JP3935346B2 - Method for solubilizing licorice oil-based extract in aqueous system - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、水系対象物への甘草油性抽出物可溶化方法に関する。より詳細には、酸性溶液や食塩溶液などからなる各種の水系対象物、例えば、飲料、液状調味料、液状化粧品、液状医薬部外品などへの甘草油性抽出物可溶化方法に関する。
【０００２】
【従来の技術】
古くから甘草（Licorice）は生薬として知られ、現在では主に食品用甘味料や医薬品・医薬部外品などの原料として使用されている。特に、その水溶性成分であるグリチルリチンやグリチルレチン酸は、抗炎症作用、抗潰瘍作用、抗アレルギー作用などの優れた薬理作用があることから、広く食品、医薬品、化粧品などに利用されてきた。さらに、甘草はグリチルリチン以外に多くのフラボノイドを含有しており、これらを含む甘草油性抽出物と呼ばれる甘草を有機溶媒で抽出した画分は、細菌やかびに対する抗菌性（月刊フードケミカル4月号94項（1989）や特開昭59−46210号公報を参照）をはじめ、抗酸化作用（Free Radic. Biol. Med. 23（2）302-313（1997）を参照）、油脂の酸化防止作用（特開昭60-180784号公報を参照）、褐変酵素阻害作用（特開昭62-29528号公報や特開平2-233795号公報を参照）などの生理的作用を有することが知られている。
【０００３】
ところで、従来、飲料製品の製造においては常に微生物汚染の危険性が存在するため、保存安定性の理由から、飲料をスチール缶やアルミニウム缶などに充填する際に加熱殺菌したり、充填した後に当該製品をレトルト殺菌したりしていた。しかしながら、近年の飲料製品の形態は従来の主流であった缶に代わり、ペットボトルの使用が急激に増加している。ペットボトルはいくつかの利点がある一方で耐熱性容器である缶と異なって非耐熱性の素材であるという都合上、上記のような方法では殺菌を行うことができないという欠点がある。さらに、消費者側の使用場面では、ペットボトルの特徴であるリキャップ性が開封後の微生物汚染につながることも危惧されている。また、ペットボトルの台頭と共に従来にはあまり見られなかった澄明性の高い飲料が各飲料メーカーから販売されるようになったが、これらは微生物汚染の危険性の排除と共に透明度の確保のために注意を払う必要がある。
【０００４】
以上のような問題を解決する一手段として、飲料に抗菌性物質を添加する方法がある。抗菌性物質を添加することで、加熱殺菌やレトルト殺菌の条件を緩和しても製品の安全性を確保することができる。また、万が一、充填時に容器内へ微生物が混入するようなことがあったとしても、製品中で微生物に対する抗菌効果が発揮される。さらに、加熱殺菌条件を緩和することで、加熱による飲料自体の品質劣化を防止することができ、飲料本来の風味の維持といった効果も期待できる。近年、食品工業界においては化学合成品である食品添加物の安全性についての基準や考え方が厳しくなってきているために化学合成品にかわって天然添加物が注目され、その需要も高まってきている。このような背景のもとにおいては、上記のように強力な抗菌作用などの優れた生理的作用を有する甘草油性抽出物は魅力ある食品添加物用素材の一つであり、既にその利用方法について検討がなされている。
【０００５】
【発明が解決しようとする課題】
飲料をはじめとする各種の水系対象物に甘草油性抽出物を添加しようとする場合に考慮しなければならないことは、甘草油性抽出物は水に対する溶解性が非常に乏しいため、そのままでは水系対象物中に均質に混合させることができないという点である。また、一般に、食品、飲料などの水系対象物中には酸や食塩や糖質など様々な物質を共存させている場合が多いので、このような対象物中においても対象物の本来の性質を損なうことなく甘草油性抽出物を均質に混合させる方法が要求される。
【０００６】
以上のような課題を解決する一手段として、甘草油性抽出物を水溶性の有機溶媒に溶解させた後に添加する方法がある。食品中に添加できる有機溶媒で、甘草油性抽出物に対する溶解能を有するものとしては、エタノールやプロピレングリコールやグリセリンがある。これらの有機溶媒に甘草油性抽出物を溶解させて水系対象物に添加する場合、水系対象物中の有機溶媒濃度を高くすれば、当然のことながら多量の甘草油性抽出物を水系対象物に溶解させることが可能となる。しかしながら、通常において許容されうる有機溶媒濃度は制限されるので、許容された濃度の有機溶媒が有する溶解能力を超える量の甘草油性抽出物を添加した場合、その成分が析出してしまう。従って、この方法では甘草油性抽出物の溶解性を確保することは困難であると言わざるを得ない。
【０００７】
また、界面活性剤などを用いて甘草油性抽出物を水分散性の製剤としてこれを添加する方法も検討されている。この方法を採用する場合、特に、その澄明性が外観上の重要要素である飲料製品などに対しては、いくら甘草油性抽出物を均質に混合させることができたとしても、甘草油性抽出物成分が液中にて濁った状態で混合されているのでは外観において好ましいとはいえないので、可溶化状態で混合されていることが必須である。
【０００８】
界面活性剤を用いた甘草油性抽出物可溶化組成物としては、例えば、特公平4-6688号（特開昭60-233015号）公報にて、甘草油性抽出物とＨＬＢが５以上のショ糖脂肪酸エステルとからなる組成物が提案され、このショ糖脂肪酸エステルを用いた甘草油性抽出物を含む組成物が純水に対して良好な溶解性を有することが示されている。しかしながら、ショ糖脂肪酸エステルは、酸性溶液中や食塩溶液中などでは凝集性を示すため、このような条件下においては甘草油性抽出物の溶解性を保つことができないことが本発明者による研究結果から明らかになった。また、特開2001-103932号公報において、甘草油性抽出物とショ糖脂肪酸エステルまたはキラヤ抽出物のいずれか一方またはその両方およびゼラチンとを水溶性アルコールに溶解させてなる組成物が提案されている。しかしながら、この組成物を用いた場合、上記のようなショ糖脂肪酸エステルが有する問題に加え、ゼラチンの影響によるゲル化やそれを防止する手段としての塩類または尿素の添加は、添加対象物本来の性状や味などの性質に影響を与えてしまうという問題がある。
【０００９】
そこで本発明は、酸性溶液や食塩溶液などからなる各種の水系対象物、例えば、飲料、液状調味料、液状化粧品、液状医薬部外品などに甘草油性抽出物を可溶化する方法であって、添加対象物本来の性状や味などの性質に影響を与えることなく、しかも、澄明性の高い添加対象物に甘草油性抽出物を可溶化した後もその澄明性を維持することができる方法を提供することを目的とする。
【００１０】
【課題を解決するための手段】
本発明者は、以上のような点に鑑み、甘草油性抽出物を純水はもとより、酸性溶液や食塩溶液などに対してもその澄明性に影響を与えることなく可溶化でき、かつ添加対象物の性状に影響を与えず、しかも甘草油性抽出物が有する優れた生理作用を十分に発揮させることのできる方法の提供を目的として鋭意研究を行った結果、ＨＬＢが１４以上のポリグリセリンラウリン酸エステルが甘草油性抽出物の可溶化に特異的に優れていることを見出した。
【００１１】
ポリグリセリン脂肪酸エステルの水系対象物への甘草油性抽出物の可溶化効果については、前出の特公平4-6688号公報に、ＨＬＢが６．３のポリグリセリンオレイン酸モノエステルが純水に対してやや良い程度の分散性を有することが示されているが、その効果は満足できるものではない。また、この公報においては酸性溶液や食塩溶液などに対する可溶化効果は検討されておらず、この公報からはポリグリセリンラウリン酸エステルのその効果を窺い知ることはできない。特開2001-48800号公報には、飲料に甘草油性抽出物を添加するに際してグリセリン脂肪酸エステルを組み合わせて用いることができるとの記載があり、特開2001-231523号公報には、飲食品に甘草油性抽出物中の主要抗菌成分であるグラブリジンを添加するに際してポリグリセリン脂肪酸エステルを組み合わせて用いることができるとの記載がある。しかしながら、いずれの公報においても詳細な検討はなされておらず、単に、グリセリン脂肪酸エステルやポリグリセリン脂肪酸エステルといった類の界面活性剤が甘草油性抽出物の可溶化に利用し得るという可能性が示されているに過ぎない。
また、特開2000-239176号公報では、多価アルコール脂肪酸エステルと甘草油性抽出物と油脂とを含有する組成物が提案され、多価アルコール脂肪酸エステルとしてポリグリセリン脂肪酸エステルが記載されており、特開平2-204417号公報には、油脂である中鎖脂肪酸トリグリセライドを用いた甘草油性抽出物組成物が記載されている。しかしながら、これらの組成物は油性の外用剤や化粧料を対象物としたものであり、油脂を含有するのでこのままでは水系対象物には不溶であるので、水系対象物への添加の際には乳化などの手段を講じる必要があり、澄明性の高い飲料などへの添加には適さない。また、特開平8-268837号公報では、植物性液状油と乳化剤と植物抽出物と水相成分を配合した乳化型組成物が提案され、植物抽出物として甘草が記載されているとともに、乳化補助剤としてデカグリセリンラウリン酸モノエステルが記載されている。しかしながら、この公報においては、デカグリセリンラウリン酸モノエステルは乳化補助剤としての利用可能性が示されているに過ぎないので、その甘草油性抽出物に対する可溶化効果を導き出すことはできないし、組成物自体も乳化型である以上、澄明性の高い飲料などへの添加には適さない。
以上のような技術背景のもとでは、ＨＬＢが１４以上のポリグリセリンラウリン酸エステルが純水はもとより、酸性溶液や食塩溶液などに対してもその澄明性に影響を与えることなく甘草油性抽出物を可溶化させるという事実は、全く予測することができなかった驚くべきものである。
【００１２】
上記の研究過程を経て完成された本発明の水系対象物への甘草油性抽出物可溶化方法は、請求項１記載の通り、ＨＬＢが１４以上のポリグリセリンラウリン酸エステルを用いることを特徴とする。
また、請求項２記載の甘草油性抽出物可溶化方法は、請求項１記載の甘草油性抽出物可溶化方法において、ポリグリセリンラウリン酸エステルがデカグリセリンラウリン酸モノエステルである。
また、請求項３記載の甘草油性抽出物可溶化方法は、請求項１または２記載の甘草油性抽出物可溶化方法において、水系対象物が酸性溶液からなる。
また、請求項４記載の甘草油性抽出物可溶化方法は、請求項１または２記載の甘草油性抽出物可溶化方法において、水系対象物が食塩溶液からなる。
また、請求項５記載の甘草油性抽出物可溶化方法は、請求項１乃至４のいずれかに記載の甘草油性抽出物可溶化方法において、水系対象物が飲料、液状調味料、液状化粧品、液状医薬部外品のいずれかである。
また、本発明の甘草油性抽出物可溶化組成物は、請求項６記載の通り、甘草油性抽出物とＨＬＢが１４以上のポリグリセリンラウリン酸エステルを含有し、水系対象物に添加されるものである。
