CN101394748A - Process for producing purified tea extract - Google Patents

Abstract

A process for producing a tea extract of low caffeine content improved in taste and color tone, in which the ratio of nonpolymeric catechins recovered is high. In one mode thereof, there is provided a process for producing a purified tea extract, comprising performing adsorption of a tea extract on a synthetic adsorbent, bringing the synthetic adsorbent into contact with an aqueous solution of organic solvent or basic aqueous solution to thereby attain elution of nonpolymeric catechins, and bringing the eluate into contact with active carbon in an aqueous solution of organic solvent.

Description

The manufacture method of purified tea extract

Technical field

The present invention relates to the manufacture method of the refined products of tea extraction.

Background technology

As the effect of catechin, reported (for example with reference to patent documentations 1) such as alpha-amylase activity inhibitions.In order to show such physiologic effect, in order to absorb a large amount of catechins, wishing has the technology that cooperates the high concentration catechin in beverage.

Make with the following method as one of this method: utilize the tea extractions such as concentrate of green-tea extract, in beverage, add catechin with dissolved state.But, according to becoming the beverage types that high concentration ground cooperates the object of catechin, for example, when in non-teas beverage such as teas beverage, soda etc., adding catechin etc., known caffeine and from the residual and painted commodity value that will significantly damage beverage of the bitter taste of green tea.

Relevant method of removing impurity such as caffeine from tea extraction, known have absorption method (patent documentation 2～4), an extraction method (patent documentation 5～6) etc.

In said method, in order to improve the containing ratio of the non-polymer catechin in the tea extraction, must be with an organic solvent, but on industrial point of view, the low problem of the rate of recovery is arranged.

The relevant method of improving the tone of tea extraction, under the known situation that in tea extract, has a cyclodextrin activated carbon is had an effect with it, thereby be adsorbed on the antibiotic deodorant (patent documentation 7) that is removed on the activated carbon so that be coloured to grade, but be difficult to be applied to beverage catechin preparation.

Known in catechin, by the content of the non-gallate body in the control non-polymer catechin, can improve the local flavor (with reference to patent documentation 8) of green-tea extract.In addition, as shown in patent documentation 9, tannase is handled, thereby part or all becomes the method that gallic acid obtains the mixture of catechin and gallic acid to make it by gallate body catechin is carried out, and can reduce becomes the gallate of bitter taste reason body catechin.But, here the method for Shi Yonging is to handle the method for the content of controlling non-gallate body by carrying out tannase, owing to the residual of enzyme (tannase) and the gallic acid that generated by the hydrolysis of gallate body, the local flavor of resulting tea extraction is insufficient.

The effective manufacturing technology of the tea extraction that the ratio of known gallate body is high (with reference to patent documentation 10), but also do not know the high effective manufacturing technology of tea extraction of ratio of non-gallate body.In addition, knownly handle tea extract, take the not technology of absorbed portion (with reference to patent documentation 11), but because residual tea local flavor etc. and bitter taste are strong, so the purposes in beverage etc. is little with synthetic adsorbent.

In addition, knownly in being filled with the post of synthetic adsorbent, extract night to carry out adsorption treatment by green tea, and the technology (with reference to patent documentation 12) of carrying out the desorption processing with 2 kinds of different ethanol waters of concentration, this is a purification techniques of removing caffeine and impurity under the prerequisite that the catechin of keeping before and after handling is formed, and it is little that its local flavor that derives from the ratio of non-gallate body improves effect.

Patent documentation 1: the spy opens flat 3-No. 133928 communiques

Patent documentation 2: the spy opens flat 5-No. 153910 communiques

Patent documentation 3: the spy opens flat 8-No. 109178 communiques

Patent documentation 4: the spy opens communique 2002-No. 335911

Patent documentation 5: the spy opens flat 1-No. 289447 communiques

Patent documentation 6: the spy opens clear 59-No. 219384 communiques

Patent documentation 7: the spy opens communique 2001-No. 299887

Patent documentation 8: the spy opens communique 2004-No. 321105

Patent documentation 9: the spy opens communique 2004-No. 222719

Patent documentation 10: the spy opens communique 2006-No. 36645

Patent documentation 11: the spy opens communique 2005-No. 170871

Patent documentation 12: the spy opens communique 2006-No. 8580

Summary of the invention

The invention provides a kind of manufacture method (1) of purified tea extract, it is characterized in that: tea extraction is adsorbed on the synthetic adsorbent, then make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent, make non-polymer catechin wash-out, then eluent is contacted with activated carbon.

In addition, the invention provides a kind of manufacture method (2) of purified tea extract, it is characterized in that: tea extraction is adsorbed on the synthetic adsorbent, then make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent, make non-polymer catechin wash-out, be adjusted into the pH of eluent below 7 and concentrate, the outstanding absurd creature that then will separate out is removed by Separation of Solid and Liquid.

In addition, the present invention provides a kind of manufacture method (3) of purified tea extract, it is characterized in that: after making tea extraction be adsorbed on the synthetic adsorbent, make cleaning solution contact synthetic adsorbent, then make aqueous solutions of organic solvent or alkaline aqueous solution contact synthetic adsorbent, fractionate out ratio as the non-gallate body of non-polymer catechin and be 55～100%, caffeine/non-polymer catechin is the tea extraction below 0.15.

The present invention also provides a kind of manufacture method (4) of purified tea extract, it is characterized in that: the hydrolysis tea extraction, then make it to be adsorbed on the synthetic adsorbent, make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent afterwards, make non-polymer catechin wash-out.

In addition, the invention provides a kind of purified tea extract, it is characterized in that: the non-polymer catechin in the solid constituent is that the ratio of the gallate body in 25～95 weight %, the non-polymer catechin is that the ratio of 0～70 weight %, gallic acid and non-polymer catechin is 0～0.1, the ratio of caffeine and non-polymer catechin is 0～0.15.

In addition, the invention provides a kind of purified tea extract, it is characterized in that: the aqueous solution that the non-polymer catechin in the solid constituent is that the ratio of the gallate body in 25～95 weight %, the non-polymer catechin is that the ratio of 0～70 weight %, gallic acid and non-polymer catechin is 0～0.1, the ratio of caffeine and non-polymer catechin is 0～0.2, the concentration of non-polymer catechin is this extract of 1 weight % is 0～0.8 at the tone of 450nm.

In addition, the invention provides a kind of purified tea extract, it is characterized in that: the non-polymer catechin in the solid constituent is that the ratio of the gallate body in 45～90 weight %, the non-polymer catechin is that 0.001～47 weight %, gallic acid amount/non-polymer catechin (weight ratio) are below 0.3.

In addition, the invention provides the purified tea extract that the manufacture method by above-mentioned (1)～(4) obtains.

The present invention also provides the container packed tea beverage that has cooperated the purified tea extract that the manufacture method by above-mentioned (1)～(4) obtains.

Rate of recovery height, the content of caffeine that the invention provides the non-polymer catechin be low, be the manufacture method of the good purified tea extract of flavor and tone.In addition, provide the beverage that has good stability by this purified tea extract.

The inventor finds, after making tea extraction be adsorbed on the synthetic adsorbent, by with aqueous solutions of organic solvent or alkaline aqueous solution optionally wash-out go out the non-polymer catechin, can reclaim the non-polymer catechin with high yield, reduce content of caffeine, can obtain being the refining thing of flavor and tone improvement.

By the present invention can obtain rate of recovery height, the content of caffeine of non-polymer catechin low, be the purified tea extract that flavor and tone are enhanced.In addition, the beverage that can obtain having good stability by purified tea extract of the present invention.

The specific embodiment

In the present invention, so-called non-polymer catechin is the general name of table body catechins such as non-body surface catechin such as catechin, nutgall catechin, catechin and gallate, nutgall catechin gallic acid ester and epicatechin, epigallocatechin, L-Epicatechin gallate, Epigallo-catechin gallate (EGCG).

In the present invention, the non-gallate body of so-called non-polymer catechin is the general name of catechin, nutgall catechin, epicatechin, epigallocatechin etc.The ratio of the non-gallate body in the so-called non-polymer catechin is the percentage by weight of the non-gallate body of above-mentioned non-polymer catechin with respect to non-polymer catechin total amount.

In the present invention, so-called non-polymer catechin nutgall body is the general name of nutgall catechin, nutgall catechin gallic acid ester, epigallocatechin, Epigallo-catechin gallate (EGCG) etc.The ratio of the nutgall body in the so-called non-polymer catechin is the percentage by weight of above-mentioned non-polymer catechin nutgall body with respect to non-polymer catechin total amount.

In the present invention, so-called non-polymer catechin table body is the general name of epicatechin, epigallocatechin, L-Epicatechin gallate, Epigallo-catechin gallate (EGCG) etc.The ratio of the table body in the so-called non-polymer catechin is the percentage by weight of above-mentioned non-polymer catechin table body with respect to non-polymer catechin total amount.

In the present invention, so-called non-polymer catechin and gallate body is the general name of catechin and gallate, nutgall catechin gallic acid ester, L-Epicatechin gallate, Epigallo-catechin gallate (EGCG) etc.

The ratio of the gallate body in the so-called non-polymer catechin is the percentage by weight of above-mentioned non-polymer catechin and gallate body with respect to non-polymer catechin total amount.

The tea extraction of Shi Yonging can be enumerated the extract that obtains from tealeaves in the present invention.Also can use the plant that contains caffeine from other, for example coffee etc. contains the extract of caffeine and the mixture of tea extract etc.The tealeaves that uses more specifically can be enumerated the tealeaves tea making that is obtained by Camellia, for example C.sinensis, C.assamica and shallow lake overgrown with wild plants north kind (cv.Yabukita) or their hybrid etc. and the tealeaves that obtains.Tea making and the tealeaves that obtains have simmer tea, kind tea, beautifully reveal tea, grind green teas such as tea, pot parched tea, be the semi-fermented tea of representative with the oolong tea, be the fermented tea of representative with black tea.In addition, also can use the tealeaves of implementing supercriticality carbon dioxide contact processing.

About extracting the method for tea, carry out according to methods in the past such as stirring extraction, an extraction.In addition, also can add organic acid or organic acid salt such as sodium ascorbate in the water when extracting in advance.In addition, also can and use inert gases such as boiling the degassing or feeding nitrogen to remove molten method oxygen, that under the non-oxide atmosphere of what is called, extract of depositing.The extract that obtains therefrom both can be directly used in the present invention, also can be used for the present invention after dry, concentrated.The form of tea extraction can be enumerated the form of liquid, slurry, semisolid, solid.

The tea extraction of Shi Yonging in the present invention, as the replacement of the extract that extracts from tealeaves, both can in water or organic solvent, dissolve or dilute the concentrate of tea extraction and used, also can and use from the extract of tealeaves and the concentrate of tea extraction.

