CN103798232A - Emamectin benzoate microsphere and preparation method thereof - Google Patents
Emamectin benzoate microsphere and preparation method thereof Download PDFInfo
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- CN103798232A CN103798232A CN201210455531.0A CN201210455531A CN103798232A CN 103798232 A CN103798232 A CN 103798232A CN 201210455531 A CN201210455531 A CN 201210455531A CN 103798232 A CN103798232 A CN 103798232A
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- emamectin
- benzoate
- microballoon
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Abstract
The invention discloses an emamectin benzoate microsphere and a preparation method thereof. The emamectin benzoate microsphere is prepared by utilizing an emulsification-volatilization method. According to the emulsification-volatilization method, solid spherical microspheres are prepared by taking polylactic acid as a carrier and taking gelatin as a dispersant, wherein the microspheres are monodispersed fine powder, and the particle size distribution of the microspheres is uniform. According to the emamectin benzoate microsphere, active ingredients are slowly released, the stability of emamectin benzoate is improved, a persistent effect is long, the work efficiency is high, and a lasting period can reach 3-6 months after the microsphere is applied once. The emamectin benzoate microsphere disclosed by the invention is suitable for being mixed with soil to be applied and can be widely used for treating soil insects and root-knot nematode of various crops.
Description
Technical field
The present invention relates to emamectin-benzoate microballoon and preparation method thereof, belong to pesticidal preparations field.
Background technology
Emamectin-benzoate belongs to efficiently, wide spectrum, non-harmful biological source insecticide, is developed by MSD Corp. of the U.S..It is the product of Avermectin structural modification, to the drug effect of most lepidopterous larvae higher than Avermectin, especially the drug effect of vegetables beet armyworm is exceeded to 2 orders of magnitude than Avermectin, antagonism diamond-back moth and cotton bollworm special efficacy, but toxicity reduces greatly than Avermectin.
The existing preparation of emamectin-benzoate mainly contains the regular dosage forms such as missible oil, microemulsion, water dispersible granules, effervescent tablet.Existing preparation exists following shortcoming: cream preparation contains a large amount of volatile organic solvents, be discharged in environment, and not only pollution of ecological environment, and cause the wasting of resources; Emamectin-benzoate, to ultraviolet-sensitive, is easy to photodissociation and lost efficacy in environment, and the lasting period is shorter; Conventional pesticide preparation is quick-acting, short in the crop growth phase term of validity, needs repeatedly dispenser, has reduced the availability of agricultural chemicals, has increased applications of pesticide amount and labor cost.
Emamectin-benzoate microballoon, has no report both at home and abroad.Microballoon (Microspheres or Microbeads) is the novel form that development in recent years is got up, it is the spherical preparation of preparing as carrier take macromolecular materials such as starch, shitosan, PLA, gelatin, medicine in microballoon disperses or is embedded in material and forms even spherical entity (medicine ball), it is a class homogeneous dispersion system, general 0.3～300 μ m of microsphere diameter size, the microballoon that diameter is less than 1 μ m is called Nano microsphere (Nanospheres) or nanoparticles.Albumin microsphere prepared by the methods such as common microballoon has the gelatine microsphere prepared by emulsification and cross linked with the natural macromolecular material such as gelatin, gum Arabic, utilize seasoning take albumin as capsule material or spraying is dry, by Starch Hydrolysis again through the spherex of the preparations such as emulsion polymerization, medicine and polyester material are dissolved in to low-boiling organic solvent are emulsifiable in again in the water that contains dispersant by heat or extraction etc. and remove polyesters microballoon prepared by the method for organic solvent.
The difference of microballoon and microcapsules is: microballoon Pesticides active ingredient is disperseed or is embedded in carrier and forms medicine ball, the hollow-core construction that the core (capsule-core) that microcapsules are formed by pesticide active ingredient and the protectiveness matrix (cyst wall or capsule skin) that polymer forms form; Both all have slow-release function, but microballoon carrier material used is generally all biodegradable, Environmental compatibility close friend, and the difficult degraded that the capsule skin of micro-capsule has in environment; It is reported, in some microcapsule product, the active ingredient that has 20% is difficult to discharge, virtually reduced the availability of pesticide active ingredient, and microballoon is easy to degraded, can discharge completely, agricultural chemicals availability is high.Therefore, microball preparation becomes the study hotspot of Novel Drug Delivery Systems at present in medicine, has developed multiple PLA, gelatine microsphere etc.But the application in agricultural chemicals is also little, abroad developed and prepared 48% 2-dichloroethylk dimethyl phosphate microballoon and the 42% gypsymoth property prepared with polysulfones lures plain microballoon with Merlon, domestic-developed Avermectin polylactic acid microsphere, pleocidin microballoon etc.
