JP4751205B2 - Method for producing purified green tea extract - Google Patents
Method for producing purified green tea extract Download PDFInfo
- Publication number
- JP4751205B2 JP4751205B2 JP2006021442A JP2006021442A JP4751205B2 JP 4751205 B2 JP4751205 B2 JP 4751205B2 JP 2006021442 A JP2006021442 A JP 2006021442A JP 2006021442 A JP2006021442 A JP 2006021442A JP 4751205 B2 JP4751205 B2 JP 4751205B2
- Authority
- JP
- Japan
- Prior art keywords
- green tea
- tea extract
- mass
- water
- organic solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 235000020688 green tea extract Nutrition 0.000 title claims description 107
- 229940094952 green tea extract Drugs 0.000 title claims description 106
- 238000004519 manufacturing process Methods 0.000 title claims description 18
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- 235000005487 catechin Nutrition 0.000 claims description 67
- 150000001765 catechin Chemical class 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 229920000642 polymer Polymers 0.000 claims description 50
- 235000013361 beverage Nutrition 0.000 claims description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 46
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- 238000011282 treatment Methods 0.000 claims description 39
- 239000003960 organic solvent Substances 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000003463 adsorbent Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 22
- 108010038851 tannase Proteins 0.000 claims description 19
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- 239000000284 extract Substances 0.000 description 18
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Landscapes
- Tea And Coffee (AREA)
Description
本発明は非重合カテキンを高濃度含有し、容器詰飲料製造時の濁りの発生しない精製緑茶抽出物の製造法に関する。 The present invention relates to a method for producing a purified green tea extract containing a high concentration of non-polymerized catechins and free of turbidity during the production of packaged beverages.
カテキン類はコレステロール上昇抑制作用やα−アミラーゼ活性阻害作用等を有することが知られている（特許文献１〜２）。カテキン類のこのような生理効果を発現させるには、成人一日あたり４〜５杯のお茶を飲むことが必要である。このため、より簡便に大量のカテキン類を摂取できるよう、飲料にカテキン類を高濃度に配合する技術が望まれている。この方法の一つとして、緑茶抽出物の濃縮物（特許文献３）等を利用して、カテキン類を飲料に溶解状態で添加する方法がある。 It is known that catechins have a cholesterol elevation inhibitory action, an α-amylase activity inhibitory action and the like (Patent Documents 1 and 2). In order to develop such physiological effects of catechins, it is necessary to drink 4-5 cups of tea per day for adults. For this reason, the technique of mix | blending catechins with high concentration in a drink is desired so that a large amount of catechins can be ingested more simply. As one of the methods, there is a method of adding catechins to a beverage in a dissolved state using a concentrate of green tea extract (Patent Document 3) or the like.
また、茶葉から抽出した水溶性成分を、合成吸着剤を充填したカラムに注入し、水又は溶剤で洗浄してからエタノール等で脱着させて高収率で高純度なカテキン類を得る方法（特許文献４）、ゲル型合成吸着剤を充填したクロマトカラムに茶葉抽出液を通液し、水でカラムを洗浄後、エタノール等で溶出させて高純度カテキン類を製造する方法（特許文献５）等が知られている。これら合成吸着剤を用いた茶抽出物の精製方法は、夾雑する物質を吸着させずに目的物質であるカテキン類を吸着し、有機溶剤で脱着させるものである。そのために、有機溶剤の使用量が多く、また操作も複雑になり、更には、澱・沈殿物に対する考慮は何もされていない。
本発明の目的は、簡便な製造工程で、高純度で高濃度の非重合体カテキン類を含有し、かつ澱・沈殿物が発生しない精製緑茶抽出物の製造法を提供することにある。 An object of the present invention is to provide a method for producing a purified green tea extract containing high-purity and high-concentration non-polymer catechins and free of starch and precipitates by a simple production process.
本発明者らは、緑茶抽出物を有機溶媒と水の混合溶液に分散し、活性炭、酸性白土又は活性白土、及び合成吸着剤で処理すると、簡便な製造工程でありながら、高濃度の非重合体カテキン類を含有し、かつ澱・沈殿物を生じない精製緑茶抽出物が得られることを見出した。 The present inventors disperse a green tea extract in a mixed solution of an organic solvent and water and treat it with activated carbon, acidic clay or activated clay, and a synthetic adsorbent. It has been found that a purified green tea extract containing coalesced catechins and free of starch / precipitate can be obtained.
本発明は、有機溶媒と水の質量比が９１／９〜９７／３の混合溶液に緑茶抽出物を分散させ、活性炭、酸性白土又は活性白土、及び合成吸着剤による接触処理を行う非重合体カテキン類を固形分中に２５〜９０質量％含有する精製緑茶抽出物の製造法を提供するものである。 The present invention relates to a non-polymer in which a green tea extract is dispersed in a mixed solution having an organic solvent and water mass ratio of 91/9 to 97/3 and subjected to contact treatment with activated carbon, acidic clay or activated clay, and a synthetic adsorbent. The present invention provides a method for producing a purified green tea extract containing catechins in a solid content of 25 to 90% by mass.
また、本発明は、上記製造法で得られた、非重合体カテキン類を固形分中に２５〜９０質量％含有する精製緑茶抽出物及びそれを配合する容器詰飲料を提供するものである。 Moreover, this invention provides the refined green tea extract which contains the non-polymer catechins obtained by the said manufacturing method in 25-90 mass% in solid content, and the container-packed drink which mix | blends it.
本発明の製造法は工程が簡易で、製造された精製緑茶抽出物は、カフェイン濃度が低く、濁り成分が低減されているにもかかわらず、高い非重合体カテキン類濃度を維持しており、かつ色相がよい。これを含有する容器詰飲料は、製造時及び長時間保存しても緑茶抽出物に含まれる濁り成分に由来する澱・沈殿が発生せず、澄明で安定した外観を呈する。 The production method of the present invention has a simple process, and the produced purified green tea extract maintains a high concentration of non-polymer catechins despite a low caffeine concentration and reduced turbidity components. And the hue is good. The container-packed drink containing this does not generate starch / precipitation derived from the turbid component contained in the green tea extract even during production and storage for a long time, and exhibits a clear and stable appearance.
本発明で用いる緑茶抽出物は、非重合体カテキン類を１種以上含有するものである。本発明において非重合体カテキン類とは、カテキン、ガロカテキン、カテキンガレート、ガロカテキンガレート等の非エピ体カテキン類及びエピカテキン、エピガロカテキン、エピカテキンガレート、エピガロカテキンガレート等のエピ体カテキン類をあわせての総称である。 The green tea extract used in the present invention contains one or more non-polymer catechins. Non-polymer catechins in the present invention are non-epimeric catechins such as catechin, gallocatechin, catechin gallate, gallocatechin gallate, and epicatechins such as epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, etc. Is a collective term.
本発明におけるガレート体率とは、カテキンガレートとガロカテキンガレートとエピカテキンガレートとエピガロカテキンガレート４種の質量和が８種からなる非重合体カテキン類の質量和に対する１００分率の値である。 The gallate body ratio in the present invention is a value of 100 fraction with respect to the mass sum of non-polymer catechins consisting of 8 kinds of catechin gallate, gallocatechin gallate, epicatechin gallate and epigallocatechin gallate. .
本発明で用いる緑茶抽出物としては、緑茶、紅茶、烏龍茶等の茶葉から得られた抽出液が挙げられる。その他のカフェイン含有植物由来、例えばコーヒー等のカフェインと茶抽出液の混合物等も用いることができる。使用する茶葉としては、より具体的には、Ｃａｍｅｌｌｉａ属、例えばＣ．ｓｉｎｅｎｓｉｓ、Ｃ．ａｓｓａｍｉｃａ及びやぶきた種又はそれらの雑種等から得られる茶葉から製茶された茶葉が挙げられる。製茶された茶葉には、煎茶、番茶、玉露、てん茶、釜炒り茶等の緑茶類がある。このような非重合体カテキン類を含有する緑茶抽出物としては、緑茶の茶葉から得られた抽出液を乾燥又は濃縮したもの等が好ましい。 Examples of the green tea extract used in the present invention include extracts obtained from tea leaves such as green tea, black tea and oolong tea. Other caffeine-containing plant origins such as a mixture of caffeine such as coffee and tea extract can also be used. More specifically, as the tea leaves to be used, Camellia genus such as C.I. sinensis, C.I. Examples include tea leaves made from tea leaves obtained from assamica and Yabukita seeds or hybrids thereof. The tea leaves produced include green teas such as sencha, bancha, gyokuro, tencha, and kettle roasted tea. As such a green tea extract containing non-polymer catechins, an extract obtained by drying or concentrating an extract obtained from green tea leaves is preferable.
茶葉からの抽出は、抽出溶媒として水を使用し、攪拌抽出等により行われる。抽出の際、水にあらかじめアスコルビン酸ナトリウム等の有機酸塩類又は有機酸を添加してもよい。また、煮沸脱気や窒素ガス等の不活性ガスを通気して溶存酸素を除去しつつ、いわゆる非酸化的雰囲気下で抽出する方法を併用してもよい。このようにして得られた抽出液は、乾燥、濃縮して本発明に使用する緑茶抽出物を得る。緑茶抽出物の形態としては、液体、スラリー、半固体、固体の状態が挙げられる。エタノール等の有機溶媒中での分散性の観点から、スラリー、半固体、固体の状態が好ましい。 Extraction from tea leaves is performed by stirring extraction or the like using water as an extraction solvent. At the time of extraction, an organic acid salt such as sodium ascorbate or an organic acid may be added to water in advance. Moreover, you may use together the method of extracting in so-called non-oxidative atmosphere, ventilating inert gas, such as boiling deaeration and nitrogen gas, and removing dissolved oxygen. The extract thus obtained is dried and concentrated to obtain the green tea extract used in the present invention. Examples of the green tea extract include liquid, slurry, semi-solid, and solid state. From the viewpoint of dispersibility in an organic solvent such as ethanol, a slurry, semi-solid, or solid state is preferable.