また、本発明の飲料は、請求項７記載の通り、請求項６記載の甘草油性抽出物可溶化組成物が添加されたものである。
また、本発明の液体調味料は、請求項８記載の通り、請求項６記載の甘草油性抽出物可溶化組成物が添加されたものである。
また、本発明の液状化粧品は、請求項９記載の通り、請求項６記載の甘草油性抽出物可溶化組成物が添加されたものである。
また、本発明の液状医薬部外品は、請求項１０記載の通り、請求項６記載の甘草油性抽出物可溶化組成物が添加されたものである。
また、本発明の水系対象物に甘草油性抽出物を可溶化させるための甘草油性抽出物可溶化剤は、請求項１１記載の通り、ＨＬＢが１４以上のポリグリセリンラウリン酸エステルを有効成分とするものである。
【００１３】
【発明の実施の形態】
本発明が適用される甘草油性抽出物の原料となる甘草は、マメ科Ｇｌｙｃｙｒｒｉｈｉｚａ属植物に属するもので、例えば、Ｇｌｙｃｙｒｒｉｈｉｚａ ｇｌａｂｒａ，Ｇ．ｕｒａｌｅｎｓｉｓ，Ｇ．ｉｎｆｌａｔａなどがある。本発明においてはこれら植物の根、根茎、葉、茎のいずれの部位でも原料として使用することができるが、根および／または根茎を原料として使用することが好ましい。また、これらは、生のものを使用しても乾燥させたものを使用してもよいが、工業的に製造されているグリチルリチンの抽出原料となっている乾燥根および乾燥根茎、あるいはグリチルリチンなどを得るために水で抽出した後の水抽出残渣を原料として使用することもできる。なお、甘草は生産地の名前を冠して呼ばれることが多く、例えば、東北甘草、西北甘草、新彊甘草、モンゴル産甘草、ロシア産甘草、アフガニスタン産甘草などを挙げることができる。
【００１４】
また、甘草の水抽出残渣とは、上記の甘草を冷水や温水や熱水、もしくは中性あるいは微アルカリ性の冷水や温水や熱水で抽出した後の固形残渣、またはこれらを組み合わせ繰り返して抽出した後の固形残渣であり、抽出後の残渣は含水および乾燥状態のいずれでもよい。甘草または甘草水抽出残渣から、本発明に係る甘草油性抽出物を得るためには、各種の有機溶媒を単独あるいは組み合わせて使用して抽出すればよい。有機溶媒としては、例えば、ベンゼン、トルエン、キシレン、エチルエーテル、メチルエチルケトン、メチルイソブチルケトン、ジクロロメタン、ジクロロエタン、クロロホルム、酢酸エチル、酢酸プロピル、酢酸ブチル、アセトン、メタノール、エタノール、プロパノール、含水メタノール、含水エタノール、含水プロパノールなどが挙げられる。さらには、超臨界流体として二酸化炭素を用いることもできる。これらの有機溶媒のなかでは、エタノールまたは含水エタノールを使用するのが食品衛生法上、問題が少ないので好ましい。
【００１５】
甘草または甘草水抽出残渣から上述した有機溶媒で甘草油性抽出物を得るための条件は特に限定されるものはないが、標準的な方法を示すと、抽出原料に対し２〜１０倍量の有機溶媒を加えて撹拌しながら常温で抽出する方法や加熱還流して抽出する方法がある。また、これらの方法をそれぞれ単独で、または組み合わせて繰り返し操作すれば、抽出効率が向上し、より好ましい。
【００１６】
得られた抽出液は、遠心分離や濾過により不溶物を取り除いた後、甘草油性抽出物としてそのまま使用することもできるし、さらに常法により濃縮して使用することもできる。これらは目的とする生理的効果が低下しない範囲で脱臭、脱色などの精製を適宜行ってもよい。この精製工程には、活性炭、合成吸着樹脂、イオン交換樹脂などを用いることが一般的である。また、適当な方法で抽出液を乾燥させれば、甘草油性抽出物として黄褐色の抽出物粉末を得ることができる。
【００１７】
本発明においては、このようにして得られた液状抽出物がそのまま、あるいは液状抽出物を濃縮したもの、さらには抽出物の粉末あるいは固形の乾燥物が甘草油性抽出物として適用される。
【００１８】
本発明において、水系対象物に甘草油性抽出物を可溶化する際の有効成分となるＨＬＢが１４以上のポリグリセリンラウリン酸エステルについて以下に説明する。まず、「ポリグリセリン」とはグリセリンの重合物であり、その平均重合度が２以上であることを意味する。ＨＬＢが１４以上のポリグリセリンラウリン酸エステルであればその平均重合度に制限はないが、平均重合度が８〜１２のものが好ましく、平均重合度が１０のもの、即ち、デカグリセリンラウリン酸エステルがより好ましい。
【００１９】
また、ポリグリセリンラウリン酸エステルとは前記ポリグリセリン分子中の水酸基にラウリン酸がエステル結合した化合物であることを意味する。本発明においてはポリグリセリンのラウリン酸による平均エステル化率が０．１〜４であるポリグリセリンラウリン酸エステルが好ましく、０．５〜１．５であるポリグリセリンラウリン酸モノエステルがより好ましい。
【００２０】
なお、ＨＬＢは親水性−疎水性バランス（Ｈｙｄｒｏｐｈｉｌｉｃ Ｌｉｐｏｐｈｉｌｉｃ Ｂａｌａｎｃｅ）を意味し、界面活性剤が果たす効果の指標値であることは周知の通りであり、グリセリンの重合度とラウリン酸によるエステル化率に依存するものである。
【００２１】
水系対象物に甘草油性抽出物を可溶化するに際してのポリグリセリンラウリン酸エステルの使用方法としては、予め、甘草油性抽出物とポリグリセリンラウリン酸エステルとを均一に混合し、甘草油性抽出物をポリグリセリンラウリン酸エステルに溶解せしめた組成物、即ち、甘草油性抽出物可溶化組成物を調製し、この組成物を水系対象物に添加する方法が好ましい。この組成物を調製するための甘草油性抽出物とポリグリセリンラウリン酸エステルの混合方法は特に限定されないが、例を挙げるとすれば微粉末状の甘草油性抽出物とポリグリセリンラウリン酸エステルとを攪拌機を用いて混合する方法、または甘草油性抽出物の乾燥物をエタノール、アセトン、イソプロピルアルコールなどの揮発性有機溶媒あるいは揮発性有機溶媒と水との混合溶媒に溶解させた後にポリグリセリンラウリン酸エステルと混合攪拌し、減圧濃縮機などを用いて溶媒を留去する方法、または液状の甘草油性抽出物あるいはその濃縮物とポリグリセリンラウリン酸エステルとを混合攪拌した後に減圧濃縮機などを用いて溶媒を留去する方法などがあり、これらの方法から適宜選択して行うことができる。
【００２２】
甘草油性抽出物とポリグリセリンラウリン酸エステルとの混合比率は、甘草油性抽出物の内容成分中に水難溶性物質が多い場合にはポリグリセリンラウリン酸エステルの比率を多くし、水難溶性物質が少ない場合にはポリグリセリンラウリン酸エステルの比率を少なくすれば良く、甘草油性抽出物の性質に合せて適宜調整すればよいが、一般的には甘草油性抽出物１重量部に対してポリグリセリンラウリン酸エステルを２〜４０重量部が好ましく、５〜２０重量部がより好ましい。ポリグリセリンラウリン酸エステルの混合比率は高ければ高いほど甘草油性抽出物の可溶化の点においては有利であるが、混合比率を高くしすぎると、添加した対象物がポリグリセリンラウリン酸エステルの特性に由来して苦味、油臭やロウ臭などを有するようになり、対象物本来の味覚や風味などに影響を与える恐れがあるので好ましくない。
【００２３】
このようにして調製した甘草油性抽出物可溶化組成物は、水系対象物に対する溶解性が極めて高く、任意の割合で対象物に添加することが可能である。なお、甘草油性抽出物可溶化組成物の粘性が高く、その取扱性に困難性を伴う場合は、水やエタノールなどのアルコールを添加して粘性を低くした組成物にしてもよいし、使用時に組成物を水やエタノールなどのアルコールで希釈して用いてもよい。また、甘草油性抽出物可溶化組成物中において、甘草油性抽出物成分は可溶化状態で存在するため、この組成物を対象物に添加した際には、添加対象物の澄明性（本発明における澄明性とは濁りまたは曇りがなく、澄んだ状態であることを意味する）に与える影響が皆無に等しい。さらに、酸や食塩や糖質など共存物質存在条件下においても添加対象物の澄明性に与える影響が極めて少ないため、飲料、液状調味料、液状化粧品、液状医薬部外品などの各種水系対象物に甘草油性抽出物を添加対象物の性状に影響を与えることなく含有させることができる。
【００２４】
本発明を適用しうる液状食品としては、例えば、飲料としては玉露、抹茶、煎茶、釜入り茶、番茶などの茶類、ウーロン茶、包種茶、白茶などの半発酵茶類、中国紅茶、イギリス紅茶などの発酵茶類、黒茶、プーアル茶などの微生物発酵茶類、ほうじ茶、玄米茶、着香茶などの加工茶類、麦茶などの穀物茶、混合茶、健康茶、薬草茶、またはこれらの飲料、コーヒー、コーヒー飲料、ココア、天然果汁、天然果汁飲料、果汁入り清涼飲料、果肉飲料、果粒入り果実飲料、トマトジュース、野菜ジュースなどの野菜系飲料、牛乳、加工乳、乳飲料、乳酸菌飲料、豆乳、豆乳飲料、スポーツ飲料、炭酸飲料、栄養飲料、アルコール飲料などがある。また、液状調味料としては、鰹だし、昆布だし、中華だし、コンソメなどの風味調味料、マヨネーズ、タルタルソース、ケチャップ、ウスターソース、お好み焼きソース、焼きそばソース、ステーキソース、ハンバーグソース、スパゲティソースドミグラスソース、グラタンソース、ホワイトソース、カレーソースなどのソース類、中華料理用調理ミックス、炊き込み御飯用調理ミックス、雑炊用調理ミックスなどの調理ミックス類、焼肉のたれ、すき焼きのたれ、焼き鳥のたれ、うなぎ蒲焼のたれ、餃子のたれなどのたれ類、麺つゆ、ラーメンスープ、なべつゆ、天つゆ、すき焼きのつゆ、おでんのつゆなどのつゆ類、浅漬けの素、キムチの素などの漬物用調味液、醤油、だしいり醤油、ポン酢などの調味液などがある。
【００２５】
また、本発明を適用しうる液状化粧品としては、例えば、洗顔クリーム、洗顔フォーム、化粧水、美容液、パック、マッサージクリーム、乳液、モイスチャークリームなどの基礎化粧品、液体洗浄料、サンスクリーンクリームなどのボディ化粧品、シャンプー、リンス、ヘアトリートメントなどの頭髪用化粧品、ヘアトニック、スキャルプトリートメントなどの頭皮用化粧品、香水、オーデコロンなどの芳香化粧品などがある。
【００２６】
また、本発明を適用しうる液状医薬部外品としては、外皮消毒剤、傷消毒保護剤、軟膏剤、ビタミン含有保健剤、入浴剤、育毛剤、養毛剤、薬用化粧品、薬用歯磨き、洗口剤、口中清涼剤、制汗スプレーなどがある。
【００２７】
【実施例】
以下、実施例を示して本発明を説明するが、かかる説明によって本発明が何ら限定されるものでない。
【００２８】
実施例１：
（１） 甘草（Ｇｌｙｃｙｒｒｈｉｚａ ｇｌａｂｒａ Ｌ．）の根茎を粉砕し、チップ状にした。この甘草チップ１．０ｋｇを１０Ｌのエタノールで一晩抽出した後固液分離し、抽出濾液約８．５Ｌを得た。得られた抽出濾液を減圧濃縮し、析出したタール状成分を固液分離により除去した。得られた上清に活性炭を加えて脱色、および脱臭し、これを濾過した。得られた濾液を減圧濃縮し、エタノール濃度７０％になるように調整して甘草油性エキス約１．０Ｌを得た。この甘草油性抽出エキスの固形分（甘草油性抽出物）濃度は２．０％であった。
【００２９】
（２）（１）で得られた甘草油性エキスを固形分として１０重量部相当になるエキス量に、表１に示す各種のポリグリセリン脂肪酸エステル、またはショ糖脂肪酸エステル９０重量部を加えて６０℃に加温して撹拌し、両者を均一に混和させた。この混合液を減圧濃縮し、エキス中に含まれていた水、およびエタノールを留去することにより、１０％の甘草油性抽出物を含有する均一な甘草油性抽出物可溶化組成物１〜１９を得た。