Emamectin-benzoate is to photo-labile, and ultraviolet degradation is serious, and field efficacy is unstable.This active ingredient is prepared as to the microballoon with slowly-releasing effect, not only suppress the decomposition of active ingredient, also there is slow releasing function, a dispenser, lasting period can reach 3～6 months, has not only saved labour, and improves the availability of agricultural chemicals, alleviate the pressure of agricultural chemicals to environment, there is more wide application prospect.
Summary of the invention
The object of this invention is to provide a kind of microball preparation take emamectin-benzoate as active ingredient.
Another object of the present invention is to provide the preparation method of described this microballoon.
This microballoon comprises that active ingredient is emamectin-benzoate 5%～40.0% by weight, is preferably 10.0%～30.0%, and is made up of high molecular polymer carrier, prepares at the oil phase of nonaqueous solvents and containing in the water of dispersant.
Applicable carrier is selected from natural polymer as protide (gelatin, albumin, fibroin albumen etc.) and polysaccharose (gum Arabic, alginate, starch, shitosan, agar etc.); Semi-synthetic macromolecule is as cellulose derivatives (methylcellulose, ethyl cellulose, carboxymethyl cellulose, cellulose acetate, O-phthalic acid cellulose etc.); Synthetic macromolecule has polyolefin (polystyrene etc.), polyacrylic resin, polymeric polyalcohols (polyethylene glycol etc.), polyesters (Merlon etc.), poly-hydroxy fatty acid class (polyglycolic acid, PLA etc.), polyaminoacid class, poly-anhydrides.Preferred carrier is PLA.
Applicable dispersant is selected from polyvinyl alcohol, gelatin, gum Arabic, carboxymethyl cellulose, sodium lignin sulfonate, calcium lignosulfonate, Sodium Polyacrylate etc., preferably gelatin.
Applicable nonaqueous solvents is selected from atoleine, carrene, chloroform, and vegetable oil is as turpentine oil or cottonseed oil, corn oil, soybean oil, peanut wet goods.Preferably carrene.
Microballoon of the present invention adopts manner known in the art preparation, as emulsification-solvent evaporation method.
Emulsification-solvent evaporation method refers to active ingredient dissolving, emulsification or is suspended in macromolecular compound solution and forms oil phase, then it is slowly added in the water that contains dispersant, form emulsion (O/W), under certain temperature, rotating speed, stir the regular hour, then by heating, decompress filter or a kind of preparation method that directly proper method such as extraction is removed solvent for dissolving macromolecule carrier and obtain globular powder.
Applicable target crop is the cereal crops such as wheat, corn, Chinese sorghum, the economic crops such as cotton, crudefiber crop, soybean, peanut, the vegetable crops such as tomato, eggplant, capsicum, lettuce, celery, wild cabbage, Kidney bean, broad bean, cowpea, pea, the ground family crops such as cucumber, pumpkin, watermelon, the solanaceous crops such as tobacco, potato, the fruit tree crops such as apple, oranges and tangerines, pears, peach, grape, strawberry, the flower plants such as chrysanthemum, China pink.
The insect that is applicable to control has root-knot nematode, the soil insects such as cutworm, wireworm, mole cricket, chafer.
The method for optimizing of using microballoon of the present invention is to mix and execute with soil, and according to controlling object, a situation arises determines suitable consumption, and conventionally formulation rate is 10～30g a.i./hm
2.
