Preparation method of theaflavin composite

A theaflavin and complex technology, which is applied in the field of preparation and purification of high-purity theaflavin complex, can solve the problems of high cost, large dead adsorption, low content of theaflavin, etc. The effect of strong miscellaneous ability and wide application range

Inactive Publication Date: 2017-07-25
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since theaflavins have a multi-hydroxyl structure, they are prone to strong adsorption with polyamides, so the requirements for elution solvents are high, the dead adsorption is large, the reuse rate of the resin is low, and the sample amount is limited and the cost is high.
[0006] In addition, due to the low content of theaflavins in black tea, the cost of extracting theaflavins from black tea is too high. Some studies have shown that crude theaflavins can be obtained by enzymatic oxidation reaction, but the material basis of functional activity is high-purity tea. flavins, so it is necessary to study how to prepare high-purity theaflavins quickly, easily, and save energy

Method used

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  • Preparation method of theaflavin composite
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  • Preparation method of theaflavin composite

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Crude theaflavins are green tea polyphenol extracts (catechins>80%, of which epigallocatechin gallate EGCG>40%) are produced by polyphenol oxidase reaction. The total substance content is 4.06% (of which TF1 is 0.67%, TF2A is 1.20%, TF2B is 0.86%, TF3 is 0.88%, and TF4 is 0.45%). According to the ratio of 19g crude theaflavin (containing 770 mg of theaflavin complex) plus 50 mL of 30% volume concentration ethanol aqueous solution, the above crude theaflavin was dissolved in ethanol aqueous solution, and the sample was loaded on the chromatograph equipped with MCI CHP20P Column (5.5cm×30cm), first eluted with 2 BV of 30% ethanol water at a flow rate of 1.0 BV / h, and then eluted with 70% ethanol water at a flow rate of 1.0 BV / h, and collected 70 % volume concentration of the ethanol water eluate, the eluate was concentrated in vacuo at 30°C to recover ethanol; then fully extracted with an equal volume of ethyl acetate, the ester layer was vacuum-dried at 45°C, and ethyl a...

Embodiment 2

[0026] Crude theaflavins are produced from green tea polyphenol extracts by polyphenol oxidase, and the content of theaflavins is 8.65% (of which TF1 is 0.98%, TF2A is 2.30%, TF2B is 2.32%, TF3 is 2.11%, TF4 is 0.93%). According to the ratio of 16 g crude theaflavin (containing 1.38 g of theaflavin complex) plus 40 mL of 40% volume concentration ethanol aqueous solution, the above crude theaflavin was dissolved in ethanol aqueous solution, and the sample was loaded on the chromatograph equipped with MCI CHP20P The column was first eluted with 4 BV 40% volume concentration of ethanol water at a flow rate of 1.0 BV / h, and then 60% volume concentration of ethanol water was eluted at a flow rate of 1.0 BV / h, and the 60% volume concentration of ethanol water was collected. Eluate, concentrate the eluate in vacuum at 30°C to recover ethanol; then fully extract with an equal volume of ethyl acetate, dry the ester layer in vacuum at 45°C, recover ethyl acetate, and dry to obtain high-pu...

Embodiment 3

[0028] The crude product of theaflavins is the commercially available Keemun black tea extract, the content of the theaflavins complex is 7.26% (0.95% for TF1, 1.40% for TF2A, 1.94% for TF2B, 2.18% for TF3, 0.80% for TF4 %). According to the ratio of 15 g of crude theaflavin (containing 1.09 g of theaflavin complex) plus 40 mL of 25% volume concentration of methanol aqueous solution, the above crude theaflavin was dissolved in methanol aqueous solution, and the sample was loaded on a chromatograph equipped with MCI CHP20P The column was first eluted with 2 BV of 25% volume concentration of methanol water at a flow rate of 1.0 BV / h, and then 80% volume concentration of methanol water was eluted at a flow rate of 1.0 BV / h, and the 80% volume concentration of methanol water was collected. Eluate, concentrate the eluate in vacuum at 30°C to recover ethanol; then fully extract with an equal volume of ethyl acetate, dry the ester layer in vacuum at 45°C, recover ethyl acetate, and d...

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Abstract

The invention discloses a preparation method of a high purity theaflavin composite, MCI resin is used for separation of a theaflavin sample without dead adsorption, the recovery rate is close to 100%, part of theaflavin composite with lower high purity can be separated again by column chromatography, repeated utilization degree is high, and no sample is lost. In the prior art, no chromatographic packed column is capable of recovering theaflavins by 100%, so that the MCI chromatographic column is especially suitable for the efficient extraction of the theaflavins. In particular, the method can improve the recovery rate, and meanwhile the purity of the theaflavin composite in a prepared product is 85% or more, even 90% or more.

Description

technical field [0001] The invention belongs to the field of preparation and purification of theaflavin complexes, and in particular relates to a preparation and purification method of high-purity theaflavin complexes. Background technique [0002] Theaflavins are a general term for a class of compounds that are easily soluble in ethyl acetate and have a benzotropolone structure. They are formed by oxidation of catechins and are important components that determine the color, aroma, and quality of black tea. , there are 22 components of theaflavins whose structures have been clarified, including theaflavins (theaflavin, TF1), theaflavins-3-gallate (theaflavins-3-gallate, TF2A), theaflavins-3′ - theaflavins-3′-gallate (TF2B), theaflavins-3,3′-digallate (TF3) and epitheaflavins-3-gallate (TF4 ) is the main component. Theaflavins are the main components of black tea, known as the "soft gold" in tea, with high safety. Theaflavins also have a wide range of physiological activit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 王冬梅叶琼仙周盈利
Owner SUN YAT SEN UNIV
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