JP2000069946A - Extract of bamboo grass and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for obtaining an extract of bamboo grass, containing iron chlorophyllines in high concentration and having green color tone from bamboo leaf by using water solvent. SOLUTION: Bamboo leaf is heat-treated in an aqueous solution of a basic compound and the treated leaf is heat-treated in the aqueous solution of an iron salt and the treated leaf is heat-treated in an aqueous solution of a basic compound to provide an iron chlorophylline compound-containing bamboo extract. The resultant bamboo extract is divided into two parts and precipitate of iron chlorophylline component is obtained by deposition using an acid from either one extract and the precipitate is mixed with the other extract to dissolve the precipitate and the solution is neutralized with an ion exchange resin (II) and the deposited silica is filtered to provide the objective bamboo extract enhanced in iron chlorophylline component concentration.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sasa extract containing chlorophyllins, which is used in pharmaceuticals, quasi-drugs, cosmetics, health foods, etc. because it has various physiologically active functions. It is. More specifically, the present invention contains iron chlorophyllin as a main component, and also contains other physiologically active components such as polysaccharides, lignin, vitamins, and organic acids that are important for living organisms. The present invention relates to a sasa extract used for pharmaceuticals, health foods and the like having a purifying action, an antiallergic action, a cell activating action and the like, and a method for producing the same.

[0002]

2. Description of the Related Art Conventionally, a method for producing an iron chlorophyllin salt has been
For example, acetone, chlorophyll is extracted from raw materials such as tea leaves and silkworm feces using an organic solvent such as methanol, and then the chlorophyll is saponified in a solution in which an alkali metal hydroxide is dissolved in methanol or the like to obtain crude chlorophyllin. Then, hydrochloric acid or the like is added to the crude chlorophyllin to obtain chlorophyllin, which is reacted with ferrous chloride using methanol or the like as a solvent to obtain crude iron chlorophyllin. Then
To this crude iron chlorophyllin is added a solution of an alkali metal hydroxide such as methanol using ether or the like as a solvent, and p
A method is known in which the solvent is distilled off after about H10, and the resultant is washed with ether, hexane or the like to obtain an alkali metal salt of iron chlorophyllin.

In this conventional method, it is indispensable to use an organic solvent for a series of reactions from a raw material such as a plant leaf to the production of an iron chlorophyllin salt. The reason is,
Chlorophyll and chlorophyllin, in which the carboxylic acid in the molecular structure is H-type, are hydrophobic and do not dissolve in water. In addition, the reaction of iron substitution is difficult to proceed in a water solvent, and attack by oxygen and the like. Accordingly, the iron chlorophyllin salt is easily decomposed, and the color tone and stability of the produced iron chlorophyllin salt are deteriorated. However, the method using an organic solvent has a drawback that the production cost is increased due to the cost and danger of the solvent itself.

In order to overcome these disadvantages, various alternatives have been proposed. For example, Kumazasa, gourd leaves and the like are treated in a water-soluble cupric salt solution to replace magnesium, which is the central metal of chlorophyll, with copper, and then heated in a dilute alkaline aqueous solution to produce copper chlorophyllin. After making this an alkali metal salt, a calcium salt is added to produce copper chlorophyllin calcium,
A method of precipitating with hydrochloric acid and converting it to an alkali metal salt with an alkali (Japanese Patent Application Laid-Open No. 57-177064) has been proposed.

Also, a method for obtaining chlorophyll from squeezed fresh vegetable leaves
(Japanese Patent Publication No. 27-2885) has also been proposed,
Since the sasa used in the present invention has a low moisture content and strong leaf quality, it is almost impossible to obtain a squeezed liquid.

Japanese Patent Application Laid-Open No. 50-49328 discloses that chlorophyll obtained from silkworm dung or the like by an extraction method using an organic solvent is saponified and then treated with hydrochloric acid to obtain phytochlorin. A method has been proposed in which an iron complex is formed into an alkali metal salt in the presence of an inhibitor to obtain an alkali metal salt of iron chlorophyllin.

