Pest repellent composition for humans
Patent Information
- Application Number
- JP2020181377
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2020-10-29
- Publication Date
- 2025-03-03
- Estimated Expiration
- 2040-10-29
AI Technical Summary
【0007】 本発明の人体用害虫忌避組成物は、有効成分である(B)ブチルアセチルアミノプロピオン酸エチルの安定な乳化系を長期間にわたり維持するため、長期安定性に優れた人体用害虫忌避製剤とすることができる。 さらに、本発明の人体用害虫忌避組成物は、溶解助剤の併用の必要がないので、皮膚刺激やベタツキを抑えて使用感を向上させることができ、さらには、有効成分の皮膚吸収をも防止することができるので、子供やペットにも好適に使用することができる。
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Abstract
Description
[Technical field]
[0001] The present invention relates to a pest repellent composition for human use and a method for producing said pest repellent composition for human use. [Background technology]
[0002] Known active ingredients of human pest repellents include DEET, icaridin, and eucalyptus oil (for example, Patent Document 1, etc.). In order to uniformly and stably maintain these active ingredients in various preparations, dissolving agents such as alcohol and surfactants are used, but these can cause skin irritation and stickiness, as well as skin absorption of the active ingredients. Considering the use of human pest repellents on children, it is desirable to improve these irritation and stickiness, and even prevent skin absorption of the active ingredients. Meanwhile, techniques for uniformly retaining the intended active ingredient in a formulation without using a solubilizing agent have been investigated, and one of these techniques is known to be a three-phase emulsification technique (for example, Patent Document 2, etc.). However, when using ethyl butylacetylaminopropionate as an active ingredient to obtain a repellent effect, if three-phase emulsification technology is used, the emulsion system breaks down over time, making it difficult to maintain the active ingredient stably in the formulation. However, no effective means for solving this problem has yet been reported. [Prior art documents] [Patent documents]
[0003] [Patent Document 1] JP 2007-277196 A [Patent Document 2] JP 2010-110685 A Summary of the Invention [Problem to be solved by the invention]
[0004] The present invention has been made in consideration of the above-mentioned circumstances, and has as its objective the provision of a pest repellent composition for human use which contains ethyl butylacetylaminopropionate as an active ingredient and has excellent long-term stability. [Means for solving the problem]
[0005] As a result of intensive research into solving the above-mentioned problems, the inventors have discovered that a human pest repellent composition having excellent long-term stability can be obtained by combining (A) an emulsifier, more specifically, one or more selected from closed vesicles formed by an amphiphilic substance that spontaneously forms closed vesicles or particles of a polycondensation polymer having hydroxyl groups, (B) ethyl butylacetylaminopropionate, and (C) propylene glycol caprate and / or propylene glycol dicaprate, and have thus completed the present invention.
[0006] Specifically, the present invention relates to the following items. 1. (A) an emulsifier; (B) ethyl butylacetylaminopropionate, (C) propylene glycol caprate and / or propylene glycol dicaprate, and (D) containing water; The emulsifier (A) is at least one selected from the group consisting of closed vesicles formed by an amphiphilic substance which spontaneously forms closed vesicles, and particles of a polycondensation polymer having a hydroxyl group. A pest repellent composition for human use. 2. (B) Ethyl butylacetylaminopropionate, (C) dissolved in propylene glycol caprate and / or propylene glycol dicaprate, When this solution is mixed with (D) water, it is emulsified using (A) an emulsifier, The emulsifier (A) is at least one selected from the group consisting of closed vesicles formed by an amphiphilic substance which spontaneously forms closed vesicles, and particles of a polycondensation polymer having a hydroxyl group. A method for producing a pest repellent composition for human use. Effect of the Invention
[0007] The pest repellent composition for human use of the present invention maintains a stable emulsion system of the active ingredient (B) ethyl butylacetylaminopropionate for a long period of time, and therefore can be made into a pest repellent formulation for human use with excellent long-term stability. Furthermore, since the pest repellent composition for human use of the present invention does not require the use of a dissolution aid, it is possible to improve the feeling of use by suppressing skin irritation and stickiness, and it is also possible to prevent the active ingredient from being absorbed through the skin, making it suitable for use by children and pets. [Brief description of the drawings]
[0008] [Figure 1] FIG. 2 is a photograph showing the appearance after one month of storage under storage conditions at 25° C. in the “three-phase emulsion stability confirmation test” in the examples. [Diagram 2] FIG. 2 is a photograph showing the appearance after one month of storage under "cycle" conditions in the "three-phase emulsion stability confirmation test" in the Examples. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0009] The pest repellent composition for human use and the method for producing said pest repellent composition for human use of the present invention will be described in detail below.
