CN110731352A - Jatropha curcas extract insecticidal sustained-release gel and preparation method thereof - Google Patents
Jatropha curcas extract insecticidal sustained-release gel and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/18—Euphorbiaceae [Spurge family], e.g. ricinus [castorbean]
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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
- A01N25/08—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 solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—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
- A01N43/04—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
- 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
- A01N43/16—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 with oxygen as the ring hetero atom
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- 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
- A01N45/00—Biocides, pest repellants or attractants, or plant growth regulators, containing compounds having three or more carbocyclic rings condensed among themselves, at least one ring not being a six-membered ring
- A01N45/02—Biocides, pest repellants or attractants, or plant growth regulators, containing compounds having three or more carbocyclic rings condensed among themselves, at least one ring not being a six-membered ring having three carbocyclic rings
Abstract
The invention provides jatropha curcas extract insecticidal slow-release gel, which belongs to the technical field of biotechnology and is prepared from the following raw materials, by weight, 15.6-34.2% of jatropha curcas leaf alkaloid extract, 20.5-30.2% of a bio-based macromolecular carrier, 30.5-52.2% of water, 1-5% of a cross-linking agent and 1-3% of an auxiliary dispersing agent.
Description
Technical Field
The invention belongs to the technical field of biotechnology, and particularly relates to jatropha curcas extract insecticidal sustained-release gels and a preparation method thereof.
Background
The plant secondary metabolites are natural products with the maximum content, such as high efficiency, low toxicity, no pollution, safety to human and livestock, unique action mode, high selectivity, no easy generation of drug resistance to natural enemies, beneficial biosafety pests and insects, and the like, and meet the requirements of people on ideal pesticides.
The barbadosnut leaves can be used as a medicine, are bitter in nature, slightly cold and toxic, and are mainly used for treating diseases such as traumatic injury, swelling and pain, fracture, skin itch, eczema, acute gastroenteritis and the like, Chinese and foreign students carry out a great deal of research on chemical components of the barbadosnut, and thus, various separation materials and separation technologies are adopted so far, reported bioactive components comprise terpenes, lignins, coumarins, flavonoids, alkaloids, proteins, lignans, phytosterols and the like, wherein alkaloids are with the largest content, and the natural alkaloids have the advantages of high efficiency, low toxicity, no pollution, safety to people and livestock, unique action mode, high selectivity, safety to natural enemies and beneficial organisms, difficulty in generation of pests and the like, meet the requirement of people on ideal pesticides, have various action modes on agricultural pests, such as poison, killing, repelling, growth inhibition and the like, and strong plant drug resistance extraction and strong bacteria resistance and bacteria extraction and purification effects, and biological purity improvement on the extraction and biological edible rate of alkaloids.
Compared with the traditional pesticide emulsion and aqueous solution, the novel pesticide preparation with slow release, low solvation, water-based and macromolecular hydrogel forms is gradually a new direction for researching pesticide formulations, aiming at the case that microcapsule suspension preparations, particle preparations, seed coating preparations, tablets, pill preparations, gel preparations, microcapsule preparations and the like are successfully applied, is widely applied to medicine to load effective components to prolong the release time so as to improve the pesticide effect, similarly, the current pesticide or insecticide is continuously developed towards the new formulation direction, aiming at the aspect of pesticide tablets, the development of hydrogel preparations such as water dispersion tablets, pesticide effervescent tablets and the like is provided, and the hydrogel preparations are often combined with sex attractants to replace cotton lure cores, so that the volatilization of active ingredients is effectively slowed down, the existing patents related to alkaloid extracts in jatropha leaf are not many, and the patents successfully taking a bio-based water-soluble macromolecule as an alkaloid carrier and further preparing slow release pesticide gels are not reported.
Disclosure of Invention
The invention aims to to provide insecticidal sustained-release gels taking jatropha curcas extract alkaloids as effective components, and another to provide a preparation method of insecticidal sustained-release gels taking jatropha curcas extract alkaloids.
