BED BUG CONTROL COMPOSITION AND PROCESS OF PREPARING THE SAME

Abstract

The present invention provides a bed bug control composition comprising an azadirachtin extracted from neem seed kernels with a minimum purity 40% but not limited to the same, mixture of plant extracts and additives. The present invention provides a composition comprising azadirachtin, geraniol oil, citronella oil, Cedar wood oil, clove oil, rosemary oil, thyme oil and others. The present invention further provides a process for preparation of bed bug composition.

Claims

1. A bed bug control composition comprising a azadirachtin extract present in an amount range from 0.1% 80% (w/w); a mixture of plant extracts present in an amount range from 1% to 90% (w/w); and additives present in an amount range from 0.1% to 90% (w/w).

2. The bed bug control composition as claimed in claim 1, wherein the azadirachtin extract has percentage purity in range from 1% to 97%.

3. The bed bug control composition as claimed in claim 2, wherein the azadirachtin extract has minimum percentage purity of 40%.

4. The bed bug control composition as claimed in claim 1, wherein the plant extract are selected from the group comprising of Cedar wood oil, Eucalyptus oil, Pepper mint oil, Eugenol, Rosemary oil, Cinnamon oil, Clove oil, Citronella oil, Geraniol, Garlic oil, Black pepper oil, Mint oil, Thyme oil, Basil oil, Camphor oil, Lemon grass oil, Henna oil, Cotton seed oil, Cedar leaf oil, Mustard oil, Corn oil, Marigold oil and combination thereof.

5. The bed bug control composition as claimed in claim 1, wherein the plant extract is a mixture of geraniol oil, citronella oil, Cedar wood oil, clove oil, rosemary oil and thyme oil.

6. The bed bug control composition as claimed in claim 5, wherein in the plant extract mixture, geraniol oil is present in an amount range from 1% to 90% (w/w).

7. The bed bug control composition as claimed in claim 5, wherein in the plant extract mixture, citronella oil is present in an amount range from 1% to 90% (w/w).

8. The bed bug control composition as claimed in claim 5, wherein in the plant extract mixture, Cedar wood oil is present in an amount range from 1% to 90% (w/w).

9. The bed bug control composition as claimed in claim 5, wherein in the plant extract mixture, clove oil is present in an amount range from 1% to 90% (w/w).

10. The bed bug control composition as claimed in claim 1, wherein in the additives comprises of solvent present in a range from 1% to 90% (w/w).

11. The bed bug control composition as claimed in claim 10, wherein in the solvent is butyl acetate or ethyl acetate.

12. The bed bug control composition as claimed in claim 1, wherein in the additives comprises of surfactants present in a range from 1 to 90% (w/w).

13. The bed bug control composition as claimed in claim 12, wherein in the surfactant is selected from the group comprising of ethoxylated alcohols, ethoxylated fatty esters, alkoxylated glycols, ethoxylated fatty acids, carboxylated alcohols, carboxylic acids, fatty acids, ethoxylated alkylphenols, fatty esters, sodium dodecylsulfide, other fatty acid-based surfactants, other natural or synthetic surfactants, or a combination thereof.

14. The bed bug control composition as claimed in claim 1, wherein in the additives comprises of emulsifiers present in an amount range from 2% to 80% (w/w).

15. The bed bug control composition as claimed in claim 14, wherein in the emulsifiers is selected from silicone based emulsifiers, non-silicone based emulsifier, Olive oil, Cashew oil, Castor oil, Sunflower oil, Pongamia oil, Sesame oil, Linseed oil, Rice Bran oil, Ground nut oil and other oils of plant and animal origin and combinations thereof

16. The bed bug control composition as claimed in claim 1, wherein the composition is formulated in form of Ready to Use (RTU) or Emulsified concentrate (EC).

