JP6793306B2 - Method for manufacturing pericarp enzyme-treated product - Google Patents
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Description
本発明は、果皮酵素処理物及びその製造方法、並びに該果皮酵素処理物を用いた飲食品及びその製造方法に関する。 The present invention relates to a pericarp enzyme-treated product and a method for producing the same, and a food or drink using the pericarp enzyme-treated product and a method for producing the same.
柑橘類のフラボノイドは、一般的に果皮に多く存在し、ガン細胞のアポトーシス誘導作用、脂質代謝改善作用、抗炎症作用等の機能性を有することが報告されている。また、該フラボノイドは、柑橘類中では糖と結合した配糖体の形で存在しているが、体内では、摂取後に腸内細菌の酵素により分解されアグリコンとなって吸収される一方で、アグリコン生成能は、各人の腸内細菌叢の違いから、個人差が大きいことが知られている。 It has been reported that citrus flavonoids are generally abundant in the pericarp and have functions such as an apoptosis-inducing action of cancer cells, a lipid metabolism improving action, and an anti-inflammatory action. In addition, the flavonoids exist in citrus fruits in the form of glycosides bound to sugar, but in the body, they are decomposed by intestinal bacterial enzymes and absorbed as aglycones, while aglycones are produced. It is known that there are large individual differences in Noh due to differences in the intestinal flora of each individual.
柑橘類中のフラボノイドの回収方法として、特許文献１には、柑橘類果実の搾汁粕に微生物あるいは酵素を加えて夾雑物を分解処理する工程を含む方法が示されており、酵素としてペクチナーゼ、セルラーゼ、アミラーゼ、プロテアーセ、リパーゼ等が例示されている。また、特許文献２には、フラボノイド配糖体或いはその共役体をフラボノイドアグリコンに酵素的に転化する方法が示されており、酵素としてグリコシダーゼ、β−グリコシダーゼ、β−ガラクトシダーゼ、β−グルクロニダーゼ、ペクチナーゼ、ヘスペリジナーゼ、アントシアナーゼ、ラムノジアスターゼ、ナリンジアナーゼ及びタカジアスターゼが例示されている。 As a method for recovering flavonoids in citrus fruits, Patent Document 1 discloses a method including a step of adding a microorganism or an enzyme to squeezed lees of citrus fruits to decompose impurities, and as enzymes, pectinase, cellulase, and the like. Amylase, protease, lipase and the like are exemplified. Further, Patent Document 2 shows a method for enzymatically converting a flavonoid glycoside or a conjugate thereof into a flavonoid aglycone, and as enzymes, glycosidase, β-glycosidase, β-galactosidase, β-glucuronidase, pectinase, etc. Hesperidinase, anthocyanase, ramnodiastase, narindianase and takadiastase are exemplified.
一方、乳化剤を使用した抽出方法としては、ポリグリセリン脂肪酸エステルを使用し、エチルアルコールおよび水の抽出溶剤混合物を用いて油溶性原料（精油）を抽出し、最終的に香料を製造する方法が知られている（特許文献３）。 On the other hand, as an extraction method using an emulsifier, a method is known in which a polyglycerin fatty acid ester is used, an oil-soluble raw material (essential oil) is extracted using a mixture of ethyl alcohol and an extraction solvent of water, and finally a fragrance is produced. (Patent Document 3).
一般的な方法で抽出した柑橘類のフラボノイドは、配糖体として抽出物中に存在しているため、機能性成分として効率的に利用するためには、吸収性に優れたフラボノイドアグリコンとすることが重要である。本発明は、前記に鑑みてなされたものであり、柑橘類のフラボノイドアグリコンを含む果皮酵素処理物及びその製造方法、並びに該果皮酵素処理物を用いた飲食品及びその製造方法を提供する。 Since citrus flavonoids extracted by a general method are present in the extract as glycosides, flavonoid aglycones having excellent absorbability may be used for efficient use as a functional component. is important. The present invention has been made in view of the above, and provides a pericarp enzyme-treated product containing a citrus flavonoid aglycone and a method for producing the same, and a food and drink and a method for producing the same using the pericarp enzyme-treated product.
発明者らは、果皮を含む柑橘類原料を、乳化剤存在下で、配糖体分解酵素で処理することで、柑橘類のフラボノイドアグリコン含有量を高められることを見出し、それによって、フラボノイドアグリコンを含む果皮酵素処理物を効率的に製造できることを見出し、本発明を完成した。 The inventors have found that the flavonoid aglycone content of citrus fruits can be increased by treating the citrus raw material containing the fruit skin with a glycoside-degrading enzyme in the presence of an emulsifier, whereby the fruit skin enzyme containing the flavonoid aglycone. The present invention has been completed by finding that the processed product can be efficiently produced.
すなわち、本発明は、以下の［１］〜［７］の態様に関する。
［１］果皮を含む柑橘類原料を、乳化剤存在下で、配糖体分解酵素で処理することを特徴とする、フラボノイドアグリコン含有果皮酵素処理物の製造方法。
［２］配糖体分解酵素がβ−グルコシダーゼ活性を有する酵素である、［１］記載の果皮酵素処理物の製造方法。
［３］乳化剤のＨＬＢ値が１０〜２０である、［１］又は［２］に記載の果皮酵素処理物の製造方法。
［４］ヘスペレチン、ナリンゲニン及びエリオジクチオールのうち１種以上のフラボノイドアグリコンを含む、［１］〜［３］の何れかに記載の果皮酵素処理物の製造方法。
［５］固形分あたり０．６％以上のフラボノイドアグリコンを含む、［１］〜［４］の何れかに記載の果皮酵素処理物の製造方法。
［６］［１］〜［５］の何れかに記載の製造方法により得られる、フラボノイドアグリコン含有果皮酵素処理物。
［７］［１］〜［５］の何れかに記載の製造方法により得られる、フラボノイドアグリコン含有果皮酵素処理物を含む飲食品の製造方法。
That is, the present invention relates to the following aspects [1] to [7].
[1] A method for producing a flavonoid aglycone-containing pericarp enzyme-treated product, which comprises treating a citrus raw material containing pericarp with a glycoside-degrading enzyme in the presence of an emulsifier.
[2] The method for producing a pericarp enzyme-treated product according to [1], wherein the glycoside-degrading enzyme is an enzyme having β-glucosidase activity.
[3] The method for producing a pericarp enzyme-treated product according to [1] or [2], wherein the HLB value of the emulsifier is 10 to 20.
[4] The method for producing a pericarp enzyme-treated product according to any one of [1] to [3], which comprises one or more flavonoid aglycones among hesperetin, naringenin and eriodictyol.
[5] The method for producing a pericarp enzyme-treated product according to any one of [1] to [4], which contains 0.6% or more of flavonoid aglycone per solid content.
