CN112457126A - Cortex meliae extract microcapsule, preparation method and application in soil improvement fertilizer - Google Patents
Cortex meliae extract microcapsule, preparation method and application in soil improvement fertilizer Download PDFInfo
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- CN112457126A CN112457126A CN202110132689.3A CN202110132689A CN112457126A CN 112457126 A CN112457126 A CN 112457126A CN 202110132689 A CN202110132689 A CN 202110132689A CN 112457126 A CN112457126 A CN 112457126A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
Abstract
The invention provides a cortex meliae extract microcapsule, a preparation method and application in soil improvement fertilizer, belonging to the technical field of Chinese herbal medicine microcapsule. The obtained cortex Meliae extract microcapsule is solid in normal state, and is convenient for storage and use. The cortex meliae extract microcapsule obtained by the invention can be well compounded with a soil improvement fertilizer, and the cortex meliae extract microcapsule and the soil improvement fertilizer are directly compounded and applied into soil when in use, can directly reach the deep part of the soil, and has good prevention and control effects on soil pests.
Description
Technical Field
The invention belongs to the technical field of microcapsules, and particularly relates to a cortex meliae extract microcapsule, a preparation method and application in a soil improvement fertilizer.
Background
The cortex Meliae is dried bark and root bark of Melia toosendan Sieb. et Zucc. or Melia azedarach L. belonging to Meliaceae. The melia azedarach mainly contains toosendanin, toosendanin terpene ketone lactone, toosendanin terpene alcohol lactone, methyl toosendanin acid, melitensinamide and the like, can be used for treating intractable damp moss, decayed teeth, ascaris, pinworm, fistulous sore and the like, and the toosendanin is a botanical pesticide which is researched and developed earlier in China and particularly has higher biological activity on various agricultural pests. CN106665610B discloses an application of toosendanin in preparation of acanthopodium insecticide, wherein the toosendanin extract obtained from Melia azedarach or Melia azedarach of Meliaceae is dissolved in ethanol and then completely dissolved in distilled water to prepare mother liquor for killing acanthopodium, the mother liquor is placed in a low-temperature environment at 4 ℃ and sealed and stored in dark for later use, and the mother liquor can selectively kill or inhibit the reproduction of acanthopodium. At present, most of pesticides aiming at chinaberry bark products are liquid preparations, when the liquid preparations are used for killing soil pests, the liquid preparations only can kill the pests on the surface layer of soil, have weak effect on the pests in the deep layer of soil, and are easy to cause drug resistance of the pests to the pesticides. And the prior art chinaberry bark insecticidal product is a liquid preparation, so that the storage, the transportation and the use of the product are inconvenient.
Disclosure of Invention
The invention aims to provide a cortex meliae extract microcapsule. The invention also aims to provide a preparation method of the microcapsule, and the obtained cortex meliae extract microcapsule is solid in a normal state and is convenient to store and use.
The invention also aims to provide an application of the microcapsule or the cortex meliae extract microcapsule obtained by the preparation method, the cortex meliae extract microcapsule obtained by the invention can be well compounded with a soil improvement fertilizer, and when the microcapsule is used, the cortex meliae extract microcapsule and the soil improvement fertilizer are directly compounded and applied into soil, so that the microcapsule can directly reach the deep part of the soil and has a good control effect on soil pests.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the invention provides a cortex meliae extract microcapsule, wherein the capsule wall of the microcapsule is made of silicon dioxide, and the capsule core of the microcapsule is a chitosan immobilized cortex meliae extract;
wherein, the cortex meliae extract is obtained by taking cortex meliae as a raw material and performing alcohol extraction and water precipitation;
the content of the cortex meliae extract in the microcapsule is 10-30%.