17. A process for preparation of a bed bug control composition comprising the steps of: weighing an azadirachtin extracted from neem seed kernels with a minimum purity 40% but not limited to the same in a predetermined amount, weighing solvent in predetermined amount, adding solvent to an azadirachtin extracted from neem seed kernels with a minimum purity 40% but not limited to the same with continuous stirring at 250 rpm for 30 minutes, adding mixture of plant extract n a predetermined amount, adding surfactant and emulsifier with continuous stirring for 60 minutes.

18. The process as claimed in claim 17, wherein stirring is carried out at ambient temperature and pressure.

Description

DESCRIPTION OF THE INVENTION

[0027] The present invention provides a novel, stable and bio-efficacious bed bug control composition. The novel composition of the present invention comprises combination of azadirachtin and plant extracts but not limited to Geraniol, Citronella oil, Cedar wood oil, Clove oil along with other additives.

[0028] It is to be noted, as used in the specification and claims, the singular forms “a”, “an”, and “the” include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to a composition containing “a compound includes a mixture of two or more compounds. It should also be noted that the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise. The expression of various quantities in the terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total composition unless otherwise specified.

[0029] The phrase “controlling bedbug” as used in the present invention includes killing of the bed bug or its offspring; killing of larval stages of the bed bug, killing of the bed bug's eggs, starving the bed bug, suffocating the bed bug, reducing the number of the bed bugs present at the target site, preventing settlement of the bed bug at the target site, rendering the bed bug inactive, or knockdown of the bed bug.

[0030] As used herein, “knockdown” activity refers to the pesticidal activity of a composition as applied directly to a bed bug.

[0031] As used herein, the term “effective amount” regarding a composition to control pest refers to that dosage of active substance sufficient to exert the desired activity.

[0032] A pest is an animal that is detrimental to humans or human affairs, or that annoys a person. Pests include all insects and spiders. The term “pest” includes organisms belonging to Arthropods, in particular Chelicerata, Tracheata, but not Crustacea. In the present invention the target pest is Cimex lectularius or Cimex hemipterus for which the composition is formulated.

[0033] As used herein, “surface” or “target surface” includes a surface to which a bed bug control composition is applied or is to be applied. Such surfaces may include, for example, a surface where bed bugs are likely to contact or otherwise be exposed to the applied bed bug control composition, to lay their eggs, and/or a surface that has been or is suspected to be infested by bed bugs.

[0034] As used herein, the term “stability” means the ability of a composition to retain its bed bug killing activity after application to a surface to be treated with bed bug control composition.

[0035] Neem (Azadirachta indica), is a tropical evergreen tree. Neem oil is derived from the fruits and seeds of a neem tree. Methods for obtaining neem oil, azadirachtin extract or other derivatives purified from neem oil are known in the art. One exemplary method for obtaining neem oil is cold pressing. The most important active constituent in neem oil is azadirachtin and the others are nimbolinin, nimbin, nimbidin, nimbidol, sodium nimbinate, gedunin, salannin, and quercetin. Azadirachtin is a chemical compound belonging to the limonoid group. The azadirachtin is a secondary metabolite present in the Neem seeds. The azadirachtin is a highly oxidized tetranortriterpenoid which boasts a plethora of oxygen functionality, comprising an enol ether, acetal, hemiacetal and tetra-substituted oxirane as well as a variety of carboxylic esters. The azadirachtin in the present invention is obtained from the seed kernels of the Neem Tree (Azadirachta indica).

[0036] An azadirachtin extracted from neem seed kernels have purity in a range of 1% to 97%, preferably a minimum purity 40%. Azadirachtin extract contributes to multiple possible modes of action, such as repellent, insect killer. Azadirachtin with the help of suitable surfactants and solvents can penetrate the cuticle of the bed bug, translocate in its body and kill the bed bug. Azadirachtin is regarded as nontoxic to mammals, to the environment, and UV or heat promotes its degradation. Neem oil and its derivatives for e.g. Azadirachtin contributes to controlling pests including insects, mites, ticks, and nematodes also by affecting the pest's behavior and physiology. In contrast, neem products are non-toxic to higher animals and most beneficial insects. The range of azadirachtin in the present invention is 0.1% to 80.0% (w/w) of the bed bug killing composition.

