JP2000279705A - Method for extraction of polyphenol component - Google Patents

Method for extraction of polyphenol component

Info

Publication number
JP2000279705A
JP2000279705A JP11090896A JP9089699A JP2000279705A JP 2000279705 A JP2000279705 A JP 2000279705A JP 11090896 A JP11090896 A JP 11090896A JP 9089699 A JP9089699 A JP 9089699A JP 2000279705 A JP2000279705 A JP 2000279705A
Authority
JP
Japan
Prior art keywords
ethyl alcohol
seeds
polyphenol
polyphenols
extract
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.)
Pending
Application number
JP11090896A
Other languages
Japanese (ja)
Inventor
Wataru Nosaka
亙 野坂
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.)
SHONAN KORYO KK
Shonan Koryo Corp
Original Assignee
SHONAN KORYO KK
Shonan Koryo 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 SHONAN KORYO KK, Shonan Koryo Corp filed Critical SHONAN KORYO KK
Priority to JP11090896A priority Critical patent/JP2000279705A/en
Publication of JP2000279705A publication Critical patent/JP2000279705A/en
Pending legal-status Critical Current

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  • Non-Alcoholic Beverages (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

PROBLEM TO BE SOLVED: To produce polyphenols with suppressed bitterness and to increase the content of polyphenols in foods without accompanying bitterness by adding an ethyl alcohol aq. soln or the like to residues of squeezed grapes or the like, extracting polyphenols with liquefied carbonic acid gas, and freezing the extract to separate the water phase. SOLUTION: When a polyphenol component is to be extracted, first, an ethyl alcohol aq. soln. or water is added by 1 to 10 pts.wt. to 10 pts.wt. of the residue of grapes after squeezed or to seeds. Then the residue or seeds are subjected to extraction by using liquefied carbonic acid gas. The extract is frozen to separate the water phase containing the polyphenol component. The proportion of ethyl alcohol in the ethyl alcohol aq. soln. to be added is <=95 vol.%. The extraction is carried out by using a liquefied carbonic acid gas extracting machine equipped with a cooling portion and a heating portion and by the method of internally circulating the liquefied carbonic acid gas. Thereby, polyphenols with suppressed bitterness can be produced and the amt. of polyphenols to be added to foods can be increased.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、ブドウ果実の搾汁
粕または種子からポリフェノール成分を抽出する方法に
関するものであり、抽出成分は食品のポリフェノール強
化等に利用される。現在、ポリフェノールは食品に抗酸
化性等の機能を賦与または強化するために添加されて用
いられている。たとえば、ポリフェノールを増量したワ
イン、チョコレート等として商品化されている。さら
に、薬効が認められる種類のポリフェノールについて
は、健康食品に組み込んだり、精製して医薬として使用
することができるのは当業者に自明のことである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for extracting a polyphenol component from squeezed cake or seeds of grape fruit, and the extracted component is used for, for example, enriching a food with polyphenol. At present, polyphenols are used in foods to add or enhance functions such as antioxidant properties. For example, it has been commercialized as wine, chocolate or the like containing an increased amount of polyphenol. Further, it is obvious to those skilled in the art that polyphenols of a type having medicinal effects can be incorporated into health foods or purified and used as medicines.

【0002】[0002]

【従来の技術】ブドウ果実の搾汁粕または種子からポリ
フェノールを抽出する方法として、水、エチルアルコー
ル等による溶媒抽出が知られている。しかし、これらの
抽出法により得られるポリフェノール成分は苦み等の呈
味として望ましくない成分を含んでいるため、たとえ
ば、飲料に添加した場合に飲料本来の味を損なう欠点が
あった。
2. Description of the Related Art As a method for extracting polyphenols from squeezed cake or seeds of grape fruits, solvent extraction with water, ethyl alcohol or the like is known. However, since the polyphenol components obtained by these extraction methods contain components that are undesirable as a taste such as bitterness, for example, when added to a beverage, there is a drawback that the original taste of the beverage is impaired.

