CN101731289A - 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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- CN101731289A CN101731289A CN200910254500A CN200910254500A CN101731289A CN 101731289 A CN101731289 A CN 101731289A CN 200910254500 A CN200910254500 A CN 200910254500A CN 200910254500 A CN200910254500 A CN 200910254500A CN 101731289 A CN101731289 A CN 101731289A
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- aconitum sinomontanum
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- water aqua
- pesticide
- emulsifier
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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 aspects such as increasing crop yield, simultaneously, the 3R problem that it causes, promptly residual (Residue), resistance (Resistance) and insect rampant (Resurgence) more also generally are subjected to people's attention.
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 had food refusal, avoid and keep away that suppress to grow, control effects such as population, insect is difficult for producing resistance simultaneously.
In the nearly 30,000 kinds of higher plants of China, there are nearly thousand plant species to have insecticidal activity approximately, the active component of these plants is good disinsection effect not only, to crops safety 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 big 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, with from high rhizome of Chinese monkshood plant, separate first obtain to go methylene light delphinine (Demethylenedelcorine), delsoline (delsoline) to have another name called consoline, 3 kinds of Diterpenes alkaloids of lepenine (lepenine) be that formulated a kind of of main active both had high antifeedant activity composition, the novel plant source pesticide that contains the feeding active composition again, 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 an aconitine-type alkaloids, and they are number of C
19And C
20The Diterpenes alkaloid.And from this plant species, separate first and obtained going methylene light delphinine (Demethylenedelcorine), delsoline (delsoline) to have another name called consoline, 3 kinds of Diterpenes alkaloids of lepenine (lepenine).And it has been carried out determination of activity through Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T, and the result shows, separates these 3 kinds of materials that obtain from the high rhizome of Chinese monkshood first, except that having higher bacteriostatic activity, its insecticidal activity is also outstanding especially.Experiment shows that preceding 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 antifeedant activity composition, and the plant that contains the feeding active composition again is still rare.The present invention is a main active with these three kinds of active ingredients, has developed a kind of novel plant source pesticide.
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 a 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 a 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 a methyl alcohol.
The preparation method of aconitum sinomontanum water aqua pesticide of the present invention:
(1) alkaloid 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 methanol extraction that adds 10 times of amounts refluxes 3 times, each 1.5h, suction filtration, merging filtrate, be concentrated into dried, methanolic extract; Add the 2%HCl dissolving then, under acid condition, divide 3 extractions, remove the ester solubility impurity with benzinum (60～90 ℃ of boiling ranges); Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times, be concentrated into dry product with chloroform.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, with ether: ethyl acetate=20: 1 is eluant, eluent, separate methylene light delphinine, delsoline, three kinds of active substances of lepenine, with the ether recrystallization, make methylene light delphinine, delsoline, three kinds of active ingredients of lepenine then.
(3) with active ingredient with dissolution with solvents after, add emulsifier, after stirring, add the excess water mixing and get final product.
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 Diterpenes alkaloids of lepenine (lepenine) be main active.These three kinds of active components are except that having higher bacteriostatic activity, and its insecticidal activity is also outstanding especially.Wherein, preceding 2 kinds have higher antifeedant activity, its to three age mythimna separata 3d food refusal rate be respectively 100% and 70.1%.The back has feeding active for a kind, and the food calling rate reaches 99.5%.Therefore the present invention is a kind of high antifeedant activity composition that both had, and contains the novel plant source pesticide of feeding active composition again.
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, wetting and spreadability on the various plants blade; On this basis, the prescription of research aqueous emulsion has obtained the best formulations of pesticide aqua of plant insecticide, is rather well received and a kind of formulation of recommending to the utmost in the present formulations of pesticide.
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, press formulation rate 66.7mL/ mu, 50mL/ mu and 40mL/ mu and contrast, examine or check its control efficiency the cabbage caterpillar in the brassicaceous vegetable cabbage field with 50% butyl ether urea wetting powder and clear water.The medicine liquid spray amount is a 40kg/ mu, and dispenser once.
Result of the test: test shows that the present invention has efficiently, low toxicity, nuisanceless, easy degraded, and plurality of advantages such as environmentally compatible, have food refusal preferably and certain lethal, can in 7 days, more efficiently control the harm of cabbage caterpillar, have potential development and application values.Anti-back 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-back 7 days, its drug effect before had the raising of certain amplitude, has reached 81.21%, 76.77% and 70.56% respectively.And do not see in the process of the test that reagent agent produces poisoning to the head cabbage varieties for examination.(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 a 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) alkaloid 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 methanol extraction that adds 10 times of amounts refluxes 3 times, each 1.5h, suction filtration, merging filtrate, be concentrated into dried, methanolic extract; Add 4000mL 2%HCl dissolving then, under acid condition, divide 3 extractions, remove the ester solubility impurity with benzinum (60～90 ℃ of boiling ranges) 6000mL; Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times, be concentrated into dry product with the 8000mL chloroform.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, with ether: ethyl acetate=20: 1 is eluant, eluent, isolates 9 kinds of materials, is recrystallized with ether then; 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 (6)
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%, solvent 12～18%, surplus is a 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%, solvent 15%, surplus is a water.
3. a kind of aconitum sinomontanum water aqua pesticide according to claim 1 and 2 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 is characterized in that: described emulsifier is by fatty alcohol-polyoxyethylene ether 50～80%, and alkylaryl polyoxyethylene polyoxypropylene ether 20～50% is formulated.
5. a kind of aconitum sinomontanum water aqua pesticide according to claim 1 and 2 is characterized in that: described solvent is a methyl alcohol.
6. the preparation method of the described aconitum sinomontanum water aqua pesticide of claim 1 is characterized in that:
(1) alkaloid 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 methanol extraction that adds 10 times of amounts refluxes 3 times, each 1.5h, suction filtration, merging filtrate, be concentrated into dried, methanolic extract; Add the 2%HCl dissolving then, under acid condition, divide 3 extractions, remove the ester solubility impurity with benzinum (60～90 ℃ of boiling ranges); Transfer pH to 9 with ammoniacal liquor again, divide the alkaloid in the extraction solution 4 times, be concentrated into dry product with chloroform.
(2) this dry product is pressed the sample preparation of column chromatography method for making sample, upper prop, with ether: ethyl acetate=20: 1 is eluant, eluent, separate methylene light delphinine, delsoline, three kinds of active substances of lepenine, with the ether recrystallization, make methylene light delphinine, delsoline, three kinds of active ingredients of lepenine then.
(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 |
Applications Claiming Priority (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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| CN101731289A true CN101731289A (en) | 2010-06-16 |
| CN101731289B 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102934632A (en) * | 2012-11-20 | 2013-02-20 | 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 |
| CN112106789A (en) * | 2020-09-11 | 2020-12-22 | 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 (1)
| Title |
|---|
| 朱见: "植物生物碱的杀虫作用及应用", 《蚕学通讯》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102934632A (en) * | 2012-11-20 | 2013-02-20 | 江苏省中国科学院植物研究所 | Application of yunaconitine in pesticides |
| 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 |
| CN112106789A (en) * | 2020-09-11 | 2020-12-22 | 安徽农业大学 | Application of delphinium ethyl acetate extract in preventing and treating diamond back moth |
| 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 |
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| CN101731289B (en) | 2013-04-17 |
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