CN111685133A - Plant protective agent, preparation method and application thereof - Google Patents
Plant protective agent, preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, 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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/12—Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/18—Euphorbiaceae [Spurge family], e.g. ricinus [castorbean]
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/32—Ranunculaceae [Buttercup family], e.g. hepatica, hydrastis or goldenseal
Abstract
The invention relates to a plant protective agent, a preparation method and application thereof, wherein the plant protective agent comprises a raw material medicine and an auxiliary agent, and the mass ratio of the raw material medicine to the auxiliary agent is 2: 3-3: 1; the raw material medicaments comprise the following components in percentage by mass: 20-45% of the pulsatilla extract, 10-30% of the chloranthus japonicus extract, 15-25% of the clematis chinensis extract, 12-25% of the pyrrosia brevifolia extract and 10-20% of the euphorbia lathyris extract. The plant protective agent has the insecticidal effect on pine moth of more than 97 percent and has the same drug effect as deltamethrin accounting for 2.5 percent of pesticide; the larch forest belt in the Qinling mountain forest area is positively protected; the killing power of the plant protective agent to the natural enemy insect, namely the pine moth black egg bee of the pine moth is far less than that of a pesticide; in addition, the plant protective agent provided by the invention has the advantages that the raw materials are all from abundant plant resources in Qinling mountains, the raw materials are easy to obtain, the residual period of the plant protective agent is short, and the damage to the ecological environment of Qinling mountains is small.
Description
Technical Field
The invention belongs to the technical field of plant protection, and particularly relates to a plant protective agent, a preparation method and application thereof.
Background
The Qinling mountains belong to a deciduous leaf forest zone in a warm temperature zone and an evergreen deciduous leaf mixed forest zone in a northern subtropical zone, and the area of a forest land accounts for 54 percent of the total area of the forest land in Shaanxi province, and is the most important forest zone in Shaanxi province; most of the trees are secondary forest, and the primary forest is mainly distributed in the mountainous areas with rare people and inconvenient traffic in counties such as Taibai, Zhou Zhi, Fuping, Ning shan and the like. The mountain in Qinling mountain is huge, the natural condition is complex, and the settlers are quite rich in animal and plant resources. The larch forest belt in the Qinling forest region of Shaanxi is one of the main forest belts in Qinling mountains, and the types of larch include Taibai larch (Taibai redwood), Huashansong, Chinese pine and the like; larch caterpillars are an important pest of larch, and are bred for three generations in one year by feeding pine needles, 400 eggs can be laid after adult moths grow, of which 100 can only grow into adults, and the damage to pine trees is great; when the pine tree breaks out, the needles and leaves are eaten, so that the branches and the trunks are burnt with the same fire, and if the branches and the trunks are serious, the pine tree is withered; and the moths have strong migration capability, and can migrate to the outside of the mountain, so that the life of people in nearby villages is influenced.
Although in some areas it may be possible to kill the pine moth by spraying with chemicals during the outbreak, for example with 2.5% deltamethrin, 20% killing pyrethrin, 20% chlorbenzuron No. 1 suspension; however, these chemical agents have a long residual effect period, and thus have a certain effect on animals and plants in Qinling mountains.
In order to avoid the disadvantages of chemical agents, some researches on botanical insecticides and some commercial products of botanical insecticides have been carried out in the prior art. The botanical pesticide is a chemical developed by utilizing plant resources, comprises active ingredients extracted from plants, the plants and compounds and derivatives synthesized according to active structures, and is a botanical preparation which prevents or reduces pests such as diseases, insects, weeds and the like from being harmful to recipient plants after the recipient plants are used according to a certain method by utilizing stable active ingredients contained in certain parts (roots, stems, leaves, flowers or fruits) of the plants. The botanical pesticide has the functions of killing pests and bacteria, no residual damage, no chemical damage and no pollution, and is one ideal pesticide for worker. However, the existing botanical insecticides are mostly used for preventing and treating plant diseases and insect pests of vegetables, tea leaves, traditional Chinese medicinal materials, flower plants and garden plants for urban landscaping, and related researches on larch caterpillars are not provided.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a plant protective agent, a preparation method and application thereof. The technical problem to be solved by the invention is realized by the following technical scheme:
the plant protective agent comprises a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 2: 3-3: 1; the raw material medicine comprises the following components in percentage by mass: 20-45% of the pulsatilla extract, 10-30% of the chloranthus japonicus extract, 15-25% of the clematis chinensis extract, 12-25% of the pyrrosia brevifolia extract and 10-20% of the euphorbia lathyris extract.
