JPH01165595A - Physiologically active substance - Google Patents

Physiologically active substance

Info

Publication number
JPH01165595A
JPH01165595A JP62325788A JP32578887A JPH01165595A JP H01165595 A JPH01165595 A JP H01165595A JP 62325788 A JP62325788 A JP 62325788A JP 32578887 A JP32578887 A JP 32578887A JP H01165595 A JPH01165595 A JP H01165595A
Authority
JP
Japan
Prior art keywords
propolis
solvent extract
physiologically active
cation exchange
exchange resin
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP62325788A
Other languages
Japanese (ja)
Inventor
Masami Torii
鳥井 真美
Hideyoshi Cho
秀吉 長
Takeshi Kanamori
武 金森
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lion Corp
Original Assignee
Lion Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lion Corp filed Critical Lion Corp
Priority to JP62325788A priority Critical patent/JPH01165595A/en
Publication of JPH01165595A publication Critical patent/JPH01165595A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To obtain the title substance impairing no original antimicrobial effect of solvent extract of propolis and having remarkably improved color tone and flavor and useful in blending with an oral cavity-applying composition such as dentifrice, by treating the solvent extract of propolis with a specific absorbent. CONSTITUTION:A solvent extract of propolis is subjected to absorption treatment with a active carbon having 5-20Angstrom average pore size and/or cation exchange resin to provide the aimed substance. Furthermore, the active carbon and cation exchange resin are preferably each used at amounts of 1-3 times and 1-4 times based on the dried weight of solvent extract of propolis. The above-mentioned absorption treatment is preferably carried out at 5-40 deg.C for 15min-3day.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、プロポリスの溶剤抽出物からなる生理活性物
質に関し、更に詳述すればキャンデー。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a physiologically active substance comprising a solvent extract of propolis, and more specifically to a candy.

チューインガム、洗口剤、歯磨等の口腔内で適用される
組成物に配合するのに適した生理活性物質に関する。
The present invention relates to physiologically active substances suitable for inclusion in compositions applied in the oral cavity, such as chewing gum, mouth rinses, and toothpastes.

〔従来の技術及び発明が解決しようとする問題点〕プロ
ポリスは、ミツバチがその行動圏にある種々の植物から
採取してきた樹脂状の物質を素材として巣箱内に塗布し
た粘着性で複雑な組成の生産物の一つであり、古くから
薬理的効能が伝承されて民間療法に利用されてきた。ま
た、主に東欧諸国では5種々の薬理試験や臨床への応用
が行なわれると共に、プロポリスに多様な生理活性効果
があることから、そ′の成分同定が盛んに研究されてき
た。
[Prior art and problems to be solved by the invention] Propolis is a sticky and complex composition that is applied inside the hive using a resin-like substance that bees collect from various plants in their home range. It is one of the products, and its pharmacological efficacy has been handed down since ancient times and has been used in folk medicine. In addition, various pharmacological tests and clinical applications have been conducted mainly in Eastern European countries, and since propolis has various physiologically active effects, the identification of its components has been actively researched.

従来、かかるプロポリスの生理活性効果、例えば抗菌効
果、抗炎症効果等を利用するため、プロポリスの溶剤抽
出物を用いることが知られているが、プロポリスの溶剤
抽出物は香味1色調が悪く、配合特性に劣るもので、特
にキャンデー、チューインガム、洗口剤、歯磨、等の口
腔内で適用される組成物に配合することは使用感の点か
ら困難であった。即ち、プロポリスの溶剤抽出物をかか
る組成物に配合する場合、一般には生理活性の有効性を
考慮すると0.1〜25%程度の配合量とすることが好
ましいが、このような配合量になるとプロポリスの持つ
泥くさい香味、舌、喉への刺激性が高くなって組成物の
風味を損ない、嗜好性を著しく低下させてしまうもので
あり、またその色調も黒褐色であるため1組成物を褐変
させてしまうものであった。
Conventionally, it has been known to use a solvent extract of propolis to utilize the physiologically active effects of propolis, such as antibacterial effects and anti-inflammatory effects, but the solvent extract of propolis has a poor flavor and color tone, and is difficult to blend. Due to its poor properties, it has been difficult to incorporate it into compositions applied in the oral cavity, such as candies, chewing gums, mouthwashes, toothpastes, etc., from the viewpoint of the feeling of use. That is, when a solvent extract of propolis is added to such a composition, it is generally preferable to use an amount of about 0.1 to 25% in consideration of the effectiveness of its physiological activity. Propolis has a muddy flavor and is highly irritating to the tongue and throat, impairing the flavor of the composition and significantly reducing palatability.Also, since its color is dark brown, it may cause browning of the composition. It was something that would end up happening.