However, a method for obtaining a Sasa extract containing iron chlorophyllins and having a green color tone by directly operating the Sasa leaves in an aqueous solvent is based on the fact that the solvent is water and the chlorophyllin is complexed. Due to various difficulties arising from the fact that the metal is iron, etc., it has not been established yet. In metals that can coordinate to the skeleton of chlorophyllins, iron is not easily complexed, and the reaction rate is even slower in an aqueous solvent. Furthermore, since the sasa used as a raw material in the present invention has a robust foliage, it is almost impossible to form a complex even when heated with an iron compound in an aqueous solvent as it is.

On the other hand, in the case of a copper complex, copper ions are very easily incorporated into the chlorophyllin skeleton as a metal species, and thus can be replaced by directly heating fresh leaves in an aqueous copper salt solution. Furthermore, since the copper complex is much more stable than the iron complex and has a bright and bright green color, it is easy to finally obtain a green extract. On the other hand, when performing a series of reactions in an aqueous solvent to obtain a Sasa extract containing iron-substituted chlorophyllin, in addition to the problem that iron ions are not easily coordinated, such as water Chlorophyllin is unstable in a highly polar solvent, and iron chlorophyllin, which has a weaker greening power than copper chlorophyllin, also has a problem that it has a poor color tone and brown solution.

[0009] This is because even when divalent iron is used at the time of iron complexation, it is easily oxidized to trivalent iron by a solvent and oxygen in the air, and this acts on chlorophyllin to give a clear green color. In addition to not being able to obtain chlorophyllin, other substances contained in sasa leaves also caused browning under the severe reaction conditions for performing chlorophyllin iron complexation of high temperature heating in the presence of iron ions. It is thought to be.

[0010]

DISCLOSURE OF THE INVENTION The present invention provides a sasa extract containing iron chlorophyllins by treating a sasa in accordance with a series of reaction steps using an aqueous solvent to obtain a greenish and stable color tone. It is an object of the present invention to provide a method of directly obtaining from Sasa leaves in a state. Also, by using only water as a solvent, it is possible to provide a method that is safe for both the consumer side and the manufacturing side, does not require equipment associated with the use of an organic solvent, and can be manufactured at a low cost. It is the purpose.

Furthermore, since substances having biologically important functions such as saccharides and lignin which are water-soluble components can be extracted together, recovery from fatigue, promotion of digestive function, blood purification action, antiallergic action are also possible. It is an object of the present invention to widely provide consumers with a chlorophyllin-containing sasa extract having a physiologically active function important to a living body such as a cell activating action.

[0012]

Means for Solving the Problems The present inventors have conducted intensive studies in order to solve the above-mentioned problems, and as a result, after heat-treating sasa leaves in an aqueous solution of a basic compound, When they were reacted with an iron salt, they were found to be easily substituted with iron, and they reached the present invention. The present invention includes the following inventions.

(1) A step of heat-treating the bamboo leaf of Sasa genus in an aqueous solution of a basic compound containing a monovalent strong basic compound, preferably in a concentration of 0.01 to 1 mol / liter, Heat-treating the treated leaves in an aqueous solution of an inorganic iron salt or an organic iron salt to replace the magnesium ion of the central metal of the chlorophyllin compound contained in the sasa leaves with iron ions, A heat treatment of a monovalent strong basic compound in a basic compound aqueous solution adjusted to a concentration of 0.1 to 10 mol / liter to extract an iron chlorophyllin compound. A method for producing a sasa extract containing components.

(2) The process according to (1), wherein an antioxidant or a reducing agent is co-present in the step of substituting the magnesium ion of the central metal of the chlorophyllin compound contained in the sasa leaves with iron ions. A method for producing a Sasa extract containing an iron chlorophyllin component.

(3) In the step of substituting the magnesium ion of the central metal of the chlorophyllin compound contained in the sasa leaves with the iron ion, histidine, tryptophan, lysine, arginine, pyridine, aniline, 3. The method for producing a Sasa extract containing an iron chlorophyllin component according to the above item 1 or 2, wherein an amino acid or an amine compound selected from the group consisting of imidazole and ethylamine is added.

