JP2001061418A - Purification of active ingredient in royal jelly - Google Patents
Purification of active ingredient in royal jellyInfo
- Publication number
- JP2001061418A JP2001061418A JP24237499A JP24237499A JP2001061418A JP 2001061418 A JP2001061418 A JP 2001061418A JP 24237499 A JP24237499 A JP 24237499A JP 24237499 A JP24237499 A JP 24237499A JP 2001061418 A JP2001061418 A JP 2001061418A
- Authority
- JP
- Japan
- Prior art keywords
- royal jelly
- molecular weight
- aqueous solution
- low
- active ingredient
- 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.)
- Granted
Links
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Jellies, Jams, And Syrups (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、ローヤルゼリーの
精製法に関し、更に詳細には抗疲労効果などのローヤル
ゼリーの効果を高めるローヤルゼリーの精製法に関す
る。The present invention relates to a method for purifying royal jelly, and more particularly, to a method for purifying royal jelly that enhances the effects of royal jelly such as anti-fatigue effect.
【０００２】[0002]
【従来の技術】ローヤルゼリーが様々な薬理作用を有し
ていることは既に知られており、この為、ローヤルゼリ
ーを有効成分とする種々の健康食品が販売されている。
このローヤルゼリーの有効成分としては、従来はデセン
酸及び／又はその塩が知られていたが、デセン酸類の含
有量と、薬効の強さに開きがあることは多くの研究者に
認識されていたことであり、この様な有効成分の探索が
行われてきたが、まだその正体は把握されていない。本
発明者らは、この様な有効成分を求め鋭意研究を重ねた
結果、分子量が２００００〜１０００００の蛋白にデセ
ン酸類とは異なる、抗疲労効果を有する有効成分が存在
することを見いだした。この様な蛋白の存在は、まだ知
られていないし、この様な成分を効率よく精製する手段
も全く知られていない。2. Description of the Related Art It is already known that royal jelly has various pharmacological actions. For this reason, various health foods containing royal jelly as an active ingredient have been sold.
As the active ingredient of this royal jelly, decenoic acid and / or a salt thereof have been conventionally known, but many researchers have recognized that there is a difference between the content of decenoic acids and the strength of the medicinal effect. That is, although such active ingredients have been searched for, their identity has not yet been grasped. The present inventors have intensively studied for such an active ingredient and, as a result, have found that a protein having a molecular weight of 20,000 to 100,000 has an active ingredient having an anti-fatigue effect different from decenoic acids. The existence of such a protein is not yet known, and no means for efficiently purifying such a component is known.
【０００３】即ち、ローヤルゼリーの有している有効成
分の濃度を高め、より有用なローヤルゼリー精製物の製
造法の開発が望まれていたが、この様な方法はまだ知ら
れていないのが現状であった。[0003] That is, it has been desired to develop a method of producing a more useful purified royal jelly by increasing the concentration of the active ingredient contained in royal jelly, but such a method has not yet been known. there were.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、この様な状
況下為されたものであり、ローヤルゼリーの有している
有効成分の濃度を高め、より有用なローヤルゼリー精製
物の製造法を提供することを課題とする。SUMMARY OF THE INVENTION The present invention has been made under such circumstances, and provides a more useful method for producing a purified royal jelly product by increasing the concentration of an active ingredient contained in royal jelly. That is the task.
【０００５】[0005]
【課題の解決手段】この様な状況に鑑みて、本発明者ら
は、ローヤルゼリーの有している有効成分の濃度を高
め、より有用なローヤルゼリー精製物の製造法を求めて
鋭意研究努力を重ねた結果、ローヤルゼリー中の分子量
２００００〜１０００００の蛋白分画に、優れた抗疲労
作用を有する有効成分が存在することを見いだした。更
に検討を重ねた結果、 ローヤルゼリーを１）低鎖長ア
ルコール水溶液可溶分を除く工程と、２）非水溶性成分
を除く工程と、３）水溶性の成分であって、高分子量の
成分を除く工程の３つの工程を経て処理することによ
り、前記抗疲労成分を高濃度に含むローヤルゼリー精製
物を得ることができることを見いだし、発明を完成させ
るに至った。以下、本発明について、実施の形態を中心
に更に詳細に説明を加える。In view of such a situation, the present inventors have made intensive research efforts to increase the concentration of the active ingredient contained in royal jelly and to find a more useful method for producing a purified royal jelly. As a result, it was found that an active ingredient having an excellent anti-fatigue action was present in a protein fraction having a molecular weight of 20,000 to 100,000 in royal jelly. As a result of further study, the royal jelly was subjected to 1) a step of removing a soluble component of a low-chain-length alcohol aqueous solution, 2) a step of removing a water-insoluble component, and 3) a water-soluble component having a high molecular weight. The inventors have found that by performing the treatment through the three steps of the removing step, it is possible to obtain a purified royal jelly product containing the anti-fatigue component in a high concentration, thereby completing the invention. Hereinafter, the present invention will be described in more detail focusing on embodiments.
