JP2010222260A - Method for producing pest damage control material - Google Patents

Abstract

[PROBLEMS] To obtain an easy-to-use insect pest control material using bamboo peach.
SOLUTION: Bamboo peach leaves are mixed with methanol or the like and fractionated into an extracted fraction and a residue. The extracted fraction is mixed with chloroform or the like and fractionated into a hydrophobic fraction and a hydrophilic fraction. The hydrophilic fraction may be further mixed with butanols and the like to be fractionated into a medium polar fraction and a water-soluble fraction.
[Selection] Figure 1

Description

  The present invention relates to a method for producing an insect pest control material mainly composed of bamboo peach.

  The bamboo peach is an evergreen shrub native to India that is widely distributed in Japan. Various unique components exist in the leaves, stems, roots, etc. of the bamboo shoots, including toxic cardiac glycosides (oleandrin). For example, Patent Document 1 and Patent Document 2 are known as prior arts that have attempted to effectively use the bamboo shoot containing such a specific component.

  Patent Document 1 discloses a method for obtaining an extract effective for prevention of downy mildew. Specifically, branches and leaves of the bamboo peach are shredded, distilled water is added to each part of the shredded bamboo peach and heated and extracted under pressure. Alcohol and acetic acid are added as necessary. The extract is filtered and concentrated by heating to obtain an extract.

  Patent Document 2 discloses a method for obtaining an insecticidal fungicide that can be diluted and sprayed onto paddy fields. Specifically, green juice is produced by mixing the bamboo leaves and purified water with a mixer. The green juice is aged with bamboo vinegar, bittern, alcohol, etc. Insecticidal fungicides are obtained by filtering after aging.

JP 2007-137867 A JP 2008-050328 A

  Since bamboo peaches are widely used as street trees and horticultural plants, a large amount of pruning waste is generated during the pruning operation. This pruning waste is treated as waste and is directly incinerated. However, as described above, the bamboo peach contains a unique component that is not often found in other plants, so if it can be used effectively, waste can be reused as a resource.

  Although the bamboo peaches can be reused by the utilization methods of the above-mentioned Patent Document 1 and Patent Document 2, there is a disadvantage that the unique components contained in the bamboo peaches are not fully utilized.

  Therefore, the present inventors have conducted intensive studies focusing on the fact that the bamboo peach is less susceptible to pest damage than other plants, and as a result, the solution etc. obtained by subjecting the bamboo peach to a predetermined treatment are insecticidal. Thus, the present invention has been completed.

  That is, an object of the present invention is to provide an insect pest attack suppressing material that can effectively use the bamboo peach and is easy to use.

  The first method for producing an insect pest attack inhibiting material according to the present invention comprises mixing a bamboo peach leaf with a highly polar solvent to fractionate an extract fraction and a residue; A second fractionation step of mixing with a low-polar solvent and fractionating the solvent side into a hydrophobic fraction and a hydrophilic fraction.

  Here, pests mean small animals that harm crops, such as aphids, ticks, and ants, or that cause harm or discomfort to humans. It means a material that can act on such pests and suppress damage caused by such pests, such as effects or growth inhibition effects. In this production method, bamboo peach leaves are used as a raw material, but the flowers, stems, roots, and the like may be included.

  The highly polar solvent means a highly hydrophilic solvent. For example, pure water, pure methanol, a mixed solution of these water and methanol, or the like can be suitably used for the highly polar solvent. On the other hand, the low polarity solvent means a solvent having low hydrophilicity and high hydrophobicity, and for example, chloroform can be suitably used.

  Thus, by first fractionating the bamboo peach leaves with a highly polar solvent, many components contained in the bamboo peach can be extracted into the extracted fraction. Further, by fractionating the extracted fraction with a low polarity solvent, it is possible to further fractionate into the hydrophobic fraction on the low polarity solvent side and the other hydrophilic fraction of the extracted bamboo peach components. it can. In this way, by sequentially fractionating using solvents having greatly different polarities, a plurality of materials having different concentration balances of various components contained in the bamboo peach leaves can be taken out.

  As will be described in detail later, since each material obtained in this manner has an effect of insecticides against pests, it can be used alone or in combination depending on the purpose of use and conditions of use. Can be used as a repellent.

  Furthermore, it is possible to include a third fractionation step in which the hydrophilic fraction is mixed with a medium-polar solvent, distributed and extracted, and fractionated into a medium-polar fraction and a water-soluble fraction. It is preferable to use butanols (isobutanol, n-butanol, or a mixture thereof) as the medium polar solvent. The medium polarity solvent is a solvent having a polarity between a high polarity solvent and a low polarity solvent.