[0037] Plant extracts are volatile oils and natural products. Plant extracts have been known for centuries in many cases and even millennia, and this term is well known in the art. Plant extracts are available commercially. A plant extract carries a distinctive odor, scent, or essence, of the plant; therefore, plant extracts convey characteristic fragrances. A botanical source is odorous if an odor can be detected by any animal, or pest not just a human; “odorous” thus is simply an indication that some volatile component is present in the plant. Because of their hydrophobic nature, plant extracts are not readily miscible in water. In the present invention the plant extracts may be any plant extracts but not limited to Cedar wood oil, Clove oil, Citronella oil, Geraniol, Eucalyptus oil, Pepper mint oil, Eugenol, Rosemary oil, Cinnamon oil, Garlic oil, Black pepper oil, Mint oil, Thyme oil, Basil oil, Camphor oil, Lemon grass oil, Henna oil, Cotton seed oil, Cedar leaf oil, Mustard oil, Corn oil, Marigold oil or any combination thereof. Preferably, the plant extract used in the present invention are geraniol oil, citronella oil, clove oil, cedar wood oil, rosemary oil, thyme oil, and others. The plant extract in the present invention provides synergistic effect with the main active ingredient azadirachtin in the composition. The range of the plant extracts is between 1% to 90% (w/w) of the bed bug killing composition.

[0038] In an embodiment of the present invention, a plant extract is a predominately volatile material or materials isolated by some physical (as opposed to chemical) process from an odorous, single-species, botanical source. The oils extracted by the physical process can contain some non-volatile material. A most widely used process for the isolation of plant extract is steam distillation of plant matter, although dry distillation, supercritical fluid extraction, and solvent extraction are also used.

[0039] The term “solvent” as used herein refers to an aromatic or aliphatic solvent, with which an active ingredient can be mixed or formulated to facilitate its application, storage, transport, and/or handling, or improve various product characteristics such as its odor. Commonly used solvent include, but are not limited to, Tert-Amyl alcohol, Benzyl alcohol, 1,4-Butanediol, 1,2,4-Butanetriol, Butanol, 2-Butanol, N-Butanol, Tert-Butyl alcohol, Di(propylene glycol) methyl ether, Diethylene glycol, Ethanol, Ethylene glycol, 2-Ethylhexanol, Furfuryl alcohol, Glycerol, Isobutanol, Isopropyl alcohol, Methanol, 2-(2-Methoxyethoxy)ethanol, 2-Methyl-1-butanol, 2-Methyl-1-pentanol, 3-Methyl-2-butanol, Neopentyl alcohol, 2-Pentanol, 1,3-Propanediol, 1-Propanol, Propylene glycol, Propylene glycol methyl ether, Benzyl benzoate, Bis(2-ethylhexyl) adipate, Bis(2-ethylhexyl) phthalate, 2-Butoxyethanol acetate, Butyl acetate, Sec-Butyl acetate, Tert-Butyl acetate, Diethyl carbonate, Dimethyl adipate, Dioctyl terephthalate, Ethyl acetate, Ethyl acetoacetate, Ethyl butyrate, Ethyl lactate, Ethylene carbonate, Hexyl acetate, Isoamyl acetate, Isobutyl acetate, Isopropyl acetate, Methyl acetate, Methyl lactate, Methyl phenylacetate, Methyl propionate, Propyl acetate, Propylene carbonate, Triacetin, methyl acetate, tert-butyl acetate, dimethyl carbonate, propylene carbonate, propylene glycol monomethyl ether, propylene glycol monopropyl ether, dipropylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monobutyl ether, propylene glycol, dipropylene glycol, propylene carbonate, ethylene glycol monomethyl ether, diethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, cyclohexane, cycloheptane, methyl cyclohexane, 1,4-dimethyl cyclohexane, benzene, amyl benzene, secondary butyl benzene, toluene, o-ethyl toluene, o-xylene, 4-ethyl-o-xylene, m-xylene, p-xylene, 2-ethyl-p-xylene. Butyl acetate is an organic compound with a molecular formula of C.sub.6H.sub.12O.sub.2 which occurs naturally in food products. It is a colorless liquid with a low viscosity, having a sweet banana-like odor. This liquid is volatile but flammable in nature. Ethyl acetate is an effective poison for use in insect collector as its vapours are a respiratory tract irritant whose vapours can kill the insect quickly without destroying it. Preferably, the solvent used is butyl acetate and ethyl acetate. The range of the solvent is between 1% to 90% (w/w) of the bed bug killing composition.