【０００６】[0006]
【発明の実施の形態】（１）本発明のローヤルゼリーの
精製法 本発明のローヤルゼリーの精製法は、ローヤルゼリー
を、１）低鎖長アルコール水溶液可溶分を除く工程と、
２）非水溶性成分を除く工程と、３）水溶性の成分であ
って、高分子量の成分を除く工程の３つの工程を経てし
ょりすることを特徴とする。これらの各工程について、
個別に以下に説明する。BEST MODE FOR CARRYING OUT THE INVENTION (1) A method for purifying royal jelly according to the present invention The method for purifying royal jelly according to the present invention comprises the steps of: (1) removing a soluble component of a low-chain-length alcohol aqueous solution;
The method is characterized by three steps: 2) a step of removing a water-insoluble component and 3) a step of removing a water-soluble component having a high molecular weight. For each of these steps,
This will be described individually below.
【０００７】（ 低鎖長アルコール水溶液可溶分を除く
工程）本発明者らが見いだしたローヤルゼリー中の抗疲
労作用を有する有効成分は、分子量が２００００〜１０
００００の蛋白であり、この様な物質は通常エタノール
水溶液などの含低鎖長アルコール水溶液には溶けないこ
とが知られている。又、本発明者らが行った分析によれ
ば、ローヤルゼリー中には本発明の主題である、抗疲労
作用を有する有効成分以外に、デセン酸などの比較的低
分子量であって、蛋白ではない成分が多く存在してい
る。又、分子量の低い蛋白も存在している。これらの低
分子量蛋白や低分子量非蛋白は含低鎖長アルコール水溶
液には溶解する。この溶性の差を用いて前記低分子量蛋
白・低分子量非蛋白を除くのがこの工程である。本赤穂
邸で使用できる低鎖長のアルコールとしては、炭素数１
〜４のものが好ましく、例えば、メタノール、エタノー
ル、ノルマルプロパノール、イソプロパノール、ノルマ
ルブタノール、セカンダリーブタノール、ターシャリー
ブタノールなどが例示できるが、経口的な投与経路でロ
ーヤルゼリー精製物を投与する場合に於いては、エタノ
ールとイソプロパノールが安全性の観点で好ましく例示
できる。特に、エタノールは溶性とも考え合わせると特
に好ましい。又、この低鎖長アルコールは含有量が１０
〜２０Ｖ／Ｖ％で含有する水溶液として使用するのが好
ましい。これは、この濃度が低すぎると、有効成分が溶
出したりして歩留まりが低下し、この濃度が高すぎる
と、低分子量蛋白・低分子量非蛋白成分が析出し、有効
成分の中に混ざってくるからである。この様な含低鎖長
アルコール水溶液は、ローヤルゼリー被精製物に対し
て、１〜１００倍量を加え良く混合・懸濁させ、有効成
分である蛋白が通過しないポアサイズのフィルターを用
いて不溶分を濾取すればよい。この様なフィルターとし
ては、ミリポアフィルターや限外濾過膜が好ましく例示
され、蛋白の回収率から考えると、分子量５０００〜２
００００用の限外濾過膜が特に好ましい。この様な限外
濾過を行うことにより、分子量が２００００以上の含低
鎖長アルコール水溶液可溶分を得ることができる。又、
この様な処理で有効成分が除かれた部分として得られる
濾液中には、従来より知られてローヤルゼリーの他の有
効成分である、デセン酸が多く含まれているので、ロー
ヤルゼリー中のデセン酸を濃縮しうると言う副次的な効
果も有することになる。(Step of Removing Soluble Content of Low Chain Alcohol Aqueous Solution) The active ingredient having an anti-fatigue action in royal jelly discovered by the present inventors has a molecular weight of 2,000 to 10
It is known that such a substance is usually insoluble in a low-chain-length alcohol aqueous solution such as an aqueous ethanol solution. According to the analysis performed by the present inventors, royal jelly, other than the active ingredient having an anti-fatigue effect, which is the subject of the present invention, has a relatively low molecular weight such as decenoic acid and is not a protein. Many components are present. There are also proteins with low molecular weight. These low-molecular-weight proteins and low-molecular-weight non-proteins are dissolved in an aqueous solution containing a low-chain-length alcohol. In this step, the low-molecular-weight protein and the low-molecular-weight non-protein are removed using the difference in solubility. Alcohol with a low chain length that can be used at Honcho Ako House
To 4 are preferable, for example, methanol, ethanol, normal propanol, isopropanol, normal butanol, secondary butanol, tertiary butanol and the like can be exemplified. , Ethanol and isopropanol are preferred from the viewpoint of safety. Particularly, ethanol is particularly preferable in consideration of solubility. The low-chain alcohol has a content of 10
It is preferably used as an aqueous solution containing 20 V / V%. This is because if the concentration is too low, the active ingredient elutes or the yield decreases, and if this concentration is too high, low molecular weight proteins and low molecular weight non-protein components precipitate and mix into the active ingredient. Because it comes. Such a low-chain-length alcohol-containing aqueous solution is added to a purified royal jelly in an amount of 1 to 100 times, mixed and suspended well, and the insoluble components are removed using a pore size filter that does not allow the protein as an active ingredient to pass through. What is necessary is just to filter. Preferred examples of such a filter include a millipore filter and an ultrafiltration membrane.