従って、プロポリスの溶剤抽出物の配合特性を改善する
ことが望まれるが、従来、特開昭61−197523号
にプロポリスの溶剤抽出物の水分散性を増し、生理活性
効果を向上させる点の提案はなされているものの、香味
1色調の改善については殆ど提案されていないのが実情
である。−本発明は上記事情に鑑みなされたもので、香
味。
Therefore, it is desired to improve the blending characteristics of the solvent extract of propolis, but previously, Japanese Patent Application Laid-Open No. 197523/1983 proposed a method for increasing the water dispersibility of the solvent extract of propolis and improving its physiologically active effect. However, the reality is that there are almost no proposals for improving one color tone of flavor. -The present invention has been made in view of the above circumstances, and is based on flavor.

色調が改善されたプロポリスの溶剤抽出物からなる生理
活性物質を提供することを目的とする。
The purpose of the present invention is to provide a physiologically active substance consisting of a solvent extract of propolis with improved color tone.

〔問題点を解決するための手段及び作用〕本発明者らは
、上記目的を達成することについて鋭意検討を行なった
結果、プロポリスの溶剤抽出物を特定の吸着剤、即ち平
均細孔径が5〜20人の活性炭や陽イオン交換樹脂で処
理することにより、プロポリス溶剤抽出物の有する抗菌
効果等の生理活性を低下させることなく、その香味9色
調を改善することができ、プロポリス特有の泥くさい香
味、舌、喉へのしびれ感が除去され、華やかな好ましい
香味の強さが保持されて嗜好性がよく、かつ色調も黄褐
色乃至淡黄色の生理活性物質が得られること、しかも上
記吸着処理により収率の低下が殆どないことを知見し、
本発明をなすに至ったものである。
[Means and effects for solving the problem] As a result of intensive studies to achieve the above object, the present inventors have found that the solvent extract of propolis is used as a specific adsorbent, that is, the average pore diameter is 5 to 5. By treating the propolis with activated carbon and cation exchange resin, it is possible to improve the nine color tones of the flavor without reducing the physiological activities such as the antibacterial effect of the solvent extract of propolis. The numbness in the tongue and throat is removed, the strength of the bright and pleasant flavor is maintained, and the physiologically active substance has good palatability, and the color is yellowish brown to light yellow. We found that there was almost no decrease in the rate,
This is what led to the present invention.

以下、本発明につき更に詳しく説明する。The present invention will be explained in more detail below.

本発明に係る生理活性物質はプロポリスの溶剤抽出物を
平均細孔径が5〜20人の活性炭及び/又は陽イオン交
換樹脂で処理することによって得られるものである。
The physiologically active substance according to the present invention is obtained by treating a solvent extract of propolis with activated carbon and/or cation exchange resin having an average pore size of 5 to 20 pores.

