JP2011019463A - Packaged beverage - Google Patents

Packaged beverage Download PDF

Info

Publication number
JP2011019463A
JP2011019463A JP2009168393A JP2009168393A JP2011019463A JP 2011019463 A JP2011019463 A JP 2011019463A JP 2009168393 A JP2009168393 A JP 2009168393A JP 2009168393 A JP2009168393 A JP 2009168393A JP 2011019463 A JP2011019463 A JP 2011019463A
Authority
JP
Japan
Prior art keywords
mass
polymer catechins
tartaric acid
packaged beverage
salt
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.)
Granted
Application number
JP2009168393A
Other languages
Japanese (ja)
Other versions
JP5550274B2 (en
Inventor
Hiroko Uchida
裕子 内田
Hiroshi Hashimoto
浩 橋本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kao Corp
Original Assignee
Kao Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kao Corp filed Critical Kao Corp
Priority to JP2009168393A priority Critical patent/JP5550274B2/en
Publication of JP2011019463A publication Critical patent/JP2011019463A/en
Application granted granted Critical
Publication of JP5550274B2 publication Critical patent/JP5550274B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Tea And Coffee (AREA)
  • Non-Alcoholic Beverages (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide easily drinkable packaged beverage improved in bitter taste and aftertaste derived from high concentration nonpolymerized catechins. <P>SOLUTION: The packaged beverage contains 0.51-5 mass% of nonpolymerized catechins (A), and 0.03-0.9 mass% of the total of tartaric acid (B) and its salt (C). <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、非重合体カテキン類を高濃度で含有する容器詰飲料に関する。   The present invention relates to a packaged beverage containing a high concentration of non-polymer catechins.

飲料に非重合体カテキン類を高濃度に配合する技術として、緑茶抽出物の濃縮物等の茶抽出物(特許文献1〜3)を利用し、非重合体カテキン類を飲料に溶解状態で添加する方法が知られている。   As a technology for blending non-polymer catechins in beverages at a high concentration, tea extracts (Patent Documents 1 to 3) such as concentrates of green tea extract are used, and non-polymer catechins are added to beverages in a dissolved state. How to do is known.

特開2002−142677号公報JP 2002-142777 A 特開平8−298930号公報JP-A-8-298930 特開平8−109178号公報JP-A-8-109178

しかしながら、飲料中に高濃度で非重合体カテキン類を含有させると、苦みが強烈で、しかも後味に不快な異味が口内に残りやすい。   However, when non-polymer catechins are contained in a beverage at a high concentration, the bitterness is intense and an unpleasant taste that is unpleasant to the aftertaste tends to remain in the mouth.

本発明者は、非重合体カテキン類を極めて高濃度で含有する容器詰飲料の呈味を改善すべく検討した結果、高濃度の非重合体カテキン類に、酒石酸(B)及びその塩(C)を一定量含有せしめたとき、高濃度非重合体カテキン類由来の苦味及び後味が改善されることを見出した。   The present inventor has studied to improve the taste of a packaged beverage containing non-polymer catechins at a very high concentration. As a result, tartaric acid (B) and its salt (C ) Was found to improve bitterness and aftertaste derived from high-concentration non-polymer catechins.

すなわち、本発明は、
非重合体カテキン類(A)を0.51〜5質量%、
酒石酸(B)及びその塩(C)を合計0.03〜0.9質量%
含有する、容器詰飲料を提供するものである。
That is, the present invention
0.51 to 5 mass% of non-polymer catechins (A),
Total tartaric acid (B) and its salt (C) 0.03-0.9 mass%
The container-packed drink which contains is provided.

また、本発明は、0.51〜5質量%の非重合体カテキン類(A)に、酒石酸(B)及びその塩(C)を合計0.03〜0.9質量%含有せしめる、高濃度非重合体カテキン類含有容器詰飲料の苦味及び後味の改善方法を提供することにある。   The present invention also provides a high concentration of 0.51 to 5% by mass of non-polymer catechins (A) containing tartaric acid (B) and its salt (C) in a total amount of 0.03 to 0.9% by mass. An object of the present invention is to provide a method for improving the bitterness and aftertaste of a non-polymer catechin-containing container-packed beverage.

本発明によれば、非重合体カテキン類を0.51〜5質量%という極めて高濃度で含有するにも拘わらず、高濃度非重合体カテキン類由来の苦味及び後味の改善された飲みやすい容器詰飲料が提供される。   ADVANTAGE OF THE INVENTION According to this invention, although it contains non-polymer catechins at the extremely high concentration of 0.51-5 mass%, the bitterness and the aftertaste derived from high concentration non-polymer catechins are easy to drink A stuffed beverage is provided.

先ず、本明細書で使用する用語について説明する。
「後味」とは、JIS Z 8144:2004に記載の「口内に残る感覚」をいう。
「非重合体カテキン類(A)」とは、カテキン、ガロカテキン、カテキンガレート及びガロカテキンガレート等の非エピ体カテキン類と、エピカテキン、エピガロカテキン、エピカテキンガレート及びエピガロカテキンガレート等のエピ体カテキン類を併せての総称であり、非重合体カテキン類の濃度は、上記8種の合計量に基づいて定義される。
First, terms used in this specification will be described.
“Aftertaste” refers to “feel remaining in the mouth” described in JIS Z 8144: 2004.
“Non-polymer catechins (A)” means non-epimeric catechins such as catechin, gallocatechin, catechin gallate, and gallocatechin gallate, and epicatechin, epigallocatechin, epicatechin gallate, and epigallocatechin gallate. The catechins are a collective term for the catechins, and the concentration of the non-polymer catechins is defined based on the total amount of the above eight types.

