CN106359467A - Preparation method of plant-derived pesticide - Google Patents
Preparation method of plant-derived pesticide Download PDFInfo
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- CN106359467A CN106359467A CN201610789665.4A CN201610789665A CN106359467A CN 106359467 A CN106359467 A CN 106359467A CN 201610789665 A CN201610789665 A CN 201610789665A CN 106359467 A CN106359467 A CN 106359467A
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- plant insecticide
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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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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]
- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- Dentistry (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a preparation method of a plant-derived pesticide. The preparation method comprises the following steps: taking cloves, drying, and pulverizing into powder; adding into an ethanol water solution, leaching, and regulating the pH value of the leaching solution to 8.0-10.0; introducing into a macropore adsorbent resin to perform impurity removal, performing reduced pressure concentration on the obtained permeation solution, and performing supercritical carbon dioxide extraction on the extractum to obtain an extract; and finally, mixing the extract with Tween-65, sodium stearoyl-2-lactylate, Span-80 and ethanol, stirring while heating, adding the mixture into water, and dispersing. According to the invention, effective pesticide components of the cloves are extracted and prepared into a microemulsion; and the obtained pesticide is efficient for pests and safe for humans and livestock, and has less environmental influence.
Description
Technical field
The invention belongs to technical field of pesticide is and in particular to a kind of preparation method of plant insecticide.
Background technology
At present although chemical synthetic pesticide is because its prevention effect is good, speed fast, it is still the important of preventing and treating diseases and pests of agronomic crop
Means, application amount is very big, but due to unreasonably abuse or the problem of itself, create serious negative effect, that is, so-called
" 3r " problem: pesticide residues (residue) cause environmental pollution, damages human and livestock health；Chemical pesticide is also also easy to produce Drug resistance
(resistance), so that pest and disease damage is difficult to control to；Chemical synthetic pesticide is big to natural enemy lethality, destroys ecological balance, holds
Easily cause pest and disease damage rampant (resurgence) again.There are both at home and abroad two purposes to botanical pesticide active matter Quality Research: one
It is to find the lead compound synthesizing new chemical pesticide from plant, most successful example such as comes from the pyrethrin pesticide of Pyrethrum
Lead compound, come from lead compound of the imidacloprid pesticide of nicotine etc.；Two is that direct application has pesticidal active substance
Plant resource explorationses new plant pesticide.Abroad mostly because resource shortage is then based on first purpose.China, because vast territory and abundant resources, plants
Thing aboundresources, a lot of plants have cultivation history.Therefore, direct appliable plant resource mostly, develops botanical pesticide.
Microemulsion is thermodynamically stable, isotropic, the appearance transparent or semi-transparent that two kinds of non soluble liquids are formed
Bright dispersion, microcosmic is made up of the microdroplet of one or two stable liquid of surfactant interface film.Due to
Microemulsion achieves the substantially innoxious of solvent, has preferable drug effect simultaneously again, can reduce pesticide to a certain extent
Usage amount, so microemulsion has the preferable feature of environmental protection, meets the developing direction of chemistry security.The dosage form of China's insecticide with
Based on cream, contain a large amount of dimethylbenzene in preparation, microemulsion improvement is carried out to these preparations, there is critically important realistic meaning.
Content of the invention
The technical problem solving: the purpose of the present invention is to overcome the deficiencies in the prior art and provide a kind of plant insecticide
Preparation method, be extracted effective insecticidal constituent of Flos Caryophylli and make microemulsion, gained insecticide to pest efficient, is pacified to people, animal
Entirely, effect on environment is little.
Technical scheme: a kind of preparation method of plant insecticide, comprise the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 3-5 times of weight portion, 50-60 DEG C of leaching
Carry 2-4h, let cool, obtain lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
In carry out supercritical carbon dioxide extraction, obtain extract；
Step 4, in parts by weight, by 10 parts of extract and Tween-65 6-12 part, sodium stearoyl lactate 4-7 part, Span
80 3-7 parts, the mixing of ethanol 30-35 part, heated and stirred, mixture is added in water 40-50 part, dispersion, obtain final product.
Further, in step 1 powder size in 80-100 mesh.
Further, in step 1, the concentration of ethanol water is 95v/v%.
Further, 15-20wt% sodium hydroxide solution is adopted to adjust ph in step 2.
Further, extraction temperature 40-55 DEG C, pressure 20-30mpa in step 3, guiding and supporting agent is dehydrated alcohol.
Further, in step 4, dispersion condition is 800-1000rpm, 10-20min.
Beneficial effect: the present invention is extracted effective insecticidal constituent of Flos Caryophylli and makes microemulsion, gained insecticide is high to insect
Effect, to people, animal safety, effect on environment is little.