Here, the concentrate of so-called tea extraction, be to concentrate by the extract that hot water or aqueous solutions of organic solvent extract tealeaves and the concentrate that obtains, for example, refer to by open clear 59-No. 219384 communiques, spy the spy and open flat 4-No. 20589 communiques, spies and open the concentrate that method that flat 5-No. 260907 communiques, spies open record in flat 5-No. 306279 communiques etc. is prepared.Particularly, also can be as tea extraction with commercially available Tokyo Food Tecno Co., (the テ ア Off ラ Application) that (the Port リ Off エ ノ Application) that Ltd. produces, her rattan garden Co., Ltd. produce, the thick catechin preparations such as (Sunphenon) that Taiyo Kagaku Co., Ltd. produces use as the solid tea extract.

The tea extraction that uses in refinement treatment of the present invention is for the purpose that reduces bitter taste, preferably implement hydrolysis process.By this hydrolysis process, the ratio of the gallate body in the non-polymer catechin descends.Among the present invention, when adopting autofrettage (4), especially preferably carry out this hydrolyzing process.The decline degree of the concentration of the non-polymer catechin and gallate body in the non-polymer catechin that is caused by hydrolysis is the flavor aspect from improvement and considers, preferred 5 weight % are above, more preferably 7 weight % above, more than the preferred especially 10 weight %.Method for hydrolysis is waited by enzyme processing, acid treatment, alkali treatment and carries out.Enzyme preferably has enzyme, thalline or the nutrient solution of tannase activity, the preferred hydrochloric acid of acid, sulfuric acid, phosphoric acid, the preferred NaOH of alkali etc.Wherein, consider the preferably hydrolysis of being undertaken by enzyme from reaction control aspect.Here, what is called has the tannase activity, refers to have the activity of decomposing tannic acid, can use enzyme arbitrarily, thalline, nutrient solution with this activity.

Particularly, as enzyme, in commercially available product, can utilize pectase PL AMANO (Amano Enzyme Inc. production), hemicellulase AMANO90 (Amano Enzyme Inc. production), tannase KTFH (KIKKOMAN Corporation production) etc. with tannase activity.Wherein, preferred tannase.For example, can enumerate the tannic acid enzyme-producing bacteria of cultivating aspergillus, Penicillium, rhizopus and the tannase that obtains.Wherein, preferably from the tannase of aspergillus oryzae.

What is called has the thalline of tannase activity, is the thalline that can produce the enzyme with tannase activity, can enumerate Aspergillus etc.For example, can enumerate aspergillus, Penicillium etc., wherein, preferred aspergillus oryzae.

What is called has the nutrient solution of tannase activity, is to cultivate the tannic acid enzyme-producing bacteria of aspergillus, Penicillium, rhizopus and the nutrient solution that obtains.Preferably can enumerate with tannic acid is that unique carbon source is cultivated the nutrient solution that obtains, and both can use highly finished product also can use not highly finished product.

When in the short as far as possible time, finishing hydrolysis, preferably utilize enzyme or nutrient solution from suppressing local flavor variation and productivity ratio aspect to be considered.

The enzyme with tannase activity or the nutrient solution of Shi Yonging preferably has the enzymatic activity of 500～100000U/g in the present invention, and enzymatic activity then just must have a large amount of enzymes in order to finish to handle if below the 500U/g in the time of industrial qualification; If enzymatic activity is more than the 100000U/g, then be difficult to control reaction system because enzyme reaction rate is too fast.Here, 1Unit is illustrated in 30 ℃ of water the enzyme amount of 1 contained micromole's ester bond in the hydrolysis tannic acid.

Non-polymer catechin concentration when handling by enzyme with tannase activity or nutrient solution, preferred 0.1～22 weight %, more preferably 0.1～15 weight %, be more preferably 0.5～10 weight %, preferred especially 0.5～3 weight %.This concentration is during less than 0.1 weight %, and the adsorbance when synthetic adsorbent adsorbs after this descends, if just need for a long time greater than 22 weight %, when the hydrolysis process, considers not preferred from productivity ratio and tea extraction taste aspect.

In order to obtain being the ratio of improved non-polymer catechin and gallate body of distinguishing the flavor of, preferably add the enzyme or the nutrient solution of 0.01～10 weight % scope with respect to the non-polymer catechin in the tea extraction.To comprise the enzyme deactivation operation and handle 2 hours best on the industrialness enzyme reaction time with interior end in order to make in interior said hydrolyzed, the concentration of enzyme or nutrient solution preferably 0.01～7 weight %, be more preferably 0.03～5 weight %.

With respect to the non-polymer catechin in the green-tea extract, preferably become 1～300Unit/g-non-polymer catechin, more preferably become 3～200Unit/g-non-polymer catechin, especially preferably become 5～150Unit/g-non-polymer catechin ground and add enzyme or nutrient solution with tannase activity.

The temperature of being handled by enzyme or nutrient solution preferably can obtain 0～70 ℃ of best enzymatic activity, be more preferably 0～60 ℃, especially preferably 5～50 ℃.

For the hydrolysis that is undertaken by enzyme or nutrient solution is finished, must make the enzymatic activity inactivation.Enzyme deactivation can be reached by heating.Preferred 70～100 ℃ of enzyme deactivation temperature when being lower than 70 ℃, because be difficult to fully make enzyme deactivation and the reaction that is hydrolyzed at short notice, can not stop enzyme reaction in the scope of the ratio of non-polymer catechin and gallate body.In addition, be below 10 seconds the time if arrive the later retention time of deactivation temperature, carry out enzyme reaction because being difficult to make the abundant inactivation of enzymatic activity; In addition, be more than 20 minutes the time in the retention time, the non-table that causes the non-polymer catechin is arranged to isomerized situation and not preferred.

The method for deactivating of enzyme reaction can be heated and be stopped by batch (-type) or the such continous way of template heat exchanger.In addition, after the inactivation that tannase is handled finishes, can be by operations such as centrifugations with limpidization of tea extraction.

When for example utilizing Aspergillus as thalline, the concentration of non-polymer catechin preferably 0.1 weight %～22 weight %, more preferably at 0.1 weight %～15 weight %, add the Aspergillus processing that is hydrolyzed in particularly preferably in the tea extraction of 0.5 weight %～15 weight %.Aspergillus has a great difference by its kind etc., with respect to the non-polymer catechin in the tea extraction, usually in the scope of 0.5 weight %～10 weight %, add in the scope of 1.0 weight %～5 weight % especially.Preferred 45 ℃～70 ℃, more preferably 50 ℃～60 ℃ of temperature conditions.Fermentation time normally 12 hours～20 days, more preferably 1 day～10.Identical during the end of the enzymatic activity inactivation of Aspergillus and hydrolysis in enzyme or nutrient solution.

Synthetic adsorbent can use the adsorbent that does not have the such functional group of ion-exchange group usually in insoluble three-dimensional crosslinking structure polymer in fact, can preferably use the adsorbent of ion-exchange capacity less than 1meq/g.The parent optimization styrene class of synthetic adsorbent, methacrylic, acrylic compounds, polyethylene kind are considered special optimization styrene class from the separation property aspect of catechin and caffeine.Can use particularly: its parent is the synthetic adsorbent of phenylethylene, for example AMBERLITE XAD4, XAD16HP, XAD1180, XAD2000 (supply with and originate: U.S. Rhom and Hass), DIAION HP20, HP21 (Mitsubishi ChemicalCorporation production), SEPABEADS SP850, SP825, SP700, SP70 (MitsubishiChemical Corporation production), VPOC1062 (Bayer AG's production); Replace nuclear and the modified styrenics of reinforcement absorption affinity, for example SEPABEADS SP205, SP206, SP207 (Mitsubishi Chemical Corporation production) with bromine atoms; Methacrylic, for example DIAION HP1MG, HP2MG (Mitsubishi Chemical Corporation production); Phenol, for example AMBERLITE XAD761 (Rhom and Hass's production); Acrylic compounds, for example AMBERLITE XAD7HP (Rhom and Hass's production); Polyethylene kind, for example TOYOPEARL, HW-40C (Tosoh Corporation production); Dextrin class, for example SEPHADEX, LH-20 (Pharmacia Corporation production) etc.

As making tea extraction be adsorbed on method on the synthetic adsorbent, employing is added synthetic adsorbent, stirring, absorption in the tea extraction and the aqueous solution thereof after, reclaim the discontinuous method of synthetic adsorbent by filter operation, or use the post be filled with synthetic adsorbent to carry out the column method of adsorption treatment, but consider the continous treatment process that preferably undertaken from the productivity ratio aspect by post with continuous processing mode.

Be filled with the post of synthetic adsorbent, preferably in advance with SV (space velocity)=0.5～10[h ^-1], with respect to the logical liquid multiple 2～10[v/v of synthetic adsorbent] logical liquid condition, clean with the 95vol% ethanol water, remove the starting monomer of synthetic adsorbent and the impurity in the starting monomer etc.After this with SV=0.5～10[h ^-1], with respect to the logical liquid multiple 1～60[v/v of synthetic adsorbent] logical liquid condition, wash and remove ethanol, will contain the synthetic adsorbent liquid displacement is aqueous systems, is improved the adsorption capacity of non-polymer catechin by this method.

Condition in post during by tea extraction liquid is: when making extract be adsorbed on the synthetic adsorbent, from considering to the adsorption efficiency aspect of synthetic adsorbent, preferred 0.1～22 weight % of the concentration of the non-polymer catechin in the tea extraction, more preferably 0.1～15 weight %, be more preferably 0.5～10 weight %, preferred especially 0.5～3 weight %.

Condition by tea extraction liquid in being filled with the post of synthetic adsorbent is: preferably with SV (space velocity)=0.5～10[h ^-1] logical liquid speed, be 0.5～20[v/v with respect to the logical liquid multiple of synthetic adsorbent] condition lead to liquid.At 10[h ^-1] during above logical liquid speed, the inadequate situation of absorption of non-polymer catechin can take place; At 20[v/v] more than logical liquid measure the time, have the unsettled situation of absorption of non-polymer catechin.

Behind the absorption tea extract, preferably clean synthetic adsorbent with water or aqueous solutions of organic solvent.In addition, in the present invention, when adopting autofrettage (3), especially preferably carry out this clean operation.Consider from catechin rate of recovery aspect, the aqueous solution of the use water below the pH7 preferably in the cleaning of synthetic adsorbent, also can with the mixed system of organic solvent in use.Organic solvent can be enumerated acetone, methyl alcohol, ethanol etc., from being used for the viewpoint preferred alcohol of food.Consider from catechin rate of recovery aspect, the organic solvent concentration that contains be 0～20 weight %, preferably 0～10 weight %, be more preferably 0～5 weight %.

In this clean operation, preferably with SV (space velocity)=0.5～10[h ^-1] logical liquid speed, with logical liquid multiple 1～10[v/v with respect to synthetic adsorbent] remove the impurity that on synthetic adsorbent, adsorbs.Consider from the rate of recovery aspect of removing effect and non-polymer catechin of impurity, more preferably with SV (space velocity)=0.5～5[h ^-1] logical liquid speed, with logical liquid multiple 1～5[v/v] clean.

