JP2000175696A - Extraction of dunaliella alga body - Google Patents
Extraction of dunaliella alga bodyInfo
- Publication number
- JP2000175696A JP2000175696A JP35518998A JP35518998A JP2000175696A JP 2000175696 A JP2000175696 A JP 2000175696A JP 35518998 A JP35518998 A JP 35518998A JP 35518998 A JP35518998 A JP 35518998A JP 2000175696 A JP2000175696 A JP 2000175696A
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- JP
- Japan
- Prior art keywords
- liters
- hexane
- crude
- extract
- ethanol
- 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.)
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Description
【発明の属する技術分野】本発明は、ドナリエラ藻体か
ら、ｎ−ヘキサンを使用して、β−カロチン油含有抽出
液を抽出するドナリエラ藻体の抽出方法に関する。[0001] The present invention relates to a method for extracting a Donariella algae from a Donariella algae by extracting a β-carotene oil-containing extract using n-hexane.
【従来の技術】従来、β−カロチン、ビタミンＡ・Ｂ群
・Ｃ、その他有用成分を含有する微細藻類のクロレラ藻
体１重量に、１０重量部の水を加えて、８０〜１００℃
の温度で約３０分間加熱し、抽出処理した後、高速遠心
分離機で分離処理して、クロレラ抽出液を得る技術手段
は、特公平５−１５６８５号公報に開示されており公知
に属する。2. Description of the Related Art Conventionally, 10 parts by weight of water is added to 1 part by weight of a chlorella alga body of microalgae containing .beta.-carotene, vitamins A, B, and C, and other useful components, and the temperature is raised to 80 to 100.degree.
A technical means for obtaining a chlorella extract by heating at a temperature of about 30 minutes for an extraction treatment and then performing a separation treatment with a high-speed centrifuge is disclosed in Japanese Patent Publication No. 5-15685 and belongs to the public.
【発明が解決しようとする課題】本発明者は、β−カロ
チンを多量に含むドナリエラ藻体粉末からβ−カロチン
油含有ドナリエラ藻体抽出液の抽出方法を達成したので
ある。The present inventor has achieved a method for extracting a β-carotene oil-containing Dunaliella algae extract from a Dunaliella algae powder containing a large amount of β-carotene.
【課題を解決するための手段】本発明は、防爆タンク中
のエタノール４００〜１０００リットルに、１０〜２０
０ｋｇのドナリエラ藻体粉末を浸漬し、４０〜５９℃で
加熱しながら３０分〜１時間半攪拌して洗浄処理したド
ナリエラ藻体の懸濁エタノール液を、遠心分離処理して
え分別した洗浄ドナリエラ藻体の３００〜４００ｋｇ
を、別の防爆タンク中のｎ−ヘキサン１２００〜１５０
０リットルに浸漬して、４０〜６０℃で加熱しながら３
０分〜１時間攪拌して抽出処理したドナリエラ藻体を、
遠心分離機で分別して得た粗ｎ−ヘキサン抽出液の３０
リットルを０．５Ｎ水酸化カリウムエタノール溶液１１