Further, the pulsatilla chinensis extract is obtained by cleaning, drying and crushing roots of pulsatilla chinensis, adding 60-70% ethanol for extraction for 1-3 times, 1-2 h each time, recovering a reflux extracting solution under reduced pressure until no ethanol smell exists, adding water for dissolution, extracting for 2-3 times with petroleum ether, combining petroleum ether extracts, concentrating under reduced pressure, and drying a concentrate in vacuum.
Further, the chloranthus japonicus extract is prepared by cleaning, drying and crushing the leaves, stems, roots or whole plants of chloranthus japonicus, and adding 70-80% ethanol for reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, distilling under reduced pressure, concentrating, and vacuum drying the concentrate to obtain the final product.
Further, the caulis akebiae extract is prepared by cleaning, drying and crushing stems of caulis akebiae, adding 80-95% ethanol, soaking for 24-48 hours, and then performing ultrasonic oscillation for 0.5-1 hour; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate.
Further, the giant knotweed extract is obtained by cleaning, drying and crushing the whole plant of the giant knotweed, adding water, decocting for 1-3 times, 1-2 hours each time, and filtering to obtain an extracting solution; mixing the extractive solutions; and adding 70-80% ethanol into the extracting solution, fully dissolving, standing for 12-24 h, taking the upper layer ethanol extract, concentrating under reduced pressure, and drying the concentrate in vacuum to obtain the plant extract.
Further, the euphorbia lathyris extract is prepared by cleaning, drying and crushing the whole plant of euphorbia lathyris, adding 70-80% ethanol, and performing reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain the final product.
Further, the auxiliary agent comprises the following raw materials in percentage by weight: 30-40% of organic solvent, 20-30% of emulsifier, 10-20% of surfactant and 20-30% of water.
Further, the surfactant is a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide and sodium dodecyl benzene sulfonate in a mass ratio of 1:2: 1.
The preparation method of the plant protective agent comprises the following steps:
washing, drying and crushing roots of Chinese pulsatilla roots, adding 60-70% ethanol for extraction for 1-3 times, extracting for 1-2 hours each time, recovering a reflux extracting solution under reduced pressure until no ethanol smell exists, adding water for dissolution, extracting for 2-3 times by using petroleum ether, combining the petroleum ether extracts, concentrating under reduced pressure, and drying a concentrate under vacuum to obtain a Chinese pulsatilla root extract;
cleaning, drying and crushing leaves, stems, roots or whole plants of chloranthus japonicus, and adding 70-80% ethanol for reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, distilling and concentrating under reduced pressure, and vacuum drying the concentrate to obtain chloranthus japonicus extract;
cleaning, drying and crushing stems of akebia quinata, adding 80-95% ethanol, soaking for 24-48 h, and then carrying out ultrasonic oscillation for 0.5-1 h; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
cleaning, drying and crushing the whole plant of the giant knotweed, adding water, decocting for 1-3 times, 1-2 hours each time, and filtering to obtain an extracting solution; mixing the extractive solutions; adding 70-80% ethanol into the extracting solution, fully dissolving, standing for 12-24 h, then taking the upper layer ethanol extract, concentrating under reduced pressure, and drying the concentrate in vacuum to obtain a pyrrosia breynia extract;
cleaning, drying and crushing the whole plant of euphorbia lathyris, adding 70-80% ethanol, and performing reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
uniformly mixing 20-45% of the pulsatilla extract, 10-30% of the chloranthus japonicus extract, 15-25% of the akebia quinata extract, 12-25% of the pyrrosia brevifolia extract and 10-20% of the euphorbia lathyris extract to obtain a raw material medicine; then adding an auxiliary agent consisting of an organic solvent, an emulsifier, a surfactant and water into the raw material medicines, and uniformly mixing to obtain the plant protectant.
