CN101731289B - Aconitum sinomontanum water aqua pesticide and preparation method thereof - Google Patents
Aconitum sinomontanum water aqua pesticide and preparation method thereof Download PDFInfo
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- CN101731289B CN101731289B CN 200910254500 CN200910254500A CN101731289B CN 101731289 B CN101731289 B CN 101731289B CN 200910254500 CN200910254500 CN 200910254500 CN 200910254500 A CN200910254500 A CN 200910254500A CN 101731289 B CN101731289 B CN 101731289B
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- aconitum sinomontanum
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- water aqua
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Abstract
The invention discloses an aconitum sinomontanum water aqua pesticide which is prepared from the following raw materials in percentage by weight: 0.4-0.8% of effective ingredient, 7-10% of emulsifier, 12-18% of solvent and the balance water. The preparation method is as follows: dissolving the effective ingredient with solvent, adding emulsifier, evenly stirring, adding the balance water, and evenly mixing. The aconitum sinomontanum water aqua pesticide takes three of Demethylenedelcorine, delsoline (alternate name is elatine) and lepenine which are obtained from the aconitum sinomontanum plant by separation for the first time to serve as the main active ingredients, and the aconitum sinomontanum water aqua pesticide is a novel botanical pesticide containing high-apastia active ingredients and food calling active ingredients. The aconitum sinomontanum water aqua pesticide has the advantages of high efficiency, low toxin, no public hazard, easy degradation, compatibility with environment and the like and has favourable effect by field experiments.
Description
Technical field
The present invention relates to a kind of botanical pesticide, is a kind of aconitum sinomontanum water aqua pesticide and preparation method thereof specifically.
Background technology
The use of chemical pesticide is in human health, indelible effect has been brought into play in the aspects such as increasing crop yield, simultaneously, the 3R problem that it causes, namely residual (Residue), resistance (Resistance) and pest resurgence (Resurgence) also generally receive people's concern.
Botanical pesticide and environment have higher harmonious degree: 1. its amount of application is to the person poultry safety; 2. easily decompose under natural environment, residual quantity is low; 3. be the natural multiple agent that is mixed, insect is had food refusal, avoids and keep away, suppress to grow, control the effects such as population, insect is difficult for producing resistance simultaneously.
In the nearly 30,000 kinds of higher plants of China, approximately there are nearly thousand Plants to have insecticidal activity, the active component of these plants is good disinsection effect not only, to Crop securify and easily degraded, the longevity of residure is short, be difficult for developing immunity to drugs, have a bright future as plant insecticide. and people only account for 10% to what their chemical property carried out studying, commercial plant pesticide is Feng Maolinjiao especially, therefore numerous plants are studied, and then be developed as vegetable insecticide, not only have very large research and development potentiality, and be to be well worth doing.
Summary of the invention
The technical problem that the present invention solves: a kind of aconitum sinomontanum water aqua pesticide and preparation method thereof is provided, take from high rhizome of Chinese monkshood plant, separate first obtain go methylene light delphinine (Demethylenedelcorine), delsoline (delsoline) to have another name called consoline, 3 kinds of Diterpenoid Alkaloids of lepenine (lepenine) both to have had high antifeeding component as formulated a kind of of main active, the novel plant source pesticide that contains again the feeding active composition, and it has been made field experiment, the result shows, and is respond well.
Mentality of designing of the present invention: the present invention has carried out system to the high rhizome of Chinese monkshood (Conitum sinomoutanum) methanolic extract and has separated and activity research, and the active insecticidal components of finding the high rhizome of Chinese monkshood is aconitine-type alkaloids, and they are number of C
19And C
20Diterpenoid Alkaloids.And from this Plants, separate first and obtained going methylene light delphinine (Demethylenedelcorine), delsoline (delsoline) to have another name called consoline, 3 kinds of Diterpenoid Alkaloids of lepenine (lepenine).And through Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T it has been carried out determination of activity, and the result shows, separates first these 3 kinds of materials that obtain from the high rhizome of Chinese monkshood, except having higher bacteriostatic activity, its insecticidal activity is also outstanding especially.Experiment shows, front 2 kinds have higher antifeedant activity, its to three age mythimna separata 3d food refusal rate be respectively 100% and 70.1%.1 kind has feeding active in addition, and the food calling rate reaches 99.5%.This both had a high antifeeding component, and the plant that contains again the feeding active composition is still rare.The present invention has developed a kind of novel plant source pesticide take these three kinds of active ingredients as main active.
The present invention is made by the raw material of following weight ratio: active ingredient 0.4%～0.8%, and emulsifier 7～10%, solvent 12～18%, surplus is water.
The present invention is preferably made by the raw material of following weight ratio: active ingredient 0.5%, and emulsifier 8%, solvent 15%, surplus is water.
Described active ingredient is by removing methylene light delphinine: delsoline: the weight ratio of lepenine=1: 3: 0.5 is formulated.Described emulsifier is by fatty alcohol-polyoxyethylene ether 50～80%, and alkylaryl polyoxyethylene polyoxypropylene ether 20～50% is formulated.Described solvent is methyl alcohol.
