CN108651448A - A kind of formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion - Google Patents
A kind of formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion Download PDFInfo
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- CN108651448A CN108651448A CN201810447913.6A CN201810447913A CN108651448A CN 108651448 A CN108651448 A CN 108651448A CN 201810447913 A CN201810447913 A CN 201810447913A CN 108651448 A CN108651448 A CN 108651448A
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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
- 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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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
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- 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
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- 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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Abstract
The present invention discloses a kind of formula of Schima superba bark saponin pest killing micro emulsion：Schima superba bark saponin 3 7%, organic solvent 5 20%, emulsifier 20 30%, remaining as distilled water；The present invention also provides the preparation methods of the Schima superba bark saponin pest killing micro emulsion, Schima superba bark saponin is dissolved in organic solvent, it is mixed again with emulsifier, it is handled in good pressure distribution homogenizer, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water be added after be homogenized 15 25min to get；The Schima superba bark saponin pest killing micro emulsion of the present invention has good field control effect to diamondback moth, cabbage caterpillar etc., the usage amount of microemulsion can be effectively reduced, reduce planting cost, also help the pollution for reducing pesticide to crop and to water and soil, there are good economic benefit and social benefit, there is good promotion prospect.
Description
Technical field
The present invention relates to technical field of pesticide, and in particular to a kind of formula and its system of Schima superba bark saponin pest killing micro emulsion
Preparation Method.
Background technology
Microemulsion (microemulsion, ME) is a kind of pesticides new formulation that the 1980s, foreign countries occurred.It is with water
For matrix, does not have to or only with a small amount of organic solvent, contain proper amount of surfactant and other auxiliary agents, be transparent single phase liquid.Micro emulsion
Agent not only saves a large amount of organic solvents using water as main solvent, and the pressure to environment has been considerably reduced after pharmacy application, right
In safeguarding that agroecological environment is of great significance, be conducive to the sustainable development of agricultural.Therefore microemulsion is a kind of friendly to environment
Good green bioagrochemicals are selectable as the novel form of substitution missible oil, and suitable for certain only such as wettable powder agent
The pesticide original medicine kind of type.
Schima superba (Shima superba Gardn.et Champ.) alias lotus wood, wood Ai Shu, He Shu, Hui Shu, horizontal bavin are
The high megaphanerophyte of Theaceae Schima superba Pterostyrax, is distributed on the south the Yangtze river basin, Fujian, Taiwan, Yunnan, Sichuan, Guizhou, Zhejiang,
The ground such as Anhui, Guangdong, Guangxi.Schima superba mainly contains triterpene and saponins, bessisterol, epicatechin, hydrolyzable tannin class, cloves
The chemical compositions such as aldehyde and Kaempferol, volatile oil.Currently, having reported that Schima superba triterpenoid saponin compound has 9 kinds.The root skin of Schima superba
It is acrid in flavour and warm in nature, enter the spleen channel, very toxic, effect：It is clearing heat and detoxicating, control furunculosis, nameless sores or boils.In terms of biological pesticide research, according to report
Road Schima superba has higher resisting rice blast bacteria, Fusarium Solani, Sclerotinia sclerotiorum, verticillium wilt of cotton bacterium activity；Schima superba is to small
Diamond-back moth and cabbage caterpillar have higher antifeedant activity and growth and development inhibitory activity；Schima superba lives to Pomacea canaliculata with stronger poisoning
Property.The applicant is in previous research work it has proven convenient that containing saponin component in Schima superba bark, by preferred, to Schima superba saponin
Extraction process is optimized, and the content of colorimetric method for determining Schima superba bark Total saponin is determined.The method is easy to operate, accurate
Really, stability is preferable, can be used for measuring Schima superba bark extract total saponin content.The application is exactly to be using Schima superba bark saponin
Raw material prepares microemulsion, deeply develops the biological pesticide value of Schima superba.
Invention content
It is an object of the invention to overcome defect of the existing technology, a kind of Schima superba bark saponin pest killing micro emulsion is provided
Formula and preparation method thereof.
To achieve the goals above, the technical solution adopted by the present invention is as follows：
The formula and preparation method thereof of the Schima superba bark saponin pest killing micro emulsion of the present invention, by the original of following mass percent
What material was prepared：Schima superba bark saponin 3-7%, organic solvent 5-20%, emulsifier 20-30%, remaining as distilled water；
The preparation method of the Schima superba bark saponin pest killing micro emulsion includes the following steps：
Schima superba bark saponin is dissolved in organic solvent, then material is put into high speed dispersion homogenizer, is added
Emulsifier makes mixed material carry out emulsifying homogeneous processing after mixing, and the rotating speed of adjustment high speed dispersion homogenizer is 3500-
7000r/min, distilled water is added by several times in the homogenate tube of high speed dispersion homogenizer and the pH value of control material is 5-8, distillation
Water be added after be homogenized 15-25min to get.