【００３０】
【表１】
実施例２：
実施例１で調製した甘草油性抽出物可溶化組成物１〜１９を純水、ｐＨ３．５の０．１Ｍクエン酸緩衝液、および５％食塩水中に甘草油性抽出物成分の濃度が０．１％となるようにそれぞれ添加し、混合した。得られた混合液を９０℃まで加温し、達温から１０分間温度を維持した後に冷却した。この溶液を室温で４日間静置し、甘草油性抽出物の溶解状態を分光光度計によりＯＤ６６０ｎｍにおける透過率を測定することで調べた。その結果を表２に示す。なお、溶解分散性が著しく悪く、均一な溶液となっていないものについては、目視により判断して表１において「分離」として示した。
その結果、純水へ添加した場合ではいくつかの組成物で澄明感の高い溶液が得られたが、ｐＨ３．５の０．１Ｍクエン酸緩衝液と５％食塩水においてはほとんどの組成物で成分の分離が観察され、結果として甘草油性抽出物を酸性溶液と食塩溶液に可溶化することはもとより、分散させることもできなかった。一方、この中でＨＬＢが１４以上のポリグリセリンラウリン酸エステルを配合した組成物１３〜１５のみがいずれの対象液に添加した場合でも際立って高い澄明性をもった溶液となり、目視的にも不溶物の存在がないことが確認された。また、ＨＬＢが１３．５のポリグリセリンラウリン酸エステルを配合した組成物１６は純水に対してのみ高い溶解澄明性が確認された。なお、組成物１３〜１７で配合したポリグリセリンラウリン酸エステルのグリセリン平均重合度と平均エステル化率を表３に示す。
【００３２】
【表２】
【表３】
実施例３：
（１） 甘草（Ｇｌｙｃｙｒｒｈｉｚａ ｇｌａｂｒａ Ｌ．）の根茎を粉砕し、チップ状にした。この甘草チップ１．０ｋｇを１０Ｌのエタノールで一晩抽出した後固液分離し、抽出濾液８．５Ｌを得た。得られた抽出濾液を減圧濃縮し、析出したタール状成分を固液分離により除去した。得られた上清に活性炭を加えて脱色、および脱臭し、これを濾過した。得られた濾液を減圧濃縮し、凍結乾燥させて固形物１９．７ｇを得た。得られた固形物を細かく粉砕し、粉末状の甘草油性抽出物を得た。
【００３５】
（２）（１）で得られた甘草油性抽出物粉末５ｇに、ＨＬＢ１６のポリグリセリンラウリン酸エステル４５ｇを加え、７０℃に加温しながらホモジナイザーで混合、均質化することにより、１０％の甘草油性抽出物を含有する粘性液体の甘草油性抽出物可溶化組成物２０を得た。
【００３６】
実施例４：
実施例３の（１）で得られた甘草油性抽出物粉末４ｇに、７０％エタノール水溶液６ｇを加えて溶解させた。さらにこの溶液にＨＬＢ１６のポリグリセリンラウリン酸エステル４０ｇを加え、７０℃に加温しながらホモジナイザーで混合、均質化することにより、８％の甘草油性抽出物を含有する粘性液体の甘草油性抽出物可溶化組成物２１を得た。
【００３７】
実施例５：
実施例３で調製した甘草油性抽出物可溶化組成物２０および実施例４で調製した甘草油性抽出物可溶化組成物２１を純水、ｐＨ３．５の０．１Ｍクエン酸緩衝液、および５％食塩水中に甘草油性抽出物成分の濃度が０．１％となるようにそれぞれ添加し、混合した。この混合液を９０℃まで加温し、達温から１０分間温度を維持した後に冷却した。この溶液を室温で４日間静置し、甘草油性抽出物の溶解状態を分光光度計によりＯＤ６６０ｎｍにおける透過率を測定することで調べた。その結果を表４に示す。
その結果、表４より明らかなように、甘草油性抽出物可溶化組成物２０および甘草油性抽出物可溶化組成物２１は、いずれの対象液に添加した場合でも際立って高い澄明性をもった溶液となり、目視的にも不溶物の存在がないことが確認された。また、甘草油性抽出物可溶化組成物２１については甘草油性抽出物可溶化組成物１３および甘草油性抽出物可溶化組成物２０に比べ、各対象液に対して添加した際に、均一な溶液となるまでの時間が短く、取り扱いやすい組成物であった。この効果は、組成物の中に含まれている含水エタノールに由来するものである。
【００３８】
【表４】
実施例６：
実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３の０．２５ｇに滅菌水を加えて２５ｍＬとし、甘草油性抽出物濃度が１０００ｐｐｍのサンプル溶液を調製した。このサンプル溶液１０ｍＬに滅菌水１０ｍＬを加えて混合しサンプル濃度を１／２とした。この操作を５回繰り返し、サンプルの希釈系列を作製した。次に、滅菌したＭＵＥＬＬＥＲ−ＨＩＮＴＯＮ液体培地（Ｍｅｒｃｋ社製）９．５ｍＬにサンプル溶液０．５ｍＬを加えてよく混ぜ合わせた。このときの培地中の甘草油性抽出物濃度は５０、２５、１２．５、６．２５、３．１２５、１．５６ｐｐｍとなる。また、対照としてサンプル溶液の代わりに滅菌水０．５ｍＬを加えた培地も作製した。このように調製した液体培地中に耐熱性芽胞細菌であるＢａｃｉｌｌｕｓ ｃｅｒｅｕｓ（ＪＣＭ２１５２），Ｂ．ｃｏａｇｕｌａｎｓ（ＩＡＭ１１１５），Ｂ．ｓｕｂｔｉｌｉｓ（ＩＡＭ １２１１８），Ｂ．ｓｔｅａｒｏｔｈｅｒｍｏｐｈｉｌｕｓ（ＩＦＯ １２５５０）の各々の培養液から調製した菌液（１×１０６ＣＦＵ／ｍＬ）の５０μＬを接種した。これらを３５℃で２日間培養後（Ｂ．ｓｔｅａｒｏｔｈｅｒｍｏｐｈｉｌｕｓのみ５５℃で２日間培養）、菌の生育の有無を目視観察し、最小発育阻止濃度（ＭＩＣ）を求めた。これらの結果を表５に示す。
【００４０】
【表５】
表５から明らかなように、甘草油性抽出物可溶化組成物１３は非常に低濃度で耐熱性芽胞細菌に対して発育阻止作用を示し、優れた抗菌剤であることが示された。
【００４２】
実施例７：
実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３の０．２５ｇに滅菌水を加えて２５ｍＬとし、甘草油性抽出物濃度が１０００ｐｐｍのサンプル溶液を調製した。このサンプル溶液１０ｍＬに滅菌水１０ｍＬを加えて混合しサンプル濃度を１／２とした。この操作を５回繰り返し、サンプルの希釈系列を作製した。次に、滅菌したＹＳＧ液体培地（栄養成分として酵母エキス、スターチ、グルコースを含む）９．５ｍＬにサンプル溶液０．５ｍＬを加えてよく混ぜ合わせた。このときの培地中の甘草油性抽出物濃度は５０、２５、１２．５、６．２５、３．１２５、１．５６ｐｐｍとなる。また、対照としてサンプル溶液の代わりに滅菌水０．５ｍＬを加えた培地も作製した。このように調製した液体培地中に耐熱性好酸性菌であるＡｌｉｃｙｃｌｏｂａｃｉｌｌｕｓ ａｃｉｄｏｃａｌｄａｒｉｕｓ（ＡＴＣＣ ２７００９），Ａ．ａｃｉｄｏｔｅｒｒｅｓｔｒｉｓ（ＡＴＣＣ ４９０２５），Ａ．ｃｙｃｌｏｈｅｐｔａｎｉｃｕｓ（ＤＳＭ ４００６）の各々の培養液から調製した菌液（１×１０６ＣＦＵ／ｍＬ）の５０μｌを接種した。これらを５０℃で５日間培養後（Ａｌｉｃｙｃｌｏｂａｃｉｌｌｕｓ ａｃｉｄｏｃａｌｄａｒｉｕｓのみ５５℃で２日間培養）、菌の生育の有無を目視観察し、最小発育阻止濃度（ＭＩＣ）を求めた。これらの結果を表６に示す。
【００４３】
【表６】
表６から明らかなように、甘草油性抽出物可溶化組成物１３は非常に低濃度で耐熱性好酸性菌に対して発育阻止作用を示し、優れた抗菌剤であることが示された。
【００４５】
実施例８：
実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３の０．３７５ｇに滅菌水を加えて２５ｍＬとし、甘草油性抽出物濃度が１５００ｐｐｍのサンプル溶液を調製した。このサンプル溶液１０ｍＬに滅菌水１０ｍＬを加えて混合しサンプル濃度を１／２とした。この操作を５回繰り返し、サンプルの希釈系列を作製した。これらサンプル溶液の１ｍＬをシャーレに分注し、滅菌後に約５０℃まで放冷したポテトデキストロース寒天培地（Ｍｅｒｃｋ社製）１９ｍＬを加えたのち、スプレッターで撹拌した。このときの培地中の甘草油性抽出物濃度は７５、３７．５、１８．８、９．４、４．６９、２．３４ｐｐｍとなる。これを冷却して平板とした後、クリーンベンチ内で３０分間乾燥させた。また、対照としてサンプル溶液の代わりに滅菌水を加えた培地も作製した。このように作製した寒天平板培地の中央部に薬剤耐性かびであるＣｈａｅｔｏｎｉｕｍ ｆｕｎｉｃｏｌａあるいはＡｒｔｈｒｉｎｉｕｍ ｓａｃｃｈａｒｉの胞子液（１×１０５ＣＦＵ／ｍＬ）の５μＬを接種した。これらを室温で１時間放置した後、２５℃で３日間培養した。培養後、菌の生育の有無を目視観察し、最小発育阻止濃度（ＭＩＣ）を求めた。これらの結果を表７に示す。
【００４６】
【表７】
表７から明らかなように、甘草油性抽出物可溶化組成物１３は非常に低濃度で薬剤耐性かびに対して発育阻止作用を示し、優れた抗かび剤であることが示された。
【００４８】
以下、本発明の甘草油性抽出物可溶化組成物を添加した各種の水系対象物の製造実施例を示す。いずれの場合においても対象物本来の性状に影響を及ぼさずに甘草油性抽出物可溶化組成物を添加することができ、また、甘草油性抽出物の特性に由来した抗菌効果を期待することができた。
【００４９】
製造実施例１：
麦茶原料大麦４０ｇを９０℃のイオン交換水８００ｇで３０分間抽出し、続いて濾紙（Ｎｏ．２、アドバンテック社製）で濾過することにより原料を除去して、７２０ｇの麦茶抽出液（ｐＨ４．９，Ｂｒｉｘ０．６°）を得た。当該麦茶抽出液を３０℃以下まで冷却し、飲用濃度(Ｂｒｉｘ０．４°)となるようにイオン交換水で希釈し、Ｌ−アスコルビン酸ナトリウムと実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を最終濃度がそれぞれ３００ｐｐｍおよび３００ｐｐｍ（甘草油性抽出物濃度として３０ｐｐｍ）となるように添加した。これに炭酸水素ナトリウムを溶解してｐＨ６．０に調整した麦茶調合液を得た。これを容器に充填し、レトルト殺菌処理（１２３℃、２０分間）を行って麦茶飲料を得た。
【００５０】
製造実施例２：
紅茶３０ｇを７０℃のイオン交換水９００ｇで５分間抽出し、続いて濾紙（Ｎｏ．２、アドバンテック社製）で濾過することにより茶葉を除去して、７８０ｇの紅茶抽出液（ｐＨ５．５，Ｂｒｉｘ１．１°、タンニン濃度３００ｍｇ／１００ｍＬ）を得た。当該紅茶抽出液を３０℃以下まで冷却し、飲用濃度（タンニン濃度６０ｍｇ／１００ｍＬ）となるようにイオン交換水で希釈し、Ｌ−アスコルビン酸と実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を最終濃度がそれぞれ２００ｐｐｍおよび１５０ｐｐｍ（甘草油性抽出物濃度として１５ｐｐｍ）となるように添加した。これに炭酸水素ナトリウムを溶解してｐＨ６．０の紅茶調合液を得た。これを容器に充填し、レトルト殺菌処理（１２１℃、７分間）を行って紅茶飲料を得た。
【００５１】
製造実施例３：
