CN112219866A

CN112219866A - Plant extract pesticide

Info

Publication number: CN112219866A
Application number: CN202011267786.5A
Authority: CN
Inventors: 张弛; 成真锐; 邵伟; 王梁; 刘波
Original assignee: Linyi University
Current assignee: Linyi University
Priority date: 2020-11-13
Filing date: 2020-11-13
Publication date: 2021-01-15
Anticipated expiration: 2040-11-13
Also published as: CN112219866B

Abstract

The invention relates to a plant extract pesticide which comprises a green walnut skin extract, thyme essential oil and a peganum harmala alkaloid extract. A large number of experiments confirm that the insecticidal effect can be improved by using the combination of the green walnut skin extract, the thyme essential oil and the peganum harmala alkaloid extract. The pesticide has the advantages of easily available raw materials, abundant resources, low cost, waste recycling and comprehensive utilization of plant resources; the processing is simple, the requirement on equipment environment is low, and the popularization and application prospect is good; can be used for preventing and treating pests such as cotton, Chinese cabbage, radish aphid, etc.

Description

Plant extract pesticide

Technical Field

The invention belongs to the technical field of crops, and relates to a plant extract pesticide.

Background

The chemical pesticide is widely applied to agriculture, forestry and animal husbandry production, but often causes pollution to the natural environment. Many artificially synthesized chemical pesticides are easy to be preserved in nature for a long time due to lack of corresponding microorganisms for decomposing the pesticides, thereby threatening the safety of soil and underground water resources on which human beings live. However, natural ingredients extracted from nature are increasingly regarded as pesticides because they are easily decomposed and do not remain in nature. In addition, some chemical pesticides, although environmentally friendly, have been gradually evolved to be resistant to pests due to their long-term use in large quantities, resulting in a decrease or even loss of efficacy. The chemically synthesized pesticide is easy to pollute the environment, and the receptor is easy to generate resistance due to single action target. Under the condition, how to avoid the pests from being selected to have the resistance capability is particularly important for effectively preventing and treating the pests by applying local natural resources in Xinjiang according to local conditions.

Plant extracts have been reported for the prevention and control of aphids, and the plant extracts in nature are used as insecticides, so that resistance is not easy to generate due to various action targets; and as a natural product, the product can be degraded in nature, and cannot pollute the environment. Walnuts are produced locally in China, particularly Xinjiang, and a large amount of green walnut shells are usually discarded as wastes and are not effectively utilized.

Disclosure of Invention

In view of the above, the present invention aims to provide a plant extract pesticide.

In order to achieve the purpose, the invention provides the following technical scheme:

1. a plant extract pesticide comprises semen Juglandis Immaturus extract, thyme essential oil, and herba Pegani Harmalae alkaloid extract.

Furthermore, in the pesticide, according to the mass volume concentration, the green walnut skin extract is 0.8-10mg/ml, the thyme essential oil is 0.02-0.5mg/ml, and the peganum harmala alkaloid extract is 0.1-3.5 mg/ml.

Furthermore, in the pesticide, according to the mass volume concentration, the green walnut skin extract is 4-6mg/ml, the thyme essential oil is 0.3-0.5mg/ml, and the peganum harmala alkaloid extract is 1.5-2 mg/ml.

Furthermore, in the pesticide, the green walnut skin extract is 4mg/ml, the thyme essential oil is 0.5mg/ml and the peganum harmala alkaloid extract is 2mg/ml according to the mass volume concentration.

Further, the preparation method of the green walnut peel extract comprises the following steps:

1) drying fresh green walnut skin, and pulverizing into powder;

2) soaking the powder in 2-3 times of 95% ethanol solution, soaking and extracting at room temperature for 2-3 days, filtering, and collecting filtrate;

3) repeating the soaking process of the step 2) for 2-3 times, combining the filtrates, and performing rotary evaporation to obtain a paste substance, namely the green walnut peel extract.

Further, the preparation method of the thyme essential oil comprises the following steps: cutting fresh thyme, extracting essential oil by steam distillation, and collecting the essential oil floating on water surface.

