JPH0848607A - Cockroach repellent - Google Patents

Abstract

(57) [Summary] [Purpose] A cockroach repellent that is harmless to the human body and is easy to handle. [Structure] A cockroach repellent containing cypress needle leaf oil as an active ingredient, or a cockroach repellent comprising a clathrate complex in which cypress needle leaf oil is contained as an active ingredient and the active ingredient is included in dextrin. [Effect] It has the same repellent efficacy as cockroach repellents containing cedar needle oil as an active ingredient, and the inclusion complex in which the active ingredient of cedar needle oil is included in dextrin has a long lasting repellent effect. is there.

Description

Detailed Description of the Invention

[0001]

This invention relates to cockroach repellents.

[0002]

2. Description of the Related Art Cockroaches are not only harmful insects such as food but also hygienic harmful insects. In recent years, they have proliferated during the winter season, and also inhabit houses and buildings all year round. Was a problem. In addition, as a conventional method for controlling cockroaches, a method of capturing using a paper-made capture device coated with an adhesive, a method of placing food containing boric acid in food in a haunting place, or phenytothione, etc. The method of using the insecticide of is known.

Of the above-mentioned conventional cockroach control methods, the lethal amount of boric acid mixed in food as food is 5 g in infants, and fenitrothion used as an insecticide is extremely poisonous. And, to eradicate cockroaches, toxic boric acid, a drug such as fenitrothion is placed in a place where it is not necessary to have a poison, such as a cupboard, sink, refrigerator, etc., so that it is easy to touch the body. The problem is that it is extremely dangerous.

Further, all of the conventional methods for controlling cockroaches are focused on killing cockroaches, so that there is a problem in that they must be handled with extreme caution.

Therefore, the applicant of the present invention, unlike the conventional capture method and insecticidal method, is harmless to humans, and as a means for easily controlling cockroaches, it was previously disclosed in Japanese Patent Application Laid-Open No. 6-87718, "Sugi. We proposed a cockroach repellent that contains the essential oil extracted from needles or the component separated from the essential oil as the active ingredient.

[0006]

[Problems to be Solved by the Invention] The cockroach repellent proposed in Japanese Patent Laid-Open No. 6-87718 has the advantages that it is harmless to the human body and that it can exhibit an excellent repellent effect even in a small amount.

[0007] In the case of the above-mentioned cedar needles, from the problems of raw material collection, securing, etc., a cockroach repellent having the same repellent effect as the essential oil obtained from the cedar needles or a component separated from the essential oil instead of the cedar wood. Was expected.

The present invention is not limited to cedar needles, but a cockroach repellent which has a persistent repellent effect and is harmless to humans from needle essential oils having an active ingredient in a low boiling point. The purpose is to provide.

[0009]

Means for Solving the Problems As a result of intensive studies to achieve the above-mentioned object, the present inventors have found that cedar needles have an active ingredient with a repellent effect in the high boiling point portion, but cypress needles have a higher repellent effect than the high boiling point portion. It was also found that they also have active ingredients with repellent effect in the low boiling point portion.

However, unlike the essential oil component obtained from the cedar needles, when the repellent effect is excellent in the low boiling point part like the essential oil component obtained from the cypress needles, the component in the low boiling point part is Since it easily volatilizes, there is a problem that the repellent efficacy is lacking in sustainability.

Therefore, as a means for imparting a sustained release property to the active ingredient so as to maintain the repellent effect, inclusion of the active ingredient with another substance, and dextrin which is humanly harmless as an inclusion substance I focused on. That is, by forming a clathrate complex of the active ingredient using dextrin, volatilization can be controlled and the active ingredient can have a sustained release property.

The cockroach repellent of the present invention has been made based on the above findings, and contains an essential oil extracted from cypress needles or a component separated from the essential oil as an active ingredient.

Another cockroach repellent comprises an inclusion complex in which an essential oil extracted from cypress needles or a component separated from the essential oil is used as an active ingredient, and which is included in dextrin.

[0014]

[Action] Essential oil extracted from cypress needles or components separated from essential oil have repellent properties against cockroaches.

The inclusion complex in which the essential oil extracted from the cypress needles or the components separated from the essential oil is clathrated with dextrin has a long repellent property.