緑茶抽出物としては、超臨界状態の二酸化炭素接触処理を施した茶葉を用いて抽出した抽出物を用いてもよい。臨界抽出に用いる茶葉は、Ｃａｍｅｌｌｉａ属に属していればよく、生茶でも製茶された茶葉でもよい。当該製茶された茶葉としては不発酵茶が特に好ましい。例えば、蒸し製茶葉では普通煎茶、深蒸し煎茶、玉露、かぶせ茶、玉緑茶、番茶などが好ましい。また釜炒り製では玉緑茶や中国緑茶がある。製茶された茶葉は蒸し製茶葉或いは湯通し（ディッピング）の方が釜入りで発生する茶葉由来の新たな香味が発生するのを抑える意味で好ましい。この方法においては、超臨界抽出を施した残渣である茶葉から非重合体カテキン類を含有する抽出物を得るものである。従来、茶葉から超臨界抽出により香気成分を得ようとする技術は種々知られている（特開２００１−２９３０７６号公報、特開平１０−７７４９６号公報、特開平６−１３３７２６号公報、特開平６−１８４５９１号公報等）が、これらはいずれも茶葉の超臨界抽出物を利用する技術であって、超臨界抽出の残渣茶葉の利用及び当該残渣茶葉中の成分については何も記載されていない。 As the green tea extract, an extract extracted using tea leaves subjected to carbon dioxide contact treatment in a supercritical state may be used. The tea leaves used for critical extraction need only belong to the genus Camellia, and may be fresh tea or tea leaves. Non-fermented tea is particularly preferred as the tea leaves produced. For example, for steamed tea leaves, ordinary sencha, deep steamed sencha, gyokuro, kabusecha, tama green tea, bancha and the like are preferred. In addition, there are tama green tea and Chinese green tea for roasting kettle. For tea leaves that have been made, steamed tea leaves or boiled tea (dipping) is preferred in terms of suppressing the occurrence of a new flavor derived from tea leaves that occurs in a kettle. In this method, an extract containing non-polymer catechins is obtained from tea leaves, which are residues after supercritical extraction. Conventionally, various techniques for obtaining aroma components from tea leaves by supercritical extraction are known (Japanese Patent Laid-Open Nos. 2001-293076, 10-77496, 6-133726, and 6). No. 184591 and the like) are all techniques using a supercritical extract of tea leaves, and nothing is described about the use of supercritical extraction residual tea leaves and the components in the residual tea leaves.
本発明に使用する緑茶抽出物には、茶葉から抽出した抽出液を乾燥、濃縮して使用する代わりに、緑茶抽出物の濃縮物を水に溶解又は希釈して用いても、茶葉からの抽出液と緑茶抽出物の濃縮物とを併用してもよい。
ここで、緑茶抽出物の濃縮物とは、茶葉から熱水又は水溶性有機溶媒により抽出された抽出物を濃縮したものであり、例えば、特開昭５９−２１９３８４号公報、特開平４−２０５８９号公報、特開平５−２６０９０７号公報、特開平５−３０６２７９号公報等に記載されている方法により調製したものをいう。具体的には、緑茶抽出物として、市販の東京フードテクノ社製「ポリフェノン」、伊藤園社製「テアフラン」、太陽化学社製「サンフェノン」等の粗カテキン製剤を固体の緑茶抽出物として用いることもできる。
For the green tea extract used in the present invention, instead of drying and concentrating the extract extracted from tea leaves, the extract from tea leaves may be used by dissolving or diluting the concentrate of green tea extract in water. You may use together a liquid and the concentrate of a green tea extract.
Here, the concentrate of green tea extract is obtained by concentrating an extract extracted from tea leaves with hot water or a water-soluble organic solvent. For example, JP-A-59-219384 and JP-A-4-20589. No. 5, 260-907, JP-A-5-306279, and the like. Specifically, as a green tea extract, a commercially available crude catechin preparation such as “Polyphenone” manufactured by Tokyo Food Techno Co., “Theafuran” manufactured by ITO EN Co., Ltd., “Sunphenon” manufactured by Taiyo Kagaku Co., Ltd. may be used as a solid green tea extract. it can.
緑茶抽出物として、緑茶抽出物をタンナーゼ処理した抽出物を用いると苦みや渋みが顕著に低減された精製緑茶抽出物が得られることから、特に好ましい。ここで使用されるタンナーゼは、非重合体カテキン類を分解する活性を有するものであればよい。具体的には、アスペルギルス属、ペニシリウム属、リゾプス属などのタンナーゼ生産菌を培養して得られるタンナーゼが使用できる。このうち、アスペルギルス オリーゼ由来のものが特に好ましい。緑茶抽出液に粉末状又は溶液状のタンナーゼを、２５Unit/L〜５００Unit/L、好ましくは５０Unit/L〜１５０Unit/Lの濃度になるように添加する。かかるタンナーゼの添加量は、固形分１mgに換算すると、０．１Unit以上、好ましくは０．２Unit以上である。ここで１Unitは、３０℃の水中においてタンニン酸に含まれるエステル結合を１マイクロモル加水分解する酵素量で定義される。その後、５℃〜５０℃、望ましくは１０℃〜４０℃に１０〜７０質量％のガレート体率に達するまでの間保持する。 As the green tea extract, it is particularly preferable to use an extract obtained by tannase-treating the green tea extract because a purified green tea extract with significantly reduced bitterness and astringency can be obtained. The tannase used here may be any as long as it has an activity of decomposing non-polymer catechins. Specifically, tannase obtained by culturing tannase-producing bacteria such as Aspergillus, Penicillium, Rhizopus and the like can be used. Of these, those derived from Aspergillus oryzae are particularly preferred. Powdered or solution tannase is added to the green tea extract so as to have a concentration of 25 Unit / L to 500 Unit / L, preferably 50 Unit / L to 150 Unit / L. The amount of tannase added is 0.1 Unit or more, preferably 0.2 Unit or more when converted to a solid content of 1 mg. Here, 1 Unit is defined as the amount of enzyme that hydrolyzes 1 micromole of an ester bond contained in tannic acid in 30 ° C. water. Thereafter, it is held at 5 ° C. to 50 ° C., preferably 10 ° C. to 40 ° C. until reaching a gallate body ratio of 10 to 70% by mass.
その後、できるだけ速やかに４５℃〜９５℃、好ましくは７５℃〜９５℃まで昇温し、タンナーゼを失活させることにより反応を停止する。当該タンナーゼの失活処理により、その後のガレート体率の低下が防止でき、目的とするガレート体率の緑茶抽出物が得られる。 Thereafter, the temperature is raised to 45 ° C. to 95 ° C., preferably 75 ° C. to 95 ° C. as soon as possible, and the reaction is stopped by deactivating tannase. By the deactivation treatment of the tannase, the subsequent decrease in the gallate body ratio can be prevented, and a green tea extract having the desired gallate body ratio can be obtained.
本発明のタンナーゼ処理においては、得られる緑茶抽出物の非重合体カテキン類中のガレート体率は苦味低減及び外観の面から１０〜７０質量％、好ましくは３０〜６０質量％の範囲に制御される。すなわち、本発明で実施されるタンナーゼ処理は、従来の重合体カテキン類に含まれるすべてのガレート体を加水分解する処理方法とは異なり、タンナーゼ処理時のガレート体率を制御する。タンナーゼ処理によるガレート体率の制御は処理時の緑茶抽出液のpH挙動によって反応の終点を決定することが好ましい。当該pHは３〜６、特に３．５〜５．５が好ましい。これにより緑茶抽出液中のガレート体量を任意の範囲で維持するタンナーゼ処理した緑茶抽出物を得ることができる。また、タンナーゼ処理後のタンナーゼ失活処理により、その後のガレート体率の低下が防止できる。 In the tannase treatment of the present invention, the percentage of gallate body in the non-polymer catechins of the green tea extract obtained is controlled in the range of 10 to 70% by mass, preferably 30 to 60% by mass in terms of bitterness reduction and appearance. The That is, the tannase treatment carried out in the present invention controls the gallate body rate during tannase treatment, unlike the treatment method in which all gallate bodies contained in the conventional polymer catechins are hydrolyzed. The control of the gallate body rate by tannase treatment preferably determines the end point of the reaction based on the pH behavior of the green tea extract during the treatment. The pH is preferably 3 to 6, particularly 3.5 to 5.5. As a result, a tannase-treated green tea extract that maintains the amount of gallate body in the green tea extract in an arbitrary range can be obtained. Moreover, the fall of the gallate body rate after that can be prevented by the tannase deactivation process after a tannase process.
使用する緑茶抽出物は、乾燥質量で、非重合体カテキン類を２５〜９０質量％、更に３０〜９０質量％含有する緑茶抽出物の濃縮物を用いるのが好ましい。 The green tea extract to be used is preferably a green tea extract concentrate containing 25 to 90% by mass, and further 30 to 90% by mass of non-polymer catechins in dry mass.
本発明の精製緑茶抽出物は、前記の緑茶抽出物を有機溶媒と水の質量比が９１／９〜９７／３の混合溶液に分散させ、活性炭、酸性白土又は活性白土、及び合成吸着剤に接触処理する工程で製造される。 The purified green tea extract of the present invention is obtained by dispersing the above green tea extract in a mixed solution having an organic solvent and water mass ratio of 91/9 to 97/3 to obtain activated carbon, acidic clay or activated clay, and a synthetic adsorbent. Manufactured in the process of contact treatment.
使用する有機溶媒としては、エタノール、メタノール、アセトン、酢酸エチル等が挙げられる。これらのうち、メタノール、エタノール、アセトンの親水性有機溶媒が好ましく、特に食品への使用を考慮するとエタノールが好ましい。水としては、イオン交換水、水道水、天然水等が挙げられる。この有機溶媒と水は、混合して又はそれぞれ別々に緑茶抽出物と混合してもよいが、混合溶液としてから緑茶抽出物と混合するのが好ましい。 Examples of the organic solvent used include ethanol, methanol, acetone, and ethyl acetate. Of these, hydrophilic organic solvents such as methanol, ethanol and acetone are preferable, and ethanol is particularly preferable in consideration of use in foods. Examples of water include ion exchange water, tap water, and natural water. The organic solvent and water may be mixed or separately mixed with the green tea extract, but it is preferable to mix with the green tea extract after forming a mixed solution.
本発明においては、緑茶抽出物を有機溶媒と水の混合溶液に分散させる時の有機溶媒と水の質量比を９１／９〜９７／３、好ましくは９１／９〜９５／５、より好ましくは９２／８〜９５／５の範囲に調整する。有機溶媒の割合が９７／３を超えるとカテキン類の抽出効率が落ちてしまい、また９１／９未満では、緑茶抽出物の精製度合いが落ち好ましくない。 In the present invention, the mass ratio of the organic solvent to water when the green tea extract is dispersed in the mixed solution of the organic solvent and water is 91/9 to 97/3, preferably 91/9 to 95/5, more preferably Adjust to the range of 92/8 to 95/5. When the ratio of the organic solvent exceeds 97/3, the extraction efficiency of catechins decreases, and when it is less than 91/9, the degree of purification of the green tea extract decreases, which is not preferable.
