KR20130089335A - Burst type lagged-release controlled composition and preparation method thereof - Google Patents

Abstract

PURPOSE: A burst type delay emission controlling composition is provided to emit a biological active component in the composition when a rainy season sets in whereby a biological active component can applied at an appropriate period. CONSTITUTION: A burst type delay emission controlling composition which as an initial emission delay characteristic includes a center part which has a water-expandable polymer and biological active components in the water-expandable polymer; and a peripheral part which is formed on the surface of the center part to surround the center part and is water-permeable. A manufacturing method of the delay emission controlling composition includes a step of adding acids into the water-expandable polymer to control the pH of the water-expandable polymer to 5.0-6.0, mixing the water-expandable polymer with a microbial cell, and freezing and drying the mixture to prepare the center part; and a step of spraying magnesium sulfate onto the center part and drying the same and spraying a peripheral part-forming solution to form the peripheral part. [Reference numerals] (AA) Dispersing; (BB) Moisture injection; (CC) Periphery; (DD) Biological vital component; (EE) Water swelling polymer

Description

Burst type delayed release control composition and a method for manufacturing the same {BURST TYPE LAGGED-RELEASE CONTROLLED COMPOSITION AND PREPARATION METHOD THEREOF}

A biologically active ingredient contained in a composition relates to a delayed release controlling composition wherein the biologically active ingredient is released at a time difference from the time of spreading as the environment in which the composition is spread.

In agricultural fields, it is necessary to control the timing of the active ingredient's active expression so that the effect is maintained for a long time by spraying an appropriate concentration of pesticides or fertilizers at one time, or the biologically active ingredient is released at a certain point of time or in a certain environment. It is requested. Although studies have been conducted on preparations for sustained release of active ingredients, time-released releases (or delayed releases) that are not sustained release, have no or minimal release of the active ingredient at the beginning of the application, and sudden release of the active ingredient occurs when certain circumstances arise. Slow release form) formulations are unknown. Methods of preparing sustained-release preparations include the preparation of the active substance in microcapsules, the inclusion of the active substance in cyclodextrins or the mixing with polymers, the active substance in the form of granules or powders, alone or in combination with additives, into particulate form. A method of coating the prepared particles with a resin or the like, a method of adsorbing an active substance to a porous carrier, and then coating the same has been proposed. As such, formulation studies for sustained release of active substances included in formulations have been made, but little studies have been conducted on time-released or delayed controlled release formulations that are not sustained release. If the formulation of formulations that can be released when a certain environment is reached, such as the rainy season, is achieved, it is convenient to pre-spray the formulations before they reach the rainy season and to attain the benefits of releasing the active substance at the appropriate time. There will be.

An initial release of the active substance provides a controlled release composition in which there is no or minimal release of the active substance and then release of the active substance when a specific environment arrives.

Burst-type delayed release control composition according to an embodiment of the present invention has an initial release inhibitory property, and the central portion and the central portion comprising a water-expandable polymer and a biologically active component contained in the water-expandable polymer The periphery is formed on the surface of the central portion to surround the permeable.

According to an embodiment of the present invention, a method of manufacturing a burst delayed controlled release composition may include adding acid to a water expandable polymer and adjusting the pH of the water expandable polymer to 5.0 to 6.0, and then adjusting the pH. Preparing a central portion by mixing the water-expandable polymer and the microbial cell and lyophilizing the same; Preparing a peripheral forming solution by irradiating gamma rays 1 to 15 kGy to a solution including sodium silicate; And after spraying and drying magnesium sulfate on the center portion, spraying the peripheral forming solution.

According to the present invention, after the burst type delayed release control composition is sprayed, the delayed release control composition maintains the shape of the central portion and the periphery surrounding the same in the dry season environment. Water is diffused into the water-expandable polymer in the center through the permeable periphery, and the volume of the water-expandable polymer in the center increases due to the diffusion of water, but when the periphery ruptures due to the pressure at the periphery of the periphery. The biologically active ingredient is finally released to the outside. When the supply of specific nutrients required for the rainy season or the supply of bactericidal components for pathogenic bacteria during the rainy season, the composition is sprayed before the rainy season to release the biologically active components inside the composition during the rainy season. By doing so, there is an effect of satisfying the convenience that the work can be performed in advance and the suitability that the biologically active ingredient can be operated at an appropriate time.

