CN112889815A - Sodium alginate insect sex pheromone microcapsule and preparation method thereof - Google Patents
Sodium alginate insect sex pheromone microcapsule and preparation method thereof Download PDFInfo
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- CN112889815A CN112889815A CN202110017718.1A CN202110017718A CN112889815A CN 112889815 A CN112889815 A CN 112889815A CN 202110017718 A CN202110017718 A CN 202110017718A CN 112889815 A CN112889815 A CN 112889815A
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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
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/02—Acyclic compounds
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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
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
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Abstract
The invention relates to the technical field of biological pesticides, in particular to a sodium alginate insect sex pheromone microcapsule and a preparation method thereof, wherein the preparation method of the sodium alginate insect sex pheromone microcapsule comprises the following steps: uniformly mixing insect sex pheromone, sodium alginate solution, weak acid, volatile alkali and calcium salt to form mixed solution; and then the mixed solution is subjected to spray drying to prepare the spray-dried microcapsule. The preparation method of the sodium alginate insect sex pheromone microcapsule is safe and environment-friendly, can control the constant release of the pheromone and keep longer action time, is convenient to implement, has strong specificity and simple preparation process, can be produced in large scale and is convenient to popularize.
Description
Technical Field
The invention relates to the technical field of biological pesticides, in particular to a sodium alginate insect sex pheromone microcapsule and a preparation method thereof.
Background
The insect sex pheromone receiving system has high specificity and specificity, plays an important role in interspecific reproductive isolation, and can make directional flight, winging, copulation and other behaviors after receiving the sex pheromone. Thousands of chemical structures of insect sex pheromones have been identified, and hundreds of species have been commercially produced.
The method for monitoring the pests comprises black light trapping and killing, direct egg searching, insect condition observation and the like, the sex attractant has the characteristics of high sensitivity, simplicity and convenience in use and the like, and the insect condition is monitored by utilizing insect sex pheromones, so that the method is an effective method and is generally accepted by people. The sex pheromone is used for trapping pests, so that the occurrence period, the damage degree, the distribution condition and the like of the pests can be predicted, the dynamic occurrence rule of the insect population is known, the chemical prevention and control are conveniently guided, other control measures are timely and effectively adopted, and the waste of manpower and material resources caused by blind prevention and control is avoided.
The sex pheromone can be released from various carriers, such as rubber plugs, polyethylene tubes, microcapsules, paraffin carriers and the like. The microcapsule is an ideal dosage form, because the insect sex pheromone microcapsule is simple and convenient in preparation process, and the active ingredients are sealed in the capsule wall, the diffusion of pheromone is limited, the illumination, the air and the moisture are isolated, the oxidation and decomposition speed of the active ingredients is reduced, and the constant release of the pheromone can be controlled and the long action time can be kept; meanwhile, the sex pheromone microcapsule can be applied by adopting a traditional medicine applying instrument, so that the manual input is reduced, and the flexibility of regulating and controlling the medicine applying speed and times is increased.
However, the microcapsule for sex pheromone in the prior art has the problems of easy environmental pollution, high price, complex preparation process and/or unstable and continuous release of sex pheromone, and can not well control pests, thereby bringing inconvenience to use.
Disclosure of Invention
In order to solve the technical problems, the invention provides an insect virus and sex pheromone microcapsule and a preparation method thereof.
In order to realize the technical effect of the invention, the following technical scheme is adopted for realizing the technical effect:
a preparation method of sodium alginate insect sex pheromone microcapsules comprises the following steps:
uniformly mixing insect sex pheromone, sodium alginate solution, weak acid, volatile alkali and calcium salt to form mixed solution; and then the mixed solution is subjected to spray drying to prepare the spray-dried microcapsule.
As a further improvement, the preparation method comprises the following steps:
the method comprises the following steps: uniformly mixing insect sex pheromone and sodium alginate solution to form a mixture A;
step two: uniformly mixing the mixture A, weak acid, volatile alkali and calcium salt to form a mixed solution B;
step three: and carrying out spray drying on the mixed solution B to prepare the spray-dried microcapsule.
As a further improvement, the pH value of the mixed solution is 5.0-6.5; the weak acid is succinic acid; the calcium salt is insoluble in the mixed solution and is dissolved along with the volatilization of the volatile alkali in the spray drying process; the volatile alkali is ammonium hydroxide; the sodium alginate solution is a sodium alginate aqueous solution; the weak acid, volatile base and calcium salt are mixed with the insect sex pheromone and sodium alginate solution in the form of weak acid solution, volatile base solution and calcium salt solution.