Eluent is (a) during the aqueous solution with an organic solvent, and as the organic solvent that is used for wash-out non-polymer catechin, the preferred water solubleness organic solvent can be enumerated acetone, methyl alcohol, ethanol etc., considers preferred alcohol from the viewpoint that is used for food.High and the impurity level aspect consideration such as tail off from the rate of recovery of non-polymer catechin, this organic solvent preferably uses with aqueous solution form, preferred 1～80 weight % of the concentration of the organic solvent in the aqueous solution, more preferably 4～60 weight %, preferred especially 10～40 weight %.

Preferably with SV (space velocity)=0.5～5[h ^-1] logical liquid speed, be 1～15[v/v with logical liquid multiple with respect to synthetic adsorbent] condition wash-out non-polymer catechin.Consider from productivity ratio and non-polymer catechin rate of recovery aspect, more preferably with SV=1～3[h ^-1] logical liquid speed, with logical liquid multiple 2～10[v/v] the condition wash-out.

From the simplification of operation be refined into this aspect consider that preferably the eluent that uses is an aqueous solutions of organic solvent in the wash-out of non-polymer catechin.

When eluent uses alkaline aqueous solution (b), as the alkaline aqueous solution that is used for wash-out non-polymer catechin, can compatibly use the aqueous solution of alkali such as alkali metal salt, alkali earth metal salt, can preferably use the alkaline aqueous solution of sodium, potassium class, for example, can compatibly use sodium hydrate aqueous solution, aqueous sodium carbonate etc.In addition, the pH of alkaline aqueous solution is 7～14 scopes preferably, consider preferred 9～13.8, preferred especially 10～13.5 from non-polymer catechin rate of recovery aspect.As the sodium class aqueous solution of pH7～14, can enumerate sodium hydrate aqueous solution below 4%, 1N aqueous sodium carbonate etc.Alkaline aqueous solution and organic solvent also can mix use.Consider from the separation property aspect of caffeine and catechin, preferred 0～90 weight % scope of the concentration of organic solvent, more preferably 0～50 weight %, be more preferably 0～20 weight %.

In the wash-out operation, the alkaline aqueous solution that is used for wash-out can use the different alkaline aqueous solution more than 2 kinds of pH, can make these alkaline aqueous solutions with the low order contact synthetic adsorbent of pH.Can go out different non-polymer catechins and other composition by wash-out in each pH zone.

Preferably with SV (space velocity)=2～10[h ^-1] logical liquid speed, with logical liquid multiple 1～30[v/v with respect to synthetic adsorbent] condition wash-out non-polymer catechin.Consider from the rate of recovery aspect of productivity ratio and non-polymer catechin, more preferably with SV=3～7[h ^-1] logical liquid speed, with logical liquid multiple 3～15[v/v] condition carry out wash-out.

Consider that from the tone of purified tea extract, rate of recovery aspect the activated carbon treatment preferably the eluent that uses is an alkaline aqueous solution in the wash-out of non-polymer catechin.

When carrying out wash-out with alkaline aqueous solution, the eluent of non-polymer catechin is an alkalescence, from the viewpoint of non-polymer catechin stability, preferably the pH of eluent is adjusted become 7 below, more preferably adjust become 1～6, be more preferably adjust become 1～5, preferred especially adjustment becomes 2～4.Particularly, can utilize with the acid neutralization, remove alkali metal ion, or remove the method for alkali metal ion with ion exchange resin with electrodialysis.Especially preferably use H type cationic ion-exchange resin as ion exchange resin.Consider, preferably adjust pH from the simplicity viewpoint of process with ion exchange resin.Particularly, cationic ion-exchange resin can use AMBERLITE200CT, IR120B, IR124, IR118, DIAIONSK1B, SK1BH, SK102, PK208, PK212 etc.

With the alkaline aqueous solution wash-out time, the eluent, the Separation of Solid and Liquid that concentrate after neutralizing are removed the impurity of separating out, and this is preferred when considering from being flavor and goods stability raising aspect.Concentrating can be by enforcements such as decompression distillation, thin-film distillation, film concentrate.Consider preferred 2～500 times, more preferably 2～250 times, preferred especially 2～125 times of concentration rates from the separate impurities aspect that is flavor and separates out.Consider preferred 0.1～60 weight % of concentration of the non-polymer catechin after concentrating, more preferably 0.2～30 weight %, preferred especially 0.5～15 weight % from being flavor and the separate impurities aspect separated out.The concrete operations mode of Separation of Solid and Liquid can be enumerated and filter and/or the centrifugation processing.The Separation of Solid and Liquid tea extraction aqueous solution and the turbidity of the water-soluble portion tea extraction aqueous solution that obtains, if 0.1～100NTU, to be more preferably 0.5～70NTU, to be more preferably be 1～50NTU, then beverage be flavor and stable aspect preferred.Turbidity is measured with 2100P type (production of Ha Star Network company), can be with the value [unit: NTU] that here the obtains index as the separation clarity.

Solid-liquid separating method can be useful in the method for using in the food industry.For example, the membrane filtration condition when carrying out Separation of Solid and Liquid with membrane filtration is that preferred temperature is 5～70 ℃, more preferably 10～40 ℃.Consider that from becoming definite turbidity aspect preferred 0.1～10 μ m of membrane aperture considers that from the separation property aspect of filtering needed time and muddy composition membrane aperture is 0.1～5 μ m, preferred especially 0.1～2 μ m more preferably.As the assay method of membrane aperture, can enumerate general assay methods such as using mercury penetration method, bubble point test, bacterial filtration, the preferred value of obtaining with bubble point test of using.The membrane material that uses in membrane filtration can use polymeric membrane, ceramic membrane, stainless steel membrane etc.

In addition, general machines such as centrifugal separator preferable separate template, cylinder type, the special type of Deacon.5～70 ℃ of the preferred temperature of centrifugation condition, be more preferably 10～40 ℃, rotating speed and time can impose a condition according to the turbidity of hope.For example, when separating disc type, preferred 3000～10000r/min, more preferably 5000～10000r/min, preferred especially 6000～10000r/min, preferred 0.2～30 minute, more preferably 0.2～20 minute, preferred especially 0.2～15 minute.

Consider from the tone aspect of improving tea extraction, preferably make eluent (comprise above-mentioned (a) and (b) any one) in aqueous solutions of organic solvent, contact activated carbon.The raw material of activated carbon can be enumerated cocoanut shell, wooden, coal etc., but preferably wooden.The tax activating method of activated carbon can be enumerated water vapour tax method alive, gas is composed the method for living, medicine tax method alive, but preferably medicine is composed the method for living.

For example, can use ZN-50, Y-10S, GS-1, GS-B (Ajinomoto Fine-TechnoCo., Inc. produce), KURARAYCOAL GLC, KURARAYCOAL PK-D, KURARAYCOAL PW-D, KURARAYCOAL GW, KURARAYCOALGA, KURARAYCOAL GA-D, KURARAYCOAL RP-15 (KURARAYCHEMICAL CO., LTD. produce), SHIRASAGI AW50, SHIRASAGI A, SHIRASAGI P, SHIRASAGI KL, SHIRASAGI M, SHIRASAGI C, CARBORAFFIN, WH2C (Japan EnviroChemicals.ltd production), GM130A, CW130A, CW130AR, CW350AR, GL 130A, SG, SGA, SGP (FutamuraChemical Co., Ltd. produce), Yashicoal, the MAS seal, plum honeybee seal, plum honeybee F prints (TaiheiChemical Industrial Co., Ltd. produce), CPG, CAL, S80A commercially available products such as (Calgon MitsubishiChemical Corporation. productions).

Consider that from the use amount aspect of improving goods tone aspect, minimizing activated carbon, the aspect that improves the rate of recovery activated carbon preferably uses following activated carbon.Preferred 0.5～the 10nm of average pore diameter (nanometer), the more preferably activated carbon of 1.0～9.0nm (nanometer), preferred especially 2.0～8.0nm (nanometer).Preferred 0.01～the 2.5mL/g of pore volume, the more preferably activated carbon of 0.1～2.0mL/g, preferred especially 0.5～1.7mL/g.In addition, the preferred 800～2000m of specific area ²/ g, more preferably 900～1600m ²/ g, preferred especially 1000～1500m ²The activated carbon of/g.In addition, these physics values all are based on the value that the nitrogen adsorption method is measured.

With respect to the non-polymer catechin in the 100 mass parts eluents, from refining effect, improve rate of recovery aspect, filter the aspect that resistance of filter cake is little the operation and consider, preferably add 1～200 mass parts, more preferably add 5～100 mass parts, especially preferably add the activated carbon of 10～80 mass parts.

The organic solvent preferred water solubleness organic solvent that uses when making it to contact with activated carbon can be enumerated acetone, methyl alcohol, ethanol etc., considers preferred alcohol from the viewpoint that is used for food.Viewpoints such as, the yield height of non-polymer catechin good from the tone of resulting goods, impurity level are few, this organic solvent must use in aqueous solution mode, organic solvent concentration preferably use 1～80 weight % aqueous solution, more preferably use 2～70 weight % aqueous solution, especially preferably use 5～50 weight % aqueous solution, more especially preferably use 7～40 weight % aqueous solution.

When making it to contact with activated carbon, from improve refining effect, rate of recovery aspect is considered, preferred 0.5～20 weight % of the concentration of the non-polymer catechin in the aqueous solutions of organic solvent, more preferably 1～15 weight %, preferred especially 2～8 weight %.

When making it to contact with activated carbon, from the eluent of synthetic adsorbent preferably by interpolation, the decompression of water and aqueous solutions of organic solvent concentrate, processing such as film concentrates, desolventizing are adjusted into definite concentration with the concentration of solvent strength and non-polymer catechin.

Method when making it to contact with activated carbon, can adopt and in eluent, add the tank diameter method that reclaims activated carbon after activated carbon, the stirring and adsorbing by filter operation, or the column method that uses the post be filled with activated carbon to make it to contact with continuous processing mode, but consider from the productivity ratio aspect, preferably with the continous treatment process of column method.

The purified tea extract that obtains by the present invention, aspect from be coupled to beverage considers, in its solid constituent, preferably contain 25～95 weight %, more preferably contain 40～95 weight %, be more preferably and contain 50～90 weight %, especially preferably contain the non-polymer catechin of 60～85 weight %.In addition, consider from being the flavor aspect, in solid constituent, preferably contain 45～90 weight %, more preferably contain 50～88 weight %, be more preferably and contain 55～85 weight %, especially preferably contain the non-polymer catechin of 60～83 weight %.