Ultrafiltration membranes for 0000 are particularly preferred. By performing such ultrafiltration, a soluble component in a low-chain-length alcohol aqueous solution having a molecular weight of 20,000 or more can be obtained. or,
The filtrate obtained as a part from which the active ingredient has been removed by such treatment contains a large amount of decenoic acid, which is another active ingredient of royal jelly which has been conventionally known. It also has the secondary effect of being able to concentrate.
【０００８】（ 非水溶性成分を除く工程 ）又、ローヤ
ルゼリー中には、本発明の主題である分子量２００００
〜１０００００の蛋白と近似した物性を有する成分とし
て、同程度の大きさの非蛋白成分が存在する。これらの
非蛋白成分と本発明の主題である蛋白成分との違いは、
水に対する溶性に違いである。本発明の主題である分子
量２００００〜１０００００の蛋白が水溶性を示すのに
対して、この様な非蛋白成分は水溶性を示さないものが
少なくない。従って、水不溶分を除去することにより、
蛋白の分子量サイズでの有効成分の精製がより効率的に
行える。この様な工程は、分子量７００００〜１５００
００用の限外濾過膜などを用いて行う、高分子量成分の
除去工程と同時に行うこともできるが、濾過膜の目詰ま
りや効率の面からすると、遠心分離などにより高分子量
成分の限外濾過による除去以前に行っておくのが好まし
い。この場合の遠心分離は、１０００〜１００００００
０ｒ．ｐ．ｍ．でバッチ式で行っても、連続式で行って
も良い。(Step of removing water-insoluble components) The royal jelly has a molecular weight of 20,000 which is the subject of the present invention.
Non-protein components of similar size exist as components having physical properties similar to proteins of １００100,000. The difference between these non-protein components and the protein component that is the subject of the present invention is that
Difference in solubility in water. While proteins having a molecular weight of 20,000 to 100,000, which are the subject of the present invention, are water-soluble, many such non-protein components are not water-soluble. Therefore, by removing water-insoluble components,
The active ingredient can be more efficiently purified at the molecular weight of the protein. Such a process has a molecular weight of 70,000 to 1,500.
It can be performed at the same time as the high molecular weight component removal step, which is performed using an ultrafiltration membrane for 00, but from the viewpoint of clogging and efficiency of the filtration membrane, ultrafiltration of the high molecular weight component by centrifugation or the like is performed. It is preferable to perform the removal before the removal. The centrifugation in this case is 1000 to 1,000,000
0r. p. m. And may be performed continuously.
【０００９】（水溶性の成分であって、高分子量の成分
を除く工程）水溶性成分であって、含低鎖長アルコール
水溶液に不溶である成分としては、本発明の主題であ
る、分子量２００００〜１０００００の抗疲労作用を有
する蛋白以外に、更に高分子量の蛋白が存在することを
本発明者は種々の検討の結果、見いだした。従って、上
記２工程のみではこの様な高分子量の蛋白は除くことは
できない。本工程は、前記２工程を補完して該高分子量
の蛋白を除く工程である。この様な高分子量の蛋白と本
発明の主題の有効成分である蛋白の決定的な差異は、分
子量であり、この様な高分子量の蛋白は、本発明の主題
である蛋白が通過し、該高分子量蛋白が通過できないポ
アサイズの限外濾過膜を使用した限外濾過によって除去
することができる。この様な限外濾過膜としては、分子
量７００００〜１５００００用の限外濾過膜が好ましく
例示できる。勿論、この様な限外濾過を用いなくとも、
この様な成分はゲル濾過により、取り除くことができ、
この様な方法も本発明の技術的範囲に属するが、作業効
率、産業応用性を考えると限外濾過を用いるのが特に好
ましい。(Step of Excluding Water-Soluble Components and High-Molecular-Weight Components) The water-soluble components which are insoluble in the aqueous solution of low-chain-length alcohol include, as the subject of the present invention, a molecular weight of 20,000. As a result of various studies, the present inventors have found that there is a protein having a higher molecular weight in addition to a protein having an anti-fatigue action of １００100,000. Therefore, such high molecular weight proteins cannot be removed only by the above two steps. This step is a step that complements the above two steps and removes the high molecular weight protein. The decisive difference between such a high molecular weight protein and the protein which is the active ingredient of the subject of the present invention is the molecular weight, and such a high molecular weight protein passes through the protein which is the subject of the present invention. It can be removed by ultrafiltration using a pore size ultrafiltration membrane through which high molecular weight proteins cannot pass. As such an ultrafiltration membrane, an ultrafiltration membrane for a molecular weight of 70,000 to 150,000 can be preferably exemplified. Of course, without using such ultrafiltration,
Such components can be removed by gel filtration,
Although such a method also belongs to the technical scope of the present invention, it is particularly preferable to use ultrafiltration in view of working efficiency and industrial applicability.