Specific embodiment
Embodiment 1
A kind of preparation method of plant insecticide, comprises the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 3 times of weight portions, 50 DEG C of extraction 4h,
Let cool, obtain lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
In carry out supercritical carbon dioxide extraction, obtain extract；
Step 4, in parts by weight, by 10 parts of extract and 6 parts of Tween-65,4 parts of sodium stearoyl lactate, Span 80 3
Part, 30 parts of mixing of ethanol, heated and stirred, mixture is added in 40 parts of water, dispersion, obtain final product.
Wherein, in step 1 powder size in 80 mesh, the concentration of ethanol water is 95v/v%；Adopt in step 2
20wt% sodium hydroxide solution adjusts ph；40 DEG C of extraction temperature, pressure 20mpa in step 3, guiding and supporting agent is dehydrated alcohol；Step 4
Middle dispersion condition is 800rpm, 20min.
Embodiment 2
A kind of preparation method of plant insecticide, comprises the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 4 times of weight portions, 50 DEG C of extraction 4h,
Let cool, obtain lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
In carry out supercritical carbon dioxide extraction, obtain extract；
Step 4, in parts by weight, by 10 parts of extract and 9 parts of Tween-65,5 parts of sodium stearoyl lactate, Span 80 4
Part, 31 parts of mixing of ethanol, heated and stirred, mixture is added in 45 parts of water, dispersion, obtain final product.
Wherein, in step 1 powder size in 80 mesh, the concentration of ethanol water is 95v/v%；Adopt in step 2
15wt% sodium hydroxide solution adjusts ph；50 DEG C of extraction temperature, pressure 25mpa in step 3, guiding and supporting agent is dehydrated alcohol；Step 4
Middle dispersion condition is 900rpm, 20min.
Embodiment 3
A kind of preparation method of plant insecticide, comprises the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 3 times of weight portions, 55 DEG C of extraction 3h,
Let cool, obtain lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
In carry out supercritical carbon dioxide extraction, obtain extract；
Step 4, in parts by weight, by 10 parts of extract and 10 parts of Tween-65,6 parts of sodium stearoyl lactate, Span 80 5
Part, 30 parts of mixing of ethanol, heated and stirred, mixture is added in 45 parts of water, dispersion, obtain final product.
Wherein, in step 1 powder size in 100 mesh, the concentration of ethanol water is 95v/v%；Adopt in step 2
15wt% sodium hydroxide solution adjusts ph；55 DEG C of extraction temperature, pressure 30mpa in step 3, guiding and supporting agent is dehydrated alcohol；Step 4
Middle dispersion condition is 1000rpm, 10min.
Embodiment 4
A kind of preparation method of plant insecticide, comprises the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 3 times of weight portions, 50 DEG C of extraction 4h,
Let cool, obtain lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
In carry out supercritical carbon dioxide extraction, obtain extract；
Step 4, in parts by weight, by 10 parts of extract and 12 parts of Tween-65,7 parts of sodium stearoyl lactate, Span 80 7
Part, 35 parts of mixing of ethanol, heated and stirred, mixture is added in 50 parts of water, dispersion, obtain final product.
Wherein, in step 1 powder size in 80 mesh, the concentration of ethanol water is 95v/v%；Adopt in step 2
20wt% sodium hydroxide solution adjusts ph；40 DEG C of extraction temperature, pressure 20mpa in step 3, guiding and supporting agent is dehydrated alcohol；Step 4
Middle dispersion condition is 800rpm, 20min.
Embodiment 5
The present embodiment is with the difference of embodiment 3: also contains 1-2wt% potassium citrate in ethanol water in step 1.
Stability of emulsion
Embodiment 1 to 5 gained insecticide is diluted 200 times with 342mg/l standard hard water, diluent stands at 30 DEG C
24h, keeps pellucidity, no grease suspends or precipitation of solid material, and can mix in any proportion with water, and emulsion is more steady
Fixed.
Cold storage stability
Take out after embodiment 1 to 5 gained insecticide is freezed at low temperature, voluntarily recover transparent at room temperature in 1h completely
State.This test is repeated 6 times and all can voluntarily recover, and shows that sample has cold storage stability well.