Preferably, it is prepared by the raw material of following mass percent：Schima superba bark saponin 5%, organic solvent 15%,
Emulsifier 25%, remaining as distilled water；
The preparation method of the Schima superba bark saponin pest killing micro emulsion includes the following steps：
Schima superba bark saponin is dissolved in organic solvent, then material is put into high speed dispersion homogenizer, is added
Emulsifier makes mixed material carry out emulsifying homogeneous processing after mixing, and the rotating speed of adjustment high speed dispersion homogenizer is 5000r/
Distilled water is added in the homogenate tube of high speed dispersion homogenizer and the pH value of control material is 7 by min by several times, and distilled water has been added
Finish after homogenate 20min to get.
Preferably, the organic solvent is any one in methanol, petroleum ether, acetone, toluene, absolute ethyl alcohol, chloroform
Kind.
Preferably, the organic solvent is methanol or absolute ethyl alcohol.
Preferably, the emulsifier be TW-80, TX-10, OP-10, BY-110, in agriculture breast 600# any one or
Arbitrary two kinds of mixture.
Preferably, the emulsifier is the mixing of the mixture, TW-80 and TX-10 of TX-10, agriculture breast 600# and TX-10
Any one in object.
Preferably, when distilled water being added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 5-10 etc.
Part, divide in the homogenate tube of 5-10 addition high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water adds in 2-5min
Enter to finish.
Preferably, the preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 50-65 DEG C, is then ground into Schima superba bark
The particle of 30-50 mesh is added Extraction solvent and extracts 2-3 times, and the dosage of each Extraction solvent is the 3-6 of Schima superba bark particle weight
Times, each extraction time is 36-60h, merges leaching liquor, and filtering is evaporated under reduced pressure Extraction solvent using Rotary Evaporators, obtains cream
Shape extract is added isometric extractant and is extracted, take extract liquor, use after distilled water dissolving paste extract is added
Extractant is evaporated under reduced pressure in Rotary Evaporators, and resultant product is Schima superba bark saponin.
Preferably, the Extraction solvent is methanol or ethyl alcohol.
Preferably, the extractant is any one in petroleum ether, chloroform or n-butanol.
The present invention is by adopting the above-described technical solution, have the advantages that：
1, the applicant provides a kind of system of Schima superba bark saponin pest killing micro emulsion on the basis of investigation and comparison for many years
Schima superba bark saponin is dissolved in organic solvent, places into high speed dispersion homogenizer and mixed with emulsifier, then by Preparation Method
Side by several times be added distillation waterside be homogenized, this method is simple and practicable, easy to operate, be added portionwise distilled water be conducive to improve have
The emulsification uniformity coefficient of solvent and emulsifier, and improve the transparent of the Schima superba bark saponin pest killing micro emulsion product finally obtained
Degree, cold storage stability, heat storage stability, microemulsion often store the performances such as stability.
2, the present invention passes through single factor experiment and orthogonal test, it is determined that the best of Schima superba bark saponin pest killing micro emulsion is matched
Technique processed is：The mass percent of Schima superba bark saponin is 5%, and the mass percent of ethyl alcohol is 15%, the matter of emulsifier TX-10
It is 25% to measure percentage, and pH value 7, distilled water supplies 100%；Under this optimised process, obtained Schima superba bark saponin desinsection
The cold storage stability of microemulsion product, heat storage stability, microemulsion often store stability, transparency temperature range, pH value meet it is micro-
Emulsion national standard.
3, the present invention also provides the extracting methods of Schima superba saponin, and the extraction of Schima superba saponin is carried out using Schima superba bark, and
Schima superba saponin extraction process is optimized, the Extraction solvent and extractant for being suitable for extracting Schima superba saponin is selected, reduces to the greatest extent
Other impurities in Schima superba saponin improve the using effect of Schima superba bark microemulsion；Secondly, the present invention is extracted from Schima superba bark
The utility value of Schima superba can be improved in Schima superba saponin, deeply develops the biological pesticide value of Schima superba, and reduction contains the micro- of Schima superba saponin
The production cost of emulsion, increases economic efficiency.
