U.S. patent application number 16/750495 was filed with the patent office on 2020-05-21 for insecticidal compositions and methods using same.
This patent application is currently assigned to Woodstream Corporation. The applicant listed for this patent is Woodstream Corporation. Invention is credited to David L. ANDERSON.
Application Number | 20200154717 16/750495 |
Document ID | / |
Family ID | 35187355 |
Filed Date | 2020-05-21 |
United States Patent
Application |
20200154717 |
Kind Code |
A1 |
ANDERSON; David L. |
May 21, 2020 |
INSECTICIDAL COMPOSITIONS AND METHODS USING SAME
Abstract
The present invention provides novel insecticidal formulations
comprising an effective concentration of: 1) at least one or more
essential oils and an insecticidal soap; 2) at least one or more
essential oils, an insecticidal soap, and pyrethrins; 3) at least
one or more essential oils and pyrethrins; 4) at least one or more
essential oils, an insecticidal soap and a synergist, such as
sodium lauryl sulfate, sodium dodecyl sulfate or lecithin; 5) at
least one or more essential oils, an insecticidal soap, a
synergist, and pyrethrins; and 6) at least one or more essential
oils, a synergist, and pyrethrins. A carrier oil, such as mineral
oil, may be added to any of the foregoing formulations.
Inventors: |
ANDERSON; David L.; (Lititz,
PA) |
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Applicant: |
Name |
City |
State |
Country |
Type |
Woodstream Corporation |
Lititz |
PA |
US |
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|
Assignee: |
Woodstream Corporation
Lititz
PA
|
Family ID: |
35187355 |
Appl. No.: |
16/750495 |
Filed: |
January 23, 2020 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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15294869 |
Oct 17, 2016 |
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16750495 |
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14220215 |
Mar 20, 2014 |
9642373 |
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15294869 |
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11105578 |
Apr 14, 2005 |
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14220215 |
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60562252 |
Apr 15, 2004 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A01N 27/00 20130101;
A01N 49/00 20130101; A01N 53/00 20130101; A01N 25/30 20130101; A01N
37/02 20130101; A01N 37/02 20130101; A01N 53/00 20130101; A01N
37/02 20130101; A01N 25/22 20130101; A01N 2300/00 20130101; A01N
41/02 20130101; A01N 25/30 20130101; A01N 31/16 20130101; A01N
57/12 20130101; A01N 25/02 20130101; A01N 27/00 20130101; A01N
65/00 20130101; A01N 41/02 20130101; A01N 57/12 20130101; A01N
49/00 20130101; A01N 65/00 20130101; A01N 25/02 20130101; A01N
25/30 20130101; A01N 53/00 20130101; A01N 31/16 20130101; A01N
2300/00 20130101; A01N 65/26 20130101; A01N 53/00 20130101; A01N
25/02 20130101 |
International
Class: |
A01N 65/26 20060101
A01N065/26; A01N 25/30 20060101 A01N025/30; A01N 25/22 20060101
A01N025/22; A01N 25/02 20060101 A01N025/02; A01N 53/00 20060101
A01N053/00; A01N 37/02 20060101 A01N037/02 |
Claims
1-39. (canceled)
40: An insecticidal composition comprising neem oil, pyrethrins,
and a pyrethrin-breakdown preventing antioxidant.
41: The insecticidal composition of claim 40 in aqueous form.
42: The insecticidal composition of claim 40 in aqueous form,
wherein the amount of neem oil is about 0.25% to about 12% by
weight, the amount of pyrethrins is about 0.01% to about 0.5% by
weight, and the remainder is water and the antioxidant.
43: The insecticidal composition of claim 40 further comprising a
carrier oil.
44: The insecticidal composition of claim 40 further comprising an
essential oil selected from the group consisting of D-limonene and
palmarosa oil.
45: The insecticidal composition of claim 40 further comprising an
essential oil selected from the group consisting of cornmint oil,
cedar oil, cinnamon oil, citronella oil, clove oil, corn oil.
garlic oil, lemongrass oil, linseed oil, peppermint oil, rosemary
oil, soybean oil, thyme oil, orange oil, lemon oil, lime oil,
grapefruit oil, tangerine oil, D-limonene, eugenol, geraniol,
palmarosa oil, and mixtures thereof.
46: The insecticidal composition of claim 40 in sprayable form.
47: The insecticidal composition of claim 40 further comprising
insecticidal soap.
48: The insecticidal composition of claim 40 further comprising an
insecticidal soap containing potassium salts of fatty acids.
49: A method of killing insects comprising applying the
insecticidal composition of claim 40 to one or more insects.
50: The method of claim 49, wherein the insecticidal composition is
in aqueous form.
51: The method of claim 49, wherein the amount of neem oil is about
0.25% to about 12% by weight, the amount of pyrethrins is about
0.01% to about 0.5% by weight, and the remainder is water and the
antioxidant.
52: The method of claim 49, wherein the insecticidal composition
further comprises a carrier oil.
53: The method of claim 49, wherein the insecticidal composition
further comprises an essential oil selected from the group
consisting of D-limonene and palmarosa oil.
54: The method of claim 49, wherein the insecticidal composition
further comprises an essential oil selected from the group
consisting of cornmint oil, cedar oil, cinnamon oil, citronella
oil, clove oil, corn oil. garlic oil, lemongrass oil, linseed oil,
peppermint oil, rosemary oil, soybean oil, thyme oil, orange oil,
lemon oil, lime oil, grapefruit oil, tangerine oil, D-limonene,
eugenol, geraniol, palmarosa oil, and mixtures thereof.
55: The method of claim 49, wherein the insecticidal composition is
in sprayable form.
56: The method of claim 49, wherein the insecticidal composition
further comprises insecticidal soap.
57: The method of claim 49, wherein the insecticidal composition
further comprises an insecticidal soap containing potassium salts
of fatty acids.
Description
RELATED APPLICATION
[0001] This application is entitled to and hereby claims the
priority of co-pending U.S. Provisional Application Ser. No.
60/562,252, filed Apr. 15, 2004.
BACKGROUND OF THE INVENTION
1. Field of Invention
[0002] This invention relates generally to insecticidal
compositions and methods of using same to control various crawling
and flying insect pests, and, in its preferred embodiments, relates
more particularly to a combination of synergistic non-poison
insecticides by themselves and in combination with a known poison
insecticide at a greatly reduced concentration, and adapted to
unexpectedly increase insect mortality and reduce kill time.