In order to achieve the purpose, the invention adopts the following technical scheme:
Jatropha curcas extract insecticidal slow-release gel is prepared from 15.6-34.2 wt% of Jatropha curcas leaf alkaloid extract, 20.5-30.2 wt% of bio-based macromolecular carrier, 30.5-52.2 wt% of water, 1-5 wt% of cross-linking agent and 1-3 wt% of auxiliary dispersing agent.
, the alkaloid extract of Jatropha curcas leaf is or more of 3-methyloxazol-2-one, 6-hydroxypurine derivative, paromomycin, 6-diethylamine benzofuran-3-one or danazol.
, the bio-based macromolecular carrier is or more of chitosan, sodium alginate, chitin or nanocellulose.
, the cross-linking agent is one or more of genipin, glutaraldehyde, urea, and calcium chloride .
, the dispersion aid is or more of acetic acid, itaconic acid, phytic acid or taurine.
, the preparation method of the jatropha curcas leaf alkaloid extract comprises the following steps of drying and crushing the collected jatropha curcas leaves, sieving the crushed jatropha curcas leaves with a 15-25-mesh sieve to obtain a jatropha curcas leaf crushed matter, placing the jatropha curcas leaf crushed matter and water in an extraction container according to the mass ratio of 1: 1-1: 3, conducting ultrasonic stirring for 10-60 min, filtering, collecting filter residues, soaking the obtained filter residues in 2-10% acetic acid or 1-5% hydrochloric acid aqueous solution for 0.5-1.0 h, filtering, collecting filtrate, conducting extraction for 5-6 times by the same method, combining all filtrates, conducting extraction by a low-boiling-point water-insoluble organic solvent with the same volume as 1/3-1/2, wherein the solvent is dichloromethane, chloroform, ethyl acetate, n-hexane, ethyl ether or cyclohexane, combining all filtrates, conducting filtration again to remove impurities, and recovering the solvent under the temperature of 24-28 ℃ and the pressure of 0.15-0.98 Kpa to obtain the jatropha curc.
The invention also provides a preparation method of the insecticidal slow-release gel containing jatropha curcas extracts, which comprises the following steps:
(1) adding 20.5-30.2 wt% of bio-based macromolecular carrier and 1-33 wt% of dispersion aid agent into 30.5-52.2 wt% of water, ultrasonically stirring at 20-30 ℃, then placing in a refrigerator for periods of time, taking out and unfreezing, continuously freezing and unfreezing for 2-4 times by the same method, centrifuging for 30-60 min at 8000-10000 r/min to remove bubbles, and standing for 20-30 min to obtain a clarified solution;
(2) adding the jatropha curcas leaf alkaloid extract with the weight percentage of 15.6-34.2% into the clear solution at the temperature of 20-30 ℃, adding the cross-linking agent with the weight percentage of 1-5% while stirring, stirring for 3-5 minutes, and standing for 3-5 hours at the temperature of 20-30 ℃ to obtain the slow-release gel.
According to the improvement of the invention in step , in step (1), the ultrasonic stirring time is 1-3 h, and the ultrasonic power is 30-50W.
According to the improvement of the invention in step , in step (1), the mixture is put into a refrigerator at the temperature of-80 to-20 ℃ for freezing for 1 to 4 hours.
According to the improvement of the invention in step , in step (2), the stirring speed before adding the cross-linking agent is 7500-12000 r/min, the stirring time is 15-30 min, and the stirring speed after adding the cross-linking agent is 5000-7500 r/min.
Compared with the prior art, the invention has the beneficial effects that:
(1) the alkaloid extract with insecticidal activity provided by the invention is derived from plant bodies, namely jatropha curcas leaves, and has the advantages of high yield, low cost, simple extraction process, environmental protection and high efficiency, wherein the extraction rate is ten thousandths (1 per thousand), and the alkaloid extract has the potential of large-scale commercial application of due to low cost and high efficiency.
