CN108271794A - A kind of margosine method for producing insecticide - Google Patents
A kind of margosine method for producing insecticide Download PDFInfo
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- CN108271794A CN108271794A CN201810118162.3A CN201810118162A CN108271794A CN 108271794 A CN108271794 A CN 108271794A CN 201810118162 A CN201810118162 A CN 201810118162A CN 108271794 A CN108271794 A CN 108271794A
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- margosine
- china tree
- degreasing
- producing 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
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- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
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Abstract
The invention discloses a kind of margosine method for producing insecticide, specifically include following steps:It is prepared by degreasing China tree powder:It will be crushed after amargosa or the drying of leaf or fruit, petroleum ether degreasing, filtering, the drying of China tree residue, as degreasing China tree powder be added;It is prepared by margosine:China tree powder is put into Soxhlet extractor, ethanol solution is added, ultrasonic extraction extracts after extracting solution concentration, distills, be drying to obtain margosine;It is prepared by China tree element pesticide:Margosine is aided with common pharmaceutical excipient, the dosage forms such as aqua, pulvis are made to get China tree element pesticide.It has the beneficial effect that:Margosine method for producing insecticide simple possible of the present invention, can improve extraction efficiency, yield, bioactivity and the stability of margosine, China tree element pesticide wide spectrum obtained, efficiently.
Description
Technical field
The present invention relates to technical field of insecticide, more particularly to a kind of margosine method for producing insecticide.
Background technology
Active ingredient of natural product refers to the compound with unique function and bioactivity extracted from regenerated resources.
Natural products ingredient is complex, it is now recognized that cellulose, chlorophyll, natural gum, tannin and inorganic salts etc. are invalid components, effectively
Ingredient has alkaloid, glucoside, flavonoids, organic acid, amino acid, terpene, anthraquinone, cumarin etc..Many of which active ingredient is
Control of insect, disease prevention and cure, the material base to keep fit and healthy.Active ingredient of natural product has safe efficient, pollution-free etc. excellent
Point, it has also become agricultural, medical, food and feed important sources.
Meliaceae plant includes 50 about 550 kinds of categories, most of to belong to evergreen or fallen leaves arbors or shrub, is distributed mainly on heat
Band and temperate zone.Meliaceae melia plant mainly have print chinaberry (Azadirachta Indica A. juss), melia toosendan (M. toosendan Sieb. et Zucc) and China tree (M. azedarach Linn).Wherein print chinaberry is distributed in South Asia, Southeast Asia and other torrid zone ground
It is regional that area, China tree and melia toosendan are distributed widely in Sichuan, Hubei, Hunan, Henan, Guizhou and SOUTH OF GANSU of China etc..Printing chinaberry is
Most well-known pesticide plant in the world.Separation identifies a variety of terpenoids with insecticidal activity from print chinaberry at present
And tens of kinds of lemon class compounds, main component nimbin are a kind of highly oxidized tetracyclic triterpene substances, are had to pest
There is the effects that food refusal, interference growth and development.Melia toosendan complete stool is toxic, and fruit is more toxic, and can do sacaricide, civil to also serve as soil
Medicine.The margosine extracted from Folium Meliae, flower, seed, bark and root skin can be used as pesticide, to red spider, cabbage caterpillar, aphid etc.
Various pests have toxic action, and being mainly shown as makes worm food refusal, inhibits insect growth develop, tag, interior suction toxic action etc..It is bitter
Chinaberry element is with a wide range of applications as natural insecticide in agricultural production.Contain a variety of active ingredients in China tree, leads
Want active constituent margosine (toosendanin) Chinese medicine is can be used as driving ascarid, antibacterial, at the same and it is a kind of with broad based growth
The insecticide of foreground has toxic action to various pests, and being mainly shown as makes worm deterrent, food refusal;Inhibit insect growth development, touch
It kills, interior suction toxic action etc..Since these insecticide active substances are derived from naturally, having good compatibility with natural environment, thus
Meliaceae plant has efficient, lasting to harmful organism, safe to non-target organism, easily decomposition, does not pollute as botanical pesticide
Environment and many advantages, such as do not destroy the ecological balance, has prodigious development prospect.In recent years, domestic and international many scientific research personnel couple
Meliaceae melia plant has carried out a large amount of research work, can meet the modern times to realize that agricultural sustainable development provides infrastructural support
Change the development of new agricultural, harmonious society and circular economy.But the rate of margosine is not high, insecticide effect obtained need
It is promoted.