本発明においては、緑茶抽出物を有機溶媒と水の混合溶液に分散する方法は特に制限されず、最終的に処理する際の有機溶媒と水の質量比が９１／９〜９７／３の範囲になっていればよい。例えば、緑茶抽出物を水に溶解した後に有機溶媒を添加していくことによって有機溶媒と水の質量比を９１／９〜９７／３の範囲にしてもよく、緑茶抽出物を有機溶媒に懸濁させた後、徐々に水を添加して同様の比率としても良い。抽出効率の点から、水に溶解後に有機溶媒を添加していく方法が好ましい。また緑茶抽出物は１回で全量添加しても良いが、２回以上、例えば２〜４回に分割して添加しても良い。 In the present invention, the method for dispersing the green tea extract in a mixed solution of an organic solvent and water is not particularly limited, and the mass ratio of the organic solvent to water in the final treatment is in the range of 91/9 to 97/3. It only has to be. For example, the organic solvent may be added after dissolving the green tea extract in water so that the mass ratio of the organic solvent to water is in the range of 91/9 to 97/3. After turbidity, water may be gradually added to obtain the same ratio. From the viewpoint of extraction efficiency, a method of adding an organic solvent after dissolving in water is preferable. The green tea extract may be added all at once, but may be added twice or more, for example, divided into 2 to 4 times.
本発明においては、有機溶媒と水の混合溶液１００質量部に対して、乾燥質量換算の緑茶抽出物を１０〜４０質量部、特に１０〜３０質量部添加して処理するのが、緑茶抽出物を効率よく処理できるので好ましい。 In the present invention, 10 to 40 parts by weight, particularly 10 to 30 parts by weight of green tea extract in terms of dry weight is added to 100 parts by weight of a mixed solution of an organic solvent and water, and the green tea extract is processed. Can be processed efficiently.
水と有機溶媒の混合溶液又はそれぞれの添加時間は、１０〜３０分程度の時間でゆっくり滴下するのが好ましい。また、カテキン類の抽出効率を上げるために攪拌状態で滴下するのが好ましい。水の滴下終了後は１０〜１２０分程度の熟成時間を設けると更に好ましい。
これらの処理は、１０〜６０℃で行うことができ、特に１０〜５０℃、更に１０〜４０℃で行うのが好ましい。
It is preferable that the mixed solution of water and the organic solvent or each addition time is slowly dropped in a time of about 10 to 30 minutes. Moreover, in order to raise the extraction efficiency of catechins, it is preferable to add dropwise with stirring. It is more preferable to provide an aging time of about 10 to 120 minutes after the completion of the dropwise addition of water.
These treatments can be carried out at 10 to 60 ° C., preferably 10 to 50 ° C., more preferably 10 to 40 ° C.
用いる活性炭としては、一般に工業レベルで使用されているものであれば特に制限されず、例えば、ＺＮ−５０（北越炭素社製）、クラレコールＧＬＣ、クラレコールＰＫ−Ｄ、クラレコールＰＷ−Ｄ（クラレケミカル社製）、白鷲ＡＷ５０、白鷲Ａ、白鷲Ｍ、白鷲Ｃ（武田薬品工業社製）等の市販品を用いることができる。
活性炭の細孔容積は０．０１〜１．１ｍＬ／ｇ、特に０．１〜０．８ｍＬ／ｇが好ましい。また、比表面積は８００〜２０００ｍ2／ｇ、特に９００〜１６００ｍ2／ｇの範囲のものが好ましい。なお、これらの物性値は窒素吸着法に基づく値である。
The activated carbon to be used is not particularly limited as long as it is generally used at an industrial level. For example, ZN-50 (made by Hokuetsu Carbon Co., Ltd.), Kuraray Coal GLC, Kuraray Coal PK-D, Kuraray Coal PW-D ( Commercial products such as Kuraray Chemical Co., Ltd.), white birch AW50, white birch A, white birch M, white birch C (manufactured by Takeda Pharmaceutical Co., Ltd.) can be used.
The pore volume of the activated carbon is preferably 0.01 to 1.1 mL / g, particularly preferably 0.1 to 0.8 mL / g. The specific surface area is 800~2000m 2 / g, particularly preferably in the range of 900~1600m 2 / g. These physical property values are values based on the nitrogen adsorption method.
活性炭は、有機溶媒と水の混合溶液１００質量部に対して０．５〜５質量部、特に０．５〜３質量部添加するのが好ましい。活性炭の添加量が少なすぎると、カフェイン除去効率が悪くなり、また多すぎるとろ過工程におけるケーク抵抗が大きくなり好ましくない。 The activated carbon is preferably added in an amount of 0.5 to 5 parts by mass, particularly 0.5 to 3 parts by mass with respect to 100 parts by mass of a mixed solution of an organic solvent and water. If the amount of activated carbon added is too small, the caffeine removal efficiency will deteriorate, and if it is too large, the cake resistance in the filtration step will increase, which is not preferable.
用いる酸性白土又は活性白土は、ともに一般的な化学成分として、ＳｉＯ2、Ａｌ2Ｏ3、Ｆｅ2Ｏ3、ＣａＯ、ＭｇＯ等を含有するものであるが、ＳｉＯ2／Ａｌ2Ｏ3比が３〜１２、特に４〜９であるのが好ましい。またＦｅ2Ｏ3を２〜５質量％、ＣａＯを０〜１．５質量％、ＭｇＯを１〜７質量％含有する組成のものが好ましい。
活性白土は天然に産出する酸性白土（モンモリロナイト系粘土）を硫酸等の鉱酸で処理したものであり、大きい比表面積と吸着能を有する多孔質構造をもった化合物である。酸性白土を更に、酸処理することにより比表面積が変化し、脱色能の改良及び物性が変化することが知られている。
The acid clay or the activated clay to be used contains SiO 2 , Al 2 O 3 , Fe 2 O 3 , CaO, MgO, etc. as general chemical components, but the SiO 2 / Al 2 O 3 ratio is It is preferably 3 to 12, particularly 4 to 9. The Fe 2 O 3 2 to 5 wt%, the CaO 0 to 1.5 wt%, preferably from compositions containing MgO 1 to 7% by weight.
Activated clay is a naturally occurring acidic clay (montmorillonite clay) treated with a mineral acid such as sulfuric acid, and is a compound having a porous structure having a large specific surface area and adsorption capacity. It is known that when acid clay is further acid-treated, the specific surface area is changed to improve the decolorization ability and change physical properties.
酸性白土又は活性白土の比表面積は、酸処理の程度等により異なるが、５０〜３５０ｍ2／ｇであるのが好ましく、ｐＨ（５質量％サスペンジョン）は２．５〜８、特に３．６〜７のものが好ましい。例えば、酸性白土としては、ミズカエース＃６００（水澤化学社製）等の市販品を用いることができる。 The specific surface area of the acid clay or activated clay varies depending on the degree of acid treatment, etc., but is preferably 50 to 350 m 2 / g, and the pH (5 mass% suspension) is 2.5 to 8, particularly 3.6 to 7 is preferred. For example, as the acid clay, a commercially available product such as Mizuka Ace # 600 (manufactured by Mizusawa Chemical Co., Ltd.) can be used.
酸性白土又は活性白土は、有機溶媒と水の混合溶液１００質量部に対して２．５〜２５質量部、特に２．５〜１５質量部添加するのが好ましい。酸性白土又は活性白土の添加量が少なすぎると、カフェイン除去効率が悪くなり、また多すぎるとろ過工程におけるケーク抵抗が大きくなり好ましくない。 The acid clay or the activated clay is preferably added in an amount of 2.5 to 25 parts by mass, particularly 2.5 to 15 parts by mass with respect to 100 parts by mass of a mixed solution of an organic solvent and water. If the amount of acid clay or activated clay added is too small, the caffeine removal efficiency will deteriorate, and if too much, the cake resistance in the filtration step will increase, which is not preferable.
また、活性炭と酸性白土又は活性白土を併用する場合の割合は、質量比で活性炭１に対して１〜１０がよく、特に活性炭：酸性白土又は活性白土＝１：１〜１：６であるのが好ましい。 Moreover, the ratio in the case of using activated carbon and acidic clay or activated clay in combination is preferably 1 to 10 with respect to the activated carbon 1 by mass ratio, particularly activated carbon: acid clay or activated clay = 1: 1 to 1: 6. Is preferred.
合成吸着剤は、一般に不溶性の三次元架橋構造ポリマーでイオン交換基のような官能基を実質的に持たないものである。好ましくは、イオン交換基が１ｍｅｑ／ｇ未満のものを用いることができる。
使用する合成吸着剤としては、その母体がスチレン系、例えばアンバーライトＸＡＤ４、ＸＡＤ１６ＨＰ（ロームアンドハース社製）；ダイヤイオンＨＰ２０、ＨＰ２１（三菱化学社製）；セパビーズＳＰ８５０、ＳＰ７０（三菱化学社製）；ＶＰＯＣ１０６２（Ｂａｙｅｒ社製）、メタクリル系、例えばダイヤイオンＨＰ２ＭＧ（三菱化学社製）、フェノール系、例えばアンバーライトＸＡＤ７６１（ロームアンドハース社製）、アクリル系、例えばアンバーライトＸＡＤ７ＨＰ（ロームアンドハース社製）、ポリビニル系、例えばＴＯＹＯＰＥＡＲＬ、ＨＷ-４０Ｃ（東ソー社製）、デキストラン系、例えばＳＥＰＨＡＤＥＸ、ＬＨ-20（ファルマシア社製）等が使用できる。
合成吸着剤としては、その母体がスチレン系、メタクリル系、アクリル系、フェノール系、ポリビニール系が好ましく、更にスチレン系、メタクリル系、フェノール系が好ましく、特にスチレン系が好ましい。スチレン系の中では、ダイヤイオンＨＰ２０、セパビーズＳＰ８２５、ＳＰ８５０が好ましい。
Synthetic adsorbents are generally insoluble three-dimensional crosslinked structure polymers that are substantially free of functional groups such as ion exchange groups. Preferably, those having an ion exchange group of less than 1 meq / g can be used.
