldehyde copolymer present in a ratio 1:1 to 1:4 wherein the composition
10 does not contain inorganic salt.
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 5% w/w to about 25% w/w fipronil, from about 10% w/w to
about 50% w/w pymetrozine, surfactant combination of sodium alkyl sulphate and
15 urea-formaldehyde copolymer present in a ratio 1:1 to 1:4 wherein the composition
does not contain inorganic salt.
In an embodiment, the present invention provides a stable insecticidal composition
comprising from about 5% w/w to about 10% w/w fipronil, from about 20% w/w to
20 about 40% w/w pymetrozine, surfactant combination of sodium alkyl sulphate and
urea-formaldehyde copolymer present in a ratio 1:1 to 1:4 wherein the composition
does not contain inorganic salt.
In an embodiment, the present invention provides a stable insecticidal composition
25 comprising from about 5% w/w to about 10% w/w fipronil, from about 20% w/w to
about 40% w/w pymetrozine, surfactant combination of sodium alkyl sulphate and
urea-formaldehyde copolymer present in a ratio 1:1 to 1:4 wherein the composition
does not contain inorganic salt.
30 In another embodiment the present composition further comprising an additional
insecticide.
In an embodiment additional insecticide is selected from group of
Acetylcholinesterase (AChE) inhibitors, GABA -gated chloride channel blockers,
20
Sodium channel modulators, Nicotinic acetylcholine receptor (nAChR) competitive
modulators, Nicotinic acetylcholine receptor (nAChR) allosteric modulators,
Glutamate -gated chloride channel (GluCl) allosteric modulators, Juvenile hormone
mimics, Chordotonal organ TRPV channel modulators, Mite growth inhibitors,
Microbial disruptors of insect midgut membranes, Inhibitors 5 of mitochondrial ATP
synthase, Uncouplers of oxidative phosphorylation via disruption of the proton
gradient, Nicotinic acetylcholine receptor (nAChR) channel blockers, Inhibitors of
chitin biosynthesis , Moulting disruptors, Ecdysone receptor agonists, Octopamine
receptor agonists, Mitochondrial complex electron transport inhibitors, Voltage10
dependent sodium channel blockers, Inhibitors of acetyl CoA carboxylase,
Chordotonal organ Modulators, multi-site miscellaneous insecticides,
bioinsecticides and mixtures thereof.
According to an embodiment of the present invention, a process for preparation of
15 insecticide composition comprising:
i) mixing at least one agrochemical active ingredient, surfactants and
blending the mixture to obtain a blend;
ii) grinding the blend to obtain ground mix of desired particle size;
iii) blending said ground mix to obtain homogeneous mixture;
20 iv) preparing dough from the homogeneous mixture and perform granulation
to obtain granules.
According to an embodiment the present invention provides a process for the
preparation of a water dispersible granular formulation comprising fipronil and
25 pymetrozine.
In an embodiment, the process for preparation of water dispersible granular
formulation comprising the steps of:
i) blending fipronil, pymetrozine, sodium alkyl sulphate, urea-formaldehyde
30 copolymer and other auxiliary ingredients to obtain a blend; ;
ii) grinding said blend to obtain ground mix of desired particle size;
iii) blending said ground mix to obtain homogeneous mixture;
iv) preparing dough from said homogeneous mixture by adding water and
extrude the granules;
21
v) drying the extruded granules.
In an embodiment, the order of addition and mixing of the granule ingredients is
not narrowly critical. In one embodiment, for example, the dry ingredients are
blended, grinded and the composition is then 5 mixed while water is added.
According to an embodiment of the present invention, water is used as carrier, a
fine water spray to prepare dough from the composition to obtain granules.
10 According to an embodiment of the present invention, one or more formulation
auxiliaries are added in water to prepare aqueous solution and said aqueous
solution is added to prepare dough from the composition to obtain granules.
According to an embodiment of the present invention, the blend of above
15 ingredients is obtained using a suitable blender such as ribbon blender, V-blender,
high intensity plough mixer or the like.
