Composition for repelling and killing ticks as well as preparation method and application of composition

Abstract

The invention provides a tick repelling and killing composition as well as a preparation method and application thereof. The composition for repelling and killing ticks disclosed by the invention comprises plant essential oil and deet, the tick repelling and contact killing composition contains the plant essential oil component, the plant essential oil and the DEET are mixed for use, a good synergistic interaction effect is achieved, and the contact killing effect is increased on the basis of the repelling effect of the DEET. The composition for repelling the contact ticks is long in repelling time and good in safety, and the toxicity of DEET is reduced. The plant essential oil capable of effectively repelling and killing ticks in a contact mode is screened and mixed with DEET, the content of DEET in the tick repelling and killing composition is reduced, the repelling effect is equivalent, meanwhile, the toxic effect caused by DEET is reduced, and the tick killing effect is improved; the tick repelling and contact killing composition is long in repelling time effect and good in contact killing effect, can replace existing organic insect repelling and insecticide, and solves the problem of drug resistance of ticks.

Description

Technical Field

[0001] The invention relates to the technical field of pest control, and in particular to a tick repellent and contact killing composition, and a preparation method and application thereof. Background Art

[0002] Ticks belong to the phylum Arthropoda, class Arachnida, subclass Acari, order Parasiticus, order Ixodida, superfamily Ixodida, commonly known as grass crawlers, parasitize mammals, birds and reptiles and suck blood from their bodies. Ticks have four stages: egg-larva-nymph-adult, and they need to suck blood at each stage from larva to adult. When ticks bite, they secrete a toxin from their mouthparts, which makes the bitten host insensitive and difficult to detect. Tick bites can cause tick paralysis and the spread of tick-borne diseases. Ticks are known to carry 83 viruses, 4 bacteria, 17 spirochetes, and 32 protozoa worldwide, with a mortality rate of up to 30%.

[0003] Currently, ticks are mostly repelled with organic synthetic insect repellents and insecticides, such as repellents containing 20% ​​DEET, which can be applied to the skin and clothing to prevent tick bites. The pyrethroid insecticide cypermethrin is neurotoxic to insects and is safe for humans and animals. However, with the long-term use of chemical preparations, ticks may develop resistance to them, weakening the repellent and contact killing effects. DEET has no contact killing effect on ticks, and it is currently believed that DEET has a certain toxicity. It is not recommended for children under 6 months old and pregnant women to use DEET.

[0004] Based on the defects of current DEET repellents, it is necessary to improve them. Summary of the invention

[0005] In view of this, the present invention proposes a tick repellent and contact killing composition and a preparation method and application thereof, so as to solve or partially solve the problems existing in the prior art.

[0006] In a first aspect, the present invention provides a tick repellent and contact killing composition, comprising plant essential oil and DEET; the plant essential oil is walnut leaf essential oil.

[0007] Preferably, the DEET is a DEET ethanol solution with a mass concentration of 20 to 25%.

[0008] Preferably, the mass ratio of the plant essential oil to DEET is (1-6):(1-2).

[0009] Preferably, the walnut leaf essential oil comprises the following components by mass fraction: phytol 11.66%, beta-eucalyptol 7.05%, diisobutyl phthalate 6.76%, dibutyl phthalate 6.63%, alpha-eucalyptol 6.53%, phyton 5.18%, guaiacol acetate 4.57%, 2-(6,10-dimethyl-2-spiro[4.5]dodecan-9-enyl)propane-2-ol 4.05%, myrtenol 3.05%, (-)-chrysanthemum Ester D 2.98%, 6,6-dimethyl-2-methylenebicyclo[3.1.1]-3-heptanol 2.97%, oleanolic acid 2.81%, farnesyl acetone 2.73%, (E)-β-farnesene 2.69%, eucalyptol 2.68%, methyl palmitate 2.4%, eugenol 2.28%, acetophenone 2.11%, 3,5-di-tert-butyl-4-hydroxybenzaldehyde 2.04%, methyl linolenate 1.61%, Δ-cadinene 1.57%, β-violet 1.38% methyl ketone, 1.25% mabehenone, 1.24% 2-(4-methyl-2,4-cyclohexadien-1-yl)-2-propane, 1.03% ethyl palmitate, 0.96% verbenol, 0.95% 3,5-di-tert-butylphenol, 0.86% nerolidol, 0.86% 2-isopropyl-2-methyloxirane, 0.76% β-ylanene, 0.7% methyl linoleate, 0.68% carvampinone, 0.68% 9-eicosine, (1R,5 S)-carveol 0.65%, α-molle alcohol 0.63%, 3,7,11,15-tetramethylhexen-1-ol 0.52%, 2-phenyl-2-propanol 0.48%, (+)-α-terpineol 0.44%, (S)-cis-verbenol 0.38%, neryl acetone 0.34%, β-butene 0.34%, carvone 0.22%, 5-isopropylbicyclo[3.1.0]hexane-2-one 0.17%, 4-terpenol 0.13%.