ウーロン茶６５％、紅茶２０％、ジャスミン５％、陳皮４％、ハイビスカス４％およびバナバ２％を配合した原料を用いて、混合茶を試作した。混合茶３０ｇを９０℃のイオン交換水９００ｇで１０分間抽出し、続いて濾紙（ＮＯ．２、アドバンテック社製）で濾過することにより、茶葉を除去して８２０ｇの混合茶抽出液（ｐＨ ４．５、Ｂｒｉｘ０．９°、タンニン濃度 １５０ｍｇ／１００ｍＬ）を得た。当該混合茶抽出液を３０℃以下まで冷却し、飲用濃度（Ｂｒｉｘ０．２°）となるようにイオン交換水で希釈した。Ｌ−アスコルビン酸と実施例３で調製した甘草油性抽出物可溶化組成物２０を最終濃度がそれぞれ２００ｐｐｍおよび２５０ｐｐｍ（甘草油性抽出物濃度として２０ｐｐｍ）となるように添加し、これに炭酸水素ナトリウムを溶解して、ｐＨ６．０の混合茶調合液を得た。これを容器に充填し、レトルト滅菌処理（１２１℃、１５分間）を行って混合茶飲料を得た。
【００５２】
製造実施例４：
コーヒー抽出液（商品名：コーヒーエキスＭ−０−２０、Ｂｒｉｘ２０、高砂珈琲社製）、牛乳、砂糖、乳化剤（商品名：サンソフトスーパーＶ−１０３ 、太陽化学社製）、実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３およびイオン交換水の各原料を４．６５：１０：５：０．２：０．０１５：８０の配合割合で混合し、１５ｐｐｍの甘草油性抽出物を含有する混合液を得た。これに適量の炭酸水素ナトリウムを加えて、ｐＨ６．８のコーヒー飲料を得た。この調合液を６０℃まで加熱しながら、よく攪拌した。この後、ホモジナイザーにより均質化（均質圧２００ｋｇ／ｃｍ２）を行った。これを容器に充填し、レトルト滅菌処理（１２１℃、２０分間）を行ってミルクコーヒーを得た。
【００５３】
製造実施例５：
緑茶３０ｇを７０℃のイオン交換水９００ｇで５分間抽出し、続いて濾紙（Ｎｏ．２、アドバンテック社製）で濾過することにより茶葉を除去して、８００ｇの緑茶抽出液（ｐＨ６．０、Ｂｒｉｘ１．１°、タンニン濃度に７０ｍｇ／１００ｍＬ）を得た。当該緑茶抽出液を３０℃以下まで冷却し、飲用濃度（タンニン濃度６０ｍｇ／１００ｍＬ）となるようにイオン交換水で希釈し、Ｌ−アスコルビン酸と実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を最終濃度がそれぞれ２００ｐｐｍおよび１００ｐｐｍ（甘草油性抽出物濃度として１０ｐｐｍ）となるように添加した。これに炭酸水素ナトリウムを溶解してｐＨ６．０の緑茶調合液を得た。これを容器に充填し、レトルト殺菌処理（１２１℃、７分間）を行って緑茶飲料を得た。
【００５４】
製造実施例６：
ウーロン茶３０ｇを９０℃のイオン交換水９００ｇで５分間抽出し、続いて濾紙（Ｎｏ．２、アドバンテック社製）で濾過することにより茶葉を除去して、８２０ｇのウーロン茶抽出液（ｐＨ５．６、Ｂｒｉｘ０．９°、タンニン濃度２５０ｍｇ／１００ｍＬ）を得た。当該ウーロン茶抽出液を３０℃以下まで冷却し、飲用濃度（タンニン濃度５０ｍｇ／１００ｍＬ）となるようにイオン交換水で希釈し、Ｌ−アスコルビン酸と実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を最終濃度がそれぞれ２００ｐｐｍおよび１５０ｐｐｍ（甘草油性抽出物濃度として１５ｐｐｍ）となるように添加した。これに炭酸水素ナトリウムを溶解してｐＨ６．０のウーロン茶調合液を得た。これを容器に充填し、レトルト殺菌処理（１２１℃、７分間）を行ってウーロン茶飲料を得た。
【００５５】
製造実施例７：
６倍濃縮オレンジ果汁８４ｇ、加糖ブドウ糖液糖９．７ｇ、クエン酸０．０６ｇ、Ｌ−アスコルビン酸０．０２２ｇ、適量の香料および実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を０．１ｇ調合し、これにイオン交換水を加えて全量を１０００ｍＬとした。これを容器に充填し、６５℃で１０分間加熱殺菌して甘草油性抽出物濃度として１０ｐｐｍを含有するオレンジ５０％果汁飲料を得た。
【００５６】
製造実施例８：
１／６濃縮オレンジ果汁１６８ｇに適当量の香料および実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を０．１ｇ（甘草油性抽出物濃度として１０ｐｐｍ）を調合し、これにイオン交換水を加えて全量を１０００ｍＬとした。これを容器に充填し、６５℃で１０分間加熱殺菌して甘草油性抽出物濃度として１０ｐｐｍを含有するオレンジ１００％果汁飲料を得た。
【００５７】
製造実施例９：
１／４濃縮モモ果汁１３１ｇ、加糖ブドウ糖液糖９．７ｇ、クエン酸０．０６ｇ、Ｌ−アスコルビン酸０．０２２ｇ、適量の香料および実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を０．１ｇ調合し、これにイオン交換水を加えて全量を１０００ｍＬとした。これを容器に充填し、６５℃で１０分間加熱殺菌して甘草油性抽出物濃度として１０ｐｐｍを含有するモモ５０％果汁飲料を得た。
【００５８】
製造実施例１０：
４号缶に牛肉１１０ｇ、ジャガイモ（６切）６０ｇ、ニンジン（６切）５０ｇ、ドミグラスソース２１５ｇを入れ、実施例４で調製した甘草油性抽出物可溶化組成物２１の０．２１７５ｇを加えてよく混ぜ合わせた。これを１１５℃で９０分間レトルト殺菌し、甘草油性抽出物濃度として４０ｐｐｍを含有するビーフシチューを得た。
【００５９】
製造実施例１１：
しょうゆ７０ｍＬ、砂糖２５ｇ、みりん５ｍＬ、鰹節煮出し液９ｇ、核酸系調味料３ｇ、食塩２ｇ、カラメル適当量、および実施例４で調製した甘草油性抽出物可溶化組成物２１の０．５ｇを調合し、これにイオン交換水を加えて全量を１０００ｍＬとして、甘草油性抽出物濃度として４０ｐｐｍを含有する２倍濃縮の麺つゆを得た。
【００６０】
製造実施例１２：
醤油９００ｍＬ、みそ５００ｇ、砂糖４００ｇ、玉葱ペースト１００ｇ、リンゴペースト２００ｇ、ごま油６０ｇ、にんにくペースト２５０ｇ、白胡麻ペースト２０ｇを調合して煮詰めて全量を２０００ｍＬとし、これに実施例４で調製した甘草油性抽出物可溶化組成物２１の１ｇを調合して、甘草油性抽出物濃度として４０ｐｐｍを含有する焼肉のたれを得た。
【００６１】
製造実施例１３：
卵１個分の卵黄に、酢小さじ１杯と塩胡椒を適量入れ混合した。次いでこれにサラダ油１２０ｍｌをゆっくりと加えながら混合し、適量の砂糖と実施例１の（２）で調製した甘草油性抽出物可溶化組成物１３を０．０８ｇ加えて混合して甘草油性抽出物濃度として約４０ｐｐｍを含有するマヨネーズを得た。
【００６２】
製造実施例１４：
オレンジ果汁２００ｍＬにイオン交換水２００ｍＬを加えて加温し、これに砂糖９０ｇと実施例４で調製した甘草油性抽出物可溶化組成物２１の０．１２５ｇを調合した。次いでこれにゼラチン９ｇを完全に溶かした後に容器に充填して冷却固化させて甘草油性抽出物濃度として２０ｐｐｍを含有するオレンジゼリーを得た。
【００６３】
製造実施例１５：
以下の配合にて常法により、生鮮食品用鮮度保持剤を作製した（単位：重量％）。
Ｌ−アスコルビン酸 ０．５
クエン酸 ０．５
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
精製水 １００に調整
【００６４】
製造実施例１６：
以下の配合にて常法により、漬物用調味液を作製した（単位：重量％）。
昆布エキス ６．０
鰹節エキス ４．０
食塩 ４．０
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
精製水 １００に調整
【００６５】
製造実施例１７：
以下の配合にて常法により、練り歯磨きを作製した（単位：重量％）。
第２リン酸カルシウム・２水塩 ４５．０
無水ケイ酸 ２．０
グリセリン １５．０
カルボキシメチルセルロースナトリウム １．０
カラギーナン ０．３
ラウリル硫酸ナトリウム １．５
サッカリンナトリウム ０．１
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
パラオキシ安息香酸エチル ０．０１
香料 適量
精製水 １００に調整
【００６６】
製造実施例１８：
以下の配合にて常法により、化粧水を作製した（単位：重量％）。
グリセリン ５．０
ＰＥＧ１５００ ２．０
尿素 ５．０
エタノール １５．０
ＰＯＥ（２０）オレイルエーテル ２．０
メチルパラベン ０．２
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．０５
精製水 １００に調整
【００６７】
製造実施例１９：
以下の配合にて常法により、保湿美容液を作製した（単位：重量％）。
ソルビトール ８．０
１，３ブチレングリコール ５．０
ＰＥＧ１５００ ７．０
ヒアルロン酸 ０．１
エタノール ７．０
ＰＯＥオレイルアルコールエーテル １．０
オリーブ油 ０．２
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
香料 適量
精製水 １００に調整
【００６８】
製造実施例２０：
以下の配合にて常法により、透明液状シャンプーを作製した（単位：重量％）。
製造実施例２１：
以下の配合にて常法により、美白乳液を作製した（単位：重量％）。
グリセリン ８．０
１，３ブチレングリコール ５．０
ＰＯＥ（１０）ベヘニルアルコールエーテル ２．０
ソルビタンセスキオレエート ２．０
セタノール ２．０
ワセリン １．０
流動パラフィン ３．０
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
２−ヒドロキシ−４メトキシベンゾフェノン 適量
オクチルメトキシシンナメート 適量
グリチルリチン酸 適量
プラセンタリキッド 適量
精製水 １００に調整
【００７０】
製造実施例２２：
以下の配合にて常法により、洗口剤を作製した（単位：重量％）。
エタノール １５．０
グリセリン １０．０
ポリオキシエチレン硬化ヒマシ油 ２．０
サッカリンナトリウム ０．１５
実施例４で調製した甘草油性抽出物可溶化組成物２１ ０．１
リン酸二水素ナトリウム ０．１
安息香酸ナトリウム ０．０５
香料 適量
着色剤 適量
精製水 １００に調整
【００７１】
【発明の効果】
本発明によれば、酸性溶液や食塩溶液などからなる各種の水系対象物、例えば、飲料、液状調味料、液状化粧品、液状医薬部外品などに甘草油性抽出物を可溶化する方法であって、添加対象物本来の性状や味などの性質に影響を与えることなく、しかも、澄明性の高い添加対象物に甘草油性抽出物を可溶化した後もその澄明性を維持することができる方法を提供することが可能となる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for solubilizing a licorice oily extract in an aqueous object. More specifically, the present invention relates to a method for solubilizing a licorice oily extract into various water-based objects composed of an acidic solution, a salt solution, and the like, for example, beverages, liquid seasonings, liquid cosmetics, and liquid quasi drugs.