(2) The insecticidal slow-release gel containing the alkaloid extract provided by the invention adopts the bio-based macromolecules to load the alkaloid extract as the effective component, namely the alkaloid extract is wrapped in a macromolecular network to delay the release speed of the alkaloid extract and improve the service time, so that the problem that the traditional water-type or water-emulsion type pesticide is easily washed away by rainwater to cause premature failure or soil pollution is effectively solved, and the service life of the pesticide is prolonged.
(3) The bio-based macromolecule provided by the invention is derived from the nature, has complete biodegradability, can be completely degraded under the natural condition after the action is finished, has the characteristics of cleanness and recyclability, avoids the use of toxic and harmful organic solvents in the preparation process, and is completely green and environment-friendly.
(4) The preparation method effectively solves the problems of high toxicity, easy loss, quick failure and complex preparation of the traditional pesticide, widens the application range of the jatropha curcas alkaloid extract, and has broad industrial and market application prospects.
Drawings
FIG. 1 is a preparation process of a Jatropha curcas extract insecticidal sustained-release gel
FIG. 2 is a photograph showing the pesticidal sustained-release gel of Jatropha curcas extract
FIG. 3 shows the release rate of the effective components in the insecticidal sustained-release gel with time
FIG. 4 is a graph showing the effect of sodium alginate content in the gel on compressive strength
Detailed Description
The present invention is further described in conjunction with the following examples, which are only a few examples of and not all examples of the present invention.
Example 1
As shown in figure 1, (1) adding chitosan 20.5Kg and acetic acid 3Kg into water 30.5Kg, ultrasonic stirring vigorously at 25 deg.C for 1h with ultrasonic power of 50W, freezing in a refrigerator at-50 deg.C for 2h, thawing, freezing and thawing for 4 times, centrifuging at 8000r/min for 30min to remove bubbles, and standing for 20min to obtain clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 25 deg.C, eluting with mixed solvent of petroleum ether/ethyl acetate (volume ratio 3:1) in 400 mesh chromatographic silica gel column for 12h, and rotary evaporating the eluate to obtain 3-methyloxazol-2-one. Adding 25.4Kg of 3-methyloxazol-2-one into the clear solution, stirring at high speed of 12000r/min for 15min, simultaneously dropwise adding 5Kg of calcium chloride, stirring at 5000r/min for 5min, and standing at 25 ℃ for 5h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 250ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving red coccid collected in the field for 6 hours, adding the hungry red coccid collected in the conical bottle, adding the hungry red coccid into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the coccid after 24 hours and 48 hours, and calculating the death rate of the coccid by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel in the embodiment is directly sprayed for 24 hours, the mortality rate of the red coccid is 90.1%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 100%, and the plant growth is not influenced.
FIG. 2 is a photograph showing an insecticidal sustained-release gel of the Jatropha curcas extract, which is illustrated in FIG. 2 and shows that the sustained-release gel of the present example has a stable morphology and structure and can be processed into various shapes; FIG. 3 is the release rate of the effective components in the insecticidal slow release gel with time, and FIG. 3 illustrates that the slow release gel has better slow release property and long action time;
example 2
(1) Adding 30.2Kg of sodium alginate and 1Kg of itaconic acid into 52.2Kg of water, performing ultrasonic vigorous stirring for 3h at 20 ℃, performing ultrasonic power of 30W, freezing in a refrigerator at-20 ℃ for 4h, taking out, thawing, continuously freezing and thawing for 2 times in the same way, centrifuging at 10000r/min for 45min to remove bubbles, and standing for 30min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the jatropha curcas leaves in dichloromethane at 20 ℃, eluting the mixture in a 500-mesh chromatographic silica gel column by using a mixed solvent of n-hexane and acetone (the volume ratio is 2:1) for 24 hours, and then carrying out rotary evaporation on the eluate to obtain the 6-hydroxypurine derivative. Adding 15.6Kg of 6-hydroxypurine derivative into the clear solution, stirring at a high speed of 10000r/min for 30min, simultaneously dripping 1Kg of glutaraldehyde, stirring at 7500r/min for 3 min, and standing at 20 ℃ for 3h to obtain the sustained-release gel.
