CN111543427B - Enzyme response type controlled release pesticide and suspending agent and preparation method thereof - Google Patents
Enzyme response type controlled release pesticide and suspending agent and preparation method thereof Download PDFInfo
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- CN111543427B CN111543427B CN202010398830.XA CN202010398830A CN111543427B CN 111543427 B CN111543427 B CN 111543427B CN 202010398830 A CN202010398830 A CN 202010398830A CN 111543427 B CN111543427 B CN 111543427B
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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
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
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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
- A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Abstract
The invention discloses an enzyme response type controlled release pesticide, a suspending agent and a preparation method thereof, wherein the enzyme response type controlled release pesticide has a core-shell structure, takes an enzyme response type lignin-xylan nano composite microsphere as a wall material, and takes a pesticide embedded in the wall material as a core material; wherein the insecticide is a hydrophobic insecticide; the enzyme response type lignin-xylan nano composite microspheres adopt water-insoluble xylan as xylan, and adopt solvent-based lignin as lignin. The controlled-release pesticide can be controlled to release the pesticide by utilizing the hydrolysis of the xylanase, so that the controllable release of the pesticide on the surface of crops is realized, the action time of the pesticide is prolonged, and the utilization rate of the pesticide is improved.
Description
Technical Field
The invention relates to an insecticide, in particular to an enzyme response type controlled release insecticide, a suspending agent and a preparation method thereof.
Background
Pesticides are an important agricultural input for improving crop productivity and preventing major biological disasters. However, in actual use, more than 90% of the pesticide flows into the environment, which not only reduces the utilization rate of the pesticide, but also causes non-point source pollution to agriculture, and the excessive pesticide residue threatens food safety. Most of the active ingredients of the pesticide are water-insoluble organic compounds, and the active ingredients of the pesticide are required to be processed into a proper formula together with auxiliary ingredients such as a carrier, a solvent, an emulsifier, a dispersant and the like so as to be conveniently sprayed. In order to improve the dispersibility of the traditional pesticide preparation, a large amount of organic solvent is used, so that the environmental pollution is further caused.
Controlled release technology refers to the fact that the active ingredient in a particular system can be released to a particular target at a designed concentration and time and with a desired effect. The existing pesticide formulations are classified according to the release characteristics of active ingredients: free-release conventional dosage forms and controlled-release dosage forms. The controlled release formulation is an ideal pesticide formulation which can reduce the resistance problem, residue problem and environmental problem caused by pesticides due to the advantages of high safety, small dosage, low leaching property, long lasting period and the like. Therefore, the improvement of the dosage form of the existing pesticide to exert the controlled release function is an effective way to reduce the pesticide loss rate and improve the utilization rate.
At present, there are patents disclosing related technologies, specifically as follows:
(1) chinese patent CN106954627A discloses a method for preparing avermectin nano-silica controlled release agent, which adopts a miniemulsion method to mix, shear and emulsify pesticide avermectin, silica monomer, cross-linking agent and emulsifier to prepare miniemulsion, and the miniemulsion promotes hydrolytic crosslinking of the silica monomer by stirring to obtain nano-silica microcapsules. A series of nano-scale small droplets are formed by a fine emulsion method, so that solvent monomers, cross-linking agents and the like are hydrolyzed and cross-linked on the surfaces of the droplets, the pesticide is better coated, and the loading rate is increased. However, the nano silicon dioxide has high price and certain environmental toxicity, increases the environmental risk of pesticides, and has too complex preparation process compared with other pesticide formulations, thereby having difficulty in industrialization;
(2) chinese patent CN106818728A discloses a pesticide-carrying microsphere suspending agent prepared by self-assembly lignin-based materials and a method thereof, wherein abamectin wrapped by lignin-based microspheres with complete spherical structures can be obtained by self-assembly and hydrophobization of sodium lignosulfonate and cationic surfactant, the hydrophobic effect between a carrier and a pesticide is adjusted by adjusting the water content, and then the aggregation degree of the lignin and the pesticide of the carrier is adjusted to prepare the lignin-based pesticide-carrying microsphere suspending agent so as to achieve the effect of embedding the pesticide. The lignin-based pesticide microsphere suspending agent has a slow release effect, and has an effective protection effect on pesticides which are easy to photolyze. However, the self-assembly reaction process is not easy to control, chloroform with great harm is used as an organic phase solvent, and the self-assembly reaction process does not have the capability of controlling release under specific conditions.