As the synthetic adsorbent used, the matrix is styrene, for example, Amberlite XAD4, XAD16HP (Rohm and Haas); Diaion HP20, HP21 (Mitsubishi Chemical); Sepabeads SP850, SP70 (Mitsubishi Chemical) VPOC1062 (manufactured by Bayer), methacrylic, such as Diaion HP2MG (manufactured by Mitsubishi Chemical), phenolic, such as Amberlite XAD761 (manufactured by Rohm and Haas), acrylic, such as Amberlite XAD7HP (manufactured by Rohm and Haas) ), Polyvinyl, such as TOYOPEARL, HW-40C (manufactured by Tosoh Corporation), dextran, such as SEPHADEX, LH-20 (manufactured by Pharmacia), etc. can be used.
As the synthetic adsorbent, the matrix is preferably styrene, methacrylic, acrylic, phenolic, or polyvinyl, more preferably styrene, methacrylic, or phenolic, and particularly preferably styrene. Among styrene-based materials, Diaion HP20 and Sepabeads SP825 and SP850 are preferable.
合成吸着剤は、有機溶媒と水の混合溶液１００質量部に対して５〜１００質量部、特に１０〜５０質量部添加するのが好ましい。合成吸着剤の添加量が少なすぎると、澱を発生させる成分の除去効率が悪くなり、また多すぎると液歩留りの点から好ましくない。 The synthetic adsorbent is preferably added in an amount of 5 to 100 parts by weight, particularly 10 to 50 parts by weight, based on 100 parts by weight of a mixed solution of an organic solvent and water. If the amount of the synthetic adsorbent added is too small, the removal efficiency of the components that generate starch deteriorates, and if it is too large, it is not preferable from the viewpoint of liquid yield.
本発明の精製緑茶抽出物の製造における、緑茶抽出物、有機溶媒と水の混合溶液並びに活性炭、酸性白土又は活性白土、及び合成吸着剤との接触順序は特に限定されない。例えば（１）有機溶媒と水の混合溶液に緑茶抽出物を添加し、活性炭接触、次いで酸性白土又は活性白土接触、次いで合成吸着剤接触する方法、（２）有機溶媒と水の混合溶液に緑茶抽出物を添加し、合成吸着剤接触、次いで酸性白土又は活性白土接触、次いで活性炭接触する方法、（３）有機溶媒と水との混合溶液に活性炭を添加し、これに緑茶抽出物を添加し、次いで合成吸着剤接触、次いで酸性白土又は活性白土接触する方法、（４）有機溶媒と水の混合溶液に酸性白土又は活性白土を添加し、これに緑茶抽出物を添加し、次いで合成吸着剤接触、次いで活性炭接触する方法等が挙げられるが、（５）有機溶媒と水の混合溶液に酸性白土又は活性白土を添加し、これに緑茶抽出物を添加し、次いで活性炭接触、次いで合成吸着剤接触する方法が好ましい。
これらの各成分添加と次の成分添加との間にはろ過を行うのが好ましい。また緑茶抽出物を２回以上に分割して添加した場合、その間にろ過を行ってもよい。
In the production of the purified green tea extract of the present invention, the order of contact with the green tea extract, a mixed solution of an organic solvent and water, activated carbon, acidic clay or activated clay, and a synthetic adsorbent is not particularly limited. For example, (1) A method in which green tea extract is added to a mixed solution of an organic solvent and water, and activated carbon is contacted with acid clay or activated clay, and then a synthetic adsorbent is contacted. (2) Green tea is mixed with a mixed solution of an organic solvent and water. Add the extract, contact with the synthetic adsorbent, then contact with the acid clay or activated clay, then contact with activated carbon, (3) Add the activated carbon to the mixed solution of organic solvent and water, add the green tea extract to this , Then contact with a synthetic adsorbent, then contact with an acidic clay or activated clay, (4) Add acidic clay or activated clay to a mixed solution of an organic solvent and water, add green tea extract to this, and then add a synthetic adsorbent (5) Add acid clay or activated clay to the mixed solution of organic solvent and water, add green tea extract to this, then contact with activated carbon, then synthetic adsorbent Touch Methods are preferred.
Filtration is preferably performed between the addition of each of these components and the addition of the next component. Moreover, when adding a green tea extract divided into 2 or more times, you may filter in the meantime.
更に、本発明において、緑茶抽出物を酸性白土又は活性白土と有機溶媒と水の混合溶液との分散液と接触混合する場合、接触するときのｐＨを４〜６の範囲に調整して行うことが、非重合体カテキン類を効率よく抽出した精製緑茶抽出物を得るために好ましい。接触の際、クエン酸、乳酸、酒石酸、コハク酸、リンゴ酸等の有機酸を、有機酸と非重合体カテキン類の質量比率（有機酸／非重合体カテキン類）が０．０２〜０．２０の範囲で添加するのが好ましい。 Furthermore, in the present invention, when the green tea extract is contact-mixed with a dispersion of acidic clay or activated clay, a mixed solution of an organic solvent and water, the pH at the time of contact is adjusted to a range of 4-6. Is preferable for obtaining a purified green tea extract in which non-polymer catechins are efficiently extracted. In the contact, an organic acid such as citric acid, lactic acid, tartaric acid, succinic acid, malic acid, or the like, and the mass ratio of the organic acid to the non-polymer catechins (organic acid / non-polymer catechins) is 0.02 to 0.00. It is preferable to add in the range of 20.
また、本発明において、緑茶抽出物を酸性白土又は活性白土と有機溶媒と水の混合溶液との分散液と接触混合する場合、接触するときの液の温度は始めに１０〜３０℃とし、その後２０〜６０℃に昇温すると、緑茶抽出物の溶解が促進されるという点及び分散液へのカテキン抽出効率が促進されるという点で好ましい。 In the present invention, when the green tea extract is contact mixed with a dispersion of a mixed solution of acidic clay or activated clay, an organic solvent and water, the temperature of the liquid at the time of contact is initially 10 to 30 ° C., and then It is preferable to raise the temperature to 20 to 60 ° C. in that the dissolution of the green tea extract is promoted and the efficiency of catechin extraction into the dispersion is promoted.
緑茶抽出物と活性炭、酸性白土又は活性白土、及び合成吸着剤との接触処理は、バッチ式、カラムによる連続処理等のいずれの方法で行ってもよい。また、緑茶抽出物と活性炭との接触方法は、活性炭カラムによる連続処理等の方法で行うのがよい。 The contact treatment between the green tea extract and the activated carbon, the acid clay or the activated clay, and the synthetic adsorbent may be performed by any method such as a batch method or a continuous treatment using a column. Moreover, the contact method between the green tea extract and the activated carbon is preferably performed by a method such as continuous treatment using an activated carbon column.
一般には、粉末状の活性炭等を添加、撹拌し、カフェインを選択的に吸着後、ろ過操作によりカフェインを除去したろ液を得る方法又は顆粒状の活性炭等を充填したカラムを用いて連続処理によりカフェインを選択的に吸着する方法等が採用される。また緑茶抽出物と合成吸着剤の接触方法も同様に、カラムによる連続処理等の方法で行うのがよい。合成吸着剤は、再生利用しても良い。 In general, powdered activated carbon or the like is added, stirred, and after selectively adsorbing caffeine, continuously by using a method of obtaining a filtrate from which caffeine has been removed by filtration or using a column filled with granular activated carbon or the like. A method of selectively adsorbing caffeine by treatment is employed. Similarly, the contact method between the green tea extract and the synthetic adsorbent is preferably performed by a method such as continuous treatment using a column. The synthetic adsorbent may be recycled.
合成吸着剤には、非重合体カテキン類は吸着されず、容器詰飲料調製時に澱を発生させる成分が吸着するものと考えられる。従って、合成吸着剤処理により吸着しなかった溶液を回収すればよい。 It is considered that the non-polymer catechins are not adsorbed on the synthetic adsorbent, and that the components that generate starch are adsorbed during preparation of the packaged beverage. Therefore, the solution that has not been adsorbed by the synthetic adsorbent treatment may be recovered.
本発明によって得られる精製緑茶抽出物は、その固形分中に、非重合体カテキン類を２５〜９０質量％含有するが、４０〜９０質量％、更に５０〜９０質量％、特に６０〜９０質量％含有する水溶液とするのが好ましい。従って、得られた溶液から有機溶媒を除去するのが好ましい。除去手段としては、減圧蒸留などの方法を用いて留去される。 The purified green tea extract obtained by the present invention contains 25 to 90% by mass of non-polymer catechins in its solid content, but is 40 to 90% by mass, more preferably 50 to 90% by mass, particularly 60 to 90% by mass. % Aqueous solution is preferable. Therefore, it is preferable to remove the organic solvent from the obtained solution. As a removing means, it is distilled off using a method such as vacuum distillation.
本発明により製造された精製緑茶抽出物は、含有する非重合体カテキン類の組成が処理前と本質的に変化していないのが好ましい。処理前後の有機溶媒と水の混合溶液中の非重合体カテキン類の収率は６０質量％以上、更に６５質量％以上、更に７０質量％以上、特に８０質量％以上が好ましい。 In the purified green tea extract produced according to the present invention, the composition of the non-polymer catechins contained is preferably essentially unchanged from that before the treatment. The yield of non-polymer catechins in the mixed solution of the organic solvent and water before and after the treatment is preferably 60% by mass or more, more preferably 65% by mass or more, further 70% by mass or more, and particularly preferably 80% by mass or more.
また、本発明により得られる精製緑茶抽出物中のカテキンガレート、エピカテキンガレート、ガロカテキンガレート及びエピガロカテキンガレートからなるガレート体の全非重合体カテキン類中での割合は、１０〜７０質量％、特に３０〜６０質量％であるのが、非重合体カテキン類の生理効果の有効性及び苦味低減の点で好ましい。 In the purified green tea extract obtained by the present invention, the proportion of gallate bodies composed of catechin gallate, epicatechin gallate, gallocatechin gallate and epigallocatechin gallate in all non-polymer catechins is 10 to 70% by mass. In particular, 30 to 60% by mass is preferable from the viewpoint of the effectiveness of physiological effects of non-polymer catechins and the reduction of bitterness.