[0002]
[Prior art]
Licorice has long been known as a herbal medicine and is now used mainly as a raw material for food sweeteners, pharmaceuticals and quasi drugs. In particular, glycyrrhizin and glycyrrhetinic acid, which are water-soluble components, have been widely used in foods, pharmaceuticals, cosmetics and the like because of their excellent pharmacological actions such as anti-inflammatory action, anti-ulcer action, and anti-allergic action. In addition, licorice contains many flavonoids in addition to glycyrrhizin, and the fraction obtained by extracting licorice, which is called licorice oily extract containing these, with an organic solvent is antibacterial against bacteria and fungi (Monthly Food Chemical April issue 94) (1989) and Japanese Patent Application Laid-Open No. 59-46210), antioxidant activity (Free Radic. Biol. Med. 23 (2) 302-313 (1997)), antioxidant action of fats and oils (see JP-A-60-180784), browning enzyme inhibitory action (JP-A 62-29528 and JP-A-2- 233795 (see Japanese Patent No. 233795)).
[0003]
By the way, since there is always a risk of microbial contamination in the production of beverage products, for reasons of storage stability, when beverages are filled into steel cans or aluminum cans, they are sterilized by heating or after filling. The product was retort sterilized. However, in recent years, the use of plastic bottles is rapidly increasing in place of cans, which have been the mainstream in the past, in the form of beverage products. While PET bottles have several advantages, they are disadvantageous in that they cannot be sterilized by the above-mentioned method because they are non-heat resistant materials unlike cans that are heat resistant containers. Furthermore, in the usage scene on the consumer side, there is a concern that the recapping property that is a characteristic of PET bottles may lead to microbial contamination after opening. Also, with the rise of PET bottles, beverages with high clarity that have not been seen in the past have been sold by beverage manufacturers, but these have been used to eliminate the risk of microbial contamination and ensure transparency. It is necessary to pay attention.
[0004]
As a means for solving the above problems, there is a method of adding an antibacterial substance to a beverage. By adding an antibacterial substance, the safety of the product can be ensured even if the conditions for heat sterilization and retort sterilization are eased. Even if microorganisms are mixed into the container at the time of filling, the antibacterial effect against the microorganisms is exhibited in the product. Furthermore, by relaxing the heat sterilization conditions, quality deterioration of the beverage itself due to heating can be prevented, and an effect of maintaining the original flavor of the beverage can be expected. In recent years, in the food industry, the standards and ideas about the safety of food additives, which are chemically synthesized products, have become stricter, so natural additives have attracted attention in place of chemically synthesized products, and their demand has also increased. Yes. Under such circumstances, licorice oily extract having excellent physiological action such as strong antibacterial action as described above is one of attractive food additive materials, and its usage has already been described. Consideration has been made.
[0005]
[Problems to be solved by the invention]
When trying to add licorice oil-based extract to various water-based objects such as beverages, licorice oil-based extract has very poor solubility in water. It is a point that it cannot mix homogeneously inside. In general, there are many cases where various substances such as acids, salt, and carbohydrates coexist in water-based objects such as foods and beverages. There is a need for a method of homogeneously mixing the licorice oily extract without loss.
[0006]
As one means for solving the above problems, there is a method of adding a licorice oily extract after dissolving it in a water-soluble organic solvent. Examples of organic solvents that can be added to foods and have solubility in licorice oil extracts include ethanol, propylene glycol, and glycerin. When the licorice oily extract is dissolved in these organic solvents and added to the aqueous target, if the concentration of the organic solvent in the aqueous target is increased, naturally a large amount of licorice oily extract is dissolved in the aqueous target. It becomes possible to make it. However, since the organic solvent concentration that can be normally tolerated is limited, when an amount of licorice oily extract that exceeds the dissolving ability of the organic solvent having an acceptable concentration is added, the component is precipitated. Therefore, it must be said that it is difficult to ensure the solubility of the licorice oily extract by this method.
[0007]
Also, a method of adding a licorice oily extract as a water-dispersible preparation using a surfactant or the like has been studied. When adopting this method, especially for beverage products whose clarity is an important factor in appearance, no matter how homogeneously the licorice oil extract can be mixed, the licorice oil extract component Since it is not preferable in terms of appearance if the liquid is mixed in a turbid state in the liquid, it is essential to be mixed in a solubilized state.
[0008]
Examples of the solubilized composition of licorice oil extract using a surfactant include, for example, Japanese Patent Publication No. 4-6688 (Japanese Patent Laid-Open No. 60-233015), licorice oil extract and sucrose having an HLB of 5 or more. A composition comprising a fatty acid ester has been proposed, and it has been shown that a composition containing a licorice oil-based extract using this sucrose fatty acid ester has good solubility in pure water. However, since the sucrose fatty acid ester exhibits aggregability in an acidic solution or a salt solution, the results of the study by the present inventors that the solubility of the licorice oily extract cannot be maintained under such conditions. It became clear from. JP-A-2001-103932 proposes a composition obtained by dissolving a licorice oily extract, one or both of a sucrose fatty acid ester or a quilla extract, and gelatin in a water-soluble alcohol. . However, when this composition is used, in addition to the problems of sucrose fatty acid esters as described above, gelation due to the influence of gelatin and addition of salts or urea as a means for preventing it are inherent to the object to be added. There is a problem of affecting properties such as properties and taste.
[0009]
Therefore, the present invention is a method for solubilizing a licorice oily extract in various aqueous objects consisting of an acidic solution, a salt solution, etc., such as beverages, liquid seasonings, liquid cosmetics, liquid quasi drugs, Providing a method that can maintain the clarity of the licorice oil-based extract after solubilization of the licorice oil-based extract in a highly clarified additive without affecting the original properties and taste of the additive The purpose is to do.
[0010]
[Means for Solving the Problems]
In view of the above points, the present inventor can solubilize a licorice oily extract not only in pure water but also in an acidic solution or a salt solution without affecting the clarity thereof, and is an addition object As a result of earnest research for the purpose of providing a method capable of sufficiently exerting the excellent physiological action of the licorice oily extract without affecting the properties of polyglycerin laurate having an HLB of 14 or more Was found to be specifically superior in solubilization of licorice oily extract.
[0011]
Regarding the solubilization effect of licorice oily extract on water-based objects of polyglycerin fatty acid ester, the above-mentioned Japanese Patent Publication No. 4-6688 states that polyglycerin oleic acid monoester with HLB of 6.3 is less than pure water. Although it has been shown to have a somewhat good degree of dispersibility, the effect is not satisfactory. Further, in this publication, the solubilizing effect on an acidic solution or a salt solution is not examined, and the effect of polyglycerin laurate cannot be known from this publication. JP-A-2001-48800 describes that glycerin fatty acid esters can be used in combination when adding a licorice oily extract to a beverage. JP-A-2001-231523 discloses licorice for food and drink. There is a description that polyglycerin fatty acid ester can be used in combination when adding grabrizine which is a main antibacterial component in the oily extract. However, no detailed examination has been made in any of the publications, and the possibility that a surfactant such as glycerin fatty acid ester or polyglycerin fatty acid ester can be used for solubilization of licorice oily extract is shown. It ’s just that.
Japanese Patent Application Laid-Open No. 2000-239176 proposes a composition containing a polyhydric alcohol fatty acid ester, a licorice oily extract and fats and oils, and a polyglycerin fatty acid ester is described as the polyhydric alcohol fatty acid ester. Kaihei 2-204417 discloses a licorice oil-based extract composition using medium-chain fatty acid triglycerides as fats and oils. However, these compositions are intended for oily external preparations and cosmetics, and since they contain oils and fats, they remain insoluble in water-based objects as they are, so when they are added to water-based objects It is necessary to take means such as emulsification, and it is not suitable for addition to beverages with high clarity. JP-A-8-268837 proposes an emulsified composition containing a vegetable liquid oil, an emulsifier, a plant extract, and an aqueous phase component, which describes licorice as a plant extract, and emulsification aids. Decaglycerin lauric acid monoester is described as an agent. However, in this publication, decaglycerin lauric acid monoester is only shown to be usable as an emulsifying aid, so that the solubilizing effect on the licorice oily extract cannot be derived, and the composition Since it itself is an emulsified type, it is not suitable for addition to beverages with high clarity.
Under the above technical background, polyglycerin laurate having an HLB of 14 or more is not limited to pure water, but also to acidic solutions and salt solutions without affecting the clarity of the licorice oily extract. The fact that it is solubilized is surprising that could not have been predicted at all.
[0012]
The method for solubilizing a licorice oily extract into an aqueous object of the present invention completed through the above research process is characterized in that, as described in claim 1, polyglycerin laurate having an HLB of 14 or more is used. .
The licorice oil extract solubilization method according to claim 2 is the licorice oil extract extract solubilization method according to claim 1, wherein the polyglycerol laurate is decaglycerol laurate monoester.
The licorice oil-based extract solubilization method according to claim 3 is the licorice oil-based extract solubilization method according to claim 1 or 2, wherein the aqueous object comprises an acidic solution.
The licorice oil-based extract solubilization method according to claim 4 is the licorice oil-based extract solubilization method according to claim 1 or 2, wherein the aqueous object comprises a saline solution.
The licorice oil-based extract solubilization method according to claim 5 is the licorice oil-based extract solubilization method according to any one of claims 1 to 4, wherein the aqueous object is a beverage, a liquid seasoning, a liquid cosmetic, a liquid. It is one of quasi drugs.
Moreover, the licorice oil-based extract solubilized composition of the present invention contains a licorice oil-based extract and a polyglycerin laurate having an HLB of 14 or more as described in claim 6 and is added to an aqueous object. is there.
In addition, the present inventionBeverageAs described in claim 7, the licorice oil-based extract solubilized composition according to claim 6 is added.
Moreover, the liquid seasoning of this invention is the thing to which the licorice oil-based extract solubilization composition of Claim 6 was added as described in Claim 8.
Moreover, the liquid cosmetics of this invention are what the licorice oil-based extract solubilization composition of Claim 6 was added as Claim 9.