[0010] The pest repellent composition for human use of the present invention contains a specific emulsifier (A). <Component (A)> The emulsifier (A) in the present invention is one or more types selected from closed vesicles (hereinafter sometimes referred to as "closed vesicles") formed from an amphiphilic substance that spontaneously forms closed vesicles, or particles of polycondensation polymers having hydroxyl groups (hereinafter sometimes referred to as "polycondensation polymer particles"). Since the closed vesicles or polycondensation polymer particles in the present invention have extremely excellent emulsification performance, the amount of water (D) in the composition containing it can be selected widely from the range of 20 to 99% by weight, and can be appropriately set according to the form of emulsion and the amount of ethyl butylacetylaminopropionate (B). The amount of the closed vesicles or polycondensation polymer particles can be appropriately set according to the amount of ethyl butylacetylaminopropionate (B), and is not particularly limited, but may be 0.0001% by weight or more and 5% by weight or less in total, and even a small amount of preferably 1.0% by weight or less, more preferably 0.75% by weight or less can maintain the emulsified state. The above amounts are all solid content. In addition, the emulsion structure is more preferably an O / W type emulsion structure.
[0011] The closed vesicles in the present invention are formed by an amphipathic substance that spontaneously forms closed vesicles. As the amphipathic substance that forms closed vesicles, it is preferable to use a derivative of polyoxyethylene hydrogenated castor oil represented by the following general formula (1).
[0012] [ka] In the formula, E, which is the average number of moles of ethylene oxide added, is 3 to 100. The upper limit of E is preferably 50, and more preferably 40. The lower limit of E is preferably 5.
[0013] Furthermore, the closed endoplasmic reticulum of the present invention may employ phospholipids or phospholipid derivatives, etc. As the phospholipid, among the structures shown in the following general formula (2), DLPC (1,2-Dilauroyl-sn-glycero-3-phospho-rac-1-choline) with a carbon chain length of 12, DMPC (1,2-Dimyristoyl-sn-glycero-3-phospho-rac-1-choline) with a carbon chain length of 14, and DPPC (1,2-Dipalmitoyl-sn-glycero-3-phospho-rac-1-choline) with a carbon chain length of 16 can be employed. [ka]
[0014] In addition, among the structures represented by the following general formula (3), the Na salt or NH 4 salt, Na salt of DMPG (1,2-Dimyristoyl-sn-glycero-3-phospho-rac-1-glycerol) with a carbon chain length of 14 or NH 4 salt, Na salt of DPPG (1,2-Dipalmitoyl-sn-glycero-3-phospho-rac-1-glycerol) with a carbon chain length of 16 or NH 4 Salt may also be employed. [ka] As the amphiphilic substance, polyoxyethylene hydrogenated castor oil, sodium dilauroyl glutamate lysine, and polyglycerol fatty acid ester are preferable. Moreover, the amphiphilic substance may be used alone or in combination of two or more kinds.
[0015] The polycondensation polymer in the polycondensation polymer particles of the present invention is not particularly limited, and may be either a natural polymer or a synthetic polymer, and may be appropriately selected according to the application. However, natural polymers are preferred because they are excellent in safety and generally inexpensive, and sugar polymers described below are more preferred because they have excellent emulsifying function. The particles include both polycondensation polymers that have been made into single particles and those in which the single particles are connected to each other, but do not include aggregates (having a network structure) before being made into single particles. The polycondensation polymer may be used alone, or two or more types may be used in combination. The sugar polymer is a polymer having a glucoside structure, such as cellulose or starch. Examples of such sugars include those produced by microorganisms using several sugars selected from monosaccharides such as ribose, xylose, rhamnose, fucose, glucose, mannose, glucuronic acid, and gluconic acid as building blocks; natural polymers such as xanthan gum, gum arabic, guar gum, karaya gum, carrageenan, pectin, fucoidan, quince seed gum, tragacanth gum, locust bean gum, galactomannan, curdlan, gellan gum, fucogel, casein, gelatin, starch, collagen, and tremella fuciformis polysaccharides; semi-synthetic polymers such as methylcellulose, ethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose, stearoxyhydroxypropylmethylcellulose, sodium carboxymethylcellulose, propylene glycol alginate, cellulose crystals, starch-sodium acrylate graft polymer, and hydrophobized hydroxypropylmethylcellulose; and synthetic polymers such as polyvinyl alcohol, polyvinylpyrrolidone, carboxyvinyl polymer, polyacrylate, and polyethylene oxide. The sugar polymer may be used alone or in combination of two or more kinds. As the sugar polymer particles, it is preferable to use a mixture of polysaccharides such as agar, hydrophobically modified alkylcellulose, carboxymethylcellulose, guar gum, or a salt thereof.