Further, the preparation method of the peganum harmala alkaloid extract comprises the following steps:

1) taking fresh peganum harmala, drying in the shade for a week at room temperature, cutting into pieces, soaking and extracting with 70-80% ethanol for 2-3 days, filtering and collecting filtrate, repeating for 2-3 times, combining the filtrates, and performing rotary evaporation and concentration to obtain an ethanol crude extract;

2) dissolving the ethanol extract in distilled water solution containing 5% hydrochloric acid, and filtering to remove insoluble part; extracting soluble part with equal volume of chloroform for 3 times, and discarding chloroform phase;

3) adjusting the pH value of the water phase to 9.0 by ammonia water, adding chloroform for extraction, taking the chloroform phase, and performing rotary evaporation;

4) and dissolving and recrystallizing the chloroform extract in 95 percent ethanol to obtain the peganum harmala alkaloid extract.

Further, the pesticide can be prepared into a commercial plant extract pesticide, and the plant extract pesticide also comprises a solvent, an emulsifier, an antifreeze agent and a defoaming agent.

Further, the solvent is one or more of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, acetone and the like; the emulsifier is one or a combination of more of Tween 20, Tween 80, glycerol lauric acid, OP-10 and the like; the antifreeze is one or a combination of more of glycerol, propylene glycol, ethylene glycol, urea, 1, 2-butanediol, calcium chloride, sodium chloride and the like; the defoaming agent is one or a combination of more of emulsified silicone oil, organic silicon, mineral oil, tributyl phosphate and the like.

Furthermore, the plant extract pesticide comprises 0.5-3% of emulsifier, 1-5% of antifreeze and 0.2-0.5% of defoaming agent by mass.

The invention has the beneficial effects that: the pesticide has the advantages of easily available raw materials, abundant resources, low cost, waste recycling and comprehensive utilization of plant resources; the preparation is an aqueous emulsion, has small organic solvent dosage, is environment-friendly and is pollution-free; the processing is simple, the requirement on equipment environment is low, and the popularization and application prospect is good; the pesticide of the invention can be used for preventing and controlling pests such as cotton, cabbage, radish aphid and the like. The green walnut skin is prepared by taking the green walnut skin and the like as raw materials, the yield of the green walnut skin is huge in a walnut producing area, and the green walnut skin is discarded as waste all the time, so that the waste is avoided, and the environment is polluted. The invention changes waste into valuable and makes effective use of waste. The two plant materials used in the invention usually grow in a large area in the wild, and livestock can not take food and are not developed and utilized, so that the livestock can be self-killed, and the resource waste is caused. Wherein the thyme is aromatic plant with high yield of essential oil, and the other plant, peganum harmala, contains a large amount of alkaloid compounds such as peganine and harmine. A large number of experiments confirm that the insecticidal effect can be improved by using the combination of the green walnut skin extract, the thyme essential oil and the peganum harmala alkaloid extract.

Drawings

In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:

FIG. 1 shows that the fatality to aphids of culture dishes of green walnut skin extracts with different concentrations is tested;

FIG. 2 shows that different concentrations of thyme essential oil culture dishes test their lethality to aphids;

FIG. 3 shows that peganum harmala alkaloid extract petri dishes with different concentrations are tested for lethality to aphids;

FIG. 4 shows that different insecticide plates were tested for their lethality to aphids.

FIG. 5 shows that different insecticides were tested for their lethality to aphids in the field.

Detailed Description

Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The experimental procedures, in which specific conditions are not specified in the examples, are generally carried out under conventional conditions or under conditions recommended by the manufacturers.

Example 1

The preparation method of the green walnut skin extract comprises the following steps:

1) drying 2kg of collected fresh green walnut skin in the sun for later use;

2) crushing the dried green walnut peels into powder by using a crusher;

3) soaking the powder in 2 times volume of 95% ethanol solution, soaking and extracting for three days at room temperature, filtering with filter paper, and collecting filtrate;

4) repeating the soaking process for 2-3 times, mixing filtrates, and rotary evaporating with rotary evaporator to obtain paste material, i.e. green walnut peel extract.

Green walnut peel extracts were formulated to different concentrations to test their lethality to aphids. The solutions with the concentrations are respectively filled into small spray bottles. The plates were placed in a petri dish with 9cm filter paper and moistened with 3ml of clear water. Half of the area of the glass dish, with the back facing upwards, was taken and stuck to the center of the filter paper sheet. Inoculating about 50 aphids with the same size with bamboo sticks, spraying 5 times with a spray bottle, repeating the experiment for three times, counting the lethality rate in 24h, and rounding the lethality rate. The aphid used in this example was the aphid radish (Lipophis erysimi).

The data statistical method comprises the following steps: firstly, detecting whether the difference among groups of data is significant by using the one-factor variance, then analyzing the data by using an LSD method, wherein the difference among the groups with different marked letters is significant, and the significance level is P < 0.05.

