Repellent-killing tick composition, and method for preparing and using the same
The combination of walnut leaf essential oil and DEET solves the problems of tick resistance and toxicity of existing repellents, and achieves the effect of long-lasting repellency and contact killing of ticks.
Patent Information
- Application Number
- CN202411728592.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-10-17
- Estimated Expiration
- 2044-11-28
AI Technical Summary
Existing tick repellents such as DEET have problems with tick resistance and toxicity, making it difficult to effectively repel and kill ticks.
A composition of walnut leaf essential oil and DEET is used. The walnut leaf essential oil is extracted by a CO2 supercritical extraction method, mixed with DEET, and added into ethanol to prepare a tick repellent and contact killing composition.
It improves the time and safety of tick repellent, reduces the toxicity of DEET, increases the contact killing effect, and solves the problem of tick resistance.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of pest control, in particular to a repellent and contact-killing tick composition and a preparation method and application thereof. BACKGROUND
[0002] Ticks belong to arthropods, arachnids, acarina, parasitic mite order, ticks, ticks, and are commonly known as grass crawlers. They parasitize the body surface of mammals, birds and reptiles to suck blood. Ticks have four stages of insect bodies, eggs, larvae, nymphs and adults. Each stage from larvae to adults needs to suck blood. When ticks bite, they will secrete a toxin from the mouth to make the bitten host feel nothing and not easy to be found. After being bitten by ticks, tick paralysis and the spread of tick-borne diseases will occur. There are 83 viruses, 4 bacteria, 17 spirochetes and 32 protozoa that ticks can carry in the world, with a mortality rate of up to 30%.
[0003] Currently, most of the repellents for ticks are organic synthetic repellents and insecticides, such as a repellent containing 20% DEET (DEET). It is applied to the skin and clothes to prevent ticks from biting. Pyrethroid insecticides, such as cypermethrin, have neurotoxicity to insects, are spectrally safe for humans and animals. However, with the long-term use of chemical drug preparations, ticks may develop resistance to them, making the repellent and contact-killing effect weaker. DEET has no contact-killing effect on ticks, and it is currently believed that DEET has a certain toxicity, so it is not recommended for children under 6 months and pregnant women to use DEET.
[0004] Based on the defects of the current DEET repellent, it is necessary to improve it. SUMMARY
[0005] Therefore, the present application provides a repellent and contact-killing tick composition and a preparation method and application thereof to solve or partially solve the problems in the prior art.
[0006] In a first aspect, the present application provides a repellent and contact-killing tick composition, comprising a 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 20-25%.
[0008] Preferably, the mass ratio of the plant essential oil and DEET is (1-6):(1-2).
[0009] Preferably, the walnut leaf essential oil comprises the following mass fraction of components: phytol 11.66%, beta-eudesmol 7.05%, diisobutyl phthalate 6.76%, dibutyl phthalate 6.63%, alpha-eudesmol 6.53%, phytone 5.18%, guaiacol acetate 4.57%, 2-(6,10-dimethyl-2-spiro[4.5]dodec-9-enyl)propan-2-ol 4.05%, myrtenol 3.05%, (-)-jasmol D 2.98%, 6,6-dimethyl-2-methylenebicyclo[3.1.1]-3-heptanol 2.97%, caryophyllin 2.81%, farnesyl acetone 2.73%, (E)-beta-farnesene 2.69%, eudesmol 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%, delta-cadinene 1.57%, beta-ionone 1.38%, maibaiene ketone 1.25%, 2-(4-methyl-2,4-cyclohexadien-1-yl)-2-propan 1.24%, ethyl palmitate 1.03%, verbenaol 0.96%, 3,5-di-tert-butylphenol 0.95%, nerolidol 0.86%, 2-isopropyl-2-methyloxirane 0.86%, beta-ylangene 0.76%, methyl linoleate 0.7%, carvomenthone 0.68%, 9-eicosyn 0.68%, (1R,5S)-carveol 0.65%, alpha-mohrenol 0.63%, 3,7,11,15-tetramethylhexadecan-1-ol 0.52%, 2-phenyl-2-propanol 0.48%, (+)-alpha-terpinyl alcohol 0.44%, (S)-cis-verbenaol 0.38%, neryl acetone 0.34%, beta-cadinene 0.34%, carvone 0.22%, 5-isopropylbicyclo[3.1.0]hexan-2-one 0.17%, 4-terpenol 0.13%.
[0010] In a second aspect, the present application further provides a preparation method of the repellent and tick-killing composition, comprising the following steps:
[0011] After mixing the plant essential oil and diethyltoluamide, the mixture is added into ethanol to obtain the repellent and tick-killing composition.
