CN112931498A - Chitosan-coated gibberellin sustained-release microcapsule and preparation method thereof - Google Patents

Chitosan-coated gibberellin sustained-release microcapsule and preparation method thereof Download PDF

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Publication number
CN112931498A
CN112931498A CN201911261384.1A CN201911261384A CN112931498A CN 112931498 A CN112931498 A CN 112931498A CN 201911261384 A CN201911261384 A CN 201911261384A CN 112931498 A CN112931498 A CN 112931498A
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gibberellin
chitosan
coated
sustained
acetic acid
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CN201911261384.1A
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Chinese (zh)
Inventor
尹恒
谢红国
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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
    • A01N25/26—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
    • 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
    • A01N43/06—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 five-membered rings
    • A01N43/12—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 five-membered rings condensed with a carbocyclic ring
    • 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

Abstract

The invention relates to a chitosan coated gibberellin sustained-release microcapsule and a preparation method thereof, belonging to the field of plant growth regulators, pesticides and agricultural fertilizers. The chitosan-coated gibberellin sustained-release microcapsule is obtained by coating gibberellin with chitosan. Under the condition of the same dosage, the gibberellin microcapsule coated by chitosan can keep the drug effect for a longer time.

Description

Chitosan-coated gibberellin sustained-release microcapsule and preparation method thereof
Technical Field
The invention relates to a chitosan coated gibberellin sustained-release microcapsule and a preparation method thereof, belonging to the field of plant growth regulators, pesticides and agricultural fertilizers.
Background
Gibberellins, a ubiquitous plant hormone. The chemical structure belongs to diterpenoid acid and is derived from a tetracyclic skeleton. Can promote the growth of stems and leaves, promote bolting and flowering in advance, promote the germination of seeds, tubers and root tubers, stimulate the growth of fruits, increase the fruiting rate or form seedless fruits and the like. It can be used for increasing yield of potato, tomato, rice, wheat, cotton, soybean, pea, tobacco, fruit tree, etc.
One major disadvantage of gibberellins is their poor stability, with only 90% or more gibberellins failing to hydrolyze over 2 hours in mildly alkaline (pH >9) or alkaline solutions. This problem is overcome by overdosing or repeated dosing by the applicator. However, when too much gibberellin is applied, the plants lose green and grow on vain, and even rust fruits, hardening and deforming fruits and other phytotoxicity problems can occur. At present, clear water or alkaline water is adopted for leaching, and medicament remediation with a relieving function is sprayed, but the problems are not solved from the preparation.
Disclosure of Invention
The invention adopts the gibberellin microcapsule coated by chitosan, and solves the problems of easy phytotoxicity, poor stability, short duration and the like of the traditional pesticide preparation.
The invention provides a chitosan-coated gibberellin sustained-release microcapsule, which is obtained by coating gibberellin with chitosan.
The molecular weight of the chitosan is preferably 100-500kDa, and the deacetylation degree is 60-99 percent.
The invention preferably selects the gibberellin and the chitosan with the mass ratio of 1: 16-100.
The particle size of the chitosan-coated gibberellin sustained-release microcapsule is preferably 0.5-20 microns.
The invention also aims to provide a preparation method of the chitosan-coated gibberellin sustained-release microcapsule, which comprises the following steps: adding the gibberellin solution into an acetic acid aqueous solution of chitosan to obtain a gibberellin emulsion; and (3) spray drying the gibberellin emulsion to obtain the chitosan coated gibberellin sustained-release microcapsule.