【0003】[0003]

【発明が解決しようとする課題】本発明者は、呈味上好
ましくない成分を押さえてポリフェノール成分を抽出す
ることを目的とし、液化炭酸ガスを用いて抽出を行うこ
とにより苦みを抑えたポリフェノール含有液を製造する
方法を提供する。
SUMMARY OF THE INVENTION An object of the present invention is to extract a polyphenol component by suppressing a component that is not preferable in taste, and to extract a polyphenol component by using liquefied carbon dioxide gas to reduce bitterness. A method for producing a liquid is provided.

【0004】[0004]

【課題を解決するための手段】本発明は、ブドウ果実の
搾汁粕または種子にエチルアルコール水溶液または水を
添加した後、液化炭酸ガスを用いて抽出を行うことによ
り、ポリフェノール成分を取得するものである。即ち、
本発明はポリフェノール成分を抽出するに際し、ブドウ
果実の搾汁粕または種子10重量部に対してエチルアル
コール水溶液または水を1〜10重量部の割合で添加し
た後、液化炭酸ガスを用いて搾汁粕または種子の抽出を
行い、次いで抽出物を凍結して前記成分を含有する水相
を分離することを特徴とする。本発明で得られるポリフ
ェノール成分は、油相分離により、主として水溶性であ
り、ポリフェノールを含む水相(以下、ポリフェノール
エキスという)は苦みが抑えられている。
SUMMARY OF THE INVENTION The present invention provides a method for obtaining a polyphenol component by adding an aqueous solution of ethyl alcohol or water to squeezed cake or seeds of grape fruit and extracting the mixture with liquefied carbon dioxide gas. It is. That is,
In the present invention, when extracting a polyphenol component, an aqueous solution of ethyl alcohol or water is added at a ratio of 1 to 10 parts by weight to 10 parts by weight of squeezed cake or seeds of grape fruit, and then squeezed using liquefied carbon dioxide gas. It is characterized in that extraction of cake or seeds is performed, and then the extract is frozen to separate an aqueous phase containing the above components. The polyphenol component obtained in the present invention is mainly water-soluble due to oil phase separation, and the bitterness of an aqueous phase containing polyphenol (hereinafter referred to as polyphenol extract) is suppressed.

【0005】[0005]

【発明の実施の形態】本発明に用いられるブドウ果実の
搾汁粕または種子とは、ブドウ果汁製造またはワイン製
造等において副産物として得られる搾汁粕または種子を
指す。搾汁粕には果皮と種子が含まれるが、種子は搾汁
粕から篩い分け等の方法により分離することができる。
ブドウの種類は特に問わず、一般に栽培されている品種
でよく、たとえば、キャンベル・アーリー、コンコー
ド、マスカット・ベリーAを用いることができる。ただ
し、果実は有核であることが望ましい。搾汁粕、種子
は、必要により破砕する。種子の破砕の場合、たとえ
ば、8.6メッシュ(2mm)以下の粒度を主体とする程度ま
で破砕するのが適当である。上記搾汁粕または種子10重
量部に対してエチルアルコール水溶液または水を1〜10
重量部の割合で添加して液化炭酸ガスによる抽出を行
う。添加するエチルアルコール水溶液中のエチルアルコ
ール含量は95容量%以下である。95容量%を超えると水
溶性成分の分離が困難となる。
BEST MODE FOR CARRYING OUT THE INVENTION The juice lees or seeds of grape fruit used in the present invention refers to the juice lees or seeds obtained as a by-product in the production of grape juice or wine. Juice cake includes pericarp and seeds, and the seeds can be separated from the juice cake by a method such as sieving.
The type of grapes is not particularly limited, and generally cultivars may be used. For example, Campbell Early, Concord, and Muscat Berry A can be used. However, it is desirable that the fruit be nucleated. Juice cake and seeds are crushed as necessary. In the case of crushing seeds, for example, it is appropriate to crush the seeds to a degree mainly having a particle size of 8.6 mesh (2 mm) or less. Ethyl alcohol aqueous solution or water is 1 to 10 parts by weight of the above juice residue or seeds by 10
Extraction with liquefied carbon dioxide gas is performed by adding in parts by weight. The ethyl alcohol content in the added ethyl alcohol aqueous solution is 95% by volume or less. If it exceeds 95% by volume, it becomes difficult to separate water-soluble components.

