CN111820245A - Plant type pesticide and preparation method thereof - Google Patents
Plant type pesticide and preparation method thereof Download PDFInfo
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- CN111820245A CN111820245A CN202010672349.5A CN202010672349A CN111820245A CN 111820245 A CN111820245 A CN 111820245A CN 202010672349 A CN202010672349 A CN 202010672349A CN 111820245 A CN111820245 A CN 111820245A
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/22—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom rings with more than six members
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/12—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
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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]
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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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Abstract
The invention relates to the technical field of pesticide preparation, in particular to a plant type pesticide and a preparation method thereof, which solve the defect that no plant type pesticide with high efficiency and low toxicity aiming at diseases such as cucurbitaceae crop gummy stem blight, rice brown streak disease and the like exists in the prior art, and comprise the following steps: s1 extracting; s2, concentrating; s3 extraction; and S4 mixing. The invention aims to provide a plant pesticide and a preparation method thereof, which takes natural components as main raw materials and does not add high-toxicity chemical synthetic components. The compound plant type medicament has a synergistic effect, has the characteristics of safety, broad spectrum and high efficiency, is suitable for pests such as melon aphids, plutella xylostella and the like, and can also effectively prevent diseases such as melon gummy stem blight, rice brown streak disease and the like.
Description
Technical Field
The invention relates to the technical field of pesticide preparation, in particular to a plant type pesticide and a preparation method thereof.
Background
The pesticide is an essential production material in agricultural production, and comprises chemical pesticide and biological pesticide, wherein the chemical pesticide easily causes a series of problems such as environmental pollution, drug resistance and the like, so that the ecological environment is seriously threatened, and the safety of human is harmed. In contrast, the plant pesticide as a biological pesticide has the advantages of high selectivity, low toxicity, easy degradation, difficult resistance generation and the like, and the product not only contains active ingredients which can effectively prevent and control diseases, pests and weeds, but also contains a large amount of ingredients which have regulating effect on plant growth, such as plant organic acid, amino acid, tannin and the like. Thus, studies on the prevention and control of plant diseases and insect pests by natural chemical components are expected.
At present, no plant pesticide with high efficiency and low toxicity for diseases such as gummy stem blight of cucurbitaceous crops, brown stripe disease of rice and the like exists. Therefore, we propose a plant type pesticide and a preparation method thereof to solve the above problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a plant pesticide and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a plant type pesticide, which comprises the following steps:
s1 extraction: extracting oleander flower with organic solvent I, filtering to obtain extract, extracting radix Sophorae Flavescentis with organic solvent I, and filtering to obtain radix Sophorae Flavescentis extract;
s2 concentration: evaporating the oleander flower extract and the sophora flavescens extract obtained in the step S1 respectively to obtain an oleander flower extract and an sophora flavescens extract;
s3 extraction: extracting the oleander flower extract obtained in the step S2 with an organic solvent II to obtain an oleander flower extract, and extracting the sophora flavescens extract obtained in the step S2 with an organic solvent III to obtain a sophora flavescens extract;
s4 mixing: mixing the extractive solution of flos Nerii and the extractive solution of radix Sophorae Flavescentis obtained in S3, adding osthole, and stirring to obtain plant pesticide.
Preferably, in the step S1, 10 to 15mL of the organic solvent i is added to every 1g of the oleander flowers, 8 to 10mL of the organic solvent i is added to every 1g of the sophora flavescens, the extraction is performed under an ultrasonic condition, the ultrasonic power is 80 to 100Hz, the extraction time is 12 to 24 hours, the temperature is 20 to 30 ℃, and the extraction times are 3 to 5 times.
Preferably, the organic solvent I is at least one of alcohol, alcohol aqueous solution and acetone, the alcohol is at least one of methanol, ethanol, propanol, propylene glycol and butanol, and the volume fraction of the alcohol in the alcohol aqueous solution is 65-80%
Preferably, in the step S2, evaporation is carried out in a rotary evaporator at the temperature of 55-65 ℃, the vacuum degree of 200-300 Pa and the rotation speed of 70-100 r/min, and the mixture is concentrated into extractum after the oleander flower and the radix sophorae flavescentis are concentrated.