FIG. 4 shows the effect of sodium alginate content in the gel on the compression strength, and FIG. 4 shows that the sustained-release gel has better compressibility and is not easy to damage due to stress, the preparation method of the invention effectively solves the problems of large toxicity, easy loss, quick failure and complex preparation of the traditional pesticide, widens the application range of the jatropha curcas alkaloid extract, and has broad industrial and market application prospects.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 250ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, repeating each experiment for 4 times with 20 heads in each bottle, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, and calculating the death rate of the test insects by using the following formula5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel in the embodiment is directly sprayed for 24 hours, the mortality rate of the red coccid is 91.1%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 99.4%, and the plant growth is not influenced.
Example 3
(1) Adding 25.6Kg of chitin and 2Kg of phytic acid into 40.3Kg of water, performing ultrasonic vigorous stirring at 30 ℃ for 2h with ultrasonic power of 40W, freezing in a refrigerator at-80 ℃ for 1h, taking out, thawing, continuously freezing and thawing for 3 times in the same way, centrifuging at 9000r/min for 60min to remove bubbles, and standing for 25min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 30 deg.C, eluting with mixed solvent of acetone/ethanol (volume ratio 5:1) in 400 mesh chromatographic silica gel column for 40h, and rotary evaporating the eluate to obtain paromomycin. Adding 29.1Kg of paromomycin into the clear solution, stirring at a high speed of 7500r/min for 20min, simultaneously adding 3Kg of genipin, stirring at 6000r/min for 4 min, and standing at 30 ℃ for 4h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 250ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, adding 45 round red round scale insects into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, calculating the death rate of the test insects by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 92.1%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 98.9%, and the plant growth is not influenced.
The method for extracting the effective components of the alkaloid extract of the jatropha curcas leaves in the embodiments 1 to 3 is as follows:
drying and crushing the collected jatropha curcas leaves, and sieving the crushed jatropha curcas leaves by a 15-mesh sieve to obtain a crushed jatropha curcas leaf; placing the pulverized Jatropha curcas leaf and water in an extraction container according to the mass ratio of 1:1, ultrasonically stirring for 10min, filtering, and collecting the filter residue; soaking the residue in 5% hydrochloric acid water solution for 1.0 hr, filtering, collecting filtrate, and extracting by the same method for 6 times; all filtrates were combined and extracted with 1/3 equal volumes of dichloromethane; mixing all filtrates, filtering again to remove impurities, and recovering solvent under reduced pressure at 24 deg.C and 0.98kpa to obtain Jatropha curcas leaf alkaloid extract.
Example 4
(1) Adding 26.6Kg of nano-cellulose and 2.5K of taurine into 48.6Kg of water, carrying out ultrasonic vigorous stirring for 2.5h at 28 ℃, carrying out ultrasonic power of 45W, then putting the mixture into a refrigerator at-60 ℃ for freezing for 2.5h, taking out the mixture for thawing, continuing freezing and thawing for 4 times by the same method, centrifuging for 40min at 8500r/min to remove bubbles, and standing for 30min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 28 deg.C, eluting with mixed solvent of diethyl ether/cyclohexane (volume ratio of 2:1) in 300 mesh chromatographic silica gel column for 30h, and rotary evaporating the eluate to obtain 6-diethylamine benzofuran-3-one. Adding 18.8Kg of 6-diethylamine benzofuran-3-one into the above clarified solution, stirring at 9000r/min for 25min at high speed, simultaneously adding 3.5Kg of urea, stirring at 7000r/min for 5min, and standing at 28 deg.C for 4.5h to obtain sustained-release gel.