【0006】抽出は、冷却部と加温部を設けた液化炭酸
ガス抽出機により、液化炭酸ガスを内部循環させる方式
により行う。冷却部の温度は、例えば、5〜15℃である
ことができ、加温部の温度は、例えば、40〜60℃である
ことができる。数時間から30時間、好ましくは、6〜20
時間の抽出を行った後、抽出機から抽出物を取り出し、
凍結により目的のポリフェノール成分を分離取得する。
このようにして得られたポリフェノール成分は、食品の
添加物として利用することができ、食品のポリフェノー
ル強化を行うことができる。例えば、本発明のポリフェ
ノールエキスは精製することなくブドウ飲料にそのまま
添加することができ、苦みが抑えられているので、飲料
本来の味を損なうことがない。また、本発明のポリフェ
ノールエキスは、精製により薬効成分を分離または単離
すれば、医薬としての用途が期待できる。
[0006] The extraction is performed by a system in which the liquefied carbon dioxide gas is internally circulated by a liquefied carbon dioxide gas extractor provided with a cooling unit and a heating unit. The temperature of the cooling unit can be, for example, 5 to 15 ° C, and the temperature of the heating unit can be, for example, 40 to 60 ° C. Several hours to 30 hours, preferably 6-20
After performing the time extraction, remove the extract from the extractor,
The desired polyphenol component is separated and obtained by freezing.
The polyphenol component thus obtained can be used as an additive for food, and can enhance the polyphenol of food. For example, the polyphenol extract of the present invention can be directly added to a grape beverage without purification and bitterness is suppressed, so that the original taste of the beverage is not impaired. In addition, the polyphenol extract of the present invention can be expected to be used as a medicine if the medicinal component is separated or isolated by purification.

【0007】[0007]

【実施例】以下、実施例により、本発明をさらに詳細に
説明するが、本発明はこれら実施例に限定されるもので
はない。実施例1 キャンベル(ブドウの品種名)の果実を搾汁した粕か
ら、水洗により種子をより分け、この種子を破砕した。
破砕品の粒度は8.6メッシュパスが82%を占めた。この
破砕品300gに71容量%エチルアルコール水溶液180gを
添加してよくなじませて、室温で1時間放置した。その
後、2.3リットル容積の炭酸ガス抽出機に充填し、2.7kg
の液化炭酸による抽出を17時間行った。炭酸ガスを放出
した後に抽出物を取り出し、凍結により水相150.9g、油
相8.8gを得た。この水相中のポリフェノール量をFolin-
Denis法(METHODS OF ANALYSIS−A.O.A.C.-Twelfth Edi
tion 1975)に準じてタンニン酸として測定した値は、
1.28w/w%であり、水相のポリフェノール全量はタン
二ン酸として1.93gであった。原料に対して0.64%であ
った。
The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples. Example 1 Seeds were separated from the cake obtained by squeezing the fruits of Campbell (grape varieties) by washing with water, and the seeds were crushed.
The 8.6 mesh pass accounted for 82% of the size of the crushed product. 180 g of a 71% by volume aqueous solution of ethyl alcohol was added to 300 g of the crushed product to mix well, and left at room temperature for 1 hour. After that, it was charged into a 2.3 liter carbon dioxide gas extractor and 2.7 kg
Was extracted with liquefied carbonic acid for 17 hours. After releasing carbon dioxide gas, the extract was taken out, and 150.9 g of an aqueous phase and 8.8 g of an oil phase were obtained by freezing. The amount of polyphenols in this aqueous phase was determined by Folin-
Denis method (METHODS OF ANALYSIS-AOAC-Twelfth Edi
1975), the value measured as tannic acid is
It was 1.28 w / w%, and the total amount of polyphenols in the aqueous phase was 1.93 g as tandinoic acid. It was 0.64% based on the raw material.