2. Description of Prior Art
[0003] Commercially available insecticides, including those
available for home use, commonly comprise active ingredients or
poisons which are not only toxic to the target insect pests, but,
if used in relatively confined environments and delivered as
aerosol sprays, can be present in sufficient concentration to also
be toxic to humans and household pets. Various undesirable side
effects may include immediate or delayed neurotoxic reactions,
and/or suffocation. Even the noxious odor of such materials can
cause headaches or upset stomachs in some individuals. These
adverse side effects are exacerbated when such compositions come in
contact with persons of increased sensitivity, or persons of small
body mass such as children or babies.
[0004] For some time, efforts have been made to develop
insecticidal compositions, particularly those intended for
residential use in aerosol form, which are effective in killing the
targeted insect pests completely and quickly, but non-toxic to
humans and pets. The Environmental Protection Agency (EPA)
regulates the use of potentially toxic ingredients in pesticidal
compositions under the Federal Insecticide, Fungicide and
Rodenticide Act (FIFRA). Certain materials considered to be either
active or inert materials by the EPA have been deregulated or
otherwise identified as acceptable safe substances under FIFRA
offering minimum risk in normal use. Other materials are currently
undergoing investigation and may be deregulated in due course.
Consumers generally consider deregulated substances non-poisonous.
Thus, the term non-poisonous as used herein is intended to convey a
compound or composition that, while highly effective in killing
targeted insect pests, is safe to use around humans, particularly
small children, and pets.
[0005] Among the insects that are found to be particularly
undesirable are cockroaches, both the American and German species.
These pests shed their skin, which, over time, disintegrates
forming what is known as cuticle in the air, a particular problem
for people suffering from asthma. Thus, not only is it important to
kill cockroaches with an effective insecticide, but also the kill
time must be sufficiently short for the carcass to be properly
disposed of before the insect can crawl into a remote area to
die.
[0006] While cockroaches are a prime target for a household spray,
for general application such materials must also be effective
against other crawling insects, such as ants, water bugs,
silverfish, crickets, spiders and centipedes. Additionally, aerosol
compositions of such insecticides of proper concentration must also
be effective against various flying insects, including flies,
mosquitoes, gnats, moths, wasps, hornets, yellow jackets and other
bees, both inside and outside of the house.
[0007] One of the materials exempted by the EPA under FIFRA is
cornmint oil (also known as Japanese mint or Mentha arvensis).
Cornmint oil includes a high concentration of menthol and is known
to contain alpha-pinene, myrcene, limonene, gamma-terpenine,
3-octanol, menthofuran, beta-caroyophyllene, germa-crene D and
beta-pinene, along with other components. As with other mint oils,
cornmint oil has been used as a flavoring agent in mouthwashes,
cough syrups, throat lozenges, chewing gum, and the like.
[0008] Recently, it has been found that when cornmint oil was
combined with a synergist such as sodium lauryl sulfate ("SLS"),
cornmint oil became a highly effective insecticide against common
household pests such as American and German cockroaches and black
ants. These findings are described in U.S. Pat. No. 5,998,484 (the
"'484 patent"), assigned to Woodstream Corporation. These findings
were surprising because prior to the '484 patent, cornmint oil had
not been shown to be particularly effective, and certainly was not
distinguished from other materials of this kind as a candidate for
special attention.
[0009] Other essential oils currently deregulated by the EPA under
FIFRA include cedar oil, cinnamon oil, citronella oil, clove oil,
corn oil, garlic oil, lemongrass oil, linseed oil, peppermint oil,
rosemary oil, soybean oil and thyme oil. Among the essential oils
proposed for exemption from registration are a number of the citrus
oils. Citrus oils would include orange oil, lemon oil, lime oil,
grapefruit oil and tangerine oil.
[0010] As with cornmint oil, it was also recently discovered that
many of these other deregulated essential oils which had not been
previously shown to be particularly effective as active
ingredients, by themselves, were in fact effective insecticidal
compositions when combined with a synergist such as lecithin or
SLS. These insecticidal compositions can be found in U.S. Pat. No.
6,548,085, also assigned to Woodstream Corporation.
[0011] Pyrethrum is a natural plant oil that occurs in the
pyrethrum daisy, Tanacetum cinerariaefolium, a member of the
chrysanthemum family (Chrysanthemum cinerariaefolium). It is found
mainly in tiny oil-containing glands on the surface of the seed
case in the tightly packed flower head. Pyrethrum flowers are also
known as Dalmatian Insect powder and Persian Insect powder. Several
trade names associated with these compounds are Buhach,
Chrysanthemum cinerariaefolium, Ofirmotox, Insect Powder, Dalmation
Insect Flowers, Firmotox, Parexan and NA 9184. The flowers of the
plant are harvested shortly after blooming and are either dried and
powdered or the oils within the flowers are extracted with
solvents. The resulting mixture of pyrethrin containing dusts and
extracts usually have an active ingredient content of about 30%.
These active insecticidal components of pyrethrum are collectively
known as pyrethrins. Two pyrethrins are most prominent, pyrethrin-I
and pyrethrin-II. The pyrethrins include other active ingredients
such as Cinerin I and II, Jasmolin I and II, pyrethrosin, pyretol,
pyrethrotoxic acid, chrysanthemine, chrysanthemumic acid. See,
Merck Index, Eleventh ed., (1989). Pyrethrin compounds have been
used primarily to control human lice, mosquitoes, cockroaches,
beetles and flies. Some "pyrethrin dusts," used to control insects
in horticultural crops, are only 0.3% to 0.5% pyrethrins, and are
used at rates of up to 50 lb/Acre. Other pyrethrin compounds may be
used in grain storage and in poultry pens and on dogs and cats to
control lice and fleas. However, the natural pyrethrins are contact
poisons which quickly penetrate the nervous system of the insect. A
few minutes after application, the insect cannot move or fly away.
The natural pyrethrins can be swiftly detoxified by enzymes in the
insect. Semisynthetic derivatives of the chrysanthemumic acids have
been developed as insecticides. These are called pyrethroids and
tend to be more effective than natural pyrethrins while they are
less toxic to mammals. One common synthetic group of pyrethroid
compounds are the allethrins, also known as allyl cinerins
(allethrin I and II).