Invention content
The purpose of the present invention is to provide a kind of margosine method for producing insecticide, the preparation method simple possible, energy
Enough improve extraction efficiency, yield, bioactivity and the stability of margosine, China tree element pesticide wide spectrum obtained, efficiently.
The present invention in view of the above technology in the problem of mentioning, the technical solution taken is:
A kind of preparation method of margosine method for producing insecticide, including prepared by degreasing China tree powder, prepared by margosine, margosine
Prepared by insecticide, specifically include following steps:
It is prepared by degreasing China tree powder:It will be crushed after amargosa or the drying of leaf or fruit, cross 20-50 mesh sieve, then press solid-liquid ratio
It is 1:20-30(g/mL)Petroleum ether degreasing 20-30min is added, filtering removes the petroleum ether phase of upper layer liquid, leaves and takes bottom
China tree residue is dried, as degreasing China tree powder, and spare, the degreasing China tree powder after the step process can improve the extraction of margosine
Efficiency and yield are conducive to the progress of alcohol reflux extraction and extractant extraction;
It is prepared by margosine:China tree powder is put into Soxhlet extractor, is 1 by solid-liquid ratio:8-12(g/mL)The second of 60-80% is added
Alcoholic solution subsequently extracts 1-2h, extracting solution warp under conditions of ultrasonic power is 70-100W, supersonic frequency is 30-40kHz
Distillation and concentration, after with extractant extract 60-100min, extract liquor through vacuum distillation, be drying to obtain margosine, the combination of steps rope
Family name and ultrasonic in combination extract margosine, and under Soxhlet counterflow condition, China tree powder continuously by extraction, more has
Conducive to the infiltration and diffusion of margosine, while during Soxhlet extraction after introducing ultrasonic field, in a liquid using ultrasonic wave
Cavitation accelerates the leaching of margosine, and the mechanical oscillation of ultrasonic wave, diffusion the effects that smashing, can accelerate the expansion of margosine
It dissipates, release;
It is prepared by China tree element pesticide:Margosine is aided with common pharmaceutical excipient, the dosage forms such as aqua, pulvis are made to get hardship
Tomatlane pesticide, the insecticide are a kind of wide spectrum, efficient, less toxic, degradable, noresidue insecticide and the not no ring of drug resistance
Protect insecticide, can prevent cabbage caterpillar, diamondback moth, Oeobia undalis, aphid, prodenia litura, tealeaves caterpillar, dish ant, planthopper, rice volume snout moth's larva,
Borer etc., has good market prospects, and can be degradable in its nature, and safe height is provided for the production of pollution-free food
The pesticide new variety of effect, and targeting object is made to be difficult to form drug resistance in a short time.
Preferably, ethanol solution contains the triethylene diamine of 0.2-0.5mM and the N-methylmorpholine of 0.1-0.2mM, three
The addition of ethylene diamine and N-methylmorpholine can dissolve the polysaccharose substance in China tree cell wall, while can also dissolve portion
Pectic substance is divided, to weaken the inhibition that it dissolves out intracellular margosine, to make swelling to improve the permeability of cell wall
Index significantly improves, and promotes cell swelling, improves the extraction efficiency and yield of margosine, while alcohol-soluble can be prevented miscellaneous
The macromolecular components such as matter or pigment are combined with ethanol molecule, reduce its competition with margosine, improve the recovery rate of margosine, and
On the structure of margosine without influence, its activity will not be destroyed.
