Plant extract tick-killing agent and preparation method thereof

Abstract

The invention discloses a plant extract tick-killing agent and a preparation method thereof. The plant extract tick-killing agent is prepared from 0.22 mg / mL to 3.5 mg / mL of rhododendron simsii extract and 8.75 mg / mL to 22.36 mg / mL of thymol essential oil, wherein the mass volume concentration of the rhododendron simsii extract is 0.22 mg / mL to 3.5 mg / mL. The azalea extract, thymol essential oil, a solvent, an emulsifier, an antifreeze agent and a defoaming agent are mixed to obtain the plant extract tick-killing agent. The prepared tick-killing agent is environment-friendly, and meanwhile, the azalea resource can be fully utilized. The adopted thyme is an aromatic plant, the essential oil yield is high, the plant essential oil has the characteristic of no residue, the influence on the ecological environment is small, and good research and market prospects are achieved. A large number of experiments confirm that the rhododendron simsii extract and the thymol essential oil are compatible and have a synergistic effect, and the tick killing effect can be improved.

Description

Technical Field

[0001] The invention belongs to the technical field of botanical insecticides and relates to a plant extract tick killer and a preparation method thereof. Background Art

[0002] At present, chemical drugs are mainly used for comprehensive prevention and control of ticks, but long-term use of chemical pesticides will cause drug residues and cause serious pollution to the natural environment. At the same time, chemical pesticides degrade slowly, and residual chemical drugs continue to accumulate among animals and plants, posing a potential food safety hazard. Since the prevention and control of ticks mainly relies on chemical pesticides, their long-term and large-scale use has caused ticks to gradually develop drug resistance, which in turn has reduced the efficacy of the drugs or even made them ineffective. Chemical drugs are easy to pollute the environment and cause resistance to the receptors they act on. Natural ingredients extracted from nature are increasingly valued as tickicides because they are easy to decompose and have no residue. Therefore, it is extremely important to choose efficient and harmless drugs to prevent and control ticks at the moment.

[0003] As natural products, plant extracts do not pollute the environment, are environmentally friendly, safe, and not prone to receptor resistance, and can overcome the disadvantages of chemical drugs. At present, the efficacy of plant extracts against other agricultural pests and parasites has been reported, but there are still few reports on natural plant extracts that can be applied to the surface of humans and animals and have significant tick-killing effects. Rhododendron is grown in large quantities in southern my country as an ornamental plant, but its flowers and leaves are left to wither naturally and have not been effectively utilized.

[0004] Based on the above analysis, a plant-based insecticide that can effectively kill ticks and does not pollute the environment is urgently needed in the industry. Summary of the invention

[0005] In view of the above analysis, the object of the present invention is to provide a plant extract tick killer which has good tick killing effect and does not pollute the environment and a preparation method thereof.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention first discloses a plant extract tick killer, wherein:

[0008] The plant extract tick killer comprises: azalea extract with a mass volume concentration of 0.22-3.5 mg / mL and thymol essential oil with a mass volume concentration of 8.75-22.36 mg / mL.

[0009] Furthermore, the azalea extract is 0.22-0.87 mg / mL, and the thymol essential oil is 8.75-10.0 mg / mL.

[0010] Furthermore, the azalea extract is 0.22 mg / mL, and the thymol essential oil is 10.0 mg / mL.

[0011] The present invention also discloses a method for preparing a plant extract tick killer, comprising the following steps:

[0012] (1) Preparation of azalea extract: grind azalea into powder using a fast grinder and soak it in a solvent 10 times its volume at room temperature for 30 minutes; boil the soaked drug and time it for 1 hour after boiling; centrifuge, filter and rotary evaporate the boiled drug to obtain a viscous drug;

[0013] (2) Preparation of thymol essential oil: chop fresh thyme into small pieces, extract the essential oil by steam distillation, and collect the essential oil floating on the water surface;

[0014] (3) Preparation of a plant extract tick killer: dissolving thymol essential oil in a solvent, and then adding an emulsifier to obtain an oil phase of an aqueous emulsion; dissolving azalea extract in water, and then adding an antifreeze agent and a defoaming agent to obtain an aqueous phase of an aqueous emulsion; and stirring and mixing the aqueous phase and the oil phase of the aqueous emulsion with the aid of ultrasound to obtain a plant extract tick killer.

[0015] Furthermore, the azalea in step (1) is one or more combinations of azalea whole flowers, azalea leaves, azalea branches, azalea roots, etc.