[0010] In a second aspect, the present invention further provides a method for preparing the tick repellent and contact killing composition, comprising the following steps:

[0011] The plant essential oil and DEET are mixed and then added into ethanol to obtain a tick repellent and contact killing composition.

[0012] Preferably, the plant essential oil and DEET are mixed and then added to ethanol with a volume concentration of 70-80% to obtain a tick repellent and contact killing composition, wherein the sum of the mass concentrations of the plant essential oil and DEET is 1-10%.

[0013] Preferably, the ethanol contains Tween-80 at a volume concentration of 0.1 to 0.2%.

[0014] In a third aspect, the present invention further provides a use of the aforementioned tick repellent and contact killing composition or the tick repellent and contact killing composition prepared by the aforementioned preparation method in the preparation of a tick repellent and contact killing drug.

[0015] Preferably, the dosage form of the tick repellent and contact killing composition is a spray or a pour-on.

[0016] Preferably, the application object is livestock or pets.

[0017] The tick repellent and contact killing composition of the present invention and its preparation method and application have the following beneficial effects compared with the prior art:

[0018] The repellent and contact-killing tick composition of the present invention contains a plant essential oil component. The mixed use of the plant essential oil and DEET has a good synergistic effect, and the contact-killing effect is increased on the basis of the repellent effect of DEET. The repellent and contact-killing tick composition of the present invention has a long repelling time, good safety, and reduced toxicity of DEET. The present invention screens plant essential oils that effectively repel and contact-kill ticks and mixes them with DEET, reduces the DEET content in the repellent and contact-killing tick composition, reduces the toxic effects brought by DEET while having a comparable repelling effect, and increases the contact-killing tick effect; the repellent and contact-killing tick composition of the present invention has a long repelling time and good contact-killing effect, can replace existing organic repellents and insecticides, and solves the problem of tick resistance. DETAILED DESCRIPTION

[0019] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] It should be noted that the order of description of the following embodiments is not intended to limit the preferred order of the embodiments. In addition, in the description of the present application, the term "including" means "including but not limited to". Various embodiments of the present invention may be in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be understood as a rigid limitation on the scope of the present invention; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the numbered ranges, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated in this article, it is meant to include any cited numbers (fractions or integers) within the indicated range.

[0021] The embodiment of the present application provides a tick repellent and contact killing composition, comprising plant essential oil and DEET; the plant essential oil is walnut leaf essential oil.

[0022] In some embodiments, the DEET is a DEET ethanol solution with a mass concentration of 20-25%.

[0023] In some embodiments, the mass ratio of plant essential oil to DEET is (1-6):(1-2).

[0024] In some embodiments, walnut leaf essential oil includes the following components by mass fraction: phytol 11.66%, beta-eucalyptol 7.05%, diisobutyl phthalate 6.76%, dibutyl phthalate 6.63%, alpha-eucalyptol 6.53%, phyton 5.18%, guaiacol acetate 4.57%, 2-(6,10-dimethyl-2-spiro[4.5]dodecan-9-enyl)propane-2-ol 4.05%, myrtenol 3.05%, (-) -Permethrin D 2.98%, 6,6-dimethyl-2-methylenebicyclo[3.1.1]-3-heptanol 2.97%, oleanolic acid 2.81%, farnesyl acetone 2.73%, (E)-β-farnesene 2.69%, eucalyptol 2.68%, methyl palmitate 2.4%, eugenol 2.28%, acetophenone 2.11%, 3,5-di-tert-butyl-4-hydroxybenzaldehyde 2.04%, methyl linolenate 1.61%, Δ-cadinene 1.57%, β-violet 1.38% of lanone, 1.25% of mabehenone, 1.24% of 2-(4-methyl-2,4-cyclohexadien-1-yl)-2-propane, 1.03% of ethyl palmitate, 0.96% of verbenol, 0.95% of 3,5-di-tert-butylphenol, 0.86% of nerolidol, 0.86% of 2-isopropyl-2-methyloxirane, 0.76% of β-ylanene, 0.7% of methyl linoleate, 0.68% of carvone, 0.68% of 9-eicosine, (1R, 5S)-carveol 0.65%, α-molle alcohol 0.63%, 3,7,11,15-tetramethylhexen-1-ol 0.52%, 2-phenyl-2-propanol 0.48%, (+)-α-terpineol 0.44%, (S)-cis-verbenol 0.38%, neryl acetone 0.34%, β-butene 0.34%, carvone 0.22%, 5-isopropylbicyclo[3.1.0]hexane-2-one 0.17%, 4-terpenol 0.13%.