1 is a conceptual diagram of a burst type delayed release controlling composition having initial release control characteristics according to an embodiment of the present invention.
FIG. 2 is a photograph showing that the core of curdlan is swelled within 24 hours when the delayed release controlling composition according to Example 1 is observed after being placed in a beaker containing distilled water.
3 is a photograph of a composition prepared according to Comparative Example 2.

Burst-type delayed release control composition according to an embodiment of the present invention has an initial release inhibitory property, and the central portion and the central portion comprising a water-expandable polymer and a biologically active component contained in the water-expandable polymer The periphery is formed on the surface of the central portion to surround the permeable. Preferably, the central and peripheral portions of the delayed release controlling composition are biodegradable materials. The delayed release controlling composition is not limited in shape or size, and may have a spherical or polyhedral shape according to a manufacturing method, since the delayed release controlling composition has a structure surrounding a water-expandable polymer containing biologically active ingredients.

The water-expandable polymer included in the center of the composition may be a polymer derived from microorganisms, preferably a biodegradable material. As the water-expandable polymer, for example, curdlan which is a polysaccharide derived from a microorganism may be used. As the polymer, in addition to curdlan, cellulose, pullulan, gellan, zuglan, levan, xantan gum, starch, Alginic acid or chitosan may be used, and the biodegradable polymer may be used in combination of two or more.

Biologically active components that can be included in the water-expandable polymer include microorganisms. The microorganism may be Gram negative bacteria. Gram-negative bacteria, despite the advantages that can be utilized as a microbial pesticide bacteria, it was difficult to formulate a practical use as a pesticide formulation, but according to the burst delayed release control composition according to an embodiment of the present invention, Gram Negative bacteria maintain viability in the water-expandable polymer polymer contained in the center of the composition, and when introduced into the water environment after spraying the composition, the water-expandable polymer in the center through the permeable periphery in the water environment Moisture diffuses inside, and the volume of the water-expandable polymer in the center increases due to the diffusion of moisture, but when the periphery ruptures because the periphery ruptures and the periphery ruptures, the Gram-negative bacteria flows to the outside and becomes a microbial pesticide. Action. In addition to micro-organisms which can be included in the composition in accordance with one embodiment of the present invention are gram-negative bacteria, such as Burke holde Liao (Burkholderia), Pseudomonas (Psudomonas), janto Pseudomonas (Xanthomonas), and Bacillus (bacillus) and Streptomyces (Streptomyces) Also included are Gram-positive bacteria that can be used as microbial pesticides.

According to an embodiment of the present invention, a method of manufacturing a burst delayed controlled release composition may include adding acid to a water expandable polymer and adjusting the pH of the water expandable polymer to 5.0 to 6.0, and then adjusting the pH. Preparing a central portion by mixing the water-expandable polymer and the microbial cell and lyophilizing the same; Preparing a peripheral forming solution by irradiating gamma rays 1 to 15 kGy to a solution including sodium silicate; And after spraying and drying magnesium sulfate on the center portion, spraying the peripheral forming solution. The core preparation step and the preparation step of the peripheral portion forming solution may be reversed.

Hereinafter, the steps for preparing the central portion will be described. The water-expandable polymers forming the core include curdlan, cellulose, pullulan, gellan, zuglan, levan, xantan gum, Starch, alginic acid or chitosan may be used, and the biodegradable polymer may be used in combination of two or more. Acetic acid or citric acid may be used to adjust the pH of the water-expandable polymer forming the center portion, wherein the pH is 5.0 to 6.0, preferably 5.6 to 6.0. A microorganism which may be included in the center of the buck holde Liao (Burkholderia), Pseudomonas (Psudomonas), Bacillus (bacillus) or Pseudomonas janto (Xanthomonas) and is, as long as they can be used as microbial pesticides are not limited to the above-mentioned microorganism. The acid is added to the water-expandable polymer to adjust the pH of the water-expandable polymer, and then the microbial cells are mixed and lyophilized to prepare the core. Before mixing the microbe cells with the water-expandable polymer, The microbial cells can be centrifuged and preferably centrifuged at 2000 to 4000 rpm.

