CN112841228B - Application of Huaxuedan in aspects of killing mites and pests, biological control medicament and preparation method thereof - Google Patents

Application of Huaxuedan in aspects of killing mites and pests, biological control medicament and preparation method thereof Download PDF

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CN112841228B
CN112841228B CN202110033679.4A CN202110033679A CN112841228B CN 112841228 B CN112841228 B CN 112841228B CN 202110033679 A CN202110033679 A CN 202110033679A CN 112841228 B CN112841228 B CN 112841228B
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huaxuedan
mites
biological control
pests
essential oil
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CN112841228A (en
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刘志龙
权美蓉
刘奇志
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China Agricultural University
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China Agricultural University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/12Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N27/00Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/02Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aliphatically bound aldehyde or keto groups, or thio analogues thereof; Derivatives thereof, e.g. acetals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/06Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing keto or thioketo groups as part of a ring, e.g. cyclohexanone, quinone; Derivatives thereof, e.g. ketals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Agronomy & Crop Science (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Biotechnology (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pest Control & Pesticides (AREA)
  • Botany (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to application of Huaxuedan in the aspects of mite killing and insect killing, a biological control medicament and a preparation method thereof, belonging to the field of biological control. The invention relates to application of Huaxuedan in the aspects of killing mites and insects, and a biological control medicament based on Huaxuedan essential oil. The biological control agent can efficiently kill harmful mites and storage pests, and is nontoxic, harmless, safe, reliable and low in cost.

Description

Application of Huaxuedan in aspects of killing mites and pests, biological control medicament and preparation method thereof
Technical Field
The invention belongs to the technical field of biological control, and relates to application of Huaxuedan in mite killing and insect killing, a biological control medicament and a preparation method thereof.
Background
In the process of grain storage, the harm of pests and mites is the most important factor influencing grain safety. The grain loss caused by the pest and mite damage accounts for 4-6% of the total stored grain amount in China every year, and is about 325 million yuan in terms of RMB. Besides causing serious economic loss, the pests and mites can increase wormhead grains, reduce the germination rate, even cause the heating and mildewing of grains, and greatly reduce the commodity value and the edible value of the grains.
At present, methods for controlling pests and mites mainly comprise a physical and mechanical control method and a chemical control method. The physical and mechanical prevention, namely the habit prevention and control method for preventing and controlling pests by utilizing the habit of pests, is a method for killing pests and mites or worsening the living environment of the pests and mites by utilizing a physical method and inhibiting the occurrence and development of the pests and mites or separating the pests from grains by adopting a mechanical method and preventing or reducing the pests. The chemical prevention method is a method for preventing and controlling pests and mites in stored grains by utilizing an insecticide. The chemical prevention and control method has the advantages of rapid and thorough insecticidal effect, wide insecticidal spectrum, low treatment cost, capability of carrying out insecticidal treatment without moving grains, labor saving and less influence by factors such as climate and the like. The chemical control method has the disadvantages that the pesticide is toxic to human and higher animals, can bring different degrees of pollution to grains, and is easy to cause the pests to generate drug resistance. Even so, chemical control is currently the most cost effective means of killing pests.
Due to the weakness and long-term unreasonable abuse of chemical pesticides, pests have resistance to the chemical pesticides, and the chemical pesticides pollute the environment in the process of using a large amount of pesticides, destroy the ecological balance of the nature, harm the health of human bodies and seriously affect our lives. Therefore, plant-derived pesticides are receiving attention from the world pesticide world today where environmental protection is increasingly important, and provide a wide development space for the development of environment-friendly pesticides. The botanical pesticide is a substance extracted from plants and having pesticide activity, and the active substance can become an effective matrix of an innovative pesticide and is further developed and developed into a new pesticide. Compared with chemical pesticides, the botanical pesticide has the advantages that the active ingredients are easily decomposed into inactive substances and cannot be accumulated in the bodies of pests, so that the botanical pesticide is not easy to cause harm to other beneficial insects or natural enemies of the pests, and helps to protect the ecological environment.