Disclosure of Invention
The invention aims to provide an enzyme response type controlled-release pesticide, a suspending agent and a preparation method thereof, solves the problem of the utilization rate of the existing pesticide, can utilize xylanase hydrolysis to control the release of the pesticide, realizes the controllable release of the pesticide on the surfaces of crop leaves, prolongs the action time of the pesticide and improves the utilization rate of the pesticide.
In order to achieve the aim, the invention provides an enzyme-responsive controlled-release pesticide based on nano lignin, which has a core-shell structure, takes enzyme-responsive lignin-xylan nanocomposite microspheres as wall materials, and takes a pesticide embedded in the wall materials as a core material.
Wherein the insecticide is a hydrophobic insecticide; the enzyme response type lignin-xylan nano composite microspheres adopt water-insoluble xylan as xylan, and adopt solvent-based lignin as lignin.
Preferably, the solvent for extracting the solvent-based lignin is a eutectic solvent comprising: choline chloride eutectic solvent. Compared with other green solvents, such as ethanol/water, green liquor and solubilizing salts, the deep eutectic solvent has higher selectivity in extracting lignin and better maintains the polysaccharide component.
Preferably, the eutectic solvent is prepared from lactic acid and choline chloride in a molar ratio of (2-3): 1. More preferably, the lactic acid and choline chloride are formulated in a molar ratio of 2.5:1, and the resulting eutectic solvent has good lignin dissolving capacity and high thermal stability.
Preferably, the steam exploded lignocellulose and the eutectic solvent are heated and stirred at 130-190 ℃. More preferably, the steam exploded lignocellulose and the eutectic solvent are heated and stirred at 130 ℃, in which case the highest lignin selectivity and cellulose retention rate can be simultaneously obtained.
Preferably, the mass ratio of the wall material to the core material is 1: 1-5: 1; in the enzyme-responsive lignin-xylan nano composite microspheres, the mass ratio of lignin to xylan is 1: 3-3: 1.
Preferably, the hydrophobic insecticide is abamectin.
Preferably, the entrapment rate of the enzyme-responsive controlled-release pesticide is 51-90%, and the particle size is 150-250 nm.
Another object of the present invention is to provide a method for preparing the nano lignin-based enzyme-responsive controlled-release pesticide, which comprises:
dissolving solvent type lignin, water-insoluble xylan and an insecticide in a polar organic solvent, uniformly mixing, dialyzing in water under the condition of keeping out of the sun, wherein the molecular interception amount is 8000-14000, stopping dialysis until the polar organic solvent cannot be detected in the water, obtaining a nano composite microsphere dispersion, and removing water to obtain nano composite microspheres; wherein the polar organic solvent is capable of dissolving solvent-based lignin, water-insoluble xylan and a pesticide, comprising: any one of dimethyl sulfoxide, acetone and tetrahydrofuran.
Preferably, the polar organic solvent is dimethyl sulfoxide (DMSO), which has a solubility parameter δ (12.9) similar to that of most lignins and can be successfully recovered industrially.
Preferably, the solvent-based lignin is extracted by using a eutectic solvent and taking lignocellulose obtained by steam flash explosion treatment as a substrate.
Preferably, the preparation of the solvent-based lignin comprises the steps of heating and stirring lignocellulose obtained through steam flash explosion treatment and a eutectic solvent at 130 ℃, cooling the mixture to 75-85 ℃ after heating is finished, adding an acetone/water mixture, filtering, washing until the pH is neutral, standing the filtrate, removing the solvent to obtain the lignin, and filtering by using a nylon membrane to obtain the solvent-based lignin.
A nano-lignin based enzyme-responsive controlled-release pesticide suspension comprising: the nano lignin-based enzyme-responsive controlled-release pesticide and water.