０リットルに加えて、４０〜６０℃で加温しながら２４
時間鹸化処理し、静置して、二層部に別れた下層の液部
を除去して得た上層部の鹸化処理後の粗ｎ−ヘキサン抽
出液を、水１００リットルに入れて、常温下で攪拌しな
がら洗浄し、クロロフィルなどの洗浄液を除去した粗ｎ
−ヘキサン抽出液を、５〜１０-2ｍｍＨｇ、５０℃で真
空蒸留処理した後、更に、真空蒸留処理後の微量にｎ−
ヘキサンを含む粗ｎ−ヘキサン抽出液の３００リットル
に、エタノール１〜１０リットルと、水１〜５リットル
とを加えて３０〜６０℃で蒸留処理して、ドナリエラ藻
体からβ−カロチン油含有抽出液を得ることから成るド
ナリエラ藻体の抽出方法である。 〔発明の詳細な説明〕本発明での洗浄処理で、ドナリエ
ラ藻体粉末１０〜２００ｋｇを、エタノール４００〜１
０００リットルに浸漬し、攪拌して洗浄するのは、ドナ
リエラ藻体粉末１０〜２００ｋｇに対して、４００リッ
トル未満のエタノールでは、浸漬状態が泥状態となり、
攪拌して洗浄する効果が得られず、また１０００リット
ルを超えても洗浄できるが、エタノールを浪費して経済
的でないからであり、なお洗浄処理で、５９℃を超える
とエタノールの蒸発が多くなり不経済となるので、４０
〜５９℃で３０分〜１時間３０分間かけて洗浄するのが
好適である。抽出処理で、ｎ−ヘキサン１２００〜１５
００リットルに対して、洗浄ドナリエラ藻体を３００〜
４００ｋｇの割合で浸漬するのは、ｎ−ヘキサンへのβ
−カロチンの溶解度は約１％で、３００〜４００ｋｇの
洗浄ドナリエラ藻体に、β−カロチンとして１０〜１２
ｋｇ含まれているので、ｎ−ヘキサンを１２００〜１５
００リットルを使用するのが好適に溶解でき、そして４
０〜６０℃で加熱しながら３０分〜１時間半攪拌して抽
出処理するのは、上記の４０〜６０℃の温度範囲がｎ−
ヘキサンに溶解するβ−カロチンの溶解度が高くなり、
かつ３０分〜１時間３０分間の範囲の抽出時間が好まし
いのである。クロロフィルなどの除去処理で、抽出処理
で得られた粗ｎ−ヘキサン抽出液の３０リットルを、１
１０リットルの０．５Ｎの水酸化カリウムエタノール溶
液に混和して、４０〜６０℃で加熱しつつ２４時間で鹸
化処理するのは、鹸化が十分に行われるからである。そ
して、鹸化処理後、放置して、二層に別れた下層部の液
層を分別して得た上層の鹸化処理後の粗ｎ−ヘキサン抽
出液（脱エタノール粗ｎ−ヘキサン抽出液）の２８．５
〜２９．５リットルを、水１００リットルに入れて、攪
拌して、水洗するとクロロフィル、水酸化カリウム、鹸
化物などが好適に水洗除去されて、２７．０〜２９．０
リットルの粗ｎ−ヘキサン抽出液が得られるのである。
脱溶剤処理で、クロロフィルなどを除去した粗ｎ−ヘキ
サン抽出液の３００リットルを、５〜１０-2ｍｍＨｇ、
５０℃で真空蒸留処理するのは、溶剤のｎ−ヘキサン抽
出液の３００リットルに、エタノール１〜１０リットル
と水１〜５リットルとを加えて、５０℃で蒸留処理する
のは、残存するｎ−ヘキサンが１０〜２０ｐｐｍに抑え
ることができるからである。本発明でのドナリエラ藻体
は、ドナリエラ・バーダウィル、ドナリエラ・サリナそ
の他のドナリエラ藻体、特にドナリエラ藻体の乾燥粉末
を意味し、また防爆タンクは、エタノールを使用し、加
熱すると爆発のおそれがある場合に使用するのが好まし
く、底部に開閉弁を持つ液流出管を備えたものが好まし
い。According to the present invention, 400 to 1000 liters of ethanol in an explosion-proof tank is added to 10 to 20 liters of ethanol.
0 kg of Donariella algae body powder is immersed in the suspension, and the suspension ethanol solution of the Donariella algae body washed and stirred by heating at 40 to 59 ° C. for 30 minutes to one and a half hours is centrifuged to separate the washed Donariella algae. 300-400kg of algae
With n-hexane 1200-150 in another explosion-proof tank
Immersed in 0 liters and heated at 40-60 ° C.
The Donariella algae bodies extracted and stirred for 0 minutes to 1 hour are
30% of the crude n-hexane extract obtained by fractionation with a centrifuge.
