JP5070361B1 - Method for producing solder GABA extract - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a production method capable of efficiently obtaining a GABA extract without extracting a water-soluble viscous polysaccharide, and obtaining an GABA extract by fractionating an anthocyanin dye and GABA.
SOLUTION: The dried solder leaves are dried, or the obtained dried product is directly or pulverized, provided with an aqueous solution of 50-80% ethanol, an extraction residue containing chlorophyll, GABA and anthocyanin pigment extracted ethanol Separated into aqueous solutions, and collected and removed ethanol from the obtained aqueous ethanol solution containing GABA and anthocyanin dyes to precipitate and remove chlorophyll, and obtain a concentrated solution in which GABA and anthocyanin dyes are concentrated. The obtained concentrated solution is applied to an adsorbent column having a function of adsorbing hydrophobic components to adsorb an anthocyanin dye, and a passing solution is obtained as a GABA extract.
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Description

  The present invention relates to a method for producing a GABA extract from handama leaves.

  Solderama is also known as Kinkiso or Suizinina, and is often eaten as a long-lived meal in Amami Oshima. Solderama is known to have health maintenance functions such as hypertension suppression, antioxidant ability, and anticancer ability. In addition, it is known that solders contain anthocyanin pigments, chlorophyll, GABA, and viscous polysaccharides [Japanese Patent Laid-Open No. 2006-117484 (Patent Document 1), Japanese Patent Laid-Open No. 2007-289057 (Patent Patents). Document 2), Japanese Patent No. 4113918 (Patent Document 3)].

  Because solder is also vulnerable to cold, it can't be harvested in winter. Therefore, a method for efficiently extracting GABA from a solder raw material and producing a GABA extract capable of effectively using GABA from the solder throughout the year is desired.

  Conventionally, there is known a method of extracting hot water by hot water extraction by hot water extraction, or by hot water extraction after heat treatment and storage by freeze-drying. Both saccharides started to dissolve, which was an obstacle to the separation of active ingredients.

  Japanese Patent No. 4113918 (Patent Document 3) discloses a dry solder obtained by steam heating a leaf of solder with a steam heating temperature of 85 to 110 ° C. and a steam heating time of 3 to 8 minutes and then drying with hot air. Is extracted with hot water, or the extract is pulverized to produce a dye extract or powder containing an anthocyanin dye.

  In JP2008-17459A (Patent Document 4), after drying the solder, the extract obtained by extraction with water and a hydrophilic organic solvent is directly or concentrated to obtain a concentrated solution or a dried product, Alternatively, it is shown that the extraction solvent is distilled off from the extract and dried to obtain a dried product.

JP 2006-117484 A JP 2007-289057 A Japanese Patent No. 4113918 JP 2008-174459 A

  The pigment extract containing the anthocyanin pigment of Patent Document 3 is heated with steam and then dried with hot air and extracted with hot water. In this method, the dried solder is extracted with hot water. Therefore, the water-soluble viscous polysaccharide is also extracted at the same time, and there is a problem that filtration or centrifugation is extremely difficult to separate the extract from the solid content.

  The extract of Patent Document 4 does not separate anthocyanin pigments from GABA.

  Therefore, the present invention provides a production method for producing a GABA extract, in which the GABA extract can be efficiently obtained without extracting the water-soluble viscous polysaccharide, and the GABA extract is obtained by fractionating anthocyanin pigments and GABA. The task is to do.

  The method for producing an extract containing GABA of the present invention for solving the above-mentioned problems is as follows: (1) drying fresh solder leaves, (2) directly or pulverizing the dried product obtained in the above step, % Ethanol aqueous solution, fractionated into an extraction residue containing chlorophyll and an aqueous ethanol solution containing GABA and anthocyanin pigments extracted, and (3) ethanol containing GABA and anthocyanin pigments obtained in the above step Chlorophyll is precipitated and removed by recovering and removing ethanol from the aqueous solution to obtain a concentrated solution in which GABA and anthocyanin pigments are concentrated. (4) The concentrated solution obtained in the above step is treated with a hydrophobic component. By using an adsorbent column with an adsorption function, the anthocyanin dye is adsorbed and the passing solution is taken as a GABA extract. Characterized in that it.