[0025] The walnut leaf essential oil of the present invention is extracted from walnut (Juglan regiaL.) leaves by using CO2 supercritical extraction method (SFE-CO2) to obtain essential oil, and the essential oil can be used to prevent ticks, and the problems of drug residues and the generation of tick resistance when using chemical drugs can be effectively avoided; the repellent and contact-killing tick composition of the present invention contains plant essential oil components, and the mixed use of plant essential oil and DEET has a good synergistic effect, and the contact-killing effect is increased on the basis of the repellent effect of DEET. The repellent and contact-killing tick composition of the present invention has a long repellent time and good safety, and reduces the toxicity of DEET. The present invention screens plant essential oils that effectively repel and contact-kill ticks and mixes them with DEET, reduces the DEET content in the repellent and contact-killing tick composition, reduces the toxic effect caused by DEET while having a comparable repellent effect, and increases the contact-killing tick effect.

[0026] Based on the same inventive concept, the present invention also provides a method for preparing the above-mentioned tick repellent and contact killing composition, comprising the following steps:

[0027] The plant essential oil and DEET are mixed and then added into ethanol to obtain a tick repellent and contact killing composition.

[0028] In some embodiments, plant essential oil and DEET are mixed and added to ethanol with a volume concentration of 70-80% to obtain a tick repellent and contact killing composition, and the sum of the mass concentrations of the plant essential oil and DEET is 1-10%.

[0029] In some embodiments, ethanol contains Tween-80 at a volume concentration of 1-2%.

[0030] Based on the same inventive concept, the present invention also provides a use of the above-mentioned repellent and contact tick-killing composition or the repellent and contact tick-killing composition prepared by the preparation method in the preparation of a repellent and contact tick-killing drug.

[0031] In some embodiments, the composition for repelling contact ticks is in the form of a spray or a pour-on.

[0032] In some embodiments, the application object of the tick repellent and contact killing composition is livestock or pets.

[0033] The following further illustrates the repellent and contact tick killing composition of the present invention and its preparation method and application with specific examples. This section further illustrates the content of the present invention in conjunction with specific examples, but should not be construed as limiting the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.

[0034] Example 1

[0035] The embodiment of the present application provides a walnut leaf essential oil, which is obtained by CO2 supercritical extraction, the chemical components in the essential oil are detected by HPLC-GC-MS, and the content of each component in the essential oil is calculated using the peak area normalization method. The main volatile components are shown in Table 1.

[0036] Table 1 - Walnut leaf essential oil components

[0037]

[0038]

[0039] Example 2

[0040] This embodiment provides a method for preparing a composition for repelling and killing ticks, comprising the following steps:

[0041] S1, preparing a solution with a mass concentration of 20% of DEET with anhydrous ethanol to obtain a 20% DEET solution for standby use;

[0042] S2. The walnut leaf essential oil in Example 1 is mixed with 5 mL of the 20% DEET solution in S1 at mass ratios of 6:1, 4:1, 2:1, 1:1, and 1:2 to prepare a 20% DEET+relative proportion essential oil composition for repelling and killing ticks, which is set aside.

[0043] A tick repellent and contact killing experiment was conducted using the tick repellent and contact killing composition prepared in Example 2 and using walnut leaf essential oil, a DEET solution with a mass concentration of 20%, and anhydrous ethanol as a comparative example.

[0044] Specifically, the tick repellent test method is as follows:

[0045] Combined with the characteristics of ticks climbing upward, the "Y"-shaped olfactometer was used to measure the repellent effect of essential oils on adult ticks. Take 20 (half male and half female) Turan fanhead ticks (Rhipicephalus turanicus) and put them into a tube with the same diameter as the bottom of the "Y"-shaped tube, connect it to the bottom of the Y-shaped tube and seal it. Add 15 μL of the repellent contact killing tick composition in different proportions in Example 2 or an equal volume of anhydrous ethanol, walnut leaf essential oil, and a 1 cm diameter circular filter paper with a mass concentration of 20% DEET solution to the left and right upper ends of the Y-shaped tube, respectively, and leave the other end untreated. Place both hands at the tube mouths at both ends to attract ticks. The test results are shown in Table 2.