The invention also provides a preparation method of the cortex meliae extract microcapsule, which comprises the following steps:
the method comprises the following steps: performing ultrasonic countercurrent extraction on cortex meliae serving as a raw material by absolute ethyl alcohol, filtering to obtain an extracting solution, concentrating the extracting solution, adding water, standing, collecting solid matters, and drying to obtain a cortex meliae extract;
step two: adding an acidic solution of chitosan into a liquid paraffin solution containing a surfactant and ethyl acetate, stirring and emulsifying, adding a glutaraldehyde solution for crosslinking, adding alkali to adjust the pH value to be alkalescent, curing, separating and drying to obtain a porous chitosan carrier;
step three: dispersing the cortex meliae extract by adopting low-concentration ethanol to obtain extract alcohol mixed liquor, placing the porous chitosan carrier in the extract alcohol mixed liquor for impregnation and adsorption, so that the cortex meliae extract is immobilized and adsorbed by the porous chitosan carrier, and drying to obtain medicine-carrying chitosan;
step four: the drug-loaded chitosan is dispersed by adopting an ethanol solution containing a surfactant, then ethyl orthosilicate is added, alkali is added to adjust the pH value to be alkalescence, silicon dioxide generated by the reaction is deposited on the surface of the drug-loaded chitosan, and the silicon dioxide-coated microcapsule, namely the cortex meliae extract microcapsule, is obtained by drying.
According to the technical scheme, the cortex meliae extract is extracted by taking cortex meliae as a raw material, then the cortex meliae extract is adsorbed and fixed by chitosan by adopting a dipping adsorption method, and finally, silicon dioxide is used as a capsule wall for microcapsule coating. The smell of the cortex meliae extract can be well masked by adopting a microcapsule coating technical means, and the microcapsule coating can well protect the components of the cortex meliae extract in the microcapsule coating and reduce the dosage loss.
The microcapsule provided by the invention has a multiple protection structure, and the external silicon dioxide capsule shell can play a role in shielding and waterproofing, so that the cortex meliae extract microcapsule has a longer storage time; inside adopts the chitosan carrier to fix, when outer silica microcapsule is bitten by the pest and is eaten and breaks, adsorb in the outside heavy concentration drug release of chitosan, produce direct poisoning effect to the pest, when the microcapsule breaks because of external effort takes place, the chitosan carrier can form the gel that has stronger adsorption after meeting water, has further fixed and guard action to inside cortex meliae extract product, can not cause the loss by a wide margin of cortex meliae extract product because of the flow of soil moisture to continue to exert soil pest's prevention and cure effect.
Further, the temperature of the ultrasonic countercurrent extraction in the first step is 65-75 ℃, the frequency of ultrasonic waves is 40-60KHz, the ultrasonic extraction time is 30-60min, and the weight of the absolute ethyl alcohol is 4-6 times of that of the cortex meliae; the method comprises the following steps of extracting a liquid extract, namely extracting the liquid extract, wherein the volume of the liquid extract is concentrated to 1/4-1/3 of the original volume to obtain a concentrated solution, the addition amount of water is 2-4 times of the volume of the concentrated solution, and standing is performed for 6-8 hours at 2-6 ℃.
Further, the acid solution of chitosan in the second step has a mass concentration of 2% -6%, and is prepared by dissolving chitosan in 1% -4% acetic acid; the deacetylation degree of the chitosan is 80-99%, and the molecular weight is 5-20 KDa. In the specific embodiment of the invention, the deacetylation degree of the selected chitosan is 97%, and the molecular weight is 10 KDa.
Further, the volume ratio of the acid solution of the chitosan to the liquid paraffin solution in the second step is (2-5): 10; in the liquid paraffin solution, the mass ratio of the surfactant to the ethyl acetate to the liquid paraffin is (2-8): (1-3): 100, respectively; wherein the surfactant is span 80. The ethyl acetate is used as a pore-foaming agent, and is used for pore-foaming of the porous chitosan carrier, so that dense and small micropores can be obtained.
Further, the glutaraldehyde solution in the second step is a glutaraldehyde aqueous solution with the mass concentration of 4% -6%, and the volume ratio of the glutaraldehyde solution to the chitosan acid solution is 1 (2-4); wherein the pH is adjusted by adding alkali, and the pH is adjusted to 8-9 by adding sodium carbonate.