[0016] The emulsifier (A) in the pest repellent composition for human use of the present invention is particularly preferably a hydrophobically modified alkyl cellulose, since the emulsified state is easily stabilized and it is highly safe for humans and animals. The hydrophobically modified alkyl cellulose is a compound in which a hydrophobic group is introduced into a water-soluble cellulose ether derivative, and is represented by the following general formula (4). [ka] In the formula, R 5 , R 6 , R7 , R 8 , R 9 and R 10 are respectively a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, and -[CH 2 CH 2 O] m H, -[CH 2 CH(CH 3 )O] m H, -CH 2 CH(OH)CH 2 OA, -[CH 2 CH(OH)CH 2 O] m -A or -[CH 2 CH 2 O] m CH 2 CH(OH)CH 2 OA, but must be -CH, except when all are simultaneously hydrogen atoms or alkyl groups having 1 to 4 carbon atoms. 2 CH(OH)CH 2 OA, -[CH 2 CH(OH)CH 2 O] m -A, -[CH 2 CH 2 O] m CH 2 CH(OH)CH 2 It contains one or more groups selected from OA, n' is an integer of 50 to 5000, m is an integer of 1 to 10, and A is a hydrophobic group. As the emulsifier (A) to be incorporated in the human pest repellent composition of the present invention, a hydrophobically modified alkyl cellulose represented by general formula (4) is preferred, in which the hydrophobic group represented by "A" in the formula is preferably an alkyl group, more preferably an alkyl group having 10 to 28 carbon atoms, particularly preferably an alkyl group having 14 to 22 carbon atoms, and specifically, a stearoyl group is most preferred.
[0017] A specific example of the hydrophobically modified alkyl cellulose in which the hydrophobic group represented by "A" in the general formula (4) is a stearoyl group is stearoxy hydroxypropyl methyl cellulose. This compound is commercially available from Daido Kasei Kogyo Co., Ltd. under the trade name of Sangelose, and such a commercially available product can also be used as the compounding component (A) of the human pest repellent composition of the present invention. The compounding amount is preferably 0.001% by weight or more and 1.0% by weight or less, more preferably 0.005% by weight or more and 0.5% by weight or less, and even more preferably 0.01% by weight or more and 0.1% by weight or less, based on the total amount of the pest repellent spray. This compounding amount range is preferable because it can maintain a stable emulsification system of (B) ethyl butylacetylaminopropionate for a long period of time. When preparing the pest repellent composition for human use of the present invention, a commonly used surfactant may be added, but it is preferable that the composition does not contain any surfactant other than the emulsifier (A).
[0018] The pest repellent composition for human use of the present invention contains (B) ethyl butylacetylaminopropionate as an active ingredient. <(B) component> The (B) ethyl butylacetylaminopropionate in the present invention is a compound having the following chemical structure: Its chemical name is 3-(Nn-butyl-N-acetyl)aminopropionic acid ethyl ester, and it is a compound known as a pest repellent component. [ka] The content of (B) ethyl butylacetylaminopropionate in the human pest repellent composition of the present invention may be appropriately determined depending on the purpose of use, the place of use, etc., but it is preferably contained in an amount of 3 to 30 wt %, and more preferably 5 to 20 wt %, based on the total amount of the human pest repellent composition.