4, when present invention extraction Schima superba bark saponin, Extraction solvent and extractant are used the rotary evaporator to vaporize, it is recyclable
Extraction solvent and extractant carry out purification recycling, both reduce production cost, improve the safety of production environment, can also subtract
The discharge of rare solvent waste, reduces environmental pollution.
5, Schima superba bark saponin pest killing micro emulsion of the invention imitates diamondback moth, cabbage caterpillar etc. with good field control
Fruit can effectively reduce the usage amount of microemulsion, reduce planting cost, also help and reduce pesticide to crop and to water and soil
Pollution, have good economic benefit and social benefit, have good promotion prospect.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
There are one thorough explanations for the one or more aspects of invention, can also realize the present invention's even without these specific details
These aspects.
Embodiment 1
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：3% Schima superba bark soap
Glucoside, 5% methanol, 20%TW-80, remaining as distilled water；
Schima superba bark saponin is dissolved in methanol, the mixed material of Schima superba bark saponin and methanol is then put into high speed
In homogeneous dispersion machine, TW-80 is added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment high speed dispersion is even
The rotating speed of matter machine is 3500r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer the simultaneously pH of control material by several times
Value be 5, distilled water be added after be homogenized 15min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 5 equal portions, divides 5 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 5min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 50 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 6 times of Schima superba bark particle weight, 3 times, every time when extraction
Between be respectively 60h, 36h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric petroleum ether is added and is extracted, takes extract liquor, is subtracted using Rotary Evaporators
Pressure evaporation petroleum ether, resultant product is Schima superba bark saponin.
Embodiment 2
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：3.3% Schima superba bark soap
Glucoside, 6% petroleum ether, 21%TX-10, remaining as distilled water；
Schima superba bark saponin is dissolved in methanol, the mixed material of Schima superba bark saponin and petroleum ether is then put into height
In fast homogeneous dispersion machine, TX-10 is added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjusts high speed dispersion
The rotating speed of homogenizer is 3700r/min, distilled water is added by several times in the homogenate tube of high speed dispersion homogenizer and control material
PH value is 5.2, distilled water be added after be homogenized 16min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 6 equal portions, divides 6 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 4.8min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 51 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 4 times, every time when extraction
Between be respectively 48h, 40h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric chloroform is added and is extracted, takes extract liquor, is depressurized using Rotary Evaporators
Chloroform is evaporated, resultant product is Schima superba bark saponin.
Embodiment 3
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：3.5% Schima superba bark soap
Glucoside, 7% acetone, 22%OP-10, remaining as distilled water；
Schima superba bark saponin is dissolved in acetone, the mixed material of Schima superba bark saponin and acetone is then put into high speed
In homogeneous dispersion machine, OP-10 is added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment high speed dispersion is even
The rotating speed of matter machine is 3900r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer the simultaneously pH of control material by several times
Value be 5.4, distilled water be added after be homogenized 17min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 7 equal portions, divides 7 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 4.5min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 52 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 3 times, every time when extraction
Between be respectively 52h, 30h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric n-butanol is added and is extracted, takes extract liquor, is subtracted using Rotary Evaporators
Pressure evaporation n-butanol, resultant product is Schima superba bark saponin.
Embodiment 4
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：3.8% Schima superba bark soap
Glucoside, 8% toluene, 23%BY-110, remaining as distilled water；
Schima superba bark saponin is dissolved in toluene, the mixed material of Schima superba bark saponin and toluene is then put into high speed
In homogeneous dispersion machine, BY-110 is added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment high speed dispersion is even
The rotating speed of matter machine is 4100r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer the simultaneously pH of control material by several times
Value be 5.6, distilled water be added after be homogenized 18min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 8 equal portions, divides 8 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 4.2min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 53 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 4 times, every time when extraction
Between be respectively 48h, 40h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric petroleum ether is added and is extracted, takes extract liquor, is subtracted using Rotary Evaporators
Pressure evaporation petroleum ether, resultant product is Schima superba bark saponin.
Embodiment 5
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：4% Schima superba bark soap
Glucoside, 9% absolute ethyl alcohol, 24% agriculture breast 600#, remaining as distilled water；
Schima superba bark saponin is dissolved in absolute ethyl alcohol, then by the mixed material of Schima superba bark saponin and absolute ethyl alcohol
It is put into high speed dispersion homogenizer, adds agriculture breast 600#, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjust
The rotating speed of high speed dispersion homogenizer is 4300r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer and is controlled by several times
The pH value of material processed be 5.8, distilled water be added after be homogenized 19min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 9 equal portions, divides 9 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 3.9min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 54 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 5 times, every time when extraction
Between be respectively 55h, 48h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric chloroform is added and is extracted, takes extract liquor, is depressurized using Rotary Evaporators
Chloroform is evaporated, resultant product is Schima superba bark saponin.