  By doing so, the water-soluble raw material which hardly contains oleandrin can be fractionated into a water-soluble fraction, and an insect pest attack suppressing material excellent in safety can be obtained.

  The second method for producing an insect pest attack inhibiting material according to the present invention comprises mixing a bamboo peach leaf with a highly polar solvent to fractionate an extract fraction and a residue; And an adsorption step for contacting the adsorbent. Examples of the adsorbent include adsorbent resin and activated carbon, and among them, activated carbon can be particularly preferably used.

  If it does so, since the predetermined | prescribed component contained in the bamboo peach leaf can be made to adsorb | suck to an adsorbent and a density | concentration balance can be changed like the 1st manufacturing method, it can utilize for an agrochemical etc. according to a use purpose. Since processing is simple, it is excellent in practicality. In particular, when activated carbon is used as an adsorbent, oleandrin, coloring components, and the like can be adsorbed and removed, so that a pest-damaging inhibitor that is easy and safe to use can be obtained.

  As described above, according to the present invention, it is possible to effectively use the bamboo peaches such as pruning scraps that are discarded in large quantities without waste, and to obtain an easy-to-use pest attack inhibitor that can be used properly according to the purpose. Can do.

It is a flowchart which shows the manufacturing process of 1st Embodiment. It is the table | surface which showed the test result of the Example. It is the table | surface which showed the test result of the Example. It is the table | surface which showed the test result of the Example. It is the table | surface which showed the test result of the Example. It is a flowchart which shows the manufacturing process of 2nd Embodiment. It is the table | surface which showed the test result of the Example.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. However, the following description is merely illustrative in nature and does not limit the present invention, its application, or its use.

-First embodiment-
In FIG. 1, an example of the manufacturing process of a pest attack suppression material is shown. First, the bamboo peach leaves are used as a raw material, and this is finely chopped with a mixer or the like. The bamboo peach leaves can be fresh or dry. Moreover, parts other than leaves, such as a flower, a stem, and a root, may be contained.

  The shredded bamboo peach leaves are extracted by mixing with a highly polar solvent such as methanol, water, or a mixed solution thereof (first fractionation process). The extraction temperature, extraction time, and extraction means can be appropriately set as necessary. For example, it may be left immersed for 2 to 3 hours at 40 ° C. to 75 ° C., or may be forcibly extracted in a short time using various extractors having a stirring function and a heating function. In short, it suffices if the components contained in the bamboo shoots can be sufficiently eluted in a highly polar solvent. After extraction, the mixed solution is separated into a solvent-side first extract (extraction fraction) and a residue (solid content such as bamboo peach leaves) using a filter cloth or the like.

  Next, extraction is performed by mixing the obtained first extract with chloroform (low polarity solvent) (second fractionation treatment). After extraction, the mixed solution is separated into chloroform (hydrophobic fraction) and second extraction solution (hydrophilic fraction). This fractionation process is preferably repeated a plurality of times. In addition, each component contained in these hydrophobic fractions and hydrophilic fractions can be used as a pest attack inhibitor.

  Furthermore, extraction is performed by mixing the obtained second extract with butanols (medium polar solvent) (third fractionation treatment). After extraction, the mixed solution is separated into butanol (medium polar fraction) and a third extract (water-soluble fraction). This treatment is also preferably repeated a plurality of times. The components contained in the medium polar fraction and the water-soluble fraction thus obtained can also be used as a pest attack inhibitor.

  That is, each fraction obtained by each fractionation process of the present production method contains the specific components contained in the bamboo shoots in different concentration balances, and each has a different insecticidal effect and the like. It recognized. The components contained in each of these fractions (insect-poisoning-inhibiting materials) have different easiness to dissolve in water and oil, and therefore can be appropriately selected and used depending on the application, or can be used in combination. In particular, the hydrophobic fraction contains oleandrin at a relatively high concentration, which is useful when oleandrin is required, and the water-soluble fraction contains oleandrin as described later. Since it is almost not included, there is an advantage of excellent safety. Next, the insecticidal effect and the like of the insect pest control material obtained from each of these fractions will be described in detail with specific examples.