[0012] Pyrethrum was used commercially many years ago as an
insecticide, primarily in the form of "oleoresin of pyrethrum".
Oleoresin of pyrethrum is an archaic pharmaceutical term for an
ether extract of the cinerariaefolium variety of Chrysanthemum. It
contains volatile oils and components having insecticidal
properties, called pyrethrins, jasmolins, and cinerins. These
materials are known to be toxic to insects, essentially non-toxic
to mammals, to lack persistence in the environment, and to be
characterized by negligible biological magnification in the food
chain.
[0013] As used herein, the term "pyrethrins" is intended to mean
pyrethrin and its active components. One of the problems with using
pyrethrins as insecticides is their high cost per unit dose. An
example of such a composition comprising a mixture of saponified
organic acids, i.e., salts of coconut oil, and pyrethrins was sold
commercially under the trademark Red Arrow about 55 years ago.
However, these mixtures did not solve the expense problem because
of their high pyrethrin content, about 40% by weight, and because
the coconut oil soaps contributed little to their insecticidal
efficacy. In fact, most commercially available fatty acid soap
compositions contain an excess of alkali which is thought to
promotes hydrolysis and inactivation of pyrethrins. Pyrethrin-based
insecticides also degrade rapidly in storage and in use.
[0014] More recently, the commercially effective use of pyrethrins
was shown when pyrethrins were combined with certain fatty acid
salts and a low molecular weight alcohol, such as isopropanol. See
for example, U.S. Pat. Nos. 4,904,645, and 4,983,591.
[0015] Insect killing soap has also been sold commercially as an
insecticide for many years. An example is the Safer.RTM. Brand
Insect Killing Soap Formulation. This insecticide soap formulation
contains about 49.52% potassium salts of fatty acids by weight, and
was used to formulate treatments containing about 1.0% to about
2.0% potassium salts of fatty acids by weight. Insecticidal soap
has also been shown to have synergistic effects when combined with
an insecticide, i.e. pyrethrin, and the soap and compositions of
soap and pyrethrins are described in U.S. Pat. Nos. 4,861,762,
4,983,591 and 5,047,424. These three patents, as well as U.S. Pat.
Nos. 6,548,085,and 5,998,484 which describe the combination of
essential oils and a synergist, are all incorporated by reference
herein as if fully set forth in their entireties.
SUMMARY OF THE INVENTION
[0016] In accordance with the present invention, it has now been
found that insecticidal soap, when combined with one or more
essential oils, has a similar effect on killing insects as
synergists such as SLS, thus resulting in a more efficacious
product. Further, by combining appropriate concentrations of
insecticidal soap and at least one essential oil, it has been found
that a lower concentration of each individual component is needed
than if they were used separately. In addition, insecticidal soap
by itself, has poor efficacy on hard bodied insects (i.e. beetles),
and the combination of an essential oil and soap provides a novel
formulation that is able to control a broader range of insects.
[0017] Essential oils which are useful in the present invention
include cornmint (mint) oil, cedar oil, cinnamon oil, citronella
oil, clove oil, corn oil, garlic oil, lemongrass oil, linseed oil,
peppermint oil, rosemary oil, soybean oil, citrus oils such as
orange oil, lemon oil, lime oil, grapefruit oil and tangerine oil,
neem oil, thyme oil, eugenol, geraniol, palmarosa oil, and
D-limonene.
[0018] Any suitable insecticidal soap could be used in the
compositions of the present invention. One insecticidal soap known
to be useful in accordance with the present invention is SAFER.RTM.
Brand Insect Killing Soap Concentrate, which is marketed by
Woodstream Corporation, of Lititz, Pa., the assignee of the present
application. This soap concentrate comprises 43.96% Emersol 213
(Oleic Acid), 5.56% potassium hydroxide, 35.61% denatured alcohol
(SD3A or SDA 3C), and 14.87% water. Other commercially available
insecticidal soaps having the same or similar ingredients could
also be used in the compositions of the present invention.
[0019] While not intending to be bound by any particular theory for
the present invention, it is believed that efficacy of the
insecticidal soap operates to kill insects by removing the waxy
layer covering their bodies resulting in dehydration and ultimately
death. Soap will also cause the rupturing of cell membranes and
disrupt the cellular osmotic relationships. Essential oils, in
contrast, work by attacking the nervous system of insects, but must
first penetrate the waxy layer covering the insect. It has now been
found that when at least one essential oil and insecticidal soap
are combined, insecticidal efficacy is improved. It is believed
that the combination has a synergistic effect in that the, soap
solubilizes the waxy outer layer of the insect and weakens the cell
membranes, thereby allowing the essential oil to penetrate the
exoskeleton and reach the insect's nervous system more quickly.
[0020] In an alternate embodiment, the Present invention provides a
synergistic composition comprising insecticidal soap, at least one
essential oil, and pyrethrins. Any suitable pyrethrin concentrate
can be used in he foregoing synergistic composition. Pyrethrin
concentrates typically include an antioxidant such as ethoxyquin, a
tocopherol, or BHT to prevent the pyrethrins from breaking down.
Further, since nyrethrins are not readily soluble in water, an
alcohol may also be included, such as SD3A or SDA 3C, or other
denatured alcohols, to help solubilize the pyrethrins. By combining
appropriate concentrations of the insecticidal soap, one or more
essential oils and pyrethrins, lower concentrations of the
individual components are needed than if they were used separately
thereby lowering overall toxicity to humans and pets.
[0021] It is a primary object of the instant invention to provide a
non-poisonous broad-spectrum insecticide containing, as an
essential active ingredient, materials that have been approved by
the EPA as safe or as offering minimum risk in products of this
nature. Consistent with this objective, this invention provides an
aerosol insecticide which is not detrimental to the health of
humans or pets and which is environmentally safe, yet effective in
killing targeted insect pests with which it comes in contact.
[0022] Another object of the instant invention is the provision of
an insecticidal composition that not only effectively kills 100% of
the targeted insects with which it comes in contact, but kills such
insects within seconds of contact so that the user can be certain
of the effectiveness of the insecticide, and the insect carcass can
be safely and easily disposed of without contaminating the
environment.
[0023] Yet a further object of this invention is the provision of
an insecticidal composition comprising a combination of ingredients
which individually are relatively ineffective, but act in concert
to provide high total killing power with a substantially decreased
kill time.