In addition, from the validity of the physiologic effect of non-polymer catechin, reduce the bitter taste aspect and consider, the ratio (ratio of gallate body) of gallate body in whole non-polymer catechins that catechin and gallate, L-Epicatechin gallate, nutgall catechin gallic acid ester and the Epigallo-catechin gallate (EGCG) in the purified tea extract that is obtained by the present invention formed preferably 0～70 weight %, to be more preferably 1～60 weight %, to be more preferably be 2～40 weight %, 10～35 weight % especially preferably.In addition, from suppressing the viewpoint of bitter taste, productivity ratio, ratio (ratio of gallate body) preferred 0.001～47 weight % of gallate body in whole non-polymer catechins, more preferably 0.01～45 weight %, be more preferably 0.1～43 weight %, preferred especially 1～40 weight %.

Be aspect the flavor in improvement and consider, caffeine concentration in the purified tea extract that obtains in the present invention with respect to the non-polymer catechin is, preferably coffee because of/non-polymer catechin (weight ratio)=0～0.2, more preferably 0～0.15, be more preferably 0～0.1, preferred especially 0～0.05, preferred more especially 0～0.035.In addition, be aspect the flavor in improvement and consider, caffeine concentration with respect to the non-polymer catechin is, preferably coffee because of/non-polymer catechin (weight ratio) below 0.2, more preferably below 0.15, be more preferably below 0.1, preferred below 0.05 especially, and 0 above, be more preferably more than 0.0001, preferred more than 0.001 especially.

In addition, be flavor, the consideration of tone aspect, the ratio (weight ratio) of gallic acid in the purified tea extract that obtains in the present invention and non-polymer catechin preferred 0～0.1, more preferably 0～0.07, preferred especially 0～0.05 from improvement.In addition, consider from being the flavor aspect, the ratio (weight ratio) of gallic acid and non-polymer catechin is below 0.3, preferably below 0.1, be more preferably below 0.07, and be more than 0, be more preferably more than 0.0001, be more preferably to be more than 0.001.

Tone aspect in the time of from be coupled to beverage, be refined into this aspect and consider, the tone of the purified tea extract that obtains in the present invention is, the concentration of non-polymer catechin be the aqueous solution of 1 weight % the tone of 450nm (/cm) preferably 0～0.8, to be more preferably 0.01～0.75, to be more preferably be 0.1～0.6, especially preferably 0.2～0.5.

In the methods of the invention, from the operation of synthetic adsorbent wash-out non-polymer catechin, also can obtain the purified tea extract (autofrettage (3)) that non-polymer catechin concentration height, content of caffeine are lowered by control wash-out operation.

Be used to obtain purified tea extract of the present invention, from the condition of synthetic adsorbent elution fractionation, from the physiological availability of non-polymer catechin, reduce the bitter taste aspect and consider, need satisfy non-gallate body ratio in the tea extraction of institute's fractionation and be 55～100 weight %, preferably 60～99 weight %, to be more preferably be 65～98 weight %, 65～90 weight % especially preferably.

In addition, condition from the synthetic adsorbent elution fractionation, be flavor aspect, the consideration of physiologic effect aspect from improvement, the caffeine concentration that preferably satisfies in the tea extraction of institute's fractionation with respect to the non-polymer catechin is, caffeine/non-polymer catechin (mass ratio)=0.15 is following, more preferably 0～0.1, be more preferably 0～0.08, preferred especially 0～0.05, preferred more especially 0～0.035.

Moreover, condition from the synthetic adsorbent elution fractionation, consider from improving the local flavor aspect, the ratio (gallic acid/non-polymer catechin) (mass ratio) that need satisfy gallic acid in the tea extraction of institute's fractionation and non-polymer catechin is below 0.1, more preferably 0～0.07, be more preferably 0～0.05, preferred especially 0～0.02.

In the present invention, condition from the synthetic adsorbent elution fractionation that obtains, tone aspect in the time of from be coupled to beverage, be refined into this aspect and consider, the tone that must satisfy the tea extraction of institute's fractionation is, the aqueous solution the when concentration of non-polymer catechin is 1 weight % the tone of 450nm (/cm) preferably below 3, to be more preferably 0.01～2, to be more preferably be 0.1～1, especially preferably 0.2～0.5.

Consider from local flavor, the physiologic effect of improving purified tea extract and the aspect that reduces cost, in the present invention, need satisfy from the condition of synthetic adsorbent elution fractionation, the component ratio of the non-polymer catechin in the tea extraction of institute's fractionation is, component ratio with non-polymer catechin before adsorbing counts 1, and non-gallate body is 1.2～10, the nutgall body is 1.0～1.3, the table body is 0.8～1.0.

Need satisfy from the condition of synthetic adsorbent elution fractionation, the ratio of the non-gallate body in the tea extraction of institute's fractionation is, ratio with the non-gallate body of tea extraction before adsorbing counts at 1 o'clock, is preferably 1.3～5, more preferably 1.4～4, is more preferably 1.45～3, preferred especially 1.5～2.Need satisfy from the condition of synthetic adsorbent elution fractionation, the ratio of the nutgall body in the tea extraction of institute's fractionation is, ratio with the nutgall body of tea extraction before adsorbing counts at 1 o'clock, and is preferred 1.01～1.28, more preferably 1.02～1.26, be more preferably 1.04～1.24, preferred especially 1.06～1.22.Need satisfy from the condition of synthetic adsorbent elution fractionation, the ratio of the table body in the tea extraction of institute's fractionation is, ratio with the table body of tea extraction before adsorbing counts at 1 o'clock, and is preferred 0.82～1.0, more preferably 0.86～0.99, be more preferably 0.90～0.99, preferred especially 0.94～0.98.

After making synthetic adsorbent absorption tea extraction, make detergent remover contact synthetic adsorbent, then make eluent contact synthetic adsorbent, fractionation is adsorbed on 10～60% of non-polymer catechin on the synthetic adsorbent in fraction.

In the non-polymer catechin of synthetic adsorbent absorption, be eluted in the amount (being referred to as the rate of recovery [%] of non-polymer catechin) of the non-polymer catechin in the fraction, can control with elution requirements such as concentration, the amounts of contact with the eluent kind.The rate of recovery of non-polymer catechin is 10～60%.From improve the catechin rate of recovery, reduce content of caffeine, improve the non-gallate body of non-polymer catechin ratio, improve the local flavor aspect and consider, preferably 15～55%, to be more preferably 20～50%, to be more preferably be 25～45%.

From the ratio aspect of reduction content of caffeine and the non-gallate body of raising non-polymer catechin, from improving local flavor aspect, the calm amount aspect consideration that is eluted to the non-polymer catechin the fraction easy to control in addition, eluent is aqueous solutions of organic solvent or alkaline aqueous solution preferably.

If carry out wash-out with aqueous solutions of organic solvent or alkaline aqueous solution, non-gallate body is more first by wash-out than gallate body.

The purified tea extract that obtains in the present invention can directly use as beverage.Method such as also can be concentrated by decompression in addition,, film concentrates is removed and is desolvated.In addition, when the goods form of wishing purified tea extract is powder, can implement powderization by methods such as spray-drying or freeze dryings.

Consider from obtaining assorted flavor and sapid container-packed beverage aspect, preferably will use the non-polymer catechin concentration of the container-packed beverage of purified tea extract of the present invention be adjusted into 0.05～0.5 weight %, preferably be adjusted into 0.06～0.5 weight %, more preferably be adjusted into 0.08～0.5 weight %, be more preferably be adjusted into 0.092～0.4 weight %, especially preferably be adjusted into 0.11～0.3 weight %, more especially preferably be adjusted into 0.12～0.3 weight %.

In addition, consider that from the validity aspect of the physiologic effect that is flavor, non-polymer catechin the ratio of the general name gallate body of being made up of catechin and gallate, L-Epicatechin gallate, nutgall catechin gallic acid ester, Epigallo-catechin gallate (EGCG) in the preferred said vesse dixie cup in whole non-polymer catechins be 0～70 weight %, be more preferably 1～60 weight %, particularly 2～40 weight %, 10～35 weight % more especially.

In addition, from the minimizing effect of bitter taste, tart flavour, more from local flavor and the consideration of tone storage stability aspect, the content of the gallic acid in the container-packed beverage of the present invention can be less than 10mg/100mL.

Container-packed beverage of the present invention can be used as the teas beverage and non-teas beverage uses.Non-teas beverage can enumerate particularly the acidic beverages that contains sweetener and fruit flavors and sports drink or or the like ooze beverage (isotonic beverage).

The sweetener that uses in container-packed beverage of the present invention can use artificial sweetener class, carbohydrate, glycerols (for example glycerine).

In fruit aroma, comprise fruit juice and spices.Usually, fruit juice is called fruit syrup, spices is made flavouring agent, can use the natural or synthetic perfume and the fruit juice that comprise these among the present invention.

With container-packed beverage of the present invention make sports drink or etc. when oozing beverage, preferably wherein contain sodium ion and/or calcium ion.

Can also contain acid as required in the beverage of the present invention.Acid can be enumerated food acids such as malic acid, citric acid, tartaric acid, fumaric acid.Acid also can be used to adjust the pH of beverage of the present invention.

Drink easily if cooperate the bitter taste inhibitor just to become in the container-packed beverage of the present invention, therefore preferred.Be not particularly limited for employed bitter taste inhibitor, but preferred cyclodextrin.Cyclodextrin can use α-, β-, gamma-cyclodextrin and branching α-, β-, gamma-cyclodextrin.In beverage, preferably contain 0.005～0.5 weight %, more preferably contain the cyclodextrin of 0.01～0.3 weight %.In container-packed beverage of the present invention, can cooperate or cooperate jointly antioxidant, various ester class, inorganic salts, pigment, emulsifying agent, preservative agent, flavouring, sweetener, acid, natural gum, emulsifying agent, oil, vitamin, amino acid, vegetable extract class, nectar extract class, pH to adjust additives such as agent, stay in grade agent separately.

Consider that from the stable aspect that is flavor and non-polymer catechin the pH of preferred container-packed beverage of the present invention is 2～7, preferred 2～6.5 in the time of 25 ℃.

In container-packed beverage of the present invention, from the meaning of guaranteeing that for the physiologic effect that obtains catechin every day must intake, every bottle (cooperate in 350～500mL) container-packed beverages of the present invention 300mg above, preferably 450mg above, be more preferably more than the 500mg.

In addition, above-mentioned container-packed beverage for example in being filled into the such container of metal can the back, can the situation of heat sterilization under, in food hygiene law, make under the sterilising conditions of defined.The container that can not distill sterilization as PET bottle, paper container etc. is adopted following method: adopt in advance and above-mentioned equal sterilising conditions, for example carry out sterilization between high temperature, short time by heat-exchangers of the plate type etc. after, be cooled to uniform temperature, recharge in the container.In addition, cooperate other compositions in the container that also can under aseptic condition, be filled.