The enzyme response type controlled release pesticide, the suspending agent and the preparation method thereof solve the problem of the utilization rate of the existing pesticide and have the following advantages:
(1) the enzyme response type controlled release pesticide has the particle size range of 150-250 nm, has smaller size and larger specific surface area, thereby having better dispersibility and utilization rate, and can effectively improve the efficacy and safety of pesticide by combining the modern nanotechnology and the controlled release pesticide, and promote the pesticide preparation to develop towards an environment-friendly direction;
(2) the enzyme-responsive controlled-release pesticide can respond to enzyme, can be hydrolyzed by xylanase to control release, and effectively overcomes the defects of unstable pesticide effect, high environmental risk, high economic cost and the like of the traditional pesticide controlled-release agent;
(3) according to the enzyme response type controlled release pesticide, the wall material is formed by the water-insoluble xylan and the solvent type lignin, a hydrophobic inner cavity is formed, the hydrophobic inner cavity is combined with the hydrophobic pesticide through hydrophobic interaction, so that the hydrophobic pesticide is embedded, on one hand, ultraviolet rays can be effectively shielded through phenolic hydroxyl on the surfaces of the lignin and xylan nanospheres, the ultraviolet degradation resistance of the pesticide is improved, the pesticide is protected, on the other hand, the nanospheres are coated to realize controlled release, and the prepared suspending agent is stable due to the large surface area and good dispersibility of the nanospheres;
(4) the enzyme response type controlled release pesticide has an obvious core-shell structure, the particle size range is 150-250 nm, the Zeta potential value is-35.333.26 mV, the stability is high, the encapsulation rate of the nano composite microspheres to the pesticide is 51% -90%, the pesticide active molecules can be released through xylanase hydrolysis, and the maximum release amount can reach about 93.1% after 7 days of enzyme hydrolysis;
(5) according to the preparation method, three raw materials are self-assembled simultaneously through a one-pot method, separation of intermediates is not needed, the reaction can be completed in one step, the nano composite microspheres wrapping the insecticide are formed, the hydrophobic part is self-assembled to form the core, the hydrophobic insecticide is combined with the core through the hydrophobic effect, and the hydrophilic part is self-assembled to form the colloidal particles, so that the preparation process is simple and efficient.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1
(1) Extraction of solvent-based lignin (DES lignin):
carrying out steam flash explosion treatment on poplar: 1kg of poplar was placed in a plastic bag and impregnated with a 0.7 wt% (based on dry wood weight) solution of dilute sulphuric acid in a solid to liquid ratio of 1:1 and left overnight at room temperature. The impregnated poplar samples were then transferred to a 2L digester and after steam flash explosion the resulting slurry was collected and filtered and the solid portion washed with 1L water and stored at 4 ℃ for future use.
DES pretreatment: adding steam flash exploded poplar and DES into a conical flask in a mass ratio of 1:20, continuously stirring and heating at 130 ℃ for 3h, cooling the reaction mixture to about 80 ℃, adding 30mL of acetone/water mixture (in a volume ratio of 50/50) to reduce the viscosity, filtering, washing the cellulose twice with 30mL of acetone/water mixture in order to remove residual choline chloride eutectic solvent and lignin in the cellulose component, washing the cellulose twice with hot water until the pH is neutral, collecting the filtrate and the washing solution, standing overnight, evaporating the acetone, precipitating the lignin component, filtering and washing with a nylon membrane with a pore diameter of 0.45 mu m, and finally freeze drying for later use.
(2) Extraction of water-insoluble xylan:
soaking 1kg of air-dried 60-mesh corn cob powder in 2.2L of 10% (w/w) sodium hydroxide solution, stirring at 100 deg.C for 2h, filtering while hot, neutralizing the filtrate with 5mol/L hydrochloric acid until pH is 7, centrifuging at 12000r/min for 5min, collecting the obtained xylan precipitate, washing with distilled water for three times, and freeze-drying the precipitate to obtain powdery water-insoluble xylan for later use.
(3) Preparing the nano composite microspheres:
dissolving 45g of solvent lignin in the step (1) and 60g of water-insoluble xylan (AVM) obtained in the step (2) and abamectin (AVM, which is a hydrophobic insecticide) in 600mL of dimethyl sulfoxide solution, uniformly mixing the solvent lignin, the water-insoluble xylan (AVM) and the Abamectin (AVM) by using a magnetic stirrer, dialyzing the solution system in tap water (periodically replacing the solution) under the condition of keeping out of the light because the AVM is easy to photolyze, stopping dialysis until no DMSO residue is detected in the wastewater, obtaining a nano composite microsphere dispersion, centrifuging for 15min by using a high-speed centrifuge of 12000r/min, removing most of water, and obtaining the nano composite microsphere precipitate.