The invention also discloses application of any one of the plant protective agents in preventing and treating larch caterpillars.
Compared with the prior art, the invention has the beneficial effects that:
the plant protective agent has the insecticidal effect on pine moth of more than 97 percent and has the same drug effect as deltamethrin accounting for 2.5 percent of pesticide; the killing power of the plant protective agent to the natural enemy insect, namely the trichogramma pine, namely the black bee of the trichogramma pine is far less than that of deltamethrin accounting for 2.5 percent of pesticide; has positive protection effect on larch forest belt in Qinling mountain forest area. In addition, the plant protective agent provided by the invention has the advantages that the raw materials are all from abundant plant resources in Qinling mountains, the raw materials are easy to obtain, the residual period of the plant protective agent is short, the influence on other animals and plants is small, and the damage to the Qinling ecological environment is small.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
The plant protective agent comprises a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 3: 2; the raw material medicine comprises the following components in percentage by mass: 30% of pulsatilla extract, 20% of chloranthus japonicus extract, 20% of clematis chinensis extract, 18% of pyrrosia brevifolia extract and 12% of euphorbia lathyris extract.
The preferable proportioning scheme of the auxiliary agent in the embodiment is as follows: 35% of organic solvent, 25% of emulsifier, 15% of surfactant and 25% of water. All the auxiliary raw materials are calculated by mass fraction.
Wherein the organic solvent can be one or more of methanol, ethanol, propanol, n-butanol, cyclohexanol, diethyl ether, petroleum ether, dichloromethane, chloroform, tetrachloromethane, and ethyl acetate. The following examples are the same and will not be described. Ethanol is preferably used as the organic solvent in this embodiment.
The emulsifier is one or more of polyoxyethylene ester and ether, sodium glyceryl laurate, ethylene oxide propylene oxide copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene and sodium dodecyl sulfate. The following examples are the same and will not be described. Sodium glyceryl laurate is preferably used as the emulsifier in this example.
The surfactant can be anionic surfactant, cationic surfactant, zwitterionic surfactant, and nonionic surfactant; preferably a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide, and sodium dodecylbenzenesulfonate in a mass ratio of 1:2: 1.
The preparation method of the plant protective agent comprises the following steps:
(1) washing root of Pulsatilla chinensis, drying, pulverizing, extracting with 65% ethanol for 2 times (each time for 1.5 hr), recovering reflux extractive solution under reduced pressure until no ethanol smell exists, dissolving in water, extracting with petroleum ether for 3 times, mixing petroleum ether extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Pulsatilla chinensis extract;
(2) cleaning leaves, stems, roots or whole plant of chloranthus japonicus, drying, pulverizing, adding 75% ethanol, reflux extracting for 2 times, each time for 1.5 hr; then mixing the ethanol extracts, distilling and concentrating under reduced pressure, and vacuum drying the concentrate to obtain chloranthus japonicus extract;
(3) cleaning, drying and crushing stems of akebia quinata, adding 90% ethanol to soak the stems for 36 hours, and then carrying out ultrasonic oscillation for 1 hour; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
(4) cleaning whole plant of herba Erodii seu Geranii, drying, pulverizing, decocting in water for 2 times, each for 1.5 hr, and filtering to obtain extractive solution; mixing the extractive solutions; adding 75% ethanol into the extractive solution, dissolving completely, standing for 18h, collecting the upper ethanol extractive solution, concentrating under reduced pressure, and vacuum drying the concentrate to obtain herba Erodii seu Geranii extract;
(5) cleaning whole plant of Euphorbiae Lathyridis semen, drying, pulverizing, adding 75% ethanol, reflux extracting for 2 times, each time for 1.5 hr; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
(6) uniformly mixing 30% of the pulsatilla chinensis extract, 20% of the chloranthus japonicus extract, 20% of the clematis chinensis extract, 18% of the pyrrosia brevifolia extract and 12% of the euphorbia lathyris extract by mass percent to obtain a raw material medicine; and then adding an auxiliary agent into the raw material medicines, and uniformly mixing to obtain the plant protective agent.
