JP4934272B2 - アスタキサンチン含有抽出物の製法およびその製法によって得られたアスタキサンチン含有抽出物 - Google Patents
アスタキサンチン含有抽出物の製法およびその製法によって得られたアスタキサンチン含有抽出物 Download PDFInfo
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- JP4934272B2 JP4934272B2 JP2004253525A JP2004253525A JP4934272B2 JP 4934272 B2 JP4934272 B2 JP 4934272B2 JP 2004253525 A JP2004253525 A JP 2004253525A JP 2004253525 A JP2004253525 A JP 2004253525A JP 4934272 B2 JP4934272 B2 JP 4934272B2
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- Prior art keywords
- astaxanthin
- extract
- containing extract
- organic solvent
- acetone
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Description
通常、このヘマトコッカスは寒天状の粘質鞘に包まれた細胞壁で覆われているので抽出する際には、藻類の細胞壁を破壊または処理が必要である。ヘマトコッカス藻からアスタキサンチンを抽出する方法としては、細胞壁を高圧下乱流により破壊、乾燥後、有機溶媒で抽出する方法(特許文献1)、ヘマトコッカスを乾燥被胞化状態で細砕して平均粒度10μm以下の細粉としたのち有機溶媒で抽出する方法(特許文献2)、ヘマトコッカス藻を水系破砕し噴霧乾燥したのち有機溶媒で抽出する方法(特許文献3)、ヘマトコッカス藻の細胞壁を破壊した乾燥物を得たのちに二酸化炭素の超臨界状態で抽出する方法(特許文献4)、ヘマトコッカス藻を熱アセトンで処理することによりに抽出する方法(特許文献5)がある。
(2)破砕機がビーズミルである(1)記載のアスタキサンチン含有抽出物の製法であり、
(3)(1)〜(2)のうちのいずれか記載の製法によって得られたアスタキサンチン含有抽出物であり、
(4)抽出物10mgをキャップ付き試験管(10ml)に入れ、酸素で置換し、封をした後、80℃で加温した状態で行なった安定性試験で4時間後のアスタキサンチン残存量が90〜100%である(3)のアスタキサンチン含有抽出物である。
未破砕のヘマトコッカス藻体中に含まれるアスタキサンチンの含量とアスタキサンチン抽出物中のアスタキサンチン含量は吸光度法(波長475nm、溶媒アセトン)で測定した。
未破砕のヘマトコッカス藻体中に含まれるアスタキサンチンを定量するための前処理方法として、本品約50mgを精密に量り、DMSO2mLを加えてテフロンホモジナイナーで5分間摩砕し、遠心分離して得た上清を100mLのメスフラスコにとる。残留物にアセトン5mLを加えて40〜50℃で5分間超音波処理し、遠心分離して得た上清を先と同じメスフラスコにとる。更にアセトン5mLで2〜3回同様に上清が無色になるまで操作を繰り返し、得られた上清を先と同じメスフラスコにとり、アセトンを加えて正確に100mLとする。この液をアセトンで希釈し適当な濃度とし吸光度を測定した。抽出物中のアスタキサンチンはアセトンで希釈し適当な濃度とし吸光度を測定した。
抽出物10mgをキャップ付き試験管(10ml)に入れ、酸素で置換し、封をした後、80℃で加温した状態で、4時間後のアスタキサンチン含量を含有率測定試験と同様に吸光度法で測定した。
室温で抽出物を社内の試験員5名による官能試験により、5段階で臭気を評価した。
(評 価) (内 容)
1: 特別なにおいを感じない。
2: わずかに特有の海草臭を感じる。
3: はっきりと特有の海草臭を感じる。
4: 特有の海草臭をやや不快に感じる。
5: 極めて不快な特有の臭気がある。
0.2〜1.0gの試料を適当量50mLのスクリューキャップ遠沈管にとり、クロロホルム:酢酸(2:3)20mLを加えて混和し、窒素ガス置換を行なった後、窒素ガスを吹き込みながら、飽和ヨウ化カリウム溶液1.0mLを静かに加える。やさしく攪拌してから、暗所に15分間放置した後、10%ヨウ化カリウム溶液20mLを加えて激しく混和してから、3,000rpmで3分間遠心処理を行う。下層を乱さないように静かに攪拌しながら0.01Nチオ硫酸ナトリウムでヨウ素の黄色が薄くなるまで滴定し、これにデンプン試薬0.5mLを添加してから、紫色が消えるまで滴定を行なう。滴定量から次式に従って過酸価物価(POV)を計算して求める。
POV(mEq/kg)=滴定量(mL)×滴定液ファクター×10/試料重量(g)
0.2〜4.0gの試料を適当量100mLのビーカーにとり、エタノール:ジエチルエーテル(1:1)を100mL加えて溶解し、0.1N水酸化カリウム溶液で滴定する。滴定量から以下の式にしたがって酸価を計算して求める。
