JPH026499A - Production of polyphenols - Google Patents

Abstract

PURPOSE:To easily obtain the subject compound having antibacterial and antitumor actions, etc., in high efficiency by passing an extracted liquid of tea through an ultrafiltration membrane having a specific fractionation molecu lar weight. CONSTITUTION:The whole leaf and stem of tea or a part of raw or dry and non-fermented tea, etc., is extracted preferably with hot water or hydrated organic solvent such as acetone. The extract is passed through an ultrafiltration membrane having a fractionation molecular weight of 6,000-100,000, concentrated and dried to obtain the powder of objective polyphenols having a purity of >=30%. The purity of the product can be further improved by the adsorption separation process using an adsorbent such as an organic or inorganic adsorbent or activated carbon.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing polyphenols. Specifically, the present invention relates to a method for producing polyphenols. Specifically, the present invention relates to a method for producing polyphenols. Concerning how to manufacture well.

[Conventional technology]

Various legends have been passed down since ancient times regarding the physiological activities of tea components, and in recent years the relationship between these components and medicinal effects has been clarified. In particular, regarding the physiological activities of tea polyphenols, -C has been reported to have antioxidant, antitumor, and antibacterial effects.

Several methods for producing polyphenols from tea have also been reported6.
Lete 'v' 7. J (time opening I!/? 130-1
3780.

Tokikai Sho 6l-130285).

However, all of these methods use three or more types of organic solvents, are complicated to operate, and are not economically preferable.

[Problem that the invention seeks to solve]

In order to effectively utilize tea polyphenols, it is necessary to overcome the drawbacks of the conventional production methods described above. In other words, there is a need for a method that is easy to operate, easy to use, and can be produced efficiently on an industrial scale.

The present invention uses tea extract with a molecular weight cut-off of 6,000 to io.
This is a method for producing polyphenols, which is characterized in that the polyphenols are passed through an ultrafiltration membrane that is o, ooo.

The term "tea" as used in the present invention refers to unfermented products, partially fermented products, and completely fermented products of fresh or dried tea leaves, wood, roots, etc., such as leaves, xylem, roots, etc. or mixtures thereof can be used.

To obtain tea extract, d1! In addition to water, preferably boiling water, an organic solvent can also be used. Examples of organic solvents include acetone and alcohol, which are preferably used in a water-containing state.

The extraction method is preferably a multi-stage countercurrent extraction method, but is not particularly limited.

Next, the extract containing polyphenols is passed through an ultrafiltration membrane. The ultrafiltration membrane used has a fraction of 1 to 6 molecules.
, OOO~100,000 Nomo c7) When the suitable 0 cut-off molecular weight is smaller than a, ooo, the passage speed of the solution containing the extracted active ingredient becomes slow, resulting in poor workability and economic efficiency. In addition, if the molecular weight cutoff exceeds 100,000, components that need to be removed will also enter the passing liquid, which is undesirable.The material and shape of the membrane are not particularly limited, and are usually commercially available. Is there a limit? Filtration membranes can be used.

The liquid passing through the ultrafiltration membrane is dried using the usual e-kon1 drying method.
By distilling off the solvent, the desired purified polyphenol powder with a purity of 30% or more can be obtained. In order to further increase the purity, a conventional adsorption separation method using an adsorbent that selectively adsorbs polyphenols is used. The target can be easily achieved by methods using carbohydrate-based flocculants, protein-based flocculants, hydrophobic resins, etc.

That is, according to the present invention, although there are some imperfections in extraction conditions and operations, purified polyphenols with a purity of 30% or more can be easily obtained, and furthermore, by combining with adsorption separation, polyphenols with a purity of 60% or more can be easily obtained. Purity can be increased with L.

[Effect]

The usefulness of the present invention will be explained in detail using test examples.

Test Example: 10 kg of Sencha was filled into 5 cylinders, 2 kg per cylinder, and semi-countercurrent continuous multi-stage extraction was carried out by flowing hot water from the first tube and sending the extracted liquid to the 2N container. After extraction, collect 2,000 mj of the initial liquid (3 to 5 cylinders) for a total of 6,
000mff1 was obtained, and this was allowed to cool and was used as a sample solution. The obtained sample liquid was divided into seven parts, each of which was passed through ultrafiltration membranes with different fractionated molecules L1. The physical properties and properties of the passed liquid were tested. The results are shown in Table 1. The solid content was expressed as the weight after drying in 100 mff1 of the ultra-F membrane-passing liquid, and the purity was expressed as a percentage of the polyphenols in the solid content.