[0012] Preferably, after mixing the plant essential oil and diethyltoluamide, the mixture is added into ethanol with a volume concentration of 70-80% to obtain the repellent and tick-killing composition, and the sum of the mass concentrations of the plant essential oil and diethyltoluamide is 1-10%.
[0013] Preferably, the ethanol contains Tween-80 with a volume concentration of 0.1-0.2%.
[0014] In a third aspect, the application further provides a use of the repellent and contact-killing tick composition or the repellent and contact-killing tick composition prepared by the preparation method in the preparation of a repellent and contact-killing tick medicine.
[0015] Preferably, the dosage form of the repellent and contact-killing tick composition is a spray or a pour-on.
[0016] Preferably, the application object is livestock or pets.
[0017] The repellent and contact-killing tick composition, the preparation method and the use thereof have the following beneficial effects relative to the prior art:
[0018] The repellent and contact-killing tick composition contains plant essential oil components, and the use of plant essential oil in combination with DEET has a good synergistic effect. On the basis of the repellent effect of DEET, the contact-killing effect is increased. The repellent and contact-killing tick composition has a long repellent time and good safety, and reduces the toxicity of DEET. The application 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 of DEET while maintaining the repellent effect, and increases the contact-killing effect of ticks. The repellent and contact-killing tick composition has a long repellent time and good contact-killing effect, can replace existing organic repellents and insecticides, and solves the problem of tick drug resistance. DETAILED DESCRIPTION
[0019] The technical solutions in the embodiments of the application will be clearly and completely described in combination with the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of the application.
[0020] It should be noted that the order of the following embodiments is not limited as the preferred order of the embodiments. In addition, in the description of the present application, the term "comprising" means "including but not limited to". Various embodiments of the application can exist in the form of a range; it should be understood that the description in the form of a range is only for the convenience and brevity, and should not be understood as a hard limitation on the scope of the application; therefore, it should be considered that the described range has been specifically disclosed all possible sub-ranges and single values in 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 in the range, such as 1, 2, 3, 4, 5 and 6, regardless of the range. In addition, whenever a numerical range is indicated in this document, it means that any cited number (fraction or integer) in the indicated range is included.
[0021] The embodiment of the present application provides a repellent and contact-killing tick composition, which comprises plant essential oil and diethyltoluamide; the plant essential oil is walnut leaf essential oil.
[0022] In some embodiments, the diethyltoluamide is an ethanol solution of diethyltoluamide with a mass concentration of 20-25%.
[0023] In some embodiments, the mass ratio of the plant essential oil and the diethyltoluamide is (1-6):(1-2).
[0024] In some embodiments, the walnut leaf essential oil comprises the following components with the following mass fractions: phytol 11.66%, beta-eudesmol 7.05%, diisobutyl phthalate 6.76%, dibutyl phthalate 6.63%, alpha-eudesmol 6.53%, phytone 5.18%, guaiacol acetate 4.57%, 2-(6,10-dimethyl-2-spiro[4.5]dodec-9-enyl)propan-2-ol 4.05%, myrtenenol 3.05%, (-)-jasmol D 2.98%, 6,6-dimethyl-2-methylenebicyclo[3.1.1]-3-heptanol 2.97%, carnaolan 2.81%, farnesyl acetone 2.73%, (E)-beta-farnesene 2.69%, eudesmol 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%, delta-cadinene 1.57%, beta-ionone 1.38%, maalieneone 1.25%, 2-(4-methyl-2,4-cyclohexadien-1-yl)-2-propan 1.24%, ethyl palmitate 1.03%, verbenenol 0.96%, 3,5-di-tert-butylphenol 0.95%, nerolidol 0.86%, 2-isopropyl-2-methyloxirane 0.86%, beta-ylangene 0.76%, methyl linoleate 0.7%, carvophyllone 0.68%, 9-eicosyn 0.68%, (1R,5S)-carveol 0.65%, alpha-mohrenol 0.63%, 3,7,11,15-tetramethylhexadecan-1-ol 0.52%, 2-phenyl-2-propanol 0.48%, (+)-alpha-terpinyl alcohol 0.44%, (S)-cis-verbenenol 0.38%, neryl ketone 0.34%, beta-cadinene 0.34%, carvone 0.22%, 5-isopropylbicyclo[3.1.0]hexan-2-one 0.17%, 4-terpenenol 0.13%.