Embodiment

(1) mensuration of catechin, caffeine and gallic acid

With filter (0.45 μ m) filtered sample solution, the high performance liquid chromatography (model SCL-10AVP) that uses Shimadzu Seisakusho Ltd. to produce, the liquid chromatography packed column L-post TM ODS (4.6mm Φ * 250mm: juridical person's chemical substance evaluation study mechanism produces) that imports octadecyl is installed, analyzes with 35 ℃ of column temperatures, gradient method.Mobile phase A liquid is that the distilled water solution, the B liquid that contain 0.1mol/L acetic acid are that acetonitrile solution, the sample injection rate that contains 0.1mol/L acetic acid is 20 μ L, and UV detector wavelength is 280nm, carries out under this condition.

(2) evaluation of the refining thing taste of tea extraction

The purified tea extract dilution that will obtain in each embodiment with deionized water becomes non-polymer catechin containing ratio and reaches 0.175%[w/v], its 40mL is added in the withstand voltage glass container of 50mL.Add 0.1 weight % sodium ascorbate therein, pH be adjusted into 6.4, carry out nitrogen replacement with 5% sodium bicarbonate aqueous solution, with autoclave 121 ℃ of heat sterilizations 10 minutes.After this, by 5 evaluation personnel preceding flavor and aftertaste are carried out the bitter taste evaluation.The bitter taste evaluation is carried out with the quinine sulfate method.

(3) the bitter taste evaluation of carrying out with quinine sulfate method (concentration test method(s) of equal value)

Quinine sulfate 2 hydrates are adjusted into the concentration of bitterness intensity corresponding to record in the table.After trying out assess sample, judge bitterness intensity with which sample of standard bitter taste solution equates.Carry out the affirmation (list of references: the scientific and technological organoleptic test of company of the new edition organoleptic test's handbook day p448 of the committee-449, Perception﹠amp of bitterness intensity by 5 evaluation personnel; Psychophysics, 5,1696,347-351)

[table 1]

The bitter taste concentration of standard solution

Bitterness intensity	Quinine sulfate 2 hydrates (g/100mL aq.)
		1	0.00023
2	0.00050
		3	0.00094
4	0.00157
		5	0.00241
6	0.00388
		7	0.00608
8	0.00985
		9	0.01572
10	0.02568

(4) mensuration of tone

Use the spectrophotometer (model U-2001 type) of HITACHI, in glass case with the ion exchange water dilute sample, be its to become non-polymer catechin concentration be the aqueous solution of 1 weight %, and measure.Spectrophotometric determination wavelength set during analysis is 450nm.

Embodiment 1

In 3kg green tea (Kenya's product, large leaf), add 88 ℃ of hot water 45kg, stir 60 minutes, intermittently extract after, after 100 order wire netting coarse filtration, for the micro mist of removing in the extract carries out the centrifugation operation, obtain 37.2kg (pH5.4) " green tea extractive liquor " (ratio of the gallate body of the non-polymer catechin concentration in the green tea extractive liquor=0.89 weight %, green tea extractive liquor=52.3 weight %, caffeine 0.17 weight %).This green tea extractive liquor is remained on 15 ℃, adding tannase (KIKKOMAN Corporation production, tannase KTFH, 500U/g) is that its concentration becomes 430ppm with respect to green tea extractive liquor, kept 55 minutes, when the ratio of gallate body becomes 30.5 weight %, solution is heated to 90 ℃, keep 2 minutes, make enzyme deactivation, stop reaction (pH5.1).Then, under 70 ℃, the condition of 6.7Kpa, carry out concentration in the mode of concentrating that reduces pressure and reach 20%, carry out spray-drying again, obtain 0.9kg pulverous " green-tea extract that tannase is handled " up to Brix concentration.In the green-tea extract that obtains, non-polymer catechin content is that the ratio of 27.8 weight %, non-polymer catechin and gallate body is that 30.3 weight %, content of caffeine are that 6.74 weight %, gallic acid are 3.58 weight %.In the 8550g deionized water, at 25 ℃ of stirring and dissolving 285g " green-tea extract that tannase is handled " 30 minutes (tannase treatment fluid).

Then, in stainless steel column 1 (internal diameter 110mm * height 230mm, volume 2185mL), fill 2209mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production).In stainless steel column 2 (internal diameter 38mm * height 770mm, volume 877.4mL), fill 852mL ion exchange resin SK1BH (Mitsubishi Chemical Corporation production).In two posts in advance all with SV=5 (h ^-1) by after 4 times of cubical contents (to potting resin) 95 (v/v) ethanol liquid, by 10 times of cubical contents (to potting resin) water to clean.After this, in post 1 with SV=1 (h ^-1) by the resulting tannase treatment fluid of 8835g (to 4 times of volumes of synthetic adsorbent), the discarded liquid that sees through.Then, with SV=2 (h ^-1) water of 2209mL (to 1 times of volume of synthetic adsorbent) cleans.After the washing, with SV=5 (h ^-1) by 13256mL (to 6 times of volumes of synthetic adsorbent) 0.1 weight % sodium hydrate aqueous solution (pH12.4).Eluent continue in post 2 by, carry out deionization, obtain 13080g (pH3.3) non-polymer catechin compound composition.Contain 0.38 weight % non-polymer catechin in this extract, the ratio of the gallate body of non-polymer catechin compound composition is 28.6 weight %.In addition, caffeine is that 0 weight %, gallic acid are 0.002 weight %.Non-polymer catechin in the tea extraction solid constituent is 69.0 weight %.It is concentrated to reduce pressure under 40 ℃, the condition of 2.6Kpa again, is concentrated to non-polymer catechin concentration 6% (turbidity 208NTU).Then, make it cellulose ethanoate film (ADVANTEC:C080A090C),, obtain " resin treatment product 1 " (turbidity 1.5NTU) with outstanding absurd creature Separation of Solid and Liquid by 0.8 μ m.Then, in stainless steel column 3 (internal diameter 22mm * height 145mm, volume 55.1mL), fill too Together SGP (Futamura Chemical Co., Ltd. produces) of 6.5g granular activated charcoal." resin treatment product 1 " preparation is become non-polymer catechin concentration 4% and concentration of alcohol becomes 20 weight %, with SV=2 (h ^-1), with this 267g in post 3 by (amount of activated carbon is 0.6 with respect to the amount of non-polymer catechin).Then, the molecular filter with 0.2 μ m filters.At last.Add the 50g ion exchange water, steam ethanol, after this, adjust amount of moisture, obtain " activated carbon treatment product 1 " (2.1NTU) with 40 ℃, the condition of 2.7Kpa.Contain 13.7 weight % non-polymer catechins in this extract, the ratio of the gallate body of non-polymer catechin compound composition is 23.5 weight %.In addition, caffeine is that 0 weight %, gallic acid amount are 0.054 weight %.Non-polymer catechin in the solid constituent is 79.6 weight %.

Comparative example 1

In embodiment 1 " resin treatment product 1 ".

Embodiment 2

In stainless steel column 4 (internal diameter 110mm * height 230mm, volume 2185mL), fill 2048mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production).To clean post in advance with embodiment 1 same method.After this, in post 4 with SV=1 (h ^-1), 8191g (4 times of volumes are to synthetic adsorbent) the tannase treatment fluid by in embodiment 1, obtaining, the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 2048mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=2 (h ^-1), by 12287mL (to 6 times of volumes of synthetic adsorbent) 20 weight % ethanol waters, obtain 12090g (pH2.1) non-polymer catechin compound composition.Contain 0.51 weight % non-polymer catechin in this extract, the ratio of the gallate body of non-polymer catechin compound composition is 27.4 weight %.In addition, caffeine is that 0.075 weight %, gallic acid amount are 0.002 weight %.Non-polymer catechin in the tea extraction solid constituent is 62.5 weight %.Again in decompression concentrates, steam ethanol with 40 ℃, 2.7Kpa, after this, adjust amount of moisture, obtain " resin treatment product 2 ".Then, to carry out and the contacting processing (amount with respect to the activated carbon of the amount of non-polymer catechin is 0.6), obtain " activated carbon treatment product 2 " (1.7NTU) of activated carbon with embodiment 1 same method.Contain 15.0 weight % non-polymer catechins in this extract, the ratio of the gallate body of non-polymer catechin compound composition is 20.9 weight %.In addition, caffeine is that 0.264 weight %, gallic acid amount are 0.057 weight %.Non-polymer catechin in the solid constituent is 72.8 weight %.

Comparative example 2

In embodiment 2 " resin treatment product 2 ".

The result that expression compares embodiment 1 and comparative example 1, embodiment 2 and comparative example 2 in table 2.

[table 2]

Reaction condition, mensuration project and sense evaluation result		Embodiment 1	Comparative example 1	Embodiment 2	Comparative example 2
						Have or not hydrolysis process		Have	Have	Have	Have
The ratio of the gallate body in the non-polymer catechin of hydrolysis process product (product before the resin treatment)	[weight %]	27.8	27.8	27.8	27.8
						Take off the method for absorption from resin		Sodium hydrate aqueous solution	Sodium hydrate aqueous solution	Ethanol water	Ethanol water
Aqueous solutions of organic solvent concentration during the contact activated carbon	[weight %]	20		20
						The non-polymer catechin	[weight %]	13.7	6.0	15.0	6.0
Non-polymer catechin in the solid constituent	[weight %]	79.6	69.0	72.8	62.5
						The ratio of the gallate body in the non-polymer catechin	[weight %]	23.5	28.6	20.9	27.4
Caffeine	[weight %]	0.000	0.000	0.264	0.882
						Gallic acid	[weight %]	0.054	0.032	0.057	0.024
The bitter taste of preceding flavor		5.0	5.0	5.0	5.0
						The bitter taste of aftertaste		5.0	5.5	5.0	5.3
Tone (450nm)		0.23	2.78	0.35	2.15

As known from Table 2, by after making synthetic adsorbent absorption tea extraction, with aqueous solutions of organic solvent or alkaline aqueous solution wash-out, then in aqueous solutions of organic solvent, implement activated carbon treatment, thereby can obtain that caffeine reduces, the bitter taste of aftertaste reduces, the purified tea extract of tone raising.Therefore, this extract is not only useful as the teas beverage, and also is useful as non-teas beverage.

Embodiment 3～6

Operation according to embodiment 1, hydrolysis process is proceeded to the ratio that is not hydrolyzed with the gallate body become about 3.5%, and the aqueous solutions of organic solvent concentration of carrying out activated carbon when contact is the operation (with respect to the amount of non-polymer catechin, the amount of activated carbon is 0.6) of 20 weight % and 60 weight %.Ecbatic in table 3.

