JP2010094506A - Deodorant and method of manufacturing deodorant - Google Patents

Deodorant and method of manufacturing deodorant Download PDF

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JP2010094506A
JP2010094506A JP2009217416A JP2009217416A JP2010094506A JP 2010094506 A JP2010094506 A JP 2010094506A JP 2009217416 A JP2009217416 A JP 2009217416A JP 2009217416 A JP2009217416 A JP 2009217416A JP 2010094506 A JP2010094506 A JP 2010094506A
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extract
deodorant
ammonia
vetiver
water
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JP5324370B2 (en
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茂 ▲高▼木
Shigeru Takagi
Reiko Kinoshita
玲子 木下
Kuniyoshi Shimizu
邦義 清水
Ryuichiro Kondo
隆一郎 近藤
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AKARU KK
KURUME RES PARK KK
KURUME RESEARCH PARK KK
Kyushu University NUC
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AKARU KK
KURUME RES PARK KK
KURUME RESEARCH PARK KK
Kyushu University NUC
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a deodorant which has high deodorizing effect and can be used for a vital body, and to provide a method of manufacturing the deodorant. <P>SOLUTION: The deodorant contains a water soluble extract of vetiver plant. The extract solution containing the water soluble extract of vetiver plant can be used for a deodorant as it is, and also can be used for the deodorant by concentrating the extract solution by a method such as centrifugal concentration, heating concentration, vacuum concentration, and autoclave concentration to be used as the deodorant. The extract solution including the water soluble extract of vetiver plant is freeze-dried and sieved, and then micropowder under 250 micrometer meshes (60 mesh) also can be used as the deodorant. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は消臭剤及び消臭剤の製造方法に関する。詳しくは、安全性が高い天然素材を用いた消臭剤及び消臭剤の製造方法に係るものである。   The present invention relates to a deodorant and a method for producing the deodorant. Specifically, the present invention relates to a deodorant using a highly safe natural material and a method for producing the deodorant.

近年、気密性の高い住宅が増え、また、居住者の清潔志向も高まり、犬や猫等のペット臭や、生活臭を消臭したいという要望が高まっている。
また、病院や老人介護施設では、患者や老人による尿失禁等に伴う不快な尿臭(アンモニア臭)を消臭したいという要望が高まっている。
In recent years, the number of houses with high airtightness has increased, and the resident's desire for cleanliness has increased, and there has been a growing demand for deodorizing pet odors such as dogs and cats and daily odors.
In hospitals and elderly care facilities, there is an increasing demand to deodorize the unpleasant urine odor (ammonia odor) associated with urinary incontinence by patients and the elderly.

また、消臭効果の高い消臭剤の有効成分としては、各種合成化合物が知られており、これらを用いた消臭剤が多く提案されている。
例えば、特許文献1には、塩素含有の酸化剤を10〜1000ppm含み、無機塩または有機塩によってpH8〜13に調整された水溶液からなる消臭剤が記載されている。
また、特許文献2には、ジャスモン酸系化合物とデルタラクトン類を消臭成分として含有する消臭剤が記載されている。
また、特許文献3には、3d遷移金属のハロゲン化物塩を含有する水溶液からなる消臭剤が記載されている。
Various synthetic compounds are known as active ingredients of a deodorant having a high deodorizing effect, and many deodorizers using these compounds have been proposed.
For example, Patent Document 1 describes a deodorant comprising an aqueous solution containing 10 to 1000 ppm of a chlorine-containing oxidizing agent and adjusted to pH 8 to 13 with an inorganic salt or an organic salt.
Patent Document 2 describes a deodorant containing a jasmonic acid compound and a delta lactone as a deodorizing component.
Patent Document 3 describes a deodorant composed of an aqueous solution containing a halide salt of a 3d transition metal.

特開2001−316213号公報JP 2001-316213 A 特開2002−253651号公報JP 2002-253651-A 特開2002−85537号公報JP 2002-85537 A

しかしながら、これら従来の消臭剤の有効成分として用いられる化合物は、臭気の分解能は高いものの、ペットや人体が直接触れるものや、ペットや人体等の生体そのものに対して使用する場合は、安全性の面で依然として問題を有していた。   However, the compounds used as active ingredients of these conventional deodorants have high odor resolution, but are safe when used on living things such as pets and human bodies directly, or on pets and human bodies. Still had problems.

本発明は、以上の点に鑑みて創案されたものであり、消臭効果が高いと共に、生体に対しても安全に使用できる消臭剤、並びにこのような消臭剤を製造する消臭剤の製造方法を提供することを目的とする。   The present invention was devised in view of the above points, and has a high deodorizing effect and can be used safely with respect to a living body, and a deodorant for producing such a deodorant. It aims at providing the manufacturing method of.

上記の目的を達成するために、本発明の消臭剤は、ベチバー植物の抽出物を含むものである。   In order to achieve the above object, the deodorant of the present invention contains an extract of a vetiver plant.

また、本発明の消臭剤において、ベチバー植物はベチバーの根であることが好ましい。   In the deodorant of the present invention, the vetiver plant is preferably a vetiver root.

また、本発明の消臭剤において、抽出物は水溶性抽出物を含んでいることが好ましい。   In the deodorizer of the present invention, the extract preferably contains a water-soluble extract.

ここで、水溶性抽出物によって、消臭剤を液体状にすることができる。   Here, the deodorant can be made liquid by the water-soluble extract.

また、本発明の消臭剤は、水溶性抽出物の液体である場合、消臭液として散布することができる。
また、この液体は水溶液であっても、コロイド分散液であってもよい。
Moreover, the deodorizer of this invention can be sprayed as a deodorizing liquid, when it is a liquid of a water-soluble extract.
The liquid may be an aqueous solution or a colloidal dispersion.

また、本発明の消臭剤において、抽出物は乾燥粉末であり、しかも乾燥粉末は、250μm以下の大きさである場合、より高いアンモニア消臭効果が得られ、好ましい。   Moreover, in the deodorizer of this invention, when an extract is a dry powder and a dry powder is a magnitude | size of 250 micrometers or less, a higher ammonia deodorizing effect is acquired and it is preferable.

また、本発明の消臭剤において、抽出物は有機溶媒抽出物を含んでいることが好ましい。   In the deodorizer of the present invention, the extract preferably contains an organic solvent extract.

また、上記の目的を達成するために、本発明の消臭剤の製造方法は、ベチバー植物から水溶性抽出物を抽出する抽出工程を有する。
また、ベチバー植物はベチバーの根であることが好ましい。
Moreover, in order to achieve said objective, the manufacturing method of the deodorizer of this invention has an extraction process which extracts a water-soluble extract from a vetiver plant.
The vetiver plant is preferably a vetiver root.

また、本発明の消臭剤の製造方法において、抽出工程の後に、ベチバー植物またはベチバーの根の水溶性抽出物を乾燥する乾燥工程を有することが好ましい。   Moreover, in the manufacturing method of the deodorizer of this invention, it is preferable to have a drying process which dries the water-soluble extract of a vetiver plant or a vetiver root after an extraction process.

また、本発明の消臭剤の製造方法において、乾燥工程は、ベチバー植物またはベチバーの根の水溶性抽出物を凍結して乾燥することが好ましい。   Moreover, in the manufacturing method of the deodorizer of this invention, it is preferable that a drying process freezes and dries the water-soluble extract of a vetiver plant or a vetiver root.

また、本発明の消臭剤の製造方法において、乾燥工程の後に、乾燥工程によって得られた乾燥粉末を250μm以下の大きさに微細化する微細化工程を有する場合、より高いアンモニア消臭効果を有する消臭剤を製造できる。   In addition, in the method for producing a deodorant of the present invention, when a drying step is followed by a refining step for refining the dried powder obtained by the drying step to a size of 250 μm or less, a higher ammonia deodorizing effect is obtained. The deodorant which has can be manufactured.

また、本発明の消臭剤の製造方法は、ベチバー植物から有機溶媒抽出物を抽出する抽出工程を有する。   Moreover, the manufacturing method of the deodorizer of this invention has an extraction process which extracts an organic-solvent extract from a vetiver plant.