(4) a step of dividing the sasa extract containing the iron chlorophyllin component obtained by the method according to any one of the above items 1 to 3 into two parts, wherein one of the sasa extracts contains an inorganic acid or an organic acid; A step of filtering off the precipitated iron chlorophyllin component, a step of mixing and dissolving the iron chlorophyllin component in the other Sasa extract, a step of neutralizing the Sasa extract from the mixed dissolution step using an ion exchange resin, Filtering a precipitate containing silica as a main component, which is precipitated in the neutralization step, and removing the precipitate by filtration.

(5) A sasa extract containing a high concentration of iron chlorophyllin, produced by the method described in (4).

[0018]

DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, when the leaves of Sasa of the genus Sasa belonging to the genus Bamboo are heat-treated with an aqueous solution of a basic compound, chlorophyll is converted into a chlorophyllin salt by saponification, and the polarity of the molecule itself is increased. Complete iron substitution in water solvent for chlorophyllins by making the highly polar Fe ions added in the process easy to approach and softening the fiber of sasa leaves and the iron salt to easily contact the chlorophyll molecules in the whole leaf. It is considered possible. At this time, the substitution rate can be controlled by changing the concentration of the basic compound or changing the treatment time with the aqueous solution of the basic compound.

The sasa leaf used in the method of the present invention may be either a fresh leaf or a dried leaf, and may be a leaf as it is or a cut state. It may further contain stems. Further, an enzyme treatment and a pulverization treatment may be performed in advance.

In the method of the present invention, as the basic compound,
Potassium hydroxide, sodium hydroxide, lithium hydroxide,
Calcium hydroxide, magnesium hydroxide, sodium carbonate, sodium phosphate, aqueous ammonia, aniline, arginine and the like are used. Among them, sodium hydroxide is most preferable in consideration of hydrolysis efficiency, cost and the like. 0.01 to 1 mol of monovalent strong basic compound as aqueous solution
An aqueous solution containing a concentration of / l is used.

In the heat treatment step in an aqueous solution of a basic compound, which is the first step of the method of the present invention, the concentration of a monovalent strong basic compound is adjusted to 0.01 to 1 part by weight of sasa leaves. 1
The reaction is performed using 3 to 100 parts by weight of an aqueous solution adjusted to mol / l. If the used amount of the basic compound aqueous solution is small, the treatment time is increased and the iron ion substitution in the next step becomes incomplete. Heat treatment in an aqueous solution of a basic compound
The treatment is performed at a temperature of 60 to 100 ° C., but treatment at 100 ° C. is preferable because the treatment time can be shortened. At low temperatures, the processing takes a long time, resulting in the generation of various chlorophyllins. Further, if the heat treatment is continued for a long time at a high concentration of the basic compound, chlorophyllins are eluted, which causes a decrease in yield. The end point of the heat treatment in the basic compound aqueous solution can also be determined by quantifying the amount of chlorophyllin eluted and determining a certain amount of elution as an index.

The iron salt which can be used in the iron ion substitution reaction as the second step of the method of the present invention includes ferrous chloride, ferric chloride, ferrous sulfate, ferric sulfate and ferric acetylacetate. Iron compounds and the like selected from naat, ferric formate, ferric nitrate, ferrous lactate, iron carbonyl and hydrates thereof can be used. The amount of these iron compounds to be used is preferably 1 to 20 mol as Fe per 50 kg of sasa leaves before treatment. If the used amount of the iron compound is small, incomplete iron substitution and deterioration of the color tone after neutralization are caused, and if it is too large, not only the cost is increased, but also a result that iron ions are not completely removed by washing with water is caused. Not preferred.

The substitution reaction can be carried out also with a ferric salt, but the reaction is slower than with a ferrous salt, and the color of the final extract becomes brown. When this ferric salt is used, it can be changed to a ferrous salt by using an antioxidant or a reducing agent.However, it is easier to use a ferrous salt from the beginning. ,preferable.

The temperature at the time of heat treatment with the iron salt is set at the boiling temperature, in order to achieve complete replacement and shortening of the treatment time.
That is, 100 ° C. is preferable. Further, since the substitution reaction does not proceed in a high alkaline region, the pH at this time is 9 or less, preferably 7 or less. When the pH is 3 or less, although the substitution is performed, a strong brown sasa extract is finally obtained. This is considered to be mainly because the sugars in the sasa leaves are browned due to strong acidity. PH at this time
For the adjustment, the above-mentioned basic compound, and inorganic and organic acids described later are used.