[0019] The human pest repellent composition of the present invention may contain one or more pest repellent components as an active ingredient other than (B) ethyl butylacetylaminopropionate, within the range that does not impair the effect of the present invention. Examples of pest repellent components that may be contained include synthetic compounds such as DEET and 2-(2-hydroxyethyl)-1-piperidine carboxylic acid 1-methylpropyl ester (hereinafter referred to as "icaridin"), as well as natural ingredients derived from plant essential oils such as p-menthane-3,8-diol, dimethyl phthalate, eucalyptol, α-pinene, geraniol, citronellal, camphor, linalool, and carane-3,4-diol.
[0020] The pest repellent composition for human use of the present invention contains (C) propylene glycol caprate and / or propylene glycol dicaprate as an active ingredient. <(C) component> The (C) propylene glycol caprate and propylene glycol dicaprate in the present invention are compounds having the following chemical structures. [ka] The content of (C) propylene glycol caprate and / or propylene glycol dicaprate in the human pest repellent composition of the present invention may be appropriately determined depending on the purpose of use and the place of use, but it is preferably contained in an amount of 1 to 30% by weight, and more preferably 5 to 20% by weight, based on the total amount of the human pest repellent composition.
[0021] The pest repellent composition for human use of the present invention contains water (D) as an active ingredient. <(D)Water> In the present invention, the water (D) refers to the total water contained in the pest repellent composition for human use, including not only purified water, ion-exchanged water, distilled water, etc., but also the water contained in each of the blended ingredients. The amount of water (D) can be selected broadly within the range of 20 to 99% by weight based on the total amount of the pest repellent composition for human use, and can be appropriately selected depending on the form of emulsion and the amount of ethyl butylacetylaminopropionate (B).
[0022] <Spray> The human pest repellent composition of the present invention can be used as a spray by formulating the composition using (A) an emulsifier, (B) ethyl butylacetylaminopropionate, (C) propylene glycol caprate and / or propylene glycol dicaprate, and (D) water, as well as other necessary formulation assistants within the range that does not impair the effects of the present invention, and filling the resulting liquid formulation into a spray container. Any spray container can be used as long as it can easily fill with the liquid formulation and function as a spray, but in consideration of versatility and high spray accuracy, the following three spray containers are preferred. (1) Mist-type spray container equipped with a pump-type nozzle that can spray: This spray container can spray at atmospheric pressure, does not require pressurized gas, and has a relatively simple container structure, making it highly safe and suitable for portability. The structure consists of an extrusion pump-type nozzle equipped with a suction tube, and a screw-type container to which this is fixed and into which the contents are filled. (2) Trigger-type spray container: This container has a pistol-shaped trigger-type spray device attached to the mouth of the container body where the contents are filled, and can spray at atmospheric pressure, making it a highly versatile spray container. The trigger-type spray container referred to here includes all trigger-type spray containers that have been partially improved to enhance the spray function. (3) Aerosol spray container: This container allows for continuous spraying by filling the container with a propellant, something that the two spray containers mentioned above cannot achieve. The aerosol spray containers mentioned here include all aerosol containers with improvements made to the spray device. In general, spraying with this spray container produces a finer mist than the two spray containers mentioned above, which are sprayed under atmospheric pressure. In particular, when the pest repellent composition for human use of the present invention is used as an insect repellent spray, (1) a mist type spray container or (2) a trigger type spray container are preferred because of their ease of use.
[0023] The pest repellent composition for human use of the present invention can be filled into the above-mentioned aerosol spray container for use. In this case, the liquid carrier used in the liquid agent filled into the aerosol spray container must be (D) water, and the following organic solvents can also be used as liquid carriers in the range that does not destroy the emulsion. Preferred organic solvents include one or more selected from fatty acid ester solvents, glycol ether solvents, heterocyclic solvents, ester solvents, and alcohol solvents, and specifically include ethyl lactate, propylene glycol diacetate, dipropylene glycol dimethyl ether, triethylene glycol monomethyl ether, diethylene glycol monobutyl ether, triethylene glycol monobutyl ether, ethylene glycol monobenzyl ether, butyl propylene diglycol, tripropylene glycol monobutyl ether, sulfolane, γ-butyrolactone, N-methyl-2-pyrrolidone, N-ethyl-2-pyrrolidone, N-octyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolidinone, propylene carbonate, methanol, ethanol, isopropanol, etc., but are not limited thereto. Among them, N-methyl-2-pyrrolidone, ethanol, isopropanol, and propylene carbonate are suitable.