本発明の容器詰飲料は、従来に比して非重合体カテキン類を極めて高濃度で含有することを特徴とするものである。具体的には、本発明の容器詰飲料中の非重合体カテキン類(A)の含有量は0.51〜5質量%であるが、0.52〜4質量%、更に0.52〜3質量%、より更に0.54〜2質量%、特に0.56〜1質量%であることが好ましい。この範囲内で非重合体カテキン類(A)を含有すると、苦味と後味の不快な異味を改善することが可能であり、また非重合体カテキン類による生理効果を十分期待できる。   The container-packed beverage of the present invention is characterized by containing non-polymer catechins at an extremely high concentration as compared with the prior art. Specifically, the content of the non-polymer catechins (A) in the packaged beverage of the present invention is 0.51 to 5% by mass, but 0.52 to 4% by mass, and further 0.52 to 3%. It is preferably 0.5% by mass, more preferably 0.54 to 2% by mass, and particularly preferably 0.56 to 1% by mass. When the non-polymer catechins (A) are contained within this range, the unpleasant taste of bitterness and aftertaste can be improved, and the physiological effect of the non-polymer catechins can be sufficiently expected.

このような非重合体カテキン類を極めて高濃度で含有する容器詰飲料は、茶抽出物、その濃縮物及びそれらの精製物から選択される少なくとも1種を配合し、非重合体カテキン類濃度を調整して得ることができる。中でも、苦味及び後味の改善の観点から、茶抽出物の精製物を配合することが好ましい。茶抽出物の精製物としては、固形分中に非重合体カテキン類を40質量%以上、更に60質量%以上、より更に65質量%以上、特に70質量%以上含有するものが好ましい。なお、固形分中の非重合体カテキン類濃度の上限は、98質量%、更に95質量%、特に90質量%であることが好ましい。ここで、本明細書において「固形分」とは、茶抽出物の精製物を105℃の電気恒温乾燥機で3時間乾燥して揮発物質を除いた残分をいう。   A container-packed beverage containing such non-polymer catechins at an extremely high concentration is blended with at least one selected from a tea extract, a concentrate thereof, and a purified product thereof, and the non-polymer catechins concentration is adjusted. It can be obtained by adjusting. Especially, it is preferable to mix | blend the refined material of a tea extract from a viewpoint of improvement of a bitter taste and aftertaste. As the purified tea extract, those containing non-polymer catechins in a solid content of 40% by mass or more, more preferably 60% by mass or more, still more 65% by mass or more, and particularly preferably 70% by mass or more are preferable. The upper limit of the non-polymer catechin concentration in the solid content is preferably 98% by mass, more preferably 95% by mass, and particularly preferably 90% by mass. As used herein, “solid content” refers to a residue obtained by drying a purified product of tea extract for 3 hours with an electric constant temperature dryer at 105 ° C. to remove volatile substances.

茶抽出物とは、茶から熱水又は水溶性有機溶媒を用いてニーダー抽出やカラム抽出等により抽出したものであって、濃縮や精製操作が行われていないものをいう。また、抽出用水にあらかじめアスコルビン酸ナトリウムなどの有機酸又は有機酸塩類を添加してもよい。
抽出に使用する茶としては、例えば、Camellia属、例えば、C.var.sinensis(やぶきた種を含む)、C.var.assamica及びそれらの雑種から選択される茶樹が好適である。その加工方法により、不発酵茶、半発酵茶、発酵茶に大別することができる。不発酵茶としては、例えば、茎茶、棒茶、芽茶、煎茶、番茶、碾茶、釜入り茶等の緑茶が例示される。また、半発酵茶としては、例えば、鉄観音、色種、黄金桂、武夷岩茶等の烏龍茶が例示される。更に、発酵茶としては、ダージリン、アッサム、スリランカ等の紅茶が例示される。これらは単独で又は2種以上を組み合わせて用いることができる。中でも、非重合体カテキン類の含有量の点から、緑茶が好適である。
The tea extract is extracted from tea using hot water or a water-soluble organic solvent by kneader extraction, column extraction, or the like, and has not been concentrated or purified. Further, an organic acid such as sodium ascorbate or an organic acid salt may be added to the extraction water in advance.
As the tea used for the extraction, for example, a tea tree selected from the genus Camellia, for example, C. var. Sinensis (including Yabukita species), C. var. Assamica, and hybrids thereof is suitable. Depending on the processing method, it can be roughly classified into unfermented tea, semi-fermented tea, and fermented tea. Examples of non-fermented tea include green tea such as stalk tea, stick tea, bud tea, sencha, bancha, strawberry tea and kettle tea. Examples of the semi-fermented tea include oolong tea such as iron kannon, color type, golden katsura, and martial arts tea. Furthermore, examples of fermented tea include black teas such as Darjeeling, Assam, Sri Lanka and the like. These can be used alone or in combination of two or more. Among these, green tea is preferable from the viewpoint of the content of non-polymer catechins.

