CN112940068A - Low-temperature extraction and purification process of botanical pesticide toosendanin - Google Patents
Low-temperature extraction and purification process of botanical pesticide toosendanin Download PDFInfo
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a low-temperature extraction and purification process of botanical pesticide toosendanin, belonging to the technical field of biology. The invention adopts low-temperature purification and purification of toosendanin, realizes the rapid layering of toosendanin ethanol extract through vacuum concentration to standard density, and realizes the high-efficiency extraction of toosendanin by extracting the upper layer of extract with ethanol again, and the concentration of the obtained toosendanin mother liquor is more than or equal to 1%. The whole process does not use petroleum ether, chitosan and other components, greatly reduces the pollution and insecurity caused by the use of organic solvents, simplifies the process flow, reduces the loss of toosendanin, greatly reduces the production cost of botanical pesticides, promotes the marketization application of the botanical pesticides, and has wide economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of biology, and particularly relates to a low-temperature extraction and purification process of toosendanin.
Background
Pesticides can be classified into biological sources, mineral sources and chemical synthesis according to their sources. The mineral source pesticide has few varieties and has little development prospect. The chemical pesticide has high efficiency and can play a role when a large number of plant diseases and insect pests occur, but the problems of 'three R' generated in the using process of the chemical pesticide, namely Residue (Residue), Resistance (Resistance) and pest rampant (Resurgence) are getting worse and worse. The production and use of chemical pesticides are gradually restricted in countries around the world, and the difficulty of developing new chemical pesticide varieties and commercializing the new chemical pesticide varieties is higher and higher, and the generation of pest resistance shortens the service life of the chemical pesticides, so that the development of the chemical pesticides is more and more difficult. In China, the production of hexachloro cyclohexane, DDT and other organochlorine pesticide varieties is stopped, and then the production of dibromochloropropane, fluoroacetamide, toxigenin, chlordimeform, aclonifen and the like is prohibited in sequence. The biological source pesticide comprises plant source pesticide and animal source pesticide, and mainly comprises plant source pesticide. The plant pesticide has the advantages that the selective toxicity of the plant pesticide to mammals meets the safety standard, the plant pesticide has no lasting residue in the environment, the action mode of preventing and treating objects belongs to stomach toxicity, the plant pesticide has no contact toxicity, non-edible beneficial insects are prevented from being damaged, the plant diseases and insect pests are not easy to generate resistance, the development and production cost is relatively low, and the like, and the interest of various countries in the world in research and development of the plant pesticide is aroused. Therefore, research and development of plant pesticides are not only needed for environmental protection and ecological protection, but also a direction for the development of pesticide industry.
Toosendanin (tosendanin) is a tetracyclic triterpene compound found in Melia plants, has various biological activities of expelling parasites, resisting cancers, resisting toxins, resisting bacteria, blocking neuromuscular junctions, inhibiting respiratory centers, diminishing inflammation and the like, and is a safe and pollution-free botanical pesticide product. The existing extraction and purification process of toosendanin is characterized in that after toosendanin is extracted, petroleum ether or chitosan is used for further purification, and the petroleum ether belongs to a flash point flammable liquid, has accumulation in a human body and is a nerve poison. The vapor or mist is irritating to eyes, mucous membrane and respiratory tract, and can cause peripheral neuritis and strong irritation to skin. And secondly, the fertilizer is harmful to the environment and can cause pollution to water, soil and atmosphere. And the petroleum ether can burn the active ingredients required by production, and the loss rate of the active ingredients is more than 30%. Flocs generated by flocculation with chitosan are not easy to filter, so that a large amount of effective components are lost. The raw material loss caused by the purification of petroleum ether and chitosan is that in the existing process, the concentration of the final product is below 0.5%, and the large amount of repeated purification can cause the production cost to rise greatly, thus being difficult to meet the actual market demand, which is also the key point for causing the difficulty in realizing the large-scale application of the botanical pesticide toosendanin.