  According to the method for producing a GABA extract of the present invention, a mixture of GABA and anthocyanin pigment is extracted with a 50 to 80% aqueous ethanol solution into a dried product obtained by drying fresh solder leaves. The leaf water that causes the ethanol concentration to decrease is not affected, and the viscous polysaccharide contained in the solder leaf is not extracted, and the extract becomes a smooth state with low viscosity. Therefore, an ethanol aqueous solution containing GABA and an anthocyanin pigment can be easily separated from a solid content. For example, an aqueous ethanol solution containing GABA and an anthocyanin dye can be obtained by using a Buchner funnel or the like, using a simple paper, by suction filtration or centrifugation to separate and remove the solid content.

  Moreover, since GABA is extracted with 50-80% ethanol aqueous solution in the dried product obtained by drying the fresh solder leaves, the concentration of ethanol does not decrease without transferring water from the solder leaves during the extraction. Ethanol can be easily recovered.

  According to the present invention, an aqueous solution of ethanol containing GABA and anthocyanin dye separated and removed is applied to an adsorbent column having a hydrophobic component adsorbing function to adsorb the anthocyanin dye and pass the GABA solution through. Since it is obtained as an extract, the GABA extract has been subjected to separation and removal of anthocyanin pigments.

  According to the present invention, GABA is extracted with a 50-80% aqueous ethanol solution to a dried product obtained by drying fresh solder leaves, and most of the chlorophyll is transferred to the extraction residue generated during the GABA extraction operation. Furthermore, by recovering and removing ethanol from the ethanol aqueous solution containing GABA and anthocyanin pigment, chlorophyll partially dissolved in the ethanol aqueous solution is precipitated. Can be removed. Therefore, the GABA extract of the present invention has been subjected to chlorophyll separation and removal treatment.

It is a figure which shows the analysis pattern in HPLC of a soldered crude extract. It is a figure which shows the analysis pattern in HPLC of a passage fraction. It is a figure which shows the analysis pattern in HPLC in a HP adsorption | suction fraction.

  The fresh solder leaves are dried by freeze-drying, reduced-pressure hot-air drying, or hot-air drying. The dried product can be crushed and stored at room temperature. To the pulverized dry solder leaves, 50-80% ethanol aqueous solution, preferably 55-75% ethanol aqueous solution, more preferably 60-70% ethanol aqueous solution is added at room temperature and stirred to extract GABA and anthocyanin pigment. If the concentration of the aqueous ethanol solution is less than 50%, viscous polysaccharides contained in the solder leaves will be extracted, and filtration or centrifugation will be difficult, which is inconvenient for obtaining an extract. It is. If the alcohol concentration exceeds 80%, the cost increases, which is not preferable from an economic viewpoint.

  The extract and solid content extracted with an aqueous ethanol solution are separated by filtration or centrifugal separation, and the solid content is separated and removed, and the extract is collected. At this time, since lyophilized solderama leaves are used as raw materials, there is no water contained in large amounts in the fresh leaves, so the ethanol concentration of the aqueous ethanol solution does not decrease. Therefore, there is an advantage that the water-soluble viscous polysaccharide contained in the solder leaf can be stably extracted without being extracted. Further, since the viscous polysaccharide is not extracted, the viscosity of the extract does not increase, and therefore the extract can be obtained very simply by filtration or centrifugation.

  Add 50-80% ethanol aqueous solution, preferably 55-75% ethanol aqueous solution, more preferably 60-70% ethanol aqueous solution to the extraction residue, and stir to extract and recover the anthocyanin pigment and GABA from the dried leaves. Thus, the recovery rate can be increased. Therefore, an anthocyanin pigment and GABA can be efficiently extracted with a small amount of solvent using a large amount of freeze-dried leaves.

  Next, ethanol is recovered and removed under reduced pressure (for example, using a rotary evaporator). At the time of this ethanol removal, chlorophyll, a contaminant, precipitates with a decrease in the ethanol concentration, which is separated and removed. Next, a small amount of water is added and concentration under reduced pressure is repeated to recover and remove ethanol, for example, by distilling off, and at the same time, chlorophyll that is contaminated is separated and removed again. The remaining aqueous solution is slightly acidic, red and transparent, and an aqueous solution containing a clean anthocyanin dye and GABA is obtained.

  Next, the aqueous solution containing the anthocyanin dye and GABA obtained in the above step is applied to an adsorbent column having a hydrophobic component adsorption function to adsorb the anthocyanin dye that is a hydrophobic component, while obtaining a flow-through fraction. . GABA is eluted in the flow-through fraction. An aqueous solution that has been washed and washed with a sufficient amount of water is added to the flow-through fraction.