As a further improvement, the insect sex pheromone is prodenia litura sex pheromone and/or beet armyworm pheromone; the insect sex pheromone is mixed with a sodium alginate solution, a weak acid, a volatile alkali and a calcium salt in the form of an insect sex pheromone solution; the solvent used for dissolving the insect sex pheromone in the insect sex pheromone solution is an organic solvent, and the organic solvent is one or more of N-hexane, ethanol, cyclohexanone, cyclohexanol, N-dimethyl phthalein amine, toluene and xylene; the mass ratio of the insect sex pheromone to the organic solvent is 1: (0.1-5); the calcium salt is calcium hydrogen phosphate.
As a further improvement, the sex pheromone of the prodenia litura is cis 9-trans 11-tetradecenol acetate and cis 9-trans 12-tetradecenol acetate; the beet armyworm sex pheromone: cis-9, trans-12-tetradecadienol acetate, cis-9-tetradecenol, and cis-11-hexadecenol acetate.
As a further improvement, the mass ratio of the insect sex pheromone to the sodium alginate to the weak acid to the calcium salt is as follows: 110 (2-10) x 106：(0.5-2)×106: a number of 0 or more and 0.5 or less times 106。
As a further improvement, the mixed solution is subjected to spray drying to prepare the spray-dried microcapsule: sucking the mixture by a peristaltic pump of the spray drying device, and atomizing the mixture by a nozzle of the spray drying device to obtain spray-dried microcapsules; the spray-dried microcapsules are in powder form; the mass ratio of the cis 9-trans 11-tetradecenol acetate to the cis 9-trans 12-tetradecenol acetate is 10: 1; the cis-9, trans-12-tetradecadienol acetate, cis-9-tetradecenol and cis-11-hexadecenol acetate are 7:3: 1.
As a further improvement, the weak acid, volatile base and calcium salt are mixed with the insect sex pheromone and sodium alginate solution in the form of a succinic acid solution, a volatile base solution and a calcium hydrogen phosphate solution; the mass fraction of the sodium alginate solution is 1-5%; the succinic acid solution accounts for 0.5-2% by mass, and the calcium hydrogen phosphate accounts for less than 0.5% by mass.
As a further improvement, the liquid suction speed of the peristaltic pump is 2.5-6mL/min, the inner diameter of the spray head is 0.5mm, and the inlet temperature of the peristaltic pump of the spray drying device is 120-160 ℃.
The invention also provides a sodium alginate insect sex pheromone microcapsule which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1) the preparation method of the sodium alginate insect sex pheromone microcapsule can be applied to control insects such as prodenia litura and beet armyworm, is safe and environment-friendly, can control constant release of pheromone and keep longer action time, is convenient to implement, has strong specificity, can be produced in large scale and is convenient to popularize.
2) The preparation method is simple. Compared with the prior art which needs a two-step method of preparing the microcapsule first and then carrying out spray drying, the method saves the operation steps.
3) The invention adopts raw materials, has low price and easily obtained raw materials.
Detailed Description
A preparation method of sodium alginate insect sex pheromone microcapsules comprises the following steps:
uniformly mixing insect sex pheromone, sodium alginate solution, weak acid, volatile alkali and calcium salt to form mixed solution; and then the mixed solution is subjected to spray drying to prepare the spray-dried microcapsule.
May be a method comprising the steps of:
the method comprises the following steps: uniformly mixing insect sex pheromone and sodium alginate solution to form a mixture A;
step two: uniformly mixing the mixture A, weak acid, volatile alkali and calcium salt to form a mixed solution B;
step three: and carrying out spray drying on the mixed solution B to prepare the spray-dried microcapsule.
Preferably, the preparation method comprises the following steps:
the method comprises the following steps: adding insect sex pheromone into sodium alginate solution, and stirring and mixing uniformly to form a mixture A;
step two: adding weak acid, volatile alkali and calcium salt into the mixture A, and stirring and mixing uniformly to form a mixed solution B;
step three: and carrying out spray drying on the mixed solution B to prepare the spray-dried microcapsule.
Preferably, the pH value of the mixed solution B is 5.0-6.5; the weak acid is succinic acid; the calcium salt is insoluble in the mixed solution (or the mixed solution B) and is dissolved along with the volatilization of the volatile alkali in the spray drying process; the volatile alkali is ammonium hydroxide.