Further, by coexisting an antioxidant, a reducing agent and the like at the time of iron complexation, a green stable Sasa extract having a good color tone can be finally obtained. This is considered to be due to the effect of suppressing iron from being oxidized to trivalent as described above, or reducing iron to divalent iron, and also suppressing browning of other substances.

The antioxidants and reducing agents include ascorbic acid, sodium ascorbate, sodium dehydroacetate, propyl gallate, sodium benzoate, tocopherol acetate, tocopherol, dibutylhydroxytoluene, trehalose, erythorbic acid, sodium sulfite, There are sodium sulfate, sodium nitrite, and the like.

The use ratio is preferably 0.05 mol to 20 mol per 50 kg of sasa leaves. If the amount is less than this, a green extract cannot be obtained in the post-process, and if it is more, the cost is increased, and if the action is strong,
It causes decomposition. The treatment time is determined by the amount of sasa leaves, the amount of the basic compound in the treatment with the basic compound aqueous solution, the treatment time, the type of iron salt, the type and amount of the antioxidant and the reducing agent, the treatment temperature, and the like. Usually, it is preferably 20 to 120 minutes under boiling.

Further, by adding an amino acid or an amine compound at the time of iron substitution, it is coordinated with iron molecules of iron chlorophyllin to suppress oxidation of coordinated iron, and finally, a stable green Kumazasa extract having a good color tone is obtained. Can be obtained. Examples of the amino acid or amine compound include histidine, tryptophan, lysine, arginine, pyridine, aniline, imidazole, and an amino acid compound selected from the group consisting of ethylamine. Although it is the reverse of what has been known so far, the phenomenon of inhibiting iron substitution occurs. Therefore, it is desirable to add iron during or at the end of substitution, or to add a very small amount at the beginning. The addition amount is 0.01 mol to 20 mol, preferably 0.1 to 1 mol per 50 kg of sasa leaves.
0 mol.

Further, the oxidation can be further suppressed by performing the process under the condition that oxygen and light are blocked during the entire replacement step, and further under an atmosphere of an inert gas such as nitrogen. At the end of the iron substitution step, water is washed to remove excess iron ions, antioxidants, reducing agents, amino acids, amine compounds, and the like.

As described above, Sasa leaves subjected to iron substitution treatment in an aqueous solvent in the presence of an antioxidant, a reducing agent or an amino acid or an amine compound are then subjected to an extraction step using an aqueous solution of a basic compound. The kind of the basic compound used here may be the same as that used in the above-mentioned heat treatment step in the basic compound aqueous solution. Sodium hydroxide is preferable as in the first step from the viewpoints of shortening of treatment time, cost and the like, and in the case of such a monovalent strong basic compound, 0.1 to 10 parts by weight based on 1 part by weight of the leaf to be treated. 1-20 parts by weight of an aqueous solution of a basic compound having a molar concentration are used. The pH is desirably 12 or more.

The extraction temperature is preferably 100 ° C., which is the boiling temperature, in order to shorten the time. The extraction time should be long enough for the extraction process to be completely achieved,
It is between 30 and 150 minutes. If the treatment time is insufficient, the extraction is incomplete and the yield is reduced. If the treatment time is too large, the viscosity and browning of the finally obtained extract are increased due to oxidation and decomposition.

When the solid-liquid separation is performed after the completion of the extraction, a method such as squeezing filtration using a metal net or a cloth made of a material resistant to alkali can be used. Sasa extract has the property of turning brown when it comes into contact with air, and turning green when closed or shut off from air. Further, when the sasa extract is neutralized to lower the pH to a weak alkalinity, the extract has a characteristic of maintaining a green color even under open conditions. This is probably due to the coordination of oxygen to the iron of iron chlorophyllin, and this is a phenomenon that the affinity changes reversibly with pH. This can also be confirmed from the fact that it becomes alkaline when added with a reducing agent and becomes bright green.