The steps (1), (2), (3), (4) and (5) are not necessarily performed in this order, and may be performed in parallel or in other orders, as long as the extraction method of each crude drug is satisfied to extract the corresponding crude drug extract. The following examples are the same and will not be described.
The embodiment also comprises the application of the prepared plant protective agent in controlling larch caterpillars.
Example two
The plant protective agent comprises a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 2: 3; the raw material medicine comprises the following components in percentage by mass: 45% of pulsatilla extract, 18% of chloranthus japonicus extract, 15% of clematis chinensis extract, 12% of pyrrosia brevifolia extract and 10% of euphorbia lathyris extract.
The preferable proportioning scheme of the auxiliary agent in the embodiment is as follows: 30% of organic solvent, 20% of emulsifier, 20% of surfactant and 30% of water. All the auxiliary raw materials are calculated by mass fraction.
In this example, n-butanol was used as an organic solvent; sodium dodecyl sulfate is adopted as an emulsifier; the surfactant is a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide and sodium dodecyl benzene sulfonate in a mass ratio of 1:2: 1.
The preparation method of the plant protective agent comprises the following steps:
(1) washing root of Pulsatilla chinensis, drying, pulverizing, extracting with 60% ethanol for 3 times (1 hr each time), recovering ethanol from the extractive solution under reduced pressure, dissolving in water, extracting with petroleum ether for 2 times, mixing the petroleum ether extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Pulsatilla chinensis extract;
(2) cleaning leaves, stems, roots or whole plant of chloranthus japonicus, drying, pulverizing, adding 70% ethanol, reflux extracting for 3 times, each time for 1 hr; then mixing the ethanol extracts, distilling and concentrating under reduced pressure, and vacuum drying the concentrate to obtain chloranthus japonicus extract;
(3) cleaning, drying and crushing stems of akebia quinata, adding 80% ethanol for soaking for 48 hours, and then carrying out ultrasonic oscillation for 1 hour; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
(4) cleaning whole plant of herba Erodii seu Geranii, drying, pulverizing, decocting in water for 1 time, decocting for 2 hr, and filtering to obtain extractive solution; adding 70% ethanol into the extractive solution, dissolving completely, standing for 24 hr, collecting the upper ethanol extractive solution, concentrating under reduced pressure, and vacuum drying the concentrate to obtain herba Erodii seu Geranii extract;
(5) cleaning whole plant of Euphorbiae Lathyridis semen, drying, pulverizing, adding 70% ethanol, reflux extracting for 3 times, each time for 1 hr; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
(6) uniformly mixing 45% of the pulsatilla chinensis extract, 18% of the chloranthus japonicus extract, 15% of the clematis chinensis extract, 12% of the pyrrosia brevifolia extract and 10% of the euphorbia lathyris extract to obtain a raw material medicine; then adding an auxiliary agent consisting of an organic solvent, an emulsifier, a surfactant and water into the raw material medicines, and uniformly mixing to obtain the plant protectant.
The embodiment also comprises the application of the prepared plant protective agent in controlling larch caterpillars.
EXAMPLE III
The plant protective agent comprises a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 3: 1; the raw material medicine comprises the following components in percentage by mass: 20% of pulsatilla extract, 30% of chloranthus japonicus extract, 20% of clematis chinensis extract, 15% of pyrrosia brevifolia extract and 15% of euphorbia lathyris extract.
The preferable proportioning scheme of the auxiliary agent in the embodiment is as follows: 40% of organic solvent, 20% of emulsifier, 10% of surfactant and 30% of water. All the auxiliary raw materials are calculated by mass fraction.
Ethanol is used as an organic solvent in the present example; sodium dodecyl sulfate is adopted as an emulsifier; the surfactant is a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide and sodium dodecyl benzene sulfonate in a mass ratio of 1:2: 1.