The volatile base may be ammonium hydroxide, and the succinic acid, ammonium hydroxide and calcium hydrogen phosphate added in step two may be added in the form of an aqueous solution of succinic acid, an aqueous solution of ammonium hydroxide and an aqueous solution of calcium hydrogen phosphate, respectively.
Preferably, the insect sex pheromone is prodenia litura sex pheromone and/or beet armyworm pheromone; the insect sex pheromone is added into a sodium alginate solution in the form of an insect sex pheromone solution, a solvent used for dissolving the insect sex pheromone in the insect sex pheromone solution is an organic solvent, and the organic solvent is one or more of N-hexane, ethanol, cyclohexanone, cyclohexanol, N-dimethyl phthalein amine, toluene and xylene; the mass ratio of the insect sex pheromone to the organic solvent is 1: (0.1-5); the calcium salt is calcium hydrogen phosphate.
Alginate is an attractive matrix for microencapsulation of various foods, goods for agricultural and pharmaceutical applications. This material is natural and relatively low cost.
Sodium alginate is derived from brown algae, is a negatively charged polysaccharide, and is a linear polyanionic high polymer formed by beta-D-mannuronic acid (M) and alpha-L-guluronic acid (G) through beta- (1,4) glycosidic bonds. Crosslinking of adjacent polymer chains is induced by electrostatic interaction with divalent cations (e.g., calcium) that fit tightly between the polygulonate regions (G blocks) on adjacent alginate chains, forming an "egg-box" structure.
As an alternative to the traditional methods of alginate bead production, the manufacturing process of the present invention is a simplified process that combines multiple sequential unit operations into one spray drying step. The suspension entering from the inlet of the spray drying apparatus comprises alginate, an insoluble calcium salt, a weak acid and a volatile base for neutralising the acid to a pH at which the calcium salt is insoluble. The cross-linking of alginate takes place during the spray-drying process: after atomization of the suspension, the evaporation of the base acidifies the droplets and the calcium salt dissolves, so that the alginate becomes droplets by ion-mediated crosslinking, and crosslinked alginate microcapsules (CLAM) can be collected in the form of a dry powder at the outlet of the spray-drying apparatus.
The present invention will be further described with reference to the following examples.
It should be noted that the raw materials used in the technical scheme provided by the present invention, except for the specific description, are prepared by conventional means or purchased through commercial channels.
Example 1
A preparation method of sodium alginate insect sex pheromone microcapsules comprises the following steps:
the method comprises the following steps: adding a solution containing 110 mu g of prodenia litura sex pheromone into 200g of a sodium alginate aqueous solution with the mass fraction of 2%, and stirring and mixing uniformly to form a mixture A;
step two: adding 100g of succinic acid aqueous solution and 100g of calcium hydrogen phosphate aqueous solution into the mixture A, titrating the pH of the liquid to 5.6 by using ammonium hydroxide aqueous solution, and uniformly stirring and mixing to form a mixture B (suspension);
step three: and (4) carrying out spray drying on the whole mixed solution B to prepare the spray-dried microcapsule. Sucking the mixture B prepared in the second step by a peristaltic pump of a spray drying device, and atomizing the mixture B by a nozzle of the spray drying device to obtain the spray-dried microcapsules.
Can be as follows: and (3) sucking the mixture B by using a peristaltic pump of a spray dryer, wherein the sucking speed is 20% of the maximum sucking speed of the peristaltic pump, the dried microcapsules are collected from a spray head under the conditions that the inlet temperature of the peristaltic pump is 120-160 ℃, the air flow of the aspirator of the spray dryer is set to be the maximum value, the inner diameter of the spray head of the spray dryer is 0.5mm, and the air flow of the spray head of the spray dryer is set to be two thirds of the maximum value, and the collected microcapsules are stored in a glass bottle in the dryer. The spray dryer is an instant SZ-2000 spray dryer in Shanghai. Sucking the mixture B by a peristaltic pump of the spray dryer, wherein the sucking speed can be as follows: 2.5-6 mL/min.
Examples 1-10 were prepared in the same manner (as described above for the examples), except that the concentrations of the aqueous sodium alginate solution, aqueous succinic acid solution, and aqueous calcium hydrogen phosphate solution were varied, and the concentrations of the respective solutions used in the specific examples are shown in Table 1.
TABLE 1
In Table 1, the concentration (%) of the aqueous solution of calcium hydrogen phosphate was 0, meaning that no calcium hydrogen phosphate solution was added. Namely, the second step in the embodiment 1 is: adding succinic acid solution into the mixture A, titrating the pH of the liquid to 5.6 by using ammonium hydroxide solution, and stirring and uniformly mixing to form a mixture B.