Preferably, in S3, 10 to 15mL of the organic solvent ii is added to each 1g of the oleander flower extract, the extraction time of the oleander flower extract is 20 to 30min, 8 to 10mL of the organic solvent iii is added to each 1g of the sophora flavescens extract, and the extraction time of the sophora flavescens extract is 20 to 30 min.
Preferably, the organic solvent II is petroleum ether and ethyl acetate, and the volume ratio of the petroleum ether to the ethyl acetate is 1: (1-5), wherein the organic solvent III is acetone and diethyl ether, and the volume ratio of the organic solvent III is 1: (1-2).
Preferably, in S4, the osthole is added in the form of an osthole solution, the mass volume concentration of the osthole solution is 40 to 200 μ g/mL, the solvent is at least one of alcohol and water, the alcohol is ethanol, and the volume ratio of the oleander flower extract, the sophora flavescens extract and the osthole solution is (1.5 to 2.0): (2.0-3.0): 10.
preferably, the method further comprises adding a synergist into the mixture of the oleander flower extract, the sophora flavescens extract and the osthole after the osthole is added.
Preferably, the synergist is added in the form of a synergist solution, the mass volume concentration of the synergist solution is 40-200 [ mu ] g/mL, the solvent is at least one of alcohol and water, the alcohol is ethanol, and the synergist is one or more of polyoxin and spinosad.
Preferably, the plant pesticide is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1. the compound plant type medicament prepared by the invention has a synergistic effect, has the characteristics of safety, broad spectrum and high efficiency, is suitable for preventing and treating two diseases of gummy stem blight of cucurbitaceae crops and brown streak disease of rice, and can also prevent and treat pests such as melon aphids, plutella xylostella and the like.
2. The invention mixes the extractive of oleander flower, the flavescent sophora root extract and osthole, and can add one or more of polyoxin and spinosad, processes and matches the active substance according to the pesticide mixing principle, then measures the biological activity, screens the combination with obvious synergy and the best matching, and screens the solvent, the synergist and the like, thus developing a broad-spectrum plant pesticide with obvious synergy, stability, better quick-acting performance, longer duration and environmental ecological safety and a preparation method thereof.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control. When "mass, concentration, temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, a range of 1 to 50 should be understood to include any number, combination of numbers, or subrange selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50, and all fractional values between the above integers, e.g., 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. With respect to sub-ranges, specifically consider "nested sub-ranges" that extend from any endpoint within the range. For example, nested sub-ranges of exemplary ranges 1-50 may include 1-10, 1-20, 1-30, and 1-40 in one direction, or 50-40, 50-30, 50-20, and 50-10 in another direction. "
The present invention will be further illustrated with reference to the following specific examples.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The Plutella xylostella (Plutella xylostella) and melon aphid (Aphis gossypii glover) in the examples described below were supplied by the agricultural sciences college of Heilongjiang province.
The plant pathogens, Rhizoctonia solani (Stagonospora cucurbitaceae) and Rhizoctonia solani (Nigrospora oryzae) in the following examples are provided by the agricultural academy of Heilongjiang province.
The osthole in the following examples is purchased from Xuancheng Baicao plant industry and trade Co., Ltd, is concentrated semi-finished dry powder, the osthole content is about 30wt%, when in use, 1g of the 30wt% osthole dry powder is weighed, 10mL of absolute ethyl alcohol is added, the solution is diluted into 3 × 104 μ g/mL solution, the solution is shaken and shaken up, and pure water is used for dilution to prepare osthole mother liquor with the mass volume concentration of 20 μ g/mL, 40 μ g/mL, 100 μ g/mL and 200 μ g/mL respectively for standby.
The first embodiment is as follows: preparation of plant-type pesticides
The plant-type pesticide is prepared according to the following steps:
(1) extraction: drying the rhizome of oleander flower and radix Sophorae Flavescentis in 70 deg.C oven respectively, pulverizing into powder with pulverizer, and sieving with 100 mesh sieve;
adding 15 times of 60% ethanol water solution (i.e. adding 15mL of 60% ethanol water solution into 1g of Nerium indicum pollen), extracting at 25 deg.C with ultrasound (power of 100 Hz) for three times (24 hr each time), mixing extractive solutions, and filtering to obtain Nerium indicum flower extractive solution;
adding 10 times of 60% ethanol water solution (10 mL of 60% ethanol water solution per 1g of radix Sophorae Flavescentis powder), ultrasonic extracting at 25 deg.C for 24 hr for three times, mixing extractive solutions, and filtering to obtain radix Sophorae Flavescentis extractive solution.