本発明に係る消臭剤は、消臭効果が高いと共に、生体に対しても安全に使用できる。
本発明に係る消臭剤の製造方法によって、消臭効果が高いと共に、生体に対しても安全に使用できる消臭剤を製造できる。
The deodorizer according to the present invention has a high deodorizing effect and can be safely used for living bodies.
With the method for producing a deodorant according to the present invention, it is possible to produce a deodorant that has a high deodorizing effect and can be safely used for a living body.

ベチバー根の抽出液のアンモニア消臭効果を示すグラフである。It is a graph which shows the ammonia deodorizing effect of the extract of a vetiver root. ベチバー根の微粉末抽出物のアンモニア消臭効果を示すグラフである。It is a graph which shows the ammonia deodorizing effect of the fine powder extract of a vetiver root. ベチバー根の抽出液と市販の天然素材系消臭剤のアンモニア消臭効果を比較したグラフである。It is the graph which compared the ammonia deodorizing effect of the extract of a vetiver root, and a commercially available natural raw material type deodorizer. 褐色成分を除去されたベチバー根の抽出液のアンモニア消臭効果を示すグラフである。It is a graph which shows the ammonia deodorizing effect of the extract of the vetiver root from which the brown component was removed. エタノール、メタノール、クロロホルムおよびイソプロパノールによってそれぞれ抽出された抽出物のアンモニア消臭試験結果を示すグラフである。It is a graph which shows the ammonia deodorization test result of the extract each extracted with ethanol, methanol, chloroform, and isopropanol. n−ヘキサン、メタノール、水および酢酸エチルによってそれぞれ抽出された抽出物のアンモニア消臭試験結果を示すグラフである。It is a graph which shows the ammonia deodorizing test result of the extract each extracted with n-hexane, methanol, water, and ethyl acetate. 酢酸エチル、メタノール、エタノールおよび水によってそれぞれ抽出された抽出物のアンモニア消臭試験結果を示すグラフである。It is a graph which shows the ammonia deodorization test result of the extract extracted with ethyl acetate, methanol, ethanol, and water, respectively. アンモニアガスと抽出物との接触から40分後における各種抽出物のアンモニア除去量のグラフである。It is a graph of the ammonia removal amount of various extracts 40 minutes after contact with ammonia gas and an extract. アンモニアガスと抽出物との接触から40分後における各種抽出物1mgあたりのアンモニア除去量のグラフである。It is a graph of the amount of ammonia removal per 1 mg of various extracts after 40 minutes from the contact between ammonia gas and the extract. 各フラクションの固形物重量を示すグラフである。It is a graph which shows the solid substance weight of each fraction. 各フラクションのアンモニア除去量を示すグラフである。It is a graph which shows the ammonia removal amount of each fraction. アンモニアガスとフラクションの接触から30分後における各フラクションのアンモニア除去量を示すグラフである。It is a graph which shows the ammonia removal amount of each fraction 30 minutes after contact with ammonia gas and a fraction. アンモニアガスとフラクションの接触から30分後における各フラクションの抽出物1mgあたりのアンモニア除去量のグラフである。It is a graph of the ammonia removal amount per 1 mg of the extract of each fraction 30 minutes after contact of ammonia gas and the fraction.

本発明を適用した消臭剤は、ベチバー植物の水溶性抽出物を含む。また、ベチバーは、インドネシア原産のイネ科の多年生草木である。   The deodorant to which the present invention is applied includes a water-soluble extract of a vetiver plant. Vetiver is a perennial plant of the grass family native to Indonesia.

また、ベチバー植物から水溶性抽出物を抽出できればどのような抽出方法でもよいが、例えば、乾燥されたベチバー植物を水に浸して、100〜125℃で30〜40分間、オートクレーブ抽出する方法や、乾燥されたベチバー植物を水に浸して、50〜65℃で1〜2時間、熱水抽出する方法が挙げられる。   Moreover, any extraction method may be used as long as a water-soluble extract can be extracted from a vetiver plant, for example, a method of immersing a dried vetiver plant in water and performing autoclave extraction at 100 to 125 ° C. for 30 to 40 minutes, Examples include a method in which a dried vetiver plant is immersed in water and extracted with hot water at 50 to 65 ° C. for 1 to 2 hours.

また、ベチバー植物の水溶性抽出物を含んだ抽出液をそのまま消臭剤として使用することができるが、抽出液を遠心濃縮、加熱濃縮、減圧濃縮、オートクレーブ濃縮等の濃縮方法で濃縮して消臭剤として使用することもできる。
また、濃縮された、ベチバー植物の水溶性抽出物を含んだ抽出液を凍結乾燥し、凍結乾燥したものを目開き250マイクロメートル(60メッシュ)以下の微粉末にして消臭剤として使用することもできる。
In addition, an extract containing a water-soluble extract of a vetiver plant can be used as a deodorant as it is, but the extract is concentrated by a concentration method such as centrifugal concentration, heat concentration, reduced pressure concentration, autoclave concentration or the like. It can also be used as an odorant.
In addition, a concentrated extract containing a water-soluble extract of a vetiver plant is freeze-dried, and the freeze-dried powder is finely powder having an opening of 250 micrometers (60 mesh) or less and used as a deodorant. You can also.

また、ベチバー植物から抽出したことにより、抽出液は褐色を呈している。しかし、抽出液に色があると衣類に散布した場合に衣類が変色してしまうため、褐色成分を除去することが好ましい。よって、例えば、抽出液を、ろ紙でろ過したり、膜孔径0.2μmのセルロース膜でろ過したり、合成吸着剤で褐色成分を吸着したりして、褐色成分を除去することが好ましい。   Moreover, the extract is exhibiting brown color by extracting from the vetiver plant. However, it is preferable to remove the brown component since the clothing will be discolored when the extract is colored when sprayed on the clothing. Therefore, for example, it is preferable to remove the brown component by filtering the extract with filter paper, filtering with a cellulose membrane having a membrane pore size of 0.2 μm, or adsorbing the brown component with a synthetic adsorbent.

また、ベチバー植物の水溶性抽出物を含む本発明の消臭剤を水に薄めて水溶液(消臭液)とし、この消臭液を加湿器等の中へ入れると部屋の臭いが消え続ける。また、洗濯水に本発明の消臭液を入れることで、衣類に付いた魚の生臭いニオイ(トリメチルアミン)、汗のニオイ(アンモニア臭)、ペット臭やタバコ臭が消臭される。また、本発明の消臭液を浴槽のお湯に入れて使用する入浴用消臭液は、加齢臭、アンモニア臭を除去しお湯の不快なニオイも抑止する。
また、本発明の消臭液によって、大腸菌やブドウ球菌等の細菌の増殖を抑えることや、ゴキブリやダニ等の害虫を寄せ付けにくくすることも期待できる。
Further, when the deodorant of the present invention containing a water-soluble extract of a vetiver plant is diluted in water to form an aqueous solution (deodorant liquid) and this deodorant liquid is put into a humidifier or the like, the odor of the room continues to disappear. In addition, by adding the deodorant of the present invention to the wash water, the fishy odor (trimethylamine), sweat odor (ammonia odor), pet odor and tobacco odor attached to the clothes are eliminated. Moreover, the deodorant for bathing which uses the deodorant of this invention in the hot water of a bathtub removes an aging odor and an ammonia odor, and also suppresses the unpleasant smell of hot water.
In addition, the deodorizing solution of the present invention can be expected to suppress the growth of bacteria such as Escherichia coli and staphylococci and make it difficult for insects such as cockroaches and mites to come close.