[6] A flavonoid aglycone-containing pericarp enzyme-treated product obtained by the production method according to any one of [1] to [5].
[7] A method for producing a food or drink containing a flavonoid aglycone-containing pericarp enzyme-treated product, which is obtained by the production method according to any one of [1] to [5].
本発明によって、柑橘類のフラボノイドアグリコンを固形分あたりに多く含む果皮酵素処理物を提供できる。さらに、柑橘類のフラボノイドアグリコン含有量を高めることができ、該フラボノイドアグリコンを多く含む果皮酵素処理物を簡便に製造できる製造方法を提供できる。また、該フラボノイドアグリコンは吸収性に優れているため、飲食品に含ませることで、体内に効率よく吸収され、機能性を効果的に発揮できうるフラボノイドアグリコン含有飲食品を提供できる。 INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a pericarp enzyme-treated product containing a large amount of citrus flavonoid aglycone per solid content. Further, it is possible to provide a production method capable of increasing the flavonoid aglycone content of citrus fruits and easily producing a pericarp enzyme-treated product containing a large amount of the flavonoid aglycone. Further, since the flavonoid aglycone is excellent in absorbability, it is possible to provide a flavonoid aglycone-containing food or drink that can be efficiently absorbed in the body and effectively exert its functionality by being included in the food or drink.
本発明の製造方法は、果皮を含む柑橘類原料を、乳化剤存在下で、配糖体分解酵素で処理する工程を含む。例えば、果皮を含む柑橘類原料に乳化剤及び配糖体分解酵素を添加し、加熱する工程を含む製造方法を例示でき、乳化剤添加後及び／又は配糖体分解酵素添加後に混合する工程を含むのが好ましい。 The production method of the present invention includes a step of treating a citrus raw material including pericarp with a glycoside-degrading enzyme in the presence of an emulsifier. For example, a production method including a step of adding an emulsifier and a glycoside-degrading enzyme to a citrus raw material including a fruit skin and heating the mixture can be exemplified, and the step of mixing after adding the emulsifier and / or adding the glycoside-degrading enzyme is included. preferable.
本発明に記載の柑橘類は、カンキツ属、キンカン属及びカラタチ属に含まれる植物であれば、生食用品種、調理（加工）用品種又は観賞用品種の何れでもよく、温州ミカン、オレンジ、ネーブル、グレープフルーツ、ブンタン、夏ミカン、ハッサク、シークワーサー、レモン、ダイダイ、キンカン、ユズ、カボス等が例示でき、単独又は二種類以上を組み合わせて使用してもよい。柑橘類原料は、果実、果皮、搾汁粕、加工残渣等、果皮を含む柑橘類原料であればよく、切断、破砕、細砕、粉砕等の処理を行った原料でもよく、前記の原料を乾燥した原料でもよい。 The citrus fruits described in the present invention may be any of raw edible varieties, cooking (processing) varieties or ornamental varieties as long as they are plants contained in the genus Kumquat, Kumquat and Karatachi. Examples include grapefruit, pomelo, summer orange, hassaku, shikuwasa, lemon, daidai, kumquat, yuzu, kabosu, etc., and may be used alone or in combination of two or more. The citrus raw material may be a citrus raw material containing fruit skin such as fruit, peel, juice cake, processing residue, etc., or may be a raw material that has been cut, crushed, crushed, crushed, or the like, and the above raw material is dried. It may be a raw material.
本発明に記載の乳化剤は、フラボノイドアグリコン含有量が高められれば特に限定されず、ポリグリセリン脂肪酸エステル、ショ糖脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル等、市販の食品用乳化剤を使用することができ、単独又は二種類以上を組み合わせて使用してもよい。ポリグリセリン脂肪酸エステル又はショ糖脂肪酸エステルが好ましく、ポリグリセリン脂肪酸エステルとしては、リョートー（登録商標）ポリグリエステル（三菱化学フーズ株式会社製）等、ショ糖脂肪酸エステルとしては、リョートーシュガーエステル（三菱化学フーズ株式会社製）等が例示できる。乳化剤のＨＬＢ値（Ｈｙｄｒｏｐｈｉｌｅ−Ｌｉｐｏｐｈｉｌｅ Ｂａｌａｎｃｅ Ｖａｌｕｅ、親水性−親油性バランス）が１０〜２０が好ましく、下限は１１以上がより好ましく、上限は１８以下がより好ましい。 The emulsifier described in the present invention is not particularly limited as long as the flavonoid aglycon content is increased, and commercially available food emulsifiers such as polyglycerin fatty acid ester, sucrose fatty acid ester, and polyoxyethylene sorbitan fatty acid ester can be used. , Alone or in combination of two or more. Polyglycerin fatty acid ester or sucrose fatty acid ester is preferable. Polyglycerin fatty acid ester is Ryoto (registered trademark) polyglycerate (manufactured by Mitsubishi Chemical Foods Co., Ltd.), and sucrose fatty acid ester is Ryoto sugar ester (Mitsubishi). Chemical Foods Co., Ltd.) and the like can be exemplified. The HLB value of the emulsifier (Hydrophile-Lipophile Balance Value, hydrophilic-lipophilic balance) is preferably 10 to 20, the lower limit is more preferably 11 or more, and the upper limit is more preferably 18 or less.
本発明は、乳化剤存在下で配糖体分解酵素により処理できればよく、乳化剤は、該酵素処理前又は酵素処理中に添加すればよい。乳化剤の添加割合は、フラボノイドアグリコン含有量が高められれば特に限定されないが、果皮を含む柑橘類原料１００重量％に対して、０．２重量％以上が好ましく、０．３重量％以上がより好ましく、０．５重量％以上がさらに好ましく、０．８重量％以上が特に好ましい。また上限は、２０重量％以下が好ましく、１５重量％以下がより好ましい。 The present invention may be treated with a glycoside-degrading enzyme in the presence of an emulsifier, and the emulsifier may be added before or during the enzyme treatment. The addition ratio of the emulsifier is not particularly limited as long as the flavonoid aglycone content is increased, but is preferably 0.2% by weight or more, more preferably 0.3% by weight or more, based on 100% by weight of the citrus raw material including the peel. 0.5% by weight or more is more preferable, and 0.8% by weight or more is particularly preferable. The upper limit is preferably 20% by weight or less, more preferably 15% by weight or less.