[0040] The term “surfactant” as used herein refers to compounds which rupture the insect cuticle and allows active ingredient in the composition to penetrate & translocate within insect body leading to death of bed bugs. The surfactants used herein include, but are not limited to Tween-85, Tween-20, Tween-80, Polyethylene glycol, Tween-60, Polysorbate, Span-80, Span-60, Trilaurin, Triolein, Span 20, Sorbitan trioleate, Isopropyl myristate, poly acrylate, ethoxylated alcohols, ethoxylated fatty esters, alkoxylated glycols, ethoxylated fatty acids, carboxylated alcohols, carboxylic acids, fatty acids, ethoxylated alkylphenols, fatty esters, sodium dodecylsulfide, other fatty acid-based surfactants, other natural or synthetic surfactants, or a combination thereof and combinations thereof. Preferably the surfactant used is ethoxylated castor oil or Tween 85. The surfactant is used in the range of 1 to 90% (w/w) of the bed bug killing composition.

[0041] The term “emulsifier” as used herein refers to compounds that stabilizes the composition of the present invention. The emulsifiers used herein include, but are not limited to silicone based emulsifiers, non-silicone based emulsifier, Olive oil, Cashew oil, Castor oil, Sunflower oil, Pongamia oil, Sesame oil, Linseed oil, Rice Bran oil, Ground nut oil and other oils of plant and animal origin and combinations thereof. The oils can be in any of their chemical forms. Preferably the emulsifier used is silicone oil. The emulsifier is used in the range of 2% to 80% (w/w) of the bed bug killing composition.

[0042] The composition of the present invention can be used as ready to use (RTU) and also can be used as emulsified concentrate (EC) formulation by dissolving in required quantity of water and sprayed on desired location. The formulation can also be used in an aerosol form. The formulation is prepared as emulsifiable concentrate or aerosol by using processes known in state of the art.

[0043] A method for controlling bed bugs, or bed bugs infestation insects in a target area comprise the step of identifying a target area suspected of having bed bugs, followed by treating the target area by applying an effective amount of bed bug control composition effective to control or kill the bed bugs, to the target area, and monitoring the effectiveness of the treatment by said methods at a regular or pre-determined time interval.

[0044] Application of the composition of the present invention results in death of bed bugs with low to no toxic effect to humans, animals, or environment. One benefit of the present application is a cost-effective alternative to synthetic chemicals, heat, cold, tenting, etc. When the composition is applied so that direct contact with the bed bug occurs, the bed bug cannot survive; such contact kill composition provides fast relief.

[0045] The following examples illustrate, but in no way are intended to limit the present invention.

Example 1: Process for Formulating Different Formulations

[0046] The primary active ingredient azadirachtin extracted from neem seed kernels with a minimum purity 40% but not limited to the same is weighed in predetermined amount as given in Table 1 and is taken in a vessel. The pre-determined amount of solvent is added slowly with a continuous stirring at 250 rpm for 30 min. To this solution other plant extracts like geraniol oil, clove oil, citronella oil, cedar wood oil, thyme oil, rosemary oil and others are added in the ranges as given in Table 1 with constant stirring at 250 rpm for 30 min. Further, surfactant and emulsifier is added to the reaction mixture with continued stirring for another 60 min to obtain a final formulation. The mixing is carried out at ambient temperature and pressure. Various examples of combinations of different plant extracts in combination with azadirachtin and other additives for the control of Bed bugs are provided in Table 1.