Further, the mass concentration of the cortex meliae extract in the extract alcohol mixed solution in the third step is 30-40%; the low-concentration ethanol is an ethanol water solution with the mass concentration of 20-30%; the drying is carried out for 8-12h at 50-60 ℃ by adopting a vacuum drying oven; the drug-loading rate of the drug-loading chitosan is 25-40%. In order to accelerate the adsorption of the chitosan carrier to the cortex meliae extract, a small amount of low-concentration acetic acid can be dripped into the adsorption system. Under the condition of the drug loading, the balance of the auxiliary material cost can be achieved, and under the concentration, the direct lethal effect can be generated on pests in soil, so that the problem of pest drug resistance caused by low-dose drugs is solved.
Further, the ethanol solution containing the surfactant in the fourth step is a 20% -30% ethanol solution of span 80, and the mass concentration of span 80 in the ethanol solution is 4% -6%.
Further, the adding amount of the tetraethoxysilane in the step four is 25-40% of the mass of the medicine-carrying chitosan; wherein, the pH is adjusted by adding alkali to be triethylamine to adjust the pH to 8-10; wherein the reaction process is carried out for 4-5h at the temperature of 45-55 ℃ and the stirring speed of 600-800 r/min.
The invention also provides an application of the microcapsule or the cortex meliae extract microcapsule obtained by the preparation method in a soil improvement fertilizer, and the soil improvement fertilizer has a control effect on soil pests through the application.
Further, in the application, the cortex meliae extract microcapsule is added into the soil improvement fertilizer according to 2% -10%; the using amount of the soil improvement fertilizer is 10-30 kg/mu.
Further, the formula of the soil improvement fertilizer provided by the invention is prepared by mixing 25 parts by weight of peat, 20 parts by weight of rapeseed cakes, 15 parts by weight of bentonite and 40 parts by weight of nitrogen-phosphorus-potassium compound fertilizer. The cortex meliae extract microcapsule prepared by the method is compounded with the soil improvement fertilizer, so that the compatibility is good, the prevention and treatment effect of the soil improvement fertilizer on soil pests can be enhanced by adding the cortex meliae extract microcapsule, and the cortex meliae extract microcapsule can uniformly reach the soil when in use by means of the dilution and dispersion effects of the soil improvement fertilizer.
The cortex meliae extract microcapsule provided by the preferred embodiment of the invention, the preparation method and the application in the soil improvement fertilizer have the beneficial effects that:
1. the cortex meliae extract microcapsule provided by the invention is solid in a normal state, and is convenient to store and use, the cortex meliae extract microcapsule prepared by the method has a multiple protection structure, and an external silicon dioxide capsule shell can play a role in shielding and waterproofing, so that the cortex meliae extract microcapsule still has a long storage time in soil; inside adopts the chitosan carrier to fix, when outer silica microcapsule is bitten by the pest and is eaten and breaks, adsorb in the outside heavy concentration drug release of chitosan, produce direct poisoning effect to the pest, when the microcapsule breaks because of external effort takes place, the chitosan carrier can form the gel that has stronger adsorption after meeting water, has further fixed and guard action to inside cortex meliae extract product, can not cause the loss by a wide margin of cortex meliae extract product because of the flow of soil moisture to continue to exert soil pest's prevention and cure effect.
2. The cortex meliae extract microcapsule prepared by the method is applied to a soil improvement fertilizer and compounded with the soil improvement fertilizer, so that the cortex meliae extract microcapsule has good compatibility, the prevention and treatment effect of the soil improvement fertilizer on soil pests can be enhanced by adding the cortex meliae extract microcapsule, and the cortex meliae extract microcapsule can uniformly reach the soil when being used by means of the dilution and dispersion effects of the soil improvement fertilizer.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1: extraction of effective substances from cortex Meliae
The method comprises the steps of taking 10kg of dried cortex meliae as a raw material, crushing, adding anhydrous ethanol with the weight 4-6 times of that of the dried cortex meliae as an extraction solvent, extracting active ingredients in the cortex meliae by adopting ultrasonic countercurrent extraction equipment, setting the extraction temperature to be 70 ℃, the ultrasonic frequency to be 40KHz, the ultrasonic extraction time to be 45min, filtering to obtain an extracting solution, concentrating the extracting solution by adopting a reduced pressure evaporator to about 1/4-1/3 of the volume of the obtained extracting solution, stopping concentration, cooling the concentrated solution to room temperature, adding water with the volume 3 times of that of the concentrated solution, standing at 4 ℃ for 6h, collecting solid matters, drying to obtain a cortex meliae extract, and detecting the content of toosendanin by HPLC to be 35.8%.