配糖体分解酵素は、配糖体のグリコシド結合を切断する活性を有するものであればよく、具体的には、グルコシダーゼ、プリメベロシダーゼ、キシロシダーゼ等を例示できる。中でもグルコシダーゼを好適に用いることができ、特にβ−グルコシダーゼ活性を有する酵素が好ましい。β−グルコシダーゼ活性を有する酵素は特に限定されるものではなく、ペニシリウム属、アスペルギルス属、シュードモナス属、リゾムコル属、クリプトコッカス属、ミクロバクテリウム属等の微生物由来の酵素が例示できる。酵素製剤としては、アロマーゼ（登録商標）（天野エンザイム株式会社製）、スミチーム（登録商標）ＢＧＡ（新日本化学工業株式会社製）、ラピダーゼ（登録商標）ＡＲ２０００（ディー・エス・エムジャパン株式会社製）等が使用できる。さらに、ペクチナーゼ、ナリンギナーゼ、ヘスペリジナーゼ等の他の酵素を併用してもよい。 The glycoside-degrading enzyme may have an activity of cleaving the glycosidic bond of the glycoside, and specific examples thereof include glucosidase, primebellosidase, and xylosidase. Among them, glucosidase can be preferably used, and an enzyme having β-glucosidase activity is particularly preferable. The enzyme having β-glucosidase activity is not particularly limited, and enzymes derived from microorganisms such as Penicillium, Aspergillus, Pseudomonas, Rizomcol, Cryptococcus, and Microbacterium can be exemplified. As enzyme preparations, Aromase (registered trademark) (manufactured by Amano Enzyme Co., Ltd.), Sumiteam (registered trademark) BGA (manufactured by Shin Nihon Kagaku Kogyo Co., Ltd.), Rapidase (registered trademark) AR2000 (manufactured by DSM Japan Co., Ltd.) ) Etc. can be used. Furthermore, other enzymes such as pectinase, naringinase and hesperidinase may be used in combination.
酵素処理は水分存在下で実施すればよく、水分は、原料中の水分でもよく、又は添加してもよい。酵素処理時の水分含量は、本発明の酵素処理物が得られれば特に限定されないが、３０〜９９重量％が好ましく、４０〜９８重量％がより好ましい。原料に水分を添加する場合は、水性溶媒を使用でき、無機塩、エタノール等を含有する水溶液でもよいが、水が好ましい。水性溶媒がエタノールを含有する場合の含量は、溶媒全体の２０重量％以下が好ましく、１０重量％以下がより好ましく、５重量％以下がさらに好ましく、２重量％以下が特に好ましい。 The enzyme treatment may be carried out in the presence of water, and the water may be the water in the raw material or may be added. The water content during the enzyme treatment is not particularly limited as long as the enzyme-treated product of the present invention can be obtained, but is preferably 30 to 99% by weight, more preferably 40 to 98% by weight. When water is added to the raw material, an aqueous solvent can be used, and an aqueous solution containing an inorganic salt, ethanol or the like may be used, but water is preferable. When the aqueous solvent contains ethanol, the content is preferably 20% by weight or less, more preferably 10% by weight or less, still more preferably 5% by weight or less, and particularly preferably 2% by weight or less.
酵素処理条件は、配糖体のグリコシド結合が切断される条件であれば特に限定されないが、例えば酵素添加量は、酵素製剤として、果皮を含む柑橘類原料を１００重量％とした場合に、好ましくは０．０１〜５重量％、より好ましくは０．０５〜３重量％である。また、処理条件は酵素の最適ｐＨ及び温度、並びにｐＨ及び温度安定性を考慮して適宜設定できるが、例えば、ｐＨ２〜８、１０〜７０℃での処理が例示でき、ｐＨ３〜７、２０〜６０℃が好ましい。処理時間は処理条件に応じて適宜調整できるが、例えば、５分間〜３０時間が例示でき、１０分間〜２４時間が好ましい。さらに、７０〜１２０℃、１分間〜６時間又は８０〜１００℃、３分間〜３時間の加熱工程を追加で行うのが好ましく、酵素の失活やフラボノイドアグリコン含有量を高めることができる。 The enzyme treatment conditions are not particularly limited as long as the glycosidic bonds of the glycosides are cleaved. For example, the amount of the enzyme added is preferably 100% by weight when the citrus raw material including the peel is 100% by weight as the enzyme preparation. It is 0.01 to 5% by weight, more preferably 0.05 to 3% by weight. Further, the treatment conditions can be appropriately set in consideration of the optimum pH and temperature of the enzyme, and the pH and temperature stability. For example, treatment at pH 2 to 8 and 10 to 70 ° C. can be exemplified, and pH 3 to 7, 20 to 20 to 20. 60 ° C is preferable. The treatment time can be appropriately adjusted according to the treatment conditions, and for example, 5 minutes to 30 hours can be exemplified, and 10 minutes to 24 hours is preferable. Further, it is preferable to additionally perform a heating step of 70 to 120 ° C. for 1 minute to 6 hours or 80 to 100 ° C. for 3 minutes to 3 hours, which can increase the inactivation of the enzyme and the flavonoid aglycone content.
本発明のフラボノイドアグリコン含有果皮酵素処理物は、フラボノイドアグリコンを固形分あたりに高含有していれば特に限定されず、そのままの形態でも利用することができるが、酵素処理後に不織布、メッシュ等を用いたろ過、遠心分離等により固液分離することで得られる液体として利用してもよいし、酵素処理物全体を乾燥させた乾燥物として利用してもよい。液体の場合はさらに濃縮及び／又は乾燥してもよい。乾燥は、ドラムドライ、エアードライ、スプレードライ、真空乾燥及び／又は凍結乾燥等により行うことができる。 The flavonoid aglycone-containing fruit skin enzyme-treated product of the present invention is not particularly limited as long as it contains a high amount of flavonoid aglycone per solid content, and can be used as it is, but a non-woven fabric, mesh or the like is used after the enzyme treatment. It may be used as a liquid obtained by solid-liquid separation by filtration, centrifugation or the like, or may be used as a dried product obtained by drying the entire enzyme-treated product. In the case of a liquid, it may be further concentrated and / or dried. The drying can be performed by drum drying, air drying, spray drying, vacuum drying and / or freeze drying and the like.
上記に記載の方法により本発明のフラボノイドアグリコン含有果皮酵素処理物を製造することができる。本発明の酵素処理物は、柑橘類の果皮由来フラボノイドアグリコンを含んでいれば特に限定されないが、ヘスペレチン、ナリンゲニン及びエリオジクチオールのうちの１種以上を含むのが好ましい。本発明の酵素処理物は、乳化剤添加のみで配糖体分解酵素未処理の果皮抽出物又は配糖体分解酵素処理のみで乳化剤無添加の処理物より多くのフラボノイドアグリコンを含んでいればよく、フラボノイドアグリコン含有量は特に限定されないが、ヘスペレチン、ナリンゲニン、エリオジクチオール等のフラボノイドアグリコンの総量として、固形分あたり０．６０重量％以上含むのが好ましく、０．７０重量％以上含むのがより好ましく、０．８０重量％以上含むのがさらに好ましく、０．９０重量％以上含むのが特に好ましい。 The flavonoid aglycone-containing pericarp enzyme-treated product of the present invention can be produced by the method described above. The enzyme-treated product of the present invention is not particularly limited as long as it contains flavonoid aglycone derived from citrus peel, but preferably contains one or more of hesperetin, naringenin and eriodictyol. The enzyme-treated product of the present invention may contain more flavonoid aglycones than the treated product containing only an emulsifier and not treated with glycoside-degrading enzyme or the treated product containing only glycoside-degrading enzyme and no emulsifier. The content of flavonoid aglycones is not particularly limited, but the total amount of flavonoid aglycones such as hesperetin, naringenin, and eriodicthiol is preferably 0.60% by weight or more, more preferably 0.70% by weight or more per solid content. , 0.80% by weight or more is more preferable, and 0.90% by weight or more is particularly preferable.