[アンモニア消臭試験1]
乾燥されたベチバーの根(ベチバー植物の一例である。)100gを1.8リットルの水に浸し、オートクレーブ抽出を121℃で40分間行なった後、遠心濃縮及びろ過を行なってオートクレーブ抽出液を得た。オートクレーブ抽出の水溶性成分の抽出率(ベチバー根100g当たりの水溶性成分の重さ)は、6.31%であった。なお、ろ過を行なっていない点以外は同様にオートクレーブ抽出を行なった結果、水溶性成分の抽出率は7.66%であった。
また、乾燥されたベチバーの根100gを1.8リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なった後、遠心濃縮及びろ過を行なって熱水抽出液を得た。熱水抽出の水溶性成分の抽出率は、6.42%であった。
次に、容量5リットルのテドラーバッグの口元の栓をはずし、検知管に合う太さのシリコンチューブに付け替え、試薬注入場所としてテドラーバッグの隅を折り曲げてテープで止めた。折り曲げていない端部に、容積が変わらないように切り口を入れ、約5mlに精秤した熱水抽出液を切り口から入れた後にテープで切り口に封をした。
そして、ポンプでテドラーバッグ内部の空気を抜き、積算流量計を用いて圧縮空気を4リットル入れ、クリップでシリコンチューブを閉じて密閉した。折り曲げてテープで止めていた部分即ち、熱水抽出液が付着していない部分にマイクロシリンジ(10マイクロリットル容)を刺し、25%アンモニア水3マイクロリットルを注入した。
そして、マイクロシリンジによって穴の開いた部分は、直ちにテープで閉じ、ドライヤーでテドラーバッグ全体を熱して溶液を気化させた(初期アンモニア濃度:600ppm)。その後、2分後、10分後、20分後、40分後及び80分後というように間隔を置き、検知器及び検知管を使用して、アンモニアの濃度を測定し、アンモニア残存率を算出した。
また、約5mlに精秤したオートクレーブ抽出液を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。
また、比較のために、約5mlに精秤した単なる水を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。結果を図1に示す。
[Ammonia deodorization test 1]
100 g of dried vetiver root (an example of a vetiver plant) is soaked in 1.8 liters of water and subjected to autoclave extraction at 121 ° C. for 40 minutes, followed by centrifugal concentration and filtration to obtain an autoclave extract. It was. The extraction rate of water-soluble components in autoclave extraction (weight of water-soluble components per 100 g of vetiver root) was 6.31%. In addition, as a result of performing autoclave extraction similarly except the point which is not filtering, the extraction rate of the water-soluble component was 7.66%.
Moreover, 100 g of dried vetiver roots were immersed in 1.8 liters of water, and hot water extraction was performed at 55-60 ° C. for 1.5 hours, followed by centrifugal concentration and filtration to obtain a hot water extract. . The extraction rate of the water-soluble component in the hot water extraction was 6.42%.
Next, the cap at the mouth of the 5 liter Tedlar bag was removed and replaced with a silicon tube having a thickness suitable for the detection tube, and the corner of the Tedlar bag was bent as a reagent injection place and stopped with tape. A cut end was put on the unfolded end so that the volume did not change, and a hot water extract precisely weighed to about 5 ml was put through the cut end, and then the cut end was sealed with tape.
Then, the air inside the Tedlar bag was evacuated with a pump, 4 liters of compressed air was introduced using an integrating flow meter, and the silicone tube was closed with a clip and sealed. A microsyringe (10 microliter volume) was stabbed into a portion that was bent and stopped with tape, that is, a portion to which the hot water extract was not attached, and 3 microliters of 25% ammonia water was injected.
Then, the portion where the hole was opened by the microsyringe was immediately closed with tape, and the entire Tedlar bag was heated with a dryer to vaporize the solution (initial ammonia concentration: 600 ppm). Then, after 2 minutes, 10 minutes, 20 minutes, 40 minutes and 80 minutes, the ammonia concentration is measured by using a detector and a detector tube at intervals, and the residual ammonia rate is calculated. did.
Moreover, after putting the autoclave extract accurately weighed to about 5 ml from the cut end, it was sealed with a tape and the same test as above was performed.
For comparison, simple water precisely weighed to about 5 ml was added from the cut end, and the cut end was sealed with tape, and the same test as described above was performed. The results are shown in FIG.

図1から判るように、乾燥されたベチバーの根から抽出された、オートクレーブ抽出液と熱水抽出液は、どちらもアンモニアの消臭を始めて2分経過した時点で50%以上(即ち、アンモニア残存率が50%以下)消臭した。   As can be seen from FIG. 1, both the autoclave extract and the hot water extract extracted from the dried vetiver roots are 50% or more when the deodorization of ammonia has started for 2 minutes (ie, ammonia remaining). The rate was 50% or less).

[アンモニア消臭試験2]
乾燥されたベチバーの根200gを1リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なって熱水抽出液を得た。
次に、得られた熱水抽出液を100℃で1.5時間、加熱濃縮した。水溶性成分の抽出率は、2.53±0.064%であった。加熱濃縮した後、凍結乾燥して抽出物を得た。
また、別途得られた熱水抽出液を、60℃で圧力100mmHgという条件で減圧濃縮した。水溶性成分の抽出率は、2.41±0.233%であった。減圧濃縮した後、凍結乾燥して抽出物を得た。
また、別途得られた熱水抽出液を、121℃で40分間、オートクレーブ濃縮した。水溶性成分の抽出率は、2.35±0.099%であった。オートクレーブ濃縮した後、凍結乾燥して抽出物を得た。
また、別途得られた熱水抽出液を、何ら濃縮せずに(水溶性成分の抽出率:2.94±0.486%)、凍結乾燥して抽出物を得た。
[Ammonia deodorization test 2]
200 g of dried vetiver roots were immersed in 1 liter of water, and hot water extraction was performed at 55 to 60 ° C. for 1.5 hours to obtain a hot water extract.
Next, the obtained hot water extract was heated and concentrated at 100 ° C. for 1.5 hours. The extraction rate of the water-soluble component was 2.53 ± 0.064%. After concentration by heating, the extract was freeze-dried to obtain an extract.
Further, the separately obtained hot water extract was concentrated under reduced pressure at 60 ° C. under a pressure of 100 mmHg. The extraction rate of the water-soluble component was 2.41 ± 0.233%. After concentration under reduced pressure, the extract was lyophilized to obtain an extract.
Moreover, the hot water extract obtained separately was autoclaved at 121 ° C. for 40 minutes. The extraction rate of the water-soluble component was 2.35 ± 0.099%. After concentrating in an autoclave, it was freeze-dried to obtain an extract.
Moreover, the hot water extract obtained separately was freeze-dried without concentrating at all (extraction rate of water-soluble component: 2.94 ± 0.486%) to obtain an extract.

そして、加熱濃縮後凍結乾燥して得られた抽出物を、目開き250マイクロメートル(60メッシュ)以下の微粉末に調整した。
一方、減圧濃縮後凍結乾燥して得られた熱水抽出物を、目開き250マイクロメートル(60メッシュ)以下の微粉末に調整した。
次に、容量5リットルのテドラーバッグの口元の栓をはずし、検知管に合う太さのシリコンチューブに付け替え、試薬注入場所としてテドラーバッグの隅を折り曲げてテープで止めた。折り曲げていない端部に、容積が変わらないように切り口を入れ、約0.4gに精秤した、目開き250マイクロメートル(60メッシュ)以下の微粉末に調整された減圧濃縮凍結乾燥抽出物を切り口から入れた後にテープで切り口に封をした。
そして、ポンプでテドラーバッグ内部の空気を抜き、積算流量計を用いて圧縮空気を4リットル入れ、クリップでシリコンチューブを閉じて密閉した。折り曲げてテープで止めていた部分即ち、目開き250マイクロメートル(60メッシュ)以下の微粉末に調整された減圧濃縮凍結乾燥抽出物が付着していない部分にマイクロシリンジ(10マイクロリットル容)を刺し、25%アンモニア水3マイクロリットルを注入した。
そして、マイクロシリンジによって穴の開いた部分は、直ちにテープで閉じ、ドライヤーでテドラーバッグ全体を熱して溶液を気化させた(初期アンモニア濃度:420ppm)。その後、2分後、10分後、20分後、40分後及び80分後というように間隔を置き、検知器及び検知管を使用して、アンモニアの濃度を測定し、アンモニア除去率を算出した。
また、約0.4gに精秤した、目開き250マイクロメートル(60メッシュ)以下の微粉末に調整された加熱濃縮凍結乾燥抽出物を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。結果を図2に示す。
And the extract obtained by freeze-drying after concentration by heating was adjusted to a fine powder having an opening of 250 micrometers (60 mesh) or less.
On the other hand, the hot water extract obtained by concentration under reduced pressure and freeze-drying was adjusted to a fine powder having an opening of 250 micrometers (60 mesh) or less.
Next, the cap at the mouth of the 5 liter Tedlar bag was removed and replaced with a silicon tube having a thickness suitable for the detection tube, and the corner of the Tedlar bag was bent as a reagent injection place and stopped with tape. A lyophilized extract concentrated under reduced pressure and adjusted to a fine powder with an opening of 250 micrometers (60 mesh) or less, which was cut into an unfolded end so that the volume did not change and was precisely weighed to about 0.4 g. After putting through the cut, the cut was sealed with tape.
Then, the air inside the Tedlar bag was evacuated with a pump, 4 liters of compressed air was introduced using an integrating flow meter, and the silicone tube was closed with a clip and sealed. Puncture a microsyringe (10 microliters) into the part that has been bent and secured with tape, that is, the part to which the vacuum concentrated lyophilized extract adjusted to a fine powder with an opening of 250 micrometers (60 mesh) or less is not attached. 3 microliters of 25% aqueous ammonia was injected.
Then, the portion where the hole was opened by the microsyringe was immediately closed with tape, and the entire tedlar bag was heated with a dryer to vaporize the solution (initial ammonia concentration: 420 ppm). Then, after 2 minutes, 10 minutes, 20 minutes, 40 minutes, and 80 minutes, the ammonia concentration is measured using a detector and a detector tube, and the ammonia removal rate is calculated. did.
In addition, a heat-concentrated freeze-dried extract adjusted to a fine powder with a mesh size of 250 micrometers (60 mesh) or less, precisely weighed to about 0.4 g, was put through the cut and sealed with a tape. The same test was conducted. The results are shown in FIG.

