JP2010207172A - Theanine-containing composition and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a theanine-containing composition that is obtained by separation from and purification of a green tea extract, contains not less than 30 mass% of theanine and has a low potassium content. <P>SOLUTION: The theanine-containing composition containing not less than 30 mass% of theanine and having a low potassium content is obtained by enzymatically treating a green tea extract using inulinase to give an enzymatically treated solution, separating the enzymatically treated solution by a column chromatography into a theanine-containing fraction and an admixture fraction other than the teanine-containing fraction to recover the theanine-containing fraction. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a theanine-containing composition containing 30% by mass or more of theanine, and a method for producing the theanine-containing composition from a green tea extract.

  L-Theanine is a kind of amino acid, a derivative of glutamic acid, and is known as one of the umami components of tea. Theanine has also been found to have physiological activities particularly favorable for elderly people, such as a brain function-improving action, in addition to physiological activities such as caffeine-induced excitement-suppressing action, blood pressure-lowering action, and relaxing action (Patent Document 1). -3).

Theanine has been confirmed to exist only in tea (Camellia sinensis or Thea sinensis) and its close relatives among plants. In tea, many theanines are contained in high-grade tea made from shoots, gyokuro, bud tea, and matcha tea obtained by covering cultivation of tea trees.
However, the theanine content in tea leaves is about 1-2% by weight of dry tea leaves, which is considerably less than tea polyphenols (10-15% by weight), so theanine-containing composition is separated from the green tea extract. Various devices are required for purification.

  For example, in Patent Document 4, a tea extract is passed through a container filled with an adsorbent at a volume ratio (tea extract / adsorbent) = 1.5 or less, and theanine in the extract is adsorbed to the adsorbent. An adsorbing step, a liquid passing step of passing water as an eluate through the container after the passage of the extract, and a water flow of the tea extract and / or the eluate through the container. The removal step of recovering the initial discharge fraction obtained by the process in an amount of 0.5 to 2 times the volume of the adsorbent to remove the contaminant component group, and the remaining discharge fraction of water as the eluate A method for producing theanine having a recovery step of recovering and obtaining a theanine-containing eluate is disclosed.

  In Patent Document 5, a tea extract having a theanine purity of 15% or more is passed through a container filled with an adsorbent at a liquid passing rate of 3 or less to obtain theanine having a purity of 60% or more. A method for producing theanine is disclosed.

Claim 1 of JP-A-08-73350 Claim 1 of JP-A-2000-229854 Claim 1 of JP-A-2001-48797 Claim 1 of JP-A-2004-010545 Claim 1 of JP2007-8865

As described above, it is not easy to separate and purify a theanine-containing composition from a green tea extract. In particular, it is not possible to separate and purify a theanine-containing composition containing 30% by mass or more of theanine. It was difficult.
Moreover, since green tea contains potassium, when it tries to obtain the theanine containing composition from a green tea extract, potassium will be contained in it. However, if renal function is normal, potassium that should be excreted may not be excreted properly if the renal function is reduced, such as in elderly people, which may cause heart-related diseases such as arrhythmia. Therefore, it is desirable to reduce potassium as much as possible for the theanine-containing composition so that even a person with impaired kidney function can take it with peace of mind.

  Accordingly, an object of the present invention is to provide a theanine-containing composition obtained by separating and purifying from a green tea extract, which contains 30% by mass or more of theanine and has a low potassium content. It is what.

The present invention proposes a new theanine-containing composition characterized in that it contains 30% by mass or more of theanine and 5% by mass or less of potassium as a new theanine-containing composition that has not been conventionally known. To do.
The theanine-containing composition of the present invention can be in any state such as powder, liquid, or gel. Further, when the theanine-containing composition is not in a dry state, the mass% of each component means a mass ratio in terms of dry mass (hereinafter the same).

  Since the theanine-containing composition of the present invention contains 30% by mass or more of theanine, it can be added to various foods and drinks for the purpose of enhancing umami or imparting various physiological activities. Can also be used. Moreover, since the potassium content is suppressed to 5% by mass or less, even a person with impaired renal function can take it with peace of mind.