Liter of a 0.5N ethanol solution of potassium hydroxide 11
In addition to 0 liters, 24
The saponified crude n-hexane extract of the upper layer obtained by removing the lower layer liquid part separated into two layers and leaving it in a saponification treatment for a period of time is placed in 100 liters of water at room temperature. Washing with agitation and removing the washing liquid such as chlorophyll
-The hexane extract is subjected to vacuum distillation at 5 to 10 -2 mmHg and 50 ° C, and then n-
To 300 liters of the crude n-hexane extract containing hexane, 1 to 10 liters of ethanol and 1 to 5 liters of water were added, and the mixture was distilled at 30 to 60 ° C. to extract β-carotene oil-containing extract from Donariella alga bodies. This is a method for extracting Donariella algae, which comprises obtaining a liquid. [Detailed Description of the Invention] In the washing treatment of the present invention, 10 to 200 kg of the powder of Donariella algae is added to 400 to 1 of ethanol.
For immersion in 000 liters, washing by stirring, for 10 to 200 kg of Donariella algae body powder, with less than 400 liters of ethanol, the immersion state becomes a mud state,
The effect of washing by stirring cannot be obtained, and washing can be performed even when the amount exceeds 1000 liters. However, it is not economical because ethanol is wasted. Because it would be uneconomical, 40
It is preferable to wash at ５９59 ° C. for 30 minutes to 1 hour 30 minutes. In the extraction treatment, n-hexane 1200 to 15
300 liters of washed Donariella algae per 100 liters
Dipping at a rate of 400 kg is based on β-
-The solubility of carotene is about 1%, 300-400 kg of washed Donariella algae, 10-12 as β-carotene
kg, so that n-hexane is
It is preferable to use 00 liters, and
The stirring process for 30 minutes to 1.5 hours while heating at 0 to 60 ° C. is performed when the temperature range of 40 to 60 ° C. is n-
The solubility of β-carotene dissolved in hexane increases,
In addition, the extraction time in the range of 30 minutes to 1 hour 30 minutes is preferable. In the removal treatment of chlorophyll and the like, 30 l of the crude n-hexane extract obtained by the extraction treatment
The reason why the mixture is mixed with 10 liters of 0.5N ethanol solution of potassium hydroxide and saponified for 24 hours while heating at 40 to 60 ° C. is that saponification is sufficiently performed. 28. A saponification-treated crude n-hexane extract (deethanol-free crude n-hexane extract) of the upper layer obtained by separating the lower liquid layer separated into two layers after the saponification treatment. 5
２９29.5 liters in 100 liters of water, stirred and washed with water, chlorophyll, potassium hydroxide, saponified substances and the like were suitably washed away with water, and 27.0-29.0.
One liter of crude n-hexane extract is obtained.
300 liters of the crude n-hexane extract from which chlorophyll and the like have been removed by desolvation treatment is added at 5 to 10 -2 mmHg
Vacuum distillation at 50 ° C. is performed by adding 1 to 10 liters of ethanol and 1 to 5 liters of water to 300 liters of an n-hexane extract of a solvent and performing distillation at 50 ° C. to remove the remaining n. This is because hexane can be suppressed to 10 to 20 ppm. The Donariella alga body in the present invention means Donariella bardawill, Donaliella salina and other Donariella alga bodies, especially dry powder of the Donaliella alga body, and the explosion-proof tank uses ethanol, and there is a possibility of explosion when heated. It is preferably used in such a case, and is preferably provided with a liquid outlet pipe having an on-off valve at the bottom.