【0008】実施例2 実施例1と同様に、キャンベル果実の種子の破砕品300
gに48容量%エチルアルコール水溶液180gを添加して
室温で1時間放置し、同様の液化炭酸抽出を行い、抽出
物を凍結分離して水相106.5g、油相10.0gを得た。こ
の水相中のポリフェノール全量を同様にタンニン酸とし
て測定した値0.96%w/wであり、水相のポリフェノー
ル全量は1.02gであった。原料に対して0.34%であっ
た。実施例3 実施例1と同様に、キャンベル果実の種子の破砕品300
gに79容量%エチルアルコール水溶液180gを添加して
室温で1時間放置し、同様の液化炭酸抽出を行い、抽出
物を凍結分離して水相141.4g、油相36.7gを得た。こ
の水相中のポリフェノール量を同様にタンニン酸として
測定した値は0.90w/w%であり、水相のポリフェノー
ル全量は1.27gであった。原料に対して0.42%であっ
た。
Example 2 As in Example 1, crushed Campbell fruit seeds 300
180 g of a 48% by volume ethyl alcohol aqueous solution was added to the resulting mixture, and the mixture was allowed to stand at room temperature for 1 hour. The same liquefied carbonic acid extraction was performed, and the extract was separated by freezing to obtain 106.5 g of an aqueous phase and 10.0 g of an oil phase. The total amount of polyphenols in this aqueous phase was 0.96% w / w, also measured as tannic acid, and the total amount of polyphenols in the aqueous phase was 1.02 g. It was 0.34% based on the raw material. Example 3 As in Example 1, a crushed product of Campbell fruit seed 300
180 g of a 79% by volume ethyl alcohol aqueous solution was added to the resulting mixture, and the mixture was allowed to stand at room temperature for 1 hour. The same liquefied carbonic acid extraction was performed, and the extract was separated by freezing to obtain 141.4 g of an aqueous phase and 36.7 g of an oil phase. The value of the amount of polyphenol in this aqueous phase also measured as tannic acid was 0.90 w / w%, and the total amount of polyphenol in the aqueous phase was 1.27 g. It was 0.42% based on the raw material.

【0009】比較例1 キャンベル果実の種子の破砕品100gを破砕せずに、70
℃の温水1kgで10分毎に攪拌しながら1時間抽出を行っ
た後、セライト濾過し、抽出液942gを得た。この抽出液
中のポリフェノール量を同様にタンニン酸として測定し
た値は0.10w/w%であり、抽出液のポリフェノール全
量は0.94gであった。原料に対して0.94%であった。比較例2 キャンベル果実の種子の破砕品100gを破砕し、70℃の
温水1kgで10分毎に攪拌しながら1時間抽出を行った
後、セライト濾過し、抽出液830gを得た。この抽出液中
のポリフェノール量を同様にタンニン酸として測定した
値は0.17w/w%であり、抽出液のポリフェノール全量
は1.41gであった。原料に対して1.41%であった。
COMPARATIVE EXAMPLE 1 100 g of crushed Campbell fruit seeds were obtained without crushing.
Extraction was performed for 1 hour while stirring with 1 kg of warm water at 10 ° C. every 10 minutes, followed by celite filtration to obtain 942 g of an extract. The value of the amount of polyphenol in this extract also measured as tannic acid was 0.10 w / w%, and the total amount of polyphenol in the extract was 0.94 g. It was 0.94% based on the raw material. Comparative Example 2 100 g of crushed Campbell fruit seeds were crushed and extracted with 1 kg of 70 ° C. hot water while stirring every 10 minutes for 1 hour, followed by celite filtration to obtain 830 g of extract. The value of the amount of polyphenol in this extract similarly measured as tannic acid was 0.17 w / w%, and the total amount of polyphenol in the extract was 1.41 g. It was 1.41% based on the raw material.