According to an embodiment of the present invention, the grinding may be
performed in a suitable device known to a skilled person in the relevant art such
20 as air jet mill, air classifier mill, hammer mill, pin disc mill or the like. Jet mills are
shear or pulverizing machines in which the particles to be milled are accelerated
by gas flows and pulverized by collision. There are a number of different types of
jet mill designs, such as double counterflow (opposing jet) and spiral (pancake)
fluid energy mills.
25
According to an embodiment of the present invention, water dispersible granules
are typically prepared through an extrusion process or pan granulation process.
According to an embodiment of the present invention, drying of granules may be
30 performed in a suitable drying equipment such as fluid bed dryer.
According to an embodiment of the present invention, the drying of extruded
granules is performed at a temperature not more than 60°C.
22
According to preferred embodiment of the present invention, the drying of granules
is performed at a temperature range of 50°C -60°C. The granules thus obtained
by granulation are subjected to drying at temperature lesser than 60°C to reduce
moisture content less than 2 % to obtain the finished composition.
5
The drying process will preferably remove as much water as possible in order to
reduce weight and to provide good stability to the granules while still in a dry
flowable state. Preferably the granules will be dried to less than 2% as weight loss
on complete drying and most preferably dried to less than 2 % as weight loss on
10 complete drying.
According to an embodiment of the present invention, materials used in the
process of the invention may be in a finely divided form, preferably in an air-milled
form which is generally the form of technical grade chemicals supplied by
15 manufacturers.
After thorough mixing or after otherwise putting the mix into a form suitable for
extrusion, extrusion takes place through suitable orifices. The size of the granules
will depend upon the size of the orifices and the extruder may thus be fitted with a
20 mesh or die selected to provide a desired size of granule. Preferably extrusion
orifices will be chosen to provide extrusions between 0.8 and 1mm in diameter.
The extrusions can vary considerably in length, e.g. up to 0.2 to 1.0 cm
The process of the invention considerably reduces the amount of oversized and
25 undersized material which must be recycled. Consequently, the granule
composition is essentially dust free.
In an embodiment the present insecticide composition is used as pesticide to
control insects in the agriculture field.
30
In an embodiment the present insecticide composition is effective as pesticides,
for example, insecticides, miticides, nematicides and soil pesticides. For instance,
the stable insecticide composition is against plant parasitic mites such as twospotted
spider mite (Tetranychus urticae), carmine spider mite (Tetranychus
23
cinnabarinus) or citrus red mite (Panonychus citri) or bulb mite (Rhizoglyphus
echinopus); aphids such as green peach aphid (Myzus persicae) or cotton aphid
(Aphis gossypii); agricultural insect pests such as diamondback moth (Plutella
xylostella), cabbage armyworm (Mamestra brassicae), common cutworm
(Spodoptera litura), colorado potato beetle (5 Leptinotarsa decemlineata), codling
moth (Laspeyresia pomonella), bollworm (Heliothis zea), tobacco budworm
(Heliothis virescens), boll weevil (Anthonomus grandis), gypsy moth (Lymantria
dispar), cucurbit leaf beetle (Aulacophora femoralis), planthoppers, leafhoppers,
scales, bugs, whiteflies, thrips, grasshoppers, anthomyiid flies, scarabs, black
10 cutworm (Agrotis ipsilon), cutworm (Agrotis segetum) or ants; hygienic insect pests
such as tropical rat mite (Ornithonyssus bacoti), cockroaches, housefly (Musca
domestica) or house mosquito (Culex pipiens pallens); stored grain insect pests
such as angoumois grain moth (Sitotroga cerealella), azuki bean weevil
(Callosobruchus chinensis), confused flour beetle (Tribolium confusum) or
15 mealworms; household goods insect pests such as casemaking clothes moth
(Tinea pellionella), black carpet beetle (Anthrenus scrophularidae) or subterranean
termites; and other parasites on domestic animals such as fleas, lice or flies.
Further, said composition is effective against insect pests such as aphids having
acquired resistance to organophosphorus, carbamate and/or synthetic pyrethroid
20 insecticides.
The compositions of the present invention can be used in agricultural lands such
as fields, paddy fields, lawns and orchards or in non-agricultural lands. The present
invention may be used to control diseases in agricultural lands for cultivating the
25 plants without any phytotoxicity to the plant.