Disclosure of Invention
The invention provides a low-temperature extraction and purification process of toosendanin, aiming at overcoming the defects in the prior art, and the process does not use any organic solvent such as petroleum ether chitosan and the like in the purification step, realizes the high-efficiency extraction and purification of the toosendanin, and has no pollution and no public nuisance. In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a low-temperature extraction and purification process of botanical pesticide toosendanin comprises the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of not higher than 40 ℃ to obtain a crude ethanol extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 1.2 to obtain fructus Toosendan concentrated solution;
(4) placing the szechwan chinaberry fruit concentrated solution in a condensing tank, standing at low temperature for layering, wherein the standing time is not less than 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the liquid and the recovered ethanol clear liquid at a temperature not higher than 32 deg.C, concentrating to obtain high-concentration toosendanin solution with relative density of 1, and sealing for storage.
Preferably, step (1) is a 40 mesh sieve.
Preferably, the concentration of the ethanol solution in the step (1) is 75%, and the solid-to-liquid ratio is 1: 10.
Preferably, the extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
Preferably, the temperature of the condensed water is reduced in the step (3), and the temperature of the condensed water is not higher than-3 ℃.
Antifreeze such as glycol can be added into the condensed water to prevent the condensed water from freezing.
Preferably, the use method of the toosendanin solution is to add necessary auxiliary materials such as an emulsifier and the like into the toosendanin to prepare 0.5% aqueous emulsion for use. The adjuvants may include emulsifier, surfactant, etc.
The specific preparation method is as follows:
adding appropriate amount of H77 surfactant, penetrant, and limonene into the toosendanin solution, and emulsifying at 30 deg.C with 7000-.
The filtration in the step (2) adopts a two-step filtration mode, firstly adopts a 600-mesh stainless steel filter screen for filtration, and then adopts a precision filter for secondary filtration.
The concentration of the finished product toosendanin solution obtained in the step (6) of the invention is more than or equal to 1 percent.
At present, in the prior art, the purification process of toosendanin adopts a petroleum ether or chitosan purification mode, toosendan fruits with the same quality are purified by adopting the prior art, a large amount of components are lost in the purification process, the final concentration of the obtained mother liquor product is far less than 0.5%, the toosendanin can be used only in the form of 0.5% of emulsion in water and the like in order to improve the concentration of the mother liquor, the use amount of the toosendan fruits is inevitably increased, the selling price of the botanical pesticide is higher than that of the common mineral source or the chemically synthesized pesticide, the use amount of the raw materials is greatly increased, and finally, the safe and pollution-free botanical pesticide is difficult to popularize in practical application and stays in a laboratory research stage for a long time, so that the due economic value and social benefit of the botanical pesticide are not realized.
Advantageous effects
The invention adopts low-temperature purification and purification of toosendanin, realizes the rapid layering of toosendanin ethanol extract through vacuum concentration to standard density, and realizes the high-efficiency extraction of toosendanin by extracting the upper layer of extract with ethanol again, and the concentration of the obtained toosendanin mother liquor is more than or equal to 1%. The whole process does not use petroleum ether, chitosan and other components, greatly reduces the pollution and insecurity caused by the use of organic solvents, simplifies the process flow, reduces the loss of toosendanin, greatly reduces the production cost of botanical pesticides, promotes the marketization application of the botanical pesticides, and has wide economic and social benefits.
Drawings
FIG. 1 is a schematic view of a condenser used in the low temperature vacuum concentration of the present invention;
FIG. 2 is a flow chart of the low-temperature extraction and purification process of the botanical pesticide toosendanin.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
A low-temperature extraction and purification process of botanical pesticide toosendanin comprises the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of 25 ℃ to obtain an ethanol crude extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 1.2 to obtain fructus Toosendan concentrated solution;
(4) placing the concentrated liquid of fructus Toosendan in a condensing tank, standing at low temperature for layering, and standing for 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the lower layer liquid and the recovered ethanol clear liquid at 30-32 deg.C, concentrating to obtain high concentration toosendanin solution with relative density of 1, and sealing for storage.
The step (1) is to pass through a 40-mesh sieve.
In the step (1), the concentration of the ethanol solution is 75%, and the solid-to-liquid ratio is 1: 10.
The extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
And (3) cooling by adopting condensed water, wherein the temperature of the condensed water is not higher than-3 ℃.