Embodiment 6
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：4.3% Schima superba bark soap
Glucoside, 10% chloroform, 12%TX-10,13% agriculture breast 600#, remaining as distilled water；
Schima superba bark saponin is dissolved in chloroform, the mixed material of Schima superba bark saponin and chloroform is then put into high speed
In homogeneous dispersion machine, TX-10, agriculture breast 600# are added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment is high
The rotating speed of speed dispersion homogenizer is 4500r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer and is controlled by several times
The pH value of material be 6, distilled water be added after be homogenized 20min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 10 equal portions, is divided 10 times
It is added in the homogenate tube of high speed dispersion homogenizer, 1 equal portions is added every time, every part of distilled water is added in 3.6min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 55 DEG C, Schima superba bark is then ground into 30 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 4 times of Schima superba bark particle weight, 3 times, every time when extraction
Between be respectively 48h, 38h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric n-butanol is added and is extracted, takes extract liquor, is subtracted using Rotary Evaporators
Pressure evaporation n-butanol, resultant product is Schima superba bark saponin.
Embodiment 7
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：4.6% Schima superba bark soap
Glucoside, 11% methanol, 13%TX-10,13%TW-80, remaining as distilled water；
Schima superba bark saponin is dissolved in methanol, the mixed material of Schima superba bark saponin and methanol is then put into high speed
In homogeneous dispersion machine, TX-10, TW-80 are added, mixed material is made to carry out emulsifying homogeneous processing, adjustment high speed after mixing
The rotating speed for disperseing homogenizer is 4700r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times and controls object
The pH value of material be 6.2, distilled water be added after be homogenized 21min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 9 equal portions, divides 9 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 3.3min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 56 DEG C, Schima superba bark is then ground into 40 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 5 times, every time when extraction
Between be respectively 50h, 48h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric petroleum ether is added and is extracted, takes extract liquor, is subtracted using Rotary Evaporators
Pressure evaporation petroleum ether, resultant product is Schima superba bark saponin.
Embodiment 8
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：4.8% Schima superba bark soap
Glucoside, 12% acetone, 13%TX-10,14%OP-10, remaining as distilled water；
Schima superba bark saponin is dissolved in acetone, the mixed material of Schima superba bark saponin and acetone is then put into high speed
In homogeneous dispersion machine, TX-10, OP-10 are added, mixed material is made to carry out emulsifying homogeneous processing, adjustment high speed after mixing
The rotating speed for disperseing homogenizer is 4900r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times and controls object
The pH value of material be 6.4, distilled water be added after be homogenized 22min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 8 equal portions, divides 8 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 3min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 57 DEG C, Schima superba bark is then ground into 40 mesh
Particle, methanol is added and extracts 2 times, the dosage of each methanol be respectively 5 times of Schima superba bark particle weight, 4 times, every time when extraction
Between be respectively 52h, 46h, merge leaching liquor, filtering, using Rotary Evaporators be evaporated under reduced pressure methanol, obtain paste extract, add
After entering distilled water dissolving paste extract, isometric chloroform is added and is extracted, takes extract liquor, is depressurized using Rotary Evaporators
Chloroform is evaporated, resultant product is Schima superba bark saponin.
Embodiment 9
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：5% Schima superba bark soap
Glucoside, 13% toluene, 14%TX-10,14%BY-110, remaining as distilled water；
Schima superba bark saponin is dissolved in toluene, the mixed material of Schima superba bark saponin and toluene is then put into high speed
In homogeneous dispersion machine, TX-10, BY-110 are added, mixed material is made to carry out emulsifying homogeneous processing, adjustment high speed after mixing
The rotating speed for disperseing homogenizer is 5100r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times and controls object
The pH value of material be 6.6, distilled water be added after be homogenized 23min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 7 equal portions, divides 7 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.7min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 58 DEG C, Schima superba bark is then ground into 40 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 6 times of Schima superba bark particle weight, 4 times, 3 times, soak every time
It is respectively 53h, 50h, 48h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric n-butanol is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates n-butanol, and resultant product is Schima superba bark saponin.