Examples of the crops on which the present compositions may be used include but
are not limited to corn, rice, wheat, barley, rye, oat, sorghum, cotton, soybean,
peanut, buckwheat, beet, rapeseed, sunflower, sugar cane, tobacco, etc.;
30 vegetables: solanaceous vegetables such as eggplant, tomato, pimento, pepper,
potato, etc., cucurbit vegetables such as cucumber, pumpkin, zucchini, water
melon, melon, squash, etc., cruciferous vegetables such as radish, white turnip,
horseradish, kohlrabi, Chinese cabbage, cabbage, leaf mustard, broccoli,
cauliflower, etc., asteraceous vegetables such as burdock, crown daisy, artichoke,
24
lettuce, etc, liliaceous vegetables such as green onion, onion, garlic, and
asparagus, ammiaceous vegetables such as carrot, parsley, celery, parsnip, etc.,
chenopodiaceous vegetables such as spinach, Swiss chard, etc., lamiaceous
vegetables such as Perilla frutescens, mint, basil, etc, strawberry, sweet potato,
Dioscorea japonica, colocasia, etc., flowers, foliage plants, 5 turf grasses, fruits:
pome fruits such apple, pear, quince, etc, stone fleshy fruits such as peach, plum,
nectarine, Prunus mume, cherry fruit, apricot, prune, etc., citrus fruits such as
orange, lemon, rime, grapefruit, etc., nuts such as chestnuts, walnuts, hazelnuts,
almond, pistachio, cashew nuts, macadamia nuts, etc. berries such as blueberry,
10 cranberry, blackberry, raspberry, etc., grape, kaki fruit, olive, plum, banana, coffee,
date palm, coconuts, etc. , trees other than fruit trees; tea, mulberry, flowering
plant, trees such as ash, birch, dogwood, Eucalyptus, Ginkgo biloba, lilac, maple,
Quercus, poplar, Judas tree, Liquidambar formosana, plane tree, zelkova,
Japanese arborvitae, fir wood, hemlock, juniper, Pinus, Picea, and Taxus
15 cuspidate, etc.
According to an embodiment, the present invention provides the use of the present
insecticidal composition for controlling insects wherein the composition comprises:
at least one agrochemical active ingredient and a surfactant combination
20 comprising a copolymer and an organosulfate.
In an embodiment the present invention provides a method of controlling insects
comprising applying to the pests or to their locus, an effective amount of insecticide
composition comprising;
25 i) at least one hydrophilic agrochemical active ingredient;
ii) at least one hydrophobic agrochemical active ingredient; and
a surfactant combination comprising a copolymer and an organosulfate.
In an embodiment the present invention provides a method of controlling insects
30 comprising applying to the pests or to their locus, an effective amount of insecticide
composition comprising;
i) at least one hydrophilic insecticide;
ii) at least one hydrophobic insecticide; and
a surfactant combination comprising a copolymer and an organosulfate.
25
According to an embodiment of the present invention, a method of controlling
unwanted pests, said method comprising applying to the pests or to their locus, an
agrochemical effective amount of present stable insecticidal compositions
5 comprising:
i) fipronil;
ii) pymetrozine; and
iii) a surfactant combination of a copolymer and an organosulfate.
10 In an embodiment the present composition does not contain an inorganic salt.
According to an embodiment of the present invention, a method of controlling
unwanted pests, said method comprising applying an insecticidally effective
amount of an insecticidal composition comprising:
15 i) fipronil;
ii) pymetrozine; and
iii) a surfactant combination of a copolymer and an organosulfate.
wherein a copolymer and an organosulfate are present in a ratio from about 1:1 to
about 1:4.
20
According to an embodiment of the present invention, a method of controlling
unwanted pests, said method comprising applying an insecticidally effective
amount of stable insecticidal compositions to the pests or to their locus, said
composition comprising fipronil, pymetrozine and a surfactant combination of a
25 copolymer and an organosulfate.
In an embodiment the present compositions are in the form of a multi-pack product
or as a kit-of-parts for controlling insects.