In the present invention, the sasa extract is further divided into two parts, an acid is added to one part to form a precipitate, and the precipitate is formed by centrifugation or the like to form a precipitate part composed of iron chlorophyllins having a strong green color. It can be separated into a strong brown mixed solution in the solution part. Then, by adding the precipitated portion composed of the strongly green iron chlorophyllins to the other portion of the Sasa extract, which has been divided into two, a stronger green solution can be obtained when neutralized in a later step. It is possible to produce a concentrated solution in which the iron chlorophyllin component content is significantly increased compared to the iron chlorophyllin-containing extract obtained from the extraction step using an aqueous alkali solution that is the final step,
This concentrated liquid is also included in the scope of the present invention. The solution remaining after separating the precipitate in the acid precipitation step can be used, for example, as an antibacterial agent.

The iron chlorophyllin-containing extract obtained from the extraction step with the aqueous alkali solution is concentrated by applying another concentration method, that is, a freeze-drying method, a reverse osmosis method, or a heat concentration method, but finally, the color It is very difficult to get a good green concentrated extract. This is probably because the brown component is also concentrated at the same time, so that the brown color of the brown component eventually exceeds the green component.

[0035] In addition, there is an advantage that the concentration of iron chlorophyllin in the extract can be freely set as a product depending on the ratio of adding the precipitated portion composed of the iron chlorophyllin component to the extract of Sasa leaf. Although there is no particular limitation on the concentration of the product extract, it is generally desirable that the concentration be about 0.1% to 2.0% by weight. If the concentration is lower than this range, the concentration of the physiologically active substance is low, and if it is too high, troubles will occur in subsequent steps due to an increase in viscosity and the like.

Other methods for separating iron chlorophyllins include a method by solvent fractionation, a method for obtaining calcium salts, a method using column chromatography, and the like.

The acid used for this acid precipitation is not particularly limited as long as the pH can be made acidic, and either an inorganic acid or an organic acid can be used. For example, hydrochloric acid, sulfuric acid, acetic acid, nitric acid, citric acid, phosphoric acid and the like can be used, but hydrochloric acid is most preferable in consideration of safety, cost, and subsequent steps. However, when an organic acid such as acetic acid is used, the decomposition of iron chlorophyllin hardly occurs, so that use of these organic acids may be suitable in some cases.

The conditions of the acid precipitation step are usually set to 15 ° C., since the lower the temperature, the more easily the sediment is easily separated.
The reaction is performed at a temperature of 10 ° C. or less. The pH at the time of acid precipitation is not particularly limited as long as the pH is in an acidic range. Usually, the reaction is carried out at a pH of 5.0 or less, but if it is too low, the release of Fe is a concern. As a method for separating the generated precipitate,
Since clogging and a decrease in yield occur in the ordinary filtration method,
Centrifugation is preferred. In the acid precipitation step, in the case of a Sasa extract having a low iron substitution rate, decomposition occurs such that iron is released, but in the case of a Sasa extract in which iron is almost completely substituted as in the method of the present invention, There is an advantage that decomposition can be suppressed to an extremely low level.

After the separation, a step of washing the precipitate with water is provided to remove the remaining brown components and to remove the generated salt and chloride ions, thereby preventing salt and potassium chloride from remaining. Is desirable. In order to prevent these substances from being mixed into the final extract, a desalting step may be further provided near the final step. Since the washed precipitate is composed mainly of green, mainly iron chlorophyllin, it can be added to the extract of the Sasa extract to increase the concentration of iron chlorophyllin, etc. The resulting extract can be produced. In the method of dissolving the precipitate component in the extract component, the precipitate component dissolves in an alkaline state, and thus can be dissolved by stirring.
If necessary, dissolution may be assisted using a homogenizer or the like.

Further, since the extract portion not subjected to the acid precipitation also contains a useful liquid component removed by the acid precipitation, the content of the iron chlorophyllin component is increased by the precipitation portion, and the extract solution is contained. The useful liquid component, for example, a physiologically active function such as a saccharide can also be effectively used. Since the color of the final extract is determined by the ratio of the brown component to the green component, by taking such a method, while containing physiologically active components such as saccharides contained in the sasa extract, the appearance of the sasa is good. A green extract that retains the image can be obtained.