[0016] Furthermore, the solvent in step (1) is one or more combinations of water, ethanol, methanol, acetone, petroleum ether, benzene, chloroform, ether, ethyl acetate, dichloromethane, etc.

[0017] Furthermore, the solvent in step (3) is one or more combinations of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, acetone, etc.

[0018] Furthermore, the emulsifier in step (3) is one or more combinations of Tween 20, Tween 80, glycerol laurate, OP-10, etc.

[0019] Furthermore, the antifreeze agent in step (3) is one or more combinations of glycerol, propylene glycol, ethylene glycol, urea, 1,2-butanediol, calcium chloride, sodium chloride, etc.

[0020] Furthermore, the defoaming agent in step (3) is one or more combinations of emulsified silicone oil, silicone, mineral oil, tributyl phosphate, etc.

[0021] Furthermore, in the plant extract tick killer agent of step (3), by mass fraction, the emulsifier accounts for 0.5%-3%, the antifreeze agent accounts for 1%-5%, and the defoaming agent accounts for 0.2%-0.5%.

[0022] The invention also discloses a plant extract tick killer prepared according to any one of the above preparation methods.

[0023] Furthermore, the plant extract tick killer comprises: azalea extract with a mass volume concentration of 0.22-3.5 mg / mL and thymol essential oil with a mass volume concentration of 8.75-22.36 mg / mL.

[0024] Furthermore, the mass volume concentration of the azalea extract is 0.22 mg / mL, and the thymol essential oil is 10.0 mg / mL.

[0025] The beneficial effects of the present invention are:

[0026] First, the two components of the tick-killing agent of the present invention have high yields, and the raw materials are easily available and low in cost, and the plant resources are comprehensively utilized; second, the preparation is an aqueous emulsion, with a small amount of organic solvent, which is environmentally friendly and pollution-free; third, the operation and processing are simple, the equipment environment requirements are low, and it is easy to prepare on a large scale, and it has good application prospects. The raw material azalea used in the present invention is an ornamental plant widely distributed in southern China and planted on a large scale. Its fallen flowers and leaves are not fully utilized, resulting in a waste of its own resources. The present invention uses azalea as a raw material and effectively utilizes resources. The thyme used in the present invention is an aromatic plant, the essential oil yield is high, and the plant essential oil has the characteristics of no residue, and the impact on the ecological environment is small, and it has a good research and market prospect. The present invention confirms through a large number of experiments that the azalea extract and thymol essential oil are compatible, and the two act synergistically to improve the tick-killing effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to make the purpose, technical solution and beneficial effects of the present invention clearer, the present invention provides the following drawings for illustration:

[0028] Figure 1 Test the lethality of Rhododendron extract to ticks in petri dishes with different concentrations;

[0029] Figure 2 Test the lethality of thymol essential oil to ticks in petri dishes with different concentrations;

[0030] Figure 3 Test the lethality of ticks in petri dishes with different concentrations of tickicide combinations;

[0031] Figure 4 The lethality rate of ticks was tested by spraying different concentrations of tickicides on animal bodies. DETAILED DESCRIPTION

[0032] The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. The experimental methods without specific conditions in the embodiments are usually carried out under conventional conditions or under conditions recommended by the manufacturer.

[0033] Example 1

[0034] Preparation method of azalea extract:

[0035] 1) Use a fast grinder to grind azalea into powder, and weigh 30g on a measuring paper;

[0036] 2) Soak the powder in 300 mL of solvent at room temperature for 30 minutes.

[0037] 3) Place the soaked medicine in step 2) in a heat-resistant glass fiber electric heating jacket, connect a cooling device, and boil it. After boiling, time it for 1 hour.

[0038] 4) The boiled medicine is centrifuged, filtered and rotary evaporated to finally obtain a viscous medicine, which is the azalea extract.

[0039] The azalea flowers are one or more combinations of azalea whole flowers, azalea leaves, azalea branches, azalea roots and the like.

[0040] The solvent is one or more combinations of water, ethanol, methanol, acetone, petroleum ether, benzene, chloroform, ether, ethyl acetate, dichloromethane, etc.

[0041] Example 2

[0042] Preparation method of thymol essential oil:

[0043] Take 200g of fresh thyme, cut into 2-3cm long segments, extract essential oil by steam distillation, collect essential oil floating on the water surface in the volatile oil extractor, store in a brown sealed small glass bottle for later use, and repeat this process until enough essential oil is obtained.

