JP5175167B2 - Carbonated beverage containing high-intensity sweetener - Google Patents
Carbonated beverage containing high-intensity sweetener Download PDFInfo
- Publication number
- JP5175167B2 JP5175167B2 JP2008319558A JP2008319558A JP5175167B2 JP 5175167 B2 JP5175167 B2 JP 5175167B2 JP 2008319558 A JP2008319558 A JP 2008319558A JP 2008319558 A JP2008319558 A JP 2008319558A JP 5175167 B2 JP5175167 B2 JP 5175167B2
- Authority
- JP
- Japan
- Prior art keywords
- caffeine
- carbonated
- beverage
- feeling
- polymerized catechin
- 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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- 235000014171 carbonated beverage Nutrition 0.000 title claims description 122
- 235000013615 non-nutritive sweetener Nutrition 0.000 title claims description 49
- 239000008123 high-intensity sweetener Substances 0.000 title claims description 48
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- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 107
- 235000005487 catechin Nutrition 0.000 claims description 107
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- 150000003445 sucroses Chemical class 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940026510 theanine Drugs 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
Landscapes
- Non-Alcoholic Beverages (AREA)
Description
本発明は、高甘味度甘味料を含有する炭酸飲料に関し、より詳細には、高甘味度甘味料を含有する炭酸飲料の香味（ボディ感、後口のキレ等）と気泡感とを向上させた、風味良好な炭酸飲料に関する。 The present invention relates to a carbonated beverage containing a high-intensity sweetener, and more specifically, to improve the flavor (body feeling, sharpness of the back mouth, etc.) and the feeling of bubbles of a carbonated beverage containing a high-intensity sweetener. Further, the present invention relates to a carbonated beverage with good flavor.
近年の健康志向の高まりから、アスパルテーム、ステビア、アセスルファムＫ、スクラロースなどの高甘味度の甘味料（本明細書中、「高甘味度甘味料」ともいう）を使用した製品が増加している。高甘味度甘味料は、蔗糖の数倍〜数千倍の甘味度を有し、ダイエット用甘味料等として多くの用途（例えば肥満などの場合のカロリー摂取制限、糖尿病などの疾患により血糖値上昇抑制等）に使用され、「低カロリー甘味料」としての特徴を持つが、甘味が持続し続けるため後味のキレが悪い、後味に高甘味度甘味料特有の異味や苦味を有するといった後味の悪さや、ボディ感（コク感、量感、味の厚みともいう）の不足といった欠点も有している。 Due to the recent increase in health-consciousness, products using high-intensity sweeteners such as aspartame, stevia, acesulfame K, and sucralose (also referred to as “high-intensity sweetener” in this specification) are increasing. High-intensity sweeteners have sweetness several times to several thousand times that of sucrose, and have many uses as diet sweeteners (for example, restriction of calorie intake in the case of obesity, increased blood sugar levels due to diseases such as diabetes) It has a characteristic as a "low calorie sweetener", but has a bad aftertaste such as a bad aftertaste because the sweetness continues and the aftertaste has a peculiar taste and bitterness peculiar to a high sweetness sweetener. In addition, it has a drawback of lack of body feeling (also referred to as richness, volume, taste thickness).
そこで、高甘味度甘味料の後味を改善する種々の成分が開示されている。例えば、特許文献１には、甘味のマスキング剤としてカフェイン等が有用であることが記載されている。しかし、カフェインは本来苦味を有するものであり、特に炭酸飲料においてはその苦味が顕著となることも知られている（特許文献２参照）。 Therefore, various components that improve the aftertaste of a high-intensity sweetener have been disclosed. For example, Patent Document 1 describes that caffeine is useful as a sweetness masking agent. However, caffeine originally has a bitter taste, and it is also known that the bitter taste becomes remarkable particularly in carbonated beverages (see Patent Document 2).
また、特許文献３には、紅茶葉を水で抽出処理して抽出液を得、次いでその抽出液を吸着剤で精製処理して得られる精製物からなる経口製品の呈味改善剤が開示され、該呈味改善剤が高甘味度甘味料による不快な後味を低減することが記載されている。そして、その有効成分である上記紅茶葉から得られる精製物（紅茶葉抽出物）の成分が、キナ酸、グルコース、フルクトース、テアニンであること、その配合量は、高甘味度甘味料に対して０．１〜５重量部であることが記載されている。さらに、特許文献４には、乳成分含有飲料の呈味性改善剤が開示され、乳成分と甘味料を配合した飲食品にポリフェノール類を添加して、すっきりとした後味、味のキレを出すことが開示されており、前記ポリフェノールが茶由来のポリフェノール、好ましくは不発酵茶（緑茶）由来のポリフェノール（（＋）−カテキン、（−）−エピカテキン、（＋）−ガロカテキン、（−）−エピガロカテキン、（−）−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および（−）−エピガロカテキンガレート）であることが記載されている。さらにまた、特許文献５には、少なくとも０．０５重量％のカテキン類又はエピカテキン類（非重合カテキン）と０．００２〜１．０重量％のカフェインとを含有する飲料が記載され、実施例にはこれを用いた炭酸飲料も開示されているが、重合カテキンとカフェインとの相乗的な作用については何ら記載も示唆もされていない。 Patent Document 3 discloses a taste improving agent for oral products comprising a purified product obtained by extracting black tea leaves with water to obtain an extract and then purifying the extract with an adsorbent. It is described that the taste improving agent reduces an unpleasant aftertaste due to a high-intensity sweetener. And the component of the refined product (tea leaf extract) obtained from the said tea leaf which is the active ingredient is quinic acid, glucose, fructose, theanine, The compounding quantity is with respect to a high sweetness degree sweetener. It is described that it is 0.1 to 5 parts by weight. Furthermore, Patent Document 4 discloses a taste improver for a milk component-containing beverage, and a polyphenol is added to a food or drink containing a milk component and a sweetener to produce a clean aftertaste and taste. Wherein the polyphenol is a tea-derived polyphenol, preferably a non-fermented tea (green tea) -derived polyphenol ((+)-catechin, (−)-epicatechin, (+)-gallocatechin, (−) — Epigallocatechin, (−)-catechin gallate, (−)-epicatechin gallate, (−)-gallocatechin gallate and (−)-epigallocatechin gallate). Furthermore, Patent Document 5 describes and implements a beverage containing at least 0.05% by weight of catechins or epicatechins (non-polymerized catechins) and 0.002 to 1.0% by weight of caffeine. The example discloses a carbonated beverage using this, but does not describe or suggest any synergistic action of polymerized catechin and caffeine.
一方、甘味剤（高甘味度甘味料）を配合した炭酸飲料が、ショ糖と甘味の質（後味のキレ）が異なるだけでなく、ショ糖を用いた場合に比べて開栓後炭酸ガスが抜けやすく、溶存炭酸ガスに由来する清涼感が速く損なわれ、嗜好性が速く低下することが指摘されている。そして、特許文献６では、これを解決する方法として、炭酸飲料に冷水可溶の天然ガム質を含有させることが開示されている。
炭酸飲料における適度な気泡は、口腔内や喉への刺激感（口あたりや喉越し）が、飲用中及び飲用後の爽快感を醸成し、あっさりとした風味とさわやかな清涼感を創出するものである。より爽快な刺激感を備える目的から、容器内ガス圧が２．０〜５．０ｋｇ／ｃｍ２の範囲となるように炭酸ガスが圧入された、いわゆる高ガス圧炭酸飲料が開発されているが、気泡による清涼感は感じさせるが、発生する気泡が粗くて持ちが悪いという問題を有し、高ガス圧炭酸飲料に求められる爽快な刺激感の点で十分に満足できるものではなかった。 Appropriate bubbles in carbonated beverages create a refreshing flavor and a refreshing refreshing sensation in the mouth and throat (around the mouth and over the throat), creating a refreshing feeling during and after drinking. It is. For the purpose of providing a more exhilarating stimulation, a so-called high gas pressure carbonated beverage in which carbon dioxide gas is injected so that the gas pressure in the container is in the range of 2.0 to 5.0 kg / cm 2 has been developed. However, although the air bubble feels a refreshing sensation, it has a problem that the generated bubbles are rough and poorly held, and is not sufficiently satisfactory in terms of the refreshing irritation required for high gas pressure carbonated beverages.
特に、高甘味度甘味料を含有する炭酸飲料では、開栓後に炭酸ガスが抜けやすいという問題について、最終製品（炭酸飲料）の味や粘度等に影響を及ぼしたり、煩雑な工程を要したりすることなしに、炭酸ガスの抜けを防止する方法は存在していなかった。 In particular, carbonated beverages containing high-intensity sweeteners may affect the taste and viscosity of the final product (carbonated beverages) and require complicated processes for the problem that carbon dioxide tends to escape after opening. Without doing so, there was no way to prevent the escape of carbon dioxide.
