CN115053917A - Matrine and ginkgolic acid plant source pesticide and preparation method thereof - Google Patents
Matrine and ginkgolic acid plant source pesticide and preparation method thereof Download PDFInfo
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- CN115053917A CN115053917A CN202210762356.3A CN202210762356A CN115053917A CN 115053917 A CN115053917 A CN 115053917A CN 202210762356 A CN202210762356 A CN 202210762356A CN 115053917 A CN115053917 A CN 115053917A
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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
- A01N25/22—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 ingredients stabilising the active ingredients
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, 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
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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
- A01N65/06—Coniferophyta [gymnosperms], e.g. cypress
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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]
- A01N65/20—Fabaceae or Leguminosae [Pea or Legume family], e.g. pea, lentil, soybean, clover, acacia, honey locust, derris or millettia
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
Abstract
The invention discloses a matrine and ginkgolic acid botanical pesticide and a preparation method thereof, belonging to the technical field of biological pesticides. The botanical pesticide is prepared from the following raw materials in parts by weight: 10-15 parts of sophora flavescens extract, 1-5 parts of ginkgolic acid extract, 0.5-1.5 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-2 parts of stabilizing agent and 0.5-1 part of antioxidant. The pure plant source pesticide of the invention adopts pure plant source components of matrine and ginkgolic acid as main functional components, can realize effective prevention and control of agricultural pests, has green, natural and pollution-free raw materials, can greatly reduce the use of high-toxicity chemical pesticides, reduce pesticide residues, reduce environmental pollution and has obvious economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of biological pesticides, and particularly relates to a matrine and ginkgolic acid botanical pesticide and a preparation method thereof.
Background
The prior art is mostly chemical pesticide, the pesticide effect is low, the residual toxicity period is long, and the growth environment of crops and the health of people and livestock are seriously influenced. The pesticide is a special chemical which can prevent and cure diseases and insect pests of agriculture and forestry and can also cause harm to human beings and animals. Therefore, the use of agricultural chemicals brings benefits to human beings on the one hand, and also brings harm to the environment in which human beings live on the other hand, and since a large amount of chemical agricultural chemicals are applied, air, water sources, soil and food are polluted, and poisons and the like are caused by the accumulation of poisons in livestock and human bodies. Moreover, long-term use of certain chemical pesticides can also lead to pest resistance. A large amount of pesticides volatilize into air, flow into water, settle and gather in soil, pollute farm animals and fish fruit products, and are transferred into human bodies through the enrichment function of a food chain to cause harm to the human bodies. The highly toxic pesticide has high efficiency and high toxicity, and can be left in the environment for a long time, so that when people and livestock eat food containing the residual pesticide, cumulative poisoning can be caused. The harm is usually displayed after long-term accumulation, and the disease is not easy to be found in time by the enrichment function of a food chain and finally enters the human body, so that the harm is more dangerous because the harm is generally not paid attention to people, the pollution range is wide, the number of people is large, and in many cases, the harm is harmful to the human body.
Therefore, there is a need for a novel botanical insecticide which is non-phytotoxic to crops, non-residue, non-polluting to the environment and agricultural products, and safe to humans and animals.
The plant-derived pesticide refers to a pesticide whose active ingredient is derived from a plant. They are generally classified as biopesticides or biogenic pesticides along with microbial or biochemical pesticides. Along with the increasing health consciousness and environmental consciousness of the public, chemical pesticides bring a plurality of negative effects on agricultural production due to the problems of environmental pollution, high residue and the like. The biological pesticide has the advantages of easy degradation in environment, safety to human and livestock, strong selectivity and the like, and meets the requirement of sustainable development of green agriculture.
Matrine is a natural botanical pesticide with low toxicity to human and livestock, is a broad-spectrum pesticide, and has the effects of contact poisoning and stomach poisoning. Has obvious control effect on armyworm, cabbage caterpillar, aphid and red spider on various crops. Matrine pesticide used in agriculture means practically all substances extracted from sophora flavescens, such as a begonia extract or total matrines. Is widely applied in agriculture, has good control effect, and is a low-toxicity, low-residue and environment-friendly pesticide. Mainly used for preventing and controlling various pests such as pine moth, tea moth, cabbage caterpillar, etc. Has multiple functions of insecticidal activity, bactericidal activity, plant growth regulating function and the like.