また、茶抽出物の濃縮物とは、茶から熱水又は水溶性有機溶媒により抽出した抽出液から溶媒を一部除去して非重合体カテキン類濃度を高めたものをいい、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号公報等に記載の方法により調製することができる。茶抽出物の濃縮物としては市販品を使用してもよく、例えば、三井農林(株)の「ポリフェノン」、伊藤園(株)の「テアフラン」、太陽化学(株)の「サンフェノン」等の緑茶抽出物の濃縮物が例示される。茶抽出物の濃縮物の形態としては、固体、水溶液、スラリー状等の種々のものが例示される。   The concentrate of tea extract refers to a product obtained by partially removing the solvent from the extract extracted from tea with hot water or a water-soluble organic solvent to increase the concentration of non-polymer catechins. It can be prepared by the methods described in JP-A-59-219384, JP-A-4-20589, JP-A-5-260907, JP-A-5-306279, and the like. Commercially available products may be used as the concentrate of the tea extract. For example, green tea such as “Polyphenone” from Mitsui Norin Co., Ltd., “Theafranc” from ITO EN, “Sunphenon” from Taiyo Kagaku Co., Ltd. An extract concentrate is illustrated. As a form of the concentrate of a tea extract, various things, such as solid, aqueous solution, and a slurry form, are illustrated.

茶抽出物の精製物は、例えば、下記(i)〜(iv)のいずれかの方法、あるいは2以上の組み合わせにより得ることができる。
(i)茶抽出物又はその濃縮物(以下、「茶抽出物等」という)を水、又は水と水溶性有機溶媒(例えば、エタノール)との混合物(以下、「有機溶媒水溶液」という)に懸濁して生じた沈殿を除去した後、溶媒を留去する方法。
(ii)茶抽出物等をタンナーゼ処理し、更に活性炭、酸性白土及び活性白土から選択される少なくとも1種の吸着剤と接触させる方法(例えば、特開2007−282568号公報)。
(iii)茶抽出物等を合成吸着剤に吸着させた後、該合成吸着剤に有機溶媒水溶液を接触させて非重合体カテキン類を脱離させる方法(例えば、特開2006−160656号公報)。
(iv)茶抽出物等を合成吸着剤に吸着させた後、該合成吸着剤に有機溶媒水溶液又は塩基性水溶液(例えば、水酸化ナトリウム水溶液)を接触させて非重合体カテキン類を脱離させ、次いで得られた脱離液を活性炭と接触させる方法(例えば、特開2008−079609号公報)。
なお、上記(iii)及び(iv)の方法においても、合成吸着剤に吸着すべき茶抽出物等として、タンナーゼ処理したものを使用してもよい。ここで、「タンナーゼ処理」とは、茶抽出物等を、タンナーゼ活性を有する酵素と接触させることをいい、例えば、特開2004−321105号公報に記載の方法を採用することができる。
The purified tea extract can be obtained, for example, by any of the following methods (i) to (iv), or by a combination of two or more.
(I) A tea extract or a concentrate thereof (hereinafter referred to as “tea extract or the like”) in water or a mixture of water and a water-soluble organic solvent (for example, ethanol) (hereinafter referred to as “organic solvent aqueous solution”). A method of removing the precipitate after suspending and then removing the solvent.
(Ii) A method in which a tea extract or the like is subjected to tannase treatment and further contacted with at least one adsorbent selected from activated carbon, acidic clay, and activated clay (for example, JP-A-2007-282568).
(Iii) A method in which a tea extract or the like is adsorbed on a synthetic adsorbent and then an organic solvent aqueous solution is brought into contact with the synthetic adsorbent to desorb non-polymer catechins (for example, JP-A-2006-160656) .
(Iv) After a tea extract or the like is adsorbed on a synthetic adsorbent, an organic solvent aqueous solution or a basic aqueous solution (for example, sodium hydroxide aqueous solution) is brought into contact with the synthetic adsorbent to desorb non-polymer catechins. Then, a method of bringing the obtained detachment solution into contact with activated carbon (for example, JP 2008-079609).
In the above methods (iii) and (iv), a tannase-treated tea extract or the like to be adsorbed on the synthetic adsorbent may be used. Here, “tannase treatment” refers to bringing a tea extract or the like into contact with an enzyme having tannase activity. For example, a method described in JP-A No. 2004-321105 can be employed.

本発明の容器詰飲料は、酸味料として酒石酸(B)及びその塩(C)を含有する。本発明の容器詰飲料中の酒石酸(B)及びその塩(C)の合計含有量は0.03〜0.9質量%であるが、苦味及び後味の改善の観点から、合計含有量の下限は0.05質量%、更に0.1質量%、より更に0.3質量%、特に0.4質量%であることが好ましく、他方上限は0.85質量%、0.8質量%、0.6質量%であることが好ましい。
本発明の容器詰飲料中に酒石酸及びその塩を上記範囲内で含有せしめることで、非重合体カテキン類由来の苦味及び後味の不快な異味を改善することができる。
The container-packed drink of this invention contains tartaric acid (B) and its salt (C) as a sour agent. The total content of tartaric acid (B) and its salt (C) in the packaged beverage of the present invention is 0.03 to 0.9% by mass, but from the viewpoint of improving bitterness and aftertaste, the lower limit of the total content Is preferably 0.05% by weight, more preferably 0.1% by weight, still more preferably 0.3% by weight, and particularly preferably 0.4% by weight, while the upper limit is 0.85% by weight, 0.8% by weight, 0%. It is preferably 6% by mass.
By including tartaric acid and its salt in the above-mentioned range in the packaged beverage of the present invention, the bitter taste derived from non-polymer catechins and the unpleasant taste of aftertaste can be improved.