(2) Concentration: concentrating the above extractive solutions respectively in rotary evaporator at 55 deg.C under vacuum degree of 300Pa and rotation speed of 70r/min until the extractive solutions become extract, and recovering the solvent in a bottle by rotary evaporator.
(3) And (3) extraction: extracting the oleander flower extract (the volume ratio of the oleander flower extract to the extracting agent is 1: 10) by using a mixed solvent of petroleum ether and ethyl acetate (v/v =3: 7) for 24 hours to obtain an oleander flower extract; extracting the radix Sophorae Flavescentis extract (volume ratio of radix Sophorae Flavescentis extract to extractant is 1: 10) with acetone-diethyl ether mixed solvent (v/v =4: 6) for 24h to obtain radix Sophorae Flavescentis extract;
(4) mixing: mixing the oleander flower extract and the sophora flavescens extract, and then adding 200 mu g/mL osthole mother liquor, wherein the volume ratio of the oleander flower extract to the sophora flavescens extract to the osthole is 2.0: 3.0: 10, stirring uniformly to obtain the plant pesticide, wherein the concentration of the osthole is 170 mu g/mL.
Example two: preparation of plant-type pesticides
The plant-type pesticide is prepared according to the following steps:
(1) extraction: respectively drying the rhizome of the oleander flower and the fruit of the lightyellow sophora root in a 70 ℃ oven, crushing the dried rhizome and the fruit of the oleander flower into powder by a crusher, and sieving the powder by a 100-mesh sieve;
adding 15 times of 80% ethanol water solution (i.e. adding 15mL of 80% ethanol water solution into 1g of Nerium indicum pollen), extracting at 25 deg.C with ultrasound (power of 100 Hz) for three times (each time for 12 hr), mixing extractive solutions, and filtering to obtain Nerium indicum flower extractive solution;
adding 8 times of 80% ethanol water solution (10 mL 80% ethanol water solution per 1g radix Sophorae Flavescentis powder), ultrasonic extracting at 25 deg.C for 12 hr for three times, mixing extractive solutions, and filtering to obtain radix Sophorae Flavescentis extractive solution.
(2) Concentration: concentrating the above extractive solutions respectively in rotary evaporator at 55 deg.C under vacuum degree of 300Pa and rotation speed of 70r/min until the extractive solutions become extract, and recovering the solvent in a bottle by rotary evaporator.
(3) And (3) extraction: extracting the oleander flower extract (the volume ratio of the extract to the extracting agent is 1: 15) with a mixed solvent of petroleum ether and ethyl acetate (v/v =3: 7) for 12h to obtain an oleander flower extract; extracting the radix Sophorae Flavescentis extract (volume ratio of radix Sophorae Flavescentis extract to extractant is 1: 10) with mixed solvent of acetone and diethyl ether (v/v =4: 6) for 12h to obtain radix Sophorae Flavescentis extractive solution;
(4) mixing: mixing the oleander flower extract and the sophora flavescens extract, and then adding 400 mu g/mL osthole mother liquor, wherein the volume ratio of the oleander flower extract to the sophora flavescens extract to the osthole is 2.0: 3.0: 10, stirring uniformly to obtain the plant pesticide, wherein the concentration of the osthole is 214 mu g/mL.
Example three: preparation of plant-type pesticides
The plant-type pesticide is prepared according to the following steps:
(1) extraction: respectively drying the rhizome of the oleander flower and the fruit of the lightyellow sophora root in a drying oven at 60 ℃, crushing the dried rhizome and the fruit of the oleander flower into powder by a crusher, and sieving the powder by a 40-mesh sieve;
adding 10 times of 70% ethanol water solution (10 mL of 70% ethanol water solution per 1g of oleander pollen), ultrasonic extracting at 25 deg.C for three times (24 hr each time), mixing extractive solutions, and filtering to obtain oleander flower extractive solution;
adding 10 times of 70% ethanol water solution (10 mL70% ethanol water solution per 1g radix Sophorae Flavescentis powder), ultrasonic extracting at 25 deg.C for three times (24 hr each time), mixing extractive solutions, and filtering to obtain radix Sophorae Flavescentis extractive solution.