また、高甘味度甘味料を含有する炭酸飲料（特に、高ガス圧の炭酸飲料）においては、高甘味度甘味料特有の異味や苦味に、炭酸の刺激が相俟って、後味の苦味がより顕著に感じられ、炭酸飲料に求められる爽快感、清涼感が損なわれるという問題がある。しかし、上記の高甘味度甘味料の後味を改善する種々の成分では、高甘味度甘味料を含有する炭酸飲料の後味を改善するのに十分満足できるほどの効果が得られず、十分な効果を得ることを期待して多量に配合すると、最終製品の味に影響を及ぼすことがあった。 Further, in carbonated beverages containing high-intensity sweeteners (especially carbonated beverages at high gas pressure), the taste and bitterness peculiar to high-intensity sweeteners are combined with the stimulation of carbonation, resulting in a bitter aftertaste. There is a problem that it feels more conspicuous and the refreshing feeling and refreshing feeling required for carbonated drinks are impaired. However, the various components that improve the aftertaste of the high-intensity sweetener cannot obtain a sufficient effect to improve the aftertaste of the carbonated beverage containing the high-intensity sweetener. When it is formulated in a large amount with the expectation of obtaining a product, the taste of the final product may be affected.
本発明の目的は、最終製品の味に異味を与えることなく、炭酸飲料（特に高ガス圧炭酸飲料）の風味を向上しうる添加剤や、風味が向上された飲料（特に高ガス圧炭酸飲料）を提供することにある。 An object of the present invention is to provide an additive that can improve the flavor of carbonated beverages (especially high gas pressure carbonated beverages) without giving a different taste to the taste of the final product, and a beverage with improved flavors (especially high gas pressure carbonated beverages). ) To provide.
本発明者らは上記課題を解決するために鋭意検討を行った結果、重合ポリフェノール、特に重合カテキンに甘味剤の後味のキレを向上させる作用があることを見出した。そして、この重合カテキンに所定濃度のカフェインを併用させることで、高甘味度甘味料の後味を相乗的に改善することができ、高甘味度甘味料を含有する炭酸飲料の後味をも改善することができることを見出した。カフェイン含有炭酸飲料では、カフェインの苦味がより顕著になることが知られているが、驚くべきことに、重合カテキンに所定濃度のカフェインを併用した場合には、カフェインの苦味が抑制され、炭酸飲料（特に、高ガス圧炭酸飲料）であってもカフェインの苦味が問題にならなかった。 As a result of intensive studies to solve the above problems, the present inventors have found that polymerized polyphenols, particularly polymerized catechins, have an effect of improving the aftertaste of sweeteners. And by using this polymerized catechin together with a predetermined concentration of caffeine, the aftertaste of a high-intensity sweetener can be synergistically improved, and the aftertaste of a carbonated beverage containing a high-intensity sweetener is also improved. I found that I can do it. In caffeine-containing carbonated beverages, it is known that the bitter taste of caffeine becomes more prominent, but surprisingly, when a predetermined concentration of caffeine is used in combination with polymerized catechin, the bitter taste of caffeine is suppressed. Even with carbonated beverages (especially high gas pressure carbonated beverages), the bitter taste of caffeine was not a problem.
そして、さらに驚くべきことに、カフェインと重合カテキンとが炭酸飲料の気泡感を相乗的に向上し、高甘味度甘味料を含有する炭酸飲料の開栓後に炭酸ガスが抜けやすいという問題を解決しうることを見出し、本発明を完成するに至った。 And more surprisingly, caffeine and polymerized catechins synergistically improve the bubble feeling of carbonated beverages, solving the problem that carbon dioxide tends to escape after opening carbonated beverages containing high-intensity sweeteners. As a result, the present invention has been completed.
すなわち本発明は、（ａ）高甘味度甘味料、（ｂ）重合カテキン０．００５重量％以上０．０５重量％未満、および（ｃ）カフェイン０．００５重量％以上０．０３重量％未満、を含有する炭酸飲料である。 That is, the present invention comprises (a) a high-intensity sweetener, (b) a polymerized catechin of 0.005 wt% or more and less than 0.05 wt%, and (c) caffeine of 0.005 wt% or more and less than 0.03 wt%. , Containing carbonated beverages.
また本発明は、前記炭酸飲料において、高甘味度甘味料が、アスパルテーム、アセスルファムＫ、ステビア、スクラロースの中から選択される１種以上の高甘味度甘味料である炭酸飲料である。 The present invention is the carbonated beverage, wherein in the carbonated beverage, the high-intensity sweetener is one or more high-intensity sweeteners selected from aspartame, acesulfame K, stevia, and sucralose.
また本発明は、前記いずれかの炭酸飲料においてＢｒｉｘが０．０１〜１．０である炭酸飲料である。 Moreover, this invention is a carbonated drink whose Brix is 0.01-1.0 in one of the said carbonated drinks.
さらに本発明は、前記いずれかの炭酸飲料において、ガス圧が２．０〜５．０ｋｇ／ｃｍ２である炭酸飲料である。 Furthermore, this invention is a carbonated beverage whose gas pressure is 2.0-5.0 kg / cm < 2 > in one of the said carbonated beverages.
さらに本発明は、前記いずれかの炭酸飲料において、重合カテキン（ｂ）に対するカフェイン（ｃ）の比率［（ｃ）／（ｂ）］（重量比）が０．１２５〜２．０である炭酸飲料である。 Furthermore, the present invention provides the carbonated beverage in which the ratio [(c) / (b)] (weight ratio) of caffeine (c) to polymerized catechin (b) is 0.125 to 2.0 in any of the carbonated beverages described above. It is a beverage.
また本発明は、前記いずれかの炭酸飲料であって、容器詰炭酸飲料であり、再栓可能な蓋部を有するものである炭酸飲料である。 Moreover, this invention is a carbonated drink which is a carbonated drink of any one of the above, and is a container-packed carbonated drink and has a lid portion that can be re-plugged.
さらに本発明は、（ｃ）カフェインと、（ｂ）重合カテキンとを含有し、重合カテキン（ｂ）に対するカフェイン（ｃ）の比率［（ｃ）／（ｂ）］（重量比）が０．１２５〜２．０である、炭酸飲料用添加剤である。 Furthermore, the present invention contains (c) caffeine and (b) polymerized catechin, and the ratio of caffeine (c) to polymerized catechin (b) [(c) / (b)] (weight ratio) is 0. It is an additive for carbonated beverages that is 125-2.0.
また本発明は、前記炭酸飲料用添加剤であって、高甘味度甘味料を含有する炭酸飲料の気泡感を改善する添加剤である。 Moreover, this invention is an additive for said carbonated drinks, Comprising: It is an additive which improves the bubble feeling of the carbonated drink containing a high sweetness degree sweetener.
本発明によると、後味が改善された高甘味度甘味料を含有する炭酸飲料が提供される。本発明の炭酸飲料は、カフェインの苦味を呈するなど、炭酸飲料自体の味へ影響を及ぼすことがなく、また甘味のピークの甘味度を落とすことなく、後味のみが改善された飲料、すなわち高甘味度甘味料の後味として持続する甘味や、後味に感じられる高甘味度甘味料特有の異味や苦味が低減された、爽快な刺激感や清涼感を有する炭酸飲料である。 According to the present invention, a carbonated beverage containing a high intensity sweetener with improved aftertaste is provided. The carbonated beverage of the present invention does not affect the taste of the carbonated beverage itself, for example, exhibits a bitter taste of caffeine, and does not reduce the sweetness of the sweetness peak, i.e., a beverage with improved aftertaste, i.e. high It is a carbonated beverage having a refreshing sensation or refreshing feeling with reduced sweetness that lasts as a aftertaste of a sweetness sweetener, and the off-taste and bitterness peculiar to high sweetness sweeteners that can be felt in the aftertaste.
本発明の高甘味度甘味料を含有する炭酸飲料は、後味が改善されるだけでなく、所定濃度の重合カテキンとカフェインとが相乗的に作用して、飲料にボディ感を付与するという特徴もある。さらに、高甘味度甘味料を用いた炭酸飲料では、開栓後の炭酸ガスが抜け易いという問題を有するが、本発明の所定濃度の重合カテキンとカフェインとを含有する炭酸飲料では、相乗的に気泡感が改善され、開栓後においても好ましい気泡感が維持されるという特徴も有する。したがって、優れた香味と炭酸感（気泡感）とを有する、ドリンカビリティの高い炭酸飲料となる。さらに、高甘味度甘味料は、ダイエット甘味料をはじめとして多くの用途（例えば肥満などの場合のカロリー摂取制限、糖尿病などの疾患により血糖値上昇抑制等）に使用され、「低カロリー甘味料」としての特徴を持つが、コク感（ボディ感、味の厚みともいう）の不足が問題となっているが、本発明の飲料では、重合カテキンとカフェインとが相乗的にコク感を補うという利点もある。 The carbonated beverage containing the high-intensity sweetener of the present invention is characterized in that not only the aftertaste is improved, but also a predetermined concentration of polymerized catechin and caffeine act synergistically to give the beverage a body feeling. There is also. Furthermore, carbonated beverages using high-intensity sweeteners have a problem that carbon dioxide gas is easily released after opening, but the carbonated beverages containing the predetermined concentrations of polymerized catechin and caffeine of the present invention are synergistic. In addition, the air bubble feeling is improved, and a preferable air bubble feeling is maintained even after opening. Therefore, it becomes a carbonated beverage with high drinkability having excellent flavor and carbonation (bubble feeling). Furthermore, high-intensity sweeteners are used for many purposes including diet sweeteners (for example, restriction of calorie intake in cases of obesity, suppression of blood sugar level increase due to diseases such as diabetes, etc.). Although there is a problem of lack of richness (body feeling, also known as thickness of taste), in the beverage of the present invention, polymerized catechin and caffeine synergistically supplement the rich feeling. There are also advantages.