【００１０】本発明のローヤルゼリーの精製法は上記
１）低鎖長アルコール水溶液可溶分を除く工程と、２）
非水溶性成分を除く工程と、３）水溶性の成分であっ
て、高分子量の成分を除く工程の３つの工程を含むこと
を特徴とする。この３つの工程の順番は特には限定され
ないが、精製効率と作業効率の面で、濾過膜の目詰まり
などを抑制できることから、１）低濃度の低鎖長アルコ
ール水溶液をローヤルゼリーに加えて、分子量５０００
〜２００００用の限外濾過膜で可溶分を取り除く工程を
第一工程とし、次いで、２）ローヤルゼリーを低濃度の
低鎖長アルコール水溶液に溶解させた溶液に過剰の水を
加え、沈殿を取り除く工程を第二工程とし、３）水性溶
液を分子量７００００〜１５００００用の限外濾過膜で
濾液を得る工程を第三工程として行うのが特に好まし
い。更に、第三工程で得られた濾液を濃縮するとローヤ
ルゼリーの精製物を固体として得ることができるが、こ
の際、本発明の主題である有効成分である蛋白の分子量
が２００００〜１０００００であることを利用して、分
子量１８０００〜２２０００用の限外濾過膜で、濾過成
分を除き濃縮する工程を加えると、濃縮の効率が上が
り、しかも必要なエネルギーが少なくなるので好まし
い。この濃縮物を減圧溜去や凍結乾燥などにかけること
により、本発明のローヤルゼリー精製物を得ることがで
きる。かかるローヤルゼリー精製物は、抗疲労作用に優
れており、抗疲労用の、食品などの組成物の原料として
好適である。この様なローヤルゼリーの精製物が、本発
明のローヤルゼリー精製物である。The method for purifying royal jelly of the present invention comprises the following steps: 1) a step of removing a soluble component in a low-chain-length alcohol aqueous solution;
The method is characterized by including three steps of a step of removing a water-insoluble component and a step of removing 3) a water-soluble component having a high molecular weight. The order of these three steps is not particularly limited. However, in terms of purification efficiency and work efficiency, clogging of the filtration membrane can be suppressed. 1) A low-concentration low-chain-length alcohol aqueous solution is added to royal jelly to obtain a molecular weight. 5000
The first step is to remove soluble matter with an ultrafiltration membrane for 20,000, and then 2) excessive water is added to a solution of royal jelly dissolved in a low-concentration aqueous solution of low-chain alcohol to remove precipitates. It is particularly preferred that the step be a second step and 3) the step of obtaining a filtrate of the aqueous solution with an ultrafiltration membrane for a molecular weight of 70,000 to 150,000 as a third step. Further, when the filtrate obtained in the third step is concentrated, a purified product of royal jelly can be obtained as a solid. At this time, it is determined that the molecular weight of the protein, which is the active ingredient which is the subject of the present invention, is 20,000 to 100,000. It is preferable to use a ultrafiltration membrane for a molecular weight of 18,000 to 22,000 to remove the components to be filtered and to increase the concentration efficiency and reduce the required energy. The purified royal jelly of the present invention can be obtained by subjecting this concentrate to distillation under reduced pressure or freeze-drying. Such a purified royal jelly has an excellent anti-fatigue action and is suitable as a raw material of a composition for foods and the like for anti-fatigue. Such a purified royal jelly is the purified royal jelly of the present invention.