A large number of experimental results show that when the concentration of the green walnut skin extract is 1mg/ml, 2mg/ml and 10mg/ml, a remarkable concentration gradient effect is presented, and as shown in figure 1, the inhibition rates of the single green walnut skin extract on aphids are respectively 24% (1mg/ml), 36% (2mg/ml) and 74% (10 mg/ml).

Example 2

Cutting fresh plant material herba Thymi 200g into 2-3 cm long segments, extracting essential oil by steam distillation, collecting the essential oil floating on water surface in volatile oil extractor, and storing in brown sealed glass bottle. This process was repeated until sufficient essential oil was obtained.

According to the technical scheme, the thyme essential oil is prepared into different concentrations to test the lethality rate of the thyme essential oil to aphids, and a large number of experimental results show that the thyme essential oil has strong killing activity to the aphids at low concentration. When the concentration is 0.02mg/ml, 0.5mg/ml and 1mg/ml, the corrected lethality rate to aphids is as follows: 20%, 84%, 96%, when the concentration is more than 0.5mg/ml, the killing activity of thyme essential oil on aphid is strong, as shown in figure 2.

Example 3

The preparation method of the peganum harmala alkaloid comprises the following steps:

1) taking a fresh plant peganum harmala with rich alkaloid content, drying in the shade at room temperature for one week, then taking 2kg of stems and leaves dried in the shade, cutting into segments with the length of 2-3 cm, soaking and extracting for three days by using 70-80% ethanol, filtering, collecting filtrate, repeating for three times, combining the filtrate, and carrying out rotary evaporation and concentration to obtain an ethanol crude extract.

2) Dissolving the ethanol extract in 2L of distilled water solution containing 5% hydrochloric acid, and filtering to remove insoluble part; extracting soluble part with chloroform of the same volume for three times, and discarding chloroform phase;

3) adjusting the pH value of the water phase to 9 by ammonia water, adding chloroform for extraction, taking the chloroform phase, and performing rotary evaporation;

The peganum harmala alkaloid extract is prepared into different concentrations to test the lethality of the peganum harmala alkaloid extract to aphids, and a large number of experimental results show that the peganum harmala alkaloid extract has lower lethality to the aphids than thyme essential oil, has certain comparability with the action strength of walnut skin and is slightly stronger than the walnut skin extract. When the concentration is 0.2mg/ml, 1mg/ml and 5mg/ml, the corrected lethality rate is as follows: 8%, 24%, 78%. The results are shown in FIG. 3.

Example 4

The method comprises the following steps: preparing the following formula from a green walnut skin extract (A), thyme essential oil (B) and a peganum harmala alkaloid extract (C) according to the method: i (A1 mg/ml), II (A0.9 mg/ml + B0.02 mg/ml + C0.1 mg/ml), III (A0.8 mg/ml + B0.02 mg/ml + C0.2 mg/ml), IV (A10 mg/ml), V (A6 mg/ml + B0.3 mg/ml + C1.5 mg/ml), VI (A4 mg/ml + B0.5 mg/ml + C2 mg/ml).

As a result: the aphid has lower influence on the aphid under the action of the green walnut peel ethanol extract with extremely low concentration (I), but the lethality of the green walnut peel ethanol extract with the same concentration is approximately doubled after a small amount of essential oil and alkaloid are added (II, III). At slightly higher concentrations of the ethanol extract of the green walnut skin (V), the effect is much higher than at lower concentrations, and the corrected lethality rate continues to increase with increasing concentrations of added essential oils and alkaloids (V, VI). The results are shown in FIG. 4.

Example 5

The field spraying effect is verified on the basis of the culture dish experiment result, and the following pesticide formula is prepared: VII (A10 mg/ml), VIII (A6 mg/ml + B0.3 mg/ml + C1.5 mg/ml), VIX (A4 mg/ml + B0.5 mg/ml + C2 mg/ml), the above solutions were filled in small spray bottles. Selecting three solanum nigrum plants infected by aphids, selecting a certain number of aphids on the back of leaves to spray, so that the insecticide solution is uniformly distributed on the bodies of the three solanum nigrum plants, repeating the experiment for three times, and counting the fatality rate after 24 hours. The results are shown in FIG. 5.