本発明のフラボノイドアグリコン含有果皮酵素処理物は、そのまま喫食しても良いが、各種飲食品に添加することにより、フラボノイドアグリコン含有果皮酵素処理物を含む、飲食品を製造できる。これにより、該酵素処理物が有する各種機能性成分を容易に各種飲食品に付加することができる。各飲食品への添加量は特に限定されないが、好ましくは０．１〜２０％、より好ましくは０．５〜１５％、さらに好ましくは１．０〜１０％である。添加する飲食品は特に限定されないが、清涼飲料、ジュース、アルコール飲料等の飲料、ケーキ、キャンデー、チョコレート等の菓子、健康食品、調味料等が例示できる。 The flavonoid aglycone-containing pericarp enzyme-treated product of the present invention may be eaten as it is, but by adding it to various foods and drinks, foods and drinks containing the flavonoid aglycone-containing pericarp enzyme-treated product can be produced. Thereby, various functional components contained in the enzyme-treated product can be easily added to various foods and drinks. The amount added to each food or drink is not particularly limited, but is preferably 0.1 to 20%, more preferably 0.5 to 15%, and even more preferably 1.0 to 10%. The food or drink to be added is not particularly limited, and examples thereof include beverages such as soft drinks, juices and alcoholic beverages, confectionery such as cakes, candies and chocolates, health foods and seasonings.
以下、実施例を示して本発明を具体的に説明するが、本発明は以下の例によって限定されるものではない。尚、本発明において、％は別記がない限り全て重量％である。 Hereinafter, the present invention will be specifically described with reference to Examples, but the present invention is not limited to the following examples. In the present invention,% is all weight% unless otherwise specified.
［実施例１］
（シークワーサー果皮酵素処理物：乳化剤及び配糖体分解酵素添加）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートー（登録商標）ポリグリエステルＯ−１５Ｄ（ＨＬＢ：１３、三菱化学フーズ株式会社製）２ｇを加えて混合した後、ペクチナーゼ製剤であるスミチーム（登録商標）ＡＰ２（新日本化学工業株式会社製）を０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼ（登録商標）（天野エンザイム株式会社製）を０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品１を１２０ｇ得た。
[Example 1]
(Shikuwasa pericarp enzyme-treated product: emulsifier and glycoside-degrading enzyme added)
After adding 50 g of tap water and 2 g of polyglycerin fatty acid ester Ryoto (registered trademark) polyglycerate O-15D (HLB: 13, manufactured by Mitsubishi Chemical Foods Co., Ltd.) as an emulsifier to 100 g of the crushed Shikuwasa peel. , 0.1 g of Sumiteam (registered trademark) AP2 (manufactured by Shin Nihon Kagaku Kogyo Co., Ltd.), which is a pectinase preparation, and Aromase (registered trademark) (manufactured by Amano Enzyme Co., Ltd.), which is a β-glucosidase preparation as a glycoside-degrading enzyme. 0.5 g was added, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of the product 1.
［実施例２］
（各ポリグリセリン脂肪酸エステル（ＨＬＢ１０以上）におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＬ−７Ｄ（ＨＬＢ：１７、三菱化学フーズ株式会社製（実施例２−１））、リョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５、三菱化学フーズ株式会社製（実施例２−２））又はリョートーポリグリエステルＳ−２４Ｄ（ＨＬＢ：１０、三菱化学フーズ株式会社製（実施例２−３））を２ｇ加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品２−１〜２−３を各１２０ｇ得た。
[Example 2]
(Shikuwasa pericarp enzyme-treated product in each polyglycerin fatty acid ester (HLB10 or higher))
To 100 g of crushed Shikuwasa peel, 50 g of tap water and Ryoto polyglycerate L-7D (HLB: 17, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 2-1)), which is a polyglycerin fatty acid ester as an emulsifier, Ryoto polygly Ester M-10D (HLB: 15, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 2-2)) or Ryoto Polyglycerate S-24D (HLB: 10, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 2-3)) After adding 2 g of each and mixing, 0.1 g of each of Sumiteam AP2, which is a pectinase preparation, and 0.5 g of aromase, which is a β-glucosidase preparation as a glycosyllytic enzyme, are added, and the enzyme treatment is performed at 60 ° C. for 2 hours. went. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of each of the products 2-1 to 2-3.
［実施例３］
（各ショ糖脂肪酸エステル（ＨＬＢ１１以上）におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてショ糖脂肪酸エステルであるリョートーシュガーエステルＳ−１６７０（ＨＬＢ：１６、三菱化学フーズ株式会社製（実施例３−１））、リョートーシュガーエステルＳ−１５７０（ＨＬＢ：１５、三菱化学フーズ株式会社製（実施例３−２））又はリョートーシュガーエステルＳ−１１７０（ＨＬＢ：１１、三菱化学フーズ株式会社製（実施例３−３））を２ｇ加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品３−１〜３−３を各１２０ｇ得た。
[Example 3]
(Shikuwasa pericarp enzyme-treated product in each sucrose fatty acid ester (HLB11 or higher))
To 100 g of crushed Shikuwasa peel, 50 g of tap water and Ryoto sugar ester S-1670 (HLB: 16, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 3-1)), which is a sucrose fatty acid ester as an emulsifier, Ryoto sugar. Emulsifier S-1570 (HLB: 15, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 3-2)) or Ryoto Sugar Ester S-1170 (HLB: 11, manufactured by Mitsubishi Chemical Foods Co., Ltd. (Example 3-3)) After adding 2 g of each and mixing, 0.1 g of each of Sumiteam AP2, which is a pectinase preparation, and 0.5 g of aromase, which is a β-glucosidase preparation as a glycosidase-degrading enzyme, are added, and the enzyme treatment is performed at 60 ° C. for 2 hours. went. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of each of the products 3-1 to 3-3.