As the adsorbent column having the hydrophobic component adsorption function, an adsorbent column packed with a synthetic adsorbent having a hydrophobic component adsorption function can be used. Examples of adsorbents having a function of adsorbing hydrophobic components include styrene-divinylbenzene synthetic adsorbents, such as DIAIO manufactured by Mitsubishi Chemical Corporation.
The flow-through fraction in the adsorbent column having the function of adsorbing the hydrophobic component is collected and concentrated with an ion exchange resin according to a conventional method to obtain a concentrated GABA extract.

[Example 1]
GABA extracted solder raw grass was washed with water and freeze-dried, and pulverized with a mill to obtain a solder powder. 2.5 g of the obtained solder powder was added to a 70% ethanol aqueous solution containing 5% acetic acid, and after stirring well, the solid content was separated and removed by centrifuging at 4,500 rpm for 20 minutes. A crude extract was obtained.

  The resulting crude solder extract was concentrated under reduced pressure using an evaporator to remove acetic acid and ethanol to obtain a 5-fold concentrated extract. This was applied to a column (diameter: 40 mm, length: 300 mm) packed with DIAION HP20 (trade name, styrene-divinylbenzene chromatographic separation material) manufactured by Mitsubishi Chemical Corporation, and eluted with distilled water. Obtained. Further, the solvent was switched to a 50% aqueous ethanol solution to obtain an HP adsorption fraction.

  The ratios of the flow-through fraction and the HP adsorption fraction with respect to the crude solder extract were 92.7% and 7.3% (recovery rate 98.2%), respectively. GABA was quantified for these flow-through fractions, HP adsorption fractions, and handama crude extract. For the GABA analysis, HPLC (High Performance Liquid Chromatography, hereinafter simply referred to as “HPLC”) manufactured by JASCO Corporation was used by PICO-TAG method.

  FIG. 1 shows the analysis pattern of the crude solder extract by HPLC, FIG. 2 shows the analysis pattern by HPLC of the pass-through fraction, and FIG. 3 shows the analysis pattern by HPLC of the HP adsorption fraction. As shown in FIG. 1 to FIG. 3, a clear GABA peak was observed in the crude solder extract and the flow-through fraction, but no GABA peak was observed in the HP adsorbed fraction. As a result of HPLC analysis, the GABA content contained in the dried solder is 49.8 mg / 100 g, and column chromatography using DIAION HP20 (trade name, styrene-divinylbenzene chromatographic separation material) manufactured by Mitsubishi Chemical Corporation. It was proved that GABA can be efficiently recovered in the pass-through fraction.

  The GABA analysis results of the freeze-dried leaves of solderama were obtained for the crude extract, the pass-through fraction, and the adsorbed fraction, respectively. Yield, ratio (%), GABA content (mg / 100 g), GABA content (%), (Mg / 100 g) was measured and shown in Table 1.

  The GABA extract obtained by the method for producing a GABA extract of the present invention has been subjected to separation and removal of anthocyanin pigments, viscous polysaccharides, and chlorophyll, and can be used for nutritional foods, pharmaceuticals, and cosmetics.

Claims (3)

(1) Dry handama leaves,
(2) The dried product obtained in the above step is directly or pulverized and separated into an aqueous residue containing 50-80% ethanol aqueous solution and containing chlorophyll-extracted residue and GABA and anthocyanin pigment extracted. And
(3) Precipitating and removing chlorophyll by recovering and removing ethanol from the ethanol aqueous solution containing GABA and anthocyanin dyes obtained in the previous step to obtain a concentrated liquid in which GABA and anthocyanin dyes are concentrated And
(4) The concentrated solution obtained in the above step is subjected to an adsorbent column having a function of adsorbing hydrophobic components to adsorb an anthocyanin dye, and a passing solution is obtained as a GABA extract. A method for producing an extract.   2. The method for producing a GABA extract according to claim 1, wherein the dried dried fresh solder leaves used in the step (1) are dried fresh dried leaves by freeze-drying, reduced-pressure hot-air drying, or hot-air drying. An aqueous ethanol solution is again applied to the extraction residue obtained in the step (2) to transfer the GABA and anthocyanin pigment still remaining in the extraction residue to the aqueous ethanol solution, and chlorophyll, which is a contaminant, is extracted to the extraction residue. Sort as
The GABA extract according to claim 1, wherein the aqueous ethanol solution obtained in the step and the aqueous ethanol solution obtained in the step (2) are mixed, and then the step (3) and the step (4) are performed. how to.

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