[0024] Yet another object of this invention is the provision of an
insecticidal composition comprising one or more essential oils,
preferably selected from the group consisting of cedar oil,
cornmint oil, cinnamon oil, citronella oil, lemongrass oil,
peppermint oil, orange oil, lemon oil, lime oil, grapefruit oil,
tangerine oil, neem oil, thyme oil, eugenol, geraniol, palmarosa
oil, and D-limonene in synergistic combination with an insecticidal
soap having about 0.5% to about 2.0% by weight of potassium salts
of fatty acids, such as oleic acid, which enhances the
effectiveness of the composition sufficiently to render the
otherwise relatively ineffective individual components functionally
enhanced and quicker-acting, thereby improving both the mortality
and the kill time. Among the deregulated essential oils, cedar oil
and cornmint oil are particularly attractive because of their
pleasant odors.
[0025] Still another object of this invention is the provision of
an insecticidal composition comprising at least one or more
essential oils, a synergist and pyrethrins, the combination of
which reduces the quantity of the pyrethrins necessary to effect
acceptable mortality rates in at least some insect populations,
even further reducing the cost and dangers of using such materials
by the general public. Compounds other than SLS and lecithin that
can be used as synergists are insecticidally effective quantities
of sodium dodecyl sulfate, potassium salts of fatty acids, ammonium
salts of fatty acids, as well as plain fatty acids like
hexadeconoic acid, lauric acid, myristic acid, and oleic acid.
[0026] Yet another object of this invention is to provide an
insecticidal composition comprising at least one or more essential
oils and an insecticidal soap composition such as the SAFER.RTM.
Insect Killing Soap Concentrate, in combination with
pyrethrins.
[0027] A further object of the present invention is the provision
of a highly effective insecticidal composition, which may be
sprayed in aerosol form from a standard pump dispenser or, which
may incorporate a propellant such as carbon dioxide (CO.sub.2),
nitrogen (N.sub.2) or the like, in a pressurized container of
conventional design, so that the composition may be sprayed
directly onto a crawling or flying insect pest.
[0028] Another object of this invention is the provision of an
insecticidal composition of the type described incorporating
mineral oil or other such material as a carrier oil to retain the
essential oils on a contacted surface for residual killing power
over an extended period of time.
[0029] These and other objects of the invention, as well as many of
the attendant advantages thereof, will become more readily apparent
when reference is made to the following detailed description of the
preferred embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] FIG. 1 is a chart showing the test results of certain
concentrations of mint oil in combination with various
concentrations of synergists, pyrethrins, and insecticidal soap on
killing German Cockroaches.
[0031] FIG. 2 is a chart showing the test results of certain
concentrations of mint oil, D-limonene or palmarosa oil in
combination with various concentrations of synergists, pyrethrins,
and insecticidal soap on killing Carpenter Ants.
[0032] FIG. 3 is a chart showing the test results of certain
concentrations of eugenol in combination with various
concentrations of synergists, pyrethrins, and insecticidal soap on
killing German Cockroaches.
[0033] FIG. 4 is a chart showing the test results of certain
concentrations of thyme oil in combination with various
concentrations of synergists, pyrethrins, and insecticidal soap on
killing German Cockroaches.
[0034] FIG. 5 is a chart showing the test results of certain
concentrations of mint oil, D-limonene and palmarosa oil in
combination with various concentrations of synergists, pyrethrins,
and insecticidal soap on killing German Cockroaches.
[0035] FIG. 6 is a chart showing the test results of certain
concentrations of various essential oils in combination with
various concentrations of pyrethrins, and insecticidal soap on
killing Carpenter Ants.
[0036] FIG. 7 is a chart showing the test results of certain
concentrations of D-limonene in combination with various
concentrations of synergists, pyrethrins, and insecticidal soap on
killing German Cockroaches.
DETAILED DESCRIPTION AND PREFERRED EMBODIMENTS
[0037] In describing a preferred embodiment of the invention
specific terminology will be resorted to for the sake of
clarity.
[0038] However, the invention is not intended to be limited to the
specific terms so selected, and it is to be understood that each
specific term includes all technical equivalents which operate in a
similar manner to accomplish a similar purpose.
[0039] It has previously been shown that the combination of certain
essential oils and a synergist, such as SLS or lecithin, is an
effective insecticidal composition in U.S. Pat. Nos. 5,998,484 and
6,548,085.
[0040] In its broadest aspects, the essential active ingredients in
the compositions of the instant invention are any of the following:
a) the combination of at least one or more essential oils and
insecticidal soap; b) the combination of at least one or more
essential oils, insecticidal soap and pyrethrins; c) the
combination of at least one or more essential oils and pyrethrins;
d) the combination of at least one or more essential oils,
insecticidal soap and a synergist; e) the combination of at least
one or more essential oils, insecticidal soap, pyrethrins and a
synergist; and f) the combination of at least one or more essential
oils, pyrethrins and a synergist. The active ingredients are
preferably dissolved in an inert carrier such as water.
[0041] The essential oils which are useful in the present invention
include cornmint (mint) oil, cedar oil, cinnamon oil, citronella
oil, clove oil, corn oil, garlic oil, lemongrass oil, linseed oil,
peppermint oil, rosemary oil, soybean oil, citrus oils such as
orange oil, lemon oil, lime oil, grapefruit oil and tangerine oil,
neem oil, thyme oil, eugenol, geraniol, palmarosa oil, and
D-limonene.
[0042] Any suitable insecticidal soap can be used in the
compositions of the present invention; however, SAFER.RTM. Brand
Insect Killing Soap Concentrate is a preferred insecticidal soap.
The SAFER.RTM. Brand Insect Killing Soap Concentrate includes
43.96% Emersol 213 (Oleic Acid), 5.56% potassium hydroxide, 35.61%
denatured alcohol (SD3A or SDA 3C), and 14.87% water. This
composition contains about 49.52% potassium salts of fatty acids by
weight.
[0043] Any suitable pyrethrin concentrate, such as those
commercially available on the market, can be used in the
compositions of the present invention. In order to prevent the
pyrethrins from breaking down, an antioxidant such as ethoxyquin, a
tocopherol, or BHT is typically present in the pyrethrin
concentrate, or otherwise should preferably be included in the
insecticidal compositions. An alcohol is also preferably included,
such as SD3A or SDA 3C, or other denatured alcohol, inasmuch as
pyrethrins are not readily soluble in the water-based compositions
of the present invention.