［実施例４］
（ポリグリセリン脂肪酸エステル各添加量におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５）１０ｇ（実施例４−１）、５ｇ（実施例４−２）、２ｇ（実施例４−３）、１ｇ（実施例４−４）、０．５ｇ（実施例４−５）又は０．２ｇ（実施例４−６）を加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品４−１〜４−６を各１２０ｇ得た。
[Example 4]
(Shikuwasa pericarp enzyme-treated product at each amount of polyglycerin fatty acid ester added)
To 100 g of the crushed Shikuwasa peel, 50 g of tap water and 10 g (Example 4-1), 5 g (Example 4-2) of Ryoto polyglycerate M-10D (HLB: 15), which is a polyglycerin fatty acid ester as an emulsifier, After adding 2 g (Example 4-3), 1 g (Example 4-4), 0.5 g (Example 4-5) or 0.2 g (Example 4-6) and mixing, it is a pectinase preparation. 0.1 g each of Sumiteam AP2 and 0.5 g of aromase, which is a β-glucosidase preparation, were added as glycoside degrading enzymes, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of each of the products 4-1 to 4-6.
［実施例５］
（ショ糖脂肪酸エステル各添加量におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてショ糖脂肪酸エステルであるリョートーシュガーエステルＰ−１５７０（ＨＬＢ：１５）５ｇ（実施例５−１）、２ｇ（実施例５−２）、１ｇ（実施例５−３）、０．５ｇ（実施例５−４）又は０．２ｇ（実施例５−５）を加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品５−１〜５−５を各１２０ｇ得た。
[Example 5]
(Shikuwasa pericarp enzyme-treated product at each added amount of sucrose fatty acid ester)
To 100 g of the crushed Shikuwasa peel, 50 g of tap water and 5 g of Ryoto sugar ester P-1570 (HLB: 15) (Example 5-1) and 2 g (Example 5-2), which are sucrose fatty acid esters as emulsifiers, After adding 1 g (Example 5-3), 0.5 g (Example 5-4) or 0.2 g (Example 5-5) and mixing, 0.1 g and each of Sumiteam AP2, which is a pectinase preparation, were added. 0.5 g each of aromase, which is a β-glucosidase preparation, was added as a glycoside-degrading enzyme, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of each of the products 5-1 to 5-5.
［実施例６］
（レモン果皮酵素処理物：乳化剤及び配糖体分解酵素添加）
粉砕処理したレモン１２０ｇに乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５）６ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．１２ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．６ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、ナイロンメッシュ（１００メッシュ）を用いて搾汁することで、実施品６を８０ｇ得た。
[Example 6]
(Lemon peel enzyme treated product: Emulsifier and glycoside degrading enzyme added)
To 120 g of the pulverized lemon, 6 g of the polyglycerin fatty acid ester Ryoto polyglycerate M-10D (HLB: 15) was added as an emulsifier and mixed, and then 0.12 g of the pectinase preparation Sumiteam AP2 and the glycoside-degrading enzyme were added. As a result, 0.6 g of aromase, which is a β-glucosidase preparation, was added, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a nylon mesh (100 mesh) to obtain 80 g of the product 6.
［実施例７］
（ユズ果皮酵素処理物：乳化剤及び配糖体分解酵素添加）
粉砕処理したユズ果皮７０ｇに、水道水３５ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５）３．５ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．０７ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．３５ｇ添加して、６０℃で１時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、実施品７を７５ｇ得た。
[Example 7]
(Yuzu peel enzyme treated product: emulsifier and glycoside degrading enzyme added)
To 70 g of the crushed yuzu peel, 35 g of tap water and 3.5 g of the polyglycerin fatty acid ester Ryotopolyglycerate M-10D (HLB: 15) as an emulsifier were added and mixed, and then the pectinase preparation Sumiteam AP2 was added to 0. 0.7 g and 0.35 g of aromase, which is a β-glucosidase preparation, were added as a glycoside-degrading enzyme, and the enzyme treatment was performed at 60 ° C. for 1 hour. Then, after performing an enzyme inactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 75 g of the product 7.
［実施例８］
（グレープフルーツ果皮酵素処理物：乳化剤及び配糖体分解酵素添加）
粉砕処理したグレープフルーツ果皮７０ｇに、水道水３５ｇ及び乳化剤としてショ糖脂肪酸エステルであるリョートーシュガーエステルＰ−１５７０（ＨＬＢ：１５）１．４ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．０７ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．３５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、凍結真空乾燥することで、実施品８（乾燥品）を１０ｇ得た。
[Example 8]
(Grapefruit peel enzyme treated product: emulsifier and glycoside degrading enzyme added)
To 70 g of crushed grapefruit peel, 35 g of tap water and 1.4 g of sucrose fatty acid ester Ryoto sugar ester P-1570 (HLB: 15) as an emulsifier were added and mixed, and then Sumiteam AP2, which is a pectinase preparation, was added to 0. 0.7 g and 0.35 g of aromase, which is a β-glucosidase preparation, were added as a glycoside-degrading enzyme, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, freeze-vacuum drying was performed to obtain 10 g of the product 8 (dried product).
［比較例１］
（シークワーサー果皮抽出物：乳化剤及び配糖体分解酵素無添加）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．１ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品１を１２０ｇ得た。
[Comparative Example 1]
(Shikuwasa peel extract: no emulsifier and glycoside degrading enzyme added)
To 100 g of the pulverized Shikuwasa peel, 50 g of tap water was added and mixed, then 0.1 g of Sumiteam AP2, which is a pectinase preparation, was added, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of Comparative Product 1.
［比較例２］
（シークワーサー果皮抽出物：乳化剤添加及び配糖体分解酵素無添加）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＯ−１５Ｄ（ＨＬＢ：１３）２ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．１ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品２を１２０ｇ得た。
[Comparative Example 2]
(Shikuwasa peel extract: no emulsifier added and no glycoside degrading enzyme added)
To 100 g of the crushed Shikuwasa peel, 50 g of tap water and 2 g of the polyglycerin fatty acid ester Ryoto polyglycerate O-15D (HLB: 13) as an emulsifier were added and mixed, and then 0.1 g of the pectinase preparation Sumiteam AP2 was added. The mixture was added and treated with an enzyme at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of Comparative Product 2.
［比較例３］
（シークワーサー果皮酵素処理物：乳化剤無添加及び配糖体分解酵素添加）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品３を１２０ｇ得た。
[Comparative Example 3]
(Shikuwasa pericarp enzyme-treated product: no emulsifier added and glycoside-degrading enzyme added)
To 100 g of the crushed Shikuwasa peel, 50 g of tap water was added and mixed, and then 0.1 g of the pectinase preparation Sumiteam AP2 and 0.5 g of the β-glucosidase preparation aromase as a glycoside-degrading enzyme were added. The enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g of Comparative Product 3.