Moreover, the liquid quasi-drug of this invention is what the licorice oil-based extract solubilization composition of Claim 6 was added as described in Claim 10.
Moreover, the licorice oil extract solubilizer for solubilizing the licorice oil extract in the water-based object of the present invention is claimed.11As described, polyglycerin laurate having an HLB of 14 or more is used as an active ingredient.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
The licorice used as the raw material of the licorice oily extract to which the present invention is applied is a legumeGlycyrihizaBelonging to the genus plant, for example,Glycyrihiza grabra,G. uralensis,G. inflataand so on. In the present invention, any part of the roots, rhizomes, leaves and stems of these plants can be used as a raw material, but roots and / or rhizomes are preferably used as a raw material. In addition, these may be raw or dried, but dry roots and dried rhizomes that are raw materials for industrially produced glycyrrhizin, or glycyrrhizin, etc. In order to obtain, the water extraction residue after extracting with water can also be used as a raw material. In addition, licorice is often called with the name of the production area, and examples thereof include Tohoku licorice, northwest licorice, Xinjiang licorice, Mongolian licorice, Russian licorice, and Afghanistan licorice.
[0014]
The licorice water extraction residue is the above-mentioned licorice extracted with cold water, hot water or hot water, neutral or slightly alkaline cold water, hot water or hot water, or a combination of these and repeated extraction. It is a later solid residue, and the residue after extraction may be either water-containing or dry. In order to obtain the licorice oily extract according to the present invention from the licorice or licorice water extraction residue, various organic solvents may be used alone or in combination. Examples of the organic solvent include benzene, toluene, xylene, ethyl ether, methyl ethyl ketone, methyl isobutyl ketone, dichloromethane, dichloroethane, chloroform, ethyl acetate, propyl acetate, butyl acetate, acetone, methanol, ethanol, propanol, hydrous methanol, hydrous ethanol. And hydrous propanol. Furthermore, carbon dioxide can also be used as the supercritical fluid. Among these organic solvents, it is preferable to use ethanol or hydrous ethanol because there are few problems in the Food Sanitation Law.
[0015]
The conditions for obtaining the licorice oil-based extract from the licorice or licorice water extraction residue with the above-mentioned organic solvent are not particularly limited. There are a method of extracting at room temperature while adding a solvent and stirring, and a method of extracting by heating to reflux. Further, it is more preferable that these methods are repeated alone or in combination to improve extraction efficiency.
[0016]
The obtained extract can be used as it is as a licorice oily extract after removing insolubles by centrifugation or filtration, and can also be used after being concentrated by a conventional method. These may be appropriately subjected to purification such as deodorization and decolorization as long as the target physiological effect is not lowered. In this purification step, it is common to use activated carbon, synthetic adsorption resin, ion exchange resin or the like. If the extract is dried by an appropriate method, a tan extract powder can be obtained as a licorice oily extract.
[0017]
In the present invention, the liquid extract thus obtained is applied as it is, or the liquid extract is concentrated, and the extract powder or solid dried product is applied as the licorice oily extract.
[0018]
In the present invention, a polyglycerin laurate having an HLB of 14 or more, which is an active ingredient in solubilizing a licorice oily extract in an aqueous object, will be described below. First, “polyglycerin” is a polymer of glycerin, and means that the average degree of polymerization is 2 or more. The average degree of polymerization is not limited as long as the HLB is 14 or more, but the average degree of polymerization is preferably 8 to 12, and the average degree of polymerization is 10, that is, decaglycerin laurate. Is more preferable.
[0019]
Further, the polyglycerin laurate means a compound in which lauric acid is ester-bonded to a hydroxyl group in the polyglycerin molecule. In the present invention, polyglycerol lauric acid ester having an average esterification ratio of polyglycerol with lauric acid of 0.1 to 4 is preferable, and polyglycerol lauric acid monoester having 0.5 to 1.5 is more preferable.
[0020]
It should be noted that HLB means a hydrophilic-hydrophobic balance, and is well known to be an index value of the effect of a surfactant. It depends on the degree of polymerization of glycerol and the esterification rate by lauric acid. It depends.
[0021]
In order to solubilize the licorice oily extract in an aqueous object, the polyglycerin lauric acid ester is used in advance by uniformly mixing the licorice oily extract and the polyglycerin lauric acid ester in advance. A method in which a composition dissolved in glycerin laurate, that is, a licorice oil-based extract solubilized composition is prepared, and this composition is added to an aqueous object is preferred. The mixing method of the licorice oily extract and the polyglycerin lauric acid ester for preparing this composition is not particularly limited. For example, a pulverized licorice oily extract and the polyglycerin lauric acid ester are mixed with a stirrer. Or by dissolving a dried product of licorice oily extract in a volatile organic solvent such as ethanol, acetone or isopropyl alcohol or a mixed solvent of volatile organic solvent and water, and polyglycerol laurate A method of distilling the solvent using a vacuum concentrator or the like, or mixing and stirring a liquid licorice oily extract or its concentrate and polyglycerin laurate, and then using a vacuum concentrator There are methods such as distilling off, and the method can be appropriately selected from these methods.
[0022]
The mixing ratio of licorice oil-based extract to polyglycerin laurate is when the content of poorly water-soluble substance is high in the content of licorice oil-based extract, and the ratio of polyglycerin laurate is increased. The ratio of polyglycerin lauric acid ester may be reduced, and it may be appropriately adjusted according to the properties of the licorice oily extract. Generally, polyglycerin lauric acid ester is used per 1 part by weight of licorice oily extract. Is preferably 2 to 40 parts by weight, and more preferably 5 to 20 parts by weight. The higher the mixing ratio of the polyglycerol lauric acid ester, the more advantageous in terms of solubilization of the licorice oily extract, but if the mixing ratio is too high, the added object will have characteristics of the polyglycerol lauric acid ester. This is not preferable because it has a bitter taste, oily odor, waxy odor and the like, and may affect the original taste and flavor of the object.
[0023]
The licorice oil-based extract solubilized composition thus prepared has extremely high solubility in water-based objects, and can be added to the objects at an arbitrary ratio. In addition, when the viscosity of the licorice oil-based extract solubilized composition is high and its handling is difficult, the composition may be reduced in viscosity by adding an alcohol such as water or ethanol. The composition may be diluted with water or alcohol such as ethanol. In addition, in the licorice oil extract solubilized composition, since the licorice oil extract component exists in a solubilized state, when this composition is added to the object, the clarity of the object to be added (in the present invention) Clarity means no turbidity or cloudiness and a clear state). In addition, since it has very little effect on the clarity of added substances even in the presence of coexisting substances such as acid, salt and sugar, various water-based objects such as beverages, liquid seasonings, liquid cosmetics, and liquid quasi drugs The licorice oily extract can be contained without affecting the properties of the object to be added.
[0024]
Examples of liquid foods to which the present invention can be applied include, for example, gyokuro, matcha, sencha, tea with a pot, tea such as bancha, semi-fermented teas such as oolong tea, confectionery tea and white tea, Chinese tea, and the United Kingdom Fermented teas such as black tea, microorganism fermented teas such as black tea and puer tea, processed teas such as roasted tea, brown rice tea, and incense tea, grain tea such as barley tea, mixed tea, health tea, medicinal tea, or these Beverages, coffee, coffee drinks, cocoa, natural fruit juices, natural fruit juice drinks, soft drinks with fruit juices, fruit drinks, fruit drinks with fruits, tomato juice, vegetable juices and other vegetable drinks, milk, processed milk, milk drinks, Examples include lactic acid bacteria beverages, soy milk, soy milk beverages, sports beverages, carbonated beverages, nutritional beverages, and alcoholic beverages. In addition, liquid seasonings include sardines, kelp soup, Chinese soup, consomme and other flavor seasonings, mayonnaise, tartar sauce, ketchup, wooser sauce, okonomiyaki sauce, yakisoba sauce, steak sauce, hamburger sauce, spaghetti sauce dough grass sauce, Sauces such as gratin sauce, white sauce, curry sauce, cooking mix for Chinese cuisine, cooking mix for cooked rice, cooking mix such as cooking mix, yakiniku sauce, sukiyaki sauce, yakitori sauce, eel grilled eel Sauces such as sauce, dumpling sauce, noodle soup, ramen soup, nabe soup, tempura soup, sukiyaki soup, oden soup sauce, seasoning for pickles such as shallow pickles, kimchi sauce, soy sauce, There are seasonings such as dairi soy sauce and ponzu.
[0025]
Examples of liquid cosmetics to which the present invention can be applied include basic cosmetics such as face-washing creams, face-washing foams, skin lotions, cosmetic liquids, packs, massage creams, milky lotions, moisture creams, liquid cleaning agents, sunscreen creams, etc. There are body cosmetics, cosmetics for hair such as shampoo, rinse and hair treatment, cosmetics for scalp such as hair tonic and scalp treatment, and aromatic cosmetics such as perfume and eau de cologne.
[0026]
Also, liquid quasi-drugs to which the present invention can be applied include skin disinfectants, wound disinfectants, ointments, vitamin-containing health agents, bath preparations, hair restorers, hair nourishing agents, medicated cosmetics, medicated toothpastes, mouthwashes , Mouth refresher, antiperspirant spray, etc.
[0027]
【Example】
EXAMPLES Hereinafter, although an Example is shown and this invention is demonstrated, this invention is not limited at all by this description.
[0028]
Example 1:
(1) Licorice (Glycyrrhiza glabra L. et al.) Was crushed into chips. 1.0 kg of this licorice chip was extracted with 10 L of ethanol overnight and then separated into solid and liquid to obtain about 8.5 L of an extract filtrate. The obtained extract filtrate was concentrated under reduced pressure, and the precipitated tar-like component was removed by solid-liquid separation. Activated charcoal was added to the obtained supernatant to decolorize and deodorize, and this was filtered. The obtained filtrate was concentrated under reduced pressure and adjusted to an ethanol concentration of 70% to obtain about 1.0 L of licorice oily extract. The solid content (licorice oily extract) concentration of this licorice oily extract was 2.0%.
[0029]
(2) Various polyglycerin fatty acid esters or 90 parts by weight of sucrose fatty acid ester shown in Table 1 are added to the amount of the extract corresponding to 10 parts by weight of the licorice oily extract obtained in (1) as 60 parts by weight. The mixture was heated to 0 ° C. and stirred, and both were mixed uniformly. By concentrating the mixture under reduced pressure and distilling off water and ethanol contained in the extract, uniform licorice oil-based extract solubilizing compositions 1 to 19 containing 10% licorice oil-based extract were obtained. Obtained.
[0030]
[Table 1]
Example 2:
The licorice oil extract solubilized compositions 1-19 prepared in Example 1 were dissolved in pure water, 0.1 M citrate buffer at pH 3.5, and 5% saline in which the concentration of the licorice oil extract component was 0.1. % Were added to each other and mixed. The obtained mixed liquid was heated to 90 ° C., and after maintaining the temperature for 10 minutes from the reached temperature, it was cooled. This solution was allowed to stand at room temperature for 4 days, and the dissolution state of the licorice oily extract was examined by measuring the transmittance at OD 660 nm with a spectrophotometer. The results are shown in Table 2. In addition, about the thing which dissolution dispersibility is remarkably bad and was not becoming a uniform solution, it judged by visual observation and showed as "separation" in Table 1.
