CN113396907A - Chitosan encapsulated hexa-methyl mite acid nano acaricide and preparation method thereof - Google Patents
Chitosan encapsulated hexa-methyl mite acid nano acaricide 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a chitosan encapsulated hexa-methyl mite acid nano acaricide and a preparation method thereof, wherein the nano acaricide is prepared from the following raw materials in percentage by mass: 46.75-55.45% of 1% chitosan, 5.70-9.86% of hexa-methyl mite acid, 4.16-6.88% of 1% sodium alginate, 0.54-0.57% of sodium tripolyphosphate and 20.86-25.14% of deionized water, wherein 1% chitosan contains 1.08-1.14% of glacial acetic acid. Has good agricultural production and plant protection application potential, and has strong application and popularization value by using a simple synthesis method, green synthesis raw materials, excellent phytophaga killing and plant resistance induction effects.
Description
Technical Field
The invention belongs to the technical field of plant protection, and particularly relates to a chitosan encapsulated hexa-methyl mite acid nano acaricide and a preparation method thereof.
Background
The healthy green food is required while high yield is pursued, so that low-toxicity and high-efficiency pesticides are urgently needed at present, the development of high-efficiency green pesticides is difficult, the effect of plant-derived pesticides is slow, the effect of chemical pesticides is fast, but the control objects are easy to generate resistance, and the phytophagous spider mites are one of typical representatives of the pesticides. The problem can be well relieved by the appearance of the nanotechnology, and each drop of pesticide can be utilized as well as possible, so that the dosage of the pesticide entering an environmental circulation system is reduced.
Phytophagous spider mites are a very serious pest mite which is widely distributed in China and even all over the world. It can be a hundred or more plant species worldwide, including several important commercial agricultural and horticultural crops. The method has strong reproductive capacity, short reproduction time, limited region, high inbred line rate, high pesticide exposure possibility and great prevention and control difficulty. Some common acaricides such as dephenolate, cycloheximide and fenbutastatin oxide are limited or strictly limited in their application in our country due to their high residue and resistance problems. There is an urgent need to find new acaricides. The discovery of novel biogenic pesticides is one of the important approaches to the development of novel pesticides.
Natural biological activity is a variety of chemicals produced by various organisms during their life activities. Since the variety of organisms is very diverse, each organism has a system for developing its own biological activities during the evolution of the organisms, forming differences in physiological and biochemical processes, thereby producing various natural substances. Therefore, the development of medicines and pesticides in natural substances is an important way for creating novel medicines. Since ancient times, China has utilized various herbs to treat different diseases. The use of yu teng, tobacco and pyrethrum as insecticides has also been known for hundreds of years. However, since the development speed of the related basic disciplines of natural products is relatively slow in the early period, the development and utilization of natural products are relatively lagged. After the 21 st century, with the continuous and rapid development of various technologies, such as extraction, separation and analysis technologies, and the wide application of a series of more advanced structure identification technologies, especially the rapid development of modern molecular biology-related technologies, the research and development of natural products become a particularly popular hotspot in the development of modern pesticides and medicines.
The chitosan is a product obtained by removing partial acetyl groups from natural polysaccharide chitin, has the advantages of biodegradability, nontoxicity, biocompatibility, mucous membrane adhesion, permeability promotion and the like, and has wide research and application in a plurality of fields such as medicine, pesticide, tissue engineering, environmental protection, agriculture, beauty and health care and the like. When applied to the agricultural field, the chitosan has the effects of no toxic or side effect on plants, good affinity, no harm to human and livestock, wide adaptability, capability of realizing biodegradation and the like, and is widely applied to the agricultural field. Chitosan is a positively charged linear polysaccharide (poly-beta- (1,4) -2-amino-2-deoxy-D-glucose) obtained by deacetylation of chitin, and is also the only nitrogen-containing basic polysaccharide. As a natural polymer material with wide application, the application of chitosan in the agricultural field becomes a research hotspot at home and abroad. The chitosan film, solution, particle and other materials prepared by various process methods are widely applied to the agricultural fields of plant disease and insect pest control, vegetable and fruit preservation, soil improvement, animal feed and other aspects.
The sodium alginate has the functions of promoting production, improving the stress resistance of plants and resisting bacteria. It is a poly-silver ion biological polysaccharide extracted from brown algae, and is widely applied to various fields of medicament preparations, tissue engineering, food development and the like due to higher biocompatibility and lower biological toxicity. The abundant anions on the surface of the composite material can generate stronger physical action with most compounds so as to form composite materials with different functions. The hydrogel with the particle size ranging from micron to nanometer can be formed between the chitosan or polylysine through electrostatic interaction, and the hydrogel can be used for drug carriers to change drug administration modes, enhance drug stability, and simultaneously improve the stability of drug release or action in different environments. The application of sodium alginate will be radiated to more strange fields, and the research on the field of agriculture is gradually carried out.