本発明で得られる精製緑茶抽出物中のカフェイン濃度は、非重合体カテキン類に対して、非重合体カテキン類／カフェイン（質量比）＝２５〜２００、更に３０〜１５０、特に３０〜１００であるのが好ましい。 The concentration of caffeine in the purified green tea extract obtained in the present invention is non-polymer catechins / caffeine (mass ratio) = 25 to 200, more preferably 30 to 150, and particularly 30 to the non-polymer catechins. 100 is preferred.
得られた精製緑茶抽出物は、カフェイン濃度が低く、濁り成分が低減されているにもかかわらず、高い非重合体カテキン類濃度を維持しており、かつ色相がよく、更に緑茶の風味がほとんどない。従って、得られた濁り成分の低減された精製緑茶抽出物は容器詰飲料として有用であり、特に緑茶、烏龍茶、ブレンド茶、紅茶、麦茶等の茶系飲料、スポーツ飲料、アイソトニック飲料、ニアウォーター等の非茶系飲料として有用である。 The obtained purified green tea extract maintains a high concentration of non-polymer catechins in spite of low caffeine concentration and reduced turbidity components, has a good hue, and has a green tea flavor. rare. Therefore, the obtained purified green tea extract with reduced turbidity component is useful as a packaged beverage, especially tea beverages such as green tea, oolong tea, blended tea, black tea, barley tea, sports beverage, isotonic beverage, near water, etc. It is useful as a non-tea beverage.
本発明の容器詰飲料中には、水に溶解状態にある非重合体カテキン類を、０．０３〜１．０質量％含有するが、好ましくは０．０４〜０．５質量％、より好ましくは０．０６〜０．４質量％、更に好ましくは０．０７〜０．４質量％、特に好ましくは０．０８〜０．３質量％、殊更好ましくは０．０９〜０．３質量％、もっとも好ましくは０．１〜０．３質量％含有する。非重合体カテキン類含量がこの範囲にあると、多量の非重合カテキン類を容易に取り易く、飲料調製直後の色調の点からも好ましい。当該非重合体カテキン類の濃度は、濁り成分の低減された緑茶抽出物の精製物の配合量によって調整することができる。
また、蓄積体脂肪燃焼促進、食事性脂肪燃焼促進及び肝臓β酸化遺伝子発現促進の効果を出すための成人一日当りの摂取量としては、非重合体カテキン類として３００ｍｇ以上、更に４５０ｍｇ以上、更に５００ｍｇ以上が好ましい。また具体的には一本あたり非重合体カテキン類を４８３ｍｇ、５５５ｍｇ及び９００ｍｇを含有する飲料の摂取によって抗肥満効果や内臓脂肪低減効果が確認されている（特開２００２−３２６９３２号公報）。
したがって本発明の容器詰飲料においても成人一日当りの摂取量としては、非重合体カテキン類として３００ｍｇ以上、更に４５０ｍｇ以上、更に５００ｍｇ以上が好ましく、一日当りの必要摂取量を確保する意味からも、本発明の容器詰飲料１本当り３００ｍｇ以上、更に４５０ｍｇ以上、更に５００ｍｇ以上の配合量があるものが好ましい。
The container-packed beverage of the present invention contains 0.03 to 1.0% by mass of non-polymer catechins dissolved in water, preferably 0.04 to 0.5% by mass, more preferably Is 0.06 to 0.4% by mass, more preferably 0.07 to 0.4% by mass, particularly preferably 0.08 to 0.3% by mass, even more preferably 0.09 to 0.3% by mass, Most preferably, the content is 0.1 to 0.3% by mass. When the content of non-polymer catechins is within this range, a large amount of non-polymer catechins can be easily taken, which is preferable from the viewpoint of the color tone immediately after preparation of the beverage. The density | concentration of the said non-polymer catechin can be adjusted with the compounding quantity of the refined | purified substance of the green tea extract in which the cloudiness component was reduced.
In addition, the daily intake for adults for promoting the effects of accumulation fat burning promotion, dietary fat burning promotion and liver β-oxidation gene expression promotion is 300 mg or more, further 450 mg or more, and further 500 mg as non-polymer catechins. The above is preferable. Specifically, anti-obesity effects and visceral fat reduction effects have been confirmed by ingesting beverages containing 483 mg, 555 mg, and 900 mg of non-polymer catechins per bottle (JP 2002-326932 A).
Therefore, in the packaged beverage of the present invention, the daily intake for adults is preferably 300 mg or more, more preferably 450 mg or more, and more preferably 500 mg or more as non-polymer catechins, from the viewpoint of securing the necessary intake per day, Those having a blending amount of 300 mg or more, further 450 mg or more, and further 500 mg or more per containerized beverage of the present invention are preferred.
本発明の容器詰飲料には、ナトリウムイオン及び／又はカリウムイオンを含有させてもよい。これらのイオンを含有させた本発明飲料は、スポーツドリンク、アイソトニック飲料等の飲料形態として有用である。スポーツドリンクとは、身体運動後に汗として失われる水分、ミネラルを速やかに補給できる飲料であると一般的に規定される。 The packaged beverage of the present invention may contain sodium ions and / or potassium ions. The beverage of the present invention containing these ions is useful as a beverage form such as a sports drink or an isotonic beverage. A sports drink is generally defined as a drink that can quickly replenish water and minerals lost as sweat after physical exercise.
主な生理電解質の中にはナトリウム及びカリウムがある。これらのイオン成分はそれらに対応する水溶性成分ないし、無機塩を添加することで含有させることができる。それらは果汁及び茶抽出物中にも存在する。本発明飲料中における電解質又はイオン成分の量は最終の飲用しうる容器詰飲料中の含有量である。電解質濃度はイオン濃度で示される。カリウムイオン成分は、カリウム塩化物、炭酸カリウム、硫酸カリウム、酢酸カリウム、炭酸水素カリウム、クエン酸カリウム、リン酸カリウム、リン酸水素カリウム、酒石酸カリウム、ソルビン酸カリウム等又はそれらの混合物のような塩として、あるいは加えられた果汁又は茶の成分として本発明飲料に配合できる。カリウムイオンは、０．００１〜０．２質量％、更に０．００２〜０．１５質量％、更に０．００３〜０．１２質量％本発明の容器詰飲料中に含有することが好ましい。同様に、ナトリウムイオン成分は、ナトリウム塩化物、炭酸ナトリウム、炭酸水素ナトリウム、クエン酸ナトリウム、リン酸ナトリウム、リン酸水素ナトリウム、酒石酸ナトリウム、安息香酸ナトリウム等及びそれらの混合物のような容易に入手しうるナトリウム塩として、あるいは加えられた果汁又は茶の成分として配合できる。ナトリウム濃度は浸透圧による水の吸収を容易にさせる上で低い方望ましいが、体から腸に水を浸透圧吸引しない程度であることが、好ましい。これを行うために必要なナトリウムの濃度は、血漿ナトリウムの場合よりも低いことが好ましい。ナトリウムイオンは、０．００１〜０．５質量％、更に０．００２〜０．４質量％、更に０．００３〜０．２質量％本発明の容器詰飲料中に含有するのが好ましい。カリウム及びナトリウムイオンに加えて、本発明容器詰飲料には０．００１〜０．５質量％、好ましくは０．００２〜０．４質量％、最も好ましくは０．００３〜０．３質量％の塩化物イオンを更に含有させることができる。塩化物イオン成分は塩化ナトリウム又は塩化カリウムのような塩の形態で配合できる。カルシウム及びマグネシウム、亜鉛、鉄のような他の微量イオンも配合してよい。これらのイオンも塩として配合してよい。飲料中に存在するイオンの合計量には、添加されたイオン量と共に、飲料中に天然で存在するイオン量を含む。例えば、塩化ナトリウムが添加された場合、その量のナトリウムイオン及びその量の塩化物イオンも、それに応じて各イオンの合計量に含まれる。
ここで、ナトリウムイオンやカリウムイオン濃度が低すぎると、飲む場面によっては味的に物足りなく感じ、効果的なミネラル補給ができなくて好ましくない。一方、多すぎると、塩類自体の味が強くなり長期間の飲用に好ましくない。
Among the main physiological electrolytes are sodium and potassium. These ionic components can be contained by adding water-soluble components or inorganic salts corresponding thereto. They are also present in fruit juices and tea extracts. The amount of the electrolyte or ionic component in the beverage of the present invention is the content in the final drinkable container-packed beverage. The electrolyte concentration is indicated by the ion concentration. The potassium ion component is a salt such as potassium chloride, potassium carbonate, potassium sulfate, potassium acetate, potassium hydrogen carbonate, potassium citrate, potassium phosphate, potassium hydrogen phosphate, potassium tartrate, potassium sorbate, etc. or a mixture thereof. Or as a component of added fruit juice or tea. It is preferable to contain a potassium ion in the container-packed drink of this invention 0.001-0.2 mass%, 0.002-0.15 mass%, furthermore 0.003-0.12 mass%. Similarly, the sodium ion component is readily available such as sodium chloride, sodium carbonate, sodium bicarbonate, sodium citrate, sodium phosphate, sodium hydrogen phosphate, sodium tartrate, sodium benzoate and the like and mixtures thereof. It can be formulated as a hydrated sodium salt or as a component of added fruit juice or tea. The sodium concentration is preferably lower in order to facilitate the absorption of water by osmotic pressure, but it is preferable that the sodium concentration is not osmotically sucked from the body into the intestine. The concentration of sodium required to do this is preferably lower than that of plasma sodium. Sodium ions are preferably contained in the packaged beverage of the present invention in an amount of 0.001 to 0.5% by mass, further 0.002 to 0.4% by mass, and further 0.003 to 0.2% by mass. In addition to potassium and sodium ions, the packaged beverage of the present invention has 0.001 to 0.5% by weight, preferably 0.002 to 0.4% by weight, most preferably 0.003 to 0.3% by weight. Chloride ions can be further included. The chloride ion component can be formulated in the form of a salt such as sodium chloride or potassium chloride. Other trace ions such as calcium and magnesium, zinc, iron may also be included. These ions may also be blended as salts. The total amount of ions present in the beverage includes the amount of ions naturally present in the beverage as well as the amount of ions added. For example, when sodium chloride is added, that amount of sodium ions and that amount of chloride ions are accordingly included in the total amount of each ion.
Here, if the sodium ion or potassium ion concentration is too low, it may be unsatisfactory in taste depending on the scene of drinking, and effective mineral supplementation cannot be achieved. On the other hand, if too much, the taste of the salt itself becomes strong, which is not preferable for long-term drinking.