この場合、プロポリスの溶剤抽出物としては、プロポリ
スを水、エチルエーテル、プロピレングリコールなどの
極性溶剤、n−ヘキサン、石油エーテル、シクロヘキサ
ン、トルエン、ベンゼンなどの非極性溶剤、或いはこれ
らの混合溶剤で抽出したものが使用されるが、特にプロ
ポリスをエタノールの60〜100容量%水溶液で抽出
することによって得られた抽出物が最も好ましく用いら
れる。なお、溶剤抽出は常法に従って行なうことができ
る。
In this case, as a solvent extract of propolis, propolis is extracted with water, a polar solvent such as ethyl ether, propylene glycol, a non-polar solvent such as n-hexane, petroleum ether, cyclohexane, toluene, benzene, or a mixed solvent thereof. In particular, an extract obtained by extracting propolis with a 60 to 100 volume % aqueous solution of ethanol is most preferably used. Incidentally, the solvent extraction can be carried out according to a conventional method.

本発明は、かかるプロポリスの溶剤抽出物を吸着剤とし
て平均細孔径が5〜20人の活性炭及び/又は陽イオン
交換樹脂を用いて1処理するものである。この場合、吸
着剤として活性炭や陽イオン交換樹脂を使用したとして
も、平均細孔径が20人を越えるものは、後述する実験
の結果から明らかなように、十分な香味改善を達成し得
ず、場合によってはかえって香味を悪化させる場合もあ
り。
In the present invention, the solvent extract of propolis is subjected to one treatment using activated carbon and/or cation exchange resin having an average pore size of 5 to 20 as an adsorbent. In this case, even if activated carbon or cation exchange resin is used as an adsorbent, if the average pore size exceeds 20, sufficient flavor improvement cannot be achieved, as is clear from the experimental results described below. In some cases, it may even worsen the flavor.

更に収率を悪くする場合もあるため1本発明の目的を達
成することができないものである。
Furthermore, since the yield may be deteriorated, the object of the present invention cannot be achieved.

ここで、活性炭や陽イオン交換樹脂としては。Here, as activated carbon and cation exchange resin.

平均細孔径が5〜20人のものを用いる以外に限定はな
いが、活性炭としては、ヤシ殻、ココナツト殻、桃等の
果実のたね、堅実の殻などから得られる活性炭が好適で
あり、特にヤシ殻炭やココナツト炭が好ましく使用され
る。また、陽イオン交換樹脂としては、強酸性型、弱酸
性型のいずれのものでもよいが1強酸性型のものがより
好ましい。
There is no limitation other than to use carbon with an average pore size of 5 to 20, but activated carbon obtained from coconut shells, coconut shells, seeds of fruits such as peaches, shells of nuts, etc. is suitable, especially activated carbon. Coconut shell charcoal and coconut charcoal are preferably used. The cation exchange resin may be either a strongly acidic type or a weakly acidic type, but a strongly acidic type is more preferable.

これらの吸着剤を用いた処理方法としては、抽出液中に
吸着剤を投入し、攪拌する方法、吸着剤を充填したカラ
ムに抽出液を通す方法など、適宜な方法を採用すること
ができる。
As a treatment method using these adsorbents, an appropriate method can be adopted, such as a method of adding the adsorbent into the extract and stirring it, or a method of passing the extract through a column filled with an adsorbent.

吸着剤の使用量は適宜選定され、特に制限されるもので
はないが、活性炭の場合はプロポリスの溶剤抽出物の乾
燥重量に対して0.05〜5倍量、特に1〜3倍量とす
ることが好ましい。陽イオン交換樹脂の場合は、その交
換容量(■当量/g乾燥樹脂)によるが、交換容量4〜
5の場合、プロポリスの溶剤抽出物の乾燥重量に対して
1〜4倍とすることが望ましい。
The amount of adsorbent to be used is appropriately selected and is not particularly limited, but in the case of activated carbon, the amount is 0.05 to 5 times, especially 1 to 3 times the dry weight of the solvent extract of propolis. It is preferable. In the case of cation exchange resin, it depends on its exchange capacity (■equivalent/g dry resin), but the exchange capacity is 4~
In the case of No. 5, it is desirable to use 1 to 4 times the dry weight of the solvent extract of propolis.