図2から判るように、乾燥されたベチバーの根から熱水抽出した後、加熱濃縮して得られた微粉末抽出物は、アンモニアの消臭を始めて2分経過した時点で80%消臭しており、また、乾燥されたベチバーの根から熱水抽出した後、減圧濃縮して得られた微粉末抽出物は、アンモニアの消臭を始めて2分経過した時点で60%消臭していた。
更に、加熱濃縮して得られた微粉末抽出物及び減圧濃縮して得られた微粉末抽出物はどちらも、アンモニアの消臭を始めて10分経過した時点で90%以上消臭していた。
従って、ベチバーの根から抽出された熱水抽出液よりも、ベチバーの根から熱水抽出した後、加熱濃縮して目開き250マイクロメートル(60メッシュ)以下の微粉末に調整された抽出物の方が、高いアンモニア消臭効果を示した。
As can be seen from FIG. 2, the fine powder extract obtained by hot water extraction from the dried vetiver root and then heating and concentration is deodorized by 80% when 2 minutes have passed since the deodorization of ammonia was started. In addition, the fine powder extract obtained by hot water extraction from dried vetiver roots and then concentration under reduced pressure was deodorized 60% when 2 minutes had passed since deodorization of ammonia was started. .
Further, both the fine powder extract obtained by heating and concentration and the fine powder extract obtained by concentration under reduced pressure were deodorized by 90% or more when 10 minutes had passed since deodorization of ammonia was started.
Therefore, the hot water extract extracted from the vetiver root is extracted with hot water from the vetiver root, and then concentrated by heating to obtain a fine powder having an opening of 250 micrometers (60 mesh) or less. The one showed a higher ammonia deodorizing effect.

[アンモニア消臭試験3]
乾燥されたベチバーの根100gを1.8リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なった後、遠心濃縮及びろ過を行ない、更に100℃で1.5時間、加熱濃縮して、ベチバー根熱水抽出液を得た。水溶性成分の抽出率は5.39%であった。
また、ベチバー根熱水抽出液と比較するため、トウモロコシ由来成分抽出液消臭剤〔ファブリーズ(登録商標)、P&G社製〕(水溶性成分の含有率:1.94g/100ml)及び、カテキン由来成分抽出液消臭剤〔リセッシュ(登録商標)、花王株式会社製〕(水溶性成分の含有率:1.11g/100ml)を用意した。
次に、容量5リットルのテドラーバッグの口元の栓をはずし、検知管に合う太さのシリコンチューブに付け替え、試薬注入場所としてテドラーバッグの隅を折り曲げてテープで止めた。折り曲げていない端部に、容積が変わらないように切り口を入れ、約3mlに精秤したベチバー根熱水抽出液を切り口から入れた後にテープで切り口に封をした。
そして、ポンプでテドラーバッグ内部の空気を抜き、積算流量計を用いて圧縮空気を4リットル入れ、クリップでシリコンチューブを閉じて密閉した。折り曲げてテープで止めていた部分即ち、ベチバー根熱水抽出液が付着していない部分にマイクロシリンジ(10マイクロリットル容)を刺し、25%アンモニア水3マイクロリットルを注入した。
そして、マイクロシリンジによって穴の開いた部分は、直ちにテープで閉じ、ドライヤーでテドラーバッグ全体を熱して溶液を気化させた(初期アンモニア濃度:400ppm)。その後、2分後、10分後、20分後及び40分後というように間隔を置き、検知器及び検知管を使用して、アンモニアの濃度を測定し、アンモニア残存率を算出した。
また、約3mlに精秤したトウモロコシ由来成分抽出液消臭剤を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。
更に、約3mlに精秤したカテキン由来成分抽出液消臭剤を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。
また、約3mlに精秤した単なる水を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。結果を図3に示す。
[Ammonia deodorization test 3]
100 g of dried vetiver root is immersed in 1.8 liters of water, and hot water extraction is performed at 55-60 ° C. for 1.5 hours, followed by centrifugal concentration and filtration, and further at 100 ° C. for 1.5 hours. Concentration by heating gave a vetiver root hot water extract. The extraction rate of the water-soluble component was 5.39%.
In addition, in order to compare with vetiver root hot water extract, corn-derived component extract deodorant [Fabries (registered trademark), manufactured by P & G Co.] (water-soluble component content: 1.94 g / 100 ml) and catechin-derived A component extract liquid deodorant [Risesh (registered trademark), manufactured by Kao Corporation] (water-soluble component content: 1.11 g / 100 ml) was prepared.
Next, the cap at the mouth of the 5 liter Tedlar bag was removed and replaced with a silicon tube having a thickness suitable for the detection tube, and the corner of the Tedlar bag was bent as a reagent injection place and stopped with tape. A cut end was put in the unfolded end so that the volume did not change, and a vetiver root hot water extract precisely weighed to about 3 ml was put through the cut end, and then the cut end was sealed with tape.
Then, the air inside the Tedlar bag was evacuated with a pump, 4 liters of compressed air was introduced using an integrating flow meter, and the silicone tube was closed with a clip and sealed. A microsyringe (10 microliter volume) was stabbed into a portion that was bent and stopped with tape, that is, a portion where the vetiver root hot water extract was not attached, and 3 microliters of 25% ammonia water was injected.
Then, the portion where the hole was opened by the microsyringe was immediately closed with tape, and the entire Tedlar bag was heated with a dryer to vaporize the solution (initial ammonia concentration: 400 ppm). Then, after 2 minutes, 10 minutes, 20 minutes, and 40 minutes, the ammonia concentration was measured using a detector and a detector tube, and the residual ammonia rate was calculated.
Moreover, after putting the corn-derived component extract deodorizer precisely weighed to about 3 ml from the cut, it was sealed with a tape and the same test as above was performed.
Further, a catechin-derived component extract deodorant precisely weighed to about 3 ml was added from the cut end, and the cut end was sealed with tape, and the same test as described above was performed.
In addition, a simple water precisely weighed to about 3 ml was added from the cut end, and then the cut end was sealed with tape, and the same test as described above was performed. The results are shown in FIG.