Embodiment
The present invention describes with the following example, but does not limit the scope of the invention.
embodiment 1: 13.7% emamectin-benzoate microballoon (D
50be 9.2 μ preparations m)
Adopt the preparation of emulsification-solvent evaporation method.Taking 1.2g PLA in 20mL carrene, be placed on magnetic stirring apparatus and stir, after PLA dissolves completely, add emamectin-benzoate 0.3g, continue stirring it is dissolved completely, is oil phase.Get 160mL distilled water, add 0.8g gelatin to dissolve at 40 ℃, as water.Magnetic agitation actuator temperature is adjusted to 30 ℃, and rotating speed is adjusted to 1000r/min left and right, adds 1d silicone defoaming agent, and oil phase is slowly joined in water, with 1000r/min rotating speed emulsification 3h, forms the emulsion (O/W) of homogeneous phase.Then magnetic agitation actuator temperature is risen to 40 ℃, rotating speed is adjusted to 500r/min, continues to stir 2h, allows carrene fully volatilize.Decompress filter, distilled water washing three times, normal temperature and pressure dried overnight, crosses 120 mesh sieves, obtains microballoon.Measuring medicine carrying amount is 13.7%, and envelop rate is 92.6%, volume central diameter D
50be 9.2 μ m, span (microspherulite diameter breadth coefficient) is 1.69.
According to the step identical with embodiment 1, can prepare following examples.
embodiment 2: 13% emamectin-benzoate microballoon (D
50be 23.4 μ preparations m)
The PLA taking is 1.8g, and gelatin consumption is 2.4g, and other preparation methods are with embodiment 1.The microballoon medicine carrying amount of preparation is 13%, and envelop rate is 88.3%, and volume central diameter is 23.4 μ m, and span is 0.75.Visible change PLA and gelatin consumption, can prepare the microballoon of different-grain diameter, processes the needs of different lasting periods with adapted soil.
embodiment 3: the preparation of 20.6% emamectin-benzoate microballoon
The PLA taking is 1.6g, and emamectin-benzoate is 0.8g, and gelatin is 2.4g, and other preparation methods are with embodiment 1.The microballoon medicine carrying amount of preparation is 20.6%, and envelop rate is 79.4%, and volume central diameter is 80.4 μ m, and span is 1.00.
embodiment 4: the preparation of 34.8% emamectin-benzoate microballoon
The PLA taking is 1.6g, and emamectin-benzoate is 1.6g, and gelatin is 2.4g, and other preparation methods are with embodiment 1.The microballoon medicine carrying amount of preparation is 34.8%, and envelop rate is 84.4%, and volume central diameter is 98.8 μ m, and span is 0.91.
Emamectin-benzoate microballoon of the present invention and preparation method thereof is described by specific embodiment.Those skilled in the art can use for reference content appropriate change raw material of the present invention, process conditions etc. and realize corresponding other objects, its relevant change does not all depart from content of the present invention, within all similar replacements and change will become apparent to those skilled in the art that and be all deemed to be included in scope of the present invention.
Claims (11)
1. an emamectin-benzoate microballoon, it is characterized in that emamectin-benzoate content is 5.0%～40.0% by weight percentage, be preferably 10.0～30.0%, and formed by high molecular polymer carrier, prepare at the oil phase of nonaqueous solvents and containing in the water of dispersant.
2. emamectin-benzoate microballoon according to claim 1, it is characterized in that: carrier is that natural polymer is as protide, polysaccharose, semi-synthetic macromolecule is as cellulose derivatives, and synthetic macromolecule has polyolefin polymeric polyalcohols, polyesters, poly-hydroxy fatty acid class, polyaminoacid class, poly-anhydrides.
3. according to the emamectin-benzoate microballoon described in claim 1～2, it is characterized in that: preferred carrier is synthetic polyphosphazene polymer lactic acid.
4. according to the emamectin-benzoate microballoon described in claim 1～3, it is characterized in that PLA bulking value concentration in oil-based system is 120～200mg/mL, wherein emamectin-benzoate and PLA by weight ratio be 1: 1～1: 5, be preferably 1: 4.
5. according to the emamectin-benzoate microballoon described in claim 1～4, it is characterized in that: nonaqueous solvents is selected from atoleine, carrene, chloroform, vegetable oil is as turpentine oil or cottonseed oil, corn oil, soybean oil, peanut oil.
6. emamectin-benzoate microballoon according to claim 5, is characterized in that: the preferred carrene of nonaqueous solvents.
7. emamectin-benzoate microballoon according to claim 1, is characterized in that: dispersant is selected from polyvinyl alcohol, gelatin, gum Arabic, carboxymethyl cellulose, sodium lignin sulfonate, calcium lignosulfonate, Sodium Polyacrylate.