At present, plant-derived pesticides all have the defects of low extraction rate of active ingredients, complex preparation process, high cost, unsatisfactory insecticidal effect and the like, and cannot continuously and effectively play a role. And a small amount of chemical insecticide can still be added into a lot of botanical insecticides, and zero pollution to the environment can still not be achieved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a pure botanical insecticide taking matrine as a main functional component, which has continuous and effective control effect on fruit and vegetable pests, is safe, environment-friendly and pollution-free.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a matrine and ginkgolic acid botanical insecticide is prepared from the following raw materials in parts by weight: 10-15 parts of sophora flavescens extract, 1-5 parts of ginkgolic acid extract, 0.5-1.5 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-2 parts of stabilizing agent and 0.5-1 part of antioxidant.
Further, the preparation method of the matrine extract comprises the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12-24 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) according to the mass-volume ratio of 1 g: adding zein into the refined extract in an amount of 30-50ml, adding ethanol solution with the same volume as the refined extract, dispersing for 5-10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20-30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
Further, the preparation method of the ginkgolic acid extract comprises the following steps: drying and crushing the ginkgo biloba exocarp, adding 70-80% acetone solution to submerge the solid, performing ultrasonic extraction at the ultrasonic frequency of 100-150Hz and the ultrasonic temperature of 40-50 ℃ for 1-2h, and filtering to obtain filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
Further, the dispersing agent is lecithin, soybean lecithin or pectin.
Further, the wetting agent is tween 60 or tween 80.
Further, the stabilizer is one of catechol, eugenol and citric acid.
Further, the antioxidant is any one of dibutyl hydroxy toluene, methyl p-hydroxybenzoate or sodium lactate.
A preparation method of matrine and ginkgolic acid botanical insecticide comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12-24 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding zein into the refined extract in an amount of 30-50ml, adding ethanol solution with the same volume as the refined extract, dispersing for 5-10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20-30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing a ginkgolic acid extract: drying and crushing the ginkgo biloba exocarp, adding 70-80% acetone solution to submerge the solid, performing ultrasonic extraction at the ultrasonic frequency of 100-150Hz and the ultrasonic temperature of 40-50 ℃ for 1-2h, and filtering to obtain filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract;
(3) uniformly mixing the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant in parts by weight, and then carrying out jet milling and drying to obtain the final product, namely the botanical insecticide.
Each of the raw materials of the present invention is commercially available. The dosage of the pesticide of the invention is recommended to be 20-50g/hm 2 。
The matrine is a botanical pesticide, has the characteristics of specificity and naturalness, can be quickly decomposed in nature, and the final products are carbon dioxide and water. And secondly, the matrine is a plant endogenous chemical substance with activity on pests, and the components are not single, but are combined by a plurality of groups with similar chemical structures and a plurality of groups with dissimilar chemical structures, supplement each other and play a role together.
The ginkgolic acid serving as a botanical pesticide is safe, environment-friendly and pollution-free, but the preparation process is complex, the pesticide effect is not lasting, and the technical effect equivalent to that of a chemical pesticide is difficult to achieve under the same cost. Similarly, the problem of high cost efficiency as a biogenic bactericide is also present.
Therefore, the inventor thinks about compounding two botanical pesticides, and wrapping matrine by zein, on one hand, the matrine can be protected, on the other hand, the slow release of functional components can be realized, and the ginkgolic acid can be tightly combined with the hydrogen bond of the zein, and the two have synergistic effect, so that the efficacy enhancement and amplification of the two botanical pesticides are realized, and the insecticidal and bacteriostatic effects are continuously and effectively exerted. Meanwhile, the components such as a dispersing agent, a wetting agent, a stabilizing agent, an antioxidant and the like are supplemented, so that the two botanical insecticides are effectively promoted to effectively play a role.