<Example>
2000 g of methanol was added to 300 g of fresh leaves of bamboo peach and pulverized with a mixer at room temperature to extract soluble components. After extraction, 160 ml of the extract (corresponding to the extracted fraction) obtained by removing the residue was taken and concentrated under reduced pressure to perform methanol removal to obtain a concentrated extract.

  Next, the obtained concentrated extract was suspended and dispersed in 200 ml of distilled water, and 100 ml of chloroform was mixed with this to extract with shaking. Shaking extraction was repeated 4 times, and the obtained chloroform was concentrated to 50 ml under reduced pressure to obtain a stock solution of test sample A (corresponding to a hydrophobic fraction).

  About the obtained aqueous solution (equivalent to a hydrophilic fraction), 100 ml of isobutanol was mixed and extracted by shaking. Shaking extraction was repeated 5 times, and the resulting isobutanol was concentrated to 50 ml under reduced pressure to obtain a stock solution of test sample B (corresponding to the medium polar fraction). An aqueous solution insoluble in isobutanol was concentrated under reduced pressure, methanol was added to prepare a 50 ml aqueous solution of 50% methanol, and this was used as a stock solution of test sample C (corresponding to a water-soluble fraction).

  In addition, since the content of oleandrin in the stock solution of test sample A was 170000 ng / ml (10200 ng / g in terms of 1 g of fresh leaves), oleandrin was compared with the stock solution of test sample A. It was confirmed that it was contained at a high concentration. Further, when the content of oleandrin was measured for the stock solution of test sample C, it was 1.5 ng / ml (0.09 ng / g in terms of 1 g of fresh leaves). It was confirmed that there was almost no andrin.

{Preparation of test sample}
A solution containing 3 g of solid content was taken out from the stock solution of each test sample and evaporated to dryness. Span 80 (sorbitan monooleate, manufactured by Wako Pure Chemical Industries) and L1695 (sugar ester, An appropriate amount (2 w / v% each) was added and watered to make a total volume of 10 ml to prepare a 30 w / v% solution. A 2 w / v% sugar ester aqueous solution was added thereto, and a 10 w / v% solution for the primary test and a 20 w / v% solution for the secondary test were prepared for each test sample (A, B, C). .

  As a comparative control, each test sample was replaced with oleandrin to prepare a 0.01 w / v% oleandrin solution for the primary test and a 0.1 w / v% solution for the secondary test.

{Test method}
In the test, various insect pests such as Iraga (3rd-instar larvae of Hilohelia Oiraga), stink bug (young larvae of Amaranthus elegans), swallowtail (4th-instar larvae), and ants (Argentina ants) were collected and used.

  A container containing each target pest was prepared for each test sample, and 2 ml each of a 10 w / v% solution of each test sample was sprayed into each of these containers using a spray (primary test). After spraying, each container was sealed and stored with a breathable lid, and the number of dead solids was calculated after 48 hours to determine the mortality rate. When no significant effect was observed in the primary test, a 20 w / v% solution was further sprayed in the same manner as in the primary test, and the mortality was determined after 48 hours (secondary test).

{Test results}
The test result with respect to the target pest of the test samples A to C is shown in FIGS. By spraying the test samples A to C, the insecticidal effect was recognized in all the target pests in a relatively short time. For example, in the primary test of Iraga test sample C shown in FIG. 2, death of one solid out of 5 solids was observed (mortality 20%), and a total of 3 solid deaths were observed in the secondary test (mortality). 60%). However, in the swallowtail swallowtail shown in FIG. 4, the insecticidal effect was not recognized only for the test sample C. Test sample C appears to lack an active ingredient against this type of pest.

  As shown by these test results, the effects of growth inhibition and insecticidal effects on pests are recognized in any fraction, and by using the ingredients contained in these fractions, the damage caused by pests is suppressed. Is possible.

-Second Embodiment-
In FIG. 6, an example of another manufacturing process of a pest attack suppression material is shown. In this manufacturing process, it was made possible to change the concentration balance of the components contained in the bamboo shoot by using an adsorbent.

  Specifically, in this production process, first, the bamboo peach leaves are finely chopped with a mixer or the like, and the chopped bamboo peach leaves are mixed with a highly polar solvent such as water for extraction (first fractionation). processing). The extraction temperature and the like can be appropriately set as necessary as in the first fractionation process of the first embodiment. After extraction, the mixed solution is separated into an extract (extraction fraction) and a residue using a filter cloth or the like.

  Next, the obtained extract is brought into contact with the adsorbent, and predetermined components contained in the extract are adsorbed on the adsorbent (adsorption processing). This adsorption process may be a batch process or a continuous process using a column or the like. In the case of batch processing, 2-3 w / w% activated carbon may be added to the extract and mixed.