Embodiment 10
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：5.3% Schima superba bark soap
Glucoside, 14% absolute ethyl alcohol, 15%TX-10,14% agriculture breast 600#, remaining as distilled water；
Schima superba bark saponin is dissolved in absolute ethyl alcohol, then by the mixed material of Schima superba bark saponin and absolute ethyl alcohol
It is put into high speed dispersion homogenizer, adds TX-10, agriculture breast 600#, mixed material is made to carry out at emulsifying homogeneous after mixing
The rotating speed of reason, adjustment high speed dispersion homogenizer is 5300r/min, and distilled water is added to the homogenate tube of high speed dispersion homogenizer by several times
In and control material pH value be 6.8, distilled water be added after be homogenized 24min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 6 equal portions, divides 6 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.5min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 59 DEG C, Schima superba bark is then ground into 40 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 5 times of Schima superba bark particle weight, 4 times, 3 times, soak every time
It is respectively 54h, 50h, 45h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric petroleum ether is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates petroleum ether, and resultant product is Schima superba bark saponin.
Embodiment 11
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：5.6% Schima superba bark soap
Glucoside, 15% chloroform, 15%TW-80,15%OP-10, remaining as distilled water；
Schima superba bark saponin is dissolved in chloroform, the mixed material of Schima superba bark saponin and chloroform is then put into high speed
In homogeneous dispersion machine, TW-80, OP-10 are added, mixed material is made to carry out emulsifying homogeneous processing, adjustment high speed after mixing
The rotating speed for disperseing homogenizer is 5500r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times and controls object
The pH value of material be 7, distilled water be added after be homogenized 25min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 5 equal portions, divides 5 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.4min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 60 DEG C, Schima superba bark is then ground into 40 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 5 times of Schima superba bark particle weight, 3 times, 3 times, soak every time
It is respectively 51h, 42h, 38h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric chloroform is added and is extracted, extract liquor is taken, is steamed using rotation
It sends out instrument and chloroform is evaporated under reduced pressure, resultant product is Schima superba bark saponin.
Embodiment 12
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：5.9% Schima superba bark soap
Glucoside, 16% methanol, 14%TW-80,15%BY-110, remaining as distilled water；
Schima superba bark saponin is dissolved in methanol, the mixed material of Schima superba bark saponin and methanol is then put into high speed
In homogeneous dispersion machine, TW-80, BY-110 are added, mixed material is made to carry out emulsifying homogeneous processing, adjustment high speed after mixing
The rotating speed for disperseing homogenizer is 5700r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times and controls object
The pH value of material be 7.2, distilled water be added after be homogenized 24min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 6 equal portions, divides 6 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.3min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 61 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 4 times of Schima superba bark particle weight, 4 times, 3 times, soak every time
It is respectively 50h, 48h, 39h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric n-butanol is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates n-butanol, and resultant product is Schima superba bark saponin.
Embodiment 13
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：6.2% Schima superba bark soap
Glucoside, 17% petroleum ether, 12%TW-80,14% agriculture breast 600#, remaining as distilled water；
Schima superba bark saponin is dissolved in petroleum ether, is then put into the mixed material of Schima superba bark saponin and petroleum ether
In high speed dispersion homogenizer, TW-80, agriculture breast 600# are added, mixed material is made to carry out emulsifying homogeneous processing after mixing, is adjusted
The rotating speed of whole high speed dispersion homogenizer is 6000r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer simultaneously by several times
The pH value of control material be 7.4, distilled water be added after be homogenized 23min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 7 equal portions, divides 7 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.2min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 62 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 5 times of Schima superba bark particle weight, 5 times, 3 times, soak every time
It is respectively 48h, 40h, 36h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric petroleum ether is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates petroleum ether, and resultant product is Schima superba bark saponin.
Embodiment 14
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：6.5% Schima superba bark soap
Glucoside, 18% petroleum ether, 11%TX-10,12%BY-110, remaining as distilled water；
Schima superba bark saponin is dissolved in petroleum ether, is then put into the mixed material of Schima superba bark saponin and petroleum ether
In high speed dispersion homogenizer, TX-10, BY-110 are added, mixed material is made to carry out emulsifying homogeneous processing after mixing, is adjusted
The rotating speed of high speed dispersion homogenizer is 6300r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer and is controlled by several times
The pH value of material processed be 7.5, distilled water be added after be homogenized 22min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 8 equal portions, divides 8 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2.1min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 62 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 5 times of Schima superba bark particle weight, 3 times, 3 times, soak every time
It is respectively 57h, 50h, 39h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric chloroform is added and is extracted, extract liquor is taken, is steamed using rotation
It sends out instrument and chloroform is evaporated under reduced pressure, resultant product is Schima superba bark saponin.