[0016]

EXAMPLES The cockroach repellent of the present invention may be used by directly filling the essential oil or a component separated from the essential oil into an open container such as a glass container or a plastic container, but the repellent persistence against cockroaches is maintained. Considering the properties, easiness of handling, storability, etc., inclusion with dextrin is preferable. Further, the active ingredient as it is, or after the active ingredient is clathrated with dextrin, it is impregnated or applied to a base material such as paper or cloth and placed in an appropriate place, or a cupboard,
It is used by impregnating or applying it on door materials such as sinks or floor materials.

First, the cockroach repellent of the present invention will be described. 1. Samples Sugi needles and cypress needles from Shizuoka Prefecture (Shizuoka University campus) were crushed with a mixer, and leaf oil obtained by steam distillation was tested in a cockroach repellent efficacy test.

[0018] Further, cockroaches (Periplaneta fuliginosa) being reared in the Wood Chemistry Laboratory, Shizuoka University
S.) 2-4th instar larvae of the black cockroach were used.

2. Contrast test of cypress needle oil, cedar needle oil, and commercial products repellent Reinforcing test slanting test was prepared by preparing repellent-impregnated filter paper samples with different impregnation amounts of hinoki needle oil. It was performed based on the card and box test method.

In the repellent test, first, an acetone solution prepared by dissolving each group component separated from cypress needle oil in acetone into filter paper (No. 2, width 3.5 cm, length 10 cm, manufactured by Toyo Roshi Kaisha, Ltd.) was dissolved in acetone. After impregnation and drying to remove acetone, the sample was folded into eight and pleated (folded in eight) to obtain a repellent-impregnated filter paper sample. Similarly, a non-impregnated filter paper sample containing no repellent was prepared.

Next, the repellent impregnated filter paper sample and the non-impregnated filter paper sample were put into a rectangular parallelepiped plastic container (height 9.7 cm, width 25.
5 cm, length 19 cm), placed 10 of the cockroaches in the container, left for 20 hours in the dark, count the number of cockroaches that were latent or stationary on each filter paper sample, The following formula

[0022]

[Equation 1]

The repellent rate (%) was calculated by The average value of the repellency was determined by repeating the test 10 times for each sample, and the results are shown in Table 1.

The slanting card and box test method of the repellent test utilizes the property that cockroaches act at night and hide in a narrow dark place during the day. That is, the repellent component is contained in the needle leaf oil, avoiding the needle leaf oil impregnated filter paper sample,
If all the test insects are latent in the unimpregnated filter paper sample, the repellency is 100%, and if they are equally latent in both the repellent component-impregnated filter paper sample and the unimpregnated filter paper sample, the repellency is 0%.
Further, when all 20 of the repellent-impregnated filter paper samples were latent, the repellent rate was -100%, and if the repellent rate became negative, the needle leaf oil contained the cockroach attractant. .

For comparison, repellent-impregnated filter paper samples having different impregnated amounts of cedar needle oil, and commercially available cockroach repellent N, N-Diethl-m-toluamide (abbreviation DET) impregnated with different repellent amounts were used. Using a filter paper sample, the cockroach repellent rate was determined in the same manner as the cockroach repellent of the above-mentioned cypress needle leaf oil. The results are shown in Table 1.

[0026]

[Table 1]

As is apparent from Table 1, the repellents containing cypress needle oil and cedar needle oil as active ingredients both have repellent effect and are commercially available cockroach repellents N, N-Diethl-mt.
It has a better repellent effect than oluamide.

Further, the amount of impregnation of cypress needle oil and cedar needle oil on the filter paper was changed to change the effective minimum concentration (minimum effectiv).
e concentration of 80% repellency; MEC ₈₀ ) value (mg
/ m ² ). As a result, the cockroach repellent efficacy MEC ₈₀ value of cedar needle oil was 300 mg / m ² , whereas the cockroach repellent efficacy MEC ₈₀ value of cypress needle oil was 10 mg / m ^2, which is higher than that of cedar needle oil. It was found that repellent efficacy was obtained at extremely low values.

Further, as is clear from Table 1, when compared with the same impregnation amount, it was determined that cypress needle oil had a slightly better repellent effect than cedar needle oil, so the boiling point of cypress needle oil It was decided to fractionate separately and examine which fraction shows the repellent effect.