[0046] Table 2 - Tick repellency test results

[0047]

[0048] From the data in Table 2, it can be seen that the repellent and contact-killing tick composition of the present invention can achieve an effective protection time of up to 1.5 hours, and the time when the first tick crawls out of the treatment group is taken as the repellent time. From the above results, it can be seen that walnut leaf essential oil has a good repellent effect on adult Rhipicephalus turanica; when the essential oil is mixed with DEET, a synergistic effect occurs, and the repellent effect after mixing at a mass ratio of 1:1 is the best, which can reach 89.33 minutes.

[0049] Tick ​​contact test

[0050] The in vitro immersion method (Adult immersion test, AIT) was adopted. Ten hungry adult ticks were taken with tweezers and placed in a 5 mL EP tube. 1 mL of each repellent and contact tick-killing composition with different proportions in Example 2 was taken and injected into different tubes respectively using walnut leaf essential oil, a DEET solution with a mass concentration of 20%, and anhydrous ethanol. The ticks were immersed in each solution. After the experiment for 5 minutes, the ticks were removed and placed on filter paper. After the drug solution on the body surface was completely wiped off, the ticks were placed in a clean test tube and placed in an incubator (27±1°C, RH≥80%) for 24 hours. The number of dead ticks was counted. The results are shown in Table 3.

[0051] Table 3 - Tick contact test results

[0052]

[0053] From the above results, it can be seen that walnut leaf essential oil has a significant contact killing effect on adult Turanian Rhipicephalus ticks; when essential oil is mixed with DEET, the higher the proportion of walnut leaf essential oil, the stronger the contact killing effect on Turanian Rhipicephalus ticks, which increases the killing effect while DEET repels ticks.

[0054] Example 3

[0055] This embodiment provides a method for preparing a composition for repelling and killing ticks, comprising the following steps:

[0056] S1. The walnut leaf essential oil in Example 1 and 20% DEET (i.e., a DEET ethanol solution with a mass concentration of 20%) are mixed in a volume ratio of 1:1 to obtain a mixed solution; the mixed solution is dissolved in an ethanol solution with a volume concentration of 70%, and diluted to prepare a repellent and contact tick-killing composition with a mixed solution volume concentration of 1 to 5% (specifically, the volume concentrations are 1%, 2%, 3%, 4%, and 5%);

[0057] This embodiment provides another method for preparing a composition for repelling and killing ticks, comprising the following steps:

[0058] S1. The walnut leaf essential oil in Example 1 is mixed with 20% DEET (i.e., a DEET ethanol solution with a mass concentration of 20%) in a volume ratio of 1:1 to obtain a mixed solution; the mixed solution is dissolved and diluted with 70% anhydrous ethanol with a volume concentration of 2% (volume concentration) of an emulsifier (Tween-80) to prepare a composition for repelling and killing ticks with a mixed solution volume concentration of 6 to 10% (specific volume concentrations are 6%, 7%, 8%, 9%, and 10%).

[0059] The above tick repellent and contact killing composition was tested for tick repellency, and a commercially available insect repellent containing 5% (mass concentration) DEET was used as a control. The repellent and contact killing effect test methods were the same as above, and the repellent test results are shown in Table 4, and the contact killing results are shown in Table 5.

[0060] Table 4 - Tick contact test results

[0061]

[0062]

[0063] Table 5 - Tick contact test results

[0064]

[0065] It can be seen from Tables 4 and 5 that as the concentration of the active ingredient increases, the longer the repellent time of the repellent contact tick spray is, the higher the number of tick deaths is.

[0066] Example 4

[0067] Skin irritation test

[0068] Nine healthy adult white rabbits were randomly divided into three groups. A 3 cm × 3 cm area was removed from the abdomen. After 24 h, the repellent tick spray was sprayed at 0.1 mL / 1 cm 2 The dose was evenly applied to the depilated area of ​​the rabbit, covered with gauze, and then fixed with a non-irritating bandage. A 70% anhydrous ethanol solution containing 2% (volume concentration) emulsifier (Tween-80) was used as a negative control, and a 2,4-dinitrochlorobenzene (5 mg / mL) solution was used as a positive control. The fixation and covering were removed after 4 hours, and the skin changes of the test site were observed at 1, 24, 48, and 72 hours. Refer to the GB_T 21604-2022 scoring standard to determine whether the spray will irritate the skin. The results are shown in Table 6. Among them, the spray for repelling and contact killing of ticks includes a mixture of 5mL of walnut leaf essential oil in Example 1, 5mL of 20% DEET (i.e., a DEET ethanol solution with a mass concentration of 20%), 2ml of Tween-80, and 488mL of 70% ethanol by volume. Table 6-Scoring results of the skin irritation experiment of the tick repellent spray

[0069]

[0070] As shown in Table 6, the 10% tick-killing spray has no irritation to the rabbit skin, and no animal died during the whole experiment, so it is safe to use.