  The present invention also provides a method for producing a new theanine-containing composition, which has not been known so far, by performing enzyme treatment of a green tea extract using inulinase to obtain an enzyme-treated solution, and the enzyme-treated solution is subjected to column chromatography. The present invention also proposes a method for producing a theanine-containing composition characterized in that the theanine-containing fraction and the other contaminated fraction are collected by chromatography to collect the theanine-containing fraction.

  According to the method for producing a theanine-containing composition of the present invention, a theanine-containing composition having a high theanine content and a low potassium content is produced as described above, without using high-quality tea or tea from coated cultivation as a raw material. be able to.

In Example 1, 2, and the comparative example 1, it is the graph which showed the separation behavior of theanine at the time of chromatographic separation. In Example 1, 2, and the comparative example 1, it is the graph which showed the separation behavior of theogarin at the time of chromatographic separation. In Example 1, 2 and Comparative Example 1, it is the graph which showed the separation behavior of glucose at the time of chromatographic separation. In Example 1, 2 and Comparative Example 1, it is the graph which showed the separation behavior of fructose at the time of carrying out chromatographic separation. In Example 1, 2, and the comparative example 1, it is the graph which showed the separation behavior of the sucrose at the time of carrying out the chromatographic separation. In Example 1, 2, and the comparative example 1, it is the graph which showed the separation behavior of potassium at the time of chromatographic separation. In Examples 1 and 2 and Comparative Example 2, it is the graph which showed the separation behavior of theanine at the time of chromatographic separation.

  Hereinafter, although embodiment of this invention is described, this invention is not limited to the following embodiment.

<Method for producing theanine-containing composition>
The theanine-containing composition according to the present embodiment (hereinafter referred to as “the theanine-containing composition”) is obtained by separating and purifying a tea extract obtained by extracting green tea as necessary, and then using an inulinase for the enzyme. Treatment, concentrating as necessary to obtain an enzyme-treated solution, and separating the obtained enzyme-treated solution into a theanine-containing fraction and other contaminated fractions by column chromatography. Can be obtained by concentrating and drying as necessary. At this time, it is preferable to perform a treatment for removing catechin or caffeine from the tea extract in advance before the enzyme treatment with inulinase. Details will be described below.

(Green Tea)
The green tea may be any of buds, leaves, and stems of Camellia sinensis var., Or a mixture thereof, and can be used regardless of the variety or production area.
Speaking from the viewpoint of containing more theanine, among green teas (sencha, gyokuro, kabusecha, bancha, tamamocha, matcha, hojicha, pot-fried tea, tencha, etc.) Gyokuro, strawberry tea, matcha tea and the like obtained by covering cultivation are preferred. However, the production method of the present invention is characterized in that the present theanine-containing composition can be obtained using lower tea leaves or tea extracts as raw materials.
Moreover, even fresh tea, that is, green tea that has not been processed yet, may have been subjected to pretreatment such as steaming.

(Extraction)
Extraction of green tea may be performed using water, warm water or hot water, or an organic solvent such as an ethanol aqueous solution or ethanol that is harmless to the human body.

  Although extraction temperature is not specifically limited, From a viewpoint of raising the extraction rate of a green tea component, it is preferable to extract with hot water of 40-100 degreeC, especially 70-100 degreeC, especially 90-100 degreeC. On the other hand, since it is preferable to extract at a low temperature from the viewpoint of increasing the extraction rate of theanine, it is preferable to extract with water at 70 ° C. or less, particularly 60 ° C. or less, especially 45 to 55 ° C. from this viewpoint.

  The tea extract obtained by extracting green tea usually contains amino acids, organic acids, polyphenols (mainly catechin), caffeine, vitamins, sugars, water-soluble dietary fiber, minerals (including potassium), etc. Will be included.

(Separation / Purification)
The tea extract obtained as described above contains more polyphenol (particularly catechin) and theanine by separation / purification means such as solvent extraction method, resin adsorption method, filtration such as ultrafiltration and reverse osmosis filtration. It is preferable to separate and purify as described above. However, such separation / purification is not necessarily performed.