【実施例１】エタノール６００リットルとドナリエラ藻
体乾燥粉末２００ｋｇとを、エタノールの引火を防ぐた
めに防爆タンクに入れて、５０℃で加熱しながら１時間
攪拌洗浄して、洗浄処理したドナリエラ藻体の懸濁エタ
ノールを防爆タンクの底部の液流出管から遠心分離機に
エアーポンプで移送し、遠心分離してエタノールを除去
して得たエタノールが僅か残留している洗浄ドナリエラ
藻体３００ｋｇを、別の防爆タンクに移して、これにｎ
−ヘキサン１４００リットルを加えて、５０℃で１時間
半攪拌して、抽出処理してからドナリエラ藻体を分別し
て得た粗ｎ−ヘキサン抽出液の１２００リットルの内３
０リットルを、タンク中の０．５Ｎ水酸化カリウムエタ
ノール溶液を１１０リットル加えて、５０℃で５時間攪
拌し、鹸化処理した後、放置して上下二層に分別した下
層部の液層を、タンクの液流出管から除去して得た上層
部の２９リットルの鹸化処理後の粗ｎ−ヘキサン抽出液
を、１００リットル水に入れ、常温下で攪拌しながら洗
浄し、クロロフィル等を含む液を除去して得た粗ｎ−ヘ
キサン抽出液２８リットルを得て、これをエアーポンプ
で真空蒸留装置に移し、真空度５-2ｍｍＨｇ、温度５０
℃で真空蒸留処理し、ｎ−ヘキサンを除去して得た粗ｎ
−ヘキサン抽出液をポンプでタンクに集めて、該粗ｎ−
ヘキサン３００リットルにエタノール５リットルと水２
リットルとを加えて、５０℃で、蒸留して、２８０リッ
トルのβ−カロチン含有ドナリエラ藻体抽出液を得た。
得られた２８０リットルのβ−カロチン含有ドナリエラ
藻体抽出液には、β−カロチン油４２％、残存ｎ−ヘキ
サン１６ｐｐｍと、必須脂肪酸のリノール酸、その他の
脂肪酸が含まれていた。Example 1 600 liters of ethanol and 200 kg of dry powder of Donariella algae were placed in an explosion-proof tank to prevent ignition of ethanol, and stirred and washed for 1 hour while heating at 50 ° C. The suspended ethanol was transferred from the liquid outflow pipe at the bottom of the explosion-proof tank to a centrifuge by an air pump, and centrifuged to remove ethanol. Transfer to explosion-proof tank
1400 liters of hexane was added thereto, and the mixture was stirred at 50 ° C. for one and a half hours, extracted, and then 3/1200 liters of the crude n-hexane extract obtained by separating the Donariella algae bodies.
0 liter, 110 liter of 0.5N potassium hydroxide ethanol solution in the tank was added, and the mixture was stirred at 50 ° C. for 5 hours, saponified, then left and separated into two upper and lower liquid layers. A 29-liter saponified crude n-hexane extract of the upper layer obtained by removing from the liquid outlet pipe of the tank is put into 100-liter water, washed with stirring at room temperature, and the solution containing chlorophyll and the like is removed. to give the crude n- hexane extract liquid 28 liter was obtained by removing, it was transferred to a vacuum distillation apparatus with an air pump, vacuum 5 -2 mmHg, temperature 50
° C to obtain a crude n obtained by removing n-hexane.
-The hexane extract is collected in a tank by a pump, and the crude n-
300 liters of hexane, 5 liters of ethanol and 2 water
Then, the mixture was distilled at 50 ° C. to obtain 280 liters of a β-carotene-containing Donariella algae extract.
The obtained 280 liter of β-carotene-containing Donariella algae extract contained 42% of β-carotene oil, 16 ppm of residual n-hexane, linoleic acid as an essential fatty acid, and other fatty acids.
【使用例】実施例で得た、β−カロチン油４２％を含む
ドナリエラ藻体抽出液２８０リットルに、コーン油１１
２リットルを加えて、β−カロチン油３０％含有するド
ナリエラ藻体抽出液に調整して、適度の粘性とし、取り
扱い易くなして、マーガリンで０．００１〜０．００２
％、プロセスチーズで０．００５〜０．０３３％、マヨ
ネーズで０．０００６〜０．０３３％とし、ソーセージ
では、０．０００６〜０．０１％として添加するのが好
ましい。[Example of use] Corn oil 11 was added to 280 liters of a Donariella algae extract containing 42% of β-carotene oil obtained in the example.