Embodiment 15
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：6.8% Schima superba bark soap
Glucoside, 19% acetone, 10%TX-10,11% agriculture breast 600#, remaining as distilled water；
Schima superba bark saponin is dissolved in acetone, the mixed material of Schima superba bark saponin and acetone is then put into high speed
In homogeneous dispersion machine, TX-10, agriculture breast 600# are added, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment is high
The rotating speed of speed dispersion homogenizer is 6600r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer and is controlled by several times
The pH value of material be 7.8, distilled water be added after be homogenized 21min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 9 equal portions, divides 9 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 63 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 4 times of Schima superba bark particle weight, 3 times, 3 times, soak every time
It is respectively 54h, 40h, 37h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric n-butanol is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates n-butanol, and resultant product is Schima superba bark saponin.
Embodiment 16
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：7% Schima superba bark soap
Glucoside, 20% absolute ethyl alcohol, 10%BY-110,10%OP-10, remaining as distilled water；
Schima superba bark saponin is dissolved in absolute ethyl alcohol, then by the mixed material of Schima superba bark saponin and absolute ethyl alcohol
It is put into high speed dispersion homogenizer, adds BY-110, OP-10, mixed material is made to carry out emulsifying homogeneous processing after mixing,
The rotating speed for adjusting high speed dispersion homogenizer is 7000r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times
And the pH value of control material be 8, distilled water be added after be homogenized 20min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 10 equal portions, is divided 10 times
It is added in the homogenate tube of high speed dispersion homogenizer, 1 equal portions is added every time, every part of distilled water is added in 2min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 64 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 6 times of Schima superba bark particle weight, 5 times, 3 times, soak every time
It is respectively 53h, 46h, 40h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric petroleum ether is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates petroleum ether, and resultant product is Schima superba bark saponin.
Embodiment 17
A kind of Schima superba bark saponin pest killing micro emulsion, is made of the raw material of following mass percent：5% Schima superba bark soap
Glucoside, 15% absolute ethyl alcohol, 25%TX-10, remaining as distilled water；
Schima superba bark saponin is dissolved in absolute ethyl alcohol, then by the mixed material of Schima superba bark saponin and absolute ethyl alcohol
It is put into high speed dispersion homogenizer, adds TX-10, mixed material is made to carry out emulsifying homogeneous processing after mixing, adjustment is high
The rotating speed of speed dispersion homogenizer is 5000r/min, and distilled water is added in the homogenate tube of high speed dispersion homogenizer and is controlled by several times
The pH value of material be 7, distilled water be added after be homogenized 20min to get；
When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 10 equal portions, is divided 10 times
It is added in the homogenate tube of high speed dispersion homogenizer, 1 equal portions is added every time, every part of distilled water is added in 2.5min and finishes；
The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 65 DEG C, Schima superba bark is then ground into 50 mesh
Particle, be added alcohol steep 3 times, the dosage of each ethyl alcohol be respectively 6 times of Schima superba bark particle weight, 5 times, 4 times, soak every time
It is respectively 48h, 46h, 40h to carry the time, merges leaching liquor, and filtering is evaporated under reduced pressure ethyl alcohol using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric petroleum ether is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporates petroleum ether, and resultant product is Schima superba bark saponin.
Orthogonal Experiment and Design
The applicant selects Schima superba tree to obtain the optimised process formula of Schima superba bark saponin pest killing micro emulsion of the present invention
The microemulsion that skin saponin mass percent is 5%, devises 3 single factor experiments, using the transparency T of microemulsion as index, leads to
Single factor experiment comparison is crossed, show that the best solvent of solute effect is ethyl alcohol, optimum addition 15%；Emulsifying effectiveness is best
Emulsifier be TX-10, optimum addition 25%；PH value transparency T of microemulsion obtained at 7 reaches highest.
On the basis of above-mentioned 3 single factor experiment results, select three be affected to 5% Schima superba bark saponin pest killing micro emulsion because
Element：Ethanol consumption, emulsifier TX-10 dosages and microemulsion pH value, 3 factor of design, 3 horizontal orthogonal test are with transparency T
Inspection target, preferably the optimum formula process conditions of 5% Schima superba bark saponin pest killing micro emulsion.Each factor level of experiment is shown in Table
1, orthogonal experiments are shown in Table 2.