本発明の飲料はまた、風味を向上させた飲料としてだけでなく、カフェインの眠気抑制作用や興奮作用、重合カテキンのリパーゼ阻害作用等の生理活性を利用した、機能性飲料（保健飲料）としても有用な飲料である。 The beverage of the present invention is not only as a beverage with improved flavor, but also as a functional beverage (health beverage) utilizing physiological activities such as drowsiness suppression and excitatory action of caffeine, lipase inhibitory action of polymerized catechin, etc. Is also a useful beverage.
（高甘味度甘味料）
本発明は、特定量の重合カテキンとカフェインとを有効成分として含有させることにより、高甘味度甘味料を配合した炭酸飲料の呈味を改善することを特徴とする。ここで、本発明でいう高甘味度甘味料の呈味の改善とは、後味として持続する甘味（後甘味）を抑える作用、炭酸の刺激と相俟って感じられる高甘味度甘味料特有の異味や苦味を抑える作用（これらを総称して本明細書中、「後味のキレ」「後味の改善」ともいう）や、炭酸飲料の気泡感（炭酸感）を向上させる作用や、飲料にボディ感（本明細書中、「コク」、「量感」ともいう）をいう）を付与する作用をいう。
(High intensity sweetener)
The present invention is characterized by improving the taste of carbonated beverages containing a high-intensity sweetener by containing specific amounts of polymerized catechin and caffeine as active ingredients. Here, the improvement in the taste of the high-intensity sweetener as referred to in the present invention refers to an action that suppresses the sweetness (post-sweetness) that lasts as an aftertaste, a characteristic of a high-intensity sweetener that can be felt in combination with the stimulation of carbonic acid. An action that suppresses off-taste and bitterness (collectively, these are also referred to as “crisp of aftertaste” and “improvement of aftertaste” in the present specification), an action to improve the bubble feeling (carbonic feeling) of carbonated drinks, It refers to the action of imparting a feeling (also referred to as “rich” or “quantity” in the present specification).
本発明で用いられる高甘味度甘味料とは、砂糖に比べて強い甘味（例えば砂糖の１００倍以上の甘味）を有する甘味料をいう。天然甘味料及び合成甘味料の高甘味度甘味料が使用でき、例えば、ペプチド系甘味料、例えばアスパルテーム、ネオテーム、アリテーム等；配糖体系甘味料、例えばステビア（ステビア抽出物およびステビアを酵素処理してブドウ糖を付加した酵素処理ステビア等のステビア誘導体およびステビアの甘味成分の中で最も甘味質のよいレバウディオサイドＡを含む）、カンゾウ抽出物等；蔗糖誘導体例えばスクラロース等；合成甘味料、例えばアセスルファムＫ、サッカリン等が挙げられる。なかでも、アスパルテーム、アセスルファムＫ、ステビア、スクラロースを用いた場合、本発明の炭酸飲料の呈味を改善する作用が顕著に発揮されることから、これらの高甘味度甘味料を用いた炭酸飲料は、本発明の炭酸飲料の好ましい態様の一つである。 The high-intensity sweetener used in the present invention refers to a sweetener having a sweetness that is stronger than that of sugar (for example, a sweetness that is at least 100 times that of sugar). Natural sweeteners and high-intensity sweeteners such as synthetic sweeteners can be used, such as peptide sweeteners such as aspartame, neotame, aritem, etc .; glycoside sweeteners such as stevia (stevia extract and stevia Stevia derivatives such as enzyme-treated stevia added with glucose and rebaudioside A having the highest sweetness among the sweet components of stevia, licorice extract, etc .; sucrose derivatives such as sucralose, etc .; synthetic sweeteners such as Examples include acesulfame K and saccharin. Among these, when aspartame, acesulfame K, stevia, and sucralose are used, the effect of improving the taste of the carbonated beverage of the present invention is remarkably exhibited, so carbonated beverages using these high-intensity sweeteners are It is one of the preferable aspects of the carbonated drink of this invention.
本発明に用いられる高甘味度甘味料は、１つまたはそれ以上の組合せで用いてもよい。また、本発明の炭酸飲料における高甘味度甘味料の配合割合は、特に限定的ではなく、その配合目的に応じて適宜選択される。炭酸飲料における通常の配合量は、上記好ましい高甘味度甘味料を用いた場合、アスパルテームで１００ｍＬ当たり０．００１〜０．１ｇ、アセスルファムＫで１００ｍＬ当たり０．００１〜０．１ｇ、ステビアで１００ｍＬ当たり０．００１〜０．１ｇ、スクラロースで１００ｍＬ当たり０．０００４〜０．４５ｇ程度である。 The high intensity sweeteners used in the present invention may be used in one or more combinations. In addition, the blending ratio of the high-intensity sweetener in the carbonated beverage of the present invention is not particularly limited, and is appropriately selected according to the blending purpose. The usual blending amount in carbonated beverages is 0.001 to 0.1 g per 100 mL for aspartame, 0.001 to 0.1 g per 100 mL for acesulfame K, and 100 mL for stevia when using the preferred high-intensity sweetener. It is about 0.0004 to 0.45 g per 100 mL with 0.001 to 0.1 g and sucralose.
（重合カテキン）
本明細書でいう「重合カテキン」とは、重合していない単量体のカテキン類（（＋）−カテキン、（−）−エピカテキン、（＋）−ガロカテキン、（−）−エピガロカテキン、（−）−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、（−）−エピガロカテキンガレート）が、茶由来酵素、酵素、光等により複数個連結した構造を持つものをいう。具体的には、以下の条件のＨＰＬＣにより分析される成分をいい、テアフラビン（栗田リサーチセンター製）と同じ溶出時間（参考溶出時間：２４分）のピークとなる成分をいう（図１参照）。
・カラム：ＴＳＫ-gel ＯＤＳ-80ＴｓＱＡ（4.6mmφx150ｍｍ、東ソー株式会社）
・移動相：
A：水：アセトニトリル：トリフルオロ酢酸＝900：100：0.5
B：水：アセトニトリル：トリフルオロ酢酸＝200：800：0.5
・流速：1.0ml/min
・カラム温度：40℃
・グラディエント条件：
分析開始から5分後まではＢ液0％、
5分から11分まででＢ液8％、
11分から21分まででＢ液10％、
21分から22分まででＢ液100％、
22分から30分まで100％保持、
30分から31分までで0％
・検出：A280nm （データ採取時間は30分）、ピーク面積で定量。
・注入量：10μL
・標準物質：ウーロンホモビスフラバンB（略記：OHBF-B）
・重合カテキンの量は、標準物質としてＯＨＢＦ−Ｂを用い、検量線を作成することにより求められる。なお、標準物質であるＯＨＢＦ−Ｂは、例えば、Chem. Pharm. Bull 37(12), 3255-3563(1989)に記載の方法や、特開２００５−３３６１１７号公報（実施例３）に記載の方法に従って合成したもの(好ましくは純度９８％以上の純度まで精製したもの)、茶葉より単離したものなどを用いることができる。
(Polymerized catechin)
As used herein, “polymerized catechin” refers to non-polymerized monomeric catechins ((+)-catechin, (−)-epicatechin, (+)-gallocatechin, (−)-epigallocatechin, (−)-Catechin gallate, (−)-epicatechin gallate, (−)-gallocatechin gallate, (−)-epigallocatechin gallate) have a structure in which a plurality of tea-derived enzymes, enzymes, light, etc. are linked together. Say things. Specifically, it refers to a component analyzed by HPLC under the following conditions, and refers to a component that has the same elution time (reference elution time: 24 minutes) as theaflavin (manufactured by Kurita Research Center) (see FIG. 1).
Column: TSK-gel ODS-80TsQA (4.6mmφx150mm, Tosoh Corporation)
・ Mobile phase:
A: Water: Acetonitrile: Trifluoroacetic acid = 900: 100: 0.5
B: Water: Acetonitrile: Trifluoroacetic acid = 200: 800: 0.5
・ Flow rate: 1.0ml / min
・ Column temperature: 40 ℃
・ Gradient condition:
From 5 minutes after the start of analysis, B solution is 0%,
From 5 minutes to 11 minutes, B liquid 8%,
From 11 minutes to 21 minutes, B solution 10%,
From 21 minutes to 22 minutes, solution B is 100%,
100% hold from 22 to 30 minutes,
0% from 30 to 31 minutes
・ Detection: A280nm (data collection time is 30 minutes), quantified by peak area.
・ Injection volume: 10μL
Reference material: Oolong homobisflavan B (abbreviation: OHBF-B)
-The amount of polymerized catechin is determined by creating a calibration curve using OHBF-B as a standard substance. In addition, OHBF-B which is a standard substance is described in, for example, the method described in Chem. Pharm. Bull 37 (12), 3255-3563 (1989) or JP 2005-336117 A (Example 3). Those synthesized according to the method (preferably purified to a purity of 98% or more), those isolated from tea leaves, and the like can be used.
この重合カテキンとしては、具体的にはテアルビジン等の慣用名で呼ばれている重合カテキンの他、式（１）のエピガロカテキンガレート二量体、 As this polymerized catechin, specifically, epigallocatechin gallate dimer of the formula (1), in addition to polymerized catechins called by common names such as thealvidin,
式（２）のエピガロカテキンガレート三量体、 Epigallocatechin gallate trimer of formula (2),
式（３）のエピガロカテキンの二量体、 A dimer of epigallocatechin of formula (3),
（式中、Ｒ１およびＲ２は、それぞれ独立してＨまたはガロイル基である。）
式（４）のエピガロカテキンの三量体
(In the formula, R 1 and R 2 are each independently H or a galloyl group.)