【００１１】（２）本発明の抗疲労用の組成物 本発明の抗疲労用の組成物は、上記精製法によって得ら
れた、本発明のローヤルゼリーの精製物を含有すること
を特徴とする。本発明の抗疲労用の組成物としては、医
薬組成物、飲料組成物、食品組成物、化粧料組成物など
が例示できるが、これらの中で特に好ましいものは、食
品組成物と化粧料組成物であり、中でも食品組成物が特
に好ましい。これは、本発明のローヤルゼリー精製物中
の有効成分である蛋白が、この様な系では特に安定に含
有させることが可能だからである。本発明の組成物にお
いて、上記ローヤルゼリー精製物の好ましい含有量は、
０．１〜６０重量％であり、更に好ましくは、０．５〜
４０重量％である。本発明の組成物では、必須成分であ
る、上記ローヤルゼリーの精製物以外に、これらの組成
物で通常使用される任意の成分を含有することができ
る。かかる任意成分としては、例えば、化粧料であれ
ば、スクワラン、ワセリン、マイクロクリスタリンワッ
クス等の炭化水素類、ホホバ油、カルナウバワックス，
オレイン酸オクチルドデシル等のエステル類、オリーブ
油、牛脂、椰子油等のトリグリセライド類、ステアリン
酸、オレイン酸、リチノレイン酸等の脂肪酸、オレイル
アルコール、ステアリルアルコール、オクチルドデカノ
ール等の高級アルコール、スルホコハク酸エステルやポ
リオキシエチレンアルキル硫酸ナトリウム等のアニオン
界面活性剤類、アルキルベタイン塩等の両性界面活性剤
類、ジアルキルアンモニウム塩等のカチオン界面活性剤
類、ソルビタン脂肪酸エステル、脂肪酸モノグリセライ
ド、これらのポリオキシエチレン付加物、ポリオキシエ
チレンアルキルエーテル、ポリオキシエチレン脂肪酸エ
ステル等の非イオン界面活性剤類、ポリエチレングリコ
ール、グリセリン、１，３−ブタンジオール等の多価ア
ルコール類、増粘・ゲル化剤、酸化防止剤、紫外線吸収
剤、色剤、防腐剤、粉体等が好ましく例示でき、食品で
あれば、調味料、香料、抗酸化剤、防腐安定剤、乳化
剤、増粘剤、結合剤、分散剤、賦形剤、増量剤、甘味
料、酸味料、被覆剤、色剤等が好ましく例示でき、医薬
であれば、緩衝塩、分散剤、可溶化剤、結合剤、崩壊
剤、等張剤、被覆剤、安定化剤、滑沢剤等が好ましく例
示できる。本発明の組成物は、これらの成分を常法に従
って処理することにより製造することができる。かくし
て得られた、本発明の組成物は、過剰な運動などをした
場合に、速やかにその疲労を取り除いたり、或いは運動
中に疲労が蓄積するのを防ぐ作用、即ち、抗疲労作用を
有し、この様な疲労回復や疲労蓄積抑制に特に好適であ
る。(2) Anti-fatigue composition of the present invention The anti-fatigue composition of the present invention is characterized by containing the purified royal jelly of the present invention obtained by the above-mentioned purification method. Examples of the anti-fatigue composition of the present invention include a pharmaceutical composition, a beverage composition, a food composition, a cosmetic composition, and the like. Among them, particularly preferred are a food composition and a cosmetic composition. And food compositions are particularly preferred. This is because the protein as an active ingredient in the purified royal jelly of the present invention can be contained particularly stably in such a system. In the composition of the present invention, the preferred content of the purified royal jelly is
0.1 to 60% by weight, and more preferably 0.5 to 60% by weight.
40% by weight. The composition of the present invention may contain, in addition to the purified royal jelly, which is an essential component, any component commonly used in these compositions. Such optional components include, for example, in the case of cosmetics, hydrocarbons such as squalane, petrolatum, microcrystalline wax, jojoba oil, carnauba wax,
Esters such as octyldodecyl oleate, triglycerides such as olive oil, tallow, coconut oil, fatty acids such as stearic acid, oleic acid and ritinoleic acid, higher alcohols such as oleyl alcohol, stearyl alcohol and octyldodecanol, sulfosuccinate esters and the like. Anionic surfactants such as sodium polyoxyethylene alkyl sulfate, amphoteric surfactants such as alkyl betaine salts, cationic surfactants such as dialkylammonium salts, sorbitan fatty acid esters, fatty acid monoglycerides, and polyoxyethylene adducts thereof , Nonionic surfactants such as polyoxyethylene alkyl ethers and polyoxyethylene fatty acid esters, polyhydric alcohols such as polyethylene glycol, glycerin and 1,3-butanediol, thickening Gelling agents, antioxidants, ultraviolet absorbers, coloring agents, preservatives, powders and the like can be preferably exemplified, and if it is food, seasonings, flavors, antioxidants, preservative stabilizers, emulsifiers, thickeners, Preferred examples include a binder, a dispersant, an excipient, a bulking agent, a sweetener, an acidulant, a coating agent, a coloring agent, and the like, and in the case of a medicine, a buffer salt, a dispersant, a solubilizer, a binder, a disintegrant. , Isotonic agents, coating agents, stabilizers, lubricants and the like. The composition of the present invention can be produced by treating these components according to a conventional method. The thus obtained composition of the present invention has an action of quickly removing fatigue when excessive exercise or the like or preventing the accumulation of fatigue during exercise, that is, has an anti-fatigue action. It is particularly suitable for such recovery from fatigue and suppression of accumulation of fatigue.
【００１２】[0012]
【実施例】以下に、実施例を挙げて、本発明について更
に詳細に説明を加えるが、本発明が、これら実施例にの
み限定を受けないことは言うまでもない。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to Examples, but it goes without saying that the present invention is not limited to only these Examples.