Advantageous effects
The pure plant source pesticide of the invention adopts pure plant source components of matrine and ginkgolic acid as main functional components, can realize effective prevention and control of agricultural pests, has green, natural and pollution-free raw materials, can greatly reduce the use of high-toxicity chemical pesticides, reduce pesticide residues, reduce environmental pollution and has obvious economic and social benefits.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
A matrine and ginkgolic acid botanical insecticide is prepared from the following raw materials in parts by weight: 10 parts of sophora flavescens extract, 1 part of ginkgolic acid extract, 1.5 parts of dispersing agent, 3 parts of wetting agent, 2 parts of stabilizing agent and 1 part of antioxidant.
The preparation method of the matrine extract comprises the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) according to the mass-volume ratio of 1 g: adding zein into 30ml of the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 5min at 2000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
The preparation method of the ginkgolic acid extract comprises the following steps: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 100Hz, the ultrasonic temperature of 40 ℃ and the ultrasonic time of 1h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
The dispersing agent is lecithin.
The wetting agent is tween 60.
The stabilizing agent is catechol.
The antioxidant is dibutyl hydroxy toluene.
A preparation method of matrine and ginkgolic acid plant source insecticide comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding zein into 30ml of the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 5min at 2000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing a ginkgolic acid extract: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 100Hz, the ultrasonic temperature of 40 ℃ and the ultrasonic time of 1h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract;
(3) uniformly mixing the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant in parts by weight, and then carrying out jet milling and drying to obtain the final product, namely the botanical insecticide.
Example 2
A matrine and ginkgolic acid botanical insecticide is prepared from the following raw materials in parts by weight: 12 parts of sophora flavescens extract, 3 parts of ginkgolic acid extract, 1 part of dispersing agent, 2 parts of wetting agent, 1 part of stabilizing agent and 0.8 part of antioxidant.
The preparation method of the matrine extract comprises the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) according to the mass-volume ratio of 1 g: adding 50ml of zein into the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
The preparation method of the ginkgolic acid extract comprises the following steps: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
The dispersing agent is soybean phospholipid.
The wetting agent is tween 80.
The stabilizer is eugenol.
The antioxidant is methyl p-hydroxybenzoate.
A preparation method of matrine and ginkgolic acid botanical insecticide comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding zein into 50ml of the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing a ginkgolic acid extract: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract;
(3) the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant are uniformly mixed according to the weight parts, and then are dried after being pulverized by air flow to obtain the final product of the botanical pesticide.
Example 3
A matrine and ginkgolic acid botanical insecticide is prepared from the following raw materials in parts by weight: 15 parts of sophora flavescens extract, 5 parts of ginkgolic acid extract, 0.5 part of dispersing agent, 1 part of wetting agent, 0.5 part of stabilizing agent and 0.5 part of antioxidant.
The preparation method of the matrine extract comprises the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) according to the mass-volume ratio of 1 g: adding 50ml of zein into the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
The preparation method of the ginkgolic acid extract comprises the following steps: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
The dispersing agent is pectin.
The wetting agent is tween 60.
The stabilizing agent is citric acid.
The antioxidant is sodium lactate.
A preparation method of matrine and ginkgolic acid botanical insecticide comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding zein into 50ml of the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing the ginkgolic acid extract: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying to obtain solid powder, i.e. ginkgolic acid extract;
(3) uniformly mixing the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant in parts by weight, and then carrying out jet milling and drying to obtain the final product, namely the botanical insecticide.
Comparative example 1
A matrine and ginkgolic acid botanical insecticide is prepared from the following raw materials in parts by weight: 15 parts of sophora flavescens extract, 5 parts of ginkgolic acid extract, 0.5 part of dispersing agent, 1 part of wetting agent, 0.5 part of stabilizing agent and 0.5 part of antioxidant.
