JP4848420B2 - マリーゴールド由来カロテノイドの単離及び精製 - Google Patents
マリーゴールド由来カロテノイドの単離及び精製 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Medicines Containing Plant Substances (AREA)
- Fodder In General (AREA)
Description
キサントフィル92.19gm/Kg又は9.22%を有するマリーゴールドオレオレジン25Kgを、100リットル容量の攪拌器付き反応器に入れる。オレオレジンを、熱媒体として反応器のジャケット中の蒸気又は熱水のいずれかを用いて、温度40℃にて10分間攪拌することにより、均質化する。エタノール性KOHは、純度95%のKOH5Kgを35リットルのエチルアルコール(1:1.4容量)に入れ、これを溶解して調製する。調製したエタノール性KOHを、均質化塊の入った反応容器にゆっくり添加する。鹸化反応は、75℃の温度で30分間行う。99%を超える鹸化度をHPLCで確認後、温度70℃に維持した脱塩熱水40リットルを、反応塊に添加し、10分間攪拌し続ける。カロテノイド結晶を伴う希釈塊を、次いでフィルタープレスに汲み上げ、結晶を回収する。望ましくない不純物を洗浄し、流出物のpHを約7.0の中性に下げるため、追加の熱水約250リットルを、フィルタープレスを介して汲み上げる。中和を確実に行った後、窒素陽圧を、圧力1.25Kgでフィルタープレスに適用し、フィルター内に閉じ込められた結晶を圧搾する。湿結晶を、次いでフィルタープレス板からトレーに集め、薄層とし、箱型乾燥機で常圧下、3時間、温度約55℃で乾燥する。
キサントフィル102.18gm/Kg又は10.22%を有するマリーゴールドオレオレジン25.5Kgを、100リットル容量の攪拌器付き反応器に入れる。
Claims (13)
- マリーゴールド花弁由来のルテインに富むカロテノイドの生成方法であって、
(a)マリーゴールド花弁を制御された嫌気性条件下でエンシレージして、花弁に存在するカロテノイドを固定し濃縮するステップと、
(b)環境にやさしい乾燥工程を介して脱水し乾燥ミールを得るステップと、
(c)前記ミールをペレット化するステップと、
(d)食品用へキサンを用いて前記ペレット化ミールを溶剤抽出し、カロテノイドエステルに富むマリーゴールドオレオレジンを得るステップと、
(e)無水アルコール中で前記オレオレジンを均質化した後、アルカリでカロテノイドエステルを加水分解するステップと、
(f)水アルコール混合物によりカロテノイド結晶を沈殿させるステップと、
(g)十分な量の熱水で洗浄し、水溶性石鹸、クロロフィリン及び他の有機不純物を除去するステップと、
(h)フィルタープレス、遠心分離機及びノッチフィルターを用いてカロテノイド結晶を濾過するステップと、
(i)著しく水分が少なく、残留有害溶剤を完全に含まない、純度レベルの高い純カロテノイド結晶を得るために乾燥するステップと、を含む方法。 - 前記マリーゴールドが、熱帯条件に適した栽培習慣により非GMO種子から栽培されたタゲテスエレクタ(Tagetes erecta)種に由来する、請求項1に記載の方法。
- 前記ステップ(a)において、前記エンシレージが、酸化防止剤及びサイレージ添加剤を用いて行われる、請求項1に記載の方法。
- 前記ステップ(b)において、環境にやさしい乾燥工程を介した前記脱水が、いかなる有害なスタック放出も完全に伴わないガス化装置により発生された発生炉ガスを用いる加熱メカニズムを備えた流動床乾燥機により行われる、請求項1に記載の方法。
- 前記ステップ(c)において、前記ペレット化が、より良い溶剤抽出を助けるのに適切な圧縮機を用いて行われる、請求項1に記載の方法。
- 前記ステップ(d)において、温度が60℃を超えず、変性酸化物を最少化する、請求項1に記載の方法。
- 前記ステップ(e)において、オレオレジンの前記均質化が、45℃を超えない温度で10分間にわたり無水アルコールを用いて行われる、請求項1に記載の方法。
- 前記ステップ(e)において、カロテノイドエステルの加水分解が、エタノール性水酸化カリウムを用いて行われる、請求項1に記載の方法。
- 前記ステップ(e)において、前記加水分解温度が、70℃〜80℃の間であり、鹸化時間が30分を超えない、請求項1に記載の方法。
- 前記ステップ(f)において、カロテノイド結晶の前記沈殿が、50:50の比率の無水アルコールと水の混合物を用いて行われる、請求項1に記載の方法。
- 前記ステップ(g)において、前記洗浄が、産物のpHを中性にするのに十分な量の60℃〜70℃の熱水を用いて行われる、請求項1に記載の方法。
- 前記ステップ(i)において、前記乾燥が、周囲圧力で50℃〜55℃又は減圧下で40℃〜45℃にて行われる、請求項1に記載の方法。
- 得られた前記純カロテノイド結晶が、粉末、ビーズレット、顆粒、油分散体及び水分散体の形態で、大量に調合され安定化される、請求項1に記載の方法。
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