(4) Preparation of enzyme-responsive controlled release pesticide suspensions:
and (4) adding water to dilute the nano composite microspheres prepared in the step (3) to 1L, and uniformly stirring to obtain the enzyme-responsive controlled-release pesticide based on the nano lignin.
Example 2
The amount of abamectin used in step (3) of example 1 was adjusted to 30g, and the other operation steps were the same as in example 1.
Example 3
The amount of the solvent-based lignin, the amount of the water-insoluble xylan and the amount of the avermectin in step (3) of example 1 were adjusted to 30g, 30g and 20g, respectively, and the other operation steps were the same as in example 1.
Example 4
The amount of solvent-based lignin, the amount of water-insoluble xylan and the amount of avermectin used in step (3) of example 1 were adjusted to 15g, 45g and 15g, respectively, and the other steps were the same as in example 1.
Example 5
The amount of solvent-based lignin, the amount of water-insoluble xylan and the amount of avermectin used in step (3) of example 1 were adjusted to 15g, 45g and 12g, respectively, and the other steps were the same as in example 1.
Example 6
The amount of abamectin used in step (3) of example 1 was adjusted to 15g, and the other operation steps were the same as in example 1.
Example 7
The amount of abamectin used in step (3) of example 4 was adjusted to 60g, and the other operation steps were the same as those of example 4.
TABLE 1 raw material usage for preparing nanocomposite microspheres according to examples 1-7 of the present invention
The performance indexes of the enzyme-responsive controlled-release insecticides prepared in examples 1 to 7 according to the present invention were measured, and the results are shown in table 2 below.
TABLE 2 Performance indices of the enzyme-responsive controlled-release insecticides of examples 1-7 of this invention
Note: zeta value is Zeta potential value; the ultraviolet degradation resistance is the activity retention degree of 24h under ultraviolet illumination.
As can be seen from the table above, the enzyme response type controlled release pesticide has an obvious core-shell structure, the particle size of the controlled release pesticide can be adjusted by adjusting the ratio of lignin to xylan, the particle size range is 150-250 nm, the Zeta potential value is about-35.33 +/-3.26 mV, and the controlled release pesticide has high stability. The encapsulation rate of the nano composite microspheres to the pesticide is 51% -90%, and the encapsulation rate of the controlled-release pesticide can be adjusted by adjusting the proportion of the wall material to the core material in the embodiment. The self-assembly process does not involve any chemical reaction, and the phenolic hydroxyl group of the solvent lignin is completely stored on the nano composite microsphere, so that the abundant phenolic hydroxyl group on the wall material can be used as an ultraviolet absorbent to protect the abamectin, and the compatibility and the uniformity of the wall material and the core material are high, so that the wall material is used as a barrier to prevent the abamectin from being photolyzed, and the nano sphere has obvious anti-ultraviolet degradation performance effect.
The drug release regulation and control method of the enzyme response type controlled release pesticide adopts 10 percent ethanol water solution (v/v) as a release medium, and adopts beech xylan with the protein concentration of 25mg/mL and 100000U/mL; the xylanase buffer solution was a 50mM citric acid-sodium citrate solution with pH 4.8. The specific enzyme response controlled release process is as follows:
7.5mL of the above buffer (50mM citric acid-sodium citrate solution at pH 4.8), 15.5mL of water, 100mL of the enzyme-responsive controlled-release insecticide, and 12mL of 2.5g/L of the above xylanase were slowly added in this order by a pipette, and the mixed solution was placed in a dialysis bag having a molecular weight of 1000; the dialysis bag was then placed in a quantity of the above-mentioned release medium and placed in a water bath shaker for release experiments. Setting the temperature of a shaking table to be 25-50 ℃ and setting the rotating speed to be 200 rpm; absorbing 1mL of release fluid from the outside of the dialysis bag at intervals, filtering the release fluid by a 0.45-micrometer pinhole filter, detecting the concentration of a sample by a liquid phase, and simultaneously supplementing 1mL of fresh release medium into a slow release system to ensure that the slow release volume is not changed.
Table 3 shows the release rates of the enzyme-responsive controlled-release insecticides of examples 1 to 7 of the present invention
Therefore, the enzyme response type controlled release pesticide has good enzyme controlled release capacity, and the controlled release performance of the controlled release pesticide can be controlled by adjusting the ratio of the wall material to the core material.