[0044] A material such as mineral oil may be incorporated into the
composition as a carrier oil to provide residual killing power on
surfaces for up to, as much as, four weeks or more. The essential
oil is dissolved in the carrier oil and prevents the rather
volatile essential oil from evaporating quickly. As a result, the
insects come in contact with the carrier oil composition that will
eventually kill them. Many other oils other than mineral oil are
capable of performing the function of the carrier oil. Some
examples are soybean oil, canola oil, corn oil, sunflower oil, neem
oil, peanut oil, sesame oil, cottonseed oil, fish oil, olive oil,
safflower oil, or castor oil. Obviously, some oils have
characteristics that make them more or less suitable for certain
applications based on odor, color, cost and availability.
[0045] The synergists which can be used in the compositions of the
present invention include SLS, sodium dodecyl sulfate and
lecithin.
[0046] The compositions of the present invention may be dispensed
in a conventional manner, e.g., from a standard pump-spray
container. Alternatively, and preferably, the aqueous insecticidal
composition may be packaged in a pressurized container such as a
conventional aerosol can or the like, utilizing an expandable gas,
such as carbon dioxide (CO.sub.2) as a propellant in a well-known
manner. For optimum effectiveness, the insecticidal composition of
this invention is sprayed directly on targeted crawling or flying
insect pests in sufficient concentrations to cause death within
seconds.
[0047] The compositions of the present invention are generally
described as follows:
[0048] 1) a composition comprising an insecticidal soap providing
from about 0.5% to about 4.0% by weight of potassium salts of fatty
acids to the overall composition, from about 0.25% to about 12% of
one or more essential oils, and the balance water;
[0049] 2) a composition comprising an insecticidal soap providing
from about 0.5% to about 4.0% by weight of potassium salts of fatty
acids to the overall composition, from about 0.25% to about 12% of
one or more essential oils, from about 0.01% to 0.5% pyrethrins,
and the balance water;
[0050] 3) a composition comprising from about 0.25% to about 12% of
one or more essential oils, from about 0.01% to 0.5% pyrethrins,
and the balance water;
[0051] 4) a composition comprising from about 0.25% to about 12% of
one or more essential oils, an insecticidal soap providing from
about 0.5% to about 4.0% by weight of potassium salts of fatty
acids, and from 0.25% to about 5% of a synergist, and the balance
water;
[0052] 5) a composition comprising from about 0.25% to about 12% of
one or more essential oils, an insecticidal soap providing from
about 0.5% to about 4.0% by weight of potassium salts of fatty
acids, from about 0.01% to 0.5% pyrethrins, and from about 0.25% to
about 5% of a synergist, and the balance water; and 6) a
composition comprising from about 0.25% to about 12% of one or more
essential oils, from about 0.01% to about 0.5% pyrethrins, and from
about 0.25% to about 5% of a synergist, and the balance water.
[0053] The above compositions may be combined with a carrier oil
should such properties be desired in the composition for various
applications. Preferably, the amount of carrier oil present in the
composition can be in the range of about 3% to about 8% by weight
of the carrier oil, such as mineral oil.
[0054] The testing described below establishes that insecticidal
soap alone is less effective in killing the targeted insects.
Further, in most instances, the tested essential oils alone either
do not kill the targeted insects, or if they eventually kill some
of the targeted insects, they generally require relatively high
concentrations of the essential oil, and/or they are relatively
slow-acting.
[0055] All treatments were dispensed using a hand pump trigger
sprayer. When the insect pests track through, and come in contact
with, previously sprayed product, the active ingredients remain on
their bodies and they eventually die. Without the mineral oil, the
composition dries, leaving no residue.
[0056] To evidence the unexpectedly improved nature of the results
obtained using the synergistic insecticidal compositions of the
instant invention, the foregoing tests were performed.
[0057] EXAMPLE 1. The following compositions were compared for
effectiveness: a) the Victor.RTM. Poison Free Ant and Roach Killer
formulation containing 4.0% mint oil as the sole active ingredient;
b) Safer.RTM. brand Insect Killing Soap formulation providing a
concentration of 2.0% potassium salts of fatty acids as the sole
active ingredient; c) a formulation of 4.0% mint oil with 2.0%
potassium salts of fatty acids; d) a formulation of 4.0% mint oil
with 2.0% potassium salts of fatty acids and 3.0% lecithin)
Victor.RTM. Poison Free Wasp & Hornet Killer formulation
containing 8% mint oil with 1% SLS as the active ingredients; f) a
formulation of 8% mint oil with 2% potassium salts of fatty acids;
and g) a formulation of 8% mint oil with 2% potassium salts of
fatty acids and 1% SLS. Previous experiments demonstrated that
treatment of insects with 1% SLS alone did not kill insects within
the 300 second time period used in testing (data not shown). All of
the above formulations were tested using the American cockroach,
Periplaneta americana, as the targeted insect.
[0058] American Cockroaches were obtained from a colony maintained
at Woodstream Corporation in Lititz, Pa. PVC pipe was used to calm
and confine the cockroaches prior to spraying. The PVC pipe is
lined with Vaseline before introducing cockroaches to prevent
escape.
[0059] The insecticidal soap used in all the following studies was
Safer.RTM. Brand Insect Killing Soap Concentrate. The soap
concentrate comprises 43.96% Emersol 213 (Oleic Acid), 5.56%
potassium hydroxide, 35.61% denatured alcohol (SD3A or SDA 3C) ,
and 14.87% water. This composition contains about 49.52% potassium
salts of fatty acids by weight, and was used to formulate
treatments containing 2.0% potassium salts of fatty acids by
weight, and is described in U.S. Pat. Nos. 4,861,762, 4,983,591 and
5,047,424, previously incorporated herein by reference.