処理温度や時間も限定されないが、処理温度は一15〜
100℃、特に5〜40℃が良く、処理時間は5分〜1
週間、望ましくは15分〜3日とすることができる。こ
の場合、色調変化は15分程度でほぼ平衡に達するが、
長時間の処理により香味及び口中刺激の面でより優れた
ものを得ることができる。
The treatment temperature and time are not limited either, but the treatment temperature is between -15 and
100℃, especially 5-40℃, treatment time is 5 minutes to 1
It can be carried out for a week, preferably from 15 minutes to 3 days. In this case, the color tone change almost reaches equilibrium in about 15 minutes, but
Long-term processing allows for better flavor and mouth irritation.

なお、上記吸着処理は複数回繰り返し行なってもよく、
また本発明の効果を損なわない範囲で他の吸着剤1例え
ば平均細孔径の大きい活性炭、シリカゲル、アルミナゲ
ル、活性アルミナ、活性白土、モレキュラーシービング
カーボン、ゼオライト系モレキュラーシーブス等を用い
た吸着処理と併用することは差支えない。
Note that the above adsorption treatment may be repeated multiple times,
In addition, adsorption treatment using other adsorbents 1 such as activated carbon with a large average pore diameter, silica gel, alumina gel, activated alumina, activated clay, molecular sieving carbon, zeolite-based molecular sieves, etc., to the extent that the effects of the present invention are not impaired. There is no problem in using them together.

本発明の生理活性物質は、キャンデー、トローチ、洗口
剤、歯磨等の口腔内で適用される組成物に対する配合適
性に優れ、従ってこれら口腔適用組成物の成分として効
果的に配合し得る。この場合、生理活性物質の口腔適用
組成物中への配合量は適宜選択されるが、通常組成物全
体の0.01〜25重量%、特に0.01〜10重量%
とすることができる。なお1口腔適用組成物のその他の
成分は、組成物の種類、使用目的等に応じて選択され、
通常配合される成分が用いられる。
The physiologically active substance of the present invention has excellent blendability in compositions applied to the oral cavity, such as candies, troches, mouth washes, and toothpastes, and therefore can be effectively blended as a component of these compositions for oral cavity application. In this case, the amount of the physiologically active substance to be incorporated into the oral composition is selected as appropriate, but is usually 0.01 to 25% by weight, particularly 0.01 to 10% by weight of the entire composition.
It can be done. Note that 1. Other components of the oral composition are selected depending on the type of composition, purpose of use, etc.
Commonly blended ingredients are used.

〔発明の効果〕〔Effect of the invention〕

本発明の生理活性物質は、プロポリスの溶剤抽出物の有
する抗菌活性、抗炎症作用、抗酸化作用等の生理活性を
維持し、しかも従来の欠陥である舌、喉への刺激性、泥
くさい香味などの問題点が除かれ、かつ色調も淡色化さ
れ、各種組成物への配合適性に優れているものである。
The physiologically active substance of the present invention maintains the physiological activities such as antibacterial activity, anti-inflammatory effect, and antioxidant effect possessed by the solvent extract of propolis, and also eliminates the conventional deficiencies such as irritation to the tongue and throat and muddy flavor. The above problems have been eliminated, the color tone has been lightened, and the composition has excellent suitability for blending into various compositions.

従って1本発明によれば、プロポリスの溶剤抽出物を使
用感や外観に問題を生じさせることなく、高濃度で食品
Therefore, according to the present invention, the solvent extract of propolis can be used in foods at high concentrations without causing any problems in the feel or appearance.

医薬、医薬部外品、香粧品、特に口腔適用組成物に配合
することを可能とするものである。
It can be incorporated into medicines, quasi-drugs, cosmetics, and especially oral compositions.

