KR100433790B1 - Sustained release preparation of preservative containing essential oil for agricultural products - Google Patents

Abstract

The present invention relates to a storage agricultural product quality preservative using natural vegetable essential oils as an active ingredient, and more particularly to a storage product quality preserving agent of a new formulation which sustains the effect of the vegetable essential oil as an active ingredient. In the present invention, a powdered microcapsule which microencapsulates a vegetable essential oil as an active ingredient into a water-soluble polymer; Provided is a new agricultural product quality preservation agent consisting of a solvent that dissolves the coating material of the microcapsule and slowly releases the vegetable essential oil contained therein. The solvent and the microcapsule are effectively packaged and contacted with each other upon use. By slowly releasing vegetable essential oil as a component, it will continue to exhibit bactericidal and insecticidal effects.

Description

SUSTAINED RELEASE PREPARATION OF PRESERVATIVE CONTAINING ESSENTIAL OIL FOR AGRICULTURAL PRODUCTS}

The present invention relates to a storage agricultural product quality preservative using natural vegetable essential oils as an active ingredient, and more particularly to a storage product quality preserving agent of a new formulation which sustains the effect of the vegetable essential oil as an active ingredient.

The main causes of the deterioration of the quality of grains such as rice are pests generated during storage, such as rice weevil, rice thief, and Hwaranggok moth. These pests multiply rapidly in rice bags or rice barrels, which not only eat nutrients and excrete in the rice, but also reduce the quality of rice by spreading mold on the body. In particular, when the humidity in the air increases, molds and bacteria such as yellowing microorganisms floating in the air will multiply in a rice bag or a rice barrel, thereby accelerating the deterioration of rice quality.

Moreover, as agricultural imports have been liberalized in recent years, foreign pests have been introduced into the country along with imported agricultural products, causing enormous damage. Therefore, in order to prevent pest damage, a fumigant such as methyl bromide (CH ₃ Br), aluminum phosphide, and chlorpicrin (Cl ₃ CNO ₂ ) is generally used to prevent pests from being distributed on a large scale such as imported agricultural products. However, these substances are not only toxic to the human body, but also cause environmental pollution problems such as destroying the ozone layer, thus requiring alternative materials that are safe for the human body and do not cause environmental pollution.

Recently, as a solution to this problem, attempts have been made to use natural substances such as vegetable essential oils, which are environmentally friendly and safe for humans, as pest control agents.

Looking at the patents related to the aromatic composition extracted from plants,

In US Pat. No. 4,455,304, Yarralian is an animal repellent composition using capsicum, describing a composition made from pepper and garlic extracts and a method of using the composition.

In US Pat. No. 4,440,783, Downing published a composition that uses isothiocyanate and lemon oil to chase animals such as raccoons and dogs from litter.

In International Patent No. 99/22751, Louis is a substitute for methyl bromide using a composition that selectively combines capsaicin, mustard oil (allyl isothiocyanate), ginger oil, lemon oil, and the like. It describes the use of soil treatments, pesticides, stored grains and building fumigators.

In addition, patents have been filed on food preservatives, films and the like using the antimicrobial effect of aryl isothiocyanate.

Regarding the preservation of the quality of stored grains such as rice, conventionally, folk remedies use garlic, pepper, and other spices in rice containers. However, by putting spices such as garlic and pepper directly, the control effect is not sufficient, and the ticks and molds attached to garlic or pepper may multiply, resulting in further deterioration of the quality of stored grains.

This folk remedy has been formulated with a mixture of red pepper and garlic essential oils. Japanese Patent Application Laid-open No. Hei 6-38678 uses spice ingredients of allicin and capsaicin in a breathable container of synthetic resin to be used as a rice preservative. Describes what to do. Rice quality preservatives using similar technologies are marketed by several companies in Korea.

However, as described above, formulations containing vegetable essential oils such as mustard oil, ginger oil, lemon oil, and the like as main ingredients have disadvantages that their effects are not sustained because the vegetable essential oils are volatile.