Trimer of epigallocatechin of formula (4)
（式中、Ｒ３、Ｒ４およびＲ５は、それぞれ独立してＨまたはガロイル基である。）
式（５）のウーロンテアニン-３'-Ｏ-ガレート
(In the formula, R 3 , R 4 and R 5 are each independently H or a galloyl group.)
Oolong theanine-3'-O-gallate of formula (5)
等の重合カテキンが例示される。 Polymerized catechins such as are exemplified.
本発明の重合カテキンは、茶葉を溶媒抽出することにより得られる。原料となる茶葉としては、不発酵茶である緑茶、半発酵茶であるウーロン茶、発酵茶である紅茶のうち、１種類又は２種類以上を用いることができるが、なかでも、重合カテキンを多く含有する半発酵茶又は発酵茶の茶葉を用いるのがよい。抽出溶媒としては、水または熱水、メタノール、エタノール、イソプロパノール、酢酸エチルなどが用いられ１種もしくは２種類以上の混合物で抽出される。この茶葉の溶媒抽出物は、抽出物をそのまま用いてもよいが、濃縮又は精製したもの、すなわち茶葉の溶媒抽出物から重合カテキン以外の成分を選択的に除去して、重合カテキンの含有率を高めたものを用いるのがよい。 The polymerized catechin of the present invention can be obtained by solvent extraction of tea leaves. As the tea leaves used as raw materials, one or more kinds of green tea that is non-fermented tea, oolong tea that is semi-fermented tea, and black tea that is fermented tea can be used. It is recommended to use semi-fermented tea or fermented tea leaves. As the extraction solvent, water or hot water, methanol, ethanol, isopropanol, ethyl acetate or the like is used, and extraction is performed with one or a mixture of two or more. This solvent extract of tea leaves may be used as it is, but concentrated or purified, that is, by selectively removing components other than polymerized catechins from the solvent extract of tea leaves, the content of polymerized catechins is increased. It is better to use a higher one.
一般に、非重合のカテキンは苦渋味を有するため、その配合量が大きくなると、飲食品自体の呈味を損なうことがある。したがって、本発明の重合カテキンとしては、上記の茶葉抽出物から非重合のカテキンを選択的に除去する処理を行った溶媒抽出物を用いるのが好ましい。この非重合のカテキンを選択的に除去する処理を行った溶媒抽出物としては、ＷＯ２００５／０７７３８４号公報に記載の非重合カテキンの４倍以上の濃度で重合カテキンを含有するもの等が例示される。 In general, since non-polymerized catechins have a bitter and astringent taste, when the amount of the catechin is increased, the taste of the food and drink itself may be impaired. Therefore, as the polymerized catechin of the present invention, it is preferable to use a solvent extract that has been subjected to a treatment for selectively removing non-polymerized catechin from the tea leaf extract. Examples of the solvent extract subjected to the treatment for selectively removing non-polymerized catechins include those containing polymerized catechins at a concentration 4 times or more that of non-polymerized catechins described in WO2005 / 077384. .
本発明で用いる重合カテキンの形態は、液状でも、噴霧乾燥や凍結粉砕などにより粉末化されたものであってもよい。 The form of the polymerized catechin used in the present invention may be liquid or powdered by spray drying or freeze pulverization.
本発明の炭酸飲料における重合カテキンの配合割合は、飲料全体に対して０．００５重量％以上、好ましくは０．０１重量％以上、より好ましくは０．０２重量％以上である。重合カテキンの配合割合が０．００５重量％未満では、高甘味度甘味料の後味を改善する作用、炭酸飲料にボディ感を付与する作用や気泡感を改善する作用が十分に得られない。また、重合カテキンの添加量に応じて、高甘味度甘味料を含有する炭酸飲料の風味改善作用（後味改善、ボディ感付与、気泡感の向上）が得られる点から、重合カテキンの配合量の上限はないが、重合カテキンの配合量が０．０５重量％以上となると、重合カテキンのもつ苦味が炭酸飲料の刺激と相俟って、炭酸飲料の香味を低下させることもあることから、重合カテキンの実質的な上限は０．０５重量％未満であり、好ましくは０．０４５重量％、より好ましくは０．０４重量％である。 The blending ratio of the polymerized catechin in the carbonated beverage of the present invention is 0.005% by weight or more, preferably 0.01% by weight or more, more preferably 0.02% by weight or more based on the whole beverage. When the blending ratio of the polymerized catechin is less than 0.005% by weight, the effect of improving the aftertaste of the high-intensity sweetener, the effect of imparting a body feeling to the carbonated beverage, and the effect of improving the feeling of bubbles cannot be obtained sufficiently. In addition, depending on the amount of polymerized catechin added, the flavor-improving effect of carbonated beverages containing high-intensity sweeteners (improving aftertaste, imparting a body feeling, improving the feeling of bubbles) can be obtained. Although there is no upper limit, when the blending amount of the polymerized catechin is 0.05% by weight or more, the bitterness of the polymerized catechin may be combined with the stimulation of the carbonated beverage, which may reduce the flavor of the carbonated beverage. The substantial upper limit of catechin is less than 0.05% by weight, preferably 0.045% by weight, more preferably 0.04% by weight.
（カフェイン）
重合カテキンは、本発明の効果、すなわち後甘味を抑える作用、高甘味度甘味料特有の異味や苦味を低減する作用等の後味改善作用や、低カロリー（ノンカロリーを含む）飲料において、ボディ感（コク感（味の厚みともいう）、量感）を付与する作用や、炭酸飲料において気泡感を向上する作用を単独でも発揮する。本発明では、カフェインを併用することで、上記重合カテキンの作用を相乗的に高めたことを特徴とするものである。
(caffeine)
Polymerized catechins are effective for improving the aftertaste such as the effect of the present invention, that is, the effect of suppressing post-sweetness, the effect of reducing the off-taste and bitterness peculiar to high-intensity sweeteners, and the body feeling in low-calorie (including non-calorie) beverages. The effect of imparting (a rich feeling (also referred to as the thickness of taste) and a sense of volume) and the effect of improving the feeling of bubbles in carbonated beverages are also exhibited alone. In the present invention, the action of the polymerized catechin is synergistically enhanced by using caffeine together.
本発明で用いられるカフェイン(caffeine)としては、合成などによって得られる一水和物（Ｃ８Ｈ１０Ｎ４Ｏ２・Ｈ２Ｏ）もしくは無水物（無水カフェイン、Ｃ８Ｈ１０Ｎ４Ｏ２）の結晶物や、カフェインを含む植物抽出物をそのまま、もしくは濃縮又は精製したもの、すなわちカフェインを含む植物抽出物からカフェイン以外の成分を選択的に除去してカフェインの含有率を高めたものを用いることができる。カフェインを含む植物抽出物は、コーヒー豆、コーラの実、茶葉、カカオ等から水または熱水、メタノール、エタノール、イソプロパノール、酢酸エチルなどの溶媒で抽出することにより製造される。 As caffeine used in the present invention, monohydrate (C 8 H 10 N 4 O 2 .H 2 O) or anhydride (anhydrous caffeine, C 8 H 10 N 4 ) obtained by synthesis or the like is used. O 2 ) crystals or plant extracts containing caffeine as they are, or concentrated or purified, ie, components other than caffeine are selectively removed from plant extracts containing caffeine to contain caffeine What increased the rate can be used. A plant extract containing caffeine is produced by extraction from coffee beans, cola fruits, tea leaves, cacao, etc. with a solvent such as water or hot water, methanol, ethanol, isopropanol, and ethyl acetate.
本発明の炭酸飲料におけるカフェインの配合割合は、飲料全体に対して０．００５〜０．０３重量％、好ましくは０．００７５〜０．０２５重量％、より好ましくは０．０１〜０．０２重量％程度である。カフェインの配合割合が０．００５重量％未満であると、重合カテキンとの相乗的な作用が発揮されない。また、０．０３重量％を超えると、カフェインの苦味が炭酸飲料の刺激と相俟って、炭酸飲料の香味を低下させることがある。本発明者らは、重合カテキンにカフェインの苦味を抑制する作用を見出しているが、０．０３重量％を超える量の炭酸飲料中で強化されたカフェインの苦味に対しては、重合カテキンでその苦味を抑制できないことがある。 The blending ratio of caffeine in the carbonated beverage of the present invention is 0.005 to 0.03% by weight, preferably 0.0075 to 0.025% by weight, more preferably 0.01 to 0.02% with respect to the whole beverage. It is about wt%. When the blending ratio of caffeine is less than 0.005% by weight, a synergistic action with polymerized catechin is not exhibited. Moreover, when it exceeds 0.03 weight%, the bitter taste of caffeine may combine with the irritation | stimulation of carbonated beverages, and may reduce the flavor of carbonated beverages. The present inventors have found that polymerized catechin has an effect of suppressing the bitter taste of caffeine, but for the bitter taste of caffeine strengthened in carbonated beverages in an amount exceeding 0.03% by weight, polymerized catechin is used. The bitterness may not be suppressed.