以下、実施例と比較例を示し5本発明を具体的に説明す
るが、本発明は下記の実施例に制限されるものではない
EXAMPLES Hereinafter, the present invention will be specifically explained with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

〔実施例、比較例〕[Example, comparative example]

プロポリスの原塊を99.5%エタノールで抽出し、そ
の抽出液に第1表に示す吸着剤を添加し〔活性炭の場合
は抽出液100mQに対し総表面積が10000n?に
なるように添加し、陽イオン交換樹脂(官能基−8o3
H,総交換容量(■各量/g乾燥樹脂4.3))の場合
は抽出液量に対して10重量/容量%になるように添加
した〕、室温で所定時間攪拌を行なった。処理後、吸着
剤を炉別し、得られた処理液(生理活性物質)の収率、
色調、香味変化及び抗菌力を評価した。結果を第2表に
示す。
The raw mass of propolis is extracted with 99.5% ethanol, and the adsorbent shown in Table 1 is added to the extract (in the case of activated carbon, the total surface area is 10,000 N for 100 mQ of the extract). Add the cation exchange resin (functional group -8o3
In the case of H, total exchange capacity (4.3% of each amount/g dry resin)), it was added in an amount of 10% by weight/volume based on the amount of the extract] and stirred at room temperature for a predetermined period of time. After treatment, the adsorbent is separated into a furnace, and the yield of the resulting treated solution (physiologically active substance) is determined.
Color tone, flavor change, and antibacterial activity were evaluated. The results are shown in Table 2.

なお、収率は溶剤抽出物の原料固形分量(g)を基準に
し、吸着処理後の固形分量(g)に対して求めた。
The yield was determined based on the raw material solid content (g) of the solvent extract and the solid content (g) after adsorption treatment.

また、抗菌力の評価方法は下記の通りである。Furthermore, the method for evaluating antibacterial activity is as follows.

坑黄左星負友抜 指標菌としてフシバクテリウム・ヌクレアトム(F u
sobacteriu+++ neucleatum)
を使用した。
Fusibacterium nucleatom (Fu
sobacterium+++ neucleatum)
It was used.

THB培地10+nuに検体を固形分0.1%(W/ 
v )相当添加した後、更にフシバクテリウム菌液を0
.5+nQ添加し、密閉試験管内で35℃条件下、4時
間培養後、30分間氷冷し、ヘッドスペース中のCH,
SH発生量をガスクロマトグラフィーにより測定した。
The sample was added to THB medium 10+nu with a solid content of 0.1% (W/
v) After adding a considerable amount, further add 0 Fucibacterium bacteria solution.
.. After adding 5+nQ and incubating in a sealed test tube at 35°C for 4 hours, cool on ice for 30 minutes, CH in the headspace,
The amount of SH generated was measured by gas chromatography.

第1表の結果より、平均細孔径5〜20人の活性炭や陽
イオン交換樹脂でプロポリスの溶剤抽出物を処理するこ
とによって得られた本発明の生理活性物質は、プロポリ
スの溶剤抽出物が本来有する抗菌効果を損なうことなく
色調及び香味が顕著に改善されたものであることが認め
られた。
From the results in Table 1, it can be seen that the physiologically active substance of the present invention obtained by treating the solvent extract of propolis with activated carbon or cation exchange resin with an average pore size of 5 to 20 It was observed that the color tone and flavor were significantly improved without impairing the antibacterial effect.

次に、本発明の抗菌剤の配合例を示す。Next, a formulation example of the antibacterial agent of the present invention will be shown.