Example 2: preparation of cortex Meliae extract microcapsule
The cortex meliae extract prepared in example 1 is sequentially immobilized by a chitosan carrier and microencapsulated by using silicon dioxide as a capsule wall material, and the specific preparation process comprises the following steps:
1) preparing a porous chitosan carrier: dissolving 4 parts by weight of chitosan in 96 parts by weight of 2% acetic acid to prepare 100 parts by weight of chitosan acid solution for later use; adding 6 parts by weight of span 80 and 2 parts by weight of ethyl acetate into 100 parts by weight of liquid paraffin, and fully mixing to obtain a liquid paraffin solution; measuring a chitosan acid solution with the volume of 30% of that of the liquid paraffin solution, adding the chitosan acid solution into the liquid paraffin solution, stirring at 600r/min for 25min to obtain an emulsion, adding a glutaraldehyde aqueous solution with the mass concentration of 5% into the obtained emulsion, and crosslinking for 5h, wherein the addition amount of the glutaraldehyde solution is 3 times of that of the chitosan acid solution; standing for 4h after crosslinking is completed, adding sodium carbonate to adjust the pH to 8-9, separating and drying to obtain the porous chitosan carrier for later use.
2) Carrying out drug loading on porous chitosan: dispersing cortex Meliae extract with 25% ethanol to obtain 35% extractive alcohol mixed solution, placing the porous chitosan carrier in the extractive alcohol mixed solution, soaking and adsorbing to make cortex Meliae extract immobilized and adsorbed by porous chitosan carrier, stopping adsorption when the content of toosendanin in the extractive alcohol mixed solution is less than 0.1% by HPLC detection, drying the obtained medicine-carrying chitosan wet product at 55 deg.C for 10 hr by vacuum drying oven, and calculating the medicine-carrying amount of the obtained medicine-carrying chitosan to be 32.5% (calculated based on the weight of cortex Meliae extract).
3) Dispersing drug-loaded chitosan by adopting a 25% ethanol solution of span 80 with the mass concentration of 5%, adding tetraethoxysilane into the drug-loaded chitosan according to 30% of the mass of the drug-loaded chitosan, adding triethylamine to adjust the pH value to 9, reacting for 4 hours at the temperature of 50 ℃ and the stirring speed of 800r/min to deposit silicon dioxide generated by the reaction on the surface of the drug-loaded chitosan, separating and drying to obtain the cortex meliae extract microcapsule particles, wherein the drug-loaded amount of the obtained cortex meliae extract microcapsule particles is about 25.9% (calculated by the mass of the cortex meliae extract).
Example 3: preparation of cortex Meliae extract microcapsule
The cortex meliae extract prepared in example 1 is sequentially immobilized by a chitosan carrier and microencapsulated by using silicon dioxide as a capsule wall material, and the specific preparation process comprises the following steps:
1) preparing a porous chitosan carrier: dissolving 4 parts by weight of chitosan in 96 parts by weight of 2% acetic acid to prepare 100 parts by weight of chitosan acid solution for later use; adding 6 parts by weight of span 80 and 2 parts by weight of ethyl acetate into 100 parts by weight of liquid paraffin, and fully mixing to obtain a liquid paraffin solution; measuring a chitosan acid solution with the volume of 30% of that of the liquid paraffin solution, adding the chitosan acid solution into the liquid paraffin solution, stirring at 600r/min for 25min to obtain an emulsion, adding a glutaraldehyde aqueous solution with the mass concentration of 5% into the obtained emulsion, and crosslinking for 5h, wherein the addition amount of the glutaraldehyde solution is 3 times of that of the chitosan acid solution; standing for 4h after crosslinking is completed, adding sodium carbonate to adjust the pH to 8-9, separating and drying to obtain the porous chitosan carrier for later use.