酒石酸(B)及びその塩(C)は、単一の光学活性体でも、ラセミ体であってもよく、これらを適宜選択して使用することができる。
また、酒石酸の塩(C)としては、例えば、無機塩基との塩、有機塩基との塩が例示される。無機塩基との塩としては、例えば、アルカリ金属塩(例えば、ナトリウム塩、カリウム塩)、アンモニウム塩が例示される。有機塩基との塩としては、例えば、アミン塩(例えば、メチルアミン塩、ジエチルアミン塩、トリエチルアミン塩、エチレンジアミン塩)、アルカノールアミン塩(例えば、モノエタノールアミン塩、ジエタノールアミン塩、トリエタノールアミン塩)、アミノ酸塩(例えば、アルギニン塩、リジン塩)が例示される。中でも、アルカリ金属塩が好ましく、具体的には、酒石酸ナトリウム、酒石酸水素カリウム等が例示される。
The tartaric acid (B) and its salt (C) may be a single optically active substance or a racemic body, and these can be appropriately selected and used.
Examples of the tartaric acid salt (C) include salts with inorganic bases and salts with organic bases. Examples of the salt with an inorganic base include alkali metal salts (for example, sodium salts and potassium salts) and ammonium salts. Examples of salts with organic bases include amine salts (eg, methylamine salts, diethylamine salts, triethylamine salts, ethylenediamine salts), alkanolamine salts (eg, monoethanolamine salts, diethanolamine salts, triethanolamine salts), amino acids Examples of the salt include arginine salt and lysine salt. Among these, alkali metal salts are preferable, and specific examples include sodium tartrate and potassium hydrogen tartrate.

本発明の容器詰飲料中の酒石酸(B)と、酒石酸の塩(C)との含有質量比[(C)/(B)]は、苦味及び後味の改善の観点から、下限が1.1、更に1.3、より更に1.4、特に1.45であることが好ましく、他方上限が2.5、更に2、より更に1.85、特に1.8であることが好ましい。   The content mass ratio [(C) / (B)] of tartaric acid (B) and the tartaric acid salt (C) in the packaged beverage of the present invention has a lower limit of 1.1 from the viewpoint of improving bitterness and aftertaste. Further, it is preferably 1.3, more preferably 1.4, particularly 1.45, and the upper limit is preferably 2.5, further 2, still more 1.85, especially 1.8.

また、本発明の容器詰飲料中の非重合体カテキン類(A)と、酒石酸(B)及びその塩(C)との含有質量比{(A)/[(B)+(C)]}は、上記と同様の観点から、下限が1、更に1.05、より更に1.1、より更に1.15、特に1.2であることが好ましく、他方上限が20、更に10、より更に5、より更に3、より更に2、より更に1.85、特に1.8であることが好ましい。   Further, the mass ratio {(A) / [(B) + (C)]} of the non-polymer catechins (A), tartaric acid (B) and salts thereof (C) in the packaged beverage of the present invention. From the same viewpoint as above, the lower limit is preferably 1, more preferably 1.05, still more preferably 1.1, still more preferably 1.15, and particularly preferably 1.2, while the upper limit is 20, further 10, and even more 5, more preferably 3, still more 2, still more 1.85, especially 1.8.

本発明の容器詰飲料は、スクラロース(D)を含有することができる。スクラロースは、甘みの立ち上がりが速いだけでなく、その甘みが安定して持続するという味質を有する。そのため、非重合体カテキン類由来の苦味が立ち上がる前にスクラロースの甘みにより飲用初期の苦味を改善することができ、更に、酒石酸及びその塩により苦味及び後味の改善ができる。したがって、スクラロースと、酒石酸及びその塩により、非重合体カテキン類由来の苦味及び後味を確実に改善することができる。
本発明の容器詰飲料中のスクラロース(D)の含有量は、苦味及び後味の改善の観点から、0.001〜1質量%、更に0.003〜0.5質量%、より更に0.007〜0.1質量%、特に0.01〜0.05質量%であることが好ましい。
The packaged beverage of the present invention can contain sucralose (D). Sucralose has not only a quick start of sweetness but also a taste that allows the sweetness to remain stable. Therefore, before the bitterness derived from non-polymer catechins rises, the initial bitterness can be improved by the sweetness of sucralose, and the bitterness and aftertaste can be improved by tartaric acid and its salts. Therefore, the bitterness and aftertaste derived from non-polymer catechins can be reliably improved by sucralose, tartaric acid and salts thereof.
The content of sucralose (D) in the packaged beverage of the present invention is 0.001 to 1% by mass, further 0.003 to 0.5% by mass, and further 0.007 from the viewpoint of improving bitterness and aftertaste. It is preferable that it is -0.1 mass%, especially 0.01-0.05 mass%.