As a result, when added to pure water, a clear solution was obtained with some compositions, but most of the compositions were obtained with 0.1M citrate buffer solution of pH 3.5 and 5% saline. Separation of the components was observed, and as a result, the licorice oily extract could not be solubilized in the acidic solution and the salt solution, but could not be dispersed. On the other hand, even when only compositions 13 to 15 containing a polyglycerin laurate having an HLB of 14 or more are added to any of the target liquids, the solution has a remarkably high clarity and is visually insoluble. It was confirmed that there was no thing. Moreover, the composition 16 which mix | blended polyglycerin lauric acid ester whose HLB is 13.5 confirmed the high dissolution clarity only with respect to the pure water. In addition, Table 3 shows the glycerin average polymerization degree and the average esterification rate of the polyglycerin lauric acid ester blended in the compositions 13 to 17.
[0032]
[Table 2]
[Table 3]
Example 3:
(1) Licorice (Glycyrrhiza glabra L. et al.) Was crushed into chips. 1.0 kg of this licorice chip was extracted overnight with 10 L of ethanol and then separated into solid and liquid to obtain 8.5 L of an extract filtrate. The obtained extract filtrate was concentrated under reduced pressure, and the precipitated tar-like component was removed by solid-liquid separation. Activated charcoal was added to the obtained supernatant to decolorize and deodorize, and this was filtered. The obtained filtrate was concentrated under reduced pressure and lyophilized to obtain 19.7 g of a solid. The obtained solid was finely pulverized to obtain a powdered licorice oily extract.
[0035]
(2) By adding 45 g of polyglycerin laurate ester of HLB16 to 5 g of licorice oily extract powder obtained in (1), mixing and homogenizing with a homogenizer while heating to 70 ° C., 10% licorice A viscous liquid licorice oily extract solubilized composition 20 containing an oily extract was obtained.
[0036]
Example 4:
6 g of 70% aqueous ethanol solution was added to 4 g of licorice oily extract powder obtained in (1) of Example 3 and dissolved. Furthermore, 40 g of polyglycerin laurate ester of HLB16 was added to this solution, and the mixture was mixed and homogenized with a homogenizer while heating to 70 ° C., thereby allowing a viscous liquid licorice oily extract containing 8% licorice oily extract. A solubilized composition 21 was obtained.
[0037]
Example 5:
The licorice oil extract solubilized composition 20 prepared in Example 3 and the licorice oil extract solubilized composition 21 prepared in Example 4 were purified with pure water, a 0.1 M citrate buffer solution at pH 3.5, and 5%. It added and mixed so that the density | concentration of a licorice oil-based extract component might be set to 0.1% in salt water. The mixture was warmed to 90 ° C., maintained at the temperature from the attained temperature for 10 minutes, and then cooled. This solution was allowed to stand at room temperature for 4 days, and the dissolution state of the licorice oily extract was examined by measuring the transmittance at OD 660 nm with a spectrophotometer. The results are shown in Table 4.
As a result, as is clear from Table 4, the licorice oil-based extract solubilized composition 20 and the licorice oil-based extract solubilized composition 21 are solutions having an extremely high clarity even when added to any target liquid. Thus, it was confirmed visually that there was no insoluble matter. In addition, when the licorice oil-based extract solubilized composition 21 was added to each target liquid, compared to the licorice oil-based extract solubilized composition 13 and the licorice oil-based extract solubilized composition 20, a uniform solution and It was a composition that had a short time to become and was easy to handle. This effect is derived from the water-containing ethanol contained in the composition.
[0038]
[Table 4]
Example 6:
Sterile water was added to 0.25 g of the licorice oily extract solubilized composition 13 prepared in Example 1 (2) to make 25 mL, and a sample solution having a licorice oily extract concentration of 1000 ppm was prepared. 10 mL of sterilized water was added to 10 mL of this sample solution and mixed to make the sample concentration 1/2. This operation was repeated 5 times to prepare a dilution series of samples. Next, 0.5 mL of the sample solution was added to 9.5 mL of a sterilized MULERLER-HINTON liquid medium (Merck) and mixed well. The concentration of the licorice oily extract in the medium at this time is 50, 25, 12.5, 6.25, 3.125, 1.56 ppm. Moreover, the culture medium which added 0.5 mL of sterilized water instead of the sample solution as a control was also produced. The liquid medium thus prepared is a thermostable spore bacteriumBacillus cereus(JCM2152),B. coagulans(IAM1115),B. subtilis(IAM 12118),B. stearothermophilusBacterial fluid prepared from each culture solution of (IFO 12550) (1 × 106CFU / mL) was inoculated with 50 μL. After culturing these at 35 ° C. for 2 days (B. stearothermophilusOnly at 55 ° C. for 2 days), the presence or absence of bacterial growth was visually observed to determine the minimum inhibitory concentration (MIC). These results are shown in Table 5.
[0040]
[Table 5]
As is apparent from Table 5, the licorice oil-based extract solubilized composition 13 exhibited a growth inhibitory action against heat-resistant spore bacteria at a very low concentration, indicating that it was an excellent antibacterial agent.
[0042]
Example 7:
Sterile water was added to 0.25 g of the licorice oily extract solubilized composition 13 prepared in Example 1 (2) to make 25 mL, and a sample solution having a licorice oily extract concentration of 1000 ppm was prepared. 10 mL of sterilized water was added to 10 mL of this sample solution and mixed to make the sample concentration 1/2. This operation was repeated 5 times to prepare a dilution series of samples. Next, 0.5 mL of the sample solution was added to 9.5 mL of a sterilized YSG liquid medium (containing yeast extract, starch, and glucose as nutrient components) and mixed well. The concentration of the licorice oily extract in the medium at this time is 50, 25, 12.5, 6.25, 3.125, 1.56 ppm. Moreover, the culture medium which added 0.5 mL of sterilized water instead of the sample solution as a control was also produced. It is a heat-resistant acidophilic bacterium in the liquid medium thus preparedAlycyclobacillus acidocaldarius(ATCC 270099),A. acidosterrestris(ATCC 49025),A. cycloheptanicus(DSM 4006) Bacteria solution prepared from each culture solution (1 × 106CFU / mL) was inoculated with 50 μl. After culturing these at 50 ° C. for 5 days (Alycyclobacillus acidocaldariusOnly at 55 ° C. for 2 days), the presence or absence of bacterial growth was visually observed to determine the minimum inhibitory concentration (MIC). These results are shown in Table 6.
[0043]
[Table 6]
As is apparent from Table 6, the licorice oil-based extract solubilized composition 13 exhibited a growth inhibitory action against heat-resistant acidophilic bacteria at a very low concentration, indicating that it was an excellent antibacterial agent.
[0045]
Example 8:
Sterile water was added to 0.375 g of the licorice oily extract solubilized composition 13 prepared in Example 1 (2) to make 25 mL, and a sample solution having a licorice oily extract concentration of 1500 ppm was prepared. 10 mL of sterilized water was added to 10 mL of this sample solution and mixed to make the sample concentration 1/2. This operation was repeated 5 times to prepare a dilution series of samples. 1 mL of these sample solutions were dispensed into a petri dish, 19 mL of potato dextrose agar medium (Merck) cooled to about 50 ° C. after sterilization was added, and the mixture was stirred with a spreader. The concentration of the licorice oily extract in the medium at this time is 75, 37.5, 18.8, 9.4, 4.69, and 2.34 ppm. After cooling this to a flat plate, it was dried in a clean bench for 30 minutes. As a control, a medium with sterilized water added instead of the sample solution was also prepared. The center of the agar plate medium prepared in this way is drug-resistant moldChaetonium funicolaOrArthrium sacchariSpore fluid (1 × 105CFU / mL) was inoculated with 5 μL. These were left at room temperature for 1 hour and then cultured at 25 ° C. for 3 days. After culturing, the presence or absence of bacterial growth was visually observed to determine the minimum inhibitory concentration (MIC). These results are shown in Table 7.
[0046]
[Table 7]
As is clear from Table 7, the licorice oil-based extract solubilized composition 13 exhibited a growth inhibitory action against drug-resistant fungi at a very low concentration, indicating that it was an excellent antifungal agent.
[0048]
Hereinafter, production examples of various water-based objects to which the licorice oil-based extract solubilized composition of the present invention is added will be shown. In any case, the licorice oil extract solubilized composition can be added without affecting the original properties of the object, and antibacterial effects derived from the characteristics of the licorice oil extract can be expected. It was.
[0049]
Production Example 1:
40 g of barley tea raw barley is extracted with 800 g of ion-exchanged water at 90 ° C. for 30 minutes, followed by filtration through filter paper (No. 2, manufactured by Advantech) to remove the raw material, and 720 g of barley tea extract (pH 4.9). , Brix 0.6 °). The barley tea extract is cooled to 30 ° C. or less, diluted with ion-exchanged water so as to have a drinking concentration (Brix 0.4 °), and licorice oily extract prepared in sodium L-ascorbate and (2) of Example 1 The product solubilized composition 13 was added so that the final concentrations were 300 ppm and 300 ppm (30 ppm as the concentration of licorice oily extract), respectively. The barley tea preparation liquid which melt | dissolved sodium hydrogencarbonate in this and was adjusted to pH 6.0 was obtained. This was filled in a container and subjected to retort sterilization treatment (123 ° C., 20 minutes) to obtain a barley tea beverage.
[0050]
Production Example 2:
30 g of black tea was extracted with 900 g of ion-exchanged water at 70 ° C. for 5 minutes, followed by filtration with filter paper (No. 2, manufactured by Advantech) to remove tea leaves, and 780 g of black tea extract (pH 5.5, Brix 1 0.1 °, tannin concentration 300 mg / 100 mL). The black tea extract is cooled to 30 ° C. or lower, diluted with ion-exchanged water so as to have a drinking concentration (tannin concentration 60 mg / 100 mL), and licorice oily extract prepared in (2) of L-ascorbic acid and Example 1 The product solubilized composition 13 was added so that the final concentrations were 200 ppm and 150 ppm, respectively (15 ppm as the concentration of licorice oily extract). Sodium bicarbonate was dissolved in this to obtain a black tea mixture having a pH of 6.0. This was filled in a container and subjected to retort sterilization treatment (121 ° C., 7 minutes) to obtain a tea beverage.
[0051]
Production Example 3:
A mixed tea was made using a raw material blended with 65% oolong tea, 20% black tea, 5% jasmine, 4% skin, 4% hibiscus and 2% banaba. 30 g of mixed tea was extracted with 900 g of ion-exchanged water at 90 ° C. for 10 minutes, followed by filtration with filter paper (NO.2, manufactured by Advantech) to remove tea leaves and 820 g of mixed tea extract (pH 4. 5, Brix 0.9 °, tannin concentration 150 mg / 100 mL). The mixed tea extract was cooled to 30 ° C. or less and diluted with ion-exchanged water so as to have a drinking concentration (Brix 0.2 °). L-ascorbic acid and licorice oil extract solubilized composition 20 prepared in Example 3 were added so that the final concentrations were 200 ppm and 250 ppm (concentration of licorice oil extract 20 ppm), respectively, and sodium bicarbonate was added thereto. It melt | dissolved and the mixed tea preparation liquid of pH 6.0 was obtained. This was filled in a container and subjected to retort sterilization treatment (121 ° C., 15 minutes) to obtain a mixed tea beverage.
[0052]
Production Example 4:
Coffee extract (trade name: coffee extract M-0-20, Brix 20, manufactured by Takasago Coffee Co., Ltd.), milk, sugar, emulsifier (trade name: Sunsoft Super V-103, manufactured by Taiyo Chemical Co., Ltd.), Example 1 ( The licorice oil-based extract solubilized composition 13 prepared in 2) and the raw materials of ion-exchanged water were mixed at a blending ratio of 4.65: 10: 5: 0.2: 0.015: 80, and 15 ppm of licorice oily property was obtained. A liquid mixture containing the extract was obtained. An appropriate amount of sodium bicarbonate was added thereto to obtain a coffee beverage having a pH of 6.8. The preparation was stirred well while heating to 60 ° C. Thereafter, homogenization with a homogenizer (homogeneous pressure 200 kg / cm2) This was filled in a container and subjected to retort sterilization (121 ° C., 20 minutes) to obtain milk coffee.