The use method of the toosendanin solution is to add necessary auxiliary materials such as an emulsifier and the like into the toosendanin to prepare 0.5 percent of aqueous emulsion for use.
The filtration in the step (2) adopts a two-step filtration mode, firstly adopts a 600-mesh stainless steel filter screen for filtration, and then adopts a precision filter for secondary filtration.
Example 2
A low-temperature extraction and purification process of botanical pesticide toosendanin comprises the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of 30 ℃ to obtain a crude ethanol extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 1.2 to obtain fructus Toosendan concentrated solution;
(4) placing the concentrated liquid of fructus Toosendan in a condensing tank, standing at low temperature for layering, and standing for 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the lower layer liquid and the recovered ethanol clear liquid at 30-32 deg.C, concentrating to obtain high concentration toosendanin solution with relative density of 1, and sealing for storage.
The step (1) is to pass through a 40-mesh sieve.
In the step (1), the concentration of the ethanol solution is 75%, and the solid-to-liquid ratio is 1: 10.
The extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
And (3) cooling by adopting condensed water, wherein the temperature of the condensed water is not higher than-3 ℃.
The use method of the toosendanin solution is to add necessary auxiliary materials such as an emulsifier and the like into the toosendanin to prepare 0.5 percent of aqueous emulsion for use.
The filtration in the step (2) adopts a two-step filtration mode, firstly adopts a 600-mesh stainless steel filter screen for filtration, and then adopts a precision filter for secondary filtration.
Example 3
A low-temperature extraction and purification process of botanical pesticide toosendanin comprises the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of 40 ℃ to obtain an ethanol crude extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 1.2 to obtain fructus Toosendan concentrated solution;
(4) placing the concentrated liquid of fructus Toosendan in a condensing tank, standing at low temperature for layering, and standing for 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the lower layer liquid and the recovered ethanol clear liquid at 30-32 deg.C, concentrating to obtain high concentration toosendanin solution with relative density of 1, and sealing for storage.
The step (1) is to pass through a 40-mesh sieve.
In the step (1), the concentration of the ethanol solution is 75%, and the solid-to-liquid ratio is 1: 10.
The extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
And (3) cooling by adopting condensed water, wherein the temperature of the condensed water is not higher than-3 ℃.
The use method of the toosendanin solution is to add necessary auxiliary materials such as an emulsifier and the like into the toosendanin to prepare 0.5 percent of aqueous emulsion for use.
The filtration in the step (2) adopts a two-step filtration mode, firstly adopts a 600-mesh stainless steel filter screen for filtration, and then adopts a precision filter for secondary filtration.
In the process steps of the invention, the low-temperature vacuum concentration adopts a conventional condenser, which is a universal device and has a schematic structural diagram as shown in figure 1; the tank body is provided with a water inlet and a water outlet, so that the condensed water cooling of the shell is realized. The lower part of the tank body is provided with a discharge hole which is directly communicated with the inside of the tank body and used for discharging the lower-layer feed liquid.
Comparative example 1
A low-temperature extraction and purification process of botanical pesticide toosendanin comprises the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of 40 ℃ to obtain an ethanol crude extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 0.8 to obtain fructus Toosendan concentrated solution;
(4) placing the concentrated liquid of fructus Toosendan in a condensing tank, standing at low temperature for layering, and standing for 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the lower layer liquid and the recovered ethanol clear liquid at a temperature not higher than 32 deg.C, concentrating to obtain high-concentration toosendanin solution with relative density of 1, and sealing for storage.
The step (1) is to pass through a 40-mesh sieve.
In the step (1), the concentration of the ethanol solution is 75%, and the solid-to-liquid ratio is 1: 10.
The extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
And (3) cooling by adopting condensed water, wherein the temperature of the condensed water is not higher than-3 ℃.
The use method of the toosendanin solution is to add necessary auxiliary materials such as an emulsifier and the like into the toosendanin to prepare 0.5 percent of aqueous emulsion for use.
The filtration in the step (2) adopts a two-step filtration mode, firstly adopts a 600-mesh stainless steel filter screen for filtration, and then adopts a precision filter for secondary filtration.