(2) Concentration: concentrating the above extractive solutions respectively in rotary evaporator at 55 deg.C under vacuum degree of 300Pa and rotation speed of 70r/min until the extractive solutions become extract, and recovering the solvent in a bottle by rotary evaporator.
(3) And (3) extraction: extracting the oleander flower extract (the volume ratio of the radix euphorbiae lantu extract to the extracting agent is 1: 10) by using a mixed solvent of petroleum ether and ethyl acetate (v/v =3: 7) for 24 hours to obtain an oleander flower extract; extracting the radix Sophorae Flavescentis extract (volume ratio of radix Sophorae Flavescentis extract to extractant is 1: 10) with acetone-diethyl ether mixed solvent (v/v =4: 6) for 24h to obtain radix Sophorae Flavescentis extract;
(4) mixing: mixing the oleander flower extract and the sophora flavescens extract, and then adding 300 mu g/mL osthole mother liquor to obtain an oleander flower extract, sophora flavescens extract and osthole mixture, wherein the volume ratio of the oleander flower extract to the sophora flavescens extract to the osthole is 1.5: 3.0: 10, the concentration of osthole in the mixture is 200 mug/mL, then 100 mug/mL of one of polyoxin and spinosad is added, 99% of the raw pesticide (Noponin Biotechnology Co., Ltd.) is dissolved by a small amount of ethanol to prepare an alcoholic solution with the concentration of 1 x 104 mug/mL, and then the alcoholic solution is diluted to 100 mug/mL by pure water, wherein the volume ratio of the mixture of the oleander flower extract, the sophora flavescens extract and the osthole to the one of the polyoxin, the acetyl 7 amine and the spinosad is 10: 1, uniformly stirring to obtain the plant pesticide, wherein the concentration of the osthole in the plant pesticide is 180 mu g/mL.
Example four: mixing osthole with flos Nerii extract and radix Sophorae Flavescentis extract, and killing parasite and resisting bacteria
In the embodiment, the oleander flower extracts refer to oleander flower extract, and the sophora flavescens extracts refer to sophora flavescens root extract.
In the toxicity test and the bioactivity test in this example, the extract stock solution in step (3) of example 3 is diluted with water to different concentrations, wherein the concentrations of the sophora flavescens extract and the oleander flower extract are calculated according to the following formulas: c = m/v, where m refers to the mass of the extraction stock and v refers to the volume of water.
The concentration of the mixture of the Chinese herbal medicines including radix Sophorae Flavescentis, flos Nerii, and osthole in this example is calculated according to the volume ratio of the radix Sophorae Flavescentis extract, the flos Nerii extract, and osthole, and c = (c)ClipvClip+ cBitter tastevBitter taste+ cSnake (snake)vSnake (snake)）/（vClip+vBitter taste+vSnake (snake)）。
(1) Toxicity determination and biological activity determination of mixed combination on diamond back moth
The toxicity of the oleander flower extract, the sophora flavescens extract and the cnidium lactone mother liquor prepared in the step (3) in the example 3 on the plutella xylostella is determined, and the experimental method is as follows:
diluting the tested medicaments (including the oleander flower extract, the sophora flavescens extract and the osthole) with clear water and 1/10 surfactant (Tween-80) to various concentrations, treating for 72h by adopting a leaf soaking method and taking clear water as a control, checking the death condition of the tested insects, recording the result, and calculating the mortality and correcting the mortality. Regression lines of the virulence of the osthole and the test single agent to the diamondback moth (third instar larva) are calculated by using a DPS data analysis system, and the osthole LC30 and the test single agent LC30 (Table 1) are obtained.