【0010】比較試験 ポリフェノール試料として、本発明にかかる実施例1の
水相、比較例1及び比較例2の抽出液、並びに市販品の
ブドウ種子エキス(キッコーマン株式会社製、粉体品)
を微炭酸のグレープ飲料(200g)に、50mg量のポリフ
ェノール(タンニン酸相当値)を強化すべく添加して、
配合1〜5を成し、冷蔵5日後に呈味を比較した。な
お、上記市販品のポリフェノール量はタンニン酸として
の測定値が39.0w/w%であった。 グレープ飲料の基本配合: コンコード濃縮果汁(68BX)10.0g グラニュー糖 15.8g クエン酸 0.2g 水 74.0g 炭酸 50.0g ポリフェノール試料(表1) 50.0g ――――――――――――――――――― 合計 200.0g
Comparative Tests As a polyphenol sample, the aqueous phase of Example 1 according to the present invention, the extracts of Comparative Examples 1 and 2, and a commercially available grape seed extract (powder made by Kikkoman Corporation)
To a slightly carbonated grape drink (200 g), to add 50 mg of polyphenol (equivalent to tannic acid),
Formulations 1 to 5 were made and the taste was compared 5 days after refrigeration. In addition, the measured value as a tannic acid was 39.0 w / w% about the polyphenol content of the said commercial item. Basic composition of grape drink: Concord concentrated fruit juice (68BX) 10.0g Granulated sugar 15.8g Citric acid 0.2g Water 74.0g Carbonic acid 50.0g Polyphenol sample (Table 1) 50.0g ―――――――――――――― ――――― Total 200.0g

【0011】[0011]

【表1】 *抽出物の添加量は、それぞれタンニン酸として50mg添加に相当する。[Table 1] * The amount of the extract added corresponds to the addition of 50 mg as tannic acid.

【0012】[0012]

【表2】 [Table 2]

【0013】実施例1添加品(配合−2)は、苦みをほ
とんど感じることなく、200g飲料にポリフェノールを5
0mg強化することができた。これに比べて、一般的製法
により得られた比較例1及び2を添加した飲料(配合−
3及び4)には、苦みが感じられた。市販品添加飲料
(配合−5)については強い苦みが感じられた。原料の
種子を破砕して抽出した場合、比較例2添加品(配合−
4)のように白濁を起こすことが一般的であるが、本発
明にかかる実施例1添加品(配合−2)では白濁を生じ
ないことも優れた特徴である。これは、液化炭酸ガス抽
出品から凍結分離で容易に油相を分離できるという利点
を有しているからである。上記の比較試験では、グレー
プ飲料について行ったが、他の飲料及び食品にも本発明
のポリフェノールエキスをそのままで、または限外濾過
等の膜処理をして、あるいは真空濃縮、吸着樹脂等によ
る精製濃縮をして利用することができる。
Example 1 The additive (formulation-2) was prepared by adding 5 g of polyphenol to a 200 g beverage with almost no bitterness.
0 mg could be fortified. In comparison, a beverage (combination-) containing Comparative Examples 1 and 2 obtained by a general production method was added.
In 3 and 4), bitterness was felt. Strong bitterness was felt for the commercially available beverage (Formulation-5). When the seeds of the raw material were crushed and extracted, Comparative Example 2
Although it is common to cause cloudiness as in 4), it is also an excellent feature that the additive of Example 1 (formulation-2) according to the present invention does not cause cloudiness. This is because it has an advantage that the oil phase can be easily separated from the liquefied carbon dioxide gas extract by freeze separation. In the above comparative tests, grape beverages were tested, but other beverages and foods were treated with the polyphenol extract of the present invention as it was, or subjected to membrane treatment such as ultrafiltration, or vacuum concentrated, purified by an adsorption resin, etc. It can be used after concentration.