更に、本発明の容器詰飲料は、スクラロース(D)以外の甘味料を含有することができる。このような甘味料としては、例えば、炭水化物、グリセロール類、人工甘味料が例示され、これらは単独で又は2種以上を組み合わせて使用することができる。
炭水化物は、単糖、オリゴ糖、複合多糖、糖アルコール又はそれらの混合物を含むものである。単糖の例としては、グルコース、フルクトースがある。
オリゴ糖として、具体的には、二糖類としてスクロース、マルトース、ラクトース、セルビオース、トレハロース等が例示され、また三糖類としてラフィノース、パノース、メレジオース、ゲンチアノース等が例示される。このオリゴ糖の代表例はサトウキビ、サトウダイコンから得られるショ糖、テンサイ糖として知られるスクロースである。
糖アルコールとしては、エリスリトール、ソルビトール、キシリトール、マルチトール、ラクチトール、パラチノース、マンニトール、タガトース等が例示される。複合多糖として好ましい例はマルトデキストリンである。
また、グリセロール類としては、グリセロール等の多価アルコールが例示される。
更に、人工甘味料としては、例えば、サッカリン、シクラメート、アセスルフェーム−K、ネオテーム、L−アスパルチル−L−フェニルアラニン低級アルキルエステル、L−アスパルチル−D−アラニンアミド、L−アスパルチル−D−セリンアミド、L−アスパルチル−ヒドロキシメチルアルカンアミド、L−アスパルチル−1−ヒドロキシエチルアルカンアミド、グリチルリチン、合成アルコキシ芳香族化合物等が例示される。
なお、これら甘味料の含有量は、本発明の目的を阻害しない範囲内で適宜決定することができる。
Furthermore, the container-packed drink of this invention can contain sweeteners other than sucralose (D). Examples of such sweeteners include carbohydrates, glycerols, and artificial sweeteners, and these can be used alone or in combination of two or more.
Carbohydrates include monosaccharides, oligosaccharides, complex polysaccharides, sugar alcohols or mixtures thereof. Examples of monosaccharides are glucose and fructose.
Specific examples of oligosaccharides include sucrose, maltose, lactose, cellobiose, trehalose and the like as disaccharides, and raffinose, panose, meledioose, gentianose and the like as trisaccharides. Typical examples of the oligosaccharide are sucrose known as sugarcane and sugar beet sugar obtained from sugarcane and sugar beet.
Examples of the sugar alcohol include erythritol, sorbitol, xylitol, maltitol, lactitol, palatinose, mannitol, tagatose and the like. A preferred example of the complex polysaccharide is maltodextrin.
Examples of glycerols include polyhydric alcohols such as glycerol.
Furthermore, examples of the artificial sweetener include saccharin, cyclamate, acesulfame-K, neotame, L-aspartyl-L-phenylalanine lower alkyl ester, L-aspartyl-D-alanine amide, L-aspartyl-D-serine amide, Examples include L-aspartyl-hydroxymethylalkanamide, L-aspartyl-1-hydroxyethylalkanamide, glycyrrhizin, and synthetic alkoxy aromatic compounds.
In addition, content of these sweeteners can be suitably determined within the range which does not inhibit the object of the present invention.

更に、本発明の容器詰飲料には、所望により酸化防止剤、香料、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、ガム、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、品質安定剤等の添加剤を単独で又は2種以上組み合わせて配合してもよい。   Further, the container-packed beverage of the present invention may optionally contain antioxidants, fragrances, inorganic acids, inorganic acid salts, inorganic salts, pigments, emulsifiers, preservatives, seasonings, gums, oils, vitamins, amino acids, fruit juice extracts. , Vegetable extracts, nectar extracts, pH adjusters, quality stabilizers and the like may be added alone or in combination of two or more.

本発明の容器詰飲料のpH(25℃)は、呈味バランス及び非重合体カテキン類の安定性の点から、2〜7、更に2.5〜6、より更に3〜5、特に3〜4であることが好ましい。   The pH (25 ° C.) of the packaged beverage of the present invention is 2 to 7, more preferably 2.5 to 6, more preferably 3 to 5, especially 3 to 3 from the viewpoint of taste balance and stability of non-polymer catechins. 4 is preferred.

また、本発明の容器詰飲料は、茶系飲料とすることも、非茶系飲料とすることもできる。茶系飲料としては、例えば、緑茶飲料、烏龍茶飲料、紅茶飲料が例示される。非茶系飲料としては、例えば、エンハンスドウォーター、スポーツドリンク、ニアウォーター、栄養サポートドリンク等の機能性飲料が例示される。ここで、機能性飲料とは保健機能食品をいい、この保健機能食品には日本国が定める特定保健用食品及び栄養機能食品などが包含される。なお、飲料の形態は、流動性でも、半流動性であってもよい。   Moreover, the container-packed drink of this invention can be made into a tea-type drink, or can also be made into a non-tea-type drink. Examples of tea-based beverages include green tea beverages, oolong tea beverages, and black tea beverages. Examples of non-tea beverages include functional beverages such as enhanced water, sports drinks, near water, and nutrition support drinks. Here, the functional beverage refers to a health functional food, and this health functional food includes foods for specified health and nutritional functional foods defined by Japan. The beverage may be fluid or semi-fluid.

本発明の容器詰飲料に使用できる容器としては、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化した紙容器、瓶等の通常の包装容器が例示される。
また、本発明の容器詰飲料は、例えば、金属缶のような容器に充填後、加熱殺菌できる場合にあっては適用されるべき法規(日本にあっては食品衛生法)に定められた殺菌条件で製造できる。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など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できる。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。さらに、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を酸性に戻すなどの操作も可能である。
Examples of containers that can be used in the container-packed beverage of the present invention include molded containers (so-called PET bottles) mainly composed of polyethylene terephthalate, metal cans, paper containers combined with metal foil and plastic film, and normal packaging containers such as bottles. Is exemplified.
In addition, the container-packed beverage of the present invention can be sterilized as stipulated by laws and regulations (Food Sanitation Law in Japan) if it can be heat-sterilized after filling into a container such as a metal can. Can be manufactured under certain conditions. For PET bottles and paper containers that cannot be sterilized by retort, sterilize under the same conditions as above, for example, after sterilizing at high temperature and short time with a plate heat exchanger, etc. The method can be 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.