［比較例４］
（各ポリグリセリン脂肪酸エステル（ＨＬＢ９以下）におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＳ−２８Ｄ（ＨＬＢ：９、三菱化学株式会社製（比較例４−１））又はリョートーポリグリエステルＯ−５０Ｄ（ＨＬＢ：７、三菱化学株式会社製（比較例４−２））を２ｇ加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品４−１及び４−２を各１２０ｇ得た。
[Comparative Example 4]
(Shikuwasa pericarp enzyme-treated product in each polyglycerin fatty acid ester (HLB9 or less))
To 100 g of crushed Shikuwasa peel, 50 g of tap water and Ryoto polyglycerate S-28D (HLB: 9, manufactured by Mitsubishi Chemical Corporation (Comparative Example 4-1)) or Ryoto polyglycerate which is a polyglycerin fatty acid ester as an emulsifier. After adding 2 g of O-50D (HLB: 7, manufactured by Mitsubishi Chemical Corporation (Comparative Example 4-2)) and mixing, 0.1 g each of Sumiteam AP2, which is a pectinase preparation, and β-glucosidase as a glycoside-degrading enzyme 0.5 g of each of the formulation aromase was added, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g each of Comparative Products 4-1 and 4-2.
［比較例５］
（各ショ糖脂肪酸エステル（ＨＬＢ９以下）におけるシークワーサー果皮酵素処理物）
粉砕処理したシークワーサー果皮１００ｇに、水道水５０ｇ及び乳化剤としてショ糖脂肪酸エステルであるリョートーシュガーエステルＳ−９７０（ＨＬＢ：９、三菱化学株式会社製（比較例５−１））、リョートーシュガーエステルＳ−７７０（ＨＬＢ：７、三菱化学株式会社製（比較例５−２））又はリョートーシュガーエステルＳ−５７０（ＨＬＢ：５、三菱化学株式会社製（比較例５−３））を２ｇ加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を各０．１ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを各０．５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品５−１〜５−３を各１２０ｇ得た。
[Comparative Example 5]
(Shikuwasa pericarp enzyme-treated product in each sucrose fatty acid ester (HLB9 or less))
To 100 g of crushed Shikuwasa peel, 50 g of tap water and Ryoto sugar ester S-970 (HLB: 9, manufactured by Mitsubishi Chemical Corporation (Comparative Example 5-1)), which is a sucrose fatty acid ester as an emulsifier, Ryoto sugar ester Add 2 g of S-770 (HLB: 7, manufactured by Mitsubishi Chemical Corporation (Comparative Example 5-2)) or Ryoto Sugar Ester S-570 (HLB: 5, manufactured by Mitsubishi Chemical Corporation (Comparative Example 5-3)). After mixing, 0.1 g of each of Sumiteam AP2, which is a pectinase preparation, and 0.5 g of aromase, which is a β-glucosidase preparation as a glycoside-degrading enzyme, were added, and the enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme inactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 120 g each of Comparative Products 5-1 to 5-3.
［比較例６］
（レモン果皮抽出物：乳化剤添加及び配糖体分解酵素無添加）
粉砕処理したレモン１２０ｇに、乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５）６ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．１２ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、ナイロンメッシュ（１００メッシュ）を用いて搾汁することで、比較品６を８０ｇ得た。
[Comparative Example 6]
(Lemon peel extract: no emulsifier added and no glycoside degrading enzyme added)
To 120 g of the pulverized lemon, 6 g of the polyglycerin fatty acid ester Ryoto polyglycerate M-10D (HLB: 15) was added as an emulsifier and mixed, and then 0.12 g of the pectinase preparation Sumiteam AP2 was added to 60. The enzyme treatment was carried out at ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a nylon mesh (100 mesh) to obtain 80 g of Comparative Product 6.
［比較例７］
（ユズ果皮酵素処理物：乳化剤後添加及び配糖体分解酵素添加）
粉砕処理したユズ果皮７０ｇに、水道水３５ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．０７ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．３５ｇ添加して、６０℃で１時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行い、続いて乳化剤としてポリグリセリン脂肪酸エステルであるリョートーポリグリエステルＭ−１０Ｄ（ＨＬＢ：１５）３．５ｇを加えて混合し、６０℃で１時間処理した後、不織布を用いて搾汁することで、比較品７を７５ｇ得た。
[Comparative Example 7]
(Yuzu peel enzyme-treated product: added after emulsifier and glycoside-degrading enzyme)
After adding 35 g of tap water to 70 g of crushed yuzu peel and mixing, 0.07 g of Sumiteam AP2, which is a pectinase preparation, and 0.35 g of aromase, which is a β-glucosidase preparation as a glycoside-degrading enzyme, were added. The enzyme treatment was performed at 60 ° C. for 1 hour. Next, enzyme inactivation treatment was performed at 80 ° C. for 15 minutes, and then 3.5 g of Ryoto polyglycerate M-10D (HLB: 15), which is a polyglycerin fatty acid ester as an emulsifier, was added and mixed, and the mixture was mixed at 60 ° C. for 1 hour. After the treatment, the juice was squeezed using a non-woven fabric to obtain 75 g of Comparative Product 7.
［比較例８］
（ユズ果皮酵素処理物：乳化剤無添加及び配糖体分解酵素添加）
粉砕処理したユズ果皮７０ｇに、水道水３５ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．０７ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．３５ｇ添加して、６０℃で１時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、不織布を用いて搾汁することで、比較品８を７５ｇ得た。
[Comparative Example 8]
(Yuzu peel enzyme treated product: no emulsifier added and glycoside degrading enzyme added)
After adding 35 g of tap water to 70 g of crushed yuzu peel and mixing, 0.07 g of Sumiteam AP2, which is a pectinase preparation, and 0.35 g of aromase, which is a β-glucosidase preparation as a glycoside-degrading enzyme, were added. The enzyme treatment was performed at 60 ° C. for 1 hour. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, the juice was squeezed using a non-woven fabric to obtain 75 g of Comparative Product 8.
［比較例９］
（グレープフルーツ果皮酵素処理物：乳化剤無添加及び配糖体分解酵素添加）
粉砕処理したグレープフルーツ果皮７０ｇに、水道水３５ｇを加えて混合した後、ペクチナーゼ製剤であるスミチームＡＰ２を０．０７ｇ及び配糖体分解酵素としてβ−グルコシダーゼ製剤であるアロマーゼを０．３５ｇ添加して、６０℃で２時間酵素処理を行った。次いで、８０℃で１５分間酵素失活処理を行った後、凍結真空乾燥することで、比較品９（乾燥品）を９ｇ得た。
[Comparative Example 9]
(Grapefruit peel enzyme-treated product: no emulsifier added and glycoside-degrading enzyme added)
After adding 35 g of tap water to 70 g of crushed grapefruit peel and mixing, 0.07 g of Sumiteam AP2, which is a pectinase preparation, and 0.35 g of aromase, which is a β-glucosidase preparation as a glycoside-degrading enzyme, were added. The enzyme treatment was performed at 60 ° C. for 2 hours. Then, after performing enzyme deactivation treatment at 80 ° C. for 15 minutes, freeze-vacuum drying was performed to obtain 9 g of Comparative Product 9 (dried product).