3. Fractionation of leaf oil component and cockroach repellent efficacy Needle leaves obtained from cypress from Shizuoka Prefecture (Shizuoka University campus) were extracted by steam distillation using a micro fractional distillation apparatus and separated at each boiling point. This gave an essential oil.

As a result of quantifying the essential oil in the cypress needle leaves using an essential oil quantitative device (steam distillation method), the essential oil content was 3.7 ml.
It was / 100g. At this time, as a pretreatment, if the cypress needles are crushed as much as possible to destroy the cells, the essential oil will be efficiently distilled out in a short time as described in JP-A-6-87718.
This is the same as the case of extracting the essential oil from the cedar needles proposed in Japanese Patent Publication.

Gas chromatographic analysis of cypress needle leaf oil components fractionated for each boiling point (carrier: OV-1, capillary
Lee column: 0.25 mm × 25 m, column temperature and retention time: 5
As a result of conducting 0 ° C. × 10 minutes, 50 to 200 ° C. (temperature increase 5 ° C./minute), 200 ° C. × 10 minutes: abbreviated GC analysis), it was confirmed that about 40 kinds of components were contained.

Therefore, the needle oil obtained from cypress is heated to 33 to 125 ° C. depending on the boiling point by using a micro fractional distillation apparatus.
Fractionation and residual fraction not fractionated at 125 ℃,
The results are shown in Table 2.

[0034]

[Table 2]

Gas chromatographic analysis was performed on each of the fractions to find that fraction-1 (hereinafter referred to as fraction 1
Component) up to a retention time of 5 minutes (hereinafter referred to as RT) and RT5 for fraction-3 (hereinafter referred to as fraction 2)
10 to 10 minutes, RT-5 to 20 minutes for fraction-5 (hereinafter referred to as fraction 3), RT20 to 30 minutes for fraction-7 (hereinafter referred to as fraction 4), and RT30 for residual fraction Since the components after the minute were contained, it was possible to roughly divide them into 5 groups according to boiling points.

Therefore, in order to make a comparative examination of the cockroach repellent efficacy of these fractions, and to clarify the relationship between the needle leaf oil component and the repellent efficacy, each fraction distilled in a nitrogen stream, that is, cypress needles Each fraction of the above 5 groups separated from oil (RT up to 5 minutes, RT up to 5 minutes, R,
T15 to 20 minutes of components, RT20 to 30 minutes of components) and residual components were divided and the repellent rate of each component was examined based on the above-mentioned repellent test method. Table 3 shows the results.

[0037]

[Table 3]

As is clear from Table 3, the repellency rates are Fraction 1 (Fr. 1) and Fraction 2 (Fr.
2), fraction 3 (Fr.3), fraction 4
(Fr.4) and the residue (R) are decreased in this order, and the higher the boiling point of the component, the lower the repellent efficacy, that is, the low boiling point component (fraction 1) fractionated first is superior in the repellent efficacy. I understand.

Further, the residual fraction component did not show repellent effect and showed a weak attracting property.

4. Gas Chromatographic Analysis of Hinoki Needle Oil The cypress oil obtained by subjecting cypress needle leaves to steam distillation and fractionated according to boiling point was subjected to gas chromatography analysis to confirm the fractionation status.

Then, when the GC-MS analysis was carried out on the fraction 1 (Fr.1) of the low boiling point component which showed the highest repellent effect, as shown in FIG.
Both C and D are monoterpenes having a molecular weight of 136, and retention time (RT) with the standard product by GC-MS analysis
It was estimated that the respective peaks were α-pinene, sabinene, myrcene, and limonene.

In addition, several samples of monoterpenes were subjected to a repellency test. As a result, Δ-carene, myrcene, α
-Terpinene has a repellent property, and α-pinene and D-limonene, which are aromatic components of wood, have no repellent effect.

5. Persistence of Cockroach Repellent Efficacy From the results shown in Table 3, it was clarified that the low boiling point component was excellent in cockroach repellent efficacy. There is a risk of chipping.