Preferably, the solid-liquid ratio of China tree powder and extractant is 1:3-6, extractant are that volume ratio is 1:0.03-0.05's
N-butanol and acetparaminosalol phenol mixture, the extractant effect of extracting is best, and polarity is closest with the polarity of margosine,
Good to the selectivity of margosine, the presence of paracetamol can enable margosine more rapidly more fully enter extraction phase, carry
High extraction yield, while conducive to the recycling of extractant so that the unstable isomers of margosine is to stable isomery
Body changes, and improves bioactivity, the safety and stability of margosine.
Compared with the prior art, the advantages of the present invention are as follows:1)Preparation method simple possible of the present invention, can accelerate margosine
Diffusion, release, improve extraction efficiency, the yield of margosine, have with short production cycle, active ingredient be not easy to be destroyed etc. it is excellent
Point has larger application potential;2)The Extraction solvent that the preparation method uses can improve the permeability of cell wall, improve hardship
The extraction efficiency and yield of chinaberry element, while the macromolecular components such as alcohol dissolubility impurity or pigment can be prevented to be combined with ethanol molecule,
Its competition with margosine is reduced, the recovery rate of margosine is improved;3)Choosing of the extractant that the preparation method uses to margosine
Selecting property is good, and margosine can be enable more rapidly more fully to enter extraction phase, improve extraction yield, and the biology for improving margosine is living
Property, safety and stability, while conducive to extractant recycling;4)The margosine that the preparation method obtains is a kind of wide
Spectrum, efficient, less toxic, degradable, noresidue insecticide and the not no environment-friendly pesticide of drug resistance, with before good market
Scape.
Specific embodiment
The present invention program is described further below by embodiment:
Embodiment 1:
A kind of preparation method of margosine method for producing insecticide, including prepared by degreasing China tree powder, prepared by margosine, margosine
Prepared by insecticide, specifically include following steps:
1)It is prepared by degreasing China tree powder:It will be crushed after amargosa or the drying of leaf or fruit, cross 20 mesh sieve, be then by solid-liquid ratio
1:30(g/mL)Petroleum ether degreasing 20min is added, filtering removes the petroleum ether phase of upper layer liquid, leaves and takes the China tree residue of bottom
Drying, as degreasing China tree powder, spare, the degreasing China tree powder after the step process can improve the extraction efficiency of margosine and obtain
Rate is conducive to the progress of alcohol reflux extraction and extractant extraction;
2)It is prepared by margosine:China tree powder is put into Soxhlet extractor, is 1 by solid-liquid ratio:12(g/mL)The ethyl alcohol of addition 60% is molten
Liquid, subsequently extracts 2h under conditions of ultrasonic power is 100W, supersonic frequency is 30kHz, and extracting solution is rear to use through distillation and concentration
Extractant extracts 60min, and extract liquor is drying to obtain margosine, the combination of steps Soxhlet and ultrasonic in combination are to hardship through vacuum distillation
Chinaberry element extracts, and under Soxhlet counterflow condition, China tree powder continuously by extraction, is more advantageous to the infiltration of margosine
And diffusion, while during Soxhlet extraction after introducing ultrasonic field, the cavitation of ultrasonic wave in a liquid being utilized to accelerate China tree
The leaching of element, and the mechanical oscillation of ultrasonic wave, diffusion the effects that smashing, can accelerate diffusion, the release of margosine;
3)It is prepared by China tree element pesticide:Margosine is aided with common pharmaceutical excipient, be made the dosage forms such as aqua, pulvis to get
China tree element pesticide, the insecticide are a kind of wide spectrum, efficient, less toxic, degradable, noresidue insecticide and not no drug resistance
Environment-friendly pesticide can prevent cabbage caterpillar, diamondback moth, Oeobia undalis, aphid, prodenia litura, tealeaves caterpillar, dish ant, planthopper, rice volume
Snout moth's larva, borer etc., have good market prospects, and can be degradable in its nature, and peace is provided for the production of pollution-free food
Complete efficient pesticide new variety, and targeting object is made to be difficult to form drug resistance in a short time.