[0060] The experimental formulations were in the following
percentages of the admixed components by weight:
Treatment 1: 2.0% Potassium Salts of Fatty Acids
TABLE-US-00001 [0061] 4.04% Safer .RTM. Brand Insect Killing Soap
Concentrate 95.96% water
Treatment 2: 4.0% Mint Oil with 2.0% Potassium Salts of Fatty
Acids
TABLE-US-00002 4.0% mint Oil 5.0% mineral Oil 4.04% Safer Insect
Killing Soap Concentrate 86.96% water
Treatment 3: 4.0% Mint Oil with 3.0% Lecithin and 2.0% Potassium
Salts of Fatty Acids
TABLE-US-00003 4.00% mint oil 5.00% mineral oil 3.00% lecithin
4.04% Safer .RTM. Brand Insect Killing Soap Concentrate 83.96%
water
[0062] Treatment 4: Victor.RTM. Poison Free Ant and Roach Insect
Killer
TABLE-US-00004 4.0% mint oil 5.0% mineral oil 3.0% lecithin 88.0%
water
Treatment 5: 8% Mint Oil with 2% Potassium Salts of Fatty Acids
TABLE-US-00005 8% mint oil 4.04% Safer .RTM. Brand Insect Killing
Soap Concentrate 87.96% water
Treatment 6: 8% Mint Oil with 1% SLS and 2% Potassium Salts of
Fatty Acids
TABLE-US-00006 8% mint Oil 1% SLS 4.04% Safer .RTM. Brand Insect
Killing Soap Concentrate 86.96% water
Treatment 7: Victor Poison Free Wasp & Hornet Killer
TABLE-US-00007 [0063] 8% mint Oil 1% SLS 91% water
[0064] The test formulations were applied to the American
cockroach. Five replications were made for each test formulation,
with one replication consisting of one (1) adult American
cockroach. At the time of test initiation, one (1) American
cockroach was placed into the PVC pipe within the testing arena.
The cockroach was allowed to acclimate for approximately 1-2
minutes before being sprayed with the test formulation. The
cockroach was sprayed from a distance of approximately 12 inches.
Each cockroach was sprayed for 3 seconds within the PVC pipe. After
spraying, the PVC pipe was removed and the kill time was recorded
in seconds. The test was stopped when the insect was killed or 300
seconds had passed.
TABLE-US-00008 TABLE 1 Mean Kill Time in Seconds for American
Cockroaches Average Kill FORMULATION (% By. Wt) Time (seconds) 2%
potassium salts of fatty acids 179.6 2.0% potassium salts of fatty
acids + 265.8 4.0% mint oil 2.0% potassium salts of fatty acids +
300 4.0% mint oil + 3% lecithin 4% mint oil + 3% lecithin 252 2%
potassium salts of fatty acids + 253 8% mint oil 2% potassium salts
of fatty acids + 135 8% mint oil + 1% SLS 8% mint oil + 1% SLS
98.6
[0065] EXAMPLE 2. A study using the methodology of Example 1 was
performed using German cockroaches (Blatella germanica). Treatments
1, 2, and 3 consisted of aerosolized test material using carbon
dioxide as the propellant. Aerosol cans were filled at LHB
Industries (St. Louis, Mo.) per Woodstream specification. Treatment
4 was formulated in the Woodstream laboratory, placed into a
bottle, and dispensed using a hand pump trigger sprayer.
[0066] The experimental formulations were in the following
percentages of the admixed components by weight:
Treatment 1: Victor.RTM. Poison Free Ant and Roach Insect
Killer
TABLE-US-00009 [0067] 4.0% mint oil 5.0% mineral oil 3.0% lecithin
88.0% water
Treatment 2: 4.0% Mint Oil with 3.0% Lecithin and 2.0% Potassium
Salts of Fatty Acids
TABLE-US-00010 4.00% mint oil 5.00% mineral oil 3.00% lecithin
4.04% Safer Brand Insect Killing Soap Concentrate 83.96% water
Treatment 3: 4.0% Mint Oil with 2.0% Potassium Salts of Fatty
Acids
TABLE-US-00011 4.0% mint Oil 5.0% mineral Oil 4.04% Safer .RTM.
Insect Killing Soap Concentrate 86.96% water
Treatment 4: 2.0% Potassium Salts of Fatty Acids
TABLE-US-00012 [0068] 4.04% Safer .RTM. Brand Insect Killing Soap
Concentrate 95.96% water
TABLE-US-00013 TABLE 2 Mean Kill Time in Seconds for German
Cockroaches Average Kill FORMULATION (% By. Wt) Time (seconds) 4.0%
mint oil + 3.0% lecithin 35.72 2.0% potassium salts of fatty acids
+ 33.81 4.0% mint oil + 3.0% lecithin 2.0% potassium salts of fatty
acids + 24.82 4.0% mint oil 2.0% potassium salts of fatty acids
38.36
[0069] EXAMPLE 3. A range of concentrations of pyrethrins from
0.01% to 0.5% by weight can be combined with 0.25% to 8% by weight
of at least two essential oils such as mint and D-limonene or
palmarosa oil and thyme oil. The formulation will include an
anti-oxidant such as ethoxyquin, a tocopherol, or BHT to prevent
the pyrethrins from breaking down. As pyrethrins are not readily
water soluble, an alcohol may also be included, such as SD3A or
SDA3C or other denatured alcohols in the composition to help
solubilize the pyrethrins. Mineral oil or an equivalent substance
can also be used at a concentration of about 5% by weight to allow
the composition to remain on the surface for up to four weeks. The
balance is water.
[0070] EXAMPLE 4. In another embodiment, two concentrations of
insecticidal soap and pyrethrin are combined with several
concentrations of at least two essential oils. The essential oil
concentrations of the composition can range from 0.25% to 8.0% by
weight. The concentration of pyrethrin in the contemplated
composition is between about 0.01% to about 0.5% by weight as
pyrethrin in this range has been shown to be effective in previous
testing. As in Example 3, an anti-oxidant like ethoxyquin, a
tocopherol, or BHT will be required to prevent the pyrethrin from
breaking down. An alcohol may also be needed to solubilize. the
pyrethrin. The concentrations of soap in the contemplated
composition are 0.5% and 2.0% by weight. Carrier oil or an
equivalent substance can also be used at a concentration of up to
about 5% by weight to allow the composition to remain on the
surface for up to four weeks. The balance is water.
[0071] Example 5. Tests were performed to determine the
effectiveness of differing concentrations of mint oil with various
combinations of lecithin, pyrethrins, potassium salts of fatty
acids and SLS on the German Cockroach (Blatella germanica). The
testing area, the PVC pipe and insects were the same as in Example
1.
[0072] The formulations of certain test components were as follows:
[0073] Safer.RTM. Brand Insecticidal Soap Concentrate: Contains
49.52% potassium salts of fatty acids by weight, as described
above; and
[0074] Pyganic MUP 20 (McLaughlin Gormley King Company, Golden
Valley, Minn.): Contains 20% pyrethrins by weight.