Disclosure of Invention
In order to overcome the problems, the invention provides a chitosan encapsulated hexa-methyl mite acid nano acaricide and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a chitosan encapsulated hexa-methyl mite acid nanometer acaricide is prepared from the following raw materials in percentage by mass: 46.75-55.45% of 1% chitosan, 5.70-9.86% of hexa-methyl mite acid, 4.16-6.88% of 1% sodium alginate, 0.54-0.57% of sodium tripolyphosphate and 20.86-25.14% of deionized water, wherein 1% chitosan contains 1.08-1.14% of glacial acetic acid.
Wherein the molecular formula of the hexa-methyl acarinic acid is C17H26O3The hexa-methyl acarid has molecular weight of 278.4, melting point of 172-174 ℃, storage condition of room temperature, certain stimulation effect on eyes, respiratory tract and skin, and chemical structural formula as follows:
the 1% chitosan has excellent performances of biological functionality, compatibility, safety, microbial degradability and the like, the chemical name of the chitosan is polyglucosamine (1-4) -2-amino-B-D glucose, the chitosan is dissolved in water to form hydrogel, and the structural formula of the chitosan is as follows:
wherein the hexa-methyl mite acid has a purity of 99.0%, and is an animal source mite-killing active ingredient derived from pupa shells of yellow moth.
Wherein 1% sodium alginate is poly silver ion biological polysaccharide extracted from brown algae, and sodium tripolyphosphate is cross-linking agent.
Wherein the acaricide has a pH <6.5 and the glacial acetic acid has a pH < 6.0.
Wherein the prevention range comprises tetranychus urticae, tetranychus cinnabarinus, panonychus citri, tetranychus theobromae and the like.
The invention also provides a preparation method of the chitosan encapsulated hexa-methyl mite acid nano acaricide, which comprises the following steps: preparing a 2% chitosan solution containing 1% glacial acetic acid, wherein the hexa-methyl mite acid solution is prepared by the following steps in a volume ratio of 10: 2, after uniformly mixing, magnetically stirring for 2 hours at the rotating speed of 800rpm, adding 2mL of 2% sodium alginate solution by using a dropper, continuously stirring for 2 hours, then dropwise adding 0.01M/L sodium tripolyphosphate solution, and stirring for 6 hours to form colloid.
The invention has the following advantages:
1. the chemical name of the raw material 1% of chitosan used in the invention is polyglucosamine (1-4) -2-amino-B-D glucose, and the chitosan has excellent performances such as biological functionality, compatibility, safety, microbial degradability and the like;
2. the active ingredient of the hexa-methyl mite acid is an animal source acaricidal active substance, and the content of the hexa-methyl mite acid in the shell of the yellow moth pupa is high; the chemical structural formula is simple, and the derivative has great plasticity in the aspect of derivative synthesis, and is expected to become a lead compound to carry out subsequent research and development of series compounds;
3. the cross-linking agent used in the invention is sodium tripolyphosphate, and the chemical structure of the cross-linking agent is amorphous water-soluble linear polyphosphate which is commonly used as an additive in food;
4. the chitosan encapsulated hexamanthalic acid nano acaricide prepared by the invention is prepared based on natural active substances, and has the characteristics of greenness, safety and high efficiency.
Drawings
FIG. 1 is a schematic representation of the release profile of hexamethonic acid and chitosan in an example of the present invention;
FIG. 2 is a schematic view of a scanning electron microscope of the inventive example of the hexa-methyl-mite acid and chitosan.
Detailed Description
The present invention will be further described below, but the present invention is not limited to these.
Examples
A chitosan encapsulated hexa-methyl mite acid nanometer acaricide is prepared from the following raw materials in percentage by mass: 46.75-55.45% of 1% chitosan, 5.70-9.86% of hexa-methyl mite acid, 4.16-6.88% of 1% sodium alginate, 0.54-0.57% of sodium tripolyphosphate and 20.86-25.14% of deionized water, wherein 1% chitosan contains 1.08-1.14% of glacial acetic acid.