【0014】[0014]

【発明の効果】本発明方法により苦みを抑制したポリフ
ェノールを製造することができ、得られたポリフェノー
ルエキスはグレープ飲料等の飲料及びその他の食品に添
加、含有させることにより、苦みを伴うことなく、飲料
その他食品にポリフェノールを増量、強化させることが
可能となった。
According to the present invention, a polyphenol with reduced bitterness can be produced by the method of the present invention, and the resulting polyphenol extract is added to and contained in beverages such as grape beverages and other foods without causing bitterness. Polyphenols can be increased and fortified in beverages and other foods.

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 ブドウ果実の搾汁粕または種子にエチル
アルコール水溶液または水を添加した後、液化炭酸ガス
を用いて抽出し、次いで抽出物を凍結して水相を分離す
ることを特徴とする、ポリフェノール成分の抽出方法。
1. A method comprising adding an aqueous solution of ethyl alcohol or water to squeezed cake or seeds of grape fruit, extracting the mixture with liquefied carbon dioxide gas, and then freezing the extract to separate an aqueous phase. , Polyphenol component extraction method.
【請求項2】 搾汁粕または種子を破砕した後にエチル
アルコール水溶液または水を添加することを特徴とす
る、ポリフェノール成分の抽出方法。
2. A method for extracting a polyphenol component, comprising adding an aqueous solution of ethyl alcohol or water after crushing squeezed cake or seeds.
【請求項3】 搾汁粕または種子10重量部に対してエ
チルアルコール水溶液または水を1〜10重量部の割合
で添加することを特徴とする、請求項1または2記載の
ポリフェノール成分の抽出方法。
3. The method for extracting a polyphenol component according to claim 1, wherein an aqueous solution of ethyl alcohol or water is added at a ratio of 1 to 10 parts by weight with respect to 10 parts by weight of the squeezed cake or seeds. .
【請求項4】 エチルアルコール水溶液中のエチルアル
コール含量が95容量%以下であることを特徴とする、
請求項1〜3のいずれか1項記載のポリフェノール成分
の抽出方法。
4. The method according to claim 1, wherein the content of ethyl alcohol in the aqueous solution of ethyl alcohol is 95% by volume or less.
The method for extracting a polyphenol component according to claim 1.
【請求項5】 請求項1〜3のいずれか1項記載の方法
により得られたポリフェノール成分。
5. A polyphenol component obtained by the method according to claim 1.
【請求項6】請求項5記載のポリフェノール成分を含有
させた飲料。
6. A beverage containing the polyphenol component according to claim 5.
JP11090896A 1999-03-31 1999-03-31 Method for extraction of polyphenol component Pending JP2000279705A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004037276A1 (en) * 2002-10-23 2004-05-06 Tarac Technologies Pty Ltd Method and composition for enhancing vascular function
WO2004089891A1 (en) * 2003-04-07 2004-10-21 Kemijski Institut Process for isolating antioxidants from plant waste material, and their use as foodstuff supplement
WO2006113700A1 (en) * 2005-04-16 2006-10-26 Unitel Technologies, Inc. Concentrated polyphenolic product and process for making the same
CN103977043A (en) * 2014-05-19 2014-08-13 湖南农业大学 Method for extracting red-flowered loropetalum polyphenol from red-flowered loropetalum leaves
CN114848692A (en) * 2022-04-27 2022-08-05 天津农学院 Extraction process and application of quinoa seedling polyphenol substances

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004037276A1 (en) * 2002-10-23 2004-05-06 Tarac Technologies Pty Ltd Method and composition for enhancing vascular function
WO2004089891A1 (en) * 2003-04-07 2004-10-21 Kemijski Institut Process for isolating antioxidants from plant waste material, and their use as foodstuff supplement
WO2006113700A1 (en) * 2005-04-16 2006-10-26 Unitel Technologies, Inc. Concentrated polyphenolic product and process for making the same
CN103977043A (en) * 2014-05-19 2014-08-13 湖南农业大学 Method for extracting red-flowered loropetalum polyphenol from red-flowered loropetalum leaves
CN114848692A (en) * 2022-04-27 2022-08-05 天津农学院 Extraction process and application of quinoa seedling polyphenol substances

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