In addition, the green tea is extracted and separated / purified as described above to obtain a tea extract, but the commercially available tea extract obtained by performing green tea extraction, separation and purification is used to A tea extract obtained by dissolving the tea extract in a solvent such as pure water can also be used.
As a commercially available tea extract, for example, Teafuran 30E (trade name; manufactured by ITO EN) can be preferably used. Teafuran 30E is a green tea extract obtained by subjecting green tea to hot water extraction and drying the extract to a catechin concentration of 30%. In addition, “Polyphenone” manufactured by Mitsui Norin Co., Ltd., “Sunphenon” manufactured by Taiyo Kagaku Co., Ltd., “Sun Oolong” manufactured by Suntory Ltd., etc. can be used as commercially available tea extracts.

(Removal of catechin or caffeine)
Since catechin contained in the green tea extract inhibits the function of inulinase, it is preferable to perform a pretreatment for removing catechin in advance before the enzyme treatment with inulinase. At this time, since caffeine is also an inhibitory component, it is preferable to remove caffeine in advance.

As a target value, for example, the catechin content in the green tea extract is preferably 5% by mass or less, particularly 3% by mass or less, particularly 1% by mass or less in terms of dry weight.
With respect to caffeine, the caffeine content in the green tea extract is preferably 5% by mass or less, particularly 3% by mass or less, especially 1% by mass or less, in terms of dry weight.

  As a method for removing catechin or caffeine, various known methods can be adopted as long as they are not methods for removing theanine together. Examples thereof include a method of adsorbing and removing catechin or caffeine by bringing a green tea extract into contact with an adsorbent, and a method of distributing and removing catechin or caffeine by a liquid-liquid distribution method using an organic solvent. However, it is not limited to this method.

  Examples of the adsorbent used in the method for adsorbing and removing catechin or caffeine include polyvinyl polypyrrolidone, polyvinyl pyrrolidone, styrene-divinylbenzene adsorbents (such as Diaion HP20 / HP21 manufactured by Mitsubishi Chemical, Sepa Beads manufactured by Mitsubishi Chemical), Methacrylate ester adsorbents (Diaion Diaion HP2MG manufactured by Mitsubishi Chemical), cross-linked dextran gels (such as Pharmacia Sephadex series), hydrophilic vinyl polymer adsorbents (such as Toyopearl HW series manufactured by Tosoh), reverse phase adsorption An adsorbent composed of one or a combination of one or more selected from an adsorbent (such as Wako Pack C18 manufactured by Wako Pure Chemical Industries) and a normal phase adsorbent (such as silica gel) can be given.

Since the green tea extract contains a large amount of catechins, it is more preferable that the green tea extract is contacted with a resin capable of adsorbing and removing both catechin and caffeine and then contacted with a resin capable of adsorbing and removing catechin.
In this case, as a resin capable of adsorbing and removing both catechin and caffeine, for example, the base of the resin is a styrene divinylbenzene series, specifically, Mitsubishi Chemical Corporation Sepabeads SP205, SP206, SP207, Organo Corporation Amberlite XAD-2 XAD-4, XAD-2000, XAD-2010, XAD-2005 styrene-based, for example, Diaion HP20, HP21, Sepabead SP800, SP825, SP850, SP875, SP70 and the like.
Examples of the resin capable of adsorbing and removing catechin include Sephadex series manufactured by Pharmacia, Biogel A series manufactured by Biorad, and Diaion HP2MG manufactured by Mitsubishi Chemical.

  Examples of the organic solvent used in the liquid-liquid distribution method include methanol, ethanol, acetone, methyl acetate, ethyl acetate, and n-butanol.

(Enzyme treatment with inulinase)
The green tea extract contains a large amount of disaccharides and polysaccharides, and these inhibit the separation of theanine and contaminating components in chromatography, thereby reducing the recovery rate of theanine (see Comparative Example 1). . On the other hand, by performing enzyme treatment using inulinase, disaccharides and polysaccharides are decomposed, and separation efficiency between theanine and contaminating components can be increased to increase the yield of theanine (Example 1 and Example). 2).
It has also been confirmed that the flavor of tea is increased by performing an enzyme treatment with inulinase (hereinafter also referred to as “inulinase treatment”).