[table 3]

Reaction condition, mensuration project and sense evaluation result		Embodiment 3	Embodiment 4	Embodiment 5	Embodiment 6
						Have or not hydrolysis process		Do not have	Do not have	Have	Have
The ratio of the gallate body in the non-polymer catechin of hydrolysis process product (product before the resin treatment)	[quality %]	55.8	54.3	3.5	3.4
						Take off the method for absorption from resin		Sodium hydrate aqueous solution	Sodium hydrate aqueous solution	Sodium hydrate aqueous solution	Sodium hydrate aqueous solution
Aqueous solutions of organic solvent concentration during the contact activated carbon	[quality %]	20	60	20	60
						The ratio of the gallate body in the non-polymer catechin	[quality %]	53.2	53.9	1.1	2.1
Tone (450nm)		0.22	0.31	0.42	0.74
						The rate of recovery in the activated carbon treatment	[quality %]	69	79	73	81

By table 3, if the aqueous solutions of organic solvent concentration relatively during the activated carbon contact is the situation of 20 weight % and 60 weight %, aspect tone, 20 weight % be preferred.Aspect the rate of recovery, 60 weight % be preferred.

Embodiment 7～9, comparative example 3～4

Mode according to embodiment 1 and embodiment 2 is operated, aqueous solutions of organic solvent concentration during the activated carbon contact is 0 weight %, 7.5 weight % and 20 weight %, carry out (with respect to the amount of non-polymer catechin, the amount of activated carbon is 0.6) with the operating of contacts of activated carbon with the tank diameter method.Ecbatic in table 4.

[table 4]

Reaction condition, mensuration project and sense evaluation result		Embodiment 7	Embodiment 8	Comparative example 3	Embodiment 9	Comparative example 4
							Having or not of hydrolysis process		Have	Have	Have	Have	Have
The ratio of the gallate body in the non-polymer catechin of hydrolysis process product (product before the resin treatment)	[weight %]	27.1	28.2	27.2	26.8	26.8
							Take off the method for absorption from resin		Sodium hydrate aqueous solution	Sodium hydrate aqueous solution	Sodium hydrate aqueous solution	Ethanol water	Ethanol water
Aqueous solutions of organic solvent concentration during the contact activated carbon	[weight %]	7.5	2.0	0	20	0
							The ratio of the gallate body in the non-polymer catechin	[weight %]	21.2	24.1	19.4	22.6	15.6
Tone (450nm)		0.48	0.43	0.86	0.61	0.97
							The rate of recovery in the activated carbon treatment	[weight %]	78	75	68	71	60

As known from Table 4, when the aqueous solutions of organic solvent concentration than will contact activated carbon the time becomes 0 weight % (when being solvent with water), when the aqueous solutions of organic solvent concentration during with the contact activated carbon became 7.5 weight % and 20 weight %, tone was good, the rate of recovery is good.

Embodiment 10

Use embodiment 1 " activated carbon treatment product 1 " to be formulated in the container-packed beverage of putting down in writing in the table 5.Carry out filling based on the sterilization treatment of food hygiene law and hot packing, with it as container-packed beverage.

Preserving the container-packed beverage of making at 37 ℃ estimated after 30 days.Outward appearance and be the flavor have good stability.

[table 5]

The raw material title	Use level (g)
		Carbohydrate	1.50
The salt salt	0.33
		Sweetener	0.01
VC	0.05
		Fruit juice	0.10
Spices	0.20
		Catechin preparation (embodiment 1)	1.28
Ion exchange water	Surplus
		Add up to	100

Embodiment 11

In the 4500g deionized water, in 25 ℃ of thick catechin preparations of stirring and dissolving 150g (Mitsui Norin Co., Ltd.'s production, non-polymer catechin concentration=32.0 weight %, the ratio=52.2 weight % of non-polymer catechin and gallate body, caffeine=5.88 weight %) 30 minutes, obtain green-tea extract lysate (pH5.3).Then, for the 861mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production) that in stainless steel column 1 (internal diameter 60mm * high 360mm, volume 1017.4mL), fills, in advance with SV=5 (h ^-1) clean with 95 (v/v) ethanol of 3444mL, then, with SV=5 (h ^-1) clean with the water of 8610mL.For the 350.6mL ion exchange resin SK1BH (Mitsubishi ChemicalCorporation production) that in stainless steel column 2 (internal diameter 38mm * height 340mm, volume 385.4mL), fills, in advance with SV=5 (h ^-1) clean with 95 (v/v) ethanol of 1402.4mL, then, with SV=5 (h ^-1) clean with the water of 3506mL.After this, with SV=1 (h ^-1) in stainless steel column 1, pass through 3435mL (to 4 times of volumes of synthetic adsorbent) green-tea extract lysate, discard through liquid.Then, with SV=2 (h ^-1) clean with the water of 861mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 12900mL (to 15 times of volumes of synthetic adsorbent) 0.1 weight % sodium hydrate aqueous solution (pH12.5), obtain non-polymer catechin eluent.Eluent continue in stainless steel column 2 by, carry out the deionization operation, obtain 12860g (pH3.5) non-polymer catechin compound composition.Containing 0.24 weight % non-polymer catechin in this extract, is 92.4% from the rate of recovery of the non-polymer catechin of tea extraction lysate, and the ratio of the gallate body of non-polymer catechin compound composition is 52.9 weight %.In addition, caffeine is 0 weight %.Non-polymer catechin in the tea extraction solid constituent is 69.2 weight %.Again under 40 ℃, the condition of 2.6Kpa, to be concentrated to the non-polymer catechin be concentration 6% (turbidity 322NTU) in decompression in decompression concentrates, and obtains " concentrated green-tea extract 1 ".Then, carry out centrifugation (8000r/min) in 15 minutes and outstanding absurd creature Separation of Solid and Liquid, obtain " purified green-tea extract 1 " (turbidity 39.5NTU) at 25 ℃.

Embodiment 12

Make " concentrating green-tea extract 1 " of in embodiment 11, obtaining, obtain " purified green-tea extract 2 " (turbidity 1.8NTU) by the cellulose ethanoate film (ADVANTEC:C080A090C) of 0.8 μ m, the separation of hanging absurd creature.

Embodiment 13

3kg green tea (Kenya's product, large leaf) is added 88 ℃ of hot water 45kg, stir 60 minutes, intermittently extract after, after 100 order wire netting coarse filtration, carry out the centrifugation operation in order to remove the micro mist in the extract, obtain 37.2kg (pH5.4) " green tea extractive liquor ".(ratio of the gallate body of the non-polymer catechin concentration in the green tea extractive liquor=0.89 weight %, green tea extractive liquor=52.3 weight %, caffeine 0.17 weight %).

This green tea extractive liquor is remained on 15 ℃ of temperature, add tannase (KIKKOMANCorporation production, tannase KTFH, 500U/g) and make its concentration become 430ppm with respect to green tea extractive liquor, kept 55 minutes, when the ratio of gallate body becomes 30.5 weight %, solution is heated to 90 ℃, keeps making enzyme deactivation in 2 minutes, stop reaction (pH5.1).Then, under 70 ℃, the condition of 6.7Kpa, carry out concentration and reach 20%, implement spray-drying again, obtain 0.9kg pulverous " green-tea extract that tannase is handled " up to Brix concentration.In resulting green-tea extract, non-polymer catechin content is that the ratio of the gallate body of 27.8 weight %, non-polymer catechin is that 30.3 weight %, content of caffeine are 6.74 weight %.In the 300g deionized water, at 25 ℃ of stirring and dissolving 10g " green-tea extract that tannase is handled " 30 minutes (tannase treatment fluid).

Then, for the 36.1mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production) that in stainless steel column 3 (internal diameter 22mm * height 96mm, volume 36.5mL), fills, in advance to clean with embodiment 1 same method, and for the 14.7mL ion exchange resin SK1BH (Mitsubishi Chemical Corporation production) that in glass column (internal diameter 16mm * height 80mm, volume 16.1mL), fills, in advance to clean with embodiment 1 same method.After this, in stainless steel column 3, with SV=1 (h ^-1) by the resulting tannase treatment fluid of 144.4g (to 4 times of volumes of synthetic adsorbent), the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 36.1mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 561.8mL (to 15 times of volumes of synthetic adsorbent) 0.1 weight % sodium hydrate aqueous solution (pH12.4).Eluent continue in glass column by, to carry out the deionization operation, obtain 552g (pH2.7) non-polymer catechin compound composition.In this extract, contain 0.21 weight % non-polymer catechin, from the rate of recovery of the non-polymer catechin of tannase treatment fluid be 90.3%, the ratio of the gallate body of non-polymer catechin compound composition is 32.5 weight %.In addition, caffeine is 0 weight %.Non-polymer catechin in the tea extraction solid constituent is 64.7 weight %.With 40 ℃, the 2.6Kpa concentration that reduces pressure, be concentrated to non-polymer catechin concentration and reach 6% (turbidity 618NTU) again, obtain " concentrating green-tea extract 2 ".Then, make it cellulose ethanoate film (ADVANTEC:C080A090C) and outstanding absurd creature Separation of Solid and Liquid, obtain " purified green-tea extract 3 " (turbidity 1.5NTU) by 0.8 μ m.

Comparative example 5

In embodiment 11, " concentrate green-tea extract 1 " before the turbidity removal.

Comparative example 6

Except the amount with ion exchange resin is kept to 1/4 amount, the adjusted value of the pH of alkaline eluant is beyond 9.1, to obtain " concentrating green-tea extract 3 " with comparative example 5 same methods.

Embodiment 14

Use embodiment 12 " purified green-tea extract 2 " to be formulated in the container-packed beverage of putting down in writing in the table 7.Carry out based on the sterilization treatment of food hygiene law and hot packing is filled and with it as container-packed beverage.

Estimate after 30 days at 37 ℃ of container-packed beverages of preserving manufacturing.Outward appearance and be the flavor have good stability.

[table 7]

The raw material title	Cooperation ratio (weight %)
		Carbohydrate	1.50
Salt	0.33
		Sweetener	0.01
VC	0.05
		Fruit juice	0.10
Spices	0.20
		Catechin preparation (embodiment 12)	2.11
Ion exchange water	Surplus
		Add up to	100.00

In embodiment 11～13, the non-polymer catechin rate of recovery height before and after handling can obtain caffeine concentration and reduce, and is flavor and stable improved purified green-tea extract.In embodiment 14, the beverage that can also make outward appearance and be the good stability of distinguishing the flavor of.In comparative example 5, bitter taste and hue difference, residual bitter taste and assorted flavor in comparative example 6.

(assay method of tannase activity)

The citric acid solution 50mmol of reagent A: pH5.5: dissolving 10.5g citric acid in 800mL distilled water be adjusted into pH5.5 with the sodium OH solution of 1N, and dilution is 1000mL.

The reagent B:0.35 weight % matrix aqueous solution (tannic acid): dissolving 175mg tannic acid in 50mL citric acid solution (reagent A).

Reagent C: 90vol% ethanolic solution.

Assay method

1. in test tube, get 1.0mL matrix solution (reagent B), kept 5 minutes at 30 ℃.