This comparative example is essentially the same process as example 3, except that step (3) is concentrated in vacuo to a relative density of 1.
Comparative example 2
This comparative example is essentially the same process as example 3, except that step (3) is concentrated in vacuo to a relative density of 1.5.
Comparative example 3
This comparative example is essentially the same process as example 3, except that step (3) is concentrated in vacuo to a relative density of 1.8.
Comparative example 4
The comparative example selects the toosendan fruit with the same quality as the examples and comparative examples of the invention, but adopts the prior petroleum ether extraction and purification. Reference may be made to the method described in CN 201710888534.6.
First, performance test
The mother liquid of toosendanin obtained in examples 1-3 and comparative examples 1-4 of the invention is subjected to performance test, and the test method refers to the enterprise standard Q/LYKN 001-containing 2019 of 1% toosendanin mother drug and Q/LYKN 002-containing 2019 of 0.5% toosendanin water emulsion.
Liquid chromatography
Summary of the process
The sample was dissolved in methanol, and the azadirachtin in the sample was separated and measured by high performance liquid chromatography using acetonitrile + water (30 + 70V/V) as a mobile phase and a stainless steel column using C18 as a packing and a variable wavelength ultraviolet detector, and quantified by an external standard method.
Reagent
Methanol: carrying out chromatographic purification;
acetonitrile: carrying out chromatographic purification;
water: newly distilling the secondary distilled water;
toosendanin standard sample: the accurate mass fraction is known, omega is more than or equal to 99.9 percent.
Instrument for measuring the position of a moving object
High performance liquid chromatograph: a variable wavelength ultraviolet detector;
a chromatography workstation;
a chromatographic column: a 250mm × 4.6mm (i.d.) stainless steel column filled with C18 filler and having a particle size of 5 μm;
microsyringe: 20 mu L of the solution;
quantitative sampling tube: 10 mu L of the solution;
a filter: the aperture of the filter membrane is about 0.45 mu m;
an ultrasonic cleaner.
Operating conditions of liquid chromatography
Mobile phase: acetonitrile + water of 30+70(V/V), filtered through a filter membrane, and degassed;
flow rate: 1.0 mL/min;
column temperature: 35 ℃;
detection wavelength: 210 nm;
sample introduction volume: 10 mu L of the solution;
retention time: toosendanin is about 22.6min, and toosendanin isomer is 28.7 min.
Standard curve
Preparation of Standard solutions
Weighing 0.01g of toosendanin standard sample (accurate to 0.00001), placing in a 20mL volumetric flask, dissolving with methanol and fixing volume, and shaking up for later use.
Preparation of sample solution
Weighing a sample containing 0.01g (accurate to 0.0001g) of toosendanin, placing the sample in a 20mL volumetric flask, dissolving the sample with methanol, fixing the volume, shaking up, filtering, and reserving the filtrate for later use.
Measurement of
Under the operating conditions, after the baseline of the instrument is stable, a plurality of needles of standard sample solution are continuously injected until the relative response value of the peak areas of the toosendanin of two adjacent needles changes by less than 1.5 percent, and the measurement is carried out according to the sequence of the standard sample solution, the sample solution and the standard sample solution.
Computing
And respectively averaging the areas of the toosendanin peaks in the two measured sample solutions and the two measured standard sample solutions of the front and the back of the sample. The mass fraction of toosendanin in the sample is calculated according to formula (1):
in the formula:
ω1-mass fraction of toosendanin in the sample, expressed in%;
A2-average value of toosendanin peak area (toosendanin + toosendanin isomers) in the sample solution;
m1the mass of the toosendanin standard sample is gram (g);
omega is the mass fraction of toosendanin in the standard sample, and is expressed by percent;
A1-the average value of the toosendanin peak areas (toosendanin + toosendanin isomers) in the sample solution;
m2the mass of the sample in grams (g).
Determination of the pH value
The procedure was as described in GB/T1601 + 1993.
Determination of the mass fraction of acetone-insoluble substances
According to GB/T19138-2003.
The performance test results are shown in table 1:
TABLE 1 mother liquor Performance test
Second, field application test
The 0.5% aqueous emulsion prepared in the embodiment 3 of the invention is verified to have the drug effect of preventing and controlling vegetable bemisia tabaci and phyllotreta striolata.