The preparation method of aconitum sinomontanum water aqua pesticide of the present invention:
(1) alkaloidal extraction: high rhizome of Chinese monkshood meal is wetting and do not touch with one's hand with the alkali lye of 10 times of amounts, and the methyl alcohol that adds 10 times of amounts extracts and refluxes 3 times, each 1.5h, and suction filtration, merging filtrate is concentrated into driedly, gets methanolic extract; Then add the 2%HCl dissolving, under acid condition, with benzinum (60～90 ℃ of boiling ranges) minute 3 extractions, remove the ester solubility impurity; Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times with chloroform, be concentrated into dry product.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, take ether: ethyl acetate=20: 1 is as eluant, eluent, separate methylene light delphinine, delsoline, three kinds of active substances of lepenine, then with the ether recrystallization, make methylene light delphinine, delsoline, three kinds of active ingredients of lepenine.
(3) with active ingredient with dissolution with solvents after, add emulsifier, after stirring, add the excess water mixing and get final product.
The advantage that the present invention compared with prior art has and effect:
1, the present invention adopt from the high rhizome of Chinese monkshood, separate first obtain to remove methylene light delphinine (Demethylenedelcorine), delsoline (delsoline), 3 kinds of Diterpenoid Alkaloids of lepenine (lepenine) be main active.These three kinds of active components are except having higher bacteriostatic activity, and its insecticidal activity is also outstanding especially.Wherein, front 2 kinds have higher antifeedant activity, its to three age mythimna separata 3d food refusal rate be respectively 100% and 70.1%.Rear a kind has feeding active, and the food calling rate reaches 99.5%.Therefore the present invention is a kind of high antifeeding component that both had, and contains again the novel plant source pesticide of feeding active composition.
2, owing to activated alkaloid in the high rhizome of Chinese monkshood is water miscible mostly, the present invention is guaranteeing under the condition that biologically active does not reduce, start with from missible oil at present commonly used, select different emulsifier, wetting agent, study that different proportionings mix at the various plants blade, wetting and spreadability; On this basis, studying the prescription of aqueous emulsion, obtained the best formulations of pesticide aqua of plant insecticide, is a kind of formulation rather well received in the present formulations of pesticide and that recommend to the utmost.
3, the technical indicator that reaches of the present invention: outward appearance: be single-phase transparency liquid, active constituent content: 0.4%～0.8%, pH=6～7, emulsifying dispersivity: qualified, heat storage stability: 54 ± 2 ℃, 14d, active ingredient resolution ratio＜5%, cold storage stability: 5 ℃, 7d, active ingredient resolution ratio ≯ 0.3%, dispersed, suspensibility: qualified.
4, field experiment result of the present invention.Xibei Univ. of Agricultural ﹠ Forest Science ﹠ Technology has carried out field experiment in August, 2008 to the present invention, compare by formulation rate 66.7mL/ mu, 50mL/ mu and 40mL/ mu and with 50% diafenthiuron wetting powder and clear water, examine or check it to the control efficiency of the cabbage caterpillar in the brassicaceous vegetable cabbage field.The medicine liquid spray amount is 40kg/ mu, and dispenser once.
Result of the test: test shows that the present invention has efficiently, low toxicity, nuisanceless, easy degraded, and the plurality of advantages such as environmentally compatible, have preferably food refusal and certain lethal, can in 7 days, more efficiently control the harm of cabbage caterpillar, have potential development and application values.Anti-rear 2 days, the preventive effect of its formulation rate 66.7mL/ mu, 50mL/ mu and 40mL/ mu was respectively 71.6%, 67.54% and 63.56%; Anti-rear 7 days, its drug effect before had the raising of certain amplitude, has reached respectively 81.21%, 76.77% and 70.56%.And have no reagent agent in the process of the test head cabbage varieties for examination is produced poisoning.(attached drug effect field trial report is a)
Embodiment
The present invention is preferably made by the raw material of following weight ratio: active ingredient 0.5%, and emulsifier 8%, methanol solvate 15%, surplus is water.
Described active ingredient is by removing methylene light delphinine: delsoline: the weight ratio of lepenine=1: 3: 0.5 is formulated.Described emulsifier is by fatty alcohol-polyoxyethylene ether 60%, and alkylaryl polyoxyethylene polyoxypropylene ether 40% is formulated.
Preparation method of the present invention:
(1) alkaloidal extraction: high rhizome of Chinese monkshood meal 10Kg is wetting and do not touch with one's hand with the alkali lye of 10 times of amounts, and the methyl alcohol that adds 10 times of amounts extracts and refluxes 3 times, each 1.5h, and suction filtration, merging filtrate is concentrated into driedly, gets methanolic extract; Then add 4000mL 2%HCl dissolving, under acid condition, divide 3 extractions with benzinum (60～90 ℃ of boiling ranges) 6000mL, remove the ester solubility impurity; Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times with the 8000mL chloroform, be concentrated into dry product.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, take ether: ethyl acetate=20: 1 is isolated 9 kinds of materials as eluant, eluent, then is recrystallized with ether; Isolated 9 kinds of materials methylene light delphinine, delsoline, three kinds of active substances of lepenine have been determined to go through active testing and multispectral discriminating.