2. add the 0.25mL sample solution, cultivated 15 minutes at 30 ℃.Add citric acid solution (reagent A) in the blank solution and replace sample solution.

3. in order to stop enzyme reaction, in sample solution and blank solution, add the ethanolic solution (reagent C) of 5.0mL.

4. measure the absorbance [sample: A of 310nm _S, blank: A ₀].

By following calculating formula calculated activity.

The activity of unit volume (U/mL)=(A _S-A ₀) * 20.3 * 1.0 (mL) * 1.04 * df/ (0.71 * 0.25 (mL) * 15 (min))=Δ A * 7.93 * df

The activity of unit mass (U/g)=(U/mL) * 1/C

20.3: contained tannic acid μ mol in 1.0mL matrix solution (reagent B).

0.71: the absorbance variable quantity under analysis condition after the 20.3 μ mol tannic acid complete hydrolysis; 1.04: conversion coefficient; Df: the coefficient of dilution; C: the tannase concentration in the sample (g/mL).

(flavor evaluation after the sterilization)

Be diluted in the tea extraction that obtains among each embodiment with deionized water, and make catechin containing ratio wherein become 0.175%[w/v], this 40mL is joined in the withstand voltage glass container of 50mL.Add 0.1 weight % sodium ascorbate therein, pH be adjusted into 6.4, carry out nitrogen replacement with 5% sodium bicarbonate aqueous solution, with autoclave 121 ℃ of heat sterilizations 10 minutes.After this, be confirmed to be the peculiar smell foreign odor of not feeling from green tea by 5 evaluation personnel.

Embodiment 15

1.8kg green tea (Chinese yunnan is economized product, large leaf) is added 90 ℃ of hot water 27kg, stir 30 minutes, intermittently extract after, after 100 order wire netting coarse filtration, centrifugation operation, carry out the filtration of No. 2 filter paper, obtain 20.4kg (pH5.3) " green tea extractive liquor ".(ratio of the gallate body of the non-polymer catechin concentration of green tea extractive liquor=0.96 weight %, green tea extractive liquor=69.5 weight %, caffeine 0.24 weight %, gallic acid=0.01 weight %).

This green tea extractive liquor is set in 25 ℃ of temperature, add tannase (KIKKOMANCorporation production, tannase KTFH, 500U/g) and make its concentration become 300ppm with respect to green tea extractive liquor, kept 85 minutes, when the ratio of gallate body becomes 52.4 weight %, solution is heated to 90 ℃, keeps making enzyme deactivation in 2 minutes, stop reaction (pH4.8, tannase treatment fluid (1)).

Then, for the 2048mL synthetic adsorbent SP-70 (Mitsubishi ChemicalCorporation production) that in stainless steel column 1 (internal diameter 110mm * height 230mm, volume 2185mL), fills, in advance with SV=5 (h ^-1) clean with 95 (v/v) ethanol of 8192mL, then, with SV=5 (h ^-1) clean with 20480mL water.For the 852mL ion exchange resin SK1BH (Mitsubishi Chemical Corporation production) that in stainless steel column 2 (internal diameter 38mm * height 770mm, volume 873mL), fills, in advance with SV=5 (h ^-1) clean with 95 (v/v) ethanol of 3408mL, then, with SV=5 (h ^-1) clean with 8520mL water.After this, in post 1, with SV=1 (h ^-1) by 8192g (to 4 times of volumes of synthetic adsorbent) tannase treatment fluid (1), the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 2048mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 30720mL (to 15 times of volumes of synthetic adsorbent) 0.1 weight % sodium hydrate aqueous solution (pH12.5), obtain the catechin eluent.Eluent continue in stainless steel column 2 by, carry out the deionization operation, obtain 28222g (pH3.0) non-polymer catechin compound composition.In this extract, contain 0.24 weight % non-polymer catechin, from the non-polymer catechin rate of recovery of tannase treatment fluid (1) be 92.9%, the ratio of the gallate body of non-polymer catechin compound composition is 55.3 weight %.In addition, caffeine is that 0 weight %, gallic acid are 0.001 weight %.Non-polymer catechin in the tea extraction solid constituent is 62.4 weight %.

Comparative example 7

Similarly carry out tannase with embodiment 15 and handle, do not carry out logical liquid and wash-out to synthetic adsorbent.

Comparative example 8

Do not carry out tannase handle beyond and embodiment 15 fully similarly carry out.

Embodiment 16

(1) 3kg green tea (Kenya's product, large leaf) is added 88 ℃ of hot water 45kg, stir 60 minutes, intermittently extract after, with 100 order wire netting coarse filtration, for the micro mist of removing in the extract carries out the centrifugation operation, obtain 37.2kg (pH5.4) " green tea extractive liquor ".(ratio of the gallate body of the non-polymer catechin concentration in the green tea extractive liquor=0.89 weight %, green tea extractive liquor=52.3 weight %, caffeine 0.17 weight %).

This green tea extractive liquor is remained on 15 ℃, add tannase (KIKKOMANCorporation production, tannase KTFH, 500U/g) and make its concentration become 430ppm with respect to green tea extractive liquor, kept 55 minutes, when the ratio of gallate body becomes 30.5 weight %, solution is heated to 90 ℃, keeps making enzyme deactivation in 2 minutes, stop reaction (pH5.1).Then, under 70 ℃, the condition of 6.7Kpa, carry out concentration, reach 20%, carry out spray-drying again, obtain 0.9kg pulverous " green-tea extract that tannase is handled " up to Brix concentration in the mode of concentrating that reduces pressure.In the resulting green-tea extract, non-polymer catechin content is that the ratio of 27.8 weight %, non-polymer catechin and gallate body is that 30.3 weight %, content of caffeine are that 6.74 weight %, gallic acid are 3.58 weight %.In the 300g deionized water, in 25 ℃ of stirring and dissolving 10g " green-tea extract that tannase is handled " 30 minutes (tannase treatment fluid (2)).

Then, for the 36.1mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production) that in stainless steel column 3 (internal diameter 22mm * height 96mm, volume 36.5mL), fills, in advance to clean with embodiment 1 same method, for the 14.7mL ion exchange resin SK1BH (Mitsubishi Chemical Corporation production) that in glass column (internal diameter 16mm * height 80mm, volume 16.1mL), fills, in advance to clean with embodiment 1 same method.After this, in post 1, with SV=1 (h ^-1) by 144.4g (to 4 times of volumes of synthetic adsorbent) resulting tannase treatment fluid (2), the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 36.1mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 561.8mL (to 15 times of volumes of synthetic adsorbent) 0.1 weight % sodium hydrate aqueous solution (pH12.4).Eluent continue in glass column by, carry out the deionization operation, obtain 552g (pH2.7) non-polymer catechin compound composition.In this extract, contain 0.21 weight % non-polymer catechin, from the rate of recovery of the non-polymer catechin of tannase treatment fluid (2) be 90.3%, the ratio of the gallate body of non-polymer catechin compound composition is 32.5 weight %.In addition, caffeine is that 0 weight %, gallic acid are 0.002 weight %.Non-polymer catechin in the tea extraction solid constituent is 64.7 weight %.

Embodiment 17

In the 300g deionized water, in 25 ℃ of thick catechin preparations of stirring and dissolving 10g (Mitsui Norin Co., Ltd.'s production, non-polymer catechin concentration=32.0 weight %, the ratio=52.0 weight % of non-polymer catechin and gallate body, caffeine=5.51 weight %, gallic acid=0.17 weight %) 30 minutes, obtain tea extraction lysate (pH5.3).Then, add tannase (KIKKOMAN Corporation production, tannase KTFH, 500U/g) and make its concentration become 500ppm with respect to the tea extraction lysate, kept 120 minutes at 15 ℃, when the ratio of gallate body becomes 4 weight %, solution is heated to 90 ℃, keep making enzyme deactivation in 2 minutes, stop reaction (pH4.2, tannase treatment fluid (3)).

Except raw material is above-mentioned tannase treatment fluid, with embodiment 16 in make with extra care under same post and the operating condition, obtain 534.2g (pH3.7) non-polymer catechin compound composition.In this extract, contain 0.18 weight % non-polymer catechin, from the non-polymer catechin rate of recovery of tannase treatment fluid (3) be 91.3%, the ratio of the gallate body of non-polymer catechin compound composition is 6.0 weight %.In addition, caffeine is that 0 weight %, gallic acid are 0.004 weight %.Non-polymer catechin in the tea extraction solid constituent is 57.6 weight %.

Embodiment 18

For the 1004mL synthetic adsorbent SP-207 (Mitsubishi Chemical Corporation production) that in stainless steel column 4 (internal diameter 60mm * height 360mm, volume 1017mL), fills with SV=5 (h ^-1) use 95 (v/v) ethanol of 4016mL to clean in advance, then, with SV=5 (h ^-1) clean with 10040mL water.For the 1338mL ion exchange resin SK1BH (Mitsubishi Chemical Corporation production) that in stainless steel column 5 (internal diameter 38mm * height 1200mm, volume 1360mL), fills with SV=5 (h ^-1) use 95 (v/v) ethanol of 5352mL to clean in advance, then, with SV=5 (h ^-1) clean with 13380mL water.In stainless steel column 4, with SV=1 (h ^-1) by 4016g (to 4 times of volumes of synthetic adsorbent) the tannase treatment fluid among the embodiment 15, the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 1004mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 5020mL (to 5 times of volumes of synthetic adsorbent) 1 weight % sodium hydrate aqueous solution (pH14.0).Eluent continues by stainless steel column 5, carries out the deionization operation, obtains 4975.5g (pH4.1) non-polymer catechin compound composition.In this extract, contain 0.63 weight % non-polymer catechin, from the non-polymer catechin rate of recovery of tannase treatment fluid (1) be 88.2%, the ratio of the gallate body of non-polymer catechin compound composition is 58.3 weight %.In addition, caffeine is that 0 weight %, gallic acid amount are 0.001 weight %.Non-polymer catechin in the tea extraction solid constituent is 59.3 weight %.

Embodiment 19

The loading of the ion exchange resin SK1BH of embodiment 16 is beyond the 3.6mL, carries out the operation same with embodiment 16.The extract that obtains contains 0.17 weight % non-polymer catechin, from the non-polymer catechin rate of recovery of tannase treatment fluid (2) be 78.2%, the ratio of the gallate body of non-polymer catechin compound composition is 35.8 weight %.In addition, caffeine is that 0 weight %, gallic acid amount are 0.001 weight %.Non-polymer catechin in the tea extraction solid constituent is 43.3 weight %.

Comparative example 9

For the 860mL synthetic adsorbent SP-70 (Mitsubishi Chemical Corporation production) that in stainless steel column 4 (internal diameter 60mm * height 360mm, volume 1017mL), fills with SV=5 (h ^-1) use 95 (v/v) ethanol of 3440mL to clean in advance, then, with SV=5 (h ^-1) clean with 8600mL water.In stainless steel column 4, with SV=1 (h ^-1), by the 3440g tannase treatment fluid (to 4 times of volumes of synthetic adsorbent) among the embodiment 15, the discarded liquid that sees through.