図3から判るように、ベチバー根熱水抽出液は、アンモニアの消臭を始めて10分経過した時点で80%を消臭(即ち、アンモニア残存率20%)したのに対して、トウモロコシ由来成分抽出液消臭剤は、アンモニアの消臭を始めて10分経過した時点で65%を消臭(即ち、アンモニア残存率35%)したに過ぎなかった。また、カテキン由来成分抽出液消臭剤は、アンモニアの消臭を始めて10分経過した時点で40%を消臭(即ち、アンモニア残存率60%)したに過ぎなかった。
更に、ベチバー根熱水抽出液は、アンモニアの消臭を始めて20分経過した後や40分経過した後もアンモニア残存率を低下させたのに対して、トウモロコシ由来成分抽出液消臭剤はアンモニアの消臭を始めて10分経過した後はほとんどアンモニア残存率に変化がなく、カテキン由来成分抽出液消臭剤にいたっては、アンモニアの消臭を始めて2分経過した後は、ほとんどアンモニア残存率に変化がなかった。
As can be seen from FIG. 3, the vetiver root hot water extract was deodorized 80% (that is, ammonia remaining rate 20%) after 10 minutes from the start of deodorization of ammonia. The extract liquid deodorant only deodorized 65% (that is, the ammonia residual ratio was 35%) when 10 minutes had passed since the deodorization of ammonia was started. In addition, the catechin-derived component extract deodorizer only deodorized 40% (that is, the ammonia remaining rate was 60%) when 10 minutes had passed since deodorization of ammonia was started.
Furthermore, the vetiver root hot water extract decreased the residual ammonia rate after 20 minutes or 40 minutes after the start of deodorization of ammonia, whereas the corn-derived component extract deodorant was ammonia. After 10 minutes from the start of deodorization, there was almost no change in the residual ammonia rate, and in the case of catechin-derived component extract liquid deodorizer, the residual ammonia rate was almost 2 minutes after the start of deodorization of ammonia. There was no change.

[アンモニア消臭試験4]
乾燥されたベチバーの根100gを1.8リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なった後、得られた熱水抽出液を、ろ紙によってろ過し、更に膜孔径0.2μmのセルロース膜によってろ過し、褐色成分が除去された第1のベチバー根熱水抽出液を得た。
また、乾燥されたベチバーの根100gを1.8リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なった後、得られた熱水抽出液を、ろ紙によってろ過し、更に膜孔径0.2μmのセルロース膜によってろ過し、その後、合成吸着剤〔ダイヤイオン(登録商標)HP20、三菱化学社製〕で更に褐色成分を吸着して、褐色成分が除去された第2のベチバー根熱水抽出液を得た。
また、乾燥されたベチバーの根100gを1.8リットルの水に浸し、熱水抽出を55〜60℃で1.5時間行なった後、得られた熱水抽出液を、ろ紙によってろ過し、更に膜孔径0.2μmのセルロース膜によってろ過し、その後、合成吸着剤〔セパビーズ(登録商標)SP207、三菱化学社製〕で更に褐色成分を吸着して、褐色成分が除去された第3のベチバー根熱水抽出液を得た。
次に、容量5リットルのテドラーバッグの口元の栓をはずし、検知管に合う太さのシリコンチューブに付け替え、試薬注入場所としてテドラーバッグの隅を折り曲げてテープで止めた。折り曲げていない端部に、容積が変わらないように切り口を入れ、約3mlに精秤した第1のベチバー根熱水抽出液を切り口から入れた後にテープで切り口に封をした。
そして、ポンプでテドラーバッグ内部の空気を抜き、積算流量計を用いて圧縮空気を4リットル入れ、クリップでシリコンチューブを閉じて密閉した。折り曲げてテープで止めていた部分即ち、第1のベチバー根熱水抽出液が付着していない部分にマイクロシリンジ(10マイクロリットル容)を刺し、25%アンモニア水3マイクロリットルを注入した。
そして、マイクロシリンジによって穴の開いた部分は、直ちにテープで閉じ、ドライヤーでテドラーバッグ全体を熱して溶液を気化させた(初期アンモニア濃度:400ppm)。その後、2分後、10分後、20分後及び40分後というように間隔を置き、検知器及び検知管を使用して、アンモニアの濃度を測定し、アンモニア残存率を算出した。
また、約3mlに精秤した第2のベチバー根熱水抽出液を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。
更に、約3mlに精秤した第3のベチバー根熱水抽出液を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。
また、約3mlに精秤した単なる水を切り口から入れた後にテープで切り口に封をして、上記と同様の試験を行なった。結果を図4に示す。
[Ammonia deodorization test 4]
100 g of dried vetiver roots were soaked in 1.8 liters of water and subjected to hot water extraction at 55 to 60 ° C. for 1.5 hours, and then the obtained hot water extract was filtered through filter paper, and further membrane The mixture was filtered through a cellulose membrane having a pore size of 0.2 μm to obtain a first vetiver root hot water extract from which the brown component was removed.
Further, after immersing 100 g of dried vetiver roots in 1.8 liters of water and performing hot water extraction at 55-60 ° C. for 1.5 hours, the obtained hot water extract was filtered through a filter paper, Further filtered through a cellulose membrane having a membrane pore size of 0.2 μm, and then the brown component was removed by further adsorbing the brown component with a synthetic adsorbent [Diaion (registered trademark) HP20, manufactured by Mitsubishi Chemical Corporation]. A vetiver root hot water extract was obtained.
Further, after immersing 100 g of dried vetiver roots in 1.8 liters of water and performing hot water extraction at 55-60 ° C. for 1.5 hours, the obtained hot water extract was filtered through a filter paper, Further filtered through a cellulose membrane having a membrane pore size of 0.2 μm, and then a third vetiver from which the brown component was removed by further adsorbing the brown component with a synthetic adsorbent [Separbeads (registered trademark) SP207, manufactured by Mitsubishi Chemical Corporation]. A root hot water extract was obtained.
Next, the cap at the mouth of the 5 liter Tedlar bag was removed and replaced with a silicon tube having a thickness suitable for the detection tube, and the corner of the Tedlar bag was bent as a reagent injection place and stopped with tape. A cut was made at the unfolded end so that the volume did not change, and the first vetiver root hot water extract precisely weighed to about 3 ml was put through the cut and then sealed with tape.
Then, the air inside the Tedlar bag was evacuated with a pump, 4 liters of compressed air was introduced using an integrating flow meter, and the silicone tube was closed with a clip and sealed. A microsyringe (10 microliter volume) was pierced into the portion that was bent and stopped with tape, that is, the portion where the first vetiver root hot water extract was not adhered, and 3 microliters of 25% ammonia water was injected.
Then, the portion where the hole was opened by the microsyringe was immediately closed with tape, and the entire Tedlar bag was heated with a dryer to vaporize the solution (initial ammonia concentration: 400 ppm). Then, after 2 minutes, 10 minutes, 20 minutes, and 40 minutes, the ammonia concentration was measured using a detector and a detector tube, and the residual ammonia rate was calculated.
Moreover, after putting the 2nd vetiver root hot water extract precisely weighed to about 3 ml from a cut end, it sealed the cut end with the tape, and performed the same test as the above.
Further, a third vetiver root hot water extract precisely weighed to about 3 ml was put through the cut end, and then the cut end was sealed with tape, and the same test as described above was performed.
In addition, a simple water precisely weighed to about 3 ml was added from the cut end, and then the cut end was sealed with tape, and the same test as described above was performed. The results are shown in FIG.

図3と図4の比較から判るように、ベチバー根熱水抽出液は、セルロース膜や合成吸着剤によって褐色成分が除去されても、カテキン由来成分抽出液消臭剤よりもアンモニア消臭効果が高かった。   As can be seen from the comparison between FIG. 3 and FIG. 4, the vetiver root hot water extract is more effective in deodorizing ammonia than the catechin-derived component extract deodorant even when the brown component is removed by the cellulose membrane or the synthetic adsorbent. it was high.