The invention preferably selects the gibberellin concentration in the gibberellin solution to be 0.5-50 mg/mL; the concentration of the surfactant in the gibberellin solution is 0-40 mg/mL; the surfactant is at least one of tween 20, tween 40, tween 60, tween 80, lecithin, polyoxyethylene 400 monolaurate, polyoxyethylene 400 monostearate and polyoxyethylene 400 monooleate; the solvent in the gibberellin solution is methanol, ethanol or ethyl acetate.
The invention preferably selects the chitosan concentration in the acetic acid water solution of the chitosan to be 0.5-20 mg/mL; the mass percentage concentration of the glacial acetic acid in the acetic acid aqueous solution is 0.2-2%.
The invention preferably selects the volume ratio of the gibberellin solution to the acetic acid aqueous solution of chitosan to be 1: 1-4.
The invention preferably selects the air inlet temperature of the spray drying to be 180-200 ℃ and the air outlet temperature to be 70-100 ℃.
The invention has the beneficial effects that:
the degradable natural polysaccharide chitosan is used as the coating material, the coating effect is good, and the degradation product has no pollution to the environment;
the chitosan-coated gibberellin microcapsule is adopted, and the once administration dosage can be higher than that of uncoated gibberellin;
under the condition of the same dosage, the gibberellin microcapsule coated by chitosan can keep the drug effect for a longer time;
besides being capable of coating gibberellin, chitosan also has activity of inducing plant immune activity improvement.
Drawings
In the figure 3 of the attached drawings of the invention,
FIG. 1 is a photomicrograph of chitosan-coated gibberellin-sustained-release microcapsules prepared in example 1;
FIG. 2 is a graph showing the cumulative release rate of the chitosan-coated gibberellin sustained-release microcapsules prepared in example 1;
FIG. 3 shows the stability of the chitosan-coated gibberellin sustained-release microcapsules prepared in example 1.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A preparation method of chitosan coated gibberellin sustained-release microcapsules comprises the following steps:
dissolving a gibberellin original drug and Tween 20 in ethyl acetate to obtain a gibberellin solution, wherein the concentrations of the gibberellin original drug and Tween 20 in the gibberellin solution are respectively 20mg/mL and 40 mg/mL;
dissolving chitosan in an acetic acid aqueous solution to obtain an acetic acid aqueous solution of chitosan, wherein the concentration of chitosan in the acetic acid aqueous solution of chitosan is 10mg/mL, the molecular weight of chitosan is 500kDa, the deacetylation degree is 90 percent, and the mass percentage concentration of glacial acetic acid in the acetic acid aqueous solution is 1 percent;
slowly dropwise adding 1 volume of gibberellin solution into 1 volume of chitosan acetic acid aqueous solution under the condition of stirring, and continuously stirring for 30min to obtain gibberellin emulsion;
spray drying gibberellin emulsion at inlet temperature of 185 deg.C and outlet temperature of 80 deg.C to obtain chitosan coated gibberellin sustained-release microcapsule with particle diameter of 0.5-15 μm.
Example 2
A preparation method of chitosan coated gibberellin sustained-release microcapsules comprises the following steps:
dissolving a gibberellin original drug and Tween 20 in ethanol to obtain a gibberellin solution, wherein the concentrations of the gibberellin original drug and the Tween 20 in the gibberellin solution are respectively 50mg/mL and 5 mg/mL;
dissolving chitosan in an acetic acid aqueous solution to obtain an acetic acid aqueous solution of chitosan, wherein the concentration of chitosan in the acetic acid aqueous solution of chitosan is 20mg/mL, the molecular weight of chitosan is 300kDa, the degree of deacetylation is 80%, and the mass percentage concentration of glacial acetic acid in the acetic acid aqueous solution is 0.2%;