2) Carrying out drug loading on porous chitosan: dispersing cortex Meliae extract with 25% ethanol to obtain 30% extractive alcohol mixed solution, placing the porous chitosan carrier in the extractive alcohol mixed solution, soaking and adsorbing to make cortex Meliae extract immobilized and adsorbed by porous chitosan carrier, stopping adsorption when the content of toosendanin in the extractive alcohol mixed solution is less than 0.1% by HPLC detection, drying the obtained medicine-carrying chitosan wet product at 50 deg.C for 12 hr by vacuum drying oven, and calculating the medicine-carrying amount of the obtained medicine-carrying chitosan to be 27.8% (calculated based on the weight of cortex Meliae extract).
3) Dispersing drug-loaded chitosan by adopting 20% ethanol solution of span 80 with the mass concentration of 6%, adding tetraethoxysilane into the drug-loaded chitosan according to 40% of the mass of the drug-loaded chitosan, adding triethylamine to adjust the pH value to 8, reacting for 5 hours at the temperature of 55 ℃ and the stirring speed of 800r/min to deposit silicon dioxide generated by the reaction on the surface of the drug-loaded chitosan, separating and drying to obtain the cortex meliae extract microcapsule particles, wherein the drug-loaded amount of the obtained cortex meliae extract microcapsule particles is about 23.6% (calculated by the mass of the cortex meliae extract).
Example 4: preparation of insect-resistant soil improvement fertilizer
And (3) adding the cortex meliae extract microcapsule particles prepared in the example 2 into a soil improvement fertilizer according to the mass percentage of 5%, and fully and uniformly mixing to obtain the cortex meliae extract microcapsule.
The formula of the soil improvement fertilizer is prepared by mixing 25 parts by weight of peat, 20 parts by weight of rapeseed cakes, 15 parts by weight of bentonite and 40 parts by weight of nitrogen-phosphorus-potassium compound fertilizer.
Example 5: preparation of insect-resistant soil improvement fertilizer
The cortex meliae extract microcapsule particles prepared in example 3 are added into a soil improvement fertilizer according to the mass percentage of 5%, and the soil improvement fertilizer is obtained by fully and uniformly mixing, wherein the soil improvement fertilizer is as shown in example 4.
Example 6: preparation of insect-resistant soil improvement fertilizer
The drug-loaded chitosan prepared in example 2 is added into a soil improvement fertilizer according to the mass percentage of 5%, and the mixture is fully and uniformly mixed to obtain the soil improvement fertilizer as shown in example 4.
Example 7: preparation of insect-resistant soil improvement fertilizer
The drug-loaded chitosan prepared in example 3 is added into a soil improvement fertilizer according to the mass percentage of 5%, and the mixture is fully and uniformly mixed to obtain the soil improvement fertilizer as shown in example 4.
Example 8: preparation of insect-resistant soil improvement fertilizer
The cortex meliae extract prepared in example 1 was added to a soil improvement fertilizer in an amount of 1.3% by mass, and the mixture was mixed well, and the soil improvement fertilizer was obtained as shown in example 4.