Above-mentioned ethanol solution contains the triethylene diamine of 0.5mM and the N-methylmorpholine of 0.1mM, triethylene diamine and N- first
The addition of base morpholine can dissolve the polysaccharose substance in China tree cell wall, while can also dissolve part pectic substance, to
Improve the permeability of cell wall makes swelling index significantly improve to weaken the inhibition that it dissolves out intracellular margosine,
Cell swelling is promoted, the extraction efficiency and yield of margosine is improved, while alcohol dissolubility impurity or pigment can be prevented etc. and is big
Molecular chaperones are combined with ethanol molecule, reduce its competition with margosine, improve the recovery rate of margosine, and to the knot of margosine
Structure will not destroy its activity without influence.
The solid-liquid ratio of above-mentioned China tree powder and extractant is 1:6, extractant is that volume ratio is 1:0.03 n-butanol and to second
Acylamino- phenol mixture, the extractant effect of extracting is best, and polarity is closest with the polarity of margosine, the choosing to margosine
Selecting property is good, and the presence of paracetamol can enable margosine more rapidly more fully enter extraction phase, improve extraction yield, together
When conducive to extractant recycling so that the unstable isomers of margosine changes to stable isomers, improves bitter
The bioactivity of chinaberry element, safety and stability.
Embodiment 2:
A kind of preparation method of margosine method for producing insecticide, including prepared by degreasing China tree powder, prepared by margosine, margosine
Prepared by insecticide, specifically include following steps:
1)It is prepared by degreasing China tree powder:It will be crushed after amargosa or the drying of leaf or fruit, cross 50 mesh sieve, be then by solid-liquid ratio
1:20(g/mL)Petroleum ether degreasing 30min is added, filtering removes the petroleum ether phase of upper layer liquid, leaves and takes the China tree residue of bottom
Drying, as degreasing China tree powder, it is spare;
2)It is prepared by margosine:China tree powder is put into Soxhlet extractor, is 1 by solid-liquid ratio:8(g/mL)The ethyl alcohol of addition 80% is molten
Liquid, subsequently extracts 1h under conditions of ultrasonic power is 70W, supersonic frequency is 40kHz, and extracting solution is rear to use through distillation and concentration
Extractant extracts 100min, and extract liquor is drying to obtain margosine through vacuum distillation;
3)It is prepared by China tree element pesticide:Margosine is aided with common pharmaceutical excipient, be made the dosage forms such as aqua, pulvis to get
China tree element pesticide.
Above-mentioned ethanol solution contains the triethylene diamine of 0.2mM and the N-methylmorpholine of 0.2mM;China tree powder and extractant
Solid-liquid ratio is 1:3, extractant is that volume ratio is 1:0.05 n-butanol and acetparaminosalol phenol mixture.
Embodiment 3:
A kind of preparation method of margosine method for producing insecticide, including prepared by degreasing China tree powder, prepared by margosine, margosine
Prepared by insecticide, specifically include following steps:
1)It is prepared by degreasing China tree powder:It will be crushed after amargosa or the drying of leaf or fruit, cross 40 mesh sieve, be then by solid-liquid ratio
1:25(g/mL)Petroleum ether degreasing 25min is added, filtering removes the petroleum ether phase of upper layer liquid, leaves and takes the China tree residue of bottom
Drying, as degreasing China tree powder, it is spare;
2)It is prepared by margosine:China tree powder is put into Soxhlet extractor, is 1 by solid-liquid ratio:10(g/mL)The ethyl alcohol of addition 70% is molten
Liquid, subsequently extracts 1.5h under conditions of ultrasonic power is 80W, supersonic frequency is 35kHz, extracting solution through distillation and concentration, after
80min is extracted with extractant, extract liquor is drying to obtain margosine through vacuum distillation;
3)It is prepared by China tree element pesticide:Margosine is aided with common pharmaceutical excipient, be made the dosage forms such as aqua, pulvis to get
China tree element pesticide.
Above-mentioned ethanol solution contains the triethylene diamine of 0.4mM and the N-methylmorpholine of 0.16mM;China tree powder and extractant
Solid-liquid ratio be 1:5, extractant is that volume ratio is 1:0.04 n-butanol and acetparaminosalol phenol mixture.