In order to confirm this point, a low boiling point component of Japanese cypress leaf oil was impregnated into a filter paper at 2,000 mg / m ² and a repellent efficacy test was conducted immediately (A), and in the atmosphere for 7 days after impregnation. When the repellency efficacy test was conducted after standing, the repellency rate of (B) was examined. As a result, (A) shows a repellency rate of 100%, whereas (B) shows a repellency rate of 21%, and the repellant component volatilizes. It was found that the repellent effect was reduced by doing so. Table 4 shows the results.

Therefore, for the purpose of sustaining the repellent effect,
Japanese cypress needle leaf oil was converted to β-cyclodextrin (abbreviation β-C
An inclusion complex which was included in D) was prepared. In the present invention, inclusion means that the active ingredient of cypress needle leaf oil is incorporated into the molecular cavity of β-cyclodextrin to form a complex.

The inclusion complex was prepared as follows. 100 ml of water was added to 1.55 g of β-cyclodextrin, to which was added a low boiling point component of hinoki needle oil of 1/2 the amount of β-cyclodextrin, and the mixture was stirred with a magnetic stirrer for 2 hours. Centrifuge this at 10,000 rpm
After centrifugation for 10 minutes to remove the supernatant and recover the precipitate, water was added to the precipitate and the mixture was stirred, and centrifugation was repeated three times, and then air-dried. An inclusion complex was prepared.

After determining the amount of cypress needle leaf oil in the inclusion complex, the inclusion complex corresponding to the impregnation amount of 2,000 mg / m ² was weighed and tested.

Then, the inclusion complex immediately after preparation and the inclusion complex left in the air for 7 to 60 days after preparation and allowed to stand for a predetermined number of days were used to prepare each inclusion complex based on the above-mentioned repellent test method. The repellency rate was examined for each. The results are shown in Table 4.

[0049]

[Table 4]

As is clear from Table 4, the inclusion complex of cypress needle oil encapsulated with β-cyclodextrin stably shows a high repellency even after being left for 7 to 60 days after inclusion. It was confirmed that the inclusion of cypress needle leaf oil with β-cyclodextrin is effective for imparting the persistence of the cockroach repellent effect.

As described above, the inclusion complex of cypress needle oil and β-cyclodextrin showed a high repellency even when the repellant was left for 30 days after the preparation of the inclusion.

6. Summary Repellents containing sugi needle oil and cypress needle oil as active ingredients are commercially available cockroach repellents N, N-Diethl-m-tolua.
It shows a repellent effect superior to that of mide (abbreviation DET). The repellent containing cypress needle oil as an active ingredient was slightly more effective than the repellent containing cypress needle oil as an active ingredient.

Further, as a result of fractionating the cypress needle oil by boiling point, a higher repellent effect was recognized in the low boiling point component than in the high boiling point component.

When a low-boiling point component of cypress needle oil is used as an active ingredient in a cockroach repellent, the low-boiling point component is liable to volatilize, and thus there is a problem that the repellent efficacy is lacking in sustainability. It can be solved by inclusion with cyclodextrin, and the inclusion complex that has been left in the air for 60 days after the inclusion preparation has a high repellent effect.

[0055]

INDUSTRIAL APPLICABILITY As described above, according to the present invention, it is harmless to the human body and excellent in repelling in a small amount as compared with N, N-Diethl-m-toluamide which is a conventional commercially available cockroach repellent. It is effective, easy to handle, and has the same repellent effect as a cockroach repellent containing cedar needle oil as an active ingredient.

When an essential oil extracted from cypress needle leaf oil or an active ingredient separated from the essential oil is clathrated with dextrin to form a clathrate complex, it is effective even if left in the air for 60 days after clathration. Sustained release of the component is obtained, and the repellent efficacy is long-lasting.

[Brief description of drawings]

FIG. 1 is a gas chromatogram of fraction 1 of cypress needle leaf oil.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yoshihiro Maekawa 200 Terashimacho, Hamamatsu City, Shizuoka Prefecture Kawai Musical Instrument Mfg. Co., Ltd.

Claims (2)

[Claims] 1. A cockroach repellent comprising, as an active ingredient, an essential oil extracted from cypress needles or a component separated from the essential oil. 2. A cockroach repellent consisting of an inclusion complex in which an essential oil extracted from cypress needle leaves or a component separated from the essential oil is used as an active ingredient and which is included in dextrin.