1 conditions of the test
1.1 test subjects and crops: bemisia tabaci (cucumber), and Phyllotreta striolata (green vegetable).
1.2 environmental or facility cultivation conditions are tested in a greenhouse of a certain vegetable field in Shandong Shouguang City, the greenhouse is cultivated, the cucumber is in fruiting period, and the green vegetable is in leaf 6-7 period.
2 test design and arrangement
2.1.1 test agents: 0.5% toosendanin aqueous emulsion (AS), a product of Linyikang biological science and technology, Inc.
2.1.2 control agents:
1.8 percent of abamectin missible oil (EC) which is a product of Shanghai Yue chemical company Limited;
phyllotreta striolata: 25 g/l bifenthrin Emulsifiable Concentrate (EC), a product of Dayao Yazhou green Dayao GmbH (China );
40% acetamiprid water dispersible granule (WG), product of Qingdaosheng Biotechnology Limited.
A blank control was also set.
TABLE 2 Experimental design of the test agents (Bemisia tabaci)
TABLE 3 Experimental design of test agents (striped flea beetle)
3.2 cell arrangement
3.2.1 cell arrangement-this test is a trend test, no repetition is set, bemisia tabaci is tested on cucumber by visual inspection; phyllotreta striolata was tested twice on green vegetables, with bifenthrin as a control for one time and acetamiprid as a control for the other time.
3.3 methods of application
3.3.1 methods of use, spraying.
3.3.2 applicator, Wake soil brand WS-16 model knapsack action manual sprayer manufactured by Shandong guard plant protection machinery Limited, with spray hole diameter of 0.7 mm.
3.3.3 the application time and times are that the bemisia tabaci and phyllotreta striolata are in the adult stage, the cucumber is in the fruiting stage and the green vegetable is in the 6-7 leaf stage during application.
The application times are that the bemisia tabaci is applied only once, and the phyllotreta striolata is applied once by using bifenthrin as a control; the acetamiprid-based control was applied twice with 6 days between applications.
3.3.4 application volume, the dosage according to the test regulation is sprayed to the leaf surface for micro-dripping.
3.3.5 the information of the pesticide for preventing and treating other diseases and insect pests, wherein other pesticides are not used for preventing and treating other diseases and insect pests 10 days before and during the test.
4 investigation method, time and times
4.1 investigation of time and frequency, the population base of the insects in the pre-medication investigation, and the quantity of the insects in the residual insects in 1, 3 and 3 days after the medication.
4.2 investigation method, 2 plants per treatment of five-point sampling method, 10 plants per plot are investigated in total, 3 leaves are investigated per bemisia tabaci, and adult quantities on the whole green vegetable are investigated by phyllotreta striolata. The base number is checked before the medicine is taken, the number of the residual live insects is checked after the medicine is taken, and the control effect is calculated by comparing with the blank area.
4.2.3 method for calculating drug effect
Percent reduction rate (%) is (number of insects before application-number of insects after application)/number of insects before application X100%
Correction control (%) (reduction rate of population insect in application region-reduction rate of population insect in blank control region)/(reduction rate of population insect in 100-blank control region) × 100%
TABLE 4 tendency test results for controlling cucumber Bemisia tabaci
TABLE 5 tendency test results for prevention and treatment of vegetable yellow flea beetle (application 1 time)
TABLE 5 tendency test results (2 applications) for controlling yellow flea beetle of green vegetables
Results and evaluation
Cucumber Bemisia tabaci: the 0.5% toosendanin AS is used for preventing and treating cucumber bemisia tabaci with two dosages of 2000 times liquid and 1000 times liquid, the prevention effect is improved along with the increase of the dosage, the quick action is good, the lasting period is long, and the control effect is 80.59% and 86.50% respectively 1 day after the first application; 79.07 percent and 83.57 percent respectively after 3 days; the control effect is 72.40 percent and 79.26 percent respectively after the drug is applied for 7 days; the control medicament 1.8% abamectin EC is used 800 times, and the correction control effect 1, 3 and 7 days after the first medicament is respectively 79.77%, 73.53% and 66.04%.