TABLE 1 toxicity assay results of Nerium indicum flower extract, Sophora flavescens extract and osthole against Plutella xylostella (72 h)
| Variety of (IV) C | LC3095% confidence interval of1 | LC30 1 | Regression line | R |
| Extract of oleander flower | 200.5380~312.2913 | 256.7438 | Y=1.5326x+0.9678 | 0.8869 |
| Sophora flavescens extract | 127.3964~189.0361 | 164.9264 | Y=1.0986x+1.2635 | 0.9231 |
| Osthole | 98.9688~231.3201 | 155.9255 | Y=1.7254x+0.8697 | 0.8493 |
1)The concentration unit is as follows: μ g.mL-1
(2) Biological activity test of osthole, radix sophorae flavescentis extract and oleander flower extract compound agent on tested insects
The botanical pesticide is prepared according to the steps in the example 3, the volume ratio of the osthole, the radix sophorae flavescentis extract and the oleander flower extract is changed, the influence of the botanical pesticide with different proportions on the biological activity test result of the tested pests is observed, and the experimental method is as follows:
respectively measuring the toxicity regression lines of the osthole mother liquor, the sophora flavescens extract and the oleander flower extract to the tested insects by adopting a Sun cloud Peel formula method, obtaining three LC50 of single dose to the tested insects, simultaneously mixing the osthole, the sophora flavescens extract and the oleander flower extract in different proportions for many times, obtaining LC50 of corresponding mixed dose, calculating the cotoxicity coefficient of the mixed dose according to the Sun cloud Peel formula method, and selecting the optimal proportion. Clear water was used as control. The results of the experiment are shown in table 2.
TABLE 2 bioassay results of the combination of osthole, Sophora flavescens Aiton extract and Nerium indicum flower extract on tested insects
Note: nerium oleander flower LC50In the amount of 342. mu.g.mL-1Kuh-seng LC50186. mu.g.mL-1Cnidium lactone is LC50170 μ g.mL-1(ii) a LC for preventing and controlling cabbage aphid and oleander flower50239 mu g.mL of the product-1Kuh-seng LC50143. mu.g.mL-1Osthole LC50Was 214. mu.g.mL-1。
As can be seen from Table 2, the osthole, the radix sophorae flavescentis extract and the oleander flower extract are subjected to ternary mixing according to different proportions, wherein the volume ratio of the oleander flower to the radix sophorae flavescentis to the osthole is 2.0/3.0/10, the synergistic effect is most obvious, and the co-toxicity coefficients of the osthole and the aphid acting on the plutella xylostella and the aphid are 285.1 and 229.2 respectively.
(3) Biological activity test of spinosad and bitter/clamp/snake compound compatibility on tested insects
Because the compounding agent with the volume ratio of the oleander flower to the radix sophorae flavescentis to the osthole of 2.0/3.0/10 is obtained in the step (2), the synergistic effect is most obvious, the compounding agent is set as a mixture and then is compatible with spinosad, the biological activity of the prepared plant pesticide on tested insects is tested, and the experimental method is as follows:
similarly, a Sun cloud Peel formula method is adopted, toxicity regression lines of the mixture (oleander flower/radix sophorae flavescentis/cnidium lactone = 2.0/3.0/10) and the spinosad to the tested insects are respectively measured, LC50 of a single dose to the tested insects is respectively obtained, meanwhile, the mixture (oleander flower/radix sophorae flavescentis/cnidium lactone = 2.0/3.0/10) of the dose is mixed with the spinosad, 99% of spinosad original drug (Baijiang Kuaixin Biotechnology limited) is dissolved by a small amount of ethanol to prepare an alcoholic solution with the concentration of 1 x 104 mu g/mL, the alcoholic solution is diluted into 100 mu g/mL by pure water to be mixed for multiple times at different proportions, LC50 of the corresponding mixture is obtained, the cotoxicity coefficient of the mixture is calculated according to the Sun cloud Peel formula method, and the optimal proportion is selected. Clear water was used as control. The results of the experiment are shown in table 3.
TABLE 3 biological test results of spinosad in combination with the clip/bitter/snake mixtures on tested insects
Note: LC in watch50The unit is mu g.mL-1The mixture represents a plant type pesticide prepared by mixing the Chinese herbal medicines/bitter/snake according to the volume ratio of 2.0/3.0/10, and the ratio of the mixture to the spinosad is the volume ratio.
As can be seen from Table 3, when the volume ratio of spinosad to the mixture of pleocidin, bitter and snake is 10/1, the synergistic effect of the compound agent is most obvious, the co-toxicity coefficients of the spinosad and the mixture of pleione, bitter and snake are 257.9 and 221.1 respectively, and the CTC is more than 120.