[各種抽出物の抽出率]
乾燥されたベチバーの根をウィレー式粉砕機にて粉砕して得られたベチバー根粉砕物1gを純水10mlに浸し、オートクレーブ抽出を121℃で40分間行なった後、ろ過した。ろ液は遠心濃縮した。次に、ろ過して得られた残渣物を純水10mlに浸し、オートクレーブ抽出を121℃で40分間行なった後、ろ過した。ろ液は遠心濃縮した。そして、得られた残渣物に対して同様にオートクレーブ抽出を行ない、残渣物を得て、ろ液は遠心濃縮した。すなわち、合計3回の抽出を行なった。
そして、抽出に用いたベチバー根の重量に対して抽出された固形物重量により、抽出率(%)を算出した。結果を、溶媒比などの抽出条件と共に表1に示す。
一方、抽出に用いる溶媒として、純水の代わりに「純水とエタノール10%」や「純水とエタノール20%」を用いて、同様にオートクレーブ抽出を行なった。
[Extraction rate of various extracts]
1 g of vetiver root pulverized product obtained by pulverizing the dried vetiver roots with a Willet pulverizer was immersed in 10 ml of pure water, followed by autoclave extraction at 121 ° C. for 40 minutes, followed by filtration. The filtrate was concentrated by centrifugation. Next, the residue obtained by filtration was immersed in 10 ml of pure water, followed by autoclave extraction at 121 ° C. for 40 minutes, followed by filtration. The filtrate was concentrated by centrifugation. And the autoclave extraction was similarly performed with respect to the obtained residue, the residue was obtained, and the filtrate was concentrated by centrifugation. That is, extraction was performed three times in total.
And extraction rate (%) was computed with the solid substance weight extracted with respect to the weight of the vetiver root used for extraction. The results are shown in Table 1 together with extraction conditions such as solvent ratio.
On the other hand, autoclave extraction was similarly performed using “pure water and ethanol 10%” or “pure water and ethanol 20%” instead of pure water as a solvent used for extraction.

また、乾燥されたベチバーの根を、切断鋏で1cm長に切断して得られた1cm長ベチバー根1gをn−ヘキサン18mlに浸し、150rpmの条件で振とう抽出を20℃で24時間行なった後、ろ過した。ろ液は遠心濃縮した。次に、ろ過して得られた残渣物をn−ヘキサン18mlに浸し、150rpmの条件で振とう抽出を20℃で24時間行なった後、ろ過した。ろ液は遠心濃縮した。そして、抽出に用いたベチバー根の重量に対して抽出された固形物重量により、抽出率(%)を算出した。結果を、溶媒比などの抽出条件と共に表1に示す。
一方、抽出に用いる有機溶媒として、n−ヘキサンの代わりに、メタノール、エタノール、酢酸エチル、クロロホルム、イソプロパノール(2−プロパノール)を用いて、同様に振とう抽出を行なった。なお、メタノールを溶媒として用いた場合には、乾燥されたベチバーの根をウィレー式粉砕機にて粉砕して得られたベチバー根粉砕物1gについても振とう抽出を行なった。
Further, 1 g of a 1 cm long vetiver root obtained by cutting the dried vetiver root into 1 cm length with a cutting shear was immersed in 18 ml of n-hexane, and subjected to extraction by shaking at 20 ° C. for 24 hours. Then, it filtered. The filtrate was concentrated by centrifugation. Next, the residue obtained by filtration was soaked in 18 ml of n-hexane, and subjected to extraction with shaking at 150 rpm for 24 hours, followed by filtration. The filtrate was concentrated by centrifugation. And extraction rate (%) was computed with the solid substance weight extracted with respect to the weight of the vetiver root used for extraction. The results are shown in Table 1 together with extraction conditions such as solvent ratio.
On the other hand, as an organic solvent used for extraction, instead of n-hexane, methanol, ethanol, ethyl acetate, chloroform, and isopropanol (2-propanol) were used for extraction with shaking. When methanol was used as a solvent, 1 g of vetiver root pulverized product obtained by pulverizing dried vetiver roots with a Willet pulverizer was also subjected to shaking extraction.

Figure 2010094506
Figure 2010094506

表1から判断すると、抽出方法に関して、ベチバー根に含まれる成分の抽出率は、抽出回数や、溶媒と成分との比率よりも、溶出に用いる溶媒に依存すると考えられる。しかし、純水を用いて加熱や加圧する(オートクレーブ)抽出方法が最も回収率が高いことから、熱や圧力をかけることによって抽出される化合物は、オートクレーブ処理した純水抽出物中のみに含まれるものと思われる。
また、有機溶媒を用いた抽出方法のみで比較すると、メタノール抽出物が最も高い抽出率を示した。また、ベチバー根粉砕物と1cm長ベチバー根いずれを用いても抽出率に大きな違いは認められなかった。従って、ベチバー根の形状としては、粉砕物と1cm長のどちらを用いても良いものと考えられる。
また、抽出物の色に関しては、有機溶媒抽出物は、淡い黄色、赤褐色あるいは茶褐色を呈することが分かった。また、純水あるいは純水に10〜20%のエタノールを添加して抽出した抽出物に関しては、淡い黄色を呈した。つまり、褐色色素成分は、有機溶媒を用いて抽出した際により多く抽出されるものと考えられる。
Judging from Table 1, regarding the extraction method, the extraction rate of the components contained in the vetiver root is considered to depend on the solvent used for elution rather than the number of extractions and the ratio of the solvent to the components. However, the extraction method that heats or pressurizes with pure water (autoclave) has the highest recovery rate, so the compound extracted by applying heat or pressure is contained only in the autoclaved pure water extract. It seems to be.
In addition, when compared only with the extraction method using an organic solvent, the methanol extract showed the highest extraction rate. In addition, no significant difference was observed in the extraction rate when using either a vetiver root pulverized product or a 1 cm long vetiver root. Therefore, it is considered that either crushed material or 1 cm length may be used as the shape of the vetiver root.
In addition, regarding the color of the extract, it was found that the organic solvent extract had a pale yellow, reddish brown or brown color. Moreover, the extract extracted by adding 10 to 20% ethanol to pure water or pure water exhibited a pale yellow color. That is, it is considered that the brown pigment component is more extracted when extracted using an organic solvent.

[アンモニア消臭試験5]
ろ紙に、ベチバーの根から各種溶媒を用いて抽出された抽出液(抽出物濃度:20mg/ml)を1ml添加し、約24時間、真空デシケータで溶媒を完全に除去させた。
次に、抽出液が添加されたろ紙とアンモニアガスを容量1リットルのテドラーバッグ内で接触させ、0分後、0.5分後、10分後、20分後および40分後の系内濃度を測定した。測定は、ガラス検知管(ガステック社製)を用いて行なった。
また、比較対照として、溶媒のみが添加されたろ紙を用意し、約24時間、真空デシケータで溶媒を完全に除去させた後、このろ紙(無添加ろ紙)とアンモニアガスを容量1リットルのテドラーバッグ内で接触させ、0分後、0.5分後、10分後、20分後および40分後の系内濃度を測定した。
また、用いた溶媒は、エタノール、メタノール、クロロホルム、イソプロパノール、n−ヘキサン、水、および酢酸エチルである。
[Ammonia deodorization test 5]
1 ml of an extract (extract concentration: 20 mg / ml) extracted from various roots of vetiver roots was added to the filter paper, and the solvent was completely removed with a vacuum desiccator for about 24 hours.
Next, the filter paper to which the extract is added is brought into contact with ammonia gas in a 1 liter Tedlar bag, and the concentration in the system after 0 minutes, 0.5 minutes, 10 minutes, 20 minutes and 40 minutes is determined. It was measured. The measurement was performed using a glass detector tube (manufactured by Gastec).
In addition, as a control for comparison, a filter paper to which only the solvent is added is prepared, and after removing the solvent completely with a vacuum desiccator for about 24 hours, the filter paper (no added filter paper) and ammonia gas are placed in a 1 liter Tedlar bag. The concentration in the system was measured after 0 minute, 0.5 minute, 10 minutes, 20 minutes and 40 minutes.
Moreover, the solvent used is ethanol, methanol, chloroform, isopropanol, n-hexane, water, and ethyl acetate.

結果を図5〜図7に示す。なお、図5(a)、図6(a)および図7(a)は、アンモニア濃度と経過時間との関係を示したグラフであり、図5(b)、図6(b)および図7(b)は、アンモニア残存率と経過時間との関係を示したグラフである。ここで、アンモニア残存率は、ブランク(無添加ろ紙)を100として算出した。   The results are shown in FIGS. 5 (a), 6 (a) and 7 (a) are graphs showing the relationship between the ammonia concentration and the elapsed time, and FIG. 5 (b), FIG. 6 (b) and FIG. (B) is the graph which showed the relationship between ammonia residual rate and elapsed time. Here, the ammonia residual ratio was calculated with a blank (non-added filter paper) as 100.