【００１３】＜実施例１＞図１に示す工程に従って、生
ローヤルゼリー１Ｋｇを精製し、本発明のローヤルゼリ
ー精製物を０．１５Ｋｇ得た。即ち、生ローヤルゼリー
１Ｋｇに５ｌの１５％エタノール水溶液を加え、良く攪
拌し、一様に分散したのを確かめて、これを分子量１０
０００用の限外濾過膜を通して、不溶部を集めた。濾過
膜を通過した部分を濃縮したところ、多量のデセン酸が
含有されていることがわかった。不溶部に８ｌの水を加
え、攪拌し、一様に分散したのを確認した上で、１００
００ｒ．ｐ．ｍ．で３０分間遠心分離し、上清を集め
た。この上清を分子量１０００００の限外濾過膜を通
し、通過部を集め、更にこの溶液を分子量２００００の
限外濾過膜を通し、不通過部分を集め、これを減圧濃縮
し、本発明のローヤルゼリー精製物１を０．１５Ｋｇ得
た。Example 1 According to the process shown in FIG. 1, 1 kg of raw royal jelly was purified to obtain 0.15 kg of a purified royal jelly of the present invention. That is, 5 liters of a 15% aqueous ethanol solution was added to 1 kg of raw royal jelly, stirred well, and confirmed to be uniformly dispersed.
The insoluble portion was collected through an ultrafiltration membrane for 000. When the portion that passed through the filtration membrane was concentrated, it was found that a large amount of decenoic acid was contained. 8 l of water was added to the insoluble portion, and the mixture was stirred and confirmed to be uniformly dispersed.
00r. p. m. For 30 minutes, and the supernatant was collected. The supernatant was passed through an ultrafiltration membrane having a molecular weight of 100,000 to collect the passing portion. The solution was further passed through an ultrafiltration membrane having a molecular weight of 20,000, and the non-passing portion was collected. 0.15 kg of the product 1 was obtained.
【００１４】＜実施例２＞上記本発明のローヤルゼリー
精製物１を餌（ＣＥ−２）に５重量％混ぜ込み、これを
ｄｄｙマウス（雄性、１群１０匹）に２週間自由摂取さ
せた。対照群はＣＥ−２のみ、比較例１群はローヤルゼ
リー精製物１をその原料である生ローヤルゼリーに置換
したものを用いた。これらのマウスを流速８ｌ／分の流
水槽で強制遊泳試験を行った。測定項目は遊泳時間で７
秒以上息継ぎができない時点を遊泳の終点とした。強制
遊泳試験の実施はサンプル投与前と投与終了の２４時間
後であった。サンプル投与後の平均遊泳時間をサンプル
投与前の平均遊泳時間で除し、抗疲労インデックスとし
た。本発明のローヤルゼリー精製物の投与群のインデッ
クスが２．３２であったのに対し、対照群のそれは０．
８３、比較例１のそれは１．７２であった。これより、
本発明の精製法により、抗疲労作用を有する有効物質が
精製物に濃縮されていることがわかる。Example 2 The above-mentioned purified royal jelly 1 of the present invention was mixed in a diet (CE-2) at 5% by weight, and ddy mice (male, 10 mice per group) were allowed to freely ingest for 2 weeks. The control group used only CE-2, and the comparative example 1 group used purified royal jelly 1 in which raw royal jelly as its raw material was substituted. These mice were subjected to a forced swimming test in a flowing water tank at a flow rate of 8 l / min. The measurement item is swimming time 7
The point at which breathing was not possible for more than a second was taken as the end point of the swim. The forced swimming test was performed before sample administration and 24 hours after the end of administration. The average swimming time after sample administration was divided by the average swimming time before sample administration to obtain an anti-fatigue index. The index of the group to which the purified royal jelly of the present invention was administered was 2.32, whereas that of the control group was 0.32.
83 and that of Comparative Example 1 was 1.72. Than this,
It is understood that the active substance having an anti-fatigue action is concentrated in the purified product by the purification method of the present invention.
【００１５】＜実施例３＞下記に示す処方に従って、錠
剤（健康食品）を作製した。即ち、処方成分をグラッド
造粒装置で、２０％エタノール水溶液２０重量部を噴霧
しながら流動相造粒し、これを４０℃で４８時間送風乾
燥し、１重量部のステアリン酸マグネシウムを加えて打
錠し錠剤を得た。これにシェラック２０重量部をエタノ
ールに溶解して、糖衣パンを用いてコーティングした。
更に３０重量部の白糖をコーティングし、糖衣錠を得
た。 結晶セルロース ２０重量部 デンプン １５重量部 ヒドロキシプロピルセルロース ４重量部 ローヤルゼリー精製物１ １０重量部Example 3 Tablets (health foods) were prepared according to the following formulation. That is, the prescription component was fluidized-phase granulated by spraying 20 parts by weight of a 20% aqueous ethanol solution using a grading apparatus, and this was blown dry at 40 ° C. for 48 hours, and 1 part by weight of magnesium stearate was added. Tablets were obtained to give tablets. 20 parts by weight of shellac were dissolved in ethanol and coated with sugar-coated bread.