(3) Biological activity test of polyoxin and mixed material of clip, bitter and snake on test strain
The compounded agent with the volume ratio of the oleander flower to the radix sophorae flavescentis to the osthole of 2.0/3.0/10 is obtained in the step (3), and the synergistic effect is most obvious, so that the compounded agent is prepared into a compound and then is compatible with polyoxin, the biological activity of the prepared plant pesticide on a test strain is tested, and the experimental method is as follows:
according to the volume ratio of 100 mu g/mL of the mixture (the volume ratio of the oleander flower to the radix sophorae flavescentis to the osthole is 2.0/3.0/10) to 40 mu g/mL of polyoxin solution (80 wt% polyoxin raw drug (biochemicals, Inc. of Liaoning department) is diluted to 40 mu g/mL by pure water) to 10: 1 mixing, testing the biological activity of the prepared plant pesticide on tested insects, wherein the experimental method comprises the following steps:
the actual and theoretical control effects of the mixture (oleander flower/kuh-seng/cnidium lactone = 2.0/3.0/10) and polyoxin on the test strains (stagonosporas cucurbitaceae and Nigrospora oryzae) were measured by Abbott's method, respectively, and the volume ratio of the mixture (oleander flower/kuh-seng/cnidium lactone = 2.0/3.0/10) and polyoxin was made to be 10: 1, calculating the synergistic coefficient (SR) of each mixture according to an Abbott formula, and selecting the optimal mixture ratio. Clear water was used as control. SR =1, the two bactericides have an additive effect after being mixed, and SR >1 shows that the two bactericides have a synergistic effect; SR <1 indicates antagonism. The combined effect of the two single agents after mixing was calculated using the Abbott formula and the results are shown in table 4.
TABLE 4 biological test results of test strains of polyoxins in combination with the mixture of the two active ingredients
Note: in the table, the mixture represents a plant type pesticide prepared by mixing oleander flower, sophora flavescens and cnidium lactone in a volume ratio of 2.0/3.0/10, and the ratio of the mixture to spinosad is a volume ratio. Wherein the concentration of the mixed preparation of the oleander flower, the lightyellow sophora root and the osthole is 100 mug/mL, and the concentration of the polyoxin is 40 mug/mL.
As can be seen from Table 4, the SR of the composition of the mixture of the pincer, bitter and snake and the polyoxin for preventing and treating the pumpkin cranberry mold and the black spore mold of rice is 1.07 and 1.10 respectively, and the SR is more than 1, which shows synergistic effect.
The calculation method for controlling the harmful insects by the plant-type pesticide in the embodiment is as follows:
mortality (%) = dead insect number/total insect number × l 00%;
corrected mortality (%) = (theoretical mortality-control mortality)/(100-control mortality) × 100%;
sakai formula: synergestic index = (actual mortality-theoretical mortality)/theoretical mortality x 100;
when the synergistic toxicity index is more than or equal to 20, the synergistic effect is achieved; when the synergistic toxicity index is less than or equal to-20, the antagonism is obtained; if the two are in between, the two are additive effects.
Sun cloud Pei formula method:
virulence index (TI) ═ standard pesticide LD 50/test pesticide LD50 × 100;
let the mixed drug be M and each single drug of the composition be A, B, C …. LC50A is lethal mid-concentration of agent a; LC50B is the lethal medium concentration of the medicament, LC50 is the lethal medium concentration of the mixture of the medicament A + the medicament B + the medicament C + …, the co-toxicity coefficient of the mixture is CTC, and the percentage content of the active ingredients is P.
When the co-toxicity coefficient is more than or equal to 120, the synergistic effect is considered; when the co-toxicity coefficient is less than or equal to 80, the antagonism can be considered; between the two, an additive effect is considered.