The control effect of the green vegetable phyllotreta striolata control by using the two dosages of 2000 times of liquid and 1000 times of liquid for the green vegetable phyllotreta striolata control by 0.5 percent toosendanin AS is improved along with the increase of the dosage, and the green vegetable phyllotreta striolata control has better quick action and longer lasting period.
The correction and control effects of 1 time of drug application are 80.87 percent and 83.20 percent respectively 1 day after the drug application; 75.90 percent and 78.96 percent respectively 3 days after the medicine is taken, and 68.06 percent and 71.47 percent respectively 7 days after the medicine is taken; the control agent of 25 g/L bifenthrin EC is used 1667 times, and the corrected control effect 1, 3 and 7 days after the control agent is 77.68%, 68.59% and 60.70% respectively. The control effect 5 days after the 2-time administration is 80.67% and 84.42%, the control agent 40% flonica WG is used for 2 times, and the control effect 5 days after the 2-time administration is 76.96%.
Safety: the test agent is safe to three crops in the test dosage range and has no phytotoxicity symptom.
And (4) conclusion: the bemisia tabaci and flea beetles are rampant pests harmful to vegetables, occur in local areas all year round, and are applied for 1 time every 5 to 7 days in a recurrent season, and the control effect of the conventional medicament in the prior production is about 70 percent. The 0.5% toosendanin AS used by the test has the control effect of about 80% which is 1000-fold and 2000-fold, is equivalent to the control effect of a local conventional medicament, has better quick-acting performance and longer lasting period, and is safe to crops.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (6)
1. A low-temperature extraction and purification process of botanical pesticide toosendanin is characterized by comprising the following steps:
(1) drying and crushing the fruits of the szechwan chinaberry fruits, sieving, adding an ethanol solution for full soaking, and then performing countercurrent ultrasonic extraction at the extraction temperature of not higher than 40 ℃ to obtain a crude ethanol extract of the szechwan chinaberry fruits;
(2) filtering the crude ethanol extract to obtain fructus Toosendan ethanol refined extract, and storing in a storage tank;
(3) vacuum concentrating the fructus Toosendan ethanol extractive solution at low temperature under vacuum degree of-0.1 MPa to relative density of 1.2 to obtain fructus Toosendan concentrated solution;
(4) placing the szechwan chinaberry fruit concentrated solution in a condensing tank, standing at low temperature for layering, wherein the standing time is not less than 24 h;
(5) standing for layering, discharging the lower layer liquid, and storing for later use; adding 95% ethanol into the upper layer paste according to the solid-liquid ratio of 1:10 for alcoholization for 20 minutes; transferring the alcoholized liquid to an alcohol precipitation tank, standing for layering again, discharging flocculate at the lower layer after 24 hours, and recovering ethanol clear liquid at the upper layer;
(6) heating and concentrating the lower layer liquid and the recovered ethanol clear liquid at a temperature not higher than 32 deg.C, concentrating to obtain high-concentration toosendanin solution with relative density of 1, and sealing for storage.
2. The low-temperature extraction and purification process of the botanical pesticide toosendanin as claimed in claim 1, wherein the step (1) is 40 mesh sieving.
3. The process for extracting and purifying the botanical pesticide toosendanin as claimed in claim 1, wherein the concentration of the ethanol solution in the step (1) is 75% and the solid-to-liquid ratio is 1: 10.
4. The low-temperature extraction and purification process of the botanical pesticide toosendanin as claimed in claim 1, wherein the extraction time of the countercurrent ultrasonic extraction in the step (1) is not less than 90 min.
5. The process for extracting and purifying the botanical pesticide toosendanin as claimed in claim 1, wherein the temperature of the condensed water in step (3) is reduced, and the temperature of the condensed water is not higher than-3 ℃.
6. The process for extracting and purifying the botanical pesticide toosendanin as claimed in claim 1, wherein the toosendanin solution is prepared by preparing toosendanin into 0.5% aqueous emulsion.
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| CN114057826B (en) * | 2021-12-22 | 2023-10-17 | 上海诗丹德标准技术服务有限公司 | Preparation method of reference substance of toosendanin |
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