本発明の容器詰飲料には、味を改善する目的で、甘味料が用いられる。甘味料としては人工甘味料類、炭水化物類、グリセロール類（例えばグリセリン）が用いられる。これらの甘味料は、本発明容器詰飲料中に０．０００１〜２０質量％、更に０．００１〜１５質量％、最も好ましくは０．００１〜１０質量％含有する。前記下限未満であると、甘みがほとんどなく、酸味、塩味とのバランスがとれない。一方上限を超えると、甘すぎて喉にひっかかる感覚が強く、喉越しが低下する。
本発明の容器詰飲料における甘味料としては、人工甘味料を使用することが好ましい。本発明で使用できる人工甘味料の例にはサッカリン及びサッカリンナトリウム、アスパルテーム、アセサルフェーム−Ｋ、スクラロース、ネオテームなどの高甘度甘味料、ソルビトール、エリスリトール、キシリトールなどの糖アルコールを使用できる。商品としては、アスパルテームからなるスリムアップシュガー、エリスリトールを含んだラカントＳ，エリスリトールとアスパルテームからなるパルスイートなどを使用できる。
A sweetener is used for the container-packed drink of this invention in order to improve a taste. As the sweetener, artificial sweeteners, carbohydrates, and glycerol (for example, glycerin) are used. These sweeteners are contained in the container-packed beverage of the present invention in an amount of 0.0001 to 20% by mass, further 0.001 to 15% by mass, and most preferably 0.001 to 10% by mass. If it is less than the lower limit, there is almost no sweetness, and sourness and saltiness cannot be balanced. On the other hand, if the upper limit is exceeded, the sensation of being too sweet and caught in the throat is strong, and the over-throat is lowered.
As the sweetener in the packaged beverage of the present invention, an artificial sweetener is preferably used. Examples of artificial sweeteners that can be used in the present invention include saccharin and saccharin sodium, aspartame, acesulfame-K, sucralose, neotame and other high-sweetness sweeteners, and sugar alcohols such as sorbitol, erythritol, and xylitol. As products, slim-up sugar made of aspartame, lacanto S containing erythritol, pal sweet made of erythritol and aspartame can be used.
目的とする容器詰飲料がエネルギー補給を兼ね備える場合には、炭水化物類の甘味料を使用する方が好ましい。
本発明で使用できる炭水化物類甘味料としては可溶性炭水化物が用いられる。可溶性炭水化物には、甘味料とエネルギー源との役割がある。本発明飲料に使用する炭水化物を選択するにあたっては、十分な胃排出及び腸吸収速度を考慮することが好ましい。
When the target packaged drink also has energy supplement, it is preferable to use a sweetener of carbohydrates.
Soluble carbohydrates are used as carbohydrate sweeteners that can be used in the present invention. Soluble carbohydrates serve as sweeteners and energy sources. In selecting the carbohydrate to be used in the beverage of the present invention, it is preferable to consider sufficient gastric emptying and intestinal absorption rate.
炭水化物はグルコース及びフルクトースの混合物でも、あるいは消化管で加水分解するか又はグルコース及びフルクトースを形成する炭水化物であってもよい。本明細書で用いられる「炭水化物」という用語は、単糖、ニ糖、オリゴ糖、複合多糖及びそれらの混合物を含む。 The carbohydrate may be a mixture of glucose and fructose, or a carbohydrate that hydrolyzes in the digestive tract or forms glucose and fructose. The term “carbohydrate” as used herein includes monosaccharides, disaccharides, oligosaccharides, complex polysaccharides and mixtures thereof.
ここで使用できる単糖にはテトロース、ペントース、ヘキソース及びケトヘキソースがある。ヘキソースの例は、ブドウ糖として知られるグルコースのようなアルドヘキソースである。本発明容器詰飲料中のグルコースの量は、０．０００１〜２０質量％、更に０．００１〜１５質量％、更に０．００１〜１０質量％であるのが好ましい。果糖として知られるフルクトースはケトヘキソースである。本発明容器詰飲料中のフルクトースの量は０．０００１〜２０質量％、更に０．００１〜１５質量％、特に０．００１〜１０質量％であるのが好ましい。
本発明飲料中においては、人工甘味料単独系、人工甘味料とグルコース系化合物、もしくは人工甘味料とフルクトース系化合物の組み合わせが好ましい。
Monosaccharides that can be used here include tetrose, pentose, hexose and ketohexose. An example of a hexose is an aldohexose such as glucose known as glucose. The amount of glucose in the container-packed beverage of the present invention is preferably 0.0001 to 20% by mass, more preferably 0.001 to 15% by mass, and further preferably 0.001 to 10% by mass. Fructose, known as fructose, is a ketohexose. The amount of fructose in the container-packed beverage of the present invention is preferably 0.0001 to 20% by mass, more preferably 0.001 to 15% by mass, and particularly preferably 0.001 to 10% by mass.
In the beverage of the present invention, an artificial sweetener alone system, an artificial sweetener and a glucose compound, or a combination of an artificial sweetener and a fructose compound is preferable.
本発明で使用できる炭水化物類甘味料としては可溶性炭水化物が用いられるが、オリゴ糖としては、これら２種の単糖を体内で生成する炭水化物（即ち、スクロース、マルトデキストリン、コーンシロップ、高フルクトースコーンシロップ）が挙げられる。この糖の重要なタイプは二糖である。二糖の例は、ショ糖又はテンサイ糖として知られるスクロースである。本発明容器詰飲料中のスクロースの量は、０．００１〜２０質量％、更に０．００１〜１５質量％、特に０．００１〜１０質量％であるのが好ましい。 Soluble carbohydrates are used as carbohydrate sweeteners that can be used in the present invention. As oligosaccharides, carbohydrates that produce these two monosaccharides in the body (ie, sucrose, maltodextrin, corn syrup, high fructose corn syrup) ). An important type of this sugar is the disaccharide. An example of a disaccharide is sucrose known as sucrose or sugar beet sugar. The amount of sucrose in the container-packed beverage of the present invention is preferably 0.001 to 20% by mass, more preferably 0.001 to 15% by mass, and particularly preferably 0.001 to 10% by mass.
本発明の容器詰飲料のｐＨは２〜６、好ましくは２〜５、より好ましくは３〜４．５がカテキンの安定性上良い。ｐＨが低すぎると飲料の酸味、刺激臭が強くなる。また、ｐＨが高すぎると風味の調和が取れなくなり、嗜好性が低下するので好ましくない。 The pH of the packaged beverage of the present invention is 2 to 6, preferably 2 to 5, and more preferably 3 to 4.5 in terms of catechin stability. If the pH is too low, the sourness and pungent odor of the beverage will become strong. On the other hand, if the pH is too high, the flavor cannot be harmonized and the palatability is lowered.
本発明の容器詰飲料は、苦渋味抑制剤を配合すると飲用しやすくなり好ましい。用いる苦渋味抑制剤は特に限定はないが、サイクロデキストリンが好ましい。サイクロデキストリンとしては、α−、β−、γ−サイクロデキストリン及び分岐α−、β−、γ−サイクロデキストリンが使用できる。サイクロデキストリンは飲料中に０．００５〜０．５質量％、更に０．０１〜０．３質量％含有するのが好ましい。 The container-packed beverage of the present invention is preferably mixed with a bitter and astringent taste suppressant because it is easy to drink. The bitter and astringent taste inhibitor to be used is not particularly limited, but cyclodextrin is preferred. As the cyclodextrin, α-, β-, γ-cyclodextrin and branched α-, β-, γ-cyclodextrin can be used. The cyclodextrin is preferably contained in the beverage in an amount of 0.005 to 0.5 mass%, more preferably 0.01 to 0.3 mass%.
更に、本発明の容器詰飲料には、酸化防止剤、香料、各種エステル類、有機酸類、有機酸塩類、無機酸類、無機酸塩類、無機塩類、色素類、乳化剤、保存料、調味料、甘味料、酸味料、ガム、乳化剤、油、ビタミン、アミノ酸、果汁エキス類、野菜エキス類、花蜜エキス類、ｐＨ調整剤又は品質安定剤等の添加剤を配合してもよい。 Furthermore, the container-packed beverage of the present invention includes antioxidants, fragrances, various esters, organic acids, organic acid salts, inorganic acids, inorganic acid salts, inorganic salts, pigments, emulsifiers, preservatives, seasonings, sweetness Additives such as additives, acidulants, gums, emulsifiers, oils, vitamins, amino acids, fruit juice extracts, vegetable extracts, nectar extracts, pH adjusters or quality stabilizers may be incorporated.
本発明の容器詰飲料に使用される容器は、一般の飲料と同様にポリエチレンテレフタレートを主成分とする成形容器（いわゆるＰＥＴボトル）、金属缶、金属箔やプラスチックフィルムと複合された紙容器、瓶等の通常の形態で提供することができる。ここでいう容器詰飲料とは希釈せずに飲用できるものをいう。 The container used for the container-packed beverage of the present invention is a molded container (so-called PET bottle) mainly composed of polyethylene terephthalate, a metal can, a paper container combined with a metal foil or a plastic film, and a bottle as in the case of general beverages. Etc. can be provided in the usual form. The term “packaged beverage” as used herein means a beverage that can be drunk without dilution.
本発明の容器詰飲料は、例えば、金属缶のように容器に充填後、加熱殺菌できる場合にあっては食品衛生法に定められた殺菌条件で製造されるが、ＰＥＴボトル、紙容器のようにレトルト殺菌できないものについては、あらかじめ上記と同等の殺菌条件、例えばプレート式熱交換器等で高温短時間殺菌後、一定の温度迄冷却して容器に充填する等の方法が採用される。また無菌下で、充填された容器に別の成分を配合して充填してもよい。更に、酸性下で加熱殺菌後、無菌下でｐＨを中性に戻すことや、中性下で加熱殺菌後、無菌下でｐＨを酸性に戻す等の操作も可能である。 The container-packed beverage of the present invention is manufactured under the sterilization conditions stipulated in the Food Sanitation Law when it can be sterilized by heating after filling into a container like a metal can, for example, a PET bottle, a paper container, etc. For those that cannot be retort sterilized, a sterilization condition equivalent to the above, for example, a method of sterilizing at high temperature and short time in a plate heat exchanger or the like and then cooling to a certain temperature and filling the container is adopted. Moreover, you may mix | blend another component with the filled container under aseptic conditions. Furthermore, after sterilization by heating under acidic conditions, the pH can be returned to neutrality under aseptic conditions, or after sterilization by heating under neutral conditions, the pH can be returned to acidic conditions under aseptic conditions.