Example 9: potting test for preventing cutworms
Preparing 150 planting pots with the volume of two gallons, dividing the planting pots into five test groups, placing the planting pots of each test group in different areas of a warm and sunny planting base, preventing soil pests in each test group from transferring by adopting isolation equipment, adopting garden soil, cleaning and killing cutworm bodies before using the garden soil, adding soil improvement fertilizer to the pot height of 1/2 when the garden soil is filled to the pot height of 1/3, placing corn seedlings, continuously filling the space in the pot with the garden soil, immediately watering the planted corn seedlings, adopting the insect-resistant soil improvement fertilizer in the invention embodiment 4 in the test group 1, adopting the insect-resistant soil improvement fertilizer in the invention embodiment 5 in the test group 2, adopting the insect-resistant soil improvement fertilizer in the invention embodiment 6 in the test group 3, adopting the insect-resistant soil improvement fertilizer in the invention embodiment 7 in the test group 4, test group 5 used the insect-resistant soil improvement fertilizer of example 8 of the present invention; on the third day of planting, 10 cutworms are placed in the soil of each planting pot, on the 10 th day of the test, 5 pots of the planting pots of the test groups 1-5 are respectively selected at random, the garden soil is poured out of the pots, the number of the cutworms in the soil is respectively counted, and the control effect percentage of the test groups 1-5 is obtained through calculation; according to the average value of the statistical results, the cutworms are supplemented to 9-11 pots in the rest planting pots, the control effect percentages of 17 th, 24 th, 31 th, 38 th and 45 th days of the test are respectively counted according to the same method, the test period is watered thoroughly once a week, the watering time and the pest placing time are separated by 3 days, and the test results are shown in the table 1:
table 1: potted plant test-result of controlling effect of cutworm
According to the table 1, the control effect of the test groups 1 to 5 on cutworms in the test period of 45 days is in a descending trend, the control effect of 5 test groups is equivalent before the 17 th day of the test, the control effect of the test group 3 is the best, the control effect of the test group 5 is obviously reduced after the 17 th day of the test, the control effect is obviously reduced after the 24 th day, the reduction range of the control effect of the test groups 1 to 4 on cutworms is obviously smaller than that of the test group 5, and the reduction range of the test groups 1 to 2 is the lowest, so that the cortex meliae extract microcapsule particles provided by the invention can play a role of long-acting control on cutworms when added into a soil improvement fertilizer.
Example 10: field test for preventing cutworms
Selecting a corn field with serious tiger damage in the suburb field of the Nanchang city as a test field, setting the corn field into 5 test groups, setting 3 test areas for each test group for repetition, and setting the area of each test area to be 0.1 mu; soil improvement fertilizer (according to 20 kg/mu) is applied during soil turning, the test group 1 adopts the insect-resistant soil improvement fertilizer in the embodiment 4, the test group 2 adopts the insect-resistant soil improvement fertilizer in the embodiment 5, the test group 3 adopts the insect-resistant soil improvement fertilizer provided in the embodiment 8, the test group 4 only applies the soil improvement fertilizer, 2.5% deltamethrin emulsifiable concentrate 500 times diluent is used for spraying the soil and plants, and the test group 5 only applies the soil improvement fertilizer without any insect-resistant agent. Corn seedlings of 5-10cm are inhibited in each test group, the row spacing of the corn plants is 0.2m multiplied by 0.6m, the percentage of the corn seedlings with stems bitten by cutworms in each test group is investigated on the 1 st day, the 3 rd day, the 7 th day, the 14 th day and the 21 st day of the corn plants, and underground pests are found in soil around the corn seedlings with stems bitten by cutworms, and the results are shown in table 2:
table 2: field test-control effect of cutworm on ground
As can be seen from Table 2, in test group 5, the corn seedlings were very bitten off without any agent; test group 4 adopts 500 times of dilution of 2.5% deltamethrin emulsifiable solution to spray soil and plants, the situation that the cutworms bite off the corn seedlings can be well controlled in seven days, and the protection effect is sharply reduced after 14 days. The test group 3 used the insect-resistant soil improvement fertilizer provided in example 8, and the insect-resistant effect was weaker in the early stage than that in the test group 4, and the insect-resistant effect was better than that in the test group 4 after 14 days. The control effect of the test groups 1 to 2 on the cutworm is lower than that of the test group 4 before 3 days, is close to that of the test group 3, the control effect of the test groups 1 to 2 on the cutworm is obviously better than that of the test groups 3 to 4 after 7 days, the overall effect is seen, the test groups 1 to 2 are better than that of the test groups 3 to 4, and the control effect of the test group 1 on the cutworm is optimal.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A cortex Meliae extract microcapsule is characterized in that the microcapsule wall material is silicon dioxide, and the microcapsule core is chitosan immobilized cortex Meliae extract;
wherein, the cortex meliae extract is obtained by taking cortex meliae as a raw material and performing alcohol extraction and water precipitation;
the content of the cortex meliae extract in the microcapsule is 10-30%.