[0025] The walnut leaf essential oil is extracted from walnut (Juglan regia L.) leaves by using CO2 supercritical extraction method (SFE-CO2), and can effectively avoid the problems of drug residues and tick drug resistance caused by using chemical drugs; the repellent and tick-killing composition contains plant essential oil components, and the mixture of the plant essential oil and DEET has good synergistic effect, and the repellent and tick-killing composition increases the tick-killing effect on the basis of the repellent effect of DEET. The repellent and tick-killing composition has long repellent time and good safety, and reduces the toxicity of DEET. The plant essential oil with effective repellent and tick-killing effect is screened out, mixed with DEET, the content of DEET in the repellent and tick-killing composition is reduced, the toxicity effect caused by DEET is reduced while the repellent effect is equivalent, and the tick-killing effect is increased.
[0026] Based on the same inventive concept, the application further provides a preparation method of the repellent and tick-killing composition.
[0027] After the plant essential oil and DEET are mixed, the mixture is added into ethanol to obtain the repellent and tick-killing composition.
[0028] In some embodiments, after the plant essential oil and DEET are mixed, the mixture is added into ethanol with a volume concentration of 70-80% to obtain the repellent and tick-killing composition, and the mass concentration of the plant essential oil and DEET is 1-10%.
[0029] In some embodiments, the ethanol contains Tween-80 with a volume concentration of 1-2%.
[0030] Based on the same inventive concept, the application further provides an application of the repellent and tick-killing composition or the repellent and tick-killing composition prepared by the preparation method in the preparation of a repellent and tick-killing drug.
[0031] In some embodiments, the dosage form of the repellent and tick-killing composition is a spray or a pouring agent.
[0032] In some embodiments, the application object of the repellent and tick-killing composition is livestock or pets.
[0033] The repellent and tick-killing composition, the preparation method and the application thereof are further described in the following specific embodiments. This part further describes the content of the application in combination with specific embodiments, but should not be understood as a limitation of the application. If not specifically described, the technical means used in the embodiments are conventional means familiar to those skilled in the art. Unless specifically described, the reagents, methods and devices used in the application are conventional reagents, methods and devices in the art.
[0034] Example 1
[0035] 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 tick repellent and contact-killing composition, comprising the following steps:
[0041] S1. Prepare a 20% DEET solution with anhydrous ethanol to obtain a 20% DEET solution for later use.
[0042] S2. The walnut leaf essential oil in Example 1 was mixed with 5 mL of the 20% DEET solution in S1 at a mass ratio of 6:1, 4:1, 2:1, 1:1, and 1:2, respectively, to prepare a 20% DEET + relative proportion of essential oil repellent and contact tick-killing composition for later use.
[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] Taking into account the characteristics of ticks climbing upwards, the repellent effect of essential oils on adult ticks was determined by using a "Y"-shaped olfactometer. 20 Rhipicephalus turanicus ticks (half male and half female) were placed in a tube with the same diameter as the bottom of the "Y"-shaped tube. The tube was connected to the bottom of the Y-shaped tube and sealed. 15 μL of the repellent contact tick-killing composition in Example 2 or an equal volume of anhydrous ethanol, walnut leaf essential oil, and a 20% DEET solution were added to the left and right upper ends of the Y-shaped tube. A 1 cm diameter circular filter paper was added to each end, leaving the other end untreated. Both hands were placed at the two ends of the tube 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, the repellent and contact-killing tick composition can achieve an effective protection time of up to 1.5h, when the time when the first tick crawls out in the treatment group is taken as the repellent time. From the above results, it can be seen that the walnut leaf essential oil has a better repellent effect on the adult Rhipicephalus turanicus; when the essential oil is mixed with DEET, a synergistic effect occurs, and the repellent effect is optimal when the essential oil and DEET are mixed at a mass ratio of 1:1, which can reach 89.33min.
[0049] Tick contact-killing test
[0050] In the adult immersion test (AIT), 10 hungry adult ticks were taken with tweezers and placed in a 5mL EP tube, 1mL of each repellent and contact-killing tick composition with different proportions in Example 2 was taken and used walnut leaf essential oil, a 20% DEET solution, and absolute ethanol with a mass concentration of 20% were injected into different tubes, and the ticks were immersed in each solution. After 5min of experiment, the ticks were removed and placed on filter paper, and after the body surface liquid was completely wiped dry, the ticks were placed in a clean test tube and placed in an incubator (27±1℃, RH≥80%) for 24h, and then the number of dead ticks was counted. The results are shown in Table 3.
[0051] Table 3-Results of tick contact-killing test
[0052]
[0053] From the above results, it can be seen that the walnut leaf essential oil has a significant contact-killing effect on the adult Rhipicephalus turanicus; when the essential oil is mixed with DEET, the higher the proportion of walnut leaf essential oil, the stronger the contact-killing effect on the adult Rhipicephalus turanicus, and the DEET not only repels ticks but also increases the killing effect.