［評価試験］
実施品１、２−１〜２−３、３−１〜３−３、４−１〜４−６、５−１〜５−５及び６〜８、並びに比較品１〜３、４−１、４−２、５−１〜５−３及び６〜９について、果皮を含む柑橘類原料に対する乳化剤添加割合（％）、ペクチナーゼ製剤添加割合（％）及び配糖体分解酵素添加割合（％）を表１〜８に示した。また、実施品及び比較品中の固形分を常圧加熱乾燥法により測定し、さらに、ＨＰＬＣを用いてフラボノイドアグリコン（ヘスペレチン、ナリンゲニン及びエリオジクチオール）含有量を下記測定条件にて測定し、固形分あたりの値として表１〜８に示した。なお、表１〜５記載の試料は何れもナリンゲニン及びエリオジクチオールは不検出だった。また、表７記載の試料は何れもエリオジクチオールは不検出で、表８記載の試料は何れもヘスペレチン及びエリオジクチオールは不検出だった。
[Evaluation test]
Implemented products 1, 2-1 to 2-3, 3-1 to 3, 4-1 to 4-6, 5-1 to 5-5 and 6 to 8, and comparative products 1, 3 and 4-1 , 4-2, 5-1-5-3 and 6-9, the emulsifier addition ratio (%), the pectinase preparation addition ratio (%) and the glycoside degrading enzyme addition ratio (%) to the citrus raw material including the peel. It is shown in Tables 1-8. In addition, the solid content in the product and the comparative product was measured by the atmospheric heating and drying method, and the flavonoid aglycone (hesperetin, naringenin and eriodictyol) content was measured by HPLC using the following measurement conditions to obtain solids. The values per minute are shown in Tables 1-8. Naringenin and eriodictyol were not detected in any of the samples shown in Tables 1 to 5. In addition, eriodictyol was not detected in any of the samples shown in Table 7, and hesperetin and eriodictyol were not detected in any of the samples shown in Table 8.
＜ＨＰＬＣ測定条件：ヘスペレチン、ナリンゲニン又はエリオジクチオール＞
検出器：ＵＶ検出器（紫外波長２６０ｎｍ）
カラム：ＩｎｅｒｔＳｕｓｔａｉｎ Ｃ１８（内径４．６ｍｍ、長さ２５０ｍｍ）
移動相Ａ：１５容量％アセトニトリル水溶液（０．１容量％リン酸含有）
移動相Ｂ：４０容量％アセトニトリル水溶液（０．１容量％リン酸含有）
グラジエント：移動相Ａから移動相Ｂへのグラジエント（４５分間）
流速：１．０ｍｌ／分
カラム温度：４０℃
標品：ヘスペレチン（東京化成工業株式会社製）、ナリンゲニン（和光純薬工業株式会社製）又はエリオジクチオール（和光純薬工業株式会社製）を８０％アセトニトリル水溶液に溶解した後、適宜希釈し、各検量線を作成した。
検体：各試料を８０％アセトニトリル水溶液で、適宜希釈したもの。
<HPLC measurement conditions: hesperetin, naringenin or eriodictyol>
Detector: UV detector (ultraviolet wavelength 260 nm)
Column: InertStain C18 (inner diameter 4.6 mm, length 250 mm)
Mobile phase A: 15% by volume acetonitrile aqueous solution (containing 0.1% by volume phosphoric acid)
Mobile phase B: 40% by volume acetonitrile aqueous solution (containing 0.1% by volume phosphoric acid)
Gradient: Gradient from mobile phase A to mobile phase B (45 minutes)
Flow velocity: 1.0 ml / min Column temperature: 40 ° C
Standard: Hesperetin (manufactured by Tokyo Chemical Industry Co., Ltd.), naringenin (manufactured by Wako Pure Chemical Industries, Ltd.) or eriodictyol (manufactured by Wako Pure Chemical Industries, Ltd.) is dissolved in an 80% aqueous acetonitrile solution and then diluted appropriately. Each calibration line was created.
Specimen: Each sample is appropriately diluted with an 80% aqueous acetonitrile solution.
表１より、シークワーサー果皮について、乳化剤及び配糖体分解酵素無添加で処理した比較品１、並びに乳化剤添加及び配糖体分解酵素無添加で処理した比較品２は何れもヘスペレチンが不検出だったのに対し、配糖体分解酵素を添加して処理した実施品１及び比較品３ではヘスペレチンが検出された。さらに、乳化剤存在下で配糖体分解酵素により処理した実施品１の固形分あたりのヘスペレチン含有量は、乳化剤非存在下で配糖体分解酵素により処理した比較品３に比べて約２倍高かった。よって、シークワーサー果皮について、乳化剤存在下で配糖体分解酵素により処理することで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 1, hesperetin was not detected in both the comparative product 1 treated with no emulsifier and glycoside degrading enzyme and the comparative product 2 treated with emulsifier added and no glycoside degrading enzyme added to the shikuwasa peel. On the other hand, hesperetin was detected in the product 1 and the comparative product 3 treated by adding a glycoside degrading enzyme. Furthermore, the hesperetin content per solid content of the product 1 treated with the glycoside-degrading enzyme in the presence of the emulsifier was about twice as high as that of the comparative product 3 treated with the glycoside-degrading enzyme in the absence of the emulsifier. Emulsifier. Therefore, it was found that the flavonoid aglycone content can be increased by treating the shikuwasa peel with a glycoside-degrading enzyme in the presence of an emulsifier.
表２より、シークワーサー果皮について、乳化剤として、ＨＬＢが１０〜１７のポリグリセリン脂肪酸エステルを用いた実施品２−１〜２−３の固形分あたりのヘスペレチン含有量は、ＨＬＢが７又は９のポリグリセリン脂肪酸エステルを用いた比較品４−１又は４−２に比べて約１．５〜２．４倍高かった。よって、シークワーサー果皮について、乳化剤として、ＨＬＢが１０以上のポリグリセリン脂肪酸エステルを用いることで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 2, the hesperetin content per solid content of the products 2-1 to 2-3 using the polyglycerin fatty acid ester having an HLB of 10 to 17 as an emulsifier for the Shikuwasa peel is a poly having an HLB of 7 or 9. It was about 1.5 to 2.4 times higher than the comparative product 4-1 or 4-2 using the glycerin fatty acid ester. Therefore, it was found that the flavonoid aglycone content can be increased by using a polyglycerin fatty acid ester having an HLB of 10 or more as an emulsifier for the shikuwasa peel.