重合カテキン（ｂ）の作用を相乗的に高めるカフェイン（ｃ）の配合割合［（ｃ）／（ｂ）］（重量比）は、０．１２５〜２．０程度であり、好ましくは０．１５〜１．０、より好ましくは０．２〜０．７５程度である。 The blending ratio [(c) / (b)] (weight ratio) of caffeine (c) that synergistically enhances the action of the polymerized catechin (b) is about 0.125 to 2.0, preferably 0. It is about 15 to 1.0, more preferably about 0.2 to 0.75.
（炭酸飲料）
本発明でいう「炭酸飲料」とは、甘味料の水溶液に、必要に応じて果汁、植物の抽出物、乳製品、フレーバー等を加え、炭酸ガスを圧入し容器に充填したものをいう。炭酸飲料は、適度な発泡による口腔内や喉への刺激感（口あたりや喉越し）が、飲用中及び飲用後の爽快感を醸成し、あっさりとした風味とさわやかな清涼感を創出するものであるが、高甘味度甘味料を使用して低カロリーの炭酸飲料とした場合には、その後味の悪さから清涼感が損なわれ、炭酸飲料としての美味しさを低下させる。しかし、本発明の重合カテキンとカフェインとを添加した炭酸飲料では、高甘味度甘味料の後味を改善する、すなわち後甘味を抑えて高甘味度甘味料特有の異味や苦味を低減して後味のキレを向上し、炭酸飲料にボディ感を付与するので、質の良い甘味料とされるショ糖を使用したときと同等の風味を有する低カロリー飲料となる。
(soda drink)
The term “carbonated beverage” as used in the present invention refers to a solution in which fruit juice, plant extract, dairy product, flavor, etc. are added to an aqueous solution of a sweetener as necessary, and carbon dioxide gas is injected into the container. Carbonated beverages create a refreshing flavor and a refreshing refreshing sensation in the mouth and throat (through the mouth and over the throat) due to moderate foaming, creating a refreshing feeling during and after drinking. However, when a high-calorie sweetener is used to produce a low-calorie carbonated drink, the refreshing feeling is lost due to the poor taste thereafter, and the taste as a carbonated drink is reduced. However, in the carbonated beverages to which the polymerized catechin and caffeine of the present invention are added, the aftertaste is improved by improving the aftertaste of the high-intensity sweetener, that is, suppressing the aftersweetness and reducing the peculiar taste and bitterness peculiar to the high-intensity sweetener. Since it improves the sharpness and gives the carbonated beverage a body feeling, it becomes a low calorie beverage having the same flavor as when sucrose, which is a good quality sweetener, is used.
ここで、低カロリー飲料とは、カロリーオフ（１００ｍＬ当たり２０ｋｃａｌ未満の飲料）やノンカロリー（１００ｍＬ当たり５ｋｃａｌ未満の飲料）などの飲料をいう。上記の高甘味度甘味料と重合カテキン及びカフェインとを含有する本発明の炭酸飲料は、このような低カロリー（ノンカロリーを含む）飲料、すなわち糖度の低い（Ｂｒｉｘ（％）０．０１〜１．０、好ましくは０．０５〜０．８程度）飲料にボディ感を付与することができることから、好ましい態様である。 Here, the low calorie beverage refers to beverages such as calorie off (beverage of less than 20 kcal per 100 mL) and non-calorie (beverage of less than 5 kcal per 100 mL). The carbonated beverage of the present invention containing the above-mentioned high-intensity sweetener, polymerized catechin and caffeine is a low-calorie (including non-calorie) beverage, that is, a low sugar content (Brix (%) 0.01 to 1.0, preferably about 0.05 to 0.8), which is a preferred embodiment because it can impart a body feeling to the beverage.
さらに、本発明の重合カテキンとカフェインとを添加した炭酸飲料では、気泡感及びフレーバーリリースが向上するという優れた効果も発揮する。本発明で炭酸飲料に関し「気泡」というときは、特別な場合を除き、飲料液中に発生している気泡を指す。容器内ガス圧が２．０〜５．０ｋｇ／ｃｍ２、好ましくは２．５〜４．５ｋｇ／ｃｍ２の範囲となるように炭酸ガスが圧入された、いわゆる高ガス圧炭酸飲料では、気泡による清涼感は感じさせるが、発生する気泡が粗くすぐに消失してしまい、高ガス圧炭酸飲料に求められる爽快な刺激という点で十分に満足できるものではなかった。また、ペットボトルやボトル缶のような再栓可能な蓋部を有する容器（単に、再栓可能な容器ともいう）に詰められた炭酸飲料では、開栓した直後に内容液（炭酸飲料）を飲みきらずに、蓋をして数時間後乃至数日後に再度飲用する場合があるが、一度開栓した炭酸飲料を時間が経過してから飲用すると、ガス圧の低下に伴い甘味と酸味のバランスが崩れて清涼感が低下する、気泡感が維持できずに炭酸飲料としての清涼感や刺激感が低下するという問題があり、特に高甘味度甘味料を用いた場合に気泡感が維持できないという問題があった。また、高ガス圧炭酸飲料では、高ガス圧で刺激味、炭酸味が強くなっているので、炭酸の刺激が突出しないように甘味料を増加した設計となっているものが多く（甘味度として、８〜１４度、好ましくは８〜１２度、より好ましくは９〜１１度程度）、開栓後のガス圧の低下により甘味が突出する、高甘味度甘味料特有の好ましくない風味が顕著になる、フレーバーリリースが悪くなる等の問題があった。しかし、本発明の重合カテキンとカフェインとを添加した炭酸飲料では、高ガス圧により発生する気泡が重合カテキンとカフェインによって相乗的にきめ細かくなり、気泡の持ちが維持されフレーバーリリースが向上するので、高ガス圧炭酸飲料に求められる清涼感や適度な刺激感を実現することができ、かつ、開栓してから時間経過後に再度飲用する形態である再栓可能な容器詰め炭酸飲料とした場合にも、開栓直後の風味や泡の性質を比較的維持できる、すなわち開栓直後のドリンカビリティを維持した炭酸飲料となる。 Furthermore, the carbonated beverage to which the polymerized catechin and caffeine of the present invention are added also exhibits an excellent effect of improving bubble feeling and flavor release. In the present invention, the term “bubbles” in relation to carbonated beverages refers to bubbles generated in the beverage liquid except in special cases. In a so-called high gas pressure carbonated beverage in which carbon dioxide gas is injected so that the gas pressure in the container is in the range of 2.0 to 5.0 kg / cm 2 , preferably 2.5 to 4.5 kg / cm 2 , However, the generated bubbles were coarse and immediately disappeared, which was not satisfactory in terms of the refreshing stimulation required for high gas pressure carbonated beverages. Also, in carbonated beverages packed in containers with recapable lids such as PET bottles and bottle cans (also simply referred to as recapable containers), the content liquid (carbonated beverages) is poured immediately after opening. It may be taken again after several hours to several days without covering it, but if you drink a carbonated beverage that has been opened once after a while, the balance between sweetness and sourness will accompany the decrease in gas pressure. The feeling of bubbling is reduced, the feeling of bubbles cannot be maintained, and the feeling of cooling and irritation as a carbonated beverage is reduced, especially when high-intensity sweeteners are used. There was a problem. In addition, high gas pressure carbonated beverages are often designed to increase the amount of sweeteners so that the stimulation of carbonic acid does not protrude, because the taste of sourness and sourness is strong at high gas pressure (as the sweetness level) 8 to 14 degrees, preferably 8 to 12 degrees, more preferably about 9 to 11 degrees), and the unpleasant flavor peculiar to high-intensity sweeteners, in which sweetness protrudes due to a decrease in gas pressure after opening, There was a problem that the flavor release became worse. However, in the carbonated beverages to which the polymerized catechin and caffeine of the present invention are added, the bubbles generated by the high gas pressure are synergistically finely divided by the polymerized catechin and caffeine, and the bubble holding is maintained and the flavor release is improved. When it is possible to realize the refreshing feeling and moderate irritation required for high gas pressure carbonated drinks, and when it is made into a refillable container-packed carbonated drink that is re-drinked after a lapse of time after opening. In addition, the flavor and foam properties immediately after opening can be maintained relatively, that is, the carbonated beverage maintains the drinkability immediately after opening.
なお、本発明で容器詰め炭酸飲料に関し、ガス圧をいうときは、特別な場合を除き、容器内におけるガス圧をいう。圧力の測定は、当業者にはよく知られており、具体的には、２０℃にした試料をガス内圧計に固定した後、一度ガス内圧計の活栓を開いてガスを抜き、再び活栓を閉じ、ガス内圧計を振り動かして指針が一定の位置に達したときの値を読み取ることにより行う。また、例えば京都電子工業(株)製 ガスボリューム測定装置 GVA-500A等を用いて測定する。 In addition, regarding the carbonated beverage packed in a container in the present invention, when referring to the gas pressure, it refers to the gas pressure in the container except in special cases. The measurement of pressure is well known to those skilled in the art. Specifically, after fixing a sample at 20 ° C. to a gas internal pressure gauge, once opening the stopcock of the gas internal pressure gauge, venting the gas, and then connecting the stopcock again Close and shake the gas pressure gauge to read the value when the pointer reaches a certain position. Further, for example, measurement is performed using a gas volume measuring device GVA-500A manufactured by Kyoto Electronics Industry Co., Ltd.