The preparation method of the plant protective agent comprises the following steps:
(1) washing root of Pulsatilla chinensis, drying, pulverizing, extracting with 70% ethanol for 1 time and 2 hr, recovering ethanol from the extractive solution under reduced pressure, dissolving in water, extracting with petroleum ether for 3 times, mixing the petroleum ether extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Pulsatilla chinensis extract;
(2) cleaning leaves, stems, roots or whole plant of chloranthus japonicus, drying, pulverizing, adding 80% ethanol, reflux extracting for 1 time for 2 hr; then concentrating the ethanol extract by reduced pressure distillation, and then drying the concentrate in vacuum to obtain the chloranthus japonicus extract;
(3) cleaning, drying and crushing stems of akebia quinata, adding 95% ethanol, soaking for 24 hours, and then carrying out ultrasonic oscillation for 0.5 hour; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
(4) cleaning whole plant of herba Erodii seu Geranii, drying, pulverizing, decocting in water for 3 times, each for 1 hr, and filtering to obtain extractive solution; mixing the extractive solutions; adding 80% ethanol into the extractive solution, dissolving completely, standing for 12 hr, collecting the upper ethanol extractive solution, concentrating under reduced pressure, and vacuum drying the concentrate to obtain herba Erodii seu Geranii extract;
(5) cleaning whole plant of Euphorbiae Lathyridis semen, drying, pulverizing, adding 80% ethanol, reflux extracting for 1 time for 2 hr; then concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
(6) uniformly mixing 20% of the pulsatilla chinensis extract, 30% of the chloranthus japonicus extract, 20% of the akebia quinata extract, 15% of the pyrrosia brevipedunculata extract and 15% of the euphorbia lathyris extract to obtain a raw material medicine; then adding an auxiliary agent consisting of an organic solvent, an emulsifier, a surfactant and water into the raw material medicines, and uniformly mixing to obtain the plant protectant.
The embodiment also comprises the application of the prepared plant protective agent in controlling larch caterpillars.
Example four
The plant protective agent comprises a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 1: 1; the raw material medicine comprises the following components in percentage by mass: 20% of pulsatilla extract, 10% of chloranthus japonicus extract, 25% of caulis akebiae extract, 25% of pyrrosia leaf extract and 20% of euphorbia lathyris extract.
The preferable proportioning scheme of the auxiliary agent in the embodiment is as follows: 35% of organic solvent, 30% of emulsifier, 15% of surfactant and 20% of water. All the auxiliary raw materials are calculated by mass fraction.
Ethanol is used as an organic solvent in the present example; sodium dodecyl sulfate is adopted as an emulsifier; the surfactant is a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide and sodium dodecyl benzene sulfonate in a mass ratio of 1:2: 1.
The preparation method of the plant protective agent comprises the following steps:
(1) washing root of Pulsatilla chinensis, drying, pulverizing, extracting with 70% ethanol for 2 times (each time for 1 hr), recovering ethanol from the extractive solution under reduced pressure, dissolving in water, extracting with petroleum ether for 2 times, mixing the petroleum ether extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Pulsatilla chinensis extract;
(2) cleaning leaves, stems, roots or whole plant of chloranthus japonicus, drying, pulverizing, adding 75% ethanol, reflux extracting for 2 times, each time for 1 hr; then mixing the ethanol extracts, distilling and concentrating under reduced pressure, and vacuum drying the concentrate to obtain chloranthus japonicus extract;
(3) cleaning, drying and crushing stems of akebia quinata, adding 95% ethanol, soaking for 24 hours, and then ultrasonically oscillating for 1 hour; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
(4) cleaning whole plant of herba Erodii seu Geranii, drying, pulverizing, decocting in water for 2 times (each time for 2 hr), and filtering to obtain extractive solution; mixing the extractive solutions; adding 75% ethanol into the extractive solution, dissolving completely, standing for 24 hr, collecting the upper ethanol extractive solution, concentrating under reduced pressure, and vacuum drying the concentrate to obtain herba Erodii seu Geranii extract;
(5) cleaning whole plant of Euphorbiae Lathyridis semen, drying, pulverizing, adding 75% ethanol, reflux extracting for 2 times, each time for 2 hr; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
(6) uniformly mixing 20% of the pulsatilla chinensis extract, 10% of the chloranthus japonicus extract, 25% of the akebia quinata extract, 25% of the pyrrosia brevipedunculata extract and 20% of the euphorbia lathyris extract to obtain a raw material medicine; then adding an auxiliary agent consisting of an organic solvent, an emulsifier, a surfactant and water into the raw material medicines, and uniformly mixing to obtain the plant protectant.