Another 30 parts by weight of sucrose was coated to give a sugar-coated tablet. Crystalline cellulose 20 parts by weight Starch 15 parts by weight Hydroxypropyl cellulose 4 parts by weight Royal jelly purified product 1 10 parts by weight
【００１６】＜実施例４＞実施例３の錠剤を用いて、疲
れやすい人１群１０人を用いて、抗疲労作用を実使用に
より確かめた。即ち、錠剤（１００ｍｇ錠）を１回２錠
１日３回３週間服用してもらい、疲労感の改善をアンケ
ートにより答えてもらった。対照群は精製物１を結晶セ
ルロースに置換したもの、比較例２群は原料である生ロ
ーヤルゼリーに置換したものを服用してもらった。疲労
の改善率は精製物１投与群が５０％であったのに対し、
比較例２群が３０％、対照群が１０％であった。これよ
り、本発明のローヤルゼリー精製物が優れた抗疲労作用
を有していることがわかる。Example 4 The anti-fatigue effect of the tablet of Example 3 was confirmed by actual use of a group of 10 people who were easily fatigued. That is, tablets (100 mg tablets) were taken twice a day three times a day for three weeks, and the improvement of the feeling of fatigue was answered by a questionnaire. The control group had the purified product 1 replaced with crystalline cellulose, and the comparative example 2 group had the raw royal jelly as the raw material replaced. The improvement rate of fatigue was 50% in the group treated with purified product 50%,
The comparative example 2 group was 30%, and the control group was 10%. This shows that the purified royal jelly of the present invention has an excellent anti-fatigue action.
【００１７】＜実施例５＞下記に示す処方に従って化粧
水を作製した。即ち、処方成分を攪拌可溶化し、化粧水
を得た。このものは。肌の疲労を改善し、みずみずしい
肌にする作用に優れていた。 ローヤルゼリー精製物１ ０．１重量部 グリセリン ５ 重量部 １，３−ブタンジオール ５ 重量部 エタノール ５ 重量部 ヘパリン類似物質 ０．１重量部 硫酸化トレハロース ０．１重量部 メチルパラベン ０．２重量部 水 ８４．５重量部Example 5 A lotion was prepared according to the following formulation. That is, the ingredients were stirred and solubilized to obtain a lotion. This one. It was excellent in improving skin fatigue and making the skin fresh and fresh. Royal jelly purified product 1 0.1 part by weight Glycerin 5 parts by weight 1,3-butanediol 5 parts by weight Ethanol 5 parts by weight Heparin analog 0.1 part by weight Sulfated trehalose 0.1 part by weight Methylparaben 0.2 parts by weight Water 84 .5 parts by weight
【００１８】[0018]
【発明の効果】本発明によれば、ローヤルゼリーの有し
ている有効成分の濃度を高め、より有用なローヤルゼリ
ー精製物の製造法を提供することができる。According to the present invention, it is possible to increase the concentration of the active ingredient contained in royal jelly and to provide a more useful method for producing a purified royal jelly.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 宮崎 博隆 神奈川県横浜市戸塚区柏尾町560 ポーラ 化成工業株式会社戸塚研究所内 (72)発明者 福島 信 神奈川県横浜市戸塚区柏尾町560 ポーラ 化成工業株式会社戸塚研究所内 Ｆターム(参考） 4B018 MD76 ME02 MF01 MF06 4B041 LC10 LD06 LK40 LP05 LP06 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Hirotaka Miyazaki 560 Pola, Kashio-cho, Totsuka-ku, Yokohama-shi, Kanagawa Prefecture Inside the Tokazuka Research Laboratories Co., Ltd. F-term in Totsuka Laboratory Co., Ltd. (reference) 4B018 MD76 ME02 MF01 MF06 4B041 LC10 LD06 LK40 LP05 LP06
Claims (9)
法であって、１）低鎖長アルコール水溶液可溶分を除く
工程と、２）非水溶性成分を除く工程と、３）水溶性の
成分であって、高分子量の成分を除く工程とを必須の構
成とすることを特徴とする、ローヤルゼリー中の有効成
分の精製法。1. A method for concentrating an active ingredient of royal jelly, comprising: 1) a step of removing a soluble component of a low-chain-length alcohol aqueous solution, 2) a step of removing a water-insoluble component, and 3) a water-soluble component. A method for purifying an active ingredient in royal jelly, which comprises a step of removing a high molecular weight component.
程が、低濃度の低鎖長アルコール水溶液をローヤルゼリ
ーに加えて、分子量５０００〜２００００用の限外濾過
膜で可溶分を取り除く方法であることを特徴とする、請
求項１に記載のローヤルゼリー中の有効成分の精製法。2. The step of removing the soluble component of the low-chain-length alcohol aqueous solution is performed by adding a low-concentration low-chain-length alcohol aqueous solution to royal jelly and removing the soluble component with an ultrafiltration membrane for molecular weight of 5,000 to 20,000. The method for purifying an active ingredient in royal jelly according to claim 1, wherein the method comprises:
リーを低濃度の低鎖長アルコール水溶液に溶解させた溶
液に過剰の水を加え、沈殿を取り除くことを特徴とす
る、請求項１又は２に記載のローヤルゼリーの精製法。3. The method according to claim 1, wherein the step of removing the water-insoluble component comprises adding excess water to a solution in which royal jelly is dissolved in a low-concentration aqueous solution of a low-chain alcohol to remove precipitates. 3. The method for purifying royal jelly according to 1.).