  In the inulinase treatment, it is preferable to add inulinase at a ratio of 0.05 to 1.0 part by mass with respect to 100 parts by mass of the amount of tea leaves used, particularly 0.05 to 0.5 part by mass, especially 0.05. It is more preferable to add at a ratio of ˜0.1 part by mass.

  As a result of tests on enzymes other than inulinase, it has been confirmed that enzymes such as hemicellulase, xylase, protease, cellulase, and pectinase cannot provide the same effects as inulinase.

(concentrated)
Since the enzyme-treated solution obtained by performing the inulinase treatment as described above has a low concentration, it is preferably concentrated before the separation treatment by column chromatography.
At this time, the degree of concentration is preferably concentrated to Brix 5 to 35, particularly Brix 15 to 35, and particularly Brix 20 to 35.

(Column chromatography)
The enzyme-treated solution obtained as described above is separated into a theanine-containing fraction and other contaminated fractions (including inactivated inulinase) by column chromatography to recover the theanine-containing fraction. That's fine.

  In column chromatography, the enzyme-treated solution is passed through a container (column) filled with an adsorbent resin to adsorb theanine, or adsorb contaminant components other than theanine to obtain the theanine-containing fraction and the fraction. What is necessary is just to adsorb-separate and remove other fractions.

The adsorption resin to be used may be any resin that can separate the theanine-containing fraction from the other contaminated fraction.
For example, as a resin capable of separating a contaminant component other than theanine and a fraction containing theanine, the resin matrix is styrene divinylbenzene, specifically, Mitsubishi Chemical Corporation Sepabeads SP205, SP206, SP207, Organo Amber Light XAD-2, XAD-4, XAD-2000, XAD-2010, XAD-2005 styrene type, for example, Diaion HP20, HP21, Sepabead SP800, SP825, SP850, SP875, SP70, etc. can be used. In particular, a modified styrene type in which a bromine atom is substituted with a nucleus to enhance the adsorptive power, such as Sepabeads SP205, SP206, SP207 (manufactured by Mitsubishi Chemical Corporation) is even more preferable.

The column chromatography here is preferably carried out by passing the distillate at SV = 4 or less, and particularly by passing the distillate at SV = 3 to 1, especially SV = 1.5 to 1. More preferably. At this time, if the distillate is passed at a speed faster than SV = 4, the separation behavior is likely to be disturbed, which is not preferable.
In addition, the liquid flow rate (Space Velocity: SV) is a unit indicating how much of the solution is passed with respect to the capacity of the adsorbent filled in the container per hour. It is shown by “flow rate / adsorbent capacity / time”. For example, SV = 1 when passing an amount of solution equal to the capacity of the adsorbent per hour.

(Concentration and drying)
The present theanine-containing composition may be prepared by concentrating or drying the thus-obtained theanine-containing fraction according to the intended use. At this time, the concentration method and the drying method are arbitrary.

<Theanine-containing composition>
By the production method as described above, the present theanine-containing composition, that is, the theanine content is 30% by mass or more, the potassium content is 5% by mass or less, and the balance is the green tea extract component other than theanine and potassium. A theanine-containing composition can be obtained.
In this case, the theanine content is more preferably 30 to 65% by mass, and particularly preferably 40 to 65% by mass. Further, the potassium content is more preferably 5% by mass or less, and particularly preferably 3 to 1% by mass.

  In addition to theanine, theogarin can also be contained by the production method as described above, so that the theanine content is 30 to 65% by mass, the theogarin content is 10 to 30% by mass, and potassium The present theanine-containing composition having a content of 5% by mass or less and the balance being green tea extract components other than theanine, theogarin and potassium can be obtained.

Further, the present theanine-containing composition has a catechin content and a caffeine content of less than 1% by mass, and the remainder is a tea extract component other than theanine, theogarin, catechin, caffeine and potassium. Can be prepared.
At this time, both the catechin content and the caffeine content are more preferably less than 1% by mass, and particularly preferably less than 0.5% by mass.

Tea extraction components other than theanine, theogarin, catechin, caffeine and potassium include glutamic acid, glutamine, aspartic acid, asparagine, serine, Na ⁺ , Mg ²⁺ , Ca ²⁺ , Cl ⁻ , SO ₄ ²⁻ , malic acid Glucose, fructose, sucrose, alcohol-insoluble polymer components, and the like.