The XUEDAN is Ligularia lapariifolia belonging to Ligularia of Compositae, Latin name Ligularia lapathifolia, and perennial herb. Fleshy, mostly, thick and long, about 5mm in diameter. The stem is upright, up to 120 cm, the upper part and inflorescence are coated by white spider-silk soft hair and short soft hair with nodes or old depilation, the lower part is smooth, the strip edge is obvious, the diameter of the base part is 0.8-1.5 cm, and the base part is surrounded by dead petiole fiber. The bush leaves and the leaves at the lower part of the stem have stems, the leaves at the middle upper part of the stem are gradually reduced upwards, the stem is not provided with a stem, the stem is embraced in a sheath shape, and the leaves are oval-shaped or oval-shaped and needle-shaped. Development or cluster-like development of the umbrella-house-like inflorescence; the bracts and the small bracts are in a linear drill shape and are extremely small; the capitate inflorescences are radial, usually 6-23, more rare, yellow in the tongue and oblong in the shape of a linear tongue. The lean fruit is long and round, and the period of the flower and fruit is 7-10 months.
At present, no report that the Huaxuedan can be used for killing pests in the field of biological control exists in the field.
Disclosure of Invention
In light of the above-described needs and gaps in the art, the present invention provides a method and a medicament that are safe and non-toxic to humans and animals, environmentally friendly, and effective in controlling pests and mites.
The technical scheme claimed by the invention is as follows:
the usage of Huaxuedan in killing mite and pest is disclosed.
The mites are harmful mites, and the pests are storage pests or agricultural pests;
preferably, the pest mites are tetranychus urticae;
preferably, the stored pests are selected from the group consisting of booklice;
preferably, the agricultural pest is selected from thrips occidentalis.
The acaricidal and insecticidal mode is contact killing or fumigating killing.
The application of the huaxuedan in the aspects of killing mites and insects is characterized in that the huaxuedan essential oil is adopted to kill the mites and the insects.
The application of the Huaxuedan in preparing the biocontrol medicine.
A biological control medicament is characterized in that the active component of the biological control medicament is Huaxuedan essential oil.
The biological control agent is selected from acaricide, and/or insecticide, and/or biological pesticide;
preferably, the acaricidal and insecticidal active ingredients of the Huaxuedan essential oil are 1, 8-cineole, (+) -nopinone, limonene and phellinus aldehyde.
A method for preparing biological control medicament, wherein it is to decoct and extract the pill of transforming blood to get final product.
The water boiling method is used for treating for 8-12 hours to obtain an oil-water mixture;
preferably, the extraction refers to extracting the oil-water mixture obtained by distillation with n-hexane;
preferably, the temperature of the water bath for extraction is 35-45 ℃, preferably 40 ℃;
preferably, the Huaxuedan is cut into pieces and soaked before distillation;
preferably, the Huaxuedan is cut, soaked and boiled in water for 8-12h, preferably 10 h.
Preferably, the mixture obtained by extraction is dried and then n-hexane is removed by evaporation;
preferably, the drying refers to drying with anhydrous sodium sulfate;
preferably, the evaporation refers to evaporation at 40-45 ℃ by using a rotary evaporator.
The invention relates to application of a hematite to prevention and control of pest mites.
The application of the Huaxuedan in preparing the product for preventing and controlling the pests and mites.
The application of the volatile oil of the Huaxuedan in preventing and controlling pests and mites.
The blood-dissolving pill total volatile oil is prepared by using blood-dissolving pills as raw materials and adopting a distillation method.
The application of the Huaxuedan total volatile oil in the medicament for preventing and controlling pests and mites is characterized in that the medicinal component of the medicament is the Huaxuedan total volatile oil.
The Huaxuedan total volatile oil is prepared by adopting a distillation method.
The boiling method comprises the steps of boiling, extracting, dehydrating and evaporating the solvent.
The pesticide for preventing and controlling pests and mites is characterized in that the pesticide effect component of the pesticide is Huaxuedan total volatile oil.
The pesticide for preventing and controlling pests and mites is characterized in that the pesticide effect component of the pesticide comprises the total volatile oil of Huaxuedan.
A method for controlling pests and mites, which is characterized by comprising the following steps:
the odor substances in the blood-dissolving pill material are diffused into the grain storage space to be prevented and treated,
The total volatile oil of the Huaxuedan volatilizes or fumigates in the grain storage space to be prevented and treated,
the total volatile oil of the Huaxuedan is sprayed on places, grains or grain storage containers where pests and mites are likely to occur.
Can be prepared into products for preventing and controlling the pests and the mites in various forms according to the requirements, and is used for preventing and controlling the pests and the mites in different scales.