Routine operation in the operating procedure of the present invention is well known to those skilled in the art, herein without repeating.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of margosine method for producing insecticide, including prepared by degreasing China tree powder, prepared by margosine, China tree element pesticide system
It is standby, it is characterised in that:The margosine preparation process is:China tree powder is put into Soxhlet extractor, ethanol solution is added, then so
Extracted afterwards in ultrasonic work(, extracting solution through distillation and concentration, after extracted with extractant, extract liquor is drying to obtain China tree through vacuum distillation
Element, the ethanol solution contain triethylene diamine and N-methylmorpholine.
2. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The ethanol solution is dense
It is 60-80% to spend, and the solid-liquid ratio of China tree powder and ethanol solution is 1:8-12(g/mL).
3. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The ethanol solution contains
There are the triethylene diamine of 0.2-0.5mM and the N-methylmorpholine of 0.1-0.2mM.
4. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The ultrasonic power is
70-100W, supersonic frequency 30-40kHz, extraction time 1-2h.
5. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The extractant is body
Product is than being 1:The n-butanol and acetparaminosalol phenol mixture of 0.03-0.05.
6. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The China tree powder and extraction
It is 1 to take the solid-liquid ratio of agent:3-6 extracts 60-100min.
7. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The degreasing China tree powder
Preparation process is:It will be crushed after amargosa or the drying of leaf or fruit, cross 20-50 mesh sieve, it is 1 then to press solid-liquid ratio:20-30
(g/mL)Petroleum ether degreasing 20-30min is added, the petroleum ether phase of upper layer liquid is removed in filtering, and the China tree residue for leaving and taking bottom dries
It does, as degreasing China tree powder.
8. a kind of margosine method for producing insecticide according to claim 1, it is characterised in that:The margosine desinsection
Agent preparation process is:Margosine is aided with common pharmaceutical excipient, the dosage forms such as aqua, pulvis are made to get margosine desinsection
Agent.
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CN201810118162.3A CN108271794A (en) | 2018-02-06 | 2018-02-06 | A kind of margosine method for producing insecticide |
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CN201810118162.3A CN108271794A (en) | 2018-02-06 | 2018-02-06 | A kind of margosine method for producing insecticide |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110623886A (en) * | 2019-10-31 | 2019-12-31 | 山东花物堂生物科技有限公司 | Preparation method of cortex meliae extract |
CN111544387A (en) * | 2020-04-18 | 2020-08-18 | 内蒙古医科大学 | Compound quercetin antibacterial nanoemulsion and preparation method thereof |
WO2022105916A1 (en) * | 2020-11-23 | 2022-05-27 | 江南大学 | Use of neem bark pigment in preparation for multifunctional wool fabric |
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CN101177448A (en) * | 2007-11-20 | 2008-05-14 | 合肥工业大学 | Method for extracting mersosin by ultrasonic field assisted with mixed solvent |
CN108378047A (en) * | 2018-02-06 | 2018-08-10 | 浦江县欧立生物技术有限公司 | The preparation method of pest killing micro emulsion |
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2018
- 2018-02-06 CN CN201810118162.3A patent/CN108271794A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101177448A (en) * | 2007-11-20 | 2008-05-14 | 合肥工业大学 | Method for extracting mersosin by ultrasonic field assisted with mixed solvent |
CN108378047A (en) * | 2018-02-06 | 2018-08-10 | 浦江县欧立生物技术有限公司 | The preparation method of pest killing micro emulsion |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110623886A (en) * | 2019-10-31 | 2019-12-31 | 山东花物堂生物科技有限公司 | Preparation method of cortex meliae extract |
CN111544387A (en) * | 2020-04-18 | 2020-08-18 | 内蒙古医科大学 | Compound quercetin antibacterial nanoemulsion and preparation method thereof |
CN111544387B (en) * | 2020-04-18 | 2021-11-02 | 内蒙古医科大学 | Compound quercetin antibacterial nanoemulsion and preparation method thereof |
WO2022105916A1 (en) * | 2020-11-23 | 2022-05-27 | 江南大学 | Use of neem bark pigment in preparation for multifunctional wool fabric |
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Application publication date: 20180713 |