In step two of each example, the same results were obtained by titrating the pH of the solution to 5.0-6.5 with ammonium hydroxide solution.
In each embodiment, the insect sex pheromone is composed of cis-9-trans-11-tetradecenol acetate and cis-9-trans-12-tetradecenol acetate according to the mass ratio of 10: 1. Of course other pheromones are possible.
In examples 1 to 12, the insect sex pheromone solution may be prepared by dissolving the insect sex pheromone in an organic solvent at a certain concentration, wherein the organic solvent is ethanol, and the mass ratio of the insect sex pheromone to the organic solvent is 1: 5.
Of course, the organic solvent used in the insect sex pheromone solution of the invention can be one or more of N-hexane, ethanol, cyclohexanone, cyclohexanol, N-dimethylphthalein amine, toluene and xylene as long as the insect sex pheromone can be dissolved. The mass ratio of the insect sex pheromone to the organic solvent can also be 1 (0.1-5).
Testing the attraction effect of sodium alginate insect sex pheromone microcapsules:
the samples were: sodium alginate insect sex pheromone microcapsules prepared in examples 1-12.
Placing each sample on the vegetable garden and other places where the prodenia litura often appears and causes harm in combination with the armyworm plates, placing three armyworm plates with the samples in each mu of land, placing one plate every 50 meters, and inspecting the prodenia litura on each armyworm plate after 30 days. The specific results are shown in table 1 below:
TABLE 2
| Examples | 1/insect sticking plate | 2/insect sticking plate | Insect sticking plate 3/insect sticking plate | Mean number of |
| Example 1 | 12 | 10 | 10 | 11 |
| Example 2 | 5 | 3 | 6 | 5 |
| Example 3 | 15 | 16 | 18 | 16 |
| Example 4 | 10 | 12 | 15 | 12 |
| Example 5 | 11 | 13 | 14 | 13 |
| Example 6 | 8 | 9 | 8 | 8 |
| Example 7 | 8 | 7 | 11 | 9 |
| Example 8 | 13 | 11 | 14 | 13 |
| Example 9 | 15 | 13 | 13 | 14 |
| Example 10 | 10 | 11 | 9 | 10 |
From the above table, it can be seen that: example 2 because no calcium hydrogen phosphate is added, the sodium alginate microcapsule is not crosslinked, which results in large pores on the wall material and fast release of the encapsulated pheromone. The prodenia litura can not be induced for a long time, and the prodenia litura adhered on the insect sticking plate is few; example 3 induces prodenia litura the most and sodium alginate is cross-linked with calcium ions to the greatest extent. The sodium alginate insect sex pheromone microcapsule can control the constant release of the sex pheromone and keep the action time longer. The insect sex pheromone can also be beet armyworm pheromone and other insect sex pheromones.
In experiments, it is found that if the sex pheromone of the prodenia litura in the examples 1 to 10 is changed into the sex pheromone of the beet armyworm (the sex pheromone of the beet armyworm can be cis-9, trans-12-tetradecenol acetate, cis-9-tetradecenol and cis-11-hexadecenol acetate according to the mass ratio of 7:3:1, the dosage is 1mg, the variety and the concentration of the solvent are the same), the sex pheromone attracting effect test is carried out by adopting the same preparation method and attracting method, and the result also has good attracting effect. For example, in examples 1 to 10, the sex pheromone of spodoptera litura is changed to the sex pheromone of beet armyworm, and the number of beet armyworm is induced as shown in Table 2; the example corresponding to example n after replacement was named example na, for example, example 1, and the example after replacing the prodenia litura sex pheromone with the beet armyworm sex pheromone is designated as example 1 a.
TABLE 3
| Examples | 1/insect sticking plate | 2/insect sticking plate | Insect sticking plate 3/insect sticking plate | Mean number of |
| Example 1a | 15 | 11 | 12 | 13 |
| Example 2a | 7 | 5 | 6 | 6 |
| Example 3a | 15 | 17 | 18 | 17 |
| Example 4a | 13 | 12 | 15 | 13 |
| Example 5a | 15 | 13 | 16 | 15 |
| Example 6a | 10 | 9 | 12 | 10 |
| Example 7a | 9 | 11 | 12 | 11 |
| Example 8a | 14 | 13 | 14 | 14 |
| Example 9a | 16 | 17 | 15 | 16 |
| Example 10a | 12 | 14 | 9 | 12 |
The preparation method can be well used for attracting the asparagus caterpillars.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (10)
1. A preparation method of sodium alginate insect sex pheromone microcapsules is characterized by comprising the following steps:
uniformly mixing insect sex pheromone, sodium alginate solution, weak acid, volatile alkali and calcium salt to form mixed solution; and then the mixed solution is subjected to spray drying to prepare the spray-dried microcapsule.