The precipitated component obtained from the acid precipitation step may be used by adding to various conventional sasa extracts which have not undergone the iron substitution step, instead of the extract from the alkali extraction step. . In this case, iron chlorophyllin is added to and contained in the components contained in the sasa leaves, so that beverages and the like with enhanced iron chlorophyllin can be produced.

The alkaline extract of sasa leaves containing iron chlorophyllin described above is a slightly viscous liquid having a unique scent, is strongly alkaline, and further contains a large amount of silicate components derived from sasa leaves. (About 1000ppm-50
(00 ppm), it is not suitable for drinking and the like as it is. Therefore, the concentrated alkali extract obtained as described above is suitable for drinking only by neutralizing with various organic acids, inorganic acids, ion exchange resins and the like, and then desilicaizing, and is widely used for pharmaceuticals and quasi-drugs. Sasa extract that can be used for products, cosmetics, health foods, etc.

This neutralization and desilicaization method is disclosed in
For example, a method described in JP-A-97692 can be employed. Specifically, there is a method of neutralizing a sasa extract containing iron chlorophyllin with an organic acid or an inorganic acid, a method of using an ion exchange resin, and the like, and any acid can be used as long as the purpose of use is not impaired. it can. For example,
Since the formation of a salt such as NaCl when hydrochloric acid is used may affect the quality of the final product, a neutralization method using an ion exchange resin that does not involve the formation of such a salt is preferred. As the ion exchange resin, either a strongly acidic or a weakly acidic ion exchange resin can be used, but since the neutralization under mild conditions is possible and the adsorption loss of useful components is small, the weakly acidic ion exchange resin is used. Neutralization using an exchange resin is desirable.

As a neutralization method using an ion-exchange resin, a column method in which an ion-exchange resin is filled in a column and an extraction solution is passed through the column to neutralize the ion-exchange resin, There is a batch method in which an exchange resin is put in, the extract is introduced, and the mixture is stirred and mixed for neutralization, and only the extract is separated and extracted through a net partition or the like. Is also good. The neutralization temperature is preferably around 20 ° C. to 40 ° C. If the temperature is lower than this range, the neutralization reaction takes a long time. Induces precipitation.

By neutralizing the alkaline sasa extract, it turns bright green as described above. This change starts at about pH 9. This neutralized liquid is a slightly viscous liquid that has a scent of sasa and exhibits a green color, depending on the quantitative ratio at the time of extraction and the like.

Next, heating is carried out in order to desilica the neutralized extract. At this time, if the extract is not added with an antioxidant, a reducing agent, an amino acid, or an amine compound at the time of iron substitution, the extract immediately turns brown. Even if the extract is neutralized and left alone at the same temperature, silica precipitation occurs, but it can be accelerated by heating to form a hard gel state that is easily separated. The temperature is from 50 ° C to 100 ° C, preferably around 90 ° C. When the scale is large, uniform heating is achieved by gentle stirring so as not to break the gel. Also, the longer the standing time in the heated state, the better, but in order to avoid decomposition of the components,
About 1 hour is preferable. At this time, iron substitution by an extremely small amount of remaining iron ions additionally occurs.

The component mainly composed of silica thus precipitated can be separated by natural filtration, centrifugation, or the like. However, this precipitate is gel-like, soft, easily clogged, and leaks. Natural filtration is more preferable than a method in which pressure is applied, such as centrifugation, pressurization, or depressurization, because it has features such as easy filtration. Further, a non-woven fabric is preferable as the filter cloth because it is less clogged and easy to remove. This filtration step may be either hot or after cooling. The silica concentration of the extract is adjusted to 100 to 500 by the silica removal treatment.
It is preferably set to ppm.

[0048] The extract which has been desilicaized can be processed into various dosage forms depending on the purpose of use. The liquid can be filled in a container such as a bottle and supplied as a liquid agent through a process such as sterilization.The extract can be further concentrated under reduced pressure,
It may be concentrated by reverse osmosis membrane, freeze-dried, or processed into granules, capsules, tablets and the like.