次に、本発明の容器詰飲料の苦味及び後味の改善方法について説明する。
本発明に係る苦味及び後味の改善方法は、0.51〜5質量%の非重合体カテキン類(A)に、酒石酸(B)及びその塩(C)を合計0.03〜0.9質量%含有せしめることを特徴とするものである。
本発明の容器詰飲料は、従来に比して極めて高濃度の非重合体カテキン類(A)を含有するため、一日に何回も非重合体カテキン類(A)を摂取することなく、例えば、容量が100mL程度の飲料の形態で非重合体カテキン類(A)を一度に多量に摂取することが可能になる。このように、手軽に飲用して非重合体カテキン類による生理効果を十分期待できる点で、高濃度非重合体カテキン類由来の苦味及び後味の改善技術は意義が高い。
Next, the improvement method of the bitterness and aftertaste of the container-packed drink of this invention is demonstrated.
In the method for improving bitterness and aftertaste according to the present invention, 0.51 to 5% by mass of non-polymer catechins (A) and tartaric acid (B) and a salt thereof (C) in total 0.03 to 0.9% by mass. % Content.
The container-packed beverage of the present invention contains an extremely high concentration of non-polymer catechins (A) as compared to the conventional one, so that without ingesting the non-polymer catechins (A) many times a day, For example, it becomes possible to take a large amount of non-polymer catechins (A) at a time in the form of a beverage having a capacity of about 100 mL. Thus, the technique for improving bitterness and aftertaste derived from high-concentration non-polymer catechins is highly significant in that it can be easily consumed and the physiological effect of non-polymer catechins can be sufficiently expected.

1.非重合体カテキン類の測定
試料溶液をフィルター(0.45μm)で濾過し、島津製作所製、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℃でグラジエント法により分析した。移動相A液は酢酸を0.1mol/L含有する蒸留水溶液、B液は酢酸を0.1mol/L含有する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。
1. Measurement of non-polymer catechins The sample solution was filtered with a filter (0.45 μm), and a high performance liquid chromatograph (model SCL-10AVP) manufactured by Shimadzu Corporation was used, and a packed column L-column TM for octadecyl group introduction liquid chromatograph was used. An ODS (4.6 mmφ × 250 mm: manufactured by the Chemical Substance Evaluation Research Organization) was attached and analyzed by a gradient method at a column temperature of 35 ° C. 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. .

2.官能試験
パネラー5名が各容器詰各飲料を試飲し、苦味及び後味について下記の基準により評価した。その後、協議により最終スコアを決定した。
2. Sensory test Five panelists sampled each container-packed beverage and evaluated the bitterness and aftertaste according to the following criteria. After that, the final score was determined by consultation.

(苦味の評価基準)
評点A:苦味が弱い。
B:苦味がやや弱い。
C:苦味がある。
D:苦味がやや強い。
E:苦味が強い。
(Evaluation criteria for bitterness)
Score A: The bitterness is weak.
B: The bitterness is slightly weak.
C: There is a bitter taste.
D: Slightly strong bitterness.
E: Strong bitterness.

(後味の評価基準)
評点A:後味に不快な異味がなく、スッキリしている。
B:後味に殆ど不快な異味がなく、スッキリしている。
C:後味に不快な異味がある。
D:後味に不快な異味がやや強く感じられる。
E:後味に不快な異味が強く感じられる。
(Evaluation criteria for aftertaste)
Score A: There is no unpleasant taste in the aftertaste, and it is refreshing.
B: There is almost no unpleasant taste in the aftertaste and it is refreshing.
C: The aftertaste has an unpleasant taste.
D: An unpleasant taste that feels uncomfortable is slightly strong.
E: Unpleasant nasty taste is strongly felt in the aftertaste.

製造例1
(1)緑茶抽出物(ポリフェノンHG、東京フードテクノ製)500gを水6500gに溶解し、「緑茶抽出液」7000g(pH5.6)を得た。この緑茶抽出液を温度25℃に保持し、タンナーゼ(キッコーマン社製タンナーゼKTFH、500U/g)を緑茶抽出液に対して700ppmとなる濃度で添加し、pHが4.24に低下した時点で酵素反応を終了した。その後、90℃に溶液を加熱して、2分間保持し酵素を失活させ、反応を止めた。次いで減圧濃縮にて55℃、2.7kpaでBrix濃度25%まで濃縮処理を行い、更に凍結乾燥して粉末状の「タンナーゼ活性を有する酵素で処理した緑茶抽出物」485g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31.8質量%、非重合体カテキンガレート体率44.4質量%であった。
(2)250r/min攪拌条件下の92質量%エタノール水溶液800g中に、(1)で得られたタンナーゼ活性を有する酵素で処理した緑茶抽出物200gを投入し、室温のまま約6時間の攪拌を続けた(pH5)。その後、生成している沈殿を2号ろ紙でろ別した。得られたろ液にイオン交換水を417g添加し、15℃、100r/min攪拌条件下で約5分間攪拌を行った。その混合溶液を小型冷却遠心分離機を用い(日立工機社製)、操作温度25℃で析出した濁り成分を遠心分離で分離した(6000rpm、5分)。分離した溶液にイオン交換水200gを添加して、40℃、2.7kpa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」を得た。緑茶抽出物の精製物は、非重合体カテキン類が15.0質量%、非重合体カテキン類中のガレート体率が44.4質量%、水分量が75.0質量%であった。
Production Example 1
(1) 500 g of green tea extract (polyphenone HG, manufactured by Tokyo Food Techno) was dissolved in 6500 g of water to obtain 7000 g of “green tea extract” (pH 5.6). This green tea extract is maintained at a temperature of 25 ° C., and tannase (Tannase KTFH, manufactured by Kikkoman Co., Ltd., 500 U / g) is added at a concentration of 700 ppm with respect to the green tea extract, and when the pH drops to 4.24 The reaction was terminated. Thereafter, the solution was heated to 90 ° C. and held for 2 minutes to deactivate the enzyme, thereby stopping the reaction. Next, concentration was performed under reduced pressure at 55 ° C. and 2.7 kpa to a Brix concentration of 25%, and lyophilized to obtain 485 g of a powdery “green tea extract treated with an enzyme having tannase activity”. The resulting green tea extract had a non-polymer catechin content of 31.8% by mass and a non-polymer catechin gallate content of 44.4% by mass.
(2) 200 g of the green tea extract treated with the enzyme having tannase activity obtained in (1) was put into 800 g of a 92 mass% ethanol aqueous solution under a stirring condition of 250 r / min and stirred for about 6 hours at room temperature. (PH 5). Thereafter, the produced precipitate was filtered off with No. 2 filter paper. To the obtained filtrate, 417 g of ion-exchanged water was added, and the mixture was stirred for about 5 minutes at 15 ° C. and 100 r / min. The mixed solution was separated by centrifugal separation (6000 rpm, 5 minutes) using a small cooling centrifuge (manufactured by Hitachi Koki Co., Ltd.) and turbid components precipitated at an operating temperature of 25 ° C. 200 g of ion-exchanged water was added to the separated solution, ethanol was distilled off at 40 ° C. and 2.7 kpa, and then the water content was adjusted to obtain a “purified green tea extract”. The purified product of the green tea extract had 15.0% by mass of non-polymer catechins, 44.4% by mass of gallate body in the non-polymer catechins, and 75.0% by mass of water.

