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Method for preparing epigallocatechin-3-gallate by resin adsorption method

A technology of epigallocatechin and gallate, which is applied in the field of natural product production, can solve the problems of small HPLC process, affecting product quality, and low product purity, so as to shorten the process cycle, reduce production costs, and produce high-quality products. The effect of high purity

Inactive Publication Date: 2009-03-18
JIMEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] A large amount of toxic organic solvent (chloroform) is used in the solvent extraction method, and the solvent residue is difficult to be accepted by the food and pharmaceutical industries; the precipitation method needs to adjust the pH, so that some polyphenols will be destroyed by oxidation, which will affect the product quality; the HPLC method has a small processing capacity , high cost; in addition, modern new separation techniques, such as preparative high-efficiency countercurrent chromatography and supercritical fluid extraction technology, have also been applied to the extraction of EGCG, but they are still in the initial stage
Column chromatography can not only overcome the disadvantages of using a large amount of toxic organic solvents in the solvent extraction method, but also avoid the disadvantages of using a large amount of heavy metal precipitants in the precipitation method. The processing capacity is large, and it is suitable for the industrial separation and preparation of EGCG, but the product purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Dosing: select tea polyphenols with an EGCG content of 67.8% as a raw material, weigh 1.5 g, and dissolve in 1000 mL of 35% ethanol aqueous solution to obtain a dark tea-red solution.

[0027] 2) Ultra-high cross-linked adsorption resin column chromatography: at normal temperature and pressure, pump 1000mL of tea polyphenol solution into the ultra-high cross-linked resin adsorption column, the resin column volume is 60mL (ie 1BV=60mL), the adsorption flow rate 1BV / h, the selected ultra-high cross-linked adsorption resin is styrene-divinylbenzene copolymer, with an average pore size of 85nm and a specific surface area of ​​1000m 2 / g, the average particle size is 0.177mm, and the effluent is collected immediately after the color leaks. After the adsorption is completed, add 60mL (1BV) of 35% ethanol aqueous solution for top washing.

[0028] 3) Macroporous resin adsorption decolorization: at normal temperature and pressure, pump 1000 ml of EGCG collection liquid into ...

Embodiment 2

[0033] 1) Dosing: select tea polyphenols with an EGCG content of 67.8% as a raw material, weigh 2 g, and dissolve with 1000 mL of 35% ethanol aqueous solution to obtain a dark tea-red solution.

[0034] 2) Ultra-high cross-linked adsorption resin column chromatography: at normal temperature and pressure, pump 1000mL of tea polyphenol solution into the ultra-high cross-linked resin adsorption column, the resin column volume is 60mL (ie 1BV=60mL), the adsorption flow rate 1BV / h, the selected ultra-high cross-linked adsorption resin is styrene-divinylbenzene copolymer, with an average pore diameter of 95nm and a specific surface area of ​​1100m 2 / g, the average particle size is 0.3mm, and the effluent starts to be collected when the color leaks. After the adsorption is completed, add 120mL (1BV) of 35% ethanol aqueous solution for top washing.

[0035] 3) Macroporous resin adsorption decolorization: at normal temperature and pressure, pump 1100 ml of EGCG collection liquid into th...

Embodiment 3

[0040] 1) Dosing: select tea polyphenols with an EGCG content of 67.8% as a raw material, weigh 2.5 g, and dissolve with 1000 mL of 35% ethanol aqueous solution to obtain a dark tea-red solution.

[0041] 2) Ultra-high cross-linked adsorption resin column chromatography: at normal temperature and pressure, pump 1000mL of tea polyphenol solution into the ultra-high cross-linked resin adsorption column, the resin column volume is 60mL (ie 1BV=60mL), the adsorption flow rate 1BV / h, the selected ultra-high cross-linked adsorption resin is styrene-divinylbenzene copolymer, the average pore size is 90nm, the specific surface area is 1050m2 / g, and the average particle size is 0.42mm. 200mL (1BV) of 35% ethanol aqueous solution was top-washed, and a total of about 1200mL of the adsorption effluent and the top-wash liquid were collected, which was the EGCG collection liquid.

[0042] 3) Macroporous resin adsorption decolorization: at normal temperature and pressure, pump 1200 ml of EGC...

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Abstract

The invention discloses a method for preparing EGCG by resin absorption method. The method uses tea extract as a raw material and comprises the following steps of: using 35 to 40 percent of ethanol water solution to dissolve the tea extract, applying ultra-high cross-linked resin absorption column on the collection liquid for chromatographic separation so as to remove other catechin components, applying a polar macroporous resin absorption column on the collection liquid for decoloration, performing nanofiltration and concentration, and using a Sephadex LH-20 column for chromatography and further purification, freezing and drying the collection liquid so as to obtain EGCG monomer. The purity of the product is more than 90 percent and the yield rate is over 30 percent. The method has simple process, makes the concentration at a normal temperature, avoids high-temperature oxygenation of the catechin, has nontoxic solvent and high-quality product, and meets the demands of food and pharmacy industries.

Description

technical field [0001] The invention relates to a production method of natural products, in particular to a method for preparing epigallocatechin gallate by using a resin adsorption method, which belongs to the field of deep processing of natural organic chemistry and agricultural products. Background technique [0002] Catechin is an important class of natural active substances in tea. In recent years, with the in-depth research on the chemical structure, physical and chemical properties and biological activities of its components, it is necessary to provide a large amount of high-purity catechin as pharmaceutical raw materials, standard products or biological substances. The precursor substances of synthetic products, the new field puts forward higher requirements for the total catechin content of the product, especially the content of epigallocatechin gallate (EGCG), and the traditional extraction technology and products can no longer meet the needs of development. needs....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62B01D15/08
Inventor 王瑞芳陈发河田标翁凌吴光斌张凌晶
Owner JIMEI UNIV
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