Taking a small amount of the sustained-release gel, diluting the gel with distilled water to obtain a liquid medicine with the concentration of 1.4mg/ml, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 250ml -mouth bottle, sealing the bottle with a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical flask, adding 45 red round scale insects into the conical flask, repeating each experiment for 4 times, taking clear water as a blank control, counting the death condition of the test insects after 24 hours and 48 hours, and counting the death condition of the test insects by using clearThe following formula calculates the mortality rate of the test insects. Simultaneously select 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 92.2%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 99.3%, and the plant growth is not influenced.
Example 5
(1) Adding 22.5Kg of chitosan and 3Kg of acetic acid into 37.8Kg of water, carrying out ultrasonic vigorous stirring for 3h at 24 ℃ with the ultrasonic power of 35W, then putting the mixture into a refrigerator at-30 ℃ for freezing for 3.5h, taking out the mixture for thawing, continuing freezing and thawing for 2 times in the same way, centrifuging at 9500r/min for 55min to remove bubbles, and standing for 25min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of the jatropha curcas in dichloromethane at 24 ℃, eluting the mixture in a 400-mesh chromatographic silica gel column by using a mixed solvent of petroleum ether/acetone (volume ratio of 4:1) for 24 hours, and then carrying out rotary evaporation on the eluate to obtain danazol. Adding 32.2Kg of danazol into the clear solution, stirring at 11000r/min for 25min at high speed, simultaneously adding 4.5Kg of genipin, stirring at 6800r/min for 3 min, and standing at 24 deg.C for 3.5h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 250ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, adding 45 round red round scale insects into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, calculating the death rate of the test insects by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 90.2%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 99.5%, and the plant growth is not influenced.
Example 6
(1) Adding 12.5Kg of nano-cellulose, 10Kg of chitosan, 1Kg of taurine and 1Kg of acetic acid into 45.8Kg of water, carrying out ultrasonic vigorous stirring for 3h at 24 ℃ and ultrasonic power of 35W, then putting the mixture into a refrigerator at-30 ℃ for freezing for 3.5h, taking out and unfreezing, continuing freezing and unfreezing for 2 times by the same method, centrifuging for 55min at 9500r/min to remove bubbles, and standing for 25min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of the jatropha curcas in dichloromethane at 24 ℃, eluting the mixture in a 400-mesh chromatographic silica gel column by using a mixed solvent of petroleum ether/acetone (volume ratio of 4:1) for 24 hours, and then carrying out rotary evaporation on the eluate to obtain danazol. Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 30 deg.C, eluting with mixed solvent of acetone/ethanol (volume ratio 5:1) in 400 mesh chromatographic silica gel column for 40h, and rotary evaporating the eluate to obtain paromomycin. Adding 14.7Kg of danazol and 10Kg of paromomycin into the clear solution, stirring at a high speed of 11000r/min for 25min, simultaneously adding 4.0Kg of glutaraldehyde and 1Kg of urea, stirring at 6800r/min for 3 min, and standing at 24 ℃ for 3.5h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 500ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, adding 45 round red round scale insects into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, calculating the death rate of the test insects by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 94.3%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 99.2%, and the plant growth is not influenced.
The method for extracting the effective components of the alkaloid extract of the jatropha curcas leaves in the embodiments 4 to 6 is as follows:
drying and crushing the collected jatropha curcas leaves, and sieving the crushed jatropha curcas leaves with a 25-mesh sieve to obtain a crushed jatropha curcas leaf; placing the pulverized Jatropha curcas leaf and water in an extraction container according to a mass ratio of 1:2, ultrasonically stirring for 60min, filtering, and collecting filter residue; soaking the residue in 2% acetic acid water solution for 0.5 hr, filtering, collecting filtrate, and extracting by the same method for 5 times; all filtrates were combined and extracted with 1/2 equal volumes of ethyl acetate; mixing all filtrates, filtering again to remove impurities, and recovering solvent at 28 deg.C under reduced pressure of 0.15kpa to obtain Jatropha curcas leaf alkaloid extract.