Hereinafter, the step of preparing the peripheral forming solution will be described. A solution containing sodium silicate and curdlan is prepared by irradiating gamma rays 1 to 15 kGy to prepare a periphery forming solution. More preferably, isopropyl alcohol is added before irradiating gamma rays to the periphery forming solution. Gamma irradiation is preferably 15 kGy or less. This is because if it exceeds 15 kGy, the peripheral portion as a coating film attached to the center portion is not formed but is formed as a separate skeleton. As for gamma irradiation dose, 3 kGy is especially preferable.

After spraying and drying magnesium sulfate at the center prepared as described above, the delayed release controlling composition according to the embodiment of the present invention may be prepared by spraying the peripheral forming solution. By spraying magnesium sulfate, it was confirmed that the peripheral forming solution was better attached to the center portion.

1 is a conceptual diagram of a burst type delayed release controlling composition having initial release control characteristics according to an embodiment of the present invention.

Referring to FIG. 1, there is shown a delayed release control composition in which a central portion includes a water-expandable polymer and a biologically active component included in the water-expandable polymer, and a coating film is formed as a periphery surrounding the center. After the composition is applied, the delayed release control composition maintains the shape of the central part and the peripheral part surrounding the same in the dry season environment, and when the water environment such as the rainy season becomes wet, the water-expandable polymer inside the central part through the permeable peripheral part As the water diffuses and the volume of the water-expandable polymer in the center increases due to the diffusion of water, the biologically active component is released to the outside when the periphery ruptures when the periphery ruptures. When the supply of specific nutrients required for the rainy season or the supply of bactericidal components for pathogenic bacteria during the rainy season, the composition is sprayed before the rainy season to release the biologically active components inside the composition during the rainy season. By doing so, there is an effect of satisfying the convenience that the work can be performed in advance and the suitability that the biologically active ingredient can be operated at an appropriate time.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by the following Examples.

Example

Example  One: Burst type  Preparation of Delayed Release Control Composition

(1) core manufacturing

After dissolving 0.00415 g of KOH and 0.13 g of curdlan in 10 mL of distilled water, 0.0039 mL of acetic acid was added to adjust the pH of the solution to 5.6 to 6.0. Burkholderia pyrrocinia ( Burkholderia pyrrocinia ) was centrifuged at 3000 rpm as a microbial cell, followed by mixing in a volume ratio of the centrifuged microbial cell to the solution at 1: 100, followed by lyophilization.

(2) peripheral manufacturing

After dissolving 5 g of sodium silicate and 2.5 g of curdlan in 480 mL of distilled water, 20 mL of isopropyl alcohol was added thereto, and then irradiated with gamma ray 3 kGy to prepare a coating solution as a peripheral forming solution.

(3) forming a periphery in the center

Burst-type delayed release control compositions were prepared by spraying MgSO 4 in the center and drying and then spraying the periphery forming solution.

Example  2

The preparation was carried out in the same manner as in Example 1, except that acetic acid was 0.039 mL in the preparation of the central portion.

Comparative example  One

Except that gamma-ray irradiation was 30 kGy in the periphery preparation was prepared in the same manner as in Example 1.

Comparative example  2

Except for the addition of isopropyl alcohol prior to gamma irradiation in the peripheral portion was prepared in the same manner as in Example 1.