Through further research, the effect of controlling pests and mites is better by using the total volatile oil extracted from the Huaxuedan as the raw material. The research of the invention shows that the total volatile oil extracted from the Huaxuedan has obvious contact poisoning and fumigation activity on pests and mites, and can prevent and reduce the damage of the pests on stored grains. The total volatile oil of the Huaxuedan is used as a natural insecticidal active substance, the activity of the volatile oil disappears or is decomposed by microorganisms after the volatile oil is used, the volatile oil does not pollute grains and the environment, is safe to people and livestock, and can be directly applied to the control of pests and mites; the total volatile oil of the Huaxuedan is extracted from plants, the active ingredients are complex and diverse, and the action mechanisms of the volatile oil are different when the volatile oil acts on a target organism, so that the target organism is difficult to generate drug resistance on each ingredient, and a lasting prevention and treatment effect is obtained; compared with chemical pesticides, the effective components of the total volatile oil of the Huaxuedan are easy to decompose after killing pests, and cannot accumulate in the pests, so that the total volatile oil is not easy to cause harm to other beneficial insects or natural enemies of the pests, and the ecological environment is protected.
In some embodiments of the invention, the Huaxuedan total volatile oil is prepared by a water boiling method.
In some embodiments of the invention, the poaching process includes the steps of poaching, extraction, dehydration, and solvent evaporation.
In one embodiment of the invention, the Huaxuedan total volatile oil is prepared by the following preparation method: chopping 8kg of the minium, soaking, fully soaking, treating for 8-12h by using a water boiling method, extracting an obtained oil-water mixture by using normal hexane, dehydrating an extracted substance by using anhydrous sodium sulfate, evaporating and concentrating in a water bath kettle at 40-45 ℃ under reduced pressure by using a rotary evaporator, and recovering normal hexane to obtain a residual oily liquid, namely the total volatile oil of the minium. The preparation method is simple, the cost of the required reagent is low, the mass production is facilitated, and the large-scale prevention and control of pests and mites are facilitated.
In other embodiments of the present invention, the pesticide for controlling pest and mite contains the total volatile oil of Huaxuedan.
According to the technical common knowledge of the skilled in the art, the above-mentioned agent for controlling pests and mites of the present invention can also be added with some plant volatile oil or other kinds of chemical substances known to those skilled in the art to have activity of killing pests and mites.
The pesticide for preventing and controlling pests and mites can be used for preventing and controlling the booklice in stored grains. Indoor toxicity measurement shows that the Huaxuedan total volatile oil has obvious insecticidal effect on the capreopsis though. Since the total volatile oil of the Plumbum preparatium is the total volatile oily components extracted from ligularia lappaca of Compositae, the effective components are complex, the number of action sites is large, the drug resistance of the booklice is not easy to generate, and the long-term effective prevention and treatment effect can be achieved.
The invention also provides a method for preventing and controlling pests and mites. The method is characterized in that: the odor substances in the material of the blood-dissolving pill are diffused into the grain storage space to be controlled, the total volatile oil of the blood-dissolving pill is volatilized or fumigated in the grain storage space to be controlled, and/or the total volatile oil of the blood-dissolving pill is sprayed on places, grains or grain storage containers where pests and mites are likely to occur. The product for preventing and treating the pests and the mites, which is prepared from the Huaxuedan, can be selected according to the actual factors such as the size of the grain storage space, the propagation speed of the pests and the mites, the grain storage environment temperature and the like, and the prevention and the treatment of the pests and the mites are carried out by adopting a proper method.
In conclusion, the pesticide for preventing and treating pests and mites belongs to botanical pesticides, is easy to decompose, does not pollute the environment, and is safe to people and livestock; the effective component of the composition is the total volatile oil of the Xuedan, has multiple action mechanisms on pests, is not easy to cause the pests to generate drug resistance, and can be used for a long time; the pesticide loses activity after being killed, cannot be accumulated in the body of pests, and protects the ecological environment; the preparation method is simple and easy to implement, has low raw material cost, is suitable for large-scale production, and can be widely used for preventing and controlling pests and mites.
Blood-dissolving pill total volatile oil: the invention is also called 'Huaxuedan essential oil', which refers to a volatile oil mixture extracted by using Huaxuedan as a raw material and adopting a conventional method for extracting total volatile oil of plants commonly used in the field, and the components of the volatile oil mixture can be different according to the different extraction processes adopted by a person skilled in the art.
The invention also discloses application of the hematite in preventing and controlling pests and mites.