30 According to an embodiment of the present invention, the kit comprises:
i) fipronil;
ii) pymetrozine; and
iii) a surfactant combination of a copolymer and an organosulfate;
26
wherein a copolymer and an organosulfate.are present in a ratio from about 1:1 to
about 1:4.
In one embodiment of the present invention, the kits may include one or more,
including all, components that may be used to 5 prepare the stable insecticide
composition. Examples of kits include hydrophilic agrochemical active ingredient,
hydrophobic agrochemical active ingredient, and/or disintegration system. One or
more of the components may already be combined together or pre-formulated. In
those embodiments where more than two components are provided in a kit, the
10 components may already be combined together and as such are packaged in a
single container such as a vial, bottle, can, pouch, bag or canister.
In other embodiments, two or more components of a kit may be packaged
separately, i. e., not pre-formulated. As such, kits may include one or more
15 separate containers such as vials, cans, bottles, pouches, bags or canisters, each
container containing a separate component for stable insecticide composition.
In both forms, a component of the kit may be applied separately from or together
with the further components or as a component of a combination composition
20 according to the invention for preparing the stable insecticide composition
according to the invention.
In an embodiment of the present invention, the stable insecticidal comprises
fipronil; pymetrozine and a surfactant combination of a copolymer and an
25 organosulfate;
wherein a copolymer and an organosulfate are present in a ratio from about 1:1 to
about 1:4 is in the form of a kit with single pack or multi pack.
In an embodiment of the present invention, the stable insecticidal composition
30 comprising (a) at least one hydrophilic agrochemical active ingredient (b) at least
one hydrophobic active ingredient and (c) surfactant combination of a copolymer
and an organosulfate is in the form of a kit with single pack or multi pack.
27
In an embodiment, the multi-pack herbicidal product comprises a package holding
a composition comprising at least one agrochemical active ingredient selected
from hydrophobic and hydrophilic agrochemical active ingredient; surfactant
combination of a copolymer and an organosulfate, wherein said composition does
not 5 contain an inorganic salt.
It will be understood that the specification and examples are illustrative but not
limitative of the present invention and that other embodiments within the spirit and
scope of the invention will suggest themselves to those skilled in the art. Other
10 embodiments can be practiced that are also within the scope of the present
invention. The following examples illustrate the invention, but by no means intend
to limit the scope of the claims.
EXAMPLES
15 Example 1: Pymetrozine + Fipronil WDG formulation
Sr.No. Ingredients
Amount (% W/W)
1 Fipronil 8
2 Pymetrozine 35
3 Sodium lauryl sulphate
10.25
4 Urea-formaldehyde copolymer 3
5 Kaolin Q. S.
Total 100
Process:
Above mentioned ingredients in specified quantity were added and blended in a
ribbon blender for 20-30 min to obtain blend. The blend was further ground in air
20 jet mill to obtain a ground mix having particle size D100 below 30 micron. The ground
mix for then blended for 20-30 min to obtain homogeneous mixture. The
homogeneous mixture was taken to prepare dough using water spray. Granules
were then extruded in a granulator having sieve size 0.8 to 1.0 mm aperture. The
extruded granules were dried on fluid bed dryer at temperature ranging between
25 50°C to 60°C. The dried granules were passed through sieve to obtain uniformly
sized granules. Undersized and oversized granules were recycled back. Finished
granules were packed in a suitable packaging.
28
Example 2
Stability test
The WDG compositions of Example 1 was tested for suspensibility, degradation of
active ingredient as well as its effect on stability of the composition. The stability
study was conducted for 14 days AHS (Accelerated Heat 5 Stability) at 54±2°C and
at ambient temperature. The results are summarized in below table.
Table 2: Stability studies of formulation of Example 1
Sr.
No.