非重合体カテキン類の測定
非重合体カテキン類組成物を蒸留水で希釈し、フィルター（０．８μｍ）でろ過後、島津製作所社製、高速液体クロマトグラフ（型式ＳＣＬ−１０ＡＶＰ）を用い、オクタデシル基導入液体クロマトグラフ用パックドカラム Ｌ−カラムＴＭ ＯＤＳ（４．６ｍｍφ×２５０ｍｍ：財団法人 化学物質評価研究機構製）を装着し、カラム温度３５℃で、Ａ液及びＢ液を用いたグラジエント法によって行った。移動相Ａ液は酢酸を０．１ｍｏｌ／Ｌ含有の蒸留水溶液、Ｂ液は酢酸を０．１ｍｏｌ／Ｌ含有のアセトニトリル溶液とし、試料注入量は２０μＬ、ＵＶ検出器波長は２８０ｎｍの条件で行った。
Measurement of non-polymer catechins The composition of non-polymer catechins was diluted with distilled water, filtered with a filter (0.8 μm), and then octadecyl using a high performance liquid chromatograph (model SCL-10AVP) manufactured by Shimadzu Corporation. Packed column for base-introduced liquid chromatograph L-column TM ODS (4.6 mmφ × 250 mm: manufactured by Chemicals Evaluation and Research Institute) was installed, and the column temperature was 35 ° C., and the gradient method using liquid A and liquid B was used. went. The mobile phase A solution was a distilled aqueous solution containing 0.1 mol / L of acetic acid, the B solution was an acetonitrile solution containing 0.1 mol / L of acetic acid, the sample injection amount was 20 μL, and the UV detector wavelength was 280 nm. .
カフェインの測定
（分析機器）
ＨＰＬＣ（日立製作所社製）装置を使用。
プロッター：Ｄ−２５００，ディティクター：Ｌ−４２００
ポンプ：Ｌ−７１００，オートサンプラー：Ｌ−７２００
カラム：ｌｎｅｒｔｓｉｌ ＯＤＳ−２、内径２．１ｍｍ×長さ２５０ｍｍ
（分析条件）
サンプル注入量：１０μＬ，流量：１．０ｍＬ／ｍｉｎ
紫外線吸光光度計検出波長：２８０ｎｍ
溶離液Ａ：０．１ｍｏｌ／Ｌ酢酸水溶液，溶離液Ｂ：０．１ｍｏｌ／Ｌ酢酸アセトニトリル溶液
濃度勾配条件（体積％）
時間（分） 溶離液Ａ 溶離液Ｂ
０ ９７ ３
５ ９７ ３
３７ ８０ ２０
４３ ８０ ２０
４３．５ ０ １００
４８．５ ０ １００
４９ ９７ ３
６２ ９７ ３
（カフェインのリテンションタイム）
カフェイン：２７．２分
ここで求めたエリア％から標準物質により質量％を求めた。
Measurement of caffeine (analytical instrument)
Uses HPLC (Hitachi, Ltd.) equipment.
Plotter: D-2500, Detector: L-4200
Pump: L-7100, Autosampler: L-7200
Column: lnersil ODS-2, inner diameter 2.1 mm × length 250 mm
(Analysis conditions)
Sample injection volume: 10 μL, flow rate: 1.0 mL / min
Ultraviolet absorptiometer detection wavelength: 280 nm
Eluent A: 0.1 mol / L acetic acid aqueous solution, eluent B: 0.1 mol / L acetic acid acetonitrile solution concentration gradient condition (volume%)
Time (min) Eluent A Eluent B
0 97 3
5 97 3
37 80 20
43 80 20
43.5 0 100
48.5 0 100
49 97 3
62 97 3
(Caffeine retention time)
Caffeine: 27.2 minutes From the area% obtained here, the mass% was obtained using a standard substance.
色相評価
（分析機器）
精製緑茶抽出物を非重合体カテキン濃度１８０ｍｇ／１００ｍＬになるようにイオン交換水で希釈し、そのサンプルを用い外観の評価を目視で行った。
Hue evaluation (analytical instrument)
The purified green tea extract was diluted with ion-exchanged water so that the non-polymer catechin concentration was 180 mg / 100 mL, and the appearance was visually evaluated using the sample.
安定性の目視評価
精製緑茶抽出物を非重合体カテキン濃度１００ｍｇ／１００ｍＬになるようにイオン交換水で希釈し、５０ｍＬバイアル瓶に入っている評価サンプルをイルミネーター上で内容物の状態を観察し、目視判定した。
Visual evaluation of stability The purified green tea extract was diluted with ion-exchanged water so that the non-polymer catechin concentration was 100 mg / 100 mL, and the evaluation sample contained in the 50 mL vial was observed on the illuminator. The visual judgment was made.
吸光度測定
Ｕ−２００１ Ｓｐｅｃｔｒｏｐｈｏｔｏｍｅｔｅｒ（ＨＩＴＡＣＨＩ社製）装置を使用。
分光光度計で６６０nmの吸光度における値を測定した。測定においては、精製緑茶抽出物をカテキン濃度１質量％になるようにイオン交換水で希釈し、そのサンプルを用いて吸光度を測定した。
Absorbance measurement U-2001 Spectrophotometer (manufactured by HITACHI) was used.
The value at an absorbance of 660 nm was measured with a spectrophotometer. In the measurement, the purified green tea extract was diluted with ion-exchanged water so that the catechin concentration was 1% by mass, and the absorbance was measured using the sample.
実施例１ 精製緑茶抽出物Ａ
酸性白土（ミズカエース＃６００、水澤化学社製）１００ｇを常温、２５０ｒ／ｍｉｎ攪拌条件下の９２．４質量％エタノール水溶液８００ｇ中に分散させ、約１０分間攪拌を行った後、緑茶抽出物（ポリフェノンＨＧ、東京フードテクノ製）２００ｇを投入し、室温のまま約３時間の攪拌を続けた（ｐＨ４．３）。その後、２号ろ紙でろ過した。その溶液を活性炭（クラレコールＧＬＣ、クラレケミカル社製）２０ｇと接触させ、続けて０．２μｍメンブランフィルターによってろ過を行った。その溶液をスチレン系合成吸着剤（ＨＰ−２０、三菱化学社製）２００ｇと接触させ、その後、２号ろ紙でろ過した。最後にイオン交換水２００ｇを添加して、４０℃、０．０２７２ｋｇ／ｃｍ2でエタノールを留去し、その後、水分量を調整して精製緑茶抽出物Ａを得た。
処理後の非重合体カテキン類／カフェイン質量比＝４６．６
処理後のガレート体率＝５３．０質量％
Example 1 Purified green tea extract A
100 g of acid clay (Mizuka Ace # 600, manufactured by Mizusawa Chemical Co., Ltd.) was dispersed in 800 g of a 92.4 mass% ethanol aqueous solution under stirring conditions at room temperature and 250 r / min. After stirring for about 10 minutes, a green tea extract (polyphenone) HG (manufactured by Tokyo Food Techno) was added, and stirring was continued for about 3 hours at room temperature (pH 4.3). Then, it filtered with No. 2 filter paper. The solution was brought into contact with 20 g of activated carbon (Kuraray Coal GLC, manufactured by Kuraray Chemical Co., Ltd.), followed by filtration through a 0.2 μm membrane filter. The solution was brought into contact with 200 g of a styrene synthetic adsorbent (HP-20, manufactured by Mitsubishi Chemical Corporation), and then filtered through No. 2 filter paper. Finally, 200 g of ion-exchanged water was added, ethanol was distilled off at 40 ° C. and 0.0272 kg / cm 2 , and then the water content was adjusted to obtain purified green tea extract A.
Non-polymer catechins / caffeine mass ratio after treatment = 46.6
Galate body ratio after treatment = 53.0 mass%
実施例２ 精製緑茶抽出物Ｂ
合成吸着剤をメタクリル系合成吸着剤（ＨＰ２ＭＧ、三菱化学社製）を用いた以外実施例１と同様の操作を行なって精製緑茶抽出物Ｂを得た。
処理後の非重合体カテキン類／カフェイン質量比＝４７．０
処理後のガレート体率＝５３．０質量％
Example 2 Purified green tea extract B
Purified green tea extract B was obtained in the same manner as in Example 1 except that methacrylic synthetic adsorbent (HP2MG, manufactured by Mitsubishi Chemical Corporation) was used as the synthetic adsorbent.
Non-polymer catechins / caffeine mass ratio after treatment = 47.0
Galate body ratio after treatment = 53.0 mass%
実施例３ 精製緑茶抽出物Ｃ
合成吸着剤をフェノール系合成吸着剤（ＸＡＤ７６１、ロームアンドハース社製）を用いた以外実施例１と同様の操作を行なって精製緑茶抽出物Ｃを得た。
処理後の非重合体カテキン類／カフェイン質量比＝６１．４
処理後のガレート体率＝５２．６質量％
Example 3 Purified Green Tea Extract C
A purified green tea extract C was obtained in the same manner as in Example 1 except that the synthetic adsorbent was a phenol-based synthetic adsorbent (XAD761, manufactured by Rohm and Haas).
Non-polymer catechins / caffeine mass ratio after treatment = 61.4
Galate fraction after treatment = 52.6% by mass
比較例１ 精製緑茶抽出物Ｄ
酸性白土（ミズカエース＃６００、水澤化学社製）１００ｇを常温、２５０ｒ／ｍｉｎ攪拌条件下の９２．４質量％エタノール水溶液８００ｇ中に分散させ、約１０分間攪拌を行った後、緑茶抽出物（ポリフェノンＨＧ、東京フードテクノ製）２００ｇを投入し、室温のまま約３時間の攪拌を続けた（ｐＨ４．３）。その後、２号ろ紙でろ過した。その溶液を活性炭（クラレコールＧＬＣ、クラレケミカル社製）２０ｇと接触させ、続けて０．２μｍメンブランフィルターによってろ過を行った。最後にイオン交換水２００ｇを添加して、４０℃、０．０２７２ｋｇ／ｃｍ2でエタノールを留去し、その後、水分量を調整して精製緑茶抽出物Ｄを得た。
処理後の非重合体カテキン類／カフェイン質量比＝４４．９
処理後のガレート体率＝５３．２質量％
Comparative Example 1 Purified green tea extract D
100 g of acid clay (Mizuka Ace # 600, manufactured by Mizusawa Chemical Co., Ltd.) was dispersed in 800 g of a 92.4 mass% ethanol aqueous solution under stirring conditions at room temperature and 250 r / min. After stirring for about 10 minutes, a green tea extract (polyphenone) HG (manufactured by Tokyo Food Techno) was added, and stirring was continued for about 3 hours at room temperature (pH 4.3). Then, it filtered with No. 2 filter paper. The solution was brought into contact with 20 g of activated carbon (Kuraray Coal GLC, manufactured by Kuraray Chemical Co., Ltd.), followed by filtration through a 0.2 μm membrane filter. Finally, 200 g of ion-exchanged water was added, ethanol was distilled off at 40 ° C. and 0.0272 kg / cm 2 , and then the water content was adjusted to obtain purified green tea extract D.