The preparation method of the matrine extract comprises the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution, extracting to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) adding ethanol solution with the same volume as the refined extractive solution, dispersing with high speed disperser at 3000r/min for 10min, and homogenizing under microjet pressure of 30MPa for 1-3 times; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
The preparation method of the ginkgolic acid extract comprises the following steps: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
The dispersing agent is pectin.
The wetting agent is tween 60.
The stabilizing agent is citric acid.
The antioxidant is sodium lactate.
A preparation method of matrine and ginkgolic acid botanical insecticide comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 24 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding 50ml of zein into the refined extract, adding ethanol solution with the same volume as the refined extract, dispersing for 10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing a ginkgolic acid extract: drying and crushing the ginkgo biloba testa, adding an acetone solution with the mass concentration of 70-80% to submerge the solid, performing ultrasonic extraction with the ultrasonic frequency of 150Hz, the ultrasonic temperature of 50 ℃ and the ultrasonic time of 2h, and filtering to obtain a filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract;
(3) uniformly mixing the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant in parts by weight, and then carrying out jet milling and drying to obtain the final product, namely the botanical insecticide.
The comparative example is the same as example 3 except that the matrine-alcohol-soluble protein is not coated.
Comparative example 2
The formulation and preparation method of the raw materials of this comparative example are substantially the same as those of example 3, except that the addition of the sophora flavescens extract and the preparation thereof are not included.
Comparative example 3
The formulation and preparation method of the comparative example are substantially the same as example 3, except that the addition of ginkgolic acid extract and the preparation thereof are not included.
Insecticidal Performance test
The experimental site:
a production base of a farmer professional cooperative society in an orchid area in Linyi city is provided with a full-automatic drip irrigation system under the ground surface of a greenhouse, and an automatic temperature and humidity monitor is installed in the greenhouse. The soil quality of the test soil is loam, the soil fertility is medium, the organic matter content is 1.5 percent, and the pH value is 6.8. The cultivation conditions (soil type, fertilization amount, watering and the like) of all the test districts are uniform and consistent, and the cultivation conditions accord with the actual local agricultural production. The administration time was 6 months and 15 days in 2020, and the investigation was performed 1 time each for 3 days and 7 days after the administration.
The survey object: cabbage diamondback moth and celery aphid
Experiment design:
adopting a random block design, setting 7 treatments which are S1-S7 respectively, repeating each treatment for three times, respectively inspecting the control effect of the treatment on cabbage diamondback moth and celery aphid, adopting a manual knapsack sprayer to spray the leaf surfaces, wherein the flow rate is 500mL/min, and the inlet cone fog nozzle:
s1: the pesticide obtained in example 1 is used in an amount of 20g/hm 2 And the water consumption is 500L/hm 2 ；
S2: example 2 insecticide, dosage 20g/hm 2 And the water consumption is 500L/hm 2 ；
S3: pesticide obtained in example 3, dosage is 20g/hm 2 And the water consumption is 500L/hm 2 ；
S4: pesticide obtained in comparative example 1, dosage is 20g/hm 2 And the water consumption is 500L/hm 2 ；
S5: pesticide obtained in comparative example 2, dosage is 20g/hm 2 And the water consumption is 500L/hm 2 ；
S6: pesticide obtained in comparative example 3, dosage is 20g/hm 2 And the water consumption is 500L/hm 2 ；
S7: 10% chlorfenapyr suspending agent, used according to the product instructions, Wuhanchu Biotech limited;
a blank control was set, which was the application of clear water.
The plants were sprayed evenly by foliar spray. The application is carried out once, and is in the early stage of low-age larva.
Sampling is carried out at five points in each cell, 2 insect plants are fixed at each point, the number of live larvae in different ages on 10 crops is investigated by listing in each cell, and the whole plant is investigated.