The embodiment also comprises the application of the prepared plant protective agent in controlling larch caterpillars.
Comparative example 1
The difference between the comparative example and the first example is that the formula does not contain the pulsatilla chinensis extract, namely the raw material medicaments comprise the following components in percentage by mass: 20% of chloranthus japonicus extract, 20% of caulis akebiae extract, 18% of herba pyrrosiae extract and 12% of euphorbia lathyris extract.
The extraction method of each raw material drug and the preparation method of the plant protectant are the same as the first embodiment.
Comparative example No. two
The difference between the comparative example and the first example is that the formula does not contain the chloranthus japonicus extract, namely the raw material medicaments comprise the following components in percentage by mass: 30% of pulsatilla extract, 20% of clematis chinensis extract, 18% of pyrrosia brevifolia extract and 12% of euphorbia lathyris extract.
The extraction method of each raw material drug and the preparation method of the plant protectant are the same as the first embodiment.
Comparative example No. three
The difference between the comparative example and the first example is that the formula does not contain the clematis chinensis extract, namely the raw material medicaments comprise the following components in percentage by mass: 30% of pulsatilla extract, 20% of chloranthus japonicus extract, 18% of pyrrosia brevifolia extract and 12% of euphorbia lathyris extract.
The extraction method of each raw material drug and the preparation method of the plant protectant are the same as the first embodiment.
Comparative example No. four
The difference between the comparative example and the first example is that the formula does not contain the extract of the pyrrosia brevipetala and the euphorbia lathyris, namely the raw material medicaments comprise the following components in percentage by mass: 30% of pulsatilla extract, 20% of chloranthus japonicus extract and 20% of clematis chinensis extract.
The extraction method of each raw material drug and the preparation method of the plant protectant are the same as the first embodiment.
Comparative example five
The formula of the comparative example is the same as that of the first example, except that the common ethanol hot extraction method is adopted for the Chinese pulsatilla root.
Comparative example six
The formula of the comparative example is the same as that of the first example, except that the extracts of the raw material medicines are extracted by a common ethanol heat extraction method.
Comparative example seven
The formula and the preparation method of the comparative example are the same as those of the first example, and the difference is that the mass ratio of the raw material medicine to the auxiliary agent is 1: 3.
Comparative example eight
The formulation and preparation method of this comparative example are the same as those of example one, except that the adjuvant used is emulsifier-free, i.e., the adjuvant is 35% organic solvent, 15% surfactant and 25% water.
The performance and effect test procedures and results of the plant protection agents prepared in examples one to four and comparative examples one to seven, respectively, were as follows:
(ii) stability test
The emulsion stability test refers to the national standard GB/T1603-2001, namely, the method for determining the stability of the pesticide emulsion, and the plant protective agent is diluted by 200 times by using water and is kept stand for 3 hours at the temperature of 30 ℃ for test; the cold storage stability test refers to the national standard GB/T19137-2003 'determination method for low temperature stability of pesticide', and the plant protectant is subjected to cold storage at 0 ℃; the heat storage stability test refers to national standard GB/Tl9136-2003 method for determining heat storage stability of pesticide, and the content of the effective components is tested after the pesticide is stored for 14 days at 54 ℃.
The test results are shown in table 1:
table 1 stability test results of the plant protective agents prepared in examples and comparative examples
As can be seen from Table 1, the plant protective agent prepared by the example of the present invention has good emulsion stability, cold storage stability and heat storage stability, and the heat storage stability is more than 99.5%.