Example 7
(1) Adding 10.2Kg of sodium alginate, 10Kg of chitin, 10Kg of chitosan and 1Kg of itaconic acid into 52.2Kg of water, violently stirring by ultrasonic at 20 ℃ for 3h with the ultrasonic power of 30W, freezing in a refrigerator at-20 ℃ for 4h, taking out, thawing, continuing to freeze and thaw for 2 times by the same method, centrifuging at 10000r/min for 45min to remove bubbles, and standing for 30min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the jatropha curcas leaves in dichloromethane at 20 ℃, eluting the mixture in a 500-mesh chromatographic silica gel column by using a mixed solvent of n-hexane and acetone (the volume ratio is 2:1) for 24 hours, and then carrying out rotary evaporation on the eluate to obtain the 6-hydroxypurine derivative. Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 30 deg.C, eluting with mixed solvent of acetone/ethanol (volume ratio 5:1) in 400 mesh chromatographic silica gel column for 40h, and rotary evaporating the eluate to obtain paromomycin. Dissolving the alkaloid extract mixture extracted from the leaves of the jatropha curcas in dichloromethane at 24 ℃, eluting the mixture in a 400-mesh chromatographic silica gel column by using a mixed solvent of petroleum ether/acetone (volume ratio of 4:1) for 24 hours, and then performing rotary evaporation on the eluate to obtain danazol. Adding 5.6Kg of 6-hydroxypurine derivative, 5Kg of paromomycin and 5Kg of danazol into the clear solution, stirring at a high speed of 10000r/min for 30min, simultaneously dropwise adding 0.5Kg of glutaraldehyde and 0.5Kg of genipin, stirring at 7500r/min for 3 min, and standing at 20 ℃ for 3h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 500ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, adding 45 round red round scale insects into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, calculating the death rate of the test insects by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 90.5%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 98.7%, and the plant growth is not influenced.
Example 8
(1) Adding 25.6Kg of chitin, 1Kg of phytic acid and 1Kg of itaconic acid into 40.3Kg of water, carrying out ultrasonic vigorous stirring for 2h at 30 ℃ with ultrasonic power of 40W, then putting the mixture into a refrigerator at-80 ℃ for freezing for 1h, taking out and unfreezing, continuing freezing and unfreezing for 3 times by the same method, centrifuging at 9000r/min for 60min to remove bubbles, and standing for 25min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 30 deg.C, eluting with mixed solvent of acetone/ethanol (volume ratio 5:1) in 400 mesh chromatographic silica gel column for 40h, and rotary evaporating the eluate to obtain paromomycin. Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 28 deg.C, eluting with mixed solvent of diethyl ether/cyclohexane (volume ratio of 2:1) in 300 mesh chromatographic silica gel column for 30h, and rotary evaporating the eluate to obtain 6-diethylamine benzofuran-3-one. Adding 19.1Kg of paromomycin and 10Kg of 6-diethylamine benzofuran-3-one into the clear solution, stirring at 7500r/min at high speed for 20min, simultaneously adding 2Kg of genipin and 1Kg of calcium chloride, stirring at 6000r/min for 4 min, and standing at 30 ℃ for 4h to obtain the sustained-release gel.
Taking a small amount of the sustained-release gel, preparing a liquid medicine with the concentration of 1.4mg/ml by using distilled water, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 500ml -mouth bottle, sealing the bottle by using a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical bottle, adding 45 round red round scale insects into the conical bottle, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, calculating the death rate of the test insects by using the following formula, and simultaneously selecting 5m2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 91.5%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 99.0%, and the plant growth is not influenced.
Example 9
(1) Adding 14.5Kg of chitosan, 6Kg of sodium alginate, 1Kg of acetic acid, 1Kg of taurine and 1Kg of phytic acid into 30.5Kg of water, carrying out ultrasonic vigorous stirring for 1h at 25 ℃, carrying out ultrasonic power of 50W, then putting the mixture into a refrigerator at-50 ℃ for freezing for 2h, taking out and unfreezing, continuously freezing and unfreezing for 4 times by the same method, centrifuging for 30min at 8000r/min to remove bubbles, and standing for 20min to obtain a clear solution.