The invention provides application of Huaxuedan in preventing and treating pest and pest mites, and can use products in various forms to prevent and treat the pest and pest mites by various methods according to actual needs. The following description is by way of example only and is not intended as a limitation on the use of the composition for controlling pest mites. The skilled person can implement various possible applications according to the technical solutions of the present invention and the knowledge of the prior art.
The application of the hematite in controlling pest mites is illustrated as follows:
1. when the stored grain is not harmed by pests and mites: the solid or semisolid medicament prepared from the blood dissolving pill can be adopted, and the medicament is placed at the four corners and the middle part of the grain storage space (the medicament is uniformly placed according to the actual size of the grain storage space), so that the odor substances in the blood dissolving pill material are slowly diffused into the grain storage space to be prevented and treated, and the grain storage is durably protected.
2. When the stored grain is damaged by pests and mites: the liquid preparation prepared from the Huaxuedan can be adopted, and the method of natural volatilization, artificial fumigation or spraying is adopted according to the damage of pests, so that the total volatile oil of the Huaxuedan is volatilized into the whole grain storage space, the pests and mites are quickly killed, and the damage is reduced to the minimum degree; after the pest and mite are completely killed, the solid or semisolid medicament prepared from the Huaxuedan is used for preventing the secondary harm of the pests for a long time.
3. When the environmental temperature of grain storage is low: the liquid preparation prepared from the Huaxuedan can be adopted, and the method of natural volatilization, artificial fumigation or spraying is adopted, so that the total volatile oil of the Huaxuedan is volatilized into a grain storage space, and the pest and acarid can be prevented.
4. When the environmental temperature of grain storage is high: the solid or semisolid preparation prepared from the Huaxuedan can be uniformly distributed in the grain storage space to prevent and control pests and mites.
Detailed Description
The present invention is described below with reference to specific examples, which are intended to be illustrative and illustrative only and are not to be construed as limiting the scope of the present invention.
Sources and access routes of test materials
Psyllid: the insect line of the Chinese university of agriculture is artificially raised, the laboratory has a storage, and the applicant declares that the necessary verification test can be issued to the public within twenty years from the application date.
The frankliniella occidentalis and the tetranychus urticae are both artificially fed in the laboratory of the applicant,
blood-resolving pill: bought from cloud medicine net
Huaxuedan essential oil: the method is suitable for leaching the medicinal material components which have volatility, can be distilled along with water vapor without being damaged, and are stable in water and insoluble or insoluble in water.
The method for preparing the Huaxuedan essential oil is as in experimental example 1. The experimental reagents which are not particularly described in the invention are all conventional reagents in the field, or are prepared by adopting conventional methods in the field, can be obtained commercially, and have the specification of laboratory pure grade.
Group 1 example, New use of Huaxuedan for biological prevention and treatment
The group of embodiments provides the application of the huaxuedan in the aspects of killing mites and insects.
In particular embodiments, the mite is a pest mite, and the pest is a storage pest or an agricultural pest;
preferably, the pest mites are tetranychus urticae;
preferably, the stored pests are selected from the group consisting of booklice;
preferably, the agricultural pest is selected from thrips occidentalis.
In some embodiments, the control refers to killing;
in other embodiments, the killing mode is contact killing or fumigation.
In a further embodiment, the Huaxuedan essential oil is used for killing mites and insects.
Group 2 examples biocontrol pharmaceutical use of Huaxuedan
The present group of embodiments provides the use of Huaxuedan for the preparation of a biological control medicament.
In particular embodiments, the biocontrol agents include, but are not limited to: insecticides, acaricides.
More specifically, the biocontrol agents may be formulated into dosage forms conventional in the art, including but not limited to: powders, wettable powders, drops, suspension concentrates, emulsifiable concentrates, sprays, aerosols, baits, mosquito-repellent incense, sticking agents, smoke agents, insecticidal coatings and the like.
Group 3 examples of biocontrol agents of the invention
The present group of embodiments provides a biological control agent. All embodiments of this group share the following common features: the active component of the biological control medicament is Huaxuedan essential oil.
In particular embodiments, the dosage form of the biocontrol agent is selected from an acaricide or insecticide, and/or, a biopesticide;
preferably, the active ingredients of the Huaxuedan essential oil comprise: the following ingredients in table 1 were identified as insecticidal active ingredients: 1, 8-cineole, (+) -nopinone, limonene, phellandrene.