[0075] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 1. Each formulation was
applied to the cockroaches. Fifteen replications were made for each
test formulation, with one adult male cockroach per replication. At
the time of test initiation, 5 cockroaches are placed in the PVC
pipe in the testing area. The cockroaches were allowed to acclimate
for about 1-2 minutes before the test began. The cockroaches are
then sprayed from a height of 12 inches into the pipe for about 3
seconds. The pipe is then removed and the kill time recorded in
seconds for each cockroach. This procedure was repeated three times
to obtain the fifteen replications.
[0076] The results of the experiments are also shown in FIG. 1. The
control and pyrethrins combined with lecithin or 1% SLS only
treatments were the least effective with kill times approaching
five minutes. The fastest kill times were observed when the mint
oil was combined with insecticidal soap and pyrethrins. Increasing
the mint oil concentration resulted in faster kill times. Based on
the results of this experiment, addition of pyrethrins to the
composition comprising mint oil and insecticidal soap resulted in a
synergistic effect, reducing kill times more than the combination
of the mint oil and insecticidal soap without pyrethrins.
[0077] Example 6. Tests were performed to determine the
effectiveness of differing concentrations of mint oil, D-limonene,
or palmarosa oil with various combinations of lecithin, pyrethrin,
potassium salts of fatty acids and SLS on the Carpenter Ant
(Camponotus pennsylvanicus). The testing area and the PVC pipe were
the same as in Example 1. The ants were obtained from Carolina
Biological Supply Company (Burlington, N.C.).
[0078] The formulations of the Safer.RTM. Brand Insecticidal Soap
Concentrate and Pyganic MUP 20 were as described previously.
[0079] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 2. Each formulation was
applied to the Carpenter Ants. Fifty replications were made for
each test formulation with one replication consisting of one ant.
At the time of test initiation, ten (10) ants were placed into the
PVC pipe in the testing area as described previously. The ants were
allowed to acclimate for 1-2 minutes before being sprayed with the
test formulation. The ants were sprayed from a distance of about 12
inches for about 3 seconds within the pipe. The pipe is then
removed and the kill time recorded in seconds for each ant. This
procedure was repeated five times to obtain the fifty
replications.
[0080] The results are also shown in FIG. 2. With the exception of
the control and essential oils alone, all treatments were effective
in killing the ants within five minutes. The fastest kill times
occurred when the ants were treated with lecithin and essential
oils, insecticidal soap and essential oils, and 1% SLS and
pyrethrins and essential oils. The combination of either lecithin
or insecticidal soap and essential oil resulted in a synergistic
effect, reducing kill times more than the combined effect of each
one separately. Addition of palmarosa oil reduced kill times more
efficaciously than the mint oil or D-limonene.
[0081] Example 7. Tests were performed to determine the
effectiveness of differing concentrations of eugenol with various
combinations of lecithin, pyrethrins, potassium salts of fatty
acids and SLS on the German Cockroach (Blatella germanica). Eugenol
is an aromatic chemical, fragrance and a spice that is derived from
clove oil and cinnamon leaf. It has a characteristic spicy odor of
clove. USP grade eugenol has uses in the food, dental and
pharmaceutical industries. Eugenol is widely used in dentistry, due
to its analgesic, antiseptic and balsamic qualities. The testing
area, PVC pipe, insects, and testing procedures were the same as in
Example 5. The formulations of Safer.RTM. Brand Insecticidal Soap
Concentrate and Pyganic MUP 20 were as described previously.
[0082] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 3. The controls and
treatments containing only pyrethrins combined with lecithin, or 1%
SLS, were least effective in killing the cockroaches. The fastest
kill times were observed when eugenol was combined with
insecticidal soap, and soap plus pyrethrins. Increasing the
concentration of eugenol decreased the kill times significantly.
The data show a synergistic effect on reducing kill times of
cockroaches when insecticidal soap at a concentration of either
0.5% or 2% by weight, is combined with eugenol at a concentration
of either 1% or 4% by weight. The synergism is also seen when
either is combined with 0.012% and 0.05% pyrethrins by weight.
[0083] Example 8. Tests were performed to determine the
effectiveness of differing concentrations of thyme oil with various
combinations of lecithin, pyrethrins, potassium salts of fatty
acids and SLS on the German Cockroach (Blatella germarrica). The
testing area, PVC pipe, insects and testing procedures were the.
same as in Example 5. The test formulations of Safer.RTM. Brand
Insecticidal Soap Concentrate and Pyganic MUP 20 were as described
previously.
[0084] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 4. The controls and
treatments containing only pyrethrins combined with lecithin or 1%
SLS were least effective in killing the cockroaches. The fastest
kill times were observed when thyme oil was combined with
insecticidal soap, or insecticidal soap plus pyrethrins. Increasing
the concentration of thyme oil decreased the kill times
significantly. The data show a synergistic effect on reducing kill
times of cockroaches when the highest concentration of thyme oil
(4% by weight), is combined with lecithin and pyrethrins, or when
thyme oil is combined either with insecticidal soap or with
insecticidal soap and pyrethrins.
[0085] Example 9. Tests were performed to determine the
effectiveness of differing concentrations of mint oil, D-Limonene
or palmarosa oil with various combinations of lecithin, pyrethrins,
potassium salts of fatty acids and SLS on the German Cockroach
(Blatella germanica). The testing area, PVC pipe, insects and
testing procedures were the same as in Example 5. The test
formulations of Safer.RTM. Brand Insecticidal Soap Concentrate and
Pyganic MUP 20 were as described previously.
[0086] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 5. As shown in FIG. 5,
most of the treatments were effective and resulted in kill times
under 2 minutes. Typically, the higher concentrations of essential
oils, by weight, resulted in reduced kill times, and palmarosa oil
was shown to produce the fastest kill times.
[0087] Based on the results set forth in FIG. 5, it can be shown
that synergy is occurring with the combination treatments of:
lecithin and essential oils; pyrethrins, lecithin and essential
oils; and pyrethrins, SLS and essential oils. The addition of mint
oil and palmarosa oil significantly improved the efficacy of
insecticidal soap. The addition of palmarosa oil significantly
improved the efficacy of pyrethrins and insecticidal soap. Other
combinations of essential oils and insecticidal soap, as well as
insecticidal soap with pyrethrins did not result in statistically
significant synergy.