Field control effectiveness test
Uniform from growing fine, growing, and the Caulis et Folium Brassicae capitatae that the medium weighting of Pieris rapae occurs does field control effectiveness test.Every medicament
Concentration processes and is repeated 3 times, and every cell is a repetition, and plot area is 30m2.Processing cell adopts random district's groups to arrange, and 0.3%
Embodiment 1 to 5 gained microemulsion, with 800 times of 0.5% chinaberry element cream for standard control medicament, to spray clear water as blank.Dispenser
Carried out with aerosol apparatus, every mu of spouting liquid is 50kg.Every cell middle row fixed point 20 plants of Caulis et Folium Brassicae capitataes of labelling, before the dispenser and after medicine
1d, 3d, 7d, 10d, 13d, 16d investigate the whole borer populations in labelling cabbage plant strain, and point 1～3 age, 4 ages, 3 grades of 5 age
Record respectively.Drug effect statistics is carried out with conventional method respectively, and carries out multiple ratio with " dtmr " method to 1d, 3d and 7d preventive effect after medicine
Relatively.Result is as follows:
| Insect population/head | 1d preventive effect/% | 3d preventive effect/% | 5d preventive effect/% | |
| Embodiment 1 | 135 | 83.45 | 88.14 | 95.62 |
| Embodiment 2 | 140 | 85.53 | 91.07 | 96.52 |
| Embodiment 3 | 143 | 87.35 | 90.42 | 95.78 |
| Embodiment 4 | 138 | 84.17 | 89.52 | 96.73 |
| Embodiment 5 | 140 | 92.15 | 96.78 | 98.63 |
| 0.5% chinaberry element cream | 140 | 13.70 | 68.76 | 88.37 |
| Comparison | 145 | 0 | 0 | 0 |
Claims (6)
1. a kind of preparation method of plant insecticide it is characterised in that: comprise the following steps:
Step 1, takes Flos Caryophylli, dries, grind into powder, adds in the ethanol water of 3-5 times of weight portion, 50-60 DEG C of extraction 2-
4h, lets cool, and obtains lixiviating solution；
Step 2, adjusts lixiviating solution ph to 8.0-10.0, imports macroporous adsorbent resin and carries out remove impurity, collects permeate；
Step 3, permeate is 1.25-1.35 through being evaporated to 60 DEG C of relative densities, and gained extractum is placed in extraction kettle
Row supercritical carbon dioxide extraction, obtains extract；
Step 4, in parts by weight, by 10 parts of extract and Tween-65 6-12 part, sodium stearoyl lactate 4-7 part, Span 80 3-
7 parts, the mixing of ethanol 30-35 part, heated and stirred, mixture is added in water 40-50 part, dispersion, obtain final product.
2. plant insecticide according to claim 1 preparation method it is characterised in that: in step 1, powder size exists
80-100 mesh.
3. plant insecticide according to claim 1 preparation method it is characterised in that: ethanol water in step 1
Concentration be 95v/v%.
4. plant insecticide according to claim 1 preparation method it is characterised in that: adopt 15- in step 2
20wt% sodium hydroxide solution adjusts ph.
5. plant insecticide according to claim 1 preparation method it is characterised in that: extraction temperature 40- in step 3
55 DEG C, pressure 20-30mpa, guiding and supporting agent is dehydrated alcohol.
6. plant insecticide according to claim 1 preparation method it is characterised in that: in step 4, dispersion condition is
800-1000rpm、10-20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610789665.4A CN106359467A (en) | 2016-08-31 | 2016-08-31 | Preparation method of plant-derived pesticide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610789665.4A CN106359467A (en) | 2016-08-31 | 2016-08-31 | Preparation method of plant-derived pesticide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106359467A true CN106359467A (en) | 2017-02-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610789665.4A Pending CN106359467A (en) | 2016-08-31 | 2016-08-31 | Preparation method of plant-derived pesticide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107047651A (en) * | 2017-05-11 | 2017-08-18 | 曾济天 | A kind of plant nanometer agricultural chemicals and preparation method thereof |
| CN107307014A (en) * | 2017-07-17 | 2017-11-03 | 铜仁市万山区大坪乡瓮岩村俊峰精果有限公司 | A kind of apple tree insecticide and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718005A (en) * | 2005-04-11 | 2006-01-11 | 西北农林科技大学 | Plant extract used as miticide |
| CN102246829A (en) * | 2011-07-28 | 2011-11-23 | 北京农学院 | Clove extract for killing nematode and preparation method thereof |
-
2016
- 2016-08-31 CN CN201610789665.4A patent/CN106359467A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718005A (en) * | 2005-04-11 | 2006-01-11 | 西北农林科技大学 | Plant extract used as miticide |
| CN102246829A (en) * | 2011-07-28 | 2011-11-23 | 北京农学院 | Clove extract for killing nematode and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 于泓鹏等: ""丁香精油的超临界CO2 和溶剂回流萃取及其GC-MS 分析"", 《分析与检测》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107047651A (en) * | 2017-05-11 | 2017-08-18 | 曾济天 | A kind of plant nanometer agricultural chemicals and preparation method thereof |
| CN107307014A (en) * | 2017-07-17 | 2017-11-03 | 铜仁市万山区大坪乡瓮岩村俊峰精果有限公司 | A kind of apple tree insecticide and preparation method thereof |
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Application publication date: 20170201 |