The population decline rate is (number of live insects before prevention-number of live insects after prevention)/number of live insects before prevention x 100%;
the correction control effect is (treatment population reduction rate-blank control population reduction rate)/(100-blank control population reduction rate) × 100%
TABLE 1 control of plutella xylostella
TABLE 2 celery aphid control experiment effect
The experimental data show that the pesticide has good quick-acting property and durability for diamondback moth and aphid, no chemical injury occurs, the control effect can be comparable to that of the traditional chemical pesticide, but the hazard is far lower than that of the chemical pesticide. The matrine and the ginkgolic acid which are wrapped by the protein act together, and the matrine and the ginkgolic acid are synergistic, so that the maximization of the efficacy function is realized. While the comparative example 1 lacking the protein coating has a significantly weaker quick-acting property and persistence than the examples, the comparative examples 2 to 3 with a single component have a significantly reduced control effect.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (8)
1. The botanical pesticide of the matrine and the ginkgolic acid is characterized by being prepared from the following raw materials in parts by weight: 10-15 parts of sophora flavescens extract, 1-5 parts of ginkgolic acid extract, 0.5-1.5 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-2 parts of stabilizing agent and 0.5-1 part of antioxidant.
2. The matrine and ginkgolic acid plant-derived pesticide as claimed in claim 1, wherein said matrine extract is prepared by the following steps:
(1) pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12-24 hr, and filtering to obtain extractive solution;
(2) adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution, extracting to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract;
(3) according to the mass-volume ratio of 1 g: adding zein into the refined extract in an amount of 30-50ml, adding ethanol solution with the same volume as the refined extract, dispersing for 5-10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20-30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract.
3. The matrine and ginkgolic acid botanical insecticide of claim 1, wherein said ginkgolic acid extract is prepared by the steps of: drying and crushing the ginkgo biloba exocarp, adding 70-80% acetone solution to submerge the solid, performing ultrasonic extraction at the ultrasonic frequency of 100-150Hz and the ultrasonic temperature of 40-50 ℃ for 1-2h, and filtering to obtain filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract.
4. The matrine and ginkgolic acid botanical pesticide of claim 1, wherein the dispersing agent is lecithin, soybean lecithin or pectin.
5. The matrine and ginkgolic acid botanical insecticide of claim 1, wherein said wetting agent is tween 60 or tween 80.
6. The matrine and ginkgolic acid botanical pesticide of claim 1, wherein the stabilizer is one of catechol, eugenol, and citric acid.
7. The matrine and ginkgolic acid plant source pesticide of claim 1, wherein said antioxidant is any one of dibutyl hydroxy toluene, methyl p-hydroxybenzoate or sodium lactate.
8. A preparation method of the matrine and ginkgolic acid plant source pesticide as claimed in any one of claims 1-7, which comprises the following steps:
(1) preparing a sophora flavescens extract: pulverizing radix Sophorae Flavescentis, soaking in ethanol solution for 12-24 hr, and filtering to obtain extractive solution; adjusting pH of the leaching solution to 8-9 with ammonia water, adding chloroform with the same volume as the leaching solution for extraction to obtain an extract, and vacuum concentrating the extract to remove solvent to obtain a refined extract; according to the mass-volume ratio of 1 g: adding zein into the refined extract in an amount of 30-50ml, adding ethanol solution with the same volume as the refined extract, dispersing for 5-10min at 3000r/min by using a high-speed disperser, and homogenizing for 1-3 times under the microjet pressure of 20-30 MPa; rotary evaporating, removing solvent, and freeze drying to obtain solid powder, i.e. matrine extract;
(2) preparing a ginkgolic acid extract: drying and crushing the ginkgo biloba exocarp, adding 70-80% acetone solution to submerge the solid, performing ultrasonic extraction at the ultrasonic frequency of 100-150Hz and the ultrasonic temperature of 40-50 ℃ for 1-2h, and filtering to obtain filtrate; purifying the filtrate with silica gel column, eluting with 80% ethanol solution for 3-5 times, vacuum concentrating the eluate to remove organic solvent to obtain refined extractive solution, and freeze drying the refined extractive solution to obtain solid powder, i.e. ginkgolic acid extract;
(3) uniformly mixing the sophora flavescens extract, the ginkgolic acid extract, the dispersing agent, the wetting agent, the stabilizing agent and the antioxidant in parts by weight, and then carrying out jet milling and drying to obtain the final product, namely the botanical insecticide.
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