Therefore, in spite of the many advantages of storage oil-based preservatives containing vegetable essential oils, there are problems in practical use, and in the case of commercialization without solving these problems, the reliability of the product has recently been low. Quality preservatives based on vegetable essential oils are being ignored by consumers.

The present invention is to solve the above problems, an object of the present invention is to gradually release the vegetable essential oil as an active ingredient in the formulation to sustain the sterilization and insecticidal effect of the formulation for a long time, the volatile vegetable essential oil components in the distribution process It is to provide a preservative product quality preservative of a new formulation that can be prevented from being lost.

In addition, the present invention provides a formulation comprising a fast-acting portion to release a sufficient amount of the active ingredient at the beginning of use to quickly exhibit the bactericidal / insecticidal effect.

Other objects and advantages of the invention will be described below, and will be better understood by practice of the invention.

Figure 1 shows one preferred embodiment of a formulation comprising a powdered microcapsules and a solvent thereof.

2 shows a cross-sectional view of FIG. 1.

<Explanation of symbols for the main parts of the drawings>

10 powdered microcapsules 11 breathable pack

20 solvent 21 sealing pack

In order to achieve the above object, in the present invention, the powdered microcapsules (10) obtained by emulsifying, crosslinking and spray-drying a vegetable essential oil having a sterilizing and insecticidal effect with a polymer aqueous solution; In the sustained preparation consisting of a solvent (20) for dissolving the vegetable essential oil contained in the microcapsules by dissolving the water-soluble polymer, the polymer is a starch or a mixture of starch and other water-soluble polymer, wherein the solvent is water and polyethylene glycol It is a mixed solution of, The solvent 20 is accommodated in the sealing pack 21, the sealing pack 21 and the powdered microcapsules 10 is a double packaging structure is accommodated in the pack 11 of the breathable material again And a sustained preparation of the storage agricultural product quality preservative, wherein the solvent and the microcapsule are brought into contact with each other by rupturing the sealing pack 21 containing the solvent when in use.

In one embodiment of the present invention, the solvent comprises a certain amount of vegetable essential oil in the extraction stock state as a fast-acting portion for the initial sterilization, insecticide effect. In this case, when the packaging of the solvent ruptures, the vegetable essential oil contained in the solvent flows out to exert its initial sterilization and insecticidal effect, and then the continuous sterilization and insecticide effect gradually dissolves the powdered microcapsules by the spilled solvent. As a result, the vegetable essential oil contained in the capsule is released and exerted.

Hereinafter, the present invention will be described in detail.

In the present invention, first, a water-soluble polymer as a coating material is microencapsulated vegetable essential oil (essential oil) as an active ingredient.

The vegetable essential oil can be used if it is a vegetable extract having a bactericidal and insecticidal effect known to be used as a quality preservative of a stored agricultural product and the same. For example, mustard oil (allyl isothiocyanate), lemon oil, citronella oil, orange oil, mandarin oil, orange terpine, citrus terpine, lemon terpine, lime terpine, ginger essential oil, thyme extract, capsicum extract (capsaicin), garlic Extracts (allysine) and the like can be used alone or in combination of two or more. In one embodiment of the present invention is used horseradish extract with allyl isothiocyanate as an active ingredient.

As the water-soluble polymer, starch, gelatin, dextran, chitosan, etc. may be used alone or in combination. In one embodiment of the present invention, starch is used as the coating material.

The process of microencapsulating vegetable essential oils using starch as a coating material comprises: (1) preparing a starch aqueous solution by dissolving food starch in water; (2) emulsifying and adding vegetable essential oil having a bactericidal and insecticidal effect to the aqueous solution of starch obtained in the step; (3) preparing a microcapsule slurry in a solution state by putting crosslinked glutaraldehyde as a crosslinking agent in the emulsion obtained in the above step; (4) spray drying the microcapsule slurry obtained in the above step to obtain a microcapsule in powder form.