  As the adsorbent, various adsorbent resins and activated carbon can be used, and activated carbon is particularly preferable. If it is activated carbon, the cost can be relatively low, and oleandrin can be adsorbed to reduce the concentration of oleandrin in the extract. It is also advantageous in that decolorization and deodorization can be performed simultaneously. The adsorption process may be performed in a plurality of stages using a plurality of adsorbents having different performances. Since the treatment liquid obtained in this manner contains a component that suppresses the damage of pests, it can be used as a pest damage suppressing material.

<Example>
Extraction was performed for 8 to 16 hours by batch processing using a tank using 50 kg of tap water with respect to 5 kg of fresh leaves of bamboo shoots. The mixed solution was heated to 60 ° C. and stirred during extraction. After the extraction, fresh bamboo peach leaves were removed to obtain an aqueous extract.

  2.5 w / w% activated carbon was added to the obtained water extract, and the mixture was stirred at 60 ° C. for 2 hours to obtain a stock solution of test sample D. In addition, when the oleandrin content of the stock solution of the test sample D was measured and found to be about 40 ng / ml, it was confirmed that the test sample D contained almost no oleandrin. .

  Next, the results of examining the effect of suppressing the occurrence of pests on the test sample D prepared from the stock solution by the following method and the test sample C of the above example are shown.

{Preparation of test sample}
A solution corresponding to a solid content of 2 g was taken from each stock solution of test samples D and C, and concentrated under reduced pressure. After adding 1 g of span 80 to the obtained residue and mixing well, 1% aqueous solution of S1670 (sugar ester, manufactured by Mitsubishi Chemical Foods) was added and dispersed to make a total volume of 100 ml. Prepared.

{Test method}
Place two pots of cabbage seedlings of about 15 cm in height on a stand in a greenhouse where flowers for sucking are planted, about 30 cm apart, one with water (control group), the other with test sample C or D (treatment area) was applied in a sufficient amount until the front and back of the leaves were wet using each spray. Next, adult female white butterflies (5 to 6) after mating were released to freely lay eggs, and the total number of eggs laid was examined. The test period was 2 days for test sample C and 4 days for test sample D. During the test, the position of the bowl was changed as appropriate so as not to be affected by the installation location.

{Test results}
The result is shown in FIG. In both test samples C and D, a large difference was observed in the total number of eggs laid between the treated group and the control group. Therefore, it was found that both of the test samples C and D showed a remarkable egg-laying inhibitory action against a white butterfly (adult) such as cabbage and had a pest-preventing effect. In particular, the preventive effect of the test sample D is excellent, and it is judged that its sustainability is also high.

  The insect pest control material obtained by the production method according to the present invention can be used for, for example, agricultural chemicals, insect repellents, insect control agents, insect growth inhibitors and the like.

Claims (7)

A first fractionation step of mixing bamboo peach leaves with a high-polarity solvent and fractionating into an extract fraction and a residue;
And a second fractionation step of fractionating the extracted fraction into a hydrophobic fraction and a hydrophilic fraction by mixing with a low-polarity solvent, and a method for producing a pest attack inhibitor. It is a manufacturing method of the insect pest attack suppression material according to claim 1, further comprising:
A method for producing a pest-damaging inhibitor comprising a third fractionation step of mixing the hydrophilic fraction with a medium-polar solvent and fractionating it into a medium-polar fraction and a water-soluble fraction. It is a manufacturing method of the insect pest attack suppression material according to claim 1 or 2,
The method for producing a pest-damaging inhibitor, wherein the high-polarity solvent is any one of a mixed solution of water and methanol, water, and methanol. It is a manufacturing method of the insect pest attack suppression material as described in any one of Claims 1-3,
The method for producing a pest-damaging inhibitor, wherein the low-polarity solvent is chloroform. It is a manufacturing method of the insect pest attack inhibiting material according to any one of claims 2 to 4,
The method for producing a pest-damaging inhibitor, wherein the medium polar solvent is a butanol. A first fractionation step of mixing bamboo peach leaves with a high-polarity solvent and fractionating into an extract fraction and a residue;
An adsorbing step of bringing the extracted fraction into contact with an adsorbent. It is a manufacturing method of the insect pest attack suppression material according to claim 6,
The method for producing a pest-damaging inhibitor, wherein the adsorbent is activated carbon.

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