[0049]

Example 1 (Alkali heat treatment step): Using a stainless steel tank,
82 mL of a 24.5% NaOH aqueous solution was added to 6 L of water, heated and boiled, and 300 g of Sasa was immersed and boiled for 20 minutes. After that, Sasa was taken out and washed well with water. (Iron replacement reaction step): Separately, 6 L of water was boiled, and 3.6 g of ferrous chloride / hydrate and 8.0 g of ascorbic acid were added. The pH was adjusted to 6 with an aqueous solution, and boiling was continued for 60 minutes.
After that, Sasa was taken out and washed well with water. (Alkali extraction process): 24.5% N in 1.5 L of distilled water
150 ml of an aOH aqueous solution was added and heated to boiling, and the sasa obtained from the substitution reaction step was immersed, and boiling was continued for 70 minutes while stirring. Then, the treated leaves were removed from the boiling treatment liquid to obtain 1.3 L of a Sasa extract containing green iron chlorophyllins. (Acid precipitation step): Extract 4 obtained from the alkali extraction step
After cooling 00 ml to around 5 ° C., the pH was adjusted to around 2.5 by adding 25% HCl, and the resulting precipitate was collected by centrifugation and washed with water to obtain 100 g of a precipitate (wet cake). . (Mixing / dissolving step): 260 ml of the Sasa extract obtained from the extracting step was taken, and the precipitate 100 obtained from the acid precipitation step was taken.
g (wet cake) was added and dissolved. (Silica removal step): The solution obtained from the mixing / dissolving step is neutralized using a weakly acidic ion exchange resin (H type), and after neutralization, heated to 88 ° C. to precipitate gelled silicic acid Was filtered off. 200 ml of Sasa extract containing green iron chlorophyllins was obtained.

Example 2 (Alkali heat treatment step): Using a stainless steel tank,
82 mL of a 24.5% NaOH aqueous solution was added to 6 L of water, heated and boiled, and 300 g of Sasa was immersed and boiled for 20 minutes. After that, Sasa was taken out and washed well with water. (Iron replacement reaction step): Separately, after boiling 6 L of water, adding 3.6 g of ferrous chloride / hydrate, immersing the washed sasa obtained from the alkali heat treatment step, and adding an aqueous sodium hydroxide solution After adjusting to pH 6 and boiling for 50 minutes, 7.0 g of histidine was added, and boiling was continued for another 10 minutes. After that, Sasa was taken out and washed well with water. (Alkali extraction process): 24.5% N in 1.5 L of distilled water
An aOH aqueous solution (150 ml) was added, and the mixture was heated and boiled.
Minute boiling was continued. Then, the treated leaves were removed from the boiling treatment liquid to obtain 1.3 L of a Sasa extract containing green iron chlorophyllins. (Acid precipitation step): Alkaline extract 4 obtained from the extraction step
After cooling 00 ml to about 5 ° C., the pH was adjusted to about 2.5 by adding 25% HCl, and the resulting precipitate was collected by centrifugation and washed with water to obtain 100 g of a precipitate (wet cake). (Mixing / dissolving step): 100 g of the precipitate (wet cake) obtained from the acid precipitation step was added to and dissolved in 260 ml of the Sasa extract obtained from the extraction step. (Desilica step): The solution obtained from the mixing / dissolving step is neutralized with a weakly acidic ion exchange resin (H type), and after neutralization, 8
The mixture was heated to 8 ° C., and the precipitated gel silicic acid was removed by filtration. Sasa extract 2 containing green iron chlorophyllins
00 ml was obtained.

Example 3 (Alkali heat treatment step): Using a stainless steel tank,
82 mL of a 24.5% NaOH aqueous solution was added to 6 L of water, heated and boiled, and 300 g of Sasa was immersed and boiled for 20 minutes. After that, Sasa was taken out and washed well with water. (Alkali extraction process): 24.5% N in 1.5 L of distilled water
150 ml of an aOH aqueous solution was added and heated to boiling, and the sasa obtained from the alkali heat treatment step was immersed and the boiling was continued for 70 minutes while stirring. Next, 1.3 L of green sasa extract was obtained by removing the treated leaves from the boiling treatment liquid. (Mixing / dissolving step): 100 g of the precipitate (wet cake) obtained from the acid precipitation step in the method of Example 1 was added to and dissolved in 260 ml of the Sasa extract obtained from the alkali extraction step. (De-silica step): The solution obtained from the mixing / dissolving step is neutralized with a weakly acidic ion exchange resin (H type), and after the neutralization, heated to 88 ° C. to precipitate the gelled silica. It was removed by filtration. 200 ml of Sasa extract containing green iron chlorophyllin was obtained.