[0024] The propellant used when filling the human pest repellent composition of the present invention into the above-mentioned aerosol spray container can be any of the known propellants, such as liquefied petroleum gas (LPG), dimethyl ether, carbon dioxide gas, and nitrogen gas. In this human pest repellent composition, the amount of propellant is 10 to 95% by volume, particularly 30 to 90% by volume, of the entire pest repellent spray, and the concentrate (the total amount of components (A), (B), (C), and (D) and formulation auxiliaries) can be 90 to 5% by volume, particularly 70 to 10% by volume. In producing the human pest repellent composition of the present invention, a method commonly used in this field can be widely used. Representative methods include adding (A) an emulsifier, (B) ethyl butylacetylaminopropionate, (C) propylene glycol caprate and / or propylene glycol dicaprate, and (D) water, and other liquid carriers and compounding ingredients as necessary, and mixing with heating (30 to 50°C) as necessary to prepare a uniform solution, and then adding rust inhibitors, preservatives, etc., and putting the resulting concentrate into an aerosol spray container, filling it with a propellant to make a product, etc. The human pest repellent composition of the present invention obtained in this way can maintain a stable and uniform state even under harsh conditions for a long period of time, and can be sprayed into the air as fine particles with one touch when desired.
[0025] <Wet tissue agent> The human pest repellent composition of the present invention can be formulated using (A) an emulsifier, (B) ethyl butylacetylaminopropionate, (C) propylene glycol caprate and / or propylene glycol dicaprate, and (D) water, as well as necessary formulation aids within the scope that does not impair the effects of the present invention, and the resulting liquid can be impregnated into a support to be used as a wet tissue preparation. To apply to the skin as a wet tissue, the weight of the support should be 20 to 80 g / m 2However, the thickness is preferably about 0.1 to 5 mm. Examples of the support that can be used include woven fabrics such as flannel, cotton, silk, polyester, nylon, and fabrics made from these materials; nonwoven fabrics such as polyester, polyolefin, nylon, cotton, rayon, vinylon, cellulose, and fabrics made from these materials; and sheet-shaped resin foams made from foamed polyethylene, polypropylene, ethylene-vinyl acetate copolymer, polyvinyl chloride, and the like. When the pest repellent composition for human use of the present invention is used as a wet tissue agent, it is preferable that the support retains 1 to 10 ml / g of the pest repellent composition for human use of the present invention in order to obtain the desired pest repellent effect.
[0026] <Other medicinal ingredients> When the pest repellent composition for human use of the present invention is used as an insect repellent spray or an insect repellent wet tissue, it may come into indirect or direct contact with human skin, so medicinal ingredients that moisturize the skin, etc. may be appropriately blended in as long as the emulsion is not destroyed. These medicinal ingredients include avocado extract, amacha extract, althea extract, arnica extract, apricot extract, apricot kernel extract, ginkgo extract, fennel extract, turmeric extract, oolong tea extract, echinacea leaf extract, phellodendron bark extract, barley extract, Dutch mustard extract, orange extract, hydrolyzed wheat powder, hydrolyzed silk, chamomilla extract, carrot extract, artemisia capillaris extract, kalkade extract, kiwi extract, cinchona extract, cucumber extract, guanosine, kumazasa extract, walnut extract, grapefruit extract, clematis extract, yeast extract, comfrey extract, cowberry extract, psyllium extract, umbilical cord extract, salvia extract, soapwort extract, bamboo extract, hawthorn extract, shiitake mushroom extract, rehmannia extract, lime root extract, linden extract, meadowsweet extract, calamus root extract, white birch extract, horsetail extract, watermelon Examples of effective extracts include ivy extract, hawthorn extract, elderberry extract, yarrow extract, peppermint extract, mallow extract, swertia britannica extract, taiso extract, thyme extract, clove extract, Imperata cylindrica extract, tomato extract, natto extract, wild rose extract, hibiscus extract, burdock extract, parsley extract, parietaria extract, burdock extract, bisabolol, coltsfoot extract, butterbur honey, tou extract, pompano extract, butcher's broom extract, grape extract, propolis, loofah extract, peppermint extract, linden extract, hop extract, pine extract, horse chestnut extract, skunk cabbage extract, soapberry extract, peach leaf extract, cornflower extract, eucalyptus extract, apple extract, lettuce extract, astragalus extract, rose extract, rosemary extract, and Roman chamomile extract.