Furthermore, the present theanine-containing composition can be prepared such that the total amount of glucose and fructose is 5% by mass or less. At this time, the total amount of glucose and fructose is preferably 5% by mass or less, and more preferably 3% by mass or less.
Moreover, the total amount of sucrose can be adjusted to 1 mass% or less. At this time, the total amount of sucrose is more preferably 1% by mass or less, and particularly preferably 0.5% by mass or less.

The composition of the preferred theanine-containing composition is as shown in Table 1.
In addition, the unit of the numerical value in Table 1 is mass% (mass ratio of solid content).

(Usage)
Since the theanine-containing composition contains 30% by mass or more of theanine, it can be added to various foods and drinks for the purpose of enhancing umami or imparting various physiological activities, and also as a supplement material as a health food. Can be used. Moreover, since the potassium content is suppressed to 5% by mass or less, even a person with impaired renal function can take it with peace of mind.

(Explanation of terms)
In the present specification, when expressed as “X to Y” (X and Y are arbitrary numbers), unless otherwise specified, “preferably greater than X” and “preferably Y” together with the meaning of “X to Y”. It means “smaller”. Further, X and Y at that time are numerical values considering rounding.
Further, when expressed as “X or more” or “Y or less” (X and Y are arbitrary numbers), it means “preferably larger than X” or “preferably smaller than Y” unless otherwise specified. To do. Further, X and Y at that time are numerical values considering rounding.

  Next, although this invention is further demonstrated based on a test example, this invention is not limited to the Example shown below.

"Analysis conditions"
Each component was quantified and the viscosity was measured as follows.

(Amino acid (theanine) analysis conditions)
HPLC system: Waters Alliance System
Column: Wakosil 3C18HG 150 × 3.0mm.ID
Mobile phase A: 50 mM acetate buffer (pH 6.0)
Mobile phase B: 100% ethanol detection: Fluorescence detector Excitation wavelength 340nm Detection wavelength 450nm
Coloring reagent: OPA reagent Sample injection volume: 5μL
Liquid feed rate: 0.43mL / min

(Theogarin analysis)
HPLC system: Waters Alliance System Column: Waters T3 150 x 3.0mm.ID
Mobile phase A: 20 mM potassium dihydrogen phosphate Mobile phase B: 20 mM potassium dihydrogen phosphate / acetonitrile = 50/50
Detection: UV detector 210nm
Test injection volume: 5μL
Volume of liquid delivered: 0.43 mL / min

(Sugar analysis)
HPLC system: DIONEX
Column: DIONEX AP1 250 × 4.6mm.ID
Mobile phase A: 150 mM NaOH
Mobile phase B: 150 mM NaOH + 500 mM sodium acetate Detection: Electrochemical detector Sample injection volume: 30 μL
Delivery rate 1.00mL / min

(Ion analysis)
HPLC system: Shimadzu ion chromatogram dual system column cation: Shim-pack IC-C3 100mm × 4.6mm.ID
Column anion: Shim-pack IC-A1 100mm × 4.6mm.ID
Mobile phase cation: 2.5 mM oxalic acid mobile phase anion: 1.2 mM potassium hydrogen phthalate / acetonitrile = 95/5
Sample injection volume: 1000 μL
Liquid feed rate: Cation 0.8mL / min Liquid feed rate: Anion 1.5mL / min

(Viscosity analysis)
The viscosity of the tea extract before enzyme treatment was measured using VISCOMETER TVB-10 (manufactured by Toki Sangyo Co., Ltd.).

(Brix measurement)
For the tea extract before the enzyme treatment, Brix was measured using ATAGO RX-5000 (manufactured by Atago Co., Ltd.).