8. emamectin-benzoate microballoon according to claim 7, is characterized in that the preferred gelatin of dispersant.
9. according to the emamectin-benzoate microballoon described in claim 7～8, it is characterized in that the bulking value specific concentration of aqueous gelatin solution is 0.5%～2.5%, be preferably 0.5%～1.5%.
10. according to the emamectin-benzoate microballoon described in claim 1～9, it is characterized in that: oil phase: the ratio of water is 1: 8～1: 15 by volume, is preferably 1: 8～1: 10.
11. according to the emamectin-benzoate microballoon described in claim 1～10, and its preparation process is:
(1) emulsification: magnetic agitation actuator temperature is adjusted to 30 ℃, rotating speed is adjusted to 1000r/min left and right, adds 1d silicone defoaming agent, oil phase is slowly joined in the water that contains dispersant, with the rotating speed emulsification 3h of 1000r/min, form the emulsion (O/W) of homogeneous phase.
(2) volatilization: magnetic agitation actuator temperature is risen to 40 ℃, and rotating speed is adjusted to 500r/min, continues to stir 2h, allows the carrene in emulsion fully volatilize.
(3) decompress filter: with distilled water washing three times, normal temperature and pressure dried overnight, crosses 120 mesh sieves, obtains microballoon.
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| CN104206399A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Pyraclostrobin nanoparticle and preparation method of pyraclostrobin nanoparticle |
| CN104206393A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Abamectin B2 microsphere and preparation method of abamectin B2 microsphere |
| CN104872170A (en) * | 2015-06-11 | 2015-09-02 | 福建农林大学 | Efficient cyhalothrin methylamino abamectin benzoate microsphere water dispersible granules |
| CN104886091A (en) * | 2015-06-30 | 2015-09-09 | 福建农林大学 | Biodegradable emamectin benzoate microsphere |
| CN105766949A (en) * | 2016-04-13 | 2016-07-20 | 福建农林大学 | Emamectin benzoate sustained release solid dispersion and preparing method thereof |
| CN105851022A (en) * | 2016-05-10 | 2016-08-17 | 中国科学院化学研究所 | Solid-state avermectin particle preparation and preparation method and application thereof |
| CN106689150A (en) * | 2016-11-14 | 2017-05-24 | 广西大学 | Method for preparing cellulose ester emamectin benzoate urea micro-capsules |
| CN106719636A (en) * | 2017-01-13 | 2017-05-31 | 北京林业大学 | A kind of preparation method of novel agrochemical bovine serum albumin(BSA) thiacloprid nano-particle |
| CN106818799A (en) * | 2017-01-13 | 2017-06-13 | 北京林业大学 | A kind of preparation method of the bovine serum albumin(BSA) fenoxycarb Nano medication for preventing and treating ditch socket of the eye elephant |
| CN106857646A (en) * | 2016-12-23 | 2017-06-20 | 孙华飞 | A kind of emamectin-benzoate mite killing suspending agent not developed immunity to drugs and preparation method thereof |
| CN106942256A (en) * | 2017-02-20 | 2017-07-14 | 北京林业大学 | A kind of new preparation method for containing thiacloprid and the protein nano ball of pheromones |
| CN107410829A (en) * | 2017-03-30 | 2017-12-01 | 湖北工业大学 | A kind of method for improving polysaccharide/albumen composition emulsion stability |
| CN108684688A (en) * | 2018-06-14 | 2018-10-23 | 国家纳米科学中心 | A kind of nano pesticide composition and preparation method thereof |
| CN109953035A (en) * | 2019-04-17 | 2019-07-02 | 中国农业科学院植物保护研究所 | Anabasine pesticide gelatine microsphere agent and the preparation method and application thereof |
| CN110367249A (en) * | 2019-07-24 | 2019-10-25 | 陕西科技大学 | A kind of degradable medicine carrying membrane material and its preparation method and application with slow-release function step by step |
| TWI700355B (en) * | 2019-09-12 | 2020-08-01 | 國立中山大學 | Gel composition used for soil remediation |