[0044] Example 3

[0045] Test on killing ticks using azalea extract alone:

[0046] The azalea extract was prepared into different concentrations to test its lethality to ticks. The solutions of different concentrations were evenly applied to the dorsal and ventral surfaces of ticks, 10 μL for each tick, and three parallel experiments were performed. The lethality was calculated after 24 hours. Data statistical method: First, a one-way ANOVA was used to test whether the differences between the data groups were significant. Then, the LSD method was used to analyze the data. The differences between the groups marked with different letters were significant, and the significance level was P<0.05.

[0047] A large number of experimental results show that when the concentration of azalea extract is 0.22mg / mL, 0.87mg / mL, and 3.5mg / mL, it exhibits an obvious concentration gradient effect, such as Figure 1 As shown, the mortality rates of single azalea extract against ticks were 35%, 60% and 87% respectively.

[0048] Example 4

[0049] Thymol alone was used to kill ticks:

[0050] Thymol essential oil was prepared into different concentrations to test its lethality to ticks. After a large number of experimental results, it was shown that thymol essential oil has killing activity against ticks. When the concentrations were 8.75 mg / mL, 10.0 mg / mL, and 22.36 mg / mL, the lethality to ticks was 30%, 50%, and 83%, respectively, showing the same concentration gradient effect. Figure 2 shown.

[0051] Example 5

[0052] Method: Rhododendron extract (A) and thymol essential oil (B) were prepared into the following formulas according to the above method: I (B 8.75 mg / mL), II (A 0.22 mg / mL), III (A 0.87 mg / mL + B 8.75 mg / mL), IV (B 22.36 mg / mL), V (A 3.5 mg / mL), VI (A 0.22 mg / mL + B 10 mg / mL).

[0053] Results: When low-concentration thymol essential oil (I) and low-concentration azalea extract (II) were used alone, the lethality rates of ticks were 30% and 35%, respectively, and the tick-killing efficiency was low; when high-concentration thymol essential oil (IV) and high-concentration azalea extract (V) were used alone, the lethality rates of ticks were 83% and 87%, respectively, which could achieve a good tick-killing effect. In group III, the azalea extract with a concentration of 0.87 mg / mL was used as the main component, and thymol essential oil with a concentration of 8.75 mg / mL was added to this. As a result, the lethality rate of ticks in this combination could reach 90%, and the tick-killing efficiency was higher than that of groups IV and V. In group VI, the concentration of thymol essential oil continued to increase and the concentration of azalea extract decreased, and the tick-killing effect continued to increase, and the lethality rate of ticks could reach 95%. Figure 3 The results showed that whether a slightly higher concentration of azalea extract was combined with a low concentration of thymol essential oil, or a low concentration of azalea extract was combined with a half-lethal concentration of thymol, the tick-killing effect was stronger than the effect of using either alone, indicating that azalea extract and thymol essential oil have a synergistic tick-killing effect.

[0054] Example 6

[0055] Verify the effect of spraying on the animal body surface based on the results of the petri dish experiment. Prepare the following insecticide formulas: VII (B 10 mg / mL), VIII (A 3.5 mg / mL), VIX (A0.87 mg / mL+B 8.75 mg / mL), X (A0.22 mg / mL+B10 mg / mL). Each group of formula solutions is placed in a small spray bottle. Select a healthy and good chicken and let it be infected with ticks. Spray the infected area with a certain number of ticks so that the tickicide solution is evenly sprayed on the animal body surface. Statistic the mortality rate after 24 hours. The results are as follows: Figure 4 shown.

[0056] Data statistical method: First, one-way ANOVA was used to detect whether the differences between the data groups were significant. Then the LSD method was used to analyze the data. The differences between the groups marked with different letters were significant, and the significance level was P<0.05.

[0057] Results: The lethality rates of thymol essential oil (VII) and azalea extract (VIII) were 46.4% and 83.3% respectively. The lethality rates of azalea extract combined with thymol essential oil (VIX) and azalea extract combined with thymol at a median lethal concentration (V) were 88.3% and 92.4% respectively. The above results are affected by many factors on the animal surface, which leads to some differences between the results and the results of tick killing in the culture dish, but the overall difference is small. The results also show that the tick killing effect of the combination of azalea extract and thymol essential oil is better than that of the two alone, and the two have a synergistic tick killing effect.