slowly dropwise adding 1 volume of gibberellin solution into 4 volumes of chitosan acetic acid aqueous solution under the condition of stirring, and continuously stirring for 30min to obtain gibberellin emulsion;
spray drying gibberellin emulsion at air inlet temperature of 190 deg.C and air outlet temperature of 80 deg.C to obtain chitosan coated gibberellin sustained-release microcapsule with particle diameter of 0.5-20 μm.
Example 3
A preparation method of chitosan coated gibberellin sustained-release microcapsules comprises the following steps:
dissolving gibberellin original drug and lecithin in ethanol to obtain gibberellin solution, wherein the concentrations of the gibberellin original drug and the lecithin in the gibberellin solution are 0.5mg/mL and 10mg/mL respectively;
dissolving chitosan in an acetic acid aqueous solution to obtain an acetic acid aqueous solution of chitosan, wherein the concentration of chitosan in the acetic acid aqueous solution of chitosan is 1mg/mL, the molecular weight of chitosan is 100kDa, the degree of deacetylation is 60%, and the mass percentage concentration of glacial acetic acid in the acetic acid aqueous solution is 2%;
slowly dropwise adding 1 volume of gibberellin solution into 2 volumes of chitosan acetic acid aqueous solution under the condition of stirring, and continuously stirring for 30min to obtain gibberellin emulsion;
spray drying gibberellin emulsion at air inlet temperature of 200 deg.C and air outlet temperature of 70 deg.C to obtain chitosan coated gibberellin sustained-release microcapsule with particle diameter of 1-10 μm.
Example 4
A preparation method of chitosan coated gibberellin sustained-release microcapsules comprises the following steps:
dissolving gibberellin original drug and lecithin in methanol to obtain gibberellin solution, wherein the concentrations of the gibberellin original drug and the lecithin in the gibberellin solution are respectively 20mg/mL and 40 mg/mL;
dissolving chitosan in an acetic acid aqueous solution to obtain an acetic acid aqueous solution of chitosan, wherein the concentration of chitosan in the acetic acid aqueous solution of chitosan is 20mg/mL, the molecular weight of chitosan is 200kDa, the degree of deacetylation is 99%, and the mass percentage concentration of glacial acetic acid in the acetic acid aqueous solution is 0.5%;
slowly dropwise adding 1 volume of gibberellin solution into 1 volume of chitosan acetic acid aqueous solution under the condition of stirring, and continuously stirring for 30min to obtain gibberellin emulsion;
spray drying gibberellin emulsion at air inlet temperature of 190 deg.C and air outlet temperature of 70 deg.C to obtain chitosan coated gibberellin sustained-release microcapsule with particle diameter of 0.5-20 μm.
Example 5
The product prepared in example 1 was selected for characterization, and the results show that: microscope characterization of chitosan coated gibberellin sustained-release microcapsule shows that its particle diameter is 0.5-15 μm, as shown in figure 1; the product is dispersed in deionized water according to the concentration of 200mg/L of completely dissolved gibberellin, and the supernatant is taken at different times to measure the absorption at 270nm of the supernatant so as to represent the release rate, and the result shows that: the release is less than 40% in 24h, less than 70% in 72h and 80% in 168h, as shown in figure 2; the product is dispersed in a phosphate buffer solution with pH6.1 according to the concentration of 200mg/L of completely dissolved gibberellin, and the supernatant is taken at different time to measure the absorption at 255nm of the supernatant so as to represent the stability of the gibberellin, and the result shows that: chitosan-coated gibberellin has significantly higher stability than gibberellin-coated drugs, as shown in figure 3.
Example 6
The chitosan-coated gibberellin sustained-release microcapsule solution and gibberellin are used for respectively treating grapes (according to the gibberellin concentration of 200mg/L) at the later stage of flowers, the rusting rate of the chitosan-coated gibberellin sustained-release microcapsule group is lower than 5%, and the rusting rate of the gibberellin naked drug group is higher than 30%.