| CN111616344A (en) * | 2020-05-18 | 2020-09-04 | 黄勇生 | Preparation method of cinnamon essential oil-cellulose nano microsphere suspension |
| CN115779144A (en) * | 2022-09-27 | 2023-03-14 | 成都奇璞生物科技有限公司 | Degradable microspheres, preparation method and application thereof, and filler for treating stress urinary incontinence |
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| CN104206399A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Pyraclostrobin nanoparticle and preparation method of pyraclostrobin nanoparticle |
| CN104206393A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Abamectin B2 microsphere and preparation method of abamectin B2 microsphere |
| CN104872170B (en) * | 2015-06-11 | 2017-06-06 | 福建农林大学 | Gamma cyhalothrin emamectin-benzoate aqueous microsphere shot agent |
| CN104872170A (en) * | 2015-06-11 | 2015-09-02 | 福建农林大学 | Efficient cyhalothrin methylamino abamectin benzoate microsphere water dispersible granules |
| CN104886091A (en) * | 2015-06-30 | 2015-09-09 | 福建农林大学 | Biodegradable emamectin benzoate microsphere |
| CN105766949A (en) * | 2016-04-13 | 2016-07-20 | 福建农林大学 | Emamectin benzoate sustained release solid dispersion and preparing method thereof |
| CN105766949B (en) * | 2016-04-13 | 2018-03-13 | 福建农林大学 | A kind of emamectin benzoate slow-release solid dispersion and preparation method thereof |
| CN105851022A (en) * | 2016-05-10 | 2016-08-17 | 中国科学院化学研究所 | Solid-state avermectin particle preparation and preparation method and application thereof |
| CN106689150A (en) * | 2016-11-14 | 2017-05-24 | 广西大学 | Method for preparing cellulose ester emamectin benzoate urea micro-capsules |
| CN106689150B (en) * | 2016-11-14 | 2019-04-12 | 广西大学 | A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule |
| CN106857646A (en) * | 2016-12-23 | 2017-06-20 | 孙华飞 | A kind of emamectin-benzoate mite killing suspending agent not developed immunity to drugs and preparation method thereof |
| CN106818799A (en) * | 2017-01-13 | 2017-06-13 | 北京林业大学 | A kind of preparation method of the bovine serum albumin(BSA) fenoxycarb Nano medication for preventing and treating ditch socket of the eye elephant |
| CN106818799B (en) * | 2017-01-13 | 2022-03-15 | 北京林业大学 | Preparation method of bovine serum albumin-fenoxycarb nano-drug for preventing and treating orbital elephant |
| CN106719636A (en) * | 2017-01-13 | 2017-05-31 | 北京林业大学 | A kind of preparation method of novel agrochemical bovine serum albumin(BSA) thiacloprid nano-particle |
| CN106719636B (en) * | 2017-01-13 | 2022-03-18 | 北京林业大学 | Preparation method of novel pesticide bovine serum albumin-thiacloprid nanoparticles |
| CN106942256A (en) * | 2017-02-20 | 2017-07-14 | 北京林业大学 | A kind of new preparation method for containing thiacloprid and the protein nano ball of pheromones |
| CN107410829A (en) * | 2017-03-30 | 2017-12-01 | 湖北工业大学 | A kind of method for improving polysaccharide/albumen composition emulsion stability |
| CN107410829B (en) * | 2017-03-30 | 2020-04-24 | 湖北工业大学 | Method for improving emulsification stability of polysaccharide/protein compound |
| CN108684688A (en) * | 2018-06-14 | 2018-10-23 | 国家纳米科学中心 | A kind of nano pesticide composition and preparation method thereof |
| CN109953035A (en) * | 2019-04-17 | 2019-07-02 | 中国农业科学院植物保护研究所 | Anabasine pesticide gelatine microsphere agent and the preparation method and application thereof |
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| TWI700355B (en) * | 2019-09-12 | 2020-08-01 | 國立中山大學 | Gel composition used for soil remediation |
| CN111616344A (en) * | 2020-05-18 | 2020-09-04 | 黄勇生 | Preparation method of cinnamon essential oil-cellulose nano microsphere suspension |
| CN115779144A (en) * | 2022-09-27 | 2023-03-14 | 成都奇璞生物科技有限公司 | Degradable microspheres, preparation method and application thereof, and filler for treating stress urinary incontinence |
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Application publication date: 20140521 |