Then, with SV=2 (h ^-1) clean with the water of 860mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=2 (h ^-1) by 5160mL (to 6 times of volumes of synthetic adsorbent) 20 weight % ethanol waters.Steam ethanol with 40 ℃, 2.7Kpa, after this, the extract that adjust the water yield, obtains contains 0.50 weight % non-polymer catechin, from the non-polymer catechin rate of recovery of tannase treatment fluid (1) be 84.4%, the ratio of the gallate body of non-polymer catechin compound composition is 45.9 weight %.In addition, caffeine is that 0.1 weight %, gallic acid amount are 0.008 weight %.Non-polymer catechin in the tea extraction solid constituent is 60.8 weight %.

Comparative example 10

In the 92.4 weight % ethanol waters of 800g, 100g Emathlite (MIZUKA-ACE #600, marshy land chemical industry (strain) are produced) is disperseed, behind the stir about 10 minutes, the green-tea extract that the tannase that input 200g obtains in embodiment 16 is handled continues in about 3 hours of stirring at room (pH4.0).After this, filter precipitation and the Emathlite that generates with No. 2 filter paper.Make the filtrate and 30g activated carbon (KURARAYCOAL GLC, KURARAY CHEMICAL CO., the LTD. produces) contact that obtain, then filter with 0.2 μ m molecular filter.At last, add the 200g ion exchange water, steam ethanol, after this, adjust the water yield and obtain " purified green-tea extract " with 40 ℃, 2.7Kpa.The extract that obtains contains 20.2 weight % non-polymer catechins, and the non-polymer catechin rate of recovery of the green-tea extract of handling from the tannase of embodiment 16 is 60.5%, the ratio of the gallate body of non-polymer catechin compound composition is 29.3 weight %.In addition, caffeine is that 0.73 weight %, gallic acid amount are 2.56 weight %.Non-polymer catechin in the tea extraction solid constituent is 56.6 weight %.

The tea extraction of embodiment 15～19, comparative example 7～10 being put down in writing based on food hygiene law carries out sterilization treatment, estimates local flavor and bitter taste.Its result of expression in table 8.

In embodiment 15～19, the rate of recovery height of the non-polymer catechin before and after can obtaining handling, the ratio of non-polymer catechin and gallate body reduce, contain hardly the tea extraction of gallic acid, the reduction of caffeine concentration.In embodiment 20, can also make outward appearance and be the beverage that flavor has good stability.Residual tart flavour and assorted flavor in comparative example 7, residual bitter taste in comparative example 8.Content of caffeine is many in comparative example 9, residual tart flavour in comparative example 10.

Embodiment 20

Use the purified green-tea extract of embodiment 17 to be formulated in the container-packed beverage of putting down in writing in the table 9.Based on food hygiene law carry out sterilization treatment and hot packing and with it as container-packed beverage.

Preserving the container-packed beverage of making at 37 ℃ estimated after 30 days.Outward appearance and be the flavor have good stability.

[table 9]

The raw material title	Use level (%)
		Carbohydrate	1.50
Salt	0.33
		Sweetener	0.01
VC	0.05
		Fruit juice	0.10
Spices	0.20
		Purified green-tea extract (embodiment 17)	70.83
Ion exchange water	Surplus
		Add up to	100.00

Embodiment 21

In the 4500g deionized water, at 25 ℃ of thick catechin preparation (MitsuiNorin Co. of stirring and dissolving 150g, Ltd. production, non-polymer catechin concentration=32.0 weight %, the ratio=47.8 weight % of non-polymer catechin and gallate body, caffeine=5.88 weight %) 30 minutes, obtain tea extraction (pH5.3).Then, for the 861mL synthetic adsorbent SP-207 (Mitsubishi Chemical Corporation production) that in stainless steel column 1 (internal diameter 60mm * height 360mm, volume 1017.4mL), fills with SV=5 (h ^-1) use 95 (v/v) ethanol of 3444mL to clean in advance, then, with SV=5 (h ^-1) clean with 8610mL water.For the 350.6mL ion exchange resin SK1BH (Mitsubishi ChemicalCorporation production) that in stainless steel column 2 (internal diameter 38mm * height 340mm, volume 385.4mL), fills with SV=5 (h ^-1) use 95 (v/v) ethanol of 1402.4mL to clean in advance, then, with SV=5 (h ^-1) clean with 3506mL water.After this, in stainless steel column 1, with SV=1 (h ^-1) by 3435g (to 4 times of volumes of synthetic adsorbent) tea extraction, the discarded liquid that sees through.Then, with SV=2 (h ^-1) clean with the water of 861mL (to 1 times of volume of synthetic adsorbent).After the washing, with SV=5 (h ^-1) by 12900mL (to 15 times of volumes of synthetic adsorbent) as 0.01 weight % sodium hydrate aqueous solution (pH11.5) of eluent, obtain fraction.Fraction continue in stainless steel column 2 by, carry out deionization and handle, obtain 12860g (pH3.5) purified tea extract.At the non-polymer catechin with absorption is 100 o'clock, and the non-polymer catechin in the purified tea extract is 31.0%.

Embodiment 22

Except with SV=2 (h ^-1) by 860mL (to 1 times of volume of synthetic adsorbent) as 20 weight % ethanol waters of eluent and do not carry out beyond the fraction deionization handles, carry out the operation same with embodiment 21.At the non-polymer catechin with absorption is 100 o'clock, and the non-polymer catechin in the purified tea extract is 41.0%.

Comparative example 11

Except with SV=5 (h ^-1) by 12900mL (to 15 times of volumes of synthetic adsorbent) in addition, carry out the operation same with embodiment 21 as 0.1 weight % sodium hydrate aqueous solution (pH12.5) of eluent.At the non-polymer catechin with absorption is 100 o'clock, and the non-polymer catechin in the purified tea extract is 92.4%.

Comparative example 12

Except with SV=2 (h ^-1) by beyond the 20 weight % ethanol waters of 5170mL (to 6 times of volumes of synthetic adsorbent) as eluent, carry out the operation same with embodiment 22.At the non-polymer catechin with absorption is 100 o'clock, and the non-polymer catechin in the purified tea extract is 85.0%.

The result of expression embodiment 21,22, comparative example 11,12 in table 10.

[table 10]

As known from Table 10, after making synthetic adsorbent absorption tea extraction, make detergent remover contact synthetic adsorbent, then make eluent contact synthetic adsorbent, fractionation conditions is satisfied fractionate out 10～60% of the non-polymer catechin that on synthetic adsorbent, adsorbs, can obtain that content of caffeine is low, the ratio height of the non-gallate body of non-polymer catechin, tea local flavor and bitter taste reduces, local flavor improves purified tea extract.Therefore, this extract is useful as the teas beverage not only, and also is useful as non-teas beverage.

Claims (17)

1. the manufacture method of a purified tea extract is characterized in that,

Tea extraction is adsorbed on the synthetic adsorbent, thereby then makes alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent make non-polymer catechin wash-out, then described eluent is contacted with activated carbon.

2. the manufacture method of a purified tea extract is characterized in that,

Tea extraction is adsorbed on the synthetic adsorbent, thereby then make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent make non-polymer catechin wash-out, the pH of eluent is adjusted into below 7, concentrates, then remove the outstanding absurd creature of separating out with Separation of Solid and Liquid.

3. the manufacture method of a purified tea extract is characterized in that,

Make after tea extraction is adsorbed on the synthetic adsorbent, make cleaning solution contact synthetic adsorbent, then make aqueous solutions of organic solvent or alkaline aqueous solution contact synthetic adsorbent, the fractionation tea extraction, ratio as the non-gallate body of non-polymer catechin in this tea extraction is 55～100%, and caffeine/non-polymer catechin is below 0.15.

4. as any 1 described manufacture method of claim 1～3,

Described tea extraction is to be hydrolyzed the extract of handling.

5. the manufacture method of a purified tea extract is characterized in that,

With the tea extraction hydrolysis, then make it after absorption on the synthetic adsorbent, thereby make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent wash-out non-polymer catechin.

6. as claim 1,2,4 or 5 described manufacture methods, it is characterized in that,

After absorption process finishes, clean synthetic adsorbent, then make alkaline aqueous solution or aqueous solutions of organic solvent contact synthetic adsorbent.

7. as any 1 described manufacture method of claim 1～6, it is characterized in that,

Described organic solvent is an ethanol.

8. as any 1 described manufacture method of claim 1～7, it is characterized in that,

Described synthetic adsorbent is acrylic resin, methacrylic resin, polythylene resin or styrene resin.

9. as claim 4 or 5 described manufacture methods, it is characterized in that,

Hydrolysis process is the processing of being undertaken by the enzyme with tannase activity, thalline or nutrient solution.

10. as any 1 described manufacture method of claim 1～9, it is characterized in that,

In the resulting purified tea extract, contain 25～90 weight % non-polymer catechins with respect to solid constituent.

11. any 1 the described manufacture method as claim 1～9 is characterized in that,

In the resulting purified tea extract, contain 25～90 weight % non-polymer catechins with respect to solid constituent, and the ratio of caffeine and non-polymer catechin is 0～0.15.

12. any 1 the described manufacture method as claim 1～9 is characterized in that,

In the resulting purified tea extract, contain 25～90 weight % non-polymer catechins with respect to solid constituent, the ratio of caffeine and non-polymer catechin is 0～0.15, the ratio of the gallate body in the non-polymer catechin is 0～70 weight %, and the ratio of gallic acid and non-polymer catechin is 0～0.1.

13. a purified tea extract is characterized in that,

The content of the non-polymer catechin in the solid constituent is 25～95 weight %, the ratio of the gallate body in the non-polymer catechin is 0～70 weight %, the ratio of gallic acid and non-polymer catechin is 0～0.1, and the ratio of caffeine and non-polymer catechin is 0～0.15.

14. a purified tea extract is characterized in that,

The content of the non-polymer catechin in the solid constituent is 25～95 weight %, the ratio of the gallate body in the non-polymer catechin is 0～70 weight %, the ratio of gallic acid and non-polymer catechin is 0～0.1, the ratio of caffeine and non-polymer catechin is 0～0.2

When the concentration that this purified tea extract is made the non-polymer catechin is the aqueous solution of 1 weight %, be 0～0.8 at the tone of 450nm.

15. a purified tea extract is characterized in that,

The content of the non-polymer catechin in the solid constituent is 45～90 weight %, and the ratio of the gallate body in the non-polymer catechin is 0.001～47 weight %, and the weight ratio of gallic acid amount/non-polymer catechin is below 0.3.

16. a purified tea extract is obtained by any 1 described manufacture method of claim 1～12.

17. a container packed tea beverage wherein cooperates any 1 described purified tea extract of claim 13～16.