また、図8に、アンモニアガスと抽出物との接触から40分後における各種抽出物のアンモニア除去量のグラフを示し、図9に、アンモニアガスと抽出物との接触から40分後における各種抽出物1mgあたりのアンモニア除去量のグラフを示す。   FIG. 8 shows a graph of the amount of ammonia removed from various extracts after 40 minutes from the contact between the ammonia gas and the extract. FIG. 9 shows various extractions after 40 minutes from the contact between the ammonia gas and the extract. The graph of the amount of ammonia removal per 1 mg of a thing is shown.

図5〜図9から分かるように、各種抽出物間のアンモニア消臭効果を比較した結果、メタノール抽出物が最も高い効果を示すことが分かった。
また、n−ヘキサンや酢酸エチルなどの比較的極性の低い溶媒の抽出物では、アンモニア消臭効果が低かった。これらの消臭効果の結果と、先に示した抽出物の性状から、ベチバー根に含まれるアンモニア消臭効果を持つ物質としては、比較的親水性が高い成分である、加熱や加圧処理によっても変性しない、褐色色素成分である等、幾つかの化学的な特徴を有すると考えられる。
また、ベチバー根に含まれる対アンモニア有効成分をより効率良く抽出する方法として、有機溶媒で抽出するのであれば、メタノール、イソプロパノール、エタノールのような比較的極性の高い溶媒を用いる方がより多くの有効成分を抽出することができ、純水で抽出するのであれば、オートクレーブ抽出を用いる方がより多くの有効成分を抽出することができると考えられる。
As can be seen from FIG. 5 to FIG. 9, as a result of comparing the ammonia deodorizing effect between the various extracts, it was found that the methanol extract showed the highest effect.
In addition, an ammonia deodorizing effect was low in an extract of a relatively low-polarity solvent such as n-hexane or ethyl acetate. From the results of these deodorizing effects and the properties of the extract shown above, as a substance having an ammonia deodorizing effect contained in the vetiver root, it is a component with relatively high hydrophilicity by heating or pressurizing treatment. It is considered that it has some chemical characteristics such as a non-denaturing and brown pigment component.
In addition, as a method for more efficiently extracting the active ingredient for ammonia contained in the vetiver root, if extraction is performed with an organic solvent, it is more likely to use a relatively polar solvent such as methanol, isopropanol, or ethanol. If the active ingredient can be extracted and extracted with pure water, it is considered that more active ingredients can be extracted by using autoclave extraction.

[シリカゲルカラム分画による消臭活性画分]
シリカゲルカラムクロマトグラフィにて、ベチバー根のメタノール抽出物を分画した。また、ベチバー根の粉砕物200.191gをメタノール1800mlで2回抽出した後、2回の抽出物を混合してエバポレータで濃縮および乾固させて試料を得た。
また、この試料を用いて、表2に示すように、n−ヘキサン100%/酢酸エチル0%からメタノール100%/酢酸エチル0%まで逐次、展開溶媒の極性を変えて溶出させて、合計81のフラクション(抽出分画物)に分画した(抽出物回収率93.20%)。
また、シリカゲルカラムクロマトグラフィ分画条件は以下のとおりである。
すなわち、シリカゲルとしてWakogelC−200(商品名、和光純薬工業社製)(75−150μm)を用い、メタノール抽出物20.265g、吸着させたシリカゲル量60.027g、カラム直径10.5cm、カラム長さ97cm、展開幅35.5cm、カラム体積30.7L、シリカゲル量1600.20gであった。
[Deodorizing active fraction by silica gel column fractionation]
The methanol extract of vetiver root was fractionated by silica gel column chromatography. Further, 200.191 g of ground vetiver roots were extracted twice with 1800 ml of methanol, and then the two extracts were mixed, concentrated and dried with an evaporator to obtain a sample.
Further, using this sample, as shown in Table 2, the elution was carried out by changing the polarity of the developing solvent sequentially from n-hexane 100% / ethyl acetate 0% to methanol 100% / ethyl acetate 0% for a total of 81 The fraction (extracted fraction) was fractionated (extract recovery rate 93.20%).
The silica gel column chromatography fractionation conditions are as follows.
That is, Wakogel C-200 (trade name, manufactured by Wako Pure Chemical Industries, Ltd.) (75-150 μm) was used as the silica gel, the methanol extract 20.265 g, the amount of adsorbed silica gel 60.027 g, the column diameter 10.5 cm, the column length The length was 97 cm, the developed width was 35.5 cm, the column volume was 30.7 L, and the amount of silica gel was 1600.20 g.

Figure 2010094506
Figure 2010094506

次に、1フラクションにつき、500〜1000mlずつ分取した。
そして、分画した後、すみやかにエバポレータにて濃縮して乾固させ、固形物重量を計測した。各フラクションの固形物重量を図10に示す。
図10から分かるように、第12フラクションから第14フラクションあたり、あるいは第61フラクションから第69フラクションにかけて、特に多くの化合物を含むことが推察された。
Next, 500-1000 ml was fractionated per fraction.
Then, after fractionation, the mixture was immediately concentrated by an evaporator to dryness, and the weight of solid matter was measured. The solid weight of each fraction is shown in FIG.
As can be seen from FIG. 10, it was inferred that a particularly large amount of compound was contained from the 12th fraction to the 14th fraction or from the 61st fraction to the 69th fraction.

次に、各フラクションの固形物2mgを溶媒10μlで溶解して得た液を、ろ紙に添加し、そして約24時間、真空デシケータにて溶媒を完全に除去した。そして、ろ紙とアンモニアガスを、容量100mlの三角フラスコ内で接触させた。各フラクションのアンモニア除去量を図11に示す。図11中、「MeOH」はメタノールを意味する。
また、アンモニア除去量は、無添加ろ紙と、試料添加ろ紙の系内アンモニア濃度から算出した。また、エピカテキンガレート(ECg)およびカテキン(C)は、これまでアンモニア消臭に効果があることが報告されていることから、比較のため使用した。
なお、使用した三角フラスコは、口に穴の開いたゴム栓が付けられ、穴には直径5mm、長さ10cmのガラス管を三角フラスコの内外に貫通するような形で差し込まれたものである。ガラス管の外側(三角フラスコから外に突出した部分)には、長さ15cmのゴムチューブを付け、そのゴムチューブを半分から折ってクリップで挟み、三角フラスコ内の気体が外へ漏れ出ないようにした。
Next, a solution obtained by dissolving 2 mg of solids in each fraction with 10 μl of solvent was added to the filter paper, and the solvent was completely removed with a vacuum desiccator for about 24 hours. Then, the filter paper and ammonia gas were brought into contact in an Erlenmeyer flask having a capacity of 100 ml. The amount of ammonia removed from each fraction is shown in FIG. In FIG. 11, “MeOH” means methanol.
Moreover, the ammonia removal amount was calculated from the ammonia concentration in the system of the non-added filter paper and the sample-added filter paper. Epicatechin gallate (ECg) and catechin (C) were used for comparison because they have been reported to be effective in deodorizing ammonia.
In addition, the used Erlenmeyer flask was attached with a rubber stopper having a hole in its mouth, and a glass tube having a diameter of 5 mm and a length of 10 cm was inserted into the hole so as to penetrate inside and outside of the Erlenmeyer flask. . At the outside of the glass tube (the part that protrudes out of the Erlenmeyer flask), attach a rubber tube with a length of 15 cm, fold the rubber tube from the half and hold it with a clip so that the gas in the Erlenmeyer flask does not leak out. I made it.