For quantitative determination of polyphenols, the degree of coloration is 0, measured by the official tannin analysis method.
Observation was made visually under white light. The numbers in the table are 3 for the exam.
Shows the average value obtained twice.

From the results above in Table 1, fractionated molecules IUl: 1, OOO1
It can be seen that at 3°000, the polyphenol recovery rate is poor. Moreover, with a membrane with a molecular weight cut off of 1.000.3,000, the processing time for the same amount of liquid increases, which is economically advantageous; Although the condition was good, the degree of coloration (dark blue coloration) was large and the contamination of colored substances was observed.

From this, the optimal molecular weight cutoff for ultrafiltration membranes is 6.0.
It can be said that the range is from 00 to ioo, ooo.

FIG. 1 shows the HPLC pattern of a liquid that passed through a membrane with a molecular weight cutoff of a, ooo. In addition, Figure 2 shows HPLC before processing.
It's a pattern. The conditions for HPLC are 1. :
OD S (4, 6<lr x 150), 1
1 Motion phase: water: DMF niacetonitrile = 85:13:2
゜Flow velocity: 0.5mj! /mi 11, chip speed: 2゜5mm/min, zumble amount: 5μ! I went there.

Table 2 shows the results of a comparison between the present invention and the conventional purification method using an organic solvent.

As shown in Table 2゜=J-Nawara''-fat, it is clear from the comparison between operations ① and ② that by carrying out the operation of the present invention, the purity of polyphenols is improved and the color tone is also improved. Ru. A similar effect was observed by comparing ■ and ■, and it was also confirmed that the appearance of an intermediate layer between the aqueous layer and ethyl acetate, which conventionally caused quality deterioration during operation, was drastically reduced, making separation easier. .

Furthermore, by using the method of the present invention, turbidity and colored substances are removed during purification using an adsorption resin or the like, so it may be possible to increase the resin service life and improve the purity.

The present invention will be explained in more detail with reference to Examples below.

(Example 1) 200 g of Sencha was extracted with 85° C. hot water for 30 minutes while stirring, and the tea confectionery was removed by filtration to obtain 3400 m of extract liquid. This liquid was filtered using an ultrafiltration device (manufactured by DDS Co., Ltd., Membrane Quib GR-81PP, molecular weight cut off 6,000). OQOmj: was obtained. e Add 1,000% water to the condensation residue.
0 mJ2 was added and the same operation was carried out to obtain 1,200 ml of permeate. Combine both liquids and use a reverse osmosis membrane (manufactured by DDS, Membrane Yu/f).
The mixture was concentrated to 20 Qmf using HC-50) and lyophilized to obtain 48.6 g of purified polyphenols with a purity of 35%.

(Example 2) 200g of autumn powder was filled into 10 cylinders at 20g per container, hot water was poured from the first cylinder, and the extracted liquid was extracted in a semi-countercurrent continuous multi-stage system using each vessel in the second cylinder. After extraction, the initial flow from the fifth cylinder is 50mj! Separate each sample (5 to 10 tubes) and make a total of 3
00mj! I got it. Is this liquid limited? A filtrate (280 mff1) was obtained using a filtration device (manufactured by Millibore, membrane type PT, fractionated molecules ito, ooo). 180ml of water to the concentrated residue
Add Q and repeat the same operation to obtain F solution L80mffi. Combine both solutions and absorb n resin (Duolite S-876,
Column packed with Sumitomo Chemical Co., Ltd. (5,0φ x 25c)
Pour into m) and absorb.2. After washing n1 with deionized water of OQOmj2, it was eluted with 800 mJ2 of a 50%:I-tanol solution, and the ethanol was distilled off by 4 condensations under reduced pressure to obtain a concentrated aqueous solution, which was then lyophilized by a conventional method to obtain a polyphenol with a purity of 70%. 21.4 g of purified product was obtained.

〔Effect of the invention〕

According to the present invention, tea polyphenols can be produced continuously and economically in large quantities depending on the raw materials. This is an extremely practical method.

Therefore, the present invention can contribute to the chemical, biochemical, physiological, and pharmaceutical utilization of tea polyphenols, which in turn can contribute to expanding tea consumption and stabilizing production, and has two industrial effects. It is immeasurable.

[Brief explanation of the drawing]

Figure 1 shows the HPLC pattern of the -U゛ liquid that passed through the ultrafiltration membrane with fractionated molecules 11:G,000, and Figure 2 shows the
The HPLC pattern of the untreated liquid is shown. Special r "Applicant Taiyo Kagaku Co., Ltd.

Claims (1)

[Claims] A method for producing polyphenols, which comprises passing a tea extract through an ultrafiltration membrane having a molecular weight cutoff of 6,000 to 100,000.