2. A process for the preparation of microcapsules according to claim 1, comprising the steps of:
the method comprises the following steps: performing ultrasonic countercurrent extraction on cortex meliae serving as a raw material by absolute ethyl alcohol, filtering to obtain an extracting solution, concentrating the extracting solution, adding water, standing, collecting solid matters, and drying to obtain a cortex meliae extract;
step two: adding an acidic solution of chitosan into a liquid paraffin solution containing a surfactant and ethyl acetate, stirring and emulsifying, adding a glutaraldehyde solution for crosslinking, adding alkali to adjust the pH value to be alkalescent, curing, separating and drying to obtain a porous chitosan carrier;
step three: dispersing the cortex meliae extract by adopting low-concentration ethanol to obtain extract alcohol mixed liquor, placing the porous chitosan carrier in the extract alcohol mixed liquor for impregnation and adsorption, so that the cortex meliae extract is immobilized and adsorbed by the porous chitosan carrier, and drying to obtain medicine-carrying chitosan;
step four: the drug-loaded chitosan is dispersed by adopting an ethanol solution containing a surfactant, then ethyl orthosilicate is added, alkali is added to adjust the pH value to be alkalescence, silicon dioxide generated by the reaction is deposited on the surface of the drug-loaded chitosan, and the silicon dioxide-coated microcapsule, namely the cortex meliae extract microcapsule, is obtained by drying.
3. The preparation method according to claim 2, wherein the temperature of the ultrasonic countercurrent extraction in the first step is 65-75 ℃, the frequency of ultrasonic wave is 40-60KHz, the time of ultrasonic extraction is 30-60min, and the weight of the absolute ethyl alcohol is 4-6 times of that of the cortex meliae;
wherein the concentration in the step one is to concentrate the volume of the extracting solution to 1/4-1/3 of the original volume to obtain a concentrated solution, the addition amount of water is 2-4 times of the volume of the concentrated solution, and the concentrated solution is stood for 6-8h at the temperature of 2-6 ℃.
4. The preparation method according to claim 2 or 3, wherein the acid solution of chitosan in step two has a mass concentration of 2% -6%, and is prepared by dissolving chitosan in 1% -4% acetic acid; the deacetylation degree of the chitosan is 80-99%, and the molecular weight is 5-20 KDa.
5. The preparation method according to claim 2, wherein the volume ratio of the acidic solution of chitosan to the liquid paraffin solution in step two is (2-5): 10;
in the liquid paraffin solution, the mass ratio of the surfactant to the ethyl acetate to the liquid paraffin is (2-8): (1-3): 100, respectively;
wherein the surfactant is span 80.
6. The preparation method according to claim 2 or 5, characterized in that the glutaraldehyde solution in the second step is a glutaraldehyde aqueous solution with a mass concentration of 4% -6%, and the volume ratio of the glutaraldehyde solution to the chitosan acid solution is 1 (2-4); wherein the pH is adjusted by adding alkali, and the pH is adjusted to 8-9 by adding sodium carbonate.
7. The preparation method according to claim 2, wherein the mass concentration of the cortex meliae extract in the alcohol mixture of the extracts in the third step is 30-40%, and the low-concentration ethanol is an ethanol aqueous solution with a mass concentration of 20-30%; the drying is carried out for 8-12h at 50-60 ℃ by adopting a vacuum drying oven; the drug-loading rate of the drug-loading chitosan is 25-40%.
8. The preparation method according to claim 2 or 7, wherein the amount of the tetraethoxysilane added in the step four is 25-40% of the mass of the drug-loaded chitosan; wherein, the pH is adjusted by adding alkali to be triethylamine to adjust the pH to 8-10; wherein the reaction process is carried out for 4-5h at the temperature of 45-55 ℃ and the stirring speed of 600-800 r/min.
9. Use of microcapsules as claimed in claim 1 or microcapsules of cortex meliae extract obtained by the process of any one of claims 2 to 8 in a soil improvement fertilizer, whereby the soil improvement fertilizer is made soil pest control.
10. The use according to claim 9, wherein the cortex meliae extract microcapsules are added in a soil improvement fertilizer in an amount of 2% to 10%; the using amount of the soil improvement fertilizer is 10-30 kg/mu.
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Application publication date: 20210309 |