Example 1
4000 ml of Tearfuran 30E solution obtained by dissolving Tearfuran 30E (tea extract manufactured by ITO EN Co., Ltd .: TF30E) in ion-exchanged water at a concentration of 1.85% by mass on a glass column having an inner diameter of 3 cm and a height of 50 cm (Tosoh Corporation) (Product: HW40EC) was passed through a resin tower packed with 300 mL at SV = 7, and when the Brix at the column outlet reached 0.5%, recovery of the resin passage liquid was started. Subsequently, 300 mL of water was passed through, and the recovery was stopped simultaneously with the end of the water pass, thereby obtaining a HW40EC passing solution.
4300 mL of the obtained HW40EC passage solution was passed through a resin column in which 250 mL of Sepabead SP207 (Mitsubishi Chemical Corporation: SP207) was packed in a glass column having an inner diameter of 3 cm and a height of 50 cm at SV = 7. When the Brix reaches 0.2%, the resin passage liquid starts to be collected, and after passing through the HW40EC passage liquid, 500 mL of water is passed, and the collection is stopped simultaneously with the end of the water passage, and the SP207 passage liquid is removed. Obtained (catechin content less than 1% by mass, caffeine content less than 1%).

The obtained SP207 passage solution was concentrated under reduced pressure, and 100 mL (Brix24.1) of this concentrated SP207 passage solution was added to Inulinase (Smizyme INS Shin Nippon Chemical Industry Co., Ltd., Inulinase activity 2,000 Units / g). A solution in which 5 mg was dissolved in water was added, and an enzyme reaction was performed at 55 ° C. to 65 ° C. for 60 minutes. At this time, the mixture was lightly stirred after the enzyme was added and then allowed to stand.
Next, the enzyme-reacted solution was heated to 95 ° C. to deactivate the enzyme, and then cooled to room temperature.

53 mL of the enzyme-treated solution thus obtained was packed in a glass column having an inner diameter of 3 cm and a height of 50 cm and 212 mL of Sepabead SP207 (manufactured by Mitsubishi Chemical Corporation: SP207) filled with a resin height of 30 cm. The solution was passed at SV = 4 (14.13 mL / min), and when the Brix at the column outlet reached 0.2%, collection of the resin-passed solution was started, and after passing the enzyme-treated solution, water was added. About 650 mL of liquid was passed through, the discharged liquid for 1 bed at the start of recovery was discarded, and the passed liquid for 3 beds was recovered after discarding.
The recovered liquid (theanine fraction) thus recovered was concentrated under reduced pressure and dried to obtain 3 g of a theanine-containing composition.

(Example 2)
In Example 1, an inulinase (SIGMA, inulinase activity: 25,000 Unit / g) was used, and the SP207 passage solution obtained by concentrating the SP207 passage solution under reduced pressure was added to 100 mL (Brix24.1) of the SP207 passage solution. About 3 g of the theanine-containing composition was obtained in the same manner as in Example 1 except that the dissolved solution was added and the enzyme reaction was performed at 37 ° C. for 60 minutes.

(Comparative Example 1)
In Example 1, 7 g of a theanine-containing composition was obtained in the same manner as in Example 1 except that the inulinase treatment was not performed. That is, the obtained SP207 passage liquid was concentrated under reduced pressure, and 53 mL of this concentrated SP207 passage liquid (Brix24.1) was placed on a glass column having an inner diameter of 3 cm and a height of 50 cm, and Sepa beads SP207 (manufactured by Mitsubishi Chemical Corporation: SP207). Was passed through a resin tower having a resin height of 30 cm and SV = 4, and the theanine-containing composition was obtained in the same manner as in Example 1 except for that point.

  Table 2 shows the Brix and viscosity of the tea extract after vacuum concentration obtained in Examples 1 and 2 and Comparative Example 1, and the amount of each component of the theanine-containing composition.

  By inulinase treatment, the viscosity was greatly reduced and the amount of monosaccharides was greatly increased. This is because disaccharides and polysaccharides were decomposed by inulinase treatment. Moreover, it was confirmed that the amount of theanine does not change even when inulinase treatment is performed, that is, it does not decompose.

(Comparison of chromatographic separation efficiency by enzyme treatment)
For Examples 1 and 2 and Comparative Example 1, the enzyme-treated liquid obtained by inulinase treatment (for Comparative Example 1, the tea extract after concentration under reduced pressure) was passed at a flow rate SV = 4, and then 0 .25bed fractions were taken and analyzed.