1 Recipe L of table9(33) factor level table
2 orthogonal experiments of table
As shown in Table 2, from orthogonal test variance analysis it is found that the shadow of the thick saponin microemulsion of 5% Schima superba bark of each factor pair
Ring degree be：Ethanol consumption (A) ﹥ emulsifier TX-10 dosage (B) ﹥ pH value (C).Being compared by K can obtain, horizontal important in A factors
Property is followed successively by K2﹥ K3﹥ K1, horizontal importance is followed successively by K in B factors2﹥ K1﹥ K3, horizontal importance is followed successively by K in C factors3﹥
K2﹥ K1.Therefore, the optimised process of 5% Schima superba bark saponin pest killing micro emulsion is combined as A2B2C3, i.e. the mass percent of ethyl alcohol is
The mass percent of 15%, emulsifier TX-10 are 25%, and pH value 7, distilled water supplies 100%.
It carries out preparing microemulsion according to the optimised process formula of table 2, repeats experiment 3 times, measure obtained microemulsion
Property indices, assay method are as follows：Pesticide pH is measured with reference to GB/T 1601-1993, is surveyed with reference to GB/T 19137-2003
Fixed cold storage stability (14d) measures heat storage stability (14d) with reference to GB/T 19136-2003, is surveyed with reference to GB/T 1603-2001
Determine microemulsion and often stores stability (30d)；Dispersibility, which measures, then uses syringe to draw aqueous emulsion sample 0.5mL, apart from the water surface
It at 2cm, is slowly added drop-wise in the graduated cylinder equipped with standard hard water, observes its dispersion and emulsification situation.Transparency T utilizes ultraviolet spectrometry
Photometer is according to T (%)=It/I0It detects, I in formulatFor transmitted intensity, I0For incident intensity.Transparency temperature range detection：
It takes 10mL samples in 25mL test tubes, agitation up and down is held in both hands with stirring, until appearance muddiness is cooled on ice bath gradually or is freezed,
The temperature for recording this turning point is placed in as transparency temperature lower limit T1, then by test tube in water-bath, slowly with the speed of 2 DEG C/min
There is temperature T2, as temperature upper limit when muddiness in heating, record, then transparency temperature ranging from T1-T2.Measurement result is shown in Table 3.
The quality measurements of 3 5% Schima superba bark saponin pest killing micro emulsion of table
As shown in Table 3, it is prepared by optimised process, repeats experiment 3 times, 5% each Schima superba bark saponin pest killing micro emulsion
All meet the national standard of microemulsion.The applicant passes through single factor experiment and orthogonal test, it is determined that 5% Schima superba bark saponin
The best preparing process of pest killing micro emulsion is：The mass percent of ethyl alcohol is 15%, and the mass percent of emulsifier TX-10 is
25%, pH value 7, distilled water supplies 100% (i.e. the technical recipe of the embodiment of the present invention 17).Under this optimised process, repeat
Experiment 3 times, cold storage stability, heat storage stability, microemulsion often store stability, transparency temperature range, pH value and meet micro emulsion
Agent national standard.
Field control effect is tested
The Schima superba obtained for the formula and preparation method of verifying Schima superba bark saponin pest killing micro emulsion provided by the invention
The insecticidal effect of bark saponin pest killing micro emulsion, using the embodiment of the present invention 17 provide Schima superba bark saponin pest killing micro emulsion into
The field control effect of diamondback moth is tested after the dilution of row different multiples, is compared using clear water, test result is shown in Table 4.
4 5% Schima superba bark saponin pest killing micro emulsion various concentration of table handles the field efficacy of diamondback moth
As shown in Table 4, the Schima superba bark saponin pest killing micro emulsion that the embodiment of the present invention 17 provides has diamondback moth good
Field control effect, but with the increase of extension rate, control effect gradually weakens, 5% Schima superba bark saponin desinsection micro emulsion
The control effect of the 100 times of liquid and 200 times of liquid of agent is not much different, therefore, in order to save use cost, 5% Schima superba bark saponin
200 times of liquid of pest killing micro emulsion are the preferable selection for preventing diamondback moth.