本発明の炭酸飲料は、上記成分（（ａ）高甘味度甘味料、（ｂ）重合カテキン、（ｃ）カフェイン）に加えて、（ｄ）フレーバーを添加して含有させると、その作用を存分に発揮させることができ、ボディ感が付与され、後味が改善され、炭酸の気泡感が向上され、かつフレーバーリリースに優れる、嗜好性の高い炭酸飲料となるので、本発明の炭酸飲料の好ましい態様の一つである。 In addition to the above components ((a) high-intensity sweetener, (b) polymerized catechin, (c) caffeine), the carbonated beverage of the present invention has its action when added with (d) flavor. The carbonated beverage of the present invention can be fully exerted, has a body feeling, improves the aftertaste, improves the feeling of carbonic acid bubbles, and is excellent in flavor release. This is one of the preferred embodiments.
上記（ａ）〜（ｄ）成分の他、通常炭酸飲料に配合される種々の成分、例えば酸味料、ｐＨ調整剤、果汁成分、酸化防止剤、保存料等を任意に添加することができる。本発明の炭酸飲料のｐＨは、通常、ｐＨ２．０〜４．５、好ましくはｐＨ２．５〜４．５程度である。 In addition to the components (a) to (d), various components that are usually blended in carbonated beverages, such as acidulants, pH adjusters, fruit juice components, antioxidants, preservatives, and the like can be optionally added. The pH of the carbonated beverage of the present invention is usually about pH 2.0 to 4.5, preferably about pH 2.5 to 4.5.
以下に、本発明を実施例により詳しく説明するが、本発明はこれらによって制限されるものではない。 EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited thereto.
＜製造例１ 重合カテキン高含有エキスの製造＞
温水（95℃）に0.15重量％の重曹を添加した7800kgの重曹液を用いて、600kgのウーロン茶葉に抽出処理を施し、ウーロン茶抽出液約7000kgを得た。この抽出液の液温を60-65℃に保持しながら、400kgの粒状活性炭（クラレ社製GW-H32/60）に通液して非重合カテキン、カフェインを除去した。この通過液（活性炭処理後の液）を減圧濃縮し、Brix11の重合カテキン高含有エキス（ウーロン茶抽出物の濃縮物；エキス）（以下、エキスＡ）約900kgを得た。得られたエキスＡ中の重合カテキン、非重合カテキン及びカフェイン濃度を、下記条件のHPLCで測定した。その結果、重量基準として重合カテキン12000ppm、非重合カテキン800ppm、カフェイン20ppmであった。
HPLC条件：
・カラム：ＴＳＫ-gel ＯＤＳ-80ＴｓＱＡ（4.6mmφx150ｍｍ、東ソー株式会社）
・移動相：
A：水：アセトニトリル：トリフルオロ酢酸＝900：100：0.5
B：水：アセトニトリル：トリフルオロ酢酸＝200：800：0.5
・流速：1.0ml/min
・カラム温度：40℃
・グラディエント条件：
分析開始から5分後まではＢ液0％、
5分から11分まででＢ液8％、
11分から21分まででＢ液10％、
21分から22分まででＢ液100％、
22分から30分まで100％保持、
30分から31分までで0％
・検出：A280nm
・標準物質：ウーロンホモビスフラバンB（ＯＨＢＦ−Ｂ）
・重合カテキンのリテンションタイム：約２５分のピークでテアフラビンとピークが一致する。
<Production Example 1 Production of Highly Polymerized Catechin Extract>
Using 7800 kg of baking soda solution in which 0.15% by weight of baking soda was added to warm water (95 ° C.), 600 kg of oolong tea leaves were subjected to extraction treatment to obtain about 7000 kg of oolong tea extract. While maintaining the liquid temperature of this extract at 60-65 ° C., it was passed through 400 kg of granular activated carbon (GW-H32 / 60 manufactured by Kuraray Co., Ltd.) to remove non-polymerized catechins and caffeine. The passing liquid (liquid after the activated carbon treatment) was concentrated under reduced pressure to obtain about 900 kg of Brix11 polymer catechin-rich extract (concentrate of oolong tea extract; extract) (hereinafter, extract A). Polymerized catechin, non-polymerized catechin and caffeine concentration in the obtained extract A were measured by HPLC under the following conditions. As a result, the weight basis was 12,000 ppm for polymerized catechin, 800 ppm for non-polymerized catechin, and 20 ppm for caffeine.
HPLC conditions:
Column: TSK-gel ODS-80TsQA (4.6mmφx150mm, Tosoh Corporation)
・ Mobile phase:
A: Water: Acetonitrile: Trifluoroacetic acid = 900: 100: 0.5
B: Water: Acetonitrile: Trifluoroacetic acid = 200: 800: 0.5
・ Flow rate: 1.0ml / min
・ Column temperature: 40 ℃
・ Gradient condition:
From 5 minutes after the start of analysis, B solution is 0%,
From 5 minutes to 11 minutes, B liquid 8%,
From 11 minutes to 21 minutes, B solution 10%,
From 21 minutes to 22 minutes, solution B is 100%,
100% hold from 22 to 30 minutes,
0% from 30 to 31 minutes
・ Detection: A280nm
Reference material: Oolong homobisflavan B (OHBF-B)
-Retention time of polymerized catechin: Theaflavin and peak coincide with each other at a peak of about 25 minutes.
＜製造例２ 重合カテキン（精製品）の製造）＞
温水（95℃）に0.15重量％の重曹を添加した重曹液を用いて、ウーロン茶葉に抽出処理を施し、ウーロン茶抽出液を得た。この抽出液を凍結乾燥し、8ｇを下記の分取クロマトグラムに供した。59.8-70分に溶出する成分をまとめて凍結乾燥を行い、これを重合カテキン（精製品）とした。
HPLC条件：
・カラム：ＯＤＳ-10/20（50*300 mm+50*100 mm、 野村化学(株)製）
・移動相：
A：水：アセトニトリル：トリフルオロ酢酸＝900：100：0.5
B：水：アセトニトリル：トリフルオロ酢酸＝200：800：0.5
・流速：60ml/min
・カラム温度：40℃
・グラディエント条件：
分析開始から52分後まではＢ液0％、
52分から52.1分まででＡ液100％、
52.1分から79分まででＡ液100％、
79分から81分まででＢ液100％、
81分から100分までＢ液100％保持
・検出：A280nm
・注入量：15ml
実施例１：後味改善作用
（１）重合カテキンの後味改善作用
ショ糖１重量％の甘味度を１としたときの甘味度５、１０に相当するアスパルテーム含有炭酸飲料を調製した。すなわち０．０２５重量％又は０．０５重量％のアスパルテームと、０．０４５重量％のクエン酸三ナトリウムと、０．０５５重量％の無水クエン酸と、８０重量％の炭酸水を混合し、全量が１００重量％となるように加水して、ｐＨ３．５のアスパルテーム含有炭酸飲料（ノンカロリー炭酸飲料）（Ｂｒｉｘ約０．１５）を調製した。これに、重合カテキンを重量基準として０〜２０００ｐｐｍ（０〜０．２重量％）となるように、製造例１で製造したエキスＡを添加した。対照として、エキスＡを添加していないものを用い、アスパルテーム特有の好ましくない後味（甘味及び苦味の後引き）について、どちらが官能的に好ましいかを専門パネラー５名で評価した。
<Production Example 2 Production of Polymerized Catechin (Fine Product)>
Oolong tea leaves were extracted using a baking soda solution obtained by adding 0.15% by weight of baking soda to warm water (95 ° C.) to obtain an oolong tea extract. This extract was freeze-dried and 8 g was subjected to the following preparative chromatogram. The components eluted at 59.8-70 minutes were combined and freeze-dried to obtain polymerized catechin (purified product).
HPLC conditions:
・ Column: ODS-10 / 20 (50 * 300 mm + 50 * 100 mm, manufactured by Nomura Chemical Co., Ltd.)
・ Mobile phase:
A: Water: Acetonitrile: Trifluoroacetic acid = 900: 100: 0.5
B: Water: Acetonitrile: Trifluoroacetic acid = 200: 800: 0.5
・ Flow rate: 60ml / min
・ Column temperature: 40 ℃
・ Gradient condition:
Until 52 minutes after the start of analysis, solution B is 0%,
Solution 52% from 52 minutes to 52.1 minutes,
Solution 5% from 52.1 to 79 minutes,
From 79 minutes to 81 minutes, 100% B liquid,
B liquid 100% retention and detection from 81 minutes to 100 minutes: A280nm
・ Injection volume: 15ml
Example 1: Aftertaste improving action (1) Aftertaste improving action of polymerized catechin Aspartame-containing carbonated beverages corresponding to a sweetness level of 5 and 10 when the sweetness level of 1% by weight of sucrose was taken as 1 were prepared. That is, 0.025 wt% or 0.05 wt% aspartame, 0.045 wt% trisodium citrate, 0.055 wt% anhydrous citric acid, and 80 wt% carbonated water are mixed, Aspartame-containing carbonated beverage (non-calorie carbonated beverage) (Brix about 0.15) having a pH of 3.5 was prepared. To this, the extract A produced in Production Example 1 was added so as to be 0 to 2000 ppm (0 to 0.2 wt%) based on the weight of the polymerized catechin. As a control, an extract to which no extract A was added was used, and five expert panelists evaluated which of the unfavorable afterpartition (sweetness and bitterness aftertaste) peculiar to aspartame was functionally preferable.