(II) laboratory virulence determination
Equal amounts of the plant protection agents of the examples and the comparative examples were selected and diluted to 100-fold liquid concentration spray respectively. Selecting fresh pine branches with pine needles, and spraying the experimental pine caterpillars and the fresh pine branches by constant amount, wherein fog drops are uniformly distributed on the surfaces of the pine needles during spraying, and the liquid medicine does not drop. And (3) putting the treated pine caterpillars and pine branches into an experimental cage. In order to ensure that the treated branches do not wither, a water culture method is adopted for moisturizing. And the experimental cage was placed in a sunny place. And continuously observing 5d, and recording data at 1d, 3d and 5d respectively and performing processing analysis. While 2.5% deltamethrin was selected for the control experiment.
The pine moth mortality was calculated using the following formula:
the test results are shown in table 2:
TABLE 2 laboratory virulence assay results for plant protection agents prepared in the examples and comparative examples
The laboratory toxicity test result shows that the death rate (5d) of the pine moth acted by the plant protective agent can reach more than 99 percent and can reach 100 percent at most; has the same drug effect as 2.5 percent of deltamethrin.
(III) forest test of Effect
The plant protective agents of the same amount of the examples and the comparative examples are selected to be respectively diluted into spray with the concentration of 100 times of the solution, and standard experimental forest lands are selected for forest pesticide effect test. And observing the placement effect of the field forest, comparing and analyzing the placement effect with the toxicity determination effect of the laboratory, and verifying whether the forest pesticide effect is consistent with the laboratory pesticide effect. The forest field is selected from fire pond teaching test forest field of northwest agriculture and forestry science and technology university.
TABLE 3 laboratory forest Effect test results for the plant protection agents prepared in the examples and comparative examples
As can be seen from forest effect test results, the death rate (5d) of the pine moth acted by the plant protective agent can reach more than 97 percent, and the pine moth has the same drug effect as 2.5 percent of deltamethrin.
(IV) determination of toxicity to Natural enemy insects
The plant protective agent disclosed by the embodiment of the invention is diluted into spray with the concentration of 100 times of the liquid, and the spray is carried out by adopting a straight-barrel type sprayer, wherein the time is controlled to be 4 s/time, so that the quantitative spraying of the test insects is ensured. During the test, the pine moth black egg bees are placed in three experimental cages, then the medicine is respectively sprayed into the cages, the medicine liquid is uniformly diffused in the cages, and then the cage door is closed; the three experimental cages were placed in a well ventilated environment and the number of deaths of the pine caterpillars black egg bees was recorded after 24 h. The measurement results are shown in table 4:
TABLE 4 determination of the virulence of natural enemy insects for the plant protection agents of the invention
From the toxicity test result of the natural enemy insects, the death rate of the natural enemy insects, namely the pine moth black oomycetes of the pine moth after the plant protective agent is acted on the natural enemy insects is not higher than 10 percent; moreover, the killing power of the plant protective agent to the natural enemy insect, namely, the trichogramma pine moth black bee of the trichogramma pine is far less than that of deltamethrin with the pesticide of 2.5 percent.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. The plant protective agent is characterized by comprising a raw material medicine and an auxiliary agent, wherein the mass ratio of the raw material medicine to the auxiliary agent is 2: 3-3: 1; the raw material medicine comprises the following components in percentage by mass: 20-45% of the pulsatilla extract, 10-30% of the chloranthus japonicus extract, 15-25% of the clematis chinensis extract, 12-25% of the pyrrosia brevifolia extract and 10-20% of the euphorbia lathyris extract.
2. The plant protectant according to claim 1, wherein the pulsatilla chinensis extract is obtained by washing, drying and crushing pulsatilla chinensis roots, adding 60-70% ethanol for extraction for 1-3 times, 1-2 h each time, recovering a reflux extract under reduced pressure until no ethanol smell exists, adding water for dissolution, extracting with petroleum ether for 2-3 times, combining the petroleum ether extracts, concentrating under reduced pressure, and drying the concentrate under vacuum.