Claims (10)
1. a kind of formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion, it is characterised in that：By following quality percentage
What the raw material of ratio was prepared：Schima superba bark saponin 3-7%, organic solvent 5-20%, emulsifier 20-30%, remaining as distillation
Water；
The preparation method of the Schima superba bark saponin pest killing micro emulsion includes the following steps：
Schima superba bark saponin is dissolved in organic solvent, then material is put into high speed dispersion homogenizer, adds emulsification
Agent makes mixed material carry out emulsifying homogeneous processing after mixing, and the rotating speed of adjustment high speed dispersion homogenizer is 3500-7000r/
Distilled water is added in the homogenate tube of high speed dispersion homogenizer and the pH value of control material is 5-8 by min by several times, and distilled water is added
After be homogenized 15-25min to get.
2. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 1, it is characterised in that：
It is prepared by the raw material of following mass percent：Schima superba bark saponin 5%, organic solvent 15%, emulsifier 25%, residue
For distilled water；
The preparation method of the Schima superba bark saponin pest killing micro emulsion includes the following steps：
Schima superba bark saponin is dissolved in organic solvent, then material is put into high speed dispersion homogenizer, adds emulsification
Agent makes mixed material carry out emulsifying homogeneous processing after mixing, and the rotating speed of adjustment high speed dispersion homogenizer is 5000r/min,
Distilled water is added by several times in the homogenate tube of high speed dispersion homogenizer and the pH value of control material is 7, after distilled water is added
Be homogenized 20min to get.
3. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 1 or 2, feature exists
In：The organic solvent is any one in methanol, petroleum ether, acetone, toluene, absolute ethyl alcohol, chloroform.
4. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 3, it is characterised in that：
The organic solvent is methanol or absolute ethyl alcohol.
5. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 1 or 2, feature exists
In：The emulsifier is TW-80, TX-10, OP-10, BY-110, any one or arbitrary two kinds mixed in agriculture breast 600#
Close object.
6. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 5, it is characterised in that：
The emulsifier is any one in the mixture of TX-10, the mixture of agriculture breast 600# and TX-10, TW-80 and TX-10.
7. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 1 or 2, feature exists
In：When distilled water is added in the homogenate tube of high speed dispersion homogenizer by several times, distilled water is divided into 5-10 equal portions, divides 5-10 times and adds
In the homogenate tube for entering high speed dispersion homogenizer, 1 equal portions are added every time, every part of distilled water is added in 2-5min and finishes.
8. the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 1 or 2, feature exists
In：The preparation method of the Schima superba bark saponin includes the following steps：
After Schima superba bark is dried in the shade, it is dried to Schima superba bark embrittlement at 50-65 DEG C, Schima superba bark is then ground into 30-50
Purpose particle is added Extraction solvent and extracts 2-3 times, and the dosage of each Extraction solvent is 3-6 times of Schima superba bark particle weight, often
Secondary extraction time is 36-60h, merges leaching liquor, and filtering is evaporated under reduced pressure Extraction solvent using Rotary Evaporators, obtains paste and carry
Object is taken, after distilled water dissolving paste extract is added, isometric extractant is added and is extracted, takes extract liquor, uses rotation
Evaporation under reduced pressure evaporation agent, resultant product are Schima superba bark saponin.
9. according to the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 8, feature
It is：The Extraction solvent is methanol or ethyl alcohol.
10. according to the formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion according to claim 8, feature
It is：The extractant is any one in petroleum ether, chloroform or n-butanol.
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Citations (3)
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|---|---|---|---|---|
| US20080311221A1 (en) * | 2007-06-14 | 2008-12-18 | Pbi/Gordon Corporation | Lewis acid and oil-soluble hybrid pesticide concentrate that spontaneously forms a water-based microemulsion |
| CN102657243A (en) * | 2012-05-04 | 2012-09-12 | 宁夏大学 | Plant alkaloid compound microemulsion and preparation method of plant alkaloid compound microemulsion |
| CN106490025A (en) * | 2016-10-31 | 2017-03-15 | 郑州思辩科技有限公司 | A kind of booth vegetable insecticidal smoke and preparation method thereof |
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2018
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|---|---|---|---|---|
| US20080311221A1 (en) * | 2007-06-14 | 2008-12-18 | Pbi/Gordon Corporation | Lewis acid and oil-soluble hybrid pesticide concentrate that spontaneously forms a water-based microemulsion |
| CN102657243A (en) * | 2012-05-04 | 2012-09-12 | 宁夏大学 | Plant alkaloid compound microemulsion and preparation method of plant alkaloid compound microemulsion |
| CN106490025A (en) * | 2016-10-31 | 2017-03-15 | 郑州思辩科技有限公司 | A kind of booth vegetable insecticidal smoke and preparation method thereof |
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