[0058] Example 7

[0059] The acaricide with rhododendron extract and thymol essential oil as main raw materials can also be prepared into a commercial finished acaricide, and the preparation method is as follows:

[0060] 1) dissolving the essential oil in a solvent, and then adding an emulsifier to obtain an oil phase in water emulsion;

[0061] 2) dissolving the azalea ethanol extract in water, and then adding an antifreeze agent and a defoaming agent to obtain an aqueous emulsion water phase;

[0062] 3) The aqueous phase and the oil phase of the aqueous emulsion are stirred and mixed, and ultrasonic wave assistance is used to prepare a brown homogeneous liquid, which is the plant extract tick killer.

[0063] Calculated by mass fraction, the plant extract tick killer contains 0.5%-3% emulsifier, 1%-5% antifreeze agent and 0.2%-0.5% defoamer.

[0064] The solvent is one or more combinations of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, acetone, etc.

[0065] The emulsifier is one or more combinations of Tween 20, Tween 80, glycerol lauric acid, OP-10 and the like.

[0066] The antifreeze agent is one or more combinations of glycerol, propylene glycol, ethylene glycol, urea, 1,2-butanediol, calcium chloride, sodium chloride, etc.

[0067] The defoaming agent is one or more combinations of emulsified silicone oil, organic silicon, mineral oil, tributyl phosphate, etc.

[0068] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made in form and details without departing from the scope defined by the claims of the present invention.

Claims

1. A plant extract tick killer, comprising: The mass volume concentration of azalea extract is 0.22-3.5 mg / mL, and the mass volume concentration of thymol essential oil is 8.75-22.36 mg / mL.

2. The plant extract acaricide according to claim 1, wherein: The content of the azalea extract is 0.22-0.87 mg / mL, and the content of the thymol essential oil is 8.75-10.0 mg / mL.

3. The plant extract acaricide according to claim 1, wherein: The content of the azalea extract is 0.22 mg / mL, and the content of the thymol essential oil is 10.0 mg / mL.

4. A method for preparing a tick killer agent derived from a plant extract according to any one of claims 1 to 3, comprising: (1) Preparation of azalea extract: Grind azalea into powder and soak it in a 10-fold volume of solvent for 30 minutes; then boil and maintain boiling for 1 hour; the boiled drug is centrifuged, filtered and rotary evaporated to obtain; (2) Preparation of thymol essential oil: chop fresh thyme into small pieces and perform steam distillation to obtain thymol essential oil; (3) Preparation of a plant extract tick killer: dissolving thymol essential oil in a solvent, and then adding an emulsifier to obtain an oil phase of an aqueous emulsion; dissolving azalea extract in water, and then adding an antifreeze agent and a defoaming agent to obtain an aqueous phase of an aqueous emulsion; and stirring and mixing the aqueous phase and the oil phase of the aqueous emulsion with the aid of ultrasound to obtain a plant extract tick killer.

5. The preparation method according to claim 4, wherein: The azalea in step (1) is selected from: one or more combinations of azalea whole flowers, azalea leaves, azalea branches, and azalea roots; The solvent is selected from: one or more combinations of water, ethanol, methanol, acetone, petroleum ether, benzene, chloroform, ether, ethyl acetate, and dichloromethane.

6. The preparation method according to claim 4, wherein: The solvent in step (3) is selected from one or more combinations of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, and acetone; The emulsifier is selected from: one or more combinations of Tween 20, Tween 80, glycerol laurate, and OP-10; The antifreeze agent is selected from: one or more combinations of glycerol, propylene glycol, ethylene glycol, urea, 1,2-butanediol, calcium chloride, and sodium chloride; The defoaming agent is selected from one or more combinations of emulsified silicone oil, organic silicone, mineral oils, and tributyl phosphate.

7. The preparation method according to claim 4, wherein: In the plant extract tick killer agent of step (3), by mass fraction, the emulsifier accounts for 0.5%-3%, the antifreeze agent accounts for 1%-5%, and the defoaming agent accounts for 0.2%-0.5%.

8. A plant extract tickicide prepared according to the preparation method of any one of claims 4 to 7.

9. The plant extract acaricide according to claim 8, wherein: The plant extract tick killer comprises: azalea extract with a mass volume concentration of 0.22-3.5 mg / mL and thymol essential oil with a mass volume concentration of 8.75-22.36 mg / mL.

10. The plant extract acaricide according to claim 9, wherein: The mass volume concentration of the azalea extract is 0.22 mg / mL, and the thymol essential oil is 10.0 mg / mL.

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