It should be noted that the experimental xylanase used in the drug release regulation method of the enzyme-responsive controlled-release pesticide of the invention is a medium-temperature xylanase, and the low-temperature xylanase can be used in practical application, so that the hydrolysis rate is higher at normal temperature; the invention evaluates the technical feasibility that the nano composite microspheres can achieve the controlled release of the pesticide through enzymatic hydrolysis, and has no specific limitation on xylanase.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (8)
1. An enzyme response type controlled release pesticide based on nano lignin is characterized in that the enzyme response type controlled release pesticide has a core-shell structure, takes enzyme response type lignin-xylan nano composite microspheres as a wall material, and takes a pesticide embedded in the wall material as a core material;
wherein the insecticide is a hydrophobic insecticide; the enzyme response type lignin-xylan nano composite microspheres adopt water-insoluble xylan as xylan, and adopt solvent-based lignin as lignin;
the solvent-based lignin extraction solvent is a eutectic solvent, the eutectic solvent is a choline chloride eutectic solvent, and the solvent-based lignin extraction solvent is prepared from lactic acid and choline chloride in a molar ratio of (2-3) to 1.
2. The nano lignin-based enzyme-responsive controlled-release pesticide according to claim 1, wherein the mass ratio of the wall material to the core material is 1: 1-5: 1; in the enzyme-responsive lignin-xylan nano composite microspheres, the mass ratio of lignin to xylan is 1: 3-3: 1.
3. The nano-lignin based enzyme-responsive controlled-release pesticide according to claim 1, wherein the hydrophobic pesticide is abamectin.
4. The nano-lignin-based enzyme-responsive controlled-release pesticide according to any one of claims 1 to 3, wherein the encapsulation efficiency of the enzyme-responsive controlled-release pesticide is 51 to 90%, and the particle size is 150nm to 250 nm.
5. A method for preparing the nano lignin-based enzyme-responsive controlled-release pesticide according to any one of claims 1 to 4, comprising:
dissolving solvent type lignin, water-insoluble xylan and an insecticide in a polar organic solvent, uniformly mixing, dialyzing in water under the condition of keeping out of the sun, wherein the molecular interception amount is 8000-14000, stopping dialysis until the polar organic solvent cannot be detected in the water, obtaining a nano composite microsphere dispersion, and removing water to obtain nano composite microspheres;
wherein the polar organic solvent can dissolve solvent lignin, water-insoluble xylan and pesticide, and is any one of dimethyl sulfoxide, acetone and tetrahydrofuran.
6. The method for preparing the nano-lignin based enzyme-responsive controlled-release pesticide as claimed in claim 5, wherein the solvent-based lignin is extracted from lignocellulose obtained by steam flash explosion treatment as a substrate by using a eutectic solvent.
7. The preparation method of the enzyme-responsive controlled-release pesticide based on the nano lignin as claimed in claim 6, wherein the preparation of the solvent-based lignin comprises the steps of heating and stirring lignocellulose obtained through steam flash explosion treatment and a eutectic solvent at 130-190 ℃, cooling a mixture to 75-85 ℃ after heating is finished, adding an acetone/water mixture, filtering, washing to neutral pH, standing a filtrate, removing the solvent to obtain the lignin, and filtering with a nylon membrane to obtain the solvent-based lignin.
8. A nano-lignin based enzyme-responsive controlled-release pesticide suspension comprising: the nano lignin-based enzyme-responsive controlled release pesticide according to any one of claims 1 to 4, and water.
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| US20100021551A1 (en) * | 2008-07-24 | 2010-01-28 | Food Industry Research And Development Institute | Process for preparing nanoparticles of chitosan in water phase |
| CN111053287A (en) * | 2020-01-07 | 2020-04-24 | 湖北中烟工业有限责任公司 | Method for preparing cigarette blasting beads by lignin-carbohydrate coated essence |
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| US20100021551A1 (en) * | 2008-07-24 | 2010-01-28 | Food Industry Research And Development Institute | Process for preparing nanoparticles of chitosan in water phase |
| CN111053287A (en) * | 2020-01-07 | 2020-04-24 | 湖北中烟工业有限责任公司 | Method for preparing cigarette blasting beads by lignin-carbohydrate coated essence |
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