実施例1
製造例1で得られた緑茶抽出物の精製物40gと、酒石酸2g、酒石酸3ナトリウム3gをイオン交換水に溶解した。次いで、これに果糖ぶどう糖液糖60g、スクラロース0.2g、酸化防止剤2.5g、香料1gを添加し、全量を1,000gとした。配合後、超高温短時間殺菌(UHT殺菌)しPETボトルに充填した。この容器詰飲料の非重合体カテキン類は0.6質量%であった。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 1
40 g of the purified green tea extract obtained in Production Example 1, 2 g of tartaric acid, and 3 g of trisodium tartrate were dissolved in ion-exchanged water. Next, 60 g of fructose-glucose liquid sugar, 0.2 g of sucralose, 2.5 g of antioxidant and 1 g of fragrance were added to make a total amount of 1,000 g. After blending, it was sterilized at ultra high temperature for a short time (UHT sterilization) and filled into a PET bottle. The non-polymer catechins in this packaged beverage were 0.6% by mass. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

実施例2
緑茶抽出物の精製物、酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 2
A packaged beverage was obtained in the same manner as in Example 1 except that the blended amounts of the purified green tea extract, tartaric acid, and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

実施例3
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 3
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

実施例4
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 4
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

実施例5
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 5
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

実施例6
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Example 6
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

比較例1
酒石酸及び酒石酸3ナトリウムを、表1に記載の配合割合のクエン酸及びクエン酸ナトリウムに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Comparative Example 1
A container-packed beverage was obtained in the same manner as in Example 1 except that tartaric acid and trisodium tartrate were changed to citric acid and sodium citrate in the mixing ratio shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

比較例2
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Comparative Example 2
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

比較例3
酒石酸、酒石酸3ナトリウムの配合量を表1に記載のものに変更したこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
比較例4
酒石酸及び酒石酸3ナトリウムを、表1に記載の配合割合のクエン酸及びクエン酸ナトリウムに変更し、酸化防止剤を使用しなかったこと以外は、実施例1と同様の操作により容器詰飲料を得た。この容器詰飲料の組成、成分分析及び官能試験の結果を表1に併せて示す。
Comparative Example 3
A packaged beverage was obtained by the same operation as in Example 1 except that the blending amounts of tartaric acid and trisodium tartrate were changed to those shown in Table 1. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.
Comparative Example 4
Tartaric acid and trisodium tartrate were changed to citric acid and sodium citrate in the blending ratios shown in Table 1, and a packaged beverage was obtained by the same operation as in Example 1 except that the antioxidant was not used. It was. Table 1 shows the composition, component analysis, and sensory test results of this packaged beverage.

Figure 2011019463
Figure 2011019463

表1から、極めて高濃度の非重合体カテキン類に、酒石酸及びその塩を一定の割合で含有せしめることで、高濃度非重合体カテキン類由来の苦味及び後味の改善された飲みやすい容器詰飲料が得られることが確認された。   From Table 1, by containing tartaric acid and its salt at a certain ratio in a very high concentration of non-polymer catechins, easy-to-drink beverages with improved bitterness and aftertaste derived from high-concentration non-polymer catechins. It was confirmed that

Claims (6)