酸価(AV/g)=滴定量(mL)×滴定液ファクター×5.611/試料重量(g)
乾燥未破砕ヘマトコッカス藻粉末1kg(バイオリール社製 アスタキサンチン含量4.6%)とミックスビタミンE(理研ビタミン、E700)
25gをアセトン1.5kgに分散させ、1mm径のガラスビーズを85%充填した防爆型のビーズミル試験機[ダイノミルKDL-PILOT、WAB社製]を用いて、適時冷却しながら室温で、ディスク周速10m/s、流速140g/min.で破砕処理を2回行い、同時にアスタキサンチンを含む脂質画分を抽出した。破砕懸濁液全量を吸引濾過により抽出濾液を回収、さらに濾過残渣を1kgのアセトンでリンス3回行い、アスタキサンチンを含む脂質成分を完全に抽出した。得られた抽出濾液全量から減圧エバポレーター(温度35℃)でアセトンを留去して、アスタキサンチン抽出物を得た。
乾燥未破砕ヘマトコッカス藻粉末1kg(Bio Real, Inc社製 アスタキサンチン含量4.6%)とミックスビタミンE(理研ビタミン、E700)25gをエタノール2kgに分散させ、1mm径のガラスビーズを85%充填した防爆型のビーズミル試験機[ダイノミルKDL-PILOT、WAB社製]を用いて、適時冷却しながら室温で、ディスク周速10m/s、流速180g/min.で破砕処理を2回行い、同時にアスタキサンチンを含む脂質画分を抽出した。破砕懸濁液全量を吸引濾過により抽出濾液を回収、さらに濾過残渣を1kgのエタノールでリンス3回行い、アスタキサンチンを含む脂質成分を完全に抽出した。得られた抽出濾液全量から減圧エバポレーター(温度45℃)でエタノールを留去して、アスタキサンチン抽出物を得た。
乾燥未破砕ヘマトコッカス藻粉末80kg(AstaReal AB社製 アスタキサンチン含量3.7%)とミックスビタミンE(理研ビタミン、E700)2kgをアセトン120kgに分散させ、1mm径のガラスビーズを85%充填した防爆型のビーズミル試験機[ダイノミルKDL-25BC、WAB製]を用いて、適時冷却しながら室温で、ディスク周束10m/s、流速100kg/hr.で破砕処理を2回行い、同時にアスタキサンチンを含む脂質画分を抽出した。破砕懸濁液全量を吸引濾過により抽出濾液を回収、さらに濾過残渣を40kgのアセトンでリンス3回行い、アスタキサンチンを含む脂質成分を完全に抽出した。得られた抽出濾液全量から減圧下(100torr、45℃)でアセトンを留去して、アスタキサンチン抽出物を得た。
乾燥未破砕ヘマトコッカス藻粉末80kg(バイオリール社製
アスタキサンチン含量4.8%)とミックスビタミンE(理研ビタミン、E700)2kgを水320kgに分散させ、マイクロスMIC−5NZ[奈良機械製]を用いて、回転数1,000rpmで32時間破砕処理し、これを噴霧乾燥(乾燥条件:入り口温度210℃、出口温度100〜102℃、アトマイザー回転数9,000rpm)した。得られた破砕乾燥藻全量を120kgのアセトン中に分散し、アスタキサンチンを含む脂質画分を抽出した。濾過により抽出濾液を回収、さらに濾過残渣を40kgのアセトンでリンス3回行い、アスタキサンチンを含む脂質成分を完全に抽出した。得られた抽出濾液は減圧下で基準値以下までアセトンを留去して、アスタキサンチン抽出物を得た。
乾燥未破砕ヘマトコッカス藻粉末1kg(バイオリール社製
アスタキサンチン含量4.6%)とミックスビタミンE(理研ビタミン、E700)25gを水4kgに分散させ、ビーズミル試験機[ダイノミルKDL-PILOT、WAB社製]を用いて、ディスク周速10m/s、流速100g/min.で破砕処理を2回行い、これを噴霧乾燥(乾燥条件:入り口温度210℃、出口温度98〜102℃、アトマイザー回転数9,000rpm)した。乾燥体1kgを容積4リットルの抽出槽に充填し、抽出槽の温度を40℃に保持し、温度40℃、圧力40MPaの超臨界状態の二酸化炭素を1時間当り10kgの供給速度で2時間供給し、圧力を5MPa、温度30℃とした分離槽の下部の抜き出し弁から抽出物を取り出してアスタキサンチン抽出物を得た。
Claims (4)
- アスタキサンチン含有ヘマトコッカス藻をエタノールまたはアセトンの有機溶媒中に懸濁させ、破砕機で破砕しながら該有機溶媒中でアスタキサンチンを抽出したのち、固形物と有機溶媒を除去することを特徴とする安定性が高く、臭気の少ないアスタキサンチン含有抽出物の製造方法。
- 破砕機がビーズミルである請求項1記載のアスタキサンチン含有抽出物の製造方法。
- 請求項1〜2のうちのいずれか記載の製造方法によって得られたアスタキサンチン含有抽出物。
- 抽出物10mgをキャップ付き試験管(10ml)に入れ、酸素で置換し、封をした後、80℃で加温した状態で行なった安定性試験で4時間後のアスタキサンチン残存量が90〜100%である請求項3記載のアスタキサンチン含有抽出物。
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