As a result: group VII only uses a single component of the green walnut peel ethanol extract with the concentration of 10mg/ml, and the insecticidal effect does not reach half-lethal; in the VIII and VIX groups, the ethanol extract of the green walnut skin is still used as the main component, but the concentration of the ethanol extract is reduced to 4-6mg/ml, and simultaneously, the plant essential oil with the concentration of 0.3-0.5mg/ml and the alkaloid with the concentration of 1.5-2mg/ml are added, so that the total concentration of the three components is less than 10mg/ml, and the obtained insecticidal effect is far better than that of the VII group. The concentration of essential oil and alkaloid is continuously increased, the concentration of the walnut peel extract is reduced, the effect is continuously increased, and the insecticidal effect is optimal and is 91% under the condition of treating VIX. The field spraying can also have the influence of other factors, so the effect of the field spraying and the effect of a culture dish have certain difference, but the overall trend is almost the same.

Example 6

Or the pesticide which takes the green walnut skin extract, the thyme essential oil and the peganum harmala alkaloid extract as main raw materials can be prepared into a commercial chemical product pesticide, and the preparation method comprises the following steps:

1) dissolving alkaloid and essential oil in a solvent, and then adding an emulsifier to obtain an aqueous emulsion oil phase;

2) dissolving the green walnut ethanol extract in water, and then adding an antifreeze agent and a defoaming agent to obtain an aqueous phase of the aqueous emulsion;

3) the aqueous phase and the oil phase of the aqueous emulsion are stirred and mixed, and a tan homogeneous solution, namely the plant extract pesticide, can be prepared by using ultrasonic wave for assistance.

According to the mass fraction, the plant extract pesticide comprises 0.5-3% of emulsifier, 1-5% of antifreeze agent and 0.2-0.5% of defoaming agent.

Wherein the solvent is: one or more of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, acetone, etc.

Wherein the emulsifier is: tween 20, tween 80, glycerol lauric acid, OP-10 and the like.

Wherein the antifreeze agent is: one or more of glycerol, propylene glycol, ethylene glycol, urea, 1, 2-butanediol, calcium chloride, sodium chloride, etc.

Wherein the defoaming agent is: one or more of emulsified silicone oil, organic silicon, mineral oil, tributyl phosphate and the like.

Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims

1. A plant extract pesticide is characterized in that the pesticide comprises a green walnut skin extract, thyme essential oil and a peganum harmala alkaloid extract.

2. The plant extract pesticide as claimed in claim 1, wherein in the pesticide, the green walnut skin extract is 0.8-10mg/ml, the thyme essential oil is 0.02-0.5mg/ml, and the peganum harmala alkaloid extract is 0.1-3.5mg/ml by mass volume concentration.

3. The plant extract pesticide as claimed in claim 2, wherein in the pesticide, the green walnut skin extract is 4-6mg/ml, the thyme essential oil is 0.3-0.5mg/ml and the peganum harmala alkaloid extract is 1.5-2mg/ml by mass volume concentration.

4. The botanical extract pesticide as claimed in any of claims 1 to 3, wherein the preparation method of the green walnut skin extract is:

1) drying fresh green walnut skin, and pulverizing into powder;

5. A plant extract insecticide as claimed in any one of claims 1 to 3, wherein said thyme essential oil is prepared by: cutting fresh thyme, extracting essential oil by steam distillation, and collecting the essential oil floating on water surface.

6. A plant extract pesticide as claimed in any one of claims 1 to 3 wherein the peganum harmala alkaloid extract is prepared by a process comprising:

7. The plant extract pesticide according to claim 1, wherein the plant extract pesticide further comprises a solvent, an emulsifier, an anti-freeze agent and an anti-foaming agent.

8. The plant extract pesticide as claimed in claim 7, wherein the solvent is one or more of ethanol, chloroform, dichloromethane, petroleum ether, methanol, ethyl acetate, acetone, etc.; the emulsifier is one or a combination of more of Tween 20, Tween 80, glycerol lauric acid, OP-10 and the like; the antifreeze is one or a combination of more of glycerol, propylene glycol, ethylene glycol, urea, 1, 2-butanediol, calcium chloride, sodium chloride and the like; the defoaming agent is one or a combination of more of emulsified silicone oil, organic silicon, mineral oil, tributyl phosphate and the like.

9. The plant extract pesticide as claimed in claim 7, wherein the plant extract pesticide comprises 0.5-3% of emulsifier, 1-5% of antifreeze agent and 0.2-0.5% of defoaming agent by mass fraction.