[0088] Example 10. This experiment was performed to compare the
effectiveness of 0%, 0.25%, 1.0% and 4% by weight of mint Oil,
D-limonene, thyme oil, eugenol, cedar oil, cinnamon oil, neem oil,
and geraniol in combination with 0.012% pyrethrins and 1.0%
potassium salts of fatty acids; 0.05% pyrethrins and 1.0% potassium
salts of fatty acids; 0.05% pyrethrins and 2.0% potassium salts of
fatty acids on the Carpenter Ant (Camponotus pennsylvanicus). The
testing area, PVC pipe, insects and testing procedures were the
same as in Example 7. The test formulations of Safer.RTM. Brand
Insecticidal Soap Concentrate and Pyganic MUP 20 were as described
previously.
[0089] The various test formulations, with percentages by weight,
are set forth in the table comprising FIG. 6. As shown in FIG. 6,
the shortest killing times were observed with the test combinations
comprising the essential oils of D-limonene or geraniol. Killing
time was reduced as the concentrations by weight of insecticidal
soap and pyrethrins were increased. Killing time reduction was also
observed as the concentrations of essential oils were
increased.
[0090] Based on the results described in FIG. 6, it can be
concluded that synergies are occurring between the test
combinations of insecticidal soap, essential oils and
pyrethrins.
[0091] Example 11. This experiment was performed to compare the
effectiveness of 0% and 1.0% mint oil, D-limonene, geraniol, and
cinnamon oil in combination with 0.012% pyrethrins and 1.0%
potassium salts of fatty acids; 0.03% pyrethrins and 1.0% potassium
salts of fatty acids; 0.05% pyrethrins and 1.0% potassium salts of
fatty acids on the House Fly (Musca domestica).
[0092] House Fly pupae were obtained from Carolina Biological and
raised to adults in the Woodstream Laboratory. Screen Covered PVC
Pipe was used to calm and confine the flies prior to spraying.
[0093] The PVC pipe is covered with screen before introducing flies
to prevent escape. The testing area and test formulations of
Safer.RTM. Brand Insecticidal Soap Concentrate and Pyganic MUP 20
were as described previously.
[0094] The test formulations were applied to the flies. Fifteen
replications were made for each test formulation with one
replication consisting of (1) adult fly. At the time of test
initiation, (5) flies were placed into the screened PVC pipe within
the testing arena. The flies were allowed to acclimate
approximately 1-2 minutes before being sprayed with the test
formulation. The flies were sprayed from a distance of
approximately 12 inches for about 3 seconds within the PVC pipe.
After spraying, the PVC pipe was removed and the kill time recorded
in seconds for each fly. This procedure was repeated five times to
obtain the fifteen replications.
[0095] The various test formulations, with percentages by weight,
are set forth in Table 3. The application of the test formulations
immediately inhibited the flying ability of the test flies. The
shortest kill times were observed with the combinations using
D-Limonene or geraniol. Speed of kill was not increased as the
percent of pyrethrins was increased. Based on these data it can be
concluded that synergies are occurring between essential oils and
potassium salts of fatty acids combined with pyrethrins. There were
no significant differences in kill times with increased
concentrations of pyrethrins indicating that synergy would be
obtained with lower concentrations of pyrethrins with the same
amount of essential oils.
TABLE-US-00014 TABLE 3 Mean Kill Time in Seconds for House Flies.
0.012% 0.03% 0.05% Pyrethrin + Pyrethrin + Pyrethrin + Essential
Oil 1.0% Soap 1.0% Soap 1.0% Soap 0% Essential Oil 41.993 44.013
53.267 1% Mint Oil 34.653 35.04 32.48 1% D-Limonene 45.273 21.747
62.887 1% Geraniol 27.327 26.787 20.7 1% Cinnamon Oil 30.5 34.533
45.367
[0096] Experiment 12. The purpose of this experiment was to
determine the effectiveness of 0%, 0.25%, 1.0% and 4% of D-limonene
by weight in combination with various concentrations of lecithin,
potassium salts of fatty acids, SLS, and pyrethrins, on the German
Cockroach (Blatella germanica). The testing area, PVC pipe, insects
and test procedures were the same as in Example 5. The test
formulations of Safer.RTM. Brand Insecticidal Soap Concentrate and
Pyganic MUP 20 were as described previously.
[0097] The various test formulations, with percentages by weight
are set forth in FIG. 7. The results of the experiments show that
the water treatments, and treatment combinations containing only
pyrethrins combined with lecithin or SLS, were least effective,
with kill times approaching or exceeding 5 minutes. The fastest
kill times were observed when D-limonene was combined with either
insecticidal soap, or insecticidal soap and pyrethrins. As was
expected, increasing the concentration of D-limonene reduced the
killing times. Treatments of insecticidal soap and insecticidal
soap combined with pyrethrins, resulted in faster kill times for
the cockroaches, than treatments containing pyrethrins combined
with lecithin or SLS. These observed differences were consistent
even with the addition of D-limonene.
[0098] Essential oils of the present invention may be used in
combination with insecticidal soap and pyrethrins to create an
insecticidal composition that will result in a synergistic
reduction of killing times for various insects. For example, cedar
oil is expected to show synergistic results with similar levels of
sodium lauryl sulfate as discussed above at levels of cedar oil
from about 0.01 to 30%, with a preferred composition comprising
from about 0.5 to 10% cedar oil; for clove oil, the broad range
would be from about 0.01 to 30%, with a preferred range of from
about 1 to 20%; for garlic oil, the broad range would be from about
0.1 to 30%, with a preferred range of from about 1 to 20%; for
lemongrass oil, the broad range would be from about 0.01 to 20%,
with a preferred range of from about 0.5 to 5%; for linseed oil,
the broad range would be from about 0.01 to 30%, with a preferred
range of from about 1 to 20%; for rosemary oil, the broad range
would be from about 0.01 to 30%, with a preferred range of from
about 1 to 30%; for soybean oil the broad range would be from about
0.01 to 80%, with a preferred range of from about 1 to 30%; and for
thyme oil, the broad range would be from about 0.01 to 30%, with a
preferred range of from about 0.5 to 10%.
[0099] Having described the invention, many modifications thereto
will become apparent to those skilled in the art to which it
pertains without deviation from the spirit of the invention as
defined by the scope of the appended claims.
* * * * *