Method for preparing four kinds of theaflavin monomer

A technology of theaflavins and monomers, which is applied in the field of preparing theaflavins monomers, can solve problems such as difficult amplification, inability to be suitable for large-scale industrial production, and separation, and achieve the effect of improving utilization and being suitable for large-scale industrial production

Inactive Publication Date: 2008-06-04
TEA RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There is an existing high-speed countercurrent chromatography to separate theaflavin (TF), theaflavin-3-gallate (TF-3-G) and theaflavin-3'-gallate (TF-3'- G) A mixture of three substances (that is, monoester theaflavin) and theaflavin digallate (TFDG), because theaflavin-3-gallate (TF-3-G) and theaflavin-3'- Gallic acid esters (TF-3'-G) are isomers with the same molecular weight, and the two cannot be separated. What the above method obtains is a mixture of the two rather than a single substance; the injection volume of high-speed countercurrent chromatography It is only suitable for the separation of a small amount of standard products. This method is difficult to scale up and cannot be suitable for large-scale industrial production.

Method used

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  • Method for preparing four kinds of theaflavin monomer
  • Method for preparing four kinds of theaflavin monomer
  • Method for preparing four kinds of theaflavin monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The theaflavin extracts on the market (the total content of the four theaflavins of TF, TF-3-G, TF-3'-G and TFDG is 40%) are used as raw materials. Weigh 2g of theaflavin extract and dissolve it in 20ml of water as the loading solution.

[0027] The polyamide resin with a particle size of 80-100 objects is filled into a test-scale column with a diameter of 20mm and a length of 800mm. The volume of the packed column bed is 180ml. The column is equipped with a heating mantle, and the resin is filled with water, 5% NaOH aqueous solution, and Water, 10% acetic acid aqueous solution, water, 95% ethanol and water are washed to remove various impurities contained.

[0028] The packed column was kept at a constant temperature of 20°C, and the column solution was loaded onto the top of the polyamide resin. At a temperature of 20°C, use a mixed solvent of ethyl acetate:ethanol:acetic acid=6:2:3 to elute various theaflavins from the column at a constant flow rate of 2BV (column b...

Embodiment 2

[0031] The mixed solvent in Example 1 is replaced by methyl isoamyl ketone: ethanol: acetic acid=6: 2: 3, and the operation in Example 1 is repeated to obtain four sections of eluate, after drying, wherein theaflavin ( TF) purity is 97%, theaflavin-3-gallate (TF-3-G) purity is 93%, theaflavin-3'-gallate (TF-3'-G) purity is 96% , Theaflavin digallate (TFDG) purity is 98%.

Embodiment 3

[0033]The theaflavin extracts on the market (the total content of the four theaflavins of TF, TF-3-G, TF-3'-G and TFDG is 60%) are used as raw materials. Weigh 4g of theaflavin extract and dissolve it in 20ml of water as the loading solution.

[0034] The polyamide resin with a particle size of 150-200 objects is filled into a test-scale column with a diameter of 25mm and a length of 600mm. The packed column bed volume is 215ml. The column is equipped with a heating mantle, and the resin is sequentially filled with water, 5% NaOH aqueous solution, Water, 10% acetic acid aqueous solution, water, 95% ethanol and water are washed to remove various impurities contained.

[0035] The packed column was kept at a constant temperature of 40°C, and the column solution was loaded onto the top of the polyamide resin. At a temperature of 40°C, first use a 10BV mixed solvent of ethyl acetate:ethanol:acetic acid=4:1:3 to elute at a constant flow rate of 2BV / hour through the pump, and then ...

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Abstract

The invention discloses a preparation method of theaflavin monomers and solves the problem that theaflavin-3-epicatechol gallate and theaflavin-3'- epicatechol gallate can not be separated in the prior art. The technical proposal of the invention is as follows: theaflavin extract solution first slowly flows through a chromatographic column filled with polyamide materials; the chromatographic column is then eluted with eluting solvent so as to collect four eluents which respectively contain theaflavin, theaflavin-3- epicatechol gallate, theaflavin-3'-epicatechol gallate and theaflavin diagallate monomers, and the eluent is a mixed solvent consisting of ester or ketone, alcohol and organic acid. The four eluents are respectively treated with concentration and four concentrated solutions obtained then are extracted for four extract liquors with organic solvent after the pH value of the solutions is regulated to the neutral and the four extract liquors are then dried to obtain four theaflavin monomers. The invention can separate out four theaflavin monomers at the same time, which significantly improves the utilization rate of the theaflavin extract.

Description

technical field [0001] The invention relates to a method for preparing theaflavin monomer. Background technique [0002] Theaflavins belong to plant phenolic pigments, which have anti-virus, anti-bacterial, anti-oxidation, anti-cancer and other effects. It has good preventive and therapeutic effects on systemic diseases, and is the most effective, most scientifically based, and most promising for development and application among the three major pigments of fermented teas (theaflavins, thearubigins, and theabrownins). compound. So far, 25 theaflavins have been isolated and identified from black tea or catechin oxides, of which 4 have the highest content in black tea, namely theaflavin (TF), theaflavin-3-galloc ester (TF-3-G), theaflavin-3'-gallate (TF-3'-G) and theaflavin digallate (TFDG). As far as the chemical components of different types of theaflavins are concerned, there is a big difference in biological activity, and the biological activity of diester theaflavins (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/04
Inventor 江和源王川丕高晴晴
Owner TEA RES INST CHINESE ACAD OF AGRI SCI
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