(2) Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 25 deg.C, eluting with mixed solvent of petroleum ether/ethyl acetate (volume ratio 3:1) in 400 mesh chromatographic silica gel column for 12h, and rotary evaporating the eluate to obtain 3-methyloxazol-2-one. Dissolving the alkaloid extract mixture extracted from the jatropha curcas leaves in dichloromethane at 20 ℃, eluting the mixture in a 500-mesh chromatographic silica gel column by using a mixed solvent of n-hexane and acetone (the volume ratio is 2:1) for 24 hours, and then carrying out rotary evaporation on the eluate to obtain the 6-hydroxypurine derivative. Dissolving the alkaloid extract mixture extracted from the leaves of Jatropha curcas in dichloromethane at 28 deg.C, eluting with mixed solvent of diethyl ether/cyclohexane (volume ratio of 2:1) in 300 mesh chromatographic silica gel column for 30h, and rotary evaporating the eluate to obtain 6-diethylamine benzofuran-3-one. 5.4Kg of 3-methyloxazole-2-one, 10Kg of 6-hydroxypurine derivative and 10Kg of 6-diethylamine benzofuran-3-one are added into the clear solution, stirred at high speed of 12000r/min for 15min, simultaneously dropwise added with 2Kg of calcium chloride, 1Kg of urea and 1Kg of genipin, stirred at 5000r/min for 5min and kept stand at 25 ℃ for 5h to obtain the slow-release gel.
Taking a small amount of the slow-release gel, diluting the gel with distilled water to prepare a liquid medicine with the concentration of 1.4mg/ml, uniformly coating the prepared liquid medicine on flat round absorbent cotton (2 +/-0.1 g), flatly paving the liquid medicine at the bottom of a 500ml -mouth bottle, sealing the bottle with a single-layer white gauze, starving the red round scale insects collected in the field for 6 hours, adding the hungry red round scale insects into the conical flask, adding 45 round red round scale insects into the conical flask, repeating each experiment for 4 times, taking clear water as a blank control, counting the death conditions of the test insects after 24 hours and 48 hours, and calculating the death rate of the test insects by using the following formula2Cabbage experimental field, according to 750kg/hm2The spraying amount of the liquid medicine is uniformly sprayed on the front and back sides of the cabbage leaves, and the growth condition of the plants is inspected after 96 hours.
The death rate is 100 percent per total number of the test insects
Through detection, after the insecticidal slow-release gel is directly sprayed for 24 hours, the mortality rate of the red coccid is 91.8%, and after the insecticidal slow-release gel is applied for 48 hours, the mortality rate of the red coccid is 98.8%, and the plant growth is not influenced.
The method for extracting the effective components of the alkaloid extract of the jatropha curcas leaves in the embodiments 7 to 9 is as follows:
drying and crushing the collected jatropha curcas leaves, and sieving the crushed jatropha curcas leaves by a 20-mesh sieve to obtain a crushed jatropha curcas leaf; placing the pulverized Jatropha curcas leaf and water in an extraction container according to a mass ratio of 1:3, ultrasonically stirring for 50min, filtering, and collecting filter residue; soaking the residue in 5% acetic acid water solution for 0.5 hr, filtering, collecting filtrate, and extracting by the same method for 5 times; all filtrates were combined and extracted with 1/2 equal volumes of chloroform; mixing all filtrates, filtering again to remove impurities, and recovering solvent at 28 deg.C under reduced pressure of 0.75kpa to obtain Jatropha curcas leaf alkaloid extract.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
- The insecticidal slow-release gel of the Jatropha curcas extract is characterized by being prepared from the following raw materials, by weight, 15.6-34.2% of the Jatropha curcas leaf alkaloid extract, 20.5-30.2% of a bio-based macromolecular carrier, 30.5-52.2% of water, 1-5% of a cross-linking agent and 1-3% of a dispersion aid.