を除く工程が、水性溶液を分子量７００００〜１５００
００用の限外濾過膜で濾液を得ることを特徴とする、請
求項１〜３何れか１項に記載のローヤルゼリーの精製
法。4. The step of removing a high-molecular-weight component, which is a water-soluble component, comprises adding an aqueous solution having a molecular weight of 70,000 to 1,500.
The method for purifying royal jelly according to any one of claims 1 to 3, wherein the filtrate is obtained using an ultrafiltration membrane for 00.
ローヤルゼリーに加えて、分子量５０００〜２００００
用の限外濾過膜で可溶分を取り除く第一工程と、２）ロ
ーヤルゼリーを低濃度の低鎖長アルコール水溶液に溶解
させた溶液に過剰の水を加え、沈殿を取り除く第二工程
と、３）水性溶液を分子量７００００〜１５００００用
の限外濾過膜で濾液を得る第三工程からなる、請求項１
〜４何れか一項に記載のローヤルゼリーの精製法。5. An aqueous solution of a low-concentration alcohol having a low concentration is added to royal jelly, and the molecular weight is 5,000 to 20,000.
A first step of removing soluble matter with an ultrafiltration membrane for use; 2) a second step of adding excess water to a solution in which royal jelly is dissolved in a low-concentration low-chain-length alcohol aqueous solution to remove precipitates; 2.) A third step of obtaining a filtrate of the aqueous solution through an ultrafiltration membrane for a molecular weight of 70,000 to 150,000.
The method for purifying royal jelly according to any one of claims 4 to 4.
の限外濾過膜で、濾過成分を除き濃縮する工程を含むこ
とを特徴とする、請求項１〜５何れか一項に記載のロー
ヤルゼリーの精製法。6. The method for purifying royal jelly according to any one of claims 1 to 5, further comprising a step of concentrating the ultrafiltration membrane for a molecular weight of 18,000 to 22,000, excluding a filtration component. .
ルゼリーの精製法に従って精製されたことを特徴とす
る、ローヤルゼリー精製物。7. A purified royal jelly, which has been purified according to the method for purifying royal jelly according to any one of claims 1 to 6.
を含有することを特徴とする、抗疲労用の組成物。8. A composition for anti-fatigue comprising the purified royal jelly according to claim 7.
に記載の抗疲労用の組成物。9. The food according to claim 8, wherein the food is a food.
The composition for anti-fatigue according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24237499A JP4169305B2 (en) | 1999-08-30 | 1999-08-30 | Purification of active ingredients in royal jelly |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24237499A JP4169305B2 (en) | 1999-08-30 | 1999-08-30 | Purification of active ingredients in royal jelly |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001061418A true JP2001061418A (en) | 2001-03-13 |
| JP4169305B2 JP4169305B2 (en) | 2008-10-22 |
Family
ID=17088229
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24237499A Expired - Fee Related JP4169305B2 (en) | 1999-08-30 | 1999-08-30 | Purification of active ingredients in royal jelly |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4169305B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004021803A1 (en) * | 2002-09-06 | 2004-03-18 | Hayashibara, Ken | Refined royal jelly |
| JP2005179235A (en) * | 2003-12-18 | 2005-07-07 | Yamada Bee Farm | Composition for preventing, treating or ameliorating disorder of feeling comprising specific molecular weight fraction obtained from water-soluble fraction of royal jelly or treated royal jelly as active ingredient |
| JP2012080828A (en) * | 2010-10-12 | 2012-04-26 | Kato Bihoen Honpo:Kk | Royal jelly |
| US10398741B2 (en) | 2015-01-22 | 2019-09-03 | Yamada Bee Company, Inc. | Composition |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108719118A (en) * | 2018-05-29 | 2018-11-02 | 中国科学院深圳先进技术研究院 | A kind of animal swimming experiment device and experimental method |
-
1999
- 1999-08-30 JP JP24237499A patent/JP4169305B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004021803A1 (en) * | 2002-09-06 | 2004-03-18 | Hayashibara, Ken | Refined royal jelly |
| JP2005179235A (en) * | 2003-12-18 | 2005-07-07 | Yamada Bee Farm | Composition for preventing, treating or ameliorating disorder of feeling comprising specific molecular weight fraction obtained from water-soluble fraction of royal jelly or treated royal jelly as active ingredient |
| JP2012080828A (en) * | 2010-10-12 | 2012-04-26 | Kato Bihoen Honpo:Kk | Royal jelly |
| US10398741B2 (en) | 2015-01-22 | 2019-09-03 | Yamada Bee Company, Inc. | Composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4169305B2 (en) | 2008-10-22 |
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