In further embodiments, the biocontrol agent further comprises a pesticide art-acceptable adjuvant common in the art, including but not limited to: emulsifiers, organic solvents, fillers, wetting agents, diluents, and the like.
Group 4 examples preparation of the biocontrol agents of the present invention
The present group of embodiments provides a method of preparing a biological control agent. All embodiments of this group share the following common features: the preparation method comprises the following steps: distilling and extracting the Huaxuedan to obtain the finished product.
In a specific embodiment, the water boiling method is used for distilling for 8-12h to obtain an oil-water mixture;
preferably, the extraction refers to extracting the oil-water mixture obtained by distillation with n-hexane;
preferably, the temperature of the water bath for extraction is 35-45 ℃, preferably 40 ℃;
preferably, the minium is cut up and soaked before the water boiling, so that essential oil can be obtained as much as possible;
preferably, the water cooking treatment is carried out for 10 hours
Preferably, the mixture obtained by extraction is dried and then n-hexane is removed by evaporation;
preferably, the drying refers to drying with anhydrous sodium sulfate;
preferably, the evaporation refers to evaporation at 40-45 ℃ by using a rotary evaporator.
Experimental example 1 preparation method of Huaxuedan essential oil
In the present invention, a method for extracting Huaxuedan essential oil is provided, but the method is not limited to the method for extracting Huaxuedan essential oil, which is only used for achieving the purpose of the present invention.
Cutting 8kg of XUEDAN plant (dried plant purchased from Yunyao medicinal net, unprocessed), distilling with water for 8-12h, extracting the obtained oil-water mixture with n-hexane, dehydrating the extract with anhydrous sodium sulfate, concentrating by rotary evaporator under reduced pressure in a 40-45 deg.C water bath, recovering n-hexane, and collecting the residual oily liquid, i.e. XUEDAN volatile oil.
Experimental example 2 GC-MS detection of Huaxuedan essential oil
The Huaxuedan essential oil prepared in example 1 is sent to the GC center of Beijing university.
An Agilent6890N gas chromatograph and an Agilent5973N mass spectrometer were used.
HP-5MS30mm × 0.25mm × 0.25 μm quartz capillary column, initial column temperature 60 deg.C maintained for 1 min, programmed temperature up to 180 deg.C at a rate of 12 deg.C/min maintained for 0.5 min, programmed temperature up to 280 deg.C at a rate of 25 deg.C/min maintained for 18 min, vaporizer temperature 280 deg.C, carrier gas helium, column flow 1.0mL/min, split ratio 1: 10.
The ionization mode EI of the mass spectrum has the electron bombardment energy of 70eV, the scanning mass range of 20-550m/z and the scanning time of 2 seconds.
Sampling 1 mu L (500 times of n-hexane diluent) of the Huaxuedan plant essential oil, analyzing and identifying by using a gas chromatography-mass spectrometer, searching a Nist05 standard mass spectrum library by using an HP-MSD chemical workstation, and detecting and identifying 33 peaks by combining related documents. The results of the evaluation are shown in Table 1 below.
TABLE 1 chemical composition of Huaxuedan essential oil
Figure BDA0002893306440000071
Figure BDA0002893306440000081
The reason why the total percentage of all the components identified in Table 1 is less than 100% is that the known components still exist in Huaxuedan essential oil, which may be new compounds, cannot be identified by the existing GC-MS detection method.
Experimental example 1 indoor toxicity measurement of Huaxuedan essential oil against Toddalia chinensis
1. Touch killing activity assay for Torulopsis
Acetone as solvent, diluting the medicine in equal proportion into 5 concentration gradients, and using acetone as blank control. Preparing circular filter paper with the diameter of 3.5cm, sucking 150ul of liquid medicine by using a liquid transfer gun, uniformly dropwise adding the liquid medicine on the filter paper, naturally volatilizing for 2min, adhering the filter paper to the bottom of a six-hole culture plate with the inner wall coated with polytetrafluoroethylene (for preventing test insects from escaping), inoculating the psyllids to the culture plate by using a zero-size writing brush, wherein 10 heads are arranged in each hole, each concentration is 4 times, and each concentration is 10 times of test insects, and the culture plate is placed in an artificial culture box (28-30 ℃, 70-75% RH). After 24 hours, the death of the test insects was observed and recorded.
The mortality rate (%). is 100 x dead number/test number.
Corrected mortality (%) -100 × (treatment-control mortality)/(1-control mortality).