2. The method for preparing sodium alginate insect sex pheromone microcapsule according to claim 1, wherein the method comprises the following steps:
the method comprises the following steps: uniformly mixing insect sex pheromone and sodium alginate solution to form a mixture A;
step two: uniformly mixing the mixture A, weak acid, volatile alkali and calcium salt to form a mixed solution B;
step three: and carrying out spray drying on the mixed solution B to prepare the spray-dried microcapsule.
3. The method for preparing sodium alginate insect sex pheromone microcapsules according to claim 1, wherein the pH of the mixed solution is 5.0-6.5; the weak acid is succinic acid; the calcium salt is insoluble in the mixed solution and is dissolved along with the volatilization of the volatile alkali in the spray drying process; the volatile alkali is ammonium hydroxide; the sodium alginate solution is a sodium alginate aqueous solution; the weak acid, volatile base and calcium salt are mixed with the insect sex pheromone and sodium alginate solution in the form of weak acid solution, volatile base solution and calcium salt solution.
4. The preparation method of the sodium alginate insect sex pheromone microcapsule as claimed in claim 1, wherein the insect sex pheromone is prodenia litura sex pheromone and/or beet armyworm pheromone; the insect sex pheromone is mixed with a sodium alginate solution, a weak acid, a volatile alkali and a calcium salt in the form of an insect sex pheromone solution; the solvent used for dissolving the insect sex pheromone in the insect sex pheromone solution is an organic solvent, and the organic solvent is one or more of N-hexane, ethanol, cyclohexanone, cyclohexanol, N-dimethyl phthalein amine, toluene and xylene; the mass ratio of the insect sex pheromone to the organic solvent is 1: (0.1-5); the calcium salt is calcium hydrogen phosphate.
5. The method for preparing sodium alginate insect sex pheromone microcapsules according to claim 1, wherein the prodenia litura sex pheromone is cis 9-trans 11-tetradecenol acetate and cis 9-trans 12-tetradecenol acetate; the beet armyworm sex pheromone: cis-9, trans-12-tetradecadienol acetate, cis-9-tetradecenol, and cis-11-hexadecenol acetate.
6. The method for preparing the sodium alginate insect sex pheromone microcapsule according to claim 1, wherein the mass ratio of the insect sex pheromone to the sodium alginate to the weak acid to the calcium salt is as follows: 110 (2-10) x 106：(0.5-2)×106: a number of 0 or more and 0.5 or less times 106。
7. The method for preparing sodium alginate insect sex pheromone microcapsule according to claim 5, wherein the mixed solution is spray-dried, and the prepared spray-dried microcapsule is: sucking the mixture by a peristaltic pump of the spray drying device, and atomizing the mixture by a nozzle of the spray drying device to obtain spray-dried microcapsules; the spray-dried microcapsules are in powder form; the mass ratio of the cis 9-trans 11-tetradecenol acetate to the cis 9-trans 12-tetradecenol acetate is 10: 1; the cis-9, trans-12-tetradecadienol acetate, cis-9-tetradecenol and cis-11-hexadecenol acetate are 7:3: 1.
8. The method for preparing sodium alginate insect sex pheromone microcapsule according to claim 1, wherein the weak acid, the volatile alkali and the calcium salt are mixed with the insect sex pheromone and the sodium alginate solution in the form of succinic acid solution, volatile alkali solution and calcium hydrogen phosphate solution; the mass fraction of the sodium alginate solution is 1-5%; the succinic acid solution accounts for 0.5-2% by mass, and the calcium hydrogen phosphate accounts for less than 0.5% by mass.
9. The preparation method of the sodium alginate insect sex pheromone microcapsule as claimed in claim 7, wherein the liquid suction speed of a peristaltic pump is 2.5-6mL/min, the inner diameter of a spray head is 0.5mm, and the inlet temperature of the peristaltic pump of a spray drying device is 120-160 ℃.
10. The sodium alginate insect sex pheromone microcapsule according to any one of claims 1 to 9, wherein the sodium alginate insect sex pheromone microcapsule is prepared by the preparation method according to any one of claims 1 to 9.
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