結果を表１に示す。表１は、エキスＡを添加した炭酸飲料の方が後味が良いと評価したパネラーの人数を示す。甘味度５及び１０のいずれの場合においても、重合カテキン１００〜１０００ｐｐｍ（０．０１〜０．１重量％）の添加で、後味の改善効果が確認された。重合カテキンを２０００ｐｐｍ（０．２重量％）添加した場合には、重合カテキンの呈味が炭酸の刺激と相俟って苦味となり、対照と比較して甘味が低下している、すなわち甘味度のピークの低下を引き起こしていると感じられた。 The results are shown in Table 1. Table 1 shows the number of panelists who evaluated that the aftertaste of the carbonated beverage to which the extract A was added was better. In both cases of sweetness levels 5 and 10, the effect of improving aftertaste was confirmed by the addition of polymerized catechin 100 to 1000 ppm (0.01 to 0.1 wt%). When 2000 ppm (0.2% by weight) of polymerized catechin was added, the taste of polymerized catechin became bitter in combination with the stimulation of carbonic acid, and the sweetness was lower than that of the control. It was felt that it was causing a drop in the peak.
（２）重合カテキン及びカフェインによる後味改善作用
上記（１）と同様にアスパルテーム及び重合カテキンを含有する炭酸飲料（甘味度１０）を調製し、さらにカフェイン（白鳥製薬株式会社、茶の素）を飲料全体に対して１００〜２００ｐｐｍ（０．０１〜０．０２重量％）の濃度となるように添加した（表２）。得られたアスパルテーム含有炭酸飲料について、カフェイン無添加を基準（対照）として、カフェインを添加することによる後味の改善作用について専門パネラー４名で評価した。評価は、対照２〜５とそれぞれ比較して、＋２点：格段に後味のキレがよく飲みやすい、＋１点：やや後味のキレが良い、０点：対照と変わらない、−１点：やや後味のキレが悪く飲みにくい、−２点：格段に後味のキレが悪く飲みにくい、という評価目安に基づいて、小数点以下の評価点（例えば＋０．５）も可能として行った。
(2) Aftertaste improving action by polymerized catechin and caffeine As in the above (1), a carbonated beverage (sweetness 10) containing aspartame and polymerized catechin was prepared, and caffeine (Shiratori Pharmaceutical Co., Ltd., Chanomoto) Was added so that it might become a density | concentration of 100-200 ppm (0.01-0.02 weight%) with respect to the whole drink (Table 2). The obtained aspartame-containing carbonated beverage was evaluated by 4 expert panelists on the aftertaste improving effect by adding caffeine, with no addition of caffeine as a reference (control). Evaluation is compared with each of Controls 2 to 5, +2 points: sharp aftertaste is easy to drink, +1 points: slightly good aftertaste, 0 points: not different from controls, -1 point: somewhat aftertaste Based on the evaluation standard that the sharpness of the film is poor and difficult to drink, -2 points: the sharpness of the aftertaste is very bad and difficult to drink, an evaluation score below the decimal point (for example, +0.5) was also made possible.
結果を表２〜５に示す。表２〜５は、パネラーの平均点を表す。カフェインを添加することで、重合カテキンの後味改善作用が増強されることが示唆された。後味改善作用がみられた重合カテキンが１００〜３００ｐｐｍの濃度では、カフェインの添加量は、１００ｐｐｍよりも１５０ｐｐｍが高いが、それ以上の濃度では顕著な増強はみられなかったことから、後味改善作用の観点ではカフェインの添加量の上限は２００ｐｐｍ程度であることが判明した。 The results are shown in Tables 2-5. Tables 2-5 represent the average points of the panelists. It was suggested that the aftertaste improving action of polymerized catechin is enhanced by adding caffeine. At a concentration of 100 to 300 ppm of polymerized catechins that showed an aftertaste improving effect, the amount of caffeine added was 150 ppm higher than 100 ppm, but no significant enhancement was observed at concentrations higher than that, thus improving aftertaste. From the viewpoint of action, it has been found that the upper limit of the amount of caffeine added is about 200 ppm.
実施例２：ボディ感増強作用（１）
重合カテキンとして製造例１で得たエキスＡを、カフェインとして市販のもの（白鳥製薬株式会社、茶の素）を用いた。
Example 2: Body feeling enhancing action (1)
As the polymerized catechin, the extract A obtained in Production Example 1 was used as a commercially available caffeine (Shiratori Pharmaceutical Co., Ltd., Chanomoto).
高甘味度甘味料として、アスパルテーム０．４ｇ、アセスルファムＫ０．１ｇを用い、クエン酸（無水）０．５５ｇ、クエン酸三ナトリウム０．５ｇと炭酸水８００ｇを混合し、０〜２００ｐｐｍ（０．０２重量％）となるカフェイン、及び／又は重合カテキンが０〜１０００ｐｐｍ（０．１重量％）となるエキスＡを混合した後、全量が１０００ｇとなるように適量の水を混合して、甘味度１０、Ｂｒｉｘ（％）約０．１６〜０．４７、ガス圧３．４ｋｇ／ｃｍ２の炭酸飲料（計２５種）を製造した。 Aspartame 0.4 g and acesulfame K 0.1 g were used as high-intensity sweeteners, 0.55 g of citric acid (anhydrous), 0.5 g of trisodium citrate and 800 g of carbonated water were mixed, and 0 to 200 ppm (0.02 Weight%) caffeine and / or an extract A in which the polymerized catechin is 0 to 1000 ppm (0.1 weight%), and then mixed with an appropriate amount of water so that the total amount becomes 1000 g. 10. Carbonated beverages (total 25 types) having a Brix (%) of about 0.16 to 0.47 and a gas pressure of 3.4 kg / cm 2 were produced.
得られた炭酸飲料について、飲料のボディ感を専門パネラー４名で評価した。評価は、表６に示すショ糖を配合して製造されるＢｒｉｘ（％）の異なる糖度（Ｂｒｉｘ（％）が約１，２，５，１０）の炭酸飲料（甘味度１０）のボディ感を、それぞれ１点（やや乏しい）、２点（やや感じる）、３点（感じる）、４点（大変感じる）として相対的に評価した。 About the obtained carbonated drink, the body feeling of the drink was evaluated by four special panelists. Evaluation is based on the body feeling of carbonated beverages (sweetness of 10) with different sugar levels (Brix (%) of about 1, 2, 5, 10) of Brix (%) manufactured by blending sucrose shown in Table 6. , Each was relatively evaluated as 1 point (slightly poor), 2 points (slightly feel), 3 points (feel), 4 points (feel very much).
表７に官能評価結果を示す（表中の値はパネラー４名の平均値を表す。尚、パネラーの評価は小数点以下の評価点も可能として行った。）。表４より明らかなとおり、重合カテキンの添加量が増加するに伴い、低Ｂｒｉｘの炭酸飲料にボディ感が付与され、重合カテキンを３００ｐｐｍ以上添加した場合には、Ｂｒｉｘ５又は１０と同程度のボディ感が得られた。一方、カフェインのみの添加はボディ感の付与に効果がみられなかったが、重合カテキンが１００ｐｐｍ以上存在する場合には、重合カテキンのボディ感付与効果を高める効果があり、特に重合カテキン２００ｐｐｍでカフェイン１００ｐｐｍ以上、重合カテキン３００ｐｐｍでカフェイン５０ｐｐｍ以上、重合カテキン４００ｐｐｍでカフェイン５０ｐｐｍ以上となる炭酸飲料は、ショ糖で調製したＢｒｉ１０の嗜好性の高い炭酸飲料とほぼ同等の量感を有していた。 The sensory evaluation results are shown in Table 7 (values in the table represent average values of 4 panelists. The panelists were evaluated with evaluation points below the decimal point also possible). As apparent from Table 4, as the added amount of the polymerized catechin increases, a body feeling is imparted to the low Brix carbonated beverage, and when the polymerized catechin is added in an amount of 300 ppm or more, a body feeling similar to Brix 5 or 10 is obtained. was gotten. On the other hand, the addition of caffeine alone was not effective in imparting body feeling, but when polymerized catechin is present in an amount of 100 ppm or more, it has the effect of enhancing the body feeling imparting effect of polymerized catechin. Carbonated beverages with 100 ppm or more of caffeine, 50 ppm or more of caffeine with 300 ppm of polymerized catechin, and 50 ppm or more of caffeine with 400 ppm of polymerized catechin have almost the same amount of taste as carbonated beverages with high taste of Bri10 prepared with sucrose. It was.