The semi-lethal dose (LD50), i.e., the dose that caused 50% mortality of adult booklice adults, was calculated using the Probit software package and is shown in Table 2.
2. Measurement of fumigating Activity of Tolyphacida
Acetone is used as solvent, and the medicine is diluted into 5 concentration gradients in equal proportion. For one repeat treatment, a 25ml ampoule was prepared and the upper half of the ampoule was coated with Teflon. The psyllids were transferred with a writing brush into small ampoules, 10 specimens per vial, and the vials containing the specimens were placed into 290ml jars. Adhering filter paper (1 × 8cm) on the bottle cap of the wide-mouth bottle, sucking 10ul of medicinal liquid with a liquid-transferring gun, dripping on the filter paper, rapidly covering, and sealing with sealing film. Each concentration is 4 times, each time 10 times of test insects are repeated, and the test insects are placed in an artificial incubator (28-30 ℃ and 70-75% RH). Acetone without medicament is used as a blank control, and dichlorvos is used as a positive control. After 24 hours, the death of the test insects was observed and recorded. Because the hemiplegy booklice have false death, the test insects should be poured into a culture dish when the death situation is observed, and the death is determined when the insects do not move after standing for 5 min. The respective calculated mortality, corrected mortality and semi-lethal doses are shown in table 5 below.
3. Tetranychus urticae contact killing activity determination
The method adopts a leaf disc method to carry out experiments on tetranychus urticae, and comprises the following specific operations: coating polytetrafluoroethylene on the inner wall of the culture plate, and drying by electric air blowing; heating water and agar at a ratio of 100:1.5 in a microwave oven, mixing, pouring into 12-hole cell culture plate with a height of about 0.5mm, and cooling to solidify; taking fresh kidney bean leaves without pesticide, and punching the leaves by using a puncher with the diameter of 19mm to prepare a circular leaf disc; dissolving certain amount of HUAXUEDANJING oil with anhydrous ethanol (amount not more than 2% of the medicinal liquid system), adding dimethyl sulfoxide (not more than 1% of the medicinal liquid system) for dissolving to obtain mother liquor, diluting with distilled water to desired concentration to obtain medicinal liquid system, and setting 5 groups of concentrations. And (3) soaking the leaf disc in the medicament for 10s, taking out, drying in the air, placing the kidney bean leaves soaked with the liquid medicament on a culture plate poured with agar with the back face facing upwards, and inoculating 10 tetranychus urticae into each hole to form the mite. Firmly sticking the porous surface of the culture plate by rice paper, and putting the culture plate into an incubator at the temperature of 26-28 ℃, the relative humidity of 65-75% and the photoperiod L: D of 16: 8; observing and recording death number under the stereoscope after 24h, determining that the person who touches with the brush pen is alive and the person who does not touch is dead, and calculating LD50. The results are shown in Table 3.
4. Frankliniella occidentalis poisoning Activity assay
Dissolving a certain amount of Huaxuedan essential oil in anhydrous ethanol (the amount is not more than 1% of the liquid medicine system), adding Tween 80 (not more than 0.5% of the liquid medicine system) for assisting dissolution, preparing a mother solution, and diluting with distilled water to a required concentration to obtain the liquid medicine system for later use; putting 1mL of liquid medicine into a glass ampoule with the volume of 22mL, uniformly rolling for a plurality of circles to form a medicine film, pouring out the liquid medicine, and airing for later use. Taking fresh hyacinth beans without pesticide, preparing the hyacinth beans into a long section of 1cm square, immersing the hyacinth beans into the pesticide for 10s, taking out the hyacinth beans, airing the hyacinth beans, and placing the hyacinth beans in an ampoule; setting 5 repetitions for each treatment, repeatedly inoculating second-instar nymphs of 10 Frankliniella occidentalis, and sealing the bottle mouth with a 150-mesh insect-proof net; and (5) placing the worm body at room temperature, observing the result after 24h, and stirring the worm body with a writing brush, wherein the worm body is recorded as dead after being immobilized. The results are shown in Table 4.
TABLE 2 test data of contact killing and death of essential oil of Huaxuedan according to the invention against Toxoplasma psyllium
Figure BDA0002893306440000091
Figure BDA0002893306440000101
The semi-lethal dose LD50 in table 2 has the meaning: the amount of the agent required for half-death of the psyllids by the mode of action of contact killing within 24 hours is 525.36ug per square centimeter of the area of the plane in which the psyllids are located.