Non-polymer catechins / caffeine mass ratio after treatment = 44.9
Galate body ratio after treatment = 53.2% by mass
比較例２ 精製緑茶抽出物Ｅ
合成吸着剤に替えて弱酸性陽イオン交換樹脂（ＤＵＯＬＩＴＥ Ｃ４７６、ロームアンドハース社製）を用いた以外実施例１と同様の操作を行なって精製緑茶抽出物Ｅを得た。
処理後の非重合体カテキン類／カフェイン質量比＝４２．６
処理後のガレート体率＝４７．６質量％
Comparative Example 2 Purified Green Tea Extract E
Purified green tea extract E was obtained in the same manner as in Example 1 except that a weakly acidic cation exchange resin (DUOLITE C476, manufactured by Rohm and Haas) was used instead of the synthetic adsorbent.
Non-polymer catechins / caffeine mass ratio after treatment = 42.6
Galate fraction after treatment = 47.6% by mass
比較例３ 精製緑茶抽出物Ｆ
合成吸着剤に替えて強塩基性陰イオン交換樹脂（ＰＡ３０８、三菱化学社製）を用いた以外実施例１と同様の操作を行なって精製緑茶抽出物Ｆを得た。
処理後の非重合体カテキン類／カフェイン質量比＝１６
処理後のガレート体率＝４３．３質量％
Comparative Example 3 Purified Green Tea Extract F
Purified green tea extract F was obtained in the same manner as in Example 1 except that a strongly basic anion exchange resin (PA308, manufactured by Mitsubishi Chemical Corporation) was used instead of the synthetic adsorbent.
Non-polymer catechins / caffeine mass ratio after treatment = 16
Galate fraction after treatment = 43.3 mass%
実施例１〜３及び比較例１〜３の製造条件及び得られた精製緑茶抽出物の分析結果を表１及び表２に示す。 Tables 1 and 2 show the production conditions of Examples 1 to 3 and Comparative Examples 1 to 3 and the analysis results of the obtained purified green tea extract.
表１及び表２に示すように、本発明の製造方法により製造された精製緑茶抽出物は、カフェイン及び濁り成分が低減されていた。 As shown in Table 1 and Table 2, the purified green tea extract produced by the production method of the present invention had reduced caffeine and turbid components.
実施例４ 容器詰飲料
表１及び表２の精製緑茶抽出物を用いて表３に記載の容器詰飲料を調製した。食品衛生法に基づく殺菌処理及びホットパック充填を行って容器詰飲料とした。
Example 4 Container-packed beverages Using the purified green tea extracts of Tables 1 and 2, container-packed beverages described in Table 3 were prepared. A sterilization treatment and hot pack filling based on the Food Sanitation Law were performed to obtain a container-packed beverage.
５名の男性モニターが、製造した容器詰飲料を３７℃で３０日間保存した後に、製造直後の非茶系容器詰飲料と共に、それぞれ５００ｍＬを単回摂取し、製造直後を基準として、雑味（長期保存時における濁りに由来する雑味）の変化を、以下の基準で評点をつけ評価した。飲用時の品温はいずれも室温付近に合わせた。保存飲料の外観も目視により評価した。結果を表３に示す。 Five male monitors store the manufactured packaged beverages at 37 ° C. for 30 days, then ingest 500 mL each together with the non-tea-based packaged beverages immediately after production, The change in miscellaneous taste derived from turbidity during long-term storage was evaluated based on the following criteria. The product temperature at the time of drinking was adjusted to around room temperature. The appearance of the stored beverage was also evaluated visually. The results are shown in Table 3.
外観における変化：
Ａ 沈殿を含め外観に変化がない
Ｂ 沈殿を含め外観にやや変化がある
Ｃ 沈殿を含め外観に変化がある
Ｄ 沈殿を含め外観に大きく変化がある
Changes in appearance:
A There is no change in appearance including precipitation B There is a slight change in appearance including precipitation C There is a change in appearance including precipitation D There is a large change in appearance including precipitation
雑味における変化：
Ａ 感じにくい
Ｂ やや感じにくい
Ｃ やや感じる
Ｄ 感じる
Changes in miscellaneous taste:
A Difficult to feel B Slightly difficult to feel C Slightly feel D Feel
表３の結果から明らかなように、本発明により緑茶抽出物を処理した精製緑茶抽出物を使用した容器詰飲料は、長期に保存しても、何れも外観の変化がなく澄明であって、雑味の変化も認められなかった。 As is apparent from the results in Table 3, the packaged beverage using the purified green tea extract treated with the green tea extract according to the present invention is clear with no change in appearance even when stored for a long period of time. There was no change in miscellaneous taste.
実施例５
（１）緑茶葉６０００ｇに８４℃の熱水９０kgを添加し、６０分間抽出したのち、２号濾紙による濾過を行い、「緑茶抽出液」６６kg（pH５．４）を得た。（緑茶抽出液の非重合体カテキン類濃度＝ ０．９質量％、緑茶抽出液のガレート体率＝５２．２質量％）
この緑茶抽出液を温度２５℃に設定し、タンナーゼ（キッコーマン社製タンナーゼKTFH）を緑茶抽出液に対して２００ppmとなる濃度で添加し、１３０分間保持し、ガレート体率４０．２質量％になったところで、９０℃に溶液を加熱して、酵素を失活させ、反応を止めた（pH４．９）。この反応液を逆浸透膜（日東電工製NTR−759HR）を用いてＢｒｉｘ濃度２５まで濃縮処理を行い、液体の「タンナーゼ処理した緑茶抽出物の濃縮物」８kgを得た。得られた緑茶抽出物は非重合体カテキン類含有量６．９質量％、ガレート体率４０．１質量％、固形分濃度２質量％に溶解した水溶液のpH＝５．０であった。
（２）また、得られた濃縮液４．５kgを噴霧乾燥して粉末状の「タンナーゼ処理した緑茶抽出物」４００ｇを得た。得られた緑茶抽出物は非重合体カテキン類含有量３３．２質量％、ガレート体率４０．１質量％、固形分濃度２質量％に溶解した時の水溶液のpH＝５．０であった。
（３）得られた緑茶抽出物を用いて、実施例１と同様の精製処理を行い、濁りが全く見られず、色相もよく、かつ苦味の低減された精製緑茶抽出物を得た。
処理後の固形分中における非重合体カテキン類濃度＝６８質量％
処理後の非重合体カテキン類／カフェイン質量比＝４６．９
処理後のガレート体率＝４１．４質量％
６６０ｎｍ吸光度＝０．０１９
（４）得られた精製緑茶抽出物を用いて、実施例４、本発明品１と同様にして容器詰飲料を得た。この飲料は長期に保存しても外観の変化がなく、かつ苦味が低減されていた。
Example 5
(1) 90 kg of hot water at 84 ° C. was added to 6000 g of green tea leaves and extracted for 60 minutes, followed by filtration with No. 2 filter paper to obtain 66 kg (pH 5.4) of “green tea extract”. (Non-polymer catechin concentration in green tea extract = 0.9 mass%, gallate body ratio in green tea extract = 52.2 mass%)
This green tea extract was set at a temperature of 25 ° C., tannase (Kikkoman Tannase KTFH) was added at a concentration of 200 ppm with respect to the green tea extract and held for 130 minutes, resulting in a gallate body ratio of 40.2% by mass. The solution was heated to 90 ° C. to deactivate the enzyme and stop the reaction (pH 4.9). The reaction solution was concentrated to a Brix concentration of 25 using a reverse osmosis membrane (NTR-759HR manufactured by Nitto Denko) to obtain 8 kg of a liquid “concentrate of tannase-treated green tea extract”. The obtained green tea extract had a non-polymer catechin content of 6.9% by mass, a gallate body ratio of 40.1% by mass, and a pH of an aqueous solution dissolved in a solid content concentration of 2% by mass = 5.0.
(2) Further, 4.5 kg of the obtained concentrated liquid was spray-dried to obtain 400 g of a powdered “tannase-treated green tea extract”. The obtained green tea extract had a non-polymer catechin content of 33.2% by mass, a gallate body ratio of 40.1% by mass, and a pH of the aqueous solution when dissolved in a solid content concentration of 2% by mass = 5.0. .
(3) Using the obtained green tea extract, the same purification treatment as in Example 1 was performed to obtain a purified green tea extract having no turbidity, good hue, and reduced bitterness.
Non-polymer catechin concentration in solid content after treatment = 68% by mass
Non-polymer catechins / caffeine mass ratio after treatment = 46.9
Galate fraction after treatment = 41.4% by mass
660 nm absorbance = 0.019
(4) Using the obtained purified green tea extract, a container-packed beverage was obtained in the same manner as in Example 4 and Product 1 of the present invention. This beverage had no change in appearance even when stored for a long time, and the bitterness was reduced.
Claims (6)
有機溶媒と水の質量比が９１／９〜９７／３の混合溶液に分散した緑茶抽出物を合成吸着剤と接触処理する工程
を含む、非重合体カテキン類を固形分中に２５〜９０質量％含有する精製緑茶抽出物の製造法。 A step of contacting a green tea extract dispersed in a mixed solution having an organic solvent and water mass ratio of 91/9 to 97/3 with activated carbon and acid clay or activated clay; and
Mass ratio of organic solvent and water comprises the step <br/> to contact treatment with the synthetic adsorbent dispersed green tea extract in a mixed solution of 91 / 9-97 / 3, the non-polymer catechins in the solid content The manufacturing method of the refined green tea extract containing 25-90 mass%.
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