表３より、シークワーサー果皮について、乳化剤として、ＨＬＢが１１〜１６のショ糖脂肪酸エステルを用いた実施品３−１〜３−３の固形分あたりのヘスペレチン含有量は、ＨＬＢが５〜９のショ糖脂肪酸エステルを用いた比較品５−１〜５−３に比べて約１．３〜２．４倍高かった。よって、シークワーサー果皮について、乳化剤として、ＨＬＢが１１以上のショ糖脂肪酸エステルを用いることで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 3, the hesperetin content per solid content of the products 3-1 to 3-3 using the sucrose fatty acid ester having an HLB of 11 to 16 as an emulsifier for the citrus depressa peel is a sucrose having an HLB of 5 to 9. It was about 1.3 to 2.4 times higher than the comparative products 5-1 to 5-3 using the sugar fatty acid ester. Therefore, it was found that the flavonoid aglycone content can be increased by using a sucrose fatty acid ester having an HLB of 11 or more as an emulsifier for the shikuwasa peel.
表４より、シークワーサー果皮について、原料に対して乳化剤として０．２％〜１０％のポリグリセリン脂肪酸エステル（ＨＬＢ：１５）を添加することで、何れもヘスペレチンが検出されることが分かった。さらに、０．２％〜１０％のポリグリセリン脂肪酸エステル（ＨＬＢ：１５）を添加した実施品４−１〜４−６の固形分あたりのヘスペレチン含有量は、乳化剤非存在下で配糖体分解酵素により処理した表１の比較品３に比べて約１．２〜２．１倍高かった。よって、シークワーサー果皮について、乳化剤として、原料に対して０．２％以上のポリグリセリン脂肪酸エステル（ＨＬＢ：１５）を添加することで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 4, it was found that hesperetin was detected in each of the Shikuwasa peels by adding 0.2% to 10% of polyglycerin fatty acid ester (HLB: 15) as an emulsifier to the raw material. Further, the hesperetin content per solid content of the products 4-1 to 4-6 to which 0.2% to 10% of polyglycerin fatty acid ester (HLB: 15) was added was glycoside decomposition in the absence of an emulsifier. It was about 1.2 to 2.1 times higher than that of Comparative Product 3 in Table 1 treated with an enzyme. Therefore, it was found that the flavonoid aglycone content can be increased by adding 0.2% or more of polyglycerin fatty acid ester (HLB: 15) as an emulsifier to the shikuwasa peel.
表５より、シークワーサー果皮について、原料に対して乳化剤として０．２％〜５％のショ糖脂肪酸エステル（ＨＬＢ：１５）を添加することで、何れもヘスペレチンが検出されることが分かった。さらに、０．２％〜５％のショ糖脂肪酸エステル（ＨＬＢ：１５）を添加した実施品５−１〜５−５の固形分あたりのヘスペレチン含有量は、乳化剤非存在下で配糖体分解酵素により処理した表１の比較品３に比べて約１．２〜１．６倍高かった。よって、シークワーサー果皮について、乳化剤として、原料に対して０．２％以上のショ糖脂肪酸エステル（ＨＬＢ：１５）を添加することで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 5, it was found that hesperetin was detected in each of the shikuwasa peels by adding 0.2% to 5% sucrose fatty acid ester (HLB: 15) as an emulsifier to the raw material. Furthermore, the hesperetin content per solid content of the products 5-1 to 5-5 to which 0.2% to 5% sucrose fatty acid ester (HLB: 15) was added was glycoside decomposition in the absence of an emulsifier. It was about 1.2 to 1.6 times higher than that of Comparative Product 3 in Table 1 treated with an enzyme. Therefore, it was found that the flavonoid aglycone content can be increased by adding 0.2% or more of sucrose fatty acid ester (HLB: 15) to the raw material as an emulsifier for the shikuwasa peel.
表６より、レモンについて、乳化剤存在下で配糖体分解酵素無添加で処理した比較品６はヘスペレチン、ナリンゲニン及びエリオジクチオールが不検出だったのに対し、乳化剤存在下で配糖体分解酵素を添加して処理した実施品６ではヘスペレチン、ナリンゲニン及びエリオジクチオールが検出された。よって、レモンについて、乳化剤存在下で配糖体分解酵素により処理することで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 6, hesperetin, naringenin and eriodictyol were not detected in Comparative Product 6 in which lemon was treated with no glycoside-degrading enzyme in the presence of an emulsifier, whereas glycoside-degrading enzyme was not detected in the presence of an emulsifier. Hesperetin, naringenin and eriodictyol were detected in the product 6 treated with the addition of. Therefore, it was found that the flavonoid aglycone content can be increased by treating lemon with a glycoside-degrading enzyme in the presence of an emulsifier.
表７より、ユズ果皮について、乳化剤存在下で配糖体分解酵素により処理した実施品７の固形分あたりのヘスペレチン及びナリンゲニンの合計含有量は、乳化剤非存在下で配糖体分解酵素により処理し、酵素を失活させた後に乳化剤を添加した比較品７及び乳化剤非存在下で配糖体分解酵素により処理した比較品８に比べて約１．６倍高かった。よって、ユズ果皮について、乳化剤存在下で配糖体分解酵素により処理することで、フラボノイドアグリコン含有量を高めることができることが分かった。 From Table 7, the total content of hesperetin and naringenin per solid content of the product 7 treated with the glycoside-degrading enzyme in the presence of the emulsifier for the yuzu peel was treated with the glycoside-degrading enzyme in the absence of the emulsifier. It was about 1.6 times higher than that of Comparative Product 7 to which an emulsifier was added after inactivating the enzyme and Comparative Product 8 treated with a glycoside-degrading enzyme in the absence of an emulsifier. Therefore, it was found that the flavonoid aglycone content can be increased by treating the yuzu peel with a glycoside-degrading enzyme in the presence of an emulsifier.
表８より、グレープフルーツ果皮について、乳化剤存在下で配糖体分解酵素により処理した実施品８の固形分あたりのナリンゲニンの含有量は、乳化剤非存在下で配糖体分解酵素により処理した比較品９に比べて約２．２倍高かった。よって、グレープフルーツ果皮について、乳化剤存在下で配糖体分解酵素により処理することで、フラボノイドアグリコン含有量を高めることができることが分かった。さらに、酵素処理物を搾汁せず乾燥させた乾燥品においてもフラボノイドアグリコンを高含有することが分かった。 From Table 8, the content of naringenin per solid content of the product 8 treated with the glycoside-degrading enzyme in the presence of the emulsifier for the grapefruit peel is the comparative product 9 treated with the glycoside-degrading enzyme in the absence of the emulsifier. It was about 2.2 times higher than that of. Therefore, it was found that the flavonoid aglycone content can be increased by treating the grapefruit peel with a glycoside-degrading enzyme in the presence of an emulsifier. Furthermore, it was found that the flavonoid aglycone content was also high in the dried product obtained by drying the enzyme-treated product without squeezing it.
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