TABLE-US-00001 TABLE 1 Different formulations of bed bug control composition Cedar Azadirachtin Citronellla wood Clove (40% Purity) Geraniol Oil oil Oil Emulsifier Surfactant Solvent Formulation (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) 1 0.1 1 1 1 1 2 1.sup.#   92.9* 2 80 1 1 1 1 2 1.sup.# 13* 3 80 2 1 1 1 2 1.sup.# 12* 4 0.33 90 1 1 1 2 1.sup.#    3.67** 5 0.33 1 1 1 1 80 1.sup.#   14.67* 6 0.33 1 1 1 1 1 90.sup.#     4.67** 7 0.33 1 3 2 1 1 .sup. 1.sup.##    90.67** *Butyl acetate; ** Ethyl acetate .sup.#Ethoxylated Castor oil; .sup.##Tween 85 Azadirachtin Citronellla Plant Paraffin (40% Purity) Geraniol Oil Extract oil Emulsifier Surfactant Solvent Formulation (% w/w) (% w/w) (% w/w) (% w/w) (carrier) (% w/w) (% w/w) (% w/w) 8 0.33 8 2 5.sup.$ 2 5 6.sup.# 71.67* 9 0.33 8 2 5.sup.$ 2 5 5.sup.# 72.67* 11 0.33 8 2 .sup. 5.sup.$$ 3 5 3.sup.# 73.67* *Butyl acetate .sup.#Castrox100 .sup.$Eugenol; .sup.$$Clove oil Azadirachtin Peppermint Paraffin (40% Purity) Geraniol Oil Eugenol oil Emulsifier Surfactant Solvent Formulation (% w/w) (% w/w) (% w/w) (% w/w) (carrier) (% w/w) (% w/w) (% w/w) 12 0.33 8 2 5 3 5 0 76.67* *Butyl acetate Azadirachtin Citronella Clove Plant Paraffin (40% Purity) Geraniol Oil Oil Extract Oil Emulsifier Surfactant Solvent Formulation (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) (% w/w) 10 0.33 8 2 3.sup.$  2.sup.@ 0 7 3.sup.# 74.67* 13 0.33 8 2 3.sup.$$ .sup. 2.sup.@@ 3 7 3.sup.# 71.67* 14 0.33 8 2 3.sup.$$   2.sup.@@@ 0 7 3.sup.# 74.67* .sup.@Rosemary oil; .sup.@@Thyme oil; .sup.@@@Cedar wood oil .sup.#Castrox-100 *Butyl acetate .sup.$Eugenol; .sup.$$Clove oil

Example 2: Shelf Life of Bed Bug Killing Formulations

[0047] The formulations from example 1 were analysed for stability through accelerated stability study at 54° C. and 50% RH. The result of the stability study is tabulated in Table 2. The stability study is known as accelerated stability study as it is not done in real time but conducted at 54° C. and 50% RH. The prepared formulations are transferred into glass vials and placed inside a stability chamber to analyse the degradation of the active material. Generally for azadirachtin, 7 days of accelerated stability study is equivalent to 6 months in real time stability.

TABLE-US-00002 TABLE 2 Shelf life stability of the bed bug control formulations Accelerated stability details % of Azadirachtin Formulation Shelf life degradation @35.sup.th S. No. details achieved day 1 Formulation 8 2 years 9.17 2 Formulation 9 2 years 8.80 3 Formulation 10 2 years 8.76 4 Formulation 11 2 years 8.90 5 Formulation 12 2 years 8.97 6 Formulation 13 2 years 9.21 7 Formulation 14 2 years 9.07

[0048] It was observed that all the formulations were stable for a shelf life period of 1 year to 2 years.