Comparative example  3 to 8

Comparative Example 3 was prepared in the same manner as in Example 1, except that 0.415 g of potassium hydroxide was added in the preparation of the central portion, and 0.5 mL of phosphoric acid was added instead of acetic acid. The composition of Comparative Examples 3 to 8 in the production of the core is shown in Table 1 below.

center Curdlan (g) KOH (g) Acid (mL) Phosphoric Acid Acetic acid Comparative Example 3 0.13 0.415 0.5 0 Comparative Example 4 0.13 0.0415 0.05 0 Comparative Example 5 0.13 0.00415 0.005 0 Comparative Example 6 0.13 0.415 0 0.39 Comparative Example 7 0 0.415 0.5 0 Comparative Example 8 0 0.415 0 0.39

Delayed Release Control Evaluation

The delayed release control compositions prepared in Example 1, Comparative Example 1 and Comparative Example 2 were placed in a beaker containing distilled water, and then the swelling release of the core of the curdlan containing microorganisms was confirmed.

3 is a photograph showing that the core of curdlan was swelled within 24 hours after the delayed release controlling composition of Example 1 was placed in a beaker containing distilled water. Referring to FIG. 3, it can be seen that the central portion swelled out within 24 hours after the delayed release control composition was exposed to the water environment.

Figure 4 is a photograph of the composition prepared in Comparative Example 2. Referring to FIG. 4, when isopropyl alcohol is not added before gamma irradiation, the coating layer, which is a peripheral part, is not formed, and thus swelling itself. Through this, it can be seen that by adding isopropyl alcohol, the coating film, which is a peripheral portion, can be stably formed.

Microbial long-term survival assessment

Microorganism long-term survival was confirmed by the following method. After the core was prepared, the freeze-dried core was preserved at room temperature for 30 days or longer, and 20 μg of the core was inoculated on each plate to confirm colony formation.

In Examples 1 and 2 it was confirmed that the microorganisms survived for more than 30 days. On the other hand, in Comparative Examples 3 to 6 the microorganisms were killed within 7 days. In the case of Comparative Examples 7 and 8, no center was formed.

Claims (12)

A central portion comprising a water expandable polymer and a biologically active component contained within the water expandable polymer; And
A permeable periphery formed on the surface of the central portion to surround the central portion,
Burst type delayed release control composition having initial release inhibition properties.
The method of claim 1,
And the water-expandable polymer is a delayed release controlling composition.
The method of claim 1,
The water-expandable polymer is curdlan (cellulose), cellulose (cellulose), pullulan (gellu), gellan (zooglan), levan (levan), xantan gum, starch , At least one selected from the group consisting of alginic acid and chitosan.
The method of claim 1,
The biologically active ingredient is a microorganism, characterized in that the delayed release control composition.
5. The method of claim 4,
The microorganism Burke holde Liao (Burkholderia), Pseudomonas (Psudomonas), Bacillus (bacillus), Streptomyces (Streptomyces) and Pseudomonas janto (Xanthomonas) selected from the group consisting of a delay release-controlling composition.
Adding acid to the water-expandable polymer to adjust the pH of the water-expandable polymer to 5.0 to 6.0, and then mixing the pH-adjusted water-expandable polymer with microbial cells to freeze-dry to prepare a central portion;
Preparing a periphery forming solution by irradiating gamma rays 1 to 15 kGy to a solution containing sodium silicate and curdlan; And
Spraying and drying magnesium sulfate at the center, and forming a peripheral part by spraying the peripheral part solution;
A method of making a delayed release controlling composition.
The method according to claim 6,
The water-expandable polymer is curdlan (cellulose), cellulose (cellulose), pullulan (gellu), gellan (zooglan), levan (levan), xantan gum, starch (starch) , At least one selected from the group consisting of alginic acid and chitosan.
The method according to claim 6,
Wherein said acid is acetic acid or citric acid.
The method according to claim 6,
The microorganism is Burkholderia , Pseudomonas ( Psudomonas ), Bacillus ( bacillus ), Streptomyces ( Streptomyces ) and Xanthomonas ( Xanthomonas ) method for producing a controlled release composition.
The method according to claim 6,
The microbial cells are centrifuged prior to mixing the microbial cells with the water-expandable polymer.
The method according to claim 6,
Isopropyl alcohol is added to the periphery forming solution prior to irradiation with gamma rays.
The method according to claim 6,
Wherein the weight ratio of sodium silicate to curdlan in the step of preparing the peripheral forming solution is 2: 1.

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