Claims (9)

1. A chitosan coated gibberellin sustained-release microcapsule is characterized in that: the chitosan coated gibberellin sustained-release microcapsule is obtained by coating gibberellin with chitosan.
2. The chitosan-coated gibberellin sustained-release microcapsule according to claim 1, wherein: the molecular weight of the chitosan is 100-500kDa, and the deacetylation degree is 60-99 percent.
3. The chitosan-coated gibberellin sustained-release microcapsule according to claim 2, wherein: the mass ratio of the gibberellin to the chitosan is 1: 16-100.
4. The chitosan-coated gibberellin sustained-release microcapsule according to claim 3, wherein: the grain diameter of the chitosan-coated gibberellin sustained-release microcapsule is 0.5-20 mu m.
5. A process for preparing a chitosan-coated gibberellin sustained-release microcapsule as claimed in claim 1, 2, 3 or 4, wherein: the preparation method comprises the following steps:
adding the gibberellin solution into an acetic acid aqueous solution of chitosan to obtain a gibberellin emulsion;
and (3) spray drying the gibberellin emulsion to obtain the chitosan coated gibberellin sustained-release microcapsule.
6. The method of claim 5, wherein: the concentration of gibberellin in the gibberellin solution is 0.5-50 mg/mL;
the concentration of the surfactant in the gibberellin solution is 0-40 mg/mL;
the surfactant is at least one of tween 20, tween 40, tween 60, tween 80, lecithin, polyoxyethylene 400 monolaurate, polyoxyethylene 400 monostearate and polyoxyethylene 400 monooleate;
the solvent in the gibberellin solution is methanol, ethanol or ethyl acetate.
7. The method of claim 6, wherein: the concentration of chitosan in the acetic acid aqueous solution of chitosan is 0.5-20 mg/mL;
the mass percentage concentration of the glacial acetic acid in the acetic acid aqueous solution is 0.2-2%.
8. The method of claim 7, wherein: the volume ratio of the gibberellin solution to the acetic acid aqueous solution of chitosan is 1: 1-4.
9. The method of claim 8, wherein: the air inlet temperature of the spray drying is 180-200 ℃, and the air outlet temperature is 70-100 ℃.
CN201911261384.1A 2019-12-10 2019-12-10 Chitosan-coated gibberellin sustained-release microcapsule and preparation method thereof Pending CN112931498A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080111389A (en) * 2007-06-18 2008-12-23 연세대학교 산학협력단 Sustained-release chitosan capsules comprising chitosan and phytic acid
CN101574083A (en) * 2009-06-19 2009-11-11 北京化工大学 Preparation methods of sustained-release microcapsule and sustained-release composite membrane for inhibiting monilinia fructicola
CN101773118A (en) * 2010-02-11 2010-07-14 中国农业大学 N,N-dimethyl piper-ridinium chloride sustained-release microcapsules and preparation method thereof
CN105613539A (en) * 2014-11-05 2016-06-01 江苏龙灯化学有限公司 Active component composition
CN108077251A (en) * 2017-05-23 2018-05-29 华东理工大学 A kind of chitosan/Lauxite monoshell layer slow-release microcapsule and preparation method thereof
CN109953020A (en) * 2017-12-14 2019-07-02 中国科学院大连化学物理研究所 A kind of Chitosan-coated Fluoxastrobin nanosphere and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080111389A (en) * 2007-06-18 2008-12-23 연세대학교 산학협력단 Sustained-release chitosan capsules comprising chitosan and phytic acid
CN101574083A (en) * 2009-06-19 2009-11-11 北京化工大学 Preparation methods of sustained-release microcapsule and sustained-release composite membrane for inhibiting monilinia fructicola
CN101773118A (en) * 2010-02-11 2010-07-14 中国农业大学 N,N-dimethyl piper-ridinium chloride sustained-release microcapsules and preparation method thereof
CN105613539A (en) * 2014-11-05 2016-06-01 江苏龙灯化学有限公司 Active component composition
CN108077251A (en) * 2017-05-23 2018-05-29 华东理工大学 A kind of chitosan/Lauxite monoshell layer slow-release microcapsule and preparation method thereof
CN109953020A (en) * 2017-12-14 2019-07-02 中国科学院大连化学物理研究所 A kind of Chitosan-coated Fluoxastrobin nanosphere and preparation method thereof

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Application publication date: 20210611