Example 3: Method for Determining the Synergy of the Bed Bug Control Composition

[0049] The indicative bio-efficacy studies were carried out as per CIB&RC norms (Central insecticides Board and Registration Committee). In the experiment bed bug control formulations are sprayed in different doses to different test surfaces like wood, glass, cement, tiles and mud using Potter tower. After spraying the different test surfaces are kept for air drying for 24 hour prior to screening test. Adult bed bugs of randomly mixed sex and age were transferred from rearing jars into test surfaces for the study. In the present study 10 adult bed bugs were transferred on to the test surfaces. Experiment was conducted in triplicate and cumulative knock down was counted at every 5 minutes intervals up to 30 minutes. Then the bed bugs were collected and placed in a recovery jar, observed for 24 hours mortality and results were expressed in percentage of mortality. In control, the test surfaces are sprayed with distilled water. The indicative bio-efficacy study is carried out on the 14 bed bug control formulations as prepared in example 1. The formulations were applied at 1 ml/sq. ft. dose on two different surfaces such as Tiles and Glass.

TABLE-US-00003 TABLE 3 Bed bug bio-efficacy results for developed formulation Bio-efficacy results of Bed bug control formulation Mortality % Formulation description Dose (ml/sq ft) Tiles Glass Formulation 1 1 12 15 Formulation 2 1 20 32 Formulation 3 1 14 16 Formulation 4 1 30 15 Formulation 5 1 19 22 Formulation 6 1 15 35 Formulation 7 1 17 19 Formulation 8 1 18 33 Formulation 9 1 27 20 Formulation 10 1 23 20 Formulation 11 1 33 30 Formulation 12 1 23 13 Formulation 13 1 27 20 Formulation 14 1 37 30

[0050] Based on the indicative bio-efficacy data in Table 3, the two best formulations (Formulation 8 and 14) were shortlisted for further bio-efficacy test. The Formulation 8 and 14 were tested at four different doses of 8, 10, 14 and 16 ml/sq. ft. on five different surfaces such as Tiles, Glass, Wood, Cement and Mud. The same procedure as described above was repeated for determining the bio-efficacy of the two compositions. It was observed that Formulation 14 is more effective than Formulation 8, at 8 ml/sq. ft. and 10 ml/sq. ft. dose produced 100% mortality on Tiles and Glass surfaces and 86.6% mortality on wood surface, Formulation 14 was also effective on cement and mud surfaces at 10 ml/sq. ft. dose respectively. Doses at 14 and 16 ml/sq. ft. of Formulation 14 on mud surface produced 70% and 90% mortality respectively. The bio-efficacy data of the two formulations is given in Table 4.

TABLE-US-00004 TABLE 4 Bed bug bio-efficacy results for developed formulation Bio-efficacy results of Bed bug control formulation Dose Formulation (ml/sq. Mortality % on various surfaces description ft.) Tiles Glass Wood Cement Mud Formulation 8 96.67 100 10 0 0 8 10 100 100 10 0 0 14 60 16 86.67 Formulation 8 100 100 23.33 13.33 0 14 10 100 100 86.67 73.33 43.33 14 70 16 90 80 90

Example 4: Method of Using the Bed Bug Control Formulation

[0051] A person desirous of getting a target surface rid of bed bugs may spray the composition of the present invention on different target surfaces where bedbugs can be found such as wood, fabric made of any material, curtain, floors, bed, cement tiles etc. Alternatively, the person can also apply the composition by using a cotton material soaked with the formulation, which is then used to wipe any surface to have activity against bedbugs. The composition can also be applied by fogging at the target area. The person may inspect the target area for signs of hatched pests 5 to 10 days after applying the bed bug control composition; and reapplying the bed bug control composition if signs of hatched bed bugs are observed.

[0052] All of the compositions and/or methods disclosed and claimed herein can be made and executed without undue experimentation in light of the present disclosure. While the compositions and methods of this invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations may be applied to the compositions and/or methods and in the steps or in the sequence of steps of the method described herein without departing from the concept, spirit and scope of the invention. All such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and concept of the invention as defined by the appended claims.