The calculation formula for controlling pathogenic bacteria by the plant-type pesticide in the embodiment is as follows:
control effect (%) = (blank control disease index-treatment disease index)/blank control disease index x 100%;
the Abbott formula calculates the combined effect of two single agents after mixing, and the calculation formula is as follows: theoretical control effect (%) =100 × (1-C1) × (1-C2);
the synergistic coefficient SR = actual control effect/theoretical control effect;
c1 and C2 each indicate the control of the effects of the two components when used alone. SR =1, then the two bactericides have the addition effect after being mixed; SR >1 shows that the composition has a synergistic effect; SR <1 indicates antagonism.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of plant type pesticide is characterized by comprising the following steps:
s1 extraction: extracting oleander flower with organic solvent I, filtering to obtain extract, extracting radix Sophorae Flavescentis with organic solvent I, and filtering to obtain radix Sophorae Flavescentis extract;
s2 concentration: evaporating the oleander flower extract and the sophora flavescens extract obtained in the step S1 respectively to obtain an oleander flower extract and an sophora flavescens extract;
s3 extraction: extracting the oleander flower extract obtained in the step S2 with an organic solvent II to obtain an oleander flower extract, and extracting the sophora flavescens extract obtained in the step S2 with an organic solvent III to obtain a sophora flavescens extract;
s4 mixing: mixing the extractive solution of flos Nerii and the extractive solution of radix Sophorae Flavescentis obtained in S3, adding osthole, and stirring to obtain plant pesticide.
2. The method for preparing a botanical pesticide as claimed in claim 1, wherein in S1, 10-15 mL of the organic solvent i is added to each 1g of the oleander flower, 8-10 mL of the organic solvent i is added to each 1g of the sophora flavescens, the extraction is performed under ultrasonic conditions, the ultrasonic power is 80-100 Hz, the extraction time is 12-24 hours, the temperature is 20-30 ℃, and the extraction times are 3-5.
3. The method for preparing a plant-type pesticide according to claim 1 or 2, wherein the organic solvent I is at least one of alcohol, aqueous alcohol solution and acetone, the alcohol is at least one of methanol, ethanol, propanol, propylene glycol and butanol, and the volume fraction of the alcohol in the aqueous alcohol solution is 65% to 80%.
4. The method for preparing a botanical pesticide as claimed in claim 1 wherein in S2, evaporation is performed in a rotary evaporator at 55-65 ℃, vacuum degree of 200-300 Pa, rotation speed of 70-100 r/min, and concentration is performed until the oleander flower and the sophora flavescens are concentrated into an extract.
5. The method for preparing a botanical pesticide as claimed in claim 1, wherein 10-15 mL of the organic solvent II is added to 1g of the oleander flower extract in S3, the extraction time of the oleander flower extract is 20-30 min, 8-10 mL of the organic solvent III is added to 1g of the sophora flavescens extract, and the extraction time of the sophora flavescens extract is 20-30 min.
6. The method for preparing a plant-type pesticide according to claim 1 or 5, wherein the organic solvent II is petroleum ether and ethyl acetate, and the volume ratio of the petroleum ether to the ethyl acetate is 1: (1-5), wherein the organic solvent III is acetone and diethyl ether, and the volume ratio of the organic solvent III is 1: (1-2).
7. The method of claim 1, wherein in step S4, the osthole is added in the form of an osthole solution, the concentration of the osthole solution is 40-200 μ g/mL by mass/volume, the solvent is at least one of alcohol and water, the alcohol is ethanol, and the volume ratio of the oleander flower extract to the sophora flavescens extract to the osthole solution is (1.5-2.0): (2.0-3.0): 10.
8. the method of claim 1, further comprising adding a synergist to the mixture of the oleander flower extract, the sophora flavescens extract and the osthole after the osthole is added.
9. The method for preparing a plant-type pesticide according to claim 8, wherein the synergist is added in the form of a synergist solution, the synergist solution has a mass volume concentration of 40-200 μ g/mL, the solvent is at least one of alcohol and water, the alcohol is ethanol, and the synergist is one or more of polyoxin and spinosad.
10. A plant-type agricultural chemical characterized by being obtained by the production method according to any one of claims 1 to 9.
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| CN113841709A (en) * | 2021-08-09 | 2021-12-28 | 福建省生命之友生物科技有限公司 | Pesticide prepared from oleander and composition thereof |
| CN115399343A (en) * | 2022-10-31 | 2022-11-29 | 山东睿鹰制药集团有限公司 | Plant composite antibacterial agent containing peony extract and preparation method and application thereof |
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| CN115399343A (en) * | 2022-10-31 | 2022-11-29 | 山东睿鹰制药集团有限公司 | Plant composite antibacterial agent containing peony extract and preparation method and application thereof |
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