〔配合例1〕キャンデイ− 砂    糖             40  重量
部水    飴              60酸味
料     o、6〃 香     料                0.
6  〃本発明抗菌剤*l          Q、8
u*1:プロポリスのエタノール抽出液を活性炭(平均
細孔径5人)で室温において15分処理したものの乾燥
固形品 〔配合例2〕チューインガム ガムベース         100  重量部香  
   料                0.1  
〃メントールパウダー      1.4 〃本発明抗
菌剤*2         1.On本2:プロポリス
のエタノール抽出液を活性炭(平均細孔径5人)で室温
において15分処理したものの乾燥固形品 〔配合例3〕洗口剤 水             70 重量部エタノール
          15   〃グリセリン    
     10   n、サッカリンナトリウム   
   0.1 〃シソ科植物希エタノール抽出物 0.
1 〃本発明抗菌剤$3         0.5 1
1京3:プロポリスの50%エタノール水溶液による抽
出液を陽イオン交換樹脂(平均細孔径15人)で室温に
おいて15分処理したものの乾燥固形品 出願人  ラ イ オ ン 株式会社 代理人  弁理士  小 島 隆 司
[Formulation Example 1] Candy Sugar 40 parts by weight Water Candy 60 Acidulant o, 6 Flavoring 0.
6 Antibacterial agent of the present invention *l Q, 8
u*1: Dry solid product obtained by treating propolis ethanol extract with activated carbon (average pore size: 5) for 15 minutes at room temperature [Formulation Example 2] Chewing gum gum base 100 parts by weight Fragrance
Fee 0.1
〃Menthol powder 1.4 〃Antibacterial agent of the present invention *2 1. On book 2: Dry solid product of propolis ethanol extract treated with activated carbon (average pore size 5) for 15 minutes at room temperature [Formulation example 3] Mouthwash water 70 parts by weight Ethanol 15 Glycerin
10 n, saccharin sodium
0.1 Dilute ethanol extract of Lamiaceae plant 0.
1 Antibacterial agent of the present invention $3 0.5 1
1Kyo 3: Dry solid product obtained by treating propolis extract with 50% ethanol aqueous solution for 15 minutes at room temperature with cation exchange resin (average pore size 15) Applicant: Lion Corporation Agent Patent Attorney Kojima Takashi

Claims (1)

【特許請求の範囲】[Claims] 1、平均細孔径が5〜20Åの活性炭及び/又は陽イオ
ン交換樹脂で処理されたプロポリス溶剤抽出物からなる
ことを特徴とする生理活性物質。
1. A physiologically active substance comprising a propolis solvent extract treated with activated carbon and/or a cation exchange resin having an average pore diameter of 5 to 20 Å.
JP62325788A 1987-12-23 1987-12-23 Physiologically active substance Pending JPH01165595A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62325788A JPH01165595A (en) 1987-12-23 1987-12-23 Physiologically active substance

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62325788A JPH01165595A (en) 1987-12-23 1987-12-23 Physiologically active substance

Publications (1)

Publication Number Publication Date
JPH01165595A true JPH01165595A (en) 1989-06-29

Family

ID=18180611

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62325788A Pending JPH01165595A (en) 1987-12-23 1987-12-23 Physiologically active substance

Country Status (1)

Country Link
JP (1) JPH01165595A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5529779A (en) * 1991-08-27 1996-06-25 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Purified propolis-extract, and its preparation and uses
EP0976399A1 (en) * 1998-07-31 2000-02-02 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Propolis extract
DE102008021756A1 (en) 2008-04-30 2009-11-05 Gehrlicher Pharmazeutische Extrakte Gmbh Propolis extract

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5529779A (en) * 1991-08-27 1996-06-25 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Purified propolis-extract, and its preparation and uses
EP0976399A1 (en) * 1998-07-31 2000-02-02 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Propolis extract
US6153227A (en) * 1998-07-31 2000-11-28 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Propolis extract
US6153228A (en) * 1998-07-31 2000-11-28 Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo Propolis extract
DE102008021756A1 (en) 2008-04-30 2009-11-05 Gehrlicher Pharmazeutische Extrakte Gmbh Propolis extract
WO2009133073A1 (en) 2008-04-30 2009-11-05 Gehrlicher Pharmazeutische Extrakte Gmbh Propolis extract

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