The Sasa extract containing iron chlorophyllin obtained in Examples 1 and 2 described above has a significantly increased iron chlorophyllin content as compared with the conventional Sasa extract containing iron chlorophyllin. The color stability is improved and the color tone is green, which is the same as the conventional product. The evaluation test result as a beverage by 10 panelists is superior to the conventional product as shown in Table 1 in comparison with the conventional product. Or no difference. The iron chlorophyllin-containing precipitate was dissolved in the extract obtained in Example 3, that is, the alkali-heat-treated leaves, and directly into the extract obtained by alkali extraction without performing the iron replacement treatment. It was neutralized with an ion exchange resin (H type), heated to 88 ° C. after the neutralization, and the gel gel silicic acid precipitated was removed by filtration.

[0053]

[Table 1]

[0054]

According to the present invention, iron substitution of chlorophylls in sasa leaves with robust foliage is completely achieved by using an aqueous solvent throughout the entire process, and easily extracted as iron chlorophyllin. And the chlorophyllin component content is dramatically increased while maintaining the green color tone of the Sasa extract, providing a Sasa extract having high stability over time. Is done.

Further, the method of the present invention does not use expensive and dangerous organic solvents, so it is safe for both the production side and the consumer side. Since it contains extracted other substances, in addition to the physiologically active function of iron chlorophyllin, it is possible to provide an extract having an excellent physiologically active function including a physiologically active substance such as a saccharide, thereby broadly promoting health. Medicines, quasi-drugs, cosmetics, etc. useful for

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) // A61K 35/78 C07F 15/02 C07F 15/02 A23L 2/00 FF term (Reference) 4B017 LC03 LE10 LG15 LK01 LK06 LK08 LK14 LL07 LL09 LP01 LP08 4B018 LB08 LB10 LE01 LE02 LE05 MD01 MD06 MD09 MD18 MD19 MD61 ME07 ME14 MF01 MF04 MF11 4C086 AA01 AA04 CB04 MA01 MA04 MA16 MA52 NA03 ZB13 CAB22 CAB22 CAB CA8 MA52 NA03 ZB13 ZB22 ZC21 4H050 AA02 AA03 AB10 AB12 AB20 AD15 AD17 BB31 WB14 WB21

Claims (5)

[Claims] 1. A step of heat-treating a bamboo leaf of Sasa genus in an aqueous solution of a basic compound, wherein said heat-treated leaf is heat-treated in an aqueous solution of an inorganic iron salt and / or an organic iron salt. Substituting the central metal of the chlorophyllin compound contained therein with iron ions, and heating the treated leaves from the substitution step in an aqueous solution of a basic compound to extract a component containing the iron chlorophyllin compound. A method for producing a sasa extract containing an iron chlorophyllin component. 2. In the step of substituting a central metal of the chlorophyllin compound contained in the sasa leaves with iron ions,
Characterized by coexisting an antioxidant or a reducing agent,
A method for producing a sasa extract containing the iron chlorophyllin component according to claim 1. 3. The step of substituting a central metal of a chlorophyllin compound contained in the sasa leaves with an iron ion,
The iron chlorophyllin component according to claim 1 or 2, wherein a compound selected from the group consisting of histidine, tryptophan, lysine, arginine, pyridine, aniline, imidazole and ethylamine is added during or at the end of the step. A method for producing a sasa extract liquid. 4. A step of dividing a sasa extract obtained by the method according to claim 1 into two parts, an iron chlorophyllin component precipitated by adding an inorganic acid or an organic acid to one of the sasa extract. Filtration, the step of mixing and dissolving the precipitated iron chlorophyllin component in the other Sasa extract, the step of neutralizing the Sasa extract from the mixed dissolution step using an ion exchange resin, and the step of precipitation in the neutralization step. A step of filtering and removing a precipitate containing silica as a main component, the method comprising producing an iron chlorophyllin component. 5. A sasa extract containing a high concentration of iron chlorophyllin, produced by the method according to claim 4.