A preparation method of a chitosan encapsulated hexa-methyl mite acid nano acaricide comprises the following steps: under the condition of the rotation speed of 800rpm, firstly 10mL of chitosan is added with 2mg of hexa-methyl-mite acid and stirred for 2h, then 2mL of sodium alginate is added dropwise and stirred for 2h, then sodium tripolyphosphate is added, and then the mixture is centrifuged by a high-speed centrifuge at the rotation speed of 12000rpm after 4 h.
Collecting a proper amount of supernatant to detect the coating rate, and detecting by using an enzyme-labeling instrument to obtain that the coating rate of the hexamanthalic acid is 95.6 percent; the hexa-methyl acarbonic acid and the chitosan are bonded together through simple bonding and hydrogen bond physical action, and form smaller particles under the condition of high-speed rotation, so that the coating rate of the medicament is increased.
As shown in Table 1, Tetranychus cinnabarinus treated with hexa-methoate @ chitosan for 48h LC50LC of 0.011mg/mL, hexa-methyl-mite-acid50The value is 0.083mg/mL, and the dosage of the raw pesticide is obviously reduced.
TABLE 1 lethal effect of Hexamic acid and chitosan on female Tetranychus cinnabarinus
As shown in fig. 1, the release rate of 69.5% is achieved after 3 days of release, so that the release of the drug is easier when chitosan is used as a wall material, and the harm of harmful mites can be controlled more quickly.
Selection of the wall material of the hexa-methyl mite:
TABLE 2 preparation of Hexamethylcarbamazepine acid and Chitosan
Table 2 shows that the suitable wall material of the hexa-methyl mite acid is chitosan, and the coating rate of the chitosan as the wall material of the hexa-methyl mite acid is higher than that of the cellulose nanocrystal suspension.
As shown in figure 2, the nano-hexamanthalic acid and chitosan have the size of about 25nm and are relatively uniform in size, and the hexamanthalic acid in the hexamanthalic acid and chitosan is easy to release, so that the effect of quickly controlling harmful mites can be achieved.
It is noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (6)
1. A chitosan encapsulated hexa-methyl mite acid nanometer acaricide is characterized in that: the composite material is prepared from the following raw materials in percentage by mass: 46.75-55.45% of 1% chitosan, 5.70-9.86% of hexa-methyl mite acid, 4.16-6.88% of 1% sodium alginate, 0.54-0.57% of sodium tripolyphosphate and 20.86-25.14% of deionized water, wherein 1% chitosan contains 1.08-1.14% of glacial acetic acid.
2. The chitosan encapsulated hexamanthalic acid nano miticide as claimed in claim 1, wherein: the hexa-methyl mite acid has the purity of 99.0 percent and is an animal source mite-killing active ingredient derived from yellow moth pupa shells.
3. The chitosan encapsulated hexamanthalic acid nano miticide as claimed in claim 1, wherein: the 1% sodium alginate is poly silver ion biological polysaccharide extracted from brown algae, and the sodium tripolyphosphate is a cross-linking agent.
4. The chitosan encapsulated hexamanthalic acid nano miticide as claimed in claim 1, wherein: the acaricide has a pH of <6.5 and glacial acetic acid has a pH of < 6.0.
5. The chitosan encapsulated hexamanthalic acid nano miticide as claimed in claim 1, wherein: the control range includes two kinds of mite, including tetranychus cinnabarinus, panonychus citri and yellow tea mite.
6. A preparation method of a chitosan encapsulated hexa-methyl mite acid nano acaricide is characterized by comprising the following steps: the method comprises the following steps: preparing a 2% chitosan solution containing 1% glacial acetic acid, wherein the hexa-methyl mite acid solution is prepared by the following steps in a volume ratio of 10: 2, after uniformly mixing, magnetically stirring for 2 hours at the rotating speed of 800rpm, adding 2mL of 2% sodium alginate solution by using a dropper, continuously stirring for 2 hours, then dropwise adding 0.01M/L sodium tripolyphosphate solution, and stirring for 6 hours to form colloid.
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CN1686560A (en) * | 2005-04-08 | 2005-10-26 | 武汉大学 | Chitin tetra ammonium salt nano-particle, its preparation method and use |
CN101167706A (en) * | 2007-10-26 | 2008-04-30 | 东南大学 | Method for synthesizing chitosan nano mcirocapsule |
CN112293477A (en) * | 2020-10-20 | 2021-02-02 | 西南大学 | Litchi fresh-keeping spray agent with VC, D-limonene and citric acid encapsulated by chitosan |
CN112314596A (en) * | 2020-10-23 | 2021-02-05 | 西南大学 | Animal-derived acaricide 20-30% amitraz acid water emulsion and preparation method and application thereof |
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