  As a result, it was confirmed that Example 1 and Example 2 subjected to inulinase treatment were improved in separation behavior of each component as compared with Comparative Example 1. That is, it was confirmed that the separation efficiency between theanine and theogarin and other contaminating components can be increased by performing an enzyme treatment with inulinase.

(Comparative Example 2)
2000 mL of ethyl acetate was added to 2000 mL of theafuran 30E solution in which Aflan 30E (tea extract manufactured by ITO EN Co., Ltd .: TF30E) was dissolved in ion exchange water at a concentration of 5% by mass, and a water fraction was obtained by liquid-liquid partition extraction.
The obtained water fraction was added with activated carbon in an amount equal to the solid content and 64 g to obtain a tea extract.
68 mL of tea extract (Brix20.2%) obtained by concentrating the tea extract thus obtained under reduced pressure was added to a glass column having an inner diameter of 3 cm and a height of 50 cm with 212 mL of Sepabead SP207 (Mitsubishi Chemical Corporation: SP207). SV = 3 was passed through a resin tower filled to a resin height of 30 cm, and 53 mL was passed after the tea extract was passed. Recovery of the resin passage liquid was started from the time when Brix at the column outlet reached 0.2%, and the discharged liquid corresponding to 1 bed at the start of recovery was discarded.
The recovered solution (theanine fraction) thus recovered was concentrated under reduced pressure and dried to obtain 3 g of a powdered theanine-containing composition.

  As a result, in Comparative Example 2, it was found that a theanine-containing composition having a theanine content of 30% by mass or more could not be obtained.

  Also in Comparative Example 2, after passing at a flow rate of SV = 3, a fraction per 0.25 bed was taken and analyzed to examine theanine separation behavior.

The separation behavior of theanine was analyzed for Examples 1 and 2 and Comparative Example 2.
As a result, the theanine elution rate of Comparative Example 2 was worse than that of the Example. The fractions at which theanine began to elute were substantially the same, but it was confirmed that they were largely displaced backward. This is considered to be because the separation efficiency is poor and the elution rate of theanine is poor because there are many unnecessary components contained in the tea extract before separation. Theogarin was analyzed but not detected. This is considered to have been removed in the treatment step before theanine separation.

  In addition, when the test results conducted so far are combined (including the test contents not shown in the present specification), theanine does not completely adsorb to SP207 when separating the theanine-containing component and the contaminated component, but it exhibits a very weak adsorption. Thus, the elution tends to be delayed because it is separated from the contaminating components. By increasing the separation flow rate (SV), extremely weak adsorption is eluted without being separated by the momentum of the water flowing through the resin space. Therefore, it was found that the SV is preferably 4 or less in order to maintain the weakest adsorption of theanine as much as possible by reducing the flow rate. From this point of view, it has been found that it is more preferably 3 to 1, and more preferably 1.5 to 1.

(Purified product result)
In the separation operation, Fr.5 to Fr.16 which are theanine and theogarin fractions were collected and used as purified products.

  As a result of the purified product, it was confirmed that the purity of theanine and theogalin was increased by inulinase treatment.

Claims (7)

  A theanine-containing composition comprising 30% by mass or more of theanine and 5% by mass or less of potassium.   The theanine-containing composition according to claim 1, wherein the theanine content is 30 to 65% by mass and the theogarin content is 10 to 30% by mass.   The theanine content according to claim 1 or 2, wherein both the catechin content and the caffeine content are less than 1% by mass, and the balance is a tea extract component other than theanine, theogarin, catechin, caffeine and potassium. Composition.   The theanine-containing composition according to any one of claims 1 to 3, wherein the total amount of glucose and fructose is 5% by mass or less.   The theanine-containing composition according to any one of claims 1 to 4, wherein the total amount of sucrose is 1% by mass or less.   Enzyme treatment of green tea extract is performed using inulinase to obtain an enzyme-treated liquid, and the enzyme-treated liquid is separated into a theanine-containing fraction and other contaminated fractions by column chromatography. A method for producing a theanine-containing composition, wherein   The method for producing a theanine-containing composition according to claim 6, wherein a treatment for removing catechin and caffeine from the green tea extract is performed before the enzyme treatment of the green tea extract using inulinase.

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