Powdered microcapsules of vegetable essential oils obtained through the above process are dissolved in a water-soluble polymer (eg, starch), which is a coating material, by using a solvent to gradually release the vegetable essential oil, which is an active ingredient contained therein.

The solvent may be used as long as it dissolves the water-soluble polymer used as the coating material of the microcapsules. For example, water, glycol, glycerin, propylene glycol, polyethyleneglycol (hydroxylamine), aminoalcohol, etc. may be used alone or in combination. Can be used. In one embodiment of the present invention, a mixed solution of water and polyethylene glycol (PEG) is used as a solvent for the microcapsules containing starch as a coating material. At this time, the solvent should not harden over time, the preferred ratio of water and polyethylene glycol is 3: 7 to 0.1: 9.9, most preferably 1: 9. As a result, when the ratio of water and polyethylene glycol 1: 9, it showed a stable effect even for more than 60 days.

In addition, the solvent may include a certain amount of vegetable essential oil in the extraction stock state as a fast-acting portion for the initial sterilization, insecticide effect. The vegetable essential oil contained in the solvent is the same as the vegetable essential oil contained in the microcapsules, and is contained in an amount sufficient for the initial effect expression until the vegetable essential oil in the capsule is released and exerts its effect. Although not particularly limited, the vegetable essential oil contained in the fast-acting portion is preferably included in the range of 0.1 to 40% by weight of the solvent.

In the formulation of the present invention, the powdered microcapsules and the solvent are separately packaged. Thus, the powdered microcapsules may be distributed in a separated state to minimize the loss of the active ingredient in the distribution process, and in use, the solvent may be added to the powdered microcapsules. As a result, the vegetable essential oil, which is an active ingredient, is slowly released into the preparation.

Figure 1 shows one preferred embodiment of a formulation comprising a powdered microcapsules and a solvent thereof. 1, the liquid solvent 20 is contained in a sealing pack 21 of a non-breathable material, which is again contained in a pack 11 made of a breathable nonwoven fabric together with the powdered microcapsules 10. do. In such a double packaging form, the solvent 20 and the powdered microcapsule 20 are brought into contact with each other by rupturing the sealed packaging 21 of the solvent inside by applying pressure from the outside during use. 2 shows a cross-sectional view of FIG. 1.

The double packaging illustrated above is just one embodiment, and the powdered microcapsule and its solvent may be packaged in various forms and provided to the consumer. The formulation of the present invention may be any form that can be added to the powdered microcapsule by finally opening the sealed solvent or rupturing the sealed packaging of the solvent when the consumer installs the preparation into a rice container or the like.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, the scope of the present invention is not limited by the following examples, and those skilled in the art to which the present invention pertains should be within the equivalent scope of the technical concept of the present invention and the claims to be described below. Of course, various modifications and variations are possible.

Example 1

Preparation of Microcapsules

1) Dissolve 40 g of food starch (substitution rate 0.005) substituted with n-octenyl in 60 g of water, and add 1 g of NaCl to increase the density of starch. A starch aqueous solution was prepared.

2) 7 g of horseradish extract (allyl isothiocyanate) having a bactericidal and insecticidal effect was added to the 40% starch aqueous solution obtained in step 1), and the mixture was rapidly stirred at 6,000 rpm for 7 minutes by a homogenizer. The emulsion was emulsified in order to obtain particles of uniform and small size.

3) 0.4 g of glutaraldehyde serving as a crosslinking agent was added to the mixed emulsion obtained in step 2) and crosslinked at 6,000 rpm for 10 minutes.

4) The microcapsules solution obtained in step 3) was introduced into a spray drying process to obtain microcapsules in powder form.

Example 2

The microcapsules obtained in Example 1; An aqueous solution of 9: 1 polyethylene glycol (PEG) and water was prepared as a solvent of the microcapsules, and the dosages were varied to prepare the formulations as follows.