[0027] The pest repellent composition for human use of the present invention can be used as an insect repellent by directly spraying or applying it to human skin or clothing, or by spraying it in a space where it is desired to repel blood-sucking insects such as mosquitoes. In particular, the pest repellent composition for human use of the present invention is preferably used as an insect repellent spray. EXAMPLES
[0028] The present invention will be described in more detail below with reference to formulation examples and test examples, but the present invention is not limited to these examples. First, a study was conducted to find the component (C) of the present invention, which is an oil agent (D) that is excellent in solubility in (B) ethyl butylacetylaminopropionate and insoluble in (D) water. In the examples, unless otherwise specified, parts refer to parts by weight.
[0029] <Oil agent screening> The following nine types of oil agents, a to i, were examined at room temperature (25°C) for the following items (1) to (3), and each oil agent was evaluated according to the following evaluation criteria. (1) Oil solution and (D) water were mixed in a weight ratio of 1:1, and the solubility was confirmed visually. (2) The oil solution and (B) ethyl butylacetylaminopropionate were mixed in a weight ratio of 1:1, and the solubility was confirmed visually. (3) The above (2) was mixed with water in a weight ratio of 1:1, and the solubility was confirmed visually. [Oils a-i] Oil solution a: Copolymer of polyethylene glycol (PEG-12) and methylpolysiloxane (manufactured by Momentive) Oil b: Olive oil (manufactured by Nippon Surfactance Industries Co., Ltd.) Oil C: Isopropyl myristate (manufactured by Sanko Chemical Industry Co., Ltd.) Oil d: Propylene glycol monocaprate (manufactured by Nippon Surfactance Industries Co., Ltd.) Oil e: Propylene glycol dicaprylate (manufactured by Nippon Surfactance Industries Co., Ltd.) Oil F: Safflower oil (manufactured by Nippon Surfactance Industries Co., Ltd.) Oil g: Tri(capryl / capric acid)glyceryl (manufactured by Nippon Surfactance Industry Co., Ltd.) Oil: Squalane oil (Kishimoto Special Liver Oil Industry Co., Ltd.) Oil: Jojoba oil (manufactured by Nikko Chemical Co., Ltd.) [Evaluation Criteria] Evaluation criteria for items (1) and (2) ○: Dissolved ×: Separated Evaluation criteria for item (3) ○: The boundary between (2) above and water is clear. △: There is a boundary between the above (2) and water, but there is slight mixing between the layers. ×: There is no boundary between the above (2) and water, or each component is significantly unevenly distributed. Overall evaluation criteria ◯: Suitable as component (C) of the present invention ×: Not suitable as component (C) of the present invention The evaluation results of study items (1) to (3) and the overall evaluation result are summarized in Table 1. Note that "-" in Table 1 means that study item (3) was not implemented because the evaluation result of study item (2) was "×".
[0030] [Table 1]
[0031] As shown in Table 1, it was confirmed that oil agent d "propylene glycol monocaprate" and oil agent e "propylene glycol dicaprate" have excellent solubility in (B) ethyl butylacetylaminopropionate of the present invention and are insoluble in (D) water, making it clear that they are suitable as component (C) of the present invention. The other oil agents were rated "x" in the above evaluation item (3), and were confirmed to be oil agents not suitable as component (C) of the present invention.
[0032] <Three-phase emulsion stability confirmation test> (1) Preparation of test samples Test sample (a) 10.0 parts by weight of (B) ethyl butylacetylaminopropionate was dissolved in 10.0 parts by weight of (C) propylene glycol dicaprate, and this solution was mixed with 1.2 parts by weight of formulation aids (preservatives, pH adjuster) and (D) purified water, and emulsified using 0.05 parts by weight of (A) hydrophobically modified hydroxypropyl methylcellulose to obtain a test sample (a) with a total amount of 100 parts by weight. Test sample (b) Test sample (b) was obtained in a total amount of 100 parts by weight by emulsifying in the same manner as test sample (a), except that (C) propylene glycol dicaprate was replaced with (C) propylene glycol caprate. Comparative test sample (c) (B) 10.0 parts by weight of ethyl butylacetylaminopropionate was mixed with 1.2 parts by weight of formulation aids (preservatives, pH adjuster) and (D) purified water, and emulsified using (A) 0.05 parts by weight of hydrophobically modified hydroxypropyl methylcellulose to obtain a comparative test sample (c) with a total amount of 100 parts by weight.