Physico chemical Properties Stability test
AMB AHS 14
Days
1 Description Complies
2 Active Ingredient Content as (%
w/w)
1)Pymetrozine 36.09 35.94
2) Fipronil 8.52 8.54
3 Suspensibility (% w/w)
99.06
99.02
98.11 98.14
4 pH (1% aqueous dispersion) at
25°C
8.96 9.27
5 Persistent foam (in mL, after 1
minute)
10 10
6 Wet sieve (% w/w material
retained on 75μm test sieve)
0.2 0.2
7 Wettability 57 5
8 LOD at 105°C, 15 min 2.38 NA
10 Disintegration 28 28
AMB: Ambient conditions
10 AHS: Accelerated heat storage conditions
LOD: Loss-on-drying
It is demonstrated in the above table that the present composition exhibited very
good suspensibility and also passed the wet sieve test.
15
29
Example 3
The composition as represent in example 1 was prepared with inorganic salt.
The stability of the composition of present invention without inorganic salt as
described in Example 2 (ammonium salt) and the comparative composition with
5 inorganic salt was evaluated.
Table 3: Stability studies of formulation with inorganic salt
Sr.
No.
Physico chemical Properties
Stability test 􀂱
With Inorganic salt
AMB AHS 14 Days
1 Description Complies
2
Active Ingredient Content as
(% w/w)
1)Pymetrozine 35.57 35.27
2) Fipronil 8.72 8.61
3 Suspensibility (% w/w)
76.52 66.17
77.47 58.32
4
pH (1% aqueous dispersion)
at 25°C
8.92 9.12
5
Persistent foam (in mL, after 1
minute)
10 10
6
Wet sieve (% w/w material
retained on 75μm test sieve)
0.84 0.95
7 Wettability 10 10
8 LOD at 105°C, 15 min 2.4 NA
10 Disintegration 28 28
AMB: Ambient
10 AHS: Accelerated heat storage conditions
It is evident from the above table that the composition containing ammonium
sulphate has low suspensibility as compared to the composition without
ammonium sulphate. Further, it is observed that suspensibility of such composition

dropped in AHS after 14 days@54􀔨. However, there was no significant change in
the suspensibility of the present composition, thus present WDG composition
remains stable and does not undergo any chemical and physical change on
storage and is also easy to handle for further use.
We claim:
1. An insecticide composition comprising:
at least one agrochemical active ingredient; and
a surfactant combination comprising a copolymer and an organosulfate, wherein the composition does not contain inorganic salt. 2. The composition as claimed in claim 1 wherein said agrochemical active ingredient is selected from hydrophilic agrochemical active ingredient, hydrophobic agrochemical active ingredient or combinations thereof.
3. The composition as claimed in claim 2 wherein said hydrophilic agrochemical active ingredient is selected from flonicamid, pymetrozine, acephate, acetamiprid and combinations thereof.
4. The composition as claimed in claim 2 wherein said hydrophobic agrochemical active ingredient is selected from fipronil, flubendiamide, indoxacarb, diafenthiuron, bifenthrin and combinations thereof.
5. The composition as claimed in claim 1 wherein the hydrophilic agrochemical active ingredient is present in an amount from 10% w/w to about 90% w/w and the hydrophobic agrochemical active ingredient is present in an amount from 10% w/w to about 90% w/w of the composition.
6. The composition as claimed in claim 1 wherein said organosulfate is alkyl sulphate or salts thereof and said copolymer is urea-formaldehyde copolymer.
7. The composition as claimed in claim 1 wherein a copolymer and an organosulfate are present in a ratio from about 1:1 to about 1:4.
8. A water dispersible granule composition comprising:
i) pymetrozine; ii) fipronil; and
iii) a surfactant combination comprising a copolymer and an organosulfate, wherein the composition does not contain inorganic salt.
9. A process of preparing insecticide composition as claimed in claim 8
comprising steps of:

i) blending a mixture of agrochemical active ingredient, a disintegration system comprising a copolymer and an organosulfate, to obtain a blend; ii) grinding the blend to obtain ground mix; and
iii) preparing dough from the homogeneous mixture and perform granulation to obtain granular composition. 10. A method of controlling insects comprising applying to the pests or to their locus, an effective amount of insecticide composition as claimed in claim 1 comprising;
at least one hydrophilic agrochemical active ingredient; at least one hydrophobic agrochemical active ingredient; and a surfactant combination comprising a copolymer and an organosulfate.