1) Prescription 1

2.5 g of microcapsules were put in a nonwoven fabric, and 5 g of an aqueous solution of PEG and water in a 9: 1 mixture was injected into the nonwoven fabric.

2) Prescription 2

5 g of microcapsules were placed in a nonwoven fabric, and 10 g of an aqueous solution of 9: 1 PEG and water was injected into the nonwoven fabric.

3) Prescription 3

10 g of microcapsules were placed in a nonwoven fabric, and 20 g of an aqueous solution of 9: 1 PEG and water was injected into the nonwoven fabric.

4) Prescription 4

20 g of the microcapsules were placed in a nonwoven fabric, and 40 g of an aqueous solution of 9: 1 PEG and water was injected into the nonwoven fabric.

Experimental Example 1

Effect of Microcapsules on the Treatment of Rice Weevil

This experiment was carried out as follows to compare the effects of microcapsules treatment on rice weevil larvae and larvae. Experimental method was inoculated 10kg of rice weevil containing eggs and larvae of rice weevil in 30L plastic container and inoculated 100 adults each and treated each of Formulations 1 to 4 of Example 2 and examined the fighting effect every 10 days. . The results are shown in Table 1 below.

Prescription Eradication rate (%) 10 days later 20 days later 30 days later 40 days later One 46.8 48.6 0 0 2 78.7 40.5 30.6 0 3 100 86.5 88.9 91.4 4 100 100 100 100

As shown in Table 1, the prescription using more than 10g of the microcapsule was found to be excellent in combating rice weevil.

Example 3

The microcapsules obtained in Example 1; Differently prepared solvents for the microcapsules were prepared as follows.

1) Prescription 5

5 g of microcapsules were placed in a nonwoven fabric, and 10 g of water was injected into the nonwoven fabric as a solvent.

2) Prescription 6

5 g of microcapsules were put in a nonwoven fabric, and 10 g of PEG was injected into the nonwoven fabric as a solvent.

3) Prescription 7

5 g of the microcapsules were put in a nonwoven fabric, and 10 g of an aqueous solution in which PEG and water were mixed 9: 1 as a solvent was injected into the nonwoven fabric.

4) Prescription 8

5 g of the microcapsules were put in a nonwoven fabric, and 10 g of an aqueous solution obtained by mixing PEG and water 3: 1 as a solvent was injected into the nonwoven fabric.

5) Prescription 9

5 g of the microcapsules were placed in a nonwoven fabric, and 10 g of an aqueous solution in which PEG and water were mixed in a 1: 1 ratio was injected into the nonwoven fabric.

Experimental Example 2

Comparison of the Effect of Solvent on Rice Weevil

This experiment was carried out as follows to compare the effects of PEG and water on rice weevil larvae and larvae. 10 kg of rice containing eggs and larvae of rice weevil were inoculated into a 30 L plastic container, and 100 adult mice were inoculated. Each of Formulations 5 to 9 of Example 3 was treated, and the eradication effect was examined at 10-day intervals. The results are shown in Table 2 below.

Prescription Eradication rate (%) 10 days later 20 days later 30 days later 5 100 100 92.9 6 0 0 0 7 96.7 96.7 96.4 8 100 100 92.9 9 100 100 100

As a result of comparing the persistence effect of rice weevil according to the ratio of PEG and water, prescription 6 without water had no effect of rice weevil, but prescription 5, 7, 8, and 9 which contained more than 10% of water It was shown that the lasting effect of weevil eradication was excellent. However, Examples 5, 8, 9 containing 20% or more water showed physical properties that the microcapsules hardened with time.

Example 4

The microcapsules obtained in Example 1 were placed in a nonwoven fabric, and an aqueous solution and horseradish extract of 9: 1 mixed with polyethylene glycol (PEG) and water were put in a plastic bag, and then put in a nonwoven fabric, and the formulation was prepared as follows. Made.

1) Prescription 10

5 g of the microcapsules were put in a nonwoven fabric, and 8g of an aqueous solution of 0.3: 1 of PEG and water and 0.3g of horseradish extract were put in a plastic bag, and then put in a nonwoven fabric.