[0054] Example 3
[0055] The present embodiment provides a preparation method of a repellent and contact-killing tick composition, comprising the following steps:
[0056] S1, the walnut leaf essential oil in Example 1 is mixed with 20% DEET (i.e. a 20% DEET ethanol solution) at a volume ratio of 1:1 to obtain a mixed solution; the mixed solution is dissolved in a 70% ethanol solution to dilute and prepare a repellent and contact-killing tick composition with a volume concentration of 1-5% (the specific volume concentrations are 1%, 2%, 3%, 4%, and 5%);
[0057] The present embodiment provides another preparation method of a repellent and contact-killing tick composition, comprising the following steps:
[0058] S1, walnut leaf essential oil in Example 1 was mixed with 20% DEET (i.e. 20% DEET ethanol solution) at a volume ratio of 1:1 to obtain a mixed solution; the mixed solution was dissolved and diluted with 70% (volume concentration) anhydrous ethanol containing 2% (volume concentration) emulsifier (Tween-80) to prepare a repellent and tick-killing composition with a volume concentration of 6-10% (specifically 6%, 7%, 8%, 9%, 10%).
[0059] The above repellent and tick-killing composition was tested for its repellent effect on ticks, with a commercially available insect repellent containing 5% (mass concentration) DEET as a control. The repellent and tick-killing effect test methods were the same as above, the repellent test results are shown in Table 4, and the tick-killing results are shown in Table 5.
[0060] Table 4-Repellent test results for ticks
[0061]
[0062]
[0063] Table 5-Tick-killing test results
[0064]
[0065] As can be seen from Tables 4 and 5, as the concentration of the active ingredient increases, the repellent time of the repellent and tick-killing spray is longer, and the number of dead ticks is higher.
[0066] Example 4
[0067] Skin irritation test
[0068] Nine healthy adult white rabbits were selected and randomly divided into three groups, and a 3cm x 3cm area was removed from the abdomen. After 24 hours, the repellent and tick-killing spray was applied at a rate of 0.1mL / 1cm 2 The dose was evenly applied to the rabbit hairless area, covered with gauze, and fixed with a non-irritating bandage. A solution containing 2% (volume concentration) emulsifier (Tween-80) in 70% (volume concentration) anhydrous ethanol was used as a negative control, and a 2,4-dinitrochlorobenzene (5mg / mL) solution was used as a positive control. After 4 hours, the fixings and coverings were removed, and the test site was observed at 1, 24, 48, and 72 hours, respectively. The spray was determined to be irritating to the skin according to the scoring standard of GB_T 21604-2022. The results are shown in Table 6. Among them, the repellent and tick-killing spray includes a mixture of 5mL walnut leaf essential oil in Example 1, 5mL 20% DEET (i.e. 20% DEET ethanol solution), 2ml Tween-80, and 488mL 70% (volume concentration) ethanol.
[0069]
[0070] From Table 6, it can be seen that the 10% deltamethrin spray has no irritation to the rabbit skin, and no animal died during the whole experiment, and is safe to use.
[0071] It can be understood that any combination of the technical features of the above-described embodiments can be made, and for the sake of brevity, all possible combinations of the technical features in the above-described embodiments are not described, however, as long as the combination of the technical features does not exist, it should be considered as the scope of the present disclosure.
[0072] The above is only a preferred embodiment of the present application, and only the technical principles of the present application are specifically described, and these descriptions are only for explaining the principles of the present application, and cannot be interpreted in any way as a limitation on the protection scope of the present application. Based on the explanation here, any modification, equivalent replacement and improvement made within the spirit and principle of the present application, and other specific embodiments of the present application that can be easily thought by those skilled in the art without creative labor, should be included in the protection scope 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; The walnut leaf essential oil is obtained by extracting walnut leaves using a CO2 supercritical extraction method; The DEET is a DEET ethanol solution with a mass concentration of 20-25%; The mass ratio of the plant essential oil to DEET is (1-6):(1-2).
2. A method for preparing the tick repellent and contact killing composition according to claim 1, 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.
3. The method for preparing the tick repellent and contact killing composition according to claim 2, wherein: 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%.
4. The method for preparing the tick repellent and contact killing composition according to claim 3, wherein: The ethanol contains Tween-80 with a volume concentration of 1-2%.
5. Use of the tick repellent composition according to claim 1 or the tick repellent composition prepared by the preparation method according to any one of claims 2 to 4 in the preparation of a tick repellent drug.
6. The use according to claim 5, wherein the composition for repelling and killing ticks by contact is in the form of a spray or a pour-on.
7. The use according to claim 5, wherein the application object is livestock or pets.
Citation Information
Patent Citations
Insect killing traditional Chinese pharmaceutical composition and preparation method thereof
CN107320671A
Tick expelling composition
CN112400917A