3. The plant protective agent according to claim 1, wherein the chloranthus japonicus extract is prepared by washing, drying and crushing leaves, stems, roots or whole plants of chloranthus japonicus, and adding 70-80% ethanol for reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, distilling under reduced pressure, concentrating, and vacuum drying the concentrate to obtain the final product.
4. The plant protective agent according to claim 1, wherein the caulis akebiae extract is prepared by cleaning, drying and crushing stems of caulis akebiae, adding 80-95% ethanol to soak for 24-48 h, and then ultrasonically shaking for 0.5-1 h; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate.
5. The plant protectant according to claim 1, wherein the extract of the grass of Chinese knotweed is obtained by washing, drying and pulverizing the whole plant of the grass of Chinese knotweed, adding water to decoct for 1 to 3 times, each time for 1 to 2 hours, and filtering to obtain an extract; mixing the extractive solutions; and adding 70-80% ethanol into the extracting solution, fully dissolving, standing for 12-24 h, taking the upper layer ethanol extract, concentrating under reduced pressure, and drying the concentrate in vacuum to obtain the plant extract.
6. The plant protection agent according to claim 1, wherein the Euphorbia lathyris extract is prepared by washing, drying and pulverizing whole plant of Euphorbia lathyris, adding 70-80% ethanol, and reflux-extracting for 1-3 times, each time for 1-2 h; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain the final product.
7. The plant protection agent as claimed in claim 1, wherein the auxiliary agent comprises the following raw materials in percentage by weight: 30-40% of organic solvent, 20-30% of emulsifier, 10-20% of surfactant and 20-30% of water.
8. The plant protection agent according to claim 7, wherein the surfactant is a mixture of stearic acid, a copolymer of ethylene oxide and propylene oxide, and sodium dodecylbenzenesulfonate in a mass ratio of 1:2: 1.
9. The preparation method of the plant protective agent is characterized by comprising the following steps:
washing, drying and crushing roots of Chinese pulsatilla roots, adding 60-70% ethanol for extraction for 1-3 times, extracting for 1-2 hours each time, recovering a reflux extracting solution under reduced pressure until no ethanol smell exists, adding water for dissolution, extracting for 2-3 times by using petroleum ether, combining the petroleum ether extracts, concentrating under reduced pressure, and drying a concentrate under vacuum to obtain a Chinese pulsatilla root extract;
cleaning, drying and crushing leaves, stems, roots or whole plants of chloranthus japonicus, and adding 70-80% ethanol for reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, distilling and concentrating under reduced pressure, and vacuum drying the concentrate to obtain chloranthus japonicus extract;
cleaning, drying and crushing stems of akebia quinata, adding 80-95% ethanol, soaking for 24-48 h, and then carrying out ultrasonic oscillation for 0.5-1 h; filtering, concentrating the filtrate by vacuum distillation, and vacuum drying the concentrate to obtain caulis Akebiae extract;
cleaning, drying and crushing the whole plant of the giant knotweed, adding water, decocting for 1-3 times, 1-2 hours each time, and filtering to obtain an extracting solution; mixing the extractive solutions; adding 70-80% ethanol into the extracting solution, fully dissolving, standing for 12-24 h, then taking the upper layer ethanol extract, concentrating under reduced pressure, and drying the concentrate in vacuum to obtain a pyrrosia breynia extract;
cleaning, drying and crushing the whole plant of euphorbia lathyris, adding 70-80% ethanol, and performing reflux extraction for 1-3 times, 1-2 hours each time; then mixing the ethanol extracts, concentrating under reduced pressure, and vacuum drying the concentrate to obtain Euphorbiae Lathyridis semen extract;
uniformly mixing 20-45% of the pulsatilla extract, 10-30% of the chloranthus japonicus extract, 15-25% of the akebia quinata extract, 12-25% of the pyrrosia brevifolia extract and 10-20% of the euphorbia lathyris extract to obtain a raw material medicine; then adding an auxiliary agent consisting of an organic solvent, an emulsifier, a surfactant and water into the raw material medicines, and uniformly mixing to obtain the plant protectant.
10. Use of the plant protection agent according to any one of claims 1 to 8 for controlling larch caterpillars.
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