[0033] (2) Stability confirmation test method The above test specimens (a) and (b) and the comparative test specimen (c) were stored for one month under two storage conditions: 25°C storage condition and a "cycle" condition in which the storage condition of "5°C for 23 hours → temperature increase (1 hour) → 40°C for 23 hours → temperature decrease (1 hour) → 5°C for 23 hours..." was repeated, and the external appearance properties were visually inspected. [Evaluation Criteria] 〇: The emulsion is stable. ×: The emulsion system is not stable. The evaluation results of test samples (a) and (b) and comparative test sample (c) are summarized in Table 2. In addition, photographs of the appearance after one month of storage under each condition are shown in Figure 1 (storage condition at 25°C) and Figure 2 ("cycle" condition). From the left, Figures 1 and 2 show test specimens (a), (b), and comparative test specimen (c).
[0034] [Table 2]
[0035] As shown in Table 2, in the test samples (a) and (b), which are specific examples of the present invention, coacervation (not oil-water separation due to emulsion destabilization, but a difference in the apparent liquid layer due to the difference in specific gravity of individual emulsion particles) was visible under both the 25°C storage condition and the "cycle" condition, and it was confirmed that a good emulsified state was maintained. On the other hand, in the case of the comparative test sample (c), which is not a specific example of the present invention, there was no problem with the stability of the emulsion system under storage conditions at 25°C, but it was confirmed that the oil components became unstable and settled under cycle conditions, posing a serious problem with the stability of the emulsion system. These results demonstrate that the pest repellent composition for human use of the present invention can maintain a stable emulsion system for a long period of time.
[0036] <Hydrolysis resistance test of three-phase emulsion repellent> (1) Test specimen The test sample (a) in the above "Three-phase emulsion stability confirmation test" was used. (2) Stability confirmation test method The above test sample (a) was stored at 50°C, 40°C, 25°C, and 5°C, and under a "cycle" condition of repeating the following conditions: "23 hours at 5°C → temperature increase (1 hour) → 23 hours at 40°C → temperature decrease (1 hour) → 23 hours at 5°C...". The remaining amount of the component (B) of the present invention after 3 months, 4 months, and 8 months was analyzed by liquid chromatography (GC-2014: manufactured by Shimadzu Corporation, OV-17: manufactured by GL Science Co., Ltd.), and the pH of the test sample was confirmed by a pH meter (LAQUA F-71S: manufactured by Horiba, Ltd.). The results are shown in Table 3. In Table 3, "-" means that the experiment was not carried out.
[0037] [Table 3]
[0038] As shown in Table 3, it was confirmed that the test sample (a), which is a specific example of the human pest repellent composition of the present invention, has an active ingredient (B) ethyl butylacetylaminopropionate and a pH that are stable for a long period of time at room temperature (25°C) and low temperatures (5°C). These results demonstrate that the pest repellent composition for human use of the present invention maintains a stable emulsion system for a long period of time and has excellent long-term stability. [Industrial Applicability]
[0039] The human pest repellent composition of the present invention uses (B) ethyl butylacetylaminopropionate and (C) propylene glycol caprate and / or propylene glycol dicaprate in combination with the emulsifier (A) of the present invention, thereby maintaining a stable emulsion system for a long period of time, and is therefore useful as a human pest repellent formulation with excellent long-term stability.
Claims
1. (A) an emulsifier, (B) ethyl butylacetylaminopropionate, (C) propylene glycol caprate and / or propylene glycol dicaprate, and (D) containing water, The emulsifier (A) is at least one selected from the group consisting of closed vesicles formed by an amphiphilic substance which spontaneously forms closed vesicles, and particles of a polycondensation polymer having a hydroxyl group. A pest repellent composition for human use.
2. (B) Ethyl butylacetylaminopropionate, (C) dissolved in propylene glycol caprate and / or propylene glycol dicaprate, When this solution is mixed with (D) water, it is emulsified using (A) an emulsifier, The emulsifier (A) is at least one selected from the group consisting of closed vesicles formed by an amphiphilic substance which spontaneously forms closed vesicles, and particles of a polycondensation polymer having a hydroxyl group. A method for producing a pest repellent composition for human use.
Citation Information
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