図11から分かるように、網羅的なスクリーニングの結果から、第17フラクション、第26〜28フラクション、第41〜43フラクション、第60〜64フラクション、第68フラクション、第69フラクション及び第74〜81フラクションは、系内のアンモニア濃度が、無添加ろ紙よりも20ppm以上減少しており、アンモニア消臭効果を持つ成分が含まれていることが推測された。
そこで、メタノール抽出物を比較対照として、これらのフラクションの中から、第17フラクション、第27フラクション、第41フラクション、第63フラクション、第69フラクション及び第78フラクションについて、容量1リットルのテドラーバッグを用いてアンモニア消臭試験を行なった。結果を図12及び図13に示す。図12は、アンモニアガスとフラクションの接触から30分後における各フラクションのアンモニア除去量を示すグラフであり、図13は、アンモニアガスとフラクションの接触から30分後における各フラクションの抽出物1mgあたりのアンモニア除去量のグラフを示す。
As can be seen from FIG. 11, from the results of comprehensive screening, the 17th fraction, the 26th to 28th fraction, the 41st to 43rd fraction, the 60th to 64th fraction, the 68th fraction, the 69th fraction and the 74th to 81st fraction. The ammonia concentration in the system was reduced by 20 ppm or more than the additive-free filter paper, and it was estimated that a component having an ammonia deodorizing effect was contained.
Therefore, using a methanol extract as a comparative control, among these fractions, the 17th fraction, the 27th fraction, the 41st fraction, the 63rd fraction, the 69th fraction and the 78th fraction were used using a 1 liter Tedlar bag. An ammonia deodorization test was conducted. The results are shown in FIGS. FIG. 12 is a graph showing the amount of ammonia removed from each fraction 30 minutes after the contact between the ammonia gas and the fraction, and FIG. 13 shows the amount per 1 mg of the extract of each fraction 30 minutes after the contact between the ammonia gas and the fraction. The graph of ammonia removal amount is shown.

図12および図13から分かるように、特に第17フラクション及び第41フラクションに関しては、メタノール抽出物と同等の消臭効果を示すことが分かった。また、各種溶媒抽出物間でのアンモニア消臭効果を検討した実験結果(図9)と比較して、抽出物1mgあたりの吸着量が減少した。
しかし、用いたフラクションは、メタノール抽出物を用いて分画して得られたもので、その効果を検討しており、第17フラクション、第27フラクション、第41フラクションおよび第63フラクションは特にアンモニアに対して有効な成分を含むことが示唆される。
また、これらの結果を、分画条件と併せて考えると、ベチバー根のメタノール抽出物に含まれる、アンモニアに対する有効成分は化学的な特徴が異なり、幾つかのまとまったフラクションに分散していることが推測される。
As can be seen from FIGS. 12 and 13, it was found that the 17th and 41st fractions exhibited the same deodorizing effect as the methanol extract. Moreover, the adsorption amount per 1 mg of extract decreased compared with the experimental result (FIG. 9) which examined the ammonia deodorizing effect between various solvent extracts.
However, the fractions used were obtained by fractionation using a methanol extract, and the effects of these fractions have been studied. The 17th, 27th, 41st and 63rd fractions are particularly ammonia. It is suggested that it contains an effective ingredient.
When these results are considered together with the fractionation conditions, the active ingredient for ammonia contained in the vetiver root methanol extract has different chemical characteristics and is dispersed in several fractions. Is guessed.

以上のように、ベチバーの根から熱水抽出された水溶性抽出物を含む抽出液(ベチバー根熱水抽出液)は、アンモニアの消臭を開始して2分経過した時点で50%以上も消臭することができるという高い消臭効果を有し、天然素材であるベチバーの根から抽出された抽出液なので、生体に対しても安全に使用できる。   As described above, the extract containing the water-soluble extract extracted from the roots of vetiver (vetiver root hot water extract) is 50% or more after 2 minutes from the start of deodorization of ammonia. It has a high deodorizing effect that it can be deodorized, and since it is an extract extracted from the roots of vetiver, which is a natural material, it can be safely used for living organisms.

更に、ベチバー根熱水抽出液は、市販されているトウモロコシ由来成分抽出液消臭剤やカテキン由来成分抽出液消臭剤よりも、時間を経るごとに高いアンモニア消臭効果を示す。   Further, the vetiver root hot water extract shows a higher ammonia deodorizing effect as time passes than commercially available corn-derived component extract deodorants and catechin-derived component extract deodorants.

また、ベチバーの根から抽出したことにより、抽出液は褐色を呈しているが、抽出液に色があると衣類に散布した場合に衣類が変色してしまうため、褐色成分を除去することが好ましいが、褐色成分を除去しても、ベチバー根熱水抽出液はカテキン由来成分抽出液消臭剤よりアンモニア消臭効果が高い。   In addition, although the extract has a brown color due to extraction from the roots of vetiver, it is preferable to remove the brown component because the color of the extract will change when sprayed on the clothing. However, even if the brown component is removed, the vetiver root hot water extract has a higher ammonia deodorizing effect than the catechin-derived component extract deodorant.

また、ベチバー根熱水抽出液は水溶液であるので、散布することができ、従って、非常に簡便に使用することができて用途も広い。また、ベチバー根熱水抽出液という天然素材のみで構成された消臭剤なので、散布しても、べたつきの心配は一切ない。   Further, since the vetiver root hot water extract is an aqueous solution, it can be sprayed, and thus can be used very easily and has a wide range of applications. In addition, since it is a deodorant composed only of a natural material called vetiver root hot water extract, there is no worry about stickiness even when sprayed.

また、ベチバーの根から有機溶媒抽出、特にメタノール抽出されたメタノール抽出物は、水抽出された水溶性抽出物よりもアンモニア除去量が多く、よって高いアンモニア消臭効果を有する。   In addition, a methanol extract obtained by organic solvent extraction, particularly methanol extraction from vetiver root, has a larger amount of ammonia removal than a water-soluble extract obtained by water extraction, and thus has a high ammonia deodorizing effect.

Claims (15)

ベチバー植物の抽出物を含む
消臭剤。
Deodorant containing vetiver plant extract.
前記ベチバー植物はベチバーの根である
請求項1に記載の消臭剤。
The deodorizer according to claim 1, wherein the vetiver plant is a vetiver root.
前記抽出物は水溶性抽出物を含んでいる
請求項1または請求項2に記載の消臭剤。
The deodorizer according to claim 1 or 2, wherein the extract contains a water-soluble extract.
前記水溶性抽出物の液体である
請求項3に記載の消臭剤。
The deodorizer according to claim 3, which is a liquid of the water-soluble extract.
前記液体は水溶液である
請求項4に記載の消臭剤。
The deodorizer according to claim 4, wherein the liquid is an aqueous solution.
前記液体はコロイド分散液である
請求項4に記載の消臭剤。
The deodorizer according to claim 4, wherein the liquid is a colloidal dispersion.
前記抽出物は、乾燥粉末である
請求項1〜3のいずれか1つに記載の消臭剤。
The deodorizer according to any one of claims 1 to 3, wherein the extract is a dry powder.
前記乾燥粉末は、250μm以下の大きさである
請求項7に記載の消臭剤。
The deodorizer according to claim 7, wherein the dry powder has a size of 250 μm or less.
前記抽出物は有機溶媒抽出物を含んでいる
請求項1または請求項2に記載の消臭剤。
The deodorizer according to claim 1 or 2, wherein the extract contains an organic solvent extract.
ベチバー植物から水溶性抽出物を抽出する抽出工程を有する
消臭剤の製造方法。
A method for producing a deodorant comprising an extraction step of extracting a water-soluble extract from a vetiver plant.
前記ベチバー植物はベチバーの根である
請求項10に記載の消臭剤の製造方法。
The method for producing a deodorant according to claim 10, wherein the vetiver plant is a vetiver root.
前記抽出工程の後に、前記水溶性抽出物を乾燥する乾燥工程を有する
請求項10または請求項11に記載の消臭剤の製造方法。
The method for producing a deodorant according to claim 10, further comprising a drying step of drying the water-soluble extract after the extraction step.
前記乾燥工程は、前記水溶性抽出物を凍結して乾燥する
請求項12に記載の消臭剤の製造方法。
The method for producing a deodorant according to claim 12, wherein in the drying step, the water-soluble extract is frozen and dried.
前記乾燥工程の後に、前記乾燥工程によって得られた乾燥粉末を250μm以下の大きさに微細化する微細化工程を有する
請求項12に記載の消臭剤の製造方法。
The method for producing a deodorant according to claim 12, further comprising a refining step for refining the dry powder obtained by the drying step to a size of 250 μm or less after the drying step.
ベチバー植物から有機溶媒抽出物を抽出する抽出工程を有する
消臭剤の製造方法。
A method for producing a deodorant comprising an extraction step of extracting an organic solvent extract from a vetiver plant.
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