[0071] It can be understood that the technical features of the above-described embodiments can be arbitrarily combined. In order to make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0072] The above are only preferred embodiments of the present application, and only specifically describe the technical principles of the present application. These descriptions are only for explaining the principles of the present application and cannot be interpreted as limiting the scope of protection of the present application in any way. Based on the explanation here, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application, and other specific implementation methods of the present application that can be associated with the technicians in this field without creative work, should be included in the scope of protection of the present application.

Claims

1. A tick repellent and contact killing composition, characterized in that: The invention comprises plant essential oil and DEET; the plant essential oil is walnut leaf essential oil.

2. The tick repellent and contact killing composition according to claim 1, characterized in that: The DEET is a DEET ethanol solution with a mass concentration of 20-25%.

3. The tick repellent and contact killing composition according to any one of claims 1 to 2, characterized in that: The mass ratio of the plant essential oil to DEET is (1-6):(1-2).

4. The tick repellent and contact killing composition according to claim 1, characterized in that: The walnut leaf essential oil comprises the following components by mass fraction: 11.66% phytol, 7.05% beta-eucalyptol, 6.76% diisobutyl phthalate, 6.63% dibutyl phthalate, 6.53% alpha-eucalyptol, 5.18% phyton, 4.57% guaiacol acetate, 4.05% 2-(6,10-dimethyl-2-spiro[4.5]dodecan-9-enyl)propane-2-ol, 3.05% myrtenol, 2.98% (-)-pyrethroid D, 6,6-dimethyl-2-methylenebicyclo[ 3.1.1]-3-heptanol 2.97%, oleanolic acid 2.81%, farnesyl acetone 2.73%, (E)-β-farnesene 2.69%, eucalyptol 2.68%, methyl palmitate 2.4%, eugenol 2.28%, acetophenone 2.11%, 3,5-di-tert-butyl-4-hydroxybenzaldehyde 2.04%, methyl linolenate 1.61%, Δ-cadinene 1.57%, β-ionone 1.38%, mabehenone 1.25%, 2-(4-methyl-2,4-cyclohexadien-1-yl)-2-propane 1.24%, ethyl palmitate 1.03%, verbenol 0.96%, 3,5-di-tert-butylphenol 0.95%, nerolidol 0.86 %, 2-isopropyl-2-methyloxirane 0.86%, β-ylanene 0.76%, methyl linoleate 0.7%, carvone 0.68%, 9-eicosine 0.68%, (1R,5S)-carveol 0.65%, α-molle alcohol 0.63%, 3,7,11,15-tetramethylhexen-1-ol 0.52%, 2-phenyl-2-propanol 0.48%, (+)-α-terpineol 0.44%, (S)-cis-verbenol 0.38%, nerolilacetone 0.34%, β-butene 0.34%, carvone 0.22%, 5-isopropylbicyclo[3.1.0]hexane-2-one 0.17%, 4-terpenol 0.13%.

5. A method for preparing the tick repellent and contact killing composition according to any one of claims 1 to 4, characterized in that: The following steps are involved: The plant essential oil and DEET are mixed and then added into ethanol to obtain a tick repellent and contact killing composition.

6. The method for preparing the tick repellent and contact killing composition according to claim 5, characterized in that: The plant essential oil and DEET are mixed and added into ethanol with a volume concentration of 70-80% to obtain a tick repellent and contact killing composition, wherein the sum of the mass concentrations of the plant essential oil and DEET is 1-10%.

7. The method for preparing the tick repellent and contact killing composition according to claim 6, characterized in that: The ethanol contains Tween-80 with a volume concentration of 1-2%.

8. Use of the tick repellent and contact killing composition according to any one of claims 1 to 4 or the tick repellent and contact killing composition prepared by the preparation method according to any one of claims 5 to 7 in the preparation of tick repellent and contact killing drugs.

9. The use according to claim 8, wherein the composition for repelling and killing ticks by contact is in the form of a spray or a pour-on.

10. The use according to claim 8, wherein the application object is livestock or pets.

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