2) Prescription 11

5 g of the microcapsules were put in a nonwoven fabric, and 8 g of an aqueous solution containing 0.5 g of PEG and water and 0.5 g of horseradish extract were put in a plastic bag, and then placed in the nonwoven fabric.

3) Prescription 12

10 g of the microcapsules were put in a nonwoven fabric, and 15 g of an aqueous solution of 0.3 g of horseradish extract and 0.3 g of horseradish extract were separately added to a nonwoven fabric.

Comparative Example 1

2 g of horseradish extract and 8 g of PEG were added to a nonwoven fabric to form a liquid formulation.

Comparative Example 2

2 g of horseradish extract was impregnated into the ceramic and then placed in a nonwoven fabric to prepare a formulation impregnated with the ceramic.

Experimental Example 3

Comparison of Rice Weevil Mitigation Effect by Formulation

The formulations of Examples 10 to 12 and Comparative Examples 1 and 2 of Example 4 were tested in the following manner to compare the combating effects on adult rice larvae and larvae. In a 30L plastic container, 10kg of rice containing eggs and larvae of rice weevil was added and 100 adults were inoculated. Formulations 10-12 of Example 4 were processed after bursting the plastic bag, and Comparative Examples 1 and 2 were treated as they were. The elimination effect was investigated every 10 days, and the results are shown in Table 3 below.

Eradication rate (%) 10 days later 20 days later 30 days later 40 days later Prescription 10 100 100 100 53.1 Prescription 11 100 100 70.8 0 Prescription 12 100 100 100 82.2 Comparative Example 1 100 100 48.6 0 Comparative Example 2 20 15.9 0 0

As a result of the comparative test of the combating effect according to the formulation, Comparative Example 1 in which the horseradish extract was added to the nonwoven fabric in a liquid state was effective initially, but the effect was not sustained over time. Comparative Example 2 impregnated in was found to have little effect. However, the formulations 10 to 12, which are dual nonwoven formulations using the microcapsules of the present invention, have been shown to be excellent in combating and sustaining effects on rice weevil.

As confirmed by the above examples and experimental examples, the storage agricultural product quality preservative of the new formulation according to the present invention has a long-term disinfecting and insecticidal effect by slowly releasing the effect of vegetable essential oil as an active ingredient in the formulation. Will be maintained. Therefore, the formulation of the present invention provides a method for utilizing natural vegetable essential oils, which have been difficult to use due to the sustainability of the effect despite the safety and environmental friendliness of the human body, as a quality preservative of the stored agricultural products, and also effective in distribution. It also solves the problem of component loss.

Claims (7)

Powdered microcapsules (10) obtained by emulsifying, crosslinking and spray drying vegetable essential oils having a bactericidal and insecticidal effect with a polymer aqueous solution; In the long-acting formulation consisting of a solvent 20 for dissolving the water-soluble polymer to slowly release the vegetable essential oil contained in the microcapsules, The polymer is starch or a mixture of starch and other water-soluble polymers, wherein the solvent is a mixture of water and polyethylene glycol, The solvent 20 is accommodated in the sealing pack 21, the sealing pack 21 and the powdered microcapsules 10 has a double packaging structure is accommodated in the pack 11 of the breathable material again, A sustained preparation of a stored agricultural product preservative, characterized in that the solvent and the microcapsules are brought into contact with each other by rupturing the sealing pack (21) containing the solvent when in use. delete The sustained preparation according to claim 1, wherein the solvent contains a predetermined amount of the vegetable essential oil in an extract stock state for initial rapid effect expression. 4. The long-acting preparation according to claim 1 or 3, wherein the vegetable essential oil is mustard oil or horseradish extract containing allyl isothiocyanate as an active ingredient. delete delete 7. The long-acting formulation of claim 6, wherein the water and polyethylene glycol are mixed at a ratio of 1: 9.