実施例３：ボディ感増強作用（２）
実施例２の重合カテキン高含有エキス（エキスＡ）を、製造例２で製造した重合カテキン（精製品）に変えること以外は、同様にして炭酸飲料を製造した。なお、重合カテキンの精製品はエタノール０．８重量％に溶解してから添加した。具体的には、重合カテキン及びカフェイン無添加（対照１）、重合カテキン２００ｐｐｍを添加（エキスＡとして添加；比較例２、精製品として添加；比較例２’）、重合カテキン３００ｐｐｍを添加（エキスＡとして添加；比較例４、精製品として添加；比較例４’）、カフェイン１５０ｐｐｍを添加（比較例５）、カフェイン１５０ｐｐｍ及び重合カテキン２００ｐｐｍを添加（エキスＡとして添加；本発明品２−２、精製品として添加；２’−２）、カフェイン１５０ｐｐｍ及び重合カテキン３００ｐｐｍを添加（エキスＡとして添加；本発明品４−２、精製品として添加；４−２’）の１０種の炭酸飲料（甘味度１０、Ｂｒｉｘ約０．１６〜０．４７、ガス圧３．４ｋｇ／ｃｍ２）を製造した。
Example 3: Body feeling enhancing action (2)
A carbonated beverage was produced in the same manner except that the highly polymerized catechin extract (Extract A) of Example 2 was changed to the polymerized catechin (refined product) produced in Production Example 2. The purified product of polymerized catechin was added after dissolving in 0.8% by weight of ethanol. Specifically, without addition of polymerized catechin and caffeine (control 1), 200 ppm of polymerized catechin was added (added as Extract A; Comparative Example 2, added as a purified product; Comparative Example 2 ′), and 300 ppm of polymerized catechin was added (extract Added as A; added as Comparative Example 4, purified product; added as Comparative Example 4 ′), 150 ppm of caffeine (Comparative Example 5), added 150 ppm of caffeine and 200 ppm of polymerized catechin (added as Extract A; product of the present invention 2- 2, added as a refined product; 2'-2), 150 ppm of caffeine and 300 ppm of polymerized catechin added (added as Extract A; product 4-2 of the present invention, added as a refined product; 4-2 ') A beverage (sweetness 10, Brix about 0.16 to 0.47, gas pressure 3.4 kg / cm 2 ) was produced.
得られた炭酸飲料について、実施例１と同様にボディ感を評価した。結果を表８に示す。精製品を用いてもほぼ同様の評価点が得られたことから、低Ｂｒｉｘ飲料のボディ感付与に有効な成分は、重合カテキン及びカフェインであることが示唆された。 About the obtained carbonated drink, the body feeling was evaluated similarly to Example 1. The results are shown in Table 8. Since almost the same evaluation score was obtained even when the purified product was used, it was suggested that the components effective for imparting a body feeling of the low Brix beverage were polymerized catechin and caffeine.
実施例４：気泡感の改善作用（１）
実施例２で製造した２５種の炭酸飲料の気泡感（炭酸飲料を口に含んだときに感じられる気泡のキメの細かさ（口当たりの良さ））について、専門パネラー４名で評価した。評価は、カフェイン及び重合カテキン無添加を基準（対照）として、実施例２の表６のＢｒｉｘ１０の炭酸飲料（ショ糖で製造された炭酸飲料）の気泡感を＋４点（対照と比較して格段に向上している）として、０点〜＋４点の５段階の評価目安に基づいて、小数点以下の評価点も可能として行った。
Example 4: Effect of improving bubble feeling (1)
The feeling of bubbles of the 25 types of carbonated beverages produced in Example 2 (the fineness of the texture of the bubbles felt when the carbonated beverages were included in the mouth (good mouth feel)) was evaluated by 4 specialist panelists. Evaluation is based on the addition of caffeine and polymerized catechin as a reference (control), and the bubble feeling of Brix 10 carbonated beverage (carbonated beverage produced with sucrose) in Table 6 of Example 2 is +4 points (compared to the control). As a result, the evaluation point below the decimal point was made possible based on the five-point evaluation standard of 0 to +4 points.
表９に結果を示す（表中の値は、パネラー４名の平均値を表す）。表９より明らかなとおり、重合カテキンの添加量が増加するに伴い、高甘味度甘味料を含有する炭酸飲料の気泡感が向上されたが、重合カテキンを４００ｐｐｍ添加してもショ糖で調製した炭酸飲料の気泡感は達成されなかった。一方、カフェインのみの添加は気泡感の向上に効果がみられなかったが、重合カテキンが１００ｐｐｍ以上存在する場合には、重合カテキンの気泡感の向上作用をカフェインが増強し、特に重合カテキン２００ｐｐｍでカフェイン１００ｐｐｍ以上、重合カテキン３００ｐｐｍでカフェイン５０ｐｐｍ以上、重合カテキン４００ｐｐｍでカフェイン５０ｐｐｍ以上となる炭酸飲料は、ショ糖で調製した嗜好性の高い炭酸飲料とほぼ同等の気泡感を有していた。 The results are shown in Table 9 (values in the table represent average values of 4 panelists). As is apparent from Table 9, as the amount of polymerized catechin added increased, the feeling of bubbles in carbonated beverages containing high-intensity sweeteners was improved, but even when 400 ppm of polymerized catechin was added, it was prepared with sucrose. The bubble feeling of the carbonated drink was not achieved. On the other hand, the addition of caffeine alone was not effective in improving the feeling of bubbles, but when polymerized catechins exist in an amount of 100 ppm or more, caffeine enhances the effect of improving the feeling of bubbles of polymerized catechins. Carbonated beverages with 200 ppm of caffeine at 100 ppm, polymerized catechin at 300 ppm and caffeine at 50 ppm and above, and polymerized catechin at 400 ppm with caffeine at 50 ppm and above have almost the same feeling of bubbles as carbonated beverages with high taste prepared with sucrose. It was.
実施例５：気泡感の改善作用（２）
実施例３の炭酸飲料について、実施例４と同様に気泡感を評価した。結果を表１０に示す。精製品を用いてもほぼ同様の評価点が得られたことから、高甘味度甘味料を含有する低Ｂｒｉｘの炭酸飲料の気泡感の改善に有効な成分は、重合カテキン及びカフェインであることが示唆された。
Example 5: Improvement of bubble feeling (2)
About the carbonated drink of Example 3, the bubble feeling was evaluated similarly to Example 4. The results are shown in Table 10. Since almost the same evaluation score was obtained using purified products, the ingredients effective in improving the bubble feeling of low Brix carbonated beverages containing high-intensity sweeteners are polymerized catechin and caffeine Was suggested.
実施例６：気泡感の改善作用（３）
実施例１および５で評価した炭酸飲料（カフェイン１５０ｐｐｍ・重合カテキン０ｐｐｍ：比較例５、カフェイン１５０ｐｐｍ・重合カテキン２００ｐｐｍ：本発明品２−２、カフェイン１５０ｐｐｍ、重合カテキン３００ｐｐｍ：本発明品４−２）３５０ｍｌずつを５００ｍＬ容ＰＥＴボトルに充填して詮をして冷蔵庫（５℃）で１週間した保存した後、再度、気泡感を評価した。結果を表１１に示す（表中の数値は、比較例５を基準（０点）とし、＋１点：やや気泡感がある、＋２点：大変気泡感がある、ことを示す）。重合カテキンが添加されていないカフェイン単独の炭酸飲料（比較例５）は、炭酸感が減少し気泡感があまり感じられないのに対し、重合カテキンを添加することで、炭酸感の強度と口中における気泡感の持続性が維持されていた（本発明品２−２、本発明品４−２）。また、重合カテキン量が増加することで、重合カテキンの炭酸感を維持する作用はさらに増強していた。重合カテキンとカフェインとを含有する炭酸飲料は、再栓して飲用する場合にも適度な炭酸感が感じられ、炭酸飲料に求められる爽快な清涼感や刺激感、気泡感が維持されることが示唆された。
Example 6: Effect of improving bubble feeling (3)
Carbonated beverages evaluated in Examples 1 and 5 (caffeine 150 ppm / polymerized catechin 0 ppm: comparative example 5, caffeine 150 ppm / polymerized catechin 200 ppm: present product 2-2, caffeine 150 ppm, polymerized catechin 300 ppm: present product 4 -2) After 350 ml each was filled into a 500 mL PET bottle and bottled and stored for 1 week in a refrigerator (5 ° C.), the feeling of bubbles was evaluated again. The results are shown in Table 11 (numerical values in the table indicate that Comparative Example 5 is used as a reference (0 point), +1 point: a slight bubble feeling, +2 point: a very bubble feeling). Caffeine-only carbonated beverages to which no polymerized catechin is added (Comparative Example 5), while the carbonic acid feeling decreases and the feeling of bubbles is not felt so much, by adding polymerized catechin, the strength of the carbonic acid feeling and the mouth The sustainability of the bubble feeling was maintained (Invention product 2-2, Invention product 4-2). Moreover, the effect | action which maintains the carbonic acid feeling of polymerized catechin was further strengthened by the amount of polymerized catechins increasing. Carbonated beverages containing polymerized catechins and caffeine should have a moderate carbonic feeling even when refilled and drink, maintaining the refreshing refreshing feeling, irritation, and feeling of bubbles required for carbonated drinks Was suggested.
比較例５の炭酸飲料は、炭酸ガスの抜けにより、甘味と酸味のバランスが崩れて甘味が強調された爽快感に欠けた飲料であったが、重合カテキンとカフェインとを含有する本発明品は、気泡感が維持されて適度な炭酸感を有し、甘味と酸味のバランスが崩れることなく、ドリンカビリティの維持された飲料であった。 The carbonated beverage of Comparative Example 5 was a beverage lacking a refreshing feeling in which the balance between sweetness and sourness was lost due to the loss of carbon dioxide gas and sweetness was emphasized, but the product of the present invention containing polymerized catechin and caffeine Was a beverage that maintained a feeling of bubbles and a moderate carbonic sensation, and maintained a drinkability without breaking the balance between sweetness and sourness.
Claims (6)
（ｂ）重合カテキン０．００５重量％以上０．０５重量％未満、および
（ｃ）カフェイン０．００５重量％以上０．０３重量％未満
を含有する、炭酸飲料。 (A) high intensity sweetener,
(B) A carbonated beverage containing 0.005% by weight or more and less than 0.05% by weight of polymerized catechin, and (c) 0.005% by weight or more and less than 0.03% by weight of caffeine.
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