- 2. The Jatropha curcas extract insecticidal sustained release gel as claimed in claim 1, wherein the Jatropha curcas leaf alkaloid extract is or more of 3-methyloxazol-2-one, 6-hydroxypurine derivative, paromomycin, 6-diethylamine benzofuran-3-one or danazol.
- 3. The jatropha curcas extract insecticidal sustained release gels of claim 1, wherein the bio-based macromolecular carrier is or more of chitosan, sodium alginate, chitin or nanocellulose.
- 4. The jatropha curcas extract insecticidal sustained release gel as claimed in claim 1, wherein the cross-linking agent is or more of genipin, glutaraldehyde, urea or calcium chloride.
- 5. The jatropha curcas extract insecticidal sustained release gel as claimed in claim 1, wherein the dispersion aid is or more of acetic acid, itaconic acid, phytic acid or taurine.
- 6. The jatropha curcas extract insecticidal sustained-release gel of any one of claims 1-5 to , wherein the preparation method of the jatropha curcas leaf alkaloid extract comprises the steps of drying and crushing the collected jatropha curcas leaves, sieving the crushed material with a 15-25-mesh sieve to obtain a jatropha curcas leaf crushed material, placing the crushed material and water in an extraction container according to the mass ratio of 1: 1-1: 3, carrying out ultrasonic stirring for 10-60 min, filtering, collecting filter residues, soaking the obtained filter residues in 2-10% acetic acid or 1-5% hydrochloric acid aqueous solution for 0.5-1.0 h, filtering, collecting the filtrate, extracting for 5-6 times by the same method, combining all the filtrates, extracting with 1/3-1/2 isometric low-boiling-point water-insoluble organic solvents, namely dichloromethane, chloroform, ethyl acetate, n-hexane, diethyl ether or cyclohexane, combining all the filtrates, filtering again to remove impurities, and recovering the solvents under the temperature of 24-28 ℃ and the pressure of 0.15-0.98 Kpa to obtain the jatropha alkaloid extract.
- The preparation method of Jatropha curcas extract insecticidal sustained-release gel, which comprises the Jatropha curcas extract insecticidal sustained-release gel of any claim 1-6 or , and is characterized by comprising the following steps:(1) adding 20.5-30.2 wt% of bio-based macromolecular carrier and 1-33 wt% of dispersion aid agent into 30.5-52.2 wt% of water, ultrasonically stirring at 20-30 ℃, then placing in a refrigerator for periods of time, taking out and unfreezing, continuously freezing and unfreezing for 2-4 times by the same method, centrifuging for 30-60 min at 8000-10000 r/min to remove bubbles, and standing for 20-30 min to obtain a clarified solution;(2) adding the jatropha curcas leaf alkaloid extract with the weight percentage of 15.6-34.2% into the clear solution at the temperature of 20-30 ℃, adding the cross-linking agent with the weight percentage of 1-5% while stirring, stirring for 3-5 minutes, and standing for 3-5 hours at the temperature of 20-30 ℃ to obtain the slow-release gel.
- 8. The preparation method of jatropha curcas extract insecticidal sustained-release gels, according to claim 7, characterized in that in step (1), the ultrasonic stirring time is 1-3 h, and the ultrasonic power is 30-50W.
- 9. The preparation method of Jatropha curcas L.extracts insecticidal sustained-release gel according to claim 7, wherein in step (1), the gel is frozen in a refrigerator at-80 to-20 ℃ for 1-4 h.
- 10. The preparation method of jatropha curcas extract insecticidal sustained-release gels, according to claim 7, characterized in that in step (2), the stirring speed before adding the cross-linking agent is 7500-12000 r/min, the stirring time is 15-30 min, and the stirring speed after adding the cross-linking agent is 5000-7500 r/min.
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