Table 3, lethal test data of the essential oil of Huaxuedan of the invention on Tetranychus urticae Koch
Figure BDA0002893306440000102
Table 4, lethality test data of Huaxuedan essential oil of the invention on Frankliniella occidentalis
Figure BDA0002893306440000111
The meanings of the semi-lethal dose LC50 in table 3 above to table 4 are: within 24 hours, the death rate of the tested individual can reach 50 percent by treating the medicinal liquid system (taking alcohol, dimethyl sulfoxide and distilled water as solvents) with the concentration of milligrams of the Huaxuedan essential oil in each milliliter of the medicinal liquid system.
TABLE 5 lethality test data of Huaxuedan essential oil of the present invention on fumigation of Toxoplasma psyllid
Figure BDA0002893306440000112
Figure BDA0002893306440000121
The semi-lethal dose LC50 in table 5 has the meaning: within 24 hours, when 0.82mg of Huaxuedan essential oil is contained in each liter of closed space, the death rate of the booklice can reach 50 percent.
As is well known in the art, only 5 to 6 effective concentrations are required in toxicological tests, and at this concentration, the individual having the insect die, and the concentrations at 100% and 0% mortality cannot be counted as effective concentrations, so that the semi-lethal dose for killing mites and insects was determined in this experimental example based on 5 series of concentrations (each concentration is set to 4 to 5 replicates) listed in tables 3 to 5, respectively.

Claims (13)

1. The application of the minium essential oil in the aspects of killing mites and insects, wherein the mites are tetranychus urticae, and the insects are ticks or frankliniella occidentalis; the acaricidal and insecticidal active ingredients of the Huaxuedan essential oil comprise: 1, 8-cineole, (+) -nopinone, limonene, phellandrene; the Plumbum preparatium is ligularia lappaca of ligularia of Compositae.
2. The use of the huaxuedan essential oil in the aspect of killing mites and insects according to claim 1, characterized in that the mode of killing mites and insects is contact killing or smoking killing.
3. Use of Huaxuedan essential oil for the preparation of a biocontrol agent selected from the group consisting of acaricides or insecticides; the mite is tetranychus urticae, and the mite is a booklice or thrips occidentalis; the acaricidal and insecticidal active ingredients of the Huaxuedan essential oil comprise: 1, 8-cineole, (+) -nopinone, limonene, phellandrene; the Plumbum preparatium is ligularia lappaca of ligularia of Compositae.
4. A biological control agent is characterized in that the active component is Huaxuedan essential oil; the biological control agent is acaricide or insecticide; the mite is tetranychus urticae, and the mite is a booklice or thrips occidentalis; the acaricidal and insecticidal active ingredients of the Huaxuedan essential oil comprise: 1, 8-cineole, (+) -nopinone, limonene, phellandrene; the Plumbum preparatium is ligularia lappaca of ligularia of Compositae.
5. A method for preparing biological control medicament, wherein to dissolve the red lead to carry on the water boiling and extract to get final product; the biological control agent is acaricide or insecticide; the mite is tetranychus urticae, and the mite is a booklice or thrips occidentalis; the water boiling method is used for treating for 8-12 hours to obtain an oil-water mixture, and the extraction refers to extracting the oil-water mixture obtained by distillation by using normal hexane; the Plumbum preparatium is ligularia lappaca of ligularia of Compositae.
6. The process of claim 5, wherein the temperature of the aqueous bath used for the extraction is 35-45 ℃.
7. The process of claim 6, wherein the temperature of the aqueous bath for extraction is 40 ℃.
8. The method of claim 5, wherein the pill is chopped and soaked before distillation.
9. The method for preparing a biological control medicament according to claim 8, wherein the Huaxuedan is cut into pieces, soaked and boiled in water for 8-12 h.
10. The method for preparing a biological control medicament according to claim 9, wherein the Huaxuedan is cut into pieces, soaked and boiled in water for 10 hours.
11. The process for the preparation of a biocontrol agent as in any of claims 5-7 wherein the mixture obtained from the extraction is dried and then evaporated to remove n-hexane.
12. The process according to claim 11, wherein the drying is carried out using anhydrous sodium sulfate.
13. The process according to claim 11, wherein the evaporation is carried out at 40-45 ℃ using a rotary evaporator.
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Citations (1)

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CN1762436A (en) * 2005-10-07 2006-04-26 张益群 Externally applied medicine of Ligularia lapathifolia

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