非重合体カテキン類(A)を0.51〜5質量%、
酒石酸(B)及びその塩(C)を合計0.03〜0.9質量%
含有する、容器詰飲料。
0.51 to 5 mass% of non-polymer catechins (A),
Total tartaric acid (B) and its salt (C) 0.03-0.9 mass%
Contains, packaged beverages.
非重合体カテキン類(A)と、酒石酸(B)及びその塩(C)との含有質量比{(A)/[(B)+(C)]}が1〜20である、請求項1記載の容器詰飲料。   The content mass ratio {(A) / [(B) + (C)]} of the non-polymer catechins (A) and tartaric acid (B) and a salt thereof (C) is 1 to 20. The packaged beverage as described. 酒石酸の塩(C)と、酒石酸(B)との含有質量比[(C)/(B)]が1.1〜2.5である、請求項1又は2記載の容器詰飲料。   The container-packed drink of Claim 1 or 2 whose content mass ratio [(C) / (B)] of the salt (C) of tartaric acid and tartaric acid (B) is 1.1-2.5. スクラロース(D)を更に含有する、請求項1〜3のいずれか1項に記載の容器詰飲料。   The container-packed drink of any one of Claims 1-3 which further contains a sucralose (D). スクラロース(D)の含有量が0.001〜1質量%である、請求項1〜4のいずれか1項に記載の容器詰飲料。   The container-packed drink of any one of Claims 1-4 whose content of sucralose (D) is 0.001-1 mass%. 0.51〜5質量%の非重合体カテキン類(A)に、酒石酸(B)及びその塩(C)を合計0.03〜0.9質量%含有せしめる、高濃度非重合体カテキン類含有容器詰飲料の苦味及び後味の改善方法。   High concentration non-polymer catechins contained in a total of 0.03 to 0.9% by mass of tartaric acid (B) and its salt (C) in 0.51 to 5% by mass of non-polymer catechins (A) A method for improving the bitterness and aftertaste of a packaged beverage.
JP2009168393A 2009-07-17 2009-07-17 Container drink Active JP5550274B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2009168393A JP5550274B2 (en) 2009-07-17 2009-07-17 Container drink

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2009168393A JP5550274B2 (en) 2009-07-17 2009-07-17 Container drink

Publications (2)

Publication Number Publication Date
JP2011019463A true JP2011019463A (en) 2011-02-03
JP5550274B2 JP5550274B2 (en) 2014-07-16

Family

ID=43630111

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2009168393A Active JP5550274B2 (en) 2009-07-17 2009-07-17 Container drink

Country Status (1)

Country Link
JP (1) JP5550274B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021234281A1 (en) * 2020-05-18 2021-11-25 Black Idol Composition for enriching cosmetic and/or dermatological food products

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10262600A (en) * 1997-03-26 1998-10-06 Sanei Gen F F I Inc Masking of astringency
JPH10313819A (en) * 1997-05-14 1998-12-02 Sanei Gen F F I Inc Sweet food
JP2003333989A (en) * 2002-05-17 2003-11-25 Kao Corp Tea drink packed in container
JP2007143528A (en) * 2005-11-30 2007-06-14 Kao Corp Packaged drink
JP2008178401A (en) * 2006-12-27 2008-08-07 Kao Corp Packaged beverage
JP2008301808A (en) * 2007-05-08 2008-12-18 Kao Corp Concentrated composition for reduced drink
WO2009028211A1 (en) * 2007-08-30 2009-03-05 Kao Corporation Instant powder drink

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10262600A (en) * 1997-03-26 1998-10-06 Sanei Gen F F I Inc Masking of astringency
JPH10313819A (en) * 1997-05-14 1998-12-02 Sanei Gen F F I Inc Sweet food
JP2003333989A (en) * 2002-05-17 2003-11-25 Kao Corp Tea drink packed in container
JP2007143528A (en) * 2005-11-30 2007-06-14 Kao Corp Packaged drink
JP2008178401A (en) * 2006-12-27 2008-08-07 Kao Corp Packaged beverage
JP2008301808A (en) * 2007-05-08 2008-12-18 Kao Corp Concentrated composition for reduced drink
WO2009028211A1 (en) * 2007-08-30 2009-03-05 Kao Corporation Instant powder drink
JP2009072188A (en) * 2007-08-30 2009-04-09 Kao Corp Instant powder drink

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021234281A1 (en) * 2020-05-18 2021-11-25 Black Idol Composition for enriching cosmetic and/or dermatological food products

Also Published As

Publication number Publication date
JP5550274B2 (en) 2014-07-16

Similar Documents

Publication Publication Date Title
JP5399864B2 (en) Purified tea extract
JP4690877B2 (en) Containerized tea beverage
JP4884003B2 (en) Container oolong tea drink
KR101475758B1 (en) Method for production of tea extract
JP2007014283A (en) Packaged green tea beverage
JP2004041186A (en) Bottled black tea drink
JP2009247215A (en) Bottled drink
JP3590028B2 (en) Semi-fermented tea or fermented tea beverage with high catechin content
JP2006042728A (en) Amino acid-containing tea beverage
JP5336340B2 (en) Method for producing purified tea extract
JP4768534B2 (en) Containerized green tea beverage
JP5366784B2 (en) Container drink
JP3766660B2 (en) Production method of packaged beverages
JP4383337B2 (en) High concentration catechin-containing container-packed oolong tea drink
JP5366739B2 (en) Containerized acidic black tea beverage
JP3590032B2 (en) Manufacturing method of green tea polyphenol
JP5550274B2 (en) Container drink
JP3638560B2 (en) Production method of semi-fermented tea beverage and fermented tea beverage
JP3597834B2 (en) Packaged beverage
JP2005160394A (en) Packed tea beverage
JP4185406B2 (en) Containerized coffee beverages
JP4383329B2 (en) Containerized tea beverage
JP3569274B2 (en) Packaged beverage
JP5185780B2 (en) Purified tea extract
JP4119830B2 (en) Method for producing tea extract

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20120704

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20130611

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20130730

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20130909

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20140513

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20140520

R151 Written notification of patent or utility model registration

Ref document number: 5550274

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R151

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

S111 Request for change of ownership or part of ownership

Free format text: JAPANESE INTERMEDIATE CODE: R313113

R350 Written notification of registration of transfer

Free format text: JAPANESE INTERMEDIATE CODE: R350