Add 2 liters and adjust to a Donariella algae extract containing 30% β-carotene oil to make it moderately viscous, easy to handle and 0.001 to 0.002 with margarine
%, 0.005 to 0.033% for processed cheese, 0.0006 to 0.033% for mayonnaise, and 0.0006 to 0.01% for sausage.
【発明の効果】本発明によれば、ドナリエラ藻体乾燥粉
末から能率良く、高含有のβ−カロチン油を含むドナリ
エラ藻体抽出液が得られ、かつ該ドナリエラ藻体の抽出
液は、そのβ−カロチン油を適宜の濃度に調整して、各
種の食品に利用することができ得る有用なドナリエラ藻
体抽出液である。According to the present invention, a Dunaliella algae extract containing a high content of β-carotene oil can be obtained efficiently from a dry powder of a Donariella algae, and the extract of the Donaliella algae is obtained by using the β -It is a useful Donariella algae extract that can be used in various foods by adjusting carotene oil to an appropriate concentration.
Claims (1)
ドナリエラ藻体粉末１０〜２００ｋｇを入れて、加熱し
ながら攪拌したドナリエラ藻体懸濁エタノール液を遠心
分離して得た洗浄ドナリエラ藻体の３００〜４００ｋｇ
を、ｎ−ヘキサン１２００〜１５００リットルに浸漬し
て、加熱しながら攪拌し、抽出処理した後、ドナリエラ
藻体を分別して得た１１００〜１３００リットルの粗−
ヘキサン抽出液の３０リットルを、０．５Ｎ水酸化カリ
ウムエタノール溶液１１０リットルに加えて、加熱しな
がら鹸化処理してから、静置して、二層部に別れた下層
の液部を除去して得た上層部の鹸化処理粗ｎ−ヘキサン
抽出液に、水を加えて、常温下で攪拌しながら洗浄し、
クロロフィルなどを除去して得た粗ｎ−ヘキサン抽出液
を、真空蒸留処理した後、該真空蒸留した粗ｎ−ヘキサ
ン抽出液の３００リットルにエタノール５リットルと水
２リットルとを加えてから、蒸留処理してβ−カロチン
油含有抽出液を抽出することを特徴とするドナリエラ藻
体の抽出方法。1. A dry Donariella algae suspension obtained by adding 10 to 200 kg of a Donariella alga body powder to 400 to 1000 liters of ethanol and centrifuging the ethanol solution of the Donariella algae suspension stirred with heating.
Is immersed in 1200 to 1500 liters of n-hexane, stirred while heating and subjected to an extraction treatment, and then 11,000 to 1300 liters of crude-obtained by separating the Donariella algae.
30 liters of the hexane extract was added to 110 liters of a 0.5N potassium hydroxide ethanol solution, saponified while heating, and then allowed to stand to remove the lower liquid part separated into two layers. To the resulting saponified crude n-hexane extract of the upper layer, water was added and washed with stirring at room temperature,
The crude n-hexane extract obtained by removing chlorophyll and the like is subjected to vacuum distillation treatment, and then 5 liters of ethanol and 2 liters of water are added to 300 liters of the vacuum-distilled crude n-hexane extract, followed by distillation. A method for extracting a Donariella algae body, which comprises treating to extract a β-carotene oil-containing extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35518998A JP2000175696A (en) | 1998-12-14 | 1998-12-14 | Extraction of dunaliella alga body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35518998A JP2000175696A (en) | 1998-12-14 | 1998-12-14 | Extraction of dunaliella alga body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000175696A true JP2000175696A (en) | 2000-06-27 |
Family
ID=18442474
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35518998A Pending JP2000175696A (en) | 1998-12-14 | 1998-12-14 | Extraction of dunaliella alga body |
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| Country | Link |
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| JP (1) | JP2000175696A (en) |
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