[0053]
Production Example 5:
30 g of green tea was extracted with 900 g of ion-exchanged water at 70 ° C. for 5 minutes, followed by filtration with filter paper (No. 2, manufactured by Advantech) to remove tea leaves, and 800 g of green tea extract (pH 6.0, Brix1) 0.1 °, tannin concentration 70 mg / 100 mL). The green tea extract is cooled to 30 ° C. or lower, diluted with ion-exchanged water so as to have a drinking concentration (tannin concentration 60 mg / 100 mL), and licorice oily extract prepared in L-ascorbic acid and (2) of Example 1 The material solubilized composition 13 was added so that the final concentrations were 200 ppm and 100 ppm (10 ppm as the concentration of licorice oily extract), respectively. Sodium bicarbonate was dissolved in this to obtain a green tea preparation liquid having a pH of 6.0. This was filled in a container and subjected to retort sterilization (121 ° C., 7 minutes) to obtain a green tea beverage.
[0054]
Production Example 6:
30 g of oolong tea was extracted with 900 g of ion-exchanged water at 90 ° C. for 5 minutes, followed by filtration with filter paper (No. 2, manufactured by Advantech) to remove tea leaves, and 820 g of oolong tea extract (pH 5.6, Brix 0). 9 °, tannin concentration 250 mg / 100 mL). The oolong tea extract is cooled to 30 ° C. or less, diluted with ion-exchanged water so as to have a drinking concentration (tannin concentration 50 mg / 100 mL), and licorice oily extract prepared in L-ascorbic acid and (1) of Example 1 The product solubilized composition 13 was added so that the final concentrations were 200 ppm and 150 ppm, respectively (15 ppm as the concentration of licorice oily extract). Sodium bicarbonate was dissolved in this to obtain a oolong tea preparation solution having a pH of 6.0. This was filled in a container and subjected to retort sterilization treatment (121 ° C., 7 minutes) to obtain a oolong tea beverage.
[0055]
Production Example 7:
6 times concentrated orange fruit juice 84g, sweetened glucose liquid sugar 9.7g, citric acid 0.06g, L-ascorbic acid 0.022g, appropriate amount of flavor and licorice oily extract solubilized composition prepared in Example 1 (2) 0.1 g of the product 13 was prepared, and ion exchange water was added thereto to make a total amount of 1000 mL. This was filled in a container and sterilized by heating at 65 ° C. for 10 minutes to obtain an orange 50% fruit juice drink containing 10 ppm as a licorice oily extract concentration.
[0056]
Production Example 8:
An appropriate amount of flavor and 0.1 g of licorice oil extract solubilized composition 13 prepared in (2) of Example 1 (10 ppm as licorice oil extract concentration) were prepared in 168 g of 1/6 concentrated orange juice. Ion exchange water was added to make a total volume of 1000 mL. This was filled in a container and sterilized by heating at 65 ° C. for 10 minutes to obtain an orange 100% fruit juice drink containing 10 ppm as a licorice oily extract concentration.
[0057]
Production Example 9:
1/4 concentrated peach juice 131 g, sweetened glucose liquid sugar 9.7 g, citric acid 0.06 g, L-ascorbic acid 0.022 g, appropriate amount of flavor and solubilized licorice oily extract prepared in Example 1 (2) 0.1 g of the composition 13 was prepared, and ion exchange water was added thereto to make a total volume of 1000 mL. This was filled in a container and sterilized by heating at 65 ° C. for 10 minutes to obtain a peach 50% fruit juice drink containing 10 ppm as a concentration of licorice oily extract.
[0058]
Production Example 10:
In No. 4 can beef 110 g, potatoes (6 slices) 60 g, carrots (6 slices) 50 g, domiglas sauce 215 g, and 0.2175 g of licorice oily extract solubilized composition 21 prepared in Example 4 may be added. Mixed. This was sterilized by retort at 115 ° C. for 90 minutes to obtain a beef stew containing 40 ppm as a licorice oily extract concentration.
[0059]
Production Example 11:
70 mL of soy sauce, 25 g of sugar, 5 mL of mirin, 9 g of bonito boiled liquid, 3 g of nucleic acid seasoning, 2 g of salt, an appropriate amount of caramel, and 0.5 g of licorice oily extract solubilized composition 21 prepared in Example 4 Then, ion-exchanged water was added to make up a total volume of 1000 mL to obtain a double concentrated noodle soup containing 40 ppm as a licorice oily extract concentration.
[0060]
Production Example 12:
Soy sauce 900 mL, miso 500 g, sugar 400 g, onion paste 100 g, apple paste 200 g, sesame oil 60 g, garlic paste 250 g, and white sesame paste 20 g were prepared and boiled to a total volume of 2000 mL. 1 g of the product solubilized composition 21 was blended to obtain a yakiniku sauce containing 40 ppm as a licorice oily extract concentration.
[0061]
Production Example 13:
An egg yolk for one egg was mixed with an appropriate amount of 1 teaspoon of vinegar and salt and pepper. Next, 120 ml of salad oil was slowly added thereto and mixed, and 0.08 g of licorice oil-based extract solubilized composition 13 prepared in (1) of Example 1 was added and mixed to mix the concentration of licorice oil-based extract. As a mayonnaise containing about 40 ppm.
[0062]
Production Example 14:
200 mL of ion-exchanged water was added to 200 mL of orange juice and heated, and 90 g of sugar and 0.125 g of licorice oily extract solubilized composition 21 prepared in Example 4 were prepared. Next, 9 g of gelatin was completely dissolved in this, then filled into a container and cooled and solidified to obtain an orange jelly containing 20 ppm as a licorice oily extract concentration.
[0063]
Production Example 15:
A freshness-preserving agent for fresh food was prepared by the conventional method with the following composition (unit: wt%).
L-ascorbic acid 0.5
Citric acid 0.5
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
Adjust to purified water 100
[0064]
Production Example 16:
A seasoning solution for pickles was prepared by the conventional method with the following composition (unit:% by weight).
Kelp extract 6.0
Bud extract 4.0
Salt 4.0
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
Adjust to purified water 100
[0065]
Production Example 17:
A toothpaste was prepared by the conventional method with the following composition (unit: wt%).
Dicalcium phosphate dihydrate 45.0
Silica anhydride 2.0
Glycerin 15.0
Sodium carboxymethylcellulose 1.0
Carrageenan 0.3
Sodium lauryl sulfate 1.5
Saccharin sodium 0.1
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
Ethyl paraoxybenzoate 0.01
Perfume
Adjust to purified water 100
[0066]
Production Example 18:
A lotion was prepared in the following manner by a conventional method (unit:% by weight).
Glycerin 5.0
PEG 1500 2.0
Urea 5.0
Ethanol 15.0
POE (20) oleyl ether 2.0
Methylparaben 0.2
Licorice oily extract solubilized composition 21 prepared in Example 4 0.05
Adjust to purified water 100
[0067]
Production Example 19:
A moisturizing serum was prepared by the following method with the following composition (unit:% by weight).
Sorbitol 8.0
1,3 Butylene glycol 5.0
PEG1500 7.0
Hyaluronic acid 0.1
Ethanol 7.0
POE oleyl alcohol ether 1.0
Olive oil 0.2
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
Perfume
Adjust to purified water 100
[0068]
Production Example 20:
A transparent liquid shampoo was prepared by the conventional method with the following composition (unit:% by weight).
Production Example 21:
A whitening milky lotion was prepared by the conventional method with the following composition (unit:% by weight).
Glycerin 8.0
1,3 Butylene glycol 5.0
POE (10) behenyl alcohol ether 2.0
Sorbitan sesquioleate 2.0
Cetanol 2.0
Vaseline 1.0
Liquid paraffin 3.0
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
2-hydroxy-4methoxybenzophenone appropriate amount
Octyl methoxycinnamate appropriate amount
Glycyrrhizic acid
Placenta liquid appropriate amount
Adjust to purified water 100
[0070]
Production Example 22:
A mouthwash was prepared in the following manner by a conventional method (unit:% by weight).
Ethanol 15.0
Glycerin 10.0
Polyoxyethylene hydrogenated castor oil 2.0
Saccharin sodium 0.15
Licorice oily extract solubilized composition 21 prepared in Example 4 0.1
Sodium dihydrogen phosphate 0.1
Sodium benzoate 0.05
Perfume
Colorant appropriate amount
Adjust to purified water 100
[0071]
【The invention's effect】
According to the present invention, there is provided a method for solubilizing a licorice oily extract in various aqueous objects consisting of an acidic solution, a salt solution, etc., for example, beverages, liquid seasonings, liquid cosmetics, liquid quasi drugs, etc. In addition, there is a method that can maintain the clarity of the licorice oil-based extract after solubilizing the licorice oil-based extract in a highly clear additive object without affecting the original properties or taste of the additive object. It becomes possible to provide.
Claims (11)
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| JP2001379172A JP3935346B2 (en) | 2001-12-12 | 2001-12-12 | Method for solubilizing licorice oil-based extract in aqueous system |
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| JP3935346B2 true JP3935346B2 (en) | 2007-06-20 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2007176919A (en) * | 2005-05-19 | 2007-07-12 | Takara Bio Inc | Chalcones compound-containing composition |
| TW200808333A (en) | 2006-04-17 | 2008-02-16 | Kaneka Corp | Licorice polyphenol preparation |
| US8236360B2 (en) * | 2007-05-02 | 2012-08-07 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract and products made there from |
| US8877266B2 (en) | 2007-05-02 | 2014-11-04 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract anti-microbial and anti-inflammatory isolates and products made there from |
| WO2009001786A1 (en) * | 2007-06-22 | 2008-12-31 | Kaneka Corporation | Composition containing physiologically active substance |
| JP4755146B2 (en) * | 2007-07-03 | 2011-08-24 | 花王株式会社 | Containerized tea beverage |
| US9919017B2 (en) | 2011-02-01 | 2018-03-20 | Kaneka Corporation | Biologically active substance-containing water-solubilizing preparation and method for producing the same |
| JP6120232B1 (en) * | 2015-12-25 | 2017-04-26 | 株式会社エコハイテクコーポレーション | Fruit and fruit ripening inhibitor |
| WO2022030559A1 (en) * | 2020-08-05 | 2022-02-10 | ライオン株式会社 | Oral liquid composition |
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| JPH06219923A (en) * | 1993-01-26 | 1994-08-09 | Nippon Zetotsuku Kk | Transparent liquid composition |
| JPH10327753A (en) * | 1997-06-04 | 1998-12-15 | Nippon Suisan Kaisha Ltd | Emulsion containing oil and fat and having excellent transparency and heat-resistance and food containing the emulsion |
| JPH11236330A (en) * | 1997-11-17 | 1999-08-31 | Taisho Pharmaceut Co Ltd | Microemulsion containing vitamin ds |
| JP2001303020A (en) * | 2000-04-24 | 2001-10-31 | Sunstar Inc | Transparent liquid composition |
| JP2002187816A (en) * | 2000-10-10 | 2002-07-05 | Noevir Co Ltd | Bleaching cosmetic |
| JP2002370961A (en) * | 2001-06-13 | 2002-12-24 | Noevir Co Ltd | Skin care preparation and method for using the same |
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