(3) by removing methylene light delphinine: delsoline: the weight ratio preparation active ingredient of lepenine=1: 3: 0.5, after the methanol solvate dissolving, add emulsifier, after stirring, add the excess water mixing and get final product.
Claims (5)
1. aconitum sinomontanum water aqua pesticide is characterized in that being made by the raw material of following weight ratio: active ingredient 0.4%～0.8%, and emulsifier 7～10%, methyl alcohol 12～18%, surplus is water.
2. a kind of aconitum sinomontanum water aqua pesticide according to claim 1 is characterized in that preferably being made by the raw material of following weight ratio: active ingredient 0.5%, and emulsifier 8%, methyl alcohol 15%, surplus is water.
3. a kind of aconitum sinomontanum water aqua pesticide according to claim 1 and 2, it is characterized in that: described active ingredient is by removing methylene light delphinine: delsoline: the weight ratio of lepenine=1: 3: 0.5 is formulated.
4. a kind of aconitum sinomontanum water aqua pesticide according to claim 1 and 2, it is characterized in that: described emulsifier is by fatty alcohol-polyoxyethylene ether 50～80%, and alkylaryl polyoxyethylene polyoxypropylene ether 20～50% is formulated.
5. the preparation method of an aconitum sinomontanum water aqua pesticide claimed in claim 1 is characterized in that:
(1) alkaloidal extraction: high rhizome of Chinese monkshood meal is wetting and do not touch with one's hand with the alkali lye of 10 times of amounts, and the methyl alcohol that adds 10 times of amounts extracts and refluxes 3 times, each 1.5h, and suction filtration, merging filtrate is concentrated into driedly, gets methanolic extract; Then add the 2%HCl dissolving, the benzinum with 60～90 ℃ of boiling ranges under acid condition divides 3 extractions, removes the ester solubility impurity; Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times with chloroform, be concentrated into dry product.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, take ether: ethyl acetate=20: 1 is as eluant, eluent, separate methylene light delphinine, delsoline, three kinds of active substances of lepenine, then with the ether recrystallization, make methylene light delphinine, delsoline, three kinds of active ingredients of lepenine.
(3) with active ingredient with dissolution with solvents after, add emulsifier, after stirring, add the excess water mixing and get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910254500 CN101731289B (en) | 2009-12-17 | 2009-12-17 | Aconitum sinomontanum water aqua pesticide and preparation method thereof |
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| CN 200910254500 CN101731289B (en) | 2009-12-17 | 2009-12-17 | Aconitum sinomontanum water aqua pesticide and preparation method thereof |
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| CN101731289A CN101731289A (en) | 2010-06-16 |
| CN101731289B true CN101731289B (en) | 2013-04-17 |
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| CN 200910254500 Expired - Fee Related CN101731289B (en) | 2009-12-17 | 2009-12-17 | Aconitum sinomontanum water aqua pesticide and preparation method thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102934632B (en) * | 2012-11-20 | 2014-04-09 | 江苏省中国科学院植物研究所 | Application of yunaconitine in pesticides |
| CN108770876A (en) * | 2018-08-06 | 2018-11-09 | 沂南县迎辉农业开发有限公司 | A kind of biological agent and preparation method of prevention ginger snout moth's larva |
| CN112106789B (en) * | 2020-09-11 | 2021-08-24 | 安徽农业大学 | Application of delphinium ethyl acetate extract in preventing and treating diamond back moth |
| CN113925067A (en) * | 2021-10-22 | 2022-01-14 | 重庆御尚生物科技有限公司 | Chinese herbal medicine preparation for preventing and treating wax moth and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290784A (en) * | 1991-07-18 | 1994-03-01 | Yueqian Qu | Aconitane derivatives used as a medication to treat addiction |
| CN1088919A (en) * | 1993-01-01 | 1994-07-06 | 中国科学院华南植物研究所 | The extraction process of lappaconitine |
-
2009
- 2009-12-17 CN CN 200910254500 patent/CN101731289B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290784A (en) * | 1991-07-18 | 1994-03-01 | Yueqian Qu | Aconitane derivatives used as a medication to treat addiction |
| CN1088919A (en) * | 1993-01-01 | 1994-07-06 | 中国科学院华南植物研究所 | The extraction process of lappaconitine |
Non-Patent Citations (2)
| Title |
|---|
| 朱见.植物生物碱的杀虫作用及应用.《蚕学通讯》.2007,35-40. |
| 植物生物碱的杀虫作用及应用;朱见;《蚕学通讯》;20071231;35-40 * |
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